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Sample records for solid phase micro

  1. Solid phase micro-extraction in environmental atmosphere

    Tao Ping; Wei Lifan; Tan Yun

    2002-01-01

    Solid phase micro-extraction (SPME) is an advanced technique of sample pretreatment in environmental atmosphere analysis, i.e., a sampling method of extracting volatile organic compounds from environmental gas. According to the primary survey on the theory and application of SPME, a suitable extraction tip, i.e., a coated fused silica fiber, is selected to construct a SPME apparatus. This SPME apparatus is used to extract volatile organic compounds from environmental atmosphere and a qualitative detection is conducted in gas chromatography-mass spectrometer system. Good experimental results are obtained

  2. Improved detection limits for phthalates by selective solid-phase micro-extraction

    Zia, Asif I.; Afsarimanesh, Nasrin; Xie, Li; Nag, Anindya; Al-Bahadly, I. H.; Yu, P. L.; Kosel, Jü rgen

    2016-01-01

    Presented research reports on an improved method and enhanced limits of detection for phthalates; a hazardous additive used in the production of plastics by solid-phase micro-extraction (SPME) polymer in comparison to molecularly imprinted solid

  3. Solid-phase micro-extraction in bioanalysis, exemplified by lidocaine determination

    de Jong, GJ; Koster, EHM

    2000-01-01

    Solid-phase micro-extraction (SPME) is a never sample preparation technique that can be used for gaseous, liquid or solid samples in conjunction with GC, HPLC or CE (e.g. [1]). The use of SPME for the analysis of drugs in biofluids is also becoming popular (e.g. [2]). The principle is that a fused

  4. Micro versus macro solid phase extraction for monitoring water contaminants: a preliminary study using trihalomethanes.

    Alexandrou, Lydon D; Spencer, Michelle J S; Morrison, Paul D; Meehan, Barry J; Jones, Oliver A H

    2015-04-15

    Solid phase extraction is one of the most commonly used pre-concentration and cleanup steps in environmental science. However, traditional methods need electrically powered pumps, can use large volumes of solvent (if multiple samples are run), and require several hours to filter a sample. Additionally, if the cartridge is open to the air volatile compounds may be lost and sample integrity compromised. In contrast, micro cartridge based solid phase extraction can be completed in less than 2 min by hand, uses only microlitres of solvent and provides comparable concentration factors to established methods. It is also an enclosed system so volatile components are not lost. The sample can also be eluted directly into a detector (e.g. a mass spectrometer) if required. However, the technology is new and has not been much used for environmental analysis. In this study we compare traditional (macro) and the new micro solid phase extraction for the analysis of four common volatile trihalomethanes (trichloromethane, bromodichloromethane, dibromochloromethane and tribromomethane). The results demonstrate that micro solid phase extraction is faster and cheaper than traditional methods with similar recovery rates for the target compounds. This method shows potential for further development in a range of applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. VOLATILE COMPOUNDS OF LITHRAEA CAUSTICA (LITRE) DETERMINATED BY SOLID PHASE MICRO-EXTRACTION (SPME)

    GARBARINO, JUAN A; SALVATORE, GIUSEPPE; PIVANOVO, MARISA; CHAMY, MARÍA CRISTINA; NICOLETTI, MARCELLO; DE IOANNES, ALFREDO

    2002-01-01

    The head space of the aerial parts of Lithraea caustica was analyzed by Solid Phase Micro-Extraction (SPME) technique, obtaining as main volatile compounds the monoterpenes, myrcene, a -pinene, , p-cymene and limonene, as well as the sesquiterpene caryophylene. De las partes áereas de Lithraea caustica y usando la técnica de Micro-Extracción en Fase Sólida (MEFS), fueron identificados y cuantificados los principales compuestos volátiles: los monoterpenos, mirceno, a -pineno, p-cimeno y lim...

  6. Micro solid-phase radioimmunoassay for detection of herpesvirus type-specific antibody: specificity and sensitivity

    Adler-Storthz, K.; Matson, D.O.; Adam, E.; Dreesman, G.R. (Baylor Univ., Houston, TX (USA). Coll. of Medicine)

    1983-02-01

    The specificity and sensitivity of a micro solid-phase radioimmunoassay (micro-SPRIA) that detects type-specific IgG antibody to herpes simplex virus types 1 and 2 (HSV1 and HSV2) were evaluated. Glycoproteins VP123 (molecular weight, 123,000) of HSV1 and VP119 (molecular weight, 119,000) of HSV2 were found to display the greatest degree of antigenic type-specificity of several HSV antigens tested with the micro-SPRIA technique. When testing a group of sera, negative for anti-HSV antibodies by microneutralization, in the micro-SPRIA, a range of negative reactivities was noted, suggesting that cut-points should be determined for each antigen preparation. The micro-SPRIA detected appropriate antibody activity in patients with recurrent infection and a marked agreement was noted in comparison to detection of anti-HSV antibodies measured with the microneutralization test. The type-specificity of the micro-SPRIA was substantiated by the independence of test results using VP119 and VP123 antigens for a random group of positive sera. The assay is rapid, specific, and sensitive and allows the testing of multiple serum samples with a standardized set of reagents.

  7. ZnO nanorod array solid phase micro-extraction fiber coating: fabrication and extraction capability

    Wang Dan; Zhang Zhuomin; Li Tiemei; Zhang Lan; Chen Guonan; Luo Lin

    2009-01-01

    In this paper, a ZnO nanorod array has been introduced as a coating to the headspace solid phase micro-extraction (HSSPME) field. The coating shows good extraction capability for volatile organic compounds (VOCs) by use of BTEX as a standard and can be considered suitable for sampling trace and small molecular VOC targets. In comparison with the randomly oriented ZnO nanorod HSSPME coating, ZnO nanorod array HSSPME fiber coating shows better extraction capability, which is attributed to the nanorod array structure of the coating. Also, this novel nanorod array coating shows good extraction selectivity to 1-propanethiol.

  8. Development of magnetic micro-solid phase extraction for analysis of phthalate esters in packaged food.

    Makkliang, Fonthip; Kanatharana, Proespichaya; Thavarungkul, Panote; Thammakhet, Chongdee

    2015-01-01

    A novel, simple and low cost magnetic multi-walled carbon nanotubes-poly (vinyl alcohol) cryogel-micro-solid phase extraction (magnetic-MWCNTs-PVA cryogel-μ-SPE) sorbent was synthesized by incorporating magnetic particles and MWCNTs into a PVA cryogel. The magnetic-MWCNTs-PVA cryogel-μ-SPE sorbent developed, with a large surface area and macro-porous structure, provided good sorbent-to-sorbent reproducibility (%RSDclear chicken soup samples in the range 0.02-0.07 μg mL(-1). Copyright © 2014 Elsevier Ltd. All rights reserved.

  9. Headspace Solid Phase Micro Extraction Gas Chromatographic Determination of Fenthion in Human Serum

    Kyriaki Machera

    2008-05-01

    Full Text Available A simple and effective analytical procedure was developed for the determination of fenthion residues in human serum samples. The sample treatment was performed using the headspace solid-phase micro extraction with polyacrylate fiber, which has the advantage to require low amount of serum (1 mL without tedious pre-treatment. The quantification of fenthion was carried out by gas chromatography-mass spectrometry and the recoveries ranged from 79 to 104% at two spiking levels for 6 replicates. Detection and quantification limits were calculated as 1.51 and 4.54 ng/mL of serum respectively. Two fenthion metabolites − fenoxon and fenthion–sulfoxide − were also identified.

  10. Optimization of Solid Phase Micro-Extraction (SPME for Monitoring Occupational Exposure to Ethyl Benzene

    H. Heidari

    2009-08-01

    Full Text Available AbstractBackground and Objectives: Analytical methods for volatile organic compounds (VOCs in different samples need extraction of compounds, by applying hazardous solvents. Solid phase micro-extraction (SPME is a solvent-free equilibrium extraction method, in which proper calibration can allow quantitative determinations of VOCs at a very good sensitivity without the use of any organic solvent. VOCs are generally present in urine only at trace levels, therefore, a sensitive procedure is needed for their trace determinations. Throughout this study, headspace solid phase micro-extraction (HS-SPME was followed by GC-FID for ethyl benzene in spiked urine was optimized.Methods: In this study, the parameters influencing SPME and gas chromatography of ethyl benzene, including extraction time, temperature, desorption temperature, desorption time, salt addition, sample pH, sample volume and sample agitation were investigated. Results: Extraction procedure was performed at 30°C for 6 min, using 0.2 gml-1 of NaCl in the sample solution. The sample volume and sample pH were optimized at 5 ml and 7 (neutral pH, respectively. Desorption of the ethyl benzene was carried out for 60 sec. at 250°C. The method was also validated with three different spiked urine samples and illustrated an appropriate reproducibility over six consecutive days as well as six within-day experiments. During this investigation, parameters of accuracy, linearity, and detection limits of the procedure were also evaluated.Conclusion: The developed method of HS- SPME-GC-FID proved to be a simple, convenient, and practical procedure, and was successfully used for measuring of ethyl benzene in spiked urine.

  11. Poly(Dimethylsiloxane)-Poly(Vinyl Alcohol) Coated Solid Phase Micro extraction Fiber for Chloropyrifos Analysis

    Wan Aini Wan Ibrahim; Nor Fairul Zukry Ahmad Rasdy; Norfazilah Muhamad

    2016-01-01

    Traditional liquid - liquid extraction of pesticides consumes large volumes of organic solvent which are hazardous to the operator and is not environment friendly. Solid phase micro extraction (SPME) is a solvent less extraction method which is safer to the operator and is environmental friendly. A sol-gel hybrid fibre coating material, poly(dimethylsiloxane)-poly(vinyl alcohol) (PDMS-PVA) was synthesized and used in head space solid phase micro extraction (HS-SPME) of chloropyrifos. The thickness of the synthesised PDMS-PVA fiber coating was 13.5 μm and it is thermally stable up to 400 degree Celsius. The PDMS-PVA sol-gel hybrid fiber was also stable to two organic solvents tested; acetonitrile and dichloromethane (1 hour dipping) and showed no significant changes in extraction performance for chloropyrifos. Extracted chloropyrifos was analysed using gas chromatography electron capture detector (GC-ECD). Optimum SPME parameters affecting the PDMS-PVA HS-SPME performance namely extraction time (15 min), extraction temperature (50 degree Celsius), desorption time (5 min), desorption temperature (260 degree Celsius) and stirring rate (120 rpm) were used for extraction. It was found that HSSPME using PDMS-PVA sol-gel fiber gave significantly better extraction performance of chloropyrifos compared to commercial 100 μm PDMS fiber. The PDMS-PVA fiber showed excellent operational performances such as temperature stability (up to 380 degree Celsius), coating lifetime (up to 170 times use) and organic solvent stability. The PDMS-PVA-HS-SPME method showed excellent recovery for chloropyrifos from tomatoes (98.0 %, 5.9 % RSD) at 0.01 μg/ g spiked level (5 times lower than maximum residue limit set by European Union). (author)

  12. Improved detection limits for phthalates by selective solid-phase micro-extraction

    Zia, Asif I.

    2016-03-30

    Presented research reports on an improved method and enhanced limits of detection for phthalates; a hazardous additive used in the production of plastics by solid-phase micro-extraction (SPME) polymer in comparison to molecularly imprinted solid-phase extraction (MISPE) polymer. The polymers were functionalized on an interdigital capacitive sensor for selective binding of phthalate molecules from a complex mixture of chemicals. Both polymers owned predetermined selectivity by formation of valuable molecular recognition sites for Bis (2-ethylhexyl) phthalate (DEHP). Polymers were immobilized on planar electrochemical sensor fabricated on a single crystal silicon substrate with 500 nm sputtered gold electrodes fabricated using MEMS fabrication techniques. Impedance spectra were obtained using electrochemical impedance spectroscopy (EIS) to determine sample conductance for evaluation of phthalate concentration in the spiked sample solutions with various phthalate concentrations. Experimental results revealed that the ability of SPME polymer to adsorb target molecules on the sensing surface is better than that of MISPE polymer for phthalates in the sensing system. Testing the extracted samples using high performance liquid chromatography with photodiode array detectors validated the results.

  13. Applications of a solid phase radioimmunoassay (SPRIA) to the micro-determination of ABO blood group

    Wu Fenqiang; Guo Jingyuan

    1995-01-01

    The authors report a simple, rapid, sensitive and accurate solid phase radioimmunoassay (SPRIA) method which has been improved. The research included the tests of its methodological parameters, sensitivity, accuracy, and the studies on its applications to the detection of blood group substances in varied forensic biological materials. The coefficient variation of intra-assay was 5.6%, and that of inter-assay was 10.15%. As to its applications to the forensic serology, the ABO blood groups of human bloodstain, hair follicular tissues and salivary stains had been tested and the results were satisfying. Later, 50 unknown type bloodly samples had been blind tested. The judging level used to identify the positive and negative wells was 800 cpm, that meant, if the radioactive count of a well were over 800 cpm, it was determined as a positive well, if that of a well were below 800 cpm, it was negative well. As SPRIA is a method of micro-determination which can micro-test the blood group antigens contained in varied forensic biological materials, it should has a good future of its applications to the forensic medicine fields

  14. Microextração por fase sólida SPME, Solid Phase Micro-Extration

    Antonio Luiz Pires Valente

    2000-08-01

    Full Text Available Fundamental aspects of Solid Phase Micro-Extraction (SPME are discussed in the present paper. The application of SPME as a microtechnique of sample preparation for gas chromatographic analysis is considered and related to existing theoretical models. Both research prototypes and commercial SPME devices are considered.

  15. Evaluation of single-walled carbon nanohorns as sorbent in dispersive micro solid-phase extraction

    Jimenez-Soto, Juan Manuel; Cardenas, Soledad [Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus de Rabanales, University of Cordoba, 14071 Cordoba (Spain); Valcarcel, Miguel, E-mail: qa1meobj@uco.es [Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus de Rabanales, University of Cordoba, 14071 Cordoba (Spain)

    2012-02-10

    Highlights: Black-Right-Pointing-Pointer The potential of single walled carbon nanohorns in dispersive solid phase microextraction has been evaluated. Black-Right-Pointing-Pointer The method was characterized for the extraction of PAHs from waters. Black-Right-Pointing-Pointer Single walled carbon nanohorns were better extractant than carbon nanotubes and carbon nanocones. Black-Right-Pointing-Pointer The limits of detection were adequate for the target analytes in environmental waters. - Abstract: A new dispersive micro solid-phase extraction method which uses single-walled carbon nanohorns (SWNHs) as sorbent is proposed. The procedure combines the excellent sorbent properties of the nanoparticles with the efficiency of the dispersion of the material in the sample matrix. Under these conditions, the interaction with the analytes is maximized. The determination of polycyclic aromatic hydrocarbons was selected as model analytical problem. Two dispersion strategies were evaluated, being the functionalization via microwave irradiation better than the use of a surfactant. The extraction was accomplished by adding 1 mL of oxidized SWHNs (o-SWNHs) dispersion to 10 mL of water sample. After extraction, the mixture was passed through a disposable Nylon filter were the nanoparticles enriched with the PAHs were retained. The elution was carried out with 100 {mu}L of hexane. The limits of detection achieved were between 30 and 60 ng L{sup -1} with a precision (as repeatability) better than 12.5%. The recoveries obtained for the analytes in three different water samples were acceptable in all instances. The performance of o-SWNHs was favourably compared with that provided by carboxylated single-walled carbon nanotubes and thermally treated carbon nanocones.

  16. Optimization of Solid Phase Micro-Extraction (SPME for Monitoring Occupational Exposure to Ethyl Benzene

    H Heidari

    2012-05-01

    Full Text Available

    Background and Objectives: Analytical methods for volatile organic compounds (VOCs in different samples need extraction of compounds, by applying hazardous solvents. Solid phase micro-extraction (SPME is a solvent-free equilibrium extraction method, in which proper calibration can allow quantitative determinations of VOCs at a very good sensitivity without the use of any organic solvent. VOCs are generally present in urine only at trace levels, therefore, a sensitive procedure is needed for their trace determinations. Throughout this study, headspace solid phase micro-extraction (HS-SPME was followed by GC-FID for ethyl benzene in spiked urine was optimized.

    Methods: In this study, the parameters influencing SPME and gas chromatography of ethyl benzene, including extraction time, temperature, desorption temperature, desorption time, salt addition, sample pH, sample volume and sample agitation were investigated.

    Results: Extraction procedure was performed at 30°C for 6 min, using 0.2 gml-1 of NaCl in the sample solution. The sample volume and sample pH were optimized at 5 ml and 7 (neutral pH, respectively. Desorption of the ethyl benzene was carried out for 60 sec. at 250°C. The method was also validated with three different spiked urine samples and illustrated an appropriate reproducibility over six consecutive days as well as six within-day experiments. During this investigation, parameters of accuracy, linearity, and detection limits of the procedure were also evaluated.

    Conclusion: The developed method of HS- SPME-GC-FID proved to be a simple, convenient, and practical procedure, and was successfully used for measuring of ethyl benzene in spiked urine.

  17. Application of solid phase micro extraction (SPME) in profiling hydrocarbons in oil spill cases

    Zuraidah Abdullah Munir; Norashikin Saim; Nurul Huda Mamat Ghani

    2008-01-01

    In environmental forensic, it is extremely important to have a fast and reliable method in identifying sources of spilled oil and petroleum products. In this study, solid phase micro extraction (SPME) method coupled to gas chromatography-mass spectrometry was developed for the analysis of hydrocarbons in diesel and petroleum contaminated soil samples. Optimization of SPME parameters such as extraction time, extraction temperature and desorption time, was performed using 100-μm poly dimethylsiloxane (PDMS) fiber. These parameters were studied at three levels by means of a central composite experimental design and the optimum experimental conditions were determined using response surface method. The developed SPME method was applied to determine the profiles of hydrocarbons in several oil contaminated soil sample. The SPME method was also used to study the effects of weathering on the profiles of hydrocarbons in unleaded gasoline, diesel and kerosene contaminated soil samples. After several days, significant losses of the lighter hydrocarbons were observed compared to the heavier ones. From these data, SPME method can be used to differentiate possible candidate sources in oil spill cases. (author)

  18. Micro solid-phase radioimmunoassay for detection of herpesvirus type-specific antibody: parameters involved in standardization

    Matson, D.O.; Adler-Storthz, K.; Adam, E.; Dreesman, G.R. (Baylor Univ., Houston, TX (USA). Coll. of Medicine)

    1983-02-01

    A micro solid-phase radioimmunoassay (micro-SPRIA) was developed to demonstrate type-specific antibodies to herpes simplex virus types 1 and 2 (HSV1 and HSV2). Glycoproteins from the 123,000 dalton region of HSV1 (VP123) and the 119,000 dalton region of HSV2 (VP119) were isolated on preparative polyacrylamide gels for use as antigens in the micro-SPRIA. Human sera selected from clinical samples by virological history and appropriate microneutralization data were used to standardize the micro-SPRIA. Optimization of the assay required the use of siliconized microtiter wells for adsorption of antigen. Maximized results were highly dependent on the concentrations of antigen, primary antibody, and secondary antibody as well as the diluents used for these principal test reagents. Incorporation of HSV glycoproteins of each respective type with the optimal condition established in this study facilitates the direct detection of type-specific antibody in human sera.

  19. Magnetic micro-solid-phase-extraction of polycyclic aromatic hydrocarbons in water.

    Naing, Nyi Nyi; Yau Li, Sam Fong; Lee, Hian Kee

    2016-04-01

    A novel sorbent, magnetic chitosan functionalized graphene oxide (MCFG) was synthesized and used in the micro-solid-phase-extraction (μ-SPE) and gas chromatography-mass spectrometric (GC-MS) analysis of polycyclic aromatic hydrocarbons (PAHs) from water. Through the use of the magnetic sorbent, the μ-SPE device also functioned as a stir bar during extraction. Three types of MCFG were prepared using glutaraldehyde cross-linked chitosan and graphene oxide with different amounts of magnetic nanoparticles (Fe3O4) (0.05g, 0.07g and 0.1g). The material was characterized using Fourier transform infrared spectroscopy and field emission scanning electron microscopy. Parameters affecting the extraction such as the type of sorbent, extraction and desorption times, volume of sample solution and type of desorption solvent were optimized. Under the most favourable conditions, the highest extraction was obtained by using the composite prepared with 0.1g of Fe3O4. For the latter material as sorbent, the linearity of the analytes was in the range of 0.01 and 100μgL(-1) for naphthalene, fluoranthene and pyrene while acenaphthylene and phenanthrene exhibited linearity in the range of 0.05 and 100μgL(-1). For fluorene and anthracene, the linearity range was from 0.01 to 50μgL(-1). The coefficients of determination (r(2)) associated with the above linear ranges were higher than 0.987. The limits of detection from GC-MS analysis of the seven PAHs were in the range 0.2-1.8ngL(-1); limits of quantification were between 0.8 and 5.9ngL(-1) while the relative standard deviations (RSDs) varied from 2.1 to 8.2%. The recoveries of the method for the compounds at spiking levels of 1 and 5μgL(-1) were in the range 67.5-106.9% with RSDs below 15%. The enrichment factors were found to be in between 67 and 302. The developed method afforded an interesting and innovative approach using MCFG as an efficient and promising sorbent. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Novel approach to microwave-assisted extraction and micro-solid-phase extraction from soil using graphite fibers as sorbent.

    Xu, Li; Lee, Hian Kee

    2008-05-30

    A single-step extraction-cleanup procedure involving microwave-assisted extraction (MAE) and micro-solid-phase extraction (micro-SPE) has been developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) from soil samples. Micro-SPE is a relatively new extraction procedure that makes use of a sorbent enclosed within a sealed polypropylene membrane envelope. In the present work, for the first time, graphite fiber was used as a sorbent material for extraction. MAE-micro-SPE was used to cleanup sediment samples and to extract and preconcentrate five PAHs in sediment samples prepared as slurries with addition of water. The best extraction conditions comprised of microwave heating at 50 degrees C for a duration of 20 min, and an elution (desorption) time of 5 min using acetonitrile with sonication. Using gas chromatography (GC)-flame ionization detection (FID), the limits of detection (LODs) of the PAHs ranged between 2.2 and 3.6 ng/g. With GC-mass spectrometry (MS), LODs were between 0.0017 and 0.0057 ng/g. The linear ranges were between 0.1 and 50 or 100 microg/g for GC-FID analysis, and 1 and 500 or 1000 ng/g for GC-MS analysis. Granular activated carbon was also used for the micro-SPE device but was found to be not as efficient in the PAH extraction. The MAE-micro-SPE method was successfully used for the extraction of PAHs in river and marine sediments, demonstrating its applicability to real environmental solid matrixes.

  1. New Methyltrimethoxysilane-(3-Mercaptopropyl)- Trimethoxysilane Coated Hollow Fiber-Solid Phase Micro extraction for Hexanal and Heptanal Analysis

    Siti Munirah Abd Wahib; Mohd Marsin Sanagi

    2016-01-01

    Determination of volatile organic compounds (VOCs) in various matrices is often accomplished using solid phase micro extraction (SPME) as a superior mode of extraction. Alternatively, another configuration of solid phase micro extraction (SPME) namely hollow fiber-solid phase micro extraction (HF-SPME) is a great approach to redress some limitations of the ordinary SPME fibers including fiber breakage, coating stripping and sample carry over. The HF-SPME technique highlights the use of hollow polypropylene (PP) membrane to hold and protect the adsorbent inside its lumen. Unlike the conventional SPME, the inexpensive HF device can be disposed after single use. Introducing extracting phase via sol-gel technology has gained great interest owing to its simple preparation method and promising way to obtain materials with good characteristics. In the present work, a new hybrid silica material based on methyltrimethoxysilane-(3-mercaptopropyl)trimethoxysilane (MTMOS-MPTMOS) was introduced as a new extractant of HF-SPME and the effectiveness of the proposed method was tested for analysis of hexanal and heptanal as the target VOC analytes. Preparation of the HF-SPME MTMOS-MPTMOS was simple in which the hybrid material was synthesized via sol-gel method and was self-polymerized in small segments of HF. Parameters affecting the efficiency of the HF-SPME MTMOS-MPTMOS in extracting both aldehydes were thoroughly investigated and analyzed by gas chromatography-flame ionization detection (GC-FID). It was found that the highest efficiency was achieved as the extraction was conducted in 30 min at a stirring rate of 1000 rpm in a 10 mL of sample solution whereby the back-extraction was performed via vortex for 3 min using 100 μL methanol as desorption solvent. Under the optimal conditions, linearity was observed over a range of 0.020-10.00 μg mL"-"1 with detection limits of 0.015 μg mL"-"1 and 0.010 μg mL"-"1 for hexanal and heptanal, respectively. The applicability of the HF

  2. Surfactant-enhanced liquid-liquid microextraction coupled to micro-solid phase extraction onto highly hydrophobic magnetic nanoparticles

    Giannoulis, Kiriakos M.; Giokas, Dimosthenis L.; Tsogas, George Z.; Vlessidis, Athanasios G.; Zhu, Qing; Pan, Qinmin

    2013-01-01

    We are presenting a simplified alternative method for dispersive liquid-liquid microextraction (DLLME) by resorting to the use of surfactants as emulsifiers and micro solid-phase extraction (μ-SPE). In this combined procedure, DLLME of hydrophobic components is initially accomplished in a mixed micellar/microemulsion extractant phase that is prepared by rapidly mixing a non-ionic surfactant and 1-octanol in aqueous medium. Then, and in contrast to classic DLLME, the extractant phase is collected by highly hydrophobic polysiloxane-coated core-shell Fe 2 O 3 (at)C magnetic nanoparticles. Hence, the sample components are the target analyte in the DLLME which, in turn, becomes the target analyte of the μ-SPE step. This 2-step approach represents a new and simple DLLME procedure that lacks tedious steps such as centrifugation, thawing, or delicate collection of the extractant phase. As a result, the analytical process is accelerated and the volume of the collected phase does not depend on the volume of the extraction solvent. The method was applied to extract cadmium in the form of its pyrrolidine dithiocarbamate chelate from spiked water samples prior to its determination by FAAS. Detection limits were brought down to the low μg L −1 levels by preconcentrating 10 mL samples with satisfactory recoveries (96.0–108.0 %). (author)

  3. Stir-bar supported micro-solid-phase extraction for the determination of polychlorinated biphenyl congeners in serum samples.

    Sajid, Muhammad; Basheer, Chanbasha

    2016-07-15

    In present work, a new configuration of micro-solid phase extraction was introduced and termed as stir-bar supported micro-solid-phase extraction (SB-μ-SPE). A tiny stir-bar was packed inside the porous polypropylene membrane along with sorbent material and the edges of membrane sheet were heat sealed to secure the contents. The packing of stir-bar inside the μ-SPE device does not allow the device to stick with the wall or any corner of the sample vial during extraction, which is, however, a frequent observation in routine μ-SPE. Moreover, it enhances effective surface area of the sorbent exposed to sample solution through continuous agitation (motion and rotation). It also completely immerses the SB-μ-SPE device in the sample solution even for non-polar sorbents. Polychlorinated biphenyls (PCBs) were selected as model compounds and the method performance was evaluated in human serum samples. After extraction, samples were analyzed by gas chromatography mass spectrometry (GC-MS). The factors that affect extraction efficiency of SB-μ-SPE were optimized. Under optimum conditions, a good linearity (0.1-100ngmL(-1)) with coefficients of determinations ranging from 0.9868 to 0.9992 was obtained. Limits of detections were ranged between 0.003 and 0.047ngmL(-1). Acceptable values for inter-day (3.2-9.1%) and intra-day (3.1-7.2%) relative standard deviations were obtained. The optimized method was successfully applied to determine the concentration of PCB congeners in human serum samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Application of micro-solid-phase extraction for the on-site extraction of heterocyclic aromatic amines in seawater.

    Basheer, Chanbasha

    2018-04-01

    An efficient on-site extraction technique to determine carcinogenic heterocyclic aromatic amines in seawater has been reported. A micro-solid-phase extraction device placed inside a portable battery-operated pump was used for the on-site extraction of seawater samples. Before on-site applications, parameters that influence the extraction efficiency (extraction time, type of sorbent materials, suitable desorption solvent, desorption time, and sample volume) were investigated and optimized in the laboratory. The developed method was then used for the on-site sampling of heterocyclic aromatic amines determination in seawater samples close to distillation plant. Once the on-site extraction completed, the small extraction device with the analytes was brought back to the laboratory for analysis using high-performance liquid chromatography with fluorescence detection. Based on the optimized conditions, the calibration curves were linear over the concentration range of 0.05-20 μg/L with correlation coefficients up to 0.996. The limits of detection were 0.004-0.026 μg/L, and the reproducibility values were between 1.3 and 7.5%. To evaluate the extraction efficiency, a comparison was made with conventional solid-phase extraction and it was applied to various fortified real seawater samples. The average relative recoveries obtained from the spiked seawater samples varied in the range 79.9-95.2%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Evaluation of needle trap micro-extraction and solid-phase micro-extraction: Obtaining comprehensive information on volatile emissions from in vitro cultures.

    Oertel, Peter; Bergmann, Andreas; Fischer, Sina; Trefz, Phillip; Küntzel, Anne; Reinhold, Petra; Köhler, Heike; Schubert, Jochen K; Miekisch, Wolfram

    2018-05-14

    Volatile organic compounds (VOCs) emitted from in vitro cultures may reveal information on species and metabolism. Owing to low nmol L -1 concentration ranges, pre-concentration techniques are required for gas chromatography-mass spectrometry (GC-MS) based analyses. This study was intended to compare the efficiency of established micro-extraction techniques - solid-phase micro-extraction (SPME) and needle-trap micro-extraction (NTME) - for the analysis of complex VOC patterns. For SPME, a 75 μm Carboxen®/polydimethylsiloxane fiber was used. The NTME needle was packed with divinylbenzene, Carbopack X and Carboxen 1000. The headspace was sampled bi-directionally. Seventy-two VOCs were calibrated by reference standard mixtures in the range of 0.041-62.24 nmol L -1 by means of GC-MS. Both pre-concentration methods were applied to profile VOCs from cultures of Mycobacterium avium ssp. paratuberculosis. Limits of detection ranged from 0.004 to 3.93 nmol L -1 (median = 0.030 nmol L -1 ) for NTME and from 0.001 to 5.684 nmol L -1 (median = 0.043 nmol L -1 ) for SPME. NTME showed advantages in assessing polar compounds such as alcohols. SPME showed advantages in reproducibility but disadvantages in sensitivity for N-containing compounds. Micro-extraction techniques such as SPME and NTME are well suited for trace VOC profiling over cultures if the limitations of each technique is taken into account. Copyright © 2018 John Wiley & Sons, Ltd.

  6. Optimization of a method based on micro-matrix solid-phase dispersion (micro-MSPD for the determination of PCBs in mussel samples

    Nieves Carro

    2017-03-01

    Full Text Available This paper reports the development and optimization of micro-matrix solid-phase dispersion (micro-MSPD of nine polychlorinated biphenyls (PCBs in mussel samples (Mytilus galloprovincialis by using a two-level factorial design. Four variables (amount of sample, anhydrous sodium sulphate, Florisil and solvent volume were considered as factors in the optimization process. The results suggested that only the interaction between the amount of anhydrous sodium sulphate and the solvent volume was statistically significant for the overall recovery of a trichlorinated compound, CB 28. Generally most of the considered species exhibited a similar behaviour, the sample and Florisil amounts had a positive effect on PCBs extractions and solvent volume and sulphate amount had a negative effect. The analytical determination and confirmation of PCBs were carried out by using GC-ECD and GC-MS/MS, respectively. The method was validated having satisfactory precision and accuracy with RSD values below 6% and recoveries between 81 and 116% for all congeners. The optimized method was applied to the extraction of real mussel samples from two Galician Rías.

  7. Polypyrrole-magnetite dispersive micro-solid-phase extraction combined with ultraviolet-visible spectrophotometry for the determination of rhodamine 6G and crystal violet in textile wastewater.

    Kamaruddin, Amirah Farhan; Sanagi, Mohd Marsin; Wan Ibrahim, Wan Aini; Md Shukri, Dyia S; Abdul Keyon, Aemi S

    2017-11-01

    Polypyrrole-magnetite dispersive micro-solid-phase extraction method combined with ultraviolet-visible spectrophotometry was developed for the determination of selected cationic dyes in textile wastewater. Polypyrrole-magnetite was used as adsorbent due to its thermal stability, magnetic properties, and ability to adsorb Rhodamine 6G and crystal violet. Dispersive micro-solid-phase extraction parameters were optimized, including sample pH, adsorbent amount, extraction time, and desorption solvent. The optimum polypyrrole-magnetite dispersive micro-solid phase-extraction conditions were sample pH 8, 60 mg polypyrrole-magnetite adsorbent, 5 min of extraction time, and acetonitrile as the desorption solvent. Under the optimized conditions, the polypyrrole-magnetite dispersive micro-solid-phase extraction with ultraviolet-visible method showed good linearity in the range of 0.05-7 mg/L (R 2  > 0.9980). The method also showed a good limit of detection for the dyes (0.05 mg/L) and good analyte recoveries (97.4-111.3%) with relative standard deviations extraction and determination of dyes at trace concentration levels. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. An Experimental Design Approach for the Analysis of Liquid Phase Products in Water for Hydrogenolysis of Glycerol using Immersed Solid-Phase Micro extraction

    Noraini Hamzah; Rozita Osman; Noraini Hamzah; Mohd Ambar Yarmo

    2013-01-01

    In this study, a response surface methodology (RSM) was applied to optimize the immersed-solid-phase micro extraction (immersed-SPME) conditions for the first time using a polyacrylate (PA) coated fiber. This was to determine liquid phase compounds in water for hydrogenolysis reaction of glycerol. There are a three-factor response surface experimental design was used to evaluate the interactive effects of extraction temperature (30-70 degree Celsius), extraction time (10-30 minutes) and desorption time (2-18 minutes) on the analysis of liquid phase compounds in water for hydrogenolysis of glycerol using immersed-solid-phase micro extraction (immersed-SPME). The extraction conditions using immersed-SPME were optimized in order to achieve high enrichment of the analytes from aqueous samples. The isolated compounds from the SPME fiber were desorbed and separated on a capillary polar column of a gas chromatography-flame ionization detector (GC-FID). The extraction time and desorption time were found significant in increasing the amount of glycerol in aqueous hydrogenolysis of glycerol. Nevertheless, the effect of extraction temperature was not significant. In terms of interactions between the effects, the relation between extraction temperature and extraction time was the most significant. The optimised immersed-SPME conditions were at extraction temperature of 27 degree Celsius, extraction time of 30 minutes and 15 minutes of desorption time. Thus, the application of SPME was found to be a rapid and effective technique in the determination of glycerol and propylene glycol compounds in aqueous hydrogenolysis glycerol. (author)

  9. Sol–gel-based silver nanoparticles-doped silica – Polydiphenylamine nanocomposite for micro-solid-phase extraction

    Bagheri, Habib, E-mail: bagheri@sharif.edu; Banihashemi, Solmaz

    2015-07-30

    A nanocomposite of silica-polydiphenylamine doped with silver nanoparticles (Ag–SiO{sub 2}-PDPA) was successfully synthesized by the sol–gel process. For its preparation, PDPA was mixed with butanethiol capped Ag nanoparticles (NPs) and added to the silica sol solution. The Ag NPs were stabilized as a result of their adsorption on the SiO{sub 2} spheres. The surface characteristic of nanocomposite was investigated using scanning electron microscopy (SEM). In this work the Ag–SiO{sub 2}-PDPA nanocomposite was employed as an efficient sorbent for micro-solid-phase extraction (μ-SPE) of some selected pesticides. An amount of 15 mg of the prepared sorbent was used to extract and determine the representatives from organophosphorous, organochlorine and aryloxyphenoxy propionic acids from aqueous samples. After the implementation of extraction process, the analytes were desorbed by methanol and determined using gas chromatography–mass spectrometry (GC–MS). Important parameters influencing the extraction and desorption processes such as pH of sample solution, salting out effect, type and volume of the desorption solvent, the sample loading and eluting flow rates along with the sample volume were experimentally optimized. Limits of detection (LODs) and the limits of quantification (LOQs) were in the range of 0.02–0.05 μg L{sup −1} and 0.1–0.2 μg L{sup −1}, respectively, using time scheduled selected ion monitoring (SIM) mode. The relative standard deviation percent (RSD %) with four replicates was in the range of 6–10%. The applicability of the developed method was examined by analyzing different environmental water samples and the relative recovery (RR %) values for the spiked water samples were found to be in the range of 86–103%. - Highlights: • A sol–gel-based silver nanoparticles doped silica-polydiphenylamine nanocomposite was synthesized. • The sorbent was applied to micro-solid-phase extraction of some selected pesticides in water

  10. Sulfonated nanocellulose for the efficient dispersive micro solid-phase extraction and determination of silver nanoparticles in food products.

    Ruiz-Palomero, Celia; Soriano, M Laura; Valcárcel, Miguel

    2016-01-08

    This paper reports a simple approach to Analytical Nanoscience and Nanotechnology (AN&N) that integrates the nanotool, sulfonated nanocellulose (s-NC), and nanoanalyte, silver nanoparticles (AgNPs), in the same analytical process by using an efficient, environmentally friendly dispersive micro solid-phase extraction (D-μSPE) capillary electrophoresis (CE) method with s-NC as sorbent material. Introducing negatively charged sulfate groups onto the surface of cellulose enhances its surface chemistry and enables the extraction and preconcentration of AgNPs of variable diameter (10, 20 and 60nm) and shell composition (citrate and polyvinylpyrrolidone coatings) from complex matrices into a cationic surfactant. In this way, AgNPs of diverse nature were successfully extracted onto the s-NC sorbent and then desorbed into an aqueous solution containing thiotic acid (TA) prior to CE without the need for any labor-intensive cleanup. The ensuing eco-friendly D-μSPE method exhibited a linear response to AgNPs with a limit of detection (LOD) of 20μg/L. Its ability to specifically recognize AgNPs of different sizes was checked in orange juice and mussels, which afforded recoveries of 70.9-108.4%. The repeatability of the method at the limit of quantitation (LOQ) level was 5.6%. Based on the results, sulfonated nanocellulose provides an efficient, cost-effective analytical nanotool for the extraction of AgNPs from food products. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Innovative separation and preconcentration technique of coagulating homogenous dispersive micro solid phase extraction exploiting graphene oxide nanosheets

    Ghazaghi, Mehri [Department of Chemistry, College of Science, Semnan University, P.O. Box: 35131-19111, Semnan (Iran, Islamic Republic of); Mousavi, Hassan Zavvar, E-mail: hzmousavi@semnan.ac.ir [Department of Chemistry, College of Science, Semnan University, P.O. Box: 35131-19111, Semnan (Iran, Islamic Republic of); Rashidi, Ali Morad [Nanotechnology Research Center, Research Institute of Petroleum Industry (RIPI), West Entrance Blvd., Olympic Village, P.O. Box: 14857-33111, Tehran (Iran, Islamic Republic of); Shirkhanloo, Hamid [Occupational and Environmental Health Research Center (OEHRC), Iranian Petroleum Industry Health Research Institute (IPIHRI), Tehran (Iran, Islamic Republic of); Rahighi, Reza [Nanotechnology Research Center, Research Institute of Petroleum Industry (RIPI), West Entrance Blvd., Olympic Village, P.O. Box: 14857-33111, Tehran (Iran, Islamic Republic of); Department of Research and Development, Sharif Ultrahigh Nanotechnologists (SUN) Company, P.O. Box: 13488-96394, Tehran (Iran, Islamic Republic of)

    2016-01-01

    A uniquely novel, fast, and facile technique is introduced for the first time in which a scant amount of graphene oxide (GO), without modification, has been utilized in dispersive mode of solid phase extraction (SPE) for an efficient yet simple separation. The proposed method of coagulating homogenous dispersive micro solid phase extraction (CHD-µSPE) is based on coagulation of homogeneous GO solution with the aid of polyetheneimine (PEI). CHD-µSPE use full adsorption capacity of GO because in this method was used GO solution obtained from synthesis process without drying step and stacking nanosheets. In optimized condition, 30 µL GO solution (7 mg mL{sup −1}), obtained in synthesis process, was injected into 1.5 mL the sample solution followed by immediate injection of 53 µL PEI solution (1 mg mL{sup −1}). After inserting PEI, GO sheets aggregate and can be readily separated by centrifugation. PEI not only cause aggregation of GO, but also form three-dimensional network of GO with easy handling in following separation steps. Lead, cadmium, and chromium were selected as model analytes and the effecting parameters including the amount of GO, concentration of PEI, sample pH, extraction time, and type of desorption solvent were investigated and optimized. The results indicate that the proposed CHD-µSPE method can be successfully applied GO in dispersive mode of SPE without effecting on good capability adsorption of GO. The novel method was applied in determination of lead, cadmium, and chromium in water, human saliva, and urine samples by electrothermal atomic absorption spectrometry. The detection limits are as low as 0.035, 0.005, and 0.012 µg L{sup −1} for Pb, Cd, and Cr respectively. The intra-day precisions (RSDs) were lower than 3.8%. CHD-µSPE method showed a good linear ranges of 0.24–15.6, 0.015–0.95 and 0.039–2.33 µg L{sup −1} for Pb, Cd and Cr respectively. Method performance was investigated by determination of mentioned

  12. Solid phase radioimmunoassays

    Wide, L.

    1977-01-01

    Solid phase coupled antibodies were introduced to facilitate the separation of bound and free labelled ligand in the competitive inhibition radioimmunoassay. Originally, the solid matrix used was in the form of small particles and since then a number of different matrices have been used such as very fine powder particles, gels, paper and plastic discs, magnetic particles and the inside surface of plastic tubes. The coupling of antibodies may be that of a covalent chemical binding, a strong physical adsorbtion, or an immunological binding to a solid phase coupled antigen. New principles of radioimmunoassay such as the solid phase sandwich techniques and the immunoradiometric assay were developped from the use of solid phase coupled antigens and antibodies. The solid phase sandwich techniques are reagent excess methods with a very wide applicability. Several of the different variants of solid phase techniques are suitable for automation. Advantages and disadvantages of solid phase radioimmunoassays when compared with those using soluble reagents are discussed. (orig.) [de

  13. Innovative separation and preconcentration technique of coagulating homogenous dispersive micro solid phase extraction exploiting graphene oxide nanosheets.

    Ghazaghi, Mehri; Mousavi, Hassan Zavvar; Rashidi, Ali Morad; Shirkhanloo, Hamid; Rahighi, Reza

    2016-01-01

    A uniquely novel, fast, and facile technique is introduced for the first time in which a scant amount of graphene oxide (GO), without modification, has been utilized in dispersive mode of solid phase extraction (SPE) for an efficient yet simple separation. The proposed method of coagulating homogenous dispersive micro solid phase extraction (CHD-µSPE) is based on coagulation of homogeneous GO solution with the aid of polyetheneimine (PEI). CHD-µSPE use full adsorption capacity of GO because in this method was used GO solution obtained from synthesis process without drying step and stacking nanosheets. In optimized condition, 30 µL GO solution (7 mg mL(-1)), obtained in synthesis process, was injected into 1.5 mL the sample solution followed by immediate injection of 53 µL PEI solution (1 mg mL(-1)). After inserting PEI, GO sheets aggregate and can be readily separated by centrifugation. PEI not only cause aggregation of GO, but also form three-dimensional network of GO with easy handling in following separation steps. Lead, cadmium, and chromium were selected as model analytes and the effecting parameters including the amount of GO, concentration of PEI, sample pH, extraction time, and type of desorption solvent were investigated and optimized. The results indicate that the proposed CHD-µSPE method can be successfully applied GO in dispersive mode of SPE without effecting on good capability adsorption of GO. The novel method was applied in determination of lead, cadmium, and chromium in water, human saliva, and urine samples by electrothermal atomic absorption spectrometry. The detection limits are as low as 0.035, 0.005, and 0.012 µg L(-1) for Pb, Cd, and Cr respectively. The intra-day precisions (RSDs) were lower than 3.8%. CHD-µSPE method showed a good linear ranges of 0.24-15.6, 0.015-0.95 and 0.039-2.33 µg L(-1) for Pb, Cd and Cr respectively. Method performance was investigated by determination of mentioned metal ions in river water, human urine and

  14. Fabrication and characterization of anode-supported micro-tubular solide oxide fuel cell by phase inversion method

    Ren, Cong

    Nowadays, the micro-tubular solid oxide fuel cells (MT-SOFCs), especially the anode supported MT-SOFCs have been extensively developed to be applied for SOFC stacks designation, which can be potentially used for portable power sources and vehicle power supply. To prepare MT-SOFCs with high electrochemical performance, one of the main strategies is to optimize the microstructure of the anode support. Recently, a novel phase inversion method has been applied to prepare the anode support with a unique asymmetrical microstructure, which can improve the electrochemical performance of the MT-SOFCs. Since several process parameters of the phase inversion method can influence the pore formation mechanism and final microstructure, it is essential and necessary to systematically investigate the relationship between phase inversion process parameters and final microstructure of the anode supports. The objective of this study is aiming at correlating the process parameters and microstructure and further preparing MT-SOFCs with enhanced electrochemical performance. Non-solvent, which is used to trigger the phase separation process, can significantly influence the microstructure of the anode support fabricated by phase inversion method. To investigate the mechanism of non-solvent affecting the microstructure, water and ethanol/water mixture were selected for the NiO-YSZ anode supports fabrication. The presence of ethanol in non-solvent can inhibit the growth of the finger-like pores in the tubes. With the increasing of the ethanol concentration in the non-solvent, a relatively dense layer can be observed both in the outside and inside of the tubes. The mechanism of pores growth and morphology obtained by using non-solvent with high concentration ethanol was explained based on the inter-diffusivity between solvent and non-solvent. Solvent and non-solvent pair with larger Dm value is benefit for the growth of finger-like pores. Three cells with different anode geometries was

  15. Selective extraction of phospholipids from dairy products by micro-solid phase extraction based on titanium dioxide microcolumns followed by MALDI-TOF-MS analysis

    Calvano, Cosima; Jensen, Ole; Zambonin, Carlo

    2009-01-01

    A new micro-solid phase extraction (micro-SPE) procedure based on titanium dioxide microcolumns was developed for the selective extraction of phospholipids (PLs) from dairy products before matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) analysis. All...... the extraction steps (loading, washing, and elution) have been optimized using a synthetic mixture of PLs standard and the procedure was subsequently applied to food samples such as milk, chocolate milk and butter. The whole method demonstrated to be simpler than traditional approaches and it appears very...

  16. Determination of amphetamine-type stimulants (ATSs) and synthetic cathinones in urine using solid phase micro-extraction fibre tips and gas chromatography-mass spectrometry

    Alsenedi, Khalid A.; Morrison, Calum

    2018-01-01

    In recent years, an increasing number of stimulant drugs and new psychoactive substances (NPSs) have caused concern in scientific communities and therefore innovative methods to extract compounds from complex biological samples are required. This work is aimed at developing and validating a clean, convenient and straightforward extraction procedure with microliter amounts of organic solvent using Solid Phase Micro-Extraction tips (SPME tips) and analysis using Gas Chromatography-Mass Spectrom...

  17. Preparation and characterization of sodium dodecyl sulfate doped polypyrrole solid phase micro extraction fiber and its application to endocrine disruptor pesticide analysis

    Korba, Korcan; Pelit, Levent; Okçu Pelit, Füsun; Özdokur, K. Volkan; Ertaş, Hasan; Eroğlu, Ahmet E.; Ertaş, Fatma Nil

    2013-01-01

    A robust in house solid-phase micro extraction (SPME) surface has been developed for the headspace (HS)-SPME determination of endocrine disruptor pesticides, namely, Chlorpyrifos, Penconazole, Procymidone, Bromopropylate and Lambda-Cyhalothrin in wine sample by using sodium dodecylsulfate doped polypyrrole SPME fiber. Pyrrole monomer was electrochemically polymerized on a stainless steel wire in laboratory conditions in virtue of diminishing the cost and enhancing the analyte retention on its...

  18. Head Space Solid Phase Micro-Extraction (HS - SPME of volatile organic compounds produced by Sporidiobolus salmonicolor (CBS 2636

    Eunice Valduga

    2010-12-01

    Full Text Available The aim of the present study was the assessment of volatile organic compounds produced by Sporidiobolus salmonicolor (CBS 2636 using methyl and ethyl ricinoleate, ricinoleic acid and castor oil as precursors. The analysis of the volatile organic compounds was carried out using Head Space Solid Phase Micro-Extraction (HS - SPME. Factorial experimental design was used for investigating extraction conditions, verifying stirring rate (0-400 rpm, temperature (25-60 ºC, extraction time (10-30 minutes, and sample volume (2-3 mL. The identification of volatile organic compounds was carried out by Gas Chromatography with Mass Spectrum Detector (GC/MSD. The conditions that resulted in maximum extraction were: 60 ºC, 10 minutes extraction, no stirring, sample volume of 2.0 mL, and addition of saturated KCl (1:10 v/v. In the bio-production of volatile organic compounds the effect of stirring rate (120-200 rpm, temperature (23-33 ºC, pH (4.0-8.0, precursor concentration (0.02-0.1%, mannitol (0-6%, and asparagine concentration (0-0.2% was investigated. The bio-production at 28 ºC, 160 rpm, pH 6,0 and with the addition of 0.02% ricinoleic acid to the medium yielded the highest production of VOCs, identified as 1,4-butanediol, 1,2,2-trimethylciclopropilamine, beta-ionone; 2,3-butanodione, pentanal, tetradecane, 2-isononenal, 4-octen-3-one, propanoic acid, and octadecane.

  19. A novel magnetic poly(aniline-naphthylamine)-based nanocomposite for micro solid phase extraction of rhodamine B

    Bagheri, Habib; Daliri, Rasoul; Roostaie, Ali

    2013-01-01

    Graphical abstract: -- Highlights: •A Fe 3 O 4 –aniline-naphthylamine nanocomposite was prepared via a simple route. •The magnetic nanocomposite was applied for isolation of RhB from water. •The nanocomposite applicability was compared with other pristine polymers. •The method was applied for the determination of RhB in different samples. -- Abstract: A novel Fe 3 O 4 –poly(aniline-naphthylamine)-based nanocomposite was synthesized by chemical oxidative polymerization process as a magnetic sorbent for micro solid phase extraction. The scanning electron microscopy images of the synthesized nanocomposite revealed that the copolymer posses a porous structure with diameters less than 50 nm. The extraction efficiency of this sorbent was examined by isolation of rhodamine B, a mutagenic and carcinogenic dye, from aquatic media in dispersion mode. Among different synthesized polymers, Fe 3 O 4 /poly(aniline-naphthylamine) nanocomposite showed a prominent efficiency. Parameters including the desorption solvent, amount of sorbent, desorption time, sample pH, ionic strength, extraction time and stirring rate were optimized. Under the optimum condition, a linear spiked calibration curve in the range of 0.35–5.00 μg L −1 with R 2 = 0.9991 was obtained. The limits of detection (3S b ) and limits of quantification (10S b ) of the method were 0.10 μg L −1 and 0.35 μg L −1 (n = 3), respectively. The relative standard deviation for water sample with 0.5 μg L −1 of RhB was 4.2% (n = 5) and the absolute recovery was 92%. The method was applied for the determination of rhodamine B in dishwashing foam, dishwashing liquid, shampoo, pencil, matches tips and eye shadows samples and the relative recovery percentage were in the range of 94–99%

  20. Micro-matrix solid-phase dispersion coupled with MEEKC for quantitative analysis of lignans in Schisandrae Chinensis Fructus using molecular sieve TS-1 as a sorbent.

    Chu, Chu; Wei, Mengmeng; Wang, Shan; Zheng, Liqiong; He, Zheng; Cao, Jun; Yan, Jizhong

    2017-09-15

    A simple and effective method was developed for determining lignans in Schisandrae Chinensis Fructus by using a micro-matrix solid phase dispersion (MSPD) technique coupled with microemulsion electrokinetic chromatography (MEEKC). Molecular sieve, TS-1, was applied as a solid supporting material in micro MSPD extraction for the first time. Parameters that affect extraction efficiency, such as type of dispersant, mass ratio of the sample to the dispersant, grinding time, elution solvent and volume were optimized. The optimal extraction conditions involve dispersing 25mg of powdered Schisandrae samples with 50mg of TS-1 by a mortar and pestle. A grinding time of 150s was adopted. The blend was then transferred to a solid-phase extraction cartridge and the target analytes were eluted with 500μL of methanol. Moreover, several parameters affecting MEEKC separation were studied, including the type of oil, SDS concentration, type and concentration of cosurfactant, and concentration of organic modifier. A satisfactory linearity (R>0.9998) was obtained, and the calculated limits of quantitation were less than 2.77μg/mL. Finally, the micro MSPD-MEEKC method was successfully applied to the analysis of lignans in complex Schisandrae fructus samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. A novel magnetic poly(aniline-naphthylamine)-based nanocomposite for micro solid phase extraction of rhodamine B

    Bagheri, Habib, E-mail: bagheri@sharif.edu; Daliri, Rasoul; Roostaie, Ali

    2013-09-10

    Graphical abstract: -- Highlights: •A Fe{sub 3}O{sub 4}–aniline-naphthylamine nanocomposite was prepared via a simple route. •The magnetic nanocomposite was applied for isolation of RhB from water. •The nanocomposite applicability was compared with other pristine polymers. •The method was applied for the determination of RhB in different samples. -- Abstract: A novel Fe{sub 3}O{sub 4}–poly(aniline-naphthylamine)-based nanocomposite was synthesized by chemical oxidative polymerization process as a magnetic sorbent for micro solid phase extraction. The scanning electron microscopy images of the synthesized nanocomposite revealed that the copolymer posses a porous structure with diameters less than 50 nm. The extraction efficiency of this sorbent was examined by isolation of rhodamine B, a mutagenic and carcinogenic dye, from aquatic media in dispersion mode. Among different synthesized polymers, Fe{sub 3}O{sub 4}/poly(aniline-naphthylamine) nanocomposite showed a prominent efficiency. Parameters including the desorption solvent, amount of sorbent, desorption time, sample pH, ionic strength, extraction time and stirring rate were optimized. Under the optimum condition, a linear spiked calibration curve in the range of 0.35–5.00 μg L{sup −1} with R{sup 2} = 0.9991 was obtained. The limits of detection (3S{sub b}) and limits of quantification (10S{sub b}) of the method were 0.10 μg L{sup −1} and 0.35 μg L{sup −1} (n = 3), respectively. The relative standard deviation for water sample with 0.5 μg L{sup −1} of RhB was 4.2% (n = 5) and the absolute recovery was 92%. The method was applied for the determination of rhodamine B in dishwashing foam, dishwashing liquid, shampoo, pencil, matches tips and eye shadows samples and the relative recovery percentage were in the range of 94–99%.

  2. Nanostructured conducting molecularly imprinted polymer for selective extraction of salicylate from urine and serum samples by electrochemically controlled solid-phase micro-extraction

    Ameli, Akram; Alizadeh, Naader

    2011-01-01

    Highlights: ► Overoxidized polypyrrole templated with salicylate has been utilized as conducting molecular imprinted polymer for EC-SPME. ► This first study reported on conducting molecular imprinted polymer was used to EC-SPME of salicylate. ► Proposed method, is particularly effective in sample clean-up and selective monitoring of salicylate in physiological samples. - Abstract: Overoxidized polypyrrole (OPPy) films templated with salicylate (SA) have been utilized as conducting molecular imprinted polymers (CMIPs) for potential-induced selective solid-phase micro-extraction processes. Various important fabrication factors for controlling the performance of the OPPy films have been investigated using fluorescence spectrometry. Several key parameters such as applied potential for uptake, release, pH of uptake and release solution were varied to achieve the optimum micro-extraction procedure. The film template with SA exhibited excellent selectivity over some interference. The calibration graphs were linear in the ranges of 5 × 10 −8 to 5 × 10 −4 and 1.2 × 10 −6 to 5 × 10 −4 mol mL −1 and the detection limit was 4 × 10 −8 mol L −1 . The OPPy film as the solid-phase micro-extraction absorbent has been applied for the selective clean-up and quantification of trace amounts of SA from physiological samples. The results of scanning electron microscopy (SEM) have confirmed the nano-structure morphologies of the films.

  3. Simultaneous determination of seven synthetic colorants in wine by dispersive micro-solid-phase extraction coupled with reversed-phase high-performance liquid chromatography.

    Zhang, Yun; Zhou, Hua; Wang, Yougang; Wu, Xianglun; Zhao, Yonggang

    2015-02-01

    A novel and effective dispersive micro-solid-phase extraction (d-µ-SPE) using ethanediamine-functionalized magnetic Fe3O4 polymer (EDA-MP) as an efficient adsorbent in wine sample was developed. Based on this, a simple and time-saving analytical method for the simultaneous determination of seven synthetic colorants (i.e., tartrazine, amaranth, carmine, sunset yellow, allura red, brilliant blue and erythrosine) in wine by reversed-phase high-performance liquid chromatography with an ultraviolet detector was established. The experimental parameters, including the chromatographic retention behavior of studied synthetic colorants, the effect of the usage amount of cross-linking monomer, the effect of the usage amount of EDA-MP on the recovery and the recyclability of the adsorbents, were studied in detail. The results showed that the EDA-MP could be reused efficiently at least six times. Under optimized conditions, the recoveries for all analytes were in the range of 88.6-105.2%, with the intraday relative standard deviations (RSDs) ranging from 2.1 to 8.2% and the interday RSDs ranging from 3.4 to 8.7%, and all the analytes had good linearities in the tested ranges with correlation coefficients (r(2)) >0.9995. The limits of quantification for seven synthetic colorants were between 0.12 and 0.45 mg L(-1). The developed method was successfully applied to wine samples, and it was confirmed that the EDA-MP particles were highly effective d-µ-SPE materials. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  4. The application of micro-column solid phase extraction techniques for the determination of rare earth elements in actinide containing matrices

    Carney, K.P.; Cummings, D.G.

    1995-01-01

    The design and characterization of an argon segmented-solid phase extraction system is described. A 200 ul volume micro-column has been constructed for the preconcentration of rare earth elements (REEs) from salt matrices containing uranium. An inductively coupled plasma atomic emission spectrometer has been utilized for simultaneous detection of Sr, Y and the REEs (namely Ce, Eu, La, Nd, Pr, Sm) at levels ranging from 5- to 2000 ppm in LiCl/KCl samples containing U. Preconcentration factors of 100 fold have been demonstrated. The precision, linear dynamic range and column performance of the system will be presented. (author). 5 refs., 5 figs., 3 tabs

  5. Preparation and evaluation of molecularly imprinted solid-phase micro-extraction fibers for selective extraction of phthalates in an aqueous sample

    He Juan; Lv Ruihe; Zhan Haijun; Wang Huizhi; Cheng Jie; Lu Kui; Wang Fengcheng

    2010-01-01

    A novel molecularly imprinted polymer (MIP) that was applied to a solid-phase micro-extraction (SPME) device, which could be coupled directly to gas chromatograph and mass spectrometer (GC/MS), was prepared using dibutyl phthalate (DBP) as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope images indicated that the MIP-coated solid-phase micro-extraction (MI-SPME) fibers were homogeneous and porous. The extraction yield of DBP with the MI-SPME fibers was higher than that of the non-imprinted polymer (NIP)-coated SPME (NI-SPME) fibers. The MI-SPME fibers had a higher selectivity to other phthalates that had similar structures as DBP. A method was developed for the determination of phthalates using MI-SPME fibers coupled with GC/MS. The extraction conditions were optimized. Detection limits for the phthalate samples were within the range of 2.17-20.84 ng L -1 . The method was applied to five kinds of phthalates dissolved in spiked aqueous samples and resulted in recoveries of up to 94.54-105.34%, respectively. Thus, the MI-SPME fibers are suitable for the extraction of trace phthalates in complicated samples.

  6. Comparison of different types of coatings in headspace solid phase micro extraction for the analysis of pesticide residues in vegetables and fruits

    Chai, Mee Kin; Tan, Guan Huat

    2008-01-01

    Despite the continuing development of solid-phase micro extraction (SPME) fiber coatings, their selection presents some difficulties for analytes in choosing the appropriate fiber for a particular application. There are many types of SPME coatings available commercially. The most widely used for determination of pesticide residues in vegetable and fruits are polydimethylsiloxane (PDMS) and polyacrylate (PA). A headspace solid phase micro extraction (HS-SPME) procedure using these two commercialized fibers (PDMS and PA) is presented for the determination of selected groups of organo chlorine and organophosphorus pesticides. The extraction performances of these compounds were compared using these two fibers. The optimal experimental procedures for the adsorption and desorption of pesticides were determined. An explanation for the extraction differences is suggested based on the different thickness, polarity of the polymeric film of fibers and the different extracting matrices. In addition, the higher detector response of the pesticides after addition of aliquots of water and an organic solvent to the vegetable and fruit samples are also discussed. The SPME fibers were reusable until a maximum of 120 extractions. Finally, the optimized procedures were applied successfully for the determination of these compounds in vegetable and fruits samples. Mean recoveries for all pesticides were between 75.0-97 % with RSD below 7 %. (author)

  7. Nanostructured conducting molecularly imprinted polymer for selective extraction of salicylate from urine and serum samples by electrochemically controlled solid-phase micro-extraction

    Ameli, Akram [Department of Chemistry, Faculty of Science, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Alizadeh, Naader, E-mail: alizaden@modares.ac.ir [Department of Chemistry, Faculty of Science, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of)

    2011-11-30

    Highlights: Black-Right-Pointing-Pointer Overoxidized polypyrrole templated with salicylate has been utilized as conducting molecular imprinted polymer for EC-SPME. Black-Right-Pointing-Pointer This first study reported on conducting molecular imprinted polymer was used to EC-SPME of salicylate. Black-Right-Pointing-Pointer Proposed method, is particularly effective in sample clean-up and selective monitoring of salicylate in physiological samples. - Abstract: Overoxidized polypyrrole (OPPy) films templated with salicylate (SA) have been utilized as conducting molecular imprinted polymers (CMIPs) for potential-induced selective solid-phase micro-extraction processes. Various important fabrication factors for controlling the performance of the OPPy films have been investigated using fluorescence spectrometry. Several key parameters such as applied potential for uptake, release, pH of uptake and release solution were varied to achieve the optimum micro-extraction procedure. The film template with SA exhibited excellent selectivity over some interference. The calibration graphs were linear in the ranges of 5 Multiplication-Sign 10{sup -8} to 5 Multiplication-Sign 10{sup -4} and 1.2 Multiplication-Sign 10{sup -6} to 5 Multiplication-Sign 10{sup -4} mol mL{sup -1} and the detection limit was 4 Multiplication-Sign 10{sup -8} mol L{sup -1}. The OPPy film as the solid-phase micro-extraction absorbent has been applied for the selective clean-up and quantification of trace amounts of SA from physiological samples. The results of scanning electron microscopy (SEM) have confirmed the nano-structure morphologies of the films.

  8. Analysis of volatiles in silver carp by headspace solid phase micro-extraction coupled with GC-MS

    Yang Yuping; Xiong Guangquan; Cheng Wei; Liao Tao; Lin Ruotai; Geng Shengrong; Li Xin; Li Xiaoding; Wu Wenjin

    2010-01-01

    In this paper, a method for the determination of volatiles using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) was presented. The extraction conditions were optimized with reference to these volatiles as hexanal, heptanal, benzaldehyde, 1-Octen-3-ol, octanal, nonanal, decenal, 2,4-heptadienal and 2,4-decadienal. The extraction of fish muscle followed by incubation on a StableFlex divinyl benzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber during 50 in at 60 obtained the most effective extraction of the analytes. The methods by HS-SPME and GC-MS were effective in detecting volatiles in the gills, scales, viscera and fish muscles. The types of volatiles in the gill were more than other organs and the number of odors compounds was 63, and the number of volatiles in scales, viscera and fish muscles was 48, 44 and 42 respectively. (authors)

  9. ZnO nanorod array polydimethylsiloxane composite solid phase micro-extraction fiber coating: fabrication and extraction capability.

    Wang, Dan; Wang, Qingtang; Zhang, Zhuomin; Chen, Guonan

    2012-01-21

    ZnO nanorod array coating is a novel kind of solid-phase microextraction (SPME) fiber coating which shows good extraction capability due to the nanostructure. To prepare the composite coating is a good way to improve the extraction capability. In this paper, the ZnO nanorod array polydimethylsiloxane (PDMS) composite SPME fiber coating has been prepared and its extraction capability for volatile organic compounds (VOCs) has been studied by headspace sampling the typical volatile mixed standard solution of benzene, toluene, ethylbenzene and xylene (BTEX). Improved detection limit and good linear ranges have been achieved for this composite SPME fiber coating. Also, it is found that the composite SPME fiber coating shows good extraction selectivity to the VOCs with alkane radicals.

  10. Dispersive solid phase micro-extraction of mercury(II from environmental water and vegetable samples with ionic liquid modified graphene oxide nanoparticles

    Nasrollahpour Atefeh

    2017-01-01

    Full Text Available A new dispersive solid phase micro-extraction (dispersive-SPME method for separation and preconcentration of mercury(II using ionic liquid modified magnetic reduced graphene oxide (IL-MrGO nanoparticles, prior to the measurement by cold vapour atomic absorption spectrometry (CV-AAS has been developed. The IL-MrGO composite was characterized by Brunauer– Emmett–Teller method (BET for adsorption-desorption measurement, thermogravimetric analysis (TGA, powder X-ray diffraction (XRD and X-ray photoelectron spectroscopy (XPS. The method is based on the sorption of mercury( II on IL-MrGO nanoparticles due to electrostatic interaction and complex formation of ionic liquid part of IL-MrGO with mercury(II. The effect of experimental parameters for preconcentration of mercury(II, such as solution type, concentration and volume of the eluent, pH, time of the sorption and desorption, amount of the sorbent and coexisting ion concentration have been optimized. Under the optimized conditions, a linear response was obtained in the concentration range of 0.08–10 ng mL-1 with a determination coefficient of 0.9995. The limit of detection (LOD of the method at a signal to noise ratio of 3 was 0.01 ng mL-1. Intra-day and inter-day precisions were obtained equal to 3.4 and 4.5 %, respectively. The dispersive solid phase micro-extraction of mercury(II on IL-MrGO nanoparticles coupled with cold vapour atomic absorption spectrometry was successfully used for extraction and determination of mercury(II in water and vegetable samples.

  11. Magnetic micro-solid-phase extraction based on magnetite-MCM-41 with gas chromatography-mass spectrometry for the determination of antidepressant drugs in biological fluids.

    Kamaruzaman, Sazlinda; Sanagi, Mohd Marsin; Yahaya, Noorfatimah; Wan Ibrahim, Wan Aini; Endud, Salasiah; Wan Ibrahim, Wan Nazihah

    2017-11-01

    A new facile magnetic micro-solid-phase extraction coupled to gas chromatography and mass spectrometry detection was developed for the extraction and determination of selected antidepressant drugs in biological fluids using magnetite-MCM-41 as adsorbent. The synthesized sorbent was characterized by several spectroscopic techniques. The maximum extraction efficiency for extraction of 500 μg/L antidepressant drugs from aqueous solution was obtained with 15 mg of magnetite-MCM-41 at pH 12. The analyte was desorbed using 100 μL of acetonitrile prior to gas chromatography determination. This method was rapid in which the adsorption procedure was completed in 60 s. Under the optimized conditions using 15 mL of antidepressant drugs sample, the calibration curve showed good linearity in the range of 0.05-500 μg/L (r 2  = 0.996-0.999). Good limits of detection (0.008-0.010 μg/L) were obtained for the analytes with good relative standard deviations of solid-phase extraction with gas chromatography and mass spectrometry is a convenient, fast, and economical method for the extraction and determination of amitriptyline and chlorpromazine in biological samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Solid phase assays

    Reese, M.G.; Johnson, L.R.; Ransom, D.K.

    1980-01-01

    In a solid phase assay for quantitative determination of biological and other analytes, a sample such as serum is contacted with a receptor for the analyte being assayed, the receptor being supported on a solid support. No tracer for the analyte is added to the sample before contacting with the receptor; instead the tracer is contacted with the receptor after unbound analyte has been removed from the receptor. The assay can be otherwise performed in a conventional manner but can give greater sensitivity. (author)

  13. In-line micro-matrix solid-phase dispersion extraction for simultaneous separation and extraction of Sudan dyes in different spices.

    Rajabi, Maryam; Sabzalian, Sedigheh; Barfi, Behruz; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

    2015-12-18

    A novel, simple, fast, and miniaturized method, termed in-line micro-matrix solid-phase dispersion (in-line MMSPD), coupled with high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of Sudan dyes (i.e. Sudan I-IV, Sudan orange G, Sudan black B, and Sudan red G) with the aid of an experimental design strategy. In this method, a matrix solid-phase dispersion (MSPD) column including a suitable mixture of polar sorbents was inserted in the mobile phase pathway, and while the interfering compounds were retained, the analytes were eluted and entered into the analytical column. In this way, the extraction, elution, and separation of the analytes were performed sequentially. Under the optimal experimental conditions (including the amount of sample, 0.0426g; amount of dispersant phase, 0.0216g of florisil, 0.0227g of silica, 0.0141g of alumina; and blending time, 112s), the limits of detection (LODs), limits of quantification, linear dynamic ranges, and recoveries were obtained to be 0.3-15.3μgkg(-1), 1-50μgkg(-1), 50-28,000μgkg(-1), and 94.5-99.1%, respectively. The results obtained showed that determination of the selected Sudan dyes in food samples using an enough sensitive and a simple analytically validated method like in-line MMSPD may offer a suitable screening method, which could be useful for food analysis and adulteration. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Solid phase transformations

    Čermák, J

    2008-01-01

    This special-topic book, devoted to ""Solid Phase Transformations"" , covers a broad range of phenomena which are of importance in a number of technological processes. Most commercial alloys undergo thermal treatment after casting, with the aim of imparting desired compositions and/or optimal morphologies to the component phases. In spite of the fact that the topic has lain at the center of physical metallurgy for a long time, there are numerous aspects which are wide open to potential investigative breakthroughs. Materials with new structures also stimulate research in the field, as well as n

  15. Solid phase extraction membrane

    Carlson, Kurt C [Nashville, TN; Langer, Roger L [Hudson, WI

    2002-11-05

    A wet-laid, porous solid phase extraction sheet material that contains both active particles and binder and that possesses excellent wet strength is described. The binder is present in a relatively small amount while the particles are present in a relatively large amount. The sheet material is sufficiently strong and flexible so as to be pleatable so that, for example, it can be used in a cartridge device.

  16. Vortex-Assisted Dispersive Micro-Solid Phase Extraction Using CTAB-Modified Zeolite NaY Sorbent Coupled with HPLC for the Determination of Carbamate Insecticides.

    Salisaeng, Pawina; Arnnok, Prapha; Patdhanagul, Nopbhasinthu; Burakham, Rodjana

    2016-03-16

    A vortex-assisted dispersive micro-solid phase extraction (VA-D-μ-SPE) based on cetyltrimethylammonium bromide (CTAB)-modified zeolite NaY was developed for preconcentration of carbamate pesticides in fruits, vegetables, and natural surface water prior to analysis by high performance liquid chromatography with photodiode array detection. The small amounts of solid sorbent were dispersed in a sample solution, and extraction occurred by adsorption in a short time, which was accelerated by vortex agitation. Finally, the sorbents were filtered from the solution, and the analytes were subsequently desorbed using an appropriate solvent. Parameters affecting the VA-D-μ-SPE performance including sorbent amount, sample volume, desorption solvent ,and vortex time were optimized. Under the optimum condition, linear dynamic ranges were achieved between 0.004-24.000 mg kg(-1) (R(2) > 0.9946). The limits of detection (LODs) ranged from 0.004-4.000 mg kg(-1). The applicability of the developed procedure was successfully evaluated by the determination of the carbamate residues in fruits (dragon fruit, rambutan, and watermelon), vegetables (cabbage, cauliflower, and cucumber), and natural surface water.

  17. Determination of Triazine Herbicides in Drinking Water by Dispersive Micro Solid Phase Extraction with Ultrahigh-Performance Liquid Chromatography-High-Resolution Mass Spectrometric Detection.

    Chen, Dawei; Zhang, Yiping; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

    2015-11-11

    A novel dispersive micro solid phase extraction (DMSPE) method based on a polymer cation exchange material (PCX) was applied to the simultaneous determination of the 30 triazine herbicides in drinking water with ultrahigh-performance liquid chromatography-high-resolution mass spectrometric detection. Drinking water samples were acidified with formic acid, and then triazines were adsorbed by the PCX sorbent. Subsequently, the analytes were eluted with ammonium hydroxide/acetonitrile. The chromatographic separation was performed on an HSS T3 column using water (4 mM ammonium formate and 0.1% formic acid) and acetonitrile (0.1% formic acid) as the mobile phase. The method achieved LODs of 0.2-30.0 ng/L for the 30 triazines, with recoveries in the range of 70.5-112.1%, and the precision of the method was better than 12.7%. These results indicated that the proposed method had the advantages of convenience and high efficiency when applied to the analysis of the 30 triazines in drinking water.

  18. Preconcentration of Trace Neonicotinoid Insecticide Residues Using Vortex-Assisted Dispersive Micro Solid-Phase Extraction with Montmorillonite as an Efficient Sorbent

    Khwankaew Moyakao

    2018-04-01

    Full Text Available In this work, we investigated montmorillonite for adsorption of neonicotinoid insecticides in vortex-assisted dispersive micro-solid phase extraction (VA-d-μ-SPE. High-performance liquid chromatography with photodiode array detection was used for quantification and determination of neonicotinoid insecticide residues, including thiamethoxam, clothianidin, imidacloprid, acetamiprid, and thiacloprid. In this method, the solid sorbent was dispersed into the aqueous sample solution and vortex agitation was performed to accelerate the extraction process. Finally, the solution was filtered from the solid sorbent with a membrane filter. The parameters affecting the extraction efficiency of the proposed method were optimized, such as amount of sorbent, sample volume, salt addition, type and volume of extraction solvent, and vortex time. The adsorbing results show that montmorillonite could be reused at least 4 times and be used as an effective adsorbent for rapid extraction/preconcentration of neonicotinoid insecticide residues. Under optimum conditions, linear dynamic ranges were achieved between 0.5 and 1000 ng mL−1 with a correlation of determination (R2 greater than 0.99. Limit of detection (LOD ranged from 0.005 to 0.065 ng mL−1, while limit of quantification (LOQ ranged from 0.008 to 0.263 ng mL−1. The enrichment factor (EF ranged from 8 to 176-fold. The results demonstrated that the proposed method not only provided a more simple and sensitive method, but also can be used as a powerful alternative method for the simultaneous determination of insecticide residues in natural surface water and fruit juice samples.

  19. Determination of perfluorinated carboxylic acids in fish fillet by micro-solid phase extraction, followed by liquid chromatography-triple quadrupole mass spectrometry.

    Lashgari, Maryam; Lee, Hian Kee

    2014-11-21

    In the current study, a simple, fast and efficient combination of protein precipitation and micro-solid phase extraction (μ-SPE) followed by liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS) was developed for the determination of perfluorinated carboxylic acids (PFCAs) in fish fillet. Ten PFCAs with different hydrocarbon chain lengths (C5-C14) were analysed simultaneously using this method. Protein precipitation by acetonitrile and μ-SPE by surfactant-incorporated ordered mesoporous silica were applied to the extraction and concentration of the PFCAs as well as for removal of interferences. Determination of the PFCAs was carried out by LC-MS/MS in negative electrospray ionization mode. MS/MS parameters were optimized for multiple reaction monitoring of the analytes. (13)C mass labelled PFOA as a stable-isotopic internal standard, was used for calibration. The detection limits of the method ranged from 0.97 ng/g to 2.7 ng/g, with a relative standard deviation of between 5.4 and 13.5. The recoveries were evaluated for each analyte and were ranged from 77% to 120%. The t-test at 95% confidence level showed that for all the analytes, the relative recoveries did not depend on their concentrations in the explored concentration range. The effect of the matrix on MS signals (suppression or enhancement) was also evaluated. Contamination at low levels was detected for some analytes in the fish samples. The protective role of the polypropylene membrane used in μ-SPE in the elimination of matrix effects was evaluated by parallel experiments in classical dispersive solid phase extraction. The results evidently showed that the polypropylene membrane was significantly effective in reducing matrix effects. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Solid phase microextraction.

    Pawliszyn, J

    2001-01-01

    Solid Phase Microextraction (SPME) uses a small volume of sorbent dispersed typically on the surface of small fibres, to isolate and concentrate analytes from sample matrix. After contact with sample, analytes are absorbed or adsorbed by the fibre phase (depending on the nature of the coating) until an equilibrium is reached in the system. The amount of an analyte extracted by the coating at equilibrium is determined by the magnitude of the partition coefficient of the analyte between the sample matrix and the coating material. After the extraction step, the fibres are transferred, with the help of a syringe-like handling device, to analytical instrument, for separation and quantitation of target analytes. This technique integrates sampling, extraction and sample introduction and is a simple way of facilitating on-site monitoring. Applications of this technique include environmental monitoring, industrial hygiene, process monitoring, clinical, forensic, food, flavour, fragrance and drug analyses, in laboratory and on-site analysis.

  1. Solid-phase spectrophotometry

    Brykina, G.D.; Marchenko, D.Yu.; Shpigun, O.A.

    1995-01-01

    Solid-phase spectrophotometry (SPS), which is based on the direct measurement of light absorption of an ion exchanger containing a substance of interest, was reviewed. Since 1976, it has been known that aborbance of an ion exchanger is directly proportional to the concentration of a particular ion in solution. A similar dependence can also be followed for other sorbents, as well as for foams, membranes, films, etc., which do not exhibit ion exchange properties. One can use absorption, diffuse reflection, and luminescence spectra parameters as an analytical signal. Thus, SPS of ion exchangers is among the analytical techniques that combine the sorption concentration and surface determination of the substance of interest. This review summarizes the advancements in SPS over the last six years and demonstrates the prospects for its development. Special attention is paid to experimental methods for measuring solid-phase absorption and to the basic procedures of sample preparation, including new ones. These two facets are of great importance for obtaining precise results and extending the capabilities of SPS

  2. Determination of residual volatile organic compounds migrated from polystyrene food packaging into food simulant by headspace solid phase micro extraction-gas chromatography

    Mohd Marsin Sanagi; Ling, Susie Lu; Zalilah Nasir; Wan Aini Wan Ibrahim; Abu Naim, Ahmedy

    2008-01-01

    The residual styrene and other volatile organic compounds (VOCs) present in the polystyrene food packaging are of concern as these compounds have the potential to migrate into the food in contact. This work describes a method for quantitative determination of VOCs, namely styrene, toluene, ethyl benzene, iso-propylbenzene and n-propylbenzene that have migrated from polystyrene food packaging into food stimulant by gas chromatography-flame ionization detection (GC-FID). Headspace solid phase micro extraction (HS-SPME) technique was applied for migration test using water as food stimulant. The effects of extraction variables including sample volume, eluotropic strength, extraction temperature, extraction time, desorption time, sample agitation, and salt addition on the amounts of the extracted analyses were studied to obtain the optimal HS-SPME conditions. The optimized method was applied to test the VOCs migrated from polystyrene bowls and cups at storage temperatures ranging from 24 to 80 degree Celsius for 30 min. Styrene and ethyl benzene were found to migrate from the samples into the food stimulant. The migration of analyze was found to be strongly dependent upon the storage temperature. The HS-SPME is useful as an alternative method to determine the migration of VOCs from food packaging material into food stimulant. (author)

  3. Magnetic nanoparticles-nylon 6 composite for the dispersive micro solid phase extraction of selected polycyclic aromatic hydrocarbons from water samples.

    Reyes-Gallardo, Emilia M; Lucena, R; Cárdenas, S; Valcárcel, M

    2014-06-06

    In this article, the easy synthesis of magnetic nanoparticles-nylon 6 composite is presented, characterized and applied in the microextraction field. The one-step synthesis of the composite is performed by a solvent changeover playing with the different solubility of the polymeric network in formic acid and water. The new material has been characterized by different techniques including infrared spectroscopy, transmission and scanning microscopy. The extraction performance of the composite under a dispersive micro solid phase extraction format has been evaluated by determining four polycyclic aromatic hydrocarbons (benzo[b]fluoranthene, fluoranthene, indeno[1,2,3-cd]pyrene and phenanthrene) in water using ultra performance liquid chromatography (UPLC) combined with photo diode array detection. The developed methodology allows the determination of the analytes with limits of detection in the range from 0.05 μg/L (benzo[b]fluoranthene) to 0.58 μg/L (phenanthrene). The repeatability of the method was better than 6.9% at the limit of quantification level. The relative recoveries varied in the interval 80-111%. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Online micro-solid-phase extraction based on boronate affinity monolithic column coupled with high-performance liquid chromatography for the determination of monoamine neurotransmitters in human urine.

    Yang, Xiaoting; Hu, Yufei; Li, Gongke

    2014-05-16

    Quantification of monoamine neurotransmitters is very important in diagnosing and monitoring of patients with neurological disorders. We developed an online analytical method to selectively determine urinary monoamine neurotransmitters, which coupled the boronate affinity monolithic column micro-solid-phase extraction with high-performance liquid chromatography (HPLC). The boronate affinity monolithic column was prepared by in situ polymerization of vinylphenylboronic acid (VPBA) and N,N'-methylenebisacrylamide (MBAA) in a stainless capillary column. The prepared monolithic column showed good permeability, high extraction selectivity and capacity. The column-to-column reproducibility was satisfactory and the enrichment factors were 17-243 for four monoamine neurotransmitters. Parameters that influence the online extraction efficiency, including pH of sample solution, flow rate of extraction and desorption, extraction volume and desorption volume were investigated. Under the optimized conditions, the developed method exhibited low limit of detection (0.06-0.80μg/L), good linearity (with R(2) between 0.9979 and 0.9993). The recoveries in urine samples were 81.0-105.5% for four monoamine neurotransmitters with intra- and inter-day RSDs of 2.1-8.2% and 3.7-10.6%, respectively. The online analytical method was sensitive, accurate, selective, reliable and applicable to analysis of trace monoamine neurotransmitters in human urine sample. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Application of solid-phase micro extraction for the determination of pesticides in vegetable samples by gas chromatography with an electron capture detector

    Chai, Mee Kin; Tan, Guan Huat; Kumari, Asha

    2008-01-01

    A solid-phase micro extraction (SPME) method has been developed for the determination of 9 pesticides in 2 vegetables -cucumber and tomato - samples, based on direct immersion mode and subsequent desorption into the injection port of a gas chromatograph with an electron capture detector (GC-ECD). The main factors affecting the SPME process such as extraction time and temperature, desorption time and temperature, the effect of salt addition and fiber depth into the liner were studied and optimized. The analytical procedure proposed consisted of a 30 minute ultrasonic extraction of the target compounds from 1.0 g vegetable samples with 5 mL of distilled water. Then, the samples were filtered and topped up with distilled water to 10 mL. The analytes in this aqueous extract were extracted for 15 minutes with a 100 μm thickness polydimethylsiloxane SPME fiber. Relative standard deviations for triplicate analyses of samples were less than 10 %. The recoveries of the pesticides studied in cucumber and tomato ranged from 52 % to 82 % and the RSD were below 10 %. Therefore, the proposed method is applicable in the analysis of pesticides in vegetable matrices. SPME has been shown to be a simple extraction technique, which has a number of advantages such as solvent free extraction, simplicity and compatibility with the chromatographic analytical system. (author)

  6. An absorbing microwave micro-solid-phase extraction device used in non-polar solvent microwave-assisted extraction for the determination of organophosphorus pesticides.

    Wang, Ziming; Zhao, Xin; Xu, Xu; Wu, Lijie; Su, Rui; Zhao, Yajing; Jiang, Chengfei; Zhang, Hanqi; Ma, Qiang; Lu, Chunmei; Dong, Deming

    2013-01-14

    A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction (μ-SPE), was developed for the extraction of ten organophosphorus pesticides in vegetable and fruit samples. Without adding any polar solvent, only one kind of non-polar solvent (hexane) was used as extraction solvent in the whole extraction step. Absorbing microwave μ-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in μ-SPE, but also the microwave absorption medium. Some experimental parameters effecting on extraction efficiency was investigated and optimized. 1.0 g of sample, 8 mL of hexane and three absorbing microwave μ-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60°C for 10 min. The extracts obtained by MAE-μ-SPE were directly analyzed by GC-MS without any clean-up process. The recoveries were in the range of 93.5-104.6%, and the relative standard deviations were lower than 8.7%. Copyright © 2012 Elsevier B.V. All rights reserved.

  7. [Determination of nitroaromatics and cyclo ketones in sea water' by gas chromatography coupled with activated carbon fiber solid-phase micro-extraction].

    Ma, Hanna; Zhu, Mengya; Wang, Yalin; Sun, Tonghua; Jia, Jinping

    2009-05-01

    A gas chromatography (GC) coupled with solid-phase micro-extraction using a special activated carbon fiber (ACF) was developed for the analysis of 6 nitroaromatics and cyclic ketones, nitrobenzene (NB), 1,3-dinitrobenzene (1,3-DNB), 2,4-dinitrotoluene (2,4-DNT), 2,6-dinitrotoluene (2,6-DNT), isophorone, 1,4-naphthaquinone (1,4-NPQ), in sea water samples. The sample was extracted for 30 min under saturation of NaCl at 1,500 r/min and 60 degrees C in head space. The desorption was performance at 280 degrees C for 2 min. The linear ranges were from 0.01 to 400 microg/L. The limits of detection (LODs) were 1.4 - 3.2 ng/L. This method has been successfully applied to the determination of nitroaromatics and cyclic ketones in the sea water samples obtained from East China Sea. The concentrations of nitrobenzene, 1,3-dinitrobenzene and 2,6-dinitrotoluene in the sea water sample were 0.756, 0.944, 0.890 microg/L, respectively. The recoveries were 86.3% - 101.8% with the relative standard deviations (RSDs) of 3.7% -7.8%. The method is suitable for analyzing nitroaromatics and cyclic ketones at low concentration levels in sea water samples.

  8. Trace determination of safranin O dye using ultrasound assisted dispersive solid-phase micro extraction: Artificial neural network-genetic algorithm and response surface methodology.

    Dil, Ebrahim Alipanahpour; Ghaedi, Mehrorang; Asfaram, Arash; Mehrabi, Fatemeh; Bazrafshan, Ali Akbar; Ghaedi, Abdol Mohammad

    2016-11-01

    In this study, ultrasound assisted dispersive solid-phase micro extraction combined with spectrophotometry (USA-DSPME-UV) method based on activated carbon modified with Fe2O3 nanoparticles (Fe2O3-NPs-AC) was developed for pre-concentration and determination of safranin O (SO). It is known that the efficiency of USA-DSPME-UV method may be affected by pH, amount of adsorbent, ultrasound time and eluent volume and the extent and magnitude of their contribution on response (in term of main and interaction part) was studied by using central composite design (CCD) and artificial neural network-genetic algorithms (ANN-GA). Accordingly by adjustment of experimental conditions suggested by ANN-GA at pH 6.5, 1.1mg of adsorbent, 10min ultrasound and 150μL of eluent volume led to achievement of best operation performance like low LOD (6.3ngmL(-1)) and LOQ (17.5ngmL(-1)) in the range of 25-3500ngmL(-1). In following stage, the SO content in real water and wastewater samples with recoveries between 93.27-99.41% with RSD lower than 3% was successfully determined. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Monitoring of gamma radiolytic degradation products of methoxychlor pesticide in water by solid phase micro-extraction using hplc and GC-MS (abstract)

    Butt, S.B.; Zafar, A.

    2011-01-01

    Monitoring, removal and management of toxic chemicals is an essential area of study regarding sustainable progress. Different approaches are adopted to eliminate these water born toxics from water and waste water. Among these gamma radiolytic is an emerging option. This ionization radiation generates highly reactive radicals that reacts with pollutants and hence eliminates these. A solid-phase micro-extraction (SPME) procedure has been developed for the successful preconcentration of organic pollutant irradiated water. A SPME fused-silica fiber coated with Polyacrylate was used as a probe to extract the organic pollutant after irradiation. In this reference, degradation of priority organic pollutant methoxychlor (1, 1, 1-Trichloro 2, 2-bis (p-methoxyphenyl) ethane, in water by gamma irradiation under varied experimental conditions has been investigated. The degree of gamma radiolytic degradation was monitored by HPLC-UV and GC-MS. For 4 kGy and 5 kGy gamma radiation dose at a rate of 200 kGyh/sup -1/ greater or equal to 95 % and 98 % MXC was degraded respectively. The degradation products were identified by Mass Spectrometry after comparing their MS spectras with the NIST 98 library. The major degradation occurs via dechlorination, dehydro chlorination, by the detachment of methoxyphenyl from MXC and by interaction of other radicals generated by the water radiolysis. (author)

  10. Speciation analysis of organotin compounds in human urine by headspace solid-phase micro-extraction and gas chromatography with pulsed flame photometric detection.

    Valenzuela, Aníbal; Lespes, Gaëtane; Quiroz, Waldo; Aguilar, Luis F; Bravo, Manuel A

    2014-07-01

    A new headspace solid-phase micro-extraction (HS-SPME) method followed by gas chromatography with pulsed flame photometric detection (GC-PFPD) analysis has been developed for the simultaneous determination of 11 organotin compounds, including methyl-, butyl-, phenyl- and octyltin derivates, in human urine. The methodology has been validated by the analysis of urine samples fortified with all analytes at different concentration levels, and recovery rates above 87% and relative precisions between 2% and 7% were obtained. Additionally, an experimental-design approach has been used to model the storage stability of organotin compounds in human urine, demonstrating that organotins are highly degraded in this medium, although their stability is satisfactory during the first 4 days of storage at 4 °C and pH=4. Finally, this methodology was applied to urine samples collected from harbor workers exposed to antifouling paints; methyl- and butyltins were detected, confirming human exposure in this type of work environment. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. High performance preconcentration of inorganic Se species by dispersive micro-solid phase extraction with a nanosilica-ionic liquid hybrid material

    Llaver, Mauricio; Coronado, Eduardo A.; Wuilloud, Rodolfo G.

    2017-12-01

    A highly sensitive and efficient dispersive micro-solid phase extraction (D-μ-SPE) method was developed for inorganic Se speciation analysis. A novel ionic liquid (IL)-nanomaterial hybrid consisting of 1-dodecyl-3-methylimidazolium bromide-functionalized nanosilica was used for the efficient retention of Se(IV) complexed with ammonium pyrrolidine dithiocarbamate, followed by elution with an ethyl acetate/Triton X-114 mixture and determination by electrothermal atomic absorption spectroscopy. The Se(VI) species was selectively determined by difference between total inorganic Se and Se(IV) after pre-reduction. The IL-nanomaterial hybrid was characterized by Fourier transform infrared spectroscopy and transmission electronic microscopy. Likewise, Se(IV) sorption capacity of the retention material and maximum amount of IL loaded on its surface were determined. Several factors concerning the functionalization, extraction and elution steps were optimized, yielding a 100% extraction efficiency for Se(IV) under optimal conditions. A limit of detection of 1.1 ng L- 1, a relative standard deviation of 5.7% and a 110-fold enhancement factor were obtained. The D-μ-SPE method was successfully applied to several water samples from different origins and compositions, including rain, tap, underground, river and sea.

  12. Preparation and characterization of sodium dodecyl sulfate doped polypyrrole solid phase micro extraction fiber and its application to endocrine disruptor pesticide analysis.

    Korba, Korcan; Pelit, Levent; Pelit, Füsun Okçu; Ozdokur, K Volkan; Ertaş, Hasan; Eroğlu, Ahmet E; Ertaş, F Nil

    2013-06-15

    A robust in house solid-phase micro extraction (SPME) surface has been developed for the headspace (HS)-SPME determination of endocrine disruptor pesticides, namely, Chlorpyrifos, Penconazole, Procymidone, Bromopropylate and Lambda-Cyhalothrin in wine sample by using sodium dodecylsulfate doped polypyrrole SPME fiber. Pyrrole monomer was electrochemically polymerized on a stainless steel wire in laboratory conditions in virtue of diminishing the cost and enhancing the analyte retention on its surface to exert better selectivity and hence the developed polymerized surface could offer to analyst to exploit it as a fiber in headspace SPME analysis. The parameters, mainly, adsorption temperature and time, desorption temperature, stirring rate and salt amount were optimized to be as 70°C and 45min, 200°C, 600rpm and 10gL(-1), respectively. Limit of detection was estimated in the range of 0.073-1.659ngmL(-1) for the pesticides studied. The developed method was applied in to red wine sample with acceptable recovery values (92-107%) which were obtained for these selected pesticides. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. In-Vial Micro-Matrix-Solid Phase Dispersion for the Analysis of Fragrance Allergens, Preservatives, Plasticizers, and Musks in Cosmetics

    Maria Celeiro

    2014-07-01

    Full Text Available Fragrance allergens, preservatives, plasticizers, and synthetic musks are usually present in cosmetic and personal care products formulations and many of them are subjected to use restrictions or labeling requirements. Matrix solid-phase dispersion (MSPD is a very suitable analytical technique for the extraction of these compounds providing a simple, low cost sample preparation, and the possibility of performing both extraction and clean-up in one step, reducing possible contamination and analyte losses. This extraction technique has been successfully applied to many cosmetics ingredients allowing obtaining quantitative recoveries. A new very simple micro-MSPD procedure performing the disruption step in a vial is proposed for the gas chromatography-mass spectrometry (GC-MS analysis of 66 chemicals usually present in cosmetics and personal care products. The method was validated showing general recoveries between 80% and 110%, relative standard deviation (RSD values lower than 15%, and limits of detection (LODs below 30 ng·g−1. The validated method was applied to a broad range of cosmetics and personal care products, including several products intended for baby care.

  14. Determination of phthalate esters from environmental water samples by micro-solid-phase extraction using TiO2 nanotube arrays before high-performance liquid chromatography.

    Zhou, Qingxiang; Fang, Zhi; Liao, Xiangkun

    2015-07-01

    We describe a highly sensitive micro-solid-phase extraction method for the pre-concentration of six phthalate esters utilizing a TiO2 nanotube array coupled to high-performance liquid chromatography with a variable-wavelength ultraviolet visible detector. The selected phthalate esters included dimethyl phthalate, diethyl phthalate, dibutyl phthalate, butyl benzyl phthalate, bis(2-ethylhexyl)phthalate and dioctyl phthalate. The factors that would affect the enrichment, such as desorption solvent, sample pH, salting-out effect, extraction time and desorption time, were optimized. Under the optimum conditions, the linear range of the proposed method was 0.3-200 μg/L. The limits of detection were 0.04-0.2 μg/L (S/N = 3). The proposed method was successfully applied to the determination of six phthalate esters in water samples and satisfied spiked recoveries were achieved. These results indicated that the proposed method was appropriate for the determination of trace phthalate esters in environmental water samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Evaluation of graphene-based sorbent in the determination of polar environmental contaminants in water by micro-solid phase extraction-high performance liquid chromatography.

    Naing, Nyi Nyi; Li, Sam Fong Yau; Lee, Hian Kee

    2016-01-04

    A facile method of extraction using porous membrane protected micro-solid phase extraction (μ-SPE) with a graphene-based sorbent followed by high performance liquid chromatography-ultraviolet detector was developed. The reduced graphene oxide (r-GO) (1mg), synthesized from graphite oxide, was enclosed in a polypropylene bag representing the μ-SPE device, which was used for the extraction of estrogens such as estrone, 17β-estradiol, 17α-ethynylestradiol and diethylstilbestrol in water. The r-GO obtained was identified and characterized by Fourier transform infrared, transmission electron microscopy, scanning electron microscopy and thermogravimetric analysis. The sorbent was loaded with sodium dodecyl sulfate by sonication to prevent agglomeration in aqueous solution. With this method, low limits of detection of between 0.24 and 0.52 ng L(-1) were achieved. For estrogen analysis a linear calibration range of 0.01-100 μg L(-1) was obtained, with the coefficients of determination (r(2)) higher than 0.992. This proposed method was successfully applied to determine estrogens in water. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Solid-phase microextraction

    Nilsson, Torben

    The objective of this study has been to develop new analytical methods using the rapid, simple and solvent-free extraction technique solid-phase microextraction (SPME) for the quantitative analysis of organic pollutants at trace level in drinking water and environmental samples. The dynamics...... of SPME were examined for halogenated and non-halogenated volatile hydrocarbons, and a standard method for their quantitative analysis in aqueous samples was developed and validated in inter-laboratory studies on the basis of reference material and in comparison with the traditional methods....... The influences of some possible interferences on the SPME process were examined, and new SPME probes were tested for the in situ monitoring of groundwater pollutants. Inter-laboratory studies were carried out also for the validation of SPME for the quantitative analysis of organochlorine, organonitrogen...

  17. A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids.

    Yahaya, Noorfatimah; Sanagi, Mohd Marsin; Abd Aziz, Noorizan; Wan Ibrahim, Wan Aini; Nur, Hadi; Loh, Saw Hong; Kamaruzaman, Sazlinda

    2017-02-01

    A rapid dispersive micro-solid phase extraction (D-μ-SPE) combined with LC/MS/MS method was developed and validated for the determination of ketoconazole and voriconazole in human urine and plasma samples. Synthesized mesoporous silica MCM-41 was used as sorbent in d-μ-SPE of the azole compounds from biological fluids. Important D-μ-SPE parameters, namely type desorption solvent, extraction time, sample pH, salt addition, desorption time, amount of sorbent and sample volume were optimized. Liquid chromatographic separations were carried out on a Zorbax SB-C 18 column (2.1 × 100 mm, 3.5 μm), using a mobile phase of acetonitrile-0.05% formic acid in 5 mm ammonium acetate buffer (70:30, v/v). A triple quadrupole mass spectrometer with positive ionization mode was used for the determination of target analytes. Under the optimized conditions, the calibration curves showed good linearity in the range of 0.1-10,000 μg/L with satisfactory limit of detection (≤0.06 μg/L) and limit of quantitation (≤0.3 μg/L). The proposed method also showed acceptable intra- and inter-day precisions for ketoconazole and voriconazole from urine and human plasma with RSD ≤16.5% and good relative recoveries in the range 84.3-114.8%. The MCM-41-D-μ-SPE method proved to be rapid and simple and requires a small volume of organic solvent (200 μL); thus it is advantageous for routine drug analysis. Copyright © 2016 John Wiley & Sons, Ltd.

  18. Sampling and analytical procedures for the determination of VOCs released into air from natural and anthropogenic sources: A comparison between SPME (Solid Phase Micro Extraction) and ST (Solid Trap) methods

    Tassi, F.; Capecchiacci, F.; Buccianti, A.; Vaselli, O.

    2012-01-01

    In the present study, two sampling and analytical methods for VOC determination in fumarolic exhalations related to hydrothermal-magmatic reservoirs in volcanic and geothermal areas and biogas released from waste landfills were compared: (a) Solid Traps (STs), consisting of three phase (Carboxen B, Carboxen C and Carbosieve S111) absorbent stainless steel tubes and (b) Solid Phase Micro Extraction (SPME) fibers, composed of DiVinylBenzene (DVB), Carboxen and PolyDimethylSiloxane. These techniques were applied to pre-concentrate VOCs discharged from: (i) low-to-high temperature fumaroles collected at Vulcano Island, Phlegrean Fields (Italy), and Nisyros Island (Greece), (ii) recovery wells in a solid waste disposal site located near Florence (Italy). A glass condensing system cooled with water was used to collect the dry fraction of the fumarolic gases, in order to allow more efficient VOC absorption avoiding any interference by water vapor and acidic gases, such as SO 2 , H 2 S, HF and HCl, typically present at relatively high concentrations in these fluids. Up to 37 organic species, in the range of 40–400 m/z, were determined by coupling gas chromatography to mass spectrometry (GC–MS). This study shows that the VOC compositions of fumaroles and biogas determined via SPME and ST are largely consistent and can be applied to the analysis of VOCs in gases released from different natural and anthropogenic environments. The SPME method is rapid and simple and more appropriate for volcanic and geothermal emissions, where VOCs are present at relatively high concentrations and prolonged gas sampling may be hazardous for the operator. The ST method, allowing the collection of large quantities of sample, is to be preferred to analyze the VOC composition of fluids from diffuse emissions and air, where these compounds are present at relatively low concentrations.

  19. Trace and ultratrace determination of heavy metal ions by energy-dispersive X-ray fluorescence spectrometry using graphene as solid sorbent in dispersive micro solid-phase extraction

    Kocot, Karina; Sitko, Rafal, E-mail: rafal.sitko@us.edu.pl

    2014-04-01

    In this paper, the adsorptive properties of graphene nanosheets were used for simultaneous preconcentration of cobalt, nickel, copper and lead ions from water samples. The developed methodology is based on dispersive micro-solid phase extraction (DMSPE) which is miniaturized and a simplified version of classical solid phase extraction technique. In proposed procedure only 200 μL of suspension containing graphene (0.2 mg), ammonium pyrrolidine dithiocarbamate (APDC) (0.8 mg) and Triton-X-100 (0.1 mg) is rapidly injected to 50 mL of water sample. Then, graphene nanosheets with adsorbed metal-APDC chelates are collected on membrane filter and measured using energy-dispersive X-ray fluorescence (EDXRF) spectrometry. The various parameters including pH, amount of APDC, sample volume, amount of Triton-X-100 and sorption time were optimized in order to obtain the best recoveries. The experiment shows that Co, Ni, Cu and Pb can be simultaneously preconcentrated at pH of 5 with high recoveries (97%, 96%, 99% and 96% for Co, Ni, Cu and Pb, respectively) and very good precision (RSDs within 2.6–3.4%). Due to the excellent enrichment factors ranging from 400 to 2500 the proposed DMSPE–EDXRF procedure offers low detection limits. For optimized measurement conditions (voltage and current of X-ray tube, primary beam filter) the detection limits are even 0.08, 0.07, 0.08 and 0.20 ng mL{sup −1} for Co, Ni, Cu and Pb, respectively. - Highlights: • Excellent detection limits using EDXRF • A new preconcentration procedure combining DMSPE and EDXRF measurement • Graphene as a promising and efficient solid sorbent in DMSPE • Simple, fast, inexpensive and environmental friendly method.

  20. Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

    Krawczyk-Coda, Magdalena

    2017-03-01

    In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

  1. Simple determination of hydrazine in waste water by headspace solid-phase micro extraction and gas chromatography-tandem mass spectrometry after derivatization with trifluoro pentanedione.

    Oh, Jin-Aa; Shin, Ho-Sang

    2017-01-15

    A headspace solid-phase micro extraction (HS-SPME) and gas chromatography-tandem mass spectrometric (GC-MS/MS) method is described to detect hydrazine after derivatization with 1,1,1-trifluoro-2,4-pentanedione (1,1,1-TFPD) to 3-methyl-5-(trifluoromethyl) pyrazole in industrial waste water. The following optimal HS-SPME conditions were used: 85 μm-carboxen-polydimethylsiloxane fibre, 100 mg L -1 TFPD, saturated NaCl, an extraction/derivatization temperature of 80 °C, a heating time of 40 min, and a pH of 9.5. Under the established conditions, the detection and quantification limits were 0.002 μg L -1 and 0.007 μg L -1  by using 5 mL of waste water and the intra- and inter-day relative standard deviations were less than 10.2% at concentrations of 0.02 and 0.1 μg L -1 . The calibration curve showed good linearity, with r 2  = 0.998; the accuracy was in the range of 98.0-103%; and the precision of the assay was less than 10.2% in industrial waste water. Hydrazine was detected over a concentration range of 0.011-0.074 μg L -1 in 5 of 20 waste water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Measurement of non-enteric emission fluxes of volatile fatty acids from a California dairy by solid phase micro-extraction with gas chromatography/mass spectrometry

    Alanis, Phillip; Sorenson, Mark; Beene, Matt; Krauter, Charles; Shamp, Brian; Hasson, Alam S.

    Dairies are a major source of volatile organic compounds (VOCs) in California's San Joaquin Valley; a region that experiences high ozone levels during summer. Short-chain carboxylic acids, or volatile fatty acids (VFAs), are believed to make up a large fraction of VOC emissions from these facilities, although there are few studies to substantiate this. In this work, a method using a flux chamber coupled to solid phase micro-extraction (SPME) fibers followed by analysis using gas chromatography/mass spectrometry was developed to quantify emissions of six VFAs (acetic acid, propanoic acid, butanoic acid, pentanoic acid, hexanoic acid and 3-methyl butanoic acid) from non-enteric sources. The technique was then used to quantify VFA fluxes from a small dairy located on the campus of California State University Fresno. Both animal feed and animal waste are found to be major sources of VFAs, with acetic acid contributing 70-90% of emissions from the sources tested. Measured total acid fluxes during spring (with an average temperature of 20 °C) were 1.84 ± 0.01, 1.06 ± 0.08, (1.3 ± 0.5) × 10 -2, (1.7 ± 0.2) × 10 -2 and (1.2 ± 0.5) × 10 -2 g m -2 h -1 from silage, total mixed rations, flushing lane, open lot and lagoon sources, respectively. VFA emissions from the sources tested total 390 ± 80 g h -1. The data indicate high fluxes of VFAs from dairy facilities, but differences in the design and operation of dairies in the San Joaquin Valley as well as seasonal variations mean that additional measurements must be made to accurately determine emissions inventories for the region.

  3. An absorbing microwave micro-solid-phase extraction device used in non-polar solvent microwave-assisted extraction for the determination of organophosphorus pesticides

    Wang Ziming; Zhao Xin; Xu Xu; Wu Lijie; Su Rui; Zhao Yajing; Jiang Chengfei; Zhang Hanqi; Ma Qiang; Lu Chunmei; Dong Deming

    2013-01-01

    Highlights: ► An absorbing microwave μ-SPE device packed with activated carbon was used. ► Absorbing microwave μ-SPE device was made and used to enrich the analytes. ► Absorbing microwave μ-SPE device was made and used to heat samples directly. ► MAE-μ-SPE was applied to the extraction of OPPs with non-polar solvent only. - Abstract: A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction (μ-SPE), was developed for the extraction of ten organophosphorus pesticides in vegetable and fruit samples. Without adding any polar solvent, only one kind of non-polar solvent (hexane) was used as extraction solvent in the whole extraction step. Absorbing microwave μ-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in μ-SPE, but also the microwave absorption medium. Some experimental parameters effecting on extraction efficiency was investigated and optimized. 1.0 g of sample, 8 mL of hexane and three absorbing microwave μ-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60 °C for 10 min. The extracts obtained by MAE-μ-SPE were directly analyzed by GC–MS without any clean-up process. The recoveries were in the range of 93.5–104.6%, and the relative standard deviations were lower than 8.7%.

  4. An absorbing microwave micro-solid-phase extraction device used in non-polar solvent microwave-assisted extraction for the determination of organophosphorus pesticides

    Wang Ziming, E-mail: wangziming@jlu.edu.cn [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); College of Environment and Resources, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); Zhao Xin; Xu Xu; Wu Lijie; Su Rui; Zhao Yajing; Jiang Chengfei; Zhang Hanqi [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); Ma Qiang [Chinese Academy of Inspection and Quarantine, Beijing 100123 (China); Lu Chunmei [College of Technology Center, Jilin Entry-Exit Inspection and Quarantine Bureau, Changchun 130062 (China); Dong Deming [College of Environment and Resources, Jilin University, 2699 Qianjin Street, Changchun 130012 (China)

    2013-01-14

    Highlights: Black-Right-Pointing-Pointer An absorbing microwave {mu}-SPE device packed with activated carbon was used. Black-Right-Pointing-Pointer Absorbing microwave {mu}-SPE device was made and used to enrich the analytes. Black-Right-Pointing-Pointer Absorbing microwave {mu}-SPE device was made and used to heat samples directly. Black-Right-Pointing-Pointer MAE-{mu}-SPE was applied to the extraction of OPPs with non-polar solvent only. - Abstract: A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction ({mu}-SPE), was developed for the extraction of ten organophosphorus pesticides in vegetable and fruit samples. Without adding any polar solvent, only one kind of non-polar solvent (hexane) was used as extraction solvent in the whole extraction step. Absorbing microwave {mu}-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in {mu}-SPE, but also the microwave absorption medium. Some experimental parameters effecting on extraction efficiency was investigated and optimized. 1.0 g of sample, 8 mL of hexane and three absorbing microwave {mu}-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60 Degree-Sign C for 10 min. The extracts obtained by MAE-{mu}-SPE were directly analyzed by GC-MS without any clean-up process. The recoveries were in the range of 93.5-104.6%, and the relative standard deviations were lower than 8.7%.

  5. Extraction and Identification of Volatile Components of Two Salvia Species Native to Iran (Salvia limbata and S. multicaulis by Using Solid Phase Micro-Extraction Method

    S. Ramezani

    2016-02-01

    Full Text Available Introduction: There are 58 species belonging to sage genus as annual and perennial plant in different regions of Iran that 18 species of them are endemic to Iran and they have different medicinal properties such as antibiotic, sedative, carminative, antispasmodic and commonly used in treatment of respiratory problems: infections, cough, cold and sore throat and cosmetics industries. The present study has aimed to evaluate the composition of essential oils achieved by Solid Phase Micro-Extraction method from aerial parts of two Salvia species native to Iran: Salvia limbata and Salvia multicaulis. Materials and Methods: The experiments were carried out at the Research Station of Agriculture College, TarbiatModares University in Tehran, Iran during the years 2011-2013. The seeds of Salvialimbata and Salvia multicauliswere collected in Ardabil and Isfahan provinces in 2009. The seeds were sown in planting trays(filled with soil and cocopeat 1:1 under controlled greenhouse condition (temperature: 26±1°C, light: 3000 lux, relative humidity: 65% in the last week of February 2011. The soil of experimental pots (soil and coco peat 2:1 was a clay silt loam with pH of 7.4. After two months,seedlings with uniform height and stem diameter with two true leaves were transferred to a growth chamber adjusted to 30/20 °C, 50% relative humidity, light intensity of approximately 3000 Lux and 16 h photoperiod.Aerial parts of two cultivated plantsincludingSalvia limbata and Salvia multicaulisat flowering stage were harvested in June 2012 and kept at 80°C until further experiments. Volatile compounds were extracted by solid phase micro-extraction (SPME method for the first time in Iran for these species. Before the SPME, the leaves lyophilized and then were used. The optimization of SPME extraction and desorption conditions were performed by analyzing dried leaves of Salvia officinalis L., used as the matrix. The sample preparation procedure was as: 15 mg of dried

  6. A hydrazone covalent organic polymer based micro-solid phase extraction for online analysis of trace Sudan dyes in food samples.

    Zhang, Chengjiang; Li, Gongke; Zhang, Zhuomin

    2015-11-06

    Covalent organic polymers (COPs) connected by covalent bonds are a new class of porous network materials with large surface area and potential superiority in sample pretreatment. In this study, a new hydrazone linked covalent organic polymer (HL-COP) adsorbent was well-designed and synthesized based on a simple Schiff-base reaction. The condensation of 1,4-phthalaldehyde and 1,3,5-benzenetricarbohydrazide as organic building blocks led to the synthesis of HL-COP with uniform particle size and good adsorption performance. This HL-COP adsorbent with high hydrophobic property and rich stacking π electrons contained abundant phenyl rings and imine (CN) groups throughout the entire molecular framework. The adsorption mechanism was explored and discussed based on π-π affinity, hydrophobic effect, hydrogen bonding and electron-donor-acceptor (EDA) interaction, which contributed to its strong recognition affinity to target compounds. Enrichment factors were 305-757 for six Sudan dyes by HL-COP micro-solid phase extraction (μ-SPE), indicating its remarkable preconcentration ability. Furthermore, the adsorption amounts by HL-COP μ-SPE were 1.0-11.0 folds as those by three commonly used commercial adsorbents. Then, HL-COP was applied as adsorbent of online μ-SPE coupled with high performance liquid chromatography (HPLC) for enrichment and analysis of trace Sudan dyes in food samples with detection limit of 0.03-0.15μg/L. The method was successfully applied for online analysis of chilli powder and sausage samples. Sudan II and Sudan III in one positive chilli powder sample were actually found and determined with concentrations of 8.3 and 6.8μg/kg, respectively. The recoveries of chilli powder and sausage samples were in range of 75.8-108.2% and 73.8-112.6% with relative standard deviations of 1.2-8.5% and 1.9-9.4% (n=5), respectively. The proposed method was accurate, reliable and convenient for the online simultaneous analysis of trace Sudan dyes in food samples

  7. Development of a multianalyte method based on micro-matrix-solid-phase dispersion for the analysis of fragrance allergens and preservatives in personal care products.

    Celeiro, Maria; Guerra, Eugenia; Lamas, J Pablo; Lores, Marta; Garcia-Jares, Carmen; Llompart, Maria

    2014-05-30

    An effective, simple and low cost sample preparation method based on matrix solid-phase dispersion (MSPD) followed by gas chromatography-mass spectrometry (GC-MS) or gas chromatography-triple quadrupole-mass spectrometry (GC-MS/MS) has been developed for the rapid simultaneous determination of 38 cosmetic ingredients, 25 fragrance allergens and 13 preservatives. All target substances are frequently used in cosmetics and personal care products and they are subjected to use restrictions or labeling requirements according to the EU Cosmetic Directive. The extraction procedure was optimized on real non-spiked rinse-off and leave-on cosmetic products by means of experimental designs. The final miniaturized process required the use of only 0.1g of sample and 1 mL of organic solvent, obtaining a final extract ready for analysis. The micro-MSPD method was validated showing satisfactory performance by GC-MS and GC-MS/MS analysis. The use of GC coupled to triple quadrupole mass detection allowed to reach very low detection limits (low ng g(-1)) improving, at the same time, method selectivity. In an attempt to improve the chromatographic analysis of preservatives, the inclusion of a derivatization step was also assessed. The proposed method was applied to a broad range of cosmetics and personal care products (shampoos, body milk, moisturizing milk, toothpaste, hand creams, gloss lipstick, sunblock, deodorants and liquid soaps among others), demonstrating the extended use of these substances. The concentration levels were ranging from the sub parts per million to the parts per mill. The number of target fragrance allergens per samples was quite high (up to 16). Several fragrances (linalool, farnesol, hexylcinnamal, and benzyl benzoate) have been detected at levels >0.1% (1,000 μg g(-1)). As regards preservatives, phenoxyethanol was the most frequently found additive reaching quite high concentration (>1,500 μg g(-1)) in five cosmetic products. BHT was detected in eight

  8. Mesoporous silica based MCM-41 as solid-phase extraction sorbent combined with micro-liquid chromatography-quadrupole-mass spectrometry for the analysis of pharmaceuticals in waters.

    Dahane, S; Martínez Galera, M; Marchionni, M E; Socías Viciana, M M; Derdour, A; Gil García, M D

    2016-05-15

    This paper reports the first application of the silica based mesoporous material MCM-41 as a sorbent in solid phase extraction, to pre-concentrate pharmaceuticals of very different polarity (atenolol, nadolol, pindolol, timolol, bisoprolol, metoprolol, betaxolol, ketoprofen, naproxen, ibuprofen, diclofenac, tolfenamic acid, flufenamic acid and meclofenamic acid) in surface waters. The analytes were extracted from 100mL water samples at pH 2.0 (containing 10(-3) mol/L of sodium chloride) by passing the solution through a cartridge filled with 100 mg of MCM-41. Following elution, the pharmaceuticals were determined by micro-liquid chromatography and triple quadrupole-mass spectrometry. Two selected reaction monitoring transitions were monitored per compound, the most intense one being used for quantification and the second one for confirmation. Matrix effect was found in real waters for most analytes and was overcome using the standard addition method, which compared favorably with the matrix matched calibration method. The detection limits in solvent (acetonitrile:water 10:90, v/v) ranged from 0.01 to 1.48 μg/L and in real water extracts from 0.10 to 3.85 μg/L (0.001-0.0385 μg/L in the water samples). The quantitation limits in solvent were in the range 0.02-4.93 μg/L, whereas in real water extracts were between 0.45 and 10.00 μg/L (0.0045 and 0.1000 μg/L in the water samples). When ultrapure water samples were spiked at two concentration levels of each pharmaceutical (0.1 and 0.2 μg/L) and quantified using solvent based calibration graphs, recoveries were near 100%. However, recoveries for most pharmaceuticals were comparable or better than de described above, when river water samples (spiked at the same concentration levels) were quantified by the standard addition method and slightly worse using the matrix matched calibration method. Five real samples (two rivers, one dam and two fountain water samples) were analyzed by the developed method, atenolol

  9. Simple and accurate measurement of carbamazepine in surface water by use of porous membrane-protected micro-solid-phase extraction coupled with isotope dilution mass spectrometry

    Teo, Hui Ling [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543 (Singapore); Wong, Lingkai [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Liu, Qinde, E-mail: liu_qinde@hsa.gov.sg [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Teo, Tang Lin; Lee, Tong Kooi [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Lee, Hian Kee, E-mail: chmleehk@nus.edu.sg [Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543 (Singapore)

    2016-03-17

    To achieve fast and accurate analysis of carbamazepine in surface water, we developed a novel porous membrane-protected micro-solid-phase extraction (μ-SPE) method, followed by liquid chromatography-isotope dilution tandem mass spectrometry (LC-IDMS/MS) analysis. The μ-SPE device (∼0.8 × 1 cm) was fabricated by heat-sealing edges of a polypropylene membrane sheet to devise a bag enclosing the sorbent. The analytes (both carbamazepine and isotope-labelled carbamazepine) were first extracted by μ-SPE device in the sample (10 mL) via agitation, then desorbed in an organic solvent (1 mL) via ultrasonication. Several parameters such as organic solvent for pre-conditioning of μ-SPE device, amount of sorbent, adsorption time, and desorption solvent and time were investigated to optimize the μ-SPE efficiency. The optimized method has limits of detection and quantitation estimated to be 0.5 ng L{sup −1} and 1.6 ng L{sup −1}, respectively. Surface water samples spiked with different amounts of carbamazepine (close to 20, 500, and 1600 ng L{sup −1}, respectively) were analysed for the validation of method precision and accuracy. Good precision was obtained as demonstrated by relative standard deviations of 0.7% for the samples with concentrations of 500 and 1600 ng kg{sup −1}, and 5.8% for the sample with concentration of 20 ng kg{sup −1}. Good accuracy was also demonstrated by the relative recoveries in the range of 96.7%–103.5% for all samples with uncertainties of 1.1%–5.4%. Owing to the same chemical properties of carbamazepine and isotope-labelled carbamazepine, the isotope ratio in the μ-SPE procedure was accurately controlled. The use of μ-SPE coupled with IDMS analysis significantly facilitated the fast and accurate measurement of carbamazepine in surface water. - Highlights: • μ-SPE coupled with IDMS for the measurement of carbamazepine. • The method is the first report of coupling μ-SPE with IDMS. • μ-SPE is fast, time

  10. Parameters optimization using experimental design for headspace solid phase micro-extraction analysis of short-chain chlorinated paraffins in waters under the European water framework directive.

    Gandolfi, F; Malleret, L; Sergent, M; Doumenq, P

    2015-08-07

    The water framework directives (WFD 2000/60/EC and 2013/39/EU) force European countries to monitor the quality of their aquatic environment. Among the priority hazardous substances targeted by the WFD, short chain chlorinated paraffins C10-C13 (SCCPs), still represent an analytical challenge, because few laboratories are nowadays able to analyze them. Moreover, an annual average quality standards as low as 0.4μgL(-1) was set for SCCPs in surface water. Therefore, to test for compliance, the implementation of sensitive and reliable analysis method of SCCPs in water are required. The aim of this work was to address this issue by evaluating automated solid phase micro-extraction (SPME) combined on line with gas chromatography-electron capture negative ionization mass spectrometry (GC/ECNI-MS). Fiber polymer, extraction mode, ionic strength, extraction temperature and time were the most significant thermodynamic and kinetic parameters studied. To determine the suitable factors working ranges, the study of the extraction conditions was first carried out by using a classical one factor-at-a-time approach. Then a mixed level factorial 3×2(3) design was performed, in order to give rise to the most influent parameters and to estimate potential interactions effects between them. The most influent factors, i.e. extraction temperature and duration, were optimized by using a second experimental design, in order to maximize the chromatographic response. At the close of the study, a method involving headspace SPME (HS-SPME) coupled to GC/ECNI-MS is proposed. The optimum extraction conditions were sample temperature 90°C, extraction time 80min, with the PDMS 100μm fiber and desorption at 250°C during 2min. Linear response from 0.2ngmL(-1) to 10ngmL(-1) with r(2)=0.99 and limits of detection and quantification, respectively of 4pgmL(-1) and 120pgmL(-1) in MilliQ water, were achieved. The method proved to be applicable in different types of waters and show key advantages, such

  11. Magnetic nanoparticles based dispersive micro-solid-phase extraction as a novel technique for coextraction of acidic and basic drugs from biological fluids and waste water.

    Asgharinezhad, Ali Akbar; Mollazadeh, Narges; Ebrahimzadeh, Homeira; Mirbabaei, Fatemeh; Shekari, Nafiseh

    2014-04-18

    The coextraction of acidic and basic drugs from different samples is a considerable and disputable concept in sample preparation strategies. In this study, for the first time, simultaneous extraction of acidic and basic drugs with magnetic nanoparticles based dispersive micro-solid phase extraction followed by high performance liquid chromatography-ultraviolet detection was introduced. Cetyltrimethyl ammonium bromide-coated Fe3O4@decanoic acid as an efficient sorbent was successfully applied to adsorb diclofenac (DIC) as an acidic and diphenhydramine (DPH) as a basic model compound. First, appropriate amount of synthetic Fe3O4@decanoic acid nanoparticles was added to aqueous solution of drugs. After adjusting the pH of the solution, cetyltrimethyl ammonium bromide (CTAB) was added to the mixture being stirred at a constant rate. After the adsorption of drugs and decantation of supernatant with a magnetic field, the sorbent was eluted with methanol by fierce vortex. The parameters affecting the extraction efficiency were optimized and obtained as: pH of the sample=9, concentration of CTAB=0.2mmolL(-1), amount of sorbent=10mg, extraction time=5min, no salt addition to sample, type and volume of the eluent=50μL methanol, and desorption time=1min. Under the optimum conditions detection limits and linear dynamic ranges were achieved in the range of 1.8-3.0, 5-1500μgL(-1) for DPH and 1.5-3.5, 5-1500μgL(-1) for DIC, respectively. The percent of extraction recovery and relative standard deviations (n=5) were in the range of 47.3-60, 5.2-9.0 for DPH and 64-76.7, 5.1-5.8 for DIC, respectively. Ultimately, the applicability of the method was successfully confirmed by the extraction and determination of DIC and DPH in human urine, plasma and waste water samples in the range of microgram per liter and satisfactory results were obtained. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Cone-shaped membrane liquid phase micro extraction

    Hong, Heng See; Sanagi, M.M.; Ibrahim, W.A.W.; Naim, A.A.

    2008-01-01

    A novel sample pre-treatment technique termed cone-shaped membrane liquid phase micro extraction (CSM-LPME) was developed and combined with micro-liquid chromatography (micro-LC) for the determination of selected pesticides in water samples. Several important extraction parameters such as types of extraction solvent, agitation rate, pH value, total exposure time and effect of salt and humic acids were investigated and optimized. Enrichment factors of >50 folds were easily achieved within 20 min of extraction. The new developed method demonstrated an excellent performance in terms of speed, cost effectiveness, reproducibility, as well as exceptional low detection limits. Current work provides a great interest to further investigate on the applicability of the CSM-LPME technique in analytical chemistry and explores the possibility of replacing conventional extraction techniques such as soxhlet, solid phase extraction (SPE) and solid phase micro extraction (SPME). (author)

  13. Micro solid phase spectrophotometry in a sequential injection lab-on-valve platform for cadmium, zinc, and copper determination in freshwaters

    Santos, Inês C.; Mesquita, Raquel B.R.; Rangel, António O.S.S.

    2015-01-01

    This work describes the development of a solid phase spectrophotometry method in a μSI-LOV system for cadmium, zinc, and copper determination in freshwaters. NTA (Nitrilotriacetic acid) beads with 60–160 μm diameter were packed in the flow cell of the LOV for a μSPE column of 1 cm length. The spectrophotometric determination is based on the colourimetric reaction between dithizone and the target metals, previously retained on NTA resin. The absorbance of the coloured product formed is measured, at 550 nm, on the surface of the NTA resin beads in a solid phase spectrophotometry approach. The developed method presented preconcentration factors in the range of 11–21 for the metal ions. A LOD of 0.23 μg L"−"1 for cadmium, 2.39 μg L"−"1 for zinc, and 0.11 μg L"−"1 for copper and a sampling rate of 12, 13, and 15 h"−"1 for cadmium, zinc, and copper were obtained, respectively. The proposed method was successfully applied to freshwater samples. - Highlights: • Multi-parametric determination of cadmium, zinc, and copper at the μg L"−"1 level. • In-line metal ions preconcentration using NTA resin. • Minimization of matrix interferences by performing solid phase spectrometry in a SI-LOV platform. • Successful application to metal ions determination in freshwaters.

  14. An Effective Method to Detect Volatile Intermediates Generated in the Bioconversion of Coal to Methane by Gas Chromatography-Mass Spectrometry after In-Situ Extraction Using Headspace Solid-Phase Micro-Extraction under Strict Anaerobic Conditions.

    Liu, Jianmin; Wang, Baoyu; Tai, Chao; Wu, Li; Zhao, Han; Guan, Jiadong; Chen, Linyong

    2016-01-01

    Bioconversion of coal to methane has gained increased attention in recent decades because of its economic and environmental advantages. However, the mechanism of this process is difficult to study in depth, partly because of difficulties associated with the analysis of intermediates generated in coal bioconversion. In this investigation, we report on an effective method to analyze volatile intermediates generated in the bioconversion of coal under strict anaerobic conditions. We conduct in-situ extraction of intermediates using headspace solid-phase micro-extraction followed by detection by gas chromatography-mass spectrometry. Bioconversion simulation equipment was modified and combined with a solid-phase micro-extraction device. In-situ extraction could be achieved by using the combined units, to avoid a breakdown in anaerobic conditions and to maintain the experiment continuity. More than 30 intermediates were identified qualitatively in the conversion process, and the variation in trends of some typical intermediates has been discussed. Volatile organic acids (C2-C7) were chosen for a quantitative study of the intermediates because of their importance during coal bioconversion to methane. Fiber coating, extraction time, and solution acidity were optimized in the solid-phase micro-extraction procedure. The pressure was enhanced during the bioconversion process to investigate the influence of headspace pressure on analyte extraction. The detection limits of the method ranged from 0.0006 to 0.02 mmol/L for the volatile organic acids and the relative standard deviations were between 4.6% and 11.5%. The volatile organic acids (C2-C7) generated in the bioconversion process were 0.01-1.15 mmol/L with a recovery range from 80% to 105%. The developed method is useful for further in-depth research on the bioconversion of coal to methane.

  15. Solid-phase peptide synthesis

    Jensen, Knud Jørgen

    2013-01-01

    This chapter provides an introduction to and overview of peptide chemistry with a focus on solid-phase peptide synthesis. The background, the most common reagents, and some mechanisms are presented. This chapter also points to the different chapters and puts them into perspective.......This chapter provides an introduction to and overview of peptide chemistry with a focus on solid-phase peptide synthesis. The background, the most common reagents, and some mechanisms are presented. This chapter also points to the different chapters and puts them into perspective....

  16. Micro solid phase spectrophotometry in a sequential injection lab-on-valve platform for cadmium, zinc, and copper determination in freshwaters

    Santos, Inês C. [CBQF–Centro de Biotecnologia e Química Fina – Laboratório Associado, Escola Superior de Biotecnologia, Universidade Católica Portuguesa/Porto, Rua Arquiteto Lobão Vital, Apartado 2511, 4202-401 Porto (Portugal); Mesquita, Raquel B.R. [CBQF–Centro de Biotecnologia e Química Fina – Laboratório Associado, Escola Superior de Biotecnologia, Universidade Católica Portuguesa/Porto, Rua Arquiteto Lobão Vital, Apartado 2511, 4202-401 Porto (Portugal); Laboratório de Hidrobiologia, Instituto de Ciências Biomédicas Abel Salazar (ICBAS), Universidade do Porto, Rua de Jorge Viterbo Ferreira no. 228, 4050-313 Porto (Portugal); Rangel, António O.S.S., E-mail: arangel@porto.ucp.pt [CBQF–Centro de Biotecnologia e Química Fina – Laboratório Associado, Escola Superior de Biotecnologia, Universidade Católica Portuguesa/Porto, Rua Arquiteto Lobão Vital, Apartado 2511, 4202-401 Porto (Portugal)

    2015-09-03

    This work describes the development of a solid phase spectrophotometry method in a μSI-LOV system for cadmium, zinc, and copper determination in freshwaters. NTA (Nitrilotriacetic acid) beads with 60–160 μm diameter were packed in the flow cell of the LOV for a μSPE column of 1 cm length. The spectrophotometric determination is based on the colourimetric reaction between dithizone and the target metals, previously retained on NTA resin. The absorbance of the coloured product formed is measured, at 550 nm, on the surface of the NTA resin beads in a solid phase spectrophotometry approach. The developed method presented preconcentration factors in the range of 11–21 for the metal ions. A LOD of 0.23 μg L{sup −1} for cadmium, 2.39 μg L{sup −1} for zinc, and 0.11 μg L{sup −1} for copper and a sampling rate of 12, 13, and 15 h{sup −1} for cadmium, zinc, and copper were obtained, respectively. The proposed method was successfully applied to freshwater samples. - Highlights: • Multi-parametric determination of cadmium, zinc, and copper at the μg L{sup −1} level. • In-line metal ions preconcentration using NTA resin. • Minimization of matrix interferences by performing solid phase spectrometry in a SI-LOV platform. • Successful application to metal ions determination in freshwaters.

  17. Multiple solid-phase microextraction

    Koster, EHM; de Jong, GJ

    2000-01-01

    Theoretical aspects of multiple solid-phase microextraction are described and the principle is illustrated with the extraction of lidocaine from aqueous solutions. With multiple extraction under non-equilibrium conditions considerably less time is required in order to obtain an extraction yield that

  18. Computational design and fabrication of core-shell magnetic molecularly imprinted polymer for dispersive micro-solid-phase extraction coupled with high-performance liquid chromatography for the determination of rhodamine 6G.

    Xie, Jin; Xie, Jie; Deng, Jian; Fang, Xiangfang; Zhao, Haiqing; Qian, Duo; Wang, Hongjuan

    2016-06-01

    A novel core-shell magnetic nano-adsorbent with surface molecularly imprinted polymer coating was fabricated and then applied to dispersive micro-solid-phase extraction followed by determination of rhodamine 6G using high-performance liquid chromatography. The molecularly imprinted polymer coating was prepared by copolymerization of dopamine and m-aminophenylboronic acid (functional monomers), in the presence of rhodamine 6G (template). The selection of the suitable functional monomers was based on the interaction between different monomers and the template using the density functional theory. The ratios of the monomers to template were further optimized by an OA9 (3(4) ) orthogonal array design. The binding performances of the adsorbent were evaluated by static, kinetic, and selective adsorption experiments. The results reveal that the adsorbent possesses remarkable affinity and binding specificity for rhodamine 6G because of the enhanced Lewis acid-base interaction between the B(Ш) embedded in the imprinted cavities and the template. The nano-adsorbent was successfully applied to dispersive micro-solid-phase extraction coupled to high-performance liquid chromatography for the trace determination of rhodamine 6G in samples with a detection limit of 2.7 nmol/L. Spiked recoveries ranged from 93.0-99.1, 89.5-92.7, and 86.9-105% in river water, matrimony vine and paprika samples, respectively, with relative standard deviations of less than 4.3%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Micro solid phase spectrophotometry in a sequential injection lab-on-valve platform for cadmium, zinc, and copper determination in freshwaters.

    Santos, Inês C; Mesquita, Raquel B R; Rangel, António O S S

    2015-09-03

    This work describes the development of a solid phase spectrophotometry method in a μSI-LOV system for cadmium, zinc, and copper determination in freshwaters. NTA (Nitrilotriacetic acid) beads with 60-160 μm diameter were packed in the flow cell of the LOV for a μSPE column of 1 cm length. The spectrophotometric determination is based on the colourimetric reaction between dithizone and the target metals, previously retained on NTA resin. The absorbance of the coloured product formed is measured, at 550 nm, on the surface of the NTA resin beads in a solid phase spectrophotometry approach. The developed method presented preconcentration factors in the range of 11-21 for the metal ions. A LOD of 0.23 μg L(-1) for cadmium, 2.39 μg L(-1) for zinc, and 0.11 μg L(-1) for copper and a sampling rate of 12, 13, and 15 h(-1) for cadmium, zinc, and copper were obtained, respectively. The proposed method was successfully applied to freshwater samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Application of zein-modified magnetite nanoparticles in dispersive magnetic micro-solid-phase extraction of synthetic food dyes in foodstuffs.

    Jangju, Azam; Farhadi, Khalil; Hatami, Mehdi; Amani, Samireh; Esma-Ali, Farzan; Moshkabadi, Aisan; Hajilari, Fatemeh

    2017-03-01

    A simple method for the simultaneous and trace analysis of four synthetic food azo dyes including carmoisine, ponceau 4R, sunset yellow, and allura red from some foodstuff samples was developed by combining dispersive μ-solid-phase extraction and high-performance liquid chromatography with diode array detection. Zein-modified magnetic Fe 3 O 4 nanoparticles were prepared and used for μ-solid-phase extraction of trace amounts of mentioned food dyes. The prepared modified magnetic nanoparticles were characterized by scanning electron microscopy and FTIR spectroscopy. The factors affecting the extraction of the target analytes such as pH, amount of sorbent, extraction time, type and volume of the desorption eluent, and desorption time were investigated. Under the optimized conditions, the method provided good repeatability with relative standard deviations lower than 5.8% (n = 9). Limit of detection values ranged between 0.3 and 0.9 ng/mL with relatively high enrichment factors (224-441). Comparing the obtained results indicated that Fe 3 O 4 nanoparticles modified by zein biopolymer show better analytical application than bare magnetic nanoparticles. The proposed method was also applied for the determination of target synthetic food dyes in foodstuff samples such as carbonated beverage, snack, and candy samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Portable Solid Phase Micro-Extraction Coupled with Ion Mobility Spectrometry System for On-Site Analysis of Chemical Warfare Agents and Simulants in Water Samples

    Liu Yang

    2014-11-01

    Full Text Available On-site analysis is an efficient approach to facilitate analysis at the location of the system under investigation as it can result in more accurate, more precise and quickly available analytical data. In our work, a novel self-made thermal desorption based interface was fabricated to couple solid-phase microextraction with ion mobility spectrometry for on-site water analysis. The portable interface can be connected with the front-end of an ion mobility spectrometer directly without other modifications. The analytical performance was evaluated via the extraction of chemical warfare agents and simulants in water samples. Several parameters including ionic strength and extraction time have been investigated in detail. The application of the developed method afforded satisfactory recoveries ranging from 72.9% to 114.4% when applied to the analysis of real water samples.

  2. Portable Solid Phase Micro-Extraction Coupled with Ion Mobility Spectrometry System for On-Site Analysis of Chemical Warfare Agents and Simulants in Water Samples

    Yang, Liu; Han, Qiang; Cao, Shuya; Yang, Jie; Yang, Junchao; Ding, Mingyu

    2014-01-01

    On-site analysis is an efficient approach to facilitate analysis at the location of the system under investigation as it can result in more accurate, more precise and quickly available analytical data. In our work, a novel self-made thermal desorption based interface was fabricated to couple solid-phase microextraction with ion mobility spectrometry for on-site water analysis. The portable interface can be connected with the front-end of an ion mobility spectrometer directly without other modifications. The analytical performance was evaluated via the extraction of chemical warfare agents and simulants in water samples. Several parameters including ionic strength and extraction time have been investigated in detail. The application of the developed method afforded satisfactory recoveries ranging from 72.9% to 114.4% when applied to the analysis of real water samples. PMID:25384006

  3. Application of carbon nanotubes modified with a Keggin polyoxometalate as a new sorbent for the hollow-fiber micro-solid-phase extraction of trace naproxen in hair samples with fluorescence spectrophotometry using factorial experimental design.

    Naddaf, Ezzat; Ebrahimi, Mahmoud; Es'haghi, Zarrin; Bamoharram, Fatemeh Farrash

    2015-07-01

    A sensitive technique to determinate naproxen in hair samples was developed using hollow-fiber micro-solid-phase combined with fluorescence spectrophotometry. The incorporation of multi-walled carbon nanotubes modified with a Keggin polyoxometalate into a silica matrix prepared by the sol-gel method was reported. In this research, the Keggin carbon nanotubes /silica composite was used in the pores and lumen of a hollow fiber as the hollow-fiber micro-solid-phase extraction device. The device was used for the microextraction of the analyte from hair and water samples under the optimized conditions. An orthogonal array experimental design with an OA24 (4(6) ) matrix was employed to optimize the conditions. The effect of six factors influencing the extraction efficiency was investigated: pH, salt, volume of donor and desorption phase, extraction and desorption time. The effect of each factor was estimated using individual contributions as response functions in the screening process. Analysis of variance was employed for estimating the main significant factors and their contributions in the extraction. Calibration curve plot displayed linearity over a range of 0.2-10 ng/mL with detection limits of 0.072 and 0.08 ng/mL for hair and aqueous samples, respectively. The relative recoveries in the hair and aqueous matrices ranged from 103-95%. The relative standard deviation for fiber-to-fiber repeatability was 3.9%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Solid phase syntheses of oligoureas

    Burgess, K.; Linthicum, D.S.; Russell, D.H.; Shin, H.; Shitangkoon, A.; Totani, R.; Zhang, A.J.; Ibarzo, J. [Texas A& M Univ., College Station, TX (United States)

    1997-02-19

    Isocyanates 7 were formed from monoprotected diamines 3 or 6, which in turn can be easily prepared from commercially available N-BOC- or N-FMOC-protected amino acid derivatives. Isocyanates 7, formed in situ, could be coupled directly to a solid support functionalized with amine groups or to amino acids anchored on resins using CH{sub 2}Cl{sub 2} as solvent and an 11 h coupling time at 25 {degree}C. Such couplings afforded peptidomimetics with an N-phthaloyl group at the N-terminus. The optimal conditions identified for removal of the N-phthaloyl group were to use 60% hydrazine in DMF for 1-3 h. Several sequences of amino acids coupled to ureas (`peptidic ureas`) and of sequential urea units (`oligoureas`) were prepared via solid phase syntheses and isolated by HPLC. Partition coefficients were measured for two of these peptidomimetics, and their water solubilities were found to be similar to the corresponding peptides. A small library of 160 analogues of the YGGFL-amide sequence was prepared via Houghten`s tea bag methodology. This library was tested for binding to the anti-{beta}-endorphin monoclonal antibody. Overall, this paper describes methodology for solid phase syntheses of oligourea derivatives with side chains corresponding to some of the protein amino acids. The chemistry involved is ideal for high-throughput syntheses and screening operations. 51 refs., 3 figs., 2 tabs.

  5. Polypyrrole/magnetic nanoparticles composite as an efficient sorbent for dispersive micro-solid-phase extraction of antidepressant drugs from biological fluids.

    Asgharinezhad, Ali Akbar; Karami, Sara; Ebrahimzadeh, Homeira; Shekari, Nafiseh; Jalilian, Niloofar

    2015-10-15

    In this study, polypyrrole/magnetic nanoparticles composites in the presence of two different dopants were synthesized with the aid of chemical oxidative polymerization process for dispersive-μ-solid phase extraction (D-μ-SPE). The synthesized magnetic sorbents were characterized by various techniques. The results exhibited that the nanocomposite modified by polypyrrole with sodium perchlorate as a dopant demonstrated higher extraction efficiency for citalopram (CIT) and sertraline (STR) as the model compounds. This nanosorbent in combination with high performance liquid chromatography-UV detection was applied for extraction, preconcentration and determination of CIT and STR in urine and plasma samples. The effect of various parameters on the extraction efficiency including: sample pH, amount of sorbent, sorption time, eluent and its volume, salt content, and elution time were investigated and optimized. The opted conditions were: sample pH, 9.0; sorbent dosage, 10mg; sorption time, 7 min; elution solvent and its volume, 0.06 mol L(-1) HCl in methanol, 120 μL; elution time, 2 min and without addition of salt to the sample. The calibration curves were linear in the concentration range of 1-800 μg L(-1). The limits of detection (LODs) were obtained in the range of 0.2-1.0 μg L(-1) for CIT and 0.3-0.7 μg L(-1) for STR, respectively. The percent of extraction recoveries and relative standard deviations (n=5) were in the range of 93.4-99, 4.8-8.4 for CIT and 94-98.4, 4.3-9.2 for STR, respectively. Finally, the applicability of the method was successfully confirmed by the extraction and determination of CIT and STR in human urine and plasma samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Micro-Texture Synthesis by Phase Randomization

    Bruno Galerne

    2011-09-01

    Full Text Available This contribution is concerned with texture synthesis by example, the process of generating new texture images from a given sample. The Random Phase Noise algorithm presented here synthesizes a texture from an original image by simply randomizing its Fourier phase. It is able to reproduce textures which are characterized by their Fourier modulus, namely the random phase textures (or micro-textures.

  7. An UHPLC-MS/MS method for simultaneous quantification of human amyloid beta peptides Aβ1-38, Aβ1-40 and Aβ1-42 in cerebrospinal fluid using micro-elution solid phase extraction.

    Lin, Ping-Ping; Chen, Wei-Li; Yuan, Fei; Sheng, Lei; Wu, Yu-Jia; Zhang, Wei-Wei; Li, Guo-Qing; Xu, Hong-Rong; Li, Xue-Ning

    2017-12-01

    Amyloid beta (Aβ) peptides in cerebrospinal fluid are extensively estimated for identification of Alzheimer's disease (AD) as diagnostic biomarkers. Unfortunately, their pervasive application is hampered by interference from Aβ propensity of self-aggregation, nonspecifically bind to surfaces and matrix proteins, and by lack of quantitive standardization. Here we report on an alternative Ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for simultaneous measurement of human amyloid beta peptides Aβ1-38, Aβ1-40 and Aβ1-42 in cerebrospinal fluid (CSF) using micro-elution solid phase extraction (SPE). Samples were pre-processing by the mixed-mode micro-elution solid phase extraction and quantification was performed in the positive ion multiple reaction monitoring (MRM) mode using electrospray ionization. The stable-isotope labeled Aβ peptides 15 N 51 - Aβ1-38, 15 N 53 - Aβ1-40 and 15 N 55 - Aβ1-42 peptides were used as internal standards. And the artificial cerebrospinal fluid (ACSF) containing 5% rat plasma was used as a surrogate matrix for calibration curves. The quality control (QC) samples at 0.25, 2 and 15ng/mL were prepared. A "linear" regression (1/x 2 weighting): y=ax+b was used to fit the calibration curves over the concentration range of 0.1-20ng/mL for all three peptides. Coefficient of variation (CV) of intra-batch and inter-batch assays were all less than 6.44% for Aβ1-38, 6.75% for Aβ1-40 and 10.74% for Aβ1-42. The precision values for all QC samples of three analytes met the acceptance criteria. Extract recoveries of Aβ1-38, Aβ1-40 and Aβ1-42 were all greater than 70.78%, both in low and high QC samples. The stability assessments showed that QC samples at both low and high levels could be stable for at least 24h at 4°C, 4h at room temperature and through three freeze-thaw cycles without sacrificing accuracy or precision. And no significant carryover effect was observed. This validated UHPLC

  8. Taylor flow hydrodynamics in gas-liquid-solid micro reactors

    Warnier, M.J.F.

    2009-01-01

    Chemical reactions in which a gas phase component reacts with a liquid phase omponent at the surface of a solid catalyst are often encountered in chemical industry. The rate of such a gas-liquid-solid reaction is often limited by the mass transfer rate of the gas phase component, which depends on

  9. A solid phase micro-radioimmunoassay to detect minute amounts of Ig class specific anti-viral antibody in a mouse model system

    Charlton, D.; Blandford, G.; Toronto Univ., Ontario

    1975-01-01

    A simple and rapid micro-radioimmunoassay was developed to detect and quantitate class specific mouse anti-sendai virus antibodies. Two different 125 I-labelled indicator systems were studied. After incubation of test serum with antigen one system used 125 I-rabbit anti-mouse IgG (RIA 1) and the second employed rabbit anti-mouse IgG, IgA or IgM followed by 125 I-sheep anti-rabbit immunoglobulin reagent (RIA 2). The RIA 2 method was adopted for routine use as it was more sensitive, gave better discrimination between sample and back-ground counts and eliminated the need for several labelled rabbit anti-mouse Ig class specific antisera. The technique was found to be about 100 times more sensitive than conventional HI tests, specific, reliable and economical of reagents and time

  10. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

    2015-08-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L- 1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L- 1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract.

  11. Novel amphiphilic polymeric ionic liquid-solid phase micro-extraction membrane for the preconcentration of aniline as degradation product of azo dye Orange G under sonication by liquid chromatography-tandem mass spectrometry.

    Cai, Mei-Qiang; Wei, Xiao-Qing; Du, Chun-Hui; Ma, Xu-Ming; Jin, Mi-Cong

    2014-07-04

    A novel amphiphilic polymeric ionic liquid membrane containing a hydrophilic bromide anion and a hydrophobic carbonyl group was synthesized in dimethylformamide (DMF) systems using the ionic liquid 1-butyl-3-vinylimidazolium bromide (BVImBr) and the methylmethacrylate (MMA) as monomers. The prepared amphiphilic ploy-methylmethacrylate-1-butyl-3-vinylimidazolium bromide (MMA-BVImBr) was characterized by a scanning electron microscope and an infrared spectrum instrument. The results of solid-phase micro-extraction membrane (SPMM) experiments showed that the adsorption capacity of membrane was about 0.76μgμg(-1) for aniline. Based on this, a sensitive method for the determination of trace aniline, as a degradation product of azo dye Orange G under sonication, was developed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The calibration curve showed a good linearity ranging from 0.5 to 10.0μgL(-1) with a correlation coefficient value of 0.9998. The limit of quantification was 0.5μgL(-1). The recoveries ranged from 90.6% to 96.1%. The intra- and inter-day relative standard deviations were less than 8.3% and 10.9%. The developed SPMM-LC-MS/MS method was used successfully for preconcentration of trace aniline produced during the sonication of Orange G solution. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. MIL-101(Cr)@GO for dispersive micro-solid-phase extraction of pharmaceutical residue in chicken breast used in microwave-assisted coupling with HPLC-MS/MS detection.

    Wang, Yudan; Dai, Xinpeng; He, Xi; Chen, Lin; Hou, Xiaohong

    2017-10-25

    In this work, MIL-101(Cr)@GO (Graphite Oxide) was synthesized using a hydrothermal synthesis method and was applied as a dispersive micro-solid-phase extraction (D-μ-SPE) sorbent for the efficient concentration of four residual drugs (metronidazole, MNZ; tinidazole, TNZ; chloramphenicol, CAP; sulfamethoxazole, SMX). Meanwhile, the extraction process was optimized by combining it with microwave-assisted extraction. Factors affecting the D-μ-SPE efficiency, such as selection of sorbent materials, pH of the sample solution, salting-out effect, amount of used material, extraction time, desorption solvent and desorption time, were studied. Under the optimal extraction conditions, the linearity ranged from 10 to 1000ngkg -1 and 1-100ngkg -1 (r 2 ≥0.9928) for the target analytes. The limits of detection were between 0.08 and 1.02ngkg -1 , and the limits of quantitation were between 0.26 and 3.40ngkg -1 . Additionally, the developed method also exhibited good precision (RSD≤2.5%), repeatability (RSD≤4.3%), high recoveries (88.9%-102.3%) and low matrix effects (78.2%-95.1%). The proposed method proved to be an efficient and reliable approach for the determination of the analytes. Finally, we successfully detected the four drugs in chicken breast. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Application of dispersive liquid-liquid microextraction and dispersive micro-solid-phase extraction for the determination of quinolones in swine muscle by high-performance liquid chromatography with diode-array detection

    Tsai, Wen-Hsien; Chuang, Hung-Yi; Chen, Ho-Hsien; Huang, Joh-Jong; Chen, Hwi-Chang; Cheng, Shou-Hsun; Huang, Tzou-Chi

    2009-01-01

    Dispersive liquid-liquid microextraction (DLLME) and dispersive micro-solid-phase extraction (DMSPE) are two simple and low-cost sample preparation methods for liquid samples. In this work, these two methods were applied to solid tissue sample for the determination of seven quinolones by high-performance liquid chromatography with diode-array detection (HPLC-DAD). After the homogenization of the swine muscle with acetonitrile and salt-promoted partitioning, small amounts of the extract were used for the DLLME and DMSPE methods. In the DLLME approach, the target analytes in the extraction solvent were rapidly extracted into a small volume of dichloromethane for drying and the residue was reconstituted for HPLC-DAD analysis. In the DMSPE approach, the target analytes in the extraction solvent were trapped by dispersive silica-based PSA (primary and secondary amine) sorbents and desorbed into a small amount of desorption solution for HPLC-DAD analysis. Under the optimal conditions, relative recoveries were determined for swine muscle spiked 50-200 μg kg -1 and quantification was achieved by matrix-matched calibration. The calibration curves of seven quinolones showed linearity with a correlation coefficient value above 0.998 for both approaches. Relative recoveries ranged from 93.0 to 104.7% and from 95.5 to 111.0% for DLLME and DMSPE, respectively. Limits of detection (LODs) ranged from 5.6 to 23.8 μg kg -1 and from 7.5 to 26.3 μg kg -1 for DLLME and DMSPE, respectively.

  14. Nonlinear acoustic waves in micro-inhomogeneous solids

    Nazarov, Veniamin

    2014-01-01

    Nonlinear Acoustic Waves in Micro-inhomogeneous Solids covers the broad and dynamic branch of nonlinear acoustics, presenting a wide variety of different phenomena from both experimental and theoretical perspectives. The introductory chapters, written in the style of graduate-level textbook, present a review of the main achievements of classic nonlinear acoustics of homogeneous media. This enables readers to gain insight into nonlinear wave processes in homogeneous and micro-inhomogeneous solids and compare it within the framework of the book. The subsequent eight chapters covering: Physical m

  15. Solid Phase Extraction and Spectrophotometric Determination of ...

    NJD

    2005-04-15

    Apr 15, 2005 ... to the economy and has significant industrial applications. The development of a ... Waters Solid Phase Extraction (SPE) device (the device can carry out twenty ... HPLC grade dimethyl formamide (DMF) (Fisher. Corporation ...

  16. solid phase extraction method for selective determination

    FATOKI

    determination of phthalate ester plasticizers in rivers and marine water samples. Of the ... samples that receive effluent from industries that use phthalate esters. ... Keywords Phthalates, Plasticizers, Solid Phase Gas Chromatography.

  17. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

    2015-01-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L −1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L −1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract. - Highlights: • Efficient retention and preconcentration of As by combining an IL with MWCNTs • Determination of As by ETAAS with direct injection of MWCNTs • Thermal degradation of MWCNTs in the graphite furnace of ETAAS • Highly sensitive speciation and determination of As in garlic

  18. Simultaneous analysis of organochlorine pesticides and polychlorinated biphenyls in air samples by using accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) coupled to gas chromatography dual electron capture detection.

    Mokbel, Haifaa; Al Dine, Enaam Jamal; Elmoll, Ahmad; Liaud, Céline; Millet, Maurice

    2016-04-01

    An analytical method associating accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) in immersion mode combined with gas chromatography dual electrons capture detectors (SPME-GC-2ECD) has been developed and studied for the simultaneous determination of 19 organochlorine pesticides (OCPs) and 22 polychlorinated biphenyls (PCBs) in air samples (active and XAD-2 passive samplers). Samples were extracted with ASE with acetonitrile using the following conditions: temperature, 150 °C; pressure, 1500 psi; static, 15 min; cycles, 3; purge, 300 s; flush, 100 %. Extracts were reduced to 1 mL, and 500 μL of this extract, filled with deionised water, was subject to SPME extraction. Experimental results indicated that the proposed method attained the best extraction efficiency under the optimised conditions: extraction of PCB-OCP mixture using 100-μm PDMS fibre at 80 °C for 40 min with no addition of salt. The performance of the proposed ASE-SPME-GC-2ECD methodology with respect to linearity, limit of quantification and detection was evaluated by spiking of XAD-2 resin with target compounds. The regression coefficient (R (2)) of most compounds was found to be high of 0.99. limits of detection (LODs) are between 0.02 and 4.90 ng m(-3), and limits of quantification (LOQs) are between 0.05 and 9.12 ng m(-3) and between 0.2 and 49 ng/sampler and 0.52 and 91 ng/sampler, respectively, for XAD-2 passive samplers. Finally, a developed procedure was applied to determine selected PCBs and OCPs in the atmosphere.

  19. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar

    2015-08-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L{sup −1} and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L{sup −1} of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract. - Highlights: • Efficient retention and preconcentration of As by combining an IL with MWCNTs • Determination of As by ETAAS with direct injection of MWCNTs • Thermal degradation of MWCNTs in the graphite furnace of ETAAS • Highly sensitive speciation and determination of As in garlic.

  20. Metal-organic framework MIL-101(Cr) as a sorbent of porous membrane-protected micro-solid-phase extraction for the analysis of six phthalate esters from drinking water: a combination of experimental and computational study.

    Wang, Ting; Wang, Jian; Zhang, Conglu; Yang, Zhao; Dai, Xinpeng; Cheng, Maosheng; Hou, Xiaohong

    2015-08-07

    An attractive metal-organic framework (MOF) MIL-101(Cr) material was synthesized at the nanoscale and applied as a sorbent in the porous membrane-protected micro-solid-phase extraction (μ-SPE) device for the pre-concentration of phthalate esters (PAEs) in drinking water samples for the first time. Parameters influencing the extraction efficiency, such as the selection of sorbent materials, pH adjustment, the effect of salt, magnetic-stirring extraction time, the desorption solvent and the desorption time, were investigated. Under the optimum conditions, the limits of detection from gas chromatography-mass spectrometric analysis for PAEs varied from 0.004 to 0.02 μg L(-1). The linear ranges were from 0.1 to 50 μg L(-1) or from 0.2 to 50 μg L(-1) for the analytes with the relative standard deviations fluctuating from 0.8 to 10.9% (n = 5). The enrichment factors (EFs) for the target PAEs were varied from 143 to 187. MIL-101(Cr) exhibited remarkable advantages compared to activated carbon and MIL-100(Fe). On the other hand, the computational method was first used to predict the adsorption of MIL-101(Cr) towards PAEs. The molecular interactions and the free binding energies between MIL-101(Cr) and PAEs were observed and calculated in terms of the molecular modeling method. MIL-101(Cr) showed high potential in the analysis of PAEs at trace levels in drinking water. The computational result was consistent with the detected enrichment factors. The computational modeling accurately predicted the extraction efficiency of MOF-based material towards the target analytes. Therefore, the combination of experimental and computational study provided a new strategy on the trace contaminant analysis.

  1. Determination of fluorine in herbs and water samples by molecular absorption spectrometry after preconcentration on nano-TiO2 using ultrasound-assisted dispersive micro solid phase extraction.

    Krawczyk-Coda, Magdalena; Stanisz, Ewa

    2017-11-01

    This work presents ultrasound-assisted dispersive micro solid phase extraction (USA DMSPE) for preconcentration of fluorine (F) in water and herb samples. TiO 2 nanoparticles (NPs) were used as an adsorbent. The determination with slurry sampling was performed via molecular absorption of calcium monofluoride (CaF) at 606.440 nm using a high-resolution continuum source electrothermal absorption spectrometry (HR-CS ET MAS). Several factors influencing the efficiency of the preconcentration technique, such as the amount of TiO 2 , pH of sample solution, ultrasonication and centrifugation time and TiO 2 slurry solution preparation before injection to HR-CS ET MAS, were investigated in detail. The conditions of detection step (wavelength, calcium amount, pyrolysis and molecule-forming temperatures) were also studied. After extraction, adsorbent with the analyte was mixed with 200 μL of H 2 O to prepare a slurry solution. The concentration limit of detection was 0.13 ng mL -1 . The achieved preconcentration factor was 7. The relative standard deviations (RSDs, %) for F in real samples were 3-15%. The accuracy of this method was evaluated by analyses of certified reference materials after spiking: INCT-MPH-2 (Mixed Polish Herbs), INCT-SBF-4 (Soya Bean Flour), ERM-CAO11b (Hard Drinking Water) and TMDA-54.5 (Lake Ontario Water). The measured F contents in reference materials were in satisfactory agreement with the added amounts, and the recoveries were found to be 97-109%. Under the developed extraction conditions, the proposed method has been successfully applied for the determination of F in real water samples (lake, sea, tap water) and herbs.

  2. A magnetic-based dispersive micro-solid-phase extraction method using the metal-organic framework HKUST-1 and ultra-high-performance liquid chromatography with fluorescence detection for determining polycyclic aromatic hydrocarbons in waters and fruit tea infusions.

    Rocío-Bautista, Priscilla; Pino, Verónica; Ayala, Juan H; Pasán, Jorge; Ruiz-Pérez, Catalina; Afonso, Ana M

    2016-03-04

    A hybrid material composed by the metal-organic framework (MOF) HKUST-1 and Fe3O4 magnetic nanoparticles (MNPs) has been synthetized in a quite simple manner, characterized, and used in a magnetic-assisted dispersive micro-solid-phase extraction (M-d-μSPE) method in combination with ultra-high-performance liquid chromatography (UHPLC) and fluorescence detection (FD). The application was devoted to the determination of 8 heavy polycyclic aromatic hydrocarbons (PAHs) in different aqueous samples, specifically tap water, wastewaters, and fruit tea infusion samples. The overall M-d-μSPE-UHPLC-FD method was optimized and validated. The method is characterized by: its simplicity in both the preparation of the hybrid material (simple mixing) and the magnetic-assisted approach (∼10min extraction time), the use of low sorbent amounts (20mg of HKUST-1 and 5mg of Fe3O4 MNPs), and the low organic solvent consumption in the overall M-d-μSPE-UHPLC-FD method (1.5mL of acetonitrile in the M-d-μSPE method and 2.8mL of acetonitrile in the UHPLC-FD run). The resulting method has high sensitivity, with LODs down to 0.8ngL(-1); adequate intermediate precision, with relative standard deviation values (RSD) always lower than 6.3% (being the range 5.9-9.0% in tap water for a spiked level of 45ngL(-1), 6.1-14% in wastewaters for a spiked level of 45ngL(-1), and 7.2-17% in fruit tea infusion samples for a spiked level of 45ngL(-1)); and adequate relative recoveries, with average values of 82% in tap water, and 94% and 75% in wastewater and fruit tea infusion samples, respectively, if using the proper matrix-matched calibration. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Iron oxide functionalized graphene oxide as an efficient sorbent for dispersive micro-solid phase extraction of sulfadiazine followed by spectrophotometric and mode-mismatched thermal lens spectrometric determination.

    Kazemi, Elahe; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Abbasi, Amir; Rashidian Vaziri, Mohammad Reza; Behjat, Abbas

    2016-01-15

    A simple and rapid dispersive micro-solid phase extraction (DMSPE) combined with mode-mismatched thermal lens spectrometry as well as fiber optic linear array spectrophotometry was developed for the separation, extraction and determination of sulfadiazine. Graphene oxide was synthesized using the modified Hummers method and functionalized with iron oxide nanoparticles by means of a simple one step chemical coprecipitation method. The synthesized iron oxide functionalized graphene oxide was utilized as an efficient sorbent in DMSPE of sulfadiazine. The retained analyte was eluted by using 180µL of a 6:4 mixture of methanol/acetic acid solution and was spectrophotometrically determined based on the formation of an azo dye through coupling with thenoyltrifluoroacetone. Under the optimized conditions, with the application of spectrophotometry technique and with a sample volume of 100mL, the method exhibited a linear dynamic range of 3-80µg L(-1) with a detection limit of 0.82µg L(-1), an enrichment factor of 200 as well as the relative standard deviations of 2.6% and 4.3% (n=6) at 150µg L(-1) level of sulfadiazine for intra- and inter-day analyses, respectively. Whereas, through the application of the thermal lens spectrometry and a sample volume of 10mL, the method exhibited a linear dynamic range of 1-800µg L(-1) with a detection limit of 0.34µg L(-1) and the relative standard deviations of 3.1% and 5.4% (n=6) at 150µg L(-1) level of sulfadiazine for intra- and inter-day analyses, respectively. The method was successfully applied to the determination of sulfadiazine in milk, honey and water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. A novel metal-organic framework composite MIL-101(Cr)@GO as an efficient sorbent in dispersive micro-solid phase extraction coupling with UHPLC-MS/MS for the determination of sulfonamides in milk samples.

    Jia, Xiuna; Zhao, Pan; Ye, Xiu; Zhang, Lianjun; Wang, Ting; Chen, Qinyu; Hou, Xiaohong

    2017-07-01

    As a novel material, metal-organic framework/graphite oxide (MIL-101(Cr)@GO) has great potential for the pretreatment of trace analytes. In the present study, MIL-101(Cr)@GO was synthesized using a solvothermal synthesis method at the nanoscale and was applied as sorbent in the dispersive micro-solid phase extraction (DMSPE) for the enrichment of the trace sulfonamides (SAs) from milk samples for the first time. Several experimental parameters including kinds of sorbents, the effect of pH, the amount of MIL-101(Cr)@GO, ionic strength, adsorption time, desorption solvent and desorption time were investigated. Under the optimal conditions, the linear ranges were from 0.1 to 10μg/L, 0.2-20μg/L or 0.5-50μg/L for the analytes with regression coefficients (r) from 0.9942 to 0.9999. The limits of detection were between 0.012 and 0.145μg/L. The recoveries ranged from 79.83% to 103.8% with relative standard deviations (RSDs)MIL-101(Cr)@GO exhibited remarkable advantages compared to MIL-101(Cr), MIL-100(Fe), activated carbon and other sorbent materials used in pretreatment methods. A simple, rapid, sensitive, inexpensive and less solvent consuming method of DMSPE-ultra-high performance liquid chromatography-tandem mass spectrometry (DMSPE-UHPLC-MS/MS) was successfully applied to the pre-concentration and determination of twelve SAs in milk samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Novel materials and methods for solid-phase extraction and liquid chromatography

    Ambrose, Diana [Iowa State Univ., Ames, IA (United States)

    1997-06-24

    This report contains a general introduction which discusses solid-phase extraction and solid-phase micro-extraction as sample preparation techniques for high-performance liquid chromatography, which is also evaluated in the study. This report also contains the Conclusions section. Four sections have been removed and processed separately: silicalite as a sorbent for solid-phase extraction; a new, high-capacity carboxylic acid functionalized resin for solid-phase extraction; semi-micro solid-phase extraction of organic compounds from aqueous and biological samples; and the high-performance liquid chromatographic determination of drugs and metabolites in human serum and urine using direct injection and a unique molecular sieve.

  6. Phase transitions in solids under high pressure

    Blank, Vladimir Davydovich

    2013-01-01

    Phase equilibria and kinetics of phase transformations under high pressureEquipment and methods for the study of phase transformations in solids at high pressuresPhase transformations of carbon and boron nitride at high pressure and deformation under pressurePhase transitions in Si and Ge at high pressure and deformation under pressurePolymorphic α-ω transformation in titanium, zirconium and zirconium-titanium alloys Phase transformations in iron and its alloys at high pressure Phase transformations in gallium and ceriumOn the possible polymorphic transformations in transition metals under pressurePressure-induced polymorphic transformations in АIBVII compoundsPhase transformations in AIIBVI and AIIIBV semiconductor compoundsEffect of pressure on the kinetics of phase transformations in iron alloysTransformations during deformation at high pressure Effects due to phase transformations at high pressureKinetics and hysteresis in high-temperature polymorphic transformations under pressureHysteresis and kineti...

  7. MicroRNAs expression profile in solid and unicystic ameloblastomas

    Setién-Olarra, A.; Bediaga, N. G.; Aguirre-Echebarria, P.; Aguirre-Urizar, J. M.; Mosqueda-Taylor, A.

    2017-01-01

    Objectives Odontogenic tumors (OT) represent a specific pathological category that includes some lesions with unpredictable biological behavior. Although most of these lesions are benign, some, such as the ameloblastoma, exhibit local aggressiveness and high recurrence rates. The most common types of ameloblastoma are the solid/multicystic (SA) and the unicystic ameloblastoma (UA); the latter considered a much less aggressive entity as compared to the SA. The microRNA system regulates the expression of many human genes while its deregulation has been associated with neoplastic development. The aim of the current study was to determine the expression profiles of microRNAs present in the two most common types of ameloblastomas. Material & methods MicroRNA expression profiles were assessed using TaqMan® Low Density Arrays (TLDAs) in 24 samples (8 SA, 8 UA and 8 control samples). The findings were validated using quantitative RTqPCR in an independent cohort of 19 SA, 8 UA and 19 dentigerous cysts as controls. Results We identified 40 microRNAs differentially regulated in ameloblastomas, which are related to neoplastic development and differentiation, and with the osteogenic process. Further validation of the top ranked microRNAs revealed significant differences in the expression of 6 of them in relation to UA, 7 in relation to SA and 1 (miR-489) that was related to both types. Conclusion We identified a new microRNA signature for the ameloblastoma and for its main types, which may be useful to better understand the etiopathogenesis of this neoplasm. In addition, we identified a microRNA (miR-489) that is suggestive of differentiating among solid from unicystic ameloblastoma. PMID:29053755

  8. The thermomechanical stability of micro-solid oxide fuel cells fabricated on anodized aluminum oxide membranes

    Kwon, Chang-Woo; Lee, Jae-Il; Kim, Ki-Bum; Lee, Hae-Weon; Lee, Jong-Ho; Son, Ji-Won

    2012-07-01

    The thermomechanical stability of micro-solid oxide fuel cells (micro-SOFCs) fabricated on an anodized aluminum oxide (AAO) membrane template is investigated. The full structure consists of the following layers: AAO membrane (600 nm)/Pt anode/YSZ electrolyte (900 nm)/porous Pt cathode. The utilization of a 600-nm-thick AAO membrane significantly improves the thermomechanical stability due to its well-known honeycomb-shaped nanopore structure. Moreover, the Pt anode layer deposited in between the AAO membrane and the YSZ electrolyte preserves its integrity in terms of maintaining the triple-phase boundary (TPB) and electrical conductivity during high-temperature operation. Both of these results guarantee thermomechanical stability of the micro-SOFC and extend the cell lifetime, which is one of the most critical issues in the fabrication of freestanding membrane-type micro-SOFCs.

  9. Extração em fase sólida (SPE e micro extração em fase sólida (SPME de piretróides em água Solid-phase extraction (SPE and solid-phase microextraction of pyrethroids in water

    Wilma Regina Barrionuevo

    2001-04-01

    Full Text Available The pyrethroids bifenthrin, permethrin, cypermethrin and deltamethrin were extracted by solid phase extraction (SPE and solid phase microextraction (SPME. The analysis were performed on a gas chromatograph with electron capture detection (GC-ECD. Octadecil Silano-C18, Florisil and Silica stationary phases were studied for SPE. Better results were obtained for Florisil which gave recoveries from 80% to 108%. Pyrethroids extraction by SPME showed a linear response and a detection limit of 10 pg ml-1. Although the data showed that the two extraction methods were able to isolate the pesticide residues from water samples, the best results were obtained by using SPME which is more sensitive, faster, cheeper, being a more useful technique for the analysis of pyrethroids in drinking water.

  10. Double salts of ionic-liquid-based surfactants in microextraction: application of their mixed hemimicelles as novel sorbents in magnetic-assisted micro-dispersive solid-phase extraction for the determination of phenols.

    Trujillo-Rodríguez, María J; Pino, Verónica; Anderson, Jared L; Ayala, Juan H; Afonso, Ana M

    2015-11-01

    The use of mixed hemimicelles of ionic liquid (IL)-based surfactants in a magnetic-based micro-dispersive solid-phase extraction (m-μdSPE) approach is described. Not only is the symmetric monocationic IL-based surfactant 1,3-didodecylimidazolium bromide (C12C12Im-Br) studied for first time in m-μdSPE, but double-salt (DS) IL (DSIL)-based surfactants are also examined. Nine DSIL-based surfactants were formed by combination of C12C12Im-Br with other IL-based surfactants, including nonsymmetric monocationic and dicationic ILs combined at three different molar fractions. The analytical application was focused on the determination of a group of eight phenols, including bisphenol A, in water samples. The best results were obtained with the DSIL formed by C12C12Im-Br (molar fraction 0.5) and 1-hexadecyl-3-methylimidazolium bromide (C16MIm-Br), after proper optimization of the overall method in combination with high-performance liquid chromatography (HPLC) and diode-array detection (DAD). The optimum conditions for 100 mL of water samples require a small amount (10 mg) of Fe3O4 magnetic nanoparticles, a low content (5.0 mg of C12C12Im-Br and 3.9 mg of C16MIm-Br) of the selected DSIL, pH 11, a sonication time of 2.5 min, and an equilibration time of 5 min with the aid of NdFeB magnets, followed by elution of phenols, evaporation, and reconstitution with 0.5 mL of acetonitrile. The overall m-μdSPE-HPLC-DAD method is characterized for limits of detection down to 1.3 μg · L(-1), intraday relative standard deviations lower than 13 % (n = 3), and interday relative standard deviations lower than 17 % (n = 9), with a spiking level of 15 μg · L(-1); with enrichment factors between 15.7 and 141, and average relative recoveries of 99.9 %.

  11. The metal-organic framework HKUST-1 as efficient sorbent in a vortex-assisted dispersive micro solid-phase extraction of parabens from environmental waters, cosmetic creams, and human urine.

    Rocío-Bautista, Priscilla; Martínez-Benito, Carla; Pino, Verónica; Pasán, Jorge; Ayala, Juan H; Ruiz-Pérez, Catalina; Afonso, Ana M

    2015-07-01

    Three metal-organic frameworks (MOFs), specifically HKUST-1, MOF-5, and MIL-53(Al), have been synthetized, characterized, studied and compared in a vortex-assisted dispersive micro-solid-phase extraction (VA-D-µ-SPE) procedure in combination with high-performance liquid chromatography (HPLC) with diode-array detection (DAD) for determining seven parabens in environmental waters (tap water, swimming pool water, and water coming from a spa pool), human urine (from two volunteers), and cosmetic creams (two commercial brands). Experimental parameters, such as nature and amount of MOF, sample volume, nature of elution solvent and its amount, vortex and centrifugation time, among others, were properly optimized. HKUST-1 was the most adequate MOF to work with. Detection limits for the overall method down to 0.1 μgL(-1) for butylparaben (BPB) and benzylparaben (BzPB) were obtained, with determination coefficients (R(2)) higher than 0.9966 for a range of 0.5-147 μgL(-1) (depending on the paraben), average relative recoveries (RR, in %) of 80.3% at the low spiked level (7 μgL(-1)), and relative standard deviation (RSD) values below 10% also at the low spiked level. The strength of the affinity between HKUST-1 and parabens was evaluated, and it ranged from 33.5% for isopropylparaben (iPPB) to 77.0% for isobutylparaben (iBPB). When analyzing complex environmental waters, RR values of 78%, inter-day precision values (as RSD) lower than 15%, and intra-day precision values lower than 7.8% were obtained, despite the observed matrix effect. When analyzing cosmetic creams, parabens were detected, with contents ranging from 0.14 ± 0.01 μgg(-1) for EPB in the healing cream analyzed to 1.12 ± 0.07 mgg(-1) for MPB in the mask cream analyzed, with precision values (RSD) lower than 12% and RR values from 63.7% for propylparaben (PPB) to 121% for iPPB. When analyzing human urine, no parabens were detected but the method could be performed with RSD values lower than 19%. These

  12. Unitized solid phase immunoassay kit and method

    1975-01-01

    A unitized solid phase kit for radioimmunoassay is disclosed. All of the necessary assay reagents are incorporated into a single tube wherein all phases of the assay procedure are performed, requiring only the addition of the patient's sample. Antibody is bound to the tube surface while labelled antigen is also present but unbound. Storage in the absence of air and water results in the stabilization of the reagents such that the system can be stored for long periods

  13. Solid phase tube radioimmunoassay for digoxin detection

    Stellner, K.; Glatz, C.; Linke, R.

    1975-01-01

    A solid phase radioimmunoassay with 125 I is described for cardiac patients. The test for the digoxin determination and the poisoning due to cardiac glycosides can be measured very accurately and carried out easily. In addition, the test determination can be automatically performed in connection with other tests. (GSE/LH) [de

  14. Multiplexed Colorimetric Solid-Phase Extraction

    Gazda, Daniel B.; Fritz, James S.; Porter, Marc D.

    2009-01-01

    Multiplexed colorimetric solid-phase extraction (MC-SPE) is an extension of colorimetric solid-phase extraction (C-SPE) an analytical platform that combines colorimetric reagents, solid phase extraction, and diffuse reflectance spectroscopy to quantify trace analytes in water. In CSPE, analytes are extracted and complexed on the surface of an extraction membrane impregnated with a colorimetric reagent. The analytes are then quantified directly on the membrane surface using a handheld diffuse reflectance spectrophotometer. Importantly, the use of solid-phase extraction membranes as the matrix for impregnation of the colorimetric reagents creates a concentration factor that enables the detection of low concentrations of analytes in small sample volumes. In extending C-SPE to a multiplexed format, a filter holder that incorporates discrete analysis channels and a jig that facilitates the concurrent operation of multiple sample syringes have been designed, enabling the simultaneous determination of multiple analytes. Separate, single analyte membranes, placed in a readout cartridge create unique, analyte-specific addresses at the exit of each channel. Following sample exposure, the diffuse reflectance spectrum of each address is collected serially and the Kubelka-Munk function is used to quantify each water quality parameter via calibration curves. In a demonstration, MC-SPE was used to measure the pH of a sample and quantitate Ag(I) and Ni(II).

  15. Bioinspired magnetite synthesis via solid precursor phases

    Lenders, J.J.M.; Mirabello, G.; Sommerdijk, N.A.J.M.

    2016-01-01

    Living organisms often exploit solid but poorly ordered mineral phases as precursors in the biomineralization of their inorganic body parts. Generally speaking, such precursor-based approaches allow the organisms-without the need of high supersaturation levels-to accumulate significant quantities of

  16. Phase 2, Solid waste retrieval strategy

    Johnson, D.M.

    1994-01-01

    Solid TRU retrieval, Phase 1 is scheduled to commence operation in 1998 at 218W-4C-T01 and complete recovery of the waste containers in 2001. Phase 2 Retrieval will recover the remaining buried TRU waste to be retrieved and provide the preliminary characterization by non-destructive means to allow interim storage until processing for disposal. This document reports on researching the characterization documents to determine the types of wastes to be retrieved and where located, waste configurations, conditions, and required methods for retrieval. Also included are discussions of wastes encompassed by Phase 2 for which there are valid reasons to not retrieve

  17. Phase 2, Solid waste retrieval strategy

    Johnson, D.M.

    1994-09-29

    Solid TRU retrieval, Phase 1 is scheduled to commence operation in 1998 at 218W-4C-T01 and complete recovery of the waste containers in 2001. Phase 2 Retrieval will recover the remaining buried TRU waste to be retrieved and provide the preliminary characterization by non-destructive means to allow interim storage until processing for disposal. This document reports on researching the characterization documents to determine the types of wastes to be retrieved and where located, waste configurations, conditions, and required methods for retrieval. Also included are discussions of wastes encompassed by Phase 2 for which there are valid reasons to not retrieve.

  18. Adhesion Dynamics in Probing Micro- and Nanoscale Thin Solid Films

    Xiaoling He

    2008-01-01

    Full Text Available This study focuses on modeling the probe dynamics in scratching and indenting thin solid films at micro- and nanoscales. The model identifies bifurcation conditions that define the stick-slip oscillation patterns of the tip. It is found that the local energy fluctuations as a function of the inelastic deformation, defect formation, material properties, and contact parameters determine the oscillation behavior. The transient variation of the localized function makes the response nonlinear at the adhesion junction. By quantifying the relation between the bifurcation parameters and the oscillation behavior, this model gives a realistic representation of the complex adhesion dynamics. Specifically, the model establishes the link between the stick-slip behavior and the inelastic deformation and the local potentials. This model justifies the experimental observations and the molecular dynamics simulation of the adhesion and friction dynamics in both the micro- and nanoscale contact.

  19. Determinação do coeficiente de atividade na diluição infinita (g¥ através da micro-extração em fase sólida (SPME Determination of activity coefficients at infinite dilution through solid phase microextraction (SPME

    Douglas B. Fonseca

    2007-01-01

    Full Text Available In this study a new approach, solid phase micro extraction (SPME, is used in the evaluation of the infinite dilution activity coefficient of the solute in a given solvent. It is the purpose of the current work to demonstrate a different approach to obtain the data needed for studying the solution thermodynamics of binary liquid mixtures as well as for designing multi-component separations. The solutes investigated at the temperature 298.15 K were toluene, ethyl benzene and xylene in the solvent methanol.

  20. Solid-phase equilibria on Pluto's surface

    Tan, Sugata P.; Kargel, Jeffrey S.

    2018-03-01

    Pluto's surface is covered by volatile ices that are in equilibrium with the atmosphere. Multicomponent phase equilibria may be calculated using a thermodynamic equation of state and, without additional assumptions, result in methane-rich and nitrogen-rich solid phases. The former is formed at temperature range between the atmospheric pressure-dependent sublimation and condensation points, while the latter is formed at temperatures lower than the sublimation point. The results, calculated for the observed 11 μbar atmospheric pressure and composition, are consistent with recent work derived from observations by New Horizons.

  1. Solid - solid and solid - liquid phase transitions of iron and iron alloys under laser shock compression

    Harmand, M.; Krygier, A.; Appel, K.; Galtier, E.; Hartley, N.; Konopkova, Z.; Lee, H. J.; McBride, E. E.; Miyanishi, K.; Nagler, B.; Nemausat, R.; Vinci, T.; Zhu, D.; Ozaki, N.; Fiquet, G.

    2017-12-01

    An accurate knowledge of the properties of iron and iron alloys at high pressures and temperatures is crucial for understanding and modelling planetary interiors. While Earth-size and Super-Earth Exoplanets are being discovered in increasingly large numbers, access to detailed information on liquid properties, melting curves and even solid phases of iron and iron at the pressures and temperatures of their interiors is still strongly limited. In this context, XFEL sources coupled with high-energy lasers afford unique opportunities to measure microscopic structural properties at far extreme conditions. Also the achievable time resolution allows the shock history and phase transition mechanisms to be followed during laser compression, improving our understanding of the high pressure and high strain experiments. Here we present recent studies devoted to investigate the solid-solid and solid-liquid transition in laser-shocked iron and iron alloys (Fe-Si, Fe-C and Fe-O alloys) using X-ray diffraction and X-ray diffuse scattering. Experiment were performed at the MEC end-station of the LCLS facility at SLAC (USA). Detection of the diffuse scattering allowed the identification of the first liquid peak position along the Hugoniot, up to 4 Mbar. The time resolution shows ultrafast (between several tens and several hundreds of picoseconds) solid-solid and solid-liquid phase transitions. Future developments at XFEL facilities will enable detailed studies of the solid and liquid structures of iron and iron alloys as well as out-of-Hugoniot studies.

  2. Aplicação de SPME (Solid Phase Micro-Extraction na análise de águas potáveis de três localidades do estado de São Paulo

    Valente Antonio Luiz Pires

    1998-01-01

    Full Text Available The technique of solid phase microextraction (SPME was used for the extraction of halogenated contaminants of water samples from three cities of the State of São Paulo and the extracts were submitted to gas chromatographic analysis with electron capture detection (GC-ECD. In the samples of water collected at the city of São Paulo the detected level of trihalomethanes (THM expressed as the sum of chloroform, dibromochloromethane and dichlorobromomethane, were higher than the permissible limit established by the Brazilian regulation. In the samples collected at the two other cities the level of any of the three THM remained below the sensitivity of the ECD.

  3. Elementary excitations and phase transformations in solids

    Cowley, R.A.

    1985-01-01

    Neutron scattering is and will continue to be a uniquely powerful tool for the study of elementary excitations and phase transformations in solids. The paper examines a few recent experiments on molecular crystals, superionic materials, paramagnetic scattering and phase transitions to see what experimental features made these experiments possible, and hence to make suggestions about future needs. It is concluded that new instruments will extend the scope of neutron scattering studies to new excitations, that there is a need for higher resolution, particularly for phase transition studies, and that it will be important to use intensity information, discrimination against unwanted inelastic processes and polarization analysis to reliably measure the excitations in new materials. (author)

  4. A thermally self-sustained micro-power plant with integrated micro-solid oxide fuel cells, micro-reformer and functional micro-fluidic carrier

    Scherrer, Barbara; Evans, Anna; Santis-Alvarez, Alejandro J.; Jiang, Bo; Martynczuk, Julia; Galinski, Henning; Nabavi, Majid; Prestat, Michel; Tölke, René; Bieberle-Hütter, Anja; Poulikakos, Dimos; Muralt, Paul; Niedermann, Philippe; Dommann, Alex; Maeder, Thomas; Heeb, Peter; Straessle, Valentin; Muller, Claude; Gauckler, Ludwig J.

    2014-07-01

    Low temperature micro-solid oxide fuel cell (micro-SOFC) systems are an attractive alternative power source for small-size portable electronic devices due to their high energy efficiency and density. Here, we report on a thermally self-sustainable reformer-micro-SOFC assembly. The device consists of a micro-reformer bonded to a silicon chip containing 30 micro-SOFC membranes and a functional glass carrier with gas channels and screen-printed heaters for start-up. Thermal independence of the device from the externally powered heater is achieved by exothermic reforming reactions above 470 °C. The reforming reaction and the fuel gas flow rate of the n-butane/air gas mixture controls the operation temperature and gas composition on the micro-SOFC membrane. In the temperature range between 505 °C and 570 °C, the gas composition after the micro-reformer consists of 12 vol.% to 28 vol.% H2. An open-circuit voltage of 1.0 V and maximum power density of 47 mW cm-2 at 565 °C is achieved with the on-chip produced hydrogen at the micro-SOFC membranes.

  5. Micro Resistojet for Small Satellites, Phase II

    National Aeronautics and Space Administration — Micro-resistojets offer an excellent combination of simplicity, performance and wet system mass for small satellites (<100 kg, <50 watts) requiring mN level...

  6. Micro Resistojet for Small Satellites, Phase I

    National Aeronautics and Space Administration — Micro-resistojets offer the best combination of simplicity, performance, wet system mass and power consumption for small satellites (<100kg, <50Watts)...

  7. Development of a novel mixed hemimicelles dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene for the separation and preconcentration of fluoxetine in different matrices before its determination by fiber optic linear array spectrophotometry and mode-mismatched thermal lens spectroscopy

    Kazemi, Elahe; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh; Abbasi, Amir; Rashidian Vaziri, Mohammad Reza; Behjat, Abbas

    2016-01-01

    This study aims at developing a novel, sensitive, fast, simple and convenient method for separation and preconcentration of trace amounts of fluoxetine before its spectrophotometric determination. The method is based on combination of magnetic mixed hemimicelles solid phase extraction and dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene as a sorbent. The magnetic graphene was synthesized by a simple coprecipitation method and characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). The retained analyte was eluted using a 100 μL mixture of methanol/acetic acid (9:1) and converted into fluoxetine-β-cyclodextrin inclusion complex. The analyte was then quantified by fiber optic linear array spectrophotometry as well as mode-mismatched thermal lens spectroscopy (TLS). The factors affecting the separation, preconcentration and determination of fluoxetine were investigated and optimized. With a 50 mL sample and under optimized conditions using the spectrophotometry technique, the method exhibited a linear dynamic range of 0.4–60.0 μg L"−"1, a detection limit of 0.21 μg L"−"1, an enrichment factor of 167, and a relative standard deviation of 2.1% and 3.8% (n = 6) at 60 μg L"−"1 level of fluoxetine for intra- and inter-day analyses, respectively. However, with thermal lens spectrometry and a sample volume of 10 mL, the method exhibited a linear dynamic range of 0.05–300 μg L"−"1, a detection limit of 0.016 μg L"−"1 and a relative standard deviation of 3.8% and 5.6% (n = 6) at 60 μg L"−"1 level of fluoxetine for intra- and inter-day analyses, respectively. The method was successfully applied to determine fluoxetine in pharmaceutical formulation, human urine and environmental water samples. - Graphical abstract: A novel, sensitive, fast, simple and convenient mixed hemimicelles dispersive micro solid

  8. Development of a novel mixed hemimicelles dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene for the separation and preconcentration of fluoxetine in different matrices before its determination by fiber optic linear array spectrophotometry and mode-mismatched thermal lens spectroscopy

    Kazemi, Elahe; Haji Shabani, Ali Mohammad [Department of Chemistry, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of); Dadfarnia, Shayessteh, E-mail: sdadfarnia@yazd.ac.ir [Department of Chemistry, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of); Abbasi, Amir [Department of Physics, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of); Rashidian Vaziri, Mohammad Reza [Laser and Optics Research School, 14155-1339, Tehran (Iran, Islamic Republic of); Behjat, Abbas [Department of Physics, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of)

    2016-01-28

    This study aims at developing a novel, sensitive, fast, simple and convenient method for separation and preconcentration of trace amounts of fluoxetine before its spectrophotometric determination. The method is based on combination of magnetic mixed hemimicelles solid phase extraction and dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene as a sorbent. The magnetic graphene was synthesized by a simple coprecipitation method and characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). The retained analyte was eluted using a 100 μL mixture of methanol/acetic acid (9:1) and converted into fluoxetine-β-cyclodextrin inclusion complex. The analyte was then quantified by fiber optic linear array spectrophotometry as well as mode-mismatched thermal lens spectroscopy (TLS). The factors affecting the separation, preconcentration and determination of fluoxetine were investigated and optimized. With a 50 mL sample and under optimized conditions using the spectrophotometry technique, the method exhibited a linear dynamic range of 0.4–60.0 μg L{sup −1}, a detection limit of 0.21 μg L{sup −1}, an enrichment factor of 167, and a relative standard deviation of 2.1% and 3.8% (n = 6) at 60 μg L{sup −1} level of fluoxetine for intra- and inter-day analyses, respectively. However, with thermal lens spectrometry and a sample volume of 10 mL, the method exhibited a linear dynamic range of 0.05–300 μg L{sup −1}, a detection limit of 0.016 μg L{sup −1} and a relative standard deviation of 3.8% and 5.6% (n = 6) at 60 μg L{sup −1} level of fluoxetine for intra- and inter-day analyses, respectively. The method was successfully applied to determine fluoxetine in pharmaceutical formulation, human urine and environmental water samples. - Graphical abstract: A novel, sensitive, fast, simple and convenient mixed hemimicelles

  9. Micro and Small Enterprises Incubator - Phase III

    The goals of the Mozambique Information and Communication Technology Micro and Small Enterprises Incubator (MICTI Incubator) are twofold: to identify sustainable opportunities for technology-based businesses in priority development areas; and to test the assumption that technology-based businesses can mentor the ...

  10. Recent Application of Solid Phase Based Techniques for Extraction and Preconcentration of Cyanotoxins in Environmental Matrices.

    Mashile, Geaneth Pertunia; Nomngongo, Philiswa N

    2017-03-04

    Cyanotoxins are toxic and are found in eutrophic, municipal, and residential water supplies. For this reason, their occurrence in drinking water systems has become a global concern. Therefore, monitoring, control, risk assessment, and prevention of these contaminants in the environmental bodies are important subjects associated with public health. Thus, rapid, sensitive, selective, simple, and accurate analytical methods for the identification and determination of cyanotoxins are required. In this paper, the sampling methodologies and applications of solid phase-based sample preparation methods for the determination of cyanotoxins in environmental matrices are reviewed. The sample preparation techniques mainly include solid phase micro-extraction (SPME), solid phase extraction (SPE), and solid phase adsorption toxin tracking technology (SPATT). In addition, advantages and disadvantages and future prospects of these methods have been discussed.

  11. Density-functional theory for fluid-solid and solid-solid phase transitions.

    Bharadwaj, Atul S; Singh, Yashwant

    2017-03-01

    We develop a theory to describe solid-solid phase transitions. The density functional formalism of classical statistical mechanics is used to find an exact expression for the difference in the grand thermodynamic potentials of the two coexisting phases. The expression involves both the symmetry conserving and the symmetry broken parts of the direct pair correlation function. The theory is used to calculate phase diagram of systems of soft spheres interacting via inverse power potentials u(r)=ε(σ/r)^{n}, where parameter n measures softness of the potential. We find that for 1/nfcc) structure while for 1/n≥0.154 the body-centred-cubic (bcc) structure is preferred. The bcc structure transforms into the fcc structure upon increasing the density. The calculated phase diagram is in good agreement with the one found from molecular simulations.

  12. Preconcentration of uranium in water samples using dispersive liquid-liquid micro- extraction coupled with solid-phase extraction and determination with inductively coupled plasma-optical emission spectrometry

    M. Rezaee,

    2015-10-01

    Full Text Available A new liquid phase microextraction method based on the dispersion of an extraction solvent into aqueous phase coupled with solid-phase extraction was investigated for the extraction, preconcentration and determination of uranium in water samples. 1-(2-Pyridylazo-2-naphthol reagent (PAN at pH 6.0 was used as a chelating agent prior to extraction. After concentration and purification of the samples in SPE C18 sorbent, 1.5 mL elution sample containing 40.0 µL chlorobenzene was injected into the 5.0 mL pure water. After extraction and centrifuging, the sedimented phase was evaporated and the residue was dissolved in nitric acid (0.5 M and was injected by injection valve into the ICP-OES. Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition were studied and optimized. Under the optimum conditions, the calibration graph was linear in the range of 0.5-500 µg L-1. The detection limit was 0.1 µg L-1. The relative standard deviation (RSD at 5.0 µg L-1 concentration level was 6.6%. Finally, the developed method was successfully applied to the extraction and determination of uranium in the well, river, mineral, waste and tap water samples and satisfactory results were obtained.DOI: http://dx.doi.org/10.4314/bcse.v29i3.4

  13. Preparation and characterization of a novel polymeric based solid-solid phase change heat storage material

    Xi Peng; Gu Xiaohua; Cheng Bowen; Wang Yufei

    2009-01-01

    Here we reported a two-step procedure for preparing a novel polymeric based solid-solid phase change heat storage material. Firstly, a copolymer monomer containing a polyethylene glycol monomethyl ether (MPEG) phase change unit and a vinyl unit was synthesized via the modification of hydrogen group of MPEG. Secondly, by copolymerization of the copolymer monomer and phenyl ethylene, a novel polymeric based solid-solid phase change heat storage material was prepared. The composition, structure and properties of the novel polymeric based solid-solid phase change material were characterized by IR, 1 H NMR, DSC, WAXD, and POM, respectively. The results show that the novel polymeric based solid-solid phase change material possesses of excellent crystal properties and high phase change enthalpy.

  14. Determinação de metil-etil-cetona em amostras de urina com amostragem por micro extração em fase sólida (MEFS em headspace associada à cromatografia gasosa com detector de ionização de chama (CG-DIC Determination of methyl ethyl ketone in urine samples by headspace solid phase micro extraction (SPME sampling associated to gas chromatography with flame-ionization detectoR (GC-FID

    Marina Venzon Antunes

    2008-01-01

    Full Text Available Methyl ethyl ketone (MEK is a solvent commonly used in chemical, paint and shoe industry. The aim of this study was to develop and validate a method for urinary quantification of MEK, employing headspace solid phase micro extraction sampling (SPME coupled to gas chromatography with flame ionization detection (GC-FID. The calibration curve (y=4.6851x-0.0011 presented good linearity with r²=0.9993. Accuracy (94-109%, intra-assay precision (4.07-5.91% and inter-assay precision (3.03-5.62% were acceptable. The quantification limit was 0.19 mg/L. This low cost method can be used routinely in the biological monitoring of occupational exposure to MEK, according to the requirements of the Brazilian legislation.

  15. Fluorine incorporation during Si solid phase epitaxy

    Impellizzeri, G.; Mirabella, S.; Romano, L.; Napolitani, E.; Carnera, A.; Grimaldi, M.G.; Priolo, F.

    2006-01-01

    We have investigated the F incorporation and segregation in preamorphized Si during solid phase epitaxy (SPE) at different temperatures and for several implanted-F energies and fluences. The Si samples were amorphized to a depth of 550 nm by implanting Si at liquid nitrogen temperature and then enriched with F at different energies (65-150 keV) and fluences (0.07-5 x 10 14 F/cm 2 ). Subsequently, the samples were regrown by SPE at different temperatures: 580, 700 and 800 deg. C. We have found that the amount of F incorporated after SPE strongly depends on the SPE temperature and on the energy and fluence of the implanted-F, opening the possibility to tailor the F profile during SPE

  16. Localization of solid micro and nano-inclusions in heterophase bioplastic blends

    Dil, Ebrahim Jalali

    Blending poly(lactic acid), PLA, with other high impact bioplastics has been introduced as an effective method for improving the toughness of PLA; however, this strategy considerably reduces the modulus and mechanical strength of PLA. The addition of solid particles is a well-known method for tuning the stiffness/toughness balance in toughened polymer matrices. Notwithstanding the significance of controlling the localization of solid inclusions in polymer blends, the literature is lacking a detailed analysis of the migration mechanisms and the effects of thermodynamic and kinetic parameters on the localization of solid particles in polymer blends. In this dissertation, the localization and migration of spherical micro- and nano-silica particles in two bioplastic blends of PLA/low density polyethylene (LDPE) and PLA/poly(butylene adipateco-terephthalate), PBAT, were studied. In the first part of this work, a detailed study on the miscibility and morphology development in the PLA/PBAT blend was carried out. The interfacial tension between PLA and PBAT was determined to be 0.6 +/- 0.15 mN/m by fitting Palierne's model on the rheological data. The miscibility of PLA/PBAT was then examined by studying the shift in the glass transition temperature (Tg) of the polymer phases at different blend compositions. The obtained results indicate a limited one-way partial miscibility of PBAT molecules in the PLA-rich phase. This partial miscibility depends significantly on the molecular weight of PBAT, which underlines its entropic nature. The morphology analysis of the blend samples revealed that the dispersed phase in PLA/PBAT blends exists in the form of fibers, even at low compositions of 1 vol.% of the dispersed phase. Finally, the co-continuity region in PLA/PBAT blends was determined using a rheological approach and it was shown that PLA/PBAT has a wide symmetric co-continuous region located between 30-40 and 60-70 vol.% of PBAT. In the second part of this project, the

  17. Solid-phase extraction of galloyl- and caffeoylquinic acids from natural sources (Galphimia glauca and Arnicae flos) using pure zirconium silicate and bismuth citrate powders as sorbents inside micro spin columns.

    Hussain, Shah; Schönbichler, Stefan A; Güzel, Yüksel; Sonderegger, Harald; Abel, Gudrun; Rainer, Matthias; Huck, Christian W; Bonn, Günther K

    2013-10-01

    Galloyl- and caffeoylquinic acids are among the most important pharmacological active groups of natural compounds. This study describes a pre-step in isolation of some selected representatives of these groups from biological samples. A selective solid-phase extraction (SPE) method for these compounds may help assign classes and isomer designations within complex mixtures. Pure zirconium silicate and bismuth citrate powders (325 mesh) were employed as two new sorbents for optimized SPE of phenolic acids. These sorbents possess electrostatic interaction sites which accounts for additional interactions for carbon acid moieties as compared to hydrophilic and hydrophobic sorbents alone. Based on this principle, a selective SPE method for 1,3,4,5-tetragalloylquinic acid (an anti-HIV and anti-asthamatic agent) as a starting compound was developed and then deployed upon other phenolic acids with success. The recoveries and selectivities of both sorbents were compared to most commonly applied and commercially available sorbents by using high performance liquid chromatography. The nature of interaction between the carrier sorbent and the acidic target molecules was investigated by studying hydrophilic (silica), hydrophobic (C18), mixed-mode (ionic and hydrophobic: Oasis(®) MAX) and predominantly electrostatic (zirconium silicate) materials. The newly developed zirconium silicate and bismuth citrate stationary phases revealed promising results for the selective extraction of galloyl- and caffeoylquinic acids from natural sources. It was observed that zirconium silicate exhibited maximum recovery and selectivity for tetragalloylquinic acid (84%), chlorogenic acid (82%) and dicaffeoylquinic acid (94%) among all the tested sorbents. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Study of the aroma formation and transformation during the manufacturing process of oolong tea by solid-phase micro-extraction and gas chromatography-mass spectrometry combined with chemometrics.

    Ma, Chengying; Li, Junxing; Chen, Wei; Wang, Wenwen; Qi, Dandan; Pang, Shi; Miao, Aiqing

    2018-06-01

    Oolong tea is a typical semi-fermented tea and is famous for its unique aroma. The aim of this study was to compare the volatile compounds during manufacturing process to reveal the formation of aroma. In this paper, a method was developed based on head-space solid phase microextraction/gas chromatography-mass spectrometry (HS-SPME/GC-MS) combined with chemometrics to assess volatile profiles during manufacturing process (fresh leaves, sun-withered leaves, rocked leaves and leaves after de-enzyming). A total of 24 aroma compounds showing significant differences during manufacturing process were identified. Subsequently, according to these aroma compounds, principal component analysis and hierarchical cluster analysis showed that the four samples were clearly distinguished from each other, which suggested that the 24 identified volatile compounds can represent the changes of volatile compounds during the four steps. Additionally, sun-withering, rocking and de-enzyming can influence the variations of volatile compounds in different degree, and we found the changes of volatile compounds in withering step were less than other two manufacturing process, indicating that the characteristic volatile compounds of oolong tea might be mainly formed in rocking stage by biological reactions and de-enzyming stage through thermal chemical transformations rather than withering stage. This study suggested that HS-SPME/GC-MS combined with chemometrics methods is accurate, sensitive, fast and ideal for rapid routine analysis of the aroma compounds changes in oolong teas during manufacturing processing. Copyright © 2018 Elsevier Ltd. All rights reserved.

  19. Informal Micro-Enterprises and Solid Waste Collection: The Case ...

    The research used both Primary and secondary data sources. One hundred sixty micro-enterprise units were included in the survey. These account for about 35% of the total micro-enterprises available in the city. Stratified random sampling was employed based on the number and type of micro-enterprises available in each ...

  20. SOLID-PHASE PEPTIDE SYNTHESIS OF ISOTOCIN WITH AMIDE ...

    SOLID-PHASE PEPTIDE SYNTHESIS OF ISOTOCIN WITH AMIDE OF ASPARAGINE PROTECTED WITH 1-TETRALINYL. TRIFLUOROMETHANESULPHONIC ACID (TFMSA) DEPROTECTION, CLEAVAGE AND AIR OXIDATION OF MERCAPTO GROUPS TO DISULPHIDE.

  1. Solid-Solid Vacuum Regolith Heat-Exchanger for Oxygen Production, Phase I

    National Aeronautics and Space Administration — This SBIR Phase-1 project will demonstrate the feasibility of using a novel coaxial counterflow solid-solid heat exchanger to recover heat energy from spent regolith...

  2. Mathematical micro-model of a solid oxide fuel cell composite cathode

    Kenney, B.; Karan, K.

    2004-01-01

    In a solid oxide fuel cell (SOFC), the cathode processes account for a majority of the overall electrochemical losses. A composite cathode comprising a mixture of ion-conducting electrolyte and electron-conducting electro-catalyst can help minimize cathode losses provided microstructural parameters such as particle-size, composition, and porosity are optimized. The cost of composite cathode research can be greatly reduced by incorporating mathematical models into the development cycle. Incorporated with reliable experimental data, it is possible to conduct a parametric study using a model and the predicted results can be used as guides for component design. Many electrode models treat the cathode process simplistically by considering only the charge-transfer reaction for low overpotentials or the gas-diffusion at high overpotentials. Further, in these models an average property of the cathode internal microstructure is assumed. This paper will outline the development of a 1-dimensional SOFC composite cathode micro-model and the experimental procedures for obtaining accurate parameter estimates. The micro-model considers the details of the cathode microstructure such as porosity, composition and particle-size of the ionic and electronic phases, and their interrelationship to the charge-transfer reaction and mass transport processes. The micro-model will be validated against experimental data to determine its usefulness for performance prediction. (author)

  3. Solid phase extraction method for determination of mitragynine in ...

    All rights reserved. ... 1Department of Pharmacology, 2Department of Applied Science, 3Police Forensic Science Center 10, Yala 95000, 4Natural ... Purpose: To develop a solid phase extraction (SPE) method that utilizes reverse-phase high.

  4. Solid-phase extraction of carotenoids.

    Shen, Yao; Hu, Yumin; Huang, Ke; Yin, Shi'an; Chen, Bo; Yao, Shouzhuo

    2009-07-24

    In this work, solid-phase extraction (SPE) trapping performance of lutein and beta-carotene, which were used as the model molecules of carotenoids, was investigated. The absorption, elution, and enrichment of carotenoids on SPE cartridges with four different sorbents, i.e. C(30), C(18), diol, and silica, were compared respectively with the help of frontal analysis technique. The high retentions of both lutein and beta-carotene were achieved on the C(18) and C(30) cartridges. The diol and silica cartridges only had good retention for lutein. The optimized SPE method for sample pretreatment for the carotenoids analysis was obtained after the investigation of trapping performance. The method was applied successfully to the analysis of biological sample, i.e. serum and human breast milk. The recovery, accuracy, and precision of SPE method comparing with those of traditional liquid-liquid extraction (LLE) method for the sample pretreatment for the analysis of carotenoids owned a number of advantages such as rapid, no chloroform used, and accurate versus LLE.

  5. Hydrodynamics of multi-phase packed bed micro-reactors

    Márquez Luzardo, N.M.

    2010-01-01

    Why to use packed bed micro-reactors for catalyst testing? Miniaturized packed bed reactors have a large surface-to-volume ratio at the reactor and particle level that favors the heat- and mass-transfer processes at all scales (intra-particle, inter-phase and inter-particle or reactor level). If the

  6. Microencapsulated Comb-Like Polymeric Solid-Solid Phase Change Materials via In-Situ Polymerization

    Wei Li

    2018-02-01

    Full Text Available To enhance the thermal stability and permeability resistance, a comb-like polymer with crystallizable side chains was fabricated as solid-solid phase change materials (PCMs inside the cores of microcapsules and nanocapsules prepared via in-situ polymerization. In this study, the effects on the surface morphology and microstructure of micro/nanocapsules caused by microencapsulating different types of core materials (i.e., n-hexadecane, ethyl hexadecanoate, hexadecyl acrylate and poly(hexadecyl acrylate were systematically studied via field emission scanning electron microscope (FE-SEM and transmission electron microscope (TEM. The confined crystallization behavior of comb-like polymer PCMs cores was investigated via differential scanning calorimeter (DSC. Comparing with low molecular organic PCMs cores, the thermal stability of PCMs microencapsulated comb-like polymer enhanced significantly, and the permeability resistance improved obviously as well. Based on these resultant analysis, the microencapsulated comb-like polymeric PCMs with excellent thermal stability and permeability resistance showed promising foreground in the field of organic solution spun, melt processing and organic coating.

  7. Private sector participation in solid waste collection in Addis Ababa (Ethiopia) by involving micro-enterprises.

    Tilaye, Mesfin; van Dijk, Meine Pieter

    2014-01-01

    Privatization of urban services focuses often on the involvement of foreign enterprises. This contribution deals with micro-privatization, the partial transfer of government responsibility for solid waste collection to micro-enterprises. It tries to shed light on whether the current private sector participation (PSP) of micro-enterprises in solid waste collection service is the best way to capture the expected advantages of private sector involvement. The article examines the relations of the micro-enterprises with beneficiaries and the public sector by focusing on the contract procedure, the tariff-setting process, the cost recovery mechanism and institutionalizing of market principles for micro-enterprises. The research was carried out using secondary and primary data sources. Primary data were collected through the interviewing of public sector officials at different levels, focus group discussions with community groups and micro-enterprises, and observation. A survey was conducted among 160 micro-enterprises in the city of Addis Ababa, Ethiopia, using a standard questionnaire. What are some of the factors contributing to the results of PSP in Addis Ababa, the capital of Ethiopia? Policies at higher levels of government definitely produced an overall climate conducive to micro-privatization and recognized the need to develop micro-enterprises, but it is not clear what role the micro-enterprises are to play in solid waste management. New opportunities were created by formalization and taken up by communities and micro-enterprises. Coverage and waste collected both increased. The initiation and institutionalization of the formalization process was not without problems. The public sector over-stressed the autonomy of micro-enterprises. The fate of the micro-enterprises is largely determined by the reforms undertaken at local government level. The rapid changes in policies at the local level made waste-collecting micro-enterprises lose confidence and more dependent

  8. Solid-phase extraction versus matrix solid-phase dispersion: Application to white grapes.

    Dopico-García, M S; Valentão, P; Jagodziñska, A; Klepczyñska, J; Guerra, L; Andrade, P B; Seabra, R M

    2007-11-15

    The use of matrix solid-phase dispersion (MSPD) was tested to, separately, extract phenolic compounds and organic acids from white grapes. This method was compared with a more conventional analytical method previously developed that combines solid liquid extraction (SL) to simultaneously extract phenolic compounds and organic acids followed by a solid-phase extraction (SPE) to separate the two types of compounds. Although the results were qualitatively similar for both techniques, the levels of extracted compounds were in general quite lower on using MSPD, especially for organic acids. Therefore, SL-SPE method was preferred to analyse white "Vinho Verde" grapes. Twenty samples of 10 different varieties (Alvarinho, Avesso, Asal-Branco, Batoca, Douradinha, Esganoso de Castelo Paiva, Loureiro, Pedernã, Rabigato and Trajadura) from four different locations in Minho (Portugal) were analysed in order to study the effects of variety and origin on the profile of the above mentioned compounds. Principal component analysis (PCA) was applied separately to establish the main sources of variability present in the data sets for phenolic compounds, organic acids and for the global data. PCA of phenolic compounds accounted for the highest variability (77.9%) with two PCs, enabling characterization of the varieties of samples according to their higher content in flavonol derivatives or epicatechin. Additionally, a strong effect of sample origin was observed. Stepwise linear discriminant analysis (SLDA) was used for differentiation of grapes according to the origin and variety, resulting in a correct classification of 100 and 70%, respectively.

  9. Combinatorial Solid-Phase Synthesis of Balanol Analogues

    Nielsen, John; Lyngsø, Lars Ole

    1996-01-01

    The natural product balanol has served as a template for the design and synthesis of a combinatorial library using solid-phase chemistry. Using a retrosynthetic analysis, the structural analogues have been assembled from three relatively accessible building blocks. The solid-phase chemistry inclu...

  10. Role of nanoparticles in analytical solid phase microextraction (SPME)

    Zielinska, K.; Leeuwen, van H.P.

    2013-01-01

    Solid phase microextraction (SPME) is commonly used to measure the free concentration of fairly hydrophobic substances in aqueous media on the basis of their partitioning between sample solution and a solid phase. Here we study the role of nanoparticles that may sorb the analyte in the sample

  11. All-solid-state flexible ultrathin micro-supercapacitors based on graphene.

    Niu, Zhiqiang; Zhang, Li; Liu, Lili; Zhu, Bowen; Dong, Haibo; Chen, Xiaodong

    2013-08-07

    Flexible, compact, ultrathin and all-solid-state micro-supercapacitors are prepared by coating H₃PO₄/PVA gel electrolyte onto micro-patterned rGO interdigitated electrodes prepared by combining photolithography with selective electrophoretic deposition. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Private sector participation in solid waste collection in addis ababa (Ethiopia) by involving Micro-enterprises

    M. Tilaye (Mesfin); M.P. van Dijk (Meine Pieter)

    2014-01-01

    markdownabstract__Abstract__ Privatization of urban services focuses often on the involvement of foreign enterprises. This contribution deals with micro-privatization, the partial transfer of government responsibility for solid waste collection to micro-enterprises. It tries to shed light on

  13. Air sampling with solid phase microextraction

    Martos, Perry Anthony

    There is an increasing need for simple yet accurate air sampling methods. The acceptance of new air sampling methods requires compatibility with conventional chromatographic equipment, and the new methods have to be environmentally friendly, simple to use, yet with equal, or better, detection limits, accuracy and precision than standard methods. Solid phase microextraction (SPME) satisfies the conditions for new air sampling methods. Analyte detection limits, accuracy and precision of analysis with SPME are typically better than with any conventional air sampling methods. Yet, air sampling with SPME requires no pumps, solvents, is re-usable, extremely simple to use, is completely compatible with current chromatographic equipment, and requires a small capital investment. The first SPME fiber coating used in this study was poly(dimethylsiloxane) (PDMS), a hydrophobic liquid film, to sample a large range of airborne hydrocarbons such as benzene and octane. Quantification without an external calibration procedure is possible with this coating. Well understood are the physical and chemical properties of this coating, which are quite similar to those of the siloxane stationary phase used in capillary columns. The log of analyte distribution coefficients for PDMS are linearly related to chromatographic retention indices and to the inverse of temperature. Therefore, the actual chromatogram from the analysis of the PDMS air sampler will yield the calibration parameters which are used to quantify unknown airborne analyte concentrations (ppb v to ppm v range). The second fiber coating used in this study was PDMS/divinyl benzene (PDMS/DVB) onto which o-(2,3,4,5,6- pentafluorobenzyl) hydroxylamine (PFBHA) was adsorbed for the on-fiber derivatization of gaseous formaldehyde (ppb v range), with and without external calibration. The oxime formed from the reaction can be detected with conventional gas chromatographic detectors. Typical grab sampling times were as small as 5 seconds

  14. Solid-solid phase transitions in Fe nanowires induced by axial strain

    Sandoval, Luis; Urbassek, Herbert M

    2009-01-01

    By means of classical molecular-dynamics simulations we investigate the solid-solid phase transition from a bcc to a close-packed crystal structure in cylindrical iron nanowires, induced by axial strain. The interatomic potential employed has been shown to be capable of describing the martensite-austenite phase transition in iron. We study the stress versus strain curves for different temperatures and show that for a range of temperatures it is possible to induce a solid-solid phase transition by axial strain before the elasticity is lost; these transition temperatures are below the bulk transition temperature. The two phases have different (non-linear) elastic behavior: the bcc phase softens, while the close-packed phase stiffens with temperature. We also consider the reversibility of the transformation in the elastic regimes, and the role of the strain rate on the critical strain necessary for phase transition.

  15. The development of the micro-solid propellant thruster array with improved repeatability

    Seo, Daeban; Kwon, Sejin; Lee, Jongkwang

    2012-01-01

    This paper presents the development of a micro-solid propellant thruster array with improved repeatability. The repeatability and low performance variation of each thruster unit with a high ignition success rate is essential in micro-solid propellant thruster array. To date, the study on the improvement of the repeatability has not yet been reported. As the first step for this study, we propose a new type of micro igniter, using a glass wafer called the heater-contact micro igniter. This igniter is also designed to improve the ignition characteristics of a glass-based micro igniter. The prototype of the igniter array is designed and fabricated to establish its fabrication process and to conduct its performance evaluation. Through the firing test, the performance of the heater-contact micro igniter is verified. The 5 × 5 sized micro-solid propellant thruster array is designed and fabricated applying the developed heater-contact igniter. The measured average thrust of each thruster unit is 2.542 N, and calculated standard deviation is 0.369 N. The calculated average total impulse and its standard deviation are 0.182 and 0.04 mNs, respectively. Based on these results, the improvement of repeatability is verified. Finally, the ignition control system of the micro-thruster array is developed. (paper)

  16. Wax Precipitation Modeled with Many Mixed Solid Phases

    Heidemann, Robert A.; Madsen, Jesper; Stenby, Erling Halfdan

    2005-01-01

    The behavior of the Coutinho UNIQUAC model for solid wax phases has been examined. The model can produce as many mixed solid phases as the number of waxy components. In binary mixtures, the solid rich in the lighter component contains little of the heavier component but the second phase shows sub......-temperature and low-temperature forms, are pure. Model calculations compare well with the data of Pauly et al. for C18 to C30 waxes precipitating from n-decane solutions. (C) 2004 American Institute of Chemical Engineers....

  17. The Effects of Solid Phase Additives on Sintering Properties of Alumina Bioceramic

    WANG Xin-yu; LI Shi-pu; HE Jian-hua; JIANG Xin; LI Jian-hua

    2003-01-01

    In order to reduce the sintering temperature and improve the preparing conditions of alumina bioceramics,the Mg-Zr-Y composite solid phase additives were added into high purity Al2O3 micro-powder by chemical coprecipitation method.The powder was shaped under 200MPa cold isostatic pressure,and then the biscuits were sintered at 1600℃ under normal pressure.The sintered alumina materials were tested and the sintering mechanism was discussed.The results show that physical properties of the material were improved comparatively.The Mg-Zr-Y composite solid additives could promote the sintering of alumina bioceramics and the mechanism is solid phase sintering.

  18. Development and Application of Solid Phase Extraction Method for ...

    NICO

    for the addition of organic modifier, sample load volume, conditioning solvent, washing solvent and ... Solid phase extraction, polycyclic aromatic hydrocarbons, water samples, ... such as polymeric, activated carbon or silica modified with.

  19. Determination of 8 Synthetic Food Dyes by Solid Phase Extraction ...

    Keywords: Synthetic colors, Food, Fruit flavored drinks, Solid phase extraction, RP-HPLC. Tropical Journal of ..... food dyes by thin-layer chromatography-fast atom bombardment ... food dyes in soft drinks containing natural pigments by.

  20. Investigation of binary solid phases by calorimetry and kinetic modelling

    Matovic, M.

    2007-01-01

    The traditional methods for the determination of liquid-solid phase diagrams are based on the assumption that the overall equilibrium is established between the phases. However, the result of the crystallization of a liquid mixture will typically be a non-equilibrium or metastable state of the solid. For a proper description of the crystallization process the equilibrium approach is insufficient and a kinetic approach is actually required. In this work, we show that during slow crystallizatio...

  1. The Structural Phase Transition in Solid DCN

    Dietrich, O. W.; Mackenzie, Gordon A.; Pawley, G. S.

    1975-01-01

    Neutron scattering measurements on deuterated hydrogen cyanide have shown that the structural phase change from a tetragonal to an orthorhombic form at 160K is a first-order transition. A transverse acoustic phonon mode, which has the symmetry of the phase change, was observed at very low energies...

  2. Solid-Phase S-Alkylation Promoted by Molecular Sieves.

    Calce, Enrica; Leone, Marilisa; Mercurio, Flavia Anna; Monfregola, Luca; De Luca, Stefania

    2015-11-20

    A solid-phase S-alkylation procedure to introduce chemical modification on the cysteine sulfhydryl group of a peptidyl resin is reported. The reaction is promoted by activated molecular sieves and consists of a solid-solid process, since both the catalyst and the substrate are in a solid state. The procedure was revealed to be efficient and versatile, particularly when used in combination with the solution S-alkylation approach, allowing for the introduction of different molecular diversities on the same peptide molecule.

  3. Multiresidue analysis of oestrogenic compounds in cow, goat, sheep and human milk using core-shell polydopamine coated magnetic nanoparticles as extraction sorbent in micro-dispersive solid-phase extraction followed by ultra-high-performance liquid chromatography tandem mass spectrometry.

    Socas-Rodríguez, Bárbara; Hernández-Borges, Javier; Herrera-Herrera, Antonio V; Rodríguez-Delgado, Miguel Ángel

    2018-03-01

    In this work, the suitability of Fe 3 O 4 nanoparticles coated with polydopamine was evaluated as sorbent for the extraction of a group of 21 compounds with oestrogenic activity including seven phytoestrogens, six mycotoxins as well as four synthetic and four natural oestrogens from different types of milk, including sheep milk, in which the evaluation of oestrogenic compounds have never been developed before. Extraction was carried out using magnetic micro-dispersive solid-phase extraction after a previous deproteinisation step. Separation, determination and quantification of the target analytes were achieved by ultra-high-performance liquid chromatography coupled to triple quadrupole-tandem mass spectrometry. The methodology was validated for five milk samples using 17β-estradiol-2,4,16,16,17-d 5 as internal standard for natural and synthetic oestrogens, β-zearalanol-10,10,11,12,12-d 5 for mycotoxins and prunetin for phytoestrogens. Recovery values ranged from 70 to 120% for the five types of matrices with relative standard deviation values lower than 18%. Limits of quantification of the method were in the range 0.55-11.8 μg L -1 for all samples. Graphical abstract General scheme of the multiresidue analysis of oestrogenic compounds in milk using core-shell polydopamine coated magnetic nanoparticles as extraction sorbent in μ-dSPE.

  4. Solid-solid phase change thermal storage application to space-suit battery pack

    Son, Chang H.; Morehouse, Jeffrey H.

    1989-01-01

    High cell temperatures are seen as the primary safety problem in the Li-BCX space battery. The exothermic heat from the chemical reactions could raise the temperature of the lithium electrode above the melting temperature. Also, high temperature causes the cell efficiency to decrease. Solid-solid phase-change materials were used as a thermal storage medium to lower this battery cell temperature by utilizing their phase-change (latent heat storage) characteristics. Solid-solid phase-change materials focused on in this study are neopentyl glycol and pentaglycerine. Because of their favorable phase-change characteristics, these materials appear appropriate for space-suit battery pack use. The results of testing various materials are reported as thermophysical property values, and the space-suit battery operating temperature is discussed in terms of these property results.

  5. Micro solid oxide fuel cell on the chip. Final report

    Stutz, M.; Hotz, N.; Bieri, N.; Poulikakos, D.

    2006-07-01

    The aim of this project is the numerical and experimental investigation of hydrocarbon-to-syngas reforming in micro reformers for incorporation into an entire micro fuel cell system. Numerical simulations are used to achieve deeper understanding of several determining aspects in such a micro reformer. These insights are used to optimize the reforming performance by proper choice of operational and geometrical parameters of a reformer. These numerical results are continued by comprehensive experimental studies. In the first chapter, the effect of wall conduction of a tubular methane micro reformer is investigated numerically. Methane is used as the representative hydrocarbon because its detailed surface reaction mechanism is known. It is found that the axial wall conduction can strongly influence the performance of the microreactor and should not be neglected without a careful a priori investigation of its impact. In the second chapter, the effect of the catalyst amount and reactor geometry on the reforming process was investigated. It was found that the hydrogen selectivity changes significantly with varying catalyst loading. Thus, the reaction path leading to higher hydrogen production becomes more important by increasing the catalyst surface site density on the active surface. Another unexpected result is the presence of optimum channel geometry and optimum catalyst amount. In the third chapter of this project, the capability of flame-made Rh/Ce{sub 0.5}Zr{sub 0.5}O{sub 2} nanoparticles catalyzing the reforming of butane to H{sub 2}- and CO-rich syngas was investigated experimentally in a packed bed reactor. The main goal of this study was the efficient reforming of butane at temperatures between 500 and 600 {sup o}C for a micro intermediate-temperature SOFC system. Our results showed that Rh/Ce{sub 0.5}Zr{sub 0.5}O{sub 2} nanoparticles proved to be a very promising material for butane-to-syngas reforming with complete butane conversion and a hydrogen yield of 77

  6. N-Acyliminium Intermediates in Solid-Phase Synthesis

    Quement, Sebastian Thordal le; Petersen, Rico; Meldal, M.

    2010-01-01

    N-Acyliminium ions are powerful intermediates in synthetic organic chemistry. Examples of their use are numerous in solution-phase synthesis, but there are unmerited few reports on these highly reactive electrophiles in solid-phase synthesis. The present review covers the literature to date and i...

  7. Investigation of binary solid phases by calorimetry and kinetic modelling

    Matovic, M.

    2007-01-01

    The traditional methods for the determination of liquid-solid phase diagrams are based on the assumption that the overall equilibrium is established between the phases. However, the result of the crystallization of a liquid mixture will typically be a non-equilibrium or metastable state of the

  8. Preparation, characterization and thermal properties of PMMA/n-heptadecane microcapsules as novel solid-liquid microPCM for thermal energy storage

    Sari, Ahmet; Alkan, Cemil; Karaipekli, Ali

    2010-01-01

    This study is focused on the preparation, characterization and thermal properties of microencapsulated n-heptadecane with polymethylmethacrylate shell. The PMMA/heptadecane microcapsules were synthesized as novel solid-liquid microencapsulated phase change material (microPCMs) by emulsion polymerization method. The chemical and thermal characterization of the microPCMs were investigated using scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and thermogravimetry analysis (TGA). The diameters of microPCMs were found in the narrow range (0.14-0.40 μm) under the stirring speed of 2000 rpm. The spherical surfaces of microPCMs were smooth and compact. The DSC results show that microPCMs have good energy storage capacity. Thermal cycling test showed that the microPCMs have good thermal reliability with respect to the changes in their thermal properties after repeated 5000 thermal cycling. TGA analyses also indicated that the microPCMs degraded in three steps and have good thermal stability. Based on all results, it can be considered that the PMMA/heptadecane microcapsules as novel solid-liquid microPCMs have good energy storage potential.

  9. Heterogeneous Ferroelectric Solid Solutions Phases and Domain States

    Topolov, Vitaly

    2012-01-01

    The book deals with perovskite-type ferroelectric solid solutions for modern materials science and applications, solving problems of complicated heterophase/domain structures near the morphotropic phase boundary and applications to various systems with morphotropic phases. In this book domain state–interface diagrams are presented for the interpretation of heterophase states in perovskite-type ferroelectric solid solutions. It allows to describe the stress relief in the presence of polydomain phases, the behavior of unit-cell parameters of coexisting phases and the effect of external electric fields. The novelty of the book consists in (i) the first systematization of data about heterophase states and their evolution in ferroelectric solid solutions (ii) the general interpretation of heterophase and domain structures at changing temperature, composition or electric field (iii) the complete analysis of interconnection domain structures, unit-cell parameters changes, heterophase structures and stress relief.

  10. Phase diagram of a Lennard-Jones solid

    Choi, Y.; Ree, T.; Ree, F.H.

    1993-01-01

    A phase diagram of a Lennard-Jones solid at kT/ε≥0.8 is constructed by our recent perturbation theory. It shows the stability of the face-centered-cubic phase except within a small pressure and temperature domain, where the hexagonal-close packed phase may occur. The theory predicts anharmonic contributions to the Helmholtz free energy (important to the crystal stability) in good agreement with Monte Carlo data

  11. Biogasification of solid wastes by two-phase anaerobic fermentation

    Ghosh, S.; Vieitez, E.R.; Liu, T.; Kato, Y.

    1997-01-01

    Municipal, industrial and agricultural solid wastes, and biomass deposits, cause large-scale pollution of land and water. Gaseous products of waste decomposition pollute the air and contribute to global warming. This paper describes the development of a two-phase fermentation system that alleviates methanogenic inhibition encountered with high-solids feed, accelerates methane fermentation of the solid bed, and captures methane (renewable energy) for captive use to reduce global warming. The innovative system consisted of a solid bed reactor packed with simulated solid waste at a density of 160 kg/m 3 and operated with recirculation of the percolated culture (bioleachate) through the bed. A rapid onset of solids hydrolysis, acidification, denitrification and hydrogen gas formation was observed under these operating conditions. However, these fermentative reactions stopped at a total fatty acids concentration of 13,000 mg/l (as acetic) at pH 5, with a reactor head-gas composition of 75 percent carbon dioxide, 20 percent nitrogen, 2 percent hydrogen and 3 percent methane. Fermentation inhibition was alleviated by moving the bioleachate to a separate methane-phase fermenter, and recycling methanogenic effluents at pH 7 to the solid bed. Coupled operation of the two reactors promoted methanogenic conversion of the high-solids feed. (author)

  12. Surface phase transitions in cu-based solid solutions

    Zhevnenko, S. N.; Chernyshikhin, S. V.

    2017-11-01

    We have measured surface energy in two-component Cu-based systems in H2 + Ar gas atmosphere. The experiments on solid Cu [Ag] and Cu [Co] solutions show presence of phase transitions on the surfaces. Isotherms of the surface energy have singularities (the minimum in the case of copper solid solutions with silver and the maximum in the case of solid solutions with cobalt). In both cases, the surface phase transitions cause deficiency of surface miscibility: formation of a monolayer (multilayer) (Cu-Ag) or of nanoscale particles (Cu-Co). At the same time, according to the volume phase diagrams, the concentration and temperature of the surface phase transitions correspond to the solid solution within the volume. The method permits determining the rate of diffusional creep in addition to the surface energy. The temperature and concentration dependence of the solid solutions' viscosity coefficient supports the fact of the surface phase transitions and provides insights into the diffusion properties of the transforming surfaces.

  13. Phase coexistence in ferroelectric solid solutions: Formation of monoclinic phase with enhanced piezoelectricity

    Xiaoyan Lu

    2016-10-01

    Full Text Available Phase morphology and corresponding piezoelectricity in ferroelectric solid solutions were studied by using a phenomenological theory with the consideration of phase coexistence. Results have shown that phases with similar energy potentials can coexist, thus induce interfacial stresses which lead to the formation of adaptive monoclinic phases. A new tetragonal-like monoclinic to rhombohedral-like monoclinic phase transition was predicted in a shear stress state. Enhanced piezoelectricity can be achieved by manipulating the stress state close to a critical stress field. Phase coexistence is universal in ferroelectric solid solutions and may provide a way to optimize ultra-fine structures and proper stress states to achieve ultrahigh piezoelectricity.

  14. A grid-connected single-phase photovoltaic micro inverter

    Wen, X. Y.; Lin, P. J.; Chen, Z. C.; Wu, L. J.; Cheng, S. Y.

    2017-11-01

    In this paper, the topology of a single-phase grid-connected photovoltaic (PV) micro-inverter is proposed. The PV micro-inverter consists of DC-DC stage with high voltage gain boost and DC-AC conversion stage. In the first stage, we apply the active clamp circuit and two voltage multipliers to achieve soft switching technology and high voltage gain. In addition, the flower pollination algorithm (FPA) is employed for the maximum power point tracking (MPPT) in the PV module in this stage. The second stage cascades a H-bridge inverter and LCL filter. To feed high quality sinusoidal power into the grid, the software phase lock, outer voltage loop and inner current loop control method are adopted as the control strategy. The performance of the proposed topology is tested by Matlab/Simulink. A PV module with maximum power 300W and maximum power point voltage 40V is applied as the input source. The simulation results indicate that the proposed topology and the control strategy are feasible.

  15. Thermodynamic Performance Study of Biomass Gasification, Solid Oxide Fuel Cell and Micro Gas Turbine Hybrid Systems

    Bang-Møller, Christian; Rokni, Masoud

    2010-01-01

    A system level modelling study of three combined heat and power systems based on biomass gasification is presented. Product gas is converted in a micro gas turbine (MGT) in the first system, in a solid oxide fuel cell (SOFC) in the second system and in a combined SOFC–MGT arrangement in the third...

  16. The preparation method of solid boron solution in silicon carbide in the form of micro powder

    Pampuch, R.; Stobierski, L.; Lis, J.; Bialoskorski, J.; Ermer, E.

    1993-01-01

    The preparation method of solid boron solution in silicon carbide in the form of micro power has been worked out. The method consists in introducing mixture of boron, carbon and silicon and heating in the atmosphere of inert gas to the 1573 K

  17. Linkage of biomolecules to solid phases for immunoassay

    Chapman, R.S.

    1998-01-01

    Topics covered by this lecture include a brief review of the principal methods of linkage of biomolecules to solid phase matrices. Copies of the key self explanatory slides are presented as figures together with reprints of two publications by the author dealing with a preferred chemistry for the covalent linkage of antibodies to hydroxyl and amino functional groups and the effects of changes in solid phase matrix and antibody coupling chemistry on the performance of a typical excess reagent immunoassay for thyroid stimulating hormone

  18. Solid-phase synthesis of complex and pharmacologically interesting heterocycles

    Nielsen, Thomas Eiland

    2009-01-01

    Efficient routes for the creation of heterocycles continue to be one of the primary goals for solid-phase synthesis. Recent advances in this field rely most notably on transition-metal-catalysis and N-acyliminium chemistry to mediate a range of cyclization processes for the generation of compounds...... with significant structural complexity and diversity. This review describes some of the most systematic solid-phase approaches that are potentially suited for pharmaceutical applications, that is, the methods described are useful for the synthesis of compound collections, and exhibit tunable stereochemistry...

  19. Colonyzer: automated quantification of micro-organism growth characteristics on solid agar

    Young Alexander

    2010-05-01

    Full Text Available Abstract Background High-throughput screens comparing growth rates of arrays of distinct micro-organism cultures on solid agar are useful, rapid methods of quantifying genetic interactions. Growth rate is an informative phenotype which can be estimated by measuring cell densities at one or more times after inoculation. Precise estimates can be made by inoculating cultures onto agar and capturing cell density frequently by plate-scanning or photography, especially throughout the exponential growth phase, and summarising growth with a simple dynamic model (e.g. the logistic growth model. In order to parametrize such a model, a robust image analysis tool capable of capturing a wide range of cell densities from plate photographs is required. Results Colonyzer is a collection of image analysis algorithms for automatic quantification of the size, granularity, colour and location of micro-organism cultures grown on solid agar. Colonyzer is uniquely sensitive to extremely low cell densities photographed after dilute liquid culture inoculation (spotting due to image segmentation using a mixed Gaussian model for plate-wide thresholding based on pixel intensity. Colonyzer is robust to slight experimental imperfections and corrects for lighting gradients which would otherwise introduce spatial bias to cell density estimates without the need for imaging dummy plates. Colonyzer is general enough to quantify cultures growing in any rectangular array format, either growing after pinning with a dense inoculum or growing with the irregular morphology characteristic of spotted cultures. Colonyzer was developed using the open source packages: Python, RPy and the Python Imaging Library and its source code and documentation are available on SourceForge under GNU General Public License. Colonyzer is adaptable to suit specific requirements: e.g. automatic detection of cultures at irregular locations on streaked plates for robotic picking, or decreasing analysis time by

  20. Detection of viral antigens by solid phase radioimmunoassay on polyethylene film

    Prokudina, E N; Semenova, N P; Zhdanov, V M

    1986-04-01

    Polyethylene film, without any pretreatment, may serve as a solid phase (SP) for RIA. Viral antigens (HBsAg, and influenza virus) are detected by SP-RIA on the film with a sensitivity of about 2-3 ng/ml or 40-60 pg/assay. The use of polyethylene film allows one to record RIA autographically. The use of micro amounts of reagents and specimens tested is an added advantage. No special equipment is necessary, the method is inexpensive, easy to perform and may be used for mass screening. (Auth.). 7 refs.; 4 figs.

  1. Using reweighting and free energy surface interpolation to predict solid-solid phase diagrams

    Schieber, Natalie P.; Dybeck, Eric C.; Shirts, Michael R.

    2018-04-01

    Many physical properties of small organic molecules are dependent on the current crystal packing, or polymorph, of the material, including bioavailability of pharmaceuticals, optical properties of dyes, and charge transport properties of semiconductors. Predicting the most stable crystalline form at a given temperature and pressure requires determining the crystalline form with the lowest relative Gibbs free energy. Effective computational prediction of the most stable polymorph could save significant time and effort in the design of novel molecular crystalline solids or predict their behavior under new conditions. In this study, we introduce a new approach using multistate reweighting to address the problem of determining solid-solid phase diagrams and apply this approach to the phase diagram of solid benzene. For this approach, we perform sampling at a selection of temperature and pressure states in the region of interest. We use multistate reweighting methods to determine the reduced free energy differences between T and P states within a given polymorph and validate this phase diagram using several measures. The relative stability of the polymorphs at the sampled states can be successively interpolated from these points to create the phase diagram by combining these reduced free energy differences with a reference Gibbs free energy difference between polymorphs. The method also allows for straightforward estimation of uncertainties in the phase boundary. We also find that when properly implemented, multistate reweighting for phase diagram determination scales better with the size of the system than previously estimated.

  2. Experimental and molecular docking investigation on metal-organic framework MIL-101(Cr) as a sorbent for vortex assisted dispersive micro-solid-phase extraction of trace 5-nitroimidazole residues in environmental water samples prior to UPLC-MS/MS analysis.

    Lu, Nan; Wang, Ting; Zhao, Pan; Zhang, Lianjun; Lun, Xiaowen; Zhang, Xueli; Hou, Xiaohong

    2016-11-01

    In the presented work, metal-organic framework (MOF) material MIL-101(Cr) (MIL, Matérial Institute Lavoisier) was used as a sorbent for vortex assisted dispersive micro-solid-phase extraction (VA-D-μ-SPE) of trace amount of metronidazole (MNZ), ronidazole (RNZ), secnidazole (SNZ), dimetridazole (DMZ), tinidazole (TNZ), and ornidazole (ONZ) in different environmental water samples. Ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) was used to quantify the target analytes. The extraction conditions, including type of sorbents, amount of MIL-101(Cr), solution pH, extraction method, extraction time, effect of salt, and elution conditions were investigated. Upon the optimal conditions, the developed method showed an excellent extraction performance with the average recovery ranging from 75.2 to 98.8 %. Good sensitivity levels were achieved with the detection limits of 0.03∼0.06 μg/L and the quantitation limits of 0.09∼0.20 μg/L. The linear ranges were varied from 0.1 to 20 for SNZ and ONZ and from 0.2 to 40 μg/L for MNZ, RNZ, DMZ, and TNZ (r 2  > 0.992), and repeatability of the method was satisfactory with the relative standard deviations (RSD) extraction and determination of 5-nitroimidazoles (5-NDZs) in 12 real water samples, showing the positive findings of MNZ and TNZ ranging from 0.3 to 1.0 μg/L. Furthermore, molecular docking was applied to explain the molecular interactions and free binding energies between MIL-101(Cr) and 5-NDZs, providing a deep insight into the adsorption mechanism. The proposed method exhibited the advantages of simplicity, rapidly, less solvent consumption, ease of operation, higher sensitivity, and lower matrix effect. Graphical abstract Schematic diagram of the extraction process and molecular docking investigation.

  3. A combination of computational-experimental study on metal-organic frameworks MIL-53(Al) as sorbent for simultaneous determination of estrogens and glucocorticoids in water and urine samples by dispersive micro-solid-phase extraction coupled to UPLC-MS/MS.

    Gao, Guihua; Li, Sijia; Li, Shuo; Wang, Yudan; Zhao, Pan; Zhang, Xiangyu; Hou, Xiaohong

    2018-04-01

    In this work, computational and experimental methods were used to study the adsorption of estrogens and glucocorticoids on metal-organic frameworks (MOFs). Computer-aided molecular simulation was applied to predict the adsorption of eight analytes on four MOFs (MIL-101(Cr), MIL-100(Fe), MIL-53(Al), and UiO-66(Zr)) by examining molecular interactions and calculating free binding energies. Subsequently, the four water-stable MOFs were synthesized and evaluated as adsorbents for the target hormones in aqueous solution. As the MOF exhibiting the highest adsorption capacity in both computations and experiments, MIL-53(Al) was chosen as a sorbent to develop a dispersive micro-solid-phase extraction procedure coupled to ultra-performance liquid chromatography tandem mass spectrometry for simultaneous determination of the target analytes in water and human urine samples. Experimental parameters affecting the extraction recoveries, including pH, ionic strength, MIL-53(Al) amount, extraction time, desorption time, and desorption solvent, were optimized. The optimized method provided a linear range of 0.005025-368.6μg/L with good correlation coefficients (0.9982 ≤ r 2 ≤ 0.9992), and limits of detection (S/N = 3) and quantification (S/N = 10) of 0.0015-1.0μg/L and 0.005-1.8μg/L, respectively. The analyte recoveries were in the range of 80.6-98.4% in water samples and 88.4-93.2% in urine samples. Furthermore, MIL-53(Al) showed good stability over 10 extraction cycles (RSD extraction efficiencies for MOFs and targets, providing new directions for the development and utilization of MOFs. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Analytical study of solids-gas two phase flow

    Hosaka, Minoru

    1977-01-01

    Fundamental studies were made on the hydrodynamics of solids-gas two-phase suspension flow, in which very small solid particles are mixed in a gas flow to enhance the heat transfer characteristics of gas cooled high temperature reactors. Especially, the pressure drop due to friction and the density distribution of solid particles are theoretically analyzed. The friction pressure drop of two-phase flow was analyzed based on the analytical result of the single-phase friction pressure drop. The calculated values of solid/gas friction factor as a function of solid/gas mass loading are compared with experimental results. Comparisons are made for Various combinations of Reynolds number and particle size. As for the particle density distribution, some factors affecting the non-uniformity of distribution were considered. The minimum of energy dispersion was obtained with the variational principle. The suspension density of particles was obtained as a function of relative distance from wall and was compared with experimental results. It is concluded that the distribution is much affected by the particle size and that the smaller particles are apt to gather near the wall. (Aoki, K.)

  5. All solid-state SBS phase conjugate mirror

    Dane, C.B.; Hackel, L.A.

    1999-03-09

    A stimulated Brillouin scattering (SBS) phase conjugate laser mirror uses a solid-state nonlinear gain medium instead of the conventional liquid or high pressure gas medium. The concept has been effectively demonstrated using common optical-grade fused silica. An energy threshold of 2.5 mJ and a slope efficiency of over 90% were achieved, resulting in an overall energy reflectivity of >80% for 15 ns, 1 um laser pulses. The use of solid-state materials is enabled by a multi-pass resonant architecture which suppresses transient fluctuations that would otherwise result in damage to the SBS medium. This all solid state phase conjugator is safer, more reliable, and more easily manufactured than prior art designs. It allows nonlinear wavefront correction to be implemented in industrial and defense laser systems whose operating environments would preclude the introduction of potentially hazardous liquids or high pressure gases. 8 figs.

  6. Solid-phase oligosaccharide and glycopeptide synthesis using glycosynthases

    Tolborg, Jakob Fjord; Petersen, Lars; Jensen, Knud Jørgen

    2002-01-01

    and the prospect of automatability. Here, we report the first application of glycosynthases to solid-phase oligosaccharide synthesis by use of the 51 kDa serine and glycine mutants of Agrobacterium sp. beta-glucosidase, Abg E358S and E358G. Acceptors were linked to PEGA resin through a backbone amide linker (BAL...

  7. Zirconium determination in rocks by solid-phase spectrophotometry

    Brykina, G.D.; Lebedeva, G.G.; Agapova, G.F.; AN SSSR, Moscow

    1990-01-01

    A method was developed for determination of zirconium in rocks by solid-phase spectrophotometry using AV-17x8-Cl anion exchanger modified with xylenol orange. Relative standard deviation at the level of (2-4.9)x10 -3 % ZrO 2 was about 0.245

  8. Solid Phase Characterization of Tank 241-C-105 Grab Samples

    Ely, T. M.; LaMothe, M. E.; Lachut, J. S.

    2016-01-01

    The solid phase characterization (SPC) of three grab samples from single-shell Tank 241-C-105 (C-105) that were received at the laboratory the week of October 26, 2015, has been completed. The three samples were received and broken down in the 11A hot cells.

  9. Phase segregation in cerium-lanthanum solid solutions

    Belliere, V.; Joorst, G; Stephan, O; de Groot, FMF; Weckhuysen, BM

    2006-01-01

    Electron energy-loss spectroscopy (EELS) in combination with scanning transmission electron microscopy ( STEM) reveals that the La enrichment at the surface of cerium-lanthanum solid solutions is an averaged effect and that segregation occurs in a mixed oxide phase. This separation occurs within a

  10. Solid-phase microextraction for the analysis of biological samples

    Theodoridis, G; Koster, EHM; de Jong, GJ

    2000-01-01

    Solid-phase microextraction (SPME) has been introduced for the extraction of organic compounds from environmental samples. This relatively new extraction technique has now also gained a lot of interest in a broad field of analysis including food, biological and pharmaceutical samples. SPME has a

  11. Development of headspace solid-phase microextraction method for ...

    A headspace solid-phase microextraction (HS-SPME) method was developed as a preliminary investigation using univariate approach for the analysis of 14 multiclass pesticide residues in fruits and vegetable samples. The gas chromatography mass spectrometry parameters (desorption temperature and time, column flow ...

  12. Solid phase radioimmunoassay for HBe Ag and anti-HBe

    Froesner, G G; Deinhardt, F [Muenchen Univ. (Germany, F.R.). Inst. fuer Hygiene und Medizinische Mikrobiologie; Sugg, U [Tuebingen Univ. (Germany, F.R.). Abt. fuer Transfusionswesen mit Blutbank; Haas, H [Staedtische Krankenanstalten Esslingen (Germany, F.R.). Zentrallabor; Overby, R L [Abbott Labs., North Chicago, IL (USA)

    1978-04-01

    A highly sensitive solid phase radioimmunoassay for the detection of hepatitis Be-antigen (HBeAg) and anti-HBe is described. Iodine-125 labelled anti-HBe is used as a tracer. The assay is about 500 foLd more sensitive than immunodiffusion.

  13. Solid-phase synthesis of 3-amino-2-pyrazolines

    Nielsen, John

    1998-01-01

    The development of a solid-phase synthesis of 3-amino-2-pyrazolines is described. Conjugate addition of hydrazines to alpha,beta-unsaturated nitriles followed by cyclization yields 3-amino-2-pyrazolines. Acylation or sulfonation of the free amino-group yields a 24 member library of 3-amino-2...

  14. A solid-phase-radioimmunoassay for total serum thyroxine

    Moedder, G.; Sokolowski, G.

    1978-01-01

    A new solid phase radioimmunoassay for total serum thyroxine was evaluated over a longer time under clinical routine conditions and compared with an established test system. The results show up that the T 4 values are precise, reliable and reproducible, the is incomplicate to handle and well suitable for semiautomatic pipetting systems. (orig.) 891 MG [de

  15. Copper welding in solid phase; Svarka medi v tverdoj faze

    Avagyan, V Sh

    1993-12-31

    An analysis of the publications on the technology of diffusion welding of copper in solid phase is carried out. The aspects of diffusion welding of copper with silver, aluminium, nickels, chromium, titanium, stainless steel and refractory metals are considered 35 refs.

  16. Solid phase separation technique for use in radioimmunoassays

    Tu, J.I.

    1979-01-01

    A radioimmunoassay procedure, and article of manufacture for carrying out that procedure, are disclosed herein. The solid phase separation technique utilized in the radioimmunoassay of this invention utilizes a test tube, the internal surface of which has been coated with two antibody layers

  17. Solid-Phase Extraction Combined with High Performance Liquid ...

    Methods: Solid-phase extraction method was employed for the extraction of the estrogen from milk and high performance liquid chromatography-diode array detector (HPLC-DAD) was used for the determination of estrogen. Results: Optimal chromatographic conditions were achieved on an Eclipse XDB-C18 column at a ...

  18. Gradiently Polymerized Solid Electrolyte Meets with Micro/Nano-Structured Cathode Array.

    Dong, Wei; Zeng, Xian-Xiang; Zhang, Xu-Dong; Li, Jin-Yi; Shi, Ji-Lei; Xiao, Yao; Shi, Yang; Wen, Rui; Yin, Ya-Xia; Wang, Tai-Shan; Wang, Chun-Ru; Guo, Yu-Guo

    2018-05-02

    The poor contact between the solid-state electrolyte and cathode materials leads to high interfacial resistance, severely limiting the rate capability of solid Li metal batteries. Herein, an integrative battery design is introduced with a gradiently polymerized solid electrolyte (GPSE), a micro-channel current collector array and nano-sized cathode particles. In-situ formed GPSE encapsulates cathode nanoparticles in the micro-channel with ductile inclusions to lower interfacial impedance, and the stiff surface layer of GPSE toward anode suppresses Li dendrites growth. Li metal batteries based on GPSE and Li-free hydrogenated V2O5 (V2O5-H) cathode exhibit an outstanding high-rate response of up to 5 C (the capacity ratio of 5 C / 1 C is 90.3%) and an ultralow capacity fade rate of 0.07% per cycle over 300 cycles. Other Li-containing cathodes as LiFePO4 and LiNi0.5Mn0.3Co0.2O2 can also operate effectively at 5 C and 2 C rate, respectively. Such an ingenious design may provide new insights into other solid metal batteries through interfacial engineering manipulation at micro and nano level.

  19. Axial dispersion of gas and solid phases in a gas—solid packed column at trickle flow

    Roes, A.W.M.; van Swaaij, Willibrordus Petrus Maria

    1979-01-01

    Axial dispersion of gas and solid phases in a gas—solid packed column at trickle flow, a promising new countercurrent operation, was evaluated using residence time distribution (RTD) experiments. The column was packed with dumped Pall rings, the gas phase was air at ambient conditions and the solid

  20. Solid-phase synthesis of molecularly imprinted nanoparticles.

    Canfarotta, Francesco; Poma, Alessandro; Guerreiro, Antonio; Piletsky, Sergey

    2016-03-01

    Molecularly imprinted polymers (MIPs) are synthetic materials, generally based on acrylic or methacrylic monomers, that are polymerized in the presence of a specific target molecule called the 'template' and capable of rebinding selectively to this target molecule. They have the potential to be low-cost and robust alternatives to biomolecules such as antibodies and receptors. When prepared by traditional synthetic methods (i.e., with free template in solution), their usefulness has been limited by high binding site heterogeneity, the presence of residual template and the fact that the production methods are complex and difficult to standardize. To overcome some of these limitations, we developed a method for the synthesis of MIP nanoparticles (nanoMIPs) using an innovative solid-phase approach, which relies on the covalent immobilization of the template molecules onto the surface of a solid support (glass beads). The obtained nanoMIPs are virtually free of template and demonstrate high affinity for the target molecule (e.g., melamine and trypsin in our published work). Because of an affinity separation step performed on the solid phase after polymerization, poor binders and unproductive polymer are removed, so the final product has more uniform binding characteristics. The overall protocol, starting from the immobilization of the template onto the solid phase and including the purification and characterization of the nanoparticles, takes up to 1 week.

  1. In-line phase contrast micro-CT reconstruction for biomedical specimens.

    Fu, Jian; Tan, Renbo

    2014-01-01

    X-ray phase contrast micro computed tomography (micro-CT) can non-destructively provide the internal structure information of soft tissues and low atomic number materials. It has become an invaluable analysis tool for biomedical specimens. Here an in-line phase contrast micro-CT reconstruction technique is reported, which consists of a projection extraction method and the conventional filter back-projection (FBP) reconstruction algorithm. The projection extraction is implemented by applying the Fourier transform to the forward projections of in-line phase contrast micro-CT. This work comprises a numerical study of the method and its experimental verification using a biomedical specimen dataset measured at an X-ray tube source micro-CT setup. The numerical and experimental results demonstrate that the presented technique can improve the imaging contrast of biomedical specimens. It will be of interest for a wide range of in-line phase contrast micro-CT applications in medicine and biology.

  2. Simulation For Synchronization Of A Micro-Grid With Three-Phase Systems

    Mohammad Jafari Far

    2015-08-01

    Full Text Available Abstract today due to the high reliability of the micro-grids they have developed significantly. They have two states of operation the island state and connection to the main grid. Under certain circumstances the micro-grid is connected to or disconnected from the network. Synchronization of a micro-grid with the network must be done when its voltage is synchronized with the voltage in the main grid. Phase lock loops are responsible to identify the voltage phase of the micro-gird and the main grid and when these two voltages are in the same phase they connect the micro-grid to the main grid. In this research the connection of a micro-grid to the main grid in the two phases of synchronous and asynchronous voltage is simulated and investigated.

  3. C18, C8, and perfluoro reversed phases on diamond for solid-phase extraction.

    Saini, Gaurav; Wiest, Landon A; Herbert, David; Biggs, Katherine N; Dadson, Andrew; Vail, Michael A; Linford, Matthew R

    2009-04-17

    In spite of advances in solid-phase extraction (SPE) technology there are certain disadvantages to current SPE silica-based, column packings. The pH range over which extraction can occur is limited and each column is generally only used once. New diamond-based reversed SPE phases (C(18), C(8), and perfluorinated) were developed in our laboratories. Studies were done which show that these phases do not have the same limitations as traditional silica-based stationary phases. The synthesis and properties of these diamond-based phases are presented, and the stability, percent recovery, and column capacity are given for the C(18) phase.

  4. Solid phase synthesis and antiprotozoal evaluation of di- and trisubstituted 5'-carboxamidoadenosine analogues.

    Rodenko, Boris; Detz, Remko J; Pinas, Victorine A; Lambertucci, Catia; Brun, Reto; Wanner, Martin J; Koomen, Gerrit-Jan

    2006-03-01

    The rapid increase of resistance to drugs commonly used in the treatment of tropical diseases such as malaria and African sleeping sickness calls for the prompt development of new safe and efficacious drugs. The pathogenic protozoan parasites lack the capability of synthesising purines de novo and they take up preformed purines from their host through various transmembrane transporters. Adenosine derivatives constitute a class of potential therapeutics due to their selective internalisation by these transporters. Automated solid-phase synthesis can speed up the process of lead finding and we pursued the solid-phase synthesis of di- and trisubstituted 5'-carboxamidoadenosine derivatives by using a safety-catch approach. While efforts with Kenner's sulfonamide linker remained fruitless, successful application of the hydrazide safety-catch linker allowed the construction of two representative combinatorial libraries. Their antiprotozoal evaluation identified two compounds with promising activity: N(6)-benzyl-5'-N-phenylcarboxamidoadenosine with an IC(50) value of 0.91 microM against Trypanosoma brucei rhodesiense and N(6)-diphenylethyl-5'-phenylcarboxamidoadenosine with an IC(50) value of 1.8 microM against chloroquine resistant Plasmodium falciparum.

  5. Liquid-phase and solid-phase radioimmunoassay with herpes simplex virus type 1 nucleocapsids

    Bystricka, M.; Rajcani, J.; Libikova, H.; Sabo, A.; Foeldes, O.; Sadlon, J.

    1985-01-01

    Liquid-phase radioimmunoassay and solid-phase radioimmunoassay are described using 125 I-labelled or immobilized nucleocapsids (NC) of herpes simplex virus (HSV) type1. These techniques appeared sensitive and specific for quantitation of HSV-NC antigens and corresponding antibodies. (author)

  6. On the study of the solid-solid phase transformation of TlBiTe2

    Chrissafis, K.; Vinga, E.S.; Paraskevopoulos, K.M.; Polychroniadis, E.K.

    2003-01-01

    The narrow gap semiconductor TlBiTe 2 undergoes a solid-solid phase transformation from the rhombohedral (D 3d ) to the cubic (O h ) phase. The present paper deals with the study of this phase transformation combining the results of Differential Scanning Calorimetry (DSC) and Transmission Electron Microscopy (TEM). It has been found that during heating the transformation is an athermal activated process, which can be described only by a combination of more than one processes while during cooling it exhibits an expectable thermal hysteresis due to the volume difference. The results of the kinetic analysis combined with the electron microscopy findings, supported also by the Fourier Transform Infrared (FTIR) spectroscopy ones, lead to the conclusion that TlBiTe 2 undergoes a multiple-step, displacive, martensitic type transformation. (Abstract Copyright [2003], Wiley Periodicals, Inc.)

  7. Studies in Solid Phase Peptide Synthesis: A Personal Perspective

    Mitchell, A R

    2007-06-01

    By the early 1970s it had became apparent that the solid phase synthesis of ribonuclease A could not be generalized. Consequently, virtually every aspect of solid phase peptide synthesis (SPPS) was reexamined and improved during the decade of the 1970s. The sensitive detection and elimination of possible side reactions (amino acid insertion, N{sup {alpha}}-trifluoroacetylation, N{sup {alpha}{var_epsilon}}-alkylation) was examined. The quantitation of coupling efficiency in SPPS as a function of chain length was studied. A new and improved support for SPPS, the 'PAM-resin', was prepared and evaluated. These and many other studies from the Merrifield laboratory and elsewhere increased the general acceptance of SPPS leading to the 1984 Nobel Prize in Chemistry for Bruce Merrifield.

  8. Semi-automated microwave assisted solid-phase peptide synthesis

    Pedersen, Søren Ljungberg

    with microwaves for SPPS has gained in popularity as it for many syntheses has provided significant improvement in terms of speed, purity, and yields, maybe especially in the synthesis of long and "difficult" peptides. Thus, precise microwave heating has emerged as one new parameter for SPPS, in addition...... to coupling reagents, resins, solvents etc. We have previously reported on microwave heating to promote a range of solid-phase reactions in SPPS. Here we present a new, flexible semi-automated instrument for the application of precise microwave heating in solid-phase synthesis. It combines a slightly modified...... Biotage Initiator microwave instrument, which is available in many laboratories, with a modified semi-automated peptide synthesizer from MultiSynTech. A custom-made reaction vessel is placed permanently in the microwave oven, thus the reactor does not have to be moved between steps. Mixing is achieved...

  9. Solid gas reaction phase diagram under high gas pressure

    Ishizaki, K.

    1992-01-01

    This paper reports that to evaluate which are the stable phases under high gas pressure conditions, a solid-gas reaction phase diagram under high gas pressure (HIP phase diagram) has been proposed by the author. The variables of the diagram are temperature, reactant gas partial pressure and total gas pressure. Up to the present time the diagrams have been constructed using isobaric conditions. In this work, the stable phases for a real HIP process were evaluated assuming an isochoric condition. To understand the effect of the total gas pressure on stability is of primary importance. Two possibilities were considered and evaluated, those are: the total gas pressure acts as an independent variable, or it only affects the fugacity values. The results of this work indicate that the total gas pressure acts as an independent variable, and in turn also affects the fugacity values

  10. Indigenous microbial capability in solid manure residues to start-up solid-phase anaerobic digesters.

    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.

  11. Binding of properdin to solid-phase immune complexes

    Junker, A; Baatrup, G; Svehag, S E

    1998-01-01

    The capacity of serum to support deposition of C3, properdin and factor B was studied by enzyme-linked immunosorbent assay using solid-phase immune complexes (IC) for activation of complement. Deposition of C3 and properdin occurred in fairly dilute normal human serum (NHS), but factor B uptake...... fixed to IC was the principal ligand for properdin in the assay. The findings could have biological implications relating to complement-mediated modification of immune complexes in disease....

  12. Solid-phase reductive amination for glycomic analysis.

    Jiang, Kuan; Zhu, He; Xiao, Cong; Liu, Ding; Edmunds, Garrett; Wen, Liuqing; Ma, Cheng; Li, Jing; Wang, Peng George

    2017-04-15

    Reductive amination is an indispensable method for glycomic analysis, as it tremendously facilitates glycan characterization and quantification by coupling functional tags at the reducing ends of glycans. However, traditional in-solution derivatization based approach for the preparation of reductively aminated glycans is quite tedious and time-consuming. Here, a simpler and more efficient strategy termed solid-phase reductive amination was investigated. The general concept underlying this new approach is to streamline glycan extraction, derivatization, and purification on non-porous graphitized carbon sorbents. Neutral and sialylated standard glycans were utilized to test the feasibility of the solid-phase method. As results, almost complete labeling of those glycans with four common labels of aniline, 2-aminobenzamide (2-AB), 2-aminobenzoic acid (2-AA) and 2-amino-N-(2-aminoethyl)-benzamide (AEAB) was obtained, and negligible desialylation occurred during sample preparation. The labeled glycans derived from glycoproteins showed excellent reproducibility in high performance liquid chromatography (HPLC) and matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) analysis. Direct comparisons based on fluorescent absorbance and relative quantification using isotopic labeling demonstrated that the solid-phase strategy enabled 20-30% increase in sample recovery. In short, the solid-phase strategy is simple, reproducible, efficient, and sensitive for glycan analysis. This method was also successfully applied for N-glycan profiling of HEK 293 cells with MALDI-TOF MS, showing its attractive application in the high-throughput analysis of mammalian glycome. Published by Elsevier B.V.

  13. Chromatography, solid-phase extraction, and capillary electrochromatography with MIPs.

    Tóth, Blanka; Horvai, George

    2012-01-01

    Most analytical applications of molecularly imprinted polymers are based on their selective adsorption properties towards the template or its analogs. In chromatography, solid phase extraction and electrochromatography this adsorption is a dynamic process. The dynamic process combined with the nonlinear adsorption isotherm of the polymers and other factors results in complications which have limited the success of imprinted polymers. This chapter explains these problems and shows many examples of successful applications overcoming or avoiding the problems.

  14. Characterization of Bitumen Micro-Mechanical Behaviors Using AFM, Phase Dynamics Theory and MD Simulation

    Yue Hou

    2017-02-01

    Full Text Available Fundamental understanding of micro-mechanical behaviors in bitumen, including phase separation, micro-friction, micro-abrasion, etc., can help the pavement engineers better understand the bitumen mechanical performances at macroscale. Recent researches show that the microstructure evolution in bitumen will directly affect its surface structure and micro-mechanical performance. In this study, the bitumen microstructure and micro-mechanical behaviors are studied using Atomic Force Microscopy (AFM experiments, Phase Dynamics Theory and Molecular Dynamics (MD Simulation. The AFM experiment results show that different phase-structure will occur at the surface of the bitumen samples under certain thermodynamic conditions at microscale. The phenomenon can be explained using the phase dynamics theory, where the effects of stability parameter and temperature on bitumen microstructure and micro-mechanical behavior are studied combined with MD Simulation. Simulation results show that the saturates phase, in contrast to the naphthene aromatics phase, plays a major role in bitumen micro-mechanical behavior. A high stress zone occurs at the interface between the saturates phase and the naphthene aromatics phase, which may form discontinuities that further affect the bitumen frictional performance.

  15. Characterization of Bitumen Micro-Mechanical Behaviors Using AFM, Phase Dynamics Theory and MD Simulation.

    Hou, Yue; Wang, Linbing; Wang, Dawei; Guo, Meng; Liu, Pengfei; Yu, Jianxin

    2017-02-21

    Fundamental understanding of micro-mechanical behaviors in bitumen, including phase separation, micro-friction, micro-abrasion, etc., can help the pavement engineers better understand the bitumen mechanical performances at macroscale. Recent researches show that the microstructure evolution in bitumen will directly affect its surface structure and micro-mechanical performance. In this study, the bitumen microstructure and micro-mechanical behaviors are studied using Atomic Force Microscopy (AFM) experiments, Phase Dynamics Theory and Molecular Dynamics (MD) Simulation. The AFM experiment results show that different phase-structure will occur at the surface of the bitumen samples under certain thermodynamic conditions at microscale. The phenomenon can be explained using the phase dynamics theory, where the effects of stability parameter and temperature on bitumen microstructure and micro-mechanical behavior are studied combined with MD Simulation. Simulation results show that the saturates phase, in contrast to the naphthene aromatics phase, plays a major role in bitumen micro-mechanical behavior. A high stress zone occurs at the interface between the saturates phase and the naphthene aromatics phase, which may form discontinuities that further affect the bitumen frictional performance.

  16. Micro tube heat exchangers for Space, Phase I

    National Aeronautics and Space Administration — Mezzo fabricates micro tube heat exchangers for a variety of applications, including aerospace, automotive racing, Department of Defense ground vehicles, economizers...

  17. Simulation For Synchronization Of A Micro-Grid With Three-Phase Systems

    Mohammad Jafari Far

    2015-01-01

    Abstract today due to the high reliability of the micro-grids they have developed significantly. They have two states of operation the island state and connection to the main grid. Under certain circumstances the micro-grid is connected to or disconnected from the network. Synchronization of a micro-grid with the network must be done when its voltage is synchronized with the voltage in the main grid. Phase lock loops are responsible to identify the voltage phase of the micro-gird and the main...

  18. Solid phase radioimmunoassays for human C-reactive protein

    Shine, B.; Beer, F.C. de; Pepys, M.B.

    1981-01-01

    Two new, rapid and sensitive radioimmunoassays for human C-reactive protein (CRP) have been established using antiserum coupled to magnetizable cellulose particles, which facilitate phase separation. A single antibody method, using solid phase anti-CRP, provides a sensitivity of 50 μg/l with a 1-h incubation time and intra- and inter-assay coefficients of variation of 10%. A double antibody method, using fluid phase rabbit anti-CRP serum and solid phase sheep anti-rabbit IgG serum, provides a sensitivity of 3 μg/l with an overnight incubation and intra- and inter-assay coefficients of variation of 10%. Among 468 sera from normal adult volunteer blood donors the median CRP concentration was 800 μg/l, interquartile range 340-1700 μg/l and range 70-29,000 μg/l. Ninety percent of samples contained less than 3 mg/l and 99% less than 10 mg/l. Low levels (14-650 μg/l) of CRP were detected both in amniotic fluids and in cerebrospinal fluids. (Auth.)

  19. New Solid Phases for Estimation of Hormones by Radioimmunoassay Technique

    Sheha, R.R.; Ayoub, H.S.M.; Shafik, M.

    2013-01-01

    The efforts in this study were initiated to develop and validate new solid phases for estimation of hormones by radioimmunoassay (RIA). The study argued the successful application of different hydroxy apatites (HAP) as new solid phases for estimation of Alpha fetoprotein (AFP), Thyroid Stimulating hormone (TSH) and Luteinizing hormone (LH) in human serum. Hydroxy apatites have different alkali earth elements were successfully prepared by a well-controlled co-precipitation method with stoichiometric ratio value 1.67. The synthesized barium and calcium hydroxy apatites were characterized using XRD and Ftir and data clarified the preparation of pure structures of both BaHAP and CaHAP with no evidence on presence of other additional phases. The prepared solid phases were applied in various radioimmunoassay systems for separation of bound and free antigens of AFP, TSH and LH hormones. The preparation of radiolabeled tracer for these antigens was carried out using chloramine-T as oxidizing agent. The influence of different parameters on the activation and coupling of the used apatite particles with the polyclonal antibodies was systematically investigated and the optimum conditions were determined. The assay was reproducible, specific and sensitive enough for regular estimation of the studied hormones. The intra-and inter-assay variation were satisfactory and also the recovery and dilution tests indicated an accurate calibration. The reliability of these apatite particles had been validated by comparing the results that obtained by using commercial kits. The results finally authenticates that hydroxyapatite particles would have a great potential to address the emerging challenge of accurate quantitation in laboratory medical application

  20. Thermodynamic phase behavior of API/polymer solid dispersions.

    Prudic, Anke; Ji, Yuanhui; Sadowski, Gabriele

    2014-07-07

    To improve the bioavailability of poorly soluble active pharmaceutical ingredients (APIs), these materials are often integrated into a polymer matrix that acts as a carrier. The resulting mixture is called a solid dispersion. In this work, the phase behaviors of solid dispersions were investigated as a function of the API as well as of the type and molecular weight of the carrier polymer. Specifically, the solubility of artemisinin and indomethacin was measured in different poly(ethylene glycol)s (PEG 400, PEG 6000, and PEG 35000). The measured solubility data and the solubility of sulfonamides in poly(vinylpyrrolidone) (PVP) K10 and PEG 35000 were modeled using the perturbed-chain statistical associating fluid theory (PC-SAFT). The results show that PC-SAFT predictions are in a good accordance with the experimental data, and PC-SAFT can be used to predict the whole phase diagram of an API/polymer solid dispersion as a function of the kind of API and polymer and of the polymer's molecular weight. This remarkably simplifies the screening process for suitable API/polymer combinations.

  1. Micro/Nano Fabricated Solid-State Thermoelectric Generator Devices for Integrated High Voltage Power Sources

    Fleurial, J.-P.; Ryan, M. A.; Snyder, G. J.; Huang, C.-K.; Whitacre, J. F.; Patel, J.; Lim, J.; Borshchevsky, A.

    2002-01-01

    Deep space missions have a strong need for compact, high power density, reliable and long life electrical power generation and storage under extreme temperature conditions. Except for electrochemical batteries and solar cells, there are currently no available miniaturized power sources. Conventional power generators devices become inefficient in extreme environments (such as encountered in Mars, Venus or outer planet missions) and rechargeable energy storage devices can only be operated in a narrow temperature range thereby limiting mission duration. The planned development of much smaller spacecrafts incorporating a variety of micro/nanodevices and miniature vehicles will require novel, reliable power technologies. It is also expected that such micro power sources could have a wide range of terrestrial applications, in particular when the limited lifetime and environmental limitations of batteries are key factors. Advanced solid-state thermoelectric combined with radioisotope or waste heat sources and low profile energy storage devices are ideally suited for these applications. The Jet Propulsion Laboratory has been actively pursuing the development of thermoelectric micro/nanodevices that can be fabricated using a combination of electrochemical deposition and integrated circuit processing techniques. Some of the technical challenges associated with these micro/nanodevice concepts, their expected level of performance and experimental fabrication and testing results to date are presented and discussed.

  2. All-solid-state micro-supercapacitors based on inkjet printed graphene electrodes

    Li, Jiantong; Mishukova, Viktoriia; Östling, Mikael

    2016-09-01

    The all-solid-state graphene-based in-plane micro-supercapacitors are fabricated simply through reliable inkjet printing of pristine graphene in interdigitated structure on silicon wafers to serve as both electrodes and current collectors, and a following drop casting of polymer electrolytes (polyvinyl alcohol/H3PO4). Benefiting from the printing processing, an attractive porous electrode microstructure with a large number of vertically orientated graphene flakes is observed. The devices exhibit commendable areal capacitance over 0.1 mF/cm2 and a long cycle life of over 1000 times. The simple and scalable fabrication technique for efficient micro-supercapacitors is promising for on-chip energy storage applications in emerging electronics.

  3. Template assisted solid state electrochemical growth of silver micro- and nanowires

    Peppler, Klaus; Janek, Juergen

    2007-01-01

    We report on a template based solid state electrochemical method for fabricating silver nanowires with predefined diameter, depending only on the pore diameter of the template. As templates we used porous silicon with pore diameters in the μm range and porous alumina with pore diameters in the nm range. The template pores were filled with silver sulfide (a mixed silver cation and electronic conductor) by direct chemical reaction of silver and sulfur. The filled template was then placed between a silver foil as anode (bottom side) and a microelectrode (top side) as cathode. An array of small cylindrical transference cells with diameters in the range of either micro- or nanometers was thus obtained. By applying a cathodic voltage to the microelectrode silver in the form of either micro- or nanowires was deposited at about 150 deg. C. The growth rate is controllable by the electric current

  4. Double antibody solid-phase radioimmunoassay for staphylococcal enterotoxin A

    Lindroth, S.; Niskanen, A.

    1977-01-01

    A double antibody solid-phase (DASP) radioimmunoassay for staphylococcal enterotoxin A is described. In the assay the antigen-antibody complex is precipitated by anti-rabbit serum which is adsorbed onto a solid carrier (cellulose). The method is sensitive to 200 pg of enterotoxin. It was possible to detect a little as 2-5 ng of enterotoxin A/ml food extract from minced meat and sausage. Enterotoxins B and C were not found to inhibit the uptake of labled enterotoxin A at a level which might distort the results of the enterotoxin A assay. The DASP technique is sensitive, rapid, and easy to perform and thus compares favorably with other radioimmunoassays for enterotoxin. (orig.) [de

  5. Novel solidsolid phase change material based on polyethylene glycol and cellulose used for temperature stabilisation

    Wojda Marta

    2014-01-01

    Full Text Available Thermal management is one of crucial issues in the development of modern electronic devices. In the recent years interest in phase change materials (PCMs as alternative cooling possibility has increased significantly. Preliminary results concerning the research into possibility of the use of solid-solid phase change materials (S-S PCMs for stabilisation temperature of electronic devices has been presented in the paper. Novel solid-solid phase change material based on polyethylene glycol and cellulose has been synthesized. Attempt to improve its thermal conductivity has been taken. Material has been synthesized for the purpose of stabilisation of temperature of electronic devices.

  6. Solid phase crystallisation of HfO2 thin films

    Modreanu, M.; Sancho-Parramon, J.; O'Connell, D.; Justice, J.; Durand, O.; Servet, B.

    2005-01-01

    In this paper, we report on the solid phase crystallisation of carbon-free HfO 2 thin films deposited by plasma ion assisted deposition (PIAD). After deposition, the HfO 2 films were annealed in N 2 ambient for 3 h at 350, 550 and 750 deg. C. Several characterisation techniques including X-ray reflectometry (XRR), X-ray diffraction (XRD), spectroscopic ellipsometry (SE) and atomic force microscopy (AFM) were used for the physical characterisation of as-deposited and annealed HfO 2 . XRD has revealed that the as-deposited HfO 2 film is in an amorphous-like state with only traces of crystalline phase and that the annealed films are in a highly crystalline state. These results are in good agreement with the SE results showing an increase of refractive index by increasing the annealing temperature. XRR results show a significant density gradient over the as-deposited film thickness, which is characteristic of the PIAD method. The AFM measurements show that the HfO 2 layers have a smooth surface even after annealing at 750 deg. C. The present study demonstrates that the solid phase crystallisation of HfO 2 PIAD thin films starts at a temperature as low as 550 deg. C

  7. Micro-Solid Oxide Fuel Cell: A multi-fuel approach for portable applications

    Patil, Tarkeshwar C.; Duttagupta, Siddhartha P.

    2016-01-01

    Highlights: • We report the oxygen ion transport properties at the electrode–electrolyte interface (EEI) of the SOFC for the first time. • This ion transport plays a key role in the overall performance of SOFCs with different fuels. • The GIIB mechanism is also studied for the first time. • GIIB is assumed to be the prime reason for low power density and ion conductivity at the EEI when using hydrocarbon fuels. • Due to its scalability, a fuel cell can serve as a power source for on-chip applications and all portable equipment. - Abstract: The impact of oxygen ion transport at the electrolyte–electrode interface of a micro-solid oxide fuel cell using different fuels is investigated. Model validation is performed to verify the results versus the reported values. Furthermore, as the hydrogen-to-carbon ratio decreases, the diffusivity of the oxygen ion increases. This increase in diffusivity is observed because the number of hydrogen atoms available as the reacting species increases in fuels with lower hydrogen-to-carbon ratios. The oxygen ion conductivity and output power density decrease as the hydrogen-to-carbon ratio of the fuels decreases. The reason behind this impact is the formation of a gas-induced ion barrier at the electrode–electrolyte interface by the CO_2 molecules formed during the reaction at the interface, thus blocking the flow of oxygen ions. As the oxygen ions become blocked, the output current contribution from the reaction also decreases and thereby affects the overall performance of the micro-solid oxide fuel cell. The experimental verification confirms this because of a significant decrease in the output power density. Furthermore, as per the application in portable devices, the appropriate choice of fuel can be chosen so that the micro-solid oxide fuel cell operates at the maximum power density.

  8. Phase nucleation and evolution mechanisms in heterogeneous solids

    Udupa, Anirudh

    Phase nucleation and evolution is a problem of critical importance in many applications. As the length scales are reduced, it becomes increasingly important to consider interfacial and micro-structural effects that can be safely ignored at larger length scales owing to randomness. The theory of phase nucleation has been addressed usually by the classical nucleation theory, which was originally derived for single component fluid systems, after making an assumption of equilibrium. The criterion has not been rigorously derived for solids, which are far from equilibrium due to dissipation by multiple physical drivers. In this thesis, a thermodynamically sound nucleation criterion is derived for systems with multiple interacting physical phenomena and multiple dissipating mechanisms. This is done, using the tools of continuum mechanics, by determining the change in free energy upon the introduction of a new nucleus into the system. The developed theory is demonstrated to be a generalization of the classical nucleation theory (CNT). The developed theory is then applied to the problem of electromigration driven void nucleation, a serious reliability concern for the microelectronics industry. The void grows and eventually severs the line making the chip nonfunctional. There are two classes of theories at present in the electromigration literature to address the problem of void nucleation, the vacancy supersaturation theory and the entropic dissipation theory, both of which are empirical and based on intuition developed from experimental observations. When the developed theory was applied to the problem of electromigration, it was found to be consistent with the vacancy supersaturation theory, but provided the correct energetic quantity, the chemical potential, which has contribution from both the vacancy concentration as well as the hydrostatic stress. An experiment, consisting of electromigration tests on serpentine lines, was developed to validate the developed

  9. Comparison of Experimental and Numerical Two-Phase Flows in a Porous Micro-Model

    Dustin Crandall

    2009-12-01

    Full Text Available Characterizing two-phase flow in porous media is important to provide estimates of sweep efficiency in enhanced oil recovery and storage estimates in potential geological CO2 sequestration repositories. To further the current understanding of two-phase flow in porous media a micro-model of interconnected channels was designed and fabricated using stereolithography to experimentally study gas-liquid flows. This flowcell was created with a wide variability of throat dimensions to represent naturally occurring porous media. Low flow rate experiments of immiscible two-phase drainage were performed within this cell. Additionally, a computational model for analyzing two-phase flows in the same flowcell was developed and used to simulate conditions not possible with our laboratory settings. The computational model was first tested for the identical conditions used in the experimental studies, and was shown to be in good agreement with the experimentally determined fractal dimension of the invading gas structure, time until breakthrough, and fluid saturation. The numerical model was then used to study two-phase air-water flows in flowcells with the same geometry and different gas-liquid-solid contact angles. The percent saturation of air and the motion of the fluids through the cell were found to vary with changes in these parameters. Finally, to simulate flows expected during geologic carbon sequestration, the fluid properties and interface conditions were set to model the flow of CO2 into a brine-saturated porous medium at representative subsurface conditions. The CO2 flows were shown to have larger gas saturations than the previous air into water studies. Thus the accuracy of the computational model was supported by the flowcell experiments, and the computational model extended the laboratory results to conditions not possible with the apparatus used in the experiments.

  10. Solid-phase vibrational redox reactions in coordinated oxides

    Kostikova, G.P.; Korol'kov, D.V.; Kostikov, Yu.P.

    1996-01-01

    The properties of multicomponent oxides (YBa 2 Cu 3 O 7-x , etc.), incorporating different valency forms of each of two (or more) different elements have been compared with the properties of the known chemical systems, where vibrational (periodic) redox-reactions are realized a fortiori. The essence of the new theoretical concept suggested consists in the following: high-T c superconductivity of the complex oxides and similar compounds originates from vibrational redox reaction proceeding in solid phase and involving different valency atoms of every element

  11. Automated Solid-Phase Radiofluorination Using Polymer-Supported Phosphazenes

    Mathiessen, Bente; Zhuravlev, Fedor

    2013-01-01

    of [18F]FDG. The combination of compact form factor, simplicity of [18F]F− recovery and processing, and column reusability can make solid phase radiofluorination an attractive radiochemistry platform for the emerging dose-on-demand instruments for bedside production of PET radiotracers.......The polymer supported phosphazene bases PS-P2tBu and the novel PS-P2PEG allowed for efficient extraction of [18F]F− from proton irradiated [18O]H2O and subsequent radiofluorination of a broad range of substrates directly on the resin. The highest radiochemical yields were obtained with aliphatic...

  12. Sensitive and fast mutation detection by solid phase chemical cleavage

    Hansen, Lise Lotte; Justesen, Just; Kruse, Torben A

    1996-01-01

    We have developed a solid phase chemical cleavage method (SpCCM) for screening large DNA fragments for mutations. All reactions can be carried out in microtiterwells from the first amplification of the patient (or test) DNA through the search for mutations. The reaction time is significantly...... reduced compared to the conventional chemical cleavage method (CCM), and even by using a uniformly labelled probe, the exact position and nature of the mutation can be revealed. The SpCCM is suitable for automatization using a workstation to carry out the reactions and a fluorescent detection-based DNA...

  13. Micro-Channel Embedded Pulsating Heat Pipes, Phase I

    National Aeronautics and Space Administration — As the need for thermal control technology becomes more demanding Micro-Channel Embedded Pulsating Heat Pipes (ME-PHPs) represents a sophisticated and enabling...

  14. Prediction of transport phenomena in near and far field: interaction solid phase/fluid phase

    Mingarro, E.

    1995-01-01

    The prediction of transport phenomena in near and far field is presented in the present report. The study begins with the analysis of solid phases stability: solubility of storage waste: UO 2 and solubility of radionuclides the redox and sorption-desorption conditions are the last aspects studied to predict the transport phenomena

  15. Insights into metals in individual fine particles from municipal solid waste using synchrotron radiation-based micro-analytical techniques

    Yumin Zhu; Hua Zhang; Liming Shao; Pinjing He

    2015-01-01

    Excessive inter-contamination with heavy metals hampers the application of biological treatment products derived from mixed or mechanically-sorted municipal solid waste (MSW).In this study,we investigated fine particles of <2 mm,which are small fractions in MSW but constitute a significant component of the total heavy metal content,using bulk detection techniques.A total of 17 individual fine particles were evaluated using synchrotron radiation-based micro-X-ray fluorescence and micro-X-ray diffraction.We also discussed the association,speciation and source apportionment of heavy metals.Metals were found to exist in a diffuse distribution with heterogeneous intensities and intense hot-spots of <10 μm within the fine particles.Zn-Cu,Pb-Fe and Fe-Mn-Cr had significant correlations in terms of spatial distribution.The overlapped enrichment,spatial association,and the mineral phases of metals revealed the potential sources of fine particles from size-reduced waste fractions (such as scraps of organic wastes or ceramics) or from the importation of other particles.The diverse sources of heavy metal pollutants within the fine particles suggested that separate collection and treatment of the biodegradable waste fraction (such as food waste) is a preferable means of facilitating the beneficial utilization of the stabilized products.

  16. Gold catalyzed nickel disilicide formation: a new solid-liquid-solid phase growth mechanism.

    Tang, Wei; Picraux, S Tom; Huang, Jian Yu; Liu, Xiaohua; Tu, K N; Dayeh, Shadi A

    2013-01-01

    The vapor-liquid-solid (VLS) mechanism is the predominate growth mechanism for semiconductor nanowires (NWs). We report here a new solid-liquid-solid (SLS) growth mechanism of a silicide phase in Si NWs using in situ transmission electron microcopy (TEM). The new SLS mechanism is analogous to the VLS one in relying on a liquid-mediating growth seed, but it is fundamentally different in terms of nucleation and mass transport. In SLS growth of Ni disilicide, the Ni atoms are supplied from remote Ni particles by interstitial diffusion through a Si NW to the pre-existing Au-Si liquid alloy drop at the tip of the NW. Upon supersaturation of both Ni and Si in Au, an octahedral nucleus of Ni disilicide (NiSi2) forms at the center of the Au liquid alloy, which thereafter sweeps through the Si NW and transforms Si into NiSi2. The dissolution of Si by the Au alloy liquid mediating layer proceeds with contact angle oscillation at the triple point where Si, oxide of Si, and the Au alloy meet, whereas NiSi2 is grown from the liquid mediating layer in an atomic stepwise manner. By using in situ quenching experiments, we are able to measure the solubility of Ni and Si in the Au-Ni-Si ternary alloy. The Au-catalyzed mechanism can lower the formation temperature of NiSi2 by 100 °C compared with an all solid state reaction.

  17. Powder metallurgy: Solid and liquid phase sintering of copper

    Sheldon, Rex; Weiser, Martin W.

    1993-01-01

    Basic powder metallurgy (P/M) principles and techniques are presented in this laboratory experiment. A copper based system is used since it is relatively easy to work with and is commercially important. In addition to standard solid state sintering, small quantities of low melting metals such as tin, zinc, lead, and aluminum can be added to demonstrate liquid phase sintering and alloy formation. The Taguchi Method of experimental design was used to study the effect of particle size, pressing force, sintering temperature, and sintering time. These parameters can be easily changed to incorporate liquid phase sintering effects and some guidelines for such substitutions are presented. The experiment is typically carried out over a period of three weeks.

  18. Solid phase 125I labelled radioimmunoassay for spermidine

    Zhao Shimin

    1991-01-01

    Using 125 I labelled monoclonal antibody against spermidine and solid phase antigen spermidine-bovine serum albumin conjugate, the radioimmunoassay for spermidine was developed. The sensitivity of this method was about 8 times higher than that of liquid phase 14 C labelled spermidine radioimmunoassay, reaching detection limit of 10 ng/ml (0.5 ng/tube). The working range of standard curve was 0-10 5 ng/ml. The new method was suitable for spermidine measurements in saliva, stomach fluid, and cerebrospinal fluid. The coefficients of variation (CV) of within and between-assay were 4% and 13%, respectively. Preliminary clinical measurements showed that the spermidine levels in saliva of cancer patients and in cerebrospinal fluid of leukemia patients were significantly elevated

  19. Investigation into mixing capability and solid dispersion preparation using the DSM Xplore Pharma Micro Extruder.

    Sakai, Toshiro; Thommes, Markus

    2014-02-01

    The goal of this investigation was to qualify the DSM Xplore Pharma Micro Extruder as a formulation screening tool for early-stage hot-melt extrusion. Dispersive and distributive mixing was investigated using soluplus, copovidone or basic butylated methacrylate copolymer with sodium chloride (NaCl) in a batch size of 5 g. Eleven types of solid dispersions were prepared using various drugs and carriers in batches of 5 g in accordance with the literature. The dispersive mixing was a function of screw speed and recirculation time and the particle size was remarkably reduced after 1 min of processing, regardless of the polymers. An inverse relationship between the particle size and specific mechanical energy (SME) was also found. The SME values were higher than those in large-scale extruders. After 1 min recirculation at 200 rpm, the uniformity of NaCl content met the criteria of the European Pharmacopoeia, indicating that distributive mixing was achieved in this time. For the solid dispersions preparations, the results from different scanning calorimetry, powder X-ray diffractometry and in-vitro dissolution tests confirmed that all solid-dispersion systems were successfully prepared. These findings demonstrated that the extruder is a useful tool to screen solid-dispersion formulations and their material properties on a small scale. © 2013 Royal Pharmaceutical Society.

  20. The Gaseous Phase as a Probe of the Astrophysical Solid Phase Chemistry

    Abou Mrad, Ninette; Duvernay, Fabrice; Isnard, Robin; Chiavassa, Thierry; Danger, Grégoire, E-mail: gregoire.danger@univ-amu.fr [Aix-Marseille Université, PIIM UMR-CNRS 7345, F-13397 Marseille (France)

    2017-09-10

    In support of space missions and spectroscopic observations, laboratory experiments on ice analogs enable a better understanding of organic matter formation and evolution in astrophysical environments. Herein, we report the monitoring of the gaseous phase of processed astrophysical ice analogs to determine if the gaseous phase can elucidate the chemical mechanisms and dominant reaction pathways occurring in the solid ice subjected to vacuum ultra-violet (VUV) irradiation at low temperature and subsequently warmed. Simple (CH{sub 3}OH), binary (H{sub 2}O:CH{sub 3}OH, CH{sub 3}OH:NH{sub 3}), and ternary ice analogs (H{sub 2}O:CH{sub 3}OH:NH{sub 3}) were VUV-processed and warmed. The evolution of volatile organic compounds in the gaseous phase shows a direct link between their relative abundances in the gaseous phase, and the radical and thermal chemistries modifying the initial ice composition. The correlation between the gaseous and solid phases may play a crucial role in deciphering the organic composition of astrophysical objects. As an example, possible solid compositions of the comet Lovejoy are suggested using the abundances of organics in its comae.

  1. The role of solid-solid phase transitions in mantle convection

    Faccenda, Manuele; Dal Zilio, Luca

    2017-01-01

    With changing pressure and temperature conditions, downwelling and upwelling crustal and mantle rocks experience several solid-solid phase transitions that affect the mineral physical properties owing to structural changes in the crystal lattice and to the absorption or release of latent heat. Variations in density, together with phase boundary deflections related to the non-null reaction slope, generate important buoyancy forces that add to those induced by thermal perturbations. These buoyancy forces are proportional to the density contrast between reactant and product phases, their volume fraction, the slope and the sharpness of the reaction, and affect the style of mantle convection depending on the system composition. In a homogeneous pyrolitic mantle there is little tendency for layered convection, with slabs that may stagnate in the transition zone because of the positive buoyancy caused by post-spinel and post-ilmenite reactions, and hot plumes that are accelerated by phase transformations in the 600-800 km depth range. By adding chemical and mineralogical heterogeneities as on Earth, phase transitions introduce bulk rock and volatiles filtering effects that generate a compositional gradient throughout the entire mantle, with levels that are enriched or depleted in one or more of these components. Phase transitions often lead to mechanical softening or hardening that can be related to a different intrinsic mechanical behaviour and volatile solubility of the product phases, the heating or cooling associated with latent heat, and the transient grain size reduction in downwelling cold material. Strong variations in viscosity would enhance layered mantle convection, causing slab stagnation and plume ponding. At low temperatures and relatively dry conditions, reactions are delayed due to the sluggish kinetics, so that non-equilibrium phase aggregates can persist metastably beyond the equilibrium phase boundary. Survival of low-density metastable olivine

  2. Zinc oxide crystal whiskers as a novel sorbent for solid-phase extraction of flavonoids.

    Wang, Licheng; Shangguan, Yangnan; Hou, Xiudan; Jia, Yong; Liu, Shujuan; Sun, Yingxin; Guo, Yong

    2017-08-15

    As a novel solid-phase extraction material, zinc oxide crystal whiskers were used to extract flavonoid compounds and showed good extraction abilities. X-ray diffraction, scanning electron microscopy with energy dispersive X-ray spectroscopy and surface area/pore volume characterized the sorbent. The zinc oxide was packed into a solid-phase extraction micro-column and its extraction ability was evaluated by four model flavonoid compounds. The sample loading and elution parameters were optimized and the zinc oxide based analytical method for flavonoids was established. It showed that the method has wide linearities from 1 to 150μg/L and low limits of detection at 0.25μg/L. The relative standard deviations of a single column repeatability and column to column reproducibility were less than 6.8% and 10.6%. Several real samples were analyzed by the established method and satisfactory results were obtained. The interactions between flavonoids and zinc oxide were calculated and proved to be from the Van der Waals' forces between the 4p and 5d orbitals from zinc atom and the neighboring π orbitals from flavonoid phenyl groups. Moreover, the zinc oxide crystal whiskers showed good stability and could be reused more than 50 times under the operation conditions. This work proves that the zinc oxide crystal whiskers are a good candidate for flavonoids enrichment. Copyright © 2017. Published by Elsevier B.V.

  3. Radioimmuoassay study of antidigitoxin antibodies in liquid phase and after coupling on a solid phase

    Collignon, A.; German, A.; Scherrmann, J.M.; Bourdon, R.

    1983-01-01

    Antidigitoxin antibodies prepared by immunizing rabbits with a digitoxin-bovine serum albumin conjugate have been studied by radioimmunoassay in the native serum (homogeneous phase antibodies) and after coupling on glass beads (heterogeneous phase antibodies). Homogeneous phase antibodies present a satisfactory titer and affinity constant and react very specifically with digitoxin. Fixation of antibodies on a solid phase induce a loss of their immunoreactivity as it is showed by modification of the inhibition curves, by a greater sensitivity to the chemical structure of the tracer and by a decrease of the affinity constant. Reactionnal kinetic and sensitivity to the incubation temperature are not modified. Heterogeneous phase antibodies present a greater stability. Both antibodies types can be used for a digitoxin radioimmunoassay [fr

  4. Solid state phase change materials for thermal energy storage in passive solar heated buildings

    Benson, D. K.; Christensen, C.

    1983-11-01

    A set of solid state phase change materials was evaluated for possible use in passive solar thermal energy storage systems. The most promising materials are organic solid solutions of pentaerythritol, pentaglycerine and neopentyl glycol. Solid solution mixtures of these compounds can be tailored so that they exhibit solid-to-solid phase transformations at any desired temperature within the range from less than 25 deg to 188 deg. Thermophysical properties such as thermal conductivity, density and volumetric expansion were measured. Computer simulations were used to predict the performance of various Trombe wall designs incorporating solid state phase change materials. Optimum performance was found to be sensitive to the choice of phase change temperatures and to the thermal conductivity of the phase change material. A molecular mechanism of the solid state phase transition is proposed and supported by infrared spectroscopic evidence.

  5. Bridging micro to macroscale fracture properties in highly heterogeneous brittle solids: weak pinning versus fingering

    Vasoya, Manish; Lazarus, Véronique; Ponson, Laurent

    2016-10-01

    The effect of strong toughness heterogeneities on the macroscopic failure properties of brittle solids is investigated in the context of planar crack propagation. The basic mechanism at play is that the crack is locally slowed down or even trapped when encountering tougher material. The induced front deformation results in a selection of local toughness values that reflect at larger scale on the material resistance. To unravel this complexity and bridge micro to macroscale in failure of strongly heterogeneous media, we propose a homogenization procedure based on the introduction of two complementary macroscopic properties: An apparent toughness defined from the loading required to make the crack propagate and an effective fracture energy defined from the rate of energy released by unit area of crack advance. The relationship between these homogenized properties and the features of the local toughness map is computed using an iterative perturbation method. This approach is applied to a circular crack pinned by a periodic array of obstacles invariant in the radial direction, which gives rise to two distinct propagation regimes: A weak pinning regime where the crack maintains a stationary shape after reaching an equilibrium position and a fingering regime characterized by the continuous growth of localized regions of the fronts while the other parts remain trapped. Our approach successfully bridges micro to macroscopic failure properties in both cases and illustrates how small scale heterogeneities can drastically affect the overall failure response of brittle solids. On a broader perspective, we believe that our approach can be used as a powerful tool for the rational design of heterogeneous brittle solids and interfaces with tailored failure properties.

  6. Solid-solid synthesis and structural phase transition process of SmF3

    Yan, Qi-Cao; Guo, Xing-Min

    2018-04-01

    Mazes of contradictory conclusions have been obtained by previous researches about structural phase transition process of SmF3. In this paper, the single crystals of SmF3 (hexagonal and orthorhombic) were prepared by solid-solid synthesis, which have shown gradual changes in crystal growth modes with the increase temperature and holding time. Furthermore, we propose the phase transition process of in SmF3. Hexagonal symmetry of SmF3 (space group Pnma) was prepared firstly by heating Sm2O3 and NH4HF2 over 40 min at 270 °C. And then orthorhombic symmetry of SmF3 (space group P63mc) was obtained by heating hexagonal symmetry over 10 h at 650 °C. The reaction of SmF3 (hexagonal) = SmF3 (orthorhombic) is extremely sluggish at a low temperature (less than 650 °C), which was seen as a Mixed Grown Region.

  7. Highly flexible, all solid-state micro-supercapacitors from vertically aligned carbon nanotubes.

    Hsia, Ben; Marschewski, Julian; Wang, Shuang; In, Jung Bin; Carraro, Carlo; Poulikakos, Dimos; Grigoropoulos, Costas P; Maboudian, Roya

    2014-02-07

    We report a highly flexible planar micro-supercapacitor with interdigitated finger electrodes of vertically aligned carbon nanotubes (VACNTs). The planar electrode structures are patterned on a thin polycarbonate substrate with a facile, maskless laser-assisted dry transfer method. Sputtered Ni is used to reduce the in-plane resistance of the VACNT electrodes. An ionogel, an ionic liquid in a semi-solid matrix, is used as an electrolyte to form a fully solid-state device. We measure a specific capacitance of 430 μF cm(-2) for a scan rate of 0.1 V s(-1) and achieve rectangular cyclic voltammograms at high scan rates of up to 100 V s(-1). Minimal change in capacitance is observed under bending. Mechanical fatigue tests with more than 1000 cycles confirm the high flexibility and durability of the novel material combination chosen for this device. Our results indicate that this scalable and facile fabrication technique shows promise for application in integrated energy storage for all solid-state flexible microdevices.

  8. Simultaneous thermal and optical imaging of two-phase flow in a micro-model.

    Karadimitriou, N K; Nuske, P; Kleingeld, P J; Hassanizadeh, S M; Helmig, R

    2014-07-21

    In the study of non-equilibrium heat transfer in multiphase flow in porous media, parameters and constitutive relations, like heat transfer coefficients between phases, are unknown. In order to study the temperature development of a relatively hot invading immiscible non-wetting fluid and, ultimately, approximate heat transfer coefficients, a transparent micro-model is used as an artificial porous medium. In the last few decades, micro-models have become popular experimental tools for two-phase flow studies. In this work, the design of an innovative, elongated, PDMS (polydimethylsiloxane) micro-model with dimensions of 14.4 × 39 mm(2) and a constant depth of 100 microns is described. A novel setup for simultaneous thermal and optical imaging of flow through the micro-model is presented. This is the first time that a closed flow cell like a micro-model is used in simultaneous thermal and optical flow imaging. The micro-model is visualized by a novel setup that allowed us to monitor and record the distribution of fluids throughout the length of the micro-model continuously and also record the thermal signature of the fluids. Dynamic drainage and imbibition experiments were conducted in order to obtain information about the heat exchange between the phases. In this paper the setup as well as analysis and qualitative results are presented.

  9. Solid-Phase Synthesis of RNA Analogs Containing Phosphorodithioate Linkages.

    Yang, Xianbin

    2017-09-18

    The oligoribonucleotide phosphorodithioate (PS2-RNA) modification uses two sulfur atoms to replace two non-bridging oxygen atoms at an internucleotide phosphorodiester backbone linkage. Like a natural phosphodiester RNA backbone linkage, a PS2-modified backbone linkage is achiral at phosphorus. PS2-RNAs are highly stable to nucleases and several in vitro assays have demonstrated their biological activity. For example, PS2-RNAs silenced mRNA in vitro and bound to protein targets in the form of PS2-aptamers (thioaptamers). Thus, the interest in and promise of PS2-RNAs has drawn attention to synthesizing, isolating, and characterizing these compounds. RNA-thiophosphoramidite monomers are commercially available from AM Biotechnologies and this unit describes an effective methodology for solid-phase synthesis, deprotection, and purification of RNAs having PS2 internucleotide linkages. © 2017 by John Wiley & Sons, Inc. Copyright © 2017 John Wiley & Sons, Inc.

  10. Characterization of solid residues from coal liquefaction processes. Phase I

    Potter, J.; McDougall, W.M.; Kybett, B.D.; Neufeld, C.

    1981-01-01

    Various coal liquefaction and beneficiation processes are being investigated by independent research groups sponsored by the Canadian Federal Government. These processes include the co-processing of heavy oils and bitumen with coal, oxygen removal and hydrogenation of coal and supercritical gas extraction of coal. The end products, gaseous and liquid fuels and insoluble organic residues, vary with the experimental conditions. The physical properties and origin of the insoluble residue may influence such factors as degree of conversion, efficiency of the process, and ultimately, gaseous and liquid yields. One of the most suitable methods of assessing the nature of the insoluble residues is the use of petrography. This report deals with petrographic assessment of the coals and residues from various coal conversion processes; attempts were made to characterize the solid phases in the residues; to assess them in a quantitative manner and where possible; to correlate the results with experimental data; and to assess their effects on conversion. (30 refs.)

  11. Use of solid-phase salt catalysts in furfural preparation

    Morozov, E.F.; Shkut, V.M.; Kebich, M.S.; Kuznetsova, T.A.

    1981-01-01

    The manufacture of furfural (I) from tanning waste, birch sawdust, or corncobs at 220-230 degrees in the presence of 2.0-3.0% double superphosphate, ammophos, (NH/sub 4/)/sub 2/SO/sub 4/, NH/sub 4/NO/sub 3/, or NH/sub 4/Cl was evaluated. Most of I is formed within 40 minutes in the presence of NH4NO3 or NH4Cl, and within 55 minutes in the presence of double superphosphate. The highest yield of I was obtained in the presence of NH4NO3 and/or NH4Cl. The solid-phase catalyst caused a little degradation of lignocellulose.

  12. Municipal solid waste development phases: Evidence from EU27.

    Vujić, Goran; Gonzalez-Roof, Alvaro; Stanisavljević, Nemanja; Ragossnig, Arne M

    2015-12-01

    Many countries in the European Union (EU) have very developed waste management systems. Some of its members have managed to reduce their landfilled waste to values close to zero during the last decade. Thus, European Union legislation is very stringent regarding waste management for their members and candidate countries, too. This raises the following questions: Is it possible for developing and developed countries to comply with the European Union waste legislation, and under what conditions? How did waste management develop in relation to the economic development in the countries of the European Union? The correlation between waste management practices and economic development was analysed for 27 of the European Union Member States for the time period between 1995 and 2007. In addition, a regression analysis was performed to estimate landfilling of waste in relation to gross domestic product for every country. The results showed a strong correlation between the waste management variables and the gross domestic product of the EU27 members. The definition of the municipal solid waste management development phases followed a closer analysis of the relation between gross domestic product and landfilled waste. The municipal solid waste management phases are characterised by high landfilling rates at low gross domestic product levels, and landfilling rates near zero at high gross domestic product levels. Hence the results emphasize the importance of wider understanding of what is required for developing countries to comply with the European Union initiatives, and highlight the importance of allowing developing countries to make their own paths of waste management development. © The Author(s) 2015.

  13. Hybrid Solid Oxide Fuel Cell and Thermoelectric Generator for Maximum Power Output in Micro-CHP Systems

    Rosendahl, Lasse; Mortensen, Paw Vestergård; Enkeshafi, Ali A.

    2011-01-01

    and market segments which are not yet quantified. This paper quantifies a micro-CHP system based on a solid oxide fuel cell (SOFC) and a high-performance TE generator. Based on a 3 kW fuel input, the hybrid SOFC implementation boosts electrical output from 945 W to 1085 W, with 1794 W available for heating...... the electricity production in micro-CHP systems by more than 15%, corresponding to system electrical efficiency increases of some 4 to 5 percentage points. This will make fuel cell-based micro-CHP systems very competitive and profitable and will also open opportunities in a number of other potential business...

  14. Amino-modified diamond as a durable stationary phase for solid-phase extraction.

    Saini, Gaurav; Yang, Li; Lee, Milton L; Dadson, Andrew; Vail, Michael A; Linford, Matthew R

    2008-08-15

    We report the formation of a highly stable amino stationary phase on diamond and demonstrate its use in solid-phase extraction (SPE). This process consists of spontaneous and self-limiting adsorption of polyallylamine (PAAm) from aqueous solution onto oxidized diamond. Thermal curing under reduced pressure or chemical cross-linking with a diepoxide was shown to fix the polymer to the particles. The resulting adsorbents are stable under even extreme pH conditions (from at least pH 0-14) and significantly more stable than a commercially available amino SPE adsorbent. Coated diamond particles were characterized by X-ray photoelectron spectroscopy (XPS) and diffuse reflectance Fourier transform-infrared spectroscopy (DRIFT). Model silicon surfaces were characterized by spectroscopic ellipsometry and wetting. Solid-phase extraction was demonstrated using cholesterol, hexadecanedioic acid, and palmitoyloleoylphosphatidylcholine as analytes, and these results were compared to those obtained with commercially available materials. Breakthrough curves indicate that, as expected, porous diamond particles have higher analyte capacity than nonporous solid particles.

  15. Comparative solution and solid-phase glycosylations toward a disaccharide library

    Agoston, K.; Kröger, Lars; Agoston, Agnes

    2009-01-01

    A comparative study on solution-phase and solid-phase oligosaccharide synthesis was performed. A 16-member library containing all regioisomers of Glc-Glc, Glc-Gal, Gal-Glc, and Gal-Gal disaccharides was synthesized both in solution and on solid phase. The various reaction conditions for different...

  16. Application of solid-phase microextraction in analytical toxicology.

    Pragst, Fritz

    2007-08-01

    Solid-phase microextraction (SPME) is a miniaturized and solvent-free sample preparation technique for chromatographic-spectrometric analysis by which the analytes are extracted from a gaseous or liquid sample by absorption in, or adsorption on, a thin polymer coating fixed to the solid surface of a fiber, inside an injection needle or inside a capillary. In this paper, the present state of practical performance and of applications of SPME to the analysis of blood, urine, oral fluid and hair in clinical and forensic toxicology is reviewed. The commercial coatings for fibers or needles have not essentially changed for many years, but there are interesting laboratory developments, such as conductive polypyrrole coatings for electrochemically controlled SPME of anions or cations and coatings with restricted-access properties for direct extraction from whole blood or immunoaffinity SPME. In-tube SPME uses segments of commercial gas chromatography (GC) capillaries for highly efficient extraction by repeated aspiration-ejection cycles of the liquid sample. It can be easily automated in combination with liquid chromatography but, as it is very sensitive to capillary plugging, it requires completely homogeneous liquid samples. In contrast, fiber-based SPME has not yet been performed automatically in combination with high-performance liquid chromatography. The headspace extractions on fibers or needles (solid-phase dynamic extraction) combined with GC methods are the most advantageous versions of SPME because of very pure extracts and the availability of automatic samplers. Surprisingly, substances with quite high boiling points, such as tricyclic antidepressants or phenothiazines, can be measured by headspace SPME from aqueous samples. The applicability and sensitivity of SPME was essentially extended by in-sample or on-fiber derivatization. The different modes of SPME were applied to analysis of solvents and inhalation narcotics, amphetamines, cocaine and metabolites

  17. Hydrocarbon fuel processing of micro solid oxide fuel cell systems[Dissertation 17455

    Stutz, M. J.

    2007-07-01

    The scope of this thesis is the numerical and experimental investigation of the fuel processing of a micro solid oxide fuel cell (SOFC) running on hydrocarbon fuel. The goal is to enhance the overall system efficiency by optimization of the reforming process in the steady state and the improvement of the start-up process. Micro SOFC are a potential alternative to the currently used batteries in portable devices. Liquid butane in a cartridge could be the energy source. This dissertation is focused on the fuel processing of the system, namely the reforming and post-combusting processes. The reformer converts the hydrocarbon fuel to a hydrogen rich gas that can be utilized by the SOFC. The post-combustor depletes the toxic and/or explosive gases before leaving the exhaust. Chapter One presents a short introduction to the field of hydrocarbon fuel processing in micro solid oxide fuel cell systems, the next three chapters deal with computational modeling of the transport phenomena inside a micro-reformer, which leads to a better understanding of the chemistry and the physics therein, hence progress in the design and operation parameters. The experimental part (i.e. Chapter Five) of this thesis focuses on the feasibility of a novel hybrid start-up method of a fuel cell system that employs existing components as an additional heat source. In Chapter Two the effect of wall heat conduction on the syngas (hydrogen and carbon monoxide) production of a micro-reformer, representing micro-fabricated channels or monoliths, is investigated. Methane is used as a model hydrocarbon fuel since its heterogeneous reaction path on rhodium is known and validated. The simulations demonstrate that the axial wall conduction strongly influences the performance of the micro-reformer and should not be neglected without a careful a priori investigation of its impact. Methane conversion and hydrogen yield are strongly dependent of the wall inner surface temperature, which is influenced by the

  18. Electrode design for direct-methane micro-tubular solid oxide fuel cell (MT-SOFC)

    Rabuni, Mohamad Fairus; Li, Tao; Punmeechao, Puvich; Li, Kang

    2018-04-01

    Herein, a micro-structured electrode design has been developed via a modified phase-inversion method. A thin electrolyte integrated with a highly porous anode scaffold has been fabricated in a single-step process and developed into a complete fuel cell for direct methane (CH4) utilisation. A continuous and well-dispersed layer of copper-ceria (Cu-CeO2) was incorporated inside the micro-channels of the anode scaffold. A complete cell was investigated for direct CH4 utilisation. The well-organised micro-channels and nano-structured Cu-CeO2 anode contributed to an increase in electrochemical reaction sites that promoted charge-transfer as well as facilitating gaseous fuel distribution, resulting in outstanding performances. Excellent electrochemical performances have been achieved in both hydrogen (H2) and CH4 operation. The power density of 0.16 Wcm-2 at 750 °C with dry CH4 as fuel is one of the highest ever reported values for similar anode materials.

  19. Accelerated testing of solid oxide fuel cell stacks for micro combined heat and power application

    Hagen, Anke; Høgh, Jens Valdemar Thorvald; Barfod, Rasmus

    2015-01-01

    State-of-the-art (SoA) solid oxide fuel cell (SOFC) stacks are tested using profiles relevant for use in micro combined heat and power (CHP) units. Such applications are characterised by dynamic load profiles. In order to shorten the needed testing time and to investigate potential acceleration...... of degradation, the profiles are executed faster than required for real applications. Operation with fast load cycling, both using hydrogen and methane/steam as fuels, does not accelerate degradation compared to constant operation, which demonstrates the maturity of SoA stacks and enables transferring knowledge...... effect for long life-times than regular short time changes of operation. In order to address lifetime testing it is suggested to build a testing program consisting of defined modules that represent different application profiles, such as one module at constant conditions, followed by modules at one set...

  20. Solid-phase glycan isolation for glycomics analysis.

    Yang, Shuang; Zhang, Hui

    2012-12-01

    Glycosylation is one of the most significant protein PTMs. The biological activities of proteins are dramatically changed by the glycans associated with them. Thus, structural analysis of the glycans of glycoproteins in complex biological or clinical samples is critical in correlation with the functions of glycans with diseases. Profiling of glycans by HPLC-MS is a commonly used technique in analyzing glycan structures and quantifying their relative abundance in different biological systems. Methods relied on MS require isolation of glycans from negligible salts and other contaminant ions since salts and ions may interfere with the glycans, resulting in poor glycan ionization. To accomplish those objectives, glycan isolation and clean-up methods including SPE, liquid-phase extraction, chromatography, and electrophoresis have been developed. Traditionally, glycans are isolated from proteins or peptides using a combination of hydrophobic and hydrophilic columns: proteins and peptides remain on hydrophobic absorbent while glycans, salts, and other hydrophilic reagents are collected as flowthrough. The glycans in the flowthrough are then purified through graphite-activated carbon column by hydrophilic interaction LC. Yet, the drawback in these affinity-based approaches is nonspecific binding. As a result, chemical methods by hydrazide or oxime have been developed for solid-phase isolation of glycans with high specificity and yield. Combined with high-resolution MS, specific glycan isolation techniques provide tremendous potentials as useful tools for glycomics analysis. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Experimental research of inclined-micro-fin flat tube on single phase convection heat transfer

    Fan Guangming; Sun Zhongning; Wang Meng

    2011-01-01

    The experimental research of heat transfer and flow resistance characteristics of single phase water in four inclined-micro-fin flat tubes with different physical dimensions was conducted. At the same time,suitable criteria were selected to evaluate the efficiency of inclined-micro-fin flat tubes within the experimental scope and the optimal working region was determined. The results indicate that inclined-micro-fin flat tubes can greatly enhance the single-phase heat transfer in turbulent flow and the maximum heat transfer coefficient attains to 5.9 times of that in smooth tube. The quantities of heat transfer for inclined-micro-fin flat tubes are three times higher than that of smooth tube with the same of heat exchange area and pump power. (authors)

  2. Solid state magnetic field sensors for micro unattended ground networks using spin dependent tunneling

    Tondra, Mark; Nordman, Catherine A.; Lange, Erik H.; Reed, Daniel; Jander, Albrect; Akou, Seraphin; Daughton, James

    2001-09-01

    Micro Unattended Ground Sensor Networks will likely employ magnetic sensors, primarily for discrimination of objects as opposed to initial detection. These magnetic sensors, then, must fit within very small cost, size, and power budgets to be compatible with the envisioned sensor suites. Also, a high degree of sensitivity is required to minimize the number of sensor cells required to survey a given area in the field. Solid state magnetoresistive sensors, with their low cost, small size, and ease of integration, are excellent candidates for these applications assuming that their power and sensitivity performance are acceptable. SDT devices have been fabricated into prototype magnetic field sensors suitable for use in micro unattended ground sensor networks. They are housed in tiny SOIC 8-pin packages and mounted on a circuit board with required voltage regulation, signal amplification and conditioning, and sensor control and communications functions. The best sensitivity results to date are 289 pT/rt. Hz at 1 Hz, and and 7 pT/rt. Hz at f > 10 kHz. Expected near term improvements in performance would bring these levels to approximately 10 pT/rt Hz at 1 Hz and approximately 1 pT/rt. Hz at > 1 kHz.

  3. Alterations of MicroRNAs in Solid Cancers and Their Prognostic Value

    Chira, Panagiota; Vareli, Katerina; Sainis, Ioannis; Papandreou, Christos; Briasoulis, Evangelos

    2010-01-01

    MicroRNAs (miRNAs) are evolutionarily conserved, naturally abundant, small, regulatory non-coding RNAs that inhibit gene expression at the post-transcriptional level in a sequence-specific manner. Each miRNA represses the protein expression of several coding genes in a manner proportional to the sequence complementarity with the target transcripts. MicroRNAs play key regulatory roles in organismal development and homeostasis. They control fundamental biological processes, such as stem-cell regulation and cellular metabolism, proliferation, differentiation, stress resistance, and apoptosis. Differential miRNA expression is found in malignant tumors in comparison to normal tissue counterparts. This indicates that miRNA deregulation contributes to the initiation and progression of cancer. Currently, miRNA expression signatures are being rigorously investigated in various tumor types, with the aim of developing novel, efficient biomarkers that can improve clinical management of cancer patients. This review discusses deregulated miRNAs in solid tumors, and focuses on their emerging prognostic potential

  4. Study on confirmation of Solid-Meal Lag Phase of Gastric Emptying

    Lee, Ji Young; Lee, Kyoung Soo; Kim, Chang Guhn; Juhng, Seon Kwan; Won, Jong Jin; Nah, Yong Ho

    1991-01-01

    The purpose of this study was to examine the existence of a lag phase of gastric emptying of solid meals. We studied solid phase gastric emptying in 26 normal subject using continuous data acquisition for 30 minutes. Each ingested a 300 g meal containing 99m Tc-labeled scrambled egg (solid 150 g, milk 150 ml). Lag phase was determined by 1) inspection of the gastric emptying curve 2) time to a 2% decrease in stomach activity 3) the time of visual appearance of duodenal activity on computer image. We concluded that solid meal lag phase exist.

  5. Study on confirmation of Solid-Meal Lag Phase of Gastric Emptying

    Lee, Ji Young; Lee, Kyoung Soo; Kim, Chang Guhn; Juhng, Seon Kwan; Won, Jong Jin; Nah, Yong Ho [Wonkwang University School of Medicine, Iksan (Korea, Republic of)

    1991-07-15

    The purpose of this study was to examine the existence of a lag phase of gastric emptying of solid meals. We studied solid phase gastric emptying in 26 normal subject using continuous data acquisition for 30 minutes. Each ingested a 300 g meal containing {sup 99m}Tc-labeled scrambled egg (solid 150 g, milk 150 ml). Lag phase was determined by 1) inspection of the gastric emptying curve 2) time to a 2% decrease in stomach activity 3) the time of visual appearance of duodenal activity on computer image. We concluded that solid meal lag phase exist.

  6. Growth of potassium niobate micro-hexagonal tablets with monoclinic phase and its excellent piezoelectric property

    Chen, Zhong; Huang, Jingyun; Wang, Ye; Yang, Yefeng; Wu, Yongjun; Ye, Zhizhen

    2012-09-01

    Potassium niobate micro-hexagonal tablets were synthesized through hydrothermal reaction with KOH, H2O and Nb2O5 as source materials by using a polycrystalline Al2O3 as substrate. X-ray diffraction, Raman spectra and selected area electron diffraction analysis results indicated that the tablets exhibit monoclinic phase structure and are highly crystallized. Meanwhile, piezoelectric property of the micro-hexagonal tablets was investigated. The as-synthesized tablets exhibit excellent piezoactivities in the experiments, and an effective piezoelectric coefficient of around 80 pm/V was obtained. The tablets have huge potential applications in micro/nano-integrated piezoelectric and optical devices.

  7. Phase stability in wear-induced supersaturated Al-Ti solid solution

    Watanabe, Y.; Yokoyama, K. [Dept. of Functional Machinery Mechanics Shinshu Univ., Ueda (Japan); Hosoda, H. [Precision and Intelligence Lab., Tokyo Inst. of Tech., Nagatsuta, Midori-ku, Yokohama (Japan)

    2002-07-01

    Al-Ti supersaturated solid solutions were introduced by wear testing and the rapid quenching of an Al/Al{sub 3}Ti composite (part of an Al/Al{sub 3}Ti functionally graded material) that was fabricated using the centrifugal method. The phase stability of the supersaturated solid solution was studied through systematic annealing of the supersaturated solid solution. It was found that the Al-Ti supersaturated solid solution decomposed into Al and Al{sub 3}Ti intermetallic compound phases during the heat treatment. The Al-Ti supersaturated solid solutions fabricated were, therefore, not an equilibrium phase, and thus decomposed into the equilibrium phases during heat treatment. It was also found that heat treatment leads to a significant hardness increase for the Al-Ti supersaturated solid solution. Finally, it was concluded that formation of the wear-induced supersaturated solid solution layer was a result of severe plastic deformation. (orig.)

  8. Solid-phase thermolysis of hexachlororuthenates (4) of onium type

    Kukushkin, Yu N; Maslov, E I; Ryabkova, T P; Lobadyuk, V I [Leningradskij Tekhnologicheskij Inst. (USSR)

    1982-10-01

    Methods of thermogravimetry, infrared spectroscopy, electron absorption spectra and magnetic moment measurings were used to a study thermal solid-phase behaviour of onium hexachlororuthenates (4) of (AH)/sub 2/(RuCl/sub 6/) and (A'H/sub 2/)(RuCl/sub 6/) type, where A-benzimidazole (BAZ), pyridine (py), ammonia, A'-phenanthroline-ortho (o-phen), ethylenediamine (en). It was established that heating of solid (BAZH)/sub 2/(RuCl/sub 6/)x2H/sub 2/O and (o-phen H/sub 2/)(RuCl/sub 6/)xH/sub 2/O in 20-500 deg C range leads to separation of crystallization water and the following extraction of hydrogen chloride with formation of cis-(Ru(BAZ)/sub 2/Cl/sub 4/) and (Ru(o-phen)Cl/sub 4/). (pyH)/sub 2/(RuCl/sub 6/) heating causes initially the separation of two moles of hydrogen chloride with formation of cis-(Ru(py)/sub 2/Cl/sub 4/); further increase of temperature leads to reduction separation of chloride with formation of (Ru(py)/sub 2/Cl/sub 3/)/sub 2/ dimer. The mixture of ruthernium chlorides is prepared under conditions of isothermal heating of (NH/sub 4/)/sub 2/(RuCl/sub 6/) and (enH/sub 2/)(RuCl/sub 6/) compounds at temperatures close to the beginning of their decomposition. The separation of intermediate ruthenium compounds of diamine type with ammonia and ethylendiamine failed.

  9. Encapsulation of fish oil into hollow solid lipid micro- and nanoparticles using carbon dioxide.

    Yang, Junsi; Ciftci, Ozan Nazim

    2017-09-15

    Fish oil was encapsulated in hollow solid lipid micro- and nanoparticles formed from fully hydrogenated soybean oil (FHSO) using a novel green method based on atomization of supercritical carbon dioxide (SC-CO 2 )-expanded lipid. The highest fish oil loading efficiency (97.5%, w/w) was achieved at 50%, w/w, initial fish oil concentration. All particles were spherical and in the dry free-flowing form; however, less smooth surface with wrinkles was observed when the initial fish oil concentration was increased up to 50%. With increasing initial fish oil concentration, melting point of the fish oil-loaded particles shifted to lower onset melting temperatures, and major polymorphic form transformed from α to β and/or β'. Oxidative stability of the loaded fish oil was significantly increased compared to the free fish oil (p<0.05). This innovative method forms free-flowing powder products that are easy-to-use solid fish oil formulation, which makes the handling and storage feasible and convenient. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. Syngas (CO-H2) production using high temperature micro-tubular solid oxide electrolysers

    Kleiminger, L.; Li, T.; Li, K.; Kelsall, G.H.

    2015-01-01

    Highlights: • CO 2 and/or H 2 O reduced to CO/H 2 in micro-tubular solid oxide electrolyser (MT-SOE). • MT-SOE: CO 2 , H 2 O | Ni-(ZrO 2 ) 0.92 (Y 2 O 3 ) 0.08 (YSZ) | YSZ | YSZ- La 0.8 Sr 0.2 MnO 3-δ |O 2. • −0.76 A cm −2 achieved at 1.5V and ca. 820°C for H 2 O electrolysis. • Ni wire cathode current collector gave better performance than (Ag wire+Ag paste). • C 18 O 2 in co-electrolysis could not distinguish cathodic and chemical reduction. - Abstract: CO 2 and/or H 2 O were reduced to CO/H 2 in micro-tubular solid oxide electrolysers with yttria-stabilized zirconia (YSZ) electrolyte, Ni-YSZ cermet cathode and strontium(II)-doped lanthanum manganite (LSM) oxygen-evolving anode. At 822 °C, the kinetics of CO 2 reduction were slower (ca. −0.49 A cm −2 at 1.8 V) than H 2 O reduction or co-reduction of CO 2 and H 2 O, which were comparable (ca. −0.83 to −0.77 A cm −2 at 1.8 V). Performances were improved (−0.85 and −1.1 A cm −2 for CO 2 and H 2 O electrolysis, respectively) by substituting the silver current collector with nickel and avoiding blockage of entrances to pores on the inner lumen of micro-tubes induced by silver paste applied previously to decrease contact losses. The change in current collector materials increased ohmic potential losses due to substituting the lower resistance Ag with Ni wire, but decreased electrode polarization losses by 80–93%. For co-electrolysis of CO 2 and H 2 O, isotopically-labelled C 18 O 2 was used to try to distinguish between direct cathodic reduction of CO 2 and its Ni-catalysed chemical reaction with hydrogen from reduction of steam. Unfortunately, oxygen was exchanged between C 18 O 2 and H 2 16 O, enriching oxygen-18 in the steam and substituting oxygen-16 in the carbon dioxide, so the anode off-gas isotopic fractions were meaningless. This occurred even in alumina and YSZ tubes without the micro-tubular reactor, i.e. in the absence of Ni catalyst, though not in quartz tubes

  11. Complementary techniques for solid oxide cell characterisation on micro- and nano-scale

    Wiedenmann, D.; Hauch, A.; Grobety, B.; Mogensen, M.; Vogt, U.

    2009-01-01

    High temperature steam electrolysis by solid oxide electrolysis cells (SOEC) is a way with great potential to transform clean and renewable energy from non-fossil sources to synthetic fuels such as hydrogen, methane or dimethyl ether, which have been identified as promising alternative energy carriers. Also, as SOEC can operate in the reverse mode as solid oxide fuel cells (SOFC), during high peak hours e.g. hydrogen can be used in a very efficient way to reconvert chemically stored energy into electrical energy. As solid oxide cells (SOC) are working at high temperatures (700-900 o C), material degradation and evaporation can occur e.g. from the cell sealing material, leading to poisoning effects and aging mechanisms which are decreasing the cell efficiency and long-term durability. In order to investigate such cell degradation processes, thorough examination on SOC often requires the chemical and structural characterisation on the microscopic and the nanoscopic level. The combination of different microscope techniques like conventional scanning electron microscopy (SEM), electron-probe microanalysis (EPMA) and the focused ion-beam (FIB) preparation technique for transmission electron microscopy (TEM) allows performing post mortem analysis on a multi scale level of cells after testing. These complementary techniques can be used to characterize structural and chemical changes over a large and representative sample area (micro-scale) on the one hand, and also on the nano-scale level for selected sample details on the other hand. This article presents a methodical approach for the structural and chemical characterisation of changes in aged cathode-supported electrolysis cells produced at Riso DTU, Denmark. Also, results from the characterisation of impurities at the electrolyte/hydrogen interface caused by evaporation from sealing material are discussed. (author)

  12. Fabricating and Characterizing the Microfluidic Solid Phase Extraction Module Coupling with Integrated ESI Emitters

    Hangbin Tang

    2018-05-01

    Full Text Available Microfluidic chips coupling with mass spectrometry (MS will be of great significance to the development of relevant instruments involving chemical and bio-chemical analysis, drug detection, food and environmental applications and so on. In our previous works, we proposed two types of microfluidic electrospray ionization (ESI chip coupling with MS: the two-phase flow focusing (FF ESI microfluidic chip and the corner-integrated ESI emitter, respectively. However the pretreatment module integrated with these ESI emitters is still a challenging problem. In this paper, we concentrated on integrating the solid phase micro-extraction (SPME module with our previous proposed on-chip ESI emitters; the fabrication processes of such SPME module are fully compatible with our previous proposed ESI emitters based on the multi-layer soft lithography. We optimized the structure of the integrated chip and characterized its performance using standard samples. Furthermore, we verified its abilities of salt removal, extraction of multiple analytes and separation through on-chip elution using mimic biological urine spiked with different drugs. The results indicated that our proposed integrated module with ESI emitters is practical and effective for real biological sample pretreatment and MS detection.

  13. Automated solid-phase peptide synthesis to obtain therapeutic peptides

    Veronika Mäde

    2014-05-01

    Full Text Available The great versatility and the inherent high affinities of peptides for their respective targets have led to tremendous progress for therapeutic applications in the last years. In order to increase the drugability of these frequently unstable and rapidly cleared molecules, chemical modifications are of great interest. Automated solid-phase peptide synthesis (SPPS offers a suitable technology to produce chemically engineered peptides. This review concentrates on the application of SPPS by Fmoc/t-Bu protecting-group strategy, which is most commonly used. Critical issues and suggestions for the synthesis are covered. The development of automated methods from conventional to essentially improved microwave-assisted instruments is discussed. In order to improve pharmacokinetic properties of peptides, lipidation and PEGylation are described as covalent conjugation methods, which can be applied by a combination of automated and manual synthesis approaches. The synthesis and application of SPPS is described for neuropeptide Y receptor analogs as an example for bioactive hormones. The applied strategies represent innovative and potent methods for the development of novel peptide drug candidates that can be manufactured with optimized automated synthesis technologies.

  14. IN SITU SOLID-PHASE EXTRACTION AND ANALYSIS OF ...

    Fragrance materials, such as synthetic musks in aqueous samples, are normally analyzed by GC/MS in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of 1-L samples. A 1-L sample, however, usually provides too little analyte for full-scan data acquisition.We have developed an on-site extraction method for extracting synthetic musks from 60 L of wastewater effluent. Such a large sample volume permits high-quality, full-scan mass spectra to be obtained for various synthetic musk compounds. Quantification of these compounds was conveniently achieved from the full-scan data directly, without preparing SIM descriptors for each compound to acquire SIM data. The research focused on in the subtasks is the development and application of state-of the-art technologies to meet the needs of the public, Office of Water, and ORD in the area of Water Quality. Located In the subtasks are the various research projects being performed in support of this Task and more in-depth coverage of each project. Briefly, each project's objective is stated below.Subtask 1: To integrate state-of-the-art technologies (polar organic chemical integrative samplers, advanced solid-phase extraction methodologies with liquid chromatography/electrospray/mass spectrometry) and apply them to studying the sources and fate of a select list of PPCPs. Application and improvement of analytical methodologies that can detect non-volatile, polar, water-s

  15. ON-SITE SOLID-PHASE EXTRACTION AND LABORATORY ...

    Fragrance materials such as synthetic musks in aqueous samples, are normally determined by gas chromatography/mass spectrometry in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of I -L samples. Full-scan mass spectra are required to verify that a target analyte has been found by comparison with the mass spectra of fragrance compounds in the NIST mass spectral library. A I -L sample usually provides insufficient analyte for full scan data acquisition. This paper describes an on-site extraction method developed at the U.S. Environmental Protection Agency (USEPA)- Las Vegas Nevada - for synthetic musks from 60 L of wastewater effluent. Such a large sample volume permits high-quality, full-scan mass spectra to be obtained for a wide array of synthetic musks. Quantification of these compounds was achieved from the full-scan data directly, without the need to acquire SIM data. The detection limits obtained with this method are an order of magnitude lower than those obtained from liquid-liquid and other solid phase extraction methods. This method is highly reproducible, and recoveries ranged from 80 to 97% in spiked sewage treatment plant effluent. The high rate of sorbent-sample mass transfer eliminated the need for a methanolic activation step, which reduced extraction time, labor, and solvent use, More samples could be extracted in the field at lower cost. After swnple extraction, the light- weight cartridges ar

  16. Application of solid-phase antibodies to radioimmunoassay

    McConway, M.G.; Chapman, R.S.

    1986-01-01

    Two types of polymeric microparticle, Dynospheres and reprecipitated acid-hydrolysed nylon 6/6, and two methods of activating these particles with either tresyl chloride or carbonyldiimidazole (CDI) prior to covalent linkage of antibodies were investigated with a view towards their respective adoption for the preparation of general solid-phase reagents for immunoassay applications. Activation of each particle and coupling of antibodies was rapid irrespective of the activator. CDI proved to be the activator of choice since it was cheap, less hazardous, more efficient and less pH dependent than tresyl chloride. Both types of microparticle remain buoyant during the RIA incubation periods and form stable pellets after centrifugation. In second antibody applications immobilisation of the first antibody occurs with a short incubation period of 30 min. Nylon microparticles have a higher antibody-coupling capacity and are the particles of choice in both first and second antibody applications. However, the nylon microparticles possess marginally higher non-specific binding characteristics. (Auth.)

  17. Solid phase epitaxy of amorphous silicon carbide: Ion fluence dependence

    Bae, I.-T.; Ishimaru, Manabu; Hirotsu, Yoshihiko; Sickafus, Kurt E.

    2004-01-01

    We have investigated the effect of radiation damage and impurity concentration on solid phase epitaxial growth of amorphous silicon carbide (SiC) as well as microstructures of recrystallized layer using transmission electron microscopy. Single crystals of 6H-SiC with (0001) orientation were irradiated with 150 keV Xe ions to fluences of 10 15 and 10 16 /cm 2 , followed by annealing at 890 deg. C. Full epitaxial recrystallization took place in a specimen implanted with 10 15 Xe ions, while retardation of recrystallization was observed in a specimen implanted with 10 16 /cm 2 Xe ions. Atomic pair-distribution function analyses and energy dispersive x-ray spectroscopy results suggested that the retardation of recrystallization of the 10 16 Xe/cm 2 implanted sample is attributed to the difference in amorphous structures between the 10 15 and 10 16 Xe/cm 2 implanted samples, i.e., more chemically disordered atomistic structure and higher Xe impurity concentration in the 10 16 Xe/cm 2 implanted sample

  18. Complement fixation by solid phase immune complexes. Reduced capacity in SLE sera

    Baatrup, G; Jonsson, H; Sjöholm, A

    1988-01-01

    We describe an ELISA for assessment of complement function based on the capacity of serum to support fixation of complement components to solid phase immune complexes (IC). Microplates were coated with aggregated bovine serum albumin (BSA) followed by rabbit anti-BSA IgG. The solid phase IC were...

  19. Facile synthesis of aliphatic isothiocyanates and thioureas on solid phase using peptide coupling reagents

    Boas, Ulrik; Andersen, Heidi Gertz; Christensen, Jørn B.

    2004-01-01

    Peptide coupling reagents can be used as versatile reagents for the formation of aliphatic isothiocyanates and thioureas on solid phase from the corresponding solid-phase anchored aliphatic primary amines. The formation of the thioureas is fast and highly chemoselective, and proceeds via formatio...

  20. Three-phase boundary length in solid-oxide fuel cells: A mathematical model

    Janardhanan, Vinod M.; Heuveline, Vincent; Deutschmann, Olaf

    A mathematical model to calculate the volume specific three-phase boundary length in the porous composite electrodes of solid-oxide fuel cell is presented. The model is exclusively based on geometrical considerations accounting for porosity, particle diameter, particle size distribution, and solids phase distribution. Results are presented for uniform particle size distribution as well as for non-uniform particle size distribution.

  1. Faults of solid-phase welding in titanium joints and their effect on strength

    Matyushkin, B.A.; Redchits, V.V.

    1982-01-01

    A possibility of the usage of thermal arc energy for the determination of the kinetics of solid-phase joint formation of the VT20 titanium alloy is found out experimentally. Positive action of diffusion annealing upon mechanical properties. of solid-phase joints is explained by the defect elimination

  2. X-ray phase-contrast micro-tomography and image analysis of wood microstructure

    Mayo, Sheridan; Evans, Robert; Chen, Fiona; Lagerstrom, Ryan

    2009-01-01

    A number of commercially important properties of wood depend on details of the wood micro- and nano- structure. CSIRO Forest Biosciences have developed SilviScan, an analytical instrument which uses a number of high-speed techniques for analyzing these properties. X-ray micro-tomographic analysis of wood samples provides detailed 3D reconstructions of the wood microstructure which can be used to validate results from SilviScan measurements. A series of wood samples was analysed using laboratory-based phase-contrast x-ray micro-tomography. Image analysis techniques were applied to the 3D data sets to extract significant features and statistical properties of the specimens. These data provide a means of verification of results from the more rapid SilviScan techniques, and will clarify the results of micro-diffraction studies of wood microfibrils.

  3. Industrial energy demand - a micro panel data analysis. Phase 1

    Bue Bjoerner, T.; Togeby, M.; Christensen, J.

    1998-10-01

    The matching of several existing databases - covering seven different years, two different databases from Statistics Denmark and various information from DEA - has been a challenging task. Despite a relatively automatic procedure the result is promising. More than 2,700 companies can be followed for more than three years and this means that the majority (65-85%) of the energy consumption in Danish industry is included. The number of observations that can be used in the analysis is better than expected. The constructed database has a large number of variables. It includes, e.g. energy consumption of eight major energy sources (and several minor fuels), individual prices for electricity and district heating, information about production value, value added, investments, company size and industrial sector. To this we have added general energy prices for other fuels, information on taxes, subsidies given to individual companies and energy agreements between authorities and individual companies. The combination of micro level, the many variables, the panel structure and the number of observations make the database unique compared to previous data (Danish as well as international) used to analyse industrial energy consumption. The database can be used for a variety of analyses. In the next section we will present simple models that can be used in the analyses of the data. These are single equation models of the energy consumption. In the future more general models can be applied, e.g. with representation of energy, labour and capital. (au)

  4. Experimental research on single phase convection heat transfer in micro-fin tube

    Fan Guangming; Sun Zhongning; Zhu Sheng

    2011-01-01

    An experimental investigation of heat transfer and flow resistance characteristics of single phase water in three micro-fin tubes with different fin height was conducted. At the same time, the efficiency of micro-fin tubes within the experimental scope was evaluated and the optimal working region was determined. Based on the experimental data in the optimal working region, correlations for predicting the heat transfer and flow resistance were also given by multiple regression method. The result indicates that the micro-fin tubes can greatly enhance the single-phase heat transfer in turbulent flow, and the increase of heat transfer coefficient is higher than the increase of flow resistance. The accuracy of the correlation is very high, of which the deviation from the experimental value is very small. (authors)

  5. Phase transitions in solid Kr-CH4 solutions and rotational excitations in phase II

    Bagatskii, M.I.; Mashchenko, D.A.; Dudkin, V.V.

    2007-01-01

    The heat capacity C p of solid Kr-n CH 4 solutions with the CH 4 concentrations n=0.82, 0.86, 0.90 as well as solutions with n=0.90, 0.95 doped with 0.002 O 2 impurity has been investigated under equilibrium vapor pressure over the internal 1-24 K. The (T,n)-phase diagram was refined and the region of two-phase states was determined for Kr-n CH 4 solid solutions. The contribution of the rotational subsystem, C r ot, to the heat capacity of the solutions has been separated. Analysis of C r ot(T) at T 1 and E 2 between the tunnel levels of the A-, T- and A-, E--nuclear-spin species of CH 4 molecules in the orientationally ordered subsystem, and to determine the effective energy gaps E 1 between lowest levels of the A- and T- species. The relations τ(n) and E 1 (n) stem from changes of the effective potential field caused as the replacement of CH 4 molecules by Kr atoms at sites of the ordered sublattices. The effective gaps E L between a group of tunnel levels of the ground-state liberation state and the nearest group of excited levels of the liberation state of the ordered CH 4 molecules in the solutions with n=0.90 (E L =52 K) and 0.95 (E L =55 K) has been estimated

  6. Radiation Polymerization in the Solid Phase; Polymerisation radiochimique en phase solide; Radiatsionnaya polimerizatsiya v tverdoj faze; Radiopolimerizacion en fase solida

    Barkalov, I. M.; Gol' danskij, V. I.; Enikolopov, N. S.; Terekhova, S. F.; Trofimova, G. M.

    1963-11-15

    The radiation polymerization of solid and frozen monomers has recently attracted a great deal of attention because of its theoretical and practical importance in chemical kinetics and radiation chemistry. The strict spacing of monomer units in a polymer brings about a sharp improvement in the physico-chemical properties without any change of chemicai composition. In the synthesis of stereo-regular polymers, the matrix principle is used, i.e. the monomer unit is strictly oriented spatially by the formation of a complex with a catalyst or some other compound. In the radiation polymerization of a number of monomers oriented in clathrate complexes of urea and thio-urea, for instance, crystal stereo-regular polymers were obtained. The simplest variation, however, is the orientation of a monomer in its own crystal lattice. Although many of the theoretical questions involved remain obscure, the technique is extremely promising. Thus, highly crystalline polyoxymethylene has already been obtained by the radiation polymerization of crystalline trioxane. Nevertheless, a more detailed theoretical investigation of the technique is required. For each separate monomer, the contribution to the general picture made by the different types of reaction taking place during irradiation and the subsequent fusion of the solid monomers (specific radiation reaction, post-polymerization and polymerization at phase transition points) needs clarification. Recent detailed research at the Institute of Chemical Physics, USSR, into the solid-phase radiation-polymerization kinetics of a number of monomers, using the calorimetric method and an EPR signal, has revealed the essential role of the specific radiation reaction during the irradiation. The polymerization process for acrylonitrile (from -196{sup o}C to -140{sup o}C) and vinyl acetate (-196{sup o}C to -100{sup o}C) ceases when irradiation is discontinued despite the retention of the shape and intensity of the EPR signal and despite the long

  7. Highly Efficient, Durable Regenerative Solid Oxide Stack, Phase I

    National Aeronautics and Space Administration — Precision Combustion, Inc. (PCI) proposes to develop a highly efficient regenerative solid oxide stack design. Novel structural elements allow direct internal...

  8. MOLECULARLY IMPRINTED SOLID PHASE EXTRACTION FOR TRACE ANALYSIS OF DIAZINON IN DRINKING WATER

    M. Rahiminejad ، S. J. Shahtaheri ، M. R. Ganjali ، A. Rahimi Forushani ، F. Golbabaei

    2009-04-01

    Full Text Available Amongst organophosphate pesticides, the one most widely used and common environmental contaminant is diazinon; thus methods for its trace analysis in environmental samples must be developed. Use of diazinon imprinted polymers such as sorbents in solid phase extraction, is a prominent and novel application area of molecular imprinted polymers. For diazinon extraction, high performance liquid chromatography analysis was demonstrated in this study. During optimization of the molecular imprinted solid phase extraction procedure for efficient solid phase extraction of diazinon, Plackett-Burman design was conducted. Eight experimental factors with critical influence on molecular imprinted solid phase extraction performance were selected, and 12 different experimental runs based on Plackett-Burman design were carried out. The applicability of diazinon imprinted polymers as the sorbent in solid phase extraction, presented obtained good recoveries of diazinon from LC-grade water. An increase in pH caused an increase in the recovery on molecular imprinted solid phase extraction. From these results, the optimal molecular imprinted solid phase extraction procedure was as follows: solid phase extraction packing with 100 mg diazinon imprinted polymers; conditioning with 5 mL of methanol and 6 mL of LC-grade water; sample loading containing diazinon (pH=10; washing with 1 mL of LC-grade water, 1 mL LC- grade water containing 30% acetonitrile and 0.5 mL of acetonitrile, respectively; eluting with 1 mL of methanol containing 2% acetic acid. The percentage recoveries obtained by the optimized molecular imprinted solid phase extraction were more than 90% with drinking water spiked at different trace levels of diazinon. Generally speaking, the molecular imprinted solid phase extraction procedure and subsequent high performance liquid chromatography analysis can be a relatively fast and proper approach for qualitative and quantitative analysis of diazinon in

  9. Phase coded, micro-power impulse radar motion sensor

    McEwan, T.E.

    1996-01-01

    A motion sensing, micro-power impulse radar MIR impresses on the transmitted signal, or the received pulse timing signal, one or more frequencies lower than the pulse repetition frequency, that become intermediate frequencies in a ''IF homodyne'' receiver. Thus, many advantages of classical RF receivers can be thereby be realized with ultra-wide band radar. The sensor includes a transmitter which transmits a sequence of electromagnetic pulses in response to a transmit timing signal at a nominal pulse repetition frequency. A receiver samples echoes of the sequence of electromagnetic pulses from objects within the field with controlled timing, in response to a receive timing signal, and generates a sample signal in response to the samples. A timing circuit supplies the transmit timing signal to the transmitter and supplies the receive timing signal to the receiver. The relative timing of the transmit timing signal and the receive timing signal is modulated between a first relative delay and a second relative delay at an intermediate frequency, causing the receiver to sample the echoes such that the time between transmissions of pulses in the sequence and samples by the receiver is modulated at the intermediate frequency. Modulation may be executed by modulating the pulse repetition frequency which drives the transmitter, by modulating the delay circuitry which controls the relative timing of the sample strobe, or by modulating amplitude of the transmitted pulses. The electromagnetic pulses will have a nominal center frequency related to pulse width, and the first relative delay and the second relative delay between which the timing signals are modulated, differ by less than the nominal pulse width, and preferably by about one-quarter wavelength at the nominal center frequency of the transmitted pulses. 5 figs

  10. Aspects pertinent to the usefulness of a solid phase radio-immuno-sorbent assay for the detection of spermatozoa antibodies in sera of infertility patients

    Hinrichs-Reiche, I.

    1987-01-01

    The solid phase Radio-Immuno-Sorbent Assay (RISA) is a highly sensitive and valid test to detect 125-iodinetagged antibodies to spermatozoa that allows qualitative and quantitative evaluations of sperm-incapacitating immunglobulin Ig G in sera from patients believed to be infertile for immunological reasons. The study failed to reveal any correlations between the results of RISA and those of micro-sperm-agglutination or micro-sperm-immobilisation tests. There was a major body of evidence pointing to possible links between female isoimmunity and male autoimmunity. (TRV) [de

  11. Pressure Effects on Solid State Phase Transformation of Aluminium Bronze in Cooling Process

    Hai-Yan, Wang; Jian-Hua, Liu; Gui-Rong, Peng; Yan, Chen; Yu-Wen, Liu; Fei, Li; Wen-Kui, Wang

    2009-01-01

    Effects of high pressure (6 GPa) on the solid state phase transformation kinetic parameters of aluminum bronze during the cooling process are investigated, based on the measurement and calculation of its solid state phase transformation temperature, duration and activation energy and the observation of its microstructures. The results show that high pressure treatment can reduce the solid phase transformation temperature and activation energy in the cooling process and can shorten the phase transformation duration, which is favorable when forming fine-grained aluminum bronze

  12. Supported liquid phase catalyst coating in micro flow Mizoroki-Heck reaction

    Stouten, S.C.; Noël, T.; Wang, Q.; Hessel, V.

    2015-01-01

    A Supported Liquid Phase Catalyst (SLPC) coating was successfully applied for the Mizoroki–Heck reaction in micro flow. Foremost, extended on stream operation was enabled and the on stream performance stability was verified. Stable catalytic activity was achieved during two consecutive runs totaling

  13. Ultrarapid mutation detection by multiplex, solid-phase chemical cleavage

    Rowley, G.; Saad, S.; Giannelli, F.; Green, P.M. [Guy`s & St. Thomas`s Hospitals, London (United Kingdom)

    1995-12-10

    The chemical cleavage of mismatches in heteroduplexes formed by probe and test DNA detects and locates any sequence change in long DNA segments ({approximately}1.8 kb), and its efficiency has been well tested in the analysis of both average (e.g., coagulation factor IX) and large, complex genes (e.g., coagulation factor VIII and dystrophin). In the latter application RT/PCR products allow the examination of all essential sequences of the gene in a minimum number of reactions. We use two specific chemical reactants (hydroxylamine and osmium tetroxide) and piperidine cleavage of the above procedure to develop a very fast mutation screening method. This is based on: (1) 5{prime} or internal fluorescent labeling to allow concurrent screening of three to four DNA fragments and (2) solid-phase chemistry to use a microliter format and reduce the time required for the procedure, from amplification of sequence to gel loading inclusive, to one person-working-day. We test the two variations of the method, one entailing 5{prime} labeling of probe DNA and the other uniform labeling of both probe and target DNA, by detecting 114 known hemophilia B (coagulation factor IX) mutations and by analyzing 129 new patients. Uniform labeling of both probe and target DNA prior to formation of the heteroduplexes leads to almost twofold redundancy in the ability to detect mutations. Alternatively, the latter procedure may offer very efficient though less than 100% screening for sequence changes with only hydroxylamine. The full method with two chemical reactions (hydroxylamine and osmium tetroxide) should allow one person to screen with virtually 100% accuracy more than 300 kb of sequence in three ABI 373 gels in 1 day. 26 refs., 7 figs., 1 tab.

  14. Investigation of impurity-helium solid phase decomposition

    Boltnev, R.E.; Gordon, E.B.; Krushinskaya, I.N.; Martynenko, M.V.; Pel'menev, A.A.; Popov, E.A.; Khmelenko, V.V.; Shestakov, A.F.

    1997-01-01

    The element composition of the impurity-helium solid phase (IHSP), grown by injecting helium gas jet, involving Ne, Ar, Kr, and Xe atoms and N 2 molecules, into superfluid helium, has been studied. The measured stoichiometric ratios, S = N H e / N I m, are well over the values expected from the model of frozen together monolayer helium clusters. The theoretical possibility for the freezing of two layers helium clusters is justified in the context of the model of IHSP helium subsystem, filled the space between rigid impurity centers. The process of decomposition of impurity-helium (IH)-samples taken out of liquid helium in the temperature range 1,5 - 12 K and the pressure range 10-500 Torr has been studied. It is found that there are two stages of samples decomposition: a slow stage characterized by sample self cooling and a fast one accompanied by heat release. These results suggest, that the IHSP consists of two types of helium - weakly bound and strongly bound helium - that can be assigned to the second and the first coordination helium spheres, respectively, formed around heavy impurity particles. A tendency for enhancement of IHSP thermo stability with increasing the impurity mass is observed. Increase of helium vapor pressure above the sample causes the improvement of IH sample stability. Upon destruction of IH samples, containing nitrogen atoms, a thermoluminescence induced by atom recombination has been detected in the temperature region 3-4,5 K. This suggests that numerous chemical reactions may be realized in solidified helium

  15. Monolithic graphene fibers for solid-phase microextraction.

    Fan, Jing; Dong, Zelin; Qi, Meiling; Fu, Ruonong; Qu, Liangti

    2013-12-13

    Monolithic graphene fibers for solid-phase microextraction (SPME) were fabricated through a dimensionally confined hydrothermal strategy and their extraction performance was evaluated. For the fiber fabrication, a glass pipeline was innovatively used as a hydrothermal reactor instead of a Teflon-lined autoclave. Compared with conventional methods for SPME fibers, the proposed strategy can fabricate a uniform graphene fiber as long as several meters or more at a time. Coupled to capillary gas chromatography (GC), the monolithic graphene fibers in a direct-immersion (DI) mode achieved higher extraction efficiencies for aromatics than those for n-alkanes, especially for polycyclic aromatic hydrocarbons (PAHs), thanks to π-π stacking interaction and hydrophobic effect. Additionally, the fibers exhibited excellent durability and can be repetitively used more than 160 times without significant loss of extraction performance. As a result, an optimum extraction condition of 40°C for 50min with 20% NaCl (w/w) was finally used for SPME of PAHs in aqueous samples. For the determination of PAHs in water samples, the proposed DI-SPME-GC method exhibited linear range of 0.05-200μg/L, limits of detection (LOD) of 4.0-50ng/L, relative standard deviation (RSD) less than 9.4% and 12.1% for one fiber and different fibers, respectively, and recoveries of 78.9-115.9%. The proposed method can be used for analysis of PAHs in environmental water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Biological treatment of soils contaminated with hydrophobic organics using slurry and solid phase techniques

    Cassidy, D.P.; Irvine, R.L.

    1995-01-01

    Both slurry-phase and solid-phase bioremediation are effective ex situ soil decontamination methods. Slurry is energy intensive relative to solid-phase treatment, but provides homogenization and uniform nutrient distribution. Limited contaminant bioavailability at concentrations above the required cleanup level reduces biodegradation rates and renders solid phase bioremediation more cost effective than complete treatment in a bioslurry reactor. Slurrying followed by solid-phase bioremediation combines the advantages and minimizes the weaknesses of each treatment method when used alone. A biological treatment system consisting of slurrying followed by aeration in solid phase bioreactors was developed and tested in the laboratory using a silty clay load contaminated with diesel fuel. The first set of experiments was designed to determine the impact of the water content and mixing time during slurrying on the ate and extent of contaminant removal in continuously aerated solid phase bioreactors. The second set of experiments compared the volatile and total diesel fuel removal in solid phase bioreactors using periodic and continuous aeration strategies

  17. High-performance micro-solid oxide fuel cells fabricated on nanoporous anodic aluminum oxide templates

    Kwon, Chang-Woo; Kim, Hyun-Mi; Kim, Ki-Bum [WCUHybrid Materials Program, Department of Materials Science and Engineering, Seoul National University, 599 Gwanak-ro, Gwanak-gu, Seoul, 151-742 (Korea, Republic of); Son, Ji-Won; Lee, Jong-Ho; Lee, Hae-Weon [High Temperature Energy Materials Center, Korea Institute of Science and Technology, 39-1, Hawolgok-dong, Seongbuk-gu, Seoul, 136-791 (Korea, Republic of)

    2011-03-22

    Micro-solid oxide fuel cells ({mu}-SOFCs) are fabricated on nanoporous anodic aluminum oxide (AAO) templates with a cell structure composed of a 600-nm-thick AAO free-standing membrane embedded on a Si substrate, sputter-deposited Pt electrodes (cathode and anode) and an yttria-stabilized zirconia (YSZ) electrolyte deposited by pulsed laser deposition (PLD). Initially, the open circuit voltages (OCVs) of the AAO-supported {mu}-SOFCs are in the range of 0.05 V to 0.78 V, which is much lower than the ideal value, depending on the average pore size of the AAO template and the thickness of the YSZ electrolyte. Transmission electron microscopy (TEM) analysis reveals the formation of pinholes in the electrolyte layer that originate from the porous nature of the underlying AAO membrane. In order to clog these pinholes, a 20-nm thick Al{sub 2}O{sub 3} layer is deposited by atomic layer deposition (ALD) on top of the 300-nm thick YSZ layer and another 600-nm thick YSZ layer is deposited after removing the top intermittent Al{sub 2}O{sub 3} layer. Fuel cell devices fabricated in this way manifest OCVs of 1.02 V, and a maximum power density of 350 mW cm{sup -2} at 500 C. (Copyright copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  18. Method for calculating solid-solid phase transitions at high temperature: An application to N2O

    Kuchta, B.; Etters, R.D.

    1992-01-01

    Two similar techniques for calculating solid-solid phase transitions at high temperatures are developed, where the contribution of the entropy may be a decisive factor. They utilize an artificial reversible path from one phase to another by application of a control parameter. Thermodynamic averages are calculated using constant-volume and constant-pressure Monte Carlo techniques. An application to N 2 O at room temperature shows that the cubic Pa3 to orthorhombic Cmca transition occurs near 4.9-GPa pressure, very close to the value calculated at very low temperatures. These results support experimental evidence that the transition pressure is virtually independent of temperature

  19. Determination of parathion in biological fluids by means of direct solid-phase microextraction.

    Gallardo, E; Barroso, M; Margalho, C; Cruz, A; Vieira, D N; López-Rivadulla, M

    2006-11-01

    A new and simple procedure for the determination of parathion in human whole blood and urine using direct immersion (DI) solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS) is presented. This technique was developed using only 100 microL of sample, and ethion was used as internal standard (IS). A 65-microm Carbowax/divinylbenzene (CW/DVB) SPME fibre was selected for sampling, and the main parameters affecting the SPME process such as extraction temperature, adsorption and desorption time, salt addition, agitation and pH effect were optimized to enhance the sensitivity of the method. This optimization was also performed to allow the qualitative determination of parathion's main metabolite, paraoxon, in blood. The limits of detection and quantitation for parathion were 3 and 10 ng/mL for urine and 25 and 50 ng/mL for blood, respectively. For paraoxon, the limit of detection was 50 ng/mL in blood. The method showed linearity between the LOQ and 50 microg/mL for both matrices, with correlation coefficients ranging from 0.9954 to 0.9999. Precision and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. The mean absolute recoveries were 35.1% for urine and 6.7% for blood. Other parameters such as dilution of sample and stability were also validated. Its simplicity and the fact that only 100 microL of sample is required to accomplish the analysis make this method useful in forensic toxicology laboratories to determine this compound in intoxications, and it can be considered an alternative to other methods normally used for the determination of this compound in biological media.

  20. Determination of Scopolamine in Human Saliva Using Solid Phase Extraction and LC/MS/MS

    Wang, Zuwei; Vaksman, Zalman; Boyd, Jason; Putcha, Lakshmi

    2007-01-01

    Purpose: Scopolamine is the preferred treatment for motion sickness during space flight because of its quick onset of action, short half-life and favorable side-effect profile. The dose administered depends on the mode of administration and usually ranges between 0.1 and 0.8 mg. Such small doses make it difficult to detect concentrations of scopolamine in biological fluids by using conventional HPLC methods. To measure scopolamine in saliva and thereby to evaluate the pharmacokinetics of scopolamine, we developed an LC/MS/MS method using off-line solid phase extraction. Method: Samples (0.5mL) were loaded onto Waters Oasis HLB co-polymer cartridges (10 mg, 1 mL) and eluted with 0.5 mL methanol without evaporation and reconstitution. HPLC separation of the eluted sample was performed using an Agilent Zorbax SB-CN column (50 x 2.1 mm) at a flow rate of 0.2 mL/min for 4 minutes. The mobile phase for separation was 90:10 (v/v) methanol: ammonium acetate (2 mM) in water, pH 5.0 +/- 0.1. Concentrations of scopolamine were determined using a Micromass Quattro Micro(TM) mass spectrometer with electrospray ionization (ESI). ESI mass spectra were acquired in positive ion mode with multiple reaction monitoring for the determination of scopolamine m/z = 304.2 yields 138.1 and internal standard (IS) hyoscyamine m/z = 290.2 yields 124.1. Results: The method is rapid, reproducible, specific and has the following parameters: scopolamine and the IS are eluted at 1.7 and 3.2 min respectively. The linear range is 50-5000 pg/mL for scopolamine in saliva with correlation coefficients > 0.99 with a CV < 0.5 %. The intra-day and inter-day CVs are < 15 % for quality control samples with concentrations of 75, 300, 750 and 3000 pg/mL of scopolamine in human saliva. Conclusion: Solid phase extraction allows more rapid sample preparation and greater precision than liquid extraction. Furthermore, we increased the sensitivity and specificity by adjusting the LC mobile phase and using an MS

  1. Influence of Homogenization and Micro/Nano Source of Starting Powders on Format Ion of the Single YAP Phase

    Michalik D.

    2016-12-01

    Full Text Available Manufacturing high purity polycrystalline YAlO3 (YAP ceramics could replace monocrystalline YAP thus recently it is an interesting task for low cost producers of scintillators. The paper presents influence of different source of initial oxide powders (micro/nano powders of Y2O3 and Al2O3 and the method of their homogenization on the formation of a YAP phase. The solid state reaction method was used to prepare YAP powder or ceramic pellets. After preheating, all samples in the form of powders and pellets were heat-treated in the temperature range of 1050-1650 °C. DTA method was applied for examination of the phase crystallization in the tested system. X-ray diffraction method (XRD was used for characterization of the phase composition. X-ray microanalysis (EDS was used to control homogeneity in the small areas. Morphology of the resultant samples are presented on SEM pictures. The results show a significant influence of the starting powders on the homogeneity, purity and temperature of formation of the main phase.

  2. Biological treatment of soils contaminated with hydrophobic organics using slurry- and solid-phase techniques

    Cassidy, Daniel H.; Irvine, Robert L.

    1995-10-01

    Both slurry-phase and solid-phase bioremediation are effective ex situ soil decontamination methods. Slurrying is energy intensive relative to solid-phase treatment, but provides homogenization and uniform nutrient distribution. Limited contaminant bioavailability at concentrations above the required cleanup level reduces biodegradation rates and renders solid phase bioremediation more cost effective than complete treatment in a bio-slurry reactor. Slurrying followed by solid-phase bioremediation combines the advantages and minimizes the weaknesses of each treatment method when used alone. A biological treatment system consisting of slurrying followed by aeration in solid phase bioreactors was developed and tested in the laboratory using a silty clay loam contaminated with diesel fuel. The first set of experiments was designed to determine the impact of the water content and mixing time during slurrying on the rate an extent of contaminant removal in continuously aerated solid phase bioreactors. The second set of experiments compared the volatile and total diesel fuel removal in solid phase bioreactors using periodic and continuous aeration strategies. Results showed that slurrying for 1.5 hours at a water content less than saturation markedly increased the rate and extent of contaminant biodegradation in the solid phase bioreactors compared with soil having no slurry pretreatment. Slurrying the soil at or above its saturation moisture content resulted in lengthy dewatering times which prohibited aeration, thereby delaying the onset of biological treatment in the solid phase bioreactors. Results also showed that properly operated periodic aeration can provide less volatile contaminant removal and a grater fraction of biological contaminant removal than continuous aeration.

  3. Phase-shifting Real-time Holographic Microscopy applied in micro-structures surface analysis

    Brito, I V; Gesualdi, M R R; Muramatsu, M; Ricardo, J

    2011-01-01

    The microscopic real-time analysis of micro structured materials is of great importance in various domains of science and technology. For other hand, the holographic interferometry comprises a group of powerful optical methods for non-destructive testing in surface analysis. The holographic microscopy uses the holographic interferometric techniques to obtain quantitative intensity and phase information of the optical waves by microscopic systems. With the development of CCD cameras, computers (hardware and software), and new materials for holographic recording, these techniques can be used to replace the classical form of registration and became promising tools in surface analysis. In this work, we developed a prototype of Photorefractive and Digital Holographic Microscope for real-time analysis of micro-structured systems based on the phase-shifting real-time holographic interferometry techniques. Using this apparatus, we are made analysis of shapes and surfaces to obtain the phase maps and the 3D profiles of some samples.

  4. Experimental study on void fraction of two-phase flow inside a micro-fin tube

    Koyama, Shigeru; Chen, Yongchang; Kitano, Ryuji; Kuwahara, Ken

    2001-01-01

    In this paper the void fraction and flow pattern of the two-phase flow in a micro-fin tube were investigated experimentally for a pure refrigerant HFC134a. The experiment was carried out at a pressure range of 0.6 and 1.2MPa with mass velocities of 90 and 180kg/m^2 s, in which the vapor quality varied from 0 to 1. The void fraction was measured by means of simultaneously closing valves of both sides of the test tube at adiabatic condition. Experimental results for the micro-fin tube were comp...

  5. Selective deposition of nanostructured ruthenium oxide using Tobacco mosaic virus for micro-supercapacitors in solid Nafion electrolyte

    Gnerlich, Markus; Ben-Yoav, Hadar; Culver, James N.; Ketchum, Douglas R.; Ghodssi, Reza

    2015-10-01

    A three-dimensional micro-supercapacitor has been developed using a novel bottom-up assembly method combining genetically modified Tobacco mosaic virus (TMV-1Cys), photolithographically defined micropillars and selective deposition of ruthenium oxide on multi-metallic microelectrodes. The three-dimensional microelectrodes consist of a titanium nitride current collector with two functionalized areas: (1) gold coating on the active electrode area promotes TMV-1Cys adhesion, and (2) sacrificial nickel pads dissolve in ruthenium tetroxide plating solution to produce ruthenium oxide on all electrically connected areas. The microfabricated electrodes are arranged in an interdigitated pattern, and the capacitance per electrode has been measured as high as 203 mF cm-2 with solid Nafion electrolyte. The process integration of bio-templated ruthenium oxide with microfabricated electrodes and solid electrolyte is an important advance towards the energy storage needs of mass produced self-sufficient micro-devices.

  6. Solid State MEMS Thrusters Using Electrically Controlled Extinguishable Solid Propellant, Phase I

    National Aeronautics and Space Administration — ET Materials, LLC developed the first ever electrically controlled extinguishable solid propellant (ECESP). The original propellant developed under Air Force SBIR...

  7. Identification and fingerprinting of biodiesel blends by solid phase extraction and gas chromatography-mass spectrometry

    Yang, Z. [Environment Canada, Ottawa, ON (Canada). Emergencies Science and Technology Section, Emergencies, Operational Analytical Laboratories and Research Support Division; China Univ. of Geosciences, Wuhan (China). School of Environmental Studies; Hollebone, B.; Wang, Z.; Yang, C.; Landriault, M. [Environment Canada, Ottawa, ON (Canada). Emergencies Science and Technology Section, Emergencies, Operational Analytical Laboratories and Research Support Division

    2009-07-01

    Interest in biodiesel as a replacement for petroleum diesel fuel is growing. In North America, biodiesels are produced by the methyl esterification of plant and animal triglycerides, resulting in complex mixtures composed of fatty acid methyl esters (FAMEs). It is important for both environmental forensic and remediation purposes to determine diesel and biodiesel origins, and the biodiesel content when it is blended with conventional petroleum diesel. This paper reported on a study that combined 2 methods to determine biodiesel levels in blended fuels. Micro-column fractionation of FAMEs involving solid phase extraction (SPE) was combined with gas chromatography-mass spectrometry (GC/MS) to achieve detailed chemical fingerprinting of blends, including the identification and quantification of individual aliphatic hydrocarbons, aromatic hydrocarbons, fatty acid alkyl esters, and free sterols. Fractionation of the fuel samples was optimized for separation of fatty acid esters, free sterols from petroleum hydrocarbons into 4 fractions, notably aliphatic, aromatic, fatty-acid ester and polar components. A sum of the FAME components was used to determine an unknown blend level in freshly-prepared samples. This study showed that this method has great potential for identifying biodiesel in diesel fuel blends and could form the basis of a method for biodiesel-contaminated environmental samples. 28 refs., 5 tabs., 4 figs.

  8. Identification and fingerprinting of biodiesel blends by solid phase extraction and gas chromatography-mass spectrometry

    Yang, Z.; China Univ. of Geosciences, Wuhan; Hollebone, B.; Wang, Z.; Yang, C.; Landriault, M.

    2009-01-01

    Interest in biodiesel as a replacement for petroleum diesel fuel is growing. In North America, biodiesels are produced by the methyl esterification of plant and animal triglycerides, resulting in complex mixtures composed of fatty acid methyl esters (FAMEs). It is important for both environmental forensic and remediation purposes to determine diesel and biodiesel origins, and the biodiesel content when it is blended with conventional petroleum diesel. This paper reported on a study that combined 2 methods to determine biodiesel levels in blended fuels. Micro-column fractionation of FAMEs involving solid phase extraction (SPE) was combined with gas chromatography-mass spectrometry (GC/MS) to achieve detailed chemical fingerprinting of blends, including the identification and quantification of individual aliphatic hydrocarbons, aromatic hydrocarbons, fatty acid alkyl esters, and free sterols. Fractionation of the fuel samples was optimized for separation of fatty acid esters, free sterols from petroleum hydrocarbons into 4 fractions, notably aliphatic, aromatic, fatty-acid ester and polar components. A sum of the FAME components was used to determine an unknown blend level in freshly-prepared samples. This study showed that this method has great potential for identifying biodiesel in diesel fuel blends and could form the basis of a method for biodiesel-contaminated environmental samples. 28 refs., 5 tabs., 4 figs.

  9. The growth and tensile deformation behavior of the silver solid solution phase with zinc

    Wu, Jiaqi; Lee, Chin C.

    2016-01-01

    The growth of homogeneous silver solid solution phase with zinc are conducted at two different compositions. X-ray diffraction (XRD) and Scanning electron microscope/Energy dispersive X-ray spectroscopy (SEM/EDX) are carried out for phase identification and chemical composition verification. The mechanical properties of silver solid solution phase with zinc are evaluated by tensile test. The engineering and true stress vs. strain curves are presented and analyzed, with those of pure silver in comparison. According to the experimental results, silver solid solution phase with zinc at both compositions show tempered yield strength, high tensile strength and large uniform strain compared to those of pure silver. Fractography further confirmed the superior ductility of silver solid solution phase with zinc at both compositions. Our preliminary but encouraging results may pave the way for the silver based alloys to be applied in industries such as electronic packaging and structure engineering.

  10. "Imaging" LEIS of micro-patterned solid oxide fuel cell electrodes

    Druce, John; Simrick, Neil; Ishihara, Tatsumi; Kilner, John

    2014-08-01

    Understanding the kinetics of oxygen exchange between the gas phase and a ceramic electrode is key to optimising the performance of electrochemical energy conversion devices such as Solid Oxide Fuel Cells. Clearly the surface chemistry of these materials is important, and surface sensitive techniques such as Low Energy Ion Scattering (LEIS) can provide important compositional information key to unravelling electrode kinetics. In this work, we use high lateral resolution LEIS to perform local analyses of a micropatterned electrode structure, of the type often used for studies of the geometrical dependences of electrode performance. We find that the results are comparable to those for bulk materials, but detect evidence of cation interdiffusion from the electrode to the electrolyte. Finally, we note that this preliminary study could open the prospect of in situ measurements of cells near operating conditions.

  11. “Imaging” LEIS of micro-patterned solid oxide fuel cell electrodes

    Druce, John, E-mail: john.druce@i2cner.kyushu-u.ac.jp [International Institute for Carbon Neutral Energy Research (wpi-I2CNER), Kyushu University, Fukuoka 819-0395 (Japan); Simrick, Neil [Department of Materials, Imperial College London, London SW7 2BP (United Kingdom); Ishihara, Tatsumi [International Institute for Carbon Neutral Energy Research (wpi-I2CNER), Kyushu University, Fukuoka 819-0395 (Japan); Kilner, John [International Institute for Carbon Neutral Energy Research (wpi-I2CNER), Kyushu University, Fukuoka 819-0395 (Japan); Department of Materials, Imperial College London, London SW7 2BP (United Kingdom)

    2014-08-01

    Understanding the kinetics of oxygen exchange between the gas phase and a ceramic electrode is key to optimising the performance of electrochemical energy conversion devices such as Solid Oxide Fuel Cells. Clearly the surface chemistry of these materials is important, and surface sensitive techniques such as Low Energy Ion Scattering (LEIS) can provide important compositional information key to unravelling electrode kinetics. In this work, we use high lateral resolution LEIS to perform local analyses of a micropatterned electrode structure, of the type often used for studies of the geometrical dependences of electrode performance. We find that the results are comparable to those for bulk materials, but detect evidence of cation interdiffusion from the electrode to the electrolyte. Finally, we note that this preliminary study could open the prospect of in situ measurements of cells near operating conditions.

  12. Experimental (solid + liquid) or (liquid + liquid) phase equilibria of (amine + nitrile) binary mixtures

    Domanska, Urszula; Marciniak, Malgorzata

    2007-01-01

    (Solid + liquid) phase diagrams have been determined for (hexylamine, or octylamine, or 1,3-diaminopropane + acetonitrile) mixtures. Simple eutectic systems have been observed in these mixtures. (Liquid + liquid) phase diagrams have been determined for (octylamine, or decylamine + propanenitrile, or + butanenitrile) mixtures. Mixtures with propanenitrile and butanenitrile show immiscibility in the liquid phase with an upper critical solution temperature, UCST. (Solid + liquid) phase diagrams have been correlated using NRTL, NRTL 1, Wilson and UNIQUAC equations. (Liquid + liquid) phase diagrams have been correlated using NRTL equation

  13. Ultrasonic detection of solid phase mass flow ratio of pneumatic conveying fly ash

    Duan, Guang Bin; Pan, Hong Li; Wang, Yong; Liu, Zong Ming

    2014-04-01

    In this paper, ultrasonic attenuation detection and weight balance are adopted to evaluate the solid mass ratio in this paper. Fly ash is transported on the up extraction fluidization pneumatic conveying workbench. In the ultrasonic test. McClements model and Bouguer-Lambert-Beer law model were applied to formulate the ultrasonic attenuation properties of gas-solid flow, which can give the solid mass ratio. While in the method of weigh balance, the averaged mass addition per second can reveal the solids mass flow ratio. By contrast these two solid phase mass ratio detection methods, we can know, the relative error is less.

  14. Materials research for passive solar systems: Solid-state phase-change materials

    Benson, D. K.; Webb, J. D.; Burrows, R. W.; McFadden, J. D. O.; Christensen, C.

    1985-03-01

    A set of solid-state phase-change materials is being evaluated for possible use in passive solar thermal energy storage systems. The most promising materials are organic solid solutions of pentaerythritol (C5H12O4), pentaglycerinve (C5H12O3), and neopentyl glycol (C5H12O2). Solid solution mixtures of these compounds can be tailored so that they exhibit solid-to-solid phase transformations at any desired temperature between 25 C and 188 C, and have latent heats of transformation etween 20 and 70 cal/g. Transformation temperatures, specific heats, and latent heats of transformation have been measured for a number of these materials. Limited cyclic experiments suggest that the solid solutions are stable. These phase-change materials exhibit large amounts of undercooling; however, the addition of certain nucleating agents as particulate dispersions in the solid phase-change material greatly reduces this effect. Computer simulations suggest that the use of an optimized solid-state phase-change material in a Trombe wall could provide better performance than a concrete Trombe wall four times thicker and nine times heavier.

  15. Phase transition of solid bismuth under high pressure

    Chen Hai-Yan; Xiang Shi-Kai; Yan Xiao-Zhen; Zhang Yi; Liu Sheng-Gang; Bi Yan; Zheng Li-Rong

    2016-01-01

    As a widely used pressure calibrator, the structural phase transitions of bismuth from phase I, to phase II, to phase III, and then to phase V with increasing pressure at 300 K have been widely confirmed. However, there are different structural versions for phase III, most of which are determined by x-ray diffraction (XRD) technology. Using x-ray absorption fine structure (XAFS) measurements combined with ab initio calculations, we show that the proposed incommensurate composite structure of bismuth of the three configurations is the best option. An abnormal continuous increase of the nearest-neighbor distance of phase III with elevated pressure is also observed. The electronic structure transformation from semimetal to metal is responsible for the complex behavior of structure transformation. (paper)

  16. Micro-Raman spectroscopy studies of the phase separation mechanisms of transition-metal phosphate glasses

    Mazali, Italo Odone; Alves, Oswaldo Luiz; Gimenez, Iara de Fatima

    2009-01-01

    Glass-ceramics are prepared by controlled separation of crystal phases in glasses, leading to uniform and dense grain structures. On the other hand, chemical leaching of soluble crystal phases yields porous glass-ceramics with important applications. Here, glass/ceramic interfaces of niobo-, vanado- and titano-phosphate glasses were studied by micro-Raman spectroscopy, whose spatial resolution revealed the multiphase structures. Phase-separation mechanisms were also determined by this technique, revealing that interface composition remained unchanged as the crystallization front advanced for niobo- and vanadophosphate glasses (interface-controlled crystallization). For titanophosphate glasses, phase composition changed continuously with time up to the equilibrium composition, indicating a spinodal-type phase separation. (author)

  17. Modeling and Analysis of a Three-Phase Solid-State Var ...

    Modeling and Analysis of a Three-Phase Solid-State Var Compensator (SSVC) ... Nigerian Journal of Technology. Journal Home ... The problems associated with the flow of reactive power in transmission and distribution lines are well known.

  18. Utilizing ion-pairing hydrophilic interaction chromatography solid phase extraction for efficient glycopeptide enrichment in glycoproteomics

    Mysling, Simon; Palmisano, Giuseppe; Højrup, Peter

    2010-01-01

    Glycopeptide enrichment is a prerequisite to enable structural characterization of protein glycosylation in glycoproteomics. Here we present an improved method for glycopeptide enrichment based on zwitter-ionic hydrophilic interaction chromatography solid phase extraction (ZIC-HILIC SPE...

  19. Evaluation of a Solid Phase DNA Binding Matrix for Downstream PCR Analysis

    Bader, Douglas E; Fisher, Glen R; Stratilo, Chad W

    2005-01-01

    A commercially available solid-phase DNA binding matrix (FTA cards) was evaluated for its ability to capture and release DNA for downstream gene amplification and detection assays using polymerase chain reaction (PCR...

  20. Ion-selective solid-phase electrode sensitive to ammonium ions

    Vlasov, Yu.G.; Milonova, M.S.; Antonov, P.P.; Bychkov, E.A.; Ehfa, A.Ya.

    1983-01-01

    Ammonium phosphomolybdate is investigated for the purpose of using it as membrane material of ammonium-selective solid-phase electrodes. Estimation of proton mobility and ion conductivity of ammonium phosphomolybdate is performed

  1. A Variational Model for Two-Phase Immiscible Electroosmotic Flow at Solid Surfaces

    Shao, Sihong; Qian, Tiezheng

    2012-01-01

    We develop a continuum hydrodynamic model for two-phase immiscible flows that involve electroosmotic effect in an electrolyte and moving contact line at solid surfaces. The model is derived through a variational approach based on the Onsager

  2. Isostructural solid-solid phase transition in monolayers of soft core-shell particles at fluid interfaces: structure and mechanics.

    Rey, Marcel; Fernández-Rodríguez, Miguel Ángel; Steinacher, Mathias; Scheidegger, Laura; Geisel, Karen; Richtering, Walter; Squires, Todd M; Isa, Lucio

    2016-04-21

    We have studied the complete two-dimensional phase diagram of a core-shell microgel-laden fluid interface by synchronizing its compression with the deposition of the interfacial monolayer. Applying a new protocol, different positions on the substrate correspond to different values of the monolayer surface pressure and specific area. Analyzing the microstructure of the deposited monolayers, we discovered an isostructural solid-solid phase transition between two crystalline phases with the same hexagonal symmetry, but with two different lattice constants. The two phases corresponded to shell-shell and core-core inter-particle contacts, respectively; with increasing surface pressure the former mechanically failed enabling the particle cores to come into contact. In the phase-transition region, clusters of particles in core-core contacts nucleate, melting the surrounding shell-shell crystal, until the whole monolayer moves into the second phase. We furthermore measured the interfacial rheology of the monolayers as a function of the surface pressure using an interfacial microdisk rheometer. The interfaces always showed a strong elastic response, with a dip in the shear elastic modulus in correspondence with the melting of the shell-shell phase, followed by a steep increase upon the formation of a percolating network of the core-core contacts. These results demonstrate that the core-shell nature of the particles leads to a rich mechanical and structural behavior that can be externally tuned by compressing the interface, indicating new routes for applications, e.g. in surface patterning or emulsion stabilization.

  3. Effect of solids, caloric content on dual-phase gastric emptying

    Van Den Maegdenbergh, V.; Urbain, J.L.; Siegel, J.A.; Mortelmans, L.; De Roo, M. (Univ. Hospital Gasthuisberg, Leuven (Belgium) Temple Univ. Hospital, Philadelphia, PA (USA))

    1990-03-01

    The dual-phase gastric emptying technique is routinely employed to determine the differential emptying of solids and liquids in a wide spectrum of gastrointestinal diseases. Composition, acidity, volume, caloric density, physical form and viscosity of the test means have been shown to be important determinants for the quantitative evaluation of gastric emptying. In this study, the authors have evaluated the effect of increasing the caloric content of the solid portion of a physiologic test mean on both solid and liquid emptying kinetics in health male volunteers. They observed that increasing solid caloric content delayed emptying of both solids and liquids. For the solid phase, the delay was accounted for by a longer lag phase and decrease in emptying rate; for liquids a longer emptying rate was also obtained. They conclude that modification of the caloric content of the solid portion of a meal not only affects the emptying of the solid phase but also alters the emptying of the liquid component of the meal.

  4. The Pictet-Spengler reaction in solid-phase combinatorial chemistry

    Nielsen, Thomas E; Diness, Frederik; Meldal, Morten

    2003-01-01

    The Pictet-Spengler reaction is an important reaction for the generation of tetrahydro-beta-carbolines and tetrahydroisoquinoline ring systems, which exhibit a range of biological and pharmacological properties. This review covers the solid-phase Pictet-Spengler reaction, as employed in solid...

  5. Solid phase microextraction speciation analysis of triclosan in aqueous mediacontaining sorbing nanoparticles

    Zielinska, K.

    2014-01-01

    Solid phase microextraction (SPME) is applied in the speciation analysis of the hydrophobic compound triclosan in an aqueous medium containing sorbing SiO2 nanoparticles (NPs). It is found that these NPs, as well as their complexes with triclosan, partition between the bulk medium and the solid

  6. Three magnetic particles solid phase radioimmunoassay for T4: Comparison of their results with established methods

    Bashir, T.

    1996-01-01

    The introduction of solid phase separation techniques is an important improvement in radioimmunoassays and immunoradiometric assays. Magnetic particle solid phase method has additional advantages over others, as the separation is rapid and centrifugation is not required. Three types of magnetic particles have been studied in T 4 RIA and the results have been compared with commercial kits and other established methods. (author). 4 refs, 9 figs, 2 tabs

  7. Three-phase boundary length in solid-oxide fuel cells: A mathematical model

    Janardhanan, Vinod M. [Institutefor Chemical Technology and Polymer Chemistry, University of Karlsruhe (TH), Kaiserstr. 12, D-76128 Karlsruhe (Germany); Heuveline, Vincent; Deutschmann, Olaf [Institute for Applied and Numerical Mathematics, University of Karlsruhe (TH), Kaiserstr. 12, D-76128 Karlsruhe (Germany)

    2008-03-15

    A mathematical model to calculate the volume specific three-phase boundary length in the porous composite electrodes of solid-oxide fuel cell is presented. The model is exclusively based on geometrical considerations accounting for porosity, particle diameter, particle size distribution, and solids phase distribution. Results are presented for uniform particle size distribution as well as for non-uniform particle size distribution. (author)

  8. Two-dimensional solid-phase extraction strategy for the selective enrichment of aminoglycosides in milk.

    Shen, Aijin; Wei, Jie; Yan, Jingyu; Jin, Gaowa; Ding, Junjie; Yang, Bingcheng; Guo, Zhimou; Zhang, Feifang; Liang, Xinmiao

    2017-03-01

    An orthogonal two-dimensional solid-phase extraction strategy was established for the selective enrichment of three aminoglycosides including spectinomycin, streptomycin, and dihydrostreptomycin in milk. A reversed-phase liquid chromatography material (C 18 ) and a weak cation-exchange material (TGA) were integrated in a single solid-phase extraction cartridge. The feasibility of two-dimensional clean-up procedure that experienced two-step adsorption, two-step rinsing, and two-step elution was systematically investigated. Based on the orthogonality of reversed-phase and weak cation-exchange procedures, the two-dimensional solid-phase extraction strategy could minimize the interference from the hydrophobic matrix existing in traditional reversed-phase solid-phase extraction. In addition, high ionic strength in the extracts could be effectively removed before the second dimension of weak cation-exchange solid-phase extraction. Combined with liquid chromatography and tandem mass spectrometry, the optimized procedure was validated according to the European Union Commission directive 2002/657/EC. A good performance was achieved in terms of linearity, recovery, precision, decision limit, and detection capability in milk. Finally, the optimized two-dimensional clean-up procedure incorporated with liquid chromatography and tandem mass spectrometry was successfully applied to the rapid monitoring of aminoglycoside residues in milk. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Solid-Phase Synthesis of PEGylated Lipopeptides Using Click Chemistry

    Jølck, Rasmus Irming; Berg, Rolf Henrik; Andresen, Thomas Lars

    2010-01-01

    A versatile methodology for efficient synthesis of PEGylated lipopeptides via CuAAC “Click” conjugation between alkyne-bearing solid-supported lipopeptides and azido-functionalized PEGs is described. This new and very robust method offers a unique platform for synthesizing PEGylated lipopeptides ...

  10. Phase and Micro-Structural Characterization of Sanitary-Ware Fired at Different Temperature

    ATHER HASSAN; YASEEN IQBAL; SYED ZAFAR ILYAS

    2017-01-01

    The three main ingredients of sanitary-ware are clay, feldspar and quartz. This ware is being widely used and has therefore, attracted the attention of researchers from time to time. Consequently, it has been extensively investigated. The present study describes the phase and micro-structural analysis of sanitary-ware samples collected from local (Durr Ceramics Peshawar) industry. XRD (X-Ray Diffraction) of samples fired at 1100oC reveals the presence of ? ? ? ? ?-quartz and primary mullite o...

  11. Phase transitions of amorphous solid acetone in confined geometry investigated by reflection absorption infrared spectroscopy.

    Shin, Sunghwan; Kang, Hani; Kim, Jun Soo; Kang, Heon

    2014-11-26

    We investigated the phase transformations of amorphous solid acetone under confined geometry by preparing acetone films trapped in amorphous solid water (ASW) or CCl4. Reflection absorption infrared spectroscopy (RAIRS) and temperature-programmed desorption (TPD) were used to monitor the phase changes of the acetone sample with increasing temperature. An acetone film trapped in ASW shows an abrupt change in the RAIRS features of the acetone vibrational bands during heating from 80 to 100 K, which indicates the transformation of amorphous solid acetone to a molecularly aligned crystalline phase. Further heating of the sample to 140 K produces an isotropic solid phase, and eventually a fluid phase near 157 K, at which the acetone sample is probably trapped in a pressurized, superheated condition inside the ASW matrix. Inside a CCl4 matrix, amorphous solid acetone crystallizes into a different, isotropic structure at ca. 90 K. We propose that the molecularly aligned crystalline phase formed in ASW is created by heterogeneous nucleation at the acetone-water interface, with resultant crystal growth, whereas the isotropic crystalline phase in CCl4 is formed by homogeneous crystal growth starting from the bulk region of the acetone sample.

  12. Temperature and phase dependence of positron lifetimes in solid cyclohexane

    Eldrup, Morten Mostgaard

    1985-01-01

    The temperature dependence of position lifetimes in both the brittle and plastic phases of cyclohaxane has been examined. Long-lived components in both phases are associated with the formation of positronium (Ps). Two long lifetimes attributable to ortho-Ps are resolvable in the plastic phase....... The longer of these (≈ 2.5 ns), which is temperature dependent, is ascribed to ortho-Ps trapped at vacancies. The shorter lifetime (≈ 0.9 ns), shows little temperature dependence. In contrast to most other plastic crystals, no sigmoidal behaviour of the average ortho-Ps lifetime is observed. A possibility...

  13. Solid phase transport in series fluidised bed reactors

    Hayes, M.R.

    1980-01-01

    In a multistage counter-current fluidised bed column, fluidised bed material is recycled within each stage and a fraction is continuously withdrawn to the next lower stage at a rate dependent only on the rate of removal of the fluidised bed material from the base of the column. It has a particular application to the ion exchange treatment of liquids containing suspended solids, for example leach solutions from uranium ores. (author)

  14. Formation of soft magnetic high entropy amorphous alloys composites containing in situ solid solution phase

    Wei, Ran; Sun, Huan; Chen, Chen; Tao, Juan; Li, Fushan

    2018-03-01

    Fe-Co-Ni-Si-B high entropy amorphous alloys composites (HEAACs), which containing high entropy solid solution phase in amorphous matrix, show good soft magnetic properties and bending ductility even in optimal annealed state, were successfully developed by melt spinning method. The crystallization phase of the HEAACs is solid solution phase with body centered cubic (BCC) structure instead of brittle intermetallic phase. In addition, the BCC phase can transformed into face centered cubic (FCC) phase with temperature rise. Accordingly, Fe-Co-Ni-Si-B high entropy alloys (HEAs) with FCC structure and a small amount of BCC phase was prepared by copper mold casting method. The HEAs exhibit high yield strength (about 1200 MPa) and good plastic strain (about 18%). Meanwhile, soft magnetic characteristics of the HEAs are largely reserved from HEAACs. This work provides a new strategy to overcome the annealing induced brittleness of amorphous alloys and design new advanced materials with excellent comprehensive properties.

  15. Vapour phase synthesis of salol over solid acids via transesterification

    Administrator

    rate of reactants, WHSV and time-on-stream on the conversion (%) of phenol and selectivity (%) of salol ... Possible reaction mechanisms for the formation of salol and diphenyl ether over ... Hence, vapour-phase conditions of the experiment.

  16. Simulating Solid-Solid Phase Transition in Shape-Memory Alloy Microstructure by Face-Offsetting Method

    Bellur Ramaswamy, Ravi S.; Tortorelli, Daniel A.; Fried, Eliot; Jiao Xiangmin

    2008-01-01

    Advances in the understanding of martensitic transformations (diffusionless, solid-solid phase transformations) have been instrumental to the recent discovery of new low hysteresis alloys. However, some key fundamental issues must be better understood to design still better alloys. Restricting attention to antiplane shear, we use finite element analysis to model the shape-memory alloy microstructure within the Abeyaratne-Knowles continuum thermomechanical framework and use an interface kinetic relation of the kind proposed by Rosakis and Tsai. Geometric singularities and topological changes associated with microstructural evolution pose significant numerical challenges. We address such challenges with a recently developed front-tracking scheme called the face-offsetting method (FOM) to explicitly model phase interfaces. Initial results demonstrate the effectiveness of FOM in resolving needle-like twinned microstructures

  17. Static and dynamic micro deformable mirror characterization by phase-shifting and time-averaged interferometry

    Liotard, Arnaud; Zamkotsian, Frédéric

    2017-11-01

    The micro-opto-electro-mechanical systems (MOEMS), based on mature technologies of micro-electronics, are essential in the design of future astronomical instruments. One of these key-components is the microdeformable mirror for wave-front correction. Very challenging topics like search of exo-planets could greatly benefit from this technology. Design, realization and characterization of micro-Deformable Mirrors are under way at Laboratoire d'Astrophysique de Marseille (LAM) in collaboration with Laboratoire d'Analyse et d'Architecture des Systèmes (LAAS). In order to measure the surface shape and the deformation parameters during operation of these devices, a high-resolution Twyman-Green interferometer has been developed. Measurements have been done on a tiltable micro-mirror (170*100μm2) designed by LAM-LAAS and realized by an American foundry, and also on an OKO deformable mirror (15mm diameter). Static characterization is made by phase shifting interferometry and dynamic measurements have been made by quantitative time-averaged interferometry. The OKO mirror has an actuator stroke of 370+/-10nm for 150V applied and its resonant frequency is 1170+/-50 Hz, and the tiltable mirror has a rotation cut-off frequency of 31+/-3 kHz.

  18. 3H and 125I radioimmunoassays of haloperidol compared with fluoroimmunoassay involving antibody coupled to magnetizable solid phase

    Rowell, F.J.; Hui, S.M.; Kamel, S.R.

    1981-01-01

    Radioimmunoassays for haloperidol are described, involving use of tritium- or 125I-labeled drug or tritium-labeled spiroperidol, and a rabbit antiserum to a drug/bovine serum albumin conjugate. The 125I-labeled drug was prepared by the Chloramine T iodination technique. A fluoroimmunoassay for haloperidol is also described in which the antiserum is coupled to magnetizable solid-phase medium, and fluorescein-labeled haloperidol is used. The assays have acceptable accuracy, precision, and reproducibility, and are specific for haloperidol and similar butyrophenones, with no significant interference from known metabolites and other drugs. Only the radioimmunoassays have sufficient sensitivity to cover the whole range of haloperidol concentrations in serum. The fluoroimmunoassay can be used to monitor high concentrations of haloperidol in 150-microL samples or the complete concentration range of 1-mL serum samples that are extracted and concentrated before assay

  19. Investigation into process of solid-phase synthesis of calcium vanadates

    Fotiev, A.A.; Krasnenko, T.I.; Slobodin, B.V.

    1983-01-01

    Processes of solid-phase synthesis of calcium vanadates by Toubandt method, measuring electric conductivity and Ca 45 and V 48 radioactive indicators are investigated. It is shown that reaction diffusion during calcium vanadates production from oxides is ensured by calcium and oxygen ions or calcium ions and electrons through the product layer, as to oxygen - through the gas phase

  20. Basal plane shift as an order parameter of transitions between antiferromagnetic phases of solid oxygen

    Gomonay, E.V.; Loktev, V.M.

    2005-01-01

    A phenomenological model in the spirit of the Landau theory of phase transitions is derived, and the conditions for existence and phase transitions between different magnetocrystal structures of solid oxygen are analyzed for wide ranges of pressure, temperature and external magnetic field

  1. Practical solid and liquid phase markers for studying gastric emptying in man

    Thomforde, G.M.; Brown, M.L.; Malagelada, J.R.

    1985-01-01

    This paper presents a method used to evaluate solid and liquid phase markers for radionuclide gastric emptying studies. The authors conducted in vitro and in vivo comparative experiments employing several radiolabeled markers. Among the solid phase markers tested, Tc-99m-sulfur colloid in vivo-labeled liver and I-131-fiber performed optimally. However, Tc-99M sulfur colloid in scrambled egg showed very acceptable performance and it is significantly easier to prepare. Among liquid phase markers, they found In-111-DTPA stabilized with 1% albumin to be a good agent and appropriate for dual isotope emptying studies

  2. Solid-Phase Reactions of Iminium Ions: Cyclized Peptide Derivatives

    Wang, Yuanyuan

    formation of N,N’-aminals by nucleophilic attack of the peptide backbone is reversible under strongly acidic conditions and the N,N’-aminal is likely to be the kinetic product of many INCIC reactions. In addition, the N,N’-aminals are stable in the absence of acid but could be converted to the THIQ...... derivatives in solution phase under acid conditions in the presence of an active C-nucleophile in the side chain. The high yielding nature of the aminal formation is confirmed by solution phase synthesis. The introduced azide and alkyne residues in the side chain of N,N’-aminal products were further......BB may undergo auto-oxidation to quinazoline-2,4-diones in the absence of a suitable nucleophile on the side chain or backbone of the peptide (Chapter 4). The structure is confirmed by comparison with products obtained from solution-phase synthesis under the same conditions, one of which was confirmed...

  3. A multi-phase equation of state for solid and liquid lead

    Robinson, C.M.

    2004-01-01

    This paper considers a multi-phase equation of state for solid and liquid lead. The thermodynamically consistent equation of state is constructed by calculating separate equations of state for the solid and liquid phases. The melt curve is the curve in the pressure, temperature plane where the Gibb's free energy of the solid and liquid phases are equal. In each phase a complete equation of state is obtained using the assumptions that the specific heat capacity is constant and that the Grueneisen parameter is proportional to the specific volume. The parameters for the equation of state are obtained from experimental data. In particular they are chosen to match melt curve and principal Hugoniot data. Predictions are made for the shock pressure required for melt to occur on shock and release

  4. Solid-phase microextraction for bioconcentration studies according to OECD TG 305

    Duering, Rolf-Alexander; Boehm, Leonard [Land Use and Nutrition (IFZ) Justus Liebig University Giessen, Institute of Soil Science and Soil Conservation, Research Centre for BioSystems, Giessen (Germany); Schlechtriem, Christian [Fraunhofer Institute for Molecular Biology and Applied Ecology (IME), Schmallenberg (Germany)

    2012-12-15

    An important aim of the European Community Regulation on chemicals and their safe use is the identification of (very) persistent, (very) bioaccumulative, and toxic substances. In other regulatory chemical safety assessments (pharmaceuticals, biocides, pesticides), the identification of such (very) persistent, (very) bioaccumulative, and toxic substances is of increasing importance. Solid-phase microextraction is especially capable of extracting total water concentrations as well as the freely dissolved fraction of analytes in the water phase, which is available for bioconcentration in fish. However, although already well established in environmental analyses to determine and quantify analytes mainly in aqueous matrices, solid-phase microextraction is still a rather unusual method in regulatory ecotoxicological research. Here, the potential benefits and drawbacks of solid-phase microextraction are discussed as an analytical routine approach for aquatic bioconcentration studies according to OECD TG 305, with a special focus on the testing of hydrophobic organic compounds characterized by log K{sub OW}> 5. (orig.)

  5. Solid phase extraction-electrospray ionization mass spectrometric method for the determination of palladium

    Pranaw Kumar; Telmore, Vijay M.; Jaison, P.G.; Sarkar, Arnab; Alamelu, D.; Aggarwal, S.K.

    2015-01-01

    Platinum group of element (PGEs) are extensively used as a catalyst and anticancer reagent. Due to the soft nature of PGEs, sulphur based donar ligands are used for the separation of these elements. Studies on the formation of different species are helpful for obtaining the ideas about separation of these elements from the complex matrices. Palladium (Pd) is studied as a representative element which is also formed by nuclear fission of fissile nuclides. In view of the relatively small amount of solvent required for separation, solid phase extraction is preferred over most of the separation methods. Solid phase extraction method using DPX as a stationary phase was previously reported for the separation of Pd in SHLLW using benzoylthiourea as a ligand. However, in case of large volume samples manual extraction by DPX is tedious task. In the present studies, the feasibility of extraction using benzoylthiourea on automated solid phase extraction system was carried out for the extraction of Pd

  6. Controlled functionalization of carbonaceous fibers for asymmetric solid-state micro-supercapacitors with high volumetric energy density.

    Yu, Dingshan; Goh, Kunli; Zhang, Qiang; Wei, Li; Wang, Hong; Jiang, Wenchao; Chen, Yuan

    2014-10-22

    A 1.8 V asymmetric solid-state flexible micro-supercapacitor is designed with one MnO2 -coated reduced graphene oxide/single-walled carbon nanotube (rGO/SWCNT) composite fiber as positive electrode and one nitrogen-doped rGO/SWCNT fiber as negative electrode, which demonstrates ultrahigh volumetric energy density, comparable to some thin-film lithium batteries, along with high power density, long cycle life, and good flexibility. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Digital holographic setups for phase object measurements in micro and macro scale

    Lédl Vít

    2015-01-01

    Full Text Available The measurement of properties of so called phase objects is being solved for more than one Century starting probably with schlieren technique 1. Classical interferometry served as a great measurement tool for several decades and was replaced by holographic interferometry, which disposes with many benefits when compared to classical interferometry. Holographic interferometry undergone an enormous development in last decade when digital holography has been established as a standard technique and most of the drawbacks were solved. The paper deals with scope of the huge applicability of digital holographic interferometry in heat and mass transfer measurement from micro to macro scale and from simple 2D measurement up to complex tomographic techniques. Recently the very complex experimental setups are under development in our labs combining many techniques leading to digital holographic micro tomography methods.

  8. A molecular dynamics calculation of solid phase of malonic acid

    Recent studies suggest that hydrogen bonds, in particular, hydrogen bond chains play an important role in determining the properties of a substance.We report an investigation into the triclinic phase of crystalline malonic acid. One of two intermolecular interaction potentials proposed here is seen to predict the lattice ...

  9. Solid phase extraction method for determination of mitragynine in ...

    phase high performance liquid chromatography (RP-HPLC) to determine mitragynine (MG) in rat and human urine, and to investigate the influence of caffeine (CF) on urinary excretion of MG in rats. Methods: A two-dimensional wash-elute ...

  10. Solid phase stability of molybdenum under compression: Sound velocity measurements and first-principles calculations

    Zhang, Xiulu [Laboratory for Shock Wave and Detonation Physics Research, Institute of Fluid Physics, P.O. Box 919-102, 621900 Mianyang, Sichuan (China); Laboratory for Extreme Conditions Matter Properties, Southwest University of Science and Technology, 621010 Mianyang, Sichuan (China); Liu, Zhongli [Laboratory for Shock Wave and Detonation Physics Research, Institute of Fluid Physics, P.O. Box 919-102, 621900 Mianyang, Sichuan (China); College of Physics and Electric Information, Luoyang Normal University, 471022 Luoyang, Henan (China); Jin, Ke; Xi, Feng; Yu, Yuying; Tan, Ye; Dai, Chengda; Cai, Lingcang [Laboratory for Shock Wave and Detonation Physics Research, Institute of Fluid Physics, P.O. Box 919-102, 621900 Mianyang, Sichuan (China)

    2015-02-07

    The high-pressure solid phase stability of molybdenum (Mo) has been the center of a long-standing controversy on its high-pressure melting. In this work, experimental and theoretical researches have been conducted to check its solid phase stability under compression. First, we performed sound velocity measurements from 38 to 160 GPa using the two-stage light gas gun and explosive loading in backward- and forward-impact geometries, along with the high-precision velocity interferometry. From the sound velocities, we found no solid-solid phase transition in Mo before shock melting, which does not support the previous solid-solid phase transition conclusion inferred from the sharp drops of the longitudinal sound velocity [Hixson et al., Phys. Rev. Lett. 62, 637 (1989)]. Then, we searched its structures globally using the multi-algorithm collaborative crystal structure prediction technique combined with the density functional theory. By comparing the enthalpies of body centered cubic structure with those of the metastable structures, we found that bcc is the most stable structure in the range of 0–300 GPa. The present theoretical results together with previous ones greatly support our experimental conclusions.

  11. Aluminum Nitride Micro-Channels Grown via Metal Organic Vapor Phase Epitaxy for MEMs Applications

    Rodak, L.E.; Kuchibhatla, S.; Famouri, P.; Ting, L.; Korakakis, D.

    2008-01-01

    Aluminum nitride (AlN) is a promising material for a number of applications due to its temperature and chemical stability. Furthermore, AlN maintains its piezoelectric properties at higher temperatures than more commonly used materials, such as Lead Zirconate Titanate (PZT) [1, 2], making AlN attractive for high temperature micro and nanoelectromechanical (MEMs and NEMs) applications including, but not limited to, high temperature sensors and actuators, micro-channels for fuel cell applications, and micromechanical resonators. This work presents a novel AlN micro-channel fabrication technique using Metal Organic Vapor Phase Epitaxy (MOVPE). AlN easily nucleates on dielectric surfaces due to the large sticking coefficient and short diffusion length of the aluminum species resulting in a high quality polycrystalline growth on typical mask materials, such as silicon dioxide and silicon nitride [3,4]. The fabrication process introduced involves partially masking a substrate with a silicon dioxide striped pattern and then growing AlN via MOVPE simultaneously on the dielectric mask and exposed substrate. A buffered oxide etch is then used to remove the underlying silicon dioxide and leave a free standing AlN micro-channel. The width of the channel has been varied from 5 ìm to 110 ìm and the height of the air gap from 130 nm to 800 nm indicating the stability of the structure. Furthermore, this versatile process has been performed on (111) silicon, c-plane sapphire, and gallium nitride epilayers on sapphire substrates. Reflection High Energy Electron Diffraction (RHEED), Atomic Force Microscopy (AFM), and Raman measurements have been taken on channels grown on each substrate and indicate that the substrate is influencing the growth of the AlN micro-channels on the SiO2 sacrificial layer.

  12. The use of solid sorbents for direct accumulation of organic compounds from water matrices : a review of solid-phase extraction techniques

    Liska, I.; Krupcik, J.; Leclercq, P.A.

    1989-01-01

    The main principles of solid-phase extraction techniques are reviewed in this paper. Various solid sorbents can be used as a suitable trap for direct accumulation of organic compounds from aqueous solutions. The trapped analytes can be desorbed by elution with suitably chosen liquid phases. These

  13. Sequential injection system incorporating a micro extraction column for automatic fractionation of metal ions in solid samples

    Chomchoei, Roongrat; Miró, Manuel; Hansen, Elo Harald

    2005-01-01

    as to the kinetics of the leaching processes and chemical associations in different soil geological phases. Special attention is also paid to the potentials of the microcolumn flowing technique for automatic processing of solid materials with variable homogeneity, as demonstrated with the sewage amended CRM483 soil...

  14. Theoretical study on phase coexistence in ferroelectric solid solutions near the tricritical point

    Lu, Xiaoyan, E-mail: luxy@hit.edu.cn, E-mail: dzk@psu.edu; Li, Hui [Key Lab of Structures Dynamic Behavior and Control of the Ministry of Education, School of Civil Engineering, Harbin Institute of Technology, Harbin 150001 (China); Zheng, Limei [Condensed Matter Science and Technology Institute, Harbin Institute of Technology, Harbin 150001 (China); Cao, Wenwu [Condensed Matter Science and Technology Institute, Harbin Institute of Technology, Harbin 150001 (China); Department of Mathematics and Materials Research Institute, The Pennsylvania State University, University Park, Pennsylvania 16802 (United States)

    2015-04-07

    Phase coexistence in ferroelectric solid solutions near the tricritical point has been theoretically analyzed by using the Landau-Devonshire theory. Results revealed that different phases having similar potential wells could coexist in a narrow composition range near the tricritical point in the classical Pb(Zr{sub 1−x}Ti{sub x})O{sub 3} system. The potential barrier between potential wells increases with the decrease of temperature. Coexisting phases or different domains of the same phase can produce adaptive strains to maintain atomic coherency at the interfaces or domain walls. Such compatibility strains have influence on the energy potential as well as the stability of relative phases, leading to the appearance of energetically unfavorable monoclinic phases. Those competing and coexisting phases also construct an easy phase transition path with small energy barrier in between, so that very small stimuli can produce large response in compositions near the morphotropic phase boundary, especially near the tricritical point.

  15. Theoretical study on phase coexistence in ferroelectric solid solutions near the tricritical point

    Lu, Xiaoyan; Li, Hui; Zheng, Limei; Cao, Wenwu

    2015-01-01

    Phase coexistence in ferroelectric solid solutions near the tricritical point has been theoretically analyzed by using the Landau-Devonshire theory. Results revealed that different phases having similar potential wells could coexist in a narrow composition range near the tricritical point in the classical Pb(Zr 1−x Ti x )O 3 system. The potential barrier between potential wells increases with the decrease of temperature. Coexisting phases or different domains of the same phase can produce adaptive strains to maintain atomic coherency at the interfaces or domain walls. Such compatibility strains have influence on the energy potential as well as the stability of relative phases, leading to the appearance of energetically unfavorable monoclinic phases. Those competing and coexisting phases also construct an easy phase transition path with small energy barrier in between, so that very small stimuli can produce large response in compositions near the morphotropic phase boundary, especially near the tricritical point

  16. New practical algorithm for modelling analyte recovery in bioanalytical reversed phase and mixed-mode solid phase extraction

    Hendriks, G.; Uges, D. R. A.; Franke, J. P.

    2008-01-01

    Solid phase extraction (SPE) is a widely used method for sample cleanup and sample concentration in bioanalytical sample preparation. A few methods to model the retention behaviour on SPE cartridges have been described previously but they are either not applicable to ionised species or are not

  17. Experimental analysis of performance degradation of micro-tubular solid oxide fuel cells fed by different fuel mixtures

    Calise, F.; Restucccia, G.; Sammes, N.

    This paper analyzes the thermodynamic and electrochemical dynamic performance of an anode supported micro-tubular solid oxide fuel cell (SOFC) fed by different types of fuel. The micro-tubular SOFC used is anode supported, consisting of a NiO and Gd 0.2Ce 0.8O 2- x (GDC) cermet anode, thin GDC electrolyte, and a La 0.6Sr 0.4Co 0.2Fe 0.8O 3- y (LSCF) and GDC cermet cathode. The fabrication of the cells under investigation is briefly summarized, with emphasis on the innovations with respect to traditional techniques. Such micro-tubular cells were tested using a Test Stand consisting of: a vertical tubular furnace, an electrical load, a galvanostast, a bubbler, gas pipelines, temperature, pressure and flow meters. The tests on the micro-SOFC were performed using H 2, CO, CH 4 and H 2O in different combinations at 550 °C, to determine the cell polarization curves under several load cycles. Long-term experimental tests were also performed in order to assess degradation of the electrochemical performance of the cell. Results of the tests were analyzed aiming at determining the sources of the cell performance degradation. Authors concluded that the cell under investigation is particularly sensitive to the carbon deposition which significantly reduces cell performance, after few cycles, when fed by light hydrocarbons. A significant performance degradation is also detected when hydrogen is used as fuel. In this case, the authors ascribe the degradation to the micro-cracks, the change in materials crystalline structure and problems with electrical connections.

  18. Fixing arsenic contained in a gas phase using solid hematite

    Balladares, E.; Gonzalez, A.; Rarra, R.; Sanchez, M.

    2004-01-01

    Feasibility to obtain ferric arsenate starting from arsenic containing gas in contact with Fe 3 O 3 has been studied. Thermodynamic stability of the system Fe-As-O was analysed in order to verify conditions to form Fe x As y O z type compounds. Experiments were made using a hematite sample suspended in a thermogravimetric device. As 4 O 6 was generated starting from solid As 2 O 3 which was circulating through the iron oxide. Final samples were analysed chemically and by means of DRX, verifying the formation of FeAsO 4 , FeAsO 4 .2h 2 O and FeAsO 4 .(H 2 O) 2 in small quantities. Tests in porous bed and pellets were carried out, studying the effect of: porosity, temperature and oxygen potential. The largest conversion obtained was 10% at 800 degree centigrade, pO 2 =50% and porosity=0.883. (Author) 9 refs

  19. Solid State KA-Band, Solid State W-Band and TWT Amplifiers, Phase I

    National Aeronautics and Space Administration — Phase I of the proposal describes plans to develop a state of the art transmitter for the W-Band and KA -Band Cloud Radar system. Our focus will be concentrated in...

  20. The synthesis and properties of the phases obtained by solid-solid reactions

    Blonska-Tabero A.

    2008-01-01

    Full Text Available The presented work encompasses the subject of the studies and the results obtained over the last years by the research workers of the Department of Inorganic Chemistry. They include mainly the studies on the reactivity of metal oxides, searching for new phases in binary and ternary systems of metal oxides as well as describing phase relations establishing in such systems. They also encompass works on the extensive characteristics of physico-chemical properties of the newly obtained compounds.

  1. Solid-state phase equilibria in the Fe-Pt-Pr ternary system at 1173 K

    Ren Jing; Gu Zhengfei; Cheng Gang; Zhou Huaiying

    2005-01-01

    The solid-state phase equilibria in the Fe-Pt-Pr ternary system at 1173 K (Pr ≤ 70%) were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersion spectroscopy (EDS) techniques. The 1173 K isothermal section consists of 13 single-phase regions, 22 two-phase regions and 10 three-phase regions. At 1173 K, we have observed that the maximum solid solubility of Pt in α-Fe is below 1.5 at.% and the solid solution region of Pt in γ-Fe is from 2 to 35 at.%; the maximum solid solubility of Fe in Pt is 18 at.%. The maximum solubility of Fe in PrPt 5 , PrPt 3 , PrPt 2 , Pr 3 Pt 4 , PrPt, Pr 3 Pt 2 and Pr 7 Pt 3 is below 1 at.%. The maximum solubility of Pr in α-(Fe, Pt), γ-(Fe, Pt), FePt, FePt 3 and (Pt, Fe) (the solid solution of Fe in Pt) is 6, 2, 4, 4.5 and 1.5 at.%, respectively. In this work, it is found that the phase Pr 3 Pt 4 does not exist in the ternary system. The binary compounds Fe 7 Pr and Fe 2 Pr and any new ternary compounds were not observed

  2. Tetragonal-cubic phase boundary in nanocrystalline ZrO2-Y2O3 solid solutions synthesized by gel-combustion

    Fabregas, Ismael O.; Craievich, Aldo F.; Fantini, Marcia C.A.; Millen, Ricardo P.; Temperini, Marcia L.A.; Lamas, Diego G.

    2011-01-01

    Research highlights: → Gel-combustion synthesis yields compositionally homogeneous, single-phased ZrO 2 -Y 2 O 3 nanopowders, that exhibit the presence at room temperature of three different phases depending on Y 2 O 3 content, namely two tetragonal forms (t' and t'') and the cubic phase. → Phase identification can be achieved by synchrotron XPD (SXPD) and Raman spectroscopy since the tetragonal forms and the cubic phase can be distinguished by these techniques. → The crystallographic features of ZrO 2 -Y 2 O 3 nanopowders were determined by SXPD. They are similar to those reported by Yashima and coworkers for compositionally homogeneous materials containing larger (micro)crystals. However, the lattice parameters are slightly different and the axial ratios c/a of our t' samples are smaller than those reported by these authors. → Compositional t'/t'' and t''/cubic phase boundaries are located at (9 ± 1) and (10.5 ± 0.5) mol% Y 2 O 3 , respectively. → For the whole series of nanocrystalline ZrO 2 -Y 2 O 3 solid solutions studied in the present work, no evidences of the presence of a mixture of phases - as reported by Yashima and coworkers for microcrystalline solid solutions - were detected. - Abstract: By means of synchrotron X-ray powder diffraction (SXPD) and Raman spectroscopy, we have detected, in a series of nanocrystalline and compositionally homogeneous ZrO 2 -Y 2 O 3 solid solutions, the presence at room temperature of three different phases depending on Y 2 O 3 content, namely two tetragonal forms and the cubic phase. The studied materials, with average crystallite sizes within the range 7-10 nm, were synthesized by a nitrate-citrate gel-combustion process. The crystal structure of these phases was also investigated by SXPD. The results presented here indicate that the studied nanocrystalline ZrO 2 -Y 2 O 3 solid solutions exhibit the same phases reported in the literature for compositionally homogeneous materials containing larger (micro

  3. Tetragonal-cubic phase boundary in nanocrystalline ZrO{sub 2}-Y{sub 2}O{sub 3} solid solutions synthesized by gel-combustion

    Fabregas, Ismael O. [CINSO (Centro de Investigaciones en Solidos), CITEFA-CONICET, J.B. de La Salle 4397, 1603 Villa Martelli, Pcia. de Buenos Aires (Argentina); Craievich, Aldo F.; Fantini, Marcia C.A. [Instituto de Fisica, Universidade de Sao Paulo, Travessa R da Rua do Matao, No. 187, Cidade Universitaria, 05508-900 Sao Paulo (Brazil); Millen, Ricardo P.; Temperini, Marcia L.A. [Instituto de Quimica, Universidade de Sao Paulo, Avenida Prof. Lineu Prestes 748, Cidade Universitaria, 05508-900 Sao Paulo (Brazil); Lamas, Diego G., E-mail: dlamas@uncoma.edu.ar [CINSO (Centro de Investigaciones en Solidos), CITEFA-CONICET, J.B. de La Salle 4397, 1603 Villa Martelli, Pcia. de Buenos Aires (Argentina); Laboratorio de Caracterizacion de Materiales, Facultad de Ingenieria, Universidad Nacional del Comahue, Buenos Aires 1400, (8300) Neuquen Capital, Prov. de Neuquen (Argentina)

    2011-04-21

    Research highlights: > Gel-combustion synthesis yields compositionally homogeneous, single-phased ZrO{sub 2}-Y{sub 2}O{sub 3} nanopowders, that exhibit the presence at room temperature of three different phases depending on Y{sub 2}O{sub 3} content, namely two tetragonal forms (t' and t'') and the cubic phase. > Phase identification can be achieved by synchrotron XPD (SXPD) and Raman spectroscopy since the tetragonal forms and the cubic phase can be distinguished by these techniques. > The crystallographic features of ZrO{sub 2}-Y{sub 2}O{sub 3} nanopowders were determined by SXPD. They are similar to those reported by Yashima and coworkers for compositionally homogeneous materials containing larger (micro)crystals. However, the lattice parameters are slightly different and the axial ratios c/a of our t' samples are smaller than those reported by these authors. > Compositional t'/t'' and t''/cubic phase boundaries are located at (9 {+-} 1) and (10.5 {+-} 0.5) mol% Y{sub 2}O{sub 3}, respectively. > For the whole series of nanocrystalline ZrO{sub 2}-Y{sub 2}O{sub 3} solid solutions studied in the present work, no evidences of the presence of a mixture of phases - as reported by Yashima and coworkers for microcrystalline solid solutions - were detected. - Abstract: By means of synchrotron X-ray powder diffraction (SXPD) and Raman spectroscopy, we have detected, in a series of nanocrystalline and compositionally homogeneous ZrO{sub 2}-Y{sub 2}O{sub 3} solid solutions, the presence at room temperature of three different phases depending on Y{sub 2}O{sub 3} content, namely two tetragonal forms and the cubic phase. The studied materials, with average crystallite sizes within the range 7-10 nm, were synthesized by a nitrate-citrate gel-combustion process. The crystal structure of these phases was also investigated by SXPD. The results presented here indicate that the studied nanocrystalline ZrO{sub 2}-Y{sub 2}O{sub 3} solid

  4. Effects of deep cryogenic treatment on the solid-state phase transformation of Cu-Al alloy in cooling process

    Wang, Yuhui; Liao, Bo; Liu, Jianhua; Chen, Shuqing; Feng, Yu; Zhang, Yanyan; Zhang, Ruijun

    2012-07-01

    The solid-state phase transformation temperature and duration of deep cryogenic treated and untreated Cu-Al alloys in cooling process were measured by differential scanning calorimetry measurement. The solid-state phase transformation activation energy and Avrami exponent were calculated according to these measurements. The effects of deep cryogenic treatment on the solid-state phase transformation were investigated based on the measurement and calculation as well as the observation of alloy's microstructure. The results show that deep cryogenic treatment can increase the solid-phase transformation activation energy and shorten the phase transformation duration, which is helpful to the formation of fine grains in Cu-Al alloy.

  5. Electroporation of micro-droplet encapsulated HeLa cells in oil phase

    Xiao, Kang

    2010-08-27

    Electroporation (EP) is a method widely used to introduce foreign genes, drugs or dyes into cells by permeabilizing the plasma membrane with an external electric field. A variety of microfluidic EP devices have been reported so far. However, further integration of prior and posterior EP processes turns out to be very complicated, mainly due to the difficulty of developing an efficient method for precise manipulation of cells in microfluidics. In this study, by means of a T-junction structure within a delicate microfluidic device, we encapsulated HeLa cells in micro-droplet of poration medium in oil phase before EP, which has two advantages: (i) precise control of cell-encapsulating droplets in oil phase is much easier than the control of cell populations or individuals in aqueous buffers; (ii) this can minimize the electrochemical reactions on the electrodes. Finally, we successfully introduced fluorescent dyes into the micro-droplet encapsulated HeLa cells in oil phase. Our results reflected a novel way to realize the integrated biomicrofluidic system for EP. © 2010 Wiley-VCH Verlag GmbH & Co. KGaA.

  6. Phase change material thermal storage for biofuel preheating in micro trigeneration application: A numerical study

    Wu, Dawei; Chen, Junlong; Roskilly, Anthony P.

    2015-01-01

    Highlights: • Engine exhaust heat driven phase change material thermal storage. • Fuel preheating for direct use of straight plant oil on diesel engine. • CFD aided design of the phase change material thermal storage. • Melting and solidification model considering natural convection. - Abstract: A biofuel micro trigeneration prototype has been developed to utilise local energy crop oils as fuel in rural areas and developing countries. Straight plant oils (SPOs) only leave behind very little carbon footprint during its simply production process compared to commercial biodiesels in refineries, but the high viscosity of SPOs causes difficulties at engine cold starts, which further results in poor fuel atomisation, compromised engine performance and fast engine deterioration. In this study, a phase change material (PCM) thermal storage is designed to recover and store engine exhaust heat to preheat SPOs at cold starts. High temperature commercial paraffin is selected as the PCM to meet the optimal preheating temperature range of 70–90 °C, in terms of the SPO property study. A numerical model of the PCM thermal storage is developed and validated by references. The PCM melting and solidification processes with the consideration of natural convection in liquid zone are simulated in ANSYS-FLUENT to verify the feasibility of the PCM thermal storage as a part of the self-contained biofuel micro trigeneration prototype

  7. Nanostructured pillars based on vertically aligned carbon nanotubes as the stationary phase in micro-CEC.

    Wu, Ren-Guei; Yang, Chung-Shi; Wang, Pen-Cheng; Tseng, Fan-Gang

    2009-06-01

    We present a micro-CEC chip carrying out a highly efficient separation of dsDNA fragments through vertically aligned multi-wall carbon nanotubes (MWCNTs) in a microchannel. The vertically aligned MWCNTs were grown directly in the microchannel to form straight nanopillar arrays as ordered and directional chromatographic supports. 1-Pyrenedodecanoic acid was employed for the surface modification of the MWCNTs' stationary phase to adsorb analytes by hydrophobic interactions. This device was used for separating dsDNA fragments of three different lengths (254, 360, and 572 bp), and fluorescence detection was employed to verify the electrokinetic transport in the MWCNT array. The micro-CEC separation of the three compounds was achieved in less than 300 s at a field strength of 66 V/cm due to superior laminar flow patterns and a lower flow resistance resulting from the vertically aligned MWCNTs being used as the stationary phase medium. In addition, a fivefold reduction of band broadening was obtained when the analyte was separated by the chromatographic MWCNT array channel instead of the CE channel. From all of the results, we suggest that an in situ grown and directional MWCNT array can potentially be useful for preparing more diversified forms of stationary phases for vertically efficient chip-based electrochromatography.

  8. Electroporation of micro-droplet encapsulated HeLa cells in oil phase

    Xiao, Kang; Zhang, Mengying; Chen, Shuyu; Wang, Limu; Chang, Donald Choy; Wen, Weijia

    2010-01-01

    Electroporation (EP) is a method widely used to introduce foreign genes, drugs or dyes into cells by permeabilizing the plasma membrane with an external electric field. A variety of microfluidic EP devices have been reported so far. However, further integration of prior and posterior EP processes turns out to be very complicated, mainly due to the difficulty of developing an efficient method for precise manipulation of cells in microfluidics. In this study, by means of a T-junction structure within a delicate microfluidic device, we encapsulated HeLa cells in micro-droplet of poration medium in oil phase before EP, which has two advantages: (i) precise control of cell-encapsulating droplets in oil phase is much easier than the control of cell populations or individuals in aqueous buffers; (ii) this can minimize the electrochemical reactions on the electrodes. Finally, we successfully introduced fluorescent dyes into the micro-droplet encapsulated HeLa cells in oil phase. Our results reflected a novel way to realize the integrated biomicrofluidic system for EP. © 2010 Wiley-VCH Verlag GmbH & Co. KGaA.

  9. Influence of Microencapsulated Phase Change Material (PCM) Addition on (Micro) Mechanical Properties of Cement Paste

    Schlangen, Erik

    2017-01-01

    Excessive cracking can be a serious durability problem for reinforced concrete structures. In recent years, addition of microencapsulated phase change materials (PCMs) to concrete has been proposed as a possible solution to crack formation related to temperature gradients. However, the addition of PCM microcapsules to cementitious materials can have some drawbacks, mainly related to strength reduction. In this work, a range of experimental techniques has been used to characterize the microcapsules and their effect on properties of composite cement pastes. On the capsule level, it was shown that they are spherical, enabling good distribution in the material during the mixing process. Force needed to break the microcapsules was shown to depend on the capsule diameter and the temperature, i.e., whether it is below or above the phase change temperature. On the cement paste level, a marked drop of compressive strength with increasing PCM inclusion level was observed. The indentation modulus has also shown to decrease, probably due to the capsules themselves, and to a lesser extent due to changes in porosity caused by their inclusion. Finally, a novel micro-cube splitting technique was used to characterize the tensile strength of the material on the micro-meter length scale. It was shown that the strength decreases with increasing PCM inclusion percentage, but this is accompanied by a decrease in measurement variability. This study will contribute to future developments of cementitious composites incorporating phase change materials for a variety of applications. PMID:28773225

  10. Structures of the particles of the condensed dispersed phase in solid fuel combustion products plasma

    Samaryan, A.A.; Chernyshev, A.V.; Nefedov, A.P.; Petrov, O.F.; Fortov, V.E.; Mikhailov, Yu.M.; Mintsev, V.B.

    2000-01-01

    The results of experimental investigations of a type of dusty plasma which has been least studied--the plasma of solid fuel combustion products--were presented. Experiments to determine the parameters of the plasma of the combustion products of synthetic solid fuels with various compositions together with simultaneous diagnostics of the degree of ordering of the structures of the particles of the dispersed condensed phase were performed. The measurements showed that the charge composition of the plasma of the solid fuels combustion products depends strongly on the easily ionized alkali-metal impurities which are always present in synthetic fuel in one or another amount. An ordered arrangement of the particles of a condensed dispersed phase in structures that form in a boundary region between the high-temperature and condensation zones was observed for samples of aluminum-coated solid fuels with a low content of alkali-metal impurities

  11. Microwave assisted solid phase extraction for separation preconcentration sulfamethoxazole in wastewater using tyre based activated carbon as solid phase material prior to spectrophotometric determination

    Mogolodi Dimpe, K.; Mpupa, Anele; Nomngongo, Philiswa N.

    2018-01-01

    This work was chiefly encouraged by the continuous consumption of antibiotics which eventually pose harmful effects on animals and human beings when present in water systems. In this study, the activated carbon (AC) was used as a solid phase material for the removal of sulfamethoxazole (SMX) in wastewater samples. The microwave assisted solid phase extraction (MASPE) as a sample extraction method was employed to better extract SMX in water samples and finally the analysis of SMX was done by the UV-Vis spectrophotometer. The microwave assisted solid phase extraction method was optimized using a two-level fractional factorial design by evaluating parameters such as pH, mass of adsorbent (MA), extraction time (ET), eluent ratio (ER) and microwave power (MP). Under optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) were 0.5 μg L- 1 and 1.7 μg L- 1, respectively, and intraday and interday precision expressed in terms of relative standard deviation were > 6%.The maximum adsorption capacity was 138 mg g- 1 for SMX and the adsorbent could be reused eight times. Lastly, the MASPE method was applied for the removal of SMX in wastewater samples collected from a domestic wastewater treatment plant (WWTP) and river water.

  12. Simple material physics experiment for studying phase diagrams and solid state transformations in alloys

    Kaur, S; Kamal, R [Punjabi Univ., Patiala (India). Dept. of Physics

    1977-09-01

    Study of phase diagram and accompanying solid state transformations is essential to determine the best possible composition, manufacturing techniques and physical properties of an alloy. A simple technique having wide applications in metallurgical industry is to study the temperature--time curve of the alloy undergoing cooling with an uniform rate. An experiment which uses this technique is described. It is widely applicable in the fields of materials science, applied solid state physics, physical metallurgy and physical chemistry.

  13. An ordered metallic glass solid solution phase that grows from the melt like a crystal

    Chapman, Karena W.; Chupas, Peter J.; Long, Gabrielle G.; Bendersky, Leonid A.; Levine, Lyle E.; Mompiou, Frédéric; Stalick, Judith K.; Cahn, John W.

    2014-01-01

    We report structural studies of an Al–Fe–Si glassy solid that is a solid solution phase in the classical thermodynamic sense. We demonstrate that it is neither a frozen melt nor nanocrystalline. The glass has a well-defined solubility limit and rejects Al during formation from the melt. The pair distribution function of the glass reveals chemical ordering out to at least 12 Å that resembles the ordering within a stable crystalline intermetallic phase of neighboring composition. Under isothermal annealing at 305 °C the glass first rejects Al, then persists for approximately 1 h with no detectable change in structure, and finally is transformed by a first-order phase transition to a crystalline phase with a structure that is different from that within the glass. It is possible that this remarkable glass phase has a fully ordered atomic structure that nevertheless possesses no long-range translational symmetry and is isotropic

  14. Characterization of rhamnolipids by liquid chromatography/mass spectrometry after solid-phase extraction.

    Behrens, Beate; Engelen, Jeannine; Tiso, Till; Blank, Lars Mathias; Hayen, Heiko

    2016-04-01

    Rhamnolipids are surface-active agents with a broad application potential that are produced in complex mixtures by bacteria of the genus Pseudomonas. Analysis from fermentation broth is often characterized by laborious sample preparation and requires hyphenated analytical techniques like liquid chromatography coupled to mass spectrometry (LC-MS) to obtain detailed information about sample composition. In this study, an analytical procedure based on chromatographic method development and characterization of rhamnolipid sample material by LC-MS as well as a comparison of two sample preparation methods, i.e., liquid-liquid extraction and solid-phase extraction, is presented. Efficient separation was achieved under reversed-phase conditions using a mixed propylphenyl and octadecylsilyl-modified silica gel stationary phase. LC-MS/MS analysis of a supernatant from Pseudomonas putida strain KT2440 pVLT33_rhlABC grown on glucose as sole carbon source and purified by solid-phase extraction revealed a total of 20 congeners of di-rhamnolipids, mono-rhamnolipids, and their biosynthetic precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) with different carbon chain lengths from C8 to C14, including three rhamnolipids with uncommon C9 and C11 fatty acid residues. LC-MS and the orcinol assay were used to evaluate the developed solid-phase extraction method in comparison with the established liquid-liquid extraction. Solid-phase extraction exhibited higher yields and reproducibility as well as lower experimental effort.

  15. Physicomechanical properties of single- and two-phase polycrystalline materials on micro- and macroscopic levels

    Kuksa, L.V.; Arzamaskova, L.M.

    2000-01-01

    The results of studies on elastic and plastic properties of the single- and two-phase polycrystalline materials in dependence on the choice of the consideration scale level are presented. The experimental and theoretical methods, making it possible to study the role of the scale factor by consideration on the micro- and macrolevel and the peculiarities of forming the physicomechanical properties of the material as a whole, are developed. The dependences, characterizing the change of the physicomechanical properties by different scales of consideration, are obtained [ru

  16. Biological nitrate removal from water and wastewater by solid-phase denitrification process.

    Wang, Jianlong; Chu, Libing

    2016-11-01

    Nitrate pollution in receiving waters has become a serious issue worldwide. Solid-phase denitrification process is an emerging technology, which has received increasing attention in recent years. It uses biodegradable polymers as both the carbon source and biofilm carrier for denitrifying microorganisms. A vast array of natural and synthetic biopolymers, including woodchips, sawdust, straw, cotton, maize cobs, seaweed, bark, polyhydroxyalkanoate (PHA), polycaprolactone (PCL), polybutylene succinate (PBS) and polylactic acid (PLA), have been widely used for denitrification due to their good performance, low cost and large available quantities. This paper presents an overview on the application of solid-phase denitrification in nitrate removal from drinking water, groundwater, aquaculture wastewater, the secondary effluent and wastewater with low C/N ratio. The types of solid carbon source, the influencing factors, the microbial community of biofilm attached on the biodegradable carriers, the potential adverse effect, and the cost of denitrification process are introduced and evaluated. Woodchips and polycaprolactone are the popular and competitive natural plant-like and synthetic biodegradable polymers used for denitrification, respectively. Most of the denitrifiers reported in solid-phase denitrification affiliated to the family Comamonadaceae in the class Betaproteobacteria. The members of genera Diaphorobacter, Acidovorax and Simplicispira were mostly reported. In future study, more attention should be paid to the simultaneous removal of nitrate and toxic organic contaminants such as pesticide and PPCPs by solid-phase denitrification, to the elucidation of the metabolic and regulatory relationship between decomposition of solid carbon source and denitrification, and to the post-treatment of the municipal secondary effluent. Solid-phase denitrification process is a promising technology for the removal of nitrate from water and wastewater. Copyright © 2016

  17. Tetraphenylimidodiphosphinate as solid phase extractant for preconcentrative separation of thorium from aqueous solution

    Na Liu; Yanfei Wang; Chuhua He

    2016-01-01

    A simple and reliable method for solid phase extraction of thorium using tetraphenylimidodiphosphinate is presented. The solid phase extraction process was optimized at equilibrium time 3 h, pH = 4.5, initial concentration 30 mg L -1 and extractant dosage 0.01 g with 98.95 % of removal efficiency and 29.68 mg g -1 of adsorption capacity. The interfering ions experiments indicated that it had almost no effect on thorium adsorption. Kinetics data follow the pseudo-first-order model and equilibrium data agreed with the Langmuir isotherm model very well. FT-IR analysis indicated that imino group and phosphoryl acted as the significant roles in the solid phase extraction process. (author)

  18. Solid-phase route to Fmoc-protected cationic amino acid building blocks

    Clausen, Jacob Dahlqvist; Linderoth, Lars; Nielsen, Hanne Mørck

    2012-01-01

    Diamino acids are commonly found in bioactive compounds, yet only few are commercially available as building blocks for solid-phase peptide synthesis. In the present work a convenient, inexpensive route to multiple-charged amino acid building blocks with varying degree of hydrophobicity...... was developed. A versatile solid-phase protocol leading to selectively protected amino alcohol intermediates was followed by oxidation to yield the desired di- or polycationic amino acid building blocks in gram-scale amounts. The synthetic sequence comprises loading of (S)-1-(p-nosyl)aziridine-2-methanol onto...... of simple neutral amino acids as well as analogs displaying high bulkiness or polycationic side chains was prepared. Two building blocks were incorporated into peptide sequences using microwave-assisted solid-phase peptide synthesis confirming their general utility....

  19. NASA satellite communications application research. Phase 2: Efficient high power, solid state amplifier for EFH communications

    Benet, James

    1993-01-01

    The final report describes the work performed from 9 Jun. 1992 to 31 Jul. 1993 on the NASA Satellite Communications Application Research (SCAR) Phase 2 program, Efficient High Power, Solid State Amplifier for EHF Communications. The purpose of the program was to demonstrate the feasibility of high-efficiency, high-power, EHF solid state amplifiers that are smaller, lighter, more efficient, and less costly than existing traveling wave tube (TWT) amplifiers by combining the output power from up to several hundred solid state amplifiers using a unique orthomode spatial power combiner (OSPC).

  20. Possible superconductivity in the Bismuth IV solid phase under pressure.

    Valladares, Ariel A; Rodríguez, Isaías; Hinojosa-Romero, David; Valladares, Alexander; Valladares, Renela M

    2018-04-13

    The first successful theory of superconductivity was the one proposed by Bardeen, Cooper and Schrieffer in 1957. This breakthrough fostered a remarkable growth of the field that propitiated progress and questionings, generating alternative theories to explain specific phenomena. For example, it has been argued that Bismuth, being a semimetal with a low number of carriers, does not comply with the basic hypotheses underlying BCS and therefore a different approach should be considered. Nevertheless, in 2016 based on BCS we put forth a prediction that Bi at ambient pressure becomes a superconductor at 1.3 mK. A year later an experimental group corroborated that in fact Bi is a superconductor with a transition temperature of 0.53 mK, a result that eluded previous work. So, since Bi is superconductive in almost all the different structures and phases, the question is why Bi-IV has been elusive and has not been found yet to superconduct? Here we present a study of the electronic and vibrational properties of Bi-IV and infer its possible superconductivity using a BCS approach. We predict that if the Bi-IV phase structure were cooled down to liquid helium temperatures it would also superconduct at a T c of 4.25 K.

  1. Determination of polycyclic aromatic hydrocarbons in drinking water samples by solid-phase nanoextraction and high-performance liquid chromatography.

    Wang, Huiyong; Campiglia, Andres D

    2008-11-01

    A novel alternative is presented for the extraction and preconcentration of polycyclic aromatic hydrocarbons (PAH) from water samples. The new approachwhich we have named solid-phase nanoextraction (SPNE)takes advantage of the strong affinity that exists between PAH and gold nanoparticles. Carefully optimization of experimental parameters has led to a high-performance liquid chromatography method with excellent analytical figures of merit. Its most striking feature correlates to the small volume of water sample (500 microL) for complete PAH analyses. The limits of detection ranged from 0.9 (anthracene) to 58 ng.L (-1) (fluorene). The relative standard deviations at medium calibration concentrations vary from 3.2 (acenaphthene) to 9.1% (naphthalene). The analytical recoveries from tap water samples of the six regulated PAH varied from 83.3 +/- 2.4 (benzo[ k]fluoranthene) to 95.7 +/- 4.1% (benzo[ g,h,i]perylene). The entire extraction procedure consumes less than 100 microL of organic solvents per sample, which makes it environmentally friendly. The small volume of extracting solution makes SPNE a relatively inexpensive extraction approach.

  2. Single-phase heat transfer enhancement in micro/minichannels using nanofluids: Theory and applications

    Hussien, Ahmed A.; Abdullah, Mohd Z.; Al-Nimr, Moh’d A.

    2016-01-01

    Highlights: • Review recent experimental and numerical studies on heat transfer in micro/minichannels and nanofluids. • Display the new applications of using nanofluids and micro/minichannels to enhance thermal performance. • Explain the factors affecting the thermal conductivity enhancement ratio of nanofluids. • The challenges of using the mini/microchannels and nanofluids. - Abstract: New cooling techniques are being explored for the dissipation of heat fluxes. Many recent studies on heat transfer in micro/minichannels (M/MCs) with nanofluids have focused on combining the advantages of both, for the purpose of obtaining higher single-phase enhancement of heat transfer. Developing of many applications such as cooling electronic device, solar cell, and automotive technology is highly demanded now a day to obtain high efficiency and reduce the operating cost. This review article summarizes recent studies, with a focus on two main topics: The first part contains the main concepts such as scaling effects of M/MCs, physical properties and convective heat transfer. The second part displays the main recent applications of M/MCs with nanofluids with the challenges to be widely used. The purpose of this article to provide exhaustive and comprehensive review of updated works published in this new area, with general conclusions.

  3. Micro-Encapsulated Phase Change Materials: A Review of Encapsulation, Safety and Thermal Characteristics

    Ahmed Hassan

    2016-10-01

    Full Text Available Phase change materials (PCMs have been identified as potential candidates for building energy optimization by increasing the thermal mass of buildings. The increased thermal mass results in a drop in the cooling/heating loads, thus decreasing the energy demand in buildings. However, direct incorporation of PCMs into building elements undermines their structural performance, thereby posing a challenge for building integrity. In order to retain/improve building structural performance, as well as improving energy performance, micro-encapsulated PCMs are integrated into building materials. The integration of microencapsulation PCMs into building materials solves the PCM leakage problem and assures a good bond with building materials to achieve better structural performance. The aim of this article is to identify the optimum micro-encapsulation methods and materials for improving the energy, structural and safety performance of buildings. The article reviews the characteristics of micro-encapsulated PCMs relevant to building integration, focusing on safety rating, structural implications, and energy performance. The article uncovers the optimum combinations of the shell (encapsulant and core (PCM materials along with encapsulation methods by evaluating their merits and demerits.

  4. Soft x-ray induced femtosecond solid-to-solid phase transition

    Tavella, F.; Höppner, H.; Tkachenko, V.; Medvedev, Nikita; Capotondi, F.; Golz, T.; Kai, Y.; Manfredda, M.; Pedersoli, E.; Prandolini, M.J.; Stojanovic, N.; Tanikawa, T.; Teubner, U.; Toleikis, S.; Ziaja, B.

    Roč. 24, Sep (2017), s. 22-27 ISSN 1574-1818 Institutional support: RVO:68378271 Keywords : soft x-ray * ultrashort x-ray pulses * grafitization of diamond * non-thermal phase transition Subject RIV: BL - Plasma and Gas Discharge Physics OBOR OECD: Fluids and plasma physics (including surface physics) Impact factor: 0.908, year: 2016

  5. Liquid-phase microextraction and fibre-optics-based cuvetteless CCD-array micro-spectrophotometry for trace analysis

    Sharma, Nisha; Pillai, Aradhana K.K.V.; Pathak, Neeraj; Jain, Archana; Verma, Krishna K.

    2009-01-01

    Liquid-phase microextraction (LPME) has been investigated for trace analysis in the present work in conjunction with fibre-optic-based micro-spectrophotometry which accommodates sample volume of 1 μL placed between the two ends of optical fibres. Methods have been evolved for the determination of (i) 1-100 μM and 0.5-20 μM of thiols by single drop microextraction (SDME) and LPME in 25 μL of the organic solvent, respectively, involving their reaction with the Ellman reagent and ion pair microextraction of thiolate ion formed; (ii) 70 μg to 7 mg L -1 of chlorine/chlorine dioxide by headspace in-drop reaction with alternative reagents, viz., mixed phenylhydrazine-4-sulphonic acid and N-(1-naphthyl)ethylenediamine dihydrochloride, o-dianisidine, o-tolidine, and N,N-diethyl-p-phenylenediamine; (iii) 0.2-4 mg L -1 of ammonia by reaction with 2,4-dinitro-1-fluorobenzene to give 2,4-dinitroaniline which was diazotized and coupled with 1-naphthylamine, the resulting dye was subjected to preconcentration by solid-phase extraction and LPME; and (iv) 25-750 μg L -1 of iodide/total iodine by oxidation of iodide by 2-iodosobenzoate, microextraction of iodine in organic solvent, and re-extraction into aqueous starch-iodide reagent drop held in the organic phase. LPME using 25-30 μL of organic solvent was found to produce more sensitive results than SDME. The cuvetteless spectrophotometry as used in combination with sample handling techniques produced limits of detection of analytes which were better than obtained by previously reported spectrophotometry.

  6. A novel deep reactive ion etched (DRIE) glass micro-model for two-phase flow experiments.

    Karadimitriou, N K; Joekar-Niasar, V; Hassanizadeh, S M; Kleingeld, P J; Pyrak-Nolte, L J

    2012-09-21

    In the last few decades, micro-models have become popular experimental tools for two-phase flow studies. In this work, the design and fabrication of an innovative, elongated, glass-etched micro-model with dimensions of 5 × 35 mm(2) and constant depth of 43 microns is described. This is the first time that a micro-model with such depth and dimensions has been etched in glass by using a dry etching technique. The micro-model was visualized by a novel setup that allowed us to monitor and record the distribution of fluids throughout the length of the micro-model continuously. Quasi-static drainage experiments were conducted in order to obtain equilibrium data points that relate capillary pressure to phase saturation. By measuring the flow rate of water through the flow network for known pressure gradients, the intrinsic permeability of the micro-model's flow network was also calculated. The experimental results were used to calibrate a pore-network model and test its validity. Finally, we show that glass-etched micro-models can be valuable tools in single and/or multi-phase flow studies and their applications.

  7. Study of colloids transport during two-phase flow using a novel polydimethylsiloxane micro-model.

    Zhang, Qiulan; Karadimitriou, N K; Hassanizadeh, S M; Kleingeld, P J; Imhof, A

    2013-07-01

    As a representation of a porous medium, a closed micro-fluidic device made of polydimethylsiloxane (PDMS), with uniform wettability and stable hydrophobic properties, was designed and fabricated. A flow network, with a mean pore size of 30 μm, was formed in a PDMS slab, covering an area of 1 mm × 10 mm. The PDMS slab was covered and bonded with a 120-μm-thick glass plate to seal the model. The glass plate was first spin-coated with a thin layer, roughly 10 μm, of PDMS. The micro-model was treated with silane in order to make it uniformly and stably hydrophobic. Fluorescent particles of 300 μm in diameter were used as colloids. It is known that more removal of colloids occurs under unsaturated conditions, compared to saturated flow in soil. At the same time, the change of saturation has been observed to cause remobilization of attached colloids. The mechanisms for these phenomena are not well understood. This is the first time that a closed micro-model, made of PDMS with uniform and stable wettability, has been used in combination with confocal microscopy to study colloid transport under transient two-phase flow conditions. With confocal microscopy, the movement of fluorescent particles and flow of two liquids within the pores can be studied. One can focus at different depths within the pores and thus determine where the particles exactly are. Thus, remobilization of attached colloids by moving fluid-fluid interfaces was visualized. In order to allow for the deposition and subsequent remobilization of colloids during two-phase flow, three micro-channels for the injection of liquids with and without colloids were constructed. An outlet channel was designed where effluent concentration breakthrough curves can be quantified by measuring the fluorescence intensity. A peak concentration also indicated in the breakthrough curve with the drainage event. The acquired images and breakthrough curve successfully confirmed the utility of the combination of such a PDMS

  8. Finite element modeling for integrated solid-solid PCM-building material with varying phase change temperatures

    Zhang, D.; Fung, A.S.; Siddiqui, O. [Ryerson Polytechnic Univ., Toronto, ON (Canada). Dept. of Mechanical and Industrial Engineering

    2008-08-15

    Solid-solid phase change materials (SSPCMs) are used to enhance thermal storage performance and reduce indoor temperature fluctuations in buildings. In this study, a finite element model (FEM) was used to investigate the thermal properties of different types of SSPCMs. An effective heat capacity method was used to develop the model. An integrated PCM-building material was analyzed in relation to temperature and heat flux profiles. Governing equations for the heat transfer process were composed of Navier-Stokes momentum equations; a mass conservation equation; and an energy conservation equation. Effective heat capacity was described as a linear function of the latent heat of fusion on both the heating and cooling processes. Data from the simulation were then compared with an experiment suing drywall, concrete and gypcrete samples. Heat flux across the surfaces and temperatures on the surfaces of the materials were measured. Data were used to validate the finite element model (FEM). Results of the study suggested that heat flux profiles are an effective means of understanding phase change processes. It was concluded that PCMs with lower phase change temperatures lengthened energy releases and improved thermal comfort in the building. 12 refs., 2 tabs., 14 figs.

  9. Finite-deformation phase-field chemomechanics for multiphase, multicomponent solids

    Svendsen, Bob; Shanthraj, Pratheek; Raabe, Dierk

    2018-03-01

    The purpose of this work is the development of a framework for the formulation of geometrically non-linear inelastic chemomechanical models for a mixture of multiple chemical components diffusing among multiple transforming solid phases. The focus here is on general model formulation. No specific model or application is pursued in this work. To this end, basic balance and constitutive relations from non-equilibrium thermodynamics and continuum mixture theory are combined with a phase-field-based description of multicomponent solid phases and their interfaces. Solid phase modeling is based in particular on a chemomechanical free energy and stress relaxation via the evolution of phase-specific concentration fields, order-parameter fields (e.g., related to chemical ordering, structural ordering, or defects), and local internal variables. At the mixture level, differences or contrasts in phase composition and phase local deformation in phase interface regions are treated as mixture internal variables. In this context, various phase interface models are considered. In the equilibrium limit, phase contrasts in composition and local deformation in the phase interface region are determined via bulk energy minimization. On the chemical side, the equilibrium limit of the current model formulation reduces to a multicomponent, multiphase, generalization of existing two-phase binary alloy interface equilibrium conditions (e.g., KKS). On the mechanical side, the equilibrium limit of one interface model considered represents a multiphase generalization of Reuss-Sachs conditions from mechanical homogenization theory. Analogously, other interface models considered represent generalizations of interface equilibrium conditions consistent with laminate and sharp-interface theory. In the last part of the work, selected existing models are formulated within the current framework as special cases and discussed in detail.

  10. A Photolabile Linker for the Solid-Phase Synthesis of Peptide Hydrazides and Heterocycles

    Qvortrup, Katrine; Komnatnyy, Vitaly V.; Nielsen, Thomas Eiland

    2014-01-01

    A photolabile hydrazine linker for the solid-phase synthesis of peptide hydrazides and hydrazine-derived heterocycles is presented. The developed protocols enable the efficient synthesis of structurally diverse peptide hydrazides derived from the standard amino adds, including those with side......-chain protected residues at the C-terminal of the resulting peptide hydrazide, and are useful for the synthesis of dihydropyrano[2,3-c]pyrazoles. The linker is compatible with most commonly used coupling reagents and protecting groups for solid-phase peptide synthesis....

  11. Solid-phase extraction and determination of trace elements in environmental samples using naphthalene adsorbent

    Pourreza, N.

    2004-01-01

    Naphthalene co-precipitated with quaternary ammonium salt such as tetraoctyl ammonium bromide and methyltrioctyl ammonium chloride have been used as adsorbent for solid phase extraction of metal ions such as Hg, Cd and Fe. The metal ions are retained on the adsorbent in a column as their complexes with suitable ligands and eluted by an eluent before instrumental measurements. The optimization of the procedures for solid phase extraction and consequent determination of trace elements and application to environmental samples especially water samples will be discussed. (author)

  12. Differing results of direct and indirect solid phase radioimmunoassay for HBsAg in acute hepatitis

    Strohm, W.D.; Legler, K.; Gerlich, W.; Stamm, B.; Zimmer, S.; Biotest-Serum-Institut G.m.b.H., Frankfurt am Main; Goettingen Univ.

    1978-01-01

    In 54 patients suffering from active viral hepatitis the indirect solid phase radioimmunoassay (ind-SPRIA) for HBsAg was positive in 9 cases the direct solid phase radioimmunoassay (d-SPRIA) being negative. In 2 further cases ind-SPRIA was positive during several weeks but d-SPRIA only once. AntiHBc could be detected in 9 of these patients. In 7 patients the usual decrease of the transaminase activity was followed by a second elavation with prolongation of the disease. The unknown factor detected by ind-SPRIA suggests a special of acute hepatitis. (orig.) [de

  13. Numerical simulation analysis of four-stage mutation of solid-liquid two-phase grinding

    Li, Junye; Liu, Yang; Hou, Jikun; Hu, Jinglei; Zhang, Hengfu; Wu, Guiling

    2018-03-01

    In order to explore the numerical simulation of solid-liquid two-phase abrasive grain polishing and abrupt change tube, in this paper, the fourth order abrupt change tube was selected as the research object, using the fluid mechanics software to simulate,based on the theory of solid-liquid two-phase flow dynamics, study on the mechanism of AFM micromachining a workpiece during polishing.Analysis at different inlet pressures, the dynamic pressure distribution pipe mutant fourth order abrasive flow field, turbulence intensity, discuss the influence of the inlet pressure of different abrasive flow polishing effect.

  14. Differing results of direct and indirect solid phase radioimmunoassay for HBsAg in acute hepatitis

    Strohm, W D; Legler, K; Gerlich, W; Stamm, B; Zimmer, S [Frankfurt Univ. (Germany, F.R.). Abt. fuer Gastroenterologie; Biotest-Serum-Institut G.m.b.H., Frankfurt am Main (Germany, F.R.); Goettingen Univ. (Germany, F.R.). Hygiene-Institut)

    1978-09-01

    In 54 patients suffering from active viral hepatitis the indirect solid phase radioimmunoassay (ind-SPRIA) for HBsAg was positive in 9 cases the direct solid phase radioimmunoassay (d-SPRIA) being negative. In 2 further cases ind-SPRIA was positive during several weeks but d-SPRIA only once. AntiHBc could be detected in 9 of these patients. In 7 patients the usual decrease of the transaminase activity was followed by a second elavation with prolongation of the disease. The unknown factor detected by ind-SPRIA suggests a special of acute hepatitis.

  15. Use of the 2-chlorotrityl chloride resin for microwave-assisted solid phase peptide synthesis.

    Ieronymaki, Matthaia; Androutsou, Maria Eleni; Pantelia, Anna; Friligou, Irene; Crisp, Molly; High, Kirsty; Penkman, Kirsty; Gatos, Dimitrios; Tselios, Theodore

    2015-09-01

    A fast and efficient microwave (MW)-assisted solid-phase peptide synthesis protocol using the 2-chlorotrityl chloride resin and the Fmoc/tBu methodology, has been developed. The established protocol combines the advantages of MW irradiation and the acid labile 2-chlorotrityl chloride resin. The effect of temperature during the MW irradiation, the degree of resin substitution during the coupling of the first amino acids and the rate of racemization for each amino acid were evaluated. The suggested solid phase methodology is applicable for orthogonal peptide synthesis and for the synthesis of cyclic peptides. © 2015 Wiley Periodicals, Inc.

  16. Modeling of Thermal Phase Noise in a Solid Core Photonic Crystal Fiber-Optic Gyroscope.

    Song, Ningfang; Ma, Kun; Jin, Jing; Teng, Fei; Cai, Wei

    2017-10-26

    A theoretical model of the thermal phase noise in a square-wave modulated solid core photonic crystal fiber-optic gyroscope has been established, and then verified by measurements. The results demonstrate a good agreement between theory and experiment. The contribution of the thermal phase noise to the random walk coefficient of the gyroscope is derived. A fiber coil with 2.8 km length is used in the experimental solid core photonic crystal fiber-optic gyroscope, showing a random walk coefficient of 9.25 × 10 -5 deg/√h.

  17. The Chemistry, Crystallization, Physicochemical Properties and Behavior of Sodium Aluminosilicate Solid Phases: Final Report

    Rosencrance, S.

    2003-01-01

    The synthesis of sodium aluminosilicate solids phases precipitated from NO 2 /NO 3 -free and NO 2 /NO 3 -rich liquors has been performed. Four sodium aluminosilicate precipitation products were formed. These are (1) X-ray/electron diffraction-indifferent amorphous phase; (2) crystalline zeolite A; (3)NO 2 /NO 3 -rich crystalline sodalite; and (4) NO 2 /NO 3 -rich crystalline cancrinite phase. Characterization of the physicochemical properties for these phases has been performed under conditions simulating Westinghouse Savannah River Company liquid waste processing

  18. Mechanism and microstructures in Ga2O3 pseudomartensitic solid phase transition.

    Zhu, Sheng-Cai; Guan, Shu-Hui; Liu, Zhi-Pan

    2016-07-21

    Solid-to-solid phase transition, although widely exploited in making new materials, challenges persistently our current theory for predicting its complex kinetics and rich microstructures in transition. The Ga2O3α-β phase transformation represents such a common but complex reaction with marked change in cation coordination and crystal density, which was known to yield either amorphous or crystalline products under different synthetic conditions. Here we, via recently developed stochastic surface walking (SSW) method, resolve for the first time the atomistic mechanism of Ga2O3α-β phase transformation, the pathway of which turns out to be the first reaction pathway ever determined for a new type of diffusionless solid phase transition, namely, pseudomartensitic phase transition. We demonstrate that the sensitivity of product crystallinity is caused by its multi-step, multi-type reaction pathway, which bypasses seven intermediate phases and involves all types of elementary solid phase transition steps, i.e. the shearing of O layers (martensitic type), the local diffusion of Ga atoms (reconstructive type) and the significant lattice dilation (dilation type). While the migration of Ga atoms across the close-packed O layers is the rate-determining step and yields "amorphous-like" high energy intermediates, the shearing of O layers contributes to the formation of coherent biphase junctions and the presence of a crystallographic orientation relation, (001)α//(201[combining macron])β + [120]α//[13[combining macron]2]β. Our experiment using high-resolution transmission electron microscopy further confirms the theoretical predictions on the atomic structure of biphase junction and the formation of (201[combining macron])β twin, and also discovers the late occurrence of lattice expansion in the nascent β phase that grows out from the parent α phase. By distinguishing pseudomartensitic transition from other types of mechanisms, we propose general rules to predict the

  19. Flipping interferometry and its application for quantitative phase microscopy in a micro-channel.

    Roitshtain, Darina; Turko, Nir A; Javidi, Bahram; Shaked, Natan T

    2016-05-15

    We present a portable, off-axis interferometric module for quantitative phase microscopy of live cells, positioned at the exit port of a coherently illuminated inverted microscope. The module creates on the digital camera an interference pattern between the image of the sample and its flipped version. The proposed simplified module is based on a retro-reflector modification in an external Michelson interferometer. The module does not contain any lenses, pinholes, or gratings and its alignment is straightforward. Still, it allows full control of the off-axis angle and does not suffer from ghost images. As experimentally demonstrated, the module is useful for quantitative phase microscopy of live cells rapidly flowing in a micro-channel.

  20. Thermal Response Of An Aerated Concrete Wall With Micro-Encapsulated Phase Change Material

    Halúzová, Dušana

    2015-06-01

    For many years Phase Change Materials (PCM) have attracted attention due to their ability to store large amounts of thermal energy. This property makes them a candidate for the use of passive heat storage. In many applications, they are used to avoid the overheating of the temperature of an indoor environment. This paper describes the behavior of phase change materials that are inbuilt in aerated concrete blocks. Two building samples of an aerated concrete wall were measured in laboratory equipment called "twin-boxes". The first box consists of a traditional aerated concrete wall; the second one has additional PCM micro-encapsulated in the wall. The heat flux through the wall was measured and compared to simulation results modeled in the ESP-r program. This experimental measurement provides a foundation for a model that can be used to analyze further building constructions.

  1. Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.

    Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

    2013-12-20

    Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including practical applications of these techniques and a critical discussion about their advantages and disadvantages. The proposed solutions fulfill the requirements resulting from the concept of sustainable development, and specifically from the implementation of green chemistry principles in analytical laboratories. Therefore, particular attention was paid to the description of possible uses of novel, selective stationary phases in extraction techniques, inter alia, polymeric ionic liquids, carbon nanotubes, and silica- and carbon-based sorbents. The methodological solutions, together with properly matched sampling devices for collecting analytes from samples with varying matrix composition, enable us to reduce the number of errors during the sample preparation prior to chromatographic analysis as well as to limit the negative impact of this analytical step on the natural environment and the health of laboratory employees. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. [Determination of patulin in fruits and jam by solid phase extraction-ultra performance liquid chromatography].

    Lü, Weichao; Shen, Shuchang; Wang, Chao

    2017-11-08

    With magnesium silicate, silica gel, diatomite and calcium sulfate as raw materials, a new solid phase extraction column was prepared through a series of processes of grinding to ethanol homogenate, drying and packing into polypropylene tube. The sample was hydrolyzed by pectinase, extracted by acetonitrile and purified by solid phase extraction. The target compounds were separated on a C18 column (100 mm×2.1 mm, 1.8 μm), using 0.8% (v/v) tetrahydrofuran solution as mobile phase with a flow rate of 0.5 mL/min. The detection wavelength was 276 nm. The effect of pectinase on extraction yield and purification effect of solid-phase extraction column were investigated. The optimum chromatographic conditions were selected. There was a good linear relationship between the peak heights and the mass concentrations of patulin in the range of 0.1 to 10 mg/L with the correlation coefficient ( R 2 ) of 1. The limit of detection for this method was 10.22 μg/kg. The spiked recoveries of samples were 86.58%-94.84% with the relative standard deviations (RSDs) of 1.45%-2.28%. The results indicated that the self-made solid phase extraction column had a good purification efficiency, and the UPLC had a high separation efficiency. The method is simple, accurate and of great significance for the quality and safety control of fruit products.

  3. Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction of herbicides in peanuts.

    Li, Na; Wang, Zhibing; Zhang, Liyuan; Nian, Li; Lei, Lei; Yang, Xiao; Zhang, Hanqi; Yu, Aimin

    2014-10-01

    Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction was developed and applied to the extraction of pesticides in high fatty matrices. The herbicides were ultrasonically extracted from peanut using ethyl acetate as extraction solvent. The separation of the analytes from a large amount of co-extractive fat was achieved by dispersive solid-phase extraction using MIL-101(Cr) as sorbent. In this step, the analytes were adsorbed on MIL-101(Cr) and the fat remained in bulk. The herbicides were separated and determined by high-performance liquid chromatography. The experimental parameters, including type and volume of extraction solvent, ultrasonication time, volume of hexane and eluting solvent, amount of MIL-101(Cr) and dispersive solid phase extraction time, were optimized. The limits of detection for herbicides range from 0.98 to 1.9 μg/kg. The recoveries of the herbicides are in the range of 89.5-102.7% and relative standard deviations are equal or lower than 7.0%. The proposed method is simple, effective and suitable for treatment of the samples containing high content of fat. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Effect of applied voltage on phase components of composite coatings prepared by micro-arc oxidation

    Zhu, Wenjun [Department of Prosthodontics, Guanghua School of Stomatology, Sun Yat-sen University, Guangzhou 510055 (China); Fang, Yu-Jing [Department of Colorectal Surgery, State Key Laboratory of Oncology in South China, Sun Yat-sen University Cancer Center, Guangzhou 510060 (China); Zheng, Huade [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641 (China); Tan, Guoxin [Guangdong University of Technology, Guangdong Province 510006 (China); Cheng, Haimei [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641 (China); Ning, Chengyun, E-mail: imcyning@scut.edu.cn [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641 (China)

    2013-10-01

    In this report, we present results from our experiments on composite coatings formed on biomedical titanium substrates by micro-arc oxidation (MAO) in constant-voltage mode. The coatings were prepared on the substrates in an aqueous electrolyte containing calcium acetate and β-glycerol phosphate disodium salt pentahydrate (β-GP). We analyzed the element distribution and phase components of the coatings prepared at different voltages by X-ray diffraction, thin-coating X-ray diffraction, electron-probe microanalysis, and Fourier-transform infrared spectroscopy. The results show that the composite coatings formed at 500 V consist of titania (TiO{sub 2}), hydroxylapatite (HA), and calcium carbonate (CaCO{sub 3}). Furthermore, the concentration of Ca, P, and Ti gradually changes with increasing applied voltage, and the phase components of the composite coatings gradually change from the bottom of the coating to the top: the bottom layer consists of TiO{sub 2}, the middle layer consists of TiO{sub 2} and HA, and the top layer consists of HA and a small amount of CaCO{sub 3}. The formation of HA directly on the coating surface by MAO technique can greatly enhance the surface bioactivity. - Highlights: • Coatings prepared on biomedical titanium substrate by micro-arc oxidation • Coatings composed of titania, hydroxyapatite and calcium carbonate • Hydroxyapatite on the coating surface can enhance the surface bioactivity.

  5. Solid solution and amorphous phase in Ti–Nb–Ta–Mn systems synthesized by mechanical alloying

    Aguilar, C., E-mail: claudio.aguilar@usm.cl [Departamento de Ingeniería Metalúrgica y Materiales, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Guzman, P. [Departamento de Ingeniería Metalúrgica y Materiales, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Lascano, S. [Departamento de Ingeniería Mecánica, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Parra, C. [Departamento de Física, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Bejar, L. [Instituto de Investigaciones Metalúrgicas, Universidad Michoacana de San Nicolás de Hidalgo, Ciudad Universitaria, Morelia C.P. 58000, Michoacán (Mexico); Medina, A. [Facultad de Ingeniería Mecánica, Universidad Michoacana de San Nicolás de Hidalgo, Ciudad Universitaria, C.P. 58000, Michoacán (Mexico); Guzman, D. [Departamento de Metalurgia, Universidad de Atacama, Av. España 485, Copiapó (Chile)

    2016-06-15

    This work discusses the formation of Ti–30Nb–13Ta–xMn (x: 2, 4 and 6 wt%) solid solution by mechanical alloying using a shaker mill. A solid solution was formed after 15 h of milling and an amorphous phase was formed after 30 h of milling, according to X-ray diffraction results. Disappearance of strongest X-ray diffraction peaks of Nb, Ta and Mn indicated the formation of solid solution, while, X-ray diffraction patterns of powders milled for 30 h showed an amorphous hump with crystalline peaks in the angular range of 35–45° in 2θ. TEM image analysis showed the presence of nanocrystalline intermetallic compounds embedded in an amorphous matrix. Mn{sub 2}Ti, MnTi and NbTi{sub 4} intermetallic compounds were detected and revealed crystallites with size ranging from 3 to 20 nm. The Gibbs free energy for the formation of solid solution and amorphous phase of three ternary systems (Ti–Nb–Ta, Ti–Nb–Mn and Ti–Ta–Mn) was calculated using extended Miedema's model. Experimental and thermodynamic data confirmed that solid solution was first formed in the alloy with 6wt% Mn followed by the formation of an amorphous phase as milling time increases. The presence of Mn promoted the formation of amorphous phase because the atomic radius difference between Mn with Ti, Nb and Ta. - Highlights: • Thermodynamics analysis of extension of solid solution of the Ti–Nb–Ta–Mn system. • Formation of amorphous phase and intermetallic compounds were observed. • Nanocrystalline intermetallic compounds were formed with the sizes between 3 and 20 nm.

  6. Estrogenic and AhR activities in dissolved phase and suspended solids from wastewater treatment plants.

    Dagnino, Sonia; Gomez, Elena; Picot, Bernadette; Cavaillès, Vincent; Casellas, Claude; Balaguer, Patrick; Fenet, Hélène

    2010-05-15

    The distribution of estrogen receptor (ERalpha) and Aryl Hydrocarbon Receptor (AhR) activities between the dissolved phase and suspended solids were investigated during wastewater treatment. Three wastewater treatment plants with different treatment technologies (waste stabilization ponds (WSPs), trickling filters (TFs) and activated sludge supplemented with a biofilter system (ASB)) were sampled. Estrogenic and AhR activities were detected in both phases in influents and effluents. Estrogenic and AhR activities in wastewater influents ranged from 41.8 to 79 ng/L E(2) Eq. and from 37.9 to 115.5 ng/L TCDD Eq. in the dissolved phase and from 5.5 to 88.6 ng/g E(2) Eq. and from 15 to 700 ng/g TCDD Eq. in the suspended solids. For both activities, WSP showed greater or similar removal efficiency than ASB and both were much more efficient than TF which had the lowest removal efficiency. Moreover, our data indicate that the efficiency of removal of ER and AhR activities from the suspended solid phase was mainly due to removal of suspended solids. Indeed, ER and AhR activities were detected in the effluent suspended solid phase indicating that suspended solids, which are usually not considered in these types of studies, contribute to environmental contamination by endocrine disrupting compounds and should therefore be routinely assessed for a better estimation of the ER and AhR activities released in the environment. Copyright 2010 Elsevier B.V. All rights reserved.

  7. Recovery evaluation of organophosphorus pesticides from bee pollen by matrix solid-phase dispersion extraction using sorbents based on silica and titania

    Torres-Perea, C; Muñoz-Rodríguez, D; Carrera-Figueiras, C; Medina-Peralta, S; Moguel-Ordóñez, Y B

    2013-01-01

    This work focused on the evaluation of the recovery of organophosphorus pesticides from bee pollen after matrix solid phase-dispersion extraction (MSPD). Materials based on silica, titania and titania modified with polivylnylimidazole or polyestirene were used as adsorbents for the extraction of pesticides. Small amounts of fortified pollen (0.1 g, at 1 micro-g/g of pesticides), adsorbent (0.4 g) and solvent elution (1 mL de acetonitrile – ACN) were used in the extractions. For recovery evaluation, pollen extracts were analyzed by gas chromatography coupled with mass spectrometry.

  8. Influence of pressure on the solid state phase transformation of Cu–Al–Bi alloy

    Gong, Li; Jian-Hua, Liu; Wen-Kui, Wang; Ri-Ping, Liu

    2010-01-01

    The solid state phase transformation of Cu-Al-Bi alloy under high pressure was investigated by x-ray diffraction, energy dispersive spectroscopy and transmission electron microscopy. Experimental results show that the initial crystalline phase in the Cu-Al-Bi alloy annealed at 750 °C under the pressures in the range of 0–6 GPa is α-Cu solid solution (named as α-Cu phase below), and high pressure has a great influence on the crystallisation process of the Cu-Al-Bi alloy. The grain size of the α-Cu phase decreases with increasing pressure as the pressure is below about 3 GPa, and then increases (P > 3 GPa). The mechanism for the effects of high pressure on the crystallisation process of the alloy has been discussed. (condensed matter: structure, thermal and mechanical properties)

  9. A reactor/separator device for use in automated solid phase immunoassay

    Farina, P.R.; Ordonez, K.P.; Siewers, I.J.

    1979-01-01

    A reactor/separator device is described for use in automated solid phase immunoassay, including radioimmunoassays. The device is a column fitted at the bottom portion with a water impermeable disc which can hold, for example, immunoabsorbents, immobilized antisera or ion exchange resins. When the contents of the column supported by the disc are brought into contact with an aqueous phase containing reagents or reactants, a chemical reaction is initiated. After the reaction, centrifugally applied pressure forces the aqueous phase through the filter disc making it water permeable and separating a desired component for subsequent analysis. The reactor/separator device of the present invention permits kinetic solid phase assays (non-equilibrium conditions) to be carried out which would be difficult to perform by other conventional methods. (author)

  10. Dose fractionation in synchrotron radiation x-ray phase micro-tomography

    Frachon, Thibaut; Weber, Loriane; Hesse, Bernhard; Rit, Simon; Dong, Pei; Olivier, Cecile; Peyrin, Françoise; Langer, Max

    2015-01-01

    Phase sensitive x-ray imaging expands the applicability of standard attenuation based techniques by offering several orders of magnitude of increase in sensitivity. Due to the short wavelength, x-ray phase is not directly measurable, but has to be put in evidence by the use of phase contrast techniques. The phase can then be reconstructed from one or several phase contrast images. In this study, we consider synchrotron x-ray phase micro-computed tomography (μCT) based on free space propagation for heterogeneous and strongly absorbing objects. This technique generally relies on acquiring several scans of the sample at different detector distances. It is also generally believed that multi-distance phase μCT needs a higher dose input than single distance phase μCT. The purpose of this work is to study the impact of different means of dose fractionation on the reconstructed image quality. We define different acquistion schemes in multi-distance in-line phase μCT. Previously, the exposure time at each sample-to-detector distance was usually kept the same. Here, we let not only the number of distances vary but also the fraction of exposure time at each distance, the total exposure time being kept constant. Phase retrieval is performed with the mixed approach algorithm. The reconstructed μCT images are compared in terms of accuracy, precision and resolution. In addition, we also compare the result of dose fractionated multi distance phase μCT to single distance phase μCT using the same total radiation dose. In the multi-distance approach, we find that using different exposure times on each distance improves the image quality in the reconstructed image. Further, we show that, despite having the same total dose delivery, the multi distance imaging method gives better image quality than the single distance method, at the cost of an additional overhead from camera displacements and reference images. We show that by optimizing the acquistion parameters in terms of

  11. Study of process parameters effect on the filling phase of micro injection moulding using weld lines as flow markers

    Tosello, Guido; Gava, Alberto; Hansen, Hans Nørgaard

    2010-01-01

    , the relationships between the filling pattern and the different process parameter settings have to be established. In this paper, a novel approach based on the use of weld lines as flow markers to trace the development of the flow front during the filling is proposed. The effects on the filling stage of process......Micro-injection moulding (micro-moulding) is a process which enables the mass production of polymer microproducts. In order to produce high-quality injection moulded micro-parts, a crucial aspect to be fully understood and optimised is the filling of the cavity by the molten polymer. As a result...... manufactured by micro-electrodischarge machining. A commercially available polystyrene grade polymer has been moulded using a high-speed injection moulding machine. The design of experiment technique was employed to determine the effect of the process parameters on the filling phase of the micro...

  12. REE interactions with hydroxyapatite. Formation of secondary solid phases

    Seco, F.; Pablo, J. de; Bruno, J.

    2005-01-01

    Full text of publication follows: Lighter rare earth elements (REE) commonly occur in nature as the phosphate mineral monazite, while the heavier REE and Yttrium occur as the phosphate mineral xenotime, which has a similar composition, but different coordination environment of the cation. The geochemical behaviour of REE is mainly controlled by their interactions with phosphate minerals such as hydroxyapatite, Ca 5 (PO 4 ) 3 OH, which is a very common phosphate phase in subsurface environments. Furthermore, is a material considered to be used in a High Level Nuclear Waste repository due to its high capacity in the retention of radionuclides. The objective of this work has been to study the reaction mechanisms and thermodynamics of the interaction of La(III) and Yb(III) with hydroxyapatite as a model for general Ln(III) and Ac(III) behaviour. The surface interaction of La(III) and Yb(III) with synthetic hydroxyapatite has been investigated in batch experiments with low REE 3+ initial concentrations in constant 0.1 M NaClO 4 , at room temperature and in N 2 (g) atmosphere to avoid carbonate complex formation. The initial kinetic experiments indicated that a short contact time is needed to reach equilibrium ( 4 .nH 2 O, where a 0.83 4 .nH 2 O with 1.78 4 medium and under N 2 (g) atmosphere. The experimental data indicate that the solubility equilibria is mainly controlled by the aqueous species REE 3+ until approximately pH=5 where the formation of aqueous complexes of the form REEHPO 4 + , REEPO 4 and REE(PO 4 ) 2 3- must be considered. (authors)

  13. HPLC WITH SOLID PHASE EXTRACTION FOR IDENTIFICATION AND DIAGNOSIS OF ORGANOPHOSPHOROUS POISONING IN GOATS

    S. Manna

    2014-12-01

    Full Text Available High performance liquid chromatographic determination of organophosphorous compound has been done by reverse phase chromatography in goats. The goats were dying showing the symptoms of organophosphorous poisoning. The viscera and stomach contents sample were received from Project Co-Ordinator, Animal Disease Research Institute, Phulnakhara, Cuttack, Orissa. The analysis of samples by HPLC with UV detector after cleaning up in Solid Phase Extraction (SPE revealed presence of malathion that was later quantified.

  14. Treatment technologies of liquid and solid wastes from two-phase olive oil mills

    Borja Padilla, Rafael; Raposo Bejines, Francisco; Rincón, Bárbara

    2006-01-01

    Over the last 10 years the manufacture of olive oil has undergone important evolutionary changes in the equipment used for the separation of olive oil from the remaining components. The latest development has been the introduction of a two-phase centrifugation process in which a horizontally-mounted centrifuge is used for a primary separation of the olive oil fraction from the vegetable solid material and vegetation water. Therefore, the new two-phase olive oil mills produce three ident...

  15. Treatment technologies of liquid and solid wastes from two-phase olive oil mills

    Rincón, Bárbara; Raposo, Francisco; Borja, Rafael

    2006-01-01

    Over the last 10 years the manufacture of olive oil has undergone important evolutionary changes in the equipment used for the separation of olive oil from the remaining components. The latest development has been the introduction of a two-phase centrifugation process in which a horizontally-mounted centrifuge is used for a primary separation of the olive oil fraction from the vegetable solid material and vegetation water. Therefore, the new two-phase olive oil mills produce three identifiabl...

  16. Melting along the Hugoniot and solid phase transition for Sn via sound velocity measurements

    Song, Ping; Cai, Ling-cang; Tao, Tian-jiong; Yuan, Shuai; Chen, Hong; Huang, Jin; Zhao, Xin-wen; Wang, Xue-jun

    2016-11-01

    It is very important to determine the phase boundaries for materials with complex crystalline phase structures to construct their corresponding multi-phase equation of state. By measuring the sound velocity of Sn with different porosities, different shock-induced melting pressures along the solid-liquid phase boundary could be obtained. The incipient shock-induced melting of porous Sn samples with two different porosities occurred at a pressure of about 49.1 GPa for a porosity of 1.01 and 45.6 GPa for a porosity of 1.02, based on measurements of the sound velocity. The incipient shock-induced melting pressure of solid Sn was revised to 58.1 GPa using supplemental measurements of the sound velocity. Trivially, pores in Sn decreased the shock-induced melting pressure. Based on the measured longitudinal sound velocity data, a refined solid phase transition and the Hugoniot temperature-pressure curve's trend are discussed. No bcc phase transition occurs along the Hugoniot for porous Sn; further investigation is required to understand the implications of this finding.

  17. Technology of preparation for low density 6Li(H,D) solid micro-target

    Wang Xisheng; Zeng Jiaquan; Li Qiang

    2002-01-01

    Low density 6 Li(H,D) micro-targets are prepared by loose sintering 6 LiH or 6 LiD powder in a tiny gold cylinder and soaking for 30 min up to 430 degree C at the rate of 10 degree C/h in argon. The dimension of the micro-targets is as tiny as 0.6-1.0 mm for diameter and 1-2 mm for length. Densities of 6 LiH and 6 LiD without Parylene C is (0.283 +- 0.009) g/cm 3 and (0.369 +- 0.009) g/cm 3 , respectively while 6 LiD targets with Parylene C is only (0.301 +- 0.010) g/cm 3 . The Parylene C has no effect on purity, deuterium abundance and 6 Li abundance of the sintered micro-targets. It's effective to keep 6 Li(H,D) purity by strict control of argon atmosphere

  18. Experimental micro mechanics methods for conventional and negative Poisson's ratio cellular solids as Cosserat continua

    Lakes, R.

    1991-01-01

    Continuum representations of micromechanical phenomena in structured materials are described, with emphasis on cellular solids. These phenomena are interpreted in light of Cosserat elasticity, a generalized continuum theory which admits degrees of freedom not present in classical elasticity. These are the rotation of points in the material, and a couple per unit area or couple stress. Experimental work in this area is reviewed, and other interpretation schemes are discussed. The applicability of Cosserat elasticity to cellular solids and fibrous composite materials is considered as is the application of related generalized continuum theories. New experimental results are presented for foam materials with negative Poisson's ratios.

  19. Highly Selective Liquid-Phase Benzylation of Anisole with Solid-Acid Zeolite Catalysts

    Poreddy, Raju; Shunmugavel, Saravanamurugan; Riisager, Anders

    2015-01-01

    Zeolites were evaluated as solid acid catalysts for the liquid-phase benzylation of anisole with benzyl alcohol, benzyl bromide, and benzyl chloride at 80 °C. Among the examined zeolites, H-mordenite-10 (H-MOR-10) demonstrated particular high activity (>99 %) and excellent selectivity (>96...

  20. Solid-phase cloning for high-throughput assembly of single and multiple DNA parts

    Lundqvist, Magnus; Edfors, Fredrik; Sivertsson, Åsa

    2015-01-01

    We describe solid-phase cloning (SPC) for high-throughput assembly of expression plasmids. Our method allows PCR products to be put directly into a liquid handler for capture and purification using paramagnetic streptavidin beads and conversion into constructs by subsequent cloning reactions. We ...

  1. Automated Solid-Phase Subcloning Based on Beads Brought into Proximity by Magnetic Force

    Hudson, Elton P.; Nikoshkov, Andrej; Uhlén, Mathias

    2012-01-01

    In the fields of proteomics, metabolic engineering and synthetic biology there is a need for high-throughput and reliable cloning methods to facilitate construction of expression vectors and genetic pathways. Here, we describe a new approach for solid-phase cloning in which both the vector and th...

  2. Dispersive solid-phase imprinting of proteins for the production of plastic antibodies

    Ashley, Jon; Feng, Xiaotong; Halder, Arnab

    2018-01-01

    We describe a novel dispersive solid-phase imprinting technique for the production of nano-sized molecularly imprinted polymers (nanoMIPs) as plastic antibodies. The template was immobilized on in-house synthesized magnetic microspheres instead of conventional glass beads. As a result, high...

  3. Practical application of solid phase spectrophotometry in analysis of materials and goods of mining and metallurgy

    Duan Qunzhang

    1999-01-01

    The author reviewed recent development and practical application of solid phase spectrophotometry in analysis of materials and goods of mining-metallurgy. Separation and preconcentration and conditions of coloring determination, sensitivity and range of detection, as well as interference of corresponding method are discussed

  4. The constitutive distributed parameter model of multicomponent chemical processes in gas, fluid and solid phase

    Niemiec, W.

    1985-01-01

    In the literature of distributed parameter modelling of real processes is not considered the class of multicomponent chemical processes in gas, fluid and solid phase. The aim of paper is constitutive distributed parameter physicochemical model, constructed on kinetics and phenomenal analysis of multicomponent chemical processes in gas, fluid and solid phase. The mass, energy and momentum aspects of these multicomponent chemical reactions and adequate phenomena are utilized in balance operations, by conditions of: constitutive invariance for continuous media with space and time memories, reciprocity principle for isotropic and anisotropic nonhomogeneous media with space and time memories, application of definitions of following derivative and equation of continuity, to the construction of systems of partial differential constitutive state equations, in the following derivative forms for gas, fluid and solid phase. Couched in this way all physicochemical conditions of multicomponent chemical processes in gas, fluid and solid phase are new form of constitutive distributed parameter model for automatics and its systems of equations are new form of systems of partial differential constitutive state equations in sense of phenomenal distributed parameter control

  5. Solid-phase synthesis of head and tail bis-acridinylated peptides

    Šebestík, Jaroslav; Matějka, P.; Hlaváček, Jan; Stibor, I.

    2004-01-01

    Roč. 45, č. 6 (2004), s. 1203-1205 ISSN 0040-4039 R&D Projects: GA ČR GA203/02/1379 Institutional research plan: CEZ:AV0Z4055905 Keywords : 9-amino acridine * solid phase synthesis * head and tail peptide conjugates Subject RIV: CC - Organic Chemistry Impact factor: 2.484, year: 2004

  6. Solid-phase synthesis of an apoptosis-inducing tetrapeptide mimicking the Smac protein

    Le Quement, Sebastian Thordal; Ishøy, Mette; Petersen, Mette Terp

    2011-01-01

    An approach for the solid-phase synthesis of apoptosis-inducing Smac peptidomimetics is presented. Using a Rink linker strategy, tetrapeptides mimicking the N-4-terminal residue of the Smac protein [(N-Me)AVPF sequence] were synthesized on PEGA resin in excellent purities and yields. Following two...

  7. A convenient procedure for the solid-phase synthesis of hydroxamic acids on PEGA resins

    Nandurkar, Nitin Subhash; Petersen, Rico; Qvortrup, Katrine

    2011-01-01

    An efficient method for the solid-phase synthesis of hydroxamic acids is described. The method comprises the nucleophilic displacement of esters immobilized on PEGA resins with hydroxylamine/sodium hydroxide in isopropanol. The hydroxyaminolysis protocol is compatible with a broad range of PEGA...

  8. Solid-phase synthesis of polyfunctional polylysine dendrons using aldehyde linkers

    Svenssen, Daniel K.; Mirsharghi, Sahar; Boas, Ulrik

    2014-01-01

    A straightforward method for the solid-phase synthesis of C-terminally modified polylysine dendrons has been developed by applying bisalkoxybenzaldehyde and trisalkoxybenzaldehyde linkers. The method has been used for the synthesis of polylysine dendrons with a variety of C-terminal ‘tail groups’...

  9. Electronic structure of elements and compounds and electronic phases of solids

    Nadykto, B.A.

    2000-01-01

    The paper reviews technique and computed energies for various electronic states of many-electron multiply charged ions, molecular ions, and electronic phases of solids. The model used allows computation of the state energy for free many-electron multiply charged ions with relative accuracy ∼10 -4 suitable for analysis of spectroscopy data

  10. Critical micelle concentration values for different surfactants measured with solid-phase microextraction fibers

    Haftka, Joris J H; Scherpenisse, Peter; Oetter, G??nter; Hodges, Geoff; Eadsforth, Charles V.; Kotthoff, Matthias; Hermens, Joop L M

    The amphiphilic nature of surfactants drives the formation of micelles at the critical micelle concentration (CMC). Solid-phase microextraction (SPME) fibres were used in the present study to measure CMC values of twelve nonionic, anionic, cationic and zwitterionic surfactants. The SPME derived CMC

  11. A new solid-phase sandwich radioimmunoassay and its application to the detection of snake venom

    Coulter, A.R.; Cox, J.C.; Sutherland, S.K.; Waddel, C.J.

    1978-01-01

    A solid-phase sandwich radioimmunoassay is described which can be used for the detection and quantitative estimation of crude snake venom and a snake neurotoxin in clinical and experimental situations. Rabbit IgG antivenom or antineurotoxin, covalently coupled to a solid phase (CH-Sepharose 4B) is incubated with sample of unknown venom concentration. Venom bound by the solid-phase antibody is detected by reaction with 125 I-labelled rabbit IgG antivenom or antineurotoxin ([ 125 I]IgG). The resultant count, T, is the total (specific and non-specific) uptake of [ 125 I]IgG. Non-specific binding N, is similarly determined, but with normal rabbit IgG antivenom or antineurotoxin ([ 125 I]IgG). The resultant count, T, is the total (specific and non-specific) uptake of [ 125 I]IgG. Non-specific binding N, is similarly determined, but with normal rabbit IgG bound to the solid phase. A T:N value greater than 1.8 for human serum or urine indicates the presence of venom in a sample (P>0.95). Positive samples are assayed at several dilutions and the venom present estimated from the specific count (T-N). Levels of 0.4 ng/ml of crude tiger snake venom (TSV) and 0.1 ng/ml of neurotoxin can be reliably detected by this procedure. (Auth.)

  12. Influence of Calcium on Microbial Reduction of Solid Phase Uranium (VI)

    Liu, Chongxuan; Jeon, Byong-Hun; Zachara, John M.; Wang, Zheming

    2007-01-01

    The effect of calcium on microbial reduction of a solid phase U(VI), sodium boltwoodite (NaUO2SiO3OH · 1.5H2O), was evaluated in a culture of a dissimilatory metal-reducing bacterium (DMRB), Shewanella oneidensis strain MR-1. Batch experiments were performed in a non-growth bicarbonate medium with lactate as electron donor at pH 7 buffered with PIPES. Calcium increased both the rate and extent of Na-boltwoodite dissolution by increasing its solubility through the formation of a ternary aqueous calcium-uranyl-carbonate species. The ternary species, however, decreased the rates of microbial reduction of aqueous U(VI). Laser-induced fluorescence spectroscopy (LIFS) and transmission electron microscopy (TEM) revealed that microbial reduction of solid phase U(VI) is a sequentially coupled process of Na-boltwoodite dissolution, U(VI) aqueous speciation, and microbial reduction of dissolved U(VI) to U(IV) that accumulated on bacterial surfaces/periplasm. The overall rates of microbial reduction of solid phase U(VI) can be described by the coupled rates of dissolution and microbial reduction that were both influenced by calcium. The results demonstrated that dissolved U(VI) concentration during microbial reduction was a complex function of solid phase U(VI) dissolution kinetics, aqueous U(VI) speciation, and microbial activity

  13. Comparison of solid and liquid-phase bioassays using ecoscores to assess contaminated soils

    Lors, Christine [Universite Lille Nord de France, 1bis rue Georges Lefevre, 59044 Lille Cedex (France); Ecole des Mines de Douai, LGCgE-MPE-GCE, 941 rue Charles-Bourseul, 59500 Douai (France); Centre National de Recherche sur les Sites et Sols Pollues, 930 Boulevard Lahure, BP 537, 59505 Douai Cedex (France); Ponge, Jean-Francois, E-mail: ponge@mnhn.fr [Museum National d' Histoire Naturelle, Departement Ecologie et Gestion de la Biodiversite, CNRS UMR 7179, 4 Avenue du Petit-Chateau, 91800 Brunoy (France); Martinez Aldaya, Maite [Museum National d' Histoire Naturelle, Departement Ecologie et Gestion de la Biodiversite, CNRS UMR 7179, 4 Avenue du Petit-Chateau, 91800 Brunoy (France); Damidot, Denis [Universite Lille Nord de France, 1bis rue Georges Lefevre, 59044 Lille Cedex (France); Ecole des Mines de Douai, LGCgE-MPE-GCE, 941 rue Charles-Bourseul, 59500 Douai (France)

    2011-10-15

    Bioassays on aqueous and solid phases of contaminated soils were compared, belonging to a wide array of trophic and response levels and using ecoscores for evaluating ecotoxicological and genotoxicological endpoints. The method was applied to four coke factory soils contaminated mainly with PAHs, but also to a lesser extent by heavy metals and cyanides. Aquatic bioassays do not differ from terrestrial bioassays when scaling soils according to toxicity but they are complementary from the viewpoint of ecological relevance. Both aquatic and terrestrial endpoints are strongly correlated with concentrations of 3-ring PAHs. This evaluation procedure allows us to propose a cost-effective battery which embraces a wide array of test organisms and response levels: it includes two rapid bioassays (Microtox) and springtail avoidance), a micronucleus test and three bioassays of a longer duration (algal growth, lettuce germination and springtail reproduction). This battery can be recommended for a cost-effective assessment of polluted/remediated soils. - Highlights: > Comparison of liquid- and solid-phase bioassays on contaminated soils, using ecoscores. > Complementarity of liquid- and solid-phase bioassays for the evaluation of environmental hazards. > Proposal for a restricted battery of 5 most sensitive tests. > Use of this restricted battery for a cost-effective assessment of polluted/remediated soils. - Aqueous and solid phases of contaminated soils give similar results in terms of toxicity but are complementary for the evaluation of environmental hazards by ecoscores.

  14. Automatic reactor for solid-phase synthesis of molecularly imprinted polymeric nanoparticles (MIP NPs) in water.

    Poma, Alessandro; Guerreiro, Antonio; Caygill, Sarah; Moczko, Ewa; Piletsky, Sergey

    We report the development of an automated chemical reactor for solid-phase synthesis of MIP NPs in water. Operational parameters are under computer control, requiring minimal operator intervention. In this study, "ready for use" MIP NPs with sub-nanomolar affinity are prepared against pepsin A, trypsin and α-amylase in only 4 hours.

  15. Automatic reactor for solid-phase synthesis of molecularly imprinted polymeric nanoparticles (MIP NPs) in water

    Poma, Alessandro; Guerreiro, Antonio; Caygill, Sarah; Moczko, Ewa; Piletsky, Sergey

    2014-01-01

    We report the development of an automated chemical reactor for solid-phase synthesis of MIP NPs in water. Operational parameters are under computer control, requiring minimal operator intervention. In this study, “ready for use” MIP NPs with sub-nanomolar affinity are prepared against pepsin A, trypsin and α-amylase in only 4 hours.

  16. Microwave-assisted solid-phase Ugi four-component condensations

    Nielsen, John

    1999-01-01

    An 18-member library was constructed from 2 isocyanides, 3 aldehydes and 3 carboxylic acids via microwave-assisted solid-phase Ugi reactions on TentaGel S RAM. Products of high purity were obtained in moderate to excellent yields after reaction times of 5 minutes or less (irradiation at 60W). (C...

  17. Rapid and convenient semi-automated microwave-assisted solid-phase synthesis of arylopeptoids

    Rasmussen, Jakob Ewald; Boccia, Marcello Massimo; Nielsen, John

    2014-01-01

    A facile and expedient route to the synthesis of arylopeptoid oligomers (N-alkylated aminomethyl benz-amides) using semi-automated microwave-assisted solid-phase synthesis is presented. The synthesis was optimized for the incorporation of side chains derived from sterically hindered or unreactive...

  18. Detection and specifity of class specific antibodies to whole bacteria cells using a solid phase radioimmunoassay

    Czerkinsky, C.; Rees, A.S.; Bergimeier, L.A.; Challacombe, S.J. (Guy' s Hospital Medical and Dental Schools, London (UK))

    1983-07-01

    A solid phase radioimmunoassay has been developed which can be used for the detection of isotype specific antibodies to whole bacteria and other particulate antigens, and is applicable to a variety of species. Bacteria are bound to the solid phase by the use either of antibodies, or of methyl glyoxal. Both methods result in a sensitive and reproducible assay, and bacteria do not appear to desorb from the solid phase. The specificity of antibodies to whole bacteria was examined by absorption of antisera with various species of bacteria and retesting, or by determining the binding of antisera to various bacteria bound to the solid phase. Both methods revealed specificity for the bacteria examined. Inhibition studies showed that antibodies to Streptococcus mutans whole cells could be inhibited by purified cell surface antigens glucosyltransferase and antigen I/II, but only minimally by lipoteichoic acid, c polysaccharide or dextran. In murine antisera antibodies of the IgG, IgM, and IgA classes could be detected at amounts of less than 1 ng/ml.

  19. Solid-phase extraction of berries’ anthocyanins and evaluation of their antioxidative properties

    Denev, P.; Číž, Milan; Ambrožová, Gabriela; Lojek, Antonín; Yanakieva, I.; Kratchanova, M.

    2010-01-01

    Roč. 123, č. 4 (2010), s. 1055-1061 ISSN 0308-8146 R&D Projects: GA MŠk(CZ) OC08058 Institutional research plan: CEZ:AV0Z50040507; CEZ:AV0Z50040702 Keywords : anthocyanins * solid-phase extraction * berry extracts Subject RIV: BO - Biophysics Impact factor: 3.458, year: 2010

  20. Investigating the Retention Mechanisms of Liquid Chromatography Using Solid-Phase Extraction Cartridges

    O'Donnell, Mary E.; Musial, Beata A.; Bretz, Stacey Lowery; Danielson, Neil D.; Ca, Diep

    2009-01-01

    Liquid chromatography (LC) experiments for the undergraduate analytical laboratory course often illustrate the application of reversed-phase LC to solve a separation problem, but rarely compare LC retention mechanisms. In addition, a high-performance liquid chromatography instrument may be beyond what some small colleges can purchase. Solid-phase…

  1. Technical note: New applications for on-line automated solid phase extraction

    MacFarlane, John D.

    1997-01-01

    This technical note explains the disadvantages of manual solid phase extraction (SPE) techniques and the benefits to be gained with automatic systems. The note reports on a number of general and highly specific applications using the Sample Preparation Unit OSP-2A.

  2. Solution and solid-phase halogen and C-H hydrogen bonding to perrhenate.

    Massena, Casey J; Riel, Asia Marie S; Neuhaus, George F; Decato, Daniel A; Berryman, Orion B

    2015-01-28

    (1)H NMR spectroscopic and X-ray crystallographic investigations of a 1,3-bis(4-ethynyl-3-iodopyridinium)benzene scaffold with perrhenate reveal strong halogen bonding in solution, and bidentate association in the solid state. A nearly isostructural host molecule demonstrates significant C-H hydrogen bonding to perrhenate in the same phases.

  3. Speciation analysis of aqueous nanoparticulate diclofenac complexes by solid-phase microextraction

    Zielinska, K.; Leeuwen, van H.P.; Thibault, S.; Town, R.M.

    2012-01-01

    The dynamic sorption of an organic compound by nanoparticles (NPs) is analyzed by solid-phase microextraction (SPME) for the example case of the pharmaceutical diclofenac in dispersions of impermeable (silica, SiO(2)) and permeable (bovine serum albumin, BSA) NPs. It is shown that only the

  4. Operando Spectroscopy of the Gas-Phase Aldol Condensation of Propanal over Solid Base Catalysts

    Hernández-giménez, Ana M.; Ruiz-martínez, Javier; Puértolas, Begoña; Pérez-ramírez, Javier; Bruijnincx, Pieter C. A.; Weckhuysen, Bert M.

    2017-01-01

    The gas-phase aldol condensation of propanal, taken as model for the aldehyde components in bio-oils, has been studied with a combined operando set-up allowing to perform FT-IR & UV–Vis diffuse reflectance spectroscopy (DRS) with on-line mass spectrometry (MS). The selected solid base catalysts, a

  5. Solid Phase Radioimmunoassay for Measuring Serum Prolactin Using Antibody Coupled Magnetizable Particles

    El-Bayoumy, A.S.A.

    2012-01-01

    The objective of the present work was to prepare solid phase radioimmunoassay (RIA) reagents. Development as well as optimization and validation of RIA system using solid phase magnetic particles for the measurement of prolactin (PRL) in human serum are described. The production of polyclonal antibodies was carried out by immunizing three Balb/C mice intraperitoneal through primary injection and two booster doses. Low density magnetizable cellulose iron oxide particles have been used to couple covalently to the IgG fraction of polyclonal anti-prolactin using carbonyl diimidazole activation method and applied as a solid phase separating agent for RIA of serum prolactin. Preparation of 125 I-PRL tracer was prepared using lactoperoxidase method and it was purified by gel filtration using sephadex G-100. The PRL standards were prepared using a highly purified PRL antigen with assay buffer as standard matrix. Optimization and validation of the assay were carried out. The results obtained provide a low cost, simple, sensitive, specific and accurate RIA system of prolactin based on magnetizable solid phase separation. These magnetic particles retain their characteristics during storage for 6 months at 4 degree C. In conclusion, this assay could be used as a useful diagnostic tool for pituitary dysfunction and possible reproductive disability.

  6. Controlled phase gate for solid-state charge-qubit architectures

    Schirmer, S.G.; Oi, D.K.L.; Greentree, Andrew D.

    2005-01-01

    We describe a mechanism for realizing a controlled phase gate for solid-state charge qubits. By augmenting the positionally defined qubit with an auxiliary state, and changing the charge distribution in the three-dot system, we are able to effectively switch the Coulombic interaction, effecting an entangling gate. We consider two architectures, and numerically investigate their robustness to gate noise

  7. Indirect solid-phase immunosorbent assay for detection of arenavirus antigens and antibodies

    Ivanov, A P; Rezapkin, G V; Dzagurova, T K; Tkachenko, E A [Institute of Poliomyelitis anU Viral Encephalities of the U.S.S.R. Academy of Medical Sciences, Moscow

    1984-05-01

    Indirect enzyme-linked immunosorbent assay (ELISA) and solid phase radioimmunoassay (SPRIA) using either enti-human or anti-mouse IgG labelled with horseradish peroxidase and /sup 125/I, respectively, were developed for the detection of Junin, Machupo, Tacaribe, Amapari, Tamiami, Lassa and LCM arenaviruses. Both methods allow high sensitivity detection of arenavirus antigens and antibodies.

  8. Chemically and geographically distinct solid-phase iron pools in the Southern Ocean

    Mtshali, TN

    2012-11-01

    Full Text Available Iron is a limiting nutrient in many parts of the oceans, including the unproductive regions of the Southern Ocean. Although the dominant fraction of the marine iron pool occurs in the form of solid-phase particles, its chemical speciation...

  9. Thermal battery. [solid metal halide electrolytes with enhanced electrical conductance after a phase transition

    Carlsten, R.W.; Nissen, D.A.

    1973-03-06

    The patent describes an improved thermal battery whose novel design eliminates various disadvantages of previous such devices. Its major features include a halide cathode, a solid metal halide electrolyte which has a substantially greater electrical conductance after a phase transition at some temperature, and a means for heating its electrochemical cells to activation temperature.

  10. Comparison of solid and liquid-phase bioassays using ecoscores to assess contaminated soils

    Lors, Christine; Ponge, Jean-Francois; Martinez Aldaya, Maite; Damidot, Denis

    2011-01-01

    Bioassays on aqueous and solid phases of contaminated soils were compared, belonging to a wide array of trophic and response levels and using ecoscores for evaluating ecotoxicological and genotoxicological endpoints. The method was applied to four coke factory soils contaminated mainly with PAHs, but also to a lesser extent by heavy metals and cyanides. Aquatic bioassays do not differ from terrestrial bioassays when scaling soils according to toxicity but they are complementary from the viewpoint of ecological relevance. Both aquatic and terrestrial endpoints are strongly correlated with concentrations of 3-ring PAHs. This evaluation procedure allows us to propose a cost-effective battery which embraces a wide array of test organisms and response levels: it includes two rapid bioassays (Microtox) and springtail avoidance), a micronucleus test and three bioassays of a longer duration (algal growth, lettuce germination and springtail reproduction). This battery can be recommended for a cost-effective assessment of polluted/remediated soils. - Highlights: → Comparison of liquid- and solid-phase bioassays on contaminated soils, using ecoscores. → Complementarity of liquid- and solid-phase bioassays for the evaluation of environmental hazards. → Proposal for a restricted battery of 5 most sensitive tests. → Use of this restricted battery for a cost-effective assessment of polluted/remediated soils. - Aqueous and solid phases of contaminated soils give similar results in terms of toxicity but are complementary for the evaluation of environmental hazards by ecoscores.

  11. Development of an interface for directly coupled solid-phase extraction and GC-MS analysis

    Öllers, M.J.H.; van Lieshout, H.P.M.; Janssen, J.G.M.; Cramers, C.A.M.G.

    Solid-phase extraction (SPE) is widely used as a sample preparation technique in numerous application areas of chromatography. Large-volume injection is an attractive technique for coupling SPE to gas chromatography (GC) because it provides improved detection limits and circumvents the need for

  12. Immunochemical cross-reactivity between albumin and solid-phase adsorbed histamine

    Poulsen, L K; Nolte, H; Søndergaard, I

    1990-01-01

    For production of an antibody against histamine, this was coupled to human serum albumin (HSA) and used for immunization of rabbits. To test the antiserum, an immunoradiometric assay was developed comprising solid-phase bound histamine, antisera and radiolabelled protein A. Titration and inhibition...

  13. A simplified radiometabolite analysis procedure for PET radioligands using a solid phase extraction with micellar medium

    Nakao, Ryuji; Halldin, Christer

    2013-01-01

    A solid phase extraction method has been developed for simple and high-speed direct determination of PET radioligands in plasma. Methods: This methodology makes use of a micellar medium and a solid-phase extraction cartridge for displacement of plasma protein bound radioligand and separation of PET radioligands from their radiometabolites without significant preparation. The plasma samples taken from monkey or human during PET measurements were mixed with a micellar eluent containing an anionic surfactant sodium dodecyl sulphate and loaded onto SPE cartridges. The amount of radioactivity corresponding to parent radioligand (retained on the cartridge) and its radioactive metabolites (eluted with micellar eluent) was measured. Results: Under the optimized conditions, excellent separation of target PET radioligands from their radiometabolites was achieved with a single elution and short run-time of 1 min. This method was successfully applied to study the metabolism for 11 C-labelled radioligands in human or monkey plasma. The amount of parent PET radioligands estimated by micellar solid phase extraction strongly corresponded with that determined by radio-LC. The improved throughput permitted the analysis of a large number of plasma samples (up to 13 samples per one PET study) for accurate estimation of metabolite-corrected input function during quantitative PET imaging studies. Conclusion: Solid phase extraction together with micellar medium is fast, sensitive and easy to use, and therefore it is an attractive alternative method to determine relative composition of PET radioligands in plasma

  14. Graft-copolymerization of styrene on polypropylene in the solid phase

    Beenen, W.; VanderWal, D.; Janssen, L.P.B.M.; Buijtenhuijs, A.; Hogt, A.H.; Wal, Douwe J. v.d.

    The graft-copolymerization of styrene on PP in the solid phase has been studied under various reaction conditions using a radical initiator. Polymerization kinetics were investigated by DSC experiments and reactions in glass ampoules. The conversion rate and grafting efficiency of styrene appeared

  15. Linkers, resins, and general procedures for solid-phase peptide synthesis

    Shelton, Anne Pernille Tofteng; Jensen, Knud Jørgen

    2013-01-01

    and linkers for solid-phase synthesis is a key parameter for successful peptide synthesis. This chapter provides an overview of the most common and useful resins and linkers for the synthesis of peptides with C-terminal amides, carboxylic acids, and more. The chapter finishes with robust protocols for general...

  16. Dynamic speciation analysis of atrazine in aqueous latex nanoparticle dispersions using solid phase microextraction (SPME)

    Benhabib, K.; Town, R.M.; Leeuwen, van H.P.

    2009-01-01

    Solid phase microextraction (SPME) is applied in the dynamic speciation analysis of the pesticide atrazine in an aqueous medium containing sorbing latex nanoparticles. It is found that the overall rate of extraction of the analyte is faster than in the absence of nanoparticles and governed by the

  17. Phase relations and Gibbs energies of spinel phases and solid solutions in the system Mg-Rh-O

    Jacob, K.T., E-mail: katob@materials.iisc.ernet.in [Department of Materials Engineering, Indian Institute of Science, Bangalore 560 012 (India); Prusty, Debadutta [Department of Materials Engineering, Indian Institute of Science, Bangalore 560 012 (India); Kale, G.M. [Institute for Materials Research, University of Leeds, Leeds, LS2 9JT (United Kingdom)

    2012-02-05

    Highlights: Black-Right-Pointing-Pointer Refinement of phase diagram for the system Mg-Rh-O and thermodynamic data for spinel compounds MgRh{sub 2}O{sub 4} and Mg{sub 2}RhO{sub 4} is presented. Black-Right-Pointing-Pointer A solid-state electrochemical cell is used for thermodynamic measurement. Black-Right-Pointing-Pointer An advanced design of the solid-state electrochemical cell incorporating buffer electrodes is deployed to minimize polarization of working electrode. Black-Right-Pointing-Pointer Regular solution model for the spinel solid solution MgRh{sub 2}O{sub 4} - Mg{sub 2}RhO{sub 4} based on ideal mixing of cations on the octahedral site is proposed. Black-Right-Pointing-Pointer Factors responsible for stabilization of tetravalent rhodium in spinel compounds are identified. - Abstract: Pure stoichiometric MgRh{sub 2}O{sub 4} could not be prepared by solid state reaction from an equimolar mixture of MgO and Rh{sub 2}O{sub 3} in air. The spinel phase formed always contained excess of Mg and traces of Rh or Rh{sub 2}O{sub 3}. The spinel phase can be considered as a solid solution of Mg{sub 2}RhO{sub 4} in MgRh{sub 2}O{sub 4}. The compositions of the spinel solid solution in equilibrium with different phases in the ternary system Mg-Rh-O were determined by electron probe microanalysis. The oxygen potential established by the equilibrium between Rh + MgO + Mg{sub 1+x}Rh{sub 2-x}O{sub 4} was measured as a function of temperature using a solid-state cell incorporating yttria-stabilized zirconia as an electrolyte and pure oxygen at 0.1 MPa as the reference electrode. To avoid polarization of the working electrode during the measurements, an improved design of the cell with a buffer electrode was used. The standard Gibbs energies of formation of MgRh{sub 2}O{sub 4} and Mg{sub 2}RhO{sub 4} were deduced from the measured electromotive force (e.m.f.) by invoking a model for the spinel solid solution. The parameters of the model were optimized using the measured

  18. Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD) and Dispersive Solid Phase Extraction (d-SPE) of Plant Samples

    Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Strzemski, Maciej; Sawicki, Jan; Staniak, Michał; Dresler, Sławomir; Szwerc, Wojciech; Mołdoch, Jarosław; Latalski, Michał

    2018-01-01

    Polyaniline (PANI) is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME). In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI) was used for dispersive solid phase extraction (d-SPE) and matrix solid–phase extraction (MSPD). The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD) quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples. PMID:29565297

  19. Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD and Dispersive Solid Phase Extraction (d-SPE of Plant Samples

    Ireneusz Sowa

    2018-03-01

    Full Text Available Polyaniline (PANI is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME. In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI was used for dispersive solid phase extraction (d-SPE and matrix solid–phase extraction (MSPD. The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples.

  20. Liquid phase micro-extraction: Towards the green methodology for ultratrace metals determination in aquatic ecosystems

    López-López J. A.

    2013-04-01

    Full Text Available Heavy metals are normally found, in natural waters, in very low concentrations. Some of them are essential for life in low level; however, in higher level they are toxic. Therefore, analyzing their bio-available fraction is of main interest. Standard methodology is based in the collection of a number of samples from a water body. Collected samples must be stored, pre-treated and then analyzed. Pre-treatment usually involves pre-concentrating the metal, with the corresponding risk of contamination or loss of analyte. This way, punctual information is obtained from every sampling campaign. As an alternative, passive sampling techniques allow the continuous and coupled sampling-pre-treatment for heavy metals analysis, giving a better approach in the characterization of the studied water body. Liquid phase micro-extraction (LPME is a green analytical alternative for liquid-liquid extraction that promotes a reduction of sample volume, solvent needed and waste generation. Using these systems, polypropylene hollow fibers (HF with pores in their walls can be used. A few micro-liters of organic solvent are supported in the pores. The sample is placed in the outer part of the fiber and a receiving phase is placed in its inner part, allowing continuous liquid extraction of the metal from the sample. Several fibers with different physical features have been employed to analyzed total concentration and bio-availability of some heavy metals (Ag, Ni, Cu in natural water samples. Thanks to fibers configuration, devices for passive sampling based in HF-LPME could be designed. Advantages of this methodology over existing ones are supported because the receiving phase is liquid. As a consequence, retained metals do not need to be eluted from the acceptor prior to instrumental analysis.

  1. Thermal conductivity of solid cyclohexane in orientationally ordered and disordered phases

    Konstantinov, V. A.; Revyakin, V. P.; Sagan, V. V.; Pursky, O. I.; Sysoev, V. M.

    2011-01-01

    Thermal conductivity Λ P of solid cyclohexane is measured at a pressure P = 0.1 MPa in the temperature range from 80 K to the melting point, which covers the ranges of low-temperature orientationally ordered phase II and high-temperature orientationally disordered phase I. Thermal conductivity Λ V is measured at a constant volume in orientationally disordered phase I. The thermal conductivity measured at atmospheric pressure decreases with increasing temperature as Λ P ∝ T −1.15 in phase II, whereas Λ P ∝ T −0.3 in phase I. As temperature increases, isochoric thermal conductivity Λ V in phase I increases gradually. The experimental data are described in terms of a modified Debye model of thermal conductivity with allowance for heat transfer by both phonons and “diffuse” modes.

  2. Thermal conductivity of microPCMs-filled epoxy matrix composites

    Su, J.F.; Wang, X.Y; Huang, Z.; Zhao, Y.H.; Yuan, X.Y.

    2011-01-01

    Microencapsulated phase change materials (microPCMs) have been widely applied in solid matrix as thermal-storage or temperature-controlling functional composites. The thermal conductivity of these microPCMs/matrix composites is an important property need to be considered. In this study, a series of microPCMs have been fabricated using the in situ polymerization with various core/shell ratio and average diameter; the thermal conductivity of microPCMs/epoxy composites were investigated in detai...

  3. Solid freeform fabrication of piezoelectric actuators by a micro-casting method

    Bos, B.; Gorter, H.; Dortmans, L.J.M.G.

    2004-01-01

    In recent years, there has been much interest in the manufacturing of piezoceramic actuators by Solid Freeform Fabrication (SFF) methods, following developments in polymer and metal shaping. With these methods, actuator shapes can be realized that are impossible or very difficult to obtain by

  4. Liquid chromatography tandem mass spectrometry method using solid-phase extraction and bead-beating-assisted matrix solid-phase dispersion to quantify the fungicide tebuconazole in controlled frog exposure study: analysis of water and animal tissue

    Hansen, Martin; Poulsen, Rikke; Luong, Xuan

    2014-01-01

    and on tissue from exposed and non-exposed adult X. laevis. Using solid-phase extraction (SPE), the analytical method allows for quantification of tebuconazole at concentrations as low as 3.89 pg mL(-1) in 10 mL water samples. Using bead-beating-assisted matrix solid-phase dispersion (MSPD), it was possible...

  5. New Approaches in Soil Organic Matter Fluorescence; A Solid Phase Fluorescence Approach

    Bowman, M. M.; Sanclements, M.; McKnight, D. M.

    2017-12-01

    Fluorescence spectroscopy is a well-established technique to investigate the composition of organic matter in aquatic systems and is increasingly applied to soil organic matter (SOM). Current methods require that SOM be extracted into a liquid prior to analysis by fluorescence spectroscopy. Soil extractions introduce an additional layer of complexity as the composition of the organic matter dissolved into solution varies based upon the selected extractant. Water is one of the most commonly used extractant, but only extracts the water-soluble fraction of the SOM with the insoluble soil organic matter fluorescence remaining in the soil matrix. We propose the use of solid phase fluorescence on whole soils as a potential tool to look at the composition of organic matter without the extraction bias and gain a more complete understand of the potential for fluorescence as a tool in terrestrial studies. To date, the limited applications of solid phase fluorescence have ranged from food and agriculture to pharmaceutical with no clearly defined methods and limitations available. We are aware of no other studies that use solid phase fluorescence and thus no clear methods to look at SOM across a diverse set of soil types and ecosystems. With this new approach to fluorescence spectroscopy there are new challenges, such as blank correction, inner filter effect corrections, and sample preparation. This work outlines a novel method for analyzing soil organic matter using solid phase fluorescence across a wide range of soils collected from the National Ecological Observatory Network (NEON) eco-domains. This method has shown that organic matter content in soils must be diluted to 2% to reduce backscattering and oversaturation of the detector in forested soils. In mineral horizons (A) there is observed quenching of the humic-like organic matter, which is likely a result of organo-mineral complexation. Finally, we present preliminary comparisons between solid and liquid phase

  6. Development of a solid-phase assay for measurement of proteolytic enzyme activity

    Varani, J.; Johnson, K.; Kaplan, J.

    1980-01-01

    A solid-phase, plate assay was developed for the measurement of proteolytic enzyme activity. In this assay procedure, radiolabeled substrates were dried onto the surface of microtiter wells. Following drying, the wells were washed two times with saline to remove the nonadherent substrate. When proteolytic enzymes were added to the wells, protein hydrolysis occurred, releasing radioactivity into the supernatant fluid. The amount of protein hydrolysis that occurred was reflected by the amount of radioactivity in the supernatant fluid. When 125 I-hemoglobin was used as the substrate, it was as susceptible to hydrolysis by trypsin in the solid-phase assay as it was in solution in a standard assay procedure. Protease activity from a variety of sources (including from viable cells as well as from extracellular sources) were also able to hydrolyze the hemoglobin on the plate. 125 I-Labeled serum albumen, fibrinogen, and rat pulmonary basement membrane were also susceptible to hydrolysis by trypsin in the solid phase. When [ 14 C]elastin was dried onto the plate, it behaved in a similar manner to elastin in solution. It was resistant to hydrolysis by nonspecific proteases such as trypsin and chymotrypsin but was highly susceptible to hydrolysis by elastase. The solid-phase plate assay has several features which recommended it for routine use. It is as sensitive as standard tube assays (and much more sensitive than routinely used colormetric assays). It is quick and convenient; there are no precipitation, centrifugation, or filtration steps. In addition, very small volumes of radioactive wastes are generated. Another advantage of the solid-phase plate assay is the resistance of the dried substrates to spontaneous breakdown and to microbial contamination. Finally, this assay is suitable for use with viable cells as well as for extracellular proteases

  7. The study of long-term stability in liquid-solid phases for HLW disposal

    Wei, Y.Y.; Tseng, C.L.; Yang, J.Y.; Ke, C.H.; Wang, T.H.; Jan, Y.L.; Lee, C.B.; Lan, P.L.; Hsu, C.N.; Tsai, S.C.; Li, M.H.; Teng, S.P.

    2005-01-01

    Full text of publication follows: This study is conducted to observe changes in both chemical properties of buffer materials and liquid phases over an experimental period of 2 years. In our experiments, bentonite powder and crushed granite are separately mixed with synthetic groundwater, synthetic seawater and de-ionised water at a fixed liquid-solid ratio of 30. A mixed set with both bentonite and granite together as solid phase is also investigated. During this study, aliquots of the liquid phases are sampled every two months and pH and Eh values are measured immediately. Concentrations of Na, Mg, K, Al, Ca, Ti, Mn, Ba, Fe, Sr, Li and Th are analyzed in the liquid phase directly by ICP-AES. After separation by centrifugation followed by freeze drying and digestion, the solid phases are analyzed as well for elemental composition. Alteration of solid phases during the experimental period is discussed. The preliminary results show that the pH values of the three solutions vary considerably in the individual experimental systems containing bentonite, granite or the mixed system. In general, higher pH values are found in DI-water for all solid phases. Eh values fluctuate a lot in the range 100 to 300 mV in all experiment sets. Different to the experiments with granite for which similar Eh values are found in all solutions, a significantly different Eh-value is found in the experiment with bentonite in DI-water as compared to the other solutions. The results from element analysis indicate that equilibrium is achieved after only two months and element concentrations change only slightly thereafter. We conclude from our experiments that both bentonite and granite keep their characteristics as radionuclide sorbents in the vicinity of a nuclear waste repository. Reaction equilibria appear to be attained rapidly. Because there are just a few alterations in this study, it would be a huge error source in analyzing from the inhomogeneous solid phase such as granite and losses

  8. Micro-channel heat sink with slurry of water with micro-encapsulated phase change material: 3D-numerical study

    Sabbah, Rami; Farid, Mohammad M.; Al-Hallaj, Said

    2009-01-01

    This study investigates the influence of using micro-encapsulated phase change material (MEPCM) on the thermal and hydraulic performance of micro-channel heat sinks used for heat dissipation of high power electronic devices. A three-dimensional, one-phase, laminar flow model of a rectangular channel using water slurry of MEPCM with temperature dependent physical properties was developed. The results showed a significant increase in the heat transfer coefficient under certain conditions for heat flux rates of 100 W/cm 2 and 500 W/cm 2 that is mainly dependant on the channel inlet and outlet temperatures and the selected MEPCM melting temperature. Lower and more uniform temperatures across the electronic device can be achieved at less pumping power compared to using water only as the cooling fluid

  9. Numerical evaluation of micro-structural parameters of porous supports in metal-supported solid oxide fuel cells

    Reiss, Georg; Frandsen, Henrik Lund; Brandstätter, Wilhelm

    2014-01-01

    Metallic supported Solid Oxide Fuel Cells (SOFCs) are considered as a durable and cost effective alternative to the state-of-the-art ceramic supported cell designs. In order to understand the mass and charge transport in the metal-support of this new type of cell a novel technique involving X......-ray tomography and micro-structural modelling is presented in this work. The simulation technique comprises a novel treatment of the boundary conditions, which leads to more accurate effective transport parameters compared to those, which can be achieved with the conventional homogenisation procedures....... Furthermore, the porosity distribution in the metal-support was determined, which provided information about the inhomogeneous nature of the material. In addition to that, transport parameters for two identified, different dense layers of the metal-support are evaluated separately. The results...

  10. Phase-field model of vapor-liquid-solid nanowire growth

    Wang, Nan; Upmanyu, Moneesh; Karma, Alain

    2018-03-01

    We present a multiphase-field model to describe quantitatively nanowire growth by the vapor-liquid-solid (VLS) process. The free-energy functional of this model depends on three nonconserved order parameters that distinguish the vapor, liquid, and solid phases and describe the energetic properties of various interfaces, including arbitrary forms of anisotropic γ plots for the solid-vapor and solid-liquid interfaces. The evolution equations for those order parameters describe basic kinetic processes including the rapid (quasi-instantaneous) equilibration of the liquid catalyst to a droplet shape with constant mean curvature, the slow incorporation of growth atoms at the droplet surface, and crystallization within the droplet. The standard constraint that the sum of the phase fields equals unity and the conservation of the number of catalyst atoms, which relates the catalyst volume to the concentration of growth atoms inside the droplet, are handled via separate Lagrange multipliers. An analysis of the model is presented that rigorously maps the phase-field equations to a desired set of sharp-interface equations for the evolution of the phase boundaries under the constraint of force balance at three-phase junctions (triple points) given by the Young-Herring relation that includes torque term related to the anisotropy of the solid-liquid and solid-vapor interface excess free energies. Numerical examples of growth in two dimensions are presented for the simplest case of vanishing crystalline anisotropy and the more realistic case of a solid-liquid γ plot with cusped minima corresponding to two sets of (10 ) and (11 ) facets. The simulations reproduce many of the salient features of nanowire growth observed experimentally, including growth normal to the substrate with tapering of the side walls, transitions between different growth orientations, and crawling growth along the substrate. They also reproduce different observed relationships between the nanowire growth

  11. Phase diagram of nanoscale alloy particles used for vapor-liquid-solid growth of semiconductor nanowires.

    Sutter, Eli; Sutter, Peter

    2008-02-01

    We use transmission electron microscopy observations to establish the parts of the phase diagram of nanometer sized Au-Ge alloy drops at the tips of Ge nanowires (NWs) that determine their temperature-dependent equilibrium composition and, hence, their exchange of semiconductor material with the NWs. We find that the phase diagram of the nanoscale drop deviates significantly from that of the bulk alloy, which explains discrepancies between actual growth results and predictions on the basis of the bulk-phase equilibria. Our findings provide the basis for tailoring vapor-liquid-solid growth to achieve complex one-dimensional materials geometries.

  12. Homogeneous nucleation in phase separation of solid 3He-4He mixtures

    Poole, M.; Smith, A.; Maidanov, V.A.; Rudavskii, E.Ya.; Grigor'ev, V.N.; Slezov, V.V.; Saunders, J.; Cowan, B.

    2003-01-01

    NMR and pressure have been measured during phase separation in solid 3 He- 4 He mixtures. Spin echoes were used to observe bounded diffusion and to estimate the diffusion coefficient, size and nuclei concentration in the 3 He-enriched phase. The characteristic phase separation time constant of the mixture was found from pressure measurements. The results argue convincingly for homogeneous nucleation. The surface tension of the nuclei is found independently from NMR and from pressure measurements; the two determinations agree well and yield a surface tension coefficient of 4.9x10 -6 J m -2

  13. The mechanism of reequilibration of solids in the presence of a fluid phase

    Putnis, Andrew; Putnis, Christine V.

    2007-01-01

    The preservation of morphology (pseudomorphism) and crystal structure during the transformation of one solid phase to another is regularly used as a criterion for a solid-state mechanism, even when there is a fluid phase present. However, a coupled dissolution-reprecipitation mechanism also preserves the morphology and transfers crystallographic information from parent to product by epitaxial nucleation. The generation of porosity in the product phase is a necessary condition for such a mechanism as it allows fluid to maintain contact with a reaction interface which moves through the parent phase from the original surface. We propose that interface-coupled dissolution-reprecipitation is a general mechanism for reequilibration of solids in the presence of a fluid phase. - Graphical abstract: A single crystal of KBr is transformed to a porous single crystal of KCl by immersion in saturated KCl solution. The image shows partial transformation of a crystal of KBr (core) to KCl (porous, milky rim) by an interface coupled dissolution-reprecipitation mechanism. The external dimensions and crystallographic orientation of the original crystal are preserved, while a reaction interface moves through the crystal

  14. Investigation of solid-phase hydrogenation of amino acids and peptides

    Zolotarev, Yu.A.; Myasoedov, N.F.; Zajtsev, D.A.; Lubnin, M.Yu.; Tatur, V.Yu.; Kozik, V.S.; Dorokhova, E.M.; Rozenberg, S.N.

    1990-01-01

    The possibility of synthesizing amino acids and peptides multiply labelled with tritium or deuterium by the method of solid-phase isotopic exchange with gaseous hydrogen isotopes was verified. Establishment of the isotopic hydrogen equilibrium between the gaseous phase and the solid phase formed by the amino acid molecules was found experimentally. The activation energy of the isotopic exchange is 13 kcal/mol. A mathematical model was set up for the isotopic exchange with a probable substitution of hydrogen atoms. Uniformly labelled amino acids were obtained in a high optical purity and with 80 to 90% hydrogen substitution by deuterium and tritium. Tritiated peptides were prepared in high yields at molar activities of 1.5 to 3.7 TBq/mmol. (author). 4 tabs

  15. Insights into metals in individual fine particles from municipal solid waste using synchrotron radiation-based micro-analytical techniques.

    Zhu, Yumin; Zhang, Hua; Shao, Liming; He, Pinjing

    2015-01-01

    Excessive inter-contamination with heavy metals hampers the application of biological treatment products derived from mixed or mechanically-sorted municipal solid waste (MSW). In this study, we investigated fine particles of heavy metal content, using bulk detection techniques. A total of 17 individual fine particles were evaluated using synchrotron radiation-based micro-X-ray fluorescence and micro-X-ray diffraction. We also discussed the association, speciation and source apportionment of heavy metals. Metals were found to exist in a diffuse distribution with heterogeneous intensities and intense hot-spots of metals revealed the potential sources of fine particles from size-reduced waste fractions (such as scraps of organic wastes or ceramics) or from the importation of other particles. The diverse sources of heavy metal pollutants within the fine particles suggested that separate collection and treatment of the biodegradable waste fraction (such as food waste) is a preferable means of facilitating the beneficial utilization of the stabilized products. Copyright © 2014. Published by Elsevier B.V.

  16. Optimisation of a propagation-based x-ray phase-contrast micro-CT system

    Nesterets, Yakov I.; Gureyev, Timur E.; Dimmock, Matthew R.

    2018-03-01

    Micro-CT scanners find applications in many areas ranging from biomedical research to material sciences. In order to provide spatial resolution on a micron scale, these scanners are usually equipped with micro-focus, low-power x-ray sources and hence require long scanning times to produce high resolution 3D images of the object with acceptable contrast-to-noise. Propagation-based phase-contrast tomography (PB-PCT) has the potential to significantly improve the contrast-to-noise ratio (CNR) or, alternatively, reduce the image acquisition time while preserving the CNR and the spatial resolution. We propose a general approach for the optimisation of the PB-PCT imaging system. When applied to an imaging system with fixed parameters of the source and detector this approach requires optimisation of only two independent geometrical parameters of the imaging system, i.e. the source-to-object distance R 1 and geometrical magnification M, in order to produce the best spatial resolution and CNR. If, in addition to R 1 and M, the system parameter space also includes the source size and the anode potential this approach allows one to find a unique configuration of the imaging system that produces the required spatial resolution and the best CNR.

  17. Transport mechanisms and wetting dynamics in molecularly thin films of long-chain alkanes at solid/vapour interface : relation to the solid-liquid phase transition

    Lazar, Paul

    2005-01-01

    Wetting and phase transitions play a very important role our daily life. Molecularly thin films of long-chain alkanes at solid/vapour interfaces (e.g. C30H62 on silicon wafers) are very good model systems for studying the relation between wetting behaviour and (bulk) phase transitions. Immediately above the bulk melting temperature the alkanes wet partially the surface (drops). In this temperature range the substrate surface is covered with a molecularly thin ordered, solid-like alkane film (...

  18. A Variational Model for Two-Phase Immiscible Electroosmotic Flow at Solid Surfaces

    Shao, Sihong

    2012-01-01

    We develop a continuum hydrodynamic model for two-phase immiscible flows that involve electroosmotic effect in an electrolyte and moving contact line at solid surfaces. The model is derived through a variational approach based on the Onsager principle of minimum energy dissipation. This approach was first presented in the derivation of a continuum hydrodynamic model for moving contact line in neutral two-phase immiscible flows (Qian, Wang, and Sheng, J. Fluid Mech. 564, 333-360 (2006)). Physically, the electroosmotic effect can be formulated by the Onsager principle as well in the linear response regime. Therefore, the same variational approach is applied here to the derivation of the continuum hydrodynamic model for charged two-phase immiscible flows where one fluid component is an electrolyte exhibiting electroosmotic effect on a charged surface. A phase field is employed to model the diffuse interface between two immiscible fluid components, one being the electrolyte and the other a nonconductive fluid, both allowed to slip at solid surfaces. Our model consists of the incompressible Navier-Stokes equation for momentum transport, the Nernst-Planck equation for ion transport, the Cahn-Hilliard phase-field equation for interface motion, and the Poisson equation for electric potential, along with all the necessary boundary conditions. In particular, all the dynamic boundary conditions at solid surfaces, including the generalized Navier boundary condition for slip, are derived together with the equations of motion in the bulk region. Numerical examples in two-dimensional space, which involve overlapped electric double layer fields, have been presented to demonstrate the validity and applicability of the model, and a few salient features of the two-phase immiscible electroosmotic flows at solid surface. The wall slip in the vicinity of moving contact line and the Smoluchowski slip in the electric double layer are both investigated. © 2012 Global-Science Press.

  19. Carbon nanotubes as adsorbent of solid-phase extraction and matrix for laser desorption/ionization mass spectrometry.

    Pan, Chensong; Xu, Songyun; Zou, Hanfa; Guo, Zhong; Zhang, Yu; Guo, Baochuan

    2005-02-01

    A method with carbon nanotubes functioning both as the adsorbent of solid-phase extraction (SPE) and the matrix for matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS) to analyze small molecules in solution has been developed. In this method, 10 microL suspensions of carbon nanotubes in 50% (vol/vol) methanol were added to the sample solution to extract analytes onto surface of carbon nanotubes because of their dramatic hydrophobicity. Carbon nanotubes in solution are deposited onto the bottom of tube with centrifugation. After removing the supernatant fluid, carbon nanotubes are suspended again with dispersant and pipetted directly onto the sample target of the MALDI-MS to perform a mass spectrometric analysis. It was demonstrated by analysis of a variety of small molecules that the resolution of peaks and the efficiency of desorption/ionization on the carbon nanotubes are better than those on the activated carbon. It is found that with the addition of glycerol and sucrose to the dispersant, the intensity, the ratio of signal to noise (S/N), and the resolution of peaks for analytes by mass spectrometry increased greatly. Compared with the previously reported method by depositing sample solution onto thin layer of carbon nanotubes, it is observed that the detection limit for analytes can be enhanced about 10 to 100 times due to solid-phase extraction of analytes in solution by carbon nanotubes. An acceptable result of simultaneously quantitative analysis of three analytes in solution has been achieved. The application in determining drugs spiked into urine has also been realized.

  20. Electron probe micro-analysis of gas bubbles in solids: a novel approach

    Verwerft, M.; Vos, B.

    1999-01-01

    The local analysis of retained noble gas in nuclear fuel is inherently difficult since the physical form under which it is stored varies from atomically dispersed to bubbles with a diameter of several hundreds of nanometers. One of the techniques that has been applied since pore than twenty years is EPMA. Although many important results have been obtained with this technique, its application to the analysis of highly inhomogeneous materials is limited. The EPMA technique is indeed difficult to apply to samples that are not homogeneous on the scale of the electron-solid interaction volume. The paper discusses the development of a method to analyse a system of as bubbles distributed in a solid matrix. This method has been based on a multiple voltage EPMA measurement combined with a scanning Electron Microscopic analysis of the bubble size distribution