Mixed-mode isolation of triazine metabolites from soil and aquifer sediments using automated solid-phase extraction

USGS Publications Warehouse

Mills, M.S.; Thurman, E.M.

1992-01-01

Reversed-phase isolation and ion-exchange purification were combined in the automated solid-phase extraction of two polar s-triazine metabolites, 2-amino-4-chloro-6-(isopropylamino)-s-triazine (deethylatrazine) and 2-amino-4-chloro-6-(ethylamino)-s-triazine (deisopropylatrazine) from clay-loam and slit-loam soils and sandy aquifer sediments. First, methanol/ water (4/1, v/v) soil extracts were transferred to an automated workstation following evaporation of the methanol phase for the rapid reversed-phase isolation of the metabolites on an octadecylresin (C18). The retention of the triazine metabolites on C18 decreased substantially when trace methanol concentrations (1%) remained. Furthermore, the retention on C18 increased with decreasing aqueous solubility and increasing alkyl-chain length of the metabolites and parent herbicides, indicating a reversed-phase interaction. The analytes were eluted with ethyl acetate, which left much of the soil organic-matter impurities on the resin. Second, the small-volume organic eluate was purified on an anion-exchange resin (0.5 mL/min) to extract the remaining soil pigments that could foul the ion source of the GC/MS system. Recoveries of the analytes were 75%, using deuterated atrazine as a surrogate, and were comparable to recoveries by soxhlet extraction. The detection limit was 0.1 ??g/kg with a coefficient of variation of 15%. The ease and efficiency of this automated method makes it viable, practical technique for studying triazine metabolites in the environment.

Automated synthesis of arabinoxylan-oligosaccharides enables characterization of antibodies that recognize plant cell wall glycans.

PubMed

Schmidt, Deborah; Schuhmacher, Frank; Geissner, Andreas; Seeberger, Peter H; Pfrengle, Fabian

2015-04-07

Monoclonal antibodies that recognize plant cell wall glycans are used for high-resolution imaging, providing important information about the structure and function of cell wall polysaccharides. To characterize the binding epitopes of these powerful molecular probes a library of eleven plant arabinoxylan oligosaccharides was produced by automated solid-phase synthesis. Modular assembly of oligoarabinoxylans from few building blocks was enabled by adding (2-naphthyl)methyl (Nap) to the toolbox of orthogonal protecting groups for solid-phase synthesis. Conjugation-ready oligosaccharides were obtained and the binding specificities of xylan-directed antibodies were determined on microarrays. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Column Liquid Chromatography.

ERIC Educational Resources Information Center

Majors, Ronald E.; And Others

1984-01-01

Reviews literature covering developments of column liquid chromatography during 1982-83. Areas considered include: books and reviews; general theory; columns; instrumentation; detectors; automation and data handling; multidimensional chromatographic and column switching techniques; liquid-solid chromatography; normal bonded-phase, reversed-phase,…

Emerging Environmental Contaminants and Soled Phase Microextraction: Janusz Pawliszyn's Legacy in the Environmental Arena

EPA Science Inventory

Solid phase microextraction (SPME) has revolutionized the way samples are extracted, enabling rapid, automated, and solventless extraction of many different sample types, including air, water, soil, and biological samples. As such, SPME is widely used for environmental, food, fo...

Automated solid-phase subcloning based on beads brought into proximity by magnetic force.

PubMed

Hudson, Elton P; Nikoshkov, Andrej; Uhlen, Mathias; Rockberg, Johan

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 the gene are immobilized to separate paramagnetic beads and brought into proximity by magnetic force. Ligation events were directly evaluated using fluorescent-based microscopy and flow cytometry. The highest ligation efficiencies were obtained when gene- and vector-coated beads were brought into close contact by application of a magnet during the ligation step. An automated procedure was developed using a laboratory workstation to transfer genes into various expression vectors and more than 95% correct clones were obtained in a number of various applications. The method presented here is suitable for efficient subcloning in an automated manner to rapidly generate a large number of gene constructs in various vectors intended for high throughput applications.

Automated Solid-Phase Subcloning Based on Beads Brought into Proximity by Magnetic Force

PubMed Central

Hudson, Elton P.; Nikoshkov, Andrej; Uhlen, Mathias; Rockberg, Johan

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 the gene are immobilized to separate paramagnetic beads and brought into proximity by magnetic force. Ligation events were directly evaluated using fluorescent-based microscopy and flow cytometry. The highest ligation efficiencies were obtained when gene- and vector-coated beads were brought into close contact by application of a magnet during the ligation step. An automated procedure was developed using a laboratory workstation to transfer genes into various expression vectors and more than 95% correct clones were obtained in a number of various applications. The method presented here is suitable for efficient subcloning in an automated manner to rapidly generate a large number of gene constructs in various vectors intended for high throughput applications. PMID:22624028

Solid-Phase Extraction Strategies to Surmount Body Fluid Sample Complexity in High-Throughput Mass Spectrometry-Based Proteomics

PubMed Central

Bladergroen, Marco R.; van der Burgt, Yuri E. M.

2015-01-01

For large-scale and standardized applications in mass spectrometry- (MS-) based proteomics automation of each step is essential. Here we present high-throughput sample preparation solutions for balancing the speed of current MS-acquisitions and the time needed for analytical workup of body fluids. The discussed workflows reduce body fluid sample complexity and apply for both bottom-up proteomics experiments and top-down protein characterization approaches. Various sample preparation methods that involve solid-phase extraction (SPE) including affinity enrichment strategies have been automated. Obtained peptide and protein fractions can be mass analyzed by direct infusion into an electrospray ionization (ESI) source or by means of matrix-assisted laser desorption ionization (MALDI) without further need of time-consuming liquid chromatography (LC) separations. PMID:25692071

The current role of on-line extraction approaches in clinical and forensic toxicology.

PubMed

Mueller, Daniel M

2014-08-01

In today's clinical and forensic toxicological laboratories, automation is of interest because of its ability to optimize processes, to reduce manual workload and handling errors and to minimize exposition to potentially infectious samples. Extraction is usually the most time-consuming step; therefore, automation of this step is reasonable. Currently, from the field of clinical and forensic toxicology, methods using the following on-line extraction techniques have been published: on-line solid-phase extraction, turbulent flow chromatography, solid-phase microextraction, microextraction by packed sorbent, single-drop microextraction and on-line desorption of dried blood spots. Most of these published methods are either single-analyte or multicomponent procedures; methods intended for systematic toxicological analysis are relatively scarce. However, the use of on-line extraction will certainly increase in the near future.

Determination of Low Concentrations of Acetochlor in Water by Automated Solid-Phase Extraction and Gas Chromatography with Mass-Selective Detection

USGS Publications Warehouse

Lindley, C.E.; Stewart, J.T.; Sandstrom, M.W.

1996-01-01

A sensitive and reliable gas chromatographic/mass spectrometric (GC/MS) method for determining acetochlor in environmental water samples was developed. The method involves automated extraction of the herbicide from a filtered 1 L water sample through a C18 solid-phase extraction column, elution from the column with hexane-isopropyl alcohol (3 + 1), and concentration of the extract with nitrogen gas. The herbicide is quantitated by capillary/column GC/MS with selected-ion monitoring of 3 characteristic ions. The single-operator method detection limit for reagent water samples is 0.0015 ??g/L. Mean recoveries ranged from about 92 to 115% for 3 water matrixes fortified at 0.05 and 0.5 ??g/L. Average single-operator precision, over the course of 1 week, was better than 5%.

Recent Approaches Toward Solid Phase Synthesis of β-Lactams

NASA Astrophysics Data System (ADS)

Mandal, Bablee; Ghosh, Pranab; Basu, Basudeb

Since the discovery of penicillin in 1929, β-lactam antibiotics have been recognized as potentially chemotherapeutic drugs of incomparable effectiveness, conjugating a broad spectrum of activity with very low toxicity. The primary motif azetidin-2-one ring (β-lactam) has been considered as specific pharmacophores and scaffolds. With the advent of combinatorial chemistry and automated parallel synthesis coupled with ample interests from the pharmaceutical industries, recent trends have been driven mostly by adopting solid phase techniques and polymer-supported synthesis of β-lactams. The present survey will present an overview of the developments on the polymer-supported and solid phase techniques for the preparation of β-lactam ring or β-lactam containing antibiotics published over the last decade. Both unsubstituted and substitutions with different functional groups at various positions of β-lactams have been synthesized using solid phase technology. However, Wang resin and application of Staudinger [2+2] cycloaddition reaction have remained hitherto the major choice. It may be expected that other solid phase approaches involving different resins would be developed in the coming years.

Automated sample preparation using membrane microtiter extraction for bioanalytical mass spectrometry.

PubMed

Janiszewski, J; Schneider, P; Hoffmaster, K; Swyden, M; Wells, D; Fouda, H

1997-01-01

The development and application of membrane solid phase extraction (SPE) in 96-well microtiter plate format is described for the automated analysis of drugs in biological fluids. The small bed volume of the membrane allows elution of the analyte in a very small solvent volume, permitting direct HPLC injection and negating the need for the time consuming solvent evaporation step. A programmable liquid handling station (Quadra 96) was modified to automate all SPE steps. To avoid drying of the SPE bed and to enhance the analytical precision a novel protocol for performing the condition, load and wash steps in rapid succession was utilized. A block of 96 samples can now be extracted in 10 min., about 30 times faster than manual solvent extraction or single cartridge SPE methods. This processing speed complements the high-throughput speed of contemporary high performance liquid chromatography mass spectrometry (HPLC/MS) analysis. The quantitative analysis of a test analyte (Ziprasidone) in plasma demonstrates the utility and throughput of membrane SPE in combination with HPLC/MS. The results obtained with the current automated procedure compare favorably with those obtained using solvent and traditional solid phase extraction methods. The method has been used for the analysis of numerous drug prototypes in biological fluids to support drug discovery efforts.

Investigation of the automated solid-phase synthesis of a 38mer peptide with difficult sequence pattern under different synthesis strategies.

PubMed

Winkler, Dirk F H; Tian, Kerry

2015-04-01

Difficult peptides are a constant challenge in solid-phase peptide synthesis. In particular, hydroxyl amino acids such as serine can cause severe breakdowns in coupling yields even several amino acids after the insertion of the critical amino acid. This paper investigates several methods of improving synthesis yields of difficult peptides including the use of different resins, activators and the incorporation of a structure-breaking pseudoproline dipeptide building block both alone and in combination with each other.

Automated solid-phase extraction workstations combined with quantitative bioanalytical LC/MS.

PubMed

Huang, N H; Kagel, J R; Rossi, D T

1999-03-01

An automated solid-phase extraction workstation was used to develop, characterize and validate an LC/MS/MS method for quantifying a novel lipid-regulating drug in dog plasma. Method development was facilitated by workstation functions that allowed wash solvents of varying organic composition to be mixed and tested automatically. Precision estimates for this approach were within 9.8% relative standard deviation (RSD) across the calibration range. Accuracy for replicate determinations of quality controls was between -7.2 and +6.2% relative error (RE) over 5-1,000 ng/ml(-1). Recoveries were evaluated for a wide variety of wash solvents, elution solvents and sorbents. Optimized recoveries were generally > 95%. A sample throughput benchmark for the method was approximately equal 8 min per sample. Because of parallel sample processing, 100 samples were extracted in less than 120 min. The approach has proven useful for use with LC/MS/MS, using a multiple reaction monitoring (MRM) approach.

Automated solid-phase extraction of phenolic acids using layered double hydroxide-alumina-polymer disks.

PubMed

Ghani, Milad; Palomino Cabello, Carlos; Saraji, Mohammad; Manuel Estela, Jose; Cerdà, Víctor; Turnes Palomino, Gemma; Maya, Fernando

2018-01-26

The application of layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks for solid-phase extraction is reported for the first time. Al 2 O 3 is embedded in a polymer matrix followed by an in situ metal-exchange process to obtain a layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disk with excellent flow-through properties. The extraction performance of the prepared disks is evaluated as a proof of concept for the automated extraction using sequential injection analysis of organic acids (p-hydroxybenzoic acid, 3,4-dihydroxybenzoic acid, gallic acid) following an anion-exchange mechanism. After the solid-phase extraction, phenolic acids were quantified by reversed-phase high-performance liquid chromatography with diode-array detection using a core-shell silica-C18 stationary phase and isocratic elution (acetonitrile/0.5% acetic acid in pure water, 5:95, v/v). High sensitivity and reproducibility were obtained with limits of detection in the range of 0.12-0.25 μg/L (sample volume, 4 mL), and relative standard deviations between 2.9 and 3.4% (10 μg/L, n = 6). Enrichment factors of 34-39 were obtained. Layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks had an average lifetime of 50 extractions. Analyte recoveries ranged from 93 to 96% for grape juice and nonalcoholic beer samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid-Phase Synthesis of Molecularly Imprinted Polymer Nanoparticles with a Reusable Template - "Plastic Antibodies".

PubMed

Poma, Alessandro; Guerreiro, Antonio; Whitcombe, Michael J; Piletska, Elena V; Turner, Anthony P F; Piletsky, Sergey A

2013-06-13

Molecularly Imprinted Polymers (MIPs) are generic alternatives to antibodies in sensors, diagnostics and separations. To displace biomolecules without radical changes in infrastructure in device manufacture, MIPs should share their characteristics (solubility, size, specificity and affinity, localized binding domain) whilst maintaining the advantages of MIPs (low-cost, short development time and high stability) hence the interest in MIP nanoparticles. Herein we report a reusable solid-phase template approach (fully compatible with automation) for the synthesis of MIP nanoparticles and their precise manufacture using a prototype automated UV photochemical reactor. Batches of nanoparticles (30-400 nm) with narrow size distributions imprinted with: melamine (d = 60 nm, K d = 6.3 × 10 -8 m), vancomycin (d = 250 nm, K d = 3.4 × 10 -9 m), a peptide (d = 350 nm, K d = 4.8 × 10 -8 m) and proteins have been produced. Our instrument uses a column packed with glass beads, bearing the template. Process parameters are under computer control, requiring minimal manual intervention. For the first time we demonstrate the reliable re-use of molecular templates in the synthesis of MIPs (≥ 30 batches of nanoMIPs without loss of performance). NanoMIPs are produced template-free and the solid-phase acts both as template and affinity separation medium.

Solid-Phase Synthesis of Molecularly Imprinted Polymer Nanoparticles with a Reusable Template – “Plastic Antibodies”

PubMed Central

Poma, Alessandro; Guerreiro, Antonio; Whitcombe, Michael J.; Piletska, Elena V.; Turner, Anthony P.F.; Piletsky, Sergey A.

2016-01-01

Molecularly Imprinted Polymers (MIPs) are generic alternatives to antibodies in sensors, diagnostics and separations. To displace biomolecules without radical changes in infrastructure in device manufacture, MIPs should share their characteristics (solubility, size, specificity and affinity, localized binding domain) whilst maintaining the advantages of MIPs (low-cost, short development time and high stability) hence the interest in MIP nanoparticles. Herein we report a reusable solid-phase template approach (fully compatible with automation) for the synthesis of MIP nanoparticles and their precise manufacture using a prototype automated UV photochemical reactor. Batches of nanoparticles (30-400 nm) with narrow size distributions imprinted with: melamine (d = 60 nm, Kd = 6.3 × 10−8 m), vancomycin (d = 250 nm, Kd = 3.4 × 10−9 m), a peptide (d = 350 nm, Kd = 4.8 × 10−8 m) and proteins have been produced. Our instrument uses a column packed with glass beads, bearing the template. Process parameters are under computer control, requiring minimal manual intervention. For the first time we demonstrate the reliable re-use of molecular templates in the synthesis of MIPs (≥ 30 batches of nanoMIPs without loss of performance). NanoMIPs are produced template-free and the solid-phase acts both as template and affinity separation medium. PMID:26869870

Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD) and Dispersive Solid Phase Extraction (d-SPE) of Plant Samples

PubMed Central

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

Revisiting low-fidelity two-fluid models for gas-solids transport

NASA Astrophysics Data System (ADS)

Adeleke, Najeem; Adewumi, Michael; Ityokumbul, Thaddeus

2016-08-01

Two-phase gas-solids transport models are widely utilized for process design and automation in a broad range of industrial applications. Some of these applications include proppant transport in gaseous fracking fluids, air/gas drilling hydraulics, coal-gasification reactors and food processing units. Systems automation and real time process optimization stand to benefit a great deal from availability of efficient and accurate theoretical models for operations data processing. However, modeling two-phase pneumatic transport systems accurately requires a comprehensive understanding of gas-solids flow behavior. In this study we discuss the prevailing flow conditions and present a low-fidelity two-fluid model equation for particulate transport. The model equations are formulated in a manner that ensures the physical flux term remains conservative despite the inclusion of solids normal stress through the empirical formula for modulus of elasticity. A new set of Roe-Pike averages are presented for the resulting strictly hyperbolic flux term in the system of equations, which was used to develop a Roe-type approximate Riemann solver. The resulting scheme is stable regardless of the choice of flux-limiter. The model is evaluated by the prediction of experimental results from both pneumatic riser and air-drilling hydraulics systems. We demonstrate the effect and impact of numerical formulation and choice of numerical scheme on model predictions. We illustrate the capability of a low-fidelity one-dimensional two-fluid model in predicting relevant flow parameters in two-phase particulate systems accurately even under flow regimes involving counter-current flow.

Chromatographic Separations Using Solid-Phase Extraction Cartridges: Separation of Wine Phenolics

NASA Astrophysics Data System (ADS)

Brenneman, Charles A.; Ebeler, Susan E.

1999-12-01

We describe a simple laboratory experiment that demonstrates the principles of chromatographic separation using solid-phase extraction columns and red wine. By adjusting pH and mobile phase composition, the wine is separated into three fractions of differing polarity. The content of each fraction can be monitored by UV-vis spectroscopy. When the experiment is combined with experiments involving HPLC or GC separations, students gain a greater appreciation for and understanding of the highly automated instrumental systems currently available. In addition, they learn about the chemistry of polyphenolic compounds, which are present in many foods and beverages and which are receiving much attention for their potentially beneficial health effects.

Differential Profiling of Volatile Organic Compound Biomarker Signatures Utilizing a Logical Statistical Filter-Set and Novel Hybrid Evolutionary Classifiers

DTIC Science & Technology

2012-04-01

for automated SPME headspace sampling and in-line with a Thermo DSQII single quadrupole mass spectrometer. Collection of organic volatiles from the...urine was accomplished using a 2cm CAR/DVB/PDMS solid phase micro extraction fiber ( SPME ), Supelco supplier, inserted by the Triplus autosampler into...automated direct injection. Volatiles gathered by the SPME fiber were analyzed through desorption of the fiber by heating to elevated temperature and

Automated processing of whole blood samples for the determination of immunosuppressants by liquid chromatography tandem-mass spectrometry.

PubMed

Vogeser, Michael; Spöhrer, Ute

2006-01-01

Liquid chromatography tandem-mass spectrometry (LC-MS/MS) is an efficient technology for routine determination of immunosuppressants in whole blood; however, time-consuming manual sample preparation remains a significant limitation of this technique. Using a commercially available robotic pipetting system (Tecan Freedom EVO), we developed an automated sample-preparation protocol for quantification of tacrolimus in whole blood by LC-MS/MS. Barcode reading, sample resuspension, transfer of whole blood aliquots into a deep-well plate, addition of internal standard solution, mixing, and protein precipitation by addition of an organic solvent is performed by the robotic system. After centrifugation of the plate, the deproteinized supernatants are submitted to on-line solid phase extraction, using column switching prior to LC-MS/MS analysis. The only manual actions within the entire process are decapping of the tubes, and transfer of the deep-well plate from the robotic system to a centrifuge and finally to the HPLC autosampler. Whole blood pools were used to assess the reproducibility of the entire analytical system for measuring tacrolimus concentrations. A total coefficient of variation of 1.7% was found for the entire automated analytical process (n=40; mean tacrolimus concentration, 5.3 microg/L). Close agreement between tacrolimus results obtained after manual and automated sample preparation was observed. The analytical system described here, comprising automated protein precipitation, on-line solid phase extraction and LC-MS/MS analysis, is convenient and precise, and minimizes hands-on time and the risk of mistakes in the quantification of whole blood immunosuppressant concentrations compared to conventional methods.

Review of high-throughput techniques for detecting solid phase Transformation from material libraries produced by combinatorial methods

NASA Technical Reports Server (NTRS)

Lee, Jonathan A.

2005-01-01

High-throughput measurement techniques are reviewed for solid phase transformation from materials produced by combinatorial methods, which are highly efficient concepts to fabricate large variety of material libraries with different compositional gradients on a single wafer. Combinatorial methods hold high potential for reducing the time and costs associated with the development of new materials, as compared to time-consuming and labor-intensive conventional methods that test large batches of material, one- composition at a time. These high-throughput techniques can be automated to rapidly capture and analyze data, using the entire material library on a single wafer, thereby accelerating the pace of materials discovery and knowledge generation for solid phase transformations. The review covers experimental techniques that are applicable to inorganic materials such as shape memory alloys, graded materials, metal hydrides, ferric materials, semiconductors and industrial alloys.

An Automated High-Throughput System to Fractionate Plant Natural Products for Drug Discovery

PubMed Central

Tu, Ying; Jeffries, Cynthia; Ruan, Hong; Nelson, Cynthia; Smithson, David; Shelat, Anang A.; Brown, Kristin M.; Li, Xing-Cong; Hester, John P.; Smillie, Troy; Khan, Ikhlas A.; Walker, Larry; Guy, Kip; Yan, Bing

2010-01-01

The development of an automated, high-throughput fractionation procedure to prepare and analyze natural product libraries for drug discovery screening is described. Natural products obtained from plant materials worldwide were extracted and first prefractionated on polyamide solid-phase extraction cartridges to remove polyphenols, followed by high-throughput automated fractionation, drying, weighing, and reformatting for screening and storage. The analysis of fractions with UPLC coupled with MS, PDA and ELSD detectors provides information that facilitates characterization of compounds in active fractions. Screening of a portion of fractions yielded multiple assay-specific hits in several high-throughput cellular screening assays. This procedure modernizes the traditional natural product fractionation paradigm by seamlessly integrating automation, informatics, and multimodal analytical interrogation capabilities. PMID:20232897

Revisiting low-fidelity two-fluid models for gas–solids transport

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

Adeleke, Najeem, E-mail: najm@psu.edu; Adewumi, Michael, E-mail: m2a@psu.edu; Ityokumbul, Thaddeus

Two-phase gas–solids transport models are widely utilized for process design and automation in a broad range of industrial applications. Some of these applications include proppant transport in gaseous fracking fluids, air/gas drilling hydraulics, coal-gasification reactors and food processing units. Systems automation and real time process optimization stand to benefit a great deal from availability of efficient and accurate theoretical models for operations data processing. However, modeling two-phase pneumatic transport systems accurately requires a comprehensive understanding of gas–solids flow behavior. In this study we discuss the prevailing flow conditions and present a low-fidelity two-fluid model equation for particulate transport. The modelmore » equations are formulated in a manner that ensures the physical flux term remains conservative despite the inclusion of solids normal stress through the empirical formula for modulus of elasticity. A new set of Roe–Pike averages are presented for the resulting strictly hyperbolic flux term in the system of equations, which was used to develop a Roe-type approximate Riemann solver. The resulting scheme is stable regardless of the choice of flux-limiter. The model is evaluated by the prediction of experimental results from both pneumatic riser and air-drilling hydraulics systems. We demonstrate the effect and impact of numerical formulation and choice of numerical scheme on model predictions. We illustrate the capability of a low-fidelity one-dimensional two-fluid model in predicting relevant flow parameters in two-phase particulate systems accurately even under flow regimes involving counter-current flow.« less

Metal-organic framework mixed-matrix disks: Versatile supports for automated solid-phase extraction prior to chromatographic separation.

PubMed

Ghani, Milad; Font Picó, Maria Francesca; Salehinia, Shima; Palomino Cabello, Carlos; Maya, Fernando; Berlier, Gloria; Saraji, Mohammad; Cerdà, Víctor; Turnes Palomino, Gemma

2017-03-10

We present for the first time the application of metal-organic framework (MOF) mixed-matrix disks (MMD) for the automated flow-through solid-phase extraction (SPE) of environmental pollutants. Zirconium terephthalate UiO-66 and UiO-66-NH 2 MOFs with different size (90, 200 and 300nm) have been incorporated into mechanically stable polyvinylidene difluoride (PVDF) disks. The performance of the MOF-MMDs for automated SPE of seven substituted phenols prior to HPLC analysis has been evaluated using the sequential injection analysis technique. MOF-MMDs enabled the simultaneous extraction of phenols with the concomitant size exclusion of molecules of larger size. The best extraction performance was obtained using a MOF-MMD containing 90nm UiO-66-NH 2 crystals. Using the selected MOF-MMD, detection limits ranging from 0.1 to 0.2μgL -1 were obtained. Relative standard deviations ranged from 3.9 to 5.3% intra-day, and 4.7-5.7% inter-day. Membrane batch-to-batch reproducibility was from 5.2 to 6.4%. Three different groundwater samples were analyzed with the proposed method using MOF-MMDs, obtaining recoveries ranging from 90 to 98% for all tested analytes. Copyright © 2017 Elsevier B.V. All rights reserved.

Automated solid-phase extraction coupled online with HPLC-FLD for the quantification of zearalenone in edible oil.

PubMed

Drzymala, Sarah S; Weiz, Stefan; Heinze, Julia; Marten, Silvia; Prinz, Carsten; Zimathies, Annett; Garbe, Leif-Alexander; Koch, Matthias

2015-05-01

Established maximum levels for the mycotoxin zearalenone (ZEN) in edible oil require monitoring by reliable analytical methods. Therefore, an automated SPE-HPLC online system based on dynamic covalent hydrazine chemistry has been developed. The SPE step comprises a reversible hydrazone formation by ZEN and a hydrazine moiety covalently attached to a solid phase. Seven hydrazine materials with different properties regarding the resin backbone, pore size, particle size, specific surface area, and loading have been evaluated. As a result, a hydrazine-functionalized silica gel was chosen. The final automated online method was validated and applied to the analysis of three maize germ oil samples including a provisionally certified reference material. Important performance criteria for the recovery (70-120 %) and precision (RSDr <25 %) as set by the Commission Regulation EC 401/2006 were fulfilled: The mean recovery was 78 % and RSDr did not exceed 8 %. The results of the SPE-HPLC online method were further compared to results obtained by liquid-liquid extraction with stable isotope dilution analysis LC-MS/MS and found to be in good agreement. The developed SPE-HPLC online system with fluorescence detection allows a reliable, accurate, and sensitive quantification (limit of quantification, 30 μg/kg) of ZEN in edible oils while significantly reducing the workload. To our knowledge, this is the first report on an automated SPE-HPLC method based on a covalent SPE approach.

Rapid determination of six carcinogenic primary aromatic amines in mainstream cigarette smoke by two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry.

PubMed

Bie, Zhenying; Lu, Wei; Zhu, You; Chen, Yusong; Ren, Hubo; Ji, Lishun

2017-01-27

A fully automated, rapid, and reliable method for simultaneous determination of six carcinogenic primary aromatic amines (AAs), including o-toluidine (o-TOL), 2, 6-dimethylaniline (2, 6-DMA), o-anisidine (o-ASD), 1-naphthylamine (1-ANP), 2-naphthylamine (2-ANP), and 4-aminobiphenyl (4-ABP), in mainstream cigarette smoke was established. The proposed method was based on two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry (SPE/LC-MS/MS). The particulate phase of the mainstream cigarette smoke was collected on a Cambridge filter pad and pretreated via ultrasonic extraction with 2% formic acid (FA), while the gas phase was trapped by 2% FA without pretreatment for determination. The two-dimensional online SPE comprised of two cartridges with different absorption characteristics was applied for sample pretreatment. Analysis was performed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) under multiple reaction monitoring mode. Each sample required about 0.5h for solid phase extraction and analysis. The limit of detections (LODs) for six AAs ranged from 0.04 to 0.58ng/cig and recoveries were within 84.5%-122.9%. The relative standard deviations of intra- and inter-day tests for 3R4F reference cigarette were less than 6% and 7%, respectively, while no more than 7% and 8% separately for a type of Virginia cigarette. The proposed method enabled minimum sample pretreatment, full automation, and high throughput with high selectivity, sensitivity, and accuracy. As a part of the validation procedure, fifteen brands of cigarettes were tested by the designed method. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of perfluorinated chemicals in food and drinking water using high-flow solid-phase extraction and ultra-high performance liquid chromatography/tandem mass spectrometry.

PubMed

Chang, Ying-Chia; Chen, Wen-Ling; Bai, Fang-Yu; Chen, Pau-Chung; Wang, Gen-Shuh; Chen, Chia-Yang

2012-01-01

For this study, we developed methods of determining ten perfluorinated chemicals in drinking water, milk, fish, beef, and pig liver using high-flow automated solid-phase extraction (SPE) and ultra-high performance liquid chromatography/tandem mass spectrometry. The analytes were separated on a core-shell Kinetex C18 column. The mobile phase was composed of methanol and 10-mM N-methylmorpholine. Milk was digested with 0.5 N potassium hydroxide in Milli-Q water, and was extracted with an Atlantic HLB disk to perform automated SPE at a flow rate ranged from 70 to 86 mL/min. Drinking water was directly extracted by the SPE. Solid food samples were digested in alkaline methanol and their supernatants were diluted and also processed by SPE. The disks were washed with 40% methanol/60% water and then eluted with 0.1% ammonium hydroxide in methanol. Suppression of signal intensity of most analytes by matrixes was lower than 50%; it was generally lower in fish and drinking water but higher in liver. Most quantitative biases and relative standard deviations were lower than 15%. The limits of detection for most analytes were sub-nanograms per liter for drinking water and sub-nanograms per gram for solid food samples. This method greatly shortened the time and labor needed for digestion, SPE, and liquid chromatography. This method has been applied to analyze 14 types of food samples. Perfluorooctanoic acid was found to be the highest among the analytes (median at 3.2-64 ng/g wet weight), followed by perfluorodecanoic acid (0.7-25 ng/g) and perfluorododecanoic acid (0.6-15 ng/g).

Analysis of ketamine and norketamine in urine by automatic solid-phase extraction (SPE) and positive ion chemical ionization-gas chromatography-mass spectrometry (PCI-GC-MS).

PubMed

Kim, Eun-mi; Lee, Ju-seon; Choi, Sang-kil; Lim, Mi-ae; Chung, Hee-sun

2008-01-30

Ketamine (KT) is widely abused for hallucination and also misused as a "date-rape" drug in recent years. An analytical method using positive ion chemical ionization-gas chromatography-mass spectrometry (PCI-GC-MS) with an automatic solid-phase extraction (SPE) apparatus was studied for the determination of KT and its major metabolite, norketamine (NK), in urine. Six ketamine suspected urine samples were provided by the police. For the research of KT metabolism, KT was administered to SD rats by i.p. at a single dose of 5, 10 and 20mg/kg, respectively, and urine samples were collected 24, 48 and 72 h after administration. For the detection of KT and NK, urine samples were extracted on an automatic SPE apparatus (RapidTrace, Zymark) with mixed mode type cartridge, Drug-Clean (200 mg, Alltech). The identification of KT and NK was by PCI-GC-MS. m/z238 (M+1), 220 for KT, m/z 224 (M+1), 207 for NK and m/z307 (M+1) for Cocaine-D(3) as internal standard were extracted from the full-scan mass spectrum and the underlined ions were used for quantitation. Extracted calibration curves were linear from 50 to 1000 ng/mL for KT and NK with correlation coefficients exceeding 0.99. The limit of detection (LOD) was 25 ng/mL for KT and NK. The limit of quantitation (LOQ) was 50 ng/mL for KT and NK. The recoveries of KT and NK at three different concentrations (86, 430 and 860 ng/mL) were 53.1 to 79.7% and 45.7 to 83.0%, respectively. The intra- and inter-day run precisions (CV) for KT and NK were less than 15.0%, and the accuracies (bias) for KT and NK were also less than 15% at the three different concentration levels (86, 430 and 860 ng/mL). The analytical method was also applied to real six KT suspected urine specimens and KT administered rat urines, and the concentrations of KT and NK were determined. Dehydronorketamine (DHNK) was also confirmed in these urine samples, however the concentration of DHNK was not calculated. SPE is simple, and needs less organic solvent than liquid-liquid extraction (LLE), and PCI-GC-MS can offer both qualitative and quantitative information for urinalysis of KT in forensic analysis.

Automated direct-immersion solid-phase microextraction using crosslinked polymeric ionic liquid sorbent coatings for the determination of water pollutants by gas chromatography.

PubMed

Cordero-Vaca, María; Trujillo-Rodríguez, María J; Zhang, Cheng; Pino, Verónica; Anderson, Jared L; Afonso, Ana M

2015-06-01

Four different crosslinked polymeric ionic liquid (PIL)-based sorbent coatings were evaluated in an automated direct-immersion solid-phase microextraction method (automated DI-SPME) in combination with gas chromatography (GC). The crosslinked PIL coatings were based on vinyl-alkylimidazolium- (ViCnIm-) or vinylbenzyl-alkylimidazolium- (ViBzCnIm-) IL monomers, and di-(vinylimidazolium)dodecane ((ViIm)2C12-) or di-(vinylbenzylimidazolium)dodecane ((ViBzIm)2C12-) dicationic IL crosslinkers. In addition, a PIL-based hybrid coating containing multi-walled carbon nanotubes (MWCNTs) was also studied. The studied PIL coatings were covalently attached to derivatized nitinol wires and mounted onto the Supelco assembly to ensure automation when acting as SPME coatings. Their behavior was evaluated in the determination of a group of water pollutants, after proper optimization. A comparison was carried out with three common commercial SPME fibers. It was observed that those PILs containing a benzyl group in their structures, either in the IL monomer and crosslinker (PIL-1-1) or only in the crosslinker (PIL-0-1), were the most efficient sorbents for the selected analytes. The validation of the overall automated DI-SPME-GC-flame ionization detector (FID) method gave limits of detection down to 135 μg · L(-1) for p-cresol when using the PIL-1-1 and down to 270 μg · L(-1) when using the PIL-0-1; despite their coating thickness: ~2 and ~5 μm, respectively. Average relative recoveries with waters were of 85 ± 14 % and 87 ± 15 % for PIL-1-1 and PIL-0-1, respectively. Precision values as relative standard deviation were always lower than 4.9 and 7.6 % (spiked level between 10 and 750 μg · L(-1), as intra-day precision). Graphical Abstract Automated DI-SPME-GC-FID using crosslinked-PILs sorbent coatings for the determination of waterpollutants.

Fully automated contour detection of the ascending aorta in cardiac 2D phase-contrast MRI.

PubMed

Codari, Marina; Scarabello, Marco; Secchi, Francesco; Sforza, Chiarella; Baselli, Giuseppe; Sardanelli, Francesco

2018-04-01

In this study we proposed a fully automated method for localizing and segmenting the ascending aortic lumen with phase-contrast magnetic resonance imaging (PC-MRI). Twenty-five phase-contrast series were randomly selected out of a large population dataset of patients whose cardiac MRI examination, performed from September 2008 to October 2013, was unremarkable. The local Ethical Committee approved this retrospective study. The ascending aorta was automatically identified on each phase of the cardiac cycle using a priori knowledge of aortic geometry. The frame that maximized the area, eccentricity, and solidity parameters was chosen for unsupervised initialization. Aortic segmentation was performed on each frame using active contouring without edges techniques. The entire algorithm was developed using Matlab R2016b. To validate the proposed method, the manual segmentation performed by a highly experienced operator was used. Dice similarity coefficient, Bland-Altman analysis, and Pearson's correlation coefficient were used as performance metrics. Comparing automated and manual segmentation of the aortic lumen on 714 images, Bland-Altman analysis showed a bias of -6.68mm 2 , a coefficient of repeatability of 91.22mm 2 , a mean area measurement of 581.40mm 2 , and a reproducibility of 85%. Automated and manual segmentation were highly correlated (R=0.98). The Dice similarity coefficient versus the manual reference standard was 94.6±2.1% (mean±standard deviation). A fully automated and robust method for identification and segmentation of ascending aorta on PC-MRI was developed. Its application on patients with a variety of pathologic conditions is advisable. Copyright © 2017 Elsevier Inc. All rights reserved.

Performance of an automated solid-phase red cell adherence system compared with that of a manual gel microcolumn assay for the identification of antibodies eluted from red blood cells.

PubMed

Finck, R H; Davis, R J; Teng, S; Goldfinger, D; Ziman, A F; Lu, Q; Yuan, S

2011-01-01

IgG antibodies coating red blood cells (RBCs) can be removed by elution procedures and their specificity determined by antibody identification studies. Although such testing is traditionally performed using the tube agglutination assay, prior studies have shown that the gel microcolumn (GMC) assay may also be used with comparable results. The purpose of this study was to compare an automated solid-phase red cell adherence (SPRCA) system with a GMC assay for the detection of antibodies eluted from RBCs. Acid eluates from 51 peripheral blood (PB) and 7 cord blood (CB) samples were evaluated by both an automated SPRCA instrument and a manual GMC assay. The concordance rate between the two systems for peripheral RBC samples was 88.2 percent (45 of 51), including cases with alloantibodies (n = 8), warm autoantibodies (n = 12), antibodies with no identifiable specificity (n = 2), and negative results (n = 23). There were six discordant cases, of which four had alloantibodies (including anti-Jka, -E, and -e) demonstrable by the SPRCA system only. In the remaining 2 cases, anti-Fya and antibodies with no identifiable specificity were demonstrable by the GMC assay only. All seven CB specimens produced concordant results, showing anti-A (n = 3), -B (n = 1), maternal anti-Jka (n = 2), or a negative result (n = 1). Automated SPRCA technology has a performance that is comparable with that of a manual GMC assay for identifying antibodies eluted from PB and CB RBCs.

Determination of phosphonoformate (foscarnet) in calf and human serum by automated solid-phase extraction and high-performance liquid chromatography with amperometric detection.

PubMed

Ba, B B; Corniot, A G; Ducint, D; Breilh, D; Grellet, J; Saux, M C

1999-03-05

An isocratic high-performance liquid chromatographic method with automated solid-phase extraction has been developed to determine foscarnet in calf and human serums. Extraction was performed with an anion exchanger, SAX, from which the analyte was eluted with a 50 mM potassium pyrophosphate buffer, pH 8.4. The mobile phase consisted of methanol-40 mM disodium hydrogenphosphate, pH 7.6 containing 0.25 mM tetrahexylammonium hydrogensulphate (25:75, v/v). The analyte was separated on a polyether ether ketone (PEEK) column 150x4.6 mm I.D. packed with Kromasil 100 C18, 5 microm. Amperometric detection allowed a quantification limit of 15 microM. The assay was linear from 15 to 240 microM. The recovery of foscarnet from calf serum ranged from 60.65+/-1.89% for 15 microM to 67.45+/-1.24% for 200 microM. The coefficient of variation was < or = 3.73% for intra-assay precision and < or =7.24% for inter-assay precision for calf serum concentrations ranged from 15 to 800 microM. For the same samples, the deviation from the nominal value ranged from -8.97% to +5.40% for same day accuracy and from -4.50% to +2.77% for day-to-day accuracy. Selectivity was satisfactory towards potential co-medications. Replacement of human serum by calf serum for calibration standards and quality control samples was validated. Automation brought more protection against biohazards and increase in productivity for routine monitoring and pharmacokinetic studies.

Simultaneous determination of polycyclic aromatic hydrocarbons and their chlorination by-products in drinking water and the coatings of water pipes by automated solid-phase microextraction followed by gas chromatography-mass spectrometry.

PubMed

Tillner, Jocelyn; Hollard, Caroline; Bach, Cristina; Rosin, Christophe; Munoz, Jean-François; Dauchy, Xavier

2013-11-08

In this study, an automated method for the simultaneous determination of polycyclic aromatic hydrocarbons (PAHs) and their chlorination by-products in drinking water was developed based on online solid-phase microextraction-gas chromatography-mass spectrometry. The main focus was the optimisation of the solid-phase microextraction step. The influence of the agitation rate, type of fibre, desorption time, extraction time, extraction temperature, desorption temperature, and solvent addition was examined. The method was developed and validated using a mixture of 17 PAHs, 11 potential chlorination by-products (chlorinated and oxidised PAHs) and 6 deuterated standards. The limit of quantification was 10 ng/L for all target compounds. The validated method was used to analyse drinking water samples from three different drinking water distribution networks and the presumably coal tar-based pipe coatings of two pipe sections. A number of PAHs were detected in all three networks although individual compositions varied. Several PAH chlorination by-products (anthraquinone, fluorenone, cyclopenta[d,e,f]phenanthrenone, 3-chlorofluoranthene, and 1-chloropyrene) were also found, their presence correlating closely with that of their respective parent compounds. Their concentrations were always below 100 ng/L. In the coatings, all PAHs targeted were detected although concentrations varied between the two coatings (76-12,635 mg/kg and 12-6295 mg/kg, respectively). A number of chlorination by-products (anthraquinone, fluorenone, cyclopenta[d,e,f]phenanthrenone, 3-chlorofluoranthene, and 1-chloropyrene) were also detected (from 40 to 985 mg/kg), suggesting that the reaction of PAHs with disinfectant agents takes place in the coatings and not in the water phase after migration. Copyright © 2013 Elsevier B.V. All rights reserved.

Solid polymer electrolyte water electrolysis system development. [to generate oxygen for manned space station applications

NASA Technical Reports Server (NTRS)

1975-01-01

Solid polymer electrolyte technology used in a water electrolysis system (WES) to generate oxygen and hydrogen for manned space station applications was investigated. A four-man rated, low pressure breadboard water electrolysis system with the necessary instrumentation and controls was fabricated and tested. A six man rated, high pressure, high temperature, advanced preprototype WES was developed. This configuration included the design and development of an advanced water electrolysis module, capable of operation at 400 psig and 200 F, and a dynamic phase separator/pump in place of a passive phase separator design. Evaluation of this system demonstrated the goal of safe, unattended automated operation at high pressure and high temperature with an accumulated gas generation time of over 1000 hours.

Automated Protein Biomarker Analysis: on-line extraction of clinical samples by Molecularly Imprinted Polymers

NASA Astrophysics Data System (ADS)

Rossetti, Cecilia; Świtnicka-Plak, Magdalena A.; Grønhaug Halvorsen, Trine; Cormack, Peter A. G.; Sellergren, Börje; Reubsaet, Léon

2017-03-01

Robust biomarker quantification is essential for the accurate diagnosis of diseases and is of great value in cancer management. In this paper, an innovative diagnostic platform is presented which provides automated molecularly imprinted solid-phase extraction (MISPE) followed by liquid chromatography-mass spectrometry (LC-MS) for biomarker determination using ProGastrin Releasing Peptide (ProGRP), a highly sensitive biomarker for Small Cell Lung Cancer, as a model. Molecularly imprinted polymer microspheres were synthesized by precipitation polymerization and analytical optimization of the most promising material led to the development of an automated quantification method for ProGRP. The method enabled analysis of patient serum samples with elevated ProGRP levels. Particularly low sample volumes were permitted using the automated extraction within a method which was time-efficient, thereby demonstrating the potential of such a strategy in a clinical setting.

Quantification of 31 illicit and medicinal drugs and metabolites in whole blood by fully automated solid-phase extraction and ultra-performance liquid chromatography-tandem mass spectrometry.

PubMed

Bjørk, Marie Kjærgaard; Simonsen, Kirsten Wiese; Andersen, David Wederkinck; Dalsgaard, Petur Weihe; Sigurðardóttir, Stella Rögn; Linnet, Kristian; Rasmussen, Brian Schou

2013-03-01

An efficient method for analyzing illegal and medicinal drugs in whole blood using fully automated sample preparation and short ultra-high-performance liquid chromatography-tandem mass spectrometry (MS/MS) run time is presented. A selection of 31 drugs, including amphetamines, cocaine, opioids, and benzodiazepines, was used. In order to increase the efficiency of routine analysis, a robotic system based on automated liquid handling and capable of handling all unit operation for sample preparation was built on a Freedom Evo 200 platform with several add-ons from Tecan and third-party vendors. Solid-phase extraction was performed using Strata X-C plates. Extraction time for 96 samples was less than 3 h. Chromatography was performed using an ACQUITY UPLC system (Waters Corporation, Milford, USA). Analytes were separated on a 100 mm × 2.1 mm, 1.7 μm Acquity UPLC CSH C(18) column using a 6.5 min 0.1 % ammonia (25 %) in water/0.1 % ammonia (25 %) in methanol gradient and quantified by MS/MS (Waters Quattro Premier XE) in multiple-reaction monitoring mode. Full validation, including linearity, precision and trueness, matrix effect, ion suppression/enhancement of co-eluting analytes, recovery, and specificity, was performed. The method was employed successfully in the laboratory and used for routine analysis of forensic material. In combination with tetrahydrocannabinol analysis, the method covered 96 % of cases involving driving under the influence of drugs. The manual labor involved in preparing blood samples, solvents, etc., was reduced to a half an hour per batch. The automated sample preparation setup also minimized human exposure to hazardous materials, provided highly improved ergonomics, and eliminated manual pipetting.

Complete automation of solid-phase extraction with subsequent liquid chromatography-tandem mass spectrometry for the quantification of benzoylecgonine, m-hydroxybenzoylecgonine, p-hydroxybenzoylecgonine, and norbenzoylecgonine in urine--application to a high-throughput urine analysis laboratory.

PubMed

Robandt, Paul P; Reda, Louis J; Klette, Kevin L

2008-10-01

A fully automated system utilizing a liquid handler and an online solid-phase extraction (SPE) device coupled with liquid chromatography-tandem mass spectrometry (LC-MS-MS) was designed to process, detect, and quantify benzoylecgonine (BZE), meta-hydroxybenzoylecgonine (m-OH BZE), para-hydroxybenzoylecgonine (p-OH BZE), and norbenzoylecgonine (nor-BZE) metabolites in human urine. The method was linear for BZE, m-OH BZE, and p-OH BZE from 1.2 to 10,000 ng/mL with limits of detection (LOD) and quantification (LOQ) of 1.2 ng/mL. Nor-BZE was linear from 5 to 10,000 ng/mL with an LOD and LOQ of 1.2 and 5 ng/mL, respectively. The intrarun precision measured as the coefficient of variation of 10 replicates of a 100 ng/mL control was less than 2.6%, and the interrun precision for 5 replicates of the same control across 8 batches was less than 4.8% for all analytes. No assay interference was noted from controls containing cocaine, cocaethylene, and ecgonine methyl ester. Excellent data concordance (R2 > 0.994) was found for direct comparison of the automated SPE-LC-MS-MS procedure and an existing gas chromatography-MS procedure using 94 human urine samples previously determined to be positive for BZE. The automated specimen handling and SPE procedure, when compared to the traditional extraction schema, eliminates the human factors of specimen handling, processing, extraction, and derivatization, thereby reducing labor costs and rework resulting from batch handling issues, and may reduce the number of fume hoods required in the laboratory.

Profiling of tryptophan-related plasma indoles in patients with carcinoid tumors by automated, on-line, solid-phase extraction and HPLC with fluorescence detection.

PubMed

Kema, I P; Meijer, W G; Meiborg, G; Ooms, B; Willemse, P H; de Vries, E G

2001-10-01

Profiling of the plasma indoles tryptophan, 5-hydroxytryptophan (5-HTP), serotonin, and 5-hydroxyindoleacetic acid (5-HIAA) is useful in the diagnosis and follow-up of patients with carcinoid tumors. We describe an automated method for the profiling of these indoles in protein-containing matrices as well as the plasma indole concentrations in healthy controls and patients with carcinoid tumors. Plasma, cerebrospinal fluid, and tissue homogenates were prepurified by automated on-line solid-phase extraction (SPE) in Hysphere Resin SH SPE cartridges containing strong hydrophobic polystyrene resin. Analytes were eluted from the SPE cartridge by column switching. Subsequent separation and detection were performed by reversed-phase HPLC combined with fluorometric detection in a total cycle time of 20 min. We obtained samples from 14 healthy controls and 17 patients with metastasized midgut carcinoid tumors for plasma indole analysis. In the patient group, urinary excretion of 5-HIAA and serotonin was compared with concentrations of plasma indoles. Within- and between-series CVs for indoles in platelet-rich plasma were 0.6-6.2% and 3.7-12%, respectively. Results for platelet-rich plasma serotonin compared favorably with those obtained by single-component analysis. Plasma 5-HIAA, but not 5-HTP was detectable in 8 of 17 patients with carcinoid tumors. In the patient group, platelet-rich plasma total tryptophan correlated negatively with platelet-rich plasma serotonin (P = 0.021; r = -0.56), urinary 5-HIAA (P = 0.003; r = -0.68), and urinary serotonin (P <0.0001; r = -0.80). The present chromatographic approach reduces analytical variation and time needed for analysis and gives more detailed information about metabolic deviations in indole metabolism than do manual, single-component analyses.

Fully automated analysis of four tobacco-specific N-nitrosamines in mainstream cigarette smoke using two-dimensional online solid phase extraction combined with liquid chromatography-tandem mass spectrometry.

PubMed

Zhang, Jie; Bai, Ruoshi; Yi, Xiaoli; Yang, Zhendong; Liu, Xingyu; Zhou, Jun; Liang, Wei

2016-01-01

A fully automated method for the detection of four tobacco-specific nitrosamines (TSNAs) in mainstream cigarette smoke (MSS) has been developed. The new developed method is based on two-dimensional online solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE/LC-MS/MS). The two dimensional SPE was performed in the method utilizing two cartridges with different extraction mechanisms to cleanup disturbances of different polarity to minimize sample matrix effects on each analyte. Chromatographic separation was achieved using a UPLC C18 reversed phase analytical column. Under the optimum online SPE/LC-MS/MS conditions, N'-nitrosonornicotine (NNN), N'-nitrosoanatabine (NAT), N'-nitrosoanabasine (NAB), and 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK) were baseline separated with good peak shapes. This method appears to be the most sensitive method yet reported for determination of TSNAs in mainstream cigarette smoke. The limits of quantification for NNN, NNK, NAT and NAB reached the levels of 6.0, 1.0, 3.0 and 0.6 pg/cig, respectively, which were well below the lowest levels of TSNAs in MSS of current commercial cigarettes. The accuracy of the measurement of four TSNAs was from 92.8 to 107.3%. The relative standard deviations of intra-and inter-day analysis were less than 5.4% and 7.5%, respectively. The main advantages of the method developed are fairly high sensitivity, selectivity and accuracy of results, minimum sample pre-treatment, full automation, and high throughput. As a part of the validation procedure, the developed method was applied to evaluate TSNAs yields for 27 top-selling commercial cigarettes in China. Copyright © 2015 Elsevier B.V. All rights reserved.

Semi-automated 96-well solid-phase extraction and gas chromatography-negative chemical ionization tandem mass spectrometry for the trace analysis of fluprostenol in rat plasma.

PubMed

Gauw, R D; Stoffolano, P J; Kuhlenbeck, D L; Patel, V S; Garver, S M; Baker, T R; Wehmeyer, K R

2000-07-21

Semi-automated 96-well plate solid-phase extraction (SPE) was used for sample preparation of fluprostenol, a prostaglandin analog, in rat plasma prior to detection by gas chromatography-negative chemical ionization tandem mass spectrometry (GC-NCI-MS-MS). A liquid handling system was utilized for all aspects of sample handling prior to SPE including transferring of samples into a 96-well format, preparation of standards as well as addition of internal standard to standards, quality control samples and study samples. SPE was performed in a 96-well plate format using octadecylsilane packing and the effluent from the SPE was dried in a custom-made 96-well apparatus. The sample residue was derivatized sequentially with pentafluorobenzylbromide followed by N-methyl-N-trimethylsilyltrifluoroacetamide. The derivatized sample was then analyzed using GC-NCI-MS-MS. The dynamic range for the method was from 7 to 5800 pg/ml with a 0.1-ml plasma sample. The methodology was evaluated over a 4-day period and demonstrated an accuracy of 90-106% with a precision of 2.4-12.9%.

Automated solid-phase radiofluorination using polymer-supported phosphazenes.

PubMed

Mathiessen, Bente; Zhuravlev, Fedor

2013-08-30

The polymer supported phosphazene bases PS-P₂(tBu) and the novel PS-P₂(PEG) 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 sulfonates (69%) and bromides (42%); the total radiosynthesis time was 35-45 min. The multivariate analysis showed that the radiochemical yields and purities were controlled by the resin load, reaction temperature, and column packing effects. The resins could be reused several times with the same or different substrates. The fully automated on-column radiofluorination methodology was applied to the radiosynthesis of the important PET radiotracers [¹⁸F]FLT and [¹⁸F]FDG. The latter was produced with 40% yield on a 120 GBq scale and passed GMP-regulated quality control required for commercial production of [1¹⁸F]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.

Engineering customized TALE nucleases (TALENs) and TALE transcription factors by fast ligation-based automatable solid-phase high-throughput (FLASH) assembly.

PubMed

Reyon, Deepak; Maeder, Morgan L; Khayter, Cyd; Tsai, Shengdar Q; Foley, Jonathan E; Sander, Jeffry D; Joung, J Keith

2013-07-01

Customized DNA-binding domains made using transcription activator-like effector (TALE) repeats are rapidly growing in importance as widely applicable research tools. TALE nucleases (TALENs), composed of an engineered array of TALE repeats fused to the FokI nuclease domain, have been used successfully for directed genome editing in various organisms and cell types. TALE transcription factors (TALE-TFs), consisting of engineered TALE repeat arrays linked to a transcriptional regulatory domain, have been used to up- or downregulate expression of endogenous genes in human cells and plants. This unit describes a detailed protocol for the recently described fast ligation-based automatable solid-phase high-throughput (FLASH) assembly method. FLASH enables automated high-throughput construction of engineered TALE repeats using an automated liquid handling robot or manually using a multichannel pipet. Using the automated approach, a single researcher can construct up to 96 DNA fragments encoding TALE repeat arrays of various lengths in a single day, and then clone these to construct sequence-verified TALEN or TALE-TF expression plasmids in a week or less. Plasmids required for FLASH are available by request from the Joung lab (http://eGenome.org). This unit also describes improvements to the Zinc Finger and TALE Targeter (ZiFiT Targeter) web server (http://ZiFiT.partners.org) that facilitate the design and construction of FLASH TALE repeat arrays in high throughput. © 2013 by John Wiley & Sons, Inc.

Engineering Customized TALE Nucleases (TALENs) and TALE Transcription Factors by Fast Ligation-based Automatable Solid-phase High-throughput (FLASH) Assembly

PubMed Central

Reyon, Deepak; Maeder, Morgan L.; Khayter, Cyd; Tsai, Shengdar Q.; Foley, Jonathan E.; Sander, Jeffry D.; Joung, J. Keith

2013-01-01

Customized DNA-binding domains made using Transcription Activator-Like Effector (TALE) repeats are rapidly growing in importance as widely applicable research tools. TALE nucleases (TALENs), composed of an engineered array of TALE repeats fused to the FokI nuclease domain, have been used successfully for directed genome editing in multiple different organisms and cell types. TALE transcription factors (TALE-TFs), consisting of engineered TALE repeat arrays linked to a transcriptional regulatory domain, have been used to up- or down-regulate expression of endogenous genes in human cells and plants. Here we describe a detailed protocol for practicing the recently described Fast Ligation-based Automatable Solid-phase High-throughput (FLASH) assembly method. FLASH enables automated high-throughput construction of engineered TALE repeats using an automated liquid handling robot or manually using a multi-channel pipet. With the automated version of FLASH, a single researcher can construct up to 96 DNA fragments encoding various length TALE repeat arrays in one day and then clone these to construct sequence-verified TALEN or TALE-TF expression plasmids in one week or less. Plas-mids required to practice FLASH are available by request from the Joung Lab (http://www.jounglab.org/). We also describe here improvements to the Zinc Finger and TALE Targeter (ZiFiT Targeter) webserver (http://ZiFiTBeta.partners.org) that facilitate the design and construction of FLASH TALE repeat arrays in high-throughput. PMID:23821439

A fully automated method for simultaneous determination of aflatoxins and ochratoxin A in dried fruits by pressurized liquid extraction and online solid-phase extraction cleanup coupled to ultra-high-pressure liquid chromatography-tandem mass spectrometry.

PubMed

Campone, Luca; Piccinelli, Anna Lisa; Celano, Rita; Russo, Mariateresa; Valdés, Alberto; Ibáñez, Clara; Rastrelli, Luca

2015-04-01

According to current demands and future perspectives in food safety, this study reports a fast and fully automated analytical method for the simultaneous analysis of the mycotoxins with high toxicity and wide spread, aflatoxins (AFs) and ochratoxin A (OTA) in dried fruits, a high-risk foodstuff. The method is based on pressurized liquid extraction (PLE), with aqueous methanol (30%) at 110 °C, of the slurried dried fruit and online solid-phase extraction (online SPE) cleanup of the PLE extracts with a C18 cartridge. The purified sample was directly analysed by ultra-high-pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for sensitive and selective determination of AFs and OTA. The proposed analytical procedure was validated for different dried fruits (vine fruit, fig and apricot), providing method detection and quantification limits much lower than the AFs and OTA maximum levels imposed by EU regulation in dried fruit for direct human consumption. Also, recoveries (83-103%) and repeatability (RSD < 8, n = 3) meet the performance criteria required by EU regulation for the determination of the levels of mycotoxins in foodstuffs. The main advantage of the proposed method is full automation of the whole analytical procedure that reduces the time and cost of the analysis, sample manipulation and solvent consumption, enabling high-throughput analysis and highly accurate and precise results.

Automated solid-phase extraction hyphenated to voltammetry for the determination of quercetin using magnetic nanoparticles and sequential injection lab-on-valve approach.

PubMed

Wang, Yang; Wang, Lu; Tian, Tian; Hu, Xiaoya; Yang, Chun; Xu, Qin

2012-05-21

In this study, an automated sequential injection lab-on-valve (SI-LOV) system was designed for the on-line matrix removal and preconcentration of quercetin. Octadecyl functionalized magnetic silica nanoparticles were prepared and packed into the microcolumn of the LOV as adsorbents. After being adsorbed through hydrophobic interaction, the analyte was eluted and subsequently introduced into the electrochemical flow cell by voltammetric quantification. The main parameters affecting the performance of solid-phase extraction, such as sample pH and flow rate, eluent solution and volume, accumulation potential and accumulation time were investigated in detail. Under the optimum experimental conditions, a linear calibration curve was obtained in the range of 1.0 × 10(-8) to 1 × 10(-5) mol L(-1) with R(2) = 0.9979. The limit of detection (LOD) and limit of quantitation (LOQ) were 1.3 × 10(-9) and 4.3 × 10(-9) mol L(-1), respectively. The relative standard deviation (RSD) for the determination of 1.0 × 10(-6) mol L(-1) quercetin was found to be 2.9% (n = 11) along with a sampling frequency of 40 h(-1). The applicability and reliability of the automated method described here had been applied to the determination of quercetin in human urine and red wine samples through recovery experiments, and the obtained results were in good agreement with those obtained by the HPLC method.

Screening for anabolic steroids in urine of forensic cases using fully automated solid phase extraction and LC-MS-MS.

PubMed

Andersen, David W; Linnet, Kristian

2014-01-01

A screening method for 18 frequently measured exogenous anabolic steroids and the testosterone/epitestosterone (T/E) ratio in forensic cases has been developed and validated. The method involves a fully automated sample preparation including enzyme treatment, addition of internal standards and solid phase extraction followed by analysis by liquid chromatography-tandem mass spectrometry (LC-MS-MS) using electrospray ionization with adduct formation for two compounds. Urine samples from 580 forensic cases were analyzed to determine the T/E ratio and occurrence of exogenous anabolic steroids. Extraction recoveries ranged from 77 to 95%, matrix effects from 48 to 78%, overall process efficiencies from 40 to 54% and the lower limit of identification ranged from 2 to 40 ng/mL. In the 580 urine samples analyzed from routine forensic cases, 17 (2.9%) were found positive for one or more anabolic steroids. Only seven different steroids including testosterone were found in the material, suggesting that only a small number of common steroids are likely to occur in a forensic context. The steroids were often in high concentrations (>100 ng/mL), and a combination of steroids and/or other drugs of abuse were seen in the majority of cases. The method presented serves as a fast and automated screening procedure, proving the suitability of LC-MS-MS for analyzing anabolic steroids. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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

PubMed

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.

Investigation on phase transitions of 1-decylammonium hydrochloride as the potential thermal energy storage material

NASA Astrophysics Data System (ADS)

Dan, Wen-Yan; Di, You-Ying; He, Dong-Hua; Liu, Yu-Pu

2011-02-01

1-Decylammonium hydrochloride was synthesized by the method of liquid phase synthesis. Chemical analysis, elemental analysis, and X-ray single crystal diffraction techniques were applied to characterize its composition and structure. Low-temperature heat capacities of the compounds were measured with a precision automated adiabatic calorimeter over the temperature range from 78 to 380 K. Three solid-solid phase transitions have been observed at the peak temperatures of 307.52 ± 0.13, 325.02 ± 0.19, and 327.26 ± 0.07 K. The molar enthalpies and entropies of three phase transitions were determined based on the analysis of heat capacity curves. Experimental molar heat capacities were fitted to two polynomial equations of the heat capacities as a function of temperature by least square method. Smoothed heat capacities and thermodynamic functions of the compound relative to the standard reference temperature 298.15 K were calculated and tabulated at intervals of 5 K based on the fitted polynomials.

Facile purification and click labeling with 2-[ 18F]fluoroethyl azide using solid phase extraction cartridges

DOE PAGES

Zhou, Dong; Chu, Wenhua; Peng, Xin; ...

2014-11-04

In this paper, a facile method was developed to purify 2-[ 18F]fluoroethyl azide ([ 18F]FEA) using a C18 cartridge and an Oasis® HLB cartridge in series, in which [18F]FEA was exclusively trapped on the HLB cartridge. [ 18F]FEA can be eluted for reactions in solution; alternatively click labeling can be carried out on the HLB cartridge itself by loading an alkyne substrate and copper (I) catalyst dissolved in DMF onto the cartridge. Finally, this solid phase extraction methodology for purification and click labeling with [ 18F]FEA, either in solution or on the cartridge, is safe, simple, reproducible in high yield,more » and compatible with automated synthesis of 18F-labeled PET tracers.« less

Automated on-line renewable solid-phase extraction-liquid chromatography exploiting multisyringe flow injection-bead injection lab-on-valve analysis.

PubMed

Quintana, José Benito; Miró, Manuel; Estela, José Manuel; Cerdà, Víctor

2006-04-15

In this paper, the third generation of flow injection analysis, also named the lab-on-valve (LOV) approach, is proposed for the first time as a front end to high-performance liquid chromatography (HPLC) for on-line solid-phase extraction (SPE) sample processing by exploiting the bead injection (BI) concept. The proposed microanalytical system based on discontinuous programmable flow features automated packing (and withdrawal after single use) of a small amount of sorbent (<5 mg) into the microconduits of the flow network and quantitative elution of sorbed species into a narrow band (150 microL of 95% MeOH). The hyphenation of multisyringe flow injection analysis (MSFIA) with BI-LOV prior to HPLC analysis is utilized for on-line postextraction treatment to ensure chemical compatibility between the eluate medium and the initial HPLC gradient conditions. This circumvents the band-broadening effect commonly observed in conventional on-line SPE-based sample processors due to the low eluting strength of the mobile phase. The potential of the novel MSFI-BI-LOV hyphenation for on-line handling of complex environmental and biological samples prior to reversed-phase chromatographic separations was assessed for the expeditious determination of five acidic pharmaceutical residues (viz., ketoprofen, naproxen, bezafibrate, diclofenac, and ibuprofen) and one metabolite (viz., salicylic acid) in surface water, urban wastewater, and urine. To this end, the copolymeric divinylbenzene-co-n-vinylpyrrolidone beads (Oasis HLB) were utilized as renewable sorptive entities in the micromachined unit. The automated analytical method features relative recovery percentages of >88%, limits of detection within the range 0.02-0.67 ng mL(-1), and coefficients of variation <11% for the column renewable mode and gives rise to a drastic reduction in operation costs ( approximately 25-fold) as compared to on-line column switching systems.

Automated synthesis of a 96 product-sized library of triazole derivatives using a solid phase supported copper catalyst.

PubMed

Jlalia, Ibtissem; Beauvineau, Claire; Beauvière, Sophie; Onen, Esra; Aufort, Marie; Beauvineau, Aymeric; Khaba, Eihab; Herscovici, Jean; Meganem, Faouzi; Girard, Christian

2010-04-28

This article deal with the parallel synthesis of a 96 product-sized library using a polymer-based copper catalyst that we developed which can be easily separated from the products by simple filtration. This gave us the opportunity to use this catalyst in an automated chemical synthesis station (Chemspeed ASW-2000). Studies and results about the preparation of the catalyst, its use in different solvent systems, its recycling capabilities and its scope and limitations in the synthesis of this library will be addressed. The synthesis of the triazole library and the very good results obtained will finally be discussed.

Evaluation and optimisation of preparative semi-automated electrophoresis systems for Illumina library preparation.

PubMed

Quail, Michael A; Gu, Yong; Swerdlow, Harold; Mayho, Matthew

2012-12-01

Size selection can be a critical step in preparation of next-generation sequencing libraries. Traditional methods employing gel electrophoresis lack reproducibility, are labour intensive, do not scale well and employ hazardous interchelating dyes. In a high-throughput setting, solid-phase reversible immobilisation beads are commonly used for size-selection, but result in quite a broad fragment size range. We have evaluated and optimised the use of two semi-automated preparative DNA electrophoresis systems, the Caliper Labchip XT and the Sage Science Pippin Prep, for size selection of Illumina sequencing libraries. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A new strategy for the preparation of peptide-targeted technetium and rhenium radiopharmaceuticals. The automated solid-phase synthesis, characterization, labeling, and screening of a peptide-ligand library targeted at the formyl peptide receptor.

PubMed

Stephenson, Karin A; Banerjee, Sangeeta Ray; Sogbein, Oyebola O; Levadala, Murali K; McFarlane, Nicole; Boreham, Douglas R; Maresca, Kevin P; Babich, John W; Zubieta, Jon; Valliant, John F

2005-01-01

A new solid-phase synthetic methodology was developed that enables libraries of peptide-based Tc(I)/Re(I) radiopharmaceuticals to be prepared using a conventional automated peptide synthesizer. Through the use of a tridentate ligand derived from N-alpha-Fmoc-l-lysine, which we refer to as a single amino acid chelate (SAAC), a series of 12 novel bioconjugates [R-NH(CO)ZLF(SAAC)G, R = ethyl, isopropyl, n-propyl, tert-butyl, n-butyl, benzyl; Z = Met, Nle] that are designed to target the formyl peptide receptor (FPR) were prepared. Construction of the library was carried out in a multiwell format on an Advanced ChemTech 348 peptide synthesizer where multi-milligram quantities of each peptide were isolated in high purity without HPLC purification. After characterization, the library components were screened for their affinity for the FPR receptor using flow cytometry where the K(d) values were found to be in the low micromolar range (0.5-3.0 microM). Compound 5j was subsequently labeled with (99m)Tc(I) and the product isolated in high radiochemical yield using a simple Sep-Pak purification procedure. The retention time of the labeled compound matched that of the fully characterized Re-analogue which was prepared through the use of the same solid-phase synthesis methodology that was used to construct the library. The work reported here is a rare example of a method by which libraries of peptide-ligand conjugates and their rhenium complexes can be prepared.

Increased alloimmunisation and transfusion reaction reporting in patients with solid-phase panreactivity.

PubMed

Olofson, Andrea M; Chandler, Rachael M; Marx-Wood, Cynthia R; Babcock, Craig A; Dunbar, Nancy M

2017-11-01

Automated solid-phase antibody screening uses red blood cell (RBC) membranes immobilised on polystyrene test wells to detect RBC specific antibodies. Despite its time-saving and labour-saving benefits, this method produces a higher rate of nonspecific reactivity compared with manual screening. Solid-phase panreactivity (SPP) is characterised by panreactivity (ie, all test cells reacting) in solid-phase testing accompanied by a negative autocontrol and a lack of reactivity when the same screening cells are tested in tube. The mechanisms underlying SPP and its clinical significance remain unclear. The goals of this study were to describe the prevalence of SPP at our institution and determine the alloimmunisation and transfusion reaction rates within this population. Data were collected on all patients undergoing type and screen testing over a 6-year period. Study patients undergoing subsequent transfusion were evaluated for reported transfusion reactions and development of new alloantibodies. Of the 76 051 patients studied, 0.7% demonstrated SPP of which 11% developed new alloantibodies. The transfusion reaction reporting rate among patients with SPP was 2%. Our data suggest that patients with SPP have higher rates of reported transfusion reactions and alloantibody development compared with those without SPP. Published by the BMJ Publishing Group Limited. For permission to use (where not already granted under a licence) please go to http://www.bmj.com/company/products-services/rights-and-licensing/.

Detecting Phase Boundaries in Hard-Sphere Suspensions

NASA Technical Reports Server (NTRS)

McDowell, Mark; Rogers, Richard B.; Gray, Elizabeth

2009-01-01

A special image-data-processing technique has been developed for use in experiments that involve observation, via optical microscopes equipped with electronic cameras, of moving boundaries between the colloidal-solid and colloidal-liquid phases of colloidal suspensions of monodisperse hard spheres. During an experiment, it is necessary to adjust the position of a microscope to keep the phase boundary within view. A boundary typically moves at a speed of the order of microns per hour. Because an experiment can last days or even weeks, it is impractical to require human intervention to keep the phase boundary in view. The present image-data-processing technique yields results within a computation time short enough to enable generation of automated-microscope-positioning commands to track the moving phase boundary

Experiment Automation with a Robot Arm using the Liquids Reflectometer Instrument at the Spallation Neutron Source

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

Zolnierczuk, Piotr A; Vacaliuc, Bogdan; Sundaram, Madhan

The Liquids Reflectometer instrument installed at the Spallation Neutron Source (SNS) enables observations of chemical kinetics, solid-state reactions and phase-transitions of thin film materials at both solid and liquid surfaces. Effective measurement of these behaviors requires each sample to be calibrated dynamically using the neutron beam and the data acquisition system in a feedback loop. Since the SNS is an intense neutron source, the time needed to perform the measurement can be the same as the alignment process, leading to a labor-intensive operation that is exhausting to users. An update to the instrument control system, completed in March 2013, implementedmore » the key features of automated sample alignment and robot-driven sample management, allowing for unattended operation over extended periods, lasting as long as 20 hours. We present a case study of the effort, detailing the mechanical, electrical and software modifications that were made as well as the lessons learned during the integration, verification and testing process.« less

The LabTube - a novel microfluidic platform for assay automation in laboratory centrifuges.

PubMed

Kloke, A; Fiebach, A R; Zhang, S; Drechsel, L; Niekrawietz, S; Hoehl, M M; Kneusel, R; Panthel, K; Steigert, J; von Stetten, F; Zengerle, R; Paust, N

2014-05-07

Assay automation is the key for successful transformation of modern biotechnology into routine workflows. Yet, it requires considerable investment in processing devices and auxiliary infrastructure, which is not cost-efficient for laboratories with low or medium sample throughput or point-of-care testing. To close this gap, we present the LabTube platform, which is based on assay specific disposable cartridges for processing in laboratory centrifuges. LabTube cartridges comprise interfaces for sample loading and downstream applications and fluidic unit operations for release of prestored reagents, mixing, and solid phase extraction. Process control is achieved by a centrifugally-actuated ballpen mechanism. To demonstrate the workflow and functionality of the LabTube platform, we show two LabTube automated sample preparation assays from laboratory routines: DNA extractions from whole blood and purification of His-tagged proteins. Equal DNA and protein yields were observed compared to manual reference runs, while LabTube automation could significantly reduce the hands-on-time to one minute per extraction.

Coupling solid-phase extraction and enzyme-linked immunosorbent assay for ultratrace determination of herbicides in pristine water

USGS Publications Warehouse

Aga, D.S.; Thurman, E.M.

1993-01-01

Solid-phase extraction (SPE) and enzyme-linked immunosorbent assay (ELISA) were coupled for automated trace analysis of pristine water samples containing 2-chloro-4-ethylamino-6-isopropylamine-s-triazine (atrazine) and 2-chloro-2???,6???-diethyl-N-(methoxymethyl)acetanilide (alachlor). The isolation of the two herbicides on a C18-resin involved the selection of an elution solvent that both removes interfering substances and is compatible with ELISA. Ethyl acetate was selected as the elution solvent followed by a solvent exchange with methanol/water (20/80, % v/v). The SPE-ELISA method has a detection limit of 5.0 ng/L (5 ppt), >90% recovery, and a relative standard deviation of ??10%. The performance of a microtiter plate-based ELISA and a magnetic particle-based ELISA coupled to SPE was also evaluated. Although the sensitivity of the two ELISA methods was comparable, the precision using magnetic particles was improved considerably (??10% versus ??20%) because of the faster reaction kinetics provided by the magnetic particles. Finally, SPE-ELISA and isotope dilution gas chromatography/ mass spectrometry correlated well (correlation coefficient of 0.96) for lake-water samples. The SPE-ELISA method is simple and may have broader applications for the inexpensive automated analysis of other contaminants in water at trace levels.

Automated Visibility & Cloud Cover Measurements with a Solid State Imaging System

DTIC Science & Technology

1989-03-01

GL-TR-89-0061 SIO Ref. 89-7 MPL-U-26/89 AUTOMATED VISIBILITY & CLOUD COVER MEASUREMENTS WITH A SOLID-STATE IMAGING SYSTEM C) to N4 R. W. Johnson W. S...include Security Classification) Automated Visibility & Cloud Measurements With A Solid State Imaging System 12. PERSONAL AUTHOR(S) Richard W. Johnson...based imaging systems , their ics and control algorithms, thus they ar.L discussed sepa- initial deployment and the preliminary application of rately

Ultrasensitive microfluidic solid-phase ELISA using an actuatable microwell-patterned PDMS chip.

PubMed

Wang, Tanyu; Zhang, Mohan; Dreher, Dakota D; Zeng, Yong

2013-11-07

Quantitative detection of low abundance proteins is of significant interest for biological and clinical applications. Here we report an integrated microfluidic solid-phase ELISA platform for rapid and ultrasensitive detection of proteins with a wide dynamic range. Compared to the existing microfluidic devices that perform affinity capture and enzyme-based optical detection in a constant channel volume, the key novelty of our design is two-fold. First, our system integrates a microwell-patterned assay chamber that can be pneumatically actuated to significantly reduce the volume of chemifluorescent reaction, markedly improving the sensitivity and speed of ELISA. Second, monolithic integration of on-chip pumps and the actuatable assay chamber allow programmable fluid delivery and effective mixing for rapid and sensitive immunoassays. Ultrasensitive microfluidic ELISA was demonstrated for insulin-like growth factor 1 receptor (IGF-1R) across at least five orders of magnitude with an extremely low detection limit of 21.8 aM. The microwell-based solid-phase ELISA strategy provides an expandable platform for developing the next-generation microfluidic immunoassay systems that integrate and automate digital and analog measurements to further improve the sensitivity, dynamic ranges, and reproducibility of proteomic analysis.

Multifunctional picoliter droplet manipulation platform and its application in single cell analysis.

PubMed

Gu, Shu-Qing; Zhang, Yun-Xia; Zhu, Ying; Du, Wen-Bin; Yao, Bo; Fang, Qun

2011-10-01

We developed an automated and multifunctional microfluidic platform based on DropLab to perform flexible generation and complex manipulations of picoliter-scale droplets. Multiple manipulations including precise droplet generation, sequential reagent merging, and multistep solid-phase extraction for picoliter-scale droplets could be achieved in the present platform. The system precision in generating picoliter-scale droplets was significantly improved by minimizing the thermo-induced fluctuation of flow rate. A novel droplet fusion technique based on the difference of droplet interfacial tensions was developed without the need of special microchannel networks or external devices. It enabled sequential addition of reagents to droplets on demand for multistep reactions. We also developed an effective picoliter-scale droplet splitting technique with magnetic actuation. The difficulty in phase separation of magnetic beads from picoliter-scale droplets due to the high interfacial tension was overcome using ferromagnetic particles to carry the magnetic beads to pass through the phase interface. With this technique, multistep solid-phase extraction was achieved among picoliter-scale droplets. The present platform had the ability to perform complex multistep manipulations to picoliter-scale droplets, which is particularly required for single cell analysis. Its utility and potentials in single cell analysis were preliminarily demonstrated in achieving high-efficiency single-cell encapsulation, enzyme activity assay at the single cell level, and especially, single cell DNA purification based on solid-phase extraction.

Validation of an automated solid-phase extraction method for the analysis of 23 opioids, cocaine, and metabolites in urine with ultra-performance liquid chromatography-tandem mass spectrometry.

PubMed

Ramírez Fernández, María del Mar; Van Durme, Filip; Wille, Sarah M R; di Fazio, Vincent; Kummer, Natalie; Samyn, Nele

2014-06-01

The aim of this work was to automate a sample preparation procedure extracting morphine, hydromorphone, oxymorphone, norcodeine, codeine, dihydrocodeine, oxycodone, 6-monoacetyl-morphine, hydrocodone, ethylmorphine, benzoylecgonine, cocaine, cocaethylene, tramadol, meperidine, pentazocine, fentanyl, norfentanyl, buprenorphine, norbuprenorphine, propoxyphene, methadone and 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine from urine samples. Samples were extracted by solid-phase extraction (SPE) with cation exchange cartridges using a TECAN Freedom Evo 100 base robotic system, including a hydrolysis step previous extraction when required. Block modules were carefully selected in order to use the same consumable material as in manual procedures to reduce cost and/or manual sample transfers. Moreover, the present configuration included pressure monitoring pipetting increasing pipetting accuracy and detecting sampling errors. The compounds were then separated in a chromatographic run of 9 min using a BEH Phenyl analytical column on a ultra-performance liquid chromatography-tandem mass spectrometry system. Optimization of the SPE was performed with different wash conditions and elution solvents. Intra- and inter-day relative standard deviations (RSDs) were within ±15% and bias was within ±15% for most of the compounds. Recovery was >69% (RSD < 11%) and matrix effects ranged from 1 to 26% when compensated with the internal standard. The limits of quantification ranged from 3 to 25 ng/mL depending on the compound. No cross-contamination in the automated SPE system was observed. The extracted samples were stable for 72 h in the autosampler (4°C). This method was applied to authentic samples (from forensic and toxicology cases) and to proficiency testing schemes containing cocaine, heroin, buprenorphine and methadone, offering fast and reliable results. Automation resulted in improved precision and accuracy, and a minimum operator intervention, leading to safer sample handling and less time-consuming procedures.

Automated Mini-Column Solid-Phase Extraction Cleanup for High-Throughput Analysis of Chemical Contaminants in Foods by Low-Pressure Gas Chromatography-Tandem Mass Spectrometry.

PubMed

Lehotay, Steven J; Han, Lijun; Sapozhnikova, Yelena

2016-01-01

This study demonstrated the application of an automated high-throughput mini-cartridge solid-phase extraction (mini-SPE) cleanup for the rapid low-pressure gas chromatography-tandem mass spectrometry (LPGC-MS/MS) analysis of pesticides and environmental contaminants in QuEChERS extracts of foods. Cleanup efficiencies and breakthrough volumes using different mini-SPE sorbents were compared using avocado, salmon, pork loin, and kale as representative matrices. Optimum extract load volume was 300 µL for the 45 mg mini-cartridges containing 20/12/12/1 (w/w/w/w) anh. MgSO 4 /PSA (primary secondary amine)/C 18 /CarbonX sorbents used in the final method. In method validation to demonstrate high-throughput capabilities and performance results, 230 spiked extracts of 10 different foods (apple, kiwi, carrot, kale, orange, black olive, wheat grain, dried basil, pork, and salmon) underwent automated mini-SPE cleanup and analysis over the course of 5 days. In all, 325 analyses for 54 pesticides and 43 environmental contaminants (3 analyzed together) were conducted using the 10 min LPGC-MS/MS method without changing the liner or retuning the instrument. Merely, 1 mg equivalent sample injected achieved <5 ng g -1 limits of quantification. With the use of internal standards, method validation results showed that 91 of the 94 analytes including pairs achieved satisfactory results (70-120 % recovery and RSD ≤ 25 %) in the 10 tested food matrices ( n  = 160). Matrix effects were typically less than ±20 %, mainly due to the use of analyte protectants, and minimal human review of software data processing was needed due to summation function integration of analyte peaks. This study demonstrated that the automated mini-SPE + LPGC-MS/MS method yielded accurate results in rugged, high-throughput operations with minimal labor and data review.

ACCELERATED SOLVENT EXTRACTION COMBINED WITH ...

EPA Pesticide Factsheets

A research project was initiated to address a recurring problem of elevated detection limits above required risk-based concentrations for the determination of semivolatile organic compounds in high moisture content solid samples. This project was initiated, in cooperation with the EPA Region 1 Laboratory, under the Regional Methods Program administered through the ORD Office of Science Policy. The aim of the project was to develop an approach for the rapid removal of water in high moisture content solids (e.g., wetland sediments) in preparation for analysis via Method 8270. Alternative methods for water removal have been investigated to enhance compound solid concentrations and improve extraction efficiency, with the use of pressure filtration providing a high-throughput alternative for removal of the majority of free water in sediments and sludges. In order to eliminate problems with phase separation during extraction of solids using Accelerated Solvent Extraction, a variation of a water-isopropanol extraction method developed at the USGS National Water Quality Laboratory in Denver, CO is being employed. The concentrations of target compounds in water-isopropanol extraction fluids are subsequently analyzed using an automated Solid Phase Extraction (SPE)-GC/MS method developed in our laboratory. The coupled approaches for dewatering, extraction, and target compound identification-quantitation provide a useful alternative to enhance sample throughput for Me

Automated Water-Purification System

NASA Technical Reports Server (NTRS)

Ahlstrom, Harlow G.; Hames, Peter S.; Menninger, Fredrick J.

1988-01-01

Reverse-osmosis system operates and maintains itself with minimal human attention, using programmable controller. In purifier, membranes surround hollow cores through which clean product water flows out of reverse-osmosis unit. No chemical reactions or phase changes involved. Reject water, in which dissolved solids concentrated, emerges from outer membrane material on same side water entered. Flow controls maintain ratio of 50 percent product water and 50 percent reject water. Membranes expected to last from 3 to 15 years.

Fully automated method for the liquid chromatographic determination of cyproterone acetate in plasma using restricted access material for sample pre-treatment.

PubMed

Christiaens, B; Chiap, P; Rbeida, O; Cello, D; Crommen, J; Hubert, Ph

2003-09-25

A new fully automated method for the quantitative analysis of an antiandrogenic substance, cyproterone acetate (CPA), in plasma samples has been developed using on-line solid-phase extraction (SPE) prior to the determination by reversed-phase liquid chromatography (LC). The automated method was based on the use of a precolumn packed with an internal-surface reversed-phase packing material (LiChrospher RP-4 ADS) for sample clean-up coupled to LC analysis on an octadecyl stationary phase using a column-switching system. A 200-microL volume of plasma sample was injected directly on the precolumn packed with restricted access material using a mixture of water-acetonitrile (90:10, v/v) as washing liquid. The analyte was then eluted in the back-flush mode with the LC mobile phase which consisted of a mixture of phosphate buffer, pH 7.0-acetonitrile (54:46, v/v). The elution profiles of CPA and blank plasma samples on the precolumn and the time needed for analyte transfer from the precolumn to the analytical column were determined. Different compositions of washing liquid and mobile phase were tested to reduce the interference of plasma endogenous components. UV detection was achieved at 280 nm. Finally, the developed method was validated using a new approach, namely the application of the accuracy profile based on the interval confidence at 90% of the total measurement error (bias+standard deviation). The limit of quantification of cyproterone acetate in plasma was determined at 15 ng mL(-1). The validated method should be applicable to the determination of CPA in patients treated by at least 50 mg day(-1).

Automated solid-phase extraction-liquid chromatography-tandem mass spectrometry analysis of 11-nor-Delta9-tetrahydrocannabinol-9-carboxylic acid in human urine specimens: application to a high-throughput urine analysis laboratory.

PubMed

Robandt, P V; Klette, K L; Sibum, M

2009-10-01

An automated solid-phase extraction coupled with liquid chromatography and tandem mass spectrometry (SPE-LC-MS-MS) method for the analysis of 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid (THC-COOH) in human urine specimens was developed. The method was linear (R(2) = 0.9986) to 1000 ng/mL with no carryover evidenced at 2000 ng/mL. Limits of quantification and detection were found to be 2 ng/mL. Interrun precision was evaluated at the 15 ng/mL level over nine batches spanning 15 days (n = 45). The coefficient of variation (%CV) was found to be 5.5% over the course of the validation. Intrarun precision of a 15 ng/mL control (n = 5) ranged from 0.58% CV to 7.4% CV for the same set of analytical batches. Interference was tested using (+/-)-11-hydroxy-Delta(9)-tetrahydrocannabinol, cannabidiol, (-)-Delta(8)-tetrahydrocannabinol, and cannabinol. One hundred and nineteen specimens previously found to contain THC-COOH by a previously validated gas chromatographic mass spectrometry (GC-MS) procedure were compared to the SPE-LC-MS-MS method. Excellent agreement was found (R(2) = 0.9925) for the parallel comparison study. The automated SPE procedure eliminates the human factors of specimen handling, extraction, and derivatization, thereby reducing labor costs and rework resulting from human error or technique issues. Additionally, method runtime is greatly reduced (e.g., during parallel studies the SPE-LC-MS-MS instrument was often finished with analysis by the time the technician finished the offline SPE and derivatization procedure prior to the GC-MS analysis).

Hematocrit-Independent Quantitation of Stimulants in Dried Blood Spots: Pipet versus Microfluidic-Based Volumetric Sampling Coupled with Automated Flow-Through Desorption and Online Solid Phase Extraction-LC-MS/MS Bioanalysis.

PubMed

Verplaetse, Ruth; Henion, Jack

2016-07-05

A workflow overcoming microsample collection issues and hematocrit (HCT)-related bias would facilitate more widespread use of dried blood spots (DBS). This report describes comparative results between the use of a pipet and a microfluidic-based sampling device for the creation of volumetric DBS. Both approaches were successfully coupled to HCT-independent, fully automated sample preparation and online liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) analysis allowing detection of five stimulants in finger prick blood. Reproducible, selective, accurate, and precise responses meeting generally accepted regulated bioanalysis guidelines were observed over the range of 5-1000 ng/mL whole blood. The applied heated flow-through solvent desorption of the entire spot and online solid phase extraction (SPE) procedure were unaffected by the blood's HCT value within the tested range of 28.0-61.5% HCT. Enhanced stability for mephedrone on DBS compared to liquid whole blood was observed. Finger prick blood samples were collected using both volumetric sampling approaches over a time course of 25 h after intake of a single oral dose of phentermine. A pharmacokinetic curve for the incurred phentermine was successfully produced using the described validated method. These results suggest that either volumetric sample collection method may be amenable to field-use followed by fully automated, HCT-independent DBS-SPE-LC-MS/MS bioanalysis for the quantitation of these representative controlled substances. Analytical data from DBS prepared with a pipet and microfluidic-based sampling devices were comparable, but the latter is easier to operate, making this approach more suitable for sample collection by unskilled persons.

Pharmacokinetic Studies of Chinese Medicinal Herbs Using an Automated Blood Sampling System and Liquid Chromatography-mass Spectrometry.

PubMed

Wu, Yu-Tse; Wu, Ming-Tsang; Lin, Chia-Chun; Chien, Chao-Feng; Tsai, Tung-Hu

2012-01-01

The safety of herbal products is one of the major concerns for the modernization of traditional Chinese medicine, and pharmacokinetic data of medicinal herbs guide us to design the rational use of the herbal formula. This article reviews the advantages of the automated blood sampling (ABS) systems for pharmacokinetic studies. In addition, three commonly used sample preparative methods, protein precipitation, liquid-liquid extraction and solid-phase extraction, are introduced. Furthermore, the definition, causes and evaluation of matrix effects in liquid chromatography-mass spectrometry (LC/MS) analysis are demonstrated. Finally, we present our previous works as practical examples of the application of ABS systems and LC/MS for the pharmacokinetic studies of Chinese medicinal herbs.

Headspace techniques in foods, fragrances and flavors: an overview.

PubMed

Rouseff, R; Cadwallader, K

2001-01-01

Headspace techniques have traditionally involved the collection of volatiles in the vapor state under either dynamic or static conditions as a means of determining concentrations in the product of interest. A brief overview of contemporary headspace applications and recent innovations are presented from the literature and Chapters in this book. New approaches used to concentrate volatiles under static conditions such as solid phase micro extraction, SPME, are examined. Advances in purge and trap applications and automation are also presented. Innovative methods of evaluating headspace volatiles using solid state sensor arrays (electronic noses) or mass spectrometers without prior separation are referenced. Numerous food and beverage headspace techniques are also reviewed. Advantages, limitations and alternatives to headspace analysis are presented.

LC-UV-solid-phase extraction-NMR-MS combined with a cryogenic flow probe and its application to the identification of compounds present in Greek oregano.

PubMed

Exarchou, Vassiliki; Godejohann, Markus; van Beek, Teris A; Gerothanassis, Ioannis P; Vervoort, Jacques

2003-11-15

Structure elucidation of natural products usually relies on a combination of NMR spectroscopy with mass spectrometry whereby NMR trails MS in terms of the minimum sample amount required. In the present study, the usefulness of on-line solid-phase extraction (SPE) in LC-NMR for peak storage after the LC separation prior to NMR analysis is demonstrated. The SPE unit allows the use of normal protonated solvents for the LC separation and fully deuterated solvents for flushing the trapped compounds to the NMR probe. Thus, solvent suppression is no longer necessary. Multiple trapping of the same analyte from repeated LC injections was utilized to solve the problem of low concentration and to obtain 2D heteronuclear NMR spectra. In addition, a combination of the SPE unit with a recently developed cryoflow NMR probe and an MS was evaluated. This on-line LC-UV-SPE-NMR-MS system was used for the automated analysis of a Greek oregano extract. Combining the data provided by the UV, MS, and NMR spectra, the flavonoids taxifolin, aromadendrin, eriodictyol, naringenin, and apigenin, the phenolic acid rosmarinic acid, and the monoterpene carvacrol were identified. This automated technique is very useful for natural product analysis, and the large sensitivity improvement leads to significantly reduced NMR acquisition times.

Determination of cannabinoids in hemp food products by use of headspace solid-phase microextraction and gas chromatography-mass spectrometry.

PubMed

Lachenmeier, Dirk W; Kroener, Lars; Musshoff, Frank; Madea, Burkhard

2004-01-01

A fully automated procedure using alkaline hydrolysis and headspace solid-phase microextraction (HS-SPME), followed by on-fiber derivatization and gas chromatographic-mass spectrometric (GC-MS) detection has been developed for determination of cannabinoids in hemp food samples. After addition of a deuterated internal standard, the sample was hydrolyzed with sodium hydroxide and submitted to direct HS-SPME. After absorption of analytes for on-fiber derivatization, the fiber was placed directly into the headspace of a second vial containing N-methyl- N-trimethylsilyltrifluoroacetamide (MSTFA), before GC-MS analysis. Linearity was good for Delta(9)-tetrahydrocannabinol (THC), cannabidiol, and cannabinol; regression coefficients were greater than 0.99. Depending on the characteristics of the matrix the detection limits obtained ranged between 0.01 and 0.17 mg kg(-1) and the precision between 0.4 and 11.8%. In comparison with conventional liquid-liquid extraction this automated HS-SPME-GC-MS procedure is substantially faster. It is easy to perform, solvent-free, and sample quantities are minimal, yet it maintains the same sensitivity and reproducibility. The applicability was demonstrated by analysis of 30 hemp food samples. Cannabinoids were detected in all of the samples and it was possible to differentiate between drug-type and fiber-type Cannabis sativa L. In comparison with other studies relatively low THC concentrations between 0.01 and 15.53 mg kg(-1) were determined.

Semi-automated solid phase extraction method for the mass spectrometric quantification of 12 specific metabolites of organophosphorus pesticides, synthetic pyrethroids, and select herbicides in human urine.

PubMed

Davis, Mark D; Wade, Erin L; Restrepo, Paula R; Roman-Esteva, William; Bravo, Roberto; Kuklenyik, Peter; Calafat, Antonia M

2013-06-15

Organophosphate and pyrethroid insecticides and phenoxyacetic acid herbicides represent important classes of pesticides applied in commercial and residential settings. Interest in assessing the extent of human exposure to these pesticides exists because of their widespread use and their potential adverse health effects. An analytical method for measuring 12 biomarkers of several of these pesticides in urine has been developed. The target analytes were extracted from one milliliter of urine by a semi-automated solid phase extraction technique, separated from each other and from other urinary biomolecules by reversed-phase high performance liquid chromatography, and detected using tandem mass spectrometry with isotope dilution quantitation. This method can be used to measure all the target analytes in one injection with similar repeatability and detection limits of previous methods which required more than one injection. Each step of the procedure was optimized to produce a robust, reproducible, accurate, precise and efficient method. The required selectivity and sensitivity for trace-level analysis (e.g., limits of detection below 0.5ng/mL) was achieved using a narrow diameter analytical column, higher than unit mass resolution for certain analytes, and stable isotope labeled internal standards. The method was applied to the analysis of 55 samples collected from adult anonymous donors with no known exposure to the target pesticides. This efficient and cost-effective method is adequate to handle the large number of samples required for national biomonitoring surveys. Published by Elsevier B.V.

Optimization of multiplexed PCR on an integrated microfluidic forensic platform for rapid DNA analysis.

PubMed

Estes, Matthew D; Yang, Jianing; Duane, Brett; Smith, Stan; Brooks, Carla; Nordquist, Alan; Zenhausern, Frederic

2012-12-07

This study reports the design, prototyping, and assay development of multiplexed polymerase chain reaction (PCR) on a plastic microfluidic device. Amplification of 17 DNA loci is carried out directly on-chip as part of a system for continuous workflow processing from sample preparation (SP) to capillary electrophoresis (CE). For enhanced performance of on-chip PCR amplification, improved control systems have been developed making use of customized Peltier assemblies, valve actuators, software, and amplification chemistry protocols. Multiple enhancements to the microfluidic chip design have been enacted to improve the reliability of sample delivery through the various on-chip modules. This work has been enabled by the encapsulation of PCR reagents into a solid phase material through an optimized Solid Phase Encapsulating Assay Mix (SPEAM) bead-based hydrogel fabrication process. SPEAM bead technology is reliably coupled with precise microfluidic metering and dispensing for efficient amplification and subsequent DNA short tandem repeat (STR) fragment analysis. This provides a means of on-chip reagent storage suitable for microfluidic automation, with the long shelf-life necessary for point-of-care (POC) or field deployable applications. This paper reports the first high quality 17-plex forensic STR amplification from a reference sample in a microfluidic chip with preloaded solid phase reagents, that is designed for integration with up and downstream processing.

Automated total and radioactive strontium separation and preconcentration in samples of environmental interest exploiting a lab-on-valve system.

PubMed

Rodríguez, Rogelio; Avivar, Jessica; Ferrer, Laura; Leal, Luz O; Cerdà, Victor

2012-07-15

A novel lab-on-valve system has been developed for strontium determination in environmental samples. Miniaturized lab-on-valve system potentially offers facilities to allow any kind of chemical and physical processes, including fluidic and microcarrier bead control, homogenous reaction and liquid-solid interaction. A rapid, inexpensive and fully automated method for the separation and preconcentration of total and radioactive strontium, using a solid phase extraction material (Sr-Resin), has been developed. Total strontium concentrations are determined by ICP-OES and (90)Sr activities by a low background proportional counter. The method has been successfully applied to different water samples of environmental interest. The proposed system offers minimization of sample handling, drastic reduction of reagent volume, improvement of the reproducibility and sample throughput and attains a significant decrease of both time and cost per analysis. The LLD of the total Sr reached is 1.8ng and the minimum detectable activity for (90)Sr is 0.008Bq. The repeatability of the separation procedure is 1.2% (n=10). Copyright © 2011 Elsevier B.V. All rights reserved.

Fiber-optic projected-fringe digital interferometry

NASA Technical Reports Server (NTRS)

Mercer, Carolyn R.; Beheim, Glenn

1990-01-01

A phase-stepped projected-fringe interferometer was developed which uses a closed-loop fiber-optic phase-control system to make very accurate surface profile measurements. The closed-loop phase-control system greatly reduces phase-stepping error, which is frequently the dominant source of error in digital interferometers. Two beams emitted from a fiber-optic coupler are combined to form an interference fringe pattern on a diffusely reflecting object. Reflections off of the fibers' output faces are used to create a phase-indicating signal for the closed-loop optical phase controller. The controller steps the phase difference between the two beams by pi/2 radians in order to determine the object's surface profile using a solid-state camera and a computer. The system combines the ease of alignment and automated data reduction of phase-stepping projected-fringe interferometry with the greatly improved phase-stepping accuracy of our closed-loop phase-controller. The system is demonstrated by measuring the profile of a plate containing several convex surfaces whose heights range from 15 to 25 micron high.

Automated extraction for the analysis of 11-nor-delta9-tetrahydrocannabinol-9-carboxylic acid (THCCOOH) in urine using a six-head probe Hamilton Microlab 2200 system and gas chromatography-mass spectrometry.

PubMed

Whitter, P D; Cary, P L; Leaton, J I; Johnson, J E

1999-01-01

An automated extraction scheme for the analysis of 11 -nor-delta9-tetrahydrocannabinol-9-carboxylic acid using the Hamilton Microlab 2200, which was modified for gravity-flow solid-phase extraction, has been evaluated. The Hamilton was fitted with a six-head probe, a modular valve positioner, and a peristaltic pump. The automated method significantly increased sample throughput, improved assay consistency, and reduced the time spent performing the extraction. Extraction recovery for the automated method was > 90%. The limit of detection, limit of quantitation, and upper limit of linearity were equivalent to the manual method: 1.5, 3.0, and 300 ng/mL, respectively. Precision at the 15-ng/mL cut-off was as follows: mean = 14.4, standard deviation = 0.5, coefficient of variation = 3.5%. Comparison of 38 patient samples, extracted by the manual and automated extraction methods, demonstrated the following correlation statistics: r = .991, slope 1.029, and y-intercept -2.895. Carryover was < 0.3% at 1000 ng/mL. Aliquoting/extraction time for the automated method (48 urine samples) was 50 min, and the manual procedure required approximately 2.5 h. The automated aliquoting/extraction method on the Hamilton Microlab 2200 and its use in forensic applications are reviewed.

Semi-automated in vivo solid-phase microextraction sampling and the diffusion-based interface calibration model to determine the pharmacokinetics of methoxyfenoterol and fenoterol in rats.

PubMed

Yeung, Joanne Chung Yan; de Lannoy, Inés; Gien, Brad; Vuckovic, Dajana; Yang, Yingbo; Bojko, Barbara; Pawliszyn, Janusz

2012-09-12

In vivo solid-phase microextraction (SPME) can be used to sample the circulating blood of animals without the need to withdraw a representative blood sample. In this study, in vivo SPME in combination with liquid-chromatography tandem mass spectrometry (LC-MS/MS) was used to determine the pharmacokinetics of two drug analytes, R,R-fenoterol and R,R-methoxyfenoterol, administered as 5 mg kg(-1) i.v. bolus doses to groups of 5 rats. This research illustrates, for the first time, the feasibility of the diffusion-based calibration interface model for in vivo SPME studies. To provide a constant sampling rate as required for the diffusion-based interface model, partial automation of the SPME sampling of the analytes from the circulating blood was accomplished using an automated blood sampling system. The use of the blood sampling system allowed automation of all SPME sampling steps in vivo, except for the insertion and removal of the SPME probe from the sampling interface. The results from in vivo SPME were compared to the conventional method based on blood withdrawal and sample clean up by plasma protein precipitation. Both whole blood and plasma concentrations were determined by the conventional method. The concentrations of methoxyfenoterol and fenoterol obtained by SPME generally concur with the whole blood concentrations determined by the conventional method indicating the utility of the proposed method. The proposed diffusion-based interface model has several advantages over other kinetic calibration models for in vivo SPME sampling including (i) it does not require the addition of a standard into the sample matrix during in vivo studies, (ii) it is simple and rapid and eliminates the need to pre-load appropriate standard onto the SPME extraction phase and (iii) the calibration constant for SPME can be calculated based on the diffusion coefficient, extraction time, fiber length and radius, and size of the boundary layer. In the current study, the experimental calibration constants of 338.9±30 mm(-3) and 298.5±25 mm(-3) are in excellent agreement with the theoretical calibration constants of 307.9 mm(-3) and 316.0 mm(-3) for fenoterol and methoxyfenoterol respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

Simple determination of fluoride in biological samples by headspace solid-phase microextraction and gas chromatography-tandem mass spectrometry.

PubMed

Kwon, Sun-Myung; Shin, Ho-Sang

2015-08-14

A simple and convenient method to detect fluoride in biological samples was developed. This method was based on derivatization with 2-(bromomethyl)naphthalene, headspace solid phase microextraction (HS-SPME) in a vial, and gas chromatography-tandem mass spectrometric detection. The HS-SPME parameters were optimized as follows: selection of CAR/PDMS fiber, 0.5% 2-(bromomethyl)naphthalene, 250 mg/L 15-crown-5-ether as a phase transfer catalyst, extraction and derivatization temperature of 95 °C, heating time of 20 min and pH of 7.0. Under the established conditions, the lowest limits of detection were 9 and 11 μg/L in 1.0 ml of plasma and urine, respectively, and the intra- and inter-day relative standard deviation was less than 7.7% at concentrations of 0.1 and 1.0 mg/L. The calibration curve showed good linearity of plasma and urine with r=0.9990 and r=0.9992, respectively. This method is simple, amenable to automation and environmentally friendly. Copyright © 2015 Elsevier B.V. All rights reserved.

Automated Sample Preparation (ASP): Development of a Rapid Method to Sequentially Isolate Nucleic Acids and Protein from Any Sample Type by a Cartridge-Based System

DTIC Science & Technology

2013-11-27

SECURITY CLASSIFICATION OF: CUBRC has developed an in-line, multi-analyte isolation technology that utilizes solid phase extraction chemistries to purify...goals. Specifically, CUBRC will design and manufacture a prototype cartridge(s) and test the prototype cartridge for its ability to isolate each...display a currently valid OMB control number. PLEASE DO NOT RETURN YOUR FORM TO THE ABOVE ADDRESS. CUBRC , Inc. P. O. Box 400 Buffalo, NY 14225 -1955

High average power diode pumped solid state laser

NASA Astrophysics Data System (ADS)

Gao, Yue; Wang, Yanjie; Chan, Amy; Dawson, Murray; Greene, Ben

2017-03-01

A new generation of high average power pulsed multi-joule solid state laser system has been developed at EOS Space Systems for various space related tracking applications. It is a completely diode pumped, fully automated multi-stage system consisting of a pulsed single longitudinal mode oscillator, three stages of pre-amplifiers, two stages of power amplifiers, completely sealed phase conjugate mirror or stimulated Brillouin scattering (SBS) cell and imaging relay optics with spatial filters in vacuum cells. It is capable of generating pulse energy up to 4.7 J, a beam quality M 2 ~ 3, pulse width between 10-20 ns, and a pulse repetition rate between 100-200 Hz. The system has been in service for more than two years with excellent performance and reliability.

The value of automated gel column agglutination technology in the identification of true inherited D blood types in massively transfused patients.

PubMed

Summers, Thomas; Johnson, Viviana V; Stephan, John P; Johnson, Gloria J; Leonard, George

2009-08-01

Massive transfusion of D- trauma patients in the combat setting involves the use of D+ red blood cells (RBCs) or whole blood along with suboptimal pretransfusion test result documentation. This presents challenges to the transfusion service of tertiary care military hospitals who ultimately receive these casualties because initial D typing results may only reflect the transfused RBCs. After patients are stabilized, mixed-field reaction results on D typing indicate the patient's true inherited D phenotype. This case series illustrates the utility of automated gel column agglutination in detecting mixed-field reactions in these patients. The transfusion service test results, including the automated gel column agglutination D typing results, of four massively transfused D- patients transfused D+ RBCs is presented. To test the sensitivity of the automated gel column agglutination method in detecting mixed-field agglutination reactions, a comparative analysis of three automated technologies using predetermined mixtures of D+ and D- RBCs is also presented. The automated gel column agglutination method detected mixed-field agglutination in D typing in all four patients and in the three prepared control specimens. The automated microwell tube method identified one of the three prepared control specimens as indeterminate, which was subsequently manually confirmed as a mixed-field reaction. The automated solid-phase method was unable to detect any mixed fields. The automated gel column agglutination method provides a sensitive means for detecting mixed-field agglutination reactions in the determination of the true inherited D phenotype of combat casualties transfused massive amounts of D+ RBCs.

[Developments in preparation and experimental method of solid phase microextraction fibers].

PubMed

Yi, Xu; Fu, Yujie

2004-09-01

Solid phase microextraction (SPME) is a simple and effective adsorption and desorption technique, which concentrates volatile or nonvolatile compounds from liquid samples or headspace of samples. SPME is compatible with analyte separation and detection by gas chromatography, high performance liquid chromatography, and other instrumental methods. It can provide many advantages, such as wide linear scale, low solvent and sample consumption, short analytical times, low detection limits, simple apparatus, and so on. The theory of SPME is introduced, which includes equilibrium theory and non-equilibrium theory. The novel development of fiber preparation methods and relative experimental techniques are discussed. In addition to commercial fiber preparation, different newly developed fabrication techniques, such as sol-gel, electronic deposition, carbon-base adsorption, high-temperature epoxy immobilization, are presented. Effects of extraction modes, selection of fiber coating, optimization of operating conditions, method sensitivity and precision, and systematical automation, are taken into considerations in the analytical process of SPME. A simple perspective of SPME is proposed at last.

Confirmatory and quantitative analysis of fatty acid esters of hydroxy fatty acids in serum by solid phase extraction coupled to liquid chromatography tandem mass spectrometry.

PubMed

López-Bascón, María Asunción; Calderón-Santiago, Mónica; Priego-Capote, Feliciano

2016-11-02

A novel class of endogenous mammalian lipids endowed with antidiabetic and anti-inflammatory properties has been recently discovered. These are fatty acid esters of hydroxy fatty acids (FAHFAs) formed by condensation between a hydroxy fatty acid and a fatty acid. FAHFAs are present in human serum and tissues at low nanomolar concentrations. Therefore, high sensitivity and selectivity profiling analysis of these compounds in clinical samples is demanded. An automated qualitative and quantitative method based on on-line coupling between solid phase extraction and liquid chromatography-tandem mass spectrometry has been here developed for determination of FAHFAs in serum with the required sensitivity and selectivity. Matrix effects were evaluated by preparation of calibration models in serum and methanol. Recovery factors ranged between 73.8 and 100% in serum. The within-day variability ranged from 7.1 to 13.8%, and the between-days variability varied from 9.3 to 21.6%, which are quite acceptable values taking into account the low concentration levels at which the target analytes are found. The method has been applied to a cohort of human serum samples to estimate the concentrations profiles as a function of the glycaemic state and obesity. Statistical analysis revealed three FAHFAs with levels significantly different depending on the glycaemic state or the body mass index. This automated method could be implemented in high-throughput analysis with minimum user assistance. Copyright © 2016 Elsevier B.V. All rights reserved.

On-line monitoring of the photocatalytic degradation of 2,4-D and dicamba using a solid-phase extraction-multisyringe flow injection system.

PubMed

Chávez-Moreno, Carmín; Ferrer, Laura; Hinojosa-Reyes, Laura; Hernández-Ramírez, Aracely; Cerdà, Víctor; Guzmán-Mar, Jorge

2013-11-15

A fully automated on-line system for monitoring the photocatalytic degradation of herbicides was developed using multisyringe flow injection analysis (MSFIA) coupled to a solid phase extraction (SPE) unit with UV detection. The calibration curves were linear in the concentration range of 100-1000 μg L(-1) for 3,6-dichloro-2-methoxybenzoic acid (dicamba) and 500-3000 μg L(-1) for 2,4-dichlorophenoxyacetic acid (2,4-D), while the detection limits were 30 and 135 μg L(-1) for dicamba and 2,4-D, respectively. The monitoring of the photocatalytic degradation (TiO2 anatase/UV 254 nm) of these two herbicides was performed by MSFIA-SPE system using a small sample volume (2 mL) in a fully automated approach. The degradation was assessed in ultrapure and drinking water with initial concentrations of 1000 and 2000 μg L(-1) for dicamba and 2,4-D, respectively. Degradation percentages of approximately 85% were obtained for both herbicides in ultrapure water after 45 min of photocatalytic treatment. A similar degradation efficiency in drinking water was observed for 2,4-D, whereas dicamba exhibited a lower degradation percentage (75%), which could be attributed to the presence of inorganic species in this kind of water. Copyright © 2013 Elsevier Ltd. All rights reserved.

Development of coatings for automated 96-blade solid phase microextraction-liquid chromatography-tandem mass spectrometry system, capable of extracting a wide polarity range of analytes from biological fluids.

PubMed

Mirnaghi, Fatemeh S; Pawliszyn, Janusz

2012-10-26

This work presents the development and evaluation of biocompatible polyacrylonitrile-polystyrene-divinylbenzene (PAN-PS-DVB) and polyacrylonitrile-phenylboronic acid (PAN-PBA) coatings for automated 96-blades (thin-film) solid phase microextraction (SPME) system, using high performance liquid chromatography (HPLC) coupled with tandem mass spectrometry (MS/MS). The SPME condition was optimized for 60 min equilibrium extraction and 40 min desorption for PAN-PS-DVB, and 120 min equilibrium extraction and 60 min desorption for PAN-PBA for parallel sample preparation of up to 96 samples. The thin film geometry of the SPME blades provided good extraction efficiency due to the larger surface area of the coating, and simultaneous sample preparation provided fast and accurate analysis. The PAN-PS-DVB and PAN-PBA 96-blade SPME coatings were evaluated for extraction of analytes in a wide range of polarity (log P=2.8 to -3.7), and they demonstrated efficient extraction recovery (3.5-98.9% for PAN-PS-DVB and 4.0-74.1% for PAN-PBA) for both polar and non-polar groups of compounds. Reusability, reproducibility, and reliability of the system were evaluated. The results demonstrated that both coatings presented chemical and mechanical stability and long-lasting extraction efficiency for more than 100 usages in phosphate-buffered saline (PBS) and human plasma. Copyright © 2012 Elsevier B.V. All rights reserved.

Development of a fully automated on-line solid phase extraction and high-performance liquid chromatography with diode array detection method for the pharmacokinetic evaluation of bavachinin: a study on absolute bioavailability and dose proportionality.

PubMed

Liu, Lei; Liu, Kang-Ning; Wen, Ya-Bin; Zhang, Han-Wen; Lu, Ya-Xin; Yin, Zheng

2012-04-15

A fully automated on-line solid-phase extraction (SPE) and high-performance liquid chromatography (HPLC) with diode array detection (DAD) method was developed for determination of bavachinin in mouse plasma. Analytical process was performed on two reversed-phase columns (SPE cartridge and analytical column) connected via a Valco 6-port switching valve. Plasma samples (10 μL) were injected directly onto a C18 SPE cartridge (MF Ph-1 C18, 10 mm × 4 mm, 5 μm) and the biological matrix was washed out for 2 min with the loading solvent (5 mM NaH(2)PO(4) buffer, pH 3.5) at a flow rate of 1 mL/min. By rotation of the switching valve, bavachinin was eluted from the SPE cartridge in the back-flush mode and transferred to the analytical column (Venusil MP C18, 4.6 mm × 150 mm, 5 μm) by the chromatographic mobile phase consisted of acetonitrile-5mM NaH(2)PO(4) buffer 65/35 (v/v, pH 3.5) at a flow rate of 1 mL/min. The complete cycle of the on-line SPE purification and chromatographic separation of the analyte was 13 min with UV detection performed at 236 nm. Calibration curve with good linearity (r=0.9997) was obtained in the range of 20-4000 ng/mL in mouse plasma. The intra-day and inter-day precisions (RSD) of bavachinin were in the range of 0.20-2.32% and the accuracies were between 98.47% and 102.95%. The lower limit of quantification (LLOQ) of the assay was 20 ng/mL. In conclusion, the established automated on-line SPE-HPLC-DAD method demonstrated good performance in terms of linearity, specificity, detection and quantification limits, precision and accuracy, and was successfully utilized to quantify bavachinin in mouse plasma to support the pharmacokinetic (PK) studies. The PK properties of bavachinin were characterized as rapid oral absorption, high clearance, and poor absolute bioavailability. Copyright © 2012. Published by Elsevier B.V.

Assessment of Operational Automated Guideway Systems - Airtrans (Phase II)

DOT National Transportation Integrated Search

1980-01-01

This study, Phase II, completes the assessment of AIRTRANS, the automated guideway system located at the Dallas-Fort Worth Airport. The Phase I assessment report: "Assessment of Operational Automated Guideway Systems--AIRTRANS (Phase I)" (PB-261 339)...

Finite element methods for the biomechanics of soft hydrated tissues: nonlinear analysis and adaptive control of meshes.

PubMed

Spilker, R L; de Almeida, E S; Donzelli, P S

1992-01-01

This chapter addresses computationally demanding numerical formulations in the biomechanics of soft tissues. The theory of mixtures can be used to represent soft hydrated tissues in the human musculoskeletal system as a two-phase continuum consisting of an incompressible solid phase (collagen and proteoglycan) and an incompressible fluid phase (interstitial water). We first consider the finite deformation of soft hydrated tissues in which the solid phase is represented as hyperelastic. A finite element formulation of the governing nonlinear biphasic equations is presented based on a mixed-penalty approach and derived using the weighted residual method. Fluid and solid phase deformation, velocity, and pressure are interpolated within each element, and the pressure variables within each element are eliminated at the element level. A system of nonlinear, first-order differential equations in the fluid and solid phase deformation and velocity is obtained. In order to solve these equations, the contributions of the hyperelastic solid phase are incrementally linearized, a finite difference rule is introduced for temporal discretization, and an iterative scheme is adopted to achieve equilibrium at the end of each time increment. We demonstrate the accuracy and adequacy of the procedure using a six-node, isoparametric axisymmetric element, and we present an example problem for which independent numerical solution is available. Next, we present an automated, adaptive environment for the simulation of soft tissue continua in which the finite element analysis is coupled with automatic mesh generation, error indicators, and projection methods. Mesh generation and updating, including both refinement and coarsening, for the two-dimensional examples examined in this study are performed using the finite quadtree approach. The adaptive analysis is based on an error indicator which is the L2 norm of the difference between the finite element solution and a projected finite element solution. Total stress, calculated as the sum of the solid and fluid phase stresses, is used in the error indicator. To allow the finite difference algorithm to proceed in time using an updated mesh, solution values must be transferred to the new nodal locations. This rezoning is accomplished using a projected field for the primary variables. The accuracy and effectiveness of this adaptive finite element analysis is demonstrated using a linear, two-dimensional, axisymmetric problem corresponding to the indentation of a thin sheet of soft tissue. The method is shown to effectively capture the steep gradients and to produce solutions in good agreement with independent, converged, numerical solutions.

Automated electrochemical synthesis and photoelectrochemical characterization of Zn1-xCo(x)O thin films for solar hydrogen production.

PubMed

Jaramillo, Thomas F; Baeck, Sung-Hyeon; Kleiman-Shwarsctein, Alan; Choi, Kyoung-Shin; Stucky, Galen D; McFarland, Eric W

2005-01-01

High-throughput electrochemical methods have been developed for the investigation of Zn1-xCo(x)O films for photoelectrochemical hydrogen production from water. A library of 120 samples containing 27 different compositions (0

Two-dimensional parallel array technology as a new approach to automated combinatorial solid-phase organic synthesis

PubMed

Brennan; Biddison; Frauendorf; Schwarcz; Keen; Ecker; Davis; Tinder; Swayze

1998-01-01

An automated, 96-well parallel array synthesizer for solid-phase organic synthesis has been designed and constructed. The instrument employs a unique reagent array delivery format, in which each reagent utilized has a dedicated plumbing system. An inert atmosphere is maintained during all phases of a synthesis, and temperature can be controlled via a thermal transfer plate which holds the injection molded reaction block. The reaction plate assembly slides in the X-axis direction, while eight nozzle blocks holding the reagent lines slide in the Y-axis direction, allowing for the extremely rapid delivery of any of 64 reagents to 96 wells. In addition, there are six banks of fixed nozzle blocks, which deliver the same reagent or solvent to eight wells at once, for a total of 72 possible reagents. The instrument is controlled by software which allows the straightforward programming of the synthesis of a larger number of compounds. This is accomplished by supplying a general synthetic procedure in the form of a command file, which calls upon certain reagents to be added to specific wells via lookup in a sequence file. The bottle position, flow rate, and concentration of each reagent is stored in a separate reagent table file. To demonstrate the utility of the parallel array synthesizer, a small combinatorial library of hydroxamic acids was prepared in high throughput mode for biological screening. Approximately 1300 compounds were prepared on a 10 μmole scale (3-5 mg) in a few weeks. The resulting crude compounds were generally >80% pure, and were utilized directly for high throughput screening in antibacterial assays. Several active wells were found, and the activity was verified by solution-phase synthesis of analytically pure material, indicating that the system described herein is an efficient means for the parallel synthesis of compounds for lead discovery. Copyright 1998 John Wiley & Sons, Inc.

Determination of aflatoxins in food samples by automated on-line in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry.

PubMed

Nonaka, Y; Saito, K; Hanioka, N; Narimatsu, S; Kataoka, H

2009-05-15

A simple and sensitive automated method for determination of aflatoxins (B1, B2, G1, and G2) in nuts, cereals, dried fruits, and spices was developed consisting of in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-mass spectrometry (LC-MS). Aflatoxins were separated within 8 min by high-performance liquid chromatography using a Zorbax Eclipse XDB-C8 column with methanol/acetonitrile (60/40, v/v): 5mM ammonium formate (45:55) as the mobile phase. Electrospray ionization conditions in the positive ion mode were optimized for MS detection of aflatoxins. The pseudo-molecular ions [M+H](+) were used to detect aflatoxins in selected ion monitoring (SIM) mode. The optimum in-tube SPME conditions were 25draw/eject cycles of 40 microL of sample using a Supel-Q PLOT capillary column as an extraction device. The extracted aflatoxins were readily desorbed from the capillary by passage of the mobile phase, and no carryover was observed. Using the in-tube SPME LC-MS with SIM method, good linearity of the calibration curve (r>0.9994) was obtained in the concentration range of 0.05-2.0 ng/mL using aflatoxin M1 as an internal standard, and the detection limits (S/N=3) of aflatoxins were 2.1-2.8 pg/mL. The in-tube SPME method showed >23-fold higher sensitivity than the direct injection method (10 microL injection volume). The within-day and between-day precision (relative standard deviations) at the concentration of 1 ng/mL aflatoxin mixture were below 3.3% and 7.7% (n=5), respectively. This method was applied successfully to analysis of food samples without interference peaks. The recoveries of aflatoxins spiked into nuts and cereals were >80%, and the relative standard deviations were <11.2%. Aflatoxins were detected at <10 ng/g in several commercial food samples.

Simultaneous determination of four trace estrogens in feces, leachate, tap and groundwater using solid-liquid extraction/auto solid-phase extraction and high-performance liquid chromatography with fluorescence detection.

PubMed

Liu, Na; Shi, Yue-e; Li, Mengyan; Zhang, Ting-di; Gao, Song

2015-10-01

A simple and selective high-performance liquid chromatography method coupled with fluorescence detection was developed for the simultaneous measurement of trace levels of four estrogens (estrone, estradiol, estriol and 17α-ethynyl estradiol) in environmental matrices. For feces samples, solid-liquid extraction was applied with a 1:1 v/v mixture of acetonitrile and ethyl acetate as the extraction solvent. For liquid samples (e.g., leachate and groundwater), hydrophobic/lipophilic balanced automated solid-phase extraction disks were selected due to their high recoveries compared to conventional C18 disks. Chromatographic separations were performed on a reversed-phase C18 column gradient-eluted with a 45:55 v/v mixture of acetonitrile and water. The detection limits were down to 1.1 × 10(-2) (estrone), 4.11 × 10(-4) (estradiol), 5.2 × 10(-3) (estriol) and 7.18 × 10(-3) μg/L (17α-ethynyl estradiol) at excitation/emission wavelengths of 288/310 nm, with recoveries in the range of 96.9 ± 3.2-105.4 ± 3.2% (n = 3). The method was successfully applied to determine estrogens in feces and water samples collected at livestock farms and a major river in Northeast China. We observed relatively high abundance and widespread distribution of all four estrogens in our sample collections, implying the urgency for a comprehensive and intricate investigation of estrogenic fate and contamination in our researched area. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Liquid chromatography-mass spectrometry platform for both small neurotransmitters and neuropeptides in blood, with automatic and robust solid phase extraction

NASA Astrophysics Data System (ADS)

Johnsen, Elin; Leknes, Siri; Wilson, Steven Ray; Lundanes, Elsa

2015-03-01

Neurons communicate via chemical signals called neurotransmitters (NTs). The numerous identified NTs can have very different physiochemical properties (solubility, charge, size etc.), so quantification of the various NT classes traditionally requires several analytical platforms/methodologies. We here report that a diverse range of NTs, e.g. peptides oxytocin and vasopressin, monoamines adrenaline and serotonin, and amino acid GABA, can be simultaneously identified/measured in small samples, using an analytical platform based on liquid chromatography and high-resolution mass spectrometry (LC-MS). The automated platform is cost-efficient as manual sample preparation steps and one-time-use equipment are kept to a minimum. Zwitter-ionic HILIC stationary phases were used for both on-line solid phase extraction (SPE) and liquid chromatography (capillary format, cLC). This approach enabled compounds from all NT classes to elute in small volumes producing sharp and symmetric signals, and allowing precise quantifications of small samples, demonstrated with whole blood (100 microliters per sample). An additional robustness-enhancing feature is automatic filtration/filter back-flushing (AFFL), allowing hundreds of samples to be analyzed without any parts needing replacement. The platform can be installed by simple modification of a conventional LC-MS system.

Automated Online Solid-Phase Derivatization for Sensitive Quantification of Endogenous S-Nitrosoglutathione and Rapid Capture of Other Low-Molecular-Mass S-Nitrosothiols.

PubMed

Wang, Xin; Garcia, Carlos T; Gong, Guanyu; Wishnok, John S; Tannenbaum, Steven R

2018-02-06

S-Nitrosothiols (RSNOs) constitute a circulating endogenous reservoir of nitric oxide and have important biological activities. In this study, an online coupling of solid-phase derivatization (SPD) with liquid chromatography-mass spectrometry (LC-MS) was developed and applied in the analysis of low-molecular-mass RSNOs. A derivatizing-reagent-modified polymer monolithic column was prepared and adapted for online SPD-LC-MS. Analytes from the LC autosampler flowed through the monolithic column for derivatization and then directly into the LC-MS for analysis. This integration of the online derivatization, LC separation, and MS detection facilitated system automation, allowing rapid, laborsaving, and sensitive detection of RSNOs. S-Nitrosoglutathione (GSNO) was quantified using this automated online method with good linearity (R 2 = 0.9994); the limit of detection was 0.015 nM. The online SPD-LC-MS method has been used to determine GSNO levels in mouse samples, 138 ± 13.2 nM of endogenous GSNO was detected in mouse plasma. Besides, the GSNO concentrations in liver (64.8 ± 11.3 pmol/mg protein), kidney (47.2 ± 6.1 pmol/mg protein), heart (8.9 ± 1.8 pmol/mg protein), muscle (1.9 ± 0.3 pmol/mg protein), hippocampus (5.3 ± 0.9 pmol/mg protein), striatum (6.7 ± 0.6 pmol/mg protein), cerebellum (31.4 ± 6.5 pmol/mg protein), and cortex (47.9 ± 4.6 pmol/mg protein) were also successfully quantified. When the derivatization was performed within 8 min, followed by LC-MS detection, samples could be rapidly analyzed compared with the offline manual method. Other low-molecular-mass RSNOs, such as S-nitrosocysteine and S-nitrosocysteinylglycine, were captured by rapid precursor-ion scanning, showing that the proposed method is a potentially powerful tool for capture, identification, and quantification of RSNOs in biological samples.

Automation of closed environments in space for human comfort and safety

NASA Technical Reports Server (NTRS)

1990-01-01

The Environmental Control and Life Support System (ECLSS) for the Space Station Freedom and future colonization of the Moon and Mars presents new challenges for present technologies. Current plans call for a crew of 8 to live in a safe, shirt-sleeve environment for 90 days without ground support. Because of these requirements, all life support systems must be self-sufficient and reliable. The ECLSS is composed of six subsystems. The temperature and humidity control (THC) subsystem maintains the cabin temperature and humidity at a comfortable level. The atmosphere control and supply (ACS) subsystem insures proper cabin pressure and partial pressures of oxygen and nitrogen. To protect the space station from fire damage, the fire detection and suppression (FDS) subsystem provides fire sensing alarms and extinguishers. The waste management (WM) subsystem compacts solid wastes for return to Earth, and collects urine for water recovery. Because it is impractical, if not impossible, to supply the station with enough fresh air and water for the duration of the space station's extended mission, these elements are recycled. The atmosphere revitalization (AR) subsystem removes CO2 and other dangerous contaminants from the air. The water recovery and management (WRM) subsystem collects and filters condensate from the cabin to replenish potable water supplies, and processes urine and other waste waters to replenish hygiene water supplies. These subsystems are not fully automated at this time. Furthermore, the control of these subsystems is not presently integrated; they are largely independent of one another. A fully integrated and automated ECLSS would increase astronauts' productivity and contribute to their safety and comfort. The Kansas State University Advanced Design Team is in the process of researching and designing controls for the automation of the ECLSS for Space Station Freedom and beyond. The approach chosen to solve this problem is to divide the design into three phases. The first phase is to research the ECLSS as a whole system and then concentrate efforts on the automation of a single subsystem. The AR subsystem was chosen for our focus. During the second phase, the system control process will then be applied to the AR subsystem.

Physics of automated driving in framework of three-phase traffic theory.

PubMed

Kerner, Boris S

2018-04-01

We have revealed physical features of automated driving in the framework of the three-phase traffic theory for which there is no fixed time headway to the preceding vehicle. A comparison with the classical model approach to automated driving for which an automated driving vehicle tries to reach a fixed (desired or "optimal") time headway to the preceding vehicle has been made. It turns out that automated driving in the framework of the three-phase traffic theory can exhibit the following advantages in comparison with the classical model of automated driving: (i) The absence of string instability. (ii) Considerably smaller speed disturbances at road bottlenecks. (iii) Automated driving vehicles based on the three-phase theory can decrease the probability of traffic breakdown at the bottleneck in mixed traffic flow consisting of human driving and automated driving vehicles; on the contrary, even a single automated driving vehicle based on the classical approach can provoke traffic breakdown at the bottleneck in mixed traffic flow.

Physics of automated driving in framework of three-phase traffic theory

NASA Astrophysics Data System (ADS)

Kerner, Boris S.

2018-04-01

We have revealed physical features of automated driving in the framework of the three-phase traffic theory for which there is no fixed time headway to the preceding vehicle. A comparison with the classical model approach to automated driving for which an automated driving vehicle tries to reach a fixed (desired or "optimal") time headway to the preceding vehicle has been made. It turns out that automated driving in the framework of the three-phase traffic theory can exhibit the following advantages in comparison with the classical model of automated driving: (i) The absence of string instability. (ii) Considerably smaller speed disturbances at road bottlenecks. (iii) Automated driving vehicles based on the three-phase theory can decrease the probability of traffic breakdown at the bottleneck in mixed traffic flow consisting of human driving and automated driving vehicles; on the contrary, even a single automated driving vehicle based on the classical approach can provoke traffic breakdown at the bottleneck in mixed traffic flow.

Automated solid-phase extraction-liquid chromatography-tandem mass spectrometry analysis of 6-acetylmorphine in human urine specimens: application for a high-throughput urine analysis laboratory.

PubMed

Robandt, P V; Bui, H M; Scancella, J M; Klette, K L

2010-10-01

An automated solid-phase extraction-liquid chromatography- tandem mass spectrometry (SPE-LC-MS-MS) method using the Spark Holland Symbiosis Pharma SPE-LC coupled to a Waters Quattro Micro MS-MS was developed for the analysis of 6-acetylmorphine (6-AM) in human urine specimens. The method was linear (R² = 0.9983) to 100 ng/mL, with no carryover at 200 ng/mL. Limits of quantification and detection were found to be 2 ng/mL. Interrun precision calculated as percent coefficient of variation (%CV) and evaluated by analyzing five specimens at 10 ng/mL over nine batches (n = 45) was 3.6%. Intrarun precision evaluated from 0 to 100 ng/mL ranged from 1.0 to 4.4%CV. Other opioids (codeine, morphine, oxycodone, oxymorphone, hydromorphone, hydrocodone, and norcodeine) did not interfere in the detection, quantification, or chromatography of 6-AM or the deuterated internal standard. The quantified values for 41 authentic human urine specimens previously found to contain 6-AM by a validated gas chromatography (GC)-MS method were compared to those obtained by the SPE-LC-MS-MS method. The SPE-LC-MS-MS procedure eliminates the human factors of specimen handling, extraction, and derivatization, thereby reducing labor costs and rework resulting from human error or technique issues. The time required for extraction and analysis was reduced by approximately 50% when compared to a validated 6-AM procedure using manual SPE and GC-MS analysis.

Automated synthesis of new ferrocenyl-modified oligonucleotides: study of their properties in solution

PubMed Central

Navarro, Aude-Emmanuelle; Spinelli, Nicolas; Moustrou, Corinne; Chaix, Carole; Mandrand, Bernard; Brisset, Hugues

2004-01-01

We have developed new ferrocenyl-modified oligonucleotide (ODN) probes for electrochemical DNA sensors. A monofunctional ferrocene containing phosphoramidite group has been prepared, and a new bisfunctional ferrocene containing phosphoramidite and dimethoxytrityl (DMT) groups has been developed. These ferrocenyl-phosphoramidites have been directly employed in an automated solid-phase DNA synthesizer using phosphoramidite chemistry. The advantages of this method are that it allows a non-specialist in nucleotide chemistry to access labeled ODNs and that it has demonstrated good results. ODNs modified at the 3′ and/or 5′ extremities have been prepared, with the incorporation of the ferrocenyl group into the chain. The 5′ position appears to be more important due to its particular behavior. The thermal stability and electrochemical properties of these new ODN ferrocenes were analyzed before and after hybridization with different ODNs. The feasibility of using these new ferrocenyl-labeled ODNs in DNA sensors has been demonstrated. PMID:15466597

Direct on-chip DNA synthesis using electrochemically modified gold electrodes as solid support

NASA Astrophysics Data System (ADS)

Levrie, Karen; Jans, Karolien; Schepers, Guy; Vos, Rita; Van Dorpe, Pol; Lagae, Liesbet; Van Hoof, Chris; Van Aerschot, Arthur; Stakenborg, Tim

2018-04-01

DNA microarrays have propelled important advancements in the field of genomic research by enabling the monitoring of thousands of genes in parallel. The throughput can be increased even further by scaling down the microarray feature size. In this respect, microelectronics-based DNA arrays are promising as they can leverage semiconductor processing techniques with lithographic resolutions. We propose a method that enables the use of metal electrodes for de novo DNA synthesis without the need for an insulating support. By electrochemically functionalizing gold electrodes, these electrodes can act as solid support for phosphoramidite-based synthesis. The proposed method relies on the electrochemical reduction of diazonium salts, enabling site-specific incorporation of hydroxyl groups onto the metal electrodes. An automated DNA synthesizer was used to couple phosphoramidite moieties directly onto the OH-modified electrodes to obtain the desired oligonucleotide sequence. Characterization was done via cyclic voltammetry and fluorescence microscopy. Our results present a valuable proof-of-concept for the integration of solid-phase DNA synthesis with microelectronics.

Analysis of trace contamination of phthalate esters in ultrapure water using a modified solid-phase extraction procedure and automated thermal desorption-gas chromatography/mass spectrometry.

PubMed

Liu, Hsu-Chuan; Den, Walter; Chan, Shu-Fei; Kin, Kuan Tzu

2008-04-25

The present study was aimed to develop a procedure modified from the conventional solid-phase extraction (SPE) method for the analysis of trace concentration of phthalate esters in industrial ultrapure water (UPW). The proposed procedure allows UPW sample to be drawn through a sampling tube containing hydrophobic sorbent (Tenax TA) to concentrate the aqueous phthalate esters. The solid trap was then demoisturized by two-stage gas drying before subjecting to thermal desorption and analysis by gas chromatography-mass spectrometry. This process removes the solvent extraction procedure necessary for the conventional SPE method, and permits automation of the analytical procedure for high-volume analyses. Several important parameters, including desorption temperature and duration, packing quantity and demoisturizing procedure, were optimized in this study based on the analytical sensitivity for a standard mixture containing five different phthalate esters. The method detection limits for the five phthalate esters were between 36 ng l(-1) and 95 ng l(-1) and recovery rates between 15% and 101%. Dioctyl phthalate (DOP) was not recovered adequately because the compound was both poorly adsorbed and desorbed on and off Tenax TA sorbents. Furthermore, analyses of material leaching from poly(vinyl chloride) (PVC) tubes as well as the actual water samples showed that di-n-butyl phthalate (DBP) and di(2-ethylhexyl) phthalate (DEHP) were the common contaminants detected from PVC contaminated UPW and the actual UPW, as well as in tap water. The reduction of DEHP in the production processes of actual UPW was clearly observed, however a DEHP concentration of 0.20 microg l(-1) at the point of use was still being quantified, suggesting that the contamination of phthalate esters could present a barrier to the future cleanliness requirement of UPW. The work demonstrated that the proposed modified SPE procedure provided an effective method for rapid analysis and contamination identification in UPW production lines.

Multiresidue determination of 114 multiclass pesticides in flue-cured tobacco by solid-phase extraction coupled with gas chromatography and tandem mass spectrometry.

PubMed

Cao, Jianmin; Sun, Na; Yu, Weisong; Pang, Xueli; Lin, Yingnan; Kong, Fanyu; Qiu, Jun

2016-12-01

A sensitive and robust multiresidue method for the simultaneous analysis of 114 pesticides in tobacco was developed based on solid-phase extraction coupled with gas chromatography and tandem mass spectrometry. In this strategy, tobacco samples were extracted with acetonitrile and cleaned up with a multilayer solid-phase extraction cartridge Cleanert TPT using acetonitrile/toluene (3:1) as the elution solvent. Two internal standards of different polarity were used to meet simultaneous pesticides quantification demands in the tobacco matrix. Satisfactory linearity in the range of 10-500 ng/mL was obtained for all 114 pesticides with linear regression coefficients higher than 0.994. The limit of detection and limit of quantification values were 0.02-5.27 and 0.06-17.6 ng/g, respectively. For most of the pesticides, acceptable recoveries in the range of 70-120% and repeatabilities (relative standard deviation) of <11% were achieved at spiking levels of 20, 100, and 400 ng/g. Compared with the reported multiresidue analytical method, the proposed method provided a cleaner test solution with smaller amounts of pigments, fatty acids as well as other undesirable interferences. The development and validation of the high sensitivity, high selectivity, easy automation, and high-throughput analytical method meant that it could be successfully used for the determination of pesticides in tobacco samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Inorganic-organic hybrid coating material for the online in-tube solid-phase microextraction of monohydroxy polycyclic aromatic hydrocarbons in urine.

PubMed

Wang, ShuLing; Xu, Hui

2016-12-01

An inorganic-organic hybrid nanocomposite (zinc oxide/polypyrrole) that represents a novel kind of coating for in-tube solid-phase microextraction is reported. The composite coating was prepared by a facile electrochemical polymerization strategy on the inner surface of a stainless-steel tube. Based on the coated tube, a novel online in-tube solid-phase microextraction with liquid chromatography and mass spectrometry method was developed and applied for the extraction of three monohydroxy polycyclic aromatic hydrocarbons in human urine. The coating displayed good extraction ability toward monohydroxy polycyclic aromatic hydrocarbons. In addition, long lifespan, excellent stability, and good compression resistance were also obtained for the coating. The experimental conditions affecting the extraction were optimized systematically. Under the optimal conditions, the limits of detection and quantification were in the range of 0.039-0.050 and 0.130-0.167 ng/mL, respectively. Good linearity (0.2-100 ng/mL) was obtained with correlation coefficients larger than 0.9967. The repeatability, expressed as relative standard deviation, ranged between 2.5% and 9.4%. The method offered the advantage of process simplicity, rapidity, automation, and sensitivity in the analysis of human urinary monohydroxy polycyclic aromatic hydrocarbons in two different cities of Hubei province. An acceptable recovery of monohydroxy polycyclic aromatic hydrocarbons (64-122%) represented the additional attractive features of the method in real urine analysis. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Automated headspace solid-phase dynamic extraction to analyse the volatile fraction of food matrices.

PubMed

Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Rubiolo, Patrizia; Sgorbini, Barbara

2004-01-23

High concentration capacity headspace techniques (headspace solid-phase microextraction (HS-SPME) and headspace sorptive extraction (HSSE)) are a bridge between static and dynamic headspace, since they give high concentration factors as does dynamic headspace (D-HS), and are as easy to apply and as reproducible as static headspace (S-HS). In 2000, Chromtech (Idstein, Germany) introduced an inside-needle technique for vapour and liquid sampling, solid-phase dynamic extraction (SPDE), also known as "the magic needle". In SPDE, analytes are concentrated on a 50 microm film of polydimethylsiloxane (PDMS) and activated carbon (10%) coated onto the inside wall of the stainless steel needle (5 cm) of a 2.5 ml gas tight syringe. When SPDE is used for headspace sampling (HS-SPDE), a fixed volume of the headspace of the sample under investigation is sucked up an appropriate number of times with the gas tight syringe and an analyte amount suitable for a reliable GC or GC-MS analysis accumulates in the polymer coating the needle wall. This article describes the preliminary results of both a study on the optimisation of sampling parameters conditioning HS-SPDE recovery, through the analysis of a standard mixture of highly volatile compounds (beta-pinene, isoamyl acetate and linalool) and of the HS-SPDE-GC-MS analyses of aromatic plants and food matrices. This study shows that HS-SPDE is a successful technique for HS-sampling with high concentration capability, good repeatability and intermediate precision, also when it is compared to HS-SPME.

In Situ Miniaturised Solid Phase Extraction (m-SPE) for Organic Pollutants in Seawater Samples

PubMed Central

Abaroa-Pérez, B.; Sánchez-Almeida, G.; Hernández-Brito, J. J.

2018-01-01

Solid phase extraction (SPE) is a consolidated technique for determining pollutants in seawater samples. The current tendency is to miniaturise systems that extract and determine pollutants in the environment, reducing the use of organic solvents, while maintaining the quality in the extraction and preconcentration. On the other hand, there is a need to develop new extraction systems that can be fitted to in situ continual monitoring buoys, especially for the marine environment. This work has developed a first model of a low-pressure micro-SPE (m-SPE) for persistent organic pollutants (POPs) that can be simply applied to in situ monitoring in the marine environment. This system reduces the volumes of sample and solvents required in the laboratory in comparison with conventional SPE. In the future, it could be used in automated or robotic systems in marine technologies such as marine gliders and oceanographic buoys. This system has been optimised and validated to determine polycyclic aromatic hydrocarbons (PAH) in seawater samples, but it could also be applied to other kinds of persistent organic pollutants (POPs) and emerging pollutants. PMID:29805837

A review on automated sorting of source-separated municipal solid waste for recycling.

PubMed

Gundupalli, Sathish Paulraj; Hait, Subrata; Thakur, Atul

2017-02-01

A crucial prerequisite for recycling forming an integral part of municipal solid waste (MSW) management is sorting of useful materials from source-separated MSW. Researchers have been exploring automated sorting techniques to improve the overall efficiency of recycling process. This paper reviews recent advances in physical processes, sensors, and actuators used as well as control and autonomy related issues in the area of automated sorting and recycling of source-separated MSW. We believe that this paper will provide a comprehensive overview of the state of the art and will help future system designers in the area. In this paper, we also present research challenges in the field of automated waste sorting and recycling. Copyright © 2016 Elsevier Ltd. All rights reserved.

Simplified Automated Image Analysis for Detection and Phenotyping of Mycobacterium tuberculosis on Porous Supports by Monitoring Growing Microcolonies

PubMed Central

den Hertog, Alice L.; Visser, Dennis W.; Ingham, Colin J.; Fey, Frank H. A. G.; Klatser, Paul R.; Anthony, Richard M.

2010-01-01

Background Even with the advent of nucleic acid (NA) amplification technologies the culture of mycobacteria for diagnostic and other applications remains of critical importance. Notably microscopic observed drug susceptibility testing (MODS), as opposed to traditional culture on solid media or automated liquid culture, has shown potential to both speed up and increase the provision of mycobacterial culture in high burden settings. Methods Here we explore the growth of Mycobacterial tuberculosis microcolonies, imaged by automated digital microscopy, cultured on a porous aluminium oxide (PAO) supports. Repeated imaging during colony growth greatly simplifies “computer vision” and presumptive identification of microcolonies was achieved here using existing publically available algorithms. Our system thus allows the growth of individual microcolonies to be monitored and critically, also to change the media during the growth phase without disrupting the microcolonies. Transfer of identified microcolonies onto selective media allowed us, within 1-2 bacterial generations, to rapidly detect the drug susceptibility of individual microcolonies, eliminating the need for time consuming subculturing or the inoculation of multiple parallel cultures. Significance Monitoring the phenotype of individual microcolonies as they grow has immense potential for research, screening, and ultimately M. tuberculosis diagnostic applications. The method described is particularly appealing with respect to speed and automation. PMID:20544033

Comparison of computer versus manual determination of pulmonary nodule volumes in CT scans

NASA Astrophysics Data System (ADS)

Biancardi, Alberto M.; Reeves, Anthony P.; Jirapatnakul, Artit C.; Apanasovitch, Tatiyana; Yankelevitz, David; Henschke, Claudia I.

2008-03-01

Accurate nodule volume estimation is necessary in order to estimate the clinically relevant growth rate or change in size over time. An automated nodule volume-measuring algorithm was applied to a set of pulmonary nodules that were documented by the Lung Image Database Consortium (LIDC). The LIDC process model specifies that each scan is assessed by four experienced thoracic radiologists and that boundaries are to be marked around the visible extent of the nodules for nodules 3 mm and larger. Nodules were selected from the LIDC database with the following inclusion criteria: (a) they must have a solid component on a minimum of three CT image slices and (b) they must be marked by all four LIDC radiologists. A total of 113 nodules met the selection criterion with diameters ranging from 3.59 mm to 32.68 mm (mean 9.37 mm, median 7.67 mm). The centroid of each marked nodule was used as the seed point for the automated algorithm. 95 nodules (84.1%) were correctly segmented, but one was considered not meeting the first selection criterion by the automated method; for the remaining ones, eight (7.1%) were structurally too complex or extensively attached and 10 (8.8%) were considered not properly segmented after a simple visual inspection by a radiologist. Since the LIDC specifications, as aforementioned, instruct radiologists to include both solid and sub-solid parts, the automated method core capability of segmenting solid tissues was augmented to take into account also the nodule sub-solid parts. We ranked the distances of the automated method estimates and the radiologist-based estimates from the median of the radiologist-based values. The automated method was in 76.6% of the cases closer to the median than at least one of the values derived from the manual markings, which is a sign of a very good agreement with the radiologists' markings.

Evaluation of ionic liquids supported on silica as a sorbent for fully automated online solid-phase extraction with LC-MS determination of sulfonamides in bovine milk samples.

PubMed

da Silva, Meire Ribeiro; Mauro Lanças, Fernando

2018-03-10

Sulfonamides are antibiotics widely used in the treatment of diseases in dairy cattle. However, their indiscriminate use for disease control may lead to their presence in tissues and milk and their determination requires a sample preparation step as part of an analytical approach. Among the several sample preparation techniques available, those based upon the use of sorptive materials have been widely employed. Recently, the application of ionic liquids immobilized on silica surfaces or polymeric materials has been evaluated for such an application. This manuscript addresses the evaluation of silica-based ionic liquid obtained by a sol-gel synthesis process by basic catalysis as sorbent for online solid-phase extraction with liquid chromatography and electrospray ionization time-of-flight mass spectrometry for sulfonamides determination. Infrared vibrational spectroscopy confirmed the presence of the ionic liquid on the silica surface, suggesting that the ionic liquid was anchored on to the silica surface. Other sorbents varying the ionic liquid alkyl chain were also synthesized and evaluated by off-line solid-phase extraction in the sulfonamide extraction. As the length of the alkyl chain increased, the amount of extracted sulfonamides decreased, possibly due to a decrease in the electrostatic interaction caused by the reduction in the polarity, as well as the presence of a hexafluorophosphate anion that increases the hydrophobic character of the material. The use of 1-butyl-3-methylimidazolium hexafluorophosphate as a selective ionic liquid sorbent enabled the isolation and sulfonamide preconcentration in bovine milk by online solid-phase extraction with liquid chromatography and electrospray ionization time-of-flight mass spectrometry. The limit of quantification for the method developed was 5-7, 5 μg/mL, with extraction recoveries ranging between 74 and 93% and intra- and interassay between 1.5-12.5 and 2.3-13.1, respectively. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimization of the transition path of the head hardening with using the genetic algorithms

NASA Astrophysics Data System (ADS)

Wróbel, Joanna; Kulawik, Adam

2016-06-01

An automated method of choice of the transition path of the head hardening in heat treatment process for the plane steel element is proposed in this communication. This method determines the points on the path of moving heat source using the genetic algorithms. The fitness function of the used algorithm is determined on the basis of effective stresses and yield point depending on the phase composition. The path of the hardening tool and also the area of the heat affected zone is determined on the basis of obtained points. A numerical model of thermal phenomena, phase transformations in the solid state and mechanical phenomena for the hardening process is implemented in order to verify the presented method. A finite element method (FEM) was used for solving the heat transfer equation and getting required temperature fields. The moving heat source is modeled with a Gaussian distribution and the water cooling is also included. The macroscopic model based on the analysis of the CCT and CHT diagrams of the medium-carbon steel is used to determine the phase transformations in the solid state. A finite element method is also used for solving the equilibrium equations giving us the stress field. The thermal and structural strains are taken into account in the constitutive relations.

Vessel suppressed chest Computed Tomography for semi-automated volumetric measurements of solid pulmonary nodules.

PubMed

Milanese, Gianluca; Eberhard, Matthias; Martini, Katharina; Vittoria De Martini, Ilaria; Frauenfelder, Thomas

2018-04-01

To evaluate whether vessel-suppressed computed tomography (VSCT) can be reliably used for semi-automated volumetric measurements of solid pulmonary nodules, as compared to standard CT (SCT) MATERIAL AND METHODS: Ninety-three SCT were elaborated by dedicated software (ClearRead CT, Riverain Technologies, Miamisburg, OH, USA), that allows subtracting vessels from lung parenchyma. Semi-automated volumetric measurements of 65 solid nodules were compared between SCT and VSCT. The measurements were repeated by two readers. For each solid nodule, volume measured on SCT by Reader 1 and Reader 2 was averaged and the average volume between readers acted as standard of reference value. Concordance between measurements was assessed using Lin's Concordance Correlation Coefficient (CCC). Limits of agreement (LoA) between readers and CT datasets were evaluated. Standard of reference nodule volume ranged from 13 to 366 mm 3 . The mean overestimation between readers was 3 mm 3 and 2.9 mm 3 on SCT and VSCT, respectively. Semi-automated volumetric measurements on VSCT showed substantial agreement with the standard of reference (Lin's CCC = 0.990 for Reader 1; 0.985 for Reader 2). The upper and lower LoA between readers' measurements were (16.3, -22.4 mm 3 ) and (15.5, -21.4 mm 3 ) for SCT and VSCT, respectively. VSCT datasets are feasible for the measurements of solid nodules, showing an almost perfect concordance between readers and with measurements on SCT. Copyright © 2018 Elsevier B.V. All rights reserved.

Coutts/Sweetgrass automated border crossing : phase I

DOT National Transportation Integrated Search

1999-03-01

The Coutts/Sweetgrass Automated Border Crossing Project was intended to improve operational efficiency of this rural border crossing facility using ITS applications. Phase I of the Coutts/Sweetgrass Automated Border Crossing Project was intended to r...

The logic of automated glycan assembly.

PubMed

Seeberger, Peter H

2015-05-19

Carbohydrates are the most abundant biopolymers on earth and part of every living creature. Glycans are essential as materials for nutrition and for information transfer in biological processes. To date, in few cases a detailed correlation between glycan structure and glycan function has been established. A molecular understanding of glycan function will require pure glycans for biological, immunological, and structural studies. Given the immense structural complexity of glycans found in living organisms and the lack of amplification methods or expression systems, chemical synthesis is the only means to access usable quantities of pure glycan molecules. While the solid-phase synthesis of DNA and peptides has become routine for decades, access to glycans has been technically difficult, time-consuming and confined to a few expert laboratories. In this Account, the development of a comprehensive approach to the automated synthesis of all classes of mammalian glycans, including glycosaminoglycans and glycosylphosphatidyl inositol (GPI) anchors, as well as bacterial and plant carbohydrates is described. A conceptual advance concerning the logic of glycan assembly was required in order to enable automated execution of the synthetic process. Based on the central glycosidic bond forming reaction, a general concept for the protecting groups and leaving groups has been developed. Building blocks that can be procured on large scale, are stable for prolonged periods of time, but upon activation result in high yields and selectivities were identified. A coupling-capping and deprotection cycle was invented that can be executed by an automated synthesis instrument. Straightforward postsynthetic protocols for cleavage from the solid support as well as purification of conjugation-ready oligosaccharides have been established. Introduction of methods to install selectively a wide variety of glycosidic linkages has enabled the rapid assembly of linear and branched oligo- and polysaccharides as large as 30-mers. Fast, reliable access to defined glycans that are ready for conjugation has given rise to glycan arrays, glycan probes, and synthetic glycoconjugate vaccines. While an ever increasing variety of glycans are accessible by automated synthesis, further methodological advances in carbohydrate chemistry are needed to make all possible glycans found in nature. These tools begin to fundamentally impact the medical but also materials aspects of the glycosciences.

Automated in-tube solid-phase microextraction coupled with liquid chromatography/electrospray ionization mass spectrometry for the determination of beta-blockers and metabolites in urine and serum samples.

PubMed

Kataoka, H; Narimatsu, S; Lord, H L; Pawliszyn, J

1999-10-01

The technique of automated in-tube solid-phase microextraction (SPME) coupled with liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS) was evaluated for the determination of beta-blockers in urine and serum samples. In-tube SPME is an extraction technique for organic compounds in aqueous samples, in which analytes are extracted from the sample directly into an open tubular capillary by repeated draw/eject cycles of sample solution. LC/MS analyses of beta-blockers were initially performed by liquid injection onto a LC column. Nine beta-blockers tested in this study gave very simple ESI mass spectra, and strong signals corresponding to [M + H]+ were observed for all beta-blockers. The beta-blockers were separated with a Hypersil BDS C18 column using acetonitrile/methanol/water/acetic acid (15:15:70:1) as a mobile phase. To optimize the extraction of beta-blockers, several in-tube SPME parameters were examined. The optimum extraction conditions were 15 draw/eject cycles of 30 microL of sample in 100 mM Tris-HCl (pH 8.5) at a flow rate of 100 microL/min using an Omegawax 250 capillary (Supelco, Bellefonte, PA). The beta-blockers extracted by the capillary were easily desorbed by mobile-phase flow, and carryover of beta-blockers was not observed. Using in-tube SPME/LC/ESI-MS with selected ion monitoring, the calibration curves of beta-blockers were linear in the range from 2 to 100 ng/mL with correlation coefficients above 0.9982 (n = 18) and detection limits (S/N = 3) of 0.1-1.2 ng/mL. This method was successfully applied to the analysis of biological samples without interference peaks. The recoveries of beta-blockers spiked into human urine and serum samples were above 84 and 71%, respectively. A serum sample from a patient administrated propranolol was analyzed using this method and both propranolol and its metabolites were detected.

Automated realization of the gallium melting and triple points

NASA Astrophysics Data System (ADS)

Yan, X.; Duan, Y.; Zhang, J. T.; Wang, W.

2013-09-01

In order to improve the automation and convenience of the process involved in realizing the gallium fixed points, an automated apparatus, based on thermoelectric and heat pipe technologies, was designed and developed. This paper describes the apparatus design and procedures for freezing gallium mantles and realizing gallium melting and triple points. Also, investigations on the melting behavior of a gallium melting point cell and of gallium triple point cells were carried out while controlling the temperature outside the gallium point cells at 30 °C, 30.5 °C, 31 °C, and 31.5 °C. The obtained melting plateau curves show dentate temperature oscillations on the melting plateaus for the gallium point cells when thermal couplings occurred between the outer and inner liquid-solid interfaces. The maximum amplitude of the temperature fluctuations was about 1.5 mK. Therefore, the temperature oscillations can be used to indicate the ending of the equilibrium phase transitions. The duration and amplitude of such temperature oscillations depend on the temperature difference between the setting temperature and the gallium point temperature; the smaller the temperature difference, the longer the duration of both the melting plateaus and the temperature fluctuations.

Robotic NDE inspection of advanced solid rocket motor casings

NASA Technical Reports Server (NTRS)

Mcneelege, Glenn E.; Sarantos, Chris

1994-01-01

The Advanced Solid Rocket Motor program determined the need to inspect ASRM forgings and segments for potentially catastrophic defects. To minimize costs, an automated eddy current inspection system was designed and manufactured for inspection of ASRM forgings in the initial phases of production. This system utilizes custom manipulators and motion control algorithms and integrated six channel eddy current data acquisition and analysis hardware and software. Total system integration is through a personal computer based workcell controller. Segment inspection demands the use of a gantry robot for the EMAT/ET inspection system. The EMAT/ET system utilized similar mechanical compliancy and software logic to accommodate complex part geometries. EMAT provides volumetric inspection capability while eddy current is limited to surface and near surface inspection. Each aspect of the systems are applicable to other industries, such as, inspection of pressure vessels, weld inspection, and traditional ultrasonic inspection applications.

Optimisation of the synthesis of vancomycin-selective molecularly imprinted polymer nanoparticles using automatic photoreactor

PubMed Central

2014-01-01

A novel optimized protocol for solid-state synthesis of molecularly imprinted polymer nanoparticles (nanoMIPs) with specificity for antibiotic vancomycin is described. The experimental objective was optimization of the synthesis parameters (factors) affecting the yield of obtained nanoparticles which have been synthesized using the first prototype of an automated solid-phase synthesizer. Applications of experimental design (or design of experiments) in optimization of nanoMIP yield were carried out using MODDE 9.0 software. The factors chosen in the model were the amount of functional monomers in the polymerization mixture, irradiation time, temperature during polymerization, and elution temperature. In general, it could be concluded that the irradiation time is the most important and the temperature was the least important factor which influences the yield of nanoparticles. Overall, the response surface methodology proved to be an effective tool in reducing time required for optimization of complex experimental conditions. PMID:24685151

Optimisation of the synthesis of vancomycin-selective molecularly imprinted polymer nanoparticles using automatic photoreactor.

PubMed

Muzyka, Kateryna; Karim, Khalku; Guerreiro, Antonio; Poma, Alessandro; Piletsky, Sergey

2014-03-31

A novel optimized protocol for solid-state synthesis of molecularly imprinted polymer nanoparticles (nanoMIPs) with specificity for antibiotic vancomycin is described. The experimental objective was optimization of the synthesis parameters (factors) affecting the yield of obtained nanoparticles which have been synthesized using the first prototype of an automated solid-phase synthesizer. Applications of experimental design (or design of experiments) in optimization of nanoMIP yield were carried out using MODDE 9.0 software. The factors chosen in the model were the amount of functional monomers in the polymerization mixture, irradiation time, temperature during polymerization, and elution temperature. In general, it could be concluded that the irradiation time is the most important and the temperature was the least important factor which influences the yield of nanoparticles. Overall, the response surface methodology proved to be an effective tool in reducing time required for optimization of complex experimental conditions.

Optimisation of the synthesis of vancomycin-selective molecularly imprinted polymer nanoparticles using automatic photoreactor

NASA Astrophysics Data System (ADS)

Muzyka, Kateryna; Karim, Khalku; Guerreiro, Antonio; Poma, Alessandro; Piletsky, Sergey

2014-03-01

A novel optimized protocol for solid-state synthesis of molecularly imprinted polymer nanoparticles (nanoMIPs) with specificity for antibiotic vancomycin is described. The experimental objective was optimization of the synthesis parameters (factors) affecting the yield of obtained nanoparticles which have been synthesized using the first prototype of an automated solid-phase synthesizer. Applications of experimental design (or design of experiments) in optimization of nanoMIP yield were carried out using MODDE 9.0 software. The factors chosen in the model were the amount of functional monomers in the polymerization mixture, irradiation time, temperature during polymerization, and elution temperature. In general, it could be concluded that the irradiation time is the most important and the temperature was the least important factor which influences the yield of nanoparticles. Overall, the response surface methodology proved to be an effective tool in reducing time required for optimization of complex experimental conditions.

Solid phase sequencing of biopolymers

DOEpatents

Cantor, Charles; Koster, Hubert

2010-09-28

This invention relates to methods for detecting and sequencing target nucleic acid sequences, to mass modified nucleic acid probes and arrays of probes useful in these methods, and to kits and systems which contain these probes. Useful methods involve hybridizing the nucleic acids or nucleic acids which represent complementary or homologous sequences of the target to an array of nucleic acid probes. These probes comprise a single-stranded portion, an optional double-stranded portion and a variable sequence within the single-stranded portion. The molecular weights of the hybridized nucleic acids of the set can be determined by mass spectroscopy, and the sequence of the target determined from the molecular weights of the fragments. Nucleic acids whose sequences can be determined include DNA or RNA in biological samples such as patient biopsies and environmental samples. Probes may be fixed to a solid support such as a hybridization chip to facilitate automated molecular weight analysis and identification of the target sequence.

Primary secondary amine as a sorbent material in dispersive solid-phase extraction clean-up for the determination of indicator polychlorinated biphenyls in environmental water samples by gas chromatography with electron capture detection.

PubMed

Guo, Yuanming; Hu, Hongmei; Li, Tiejun; Xue, Lijian; Zhang, Xiaoning; Zhong, Zhi; Zhang, Yurong; Jin, Yanjian

2017-08-01

A simple, rapid, and novel method has been developed and validated for determination of seven indicator polychlorinated biphenyls in water samples by gas chromatography with electron capture detection. 1 L of water samples containing 30 g of anhydrous sodium sulfate was first liquid-liquid extracted with an automated Jipad-6XB vertical oscillator using n-hexane/dichloromethane (1:1, v/v). The concentrated extract was cleaned up by dispersive solid-phase extraction with 100 mg of primary secondary amine as sorbent material. The linearity of this method ranged from 1.25 to 100 μg/L, with regression coefficients ranging between 0.9994 and 0.9999. The limits of detection were in the ng/L level, ranging between 0.2 and 0.3 ng/L. The recoveries of seven spiked polychlorinated biphenyls with external calibration method at different concentration levels in tap water, lake water, and sea water were in the ranges of 85-112, 76-116, and 72-108%, respectively, and with relative standard deviations of 3.3-4.5, 3.4-5.6, and 3.1-4.8% (n = 5), respectively. The performance of the proposed method was compared with traditional liquid-liquid extraction and solid-phase extraction clean-up methods, and comparable efficiencies were obtained. It is concluded that this method can be successfully applied for the determination of polychlorinated biphenyls in different water samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Bibliographic Automation of Large Library Operations Using a Time-Sharing System: Phase I. Final Report.

ERIC Educational Resources Information Center

Epstein, A. H.; And Others

The first phase of an ongoing library automation project at Stanford University is described. Project BALLOTS (Bibliographic Automation of Large Library Operations Using a Time-Sharing System) seeks to automate the acquisition and cataloging functions of a large library using an on-line time-sharing computer. The main objectives are to control…

Automated protein hydrolysis delivering sample to a solid acid catalyst for amino acid analysis.

PubMed

Masuda, Akiko; Dohmae, Naoshi

2010-11-01

In this study, we developed an automatic protein hydrolysis system using strong cation-exchange resins as solid acid catalysts. Examining several kinds of inorganic solid acids and cation-exchange resins, we found that a few cation-exchange resins worked as acid catalysts for protein hydrolysis when heated in the presence of water. The most efficient resin yielded amounts of amino acids that were over 70% of those recovered after conventional hydrolysis with hydrochloric acid and resulted in amino acid compositions matching the theoretical values. The solid-acid hydrolysis was automated by packing the resin into columns, combining the columns with a high-performance liquid chromatography system, and heating them. The amino acids that constitute a protein can thereby be determined, minimizing contamination from the environment.

Multiresidue analysis of 24 Water Framework Directive priority substances by on-line solid phase extraction-liquid chromatography tandem mass spectrometry in environmental waters.

PubMed

Rubirola, Adrià; Boleda, Mª Rosa; Galceran, Mª Teresa

2017-04-14

This paper reports the development of a fully multiresidue and automated on-line solid phase extraction (SPE) - liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the determination of 24 priority substances (PS) belonging to different classes (pesticides, hormones or pharmaceuticals) included in the Directive 2013/39/UE and the recent Watch List (Decision 2015/495) in water samples (drinking water, surface water, and effluent wastewaters). LC-MS/MS conditions and on-line SPE parameters such as sorbent type, sample and wash volumes were optimized. The developed method is highly sensitive (limits of detection between 0.1 and 1.4ngL -1 ) and precise (relative standard deviations lower than 8%). As part of the method validation studies, linearity, accuracy and matrix effects were assessed. The main advantage of this method over traditional off-line procedures is the minimization of tedious sample preparation increasing productivity and sample throughput. The optimized method was applied to the analysis of water samples and the results revealed the presence of 16 PS in river water and effluent water of wastewater treatment plants. Copyright © 2017 Elsevier B.V. All rights reserved.

An organically modified silica aerogel for online in-tube solid-phase microextraction.

PubMed

Bu, Yanan; Feng, Juanjuan; Tian, Yu; Wang, Xiuqin; Sun, Min; Luo, Chuannan

2017-09-29

Aerogels have received considerable attentions because of its porous, high specific surface, unique properties and environmental friendliness. In this work, an organically modified silica aerogel was functionalized on the basalt fibers (BFs) and filled into a poly(ether ether ketone) (PEEK) tube, which was coupled with high performance liquid chromatography (HPLC) for in-tube solid-phase microextraction (IT-SPME). The aerogel was characterized by scanning electron microscopy (SEM) and fourier transform infrared spectrometry (FT-IR). The extraction efficiency of the tube was systematically investigated and shown enrichment factors from 2346 to 3132. An automated, sensitive and selective method was developed for the determination of five estrogens. The linear range was from 0.03 to 100μgL -1 with correlation coefficients (r) higher than 0.9989, and low detection limits (LODs) were 0.01-0.05μgL -1 . The relative standard deviations (RSDs) for intra-day and inter-day were less than 4.5% and 6.7% (n=6), respectively. Finally, the analysis method was successfully applied to detect estrogens in sewage and emollient water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

[Corrected Title: Solid-Phase Extraction of Polar Compounds from Water] Automated Electrostatics Environmental Chamber

NASA Technical Reports Server (NTRS)

Sauer, Richard; Rutz, Jeffrey; Schultz, John

2005-01-01

A solid-phase extraction (SPE) process has been developed for removing alcohols, carboxylic acids, aldehydes, ketones, amines, and other polar organic compounds from water. This process can be either a subprocess of a water-reclamation process or a means of extracting organic compounds from water samples for gas-chromatographic analysis. This SPE process is an attractive alternative to an Environmental Protection Administration liquid-liquid extraction process that generates some pollution and does not work in a microgravitational environment. In this SPE process, one forces a water sample through a resin bed by use of positive pressure on the upstream side and/or suction on the downstream side, thereby causing organic compounds from the water to be adsorbed onto the resin. If gas-chromatographic analysis is to be done, the resin is dried by use of a suitable gas, then the adsorbed compounds are extracted from the resin by use of a solvent. Unlike the liquid-liquid process, the SPE process works in both microgravity and Earth gravity. In comparison with the liquid-liquid process, the SPE process is more efficient, extracts a wider range of organic compounds, generates less pollution, and costs less.

NAA-modified DNA oligonucleotides with zwitterionic backbones: stereoselective synthesis of A-T phosphoramidite building blocks.

PubMed

Schmidtgall, Boris; Höbartner, Claudia; Ducho, Christian

2015-01-01

Modifications of the nucleic acid backbone are essential for the development of oligonucleotide-derived bioactive agents. The NAA-modification represents a novel artificial internucleotide linkage which enables the site-specific introduction of positive charges into the otherwise polyanionic backbone of DNA oligonucleotides. Following initial studies with the introduction of the NAA-linkage at T-T sites, it is now envisioned to prepare NAA-modified oligonucleotides bearing the modification at X-T motifs (X = A, C, G). We have therefore developed the efficient and stereoselective synthesis of NAA-linked 'dimeric' A-T phosphoramidite building blocks for automated DNA synthesis. Both the (S)- and the (R)-configured NAA-motifs were constructed with high diastereoselectivities to furnish two different phosphoramidite reagents, which were employed for the solid phase-supported automated synthesis of two NAA-modified DNA oligonucleotides. This represents a significant step to further establish the NAA-linkage as a useful addition to the existing 'toolbox' of backbone modifications for the design of bioactive oligonucleotide analogues.

Applications of immobilized catalysts in continuous flow processes.

PubMed

Kirschning, Andreas; Jas, Gerhard

2004-01-01

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

Solid-phase synthesis of protein-polymers on reversible immobilization supports.

PubMed

Murata, Hironobu; Carmali, Sheiliza; Baker, Stefanie L; Matyjaszewski, Krzysztof; Russell, Alan J

2018-02-27

Facile automated biomacromolecule synthesis is at the heart of blending synthetic and biologic worlds. Full access to abiotic/biotic synthetic diversity first occurred when chemistry was developed to grow nucleic acids and peptides from reversibly immobilized precursors. Protein-polymer conjugates, however, have always been synthesized in solution in multi-step, multi-day processes that couple innovative chemistry with challenging purification. Here we report the generation of protein-polymer hybrids synthesized by protein-ATRP on reversible immobilization supports (PARIS). We utilized modified agarose beads to covalently and reversibly couple to proteins in amino-specific reactions. We then modified reversibly immobilized proteins with protein-reactive ATRP initiators and, after ATRP, we released and analyzed the protein polymers. The activity and stability of PARIS-synthesized and solution-synthesized conjugates demonstrated that PARIS was an effective, rapid, and simple method to generate protein-polymer conjugates. Automation of PARIS significantly reduced synthesis/purification timelines, thereby opening a path to changing how to generate protein-polymer conjugates.

Automated glycan assembly of xyloglucan oligosaccharides.

PubMed

Dallabernardina, Pietro; Schuhmacher, Frank; Seeberger, Peter H; Pfrengle, Fabian

2016-01-07

We report the automated glycan assembly of oligosaccharide fragments related to the hemicellulose xyloglucan (XG). Iterative addition of monosaccharide and disaccharide building blocks to a solid support provided seven cellulose and xyloglucan fragments including XXGG- and XXXG-type oligosaccharides.

Planning for Office Automation.

ERIC Educational Resources Information Center

Mick, Colin K.

1983-01-01

Outlines a practical approach to planning for office automation termed the "Focused Process Approach" (the "what" phase, "how" phase, "doing" phase) which is a synthesis of the problem-solving and participatory planning approaches. Thirteen references are provided. (EJS)

Quantum simulation of a Fermi-Hubbard model using a semiconductor quantum dot array.

PubMed

Hensgens, T; Fujita, T; Janssen, L; Li, Xiao; Van Diepen, C J; Reichl, C; Wegscheider, W; Das Sarma, S; Vandersypen, L M K

2017-08-02

Interacting fermions on a lattice can develop strong quantum correlations, which are the cause of the classical intractability of many exotic phases of matter. Current efforts are directed towards the control of artificial quantum systems that can be made to emulate the underlying Fermi-Hubbard models. Electrostatically confined conduction-band electrons define interacting quantum coherent spin and charge degrees of freedom that allow all-electrical initialization of low-entropy states and readily adhere to the Fermi-Hubbard Hamiltonian. Until now, however, the substantial electrostatic disorder of the solid state has meant that only a few attempts at emulating Fermi-Hubbard physics on solid-state platforms have been made. Here we show that for gate-defined quantum dots this disorder can be suppressed in a controlled manner. Using a semi-automated and scalable set of experimental tools, we homogeneously and independently set up the electron filling and nearest-neighbour tunnel coupling in a semiconductor quantum dot array so as to simulate a Fermi-Hubbard system. With this set-up, we realize a detailed characterization of the collective Coulomb blockade transition, which is the finite-size analogue of the interaction-driven Mott metal-to-insulator transition. As automation and device fabrication of semiconductor quantum dots continue to improve, the ideas presented here will enable the investigation of the physics of ever more complex many-body states using quantum dots.

Monolithic methacrylate packed 96-tips for high throughput bioanalysis.

PubMed

Altun, Zeki; Skoglund, Christina; Abdel-Rehim, Mohamed

2010-04-16

In the pharmaceutical industry the growing number of samples to be analyzed requires high throughput and fully automated analytical techniques. Commonly used sample-preparation methods are solid-phase extraction (SPE), liquid-liquid extraction (LLE) and protein precipitation. In this paper we will discus a new sample-preparation technique based on SPE for high throughput drug extraction developed and used by our group. This new sample-preparation method is based on monolithic methacrylate polymer as packing sorbent for 96-tip robotic device. Using this device a 96-well plate could be handled in 2-4min. The key aspect of the monolithic phase is that monolithic material can offer both good binding capacity and low back-pressure properties compared to e.g. silica phases. The present paper presents the successful application of monolithic 96-tips and LC-MS/MS by the sample preparation of busulphan, rescovitine, metoprolol, pindolol and local anaesthetics from human plasma samples and cyklophosphamid from mice blood samples. Copyright 2009 Elsevier B.V. All rights reserved.

Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group; determination of glyphosate, aminomethylphosphonic acid, and glufonsinate in water using online solid-phase extraction and high-performance liquid chromat

USGS Publications Warehouse

Lee, E.A.; Strahan, A.P.; Thurman, E.M.

2001-01-01

An analytical method for the determination of glyphosate, its principal degradation compound, aminomethylphosphonic acid (AMPA), and glufosinate in water with varying matrices has been developed. Four different sample matrices fortified at 0.2 and 2.0 ?g/L (micrograms per liter) were analyzed using precolumn derivatization with 9-fluorenylmethylchloroformate (FMOC). After derivatization, cleanup and concentration were accomplished using automated online solid-phase extraction followed by elution with the mobile phase allowing for direct injection into a liquid chromatograph/mass spectrometer (LC/MS). Analytical conditions for MS detection were optimized, and quantitation was carried out using the following representative ions: 390 and 168 for glyphosate; 332, 110, and 136 for AMPA; and 402, 180, and 206 for glufosinate. Matrix effects were minimized by utilizing standard addition for quantification and an isotope-labeled glyphosate (2-13C,15N) as the internal standard. Method detection limits (MDLs) were 0.084 ?g/L for glyphosate, 0.078 ?g/L for AMPA, and 0.057 ?g/L for glufosinate. The method reporting limits (MRLs) were set at 0.1 ?g/L for all three compounds. The mean recovery values ranged from 88.0 to 128.7 percent, and relative standard deviation values ranged from 5.6 to 32.6 percent.

Integrated electrokinetically driven microfluidic devices with pH-mediated solid-phase extraction coupled to microchip electrophoresis for preterm birth biomarkers.

PubMed

Sonker, Mukul; Knob, Radim; Sahore, Vishal; Woolley, Adam T

2017-07-01

Integration in microfluidics is important for achieving automation. Sample preconcentration integrated with separation in a microfluidic setup can have a substantial impact on rapid analysis of low-abundance disease biomarkers. Here, we have developed a microfluidic device that uses pH-mediated solid-phase extraction (SPE) for the enrichment and elution of preterm birth (PTB) biomarkers. Furthermore, this SPE module was integrated with microchip electrophoresis for combined enrichment and separation of multiple analytes, including a PTB peptide biomarker (P1). A reversed-phase octyl methacrylate monolith was polymerized as the SPE medium in polyethylene glycol diacrylate modified cyclic olefin copolymer microfluidic channels. Eluent for pH-mediated SPE of PTB biomarkers on the monolith was optimized using different pH values and ionic concentrations. Nearly 50-fold enrichment was observed in single channel SPE devices for a low nanomolar solution of P1, with great elution time reproducibility (<7% RSD). The monolith binding capacity was determined to be 400 pg (0.2 pmol). A mixture of a model peptide (FA) and a PTB biomarker (P1) was extracted, eluted, injected, and then separated by microchip electrophoresis in our integrated device with ∼15-fold enrichment. This device shows important progress towards an integrated electrokinetically operated platform for preconcentration and separation of biomarkers. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

RNA isolation from mammalian cells using porous polymer monoliths: an approach for high-throughput automation.

PubMed

Chatterjee, Anirban; Mirer, Paul L; Zaldivar Santamaria, Elvira; Klapperich, Catherine; Sharon, Andre; Sauer-Budge, Alexis F

2010-06-01

The life science and healthcare communities have been redefining the importance of ribonucleic acid (RNA) through the study of small molecule RNA (in RNAi/siRNA technologies), micro RNA (in cancer research and stem cell research), and mRNA (gene expression analysis for biologic drug targets). Research in this field increasingly requires efficient and high-throughput isolation techniques for RNA. Currently, several commercial kits are available for isolating RNA from cells. Although the quality and quantity of RNA yielded from these kits is sufficiently good for many purposes, limitations exist in terms of extraction efficiency from small cell populations and the ability to automate the extraction process. Traditionally, automating a process decreases the cost and personnel time while simultaneously increasing the throughput and reproducibility. As the RNA field matures, new methods for automating its extraction, especially from low cell numbers and in high throughput, are needed to achieve these improvements. The technology presented in this article is a step toward this goal. The method is based on a solid-phase extraction technology using a porous polymer monolith (PPM). A novel cell lysis approach and a larger binding surface throughout the PPM extraction column ensure a high yield from small starting samples, increasing sensitivity and reducing indirect costs in cell culture and sample storage. The method ensures a fast and simple procedure for RNA isolation from eukaryotic cells, with a high yield both in terms of quality and quantity. The technique is amenable to automation and streamlined workflow integration, with possible miniaturization of the sample handling process making it suitable for high-throughput applications.

Automated Fmoc-based solid-phase synthesis of peptide thioesters with self-purification effect and application in the construction of immobilized SH3 domains.

PubMed

Mende, Franziska; Beisswenger, Michael; Seitz, Oliver

2010-08-18

Peptide thioesters are important building blocks in the total synthesis of proteins and protein domains via fragment ligation. However, synthetic access of peptide thioesters still is a bottleneck of this powerful ligation chemistry. The commonly used methods for the Fmoc-based synthesis of peptide thioesters involve nonautomated solution steps that have to be performed after the solid-phase assembly of the peptide. Usually, HPLC purification is required. Herein, a method that enables crude peptides to be used in divergent native chemical ligations reactions is described. We present an Fmoc-based solid-phase synthesis of peptide thioesters with self-purification which facilitates access to these important building blocks, since the often cumbersome HPLC purification can be avoided. Fmoc-protected amino acids are coupled on a safety catch sulfonamide resin. The self-purifying effect is achieved through the combination of (a) N-terminal coupling of a cleavable cyclization linker and subsequent backbone-to-side chain cyclization, (b) activation of the sulfonamide linkage by alkylation, (c) thiolysis for the selective detachment of truncation products, and (d) TFA cleavage for the liberation of the desired peptide thioester in unprotected form. We have previously shown a method wherein cyclization was performed after carboxymethylation of the sulfonamide. However, the automation of this method was difficult and side reactions at methionine residues hampered the general applicability. The new design involves peptide synthesis on a modified carboxy-functionalized sulfonamide linker, a substantially milder activation of the sulfonamide bond and the use of monomethoxytrityl as well as 2-phenyl-isopropyl protecting groups. This approach solved the problems with methionine containing peptides and enabled the complete automation of the self-purifying synthesis of peptide thioesters. The study also addressed problems in the synthesis of difficult peptides. Aggregated truncation products can resist extraction and contaminate full-length thioesters obtained after TFA cleavage. It is shown that significant enhancements of the purity were achieved when mild acidic extractions were included in the wash protocols after thiolysis. The potential of the method was demonstrated in the parallel synthesis of 20-40 amino acid long peptide thioesters, which were obtained in excellent purities. The thioesters and cysteinyl peptides were used without purification in the assembly of immobilized SH3 protein domains of SHO1 in yeast. A cysteine scan by native chemical ligation suggested single amino acid to cysteine substitutions that (a) confer useful ligation yields, (b) support correct folding, and (c) sustain the function of the folded protein domain. The chemical synthesis of the SH3-domain of SHO1 succeeded in highest yields when cysteine placements at positions S23, F24, and E36 were avoided. The synthetic SH3 mutants were examined in a binding assay, which indicated that N27C, L30C, and D34C mutations provide functional SH3-domain.

Automated biowaste sampling system, solids subsystem operating model, part 2

NASA Technical Reports Server (NTRS)

Fogal, G. L.; Mangialardi, J. K.; Stauffer, R. E.

1973-01-01

The detail design and fabrication of the Solids Subsystem were implemented. The system's capacity for the collection, storage or sampling of feces and vomitus from six subjects was tested and verified.

Magnetic solid-phase extraction using carbon nanotubes as sorbents: a review.

PubMed

Herrero-Latorre, C; Barciela-García, J; García-Martín, S; Peña-Crecente, R M; Otárola-Jiménez, J

2015-09-10

Magnetic solid-phase extraction (M-SPE) is a procedure based on the use of magnetic sorbents for the separation and preconcentration of different organic and inorganic analytes from large sample volumes. The magnetic sorbent is added to the sample solution and the target analyte is adsorbed onto the surface of the magnetic sorbent particles (M-SPs). Analyte-M-SPs are separated from the sample solution by applying an external magnetic field and, after elution with the appropriate solvent, the recovered analyte is analyzed. This approach has several advantages over traditional solid phase extraction as it avoids time-consuming and tedious on-column SPE procedures and it provides a rapid and simple analyte separation that avoids the need for centrifugation or filtration steps. As a consequence, in the past few years a great deal of research has been focused on M-SPE, including the development of new sorbents and novel automation strategies. In recent years, the use of magnetic carbon nanotubes (M-CNTs) as a sorption substrate in M-SPE has become an active area of research. These materials have exceptional mechanical, electrical, optical and magnetic properties and they also have an extremely large surface area and varied possibilities for functionalization. This review covers the synthesis of M-CNTs and the different approaches for the use of these compounds in M-SPE. The performance, general characteristics and applications of M-SPE based on magnetic carbon nanotubes for organic and inorganic analysis have been evaluated on the basis of more than 110 references. Finally, some important challenges with respect the use of magnetic carbon nanotubes in M-SPE are discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

Combinatorial chemistry on solid support in the search for central nervous system agents.

PubMed

Zajdel, Paweł; Pawłowski, Maciej; Martinez, Jean; Subra, Gilles

2009-08-01

The advent of combinatorial chemistry was one of the most important developments, that has significantly contributed to the drug discovery process. Within just a few years, its initial concept aimed at production of libraries containing huge number of compounds (thousands to millions), so called screening libraries, has shifted towards preparation of small and medium-sized rationally designed libraries. When applicable, the use of solid supports for the generation of libraries has been a real breakthrough in enhancing productivity. With a limited amount of resin and simple manual workups, the split/mix procedure may generate thousands of bead-tethered compounds. Beads can be chemically or physically encoded to facilitate the identification of a hit after the biological assay. Compartmentalization of solid supports using small reactors like teabags, kans or pellicular discrete supports like Lanterns resulted in powerful sort and combine technologies, relying on codes 'written' on the reactor, and thus reducing the need for automation and improving the number of compounds synthesized. These methods of solid-phase combinatorial chemistry have been recently supported by introduction of solid-supported reagents and scavenger resins. The first part of this review discusses the general premises of combinatorial chemistry and some methods used in the design of primary and focused combinatorial libraries. The aim of the second part is to present combinatorial chemistry methodologies aimed at discovering bioactive compounds acting on diverse GPCR involved in central nervous system disorders.

Automated Control of the Organic and Inorganic Composition of Aloe vera Extracts Using (1)H NMR Spectroscopy.

PubMed

Monakhova, Yulia B; Randel, Gabriele; Diehl, Bernd W K

2016-09-01

Recent classification of Aloe vera whole-leaf extract by the International Agency for Research and Cancer as a possible carcinogen to humans as well as the continuous adulteration of A. vera's authentic material have generated renewed interest in controlling A. vera. The existing NMR spectroscopic method for the analysis of A. vera, which is based on a routine developed at Spectral Service, was extended. Apart from aloverose, glucose, malic acid, lactic acid, citric acid, whole-leaf material (WLM), acetic acid, fumaric acid, sodium benzoate, and potassium sorbate, the quantification of Mg(2+), Ca(2+), and fructose is possible with the addition of a Cs-EDTA solution to sample. The proposed methodology was automated, which includes phasing, baseline-correction, deconvolution (based on the Lorentzian function), integration, quantification, and reporting. The NMR method was applied to 41 A. vera preparations in the form of liquid A. vera juice and solid A. vera powder. The advantages of the new NMR methodology over the previous method were discussed. Correlation between the new and standard NMR methodologies was significant for aloverose, glucose, malic acid, lactic acid, citric acid, and WLM (P < 0.0001, R(2) = 0.99). NMR was found to be suitable for the automated simultaneous quantitative determination of 13 parameters in A. vera.

Non-Contact Conductivity Measurement for Automated Sample Processing Systems

NASA Technical Reports Server (NTRS)

Beegle, Luther W.; Kirby, James P.

2012-01-01

A new method has been developed for monitoring and control of automated sample processing and preparation especially focusing on desalting of samples before analytical analysis (described in more detail in Automated Desalting Apparatus, (NPO-45428), NASA Tech Briefs, Vol. 34, No. 8 (August 2010), page 44). The use of non-contact conductivity probes, one at the inlet and one at the outlet of the solid phase sample preparation media, allows monitoring of the process, and acts as a trigger for the start of the next step in the sequence (see figure). At each step of the muti-step process, the system is flushed with low-conductivity water, which sets the system back to an overall low-conductivity state. This measurement then triggers the next stage of sample processing protocols, and greatly minimizes use of consumables. In the case of amino acid sample preparation for desalting, the conductivity measurement will define three key conditions for the sample preparation process. First, when the system is neutralized (low conductivity, by washing with excess de-ionized water); second, when the system is acidified, by washing with a strong acid (high conductivity); and third, when the system is at a basic condition of high pH (high conductivity). Taken together, this non-contact conductivity measurement for monitoring sample preparation will not only facilitate automation of the sample preparation and processing, but will also act as a way to optimize the operational time and use of consumables

Physical and digital simulations for IVA robotics

NASA Technical Reports Server (NTRS)

Hinman, Elaine; Workman, Gary L.

1992-01-01

Space based materials processing experiments can be enhanced through the use of IVA robotic systems. A program to determine requirements for the implementation of robotic systems in a microgravity environment and to develop some preliminary concepts for acceleration control of small, lightweight arms has been initiated with the development of physical and digital simulation capabilities. The physical simulation facilities incorporate a robotic workcell containing a Zymark Zymate II robot instrumented for acceleration measurements, which is able to perform materials transfer functions while flying on NASA's KC-135 aircraft during parabolic manuevers to simulate reduced gravity. Measurements of accelerations occurring during the reduced gravity periods will be used to characterize impacts of robotic accelerations in a microgravity environment in space. Digital simulations are being performed with TREETOPS, a NASA developed software package which is used for the dynamic analysis of systems with a tree topology. Extensive use of both simulation tools will enable the design of robotic systems with enhanced acceleration control for use in the space manufacturing environment.

Automated measurement of vocal fold vibratory asymmetry from high-speed videoendoscopy recordings.

PubMed

Mehta, Daryush D; Deliyski, Dimitar D; Quatieri, Thomas F; Hillman, Robert E

2011-02-01

In prior work, a manually derived measure of vocal fold vibratory phase asymmetry correlated to varying degrees with visual judgments made from laryngeal high-speed videoendoscopy (HSV) recordings. This investigation extended this work by establishing an automated HSV-based framework to quantify 3 categories of vocal fold vibratory asymmetry. HSV-based analysis provided for cycle-to-cycle estimates of left-right phase asymmetry, left-right amplitude asymmetry, and axis shift during glottal closure for 52 speakers with no vocal pathology producing comfortable and pressed phonation. An initial cross-validation of the automated left-right phase asymmetry measure was performed by correlating the measure with other objective and subjective assessments of phase asymmetry. Vocal fold vibratory asymmetry was exhibited to a similar extent in both comfortable and pressed phonations. The automated measure of left-right phase asymmetry strongly correlated with manually derived measures and moderately correlated with visual-perceptual ratings. Correlations with the visual-perceptual ratings remained relatively consistent as the automated measure was derived from kymograms taken at different glottal locations. An automated HSV-based framework for the quantification of vocal fold vibratory asymmetry was developed and initially validated. This framework serves as a platform for investigating relationships between vocal fold tissue motion and acoustic measures of voice function.

A solid-phase microextraction GC/MS/MS method for rapid quantitative analysis of food and beverages for the presence of legally restricted biologically active flavorings.

PubMed

Bousova, Katerina; Mittendorf, Klaus; Senyuva, Hamide

2011-01-01

A method was developed using automated headspace solid-phase microextraction coupled with GC/MS/MS to simultaneously determine the presence of seven biologically active flavoring substances whose levels of use in processed foods is controlled by statutory limits. The method can be applied to identify and quantify the presence of 1,2-benzopyrone (coumarin), beta-asarone, 1-allyl-4-methoxybenzene (estragole), menthofuran, 4-allyl-1 ,2-dimethoxybenzene (methyl eugenol), pulegone, and thujone at levels ranging from 0.5 to 3000 mg/kg. The method has been optimized and validated for three different generic food types categorized on the basis of composition and anticipated use levels of flavorings and food ingredients. The food categories are alcoholic and nonalcoholic beverages; semisolid processed foods (e.g., soups, sauces, confectionary, etc.); and solid foods (muesli, bakery products, etc.). The method is simple, inexpensive, and rapid, and eliminates the use of flammable and toxic solvents. There is no sample preparation, and using MSIMS, unequivocal confirmation of identification is achieved even in highly complex matrixes containing many potential interfering volatiles. The method precision for spiked samples ranged from 2 to 21%, with the greatest variability associated with solid matrixes. The LOD and LOQ values were well below 0.1 and 0.5 mg/kg, respectively, in all cases for individual substances, fulfilling requirements for enforcement purposes. The robustness of the method was demonstrated in a small survey of retail samples of four spirits, five flavored milks, three energy drinks, five liqueurs, five soups, 10 sauces, five herbal teas, and three breakfast cereals.

Automated, Ultra-Sterile Solid Sample Handling and Analysis on a Chip

NASA Technical Reports Server (NTRS)

Mora, Maria F.; Stockton, Amanda M.; Willis, Peter A.

2013-01-01

There are no existing ultra-sterile lab-on-a-chip systems that can accept solid samples and perform complete chemical analyses without human intervention. The proposed solution is to demonstrate completely automated lab-on-a-chip manipulation of powdered solid samples, followed by on-chip liquid extraction and chemical analysis. This technology utilizes a newly invented glass micro-device for solid manipulation, which mates with existing lab-on-a-chip instrumentation. Devices are fabricated in a Class 10 cleanroom at the JPL MicroDevices Lab, and are plasma-cleaned before and after assembly. Solid samples enter the device through a drilled hole in the top. Existing micro-pumping technology is used to transfer milligrams of powdered sample into an extraction chamber where it is mixed with liquids to extract organic material. Subsequent chemical analysis is performed using portable microchip capillary electrophoresis systems (CE). These instruments have been used for ultra-highly sensitive (parts-per-trillion, pptr) analysis of organic compounds including amines, amino acids, aldehydes, ketones, carboxylic acids, and thiols. Fully autonomous amino acid analyses in liquids were demonstrated; however, to date there have been no reports of completely automated analysis of solid samples on chip. This approach utilizes an existing portable instrument that houses optics, high-voltage power supplies, and solenoids for fully autonomous microfluidic sample processing and CE analysis with laser-induced fluorescence (LIF) detection. Furthermore, the entire system can be sterilized and placed in a cleanroom environment for analyzing samples returned from extraterrestrial targets, if desired. This is an entirely new capability never demonstrated before. The ability to manipulate solid samples, coupled with lab-on-a-chip analysis technology, will enable ultraclean and ultrasensitive end-to-end analysis of samples that is orders of magnitude more sensitive than the ppb goal given in the Science Instruments.

USSR Report, Cybernetics, Computers and Automation Technology.

DTIC Science & Technology

1987-03-02

Studies in the Area of EPR of Non- Ordered Solids, Spectral Recording, Processing and Analysis System (A.N. Bals, L.M. Kuzmina ; AVTOMETRIYA, No 2, Feb...L.M. Kuzmina , Riga] [Abstract] An automated system has been developed for electron paramagnetic resonance studies, oriented toward achievement of

Oligonucleotide labeling methods. 3. Direct labeling of oligonucleotides employing a novel, non-nucleosidic, 2-aminobutyl-1,3-propanediol backbone.

PubMed Central

Nelson, P S; Kent, M; Muthini, S

1992-01-01

Novel CE-phosphoramidite (7a-e) and CPG (8a, c, d, e) reagents have been prepared from a unique 2-aminobutyl-1,3-propanediol backbone. The reagents have been used to directly label oligonucleotides with fluorescein, acridine, and biotin via automated DNA synthesis. The versatile 2-aminobutyl-1,3-propanediol backbone allows for labeling at any position (5', internal, and 3') during solid phase oligonucleotide synthesis. Multiple labels can be achieved by repetitive coupling cycles. Furthermore, the 3-carbon atom internucleotide phosphate distance is retained when inserted internally. Using this method, individual oligonucleotides possessing two and three different reporter molecules have been prepared. PMID:1475185

Synthesis and Primary Characterization of Self-Assembled Peptide-Based Hydrogels

PubMed Central

Nagarkar, Radhika P.; Schneider, Joel P.

2009-01-01

Summary Hydrogels based on peptide self-assembly form an important class of biomaterials that find application in tissue engineering and drug delivery. It is essential to prepare peptides with high purity to achieve batch-to-batch consistency affording hydrogels with reproducible properties. Automated solid-phase peptide synthesis coupled with optimized Fmoc (9-fluorenylmethoxycarbonyl) chemistry to obtain peptides in high yield and purity is discussed. Details of isolating a desired peptide from crude synthetic mixtures and assessment of the peptide’s final purity by high-performance liquid chromatography and mass spectrometry are provided. Beyond the practical importance of synthesis and primary characterization, techniques used to investigate the properties of hydrogels are briefly discussed. PMID:19031061

Determination of 74 new psychoactive substances in serum using automated in-line solid-phase extraction-liquid chromatography-tandem mass spectrometry.

PubMed

Lehmann, Sabrina; Kieliba, Tobias; Beike, Justus; Thevis, Mario; Mercer-Chalmers-Bender, Katja

2017-10-01

A detailed description is given of the development and validation of a fully automated in-line solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) method capable of detecting 90 central-stimulating new psychoactive substances (NPS) and 5 conventional amphetamine-type stimulants (amphetamine, 3,4-methylenedioxy-methamphetamine (MDMA), 3,4-methylenedioxy-amphetamine (MDA), 3,4-methylenedioxy-N-ethyl-amphetamine (MDEA), methamphetamine) in serum. The aim was to apply the validated method to forensic samples. The preparation of 150μL of serum was performed by an Instrument Top Sample Preparation (ITSP)-SPE with mixed mode cation exchanger cartridges. The extracts were directly injected into an LC-MS/MS system, using a biphenyl column and gradient elution with 2mM ammonium formate/0.1% formic acid and acetonitrile/0.1% formic acid as mobile phases. The chromatographic run time amounts to 9.3min (including re-equilibration). The total cycle time is 11min, due to the interlacing between sample preparation and analysis. The method was fully validated using 69 NPS and five conventional amphetamine-type stimulants, according to the guidelines of the Society of Toxicological and Forensic Chemistry (GTFCh). The guidelines were fully achieved for 62 analytes (with a limit of detection (LOD) between 0.2 and 4μg/L), whilst full validation was not feasible for the remaining 12 analytes. For the fully validated analytes, the method achieved linearity in the 5μg/L (lower limit of quantification, LLOQ) to 250μg/L range (coefficients of determination>0.99). Recoveries for 69 of these compounds were greater than 50%, with relative standard deviations≤15%. The validated method was then tested for its capability in detecting a further 21 NPS, thus totalling 95 tested substances. An LOD between 0.4 and 1.6μg/L was obtained for these 21 additional qualitatively-measured substances. The method was subsequently successfully applied to 28 specimens from routine forensic case work, of which 7 samples were determined to be positive for NPS consumption. Copyright © 2017 Elsevier B.V. All rights reserved.

Rapid and automated analysis of aflatoxin M1 in milk and dairy products by online solid phase extraction coupled to ultra-high-pressure-liquid-chromatography tandem mass spectrometry.

PubMed

Campone, Luca; Piccinelli, Anna Lisa; Celano, Rita; Pagano, Imma; Russo, Mariateresa; Rastrelli, Luca

2016-01-08

This study reports a fast and automated analytical procedure for the analysis of aflatoxin M1 (AFM1) in milk and dairy products. The method is based on the simultaneous protein precipitation and AFM1 extraction, by salt-induced liquid-liquid extraction (SI-LLE), followed by an online solid-phase extraction (online SPE) coupled to ultra-high-pressure-liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis to the automatic pre-concentration, clean up and sensitive and selective determination of AFM1. The main parameters affecting the extraction efficiency and accuracy of the analytical method were studied in detail. In the optimal conditions, acetonitrile and NaCl were used as extraction/denaturant solvent and salting-out agent in SI-LLE, respectively. After centrifugation, the organic phase (acetonitrile) was diluted with water (1:9 v/v) and purified (1mL) by online C18 cartridge coupled with an UHPLC column. Finally, selected reaction monitoring (SRM) acquisition mode was applied to the detection of AFM1. Validation studies were carried out on different dairy products (whole and skimmed cow milk, yogurt, goat milk, and powder infant formula), providing method quantification limits about 25 times lower than AFM1 maximum levels permitted by EU regulation 1881/2006 in milk and dairy products for direct human consumption. Recoveries (86-102%) and repeatability (RSD<3, n=6) meet the performance criteria required by EU regulation N. 401/2006 for the determination of the levels of mycotoxins in foodstuffs. Moreover, no matrix effects were observed in the different milk and dairy products studied. The proposed method improves the performance of AFM1 analysis in milk samples as AFM1 determination is performed with a degree of accuracy higher than the conventional methods. Other advantages are the reduction of sample preparation procedure, time and cost of the analysis, enabling high sample throughput that meet the current concerns of food safety and the public health protection. Copyright © 2015 Elsevier B.V. All rights reserved.

Automation of (64)Cu production at Turku PET Centre.

PubMed

Elomaa, Viki-Veikko; Jurttila, Jori; Rajander, Johan; Solin, Olof

2014-07-01

At Turku PET Centre automation for handling solid targets for the production of (64)Cu has been built. The system consists of a module for moving the target from the irradiation position into a lead transport shield and a robotic-arm assisted setup for moving the target within radiochemistry laboratory. The main motivation for designing automation arises from radiation hygiene. Copyright © 2014 Elsevier Ltd. All rights reserved.

Nucleic Acid Detection Methods

DOEpatents

Smith, Cassandra L.; Yaar, Ron; Szafranski, Przemyslaw; Cantor, Charles R.

1998-05-19

The invention relates to methods for rapidly determining the sequence and/or length a target sequence. The target sequence may be a series of known or unknown repeat sequences which are hybridized to an array of probes. The hybridized array is digested with a single-strand nuclease and free 3'-hydroxyl groups extended with a nucleic acid polymerase. Nuclease cleaved heteroduplexes can be easily distinguish from nuclease uncleaved heteroduplexes by differential labeling. Probes and target can be differentially labeled with detectable labels. Matched target can be detected by cleaving resulting loops from the hybridized target and creating free 3-hydroxyl groups. These groups are recognized and extended by polymerases added into the reaction system which also adds or releases one label into solution. Analysis of the resulting products using either solid phase or solution. These methods can be used to detect characteristic nucleic acid sequences, to determine target sequence and to screen for genetic defects and disorders. Assays can be conducted on solid surfaces allowing for multiple reactions to be conducted in parallel and, if desired, automated.

Recent Advances in On-Line Methods Based on Extraction for Speciation Analysis of Chromium in Environmental Matrices.

PubMed

Trzonkowska, Laura; Leśniewska, Barbara; Godlewska-Żyłkiewicz, Beata

2016-07-03

The biological activity of Cr(III) and Cr(VI) species, their chemical behavior, and toxic effects are dissimilar. The speciation analysis of Cr(III) and Cr(VI) in environmental matrices is then of great importance and much research has been devoted to this area. This review presents recent developments in on-line speciation analysis of chromium in such samples. Flow systems have proved to be excellent tools for automation of sample pretreatment, separation/preconcentration of chromium species, and their detection by various instrumental techniques. Analytical strategies used in chromium speciation analysis discussed in this review are divided into categories based on selective extraction/separation of chromium species on solid sorbents and liquid-liquid extraction of chromium species. The most popular strategy is that based on solid-phase extraction. Therefore, this review shows the potential of novel materials designed and used for selective binding of chromium species. The progress in miniaturization of measurement systems is also presented.

Solution- and solid-phase parallel synthesis of 4-alkoxy-substituted pyrimidines with high molecular diversity.

PubMed

Font, David; Heras, Montserrat; Villalgordo, José M

2003-01-01

A simple and straightforward methodology toward the synthesis of novel 2,6-disubstituted-4-alkoxypyrimidine derivatives of type 16 and 19 has been developed. This methodology, initially developed in solution, can be perfectly adapted to the solid support under analogous conditions, taking full advantage of automated parallel synthesis systems. This successful methodology benefits from the key role played by the thioether linkage placed at the 2-position in 3, 9, or 13 in a double manner: on one side, the steric effect exerted by the thioether linkage is likely to be responsible for the very high observed selectivity toward the formation of the O-alkylation products. On the other side, this sulfur linkage can serve not only as a robust point of attachment for the heterocycle, stable to a number of reaction conditions, but also as a means of introducing a new element of diversity through activation to the corresponding sulfone (safety-catch linker concept) and subsequent ipso-substitution reaction with a variety of different N-nucleophiles.

Solid phase sequencing of double-stranded nucleic acids

DOEpatents

Fu, Dong-Jing; Cantor, Charles R.; Koster, Hubert; Smith, Cassandra L.

2002-01-01

This invention relates to methods for detecting and sequencing of target double-stranded nucleic acid sequences, to nucleic acid probes and arrays of probes useful in these methods, and to kits and systems which contain these probes. Useful methods involve hybridizing the nucleic acids or nucleic acids which represent complementary or homologous sequences of the target to an array of nucleic acid probes. These probe comprise a single-stranded portion, an optional double-stranded portion and a variable sequence within the single-stranded portion. The molecular weights of the hybridized nucleic acids of the set can be determined by mass spectroscopy, and the sequence of the target determined from the molecular weights of the fragments. Nucleic acids whose sequences can be determined include nucleic acids in biological samples such as patient biopsies and environmental samples. Probes may be fixed to a solid support such as a hybridization chip to facilitate automated determination of molecular weights and identification of the target sequence.

Benefits of smart pumps for automated changeovers of vasoactive drug infusion pumps: a quasi-experimental study.

PubMed

Cour, M; Hernu, R; Bénet, T; Robert, J M; Regad, D; Chabert, B; Malatray, A; Conrozier, S; Serra, P; Lassaigne, M; Vanhems, P; Argaud, L

2013-11-01

Manual changeover of vasoactive drug infusion pumps (CVIP) frequently lead to haemodynamic instability. Some of the newest smart pumps allow automated CVIP. The aim of this study was to compare automated CVIP with manual 'Quick Change' relays. We performed a prospective, quasi-experimental study, in a university-affiliated intensive care unit (ICU). All adult patients receiving continuous i.v. infusion of vasoactive drugs were included. CVIP were successively performed manually (Phase 1) and automatically (Phase 2) during two 6-month periods. The primary endpoint was the frequency of haemodynamic incidents related to the relays, which were defined as variations of mean arterial pressure >15 mm Hg or heart rate >15 bpm. The secondary endpoints were the nursing time dedicated to relays and the number of interruptions in care because of CVIP. A multivariate mixed effects logistic regression was fitted for analytic analysis. We studied 1329 relays (Phase 1: 681, Phase 2: 648) from 133 patients (Phase 1: 63, Phase 2: 70). Incidents related to CVIP decreased from 137 (20%) in Phase 1 to 73 (11%) in Phase 2 (P<0.001). Automated relays were independently associated with a 49% risk reduction of CVIP-induced incidents (adjusted OR=0.51, 95% confidence interval 0.34-0.77, P=0.001). Time dedicated to the relays and the number of interruptions in care to manage CVIP were also significantly reduced with automated relays vs manual relays (P=0.001). These results demonstrate the benefits of automated CVIP using smart pumps in limiting the frequency of haemodynamic incidents related to relays and in reducing the nursing workload.

EPA Method 3135.2I: Cyanide, Total and Amenable in Aqueous and Solid Samples Automated Colorimetric With Manual Digestion

EPA Pesticide Factsheets

This method describes procedures for preparation and analysis of solid, water and wipe samples for detection and measurement of cyanide amendable to chlorination using acid digestion and spectrophotometry.

Impact of assay design on test performance: lessons learned from 25-hydroxyvitamin D.

PubMed

Farrell, Christopher-John L; Soldo, Joshua; McWhinney, Brett; Bandodkar, Sushil; Herrmann, Markus

2014-11-01

Current automated immunoassays vary significantly in many aspects of their design. This study sought to establish if the theoretical advantages and disadvantages associated with different design formats of automated 25-hydroxyvitamin D (25-OHD) assays are translated into variations in assay performance in practice. 25-OHD was measured in 1236 samples using automated assays from Abbott, DiaSorin, Roche and Siemens. A subset of 362 samples had up to three liquid chromatography-tandem mass spectrometry 25-OHD analyses performed. 25-OHD₂ recovery, dilution recovery, human anti-animal antibody (HAAA) interference, 3-epi-25-OHD₃ cross-reactivity and precision of the automated assays were evaluated. The assay that combined release of 25-OHD with analyte capture in a single step showed the most accurate 25-OHD₂ recovery and the best dilution recovery. The use of vitamin D binding protein (DBP) as the capture moiety was associated with 25-OHD₂ under-recovery, a trend consistent with 3-epi-25-OHD₃ cross-reactivity and immunity to HAAA interference. Assays using animal-derived antibodies did not show 3-epi-25-OHD₃ cross-reactivity but were variably susceptible to HAAA interference. Not combining 25-OHD release and capture in one step and use of biotin-streptavidin interaction for solid phase separation were features of the assays with inferior accuracy for diluted samples. The assays that used a backfill assay format showed the best precision at high concentrations but this design did not guarantee precision at low 25-OHD concentrations. Variations in design among automated 25-OHD assays influence their performance characteristics. Consideration of the details of assay design is therefore important when selecting and validating new assays.

Molecularly imprinted polymer cartridges coupled on-line with high performance liquid chromatography for simple and rapid analysis of dextromethorphan in human plasma samples.

PubMed

Moein, Mohammad Mahdi; Javanbakht, Mehran; Akbari-Adergani, Behrouz

2011-04-01

In this paper, a novel method is described for automated determination of dextromethorphan in biological fluids using molecularly imprinted solid-phase extraction (MISPE) as a sample clean-up technique combined with high performance liquid chromatography (HPLC). The water-compatible molecularly imprinted polymers (MIPs) were prepared using methacrylic acid as functional monomer, ethylene glycol dimethacrylate as cross-linker, chloroform as porogen and dextromethorphan as template molecule. These imprinted polymers were used as solid-phase extraction sorbent for the extraction of dextromethorphan from human plasma samples. Various parameters affecting the extraction efficiency of the MIP cartridges were evaluated. The high selectivity of the sorbent coupled to the high performance liquid chromatographic system permitted a simple and rapid analysis of this drug in plasma samples with limits of detection (LOD) and quantification (LOQ) of 0.12 ng/mL and 0.35 ng/mL, respectively. The MIP selectivity was evaluated by analyzing of the dextromethorphan in presence of several substances with similar molecular structures and properties. Results from the HPLC analyses showed that the recoveries of dextromethorphan using MIP cartridges from human plasma samples in the range of 1-50 ng/mL were higher than 87%. Copyright © 2011 Elsevier B.V. All rights reserved.

Determination of transformation products of unsymmetrical dimethylhydrazine in water using vacuum-assisted headspace solid-phase microextraction.

PubMed

Orazbayeva, Dina; Kenessov, Bulat; Psillakis, Elefteria; Nassyrova, Dayana; Bektassov, Marat

2018-06-22

A new, sensitive and simple method based on vacuum-assisted headspace solid-phase microextraction (Vac-HSSPME) followed by gas chromatography-mass-spectrometry (GC-MS), is proposed for the quantification of rocket fuel unsymmetrical dimethylhydrazine (UDMH) transformation products in water samples. The target transformation products were: pyrazine, 1-methyl-1H-pyrazole, N-nitrosodimethylamine, N,N-dimethylformamide, 1-methyl-1Н-1,2,4-triazole, 1-methyl-imidazole and 1H-pyrazole. For these analytes and within shorter sampling times, Vac-HSSPME yielded detection limits (0.5-100 ng L -1 ) 3-10 times lower than those reported for regular HSSPME. Vac-HSSPME sampling for 30 min at 50 °C yielded the best combination of analyte responses and their standard deviations (<15%). 1-Formyl-2,2-dimethylhydrazine and formamide were discarded because of the poor precision and accuracy when using Vac-HSSPME. The recoveries for the rest of the analytes ranged between 80 and 119%. The modified Mininert valve and Thermogreen septum could be used for automated extraction as it ensured stable analyte signals even after long waiting times (>24 h). Finally, multiple Vac-HSSME proved to be an efficient tool for controlling the matrix effect and quantifying UDMH transformation products. Copyright © 2018 Elsevier B.V. All rights reserved.

Determination of glutaraldehyde in water samples by headspace solid-phase microextraction and gas chromatography-mass spectrometry after derivatization with 2,2,2-trifluoroethylhydrazine.

PubMed

Kang, Hye-In; Shin, Ho-Sang

2016-05-27

A simple and convenient headspace solid-phase microextraction (HS-SPME) gas chromatography mass spectrometry (GC-MS) method was described for the determination of glutaraldehyde in water. Glutaraldehyde in water reacted with 2,2,2-trifluoroethylhydrazine (TFEH) in a headspace vial and the formed TFEH derivatives were vaporized and adsorbed onto a fiber. The optimal HS-SPME conditions were achieved with a 50/30μm-divinylbenzene-carboxen-polydimethylsiloxane fiber, 0.06% 2,2,2-TFEH, 25% salt, an extraction/derivatization temperature of 80°C, a heating time of 30min, and a pH of 6.5. The desorption was performed for 1min at 240°C. Under the established conditions, the lowest limits of detection were 0.3μg/L and 0.1μg/L in 6.0mL of surface water and drinking water, respectively, and the intra- and inter-day relative standard deviation was less than 9.1% at concentrations of 50, 100 and 500μg/L. The calibration curve showed good linearity with R=0.9995 and R=0.9993 in surface water and drinking water, respectively. This method is simple, amenable to automation and environmentally friendly. Copyright © 2016 Elsevier B.V. All rights reserved.

A high-throughput solid-phase extraction microchip combined with inductively coupled plasma-mass spectrometry for rapid determination of trace heavy metals in natural water.

PubMed

Shih, Tsung-Ting; Hsieh, Cheng-Chuan; Luo, Yu-Ting; Su, Yi-An; Chen, Ping-Hung; Chuang, Yu-Chen; Sun, Yuh-Chang

2016-04-15

Herein, a hyphenated system combining a high-throughput solid-phase extraction (htSPE) microchip with inductively coupled plasma-mass spectrometry (ICP-MS) for rapid determination of trace heavy metals was developed. Rather than performing multiple analyses in parallel for the enhancement of analytical throughput, we improved the processing speed for individual samples by increasing the operation flow rate during SPE procedures. To this end, an innovative device combining a micromixer and a multi-channeled extraction unit was designed. Furthermore, a programmable valve manifold was used to interface the developed microchip and ICP-MS instrumentation in order to fully automate the system, leading to a dramatic reduction in operation time and human error. Under the optimized operation conditions for the established system, detection limits of 1.64-42.54 ng L(-1) for the analyte ions were achieved. Validation procedures demonstrated that the developed method could be satisfactorily applied to the determination of trace heavy metals in natural water. Each analysis could be readily accomplished within just 186 s using the established system. This represents, to the best of our knowledge, an unprecedented speed for the analysis of trace heavy metal ions. Copyright © 2016 Elsevier B.V. All rights reserved.

Rapid simultaneous determination of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, and 3,4-methylenedioxyethylamphetamine in urine by solid-phase extraction and GC-MS: a method optimized for high-volume laboratories.

PubMed

Stout, Peter R; Horn, Carl K; Klette, Kevin L

2002-01-01

To facilitate analysis of high sample volumes, an extraction, derivatization and gas chromatographic-mass spectrometric analysis method was developed to simultaneously determine amphetamine (AMP), methamphetamine (MAMP), 3,4-methylenedioxyamphetamine (MDA) 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyethylamphetamine (MDEA) in urine. This method utilized a positive-pressure manifold cation-exchange polymer-based solid-phase extraction followed by elution directly into automated liquid sampler (ALS) vials. Rapid derivatization was accomplished using heptafluorobutyric anhydride (HFBA). Recoveries averaged 90% or greater for each of the compounds. Limits of detection were 62.5 ng/mL (AMP and MDEA), 15.6 ng/mL (MAMP), and 31.3 ng/mL (MDA and MDMA) using a 2-mL sample volume. The method was linear to 5000 ng/mL for all compounds using MDMA-d5 and MAMP-d14 as internal standards. Over 200 human urine samples previously determined to contain the target analytes were analyzed using the method. Excellent agreement was seen with previous quantitations. The method was challenged with 75 potentially interfering compounds and no interferences were seen. These interfering compounds included ephedrine, pseudoephedrine, phenylpropanolamine, and phenethylamine. The method resulted in dramatic reductions in processing time and waste production.

Spectral neighbor analysis method for automated generation of quantum-accurate interatomic potentials

NASA Astrophysics Data System (ADS)

Thompson, A. P.; Swiler, L. P.; Trott, C. R.; Foiles, S. M.; Tucker, G. J.

2015-03-01

We present a new interatomic potential for solids and liquids called Spectral Neighbor Analysis Potential (SNAP). The SNAP potential has a very general form and uses machine-learning techniques to reproduce the energies, forces, and stress tensors of a large set of small configurations of atoms, which are obtained using high-accuracy quantum electronic structure (QM) calculations. The local environment of each atom is characterized by a set of bispectrum components of the local neighbor density projected onto a basis of hyperspherical harmonics in four dimensions. The bispectrum components are the same bond-orientational order parameters employed by the GAP potential [1]. The SNAP potential, unlike GAP, assumes a linear relationship between atom energy and bispectrum components. The linear SNAP coefficients are determined using weighted least-squares linear regression against the full QM training set. This allows the SNAP potential to be fit in a robust, automated manner to large QM data sets using many bispectrum components. The calculation of the bispectrum components and the SNAP potential are implemented in the LAMMPS parallel molecular dynamics code. We demonstrate that a previously unnoticed symmetry property can be exploited to reduce the computational cost of the force calculations by more than one order of magnitude. We present results for a SNAP potential for tantalum, showing that it accurately reproduces a range of commonly calculated properties of both the crystalline solid and the liquid phases. In addition, unlike simpler existing potentials, SNAP correctly predicts the energy barrier for screw dislocation migration in BCC tantalum.

Direct Sampling and Analysis from Solid Phase Extraction Cards using an Automated Liquid Extraction Surface Analysis Nanoelectrospray Mass Spectrometry System

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

Walworth, Matthew J; ElNaggar, Mariam S; Stankovich, Joseph J

Direct liquid extraction based surface sampling, a technique previously demonstrated with continuous flow and autonomous pipette liquid microjunction surface sampling probes, has recently been implemented as the Liquid Extraction Surface Analysis (LESA) mode on the commercially available Advion NanoMate chip-based infusion nanoelectrospray ionization system. In the present paper, the LESA mode was applied to the analysis of 96-well format custom solid phase extraction (SPE) cards, with each well consisting of either a 1 or 2 mm diameter monolithic hydrophobic stationary phase. These substrate wells were conditioned, loaded with either single or multi-component aqueous mixtures, and read out using the LESAmore » mode of a TriVersa NanoMate or a Nanomate 100 coupled to an ABI/Sciex 4000QTRAPTM hybrid triple quadrupole/linear ion trap mass spectrometer and a Thermo LTQ XL linear ion trap mass spectrometer. Extraction conditions, including extraction/nanoESI solvent composition, volume, and dwell times, were optimized in the analysis of targeted compounds. Limit of detection and quantitation as well as analysis reproducibility figures of merit were measured. Calibration data was obtained for propranolol using a deuterated internal standard which demonstrated linearity and reproducibility. A 10x increase in signal and cleanup of micromolar Angiotensin II from a concentrated salt solution was demonstrated. Additionally, a multicomponent herbicide mixture at ppb concentration levels was analyzed using MS3 spectra for compound identification in the presence of isobaric interferences.« less

Direct-write liquid phase transformations with a scanning transmission electron microscope

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

Unocic, Raymond R.; Lupini, Andrew R.; Borisevich, Albina Y.

The highly energetic electron beam from a scanning transmission electron microscope (STEM) can induce local changes in the state of matter, ranging from local knock-out and atomic movement, to amorphization/crystallization, and chemical/electrochemical reactions occuring at localized liquid-solid and gas-solid interfaces. To date, fundamental studies of e-beam induced phenomena and practical applications have been limited by conventional e-beam rastering modes that allow only for uniform e-beam exposures. Here we develop an automated liquid phase nanolithography method that is capable of directly writing nanometer scaled features within silicon nitride encapsulated liquid cells. An external beam control system, connected to the scan coilsmore » of an aberration-corrected STEM, is used to precisely control the position, dwell time, and scan velocity of a sub-nanometer STEM probe. Site-specific locations in a sealed liquid cell containing an aqueous solution of H 2PdCl 4 are irradiated to controllably deposit palladium onto silicon nitride membranes. We determine the threshold electron dose required for the radiolytic deposition of metallic palladium, explore the influence of electron dose on the feature size and morphology of nanolithographically patterned nanostructures, and propose a feedback-controlled monitoring method for active control of the nanofabricated structures through STEM detector signal monitoring. As a result, this approach enables both fundamental studies of electron beam induced interactions with matter, as well as opens a pathway to fabricate nanostructures with tailored architectures and chemistries via shape-controlled nanolithographic patterning from liquid phase precursors.« less

Direct-write liquid phase transformations with a scanning transmission electron microscope

DOE PAGES

Unocic, Raymond R.; Lupini, Andrew R.; Borisevich, Albina Y.; ...

2016-08-03

The highly energetic electron beam from a scanning transmission electron microscope (STEM) can induce local changes in the state of matter, ranging from local knock-out and atomic movement, to amorphization/crystallization, and chemical/electrochemical reactions occuring at localized liquid-solid and gas-solid interfaces. To date, fundamental studies of e-beam induced phenomena and practical applications have been limited by conventional e-beam rastering modes that allow only for uniform e-beam exposures. Here we develop an automated liquid phase nanolithography method that is capable of directly writing nanometer scaled features within silicon nitride encapsulated liquid cells. An external beam control system, connected to the scan coilsmore » of an aberration-corrected STEM, is used to precisely control the position, dwell time, and scan velocity of a sub-nanometer STEM probe. Site-specific locations in a sealed liquid cell containing an aqueous solution of H 2PdCl 4 are irradiated to controllably deposit palladium onto silicon nitride membranes. We determine the threshold electron dose required for the radiolytic deposition of metallic palladium, explore the influence of electron dose on the feature size and morphology of nanolithographically patterned nanostructures, and propose a feedback-controlled monitoring method for active control of the nanofabricated structures through STEM detector signal monitoring. As a result, this approach enables both fundamental studies of electron beam induced interactions with matter, as well as opens a pathway to fabricate nanostructures with tailored architectures and chemistries via shape-controlled nanolithographic patterning from liquid phase precursors.« less

Determination of 15 N-nitrosodimethylamine precursors in different water matrices by automated on-line solid-phase extraction ultra-high-performance-liquid chromatography tandem mass spectrometry.

PubMed

Farré, Maria José; Insa, Sara; Mamo, Julian; Barceló, Damià

2016-08-05

A new methodology based on on-line solid-phase extraction (SPE) ultra-high-performance-liquid chromatography coupled to a triple quadrupole mass spectrometer (UHPLC-MS-MS) for the determination of 15 individual anthropogenic N-nitrosodimethylamine (NDMA) precursors was developed. On-line SPE was performed by passing 2mL of the water sample through a Hypersil GOLD aQ column and chromatographic separation was done using a Kinetex Biphenyl column using methanol and 0.1% formic acid aqueous solution as a mobile phase. For unequivocal identification and confirmation, two selected reaction monitoring (SRM) transitions were monitored per compound. Quantification was performed by internal standard approach and matrix match calibration. The main advantages of the developed method are high sensitivity (limits of detection in the sub ng/L range), selectivity due to the use of tandem mass spectrometry, precision and minimum sample manipulation as well as fast analytical response. Process efficiency and recovery were also evaluated for all the target compounds. As part of the validation procedure, the method was applied in a sampling campaign for the analysis of influent and secondary effluent of a wastewater treatment plant (WWTP) in Girona, Spain. Additionally, the effluent from a nanofiltration (NF) membrane system used for water recycling was monitored. The percentage of NDMA formation explained by the measured precursors was also quantified. Copyright © 2016 Elsevier B.V. All rights reserved.

Development and Experimental Evaluation of an Automated Multi-Media Course on Transistors.

ERIC Educational Resources Information Center

Whitted, J.H., Jr.; And Others

A completely automated multi-media self-study program for teaching a portion of electronic solid-state fundamentals was developed. The subject matter areas included were fundamental theory of transistors, transistor amplifier fundamentals, and simple mathematical analysis of transistors including equivalent circuits, parameters, and characteristic…

Manufacturing Technology for Apparel Automation. Phase 1, 2 and 3 Activity.

DTIC Science & Technology

1987-10-15

A189 129 MANUFACTURING TECHNOLOGY FOR APPAREL AUTOMATION PHASE I t/l 2 AND I ACTIVITY(U) NORTH CAROLINA STATE UNIV ATRALEIGH SCHOOL OF TEXTILES E M...34III 1.8 - iai T ON HART St 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 MTC FILE coax Report: NCSU/DLA-87/2 CDRL A004 MANUFACTURING TECHNOLOGY FOR APPAREL...I Report: NCSU/DLA-87/2 CDRL A004 MANUFACTURING TECHNOLOGY FOR APPAREL AUTOMATION Phase I, II and III Activity Edwin M. McPherson North Carolina

Automated GC-MS analysis of free amino acids in biological fluids.

PubMed

Kaspar, Hannelore; Dettmer, Katja; Gronwald, Wolfram; Oefner, Peter J

2008-07-15

A gas chromatography-mass spectrometry (GC-MS) method was developed for the quantitative analysis of free amino acids as their propyl chloroformate derivatives in biological fluids. Derivatization with propyl chloroformate is carried out directly in the biological samples without prior protein precipitation or solid-phase extraction of the amino acids, thereby allowing automation of the entire procedure, including addition of reagents, extraction and injection into the GC-MS. The total analysis time was 30 min and 30 amino acids could be reliably quantified using 19 stable isotope-labeled amino acids as internal standards. Limits of detection (LOD) and lower limits of quantification (LLOQ) were in the range of 0.03-12 microM and 0.3-30 microM, respectively. The method was validated using a certified amino acid standard and reference plasma, and its applicability to different biological fluids was shown. Intra-day precision for the analysis of human urine, blood plasma, and cell culture medium was 2.0-8.8%, 0.9-8.3%, and 2.0-14.3%, respectively, while the inter-day precision for human urine was 1.5-14.1%.

Large Scale Screening of Low Cost Ferritic Steel Designs For Advanced Ultra Supercritical Boiler Using First Principles Methods

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

Ouyang, Lizhi

Advanced Ultra Supercritical Boiler (AUSC) requires materials that can operate in corrosive environment at temperature and pressure as high as 760°C (or 1400°F) and 5000psi, respectively, while at the same time maintain good ductility at low temperature. We develop automated simulation software tools to enable fast large scale screening studies of candidate designs. While direct evaluation of creep rupture strength and ductility are currently not feasible, properties such as energy, elastic constants, surface energy, interface energy, and stack fault energy can be used to assess their relative ductility and creeping strength. We implemented software to automate the complex calculations tomore » minimize human inputs in the tedious screening studies which involve model structures generation, settings for first principles calculations, results analysis and reporting. The software developed in the project and library of computed mechanical properties of phases found in ferritic steels, many are complex solid solutions estimated for the first time, will certainly help the development of low cost ferritic steel for AUSC.« less

Development of an Automated Seed Sowing and Induced Germination System for Space Flight Application

NASA Technical Reports Server (NTRS)

Heyenga, A. G.; Kliss, Mark

1995-01-01

The successful utilization of higher plants in space flight is likely to require the effective transition of plants through all phases of growth and development. A particularly sensitive and critical stage in this cycle is seed germination. The present inflight capability to manipulate seed from a state of dormancy to germination and the performance of such activity under aseptic conditions is extremely limited. An Automated Sowing Mechanism (ASM) has been designed to address this area of science and technology. The self-contained system is readily compatible with the existing Shuttle middeck locker Plant Growth Unit (PGU) and planned Plant Growth Facility (PGF), presenting an opportunity to extend the experimental capability of these systems. The ASM design encompasses the controlled transition of seed from a dry to hydrated state utilizing solid media substrate as the source of water and nutrient support. System activation has been achieved with both photo and timing mechanisms. Controlled induced germination and development of various plant species has been achieved in ground-based trials. The system is presently being prepared for a KC-135 flight test.

Detection of ALK translocation in non-small cell lung carcinoma (NSCLC) and its clinicopathological significance using the Ventana immunohistochemical staining method: a single-center large-scale investigation of 1, 504 Chinese Han patients

PubMed Central

Yang, Lin; Ling, Yun; Guo, Lei; Ma, Di; Xue, Xuemin; Wang, Bingning; Li, Junling; Ying, Jianming

2016-01-01

Objective The novel fully automated immunohistochemistry (IHC) assay-Ventana anaplastic lymphoma kinase (ALK)-D5F3 for screening ALK rearrangements has been approved by China’s Food and Drug Administration in 2013, our previous study disclosed a highly specificity and sensitivity nearly 100%, and its efficacy needs to be evaluated in a large cohort of primary lung adenocarcinoma patients, and to compare clinicopathological features with ALK (+) and ALK (-) lung adenocarcinoma. Methods A total of 1,504 consecutive surgical lung adenocarcinoma cases of Chinese Han population were collected and re-diagnosed according to the 2011 multidisciplinary classification of lung adenocarcinoma. Fully automated Ventana ALK-D5F3 IHC staining with a binary scoring was adopted to evaluate staining and correlated with clinicopathological characters, including age, sex, differentiation degree, histological subtype, lymph node metastasis, and clinical staging. ALK (+) patients were followed-up, and targeted therapy of ALK-inhibitors was adopted and observed in patients with stage IV according to the NCCN guideline. Results ALK positive adenocarcinomas were identified in 6.6% of the surgically resected 1,504 NSCLCs, and significantly younger than the negative group (P<0.05).Mucinous adenocarcinoma (28.2%) was determined to be predominant in ALK (+) cases, followed by the solid type (11.7%), specific type (6.8%), papillary type (5.6%), acinar type (5.5%), and lepidic type (3.1%), and the differences were statistically significant (χ2=42.011, P<0.05). ALK (+) adenocarcinoma with lymph node metastasis (10.8%) were significantly higher than that without lymph node metastasis (4.5%) (χ2=19.809, P<0.05); and ALK (+) in phase IV (20%) was significantly higher than phase III (12.9%), phase II (4.2%), phase I (4.5%), and phase 0 (0) (χ2=36.068, P<0.05). Multivariate logistic regression disclosed that patient age, AJCC staging, and histological mucinous subtype were correlated with ALK positive staining (OR=0.959, 1.578, 5.036, respectively). Sixty eight patients had followed-up results, five patients out of which primarily diagnosed or progressed into Stage IV benefited well from targeted therapy with Crizotinib. Conclusions The ALK fusion protein was seen in 6.6% Chinese NSCLC patients, and mostly seen in younger, clinically higher staging, mucinous and solid predominant adenocarcinoma. Clinical trials in patients of Stage IV confirmed that ALK-D5F3 Ventana IHC is serviceable in screening ALK-positive candidates for molecular targeted therapy. PMID:27877008

Detection of ALK translocation in non-small cell lung carcinoma (NSCLC) and its clinicopathological significance using the Ventana immunohistochemical staining method: a single-center large-scale investigation of 1, 504 Chinese Han patients.

PubMed

Yang, Lin; Ling, Yun; Guo, Lei; Ma, Di; Xue, Xuemin; Wang, Bingning; Li, Junling; Ying, Jianming

2016-10-01

The novel fully automated immunohistochemistry (IHC) assay-Ventana anaplastic lymphoma kinase (ALK)-D5F3 for screening ALK rearrangements has been approved by China's Food and Drug Administration in 2013, our previous study disclosed a highly specificity and sensitivity nearly 100%, and its efficacy needs to be evaluated in a large cohort of primary lung adenocarcinoma patients, and to compare clinicopathological features with ALK (+) and ALK (-) lung adenocarcinoma. A total of 1,504 consecutive surgical lung adenocarcinoma cases of Chinese Han population were collected and re-diagnosed according to the 2011 multidisciplinary classification of lung adenocarcinoma. Fully automated Ventana ALK-D5F3 IHC staining with a binary scoring was adopted to evaluate staining and correlated with clinicopathological characters, including age, sex, differentiation degree, histological subtype, lymph node metastasis, and clinical staging. ALK (+) patients were followed-up, and targeted therapy of ALK-inhibitors was adopted and observed in patients with stage IV according to the NCCN guideline. ALK positive adenocarcinomas were identified in 6.6% of the surgically resected 1,504 NSCLCs, and significantly younger than the negative group (P<0.05).Mucinous adenocarcinoma (28.2%) was determined to be predominant in ALK (+) cases, followed by the solid type (11.7%), specific type (6.8%), papillary type (5.6%), acinar type (5.5%), and lepidic type (3.1%), and the differences were statistically significant (χ 2 =42.011, P<0.05). ALK (+) adenocarcinoma with lymph node metastasis (10.8%) were significantly higher than that without lymph node metastasis (4.5%) (χ 2 =19.809, P<0.05); and ALK (+) in phase IV (20%) was significantly higher than phase III (12.9%), phase II (4.2%), phase I (4.5%), and phase 0 (0) (χ 2 =36.068, P<0.05). Multivariate logistic regression disclosed that patient age, AJCC staging, and histological mucinous subtype were correlated with ALK positive staining (OR=0.959, 1.578, 5.036, respectively). Sixty eight patients had followed-up results, five patients out of which primarily diagnosed or progressed into Stage IV benefited well from targeted therapy with Crizotinib. The ALK fusion protein was seen in 6.6% Chinese NSCLC patients, and mostly seen in younger, clinically higher staging, mucinous and solid predominant adenocarcinoma. Clinical trials in patients of Stage IV confirmed that ALK-D5F3 Ventana IHC is serviceable in screening ALK-positive candidates for molecular targeted therapy.

Parallel solution-phase synthesis of a 2-aminothiazole library including fully automated work-up.

PubMed

Buchstaller, Hans-Peter; Anlauf, Uwe

2011-02-01

A straightforward and effective procedure for the solution phase preparation of a 2-aminothiazole combinatorial library is described. Reaction, work-up and isolation of the title compounds as free bases was accomplished in a fully automated fashion using the Chemspeed ASW 2000 automated synthesizer. The compounds were obtained in good yields and excellent purities without any further purification procedure.

Titanium(IV) isopropoxide mediated solution phase reductive amination on an automated platform: application in the generation of urea and amide libraries.

PubMed

Bhattacharyya, S; Fan, L; Vo, L; Labadie, J

2000-04-01

Amine libraries and their derivatives are important targets for high throughput synthesis because of their versatility as medicinal agents and agrochemicals. As a part of our efforts towards automated chemical library synthesis, a titanium(IV) isopropoxide mediated solution phase reductive amination protocol was successfully translated to automation on the Trident(TM) library synthesizer of Argonaut Technologies. An array of 24 secondary amines was prepared in high yield and purity from 4 primary amines and 6 carbonyl compounds. These secondary amines were further utilized in a split synthesis to generate libraries of ureas, amides and sulfonamides in solution phase on the Trident(TM). The automated runs included 192 reactions to synthesize 96 ureas in duplicate and 96 reactions to synthesize 48 amides and 48 sulfonamides. A number of polymer-assisted solution phase protocols were employed for parallel work-up and purification of the products in each step.

Attractive design: an elution solvent optimization platform for magnetic-bead-based fractionation using digital microfluidics and design of experiments.

PubMed

Lafrenière, Nelson M; Mudrik, Jared M; Ng, Alphonsus H C; Seale, Brendon; Spooner, Neil; Wheeler, Aaron R

2015-04-07

There is great interest in the development of integrated tools allowing for miniaturized sample processing, including solid phase extraction (SPE). We introduce a new format for microfluidic SPE relying on C18-functionalized magnetic beads that can be manipulated in droplets in a digital microfluidic platform. This format provides the opportunity to tune the amount (and potentially the type) of stationary phase on-the-fly, and allows the removal of beads after the extraction (to enable other operations in same device-space), maintaining device reconfigurability. Using the new method, we employed a design of experiments (DOE) operation to enable automated on-chip optimization of elution solvent composition for reversed phase SPE of a model system. Further, conditions were selected to enable on-chip fractionation of multiple analytes. Finally, the method was demonstrated to be useful for online cleanup of extracts from dried blood spot (DBS) samples. We anticipate this combination of features will prove useful for separating a wide range of analytes, from small molecules to peptides, from complex matrices.

Managing the Implementation of Mission Operations Automation

NASA Technical Reports Server (NTRS)

Sodano, R.; Crouse, P.; Odendahl, S.; Fatig, M.; McMahon, K.; Lakin, J.

2006-01-01

Reducing the cost of mission operations has necessitated a high level of automation both on spacecraft and ground systems. While automation on spacecraft is implemented during the design phase, ground system automation tends to be implemented during the prime mission operations phase. Experience has shown that this tendency for late automation development can be hindered by several factors: additional hardware and software resources may need to be procured; software must be developed and tested on a non-interference basis with primary operations with limited manpower; and established procedures may not be suited for automation requiring substantial rework. In this paper we will review the experience of successfully automating mission operations for seven on-orbit missions: the Compton Gamma Ray Observatory (CGRO), the Rossi X-Ray Timing Explorer (RXTE), the Advanced Composition Explorer (ACE), the Far Ultraviolet Spectroscopic Explorer (FUSE), Interplanetary Physics Laboratory (WIND), Polar Plasma Laboratory (POLAR), and the Imager for Magnetopause-to-Aurora Global Exploration (IMAGE). We will provide lessons learned in areas such as: spacecraft recorder management, procedure development, lights out commanding from the ground system vs. stored command loads, spacecraft contingency response time, and ground station interfaces. Implementing automation strategies during the mission concept and spacecraft integration and test phase as the most efficient method will be discussed.

Industrial Technology Modernization Program. Project 28. Automation of Receiving, Receiving Inspection and Stores

DTIC Science & Technology

1987-06-15

001 GENERAL DYNAMICS 00 FORT WORTH DIVISION INDUSTRIAL TECHNOLOGY MODERNIZATION PROGRAM Phase 2 Final Project Repc t JUNG 0 ?7 PROJECT 28 AUTOMATION...DYNAMICS FORT WORTH DIVISION INDUSTRIAL TECHNOLOGY MODERNIZATION PROGRAM Phase 2 Final Project Report PROJECT 28 AUTOMATION OF RECEIVING, RECEIVING...13 6 PROJECT ASSUMPTIONS 20 7 PRELIMINARY/FINAL DESIGN AND FINDINGS 21 8 SYSTEM/EQUIPMENT/MACHINING SPECIFICATIONS 37 9 VENDOR/ INDUSTRY ANALYSIS

Fully automated SPE-based synthesis and purification of 2-[18F]fluoroethyl-choline for human use.

PubMed

Schmaljohann, Jörn; Schirrmacher, Esther; Wängler, Björn; Wängler, Carmen; Schirrmacher, Ralf; Guhlke, Stefan

2011-02-01

2-[(18)F]Fluoroethyl-choline ([(18)F]FECH) is a promising tracer for the detection of prostate cancer as well as brain tumors with positron emission tomography (PET). [(18)F]FECH is actively transported into mammalian cells, becomes phosphorylated by choline kinase and gets incorporated into the cell membrane after being metabolized to phosphatidylcholine. So far, its synthesis is a two-step procedure involving at least one HPLC purification step. To allow a wider dissemination of this tracer, finding a purification method avoiding HPLC is highly desirable and would result in easier accessibility and more reliable production of [(18)F]FECH. [(18)F]FECH was synthesized by reaction of 2-bromo-1-[(18)F]fluoroethane ([(18)F]BFE) with dimethylaminoethanol (DMAE) in DMSO. We applied a novel and very reliable work-up procedure for the synthesis of [(18)F]BFE. Based on a combination of three different solid-phase cartridges, the purification of [(18)F]BFE from its precursor 2-bromoethyl-4-nitrobenzenesulfonate (BENos) could be achieved without using HPLC. Following the subsequent reaction of the purified [(18)F]BFE with DMAE, the final product [(18)F]FECH was obtained as a sterile solution by passing the crude reaction mixture through a combination of two CM plus cartridges and a sterile filter. The fully automated synthesis was performed using as well a Raytest SynChrom module (Raytest, Germany) or a Scintomics HotboxIII module (Scintomics, Germany). The radiotracer [(18)F]FECH can be synthesized in reliable radiochemical yields (RCY) of 37±5% (Synchrom module) and 33±5% (Hotbox III unit) in less than 1 h using these two fully automated commercially available synthesis units without HPLC involvement for purification. Detailed quality control of the final injectable [(18)F]FECH solution proved the high radiochemical purity and the absence of Kryptofix2.2.2, DMAE and DMSO used in the course of synthesis. Sterility and bacterial endotoxin testing following standard procedures verified that the described production method for [(18)F]FECH is suitable for human applications. The routine production of [(18)F]FECH with sufficient RCYs was established by reliable and fast solid-phase extraction purifications of both the secondary labeling precursor [(18)F]BFE and the final product [(18)F]FECH, avoiding complex and sensitive HPLC equipment. The purity of the product was >95%, rendering the tracer suitable for human application. The newly developed purification procedure for [(18)F]BFE significantly reduces the complexity of the automated synthesis unit, hence reducing the cost for routine production in a clinical setup and allowing easy transfer to different synthesis modules. Copyright © 2011 Elsevier Inc. All rights reserved.

Modified sedimentation-dispersion model for solids in a three-phase slurry column

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

Smith, D.N.; Ruether, J.A.; Shah, Y.T.

1986-03-01

Solids distribution data for a three-phase, batch-fluidized slurry bubble column (SBC) are presented, using air as the gas phase, pure liquids and solutions as the liquid phase, and glass beads and carborundum catalyst powder as the solid phase. Solids distribution data for the three-phase SBC operated in a continuous mode of operation are also presented, using nitrogen as the gas phase, water as the liquid phase, and glass beads as the solid phase. A new model to provide a reasonable approach to predict solids concentration distributions for systems containing polydispersed solids is presented. The model is a modification of standardmore » sedimentation-dispersion model published earlier. Empirical correlations for prediction of hindered settling velocity and solids dispersion coefficient for systems containing polydispersed solids are presented. A new method of evaluating critical gas velocity (CGV) from concentrations of the sample withdrawn at the same port of the SBC is presented. Also presented is a new mapping for CGV which separates the two regimes in the SBC, namely, incomplete fluidization and complete fluidization.« less

Automated production of 124I and 64Cu using IBA Terimo and Pinctada metal electroplating and processing modules

NASA Astrophysics Data System (ADS)

Poniger, S. S.; Tochon-Danguy, H. J.; Panopoulos, H. P.; O'Keefe, G. J.; Peake, D.; Rasool, R.; Scott, A. M.

2012-12-01

There is worldwide growing interest for the production of long-lived positron emitters for molecular imaging and the development of novel immuno-PET techniques for drugs discovery. The desire to produce solid target isotopes in Australia has significantly increased over the years and several research projects for labelling of peptides, proteins and biomolecules, including labelling of recombinant antibodies has been limited due to the availability of suitable isotopes. This has led to the recent installation and commissioning of a new lab dedicated to fully automated solid target isotope production, including 124I, 64Cu, 89Zr and 86Y.

Online solid phase extraction liquid chromatography using bonded zwitterionic stationary phases and tandem mass spectrometry for rapid environmental trace analysis of highly polar hydrophilic compounds - Application for the antiviral drug Zanamivir.

PubMed

Lindberg, Richard H; Fedorova, Ganna; Blum, Kristin M; Pulit-Prociak, Jolanta; Gillman, Anna; Järhult, Josef; Appelblad, Patrik; Söderström, Hanna

2015-08-15

Zanamivir (Za) is a highly polar and hydrophilic antiviral drug used for the treatment of influenza A viruses. Za has been detected in rivers of Japan and it's environmental occurrence has the risk of inducing antiviral resistant avian influenza viruses. In this study, a rapid automated online solid phase extraction liquid chromatography method using bonded zwitterionic stationary phases and tandem mass spectrometry (SPE/LC-MS/MS) for trace analysis of Za was developed. Furthermore, an internal standard (IS) calibration method capable of quantifying Za in Milli-Q, surface water, sewage effluent and sewage influent was evaluated. Optimum pre-extraction sample composition was found to be 95/5 v/v acetonitrile/water sample and 1% formic acid. The developed method showed acceptable linearities (r(2)≥0.994), filtration recovery (≥91%), and intra-day precisions (RSD≤16%), and acceptable and environmentally relevant LOQs (≤20ngL(-1)). Storage tests showed no significant losses of Za during 20 days and +4/-20°C (≤12%) with the exception of influent samples, which should be kept at -20°C to avoid significant Za losses. The applicability of the method was demonstrated in a study on phototransformation of Za in unfiltered and filtered surface water during 28 days of artificial UV irradiation exposure. No significant (≤12%) phototransformation was found in surface water after 28 days suggesting a relatively high photostability of Za and that Za should be of environmental concern. Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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.

Application of DEN refinement and automated model building to a difficult case of molecular-replacement phasing: the structure of a putative succinyl-diaminopimelate desuccinylase from Corynebacterium glutamicum.

PubMed

Brunger, Axel T; Das, Debanu; Deacon, Ashley M; Grant, Joanna; Terwilliger, Thomas C; Read, Randy J; Adams, Paul D; Levitt, Michael; Schröder, Gunnar F

2012-04-01

Phasing by molecular replacement remains difficult for targets that are far from the search model or in situations where the crystal diffracts only weakly or to low resolution. Here, the process of determining and refining the structure of Cgl1109, a putative succinyl-diaminopimelate desuccinylase from Corynebacterium glutamicum, at ∼3 Å resolution is described using a combination of homology modeling with MODELLER, molecular-replacement phasing with Phaser, deformable elastic network (DEN) refinement and automated model building using AutoBuild in a semi-automated fashion, followed by final refinement cycles with phenix.refine and Coot. This difficult molecular-replacement case illustrates the power of including DEN restraints derived from a starting model to guide the movements of the model during refinement. The resulting improved model phases provide better starting points for automated model building and produce more significant difference peaks in anomalous difference Fourier maps to locate anomalous scatterers than does standard refinement. This example also illustrates a current limitation of automated procedures that require manual adjustment of local sequence misalignments between the homology model and the target sequence.

Application of DEN refinement and automated model building to a difficult case of molecular-replacement phasing: the structure of a putative succinyl-diaminopimelate desuccinylase from Corynebacterium glutamicum

PubMed Central

Brunger, Axel T.; Das, Debanu; Deacon, Ashley M.; Grant, Joanna; Terwilliger, Thomas C.; Read, Randy J.; Adams, Paul D.; Levitt, Michael; Schröder, Gunnar F.

2012-01-01

Phasing by molecular replacement remains difficult for targets that are far from the search model or in situations where the crystal diffracts only weakly or to low resolution. Here, the process of determining and refining the structure of Cgl1109, a putative succinyl-diaminopimelate desuccinylase from Corynebacterium glutamicum, at ∼3 Å resolution is described using a combination of homology modeling with MODELLER, molecular-replacement phasing with Phaser, deformable elastic network (DEN) refinement and automated model building using AutoBuild in a semi-automated fashion, followed by final refinement cycles with phenix.refine and Coot. This difficult molecular-replacement case illustrates the power of including DEN restraints derived from a starting model to guide the movements of the model during refinement. The resulting improved model phases provide better starting points for automated model building and produce more significant difference peaks in anomalous difference Fourier maps to locate anomalous scatterers than does standard refinement. This example also illustrates a current limitation of automated procedures that require manual adjustment of local sequence misalignments between the homology model and the target sequence. PMID:22505259

Tactical Intelligence Applications Experimentation (TIAX) Report. Intelligence Preparation of the Battlefield (IPB)-An Automated Approach to Terrain and Mobility Corridor Analysis

DTIC Science & Technology

1978-10-20

Preparation of the Battlefield (IPB) - Phase A An Automated Approach to Terrain and Mobility Cocridor Analysis Prepared For The ;*ttlefield Systems... the Battlefield (IPB) - Phase A An Automated Approach to Terrain and Mobility Corridcr Analysis, Prepared For The Battlefield Systems Integration... series of snapshots developed for Option A. The situation snapshots would be deteloped in like manner for each option, and stored in an

Simultaneous Analysis of 22 Volatile Organic Compounds in Cigarette Smoke Using Gas Sampling Bags for High-Throughput Solid-Phase Microextraction

PubMed Central

Sampson, Maureen M.; Chambers, David M.; Pazo, Daniel Y.; Moliere, Fallon; Blount, Benjamin C.; Watson, Clifford H.

2015-01-01

Quantifying volatile organic compounds (VOCs) in cigarette smoke is necessary to establish smoke-related exposure estimates and evaluate emerging products and potential reduced-exposure products. In response to this need, we developed an automated, multi-VOC quantification method for machine-generated, mainstream cigarette smoke using solidphase microextraction gas chromatography–mass spectrometry (SPME-GC–MS). This method was developed to simultaneously quantify a broad range of smoke VOCs (i.e., carbonyls and volatiles, which historically have been measured by separate assays) for large exposure assessment studies. Our approach collects and maintains vapor-phase smoke in a gas sampling bag, where it is homogenized with isotopically labeled analogue internal standards and sampled using gas-phase SPME. High throughput is achieved by SPME automation using a CTC Analytics platform and custom bag tray. This method has successfully quantified 22 structurally diverse VOCs (e.g., benzene and associated monoaromatics, aldehydes and ketones, furans, acrylonitrile, 1,3-butadiene, vinyl chloride, and nitromethane) in the microgram range in mainstream smoke from 1R5F and 3R4F research cigarettes smoked under ISO (Cambridge Filter or FTC) and Intense (Health Canada or Canadian Intense) conditions. Our results are comparable to previous studies with few exceptions. Method accuracy was evaluated with third-party reference samples (≤15% error). Short-term diffusion losses from the gas sampling bag were minimal, with a 10% decrease in absolute response after 24 h. For most analytes, research cigarette inter- and intrarun precisions were ≤20% relative standard deviation (RSD). This method provides an accurate and robust means to quantify VOCs in cigarette smoke spanning a range of yields that is sufficient to characterize smoke exposure estimates. PMID:24933649

Spectral neighbor analysis method for automated generation of quantum-accurate interatomic potentials

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

Thompson, Aidan P.; Swiler, Laura P.; Trott, Christian R.

2015-03-15

Here, we present a new interatomic potential for solids and liquids called Spectral Neighbor Analysis Potential (SNAP). The SNAP potential has a very general form and uses machine-learning techniques to reproduce the energies, forces, and stress tensors of a large set of small configurations of atoms, which are obtained using high-accuracy quantum electronic structure (QM) calculations. The local environment of each atom is characterized by a set of bispectrum components of the local neighbor density projected onto a basis of hyperspherical harmonics in four dimensions. The bispectrum components are the same bond-orientational order parameters employed by the GAP potential [1].more » The SNAP potential, unlike GAP, assumes a linear relationship between atom energy and bispectrum components. The linear SNAP coefficients are determined using weighted least-squares linear regression against the full QM training set. This allows the SNAP potential to be fit in a robust, automated manner to large QM data sets using many bispectrum components. The calculation of the bispectrum components and the SNAP potential are implemented in the LAMMPS parallel molecular dynamics code. We demonstrate that a previously unnoticed symmetry property can be exploited to reduce the computational cost of the force calculations by more than one order of magnitude. We present results for a SNAP potential for tantalum, showing that it accurately reproduces a range of commonly calculated properties of both the crystalline solid and the liquid phases. In addition, unlike simpler existing potentials, SNAP correctly predicts the energy barrier for screw dislocation migration in BCC tantalum.« less

Spectral neighbor analysis method for automated generation of quantum-accurate interatomic potentials

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

Thompson, A.P., E-mail: athomps@sandia.gov; Swiler, L.P., E-mail: lpswile@sandia.gov; Trott, C.R., E-mail: crtrott@sandia.gov

2015-03-15

We present a new interatomic potential for solids and liquids called Spectral Neighbor Analysis Potential (SNAP). The SNAP potential has a very general form and uses machine-learning techniques to reproduce the energies, forces, and stress tensors of a large set of small configurations of atoms, which are obtained using high-accuracy quantum electronic structure (QM) calculations. The local environment of each atom is characterized by a set of bispectrum components of the local neighbor density projected onto a basis of hyperspherical harmonics in four dimensions. The bispectrum components are the same bond-orientational order parameters employed by the GAP potential [1]. Themore » SNAP potential, unlike GAP, assumes a linear relationship between atom energy and bispectrum components. The linear SNAP coefficients are determined using weighted least-squares linear regression against the full QM training set. This allows the SNAP potential to be fit in a robust, automated manner to large QM data sets using many bispectrum components. The calculation of the bispectrum components and the SNAP potential are implemented in the LAMMPS parallel molecular dynamics code. We demonstrate that a previously unnoticed symmetry property can be exploited to reduce the computational cost of the force calculations by more than one order of magnitude. We present results for a SNAP potential for tantalum, showing that it accurately reproduces a range of commonly calculated properties of both the crystalline solid and the liquid phases. In addition, unlike simpler existing potentials, SNAP correctly predicts the energy barrier for screw dislocation migration in BCC tantalum.« less

Fast trace determination of nine odorant and estrogenic chloro- and bromo-phenolic compounds in real water samples through automated solid-phase extraction coupled with liquid chromatography tandem mass spectrometry.

PubMed

Yuan, Su-Fen; Liu, Ze-Hua; Lian, Hai-Xian; Yang, Chuang-Tao; Lin, Qing; Yin, Hua; Lin, Zhang; Dang, Zhi

2018-02-01

A fast and reliable method was developed for simultaneous trace determination of nine odorous and estrogenic chloro- and bromo-phenolic compounds (CPs and BPs) in water samples using solid-phase extraction (SPE) coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS). For sample preparation, the extraction efficiencies of two widely applied cartridges Oasis HLB and Sep-Pak C18 were compared, and the Oasis HLB cartridge showed much better extraction performance; pH of water sample also plays important role on extraction, and pH = 2-3 was found to be most appropriate. For separation of the target compounds, small addition of ammonium hydroxide can obviously improve the detection sensitivity, and the optimized addition concentration was determined as 0.2%. The developed efficient method was validated and showed excellent linearity (R 2  > 0.995), low limit of detection (LOD, 1.9-6.2 ng/L), and good recovery efficiencies of 57-95% in surface and tap water with low relative standard deviation (RSD, 1.3-17.4%). The developed method was finally applied to one tap and one surface water samples and most of these nine targets were detected, but all of them were below their odor thresholds, and their estrogen equivalent (EEQ) were also very low.

Solid-phase extraction and GC-MS analysis of THC-COOH method optimized for a high-throughput forensic drug-testing laboratory.

PubMed

Stout, P R; Horn, C K; Klette, K L

2001-10-01

In order to facilitate the confirmation analysis of large numbers of urine samples previously screened positive for delta9-tetrahydrocannabinol (THC), an extraction, derivitization, and GC-MS analysis method was developed. This method utilized a positive pressure manifold anion-exchange polymer-based solid-phase extraction followed by elution directly into the automated liquid sampling (ALS) vials. Rapid derivitization was accomplished using pentafluoropropionic anhydride/pentafluoropropanol (PFPA/PFPOH). Recoveries averaged 95% with a limit of detection of 0.875 ng/mL with a 3-mL sample volume. Performance of 11-nor-delta9-tetrahydrocannabinol-9-carboxylic acid (THC-COOH)-d3 and THC-COOH-d9 internal standards were evaluated. The method was linear to 900 ng/mL THC-COOH using THC-COOH-d9 with negligible contribution from the internal standard to very weak samples. Excellent agreement was seen with previous quantitations of human urine samples. More than 1000 human urine samples were analyzed using the method with 300 samples analyzed using an alternate qualifier ion (m/z 622) after some interference was observed with a qualifier ion (m/z 489). The 622 ion did not exhibit any interference even in samples with interfering peaks present in the 489 ion. The method resulted in dramatic reductions in processing time, waste production, and exposure hazards to laboratory personnel.

Rotating Rod Renewable Microcolumns for Automated, Solid-Phase DNA Hybridization

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

Bruckner-Lea, Cynthia J.; Stottlemyre, Mark R.; Holman, David A.

1999-12-01

The development of a new temperature-controlled renewable microcolumn flow cell for solid-phase nucleic acid analysis in a sequential injection system is described. The flow cell includes a stepper motor-driven rotating rod with the working end cut to a 45 degree angle. In one position, the end of the rod prevents passage of microbeads while allowing fluid flow; rotation of the rod by 180 degrees release the beads. This system was used to rapidly test many hybridization and elution protocols to examine the temperature and solution conditions required for sequence specific nucleic acid hybridization. Target nucleic acids labeled with a near-infraredmore » fluorescent dye were detected immediately post-column using a flow-through fluorescence detector, with a detection limit of 40 pM dye concentration at a flow rate of 5 mu l/s. Temperature control of the column and the presence of Triton X-100 surfactant were critical for specific hybridization. Perfusion of the column with complementary oligonucleotide (200 mu l, 10nM) resulted in hybridization with 8% of the DNA binding sites on the microbeads with a solution residence time of less than a second and a total sample perfusion time of 40 seconds. The use of the renewable column system for detection of an unlabeled PCR product in a sandwich assay was also demonstrated.« less

On-line solid phase extraction coupled to capillary LC-ESI-MS for determination of fluoxetine in human blood plasma.

PubMed

Saber, Amr L

2009-04-15

An instrumental setup including on-line solid phased extraction coupled to capillary liquid chromatography-electrospray ionization-mass spectrometry (SPE-capLC-ESI-MS) has been constructed to improve the sensitivity for quantification of fluoxetine hydrochloride in human plasma. Prior to injection, 0.5 mL of plasma spiked with metronidazole (internal standard) was mixed with ammonium formate buffer for effective chloroform liquid-liquid extraction. The method was validated in the range 5-60 ng mL(-1) fluoxetine, yielding a correlation coefficient of 0.999 (r(2)). The within-assay and between-assay precisions were between (8.5 and 11%) and (6.6 and 7.5%), respectively. The method was used to determine the amount of fluoxetine in a healthy male 14 h after an intake of one capsule of the antidepressant and anorectic Flutin, which contains 20mg fluoxetine per each capsule. Fluoxetine was detected, and the concentration was calculated to 9.0 ng mL(-1) plasma. In the preliminary experiments, conventional LC-UV instrumentation was employed. However, it was found that employing a capillary column with an inner diameter of (0.3mm I.D. x 50 mm, Zorbax C(18)) increased the sensitivity by a factor of approximately 100, when injecting the same mass of analyte. Incorporating an easily automated C(18) reversed phase column switching system with SPE (1.0mm I.D. x 5.0mm, 5 microm) made it possible to inject up to 100 microL of solution, and the total analysis time was 5.5 min.

Multi-step high-throughput conjugation platform for the development of antibody-drug conjugates.

PubMed

Andris, Sebastian; Wendeler, Michaela; Wang, Xiangyang; Hubbuch, Jürgen

2018-07-20

Antibody-drug conjugates (ADCs) form a rapidly growing class of biopharmaceuticals which attracts a lot of attention throughout the industry due to its high potential for cancer therapy. They combine the specificity of a monoclonal antibody (mAb) and the cell-killing capacity of highly cytotoxic small molecule drugs. Site-specific conjugation approaches involve a multi-step process for covalent linkage of antibody and drug via a linker. Despite the range of parameters that have to be investigated, high-throughput methods are scarcely used so far in ADC development. In this work an automated high-throughput platform for a site-specific multi-step conjugation process on a liquid-handling station is presented by use of a model conjugation system. A high-throughput solid-phase buffer exchange was successfully incorporated for reagent removal by utilization of a batch cation exchange step. To ensure accurate screening of conjugation parameters, an intermediate UV/Vis-based concentration determination was established including feedback to the process. For conjugate characterization, a high-throughput compatible reversed-phase chromatography method with a runtime of 7 min and no sample preparation was developed. Two case studies illustrate the efficient use for mapping the operating space of a conjugation process. Due to the degree of automation and parallelization, the platform is capable of significantly reducing process development efforts and material demands and shorten development timelines for antibody-drug conjugates. Copyright © 2018 Elsevier B.V. All rights reserved.

Prime Contract Awards Alphabetically by Contractor, State or Country, and Place. Part 18 (University of Virginia, Carsonville, Virginia - Zymark Corporation, Hopkinton, Massachusetts), FY1991

DTIC Science & Technology

1991-01-01

C 44 ) C4 04 444)c_ _) I LC.) InflQAQ -4 < -4 -4< a 4 c - I 0)-CI I~ 000 10) 1" W .) 0 0007 10 10 LA LAY) LADO I I aH0 HO cc.4-4r 0 n r -I0 07 nc oq 0...4 (D C) -. C-4 0 IN -, r) IN N4 I3U to 04 a c( 0v o00 E co o CL0 to0 Or. Mb" be - -0) -oIn 3 1 0 3 1.W4 00 LC L.N 1C,) ENc >-0 I-N 0.0 L 6--4 L...4N E c’ m.40704mmo7 41,07 00C 0)07 -4 W07 ENC 0 If w4 6 04 66 AS0) .=07 00o momI-4-.c) 00) 4--4.-4 -40 0(D al 064 - XN0 0)1 C6 8 I CO. H:30 00 U-4

Composition and automated crystal orientation mapping of rapid solidification products in hypoeutectic Al-4 at.%Cu alloys

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

Zweiacker, K. W.; Liu, Can; Gordillo, M. A.

Rmore » apid solidification can produce metastable phases and unusual microstructure modifications in multi-component alloys during additive manufacturing or laser beam welding. Composition and phase mapping by transmission electron microscopy have been used in this paper to characterize the morphologically distinct zones developing in hypoeutectic Al-4 at.% Cu alloy after pulsed laser melting for different crystal growth rate regimes. Deviations of the compositions of the alloy phases from equilibrium predictions and unique orientation relationships between the solidification transformation products have been determined. Specifically, for the columnar growth zone at solidification rates of 0.8 m s - 1 < v < v a = 1.8 m s - 1 , two distinct orientation relationships were established between the concomitantly forming non-equilibrium phases, supersaturated α-Al solid solution and the discontinuously distributed α-Al 2Cu-based θ'-phase, which can be described as {110} θ ∥ {001} α, [001] θ ∥ [110] α and {001} θ ∥ {001} α, [100] θ ∥ [100] α. These orientation relationships permit formation of coherent interphase interfaces with low interfacial free energy. Finally, this endows a kinetic advantage to the thermodynamically less stable θ'-Al 2Cu phase relative to the more stable equilibrium θ-Al 2Cu phase during formation of the morphologically modified eutectic of the columnar growth zone grains, since repeated nucleation is required to establish the discontinuous distribution of θ'-Al 2Cu phase.« less

Composition and automated crystal orientation mapping of rapid solidification products in hypoeutectic Al-4 at.%Cu alloys

DOE PAGES

Zweiacker, K. W.; Liu, Can; Gordillo, M. A.; ...

2017-12-05

Rmore » apid solidification can produce metastable phases and unusual microstructure modifications in multi-component alloys during additive manufacturing or laser beam welding. Composition and phase mapping by transmission electron microscopy have been used in this paper to characterize the morphologically distinct zones developing in hypoeutectic Al-4 at.% Cu alloy after pulsed laser melting for different crystal growth rate regimes. Deviations of the compositions of the alloy phases from equilibrium predictions and unique orientation relationships between the solidification transformation products have been determined. Specifically, for the columnar growth zone at solidification rates of 0.8 m s - 1 < v < v a = 1.8 m s - 1 , two distinct orientation relationships were established between the concomitantly forming non-equilibrium phases, supersaturated α-Al solid solution and the discontinuously distributed α-Al 2Cu-based θ'-phase, which can be described as {110} θ ∥ {001} α, [001] θ ∥ [110] α and {001} θ ∥ {001} α, [100] θ ∥ [100] α. These orientation relationships permit formation of coherent interphase interfaces with low interfacial free energy. Finally, this endows a kinetic advantage to the thermodynamically less stable θ'-Al 2Cu phase relative to the more stable equilibrium θ-Al 2Cu phase during formation of the morphologically modified eutectic of the columnar growth zone grains, since repeated nucleation is required to establish the discontinuous distribution of θ'-Al 2Cu phase.« less

Nucleic acid detection methods

DOEpatents

Smith, C.L.; Yaar, R.; Szafranski, P.; Cantor, C.R.

1998-05-19

The invention relates to methods for rapidly determining the sequence and/or length a target sequence. The target sequence may be a series of known or unknown repeat sequences which are hybridized to an array of probes. The hybridized array is digested with a single-strand nuclease and free 3{prime}-hydroxyl groups extended with a nucleic acid polymerase. Nuclease cleaved heteroduplexes can be easily distinguish from nuclease uncleaved heteroduplexes by differential labeling. Probes and target can be differentially labeled with detectable labels. Matched target can be detected by cleaving resulting loops from the hybridized target and creating free 3-hydroxyl groups. These groups are recognized and extended by polymerases added into the reaction system which also adds or releases one label into solution. Analysis of the resulting products using either solid phase or solution. These methods can be used to detect characteristic nucleic acid sequences, to determine target sequence and to screen for genetic defects and disorders. Assays can be conducted on solid surfaces allowing for multiple reactions to be conducted in parallel and, if desired, automated. 18 figs.

Computer-controlled high-resolution capacitance dilatometer/oven system: Design, instrumentation, and performance

NASA Astrophysics Data System (ADS)

Johansen, T. H.; Feder, J.; Jøssang, T.

1986-06-01

A fully automated apparatus has been designed for measurements of dilatation in solid samples under well-defined thermal conditions. The oven can be thermally stabilized to better than 0.1 mK over a temperature range of -60 to 150 °C using a two-stage control strategy. Coarse control is obtained by heat exchange with a circulating thermal fluid, whereas the fine regulation is based on a solid-state heat pump—a Peltier element, acting as heating and cooling source. The bidirectional action of the Peltier element permits the sample block to be controlled at the average temperature of the surroundings, thus making an essentially adiabatic system with a minimum of thermal gradients in the sample block. The dilatometer cell integrated in the oven assembly is of the parallel plate air capacitor type, and the apparatus has been successfully used with a sensitivity of 0.07 Å. Our system is well suited for measurements near structural phase transitions with a relative resolution of Δt=(T-Tc)/Tc=2×10-7 in temperature and ΔL/L=1×10-9 in strain.

40 CFR 227.32 - Liquid, suspended particulate, and solid phases of a material.

Code of Federal Regulations, 2010 CFR

2010-07-01

... solid phases of a material. 227.32 Section 227.32 Protection of Environment ENVIRONMENTAL PROTECTION... MATERIALS Definitions § 227.32 Liquid, suspended particulate, and solid phases of a material. (a) For the... obtained above prior to centrifugation and filtration. The solid phase includes all material settling to...

40 CFR 227.32 - Liquid, suspended particulate, and solid phases of a material.

Code of Federal Regulations, 2011 CFR

2011-07-01

... solid phases of a material. 227.32 Section 227.32 Protection of Environment ENVIRONMENTAL PROTECTION... MATERIALS Definitions § 227.32 Liquid, suspended particulate, and solid phases of a material. (a) For the... obtained above prior to centrifugation and filtration. The solid phase includes all material settling to...

Crystallographic analysis of the solid-state dewetting of polycrystalline gold film using automated indexing in a transmission electron microscope

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

Jang, S. A.; Lee, H. J.; Oh, Y. J., E-mail: yjoh@hanbat.ac.kr

We analyzed the effect of crystallographic anisotropy on the morphological evolution of a 12-nm-thick gold film during solid-state dewetting at high temperatures using automated indexing tool in a transmission electron microscopy. Dewetting initiated at grain-boundary triple junctions adjacent to large grains resulting from abnormal grain growth driven by (111) texture development. Voids at the junctions developed shapes with faceted edges bounded by low-index crystal planes. The kinetic mobility of the edges varied with the crystal orientation normal to the edges, with a predominance of specific edges with the slowest retraction rates as the annealing time was increased.

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

NASA Astrophysics Data System (ADS)

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.

Automation of the Environmental Control and Life Support System

NASA Technical Reports Server (NTRS)

Dewberry, Brandon S.; Carnes, J. Ray

1990-01-01

The objective of the Environmental Control and Life Support System (ECLSS) Advanced Automation Project is to recommend and develop advanced software for the initial and evolutionary Space Station Freedom (SSF) ECLS system which will minimize the crew and ground manpower needed for operations. Another objective includes capturing ECLSS design and development knowledge for future missions. This report summarizes our results from Phase I, the ECLSS domain analysis phase, which we broke down into three steps: 1) Analyze and document the baselined ECLS system, 2) envision as our goal an evolution to a fully automated regenerative life support system, built upon an augmented baseline, and 3) document the augmentations (hooks and scars) and advanced software systems which we see as necessary in achieving minimal manpower support for ECLSS operations. In addition, Phase I included development of an advanced software life cycle testing tools will be used in the development of the software. In this way, we plan in preparation for phase II and III, the development and integration phases, respectively. Automated knowledge acquisition, engineering, verification, and can capture ECLSS development knowledge for future use, develop more robust and complex software, provide feedback to the KBS tool community, and insure proper visibility of our efforts.

A Case Study of Reverse Engineering Integrated in an Automated Design Process

NASA Astrophysics Data System (ADS)

Pescaru, R.; Kyratsis, P.; Oancea, G.

2016-11-01

This paper presents a design methodology which automates the generation of curves extracted from the point clouds that have been obtained by digitizing the physical objects. The methodology is described on a product belonging to the industry of consumables, respectively a footwear type product that has a complex shape with many curves. The final result is the automated generation of wrapping curves, surfaces and solids according to the characteristics of the customer's foot, and to the preferences for the chosen model, which leads to the development of customized products.

Quantitative determination of opioids in whole blood using fully automated dried blood spot desorption coupled to on-line SPE-LC-MS/MS.

PubMed

Verplaetse, Ruth; Henion, Jack

2016-01-01

Opioids are well known, widely used painkillers. Increased stability of opioids in the dried blood spot (DBS) matrix compared to blood/plasma has been described. Other benefits provided by DBS techniques include point-of-care collection, less invasive micro sampling, more economical shipment, and convenient storage. Current methodology for analysis of micro whole blood samples for opioids is limited to the classical DBS workflow, including tedious manual punching of the DBS cards followed by extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS) bioanalysis. The goal of this study was to develop and validate a fully automated on-line sample preparation procedure for the analysis of DBS micro samples relevant to the detection of opioids in finger prick blood. To this end, automated flow-through elution of DBS cards was followed by on-line solid-phase extraction (SPE) and analysis by LC-MS/MS. Selective, sensitive, accurate, and reproducible quantitation of five representative opioids in human blood at sub-therapeutic, therapeutic, and toxic levels was achieved. The range of reliable response (R(2)  ≥0.997) was 1 to 500 ng/mL whole blood for morphine, codeine, oxycodone, hydrocodone; and 0.1 to 50 ng/mL for fentanyl. Inter-day, intra-day, and matrix inter-lot accuracy and precision was less than 15% (even at lower limits of quantitation (LLOQ) level). The method was successfully used to measure hydrocodone and its major metabolite norhydrocodone in incurred human samples. Our data support the enormous potential of DBS sampling and automated analysis for monitoring opioids as well as other pharmaceuticals in both anti-doping and pain management regimens. Copyright © 2015 John Wiley & Sons, Ltd.

Synthesis of oligonucleotides on a soluble support

PubMed Central

2017-01-01

Oligonucleotides are usually prepared in lab scale on a solid support with the aid of a fully automated synthesizer. Scaling up of the equipment has allowed industrial synthesis up to kilogram scale. In spite of this, solution-phase synthesis has received continuous interest, on one hand as a technique that could enable synthesis of even larger amounts and, on the other hand, as a gram scale laboratory synthesis without any special equipment. The synthesis on a soluble support has been regarded as an approach that could combine the advantageous features of both the solution and solid-phase syntheses. The critical step of this approach is the separation of the support-anchored oligonucleotide chain from the monomeric building block and other small molecular reagents and byproducts after each coupling, oxidation and deprotection step. The techniques applied so far include precipitation, extraction, chromatography and nanofiltration. As regards coupling, all conventional chemistries, viz. phosphoramidite, H-phosphonate and phosphotriester strategies, have been attempted. While P(III)-based phosphoramidite and H-phosphonate chemistries are almost exclusively used on a solid support, the “outdated” P(V)-based phosphotriester chemistry still offers one major advantage for the synthesis on a soluble support; the omission of the oxidation step simplifies the coupling cycle. Several of protocols developed for the soluble-supported synthesis allow the preparation of both DNA and RNA oligomers of limited length in gram scale without any special equipment, being evidently of interest for research groups that need oligonucleotides in large amounts for research purposes. However, none of them has really tested at such a scale that the feasibility of their industrial use could be critically judged. PMID:28781703

Formally verifying human–automation interaction as part of a system model: limitations and tradeoffs

PubMed Central

Bass, Ellen J.

2011-01-01

Both the human factors engineering (HFE) and formal methods communities are concerned with improving the design of safety-critical systems. This work discusses a modeling effort that leveraged methods from both fields to perform formal verification of human–automation interaction with a programmable device. This effort utilizes a system architecture composed of independent models of the human mission, human task behavior, human-device interface, device automation, and operational environment. The goals of this architecture were to allow HFE practitioners to perform formal verifications of realistic systems that depend on human–automation interaction in a reasonable amount of time using representative models, intuitive modeling constructs, and decoupled models of system components that could be easily changed to support multiple analyses. This framework was instantiated using a patient controlled analgesia pump in a two phased process where models in each phase were verified using a common set of specifications. The first phase focused on the mission, human-device interface, and device automation; and included a simple, unconstrained human task behavior model. The second phase replaced the unconstrained task model with one representing normative pump programming behavior. Because models produced in the first phase were too large for the model checker to verify, a number of model revisions were undertaken that affected the goals of the effort. While the use of human task behavior models in the second phase helped mitigate model complexity, verification time increased. Additional modeling tools and technological developments are necessary for model checking to become a more usable technique for HFE. PMID:21572930

Best-Quality Vessel Identification Using Vessel Quality Measure in Multiple-Phase Coronary CT Angiography.

PubMed

Hadjiiski, Lubomir; Liu, Jordan; Chan, Heang-Ping; Zhou, Chuan; Wei, Jun; Chughtai, Aamer; Kuriakose, Jean; Agarwal, Prachi; Kazerooni, Ella

2016-01-01

The detection of stenotic plaques strongly depends on the quality of the coronary arterial tree imaged with coronary CT angiography (cCTA). However, it is time consuming for the radiologist to select the best-quality vessels from the multiple-phase cCTA for interpretation in clinical practice. We are developing an automated method for selection of the best-quality vessels from coronary arterial trees in multiple-phase cCTA to facilitate radiologist's reading or computerized analysis. Our automated method consists of vessel segmentation, vessel registration, corresponding vessel branch matching, vessel quality measure (VQM) estimation, and automatic selection of best branches based on VQM. For every branch, the VQM was calculated as the average radial gradient. An observer preference study was conducted to visually compare the quality of the selected vessels. 167 corresponding branch pairs were evaluated by two radiologists. The agreement between the first radiologist and the automated selection was 76% with kappa of 0.49. The agreement between the second radiologist and the automated selection was also 76% with kappa of 0.45. The agreement between the two radiologists was 81% with kappa of 0.57. The observer preference study demonstrated the feasibility of the proposed automated method for the selection of the best-quality vessels from multiple cCTA phases.

Rapid Automated Sample Preparation for Biological Assays

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

Shusteff, M

Our technology utilizes acoustic, thermal, and electric fields to separate out contaminants such as debris or pollen from environmental samples, lyse open cells, and extract the DNA from the lysate. The objective of the project is to optimize the system described for a forensic sample, and demonstrate its performance for integration with downstream assay platforms (e.g. MIT-LL's ANDE). We intend to increase the quantity of DNA recovered from the sample beyond the current {approx}80% achieved using solid phase extraction methods. Task 1: Develop and test an acoustic filter for cell extraction. Task 2: Develop and test lysis chip. Task 3:more » Develop and test DNA extraction chip. All chips have been fabricated based on the designs laid out in last month's report.« less

Simulation and Automation of Microwave Frequency Control in Dynamic Nuclear Polarization for Solid Polarized Targets

NASA Astrophysics Data System (ADS)

Perera, Gonaduwage; Johnson, Ian; Keller, Dustin

2017-09-01

Dynamic Nuclear Polarization (DNP) is used in most of the solid polarized target scattering experiments. Those target materials must be irradiated using microwaves at a frequency determined by the difference in the nuclear Larmor and electron paramagnetic resonance (EPR) frequencies. But the resonance frequency changes with time as a result of radiation damage. Hence the microwave frequency should be adjusted accordingly. Manually adjusting the frequency can be difficult, and improper adjustments negatively impact the polarization. In order to overcome these difficulties, two controllers were developed which automate the process of seeking and maintaining the optimal frequency: one being a standalone controller for a traditional DC motor and the other a LabVIEW VI for a stepper motor configuration. Further a Monte-Carlo simulation was developed which can accurately model the polarization over time as a function of microwave frequency. In this talk, analysis of the simulated data and recent improvements to the automated system will be presented. DOE.

Confocal nanoscanning, bead picking (CONA): PickoScreen microscopes for automated and quantitative screening of one-bead one-compound libraries.

PubMed

Hintersteiner, Martin; Buehler, Christof; Uhl, Volker; Schmied, Mario; Müller, Jürgen; Kottig, Karsten; Auer, Manfred

2009-01-01

Solid phase combinatorial chemistry provides fast and cost-effective access to large bead based libraries with compound numbers easily exceeding tens of thousands of compounds. Incubating one-bead one-compound library beads with fluorescently labeled target proteins and identifying and isolating the beads which contain a bound target protein, potentially represents one of the most powerful generic primary high throughput screening formats. On-bead screening (OBS) based on this detection principle can be carried out with limited automation. Often hit bead detection, i.e. recognizing beads with a fluorescently labeled protein bound to the compound on the bead, relies on eye-inspection under a wide-field microscope. Using low resolution detection techniques, the identification of hit beads and their ranking is limited by a low fluorescence signal intensity and varying levels of the library beads' autofluorescence. To exploit the full potential of an OBS process, reliable methods for both automated quantitative detection of hit beads and their subsequent isolation are needed. In a joint collaborative effort with Evotec Technologies (now Perkin-Elmer Cellular Technologies Germany GmbH), we have built two confocal bead scanner and picker platforms PS02 and a high-speed variant PS04 dedicated to automated high resolution OBS. The PS0X instruments combine fully automated confocal large area scanning of a bead monolayer at the bottom of standard MTP plates with semiautomated isolation of individual hit beads via hydraulic-driven picker capillaries. The quantification of fluorescence intensities with high spatial resolution in the equatorial plane of each bead allows for a reliable discrimination between entirely bright autofluorescent beads and real hit beads which exhibit an increased fluorescence signal at the outer few micrometers of the bead. The achieved screening speed of up to 200,000 bead assayed in less than 7 h and the picking time of approximately 1 bead/min allow exploitation of one-bead one-compound libraries with high sensitivity, accuracy, and speed.

AAAS: Automated Affirmative Action System. General Description, Phase 1.

ERIC Educational Resources Information Center

Institute for Services to Education, Inc., Washington, DC. TACTICS Management Information Systems Directorate.

This document describes phase 1 of the Automated Affirmative Action System (AAAS) of the Tuskegee Institute, which was designed to organize an inventory of any patterns of job classification and assignment identifiable by sex or minority group; any job classification or organizational unit where women and minorities are not employed or are…

Robot graphic simulation testbed

NASA Technical Reports Server (NTRS)

Cook, George E.; Sztipanovits, Janos; Biegl, Csaba; Karsai, Gabor; Springfield, James F.

1991-01-01

The objective of this research was twofold. First, the basic capabilities of ROBOSIM (graphical simulation system) were improved and extended by taking advantage of advanced graphic workstation technology and artificial intelligence programming techniques. Second, the scope of the graphic simulation testbed was extended to include general problems of Space Station automation. Hardware support for 3-D graphics and high processing performance make high resolution solid modeling, collision detection, and simulation of structural dynamics computationally feasible. The Space Station is a complex system with many interacting subsystems. Design and testing of automation concepts demand modeling of the affected processes, their interactions, and that of the proposed control systems. The automation testbed was designed to facilitate studies in Space Station automation concepts.

Seasonal multiphase equilibria in the atmospheres of Titan and Pluto

NASA Astrophysics Data System (ADS)

Tan, S. P.; Kargel, J. S.

2017-12-01

At the extremely low temperatures in Titan's upper troposphere and on Pluto's surface, the atmospheres as a whole are subject to freeze into solid solutions, not pure ices. The presence of the solid phases introduces conditions with rich phase equilibria upon seasonal changes, even if the temperature undergoes only small changes. For the first time, the profile of atmospheric methane in Titan's troposphere will be reproduced complete with the solid solutions. This means that the freezing point, i.e. the altitude where the first solid phase appears, is determined. The seasonal change will also be evaluated both at the equator and the northern polar region. For Pluto, also for the first time, the seasonal solid-vapor equilibria will be evaluated. The fate of the two solid phases, the methane-rich and carbon-monoxide-rich solid solutions, will be analyzed upon temperature and pressure changes. Such investigations are enabled by the development of a molecular-based thermodynamic model for cryogenic chemical systems, referred to as CRYOCHEM, which includes solid solutions in its phase-equilibria calculations. The atmospheres of Titan and Pluto are modeled as ternary gas mixtures: nitrogen-methane-ethane and nitrogen-methane-carbon monoxide, respectively. Calculations using CRYOCHEM can provide us with compositions not only in two-phase equilibria, but also that in three-phase equilibria. Densities of all phases involved will also be calculated. For Titan, density inversion between liquid and solid phases will be identified and presented. In the inversion, the density of solid phase is less than that in the liquid phase. The method and results of this work will be useful for further investigations and modeling on the atmospheres of Titan, Pluto, and other bodies with similar conditions in the Solar System and beyond.

Automated method for simultaneous lead and strontium isotopic analysis applied to rainwater samples and airborne particulate filters (PM10).

PubMed

Beltrán, Blanca; Avivar, Jessica; Mola, Montserrat; Ferrer, Laura; Cerdà, Víctor; Leal, Luz O

2013-09-03

A new automated, sensitive, and fast system for the simultaneous online isolation and preconcentration of lead and strontium by sorption on a microcolumn packed with Sr-resin using an inductively coupled plasma mass spectrometry (ICP-MS) detector was developed, hyphenating lab-on-valve (LOV) and multisyringe flow injection analysis (MSFIA). Pb and Sr are directly retained on the sorbent column and eluted with a solution of 0.05 mol L(-1) ammonium oxalate. The detection limits achieved were 0.04 ng for lead and 0.03 ng for strontium. Mass calibration curves were used since the proposed system allows the use of different sample volumes for preconcentration. Mass linear working ranges were between 0.13 and 50 ng and 0.1 and 50 ng for lead and strontium, respectively. The repeatability of the method, expressed as RSD, was 2.1% and 2.7% for Pb and Sr, respectively. Environmental samples such as rainwater and airborne particulate (PM10) filters as well as a certified reference material SLRS-4 (river water) were satisfactorily analyzed obtaining recoveries between 90 and 110% for both elements. The main features of the LOV-MSFIA-ICP-MS system proposed are the capability to renew solid phase extraction at will in a fully automated way, the remarkable stability of the column which can be reused up to 160 times, and the potential to perform isotopic analysis.

Advances in the simulation and automated measurement of well-sorted granular material: 1. Simulation

USGS Publications Warehouse

Daniel Buscombe,; Rubin, David M.

2012-01-01

1. In this, the first of a pair of papers which address the simulation and automated measurement of well-sorted natural granular material, a method is presented for simulation of two-phase (solid, void) assemblages of discrete non-cohesive particles. The purpose is to have a flexible, yet computationally and theoretically simple, suite of tools with well constrained and well known statistical properties, in order to simulate realistic granular material as a discrete element model with realistic size and shape distributions, for a variety of purposes. The stochastic modeling framework is based on three-dimensional tessellations with variable degrees of order in particle-packing arrangement. Examples of sediments with a variety of particle size distributions and spatial variability in grain size are presented. The relationship between particle shape and porosity conforms to published data. The immediate application is testing new algorithms for automated measurements of particle properties (mean and standard deviation of particle sizes, and apparent porosity) from images of natural sediment, as detailed in the second of this pair of papers. The model could also prove useful for simulating specific depositional structures found in natural sediments, the result of physical alterations to packing and grain fabric, using discrete particle flow models. While the principal focus here is on naturally occurring sediment and sedimentary rock, the methods presented might also be useful for simulations of similar granular or cellular material encountered in engineering, industrial and life sciences.

Automated production of [18 F]FTHA according to GMP.

PubMed

Savisto, Nina; Viljanen, Tapio; Kokkomäki, Esa; Bergman, Jörgen; Solin, Olof

2018-02-01

14-(R,S)-[ 18 F]fluoro-6-thia-heptadecanoic acid is a tracer for fatty acid imaging by positron emission tomography. High demand for this tracer required us to replace semiautomatic synthesis with a fully automated procedure. An automated synthesis device was constructed in-house for multistep nucleophilic 18 F-fluorination and a control system was developed. The synthesis device was combined with a sterile filtration unit and both were qualified. 14-(R,S)-[ 18 F]fluoro-6-thia-heptadecanoic acid was produced according to good manufacturing practice guidelines set by the European Union. The synthesis includes an initial nucleophilic labelling reaction, deprotection, preparative HPLC separation, purification of the final product, and formulation for injection. The duration and temperature of the reaction and hydrolysis were optimized, and the radiochemical stability of the formulated product was determined. The rotary evaporator used to evaporate the solvent after HPLC purification was replaced with solid phase extraction purification. We also replaced the human serum albumin used in the earlier procedure with a phosphate buffer-ascorbic acid mixture in the final formulation solution. From 2011 to 2016, we performed 219 synthesis procedures, 94% of which were successful. The radiochemical yield of 14-(R,S)-[ 18 F]fluoro-6-thia-heptadecanoic acid, decay-corrected to the end of bombardment, was 13% ± 6.3%. The total amount of formulated end product was 1.7 ± 0.8 GBq at end of synthesis. Copyright © 2017 John Wiley & Sons, Ltd.

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

NASA Astrophysics Data System (ADS)

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.

Preliminary Framework for Human-Automation Collaboration

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

Oxstrand, Johanna Helene; Le Blanc, Katya Lee; Spielman, Zachary Alexander

The Department of Energy’s Advanced Reactor Technologies Program sponsors research, development and deployment activities through its Next Generation Nuclear Plant, Advanced Reactor Concepts, and Advanced Small Modular Reactor (aSMR) Programs to promote safety, technical, economical, and environmental advancements of innovative Generation IV nuclear energy technologies. The Human Automation Collaboration (HAC) Research Project is located under the aSMR Program, which identifies developing advanced instrumentation and controls and human-machine interfaces as one of four key research areas. It is expected that the new nuclear power plant designs will employ technology significantly more advanced than the analog systems in the existing reactor fleetmore » as well as utilizing automation to a greater extent. Moving towards more advanced technology and more automation does not necessary imply more efficient and safer operation of the plant. Instead, a number of concerns about how these technologies will affect human performance and the overall safety of the plant need to be addressed. More specifically, it is important to investigate how the operator and the automation work as a team to ensure effective and safe plant operation, also known as the human-automation collaboration (HAC). The focus of the HAC research is to understand how various characteristics of automation (such as its reliability, processes, and modes) effect an operator’s use and awareness of plant conditions. In other words, the research team investigates how to best design the collaboration between the operators and the automated systems in a manner that has the greatest positive impact on overall plant performance and reliability. This report addresses the Department of Energy milestone M4AT-15IN2302054, Complete Preliminary Framework for Human-Automation Collaboration, by discussing the two phased development of a preliminary HAC framework. The framework developed in the first phase was used as the basis for selecting topics to be investigated in more detail. The results and insights gained from the in-depth studies conducted during the second phase were used to revise the framework. This report describes the basis for the framework developed in phase 1, the changes made to the framework in phase 2, and the basis for the changes. Additional research needs are identified and presented in the last section of the report.« less

Automated solar panel assembly line

NASA Technical Reports Server (NTRS)

Somberg, H.

1981-01-01

The initial stage of the automated solar panel assembly line program was devoted to concept development and proof of approach through simple experimental verification. In this phase, laboratory bench models were built to demonstrate and verify concepts. Following this phase was machine design and integration of the various machine elements. The third phase was machine assembly and debugging. In this phase, the various elements were operated as a unit and modifications were made as required. The final stage of development was the demonstration of the equipment in a pilot production operation.

Methods for the preparation and analysis of solids and suspended solids for total mercury

USGS Publications Warehouse

Olund, Shane D.; DeWild, John F.; Olson, Mark L.; Tate, Michael T.

2004-01-01

The methods documented in this report are utilized by the Wisconsin District Mercury Lab for analysis of total mercury in solids (soils and sediments) and suspended solids (isolated on filters). Separate procedures are required for the different sample types. For solids, samples are prepared by room-temperature acid digestion and oxidation with aqua regia. The samples are brought up to volume with a 5 percent bromine monochloride solution to ensure complete oxidation and heated at 50?C in an oven overnight. Samples are then analyzed with an automated flow injection system incorporating a cold vapor atomic fluorescence spectrometer. A method detection limit of 0.3 ng of mercury per digestion bomb was established using multiple analyses of an environmental sample. Based on the range of masses processed, the minimum sample reporting limit varies from 0.6 ng/g to 6 ng/g. Suspended solids samples are oxidized with a 5 percent bromine monochloride solution and held at 50?C in an oven for 5 days. The samples are then analyzed with an automated flow injection system incorporating a cold vapor atomic fluorescence spectrometer. Using a certified reference material as a surrogate for an environmental sample, a method detection limit of 0.059 ng of mercury per filter was established. The minimum sample reporting limit varies from 0.059 ng/L to 1.18 ng/L, depending on the volume of water filtered.

Benzocaine polymorphism: pressure-temperature phase diagram involving forms II and III.

PubMed

Gana, Inès; Barrio, Maria; Do, Bernard; Tamarit, Josep-Lluís; Céolin, René; Rietveld, Ivo B

2013-11-18

Understanding the phase behavior of an active pharmaceutical ingredient in a drug formulation is required to avoid the occurrence of sudden phase changes resulting in decrease of bioavailability in a marketed product. Benzocaine is known to possess three crystalline polymorphs, but their stability hierarchy has so far not been determined. A topological method and direct calorimetric measurements under pressure have been used to construct the topological pressure-temperature diagram of the phase relationships between the solid phases II and III, the liquid, and the vapor phase. In the process, the transition temperature between solid phases III and II and its enthalpy change have been determined. Solid phase II, which has the highest melting point, is the more stable phase under ambient conditions in this phase diagram. Surprisingly, solid phase I has not been observed during the study, even though the scarce literature data on its thermal behavior appear to indicate that it might be the most stable one of the three solid phases. Copyright © 2013 Elsevier B.V. All rights reserved.

The global phase diagram of the Gay-Berne model

NASA Astrophysics Data System (ADS)

de Miguel, Enrique; Vega, Carlos

2002-10-01

The phase diagram of the Gay-Berne model with anisotropy parameters κ=3, κ'=5 has been evaluated by means of computer simulations. For a number of temperatures, NPT simulations were performed for the solid phase leading to the determination of the free energy of the solid at a reference density. Using the equation of state and free energies of the isotropic and nematic phases available in the existing literature the fluid-solid equilibrium was calculated for the temperatures selected. Taking these fluid-solid equilibrium results as the starting points, the fluid-solid equilibrium curve was determined for a wide range of temperatures using Gibbs-Duhem integration. At high temperatures the sequence of phases encountered on compression is isotropic to nematic, and then nematic to solid. For reduced temperatures below T=0.85 the sequence is from the isotropic phase directly to the solid state. In view of this we locate the isotropic-nematic-solid triple point at TINS=0.85. The present results suggest that the high-density phase designated smectic B in previous simulations of the model is in fact a molecular solid and not a smectic liquid crystal. It seems that no thermodynamically stable smectic phase appears for the Gay-Berne model with the choice of parameters used in this work. We locate the vapor-isotropic liquid-solid triple point at a temperature TVIS=0.445. Considering that the critical temperatures is Tc=0.473, the Gay-Berne model used in this work presents vapor-liquid separation over a rather narrow range of temperatures. It is suggested that the strong lateral attractive interactions present in the Gay-Berne model stabilizes the layers found in the solid phase. The large stability of the solid phase, particularly at low temperatures, would explain the unexpectedly small liquid range observed in the vapor-liquid region.

NASA Tech Briefs, November 2009

NASA Technical Reports Server (NTRS)

2009-01-01

Topics covered include: Cryogenic Chamber for Servo-Hydraulic Materials Testing; Apparatus Measures Thermal Conductance Through a Thin Sample from Cryogenic to Room Temperature; Rover Attitude and Pointing System Simulation Testbed; Desktop Application Program to Simulate Cargo-Air-Drop Tests; Multimodal Friction Ignition Tester; Small-Bolt Torque-Tension Tester; Integrated Spacesuit Audio System Enhances Speech Quality and Reduces Noise; Hardware Implementation of a Bilateral Subtraction Filter; Simple Optoelectronic Feedback in Microwave Oscillators; Small X-Band Oscillator Antennas; Free-Space Optical Interconnect Employing VCSEL Diodes; Discrete Fourier Transform Analysis in a Complex Vector Space; Miniature Scroll Pumps Fabricated by LIGA; Self-Assembling, Flexible, Pre-Ceramic Composite Preforms; Flight-speed Integral Image Analysis Toolkit; Work Coordination Engine; Multi-Mission Automated Task Invocation Subsystem; Autonomously Calibrating a Quadrupole Mass Spectrometer; Determining Spacecraft Reaction Wheel Friction Parameters; Composite Silica Aerogels Opacified with Titania; Multiplexed Colorimetric Solid-Phase Extraction; Detecting Airborne Mercury by Use of Polymer/Carbon Films; Lattice-Matched Semiconductor Layers on Single Crystalline Sapphire Substrate; Pressure-Energized Seal Rings to Better Withstand Flows; Rollerjaw Rock Crusher; Microwave Sterilization and Depyrogenation System; Quantifying Therapeutic and Diagnostic Efficacy in 2D Microvascular Images; NiF2/NaF:CaF2/Ca Solid-State High-Temperature Battery Cells; Critical Coupling Between Optical Fibers and WGM Resonators; Microwave Temperature Profiler Mounted in a Standard Airborne Research Canister; Alternative Determination of Density of the Titan Atmosphere; Solar Rejection Filter for Large Telescopes; Automated CFD for Generation of Airfoil Performance Tables; Progressive Classification Using Support Vector Machines; Active Learning with Irrelevant Examples; A Data Matrix Method for Improving the Quantification of Element Percentages of SEM/EDX Analysis; Deployable Shroud for the International X-Ray Observatory; Improved Model of a Mercury Ring Damper; Optoelectronic pH Meter: Further Details; X-38 Advanced Sublimator; and Solar Simulator Represents the Mars Surface Solar Environment.

Determination of volatile organic hydrocarbons in water samples by solid-phase dynamic extraction.

PubMed

Jochmann, Maik A; Yuan, Xue; Schmidt, Torsten C

2007-03-01

In the present study a headspace solid-phase dynamic extraction method coupled to gas chromatography-mass spectrometry (HS-SPDE-GC/MS) for the trace determination of volatile halogenated hydrocarbons and benzene from groundwater samples was developed and evaluated. As target compounds, benzene as well as 11 chlorinated and brominated hydrocarbons (vinyl chloride, dichloromethane, cis-1,2-dichloroethylene, trans-1,2-dichloroethylene, carbon tetrachloride, chloroform, trichloroethylene, tetrachloroethylene, bromoform) of environmental and toxicological concern were included in this study. The analytes were extracted using a SPDE needle device, coated with a poly(dimethylsiloxane) with 10% embedded activated carbon phase (50-microm film thickness and 56-mm film length) and were analyzed by GC/MS in full-scan mode. Parameters that affect the extraction yield such as extraction and desorption temperature, salting-out, extraction and desorption flow rate, extraction volume and desorption volume, the number of extraction cycles, and the pre-desorption time have been evaluated and optimized. The linearity of the HS-SPDE-GC/MS method was established over several orders of magnitude. Method detection limits (MDLs) for the compounds investigated ranged between 12 ng/L for cis-dichloroethylene and trans-dichloroethylene and 870 ng/L for vinyl chloride. The method was thoroughly validated, and the precision at two concentration levels (0.1 mg/L and a concentration 5 times above the MDL) was between 3.1 and 16% for the analytes investigated. SPDE provides high sensitivity, short sample preparation and extraction times and a high sample throughput because of full automation. Finally, the applicability to real environmental samples is shown exemplarily for various groundwater samples from a former waste-oil recycling facility. Groundwater from the site showed a complex contamination with chlorinated volatile organic compounds and aromatic hydrocarbons.

Automated, Parametric Geometry Modeling and Grid Generation for Turbomachinery Applications

NASA Technical Reports Server (NTRS)

Harrand, Vincent J.; Uchitel, Vadim G.; Whitmire, John B.

2000-01-01

The objective of this Phase I project is to develop a highly automated software system for rapid geometry modeling and grid generation for turbomachinery applications. The proposed system features a graphical user interface for interactive control, a direct interface to commercial CAD/PDM systems, support for IGES geometry output, and a scripting capability for obtaining a high level of automation and end-user customization of the tool. The developed system is fully parametric and highly automated, and, therefore, significantly reduces the turnaround time for 3D geometry modeling, grid generation and model setup. This facilitates design environments in which a large number of cases need to be generated, such as for parametric analysis and design optimization of turbomachinery equipment. In Phase I we have successfully demonstrated the feasibility of the approach. The system has been tested on a wide variety of turbomachinery geometries, including several impellers and a multi stage rotor-stator combination. In Phase II, we plan to integrate the developed system with turbomachinery design software and with commercial CAD/PDM software.

Precipitation in Al–Mg solid solution prepared by solidification under high pressure

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

Jie, J.C., E-mail: jiejc@dlut.edu.cn; School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001; Wang, H.W.

2014-01-15

The precipitation in Al–Mg solid solution containing 21.6 at.% Mg prepared by solidification under 2 GPa was investigated. The results show that the γ-Al{sub 12}Mg{sub 17} phase is formed and the β′ phase cannot be observed in the solid solution during ageing process. The precipitation of γ and β phases takes place in a non-uniform manner during heating process, i.e. the γ and β phases are first formed in the interdendritic region, which is caused by the inhomogeneous distribution of Mg atoms in the solid solution solidified under high pressure. Peak splitting of X-ray diffraction patterns of Al(Mg) solid solutionmore » appears, and then disappears when the samples are aged at 423 K for different times, due to the non-uniform precipitation in Al–Mg solid solution. The direct transformation from the γ to β phase is observed after ageing at 423 K for 24 h. It is considered that the β phase is formed through a peritectoid reaction of α + γ → β which needs the diffusion of Mg atoms across the interface of α/γ phases. - Highlights: • The γ phase is formed and the β′ phase is be observed in Al(Mg) solid solution. • Peak splitting of XRD pattern of Al(Mg) solid solution appears during aged at 150 °C. • The β phase is formed through a peritectoid reaction of α + γ → β.« less

Proof-of-concept automation of propellant processing

NASA Technical Reports Server (NTRS)

Ramohalli, Kumar; Schallhorn, P. A.

1989-01-01

For space-based propellant production, automation of the process is needed. Currently, all phases of terrestrial production have some form of human interaction. A mixer was acquired to help perform the tasks of automation. A heating system to be used with the mixer was designed, built, and installed. Tests performed on the heating system verify design criteria. An IBM PS/2 personal computer was acquired for the future automation work. It is hoped that some the mixing process itself will be automated. This is a concept demonstration task; proving that propellant production can be automated reliably.

Environmental effects of dredging. Documentation of the settle module for ADDAMS: Design of confined disposal facilities for solids retention and initial storage. Technical notes

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

Hayes, D.F.; Schroeder, P.R.

This technical note documents the SETTLE computer program which facilitates the design of a confined disposal facility (CDF) to retain solids, provide initial storage, and meet effluent discharge limitations for suspended solids during a dredged matenal disposal operation. Detailed information can be found in Engineer Manual 1110-2-5027, Confined Dredged Material Disposal. SETTLE is a part of the Automated Dredging and Disposal Alternatives Management System (ADDAMS).

Understanding and Mitigating Vortex-Dominated, Tip-Leakage and End-Wall Losses in a Transonic Splittered Rotor Stage

DTIC Science & Technology

2015-04-23

blade geometry parameters the TPL design 9   tool was initiated by running the MATLAB script (*.m) Main_SpeedLine_Auto. Main_SpeedLine_Auto...SolidWorks for solid model generation of the blade shapes. Computational Analysis With solid models generated of the gas -path air wedge, automated...287 mm (11.3 in) Constrained by existing TCR geometry Number of Passages 12 None A blade tip-down design approach was used. The outputs of the

Studies and Analyses of Aided Adversarial Decision Making. Phase 2: Research on Human Trust in Automation

DTIC Science & Technology

1998-04-01

34AFRL-HE-WP-TR-1999-0216 UNITED STATES AIR FORCE RESEARCH LABORATORY STUDIES AND ANALYSES OF AIDED ADVERSARIAL DECISION MAKING PHASE 2: RESEARCH ON...Analyses of Aided Adversarial Decision Making . C: F41624-94-D-6000 Phase 2: Research on Human Trust in Automation PE: 62202F PR: 7184 6. AUTHOR(S) TA...Buffalo. This work focused on Aided Adversarial Decision Making (AADM) in Information Warfare (1W) environments. Previous work examined informational

Automated Engineering Design (AED); An approach to automated documentation

NASA Technical Reports Server (NTRS)

Mcclure, C. W.

1970-01-01

The automated engineering design (AED) is reviewed, consisting of a high level systems programming language, a series of modular precoded subroutines, and a set of powerful software machine tools that effectively automate the production and design of new languages. AED is used primarily for development of problem and user-oriented languages. Software production phases are diagramed, and factors which inhibit effective documentation are evaluated.

Scalability, Scintillation Readout and Charge Drift in a Kilogram Scale Solid Xenon Particle Detector

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

Yoo, J.; Cease, H.; Jaskierny, W. F.

2014-10-23

We report a demonstration of the scalability of optically transparent xenon in the solid phase for use as a particle detector above a kilogram scale. We employ a liquid nitrogen cooled cryostat combined with a xenon purification and chiller system to measure the scintillation light output and electron drift speed from both the solid and liquid phases of xenon. Scintillation light output from sealed radioactive sources is measured by a set of high quantum efficiency photomultiplier tubes suitable for cryogenic applications. We observed a reduced amount of photons in solid phase compared to that in liquid phase. We used amore » conventional time projection chamber system to measure the electron drift time in a kilogram of solid xenon and observed faster electron drift speed in the solid phase xenon compared to that in the liquid phase.« less

Fuel spill identification using solid-phase extraction and solid-phase microextraction. 1. Aviation turbine fuels.

PubMed

Lavine, B K; Brzozowski, D M; Ritter, J; Moores, A J; Mayfield, H T

2001-12-01

The water-soluble fraction of aviation jet fuels is examined using solid-phase extraction and solid-phase microextraction. Gas chromatographic profiles of solid-phase extracts and solid-phase microextracts of the water-soluble fraction of kerosene- and nonkerosene-based jet fuels reveal that each jet fuel possesses a unique profile. Pattern recognition analysis reveals fingerprint patterns within the data characteristic of fuel type. By using a novel genetic algorithm (GA) that emulates human pattern recognition through machine learning, it is possible to identify features characteristic of the chromatographic profile of each fuel class. The pattern recognition GA identifies a set of features that optimize the separation of the fuel classes in a plot of the two largest principal components of the data. Because principal components maximize variance, the bulk of the information encoded by the selected features is primarily about the differences between the fuel classes.

Sequential injection-bead injection-lab-on-valve coupled to high-performance liquid chromatography for online renewable micro-solid-phase extraction of carbamate residues in food and environmental samples.

PubMed

Vichapong, Jitlada; Burakham, Rodjana; Srijaranai, Supalax; Grudpan, Kate

2011-07-01

A sequential injection-bead injection-lab-on-valve system was hyphenated to HPLC for online renewable micro-solid-phase extraction of carbamate insecticides. The carbamates studied were isoprocarb, methomyl, carbaryl, carbofuran, methiocarb, promecarb, and propoxur. LiChroprep(®) RP-18 beads (25-40 μm) were employed as renewable sorbent packing in a microcolumn situated inside the LOV platform mounted above the multiposition valve of the sequential injection system. The analytes sorbed by the microcolumn were eluted using 80% acetonitrile in 0.1% acetic acid before online introduction to the HPLC system. Separation was performed on an Atlantis C-18 column (4.6 × 150 mm, 5 μm) utilizing gradient elution with a flow rate of 1.0 mL/min and a detection wavelength at 270 nm. The sequential injection system offers the means of performing automated handling of sample preconcentration and matrix removal. The enrichment factors ranged between 20 and 125, leading to limits of detection (LODs) in the range of 1-20 μg/L. Good reproducibility was obtained with relative standard deviations of <0.7 and 5.4% for retention time and peak area, respectively. The developed method has been successfully applied to the determination of carbamate residues in fruit, vegetable, and water samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of hydrazine in drinking water: Development and multivariate optimization of a rapid and simple solid phase microextraction-gas chromatography-triple quadrupole mass spectrometry protocol.

PubMed

Gionfriddo, Emanuela; Naccarato, Attilio; Sindona, Giovanni; Tagarelli, Antonio

2014-07-04

In this work, the capabilities of solid phase microextraction were exploited in a fully optimized SPME-GC-QqQ-MS analytical approach for hydrazine assay. A rapid and easy method was obtained by a simple derivatization reaction with propyl chloroformate and pyridine carried out directly in water samples, followed by automated SPME analysis in the same vial without further sample handling. The affinity of the different derivatized compounds obtained towards five commercially available SPME coatings was evaluated, in order to achieve the best extraction efficiency. GC analyses were carried out using a GC-QqQ-MS instrument in selected reaction monitoring (SRM) acquisition mode which has allowed the achievement of high specificity by selecting appropriate precursor-product ion couples improving the capability in analyte identification. The multivariate approach of experimental design was crucial in order to optimize derivatization reaction, SPME process and tandem mass spectrometry parameters. Accuracy of the proposed protocol, tested at 60, 200 and 800 ng L(-1), provided satisfactory values (114.2%, 83.6% and 98.6%, respectively), whereas precision (RSD%) at the same concentration levels were of 10.9%, 7.9% and 7.7% respectively. Limit of detection and quantification of 4.4 and 8.3 ng L(-1) were obtained. The reliable application of the proposed protocol to real drinking water samples confirmed its capability to be used as analytical tool for routine analyses. Copyright © 2014 Elsevier B.V. All rights reserved.

A Wide Linearity Range Method for the Determination of Lenalidomide in Plasma by High-Performance Liquid Chromatography: Application to Pharmacokinetic Studies.

PubMed

Guglieri-López, Beatriz; Pérez-Pitarch, Alejandro; Martinez-Gómez, Maria Amparo; Porta-Oltra, Begoña; Climente-Martí, Mónica; Merino-Sanjuán, Matilde

2016-12-01

A wide linearity range analytical method for the determination of lenalidomide in patients with multiple myeloma for pharmacokinetic studies is required. Plasma samples were ultrasonicated for protein precipitation. A solid-phase extraction was performed. The eluted samples were evaporated to dryness under vacuum, and the solid obtained was diluted and injected into the high-performance liquid chromatography (HPLC) system. Separation of lenalidomide was performed on an Xterra RP C18 (250 mm length × 4.6 mm i.d., 5 µm) using a mobile phase consisting of phosphate buffer/acetonitrile (85:15, v/v, pH 3.2) at a flow rate of 0.5 mL · min -1 The samples were monitored at a wavelength of 311 nm. A linear relationship with good correlation coefficient (r = 0.997, n = 9) was found between the peak area and lenalidomide concentrations in the range of 100 to 950 ng · mL -1 The limits of detection and quantitation were 28 and 100 ng · mL -1 , respectively. The intra- and interassay precisions were satisfactory, and the accuracy of the method was proved. In conclusion, the proposed method is suitable for the accurate quantification of lenalidomide in human plasma with a wide linear range, from 100 to 950 ng · mL -1 This is a valuable method for pharmacokinetic studies of lenalidomide in human subjects. © 2016 Society for Laboratory Automation and Screening.

Critical comparison of the on-line and off-line molecularly imprinted solid-phase extraction of patulin coupled with liquid chromatography.

PubMed

Lhotská, Ivona; Holznerová, Anežka; Solich, Petr; Šatínský, Dalibor

2017-12-01

Reaching trace amounts of mycotoxin contamination requires sensitive and selective analytical tools for their determination. Improving the selectivity of sample pretreatment steps covering new and modern extraction techniques is one way to achieve it. Molecularly imprinted polymers as selective sorbent for extraction undoubtedly meet these criteria. The presented work is focused on the hyphenation of on-line molecularly imprinted solid-phase extraction with a chromatography system using a column-switching approach. Making a critical comparison with a simultaneously developed off-line extraction procedure, evaluation of pros and cons of each method, and determining the reliability of both methods on a real sample analysis were carried out. Both high-performance liquid chromatography methods, using off-line extraction on molecularly imprinted polymer and an on-line column-switching approach, were validated, and the validation results were compared against each other. Although automation leads to significant time savings, fewer human errors, and required no handling of toxic solvents, it reached worse detection limits (15 versus 6 μg/L), worse recovery values (68.3-123.5 versus 81.2-109.9%), and worse efficiency throughout the entire clean-up process in comparison with the off-line extraction method. The difficulties encountered, the compromises made during the optimization of on-line coupling and their critical evaluation are presented in detail. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

NASA Astrophysics Data System (ADS)

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.

Infrared Spectroscopy as a Chemical Fingerprinting Tool

NASA Technical Reports Server (NTRS)

Huff, Tim; Munafo, Paul M. (Technical Monitor)

2002-01-01

Infrared (IR) spectroscopy is a powerful analytical tool in the chemical fingerprinting of materials. The technique is rapid, reproducible and usually non-invasive. With the appropriate accessories, the technique can be used to examine samples in either a solid, liquid or gas phase. Solid samples of varying sizes and shapes may be used, and with the addition of microscopic IR (microspectroscopy) capabilities, minute materials such as single fibers and threads may be examined. With the addition of appropriate software, microspectroscopy can be used for automated discrete point or compositional surface area mapping, with the latter providing a means to record changes in the chemical composition of a material surface over a defined area. Both aqueous and non-aqueous free-flowing solutions can be analyzed using appropriate IR techniques, as can viscous liquids such as heavy oils and greases. Due to the ability to characterize gaseous samples, IR spectroscopy can also be coupled with thermal processes such as thermogravimetric (TG) analyses to provide both thermal and chemical data in a single run. In this configuration, solids (or liquids) heated in a TG analyzer undergo decomposition, with the evolving gases directed into the IR spectrometer. Thus, information is provided on the thermal properties of a material and the order in which its chemical constituents are broken down during incremental heating. Specific examples of these varied applications will be cited, with data interpretation and method limitations further discussed.

Integrated topology and shape optimization in structural design

NASA Technical Reports Server (NTRS)

Bremicker, M.; Chirehdast, M.; Kikuchi, N.; Papalambros, P. Y.

1990-01-01

Structural optimization procedures usually start from a given design topology and vary its proportions or boundary shapes to achieve optimality under various constraints. Two different categories of structural optimization are distinguished in the literature, namely sizing and shape optimization. A major restriction in both cases is that the design topology is considered fixed and given. Questions concerning the general layout of a design (such as whether a truss or a solid structure should be used) as well as more detailed topology features (e.g., the number and connectivities of bars in a truss or the number of holes in a solid) have to be resolved by design experience before formulating the structural optimization model. Design quality of an optimized structure still depends strongly on engineering intuition. This article presents a novel approach for initiating formal structural optimization at an earlier stage, where the design topology is rigorously generated in addition to selecting shape and size dimensions. A three-phase design process is discussed: an optimal initial topology is created by a homogenization method as a gray level image, which is then transformed to a realizable design using computer vision techniques; this design is then parameterized and treated in detail by sizing and shape optimization. A fully automated process is described for trusses. Optimization of two dimensional solid structures is also discussed. Several application-oriented examples illustrate the usefulness of the proposed methodology.

Rapid classification of landsat TM imagery for phase 1 stratification using the automated NDVI threshold supervised classification (ANTSC) methodology

Treesearch

William H. Cooke; Dennis M. Jacobs

2002-01-01

FIA annual inventories require rapid updating of pixel-based Phase 1 estimates. Scientists at the Southern Research Station are developing an automated methodology that uses a Normalized Difference Vegetation Index (NDVI) for identifying and eliminating problem FIA plots from the analysis. Problem plots are those that have questionable land useiland cover information....

Artificial intelligence and expert systems in-flight software testing

NASA Technical Reports Server (NTRS)

Demasie, M. P.; Muratore, J. F.

1991-01-01

The authors discuss the introduction of advanced information systems technologies such as artificial intelligence, expert systems, and advanced human-computer interfaces directly into Space Shuttle software engineering. The reconfiguration automation project (RAP) was initiated to coordinate this move towards 1990s software technology. The idea behind RAP is to automate several phases of the flight software testing procedure and to introduce AI and ES into space shuttle flight software testing. In the first phase of RAP, conventional tools to automate regression testing have already been developed or acquired. There are currently three tools in use.

Energy and Resource Saving of Steelmaking Process: Utilization of Innovative Multi-phase Flux During Dephosphorization Process

NASA Astrophysics Data System (ADS)

Matsuura, Hiroyuki; Hamano, Tasuku; Zhong, Ming; Gao, Xu; Yang, Xiao; Tsukihashi, Fumitaka

2014-09-01

An increase in the utilization efficiency of CaO, one of the major fluxing agents used in various steelmaking processes, is required to reduce the amount of discharged slag and energy consumption of the process. The authors have intensively focused on the development of innovative dephosphorization process by using so called "multi-phase flux" composed of solid and liquid phases. This article summarizes the research on the above topic done by the authors, in which the formation mechanisms of P2O5-containing phase during CaO or 2CaO·SiO2 dissolution into molten slag, the phase relationship between solid and liquid phases at equilibrium, and thermodynamic properties of P2O5-containing phase have been clarified. The reactions between solid CaO or 2CaO·SiO2 and molten CaO-FeO x -SiO2-P2O5 slag were observed by dipping solid specimen in the synthesized slag at 1573 K or 1673 K. The formation of the CaO-FeO layer and dual-phase layer of solid 2CaO·SiO2 and FeO x -rich liquid phase was observed around the interface from the solid CaO side toward the bulk slag phase side. Condensation of P2O5 into 2CaO·SiO2 phase as 2CaO·SiO2-3CaO·P2O5 solid solution was observed in both cases of CaO and 2CaO·SiO2 as solid specimens. Measurement of the phase relationship for the CaO-FeO x -SiO2-P2O5 system confirmed the condensation of P2O5 in solid phase at low oxygen partial pressure. The thermodynamics of 2CaO·SiO2-3CaO·P2O5 solid solution are to be clarified to quantitatively simulate the dephosphorization process, and the current results are also introduced. Based on the above results, the reduction of CaO consumption, the discharged slag curtailment, and energy-saving effects have been discussed.

Automated power distribution system hardware. [for space station power supplies

NASA Technical Reports Server (NTRS)

Anderson, Paul M.; Martin, James A.; Thomason, Cindy

1989-01-01

An automated power distribution system testbed for the space station common modules has been developed. It incorporates automated control and monitoring of a utility-type power system. Automated power system switchgear, control and sensor hardware requirements, hardware design, test results, and potential applications are discussed. The system is designed so that the automated control and monitoring of the power system is compatible with both a 208-V, 20-kHz single-phase AC system and a high-voltage (120 to 150 V) DC system.

Synthesis of G-N2-(CH2)3-N2-G Trimethylene DNA interstrand cross-links

PubMed Central

Gruppi, Francesca; Salyard, Tracy L. Johnson; Rizzo, Carmelo J.

2014-01-01

The synthesis of G-N2-(CH2)3-N2-G trimethylene DNA interstrand cross-links (ICLs) in a 5′-CG-3′ and 5′-GC-3′ sequence from oligodeoxynucleotides containing N2-(3-aminopropyl)-2′-deoxyguanosine and 2-fluoro-O6-(trimethylsilylethyl)inosine is presented. Automated solid-phase DNA synthesis was used for unmodified bases and modified nucleotides were incorporated via their corresponding phosphoramidite reagent by a manual coupling protocol. The preparation of the phosphoramidite reagents for incorporation of N2-(3-aminopropyl)-2′-deoxyguanosine is reported. The high-purity trimethylene DNA interstrand cross-link product is obtained through a nucleophilic aromatic substitution reaction between the N2-(3-aminopropyl)-2′-deoxyguanosine and 2-fluoro-O6-(trimethylsilylethyl)inosine containing oligodeoxynucleotides. PMID:25431636

A simple dual online ultra-high pressure liquid chromatography system (sDO-UHPLC) for high throughput proteome analysis.

PubMed

Lee, Hangyeore; Mun, Dong-Gi; Bae, Jingi; Kim, Hokeun; Oh, Se Yeon; Park, Young Soo; Lee, Jae-Hyuk; Lee, Sang-Won

2015-08-21

We report a new and simple design of a fully automated dual-online ultra-high pressure liquid chromatography system. The system employs only two nano-volume switching valves (a two-position four port valve and a two-position ten port valve) that direct solvent flows from two binary nano-pumps for parallel operation of two analytical columns and two solid phase extraction (SPE) columns. Despite the simple design, the sDO-UHPLC offers many advantageous features that include high duty cycle, back flushing sample injection for fast and narrow zone sample injection, online desalting, high separation resolution and high intra/inter-column reproducibility. This system was applied to analyze proteome samples not only in high throughput deep proteome profiling experiments but also in high throughput MRM experiments.

Review of online coupling of sample preparation techniques with liquid chromatography.

PubMed

Pan, Jialiang; Zhang, Chengjiang; Zhang, Zhuomin; Li, Gongke

2014-03-07

Sample preparation is still considered as the bottleneck of the whole analytical procedure, and efforts has been conducted towards the automation, improvement of sensitivity and accuracy, and low comsuption of organic solvents. Development of online sample preparation techniques (SP) coupled with liquid chromatography (LC) is a promising way to achieve these goals, which has attracted great attention. This article reviews the recent advances on the online SP-LC techniques. Various online SP techniques have been described and summarized, including solid-phase-based extraction, liquid-phase-based extraction assisted with membrane, microwave assisted extraction, ultrasonic assisted extraction, accelerated solvent extraction and supercritical fluids extraction. Specially, the coupling approaches of online SP-LC systems and the corresponding interfaces have been discussed and reviewed in detail, such as online injector, autosampler combined with transport unit, desorption chamber and column switching. Typical applications of the online SP-LC techniques have been summarized. Then the problems and expected trends in this field are attempted to be discussed and proposed in order to encourage the further development of online SP-LC techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

Quantification of six herbicide metabolites in human urine.

PubMed

Norrgran, Jessica; Bravo, Roberto; Bishop, Amanda M; Restrepo, Paula; Whitehead, Ralph D; Needham, Larry L; Barr, Dana B

2006-01-18

We developed a sensitive, selective and precise method for measuring herbicide metabolites in human urine. Our method uses automated liquid delivery of internal standards and acetate buffer and a mixed polarity polymeric phase solid phase extraction of a 2 mL urine sample. The concentrated eluate is analyzed using high-performance liquid chromatography-tandem mass spectrometry. Isotope dilution calibration is used for quantification of all analytes. The limits of detection of our method range from 0.036 to 0.075 ng/mL. The within- and between-day variation in pooled quality control samples range from 2.5 to 9.0% and from 3.2 to 16%, respectively, for all analytes at concentrations ranging from 0.6 to 12 ng/mL. Precision was similar with samples fortified with 0.1 and 0.25 ng/mL that were analyzed in each run. We validated our selective method against a less selective method used previously in our laboratory by analyzing human specimens using both methods. The methods produced results that were in agreement, with no significant bias observed.

Crystallization process

DOEpatents

Adler, Robert J.; Brown, William R.; Auyang, Lun; Liu, Yin-Chang; Cook, W. Jeffrey

1986-01-01

An improved crystallization process is disclosed for separating a crystallizable material and an excluded material which is at least partially excluded from the solid phase of the crystallizable material obtained upon freezing a liquid phase of the materials. The solid phase is more dense than the liquid phase, and it is separated therefrom by relative movement with the formation of a packed bed of solid phase. The packed bed is continuously formed adjacent its lower end and passed from the liquid phase into a countercurrent flow of backwash liquid. The packed bed extends through the level of the backwash liquid to provide a drained bed of solid phase adjacent its upper end which is melted by a condensing vapor.

Solid State Lighting Program (Falcon)

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

Meeks, Steven

2012-06-30

Over the past two years, KLA-Tencor and partners successfully developed and deployed software and hardware tools that increase product yield for High Brightness LED (HBLED) manufacturing and reduce product development and factory ramp times. This report summarizes our development effort and details of how the results of the Solid State Light Program (Falcon) have started to help HBLED manufacturers optimize process control by enabling them to flag and correct identified killer defect conditions at any point of origin in the process manufacturing flow. This constitutes a quantum leap in yield management over current practice. Current practice consists of die dispositioningmore » which is just rejection of bad die at end of process based upon probe tests, loosely assisted by optical in-line monitoring for gross process deficiencies. For the first time, and as a result of our Solid State Lighting Program, our LED manufacturing partners have obtained the software and hardware tools that optimize individual process steps to control killer defects at the point in the processes where they originate. Products developed during our two year program enable optimized inspection strategies for many product lines to minimize cost and maximize yield. The Solid State Lighting Program was structured in three phases: i) the development of advanced imaging modes that achieve clear separation between LED defect types, improves signal to noise and scan rates, and minimizes nuisance defects for both front end and back end inspection tools, ii) the creation of defect source analysis (DSA) software that connect the defect maps from back-end and front-end HBLED manufacturing tools to permit the automatic overlay and traceability of defects between tools and process steps, suppress nuisance defects, and identify the origin of killer defects with process step and conditions, and iii) working with partners (Philips Lumileds) on product wafers, obtain a detailed statistical correlation of automated defect and DSA map overlay to failed die identified using end product probe test results. Results from our two year effort have led to “automated end-to-end defect detection” with full defect traceability and the ability to unambiguously correlate device killer defects to optically detected features and their point of origin within the process. Success of the program can be measured by yield improvements at our partner’s facilities and new product orders.« less

Dramatically different kinetics and mechanism at solid/liquid and solid/gas interfaces for catalytic isopropanol oxidation over size-controlled platinum nanoparticles.

PubMed

Wang, Hailiang; Sapi, Andras; Thompson, Christopher M; Liu, Fudong; Zherebetskyy, Danylo; Krier, James M; Carl, Lindsay M; Cai, Xiaojun; Wang, Lin-Wang; Somorjai, Gabor A

2014-07-23

We synthesize platinum nanoparticles with controlled average sizes of 2, 4, 6, and 8 nm and use them as model catalysts to study isopropanol oxidation to acetone in both the liquid and gas phases at 60 °C. The reaction at the solid/liquid interface is 2 orders of magnitude slower than that at the solid/gas interface, while catalytic activity increases with the size of platinum nanoparticles for both the liquid-phase and gas-phase reactions. The activation energy of the gas-phase reaction decreases with the platinum nanoparticle size and is in general much higher than that of the liquid-phase reaction which is largely insensitive to the size of catalyst nanoparticles. Water substantially promotes isopropanol oxidation in the liquid phase. However, it inhibits the reaction in the gas phase. The kinetic results suggest different mechanisms between the liquid-phase and gas-phase reactions, correlating well with different orientations of IPA species at the solid/liquid interface vs the solid/gas interface as probed by sum frequency generation vibrational spectroscopy under reaction conditions and simulated by computational calculations.

Solidification and solid-state transformation sciences in metals additive manufacturing

DOE PAGES

Kirka, Michael M.; Nandwana, Peeyush; Lee, Yousub; ...

2017-02-11

Additive manufacturing (AM) of metals is rapidly emerging as an established manufacturing process for metal components. Unlike traditional metals fabrication processes, metals fabricated via AM undergo localized thermal cycles during fabrication. As a result, AM presents the opportunity to control the liquid-solid phase transformation, i.e. material texture. But, thermal cycling presents challenges from the standpoint of solid-solid phase transformations. We will discuss the opportunities and challenges in metals AM in the context of texture control and associated solid-solid phase transformations in Ti-6Al-4V and Inconel 718.

Microwave spectroscopic observation of distinct electron solid phases in wide quantum wells

NASA Astrophysics Data System (ADS)

Hatke, A. T.; Liu, Yang; Magill, B. A.; Moon, B. H.; Engel, L. W.; Shayegan, M.; Pfeiffer, L. N.; West, K. W.; Baldwin, K. W.

2014-06-01

In high magnetic fields, two-dimensional electron systems can form a number of phases in which interelectron repulsion plays the central role, since the kinetic energy is frozen out by Landau quantization. These phases include the well-known liquids of the fractional quantum Hall effect, as well as solid phases with broken spatial symmetry and crystalline order. Solids can occur at the low Landau-filling termination of the fractional quantum Hall effect series but also within integer quantum Hall effects. Here we present microwave spectroscopy studies of wide quantum wells that clearly reveal two distinct solid phases, hidden within what in d.c. transport would be the zero diagonal conductivity of an integer quantum-Hall-effect state. Explanation of these solids is not possible with the simple picture of a Wigner solid of ordinary (quasi) electrons or holes.

Extinguishment of a Diffusion Flame Over a PMMA Cylinder by Depressurization in Reduced-Gravity

NASA Technical Reports Server (NTRS)

Goldmeer, Jeffrey Scott

1996-01-01

Extinction of a diffusion flame burning over horizontal PMMA (Polymethyl methacrylate) cylinders in low-gravity was examined experimentally and via numerical simulations. Low-gravity conditions were obtained using the NASA Lewis Research Center's reduced-gravity aircraft. The effects of velocity and pressure on the visible flame were examined. The flammability of the burning solid was examined as a function of pressure and the solid-phase centerline temperature. As the solid temperature increased, the extinction pressure decreased, and with a centerline temperature of 525 K, the flame was sustained to 0.1 atmospheres before extinguishing. The numerical simulation iteratively coupled a two-dimensional quasi-steady, gas-phase model with a transient solid-phase model which included conductive heat transfer and surface regression. This model employed an energy balance at the gas/solid interface that included the energy conducted by the gas-phase to the gas/solid interface, Arrhenius pyrolysis kinetics, surface radiation, and the energy conducted into the solid. The ratio of the solid and gas-phase conductive fluxes Phi was a boundary condition for the gas-phase model at the solid-surface. Initial simulations modeled conditions similar to the low-gravity experiments and predicted low-pressure extinction limits consistent with the experimental limits. Other simulations examined the effects of velocity, depressurization rate and Phi on extinction.

Simultaneous analysis of nine aromatic amines in mainstream cigarette smoke using online solid-phase extraction combined with liquid chromatography-tandem mass spectrometry.

PubMed

Zhang, Jie; Bai, Ruoshi; Zhou, Zhaojuan; Liu, Xingyu; Zhou, Jun

2017-04-01

A fully automated analytical method was developed and validated by this present study. The method was based on two-dimensional (2D) online solid-phase extraction liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) to determine nine aromatic amines (AAs) in mainstream smoke (MSS) simultaneously. As a part of validation process, AAs yields for 16 top-selling commercial cigarettes from China market were evaluated by the developed method under both Health Canada Intensive (HCI) and ISO machine smoking regimes. The gas phase of MSS was trapped by 25 mL 0.6 M hydrochloric acid solution, while the particulate phase was collected on a glass fiber filter. Then, the glass fiber pad was extracted with hydrochloric acid solution in an ultrasonic bath. The extract was analyzed with 2D online SPE-LC-MS/MS. In order to minimize the matrix effects of sample on each analyte, two cartridges with different extraction mechanisms were utilized to cleanup disturbances of different polarity, which were performed by the 2D SPE. A phenyl-hexyl analytical column was used to achieve a chromatographic separation. Under the optimized conditions, the isomers of p-toluidine, m-toluidine and o-toluidine, 3-aminobiphenyl and 4-aminobiphenyl, and 1-naphthylamine and 2-naphthylamine were baseline separated with good peak shapes for the first time. The limits of detection for nine AAs ranged from 0.03 to 0.24 ng cig -1 . The recovery of the measurement of nine AAs was from 84.82 to 118.47%. The intra-day and inter-day precisions of nine AAs were less than 10 and 16%, respectively. Compared with ISO machine smoking regime, the AAs yields in MSS were 1.17 to 3.41 times higher under HCI machine smoking regime. Graphical abstract New method using online SPE-LC/MS/MS for analysis of aromatic amines in mainstream cigarette smoke.

Solventless and solvent-minimized sample preparation techniques for determining currently used pesticides in water samples: a review.

PubMed

Tankiewicz, Maciej; Fenik, Jolanta; Biziuk, Marek

2011-10-30

The intensification of agriculture means that increasing amounts of toxic organic and inorganic compounds are entering the environment. The pesticides generally applied nowadays are regarded as some of the most dangerous contaminants of the environment. Their presence in the environment, especially in water, is hazardous because they cause human beings to become more susceptible to disease. For these reasons, it is essential to monitor pesticide residues in the environment with the aid of all accessible analytical methods. The analysis of samples for the presence of pesticides is problematic, because of the laborious and time-consuming operations involved in preparing samples for analysis, which themselves may be a source of additional contaminations and errors. To date, it has been standard practice to use large quantities of organic solvents in the sample preparation process; but as these solvents are themselves hazardous, solventless and solvent-minimized techniques are coming into use. This paper discusses the most commonly used over the last 15 years sample preparation techniques for monitoring organophosphorus and organonitrogen pesticides residue in water samples. Furthermore, a significant trend in sample preparation, in accordance with the principles of 'Green Chemistry' is the simplification, miniaturization and automation of analytical techniques. In view of this aspect, several novel techniques are being developed in order to reduce the analysis step, increase the sample throughput and to improve the quality and the sensitivity of analytical methods. The paper describes extraction techniques requiring the use of solvents - liquid-liquid extraction (LLE) and its modifications, membrane extraction techniques, hollow fibre-protected two-phase solvent microextraction, liquid phase microextraction based on the solidification of a floating organic drop (LPME-SFO), solid-phase extraction (SPE) and single-drop microextraction (SDME) - as well as solvent-free techniques - solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). The advantages and drawbacks of these techniques are also discussed, and some solutions to their limitations are proposed. Copyright © 2011 Elsevier B.V. All rights reserved.

Automated hand hygiene auditing with and without an intervention.

PubMed

Kwok, Yen Lee Angela; Juergens, Craig P; McLaws, Mary-Louise

2016-12-01

Daily feedback from continuous automated auditing with a peer reminder intervention was used to improve compliance. Compliance rates from covert and overt automated auditing phases with and without intervention were compared with human mandatory audits. An automated system was installed to covertly detect hand hygiene events with each depression of the alcohol-based handrub dispenser for 5 months. The overt phase included key clinicians trained to share daily rates with clinicians, set compliance goals, and nudge each other to comply for 6 months. During a further 6 months, the intervention continued without being refreshed. Hand Hygiene Australia (HHA) human audits were performed quarterly during the intervention in accordance with the World Health Organization guidelines. Percentage point (PP) differences between compliance rates were used to determine change. HHA rates for June 2014 were 85% and 87% on the medical and surgical wards, respectively. These rates were 55 PPs and 38 PPs higher than covert automation rates for June 2014 on the medical and surgical ward at 30% and 49%, respectively. During the intervention phase, average compliance did not change on the medical ward from their covert rate, whereas the surgical ward improved compared with the covert phase by 11 PPs to 60%. On average, compliance during the intervention without being refreshed did not change on the medical ward, whereas the average rate on the surgical ward declined by 9 PPs. Automation provided a unique opportunity to respond to daily rates, but compliance will return to preintervention levels once active intervention ceases or human auditors leave the ward, unless clinicians are committed to change. Crown Copyright © 2016. Published by Elsevier Inc. All rights reserved.

SOLID-LIQUID PHASE TRANSFER CATALYZED SYNTHESIS OF CINNAMYL ACETATE-KINETICS AND ANALYSIS OF FACTORS AFFECTING THE REACTION IN A BATCH REACTOR

EPA Science Inventory

The use of solid-liquid phase transfer catalysis has an advantage of carrying out reaction between two immiscible substrates, one in solid phase and the other in liquid phase, with high selectivity and at relatively low temperatures. In this study we investigated the synthesis ci...

Study of aluminum particle combustion in solid propellant plumes using digital in-line holography and imaging pyrometry

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

Chen, Yi; Guildenbecher, Daniel R.; Hoffmeister, Kathryn N. G.

The combustion of molten metals is an important area of study with applications ranging from solid aluminized rocket propellants to fireworks displays. Our work uses digital in-line holography (DIH) to experimentally quantify the three-dimensional position, size, and velocity of aluminum particles during combustion of ammonium perchlorate (AP) based solid-rocket propellants. Additionally, spatially resolved particle temperatures are simultaneously measured using two-color imaging pyrometry. To allow for fast characterization of the properties of tens of thousands of particles, automated data processing routines are proposed. In using these methods, statistics from aluminum particles with diameters ranging from 15 to 900 µm are collectedmore » at an ambient pressure of 83 kPa. In the first set of DIH experiments, increasing initial propellant temperature is shown to enhance the agglomeration of nascent aluminum at the burning surface, resulting in ejection of large molten aluminum particles into the exhaust plume. The resulting particle number and volume distributions are quantified. In the second set of simultaneous DIH and pyrometry experiments, particle size and velocity relationships as well as temperature statistics are explored. The average measured temperatures are found to be 2640 ± 282 K, which compares well with previous estimates of the range of particle and gas-phase temperatures. The novel methods proposed here represent new capabilities for simultaneous quantification of the joint size, velocity, and temperature statistics during the combustion of molten metal particles. The proposed techniques are expected to be useful for detailed performance assessment of metalized solid-rocket propellants.« less

Study of aluminum particle combustion in solid propellant plumes using digital in-line holography and imaging pyrometry

DOE PAGES

Chen, Yi; Guildenbecher, Daniel R.; Hoffmeister, Kathryn N. G.; ...

2017-05-05

The combustion of molten metals is an important area of study with applications ranging from solid aluminized rocket propellants to fireworks displays. Our work uses digital in-line holography (DIH) to experimentally quantify the three-dimensional position, size, and velocity of aluminum particles during combustion of ammonium perchlorate (AP) based solid-rocket propellants. Additionally, spatially resolved particle temperatures are simultaneously measured using two-color imaging pyrometry. To allow for fast characterization of the properties of tens of thousands of particles, automated data processing routines are proposed. In using these methods, statistics from aluminum particles with diameters ranging from 15 to 900 µm are collectedmore » at an ambient pressure of 83 kPa. In the first set of DIH experiments, increasing initial propellant temperature is shown to enhance the agglomeration of nascent aluminum at the burning surface, resulting in ejection of large molten aluminum particles into the exhaust plume. The resulting particle number and volume distributions are quantified. In the second set of simultaneous DIH and pyrometry experiments, particle size and velocity relationships as well as temperature statistics are explored. The average measured temperatures are found to be 2640 ± 282 K, which compares well with previous estimates of the range of particle and gas-phase temperatures. The novel methods proposed here represent new capabilities for simultaneous quantification of the joint size, velocity, and temperature statistics during the combustion of molten metal particles. The proposed techniques are expected to be useful for detailed performance assessment of metalized solid-rocket propellants.« less

Rapid Classification of Landsat TM Imagery for Phase 1 Stratification Using the Automated NDVI Threshold Supervised Classification (ANTSC) Methodology

Treesearch

William H. Cooke; Dennis M. Jacobs

2005-01-01

FIA annual inventories require rapid updating of pixel-based Phase 1 estimates. Scientists at the Southern Research Station are developing an automated methodology that uses a Normalized Difference Vegetation Index (NDVI) for identifying and eliminating problem FIA plots from the analysis. Problem plots are those that have questionable land use/land cover information....

Automated Target Acquisition, Recognition and Tracking (ATTRACT). Phase 1

NASA Technical Reports Server (NTRS)

Abdallah, Mahmoud A.

1995-01-01

The primary objective of phase 1 of this research project is to conduct multidisciplinary research that will contribute to fundamental scientific knowledge in several of the USAF critical technology areas. Specifically, neural networks, signal processing techniques, and electro-optic capabilities are utilized to solve problems associated with automated target acquisition, recognition, and tracking. To accomplish the stated objective, several tasks have been identified and were executed.

Designing, Evaluating, and Deploying Automated Scoring Systems with Validity in Mind: Methodological Design Decisions

ERIC Educational Resources Information Center

Rupp, André A.

2018-01-01

This article discusses critical methodological design decisions for collecting, interpreting, and synthesizing empirical evidence during the design, deployment, and operational quality-control phases for automated scoring systems. The discussion is inspired by work on operational large-scale systems for automated essay scoring but many of the…

Numerical modelling of biomass combustion: Solid conversion processes in a fixed bed furnace

NASA Astrophysics Data System (ADS)

Karim, Md. Rezwanul; Naser, Jamal

2017-06-01

Increasing demand for energy and rising concerns over global warming has urged the use of renewable energy sources to carry a sustainable development of the world. Bio mass is a renewable energy which has become an important fuel to produce thermal energy or electricity. It is an eco-friendly source of energy as it reduces carbon dioxide emissions. Combustion of solid biomass is a complex phenomenon due to its large varieties and physical structures. Among various systems, fixed bed combustion is the most commonly used technique for thermal conversion of solid biomass. But inadequate knowledge on complex solid conversion processes has limited the development of such combustion system. Numerical modelling of this combustion system has some advantages over experimental analysis. Many important system parameters (e.g. temperature, density, solid fraction) can be estimated inside the entire domain under different working conditions. In this work, a complete numerical model is used for solid conversion processes of biomass combustion in a fixed bed furnace. The combustion system is divided in to solid and gas phase. This model includes several sub models to characterize the solid phase of the combustion with several variables. User defined subroutines are used to introduce solid phase variables in commercial CFD code. Gas phase of combustion is resolved using built-in module of CFD code. Heat transfer model is modified to predict the temperature of solid and gas phases with special radiation heat transfer solution for considering the high absorptivity of the medium. Considering all solid conversion processes the solid phase variables are evaluated. Results obtained are discussed with reference from an experimental burner.

Theory of amorphous ices.

PubMed

Limmer, David T; Chandler, David

2014-07-01

We derive a phase diagram for amorphous solids and liquid supercooled water and explain why the amorphous solids of water exist in several different forms. Application of large-deviation theory allows us to prepare such phases in computer simulations. Along with nonequilibrium transitions between the ergodic liquid and two distinct amorphous solids, we establish coexistence between these two amorphous solids. The phase diagram we predict includes a nonequilibrium triple point where two amorphous phases and the liquid coexist. Whereas the amorphous solids are long-lived and slowly aging glasses, their melting can lead quickly to the formation of crystalline ice. Further, melting of the higher density amorphous solid at low pressures takes place in steps, transitioning to the lower-density glass before accessing a nonequilibrium liquid from which ice coarsens.

Community pharmacies automation: any impact on counselling duration and job satisfaction?

PubMed

Cavaco, Afonso Miguel; Krookas, Anette Aaland

2014-04-01

One key indicator of the quality of health practitioners-patient interaction is the encounters' duration. Automation have been presented as beneficial to pharmacy staff work with patients and thus with a potential impact on pharmacists' and technicians' job satisfaction. To compare the interaction length between pharmacy staff and patients, as well as their job satisfaction, in community pharmacies with and without automation. Portuguese community pharmacies with and without automation. This cross-sectional study followed a quasi-experimental design, divided in two phases. In the first, paired community pharmacies with and without automation were purposively selected for a non-participant overt observation. The second phase comprised a job satisfaction questionnaire of both pharmacists and technical staff. Practitioners and patients demographic and interactional data, as well as job satisfaction, were statistically compared across automation. Interaction length and job satisfaction. Sixty-eight practitioners from 10 automated and non-automated pharmacies produced 721 registered interaction episodes. Automation had no significant influence in interaction duration, controlling for gender and professional categories, being significantly longer with older patients (p = 0.017). On average, staff working at the pharmacy counter had 45 % of free time from direct patient contact. The mean overall satisfaction in this sample was 5.52 (SD = 0.98) out of a maximum score of seven, with no significant differences with automation as well as between professional categories, only with a significant lower job satisfaction for younger pharmacists. As with previous studies in other settings, duration of the interactions was not influenced by pharmacy automation, as well as practitioners' job satisfaction, while practitioners' time constrains seem to be a subjective perception.

Determination of 1-chloro-4-[2,2,2-trichloro-1-(4-chlorophenyl)ethyl]benzene and related compounds in marine pore water by automated thermal desorption-gas chromatography/mass spectrometry using disposable optical fiber

USGS Publications Warehouse

Eganhouse, Robert P.; DiFilippo, Erica L

2015-01-01

A method is described for determination of ten DDT-related compounds in marine pore water based on equilibrium solid-phase microextraction (SPME) using commercial polydimethylsiloxane-coated optical fiber with analysis by automated thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS). Thermally cleaned fiber was directly exposed to sediments and allowed to reach equilibrium under static conditions at the in situ field temperature. Following removal, fibers were rinsed, dried and cut into appropriate lengths for storage in leak-tight containers at -20°C. Analysis by TD-GC/MS under full scan (FS) and selected ion monitoring (SIM) modes was then performed. Pore-water method detection limits in FS and SIM modes were estimated at 0.05-2.4ng/L and 0.7-16pg/L, respectively. Precision of the method, including contributions from fiber handling, was less than 10%. Analysis of independently prepared solutions containing eight DDT compounds yielded concentrations that were within 6.9±5.5% and 0.1±14% of the actual concentrations in FS and SIM modes, respectively. The use of optical fiber with automated analysis allows for studies at high temporal and/or spatial resolution as well as for monitoring programs over large spatial and/or long temporal scales with adequate sample replication. This greatly enhances the flexibility of the technique and improves the ability to meet quality control objectives at significantly lower cost.

[Study on blood pressure standard in children using the automatic sphygmomanometer].

PubMed

Niida, Mami; Hataya, Hiroshi; Honda, Masataka

2015-01-01

In Japan, two treatment guidelines exist for pediatric patients with hypertension. The Guidelines for Drug Therapy in Pediatric Patients with Cardiovascular Diseases (JCS2012), by the Japanese Circulation Society, cite the stethoscopy-based American guidelines. The Guidelines for the Management of Hypertension (JSH2009), by the Japanese Society of Hypertension, focus on Japanese data obtained from automated sphygmomanometry. The frequent use of automated sphygmomanometers in clinical practice implies that the JSH2009 guidelines might be better; however with strict low reference values for the diastolic phase, overtreatment may result. Only the Japanese Circulation Society's guidelines include a therapeutic strategy, and the Chronic Kidney Disease (CKD) Guide, CKD Guidelines, and school urinary screening tests all cite these guidelines on stethoscopy-based blood pressure determination. Stethoscopy should be conducted during a medical examination; however, due to limited time in clinical practice, most physicians use automated sphygmomanometers while nevertheless relying on the Japanese Circulation Society reference values--which are stethoscopy-based. To find a compromise, we compared reference values in Japan with those from South Korea (automated sphygmomanometer-based) and those from the United States (stethoscopy-based). Moreover, we examined the results of recent accuracy tests for automated sphygmomanometers. Although the JSH2009 reference values for the systolic phase were consistent with those in the United States (stethoscopy-based), the reference values for the diastolic phase were lower. We observed the same tendency when comparing JSH2009 reference values with those in South Korea (automated sphygmomanometer-based). Conversely, there were only small differences between automated sphygmomanometry and mercury measurement, and we found it was possible to substitute the values from automated sphygmomanometry for stethoscopy. A large-scale study that takes into account patient height, measurement method, and treatment criteria is required to establish appropriate reference values. Even if automated sphygmomanometry is used until appropriate values are established, we consider the criteria provided in the American guidelines as appropriate.

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

Kirka, Michael M.; Nandwana, Peeyush; Lee, Yousub

Additive manufacturing (AM) of metals is rapidly emerging as an established manufacturing process for metal components. Unlike traditional metals fabrication processes, metals fabricated via AM undergo localized thermal cycles during fabrication. As a result, AM presents the opportunity to control the liquid-solid phase transformation, i.e. material texture. But, thermal cycling presents challenges from the standpoint of solid-solid phase transformations. We will discuss the opportunities and challenges in metals AM in the context of texture control and associated solid-solid phase transformations in Ti-6Al-4V and Inconel 718.

Biodegradation testing of chemicals with high Henry's constants - Separating mass and effective concentration reveals higher rate constants.

PubMed

Birch, Heidi; Andersen, Henrik R; Comber, Mike; Mayer, Philipp

2017-05-01

During simulation-type biodegradation tests, volatile chemicals will continuously partition between water phase and headspace. This study addressed how (1) this partitioning affects test results and (2) can be accounted for by combining equilibrium partition and dynamic biodegradation models. An aqueous mixture of 9 (semi)volatile chemicals was first generated using passive dosing and then diluted with environmental surface water producing concentrations in the ng/L to μg/L range. After incubation for 2 h to 4 weeks, automated Headspace Solid Phase Microextraction (HS-SPME) was applied directly on the test systems to measure substrate depletion by biodegradation relatively to abiotic controls. HS-SPME was also applied to determine air to water partitioning ratios. Biodegradation rate constants relating to the chemical in the water phase, k water , were generally a factor 1 to 11 times higher than biodegradation rate constants relating to the total mass of chemical in the test system, k system , with one exceptional factor of 72 times for a long chain alkane. True water phase degradation rate constants were found (i) more appropriate for risk assessment than test system rate constants, (ii) to facilitate extrapolation to other air-water systems and (iii) to be better defined input parameters for aquatic exposure and fate models. Copyright © 2017 Elsevier Ltd. All rights reserved.

Evolution and role of corded cell aggregation in Mycobacterium tuberculosis cultures.

PubMed

Caceres, Neus; Vilaplana, Cristina; Prats, Clara; Marzo, Elena; Llopis, Isaac; Valls, Joaquim; Lopez, Daniel; Cardona, Pere-Joan

2013-11-01

The aim of this study was to evaluate the evolution and role of corded cell aggregation in Mycobacterium tuberculosis cultures according to growth time and conditions. Thus, in standard culture using aerated 7H9 Middlebrook broth supplemented with 0.05% Tween 80, a dramatic CFU decrease was observed at the end of the exponential phase. This phase was followed by a stable stationary phase that led to dissociation between the optical density (O.D.) and CFU values, together with the formation of opaque colonies in solid culture. Further analysis revealed that this was due to cording. Scanning electron microscopy showed that cording led to the formation of very stable coiled structures and corded cell aggregations which proved impossible to disrupt by any of the physical means tested. Modulation of cording with a high but non-toxic concentration of Tween 80 led to a slower growth rate, avoidance of a sudden drop-off to the stationary phase, the formation of weaker cording structures and the absence of opaque colonies, together with a lower survival at later time-points. An innovative automated image analysis technique has been devised to characterize the cording process. This analysis has led to important practical consequences for the elaboration of M. tuberculosis inocula and suggests the importance of biofilm formation in survival of the bacilli in the extracellular milieu. Copyright © 2013. Published by Elsevier Ltd.

Prime Contractors with Awards over $25,000 by Name, Location, and Contract Number. Part 7 (Technology Systems Inc, Wiscasset, Maine -- Zymark Corporation, Hopkinton, Massachusetts), FY1991

DTIC Science & Technology

1991-01-01

z V3 3z I .0J 0(. to0 0 ~ ml cci 0< ix F 3. l4 -I XI- 8 33 0 0 02~~ t; . 4L C0 3 w- = uc3 U (nl 3 C: go 0~~~ 3 8 t)0 0 0 C.)39. U 0 u3 F3 6i6t I -4 4...w cc~~- (n CI9- £. 4 1 6: 2) 2 0 - 1. w 9. W 423 u U .. ) w 0 ~ 4 acca CiC d x HH ul 1-4 H 1-4 HH OUR t- OD- =-4 m~ w ODI (’ S 000 D n01 0 IOD 0000 N...4W 0 F3 U9H -W) H .4. 0 m220 = C4 ix I C, gal 4 22 0~ 0 Ow. 0W". 0 ) U) 02 0 00 0 4 4 E .4 .4 w M 8 n2 0 0202402-02 蓤. 0. 2 2 .40 0 0 w Ld =) 8. Ca

Phase relations in the system NaCl-KCl-H2O: V. Thermodynamic-PTX analysis of solid-liquid equilibria at high temperatures and pressures

USGS Publications Warehouse

Sterner, S.M.; Chou, I.-Ming; Downs, R.T.; Pitzer, Kenneth S.

1992-01-01

The Gibbs energies of mixing for NaCl-KCl binary solids and liquids and solid-saturated NaCl-KCl-H2O ternary liquids were modeled using asymmetric Margules treatments. The coefficients of the expressions were calibrated using an extensive array of binary solvus and solidus data, and both binary and ternary liquidus data. Over the PTX range considered, the system exhibits complete liquid miscibility among all three components and extensive solid solution along the anhydrous binary. Solid-liquid and solid-solid phase equilibria were calculated by using the resulting equations and invoking the equality of chemical potentials of NaCl and KCl between appropriate phases at equilibrium. The equations reproduce the ternary liquidus and predict activity coefficients for NaCl and KCl components in the aqueous liquid under solid-saturation conditions between 673 and 1200 K from vapor saturation up to 5 kbar. In the NaCl-KCl anhydrous binary system, the equations describe phase equilibria and predict activity coefficients of the salt components for all stable compositions of solid and liquid phases between room temperature and 1200 K and from 1 bar to 5 kbar. ?? 1992.

Automation of ⁹⁹Tc extraction by LOV prior ICP-MS detection: application to environmental samples.

PubMed

Rodríguez, Rogelio; Leal, Luz; Miranda, Silvia; Ferrer, Laura; Avivar, Jessica; García, Ariel; Cerdà, Víctor

2015-02-01

A new, fast, automated and inexpensive sample pre-treatment method for (99)Tc determination by inductively coupled plasma-mass spectrometry (ICP-MS) detection is presented. The miniaturized approach is based on a lab-on-valve (LOV) system, allowing automatic separation and preconcentration of (99)Tc. Selectivity is provided by the solid phase extraction system used (TEVA resin) which retains selectively pertechnetate ion in diluted nitric acid solution. The proposed system has some advantages such as minimization of sample handling, reduction of reagents volume, improvement of intermediate precision and sample throughput, offering a significant decrease of both time and cost per analysis in comparison to other flow techniques and batch methods. The proposed LOV system has been successfully applied to different samples of environmental interest (water and soil) with satisfactory recoveries, between 94% and 98%. The detection limit (LOD) of the developed method is 0.005 ng. The high durability of the resin and its low amount (32 mg), its good intermediate precision (RSD 3.8%) and repeatability (RSD 2%) and its high extraction frequency (up to 5 h(-1)) makes this method an inexpensive, high precision and fast tool for monitoring (99)Tc in environmental samples. Copyright © 2014 Elsevier B.V. All rights reserved.

An automated flow injection system for metal determination by flame atomic absorption spectrometry involving on-line fabric disk sorptive extraction technique.

PubMed

Anthemidis, A; Kazantzi, V; Samanidou, V; Kabir, A; Furton, K G

2016-08-15

A novel flow injection-fabric disk sorptive extraction (FI-FDSE) system was developed for automated determination of trace metals. The platform was based on a minicolumn packed with sol-gel coated fabric media in the form of disks, incorporated into an on-line solid-phase extraction system, coupled with flame atomic absorption spectrometry (FAAS). This configuration provides minor backpressure, resulting in high loading flow rates and shorter analytical cycles. The potentials of this technique were demonstrated for trace lead and cadmium determination in environmental water samples. The applicability of different sol-gel coated FPSE media was investigated. The on-line formed complex of metal with ammonium pyrrolidine dithiocarbamate (APDC) was retained onto the fabric surface and methyl isobutyl ketone (MIBK) was used to elute the analytes prior to atomization. For 90s preconcentration time, enrichment factors of 140 and 38 and detection limits (3σ) of 1.8 and 0.4μgL(-1) were achieved for lead and cadmium determination, respectively, with a sampling frequency of 30h(-1). The accuracy of the proposed method was estimated by analyzing standard reference materials and spiked water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Detection and identification of drugs and toxicants in human body fluids by liquid chromatography-tandem mass spectrometry under data-dependent acquisition control and automated database search.

PubMed

Oberacher, Herbert; Schubert, Birthe; Libiseller, Kathrin; Schweissgut, Anna

2013-04-03

Systematic toxicological analysis (STA) is aimed at detecting and identifying all substances of toxicological relevance (i.e. drugs, drugs of abuse, poisons and/or their metabolites) in biological material. Particularly, gas chromatography-mass spectrometry (GC/MS) represents a competent and commonly applied screening and confirmation tool. Herein, we present an untargeted liquid chromatography-tandem mass spectrometry (LC/MS/MS) assay aimed to complement existing GC/MS screening for the detection and identification of drugs in blood, plasma and urine samples. Solid-phase extraction was accomplished on mixed-mode cartridges. LC was based on gradient elution in a miniaturized C18 column. High resolution electrospray ionization-MS/MS in positive ion mode with data-dependent acquisition control was used to generate tandem mass spectral information that enabled compound identification via automated library search in the "Wiley Registry of Tandem Mass Spectral Data, MSforID". Fitness of the developed LC/MS/MS method for application in STA in terms of selectivity, detection capability and reliability of identification (sensitivity/specificity) was demonstrated with blank samples, certified reference materials, proficiency test samples, and authentic casework samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Trace metal determination in natural waters by automated solid phase extraction system and ICP-MS: the influence of low level Mg and Ca.

PubMed

Wang, Bo-Shian; Lee, Chih-Ping; Ho, Tung-Yuan

2014-10-01

A fully automated high pressure pretreatment system with Nobias Chelate-PA1 resin (PA1) was developed for trace metal determination by ICP-MS in natural waters. By varying the concentrations of Mg and Ca to mimic the concentrations in the eluate obtained by PA1 or iminodiacetate type resins, the overall analytical performance of the system was assessed for the determination of Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Y, Cd, Ag, Pb and REE. Comparing with the low mM level Mg and Ca (both ranging from 1 to 4mM) eluted by iminodiacetate type resins, the eluate obtained by PA1 contains sub-μM level Mg and Ca, which remarkably decrease matrix effect in ICP-MS analysis and significantly improve the analytical performance. With recovery better than 90% for most the trace metals examined, the accuracy was further verified through the analysis of five natural water reference materials with salinity spanning from 0 to 35‰. We have successfully applied the pretreatment system to determine trace metals in the seawater samples collected in the Western Philippine Sea through Taiwan GEOTRACES cruise. Copyright © 2014 Elsevier B.V. All rights reserved.

Automated data collection based on RoboDiff at the ESRF beamline MASSIF-1

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

Nurizzo, Didier, E-mail: Didier.nurizzo@esrf.fr; Guichard, Nicolas; McSweeney, Sean

2016-07-27

The European Synchrotron Radiation Facility has a long standing history in the automation of experiments in Macromolecular Crystallography. MASSIF-1 (Massively Automated Sample Screening and evaluation Integrated Facility), a beamline constructed as part of the ESRF Upgrade Phase I program, has been open to the external user community since July 2014 and offers a unique completely automated data collection service to both academic and industrial structural biologists.

Phase diagram of two-dimensional hard ellipses.

PubMed

Bautista-Carbajal, Gustavo; Odriozola, Gerardo

2014-05-28

We report the phase diagram of two-dimensional hard ellipses as obtained from replica exchange Monte Carlo simulations. The replica exchange is implemented by expanding the isobaric ensemble in pressure. The phase diagram shows four regions: isotropic, nematic, plastic, and solid (letting aside the hexatic phase at the isotropic-plastic two-step transition [E. P. Bernard and W. Krauth, Phys. Rev. Lett. 107, 155704 (2011)]). At low anisotropies, the isotropic fluid turns into a plastic phase which in turn yields a solid for increasing pressure (area fraction). Intermediate anisotropies lead to a single first order transition (isotropic-solid). Finally, large anisotropies yield an isotropic-nematic transition at low pressures and a high-pressure nematic-solid transition. We obtain continuous isotropic-nematic transitions. For the transitions involving quasi-long-range positional ordering, i.e., isotropic-plastic, isotropic-solid, and nematic-solid, we observe bimodal probability density functions. This supports first order transition scenarios.

Binary Solid-Liquid Phase Diagram of Phenol and t-Butanol: An Undergraduate Physical Chemistry Experiment

ERIC Educational Resources Information Center

Xu, Xinhua; Wang, Xiaogang; Wu, Meifen

2014-01-01

The determination of the solid-liquid phase diagram of a binary system is always used as an experiment in the undergraduate physical chemistry laboratory courses. However, most phase diagrams investigated in the lab are simple eutectic ones, despite the fact that complex binary solid-liquid phase diagrams are more common. In this article, the…

Phase transitions of amorphous solid acetone in confined geometry investigated by reflection absorption infrared spectroscopy.

PubMed

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.

ARTIP: Automated Radio Telescope Image Processing Pipeline

NASA Astrophysics Data System (ADS)

Sharma, Ravi; Gyanchandani, Dolly; Kulkarni, Sarang; Gupta, Neeraj; Pathak, Vineet; Pande, Arti; Joshi, Unmesh

2018-02-01

The Automated Radio Telescope Image Processing Pipeline (ARTIP) automates the entire process of flagging, calibrating, and imaging for radio-interferometric data. ARTIP starts with raw data, i.e. a measurement set and goes through multiple stages, such as flux calibration, bandpass calibration, phase calibration, and imaging to generate continuum and spectral line images. Each stage can also be run independently. The pipeline provides continuous feedback to the user through various messages, charts and logs. It is written using standard python libraries and the CASA package. The pipeline can deal with datasets with multiple spectral windows and also multiple target sources which may have arbitrary combinations of flux/bandpass/phase calibrators.

Eye blink detection for different driver states in conditionally automated driving and manual driving using EOG and a driver camera.

PubMed

Schmidt, Jürgen; Laarousi, Rihab; Stolzmann, Wolfgang; Karrer-Gauß, Katja

2018-06-01

In this article, we examine the performance of different eye blink detection algorithms under various constraints. The goal of the present study was to evaluate the performance of an electrooculogram- and camera-based blink detection process in both manually and conditionally automated driving phases. A further comparison between alert and drowsy drivers was performed in order to evaluate the impact of drowsiness on the performance of blink detection algorithms in both driving modes. Data snippets from 14 monotonous manually driven sessions (mean 2 h 46 min) and 16 monotonous conditionally automated driven sessions (mean 2 h 45 min) were used. In addition to comparing two data-sampling frequencies for the electrooculogram measures (50 vs. 25 Hz) and four different signal-processing algorithms for the camera videos, we compared the blink detection performance of 24 reference groups. The analysis of the videos was based on very detailed definitions of eyelid closure events. The correct detection rates for the alert and manual driving phases (maximum 94%) decreased significantly in the drowsy (minus 2% or more) and conditionally automated (minus 9% or more) phases. Blinking behavior is therefore significantly impacted by drowsiness as well as by automated driving, resulting in less accurate blink detection.

Solid electrolyte-electrode system for an electrochemical cell

DOEpatents

Tuller, Harry L.; Kramer, Steve A.; Spears, Marlene A.

1995-01-01

An electrochemical device including a solid electrolyte and solid electrode composed of materials having different chemical compositions and characterized by different electrical properties but having the same crystalline phase is provided. A method for fabricating an electrochemical device having a solid electrode and solid electrolyte characterized by the same crystalline phase is also provided.

Solid/FEM integration at SNLA

NASA Technical Reports Server (NTRS)

Chavez, Patrick F.

1987-01-01

The effort at Sandia National Labs. on the methodologies and techniques being used to generate strict hexahedral finite element meshes from a solid model is described. The functionality of the modeler is used to decompose the solid into a set of nonintersecting meshable finite element primitives. The description of the decomposition is exported, via a Boundary Representative format, to the meshing program which uses the information for complete finite element model specification. Particular features of the program are discussed in some detail along with future plans for development which includes automation of the decomposition using artificial intelligence techniques.

Two-dimensional solid-phase extraction strategy for the selective enrichment of aminoglycosides in milk.

PubMed

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.

Automated longwall guidance and control systems, phase 1

NASA Technical Reports Server (NTRS)

Rybak, S. C.

1978-01-01

Candidate vertical control systems (VCS) and face advancement systems (FAS) required to satisfactorily automate the longwall system were analyzed and simulated in order to develop an overall longwall system configuration for preliminary design.

Automated vessel segmentation using cross-correlation and pooled covariance matrix analysis.

PubMed

Du, Jiang; Karimi, Afshin; Wu, Yijing; Korosec, Frank R; Grist, Thomas M; Mistretta, Charles A

2011-04-01

Time-resolved contrast-enhanced magnetic resonance angiography (CE-MRA) provides contrast dynamics in the vasculature and allows vessel segmentation based on temporal correlation analysis. Here we present an automated vessel segmentation algorithm including automated generation of regions of interest (ROIs), cross-correlation and pooled sample covariance matrix analysis. The dynamic images are divided into multiple equal-sized regions. In each region, ROIs for artery, vein and background are generated using an iterative thresholding algorithm based on the contrast arrival time map and contrast enhancement map. Region-specific multi-feature cross-correlation analysis and pooled covariance matrix analysis are performed to calculate the Mahalanobis distances (MDs), which are used to automatically separate arteries from veins. This segmentation algorithm is applied to a dual-phase dynamic imaging acquisition scheme where low-resolution time-resolved images are acquired during the dynamic phase followed by high-frequency data acquisition at the steady-state phase. The segmented low-resolution arterial and venous images are then combined with the high-frequency data in k-space and inverse Fourier transformed to form the final segmented arterial and venous images. Results from volunteer and patient studies demonstrate the advantages of this automated vessel segmentation and dual phase data acquisition technique. Copyright © 2011 Elsevier Inc. All rights reserved.

Automated solar cell assembly team process research

NASA Astrophysics Data System (ADS)

Nowlan, M. J.; Hogan, S. J.; Darkazalli, G.; Breen, W. F.; Murach, J. M.; Sutherland, S. F.; Patterson, J. S.

1994-06-01

This report describes work done under the Photovoltaic Manufacturing Technology (PVMaT) project, Phase 3A, which addresses problems that are generic to the photovoltaic (PV) industry. Spire's objective during Phase 3A was to use its light soldering technology and experience to design and fabricate solar cell tabbing and interconnecting equipment to develop new, high-yield, high-throughput, fully automated processes for tabbing and interconnecting thin cells. Areas that were addressed include processing rates, process control, yield, throughput, material utilization efficiency, and increased use of automation. Spire teamed with Solec International, a PV module manufacturer, and the University of Massachusetts at Lowell's Center for Productivity Enhancement (CPE), automation specialists, who are lower-tier subcontractors. A number of other PV manufacturers, including Siemens Solar, Mobil Solar, Solar Web, and Texas instruments, agreed to evaluate the processes developed under this program.

Development of advanced image analysis techniques for the in situ characterization of multiphase dispersions occurring in bioreactors.

PubMed

Galindo, Enrique; Larralde-Corona, C Patricia; Brito, Teresa; Córdova-Aguilar, Ma Soledad; Taboada, Blanca; Vega-Alvarado, Leticia; Corkidi, Gabriel

2005-03-30

Fermentation bioprocesses typically involve two liquid phases (i.e. water and organic compounds) and one gas phase (air), together with suspended solids (i.e. biomass), which are the components to be dispersed. Characterization of multiphase dispersions is required as it determines mass transfer efficiency and bioreactor homogeneity. It is also needed for the appropriate design of contacting equipment, helping in establishing optimum operational conditions. This work describes the development of image analysis based techniques with advantages (in terms of data acquisition and processing), for the characterization of oil drops and bubble diameters in complex simulated fermentation broths. The system consists of fully digital acquisition of in situ images obtained from the inside of a mixing tank using a CCD camera synchronized with a stroboscopic light source, which are processed with a versatile commercial software. To improve the automation of particle recognition and counting, the Hough transform (HT) was used, so bubbles and oil drops were automatically detected and the processing time was reduced by 55% without losing accuracy with respect to a fully manual analysis. The system has been used for the detailed characterization of a number of operational conditions, including oil content, biomass morphology, presence of surfactants (such as proteins) and viscosity of the aqueous phase.

Adsorption of the Three-phase Emulsion on Various Solid Surfaces.

PubMed

Enomoto, Yasutaka; Imai, Yoko; Tajima, Kazuo

2017-07-01

The present study investigates the adsorption of the three-phase emulsion on various solid/water interfaces. Vesicles can be used as emulsifiers in the three-phase emulsions and act as an independent phase unlike the surfactant used in conventional emulsions; therefore, it is expected that the three-phase emulsion formed by the adhesion of vesicles to the oil/water interface will adsorb on various solid/water interfaces. The cationic three-phase emulsion was prepared to encourage emulsion adsorption on negatively charged solid substrates in water. The emulsifier polyoxyethylene-(10) hydrogenated castor oil was rendered cationic by mixing with the surfactant cetyltrimethylammonium bromide and then used to prepare the cationic three-phase emulsion of hexadecane-in-water. Three solid substrates (silicon, glass, and copper) were dipped in the cationic emulsion and the emulsion was found to adsorb on the solid substrates while maintaining its structure. The amount of hexadecane adsorbed on the various surfaces was investigated by gas chromatography and found to increase with increasing hexadecane concentration in the emulsion and eventually plateaued just like molecular adsorption. The maximum surface coverage of the emulsion on the substrates was approximately 80%. However, even the equivalent nonionic three-phase emulsion was found to adsorb on the three solid surfaces. This was attributed to a novel mechanism of irreversible adhesion via the van der Waals attractive force.

Manual Solid-Phase Peptide Synthesis of Metallocene-Peptide Bioconjugates

ERIC Educational Resources Information Center

Kirin, Srecko I.; Noor, Fozia; Metzler-Nolte, Nils; Mier, Walter

2007-01-01

A simple and relatively inexpensive procedure for preparing a biologically active peptide using solid phase peptide synthesis (SPPS) is described. Fourth-year undergraduate students have gained firsthand experience from the solid-phase synthesis techniques and they have become familiar with modern analytical techniques based on the particular…

Effect of solid-meal caloric content on gastric emptying kinetics of solids and liquids.

PubMed

Urbain, J L; Siegel, J A; Mortelmans, L; van Cutsem, E; van den Maegdenbergh, V; de Roo, M

1989-08-01

In this study, we have evaluated the effect of the caloric content of a physiological test meal on the gastric emptying kinetics of solids and liquids. 22 healthy male volunteers were studied in two groups matched for age. After an overnight fast, each volunteer underwent the same test procedure; in the first group (G I), 10 volunteers received a meal consisting of bread, 111In-DTPA water and 1 scrambled egg labeled with 99mTc-labelled sulphur colloid; in the second group (G II) 12 volunteers were given the same meal but with 2 labeled eggs in order to increase the caloric content of the solid phase meal. Simultaneous anterior and posterior images were recorded using a dual-headed gamma camera. Solid and liquid geometric mean data were analyzed to determine the lag phase, the emptying rate and the half-emptying time for both solids and liquids. Solid and liquid gastric half-emptying times were significantly prolonged in G II compared to G I volunteers. For the solid phased, the delay was accounted for by a longer lag phase and a decrease in the equilibrium emptying rate. The emptying rate of the liquid phase was significantly decreased in G II compared to G I. Within each group, no statistically significant difference was observed between solid and liquid emptying rates. We conclude that the caloric content of the solid portion of a meal not only alters the emptying of the solid phase but also affects the emptying of the liquid component of the meal.

Development of automation and robotics for space via computer graphic simulation methods

NASA Technical Reports Server (NTRS)

Fernandez, Ken

1988-01-01

A robot simulation system, has been developed to perform automation and robotics system design studies. The system uses a procedure-oriented solid modeling language to produce a model of the robotic mechanism. The simulator generates the kinematics, inverse kinematics, dynamics, control, and real-time graphic simulations needed to evaluate the performance of the model. Simulation examples are presented, including simulation of the Space Station and the design of telerobotics for the Orbital Maneuvering Vehicle.

Theory of amorphous ices

PubMed Central

Limmer, David T.; Chandler, David

2014-01-01

We derive a phase diagram for amorphous solids and liquid supercooled water and explain why the amorphous solids of water exist in several different forms. Application of large-deviation theory allows us to prepare such phases in computer simulations. Along with nonequilibrium transitions between the ergodic liquid and two distinct amorphous solids, we establish coexistence between these two amorphous solids. The phase diagram we predict includes a nonequilibrium triple point where two amorphous phases and the liquid coexist. Whereas the amorphous solids are long-lived and slowly aging glasses, their melting can lead quickly to the formation of crystalline ice. Further, melting of the higher density amorphous solid at low pressures takes place in steps, transitioning to the lower-density glass before accessing a nonequilibrium liquid from which ice coarsens. PMID:24858957

Electron drift in a large scale solid xenon

DOE PAGES

Yoo, J.; Jaskierny, W. F.

2015-08-21

A study of charge drift in a large scale optically transparent solid xenon is reported. A pulsed high power xenon light source is used to liberate electrons from a photocathode. The drift speeds of the electrons are measured using a 8.7 cm long electrode in both the liquid and solid phase of xenon. In the liquid phase (163 K), the drift speed is 0.193 ± 0.003 cm/μs while the drift speed in the solid phase (157 K) is 0.397 ± 0.006 cm/μs at 900 V/cm over 8.0 cm of uniform electric fields. Furthermore, it is demonstrated that a factor twomore » faster electron drift speed in solid phase xenon compared to that in liquid in a large scale solid xenon.« less

Grain Floatation During Equiaxed Solidification of an Al-Cu Alloy in a Side-Cooled Cavity: Part II—Numerical Studies

NASA Astrophysics Data System (ADS)

Kumar, Arvind; Walker, Mike J.; Sundarraj, Suresh; Dutta, Pradip

2011-08-01

In this article, a single-phase, one-domain macroscopic model is developed for studying binary alloy solidification with moving equiaxed solid phase, along with the associated transport phenomena. In this model, issues such as thermosolutal convection, motion of solid phase relative to liquid and viscosity variations of the solid-liquid mixture with solid fraction in the mobile zone are taken into account. Using the model, the associated transport phenomena during solidification of Al-Cu alloys in a rectangular cavity are predicted. The results for temperature variation, segregation patterns, and eutectic fraction distribution are compared with data from in-house experiments. The model predictions compare well with the experimental results. To highlight the influence of solid phase movement on convection and final macrosegregation, the results of the current model are also compared with those obtained from the conventional solidification model with stationary solid phase. By including the independent movement of the solid phase into the fluid transport model, better predictions of macrosegregation, microstructure, and even shrinkage locations were obtained. Mechanical property prediction models based on microstructure will benefit from the improved accuracy of this model.

Solid phase pegylation of hemoglobin.

PubMed

Suo, Xiaoyan; Zheng, Chunyang; Yu, Pengzhan; Lu, Xiuling; Ma, Guanghui; Su, Zhiguo

2009-01-01

A solid phase conjugation process was developed for attachment of polyethylene glycol to hemoglobin molecule. Bovine hemoglobin was loaded onto an ion exchange chromatography column and adsorbed by the solid medium. Succinimidyl carbonate mPEG was introduced in the mobile phase after the adsorption. Pegylation took place between the hemoglobin on the solid phase, and the pegylation reagent in the liquid phase. A further elution was carried out to separate the pegylated and the unpegylated protein. Analysis by HPSEC, SDS-PAGE, and MALLS demonstrated that the fractions eluted from the solid phase contained well-defined components. Pegylated hemoglobin with one PEG chain was obtained with the yield of 75%, in comparison to the yield of 30% in the liquid phase pegylation. The P(50) values of the mono-pegylated hemoglobin, prepared with SC-mPEG 5 kDa, 10 kDa and 20 kDa, were 19.97, 20.23 and 20.54 mmHg, which were much closer to the value of red blood cells than that of pegylated hemoglobin prepared with the conventional method.

Mechanism of Formation of Li 7 P 3 S 11 Solid Electrolytes through Liquid Phase Synthesis

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

Wang, Yuxing; Lu, Dongping; Bowden, Mark

Crystalline Li7P3S11 is a promising solid electrolyte for all solid state lithium/lithium ion batteries. A controllable liquid phase synthesis of Li7P3S11 is more desirable compared to conventional mechanochemical synthesis, but recent attempts suffer from reduced ionic conductivities. Here we elucidate the formation mechanism of crystalline Li7P3S11 synthesized in the liquid phase (acetonitrile, or ACN). We conclude that the crystalline Li7P3S11 forms through a two-step reaction: 1) formation of solid Li3PS4∙ACN and amorphous Li2S∙P2S5 phases in the liquid phase; 2) solid-state conversion of the two phases. The implication of this two-step reaction mechanism to the morphology control and the transport propertiesmore » of liquid phase synthesized Li7P3S11 is identified and discussed.« less

Shape optimization of three-dimensional stamped and solid automotive components

NASA Technical Reports Server (NTRS)

Botkin, M. E.; Yang, R.-J.; Bennett, J. A.

1987-01-01

The shape optimization of realistic, 3-D automotive components is discussed. The integration of the major parts of the total process: modeling, mesh generation, finite element and sensitivity analysis, and optimization are stressed. Stamped components and solid components are treated separately. For stamped parts a highly automated capability was developed. The problem description is based upon a parameterized boundary design element concept for the definition of the geometry. Automatic triangulation and adaptive mesh refinement are used to provide an automated analysis capability which requires only boundary data and takes into account sensitivity of the solution accuracy to boundary shape. For solid components a general extension of the 2-D boundary design element concept has not been achieved. In this case, the parameterized surface shape is provided using a generic modeling concept based upon isoparametric mapping patches which also serves as the mesh generator. Emphasis is placed upon the coupling of optimization with a commercially available finite element program. To do this it is necessary to modularize the program architecture and obtain shape design sensitivities using the material derivative approach so that only boundary solution data is needed.

Design Through Manufacturing: The Solid Model-Finite Element Analysis Interface

NASA Technical Reports Server (NTRS)

Rubin, Carol

2002-01-01

State-of-the-art computer aided design (CAD) presently affords engineers the opportunity to create solid models of machine parts reflecting every detail of the finished product. Ideally, in the aerospace industry, these models should fulfill two very important functions: (1) provide numerical. control information for automated manufacturing of precision parts, and (2) enable analysts to easily evaluate the stress levels (using finite element analysis - FEA) for all structurally significant parts used in aircraft and space vehicles. Today's state-of-the-art CAD programs perform function (1) very well, providing an excellent model for precision manufacturing. But they do not provide a straightforward and simple means of automating the translation from CAD to FEA models, especially for aircraft-type structures. Presently, the process of preparing CAD models for FEA consumes a great deal of the analyst's time.

Engineered glass seals for solid-oxide fuel cells

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

Surdoval, Wayne; Lara-Curzio, Edgar; Stevenson, Jeffry

2017-02-07

A seal for a solid oxide fuel cell includes a glass matrix having glass percolation therethrough and having a glass transition temperature below 650.degree. C. A deformable second phase material is dispersed in the glass matrix. The second phase material can be a compliant material. The second phase material can be a crushable material. A solid oxide fuel cell, a precursor for forming a seal for a solid oxide fuel cell, and a method of making a seal for a solid oxide fuel cell are also disclosed.

Solid electrolyte-electrode system for an electrochemical cell

DOEpatents

Tuller, H.L.; Kramer, S.A.; Spears, M.A.

1995-04-04

An electrochemical device including a solid electrolyte and solid electrode composed of materials having different chemical compositions and characterized by different electrical properties but having the same crystalline phase is provided. A method for fabricating an electrochemical device having a solid electrode and solid electrolyte characterized by the same crystalline phase is also provided. 17 figures.

Using Simulation as an Investigational Methodology to Explore the Impact of Technology on Team Communication and Patient Management: A Pilot Evaluation of the Effect of an Automated Compression Device.

PubMed

Gittinger, Matthew; Brolliar, Sarah M; Grand, James A; Nichol, Graham; Fernandez, Rosemarie

2017-06-01

This pilot study used a simulation-based platform to evaluate the effect of an automated mechanical chest compression device on team communication and patient management. Four-member emergency department interprofessional teams were randomly assigned to perform manual chest compressions (control, n = 6) or automated chest compressions (intervention, n = 6) during a simulated cardiac arrest with 2 phases: phase 1 baseline (ventricular tachycardia), followed by phase 2 (ventricular fibrillation). Patient management was coded using an Advanced Cardiovascular Life Support-based checklist. Team communication was categorized in the following 4 areas: (1) teamwork focus; (2) huddle events, defined as statements focused on re-establishing situation awareness, reinforcing existing plans, and assessing the need to adjust the plan; (3) clinical focus; and (4) profession of team member. Statements were aggregated for each team. At baseline, groups were similar with respect to total communication statements and patient management. During cardiac arrest, the total number of communication statements was greater in teams performing manual compressions (median, 152.3; interquartile range [IQR], 127.6-181.0) as compared with teams using an automated compression device (median, 105; IQR, 99.5-123.9). Huddle events were more frequent in teams performing automated chest compressions (median, 4.0; IQR, 3.1-4.3 vs. 2.0; IQR, 1.4-2.6). Teams randomized to the automated compression intervention had a delay to initial defibrillation (median, 208.3 seconds; IQR, 153.3-222.1 seconds) as compared with control teams (median, 63.2 seconds; IQR, 30.1-397.2 seconds). Use of an automated compression device may impact both team communication and patient management. Simulation-based assessments offer important insights into the effect of technology on healthcare teams.

Rapid determination of the volatile components in tobacco by ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction with gas chromatography-mass spectrometry.

PubMed

Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

2016-03-01

An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evolution of solid rocket booster component testing

NASA Technical Reports Server (NTRS)

Lessey, Joseph A.

1989-01-01

The evolution of one of the new generation of test sets developed for the Solid Rocket Booster of the U.S. Space Transportation System. Requirements leading to factory checkout of the test set are explained, including the evolution from manual to semiautomated toward fully automated status. Individual improvements in the built-in test equipment, self-calibration, and software flexibility are addressed, and the insertion of fault detection to improve reliability is discussed.

Numerical investigation of influence on heat transfer characteristics to pneumatically conveyed dense phase flow by selecting models and boundary conditions

NASA Astrophysics Data System (ADS)

Zheng, Y.; Liu, Q.; Li, Y.

2012-03-01

Solids moving with a gas stream in a pipeline can be found in many industrial processes, such as power generation, chemical, pharmaceutical, food and commodity transfer processes. A mass flow rate of the solids is important characteristic that is often required to be measured (and controlled) to achieve efficient utilization of energy and raw materials in pneumatic conveying systems. The methods of measuring the mass flow rate of solids in a pneumatic pipeline can be divided into direct and indirect (inferential) measurements. A thermal solids' mass flow-meter, in principle, should ideally provide a direct measurement of solids flow rate, regardless of inhomogeneities in solids' distribution and environmental impacts. One key issue in developing a thermal solids' mass flow-meter is to characterize the heat transfer between the hot pipe wall and the gas-solids dense phase flow. The Eulerian continuum modeling with gas-solid two phases is the most common method for pneumatic transport. To model a gas-solid dense phase flow passing through a heated region, the gas phase is described as a continuous phase and the particles as the second phase. This study aims to describe the heat transfer characteristics between the hot wall and the gas-solids dense phase flow in pneumatic pipelines by modeling a turbulence gas-solid plug passing through the heated region which involves several actual and crucial issues: selections of interphase exchange coefficient, near-wall region functions and different wall surface temperatures. A sensitivity analysis was discussed to identify the influence on the heat transfer characteristics by selecting different interphase exchange coefficient models and different boundary conditions. Simulation results suggest that sensitivity analysis in the choice of models is very significant. The simulation results appear to show that a combination of choosing the Syamlal-O'Brien interphase exchange coefficient model and the standard k-ɛ model along with the standard wall function model might be the best approach, by which, the simulation data seems to be closest to the experimental results.

Liquid-phase and solid-phase microwave irradiations for reduction of graphite oxide

NASA Astrophysics Data System (ADS)

Zhao, Na; Wen, Chen-Yu; Zhang, David Wei; Wu, Dong-Ping; Zhang, Zhi-Bin; Zhang, Shi-Li

2014-12-01

In this paper, two microwave irradiation methods: (i) liquid-phase microwave irradiation (MWI) reduction of graphite oxide suspension dissolved in de-ionized water and N, N-dimethylformamide, respectively, and (ii) solid-phase MWI reduction of graphite oxide powder have been successfully carried out to reduce graphite oxide. The reduced graphene oxide products are thoroughly characterized by scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectral analysis, Raman spectroscopy, UV-Vis absorption spectral analysis, and four-point probe conductivity measurements. The results show that both methods can efficiently remove the oxygen-containing functional groups attached to the graphite layers, though the solid-phase MWI reduction method can obtain far more efficiently a higher quality-reduced graphene oxide with fewer defects. The I(D)/I(G) ratio of the solid-phase MWI sample is as low as 0.46, which is only half of that of the liquid-phase MWI samples. The electrical conductivity of the reduced graphene oxide by the solid method reaches 747.9 S/m, which is about 25 times higher than that made by the liquid-phase method.

Using automated feeders to wean calves fed large amounts of milk according to their ability to eat solid feed.

PubMed

de Passillé, Anne Marie; Rushen, Jeffrey

2016-05-01

Dairy calves weaned off milk at an early age show signs of hunger and can lose weight. We examined whether using automated feeders to wean calves according to individual voluntary solid feed intake reduced the effects of weaning. Female Holstein calves were housed in groups of 5 to 9. All calves were fed 12 L/d milk and ad libitum grain starter and hay from automated feeders immediately after grouping, and were allocated to 3 weaning strategies: (1) early-weaned (EW; n=14): weaning began on d 40, and milk allowance gradually decreased until weaning was complete on d 48; (2) late-weaned (LW; n=14): weaning began on d 80 and was completed on d 89; (3) weaned by starter intake (WSI; n=28): weaning began when calves consumed 200g/d of starter and was completed when the calves consumed 1,400g/d. Each day, the automated feeders recorded quantities of milk, starter, and hay eaten by all calves, as well as the frequency of visits to the milk feeder; we used unrewarded visit frequency as a sign of hunger. Body weights (BW) were recorded weekly. We estimated daily digestible energy (DE) intake for each calf based on the milk, hay, and starter consumed. Average daily gains (ADG) were expressed as percent of BW. For calves in WSI, weaning began at 54.7±18.9 d (mean ± SD) of age, the duration of weaning was 21.1±10.6 d, and weaning ended at 75.8±10.7 d of age. Both LW and WSI calves had better ADG from wk 3 to 13 than EW calves. Calves in the WSI group drank less milk and ate more starter than LW calves but had similar ADG. During the period of weaning, EW calves made more unrewarded visits to the milk feeder than LW and WSI calves. Three EW calves lost weight during weaning, whereas all LW and WSI calves gained weight. Calves differ greatly in when they begin to eat solid feed and how quickly they increase the intake in response to a decrease in milk allowance. An advantage of automated feeders is that calves can be weaned at variable ages depending on their ability and willingness to eat solid feed, which reduces signs of hunger and improves weight gains during weaning. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Estimating production and consumption of solid reactive Fe phases in marine sediments from concentration profiles

EPA Science Inventory

1D diffusion models may be used to estimate rates of production and consumption of dissolved metabolites in marine sediments, but are applied less often to the solid phase. Here we used a numerical inverse method to estimate solid phase Fe(III) and Fe(II) consumption and product...

Clinical Chemistry Laboratory Automation in the 21st Century - Amat Victoria curam (Victory loves careful preparation)

PubMed Central

Armbruster, David A; Overcash, David R; Reyes, Jaime

2014-01-01

The era of automation arrived with the introduction of the AutoAnalyzer using continuous flow analysis and the Robot Chemist that automated the traditional manual analytical steps. Successive generations of stand-alone analysers increased analytical speed, offered the ability to test high volumes of patient specimens, and provided large assay menus. A dichotomy developed, with a group of analysers devoted to performing routine clinical chemistry tests and another group dedicated to performing immunoassays using a variety of methodologies. Development of integrated systems greatly improved the analytical phase of clinical laboratory testing and further automation was developed for pre-analytical procedures, such as sample identification, sorting, and centrifugation, and post-analytical procedures, such as specimen storage and archiving. All phases of testing were ultimately combined in total laboratory automation (TLA) through which all modules involved are physically linked by some kind of track system, moving samples through the process from beginning-to-end. A newer and very powerful, analytical methodology is liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS). LC-MS/MS has been automated but a future automation challenge will be to incorporate LC-MS/MS into TLA configurations. Another important facet of automation is informatics, including middleware, which interfaces the analyser software to a laboratory information systems (LIS) and/or hospital information systems (HIS). This software includes control of the overall operation of a TLA configuration and combines analytical results with patient demographic information to provide additional clinically useful information. This review describes automation relevant to clinical chemistry, but it must be recognised that automation applies to other specialties in the laboratory, e.g. haematology, urinalysis, microbiology. It is a given that automation will continue to evolve in the clinical laboratory, limited only by the imagination and ingenuity of laboratory scientists. PMID:25336760

Clinical Chemistry Laboratory Automation in the 21st Century - Amat Victoria curam (Victory loves careful preparation).

PubMed

Armbruster, David A; Overcash, David R; Reyes, Jaime

2014-08-01

The era of automation arrived with the introduction of the AutoAnalyzer using continuous flow analysis and the Robot Chemist that automated the traditional manual analytical steps. Successive generations of stand-alone analysers increased analytical speed, offered the ability to test high volumes of patient specimens, and provided large assay menus. A dichotomy developed, with a group of analysers devoted to performing routine clinical chemistry tests and another group dedicated to performing immunoassays using a variety of methodologies. Development of integrated systems greatly improved the analytical phase of clinical laboratory testing and further automation was developed for pre-analytical procedures, such as sample identification, sorting, and centrifugation, and post-analytical procedures, such as specimen storage and archiving. All phases of testing were ultimately combined in total laboratory automation (TLA) through which all modules involved are physically linked by some kind of track system, moving samples through the process from beginning-to-end. A newer and very powerful, analytical methodology is liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS). LC-MS/MS has been automated but a future automation challenge will be to incorporate LC-MS/MS into TLA configurations. Another important facet of automation is informatics, including middleware, which interfaces the analyser software to a laboratory information systems (LIS) and/or hospital information systems (HIS). This software includes control of the overall operation of a TLA configuration and combines analytical results with patient demographic information to provide additional clinically useful information. This review describes automation relevant to clinical chemistry, but it must be recognised that automation applies to other specialties in the laboratory, e.g. haematology, urinalysis, microbiology. It is a given that automation will continue to evolve in the clinical laboratory, limited only by the imagination and ingenuity of laboratory scientists.

Automated identification of best-quality coronary artery segments from multiple-phase coronary CT angiography (cCTA) for vessel analysis

NASA Astrophysics Data System (ADS)

Zhou, Chuan; Chan, Heang-Ping; Hadjiiski, Lubomir M.; Chughtai, Aamer; Wei, Jun; Kazerooni, Ella A.

2016-03-01

We are developing an automated method to identify the best quality segment among the corresponding segments in multiple-phase cCTA. The coronary artery trees are automatically extracted from different cCTA phases using our multi-scale vessel segmentation and tracking method. An automated registration method is then used to align the multiple-phase artery trees. The corresponding coronary artery segments are identified in the registered vessel trees and are straightened by curved planar reformation (CPR). Four features are extracted from each segment in each phase as quality indicators in the original CT volume and the straightened CPR volume. Each quality indicator is used as a voting classifier to vote the corresponding segments. A newly designed weighted voting ensemble (WVE) classifier is finally used to determine the best-quality coronary segment. An observer preference study is conducted with three readers to visually rate the quality of the vessels in 1 to 6 rankings. Six and 10 cCTA cases are used as training and test set in this preliminary study. For the 10 test cases, the agreement between automatically identified best-quality (AI-BQ) segments and radiologist's top 2 rankings is 79.7%, and between AI-BQ and the other two readers are 74.8% and 83.7%, respectively. The results demonstrated that the performance of our automated method was comparable to those of experienced readers for identification of the best-quality coronary segments.

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

PubMed

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.

Analysis of nitrosamines in water by automated SPE and isotope dilution GC/HRMS Occurrence in the different steps of a drinking water treatment plant, and in chlorinated samples from a reservoir and a sewage treatment plant effluent.

PubMed

Planas, Carles; Palacios, Oscar; Ventura, Francesc; Rivera, Josep; Caixach, Josep

2008-08-15

A method based on automated solid-phase extraction (SPE) and isotope dilution gas chromatography/high resolution mass spectrometry (GC/HRMS) has been developed for the analysis of nine nitrosamines in water samples. The combination of automated SPE and GC/HRMS for the analysis of nitrosamines has not been reported previously. The method shows as advantages the selectivity and sensitivity of GC/HRMS analysis and the high efficiency of automated SPE with coconut charcoal EPA 521 cartridges. Low method detection limits (MDLs) were achieved, along with a greater facility of the procedure and less dependence on the operator with regard to the methods based on manual SPE. Quality requirements for isotope dilution-based methods were accomplished for most analysed nitrosamines, regarding to trueness (80-120%), method precision (<15%) and MDLs (0.08-1.7 ng/L). Nineteen water samples (16 samples from a drinking water treatment plant {DWTP}, 2 chlorinated samples from a sewage treatment plant {STP} effluent, and 1 chlorinated sample from a reservoir) were analysed. Concentrations of nitrosamines in the STP effluent were 309.4 and 730.2 ng/L, being higher when higher doses of chlorine were applied. N-Nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA) were the main compounds identified in the STP effluent, and NDEA was detected above 200 ng/L, regulatory level for NDMA in effluents stated in Ontario (Canada). Lower concentrations of nitrosamines were found in the reservoir (20.3 ng/L) and in the DWTP samples (n.d. -28.6 ng/L). NDMA and NDEA were respectively found in the reservoir and in treated and highly chlorinated DWTP samples at concentrations above 10 ng/L (guide value established in different countries). The highest concentrations of nitrosamines were found after chlorination and ozonation processes (ozonated, treated and highly chlorinated water) in DWTP samples.

Prokaryotic expression of bone sialoprotein and identification of casein kinase II phosphorylation sites.

PubMed

Saad, Fawzy A; Salih, Erdjan; Wunderlich, Livius; Flückiger, Rudolf; Glimcher, Melvin J

2005-07-29

Bone sialoprotein is an extracellular noncollagenous acidic protein that plays a role in bone mineralization and remodeling. Its expression is restricted to mineralized tissues and is subjected to variety of posttranslational modifications including phosphorylation and glycosylation. We have expressed the full-length and half domains of bovine bone sialoprotein in a prokaryotic system and identified the phosphorylation sites of casein kinase II. The N-terminal automated solid-phase sequencing defined four phosphorylated peptides: residues 28-38 (LEDS(P)EENGVFK), 51-86 (FYPELKRFAVQSSS(P)DS(P)S(P)EENGNGDS(P)S(P)EEEEEEEETS(P)), 151-165 (EDES(P)DEEEEEEEEEE), and 295-305 (GRGYDS(P)YDGQD). Nine phosphoserines were identified within the four peptides. Seven of them were in the N-terminus (S31, S64, S66, S67, S75, S76, and S86) and two were in the C-terminus (S154 and S300) of the protein.

Quantitative Analysis and Stability of the Rodenticide TETS ...

EPA Pesticide Factsheets

Journal Article The determination of the rodenticide tetramethylenedisulfotetramine (TETS) in drinking water is reportable through the use of automated sample preparation via solid phase extraction and detection using isotope dilution gas chromatography-mass spectrometry. The method was characterized over twenty-two analytical batches with quality control samples. Accuracies for low and high concentration quality control pools were 100 and 101%, respectively. The minimum reporting level (MRL) for TETS in this method is 0.50 ug/L. Five drinking waters representing a range of water quality parameters and disinfection practices were fortified with TETS at ten times the MRL and analyzed over a 28 day period to determine the stability of TETS in these waters. The amount of TETS measured in these samples averaged 100 ± 6% of the amount fortified suggesting that tap water samples may be held for up to 28 days prior to analysis.

Synthesis of Mikto-Arm Star Peptide Conjugates.

PubMed

Koo, Jin Mo; Su, Hao; Lin, Yi-An; Cui, Honggang

2018-01-01

Mikto-arm star peptide conjugates are an emerging class of self-assembling peptide-based structural units that contain three or more auxiliary segments of different chemical compositions and/or functionalities. This group of molecules exhibit interesting self-assembly behavior in solution due to their chemically asymmetric topology. Here we describe the detailed procedure for synthesis of an ABC Mikto-arm star peptide conjugate in which two immiscible entities (a saturated hydrocarbon and a hydrophobic and lipophobic fluorocarbon) are conjugated onto a short β-sheet forming peptide sequence, GNNQQNY, derived from the Sup35 prion, through a lysine junction. Automated and manual Fmoc-solid phase synthesis techniques are used to synthesize the Mikto-arm star peptide conjugates, followed by HPLC purification. We envision that this set of protocols can afford a versatile platform to synthesize a new class of peptidic building units for diverse applications.

Process control of GMAW by detection of discontinuities in the molten weld pool

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

Carlson, N.M.; Kunerth, D.C.; Johnson, J.A.

1988-01-01

The use of ultrasonic sensors to detect discontinuities associated with the molten pool is one phase of a project to automate the welding process. In this work, ultrasonic sensors were used to interrogate the region around the molten/solid interface during gas metal arc welding (GMAW). The ultrasonic echoes from the interface and the molten pool provide information about the quality of the fusion zone and the molten pool. This information can be sent to a controller that can vary the welding parameters to correct the process. Previously ultrasonic shear waves were used to determine if the geometry of the molten/solidmore » interface was indicative of an acceptable weld. In this work, longitudinal waves were used to interrogate the molten weld pool for discontinuities. Unacceptable welding conditions that can result in porosity, incomplete penetration, or undercut were detected. 8 refs., 4 figs.« less

Thermal expansion and magnetostriction measurements at cryogenic temperature using the strain gage method

NASA Astrophysics Data System (ADS)

Wang, Wei; Liu, Huiming; Huang, Rongjin; Zhao, Yuqiang; Huang, Chuangjun; Guo, Shibin; Shan, Yi; Li, Laifeng

2018-03-01

Thermal expansion and magnetostriction, the strain responses of a material to temperature and a magnetic field, especially properties at low temperature, are extremely useful to study electronic and phononic properties, phase transitions, quantum criticality, and other interesting phenomena in cryogenic engineering and materials science. However, traditional dilatometers cannot provide magnetic field and ultra low temperature (＜77 K) environment easily. This paper describes the design and test results of thermal expansion and magnetostriction at cryogenic temperature using the strain gage method based on a Physical Properties Measurements System (PPMS). The interfacing software and automation were developed using LabVIEW. The sample temperature range can be tuned continuously between 1.8 K and 400 K. With this PPMS-aided measuring system, we can observe temperature and magnetic field dependence of the linear thermal expansion of different solid materials easily and accurately.

Automated on-line SPE LC-MS/MS method to quantitate 6beta-hydroxycortisol and cortisol in human urine: use of the 6beta-hydroxycortisol to cortisol ratio as an indicator of CYP3A4 activity.

PubMed

Barrett, Yu Chen; Akinsanya, Billy; Chang, Shu-Ying; Vesterqvist, Ole

2005-07-25

A sensitive method for quantitation of urinary 6beta-hydroxycortisol (6beta-HC) and cortisol using on-line SPE and LC-MS/MS was developed and validated. Human urine samples were injected directly onto an on-line solid phase extraction apparatus, Prospekt-2, followed by HPLC separation and electrospray triple quadrupole LC-MS/MS detection. The inter-day precision for the 6beta-HC:cortisol ratio was 7-9%. The lower limit of quantitation was 1 and 0.2 ng/mL for 6beta-HC and cortisol, respectively. Using the method we observed a diurnal variation on the 6beta-HC:cortisol ratio in healthy volunteers with the maximal ratio observed in the 2-10 pm urine collection period.

Cost assessment of the automated VERSANT 440 Molecular System versus the semi-automated System 340 bDNA Analyzer platforms.

PubMed

Elbeik, Tarek; Loftus, Richard A; Beringer, Scott

2007-11-01

Labor, supply and waste were evaluated for HIV-1 and HCV bDNA on the semi-automated System 340 bDNA Analyzer and the automated VERSANT 440 Molecular System (V440). HIV-1 sample processing was evaluated using a 24- and 48-position centrifuge rotor. Vigilance time (hands-on manipulations plus incubation time except initial target hybridization) and disposables were approximately 37 and 12% lower for HIV-1, and 64 and 31% lower for HCV bDNA, respectively, with V440. Biohazardous solid waste was approximately twofold lower for both assays and other waste types were the same for either assay on both platforms. HIV-1 sample processing vigilance time for the 48-position rotor was reduced by 2 h. V440 provides cost savings and improved workflow.

Massachusetts Institute of Technology Consortium Agreement

DTIC Science & Technology

1999-03-01

This is the third progress report of the M.I.T. Home Automation and Healthcare Consortium-Phase Two. It covers majority of the new findings, concepts...research projects of home automation and healthcare, ranging from human modeling, patient monitoring, and diagnosis to new sensors and actuators, physical...aids, human-machine interface and home automation infrastructure. This report contains several patentable concepts, algorithms, and designs.

Modulated structure and molecular dissociation of solid chlorine at high pressures

NASA Astrophysics Data System (ADS)

Li, Peifang; Gao, Guoying; Ma, Yanming

2012-08-01

Among diatomic molecular halogen solids, high pressure structures of solid chlorine (Cl2) remain elusive and least studied. We here report first-principles structural search on solid Cl2 at high pressures through our developed particle-swarm optimization algorithm. We successfully reproduced the known molecular Cmca phase (phase I) at low pressure and found that it remains stable up to a high pressure 142 GPa. At 150 GPa, our structural searches identified several energetically competitive, structurally similar, and modulated structures. Analysis of the structural results and their similarity with those in solid Br2 and I2, it was suggested that solid Cl2 adopts an incommensurate modulated structure with a modulation wave close to 2/7 in a narrow pressure range 142-157 GPa. Eventually, our simulations at >157 GPa were able to predict the molecular dissociation of solid Cl2 into monatomic phases having body centered orthorhombic (bco) and face-centered cubic (fcc) structures, respectively. One unique monatomic structural feature of solid Cl2 is the absence of intermediate body centered tetragonal (bct) structure during the bco → fcc transition, which however has been observed or theoretically predicted in solid Br2 and I2. Electron-phonon coupling calculations revealed that solid Cl2 becomes superconductors within bco and fcc phases possessing a highest superconducting temperature of 13.03 K at 380 GPa. We further probed the molecular Cmca → incommensurate phase transition mechanism and found that the softening of the Ag vibrational (rotational) Raman mode in the Cmca phase might be the driving force to initiate the transition.

NASA Tech Briefs, September 2005

NASA Technical Reports Server (NTRS)

2005-01-01

Topivs include: Diamond-Coated Carbon Nanotubes for Efficient Field Emission; Improved Anode Coatings for Direct Methanol Fuel Cells; Advanced Ablative Insulators and Methods of Making Them; PETIs as High-Temperature Resin-Transfer-Molding Materials; Stable Polyimides for Terrestrial and Space Uses; Low-Density, Aerogel-Filled Thermal-Insulation Tiles; High-Performance Polymers Having Low Melt Viscosities; Nonflammable, Hydrophobic Aerogel Composites for Insulation; Front-Side Microstrip Line Feeding a Raised Antenna Patch; Medium-Frequency Pseudonoise Georadar; Facilitating Navigation Through Large Archives; Program for Weibull Analysis of Fatigue Data; Comprehensive Micromechanics-Analysis Code - Version 4.0; Component-Based Visualization System; Software for Engineering Simulations of a Spacecraft; LabVIEW Interface for PCI-SpaceWire Interface Card; Path Following with Slip Compensation for a Mars Rover; International Space Station Electric Power System Performance Code-SPACE; Software for Automation of Real-Time Agents, Version 2; Software for Optimizing Plans Involving Interdependent Goals; Computing Gravitational Fields of Finite-Sized Bodies; Custom Sky-Image Mosaics from NASA's Information Power Grid; ANTLR Tree Grammar Generator and Extensions; Generic Kalman Filter Software; Alignment Stage for a Cryogenic Dilatometer; Rugged Iris Mechanism; Treatments To Produce Stabilized Aluminum Mirrors for Cryogenic Uses; Making AlNx Tunnel Barriers Using a Low-Energy Nitrogen-Ion Beam; Making Wide-IF SIS Mixers with Suspended Metal-Beam Leads; Sol-Gel Glass Holographic Light-Shaping Diffusers; Automated Counting of Particles To Quantify Cleanliness; Phase Correction for GPS Antenna with Nonunique Phase Center; Compact Infrasonic Windscreen; Broadband External-Cavity Diode Laser; High-Efficiency Solar Cells Using Photonic-Bandgap Materials; Generating Solid Models from Topographical Data; Computationally Lightweight Air-Traffic-Control Simulation; Spool Valve for Switching Air Flows Between Two Beds; Partial Model of Insulator/ Insulator Contact Charging; Asymmetric Electrostatic Radiation Shielding for Spacecraft; and Reusable Hybrid Propellant Modules for Outer-Space Transport.

Solid-solution CrCoCuFeNi high-entropy alloy thin films synthesized by sputter deposition

DOE PAGES

An, Zhinan; Jia, Haoling; Wu, Yueying; ...

2015-05-04

The concept of high configurational entropy requires that the high-entropy alloys (HEAs) yield single-phase solid solutions. However, phase separations are quite common in bulk HEAs. A five-element alloy, CrCoCuFeNi, was deposited via radio frequency magnetron sputtering and confirmed to be a single-phase solid solution through the high-energy synchrotron X-ray diffraction, energy-dispersive spectroscopy, wavelength-dispersive spectroscopy, and transmission electron microscopy. The formation of the solid-solution phase is presumed to be due to the high cooling rate of the sputter-deposition process.

Method for making an electrochemical cell

DOEpatents

Tuller, Harry L.; Kramer, Steve A.; Spears, Marlene A.; Pal, Uday B.

1996-01-01

An electrochemical device including a solid electrolyte and solid electrode composed of materials having different chemical compositions and characterized by different electrical properties but having the same crystalline phase is provided. A method for fabricating an electrochemical device having a solid electrode and solid electrolyte characterized by the same crystalline phase is provided.

Benefits Estimation Model for Automated Vehicle Operations: Phase 2 Final Report

DOT National Transportation Integrated Search

2018-01-01

Automated vehicles have the potential to bring about transformative safety, mobility, energy, and environmental benefits to the surface transportation system. They are also being introduced into a complex transportation system, where second-order imp...

A Description of the Phase I Automated Terminal Services Concept

DTIC Science & Technology

1976-11-01

SYSTEM FIGURE 1-2: ATS COST ELEMENTS (THOUSANDS, PER SITE ) 1-4 FIGURE 2-1: ELEMENTS FOR AUTOMATED TERMINAL SERVICE 2-2 FIGURE 2-2: ARTIST’S CONCEPTION...OF AN AUTOMATED 2-7 TERMINAL SERVICES SITE FIGURE 3-1: AUTOMATED TERMINAL SERVICES 3-3 FIGURE 3-2: ATS SERVICE REGIONS 3-5 FIGURE 3-3: RECOMMENDED...are developed (e.g., advanced control and DABS data link functions). Software and hardwa’re retrofits could be done at particular sites as system

Application of the informational reference system OZhUR to the automated processing of data from satellites of the Kosmos series

NASA Technical Reports Server (NTRS)

Pokras, V. M.; Yevdokimov, V. P.; Maslov, V. D.

1978-01-01

The structure and potential of the information reference system OZhUR designed for the automated data processing systems of scientific space vehicles (SV) is considered. The system OZhUR ensures control of the extraction phase of processing with respect to a concrete SV and the exchange of data between phases.The practical application of the system OZhUR is exemplified in the construction of a data processing system for satellites of the Cosmos series. As a result of automating the operations of exchange and control, the volume of manual preparation of data is significantly reduced, and there is no longer any need for individual logs which fix the status of data processing. The system Ozhur is included in the automated data processing system Nauka which is realized in language PL-1 in a binary one-address system one-state (BOS OS) electronic computer.

Pressure induced solid-solid reconstructive phase transition in LiGa O2 dominated by elastic strain

NASA Astrophysics Data System (ADS)

Hu, Qiwei; Yan, Xiaozhi; Lei, Li; Wang, Qiming; Feng, Leihao; Qi, Lei; Zhang, Leilei; Peng, Fang; Ohfuji, Hiroaki; He, Duanwei

2018-01-01

Pressure induced solid-solid reconstructive phase transitions for graphite-diamond, and wurtzite-rocksalt in GaN and AlN occur at significantly higher pressure than expected from equilibrium coexistence and their transition paths are always inconsistent with each other. These indicate that the underlying nucleation and growth mechanism in the solid-solid reconstructive phase transitions are poorly understood. Here, we propose an elastic-strain dominated mechanism in a reconstructive phase transition, β -LiGa O2 to γ -LiGa O2 , based on in situ high-pressure angle dispersive x-ray diffraction and single-crystal Raman scattering. This mechanism suggests that the pressure induced solid-solid reconstructive phase transition is neither purely diffusionless nor purely diffusive, as conventionally assumed, but a combination. The large elastic strains are accumulated, with the coherent nucleation, in the early stage of the transition. The elastic strains along the 〈100 〉 and 〈001 〉 directions are too large to be relaxed by the shear stress, so an intermediate structure emerges reducing the elastic strains and making the transition energetically favorable. At higher pressures, when the elastic strains become small enough to be relaxed, the phase transition to γ -LiGa O2 begins and the coherent nucleation is substituted with a semicoherent one with Li and Ga atoms disordered.

Simple and rapid analysis of endocrine disruptors in liquid medicines and intravenous injection solutions by automated in-tube solid-phase microextraction/high performance liquid chromatography.

PubMed

Mitani, Kurie; Narimatsu, Shizuo; Izushi, Fumio; Kataoka, Hiroyuki

2003-07-14

A simple and rapid method was developed for analyzing contamination of endocrine disruptors in liquid medicines and intravenous injection solutions. Endocrine disrupting compounds such as bisphenol A (BPA), alkylphenols and phthalates were quantitated by on-line in-tube solid-phase microextraction coupled with high performance liquid chromatography (in-tube SPME/HPLC) with UV detection. The liquid medicines and intravenous injection solutions could be used directly without any pretreatment, and the BPA, alkylphenols and phthalates in these solutions were automatically analyzed. The limits of quantification for these compounds were 1-10 ng/ml. Recoveries of these compounds spiked to the intravenous injection solutions was over 80%, except for some phthalates. Di-n-butyl phthalate (DBP) was detected at a concentration of 7-60 ng/ml in most intravenous injection solutions in plastic containers, but it was not detected in solutions in glass bottles. Diethyl phthalate, di-n-propyl phthalate, DBP and di-2-ethylhexyl phthalate (DEHP) were also detected in syrup, lotion and eye drops in plastic containers. On the other hand, BPA and alkylphenols were not detected at all in these solutions. DEHP contamination from an administration set increased when total vitamin formulation was added to the infusion solution. DEHP was easily leached from polyvinyl chloride tubing by polysorbate 80. The in-tube SPME/HPLC method is simple, rapid and automatic, and it provides a useful tool for the screening and determination of endocrine disruptor contamination in liquid medicines and intravenous injection solutions.

Comparison of the solid-phase extraction efficiency of a bounded and an included cyclodextrin-silica microporous composite for polycyclic aromatic hydrocarbons determination in water samples.

PubMed

Mauri-Aucejo, Adela; Amorós, Pedro; Moragues, Alaina; Guillem, Carmen; Belenguer-Sapiña, Carolina

2016-08-15

Solid-phase extraction is one of the most important techniques for sample purification and concentration. A wide variety of solid phases have been used for sample preparation over time. In this work, the efficiency of a new kind of solid-phase extraction adsorbent, which is a microporous material made from modified cyclodextrin bounded to a silica network, is evaluated through an analytical method which combines solid-phase extraction with high-performance liquid chromatography to determine polycyclic aromatic hydrocarbons in water samples. Several parameters that affected the analytes recovery, such as the amount of solid phase, the nature and volume of the eluent or the sample volume and concentration influence have been evaluated. The experimental results indicate that the material possesses adsorption ability to the tested polycyclic aromatic hydrocarbons. Under the optimum conditions, the quantification limits of the method were in the range of 0.09-2.4μgL(-1) and fine linear correlations between peak height and concentration were found around 1.3-70μgL(-1). The method has good repeatability and reproducibility, with coefficients of variation under 8%. Due to the concentration results, this material may represent an alternative for trace analysis of polycyclic aromatic hydrocarbons in water trough solid-phase extraction. Copyright © 2016 Elsevier B.V. All rights reserved.

The Iron-Iron Carbide Phase Diagram: A Practical Guide to Some Descriptive Solid State Chemistry.

ERIC Educational Resources Information Center

Long, Gary J.; Leighly, H. P., Jr.

1982-01-01

Discusses the solid state chemistry of iron and steel in terms of the iron-iron carbide phase diagram. Suggests that this is an excellent way of introducing the phase diagram (equilibrium diagram) to undergraduate students while at the same time introducing the descriptive solid state chemistry of iron and steel. (Author/JN)

Automated classification of cell morphology by coherence-controlled holographic microscopy

NASA Astrophysics Data System (ADS)

Strbkova, Lenka; Zicha, Daniel; Vesely, Pavel; Chmelik, Radim

2017-08-01

In the last few years, classification of cells by machine learning has become frequently used in biology. However, most of the approaches are based on morphometric (MO) features, which are not quantitative in terms of cell mass. This may result in poor classification accuracy. Here, we study the potential contribution of coherence-controlled holographic microscopy enabling quantitative phase imaging for the classification of cell morphologies. We compare our approach with the commonly used method based on MO features. We tested both classification approaches in an experiment with nutritionally deprived cancer tissue cells, while employing several supervised machine learning algorithms. Most of the classifiers provided higher performance when quantitative phase features were employed. Based on the results, it can be concluded that the quantitative phase features played an important role in improving the performance of the classification. The methodology could be valuable help in refining the monitoring of live cells in an automated fashion. We believe that coherence-controlled holographic microscopy, as a tool for quantitative phase imaging, offers all preconditions for the accurate automated analysis of live cell behavior while enabling noninvasive label-free imaging with sufficient contrast and high-spatiotemporal phase sensitivity.

Automated classification of cell morphology by coherence-controlled holographic microscopy.

PubMed

Strbkova, Lenka; Zicha, Daniel; Vesely, Pavel; Chmelik, Radim

2017-08-01

In the last few years, classification of cells by machine learning has become frequently used in biology. However, most of the approaches are based on morphometric (MO) features, which are not quantitative in terms of cell mass. This may result in poor classification accuracy. Here, we study the potential contribution of coherence-controlled holographic microscopy enabling quantitative phase imaging for the classification of cell morphologies. We compare our approach with the commonly used method based on MO features. We tested both classification approaches in an experiment with nutritionally deprived cancer tissue cells, while employing several supervised machine learning algorithms. Most of the classifiers provided higher performance when quantitative phase features were employed. Based on the results, it can be concluded that the quantitative phase features played an important role in improving the performance of the classification. The methodology could be valuable help in refining the monitoring of live cells in an automated fashion. We believe that coherence-controlled holographic microscopy, as a tool for quantitative phase imaging, offers all preconditions for the accurate automated analysis of live cell behavior while enabling noninvasive label-free imaging with sufficient contrast and high-spatiotemporal phase sensitivity. (2017) COPYRIGHT Society of Photo-Optical Instrumentation Engineers (SPIE).

Space station advanced automation

NASA Technical Reports Server (NTRS)

Woods, Donald

1990-01-01

In the development of a safe, productive and maintainable space station, Automation and Robotics (A and R) has been identified as an enabling technology which will allow efficient operation at a reasonable cost. The Space Station Freedom's (SSF) systems are very complex, and interdependent. The usage of Advanced Automation (AA) will help restructure, and integrate system status so that station and ground personnel can operate more efficiently. To use AA technology for the augmentation of system management functions requires a development model which consists of well defined phases of: evaluation, development, integration, and maintenance. The evaluation phase will consider system management functions against traditional solutions, implementation techniques and requirements; the end result of this phase should be a well developed concept along with a feasibility analysis. In the development phase the AA system will be developed in accordance with a traditional Life Cycle Model (LCM) modified for Knowledge Based System (KBS) applications. A way by which both knowledge bases and reasoning techniques can be reused to control costs is explained. During the integration phase the KBS software must be integrated with conventional software, and verified and validated. The Verification and Validation (V and V) techniques applicable to these KBS are based on the ideas of consistency, minimal competency, and graph theory. The maintenance phase will be aided by having well designed and documented KBS software.

An Investigation into the Polymorphism and Crystallization of Levetiracetam and the Stability of its Solid Form.

PubMed

Xu, Kailin; Xiong, Xinnuo; Guo, Liuqi; Wang, Lili; Li, Shanshan; Tang, Peixiao; Yan, Jin; Wu, Di; Li, Hui

2015-12-01

Levetiracetam (LEV) crystals were prepared using different solvents at different temperatures. The LEV crystals were systematically characterized by X-ray powder diffraction (XRPD) and morphological analysis. The results indicated that many kinds of crystal habits exist in a solid form of LEV. To investigate the effects of LEV concentration, crystallization temperature, and crystallization type on crystallization and solid phase transformation of LEV, multiple methods were performed for LEV aqueous solution to determine if a new solid form exists in solid-state LEV. However, XRPD data demonstrate that the LEV solid forms possess same spatial arrangements that are similar to the original solid form. This result indicates that the LEV concentration, crystallization temperature, and crystallization type in aqueous solution have no influence on the crystallization and solid phase transformation of LEV. Moreover, crystallization by sublimation, melt cooling, and quench cooling, as well as mechanical effect, did not result in the formation of new LEV solid state. During melt cooling, the transformation of solid form LEV is a direct process from melting amorphous phase to the original LEV crystal phase, and the conversion rate is very quick. In addition, stability investigation manifested that LEV solid state is very stable under various conditions. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Autovalidation and automation of the postanalytical phase of routine hematology and coagulation analyses in a university hospital laboratory.

PubMed

Mlinaric, Ana; Milos, Marija; Coen Herak, Désirée; Fucek, Mirjana; Rimac, Vladimira; Zadro, Renata; Rogic, Dunja

2018-02-23

The need to satisfy high-throughput demands for laboratory tests continues to be a challenge. Therefore, we aimed to automate postanalytical phase in hematology and coagulation laboratory by autovalidation of complete blood count (CBC) and routine coagulation test results (prothrombin time [PT], international normalized ratio [PT-INR], activated partial thromboplastin time [APTT], fibrinogen, antithrombin activity [AT] and thrombin time [TT]). Work efficacy and turnaround time (TAT) before and after implementation of automated solutions will be compared. Ordering panels tailored to specific patient populations were implemented. Rerun and reflex testing rules were set in the respective analyzers' software (Coulter DxH Connectivity 1601, Beckman Coulter, FL, USA; AutoAssistant, Siemens Healthcare Diagnostics, Germany), and sample status information was transferred into the laboratory information system. To evaluate if the automation improved TAT and efficacy, data from manually verified results in September and October of 2015 were compared with the corresponding period in 2016 when autovalidation was implemented. Autovalidation rates of 63% for CBC and 65% for routine coagulation test results were achieved. At the TAT of 120 min, the percentage of reported results increased substantially for all analyzed tests, being above 90% for CBC, PT, PT-INR and fibrinogen and 89% for APTT. This output was achieved with three laboratory technicians less compared with the period when the postanalytical phase was not automated. Automation allowed optimized laboratory workflow for specific patient populations, thereby ensuring standardized results reporting. Autovalidation of test results proved to be an efficient tool for improvement of laboratory work efficacy and TAT.

Building of Equations of State with Numerous Phase Transitions — Application to Bismuth

NASA Astrophysics Data System (ADS)

Heuzé, Olivier

2006-07-01

We propose an algorithm to build complete equation of state EOS including several solid/solid or solid/liquid phase transitions. Each phase has its own EOS and independent parameters. The phase diagram is deduced from the thermodynamic equilibrium assumption. Until now, such an approach was used in simple cases and limited to 2 or 3 phases. We have applied it in the general case to bismuth for which up to 13 phases have been identified. This study shows the great influence of binary mixtures and triple points properties in released isentropes after shock waves.

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

PubMed

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/n<0.154 systems freeze into the face centered cubic (fcc) 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.

Human factors phase III : effects of train control technology on operator performance

DOT National Transportation Integrated Search

2005-01-01

This report describes a study evaluating the effects of train control technology on locomotive engineer performance. Several types : of train control systems were evaluated: partial automation (cruise control and programmed stop) and full automation ...

Automating Small Libraries.

ERIC Educational Resources Information Center

Swan, James

1996-01-01

Presents a four-phase plan for small libraries strategizing for automation: inventory and weeding, data conversion, implementation, and enhancements. Other topics include selecting a system, MARC records, compatibility, ease of use, industry standards, searching capabilities, support services, system security, screen displays, circulation modules,…

Human factors phase III : effects of train control technology on operator performance.

DOT National Transportation Integrated Search

2005-01-31

This report describes a study evaluating the effects of train control technology on locomotive engineer performance. Several types of train control systems were evaluated: partial automation (cruise control and programmed stop) and full automation we...

Assessment of Operational Automated Guideway Systems - Airtrans (Phase I)

DOT National Transportation Integrated Search

1976-09-01

This report presents the results of an evaluation study of AIRTRANS, a unique, automated guideway system located at the Dallas/Fort Worth Airport. AIRTRANS was designed to move passengers, employees, baggage, mail, trash and supplies. The newest and ...

Two-phase anaerobic digestion of vegetable market waste fraction of municipal solid waste and development of improved technology for phase separation in two-phase reactor.

PubMed

Majhi, Bijoy Kumar; Jash, Tushar

2016-12-01

Biogas production from vegetable market waste (VMW) fraction of municipal solid waste (MSW) by two-phase anaerobic digestion system should be preferred over the single-stage reactors. This is because VMW undergoes rapid acidification leading to accumulation of volatile fatty acids and consequent low pH resulting in frequent failure of digesters. The weakest part in the two-phase anaerobic reactors was the techniques applied for solid-liquid phase separation of digestate in the first reactor where solubilization, hydrolysis and acidogenesis of solid organic waste occur. In this study, a two-phase reactor which consisted of a solid-phase reactor and a methane reactor was designed, built and operated with VMW fraction of Indian MSW. A robust type filter, which is unique in its implementation method, was developed and incorporated in the solid-phase reactor to separate the process liquid produced in the first reactor. Experiments were carried out to assess the long term performance of the two-phase reactor with respect to biogas production, volatile solids reduction, pH and number of occurrence of clogging in the filtering system or choking in the process liquid transfer line. The system performed well and was operated successfully without the occurrence of clogging or any other disruptions throughout. Biogas production of 0.86-0.889m 3 kg -1 VS, at OLR of 1.11-1.585kgm -3 d -1 , were obtained from vegetable market waste, which were higher than the results reported for similar substrates digested in two-phase reactors. The VS reduction was 82-86%. The two-phase anaerobic digestion system was demonstrated to be stable and suitable for the treatment of VMW fraction of MSW for energy generation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Mechanism and microstructures in Ga2O3 pseudomartensitic solid phase transition.

PubMed

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 product crystallinity of solid phase transition. The new knowledge on the kinetics of pseudomartensitic transition complements the theory of diffusionless solid phase transition.

Thermodynamic Investigation of the Effect of Interface Curvature on the Solid-Liquid Equilibrium and Eutectic Point of Binary Mixtures.

PubMed

Liu, Fanghui; Zargarzadeh, Leila; Chung, Hyun-Joong; Elliott, Janet A W

2017-10-12

Thermodynamic phase behavior is affected by curved interfaces in micro- and nanoscale systems. For example, capillary freezing point depression is associated with the pressure difference between the solid and liquid phases caused by interface curvature. In this study, the thermal, mechanical, and chemical equilibrium conditions are derived for binary solid-liquid equilibrium with a curved solid-liquid interface due to confinement in a capillary. This derivation shows the equivalence of the most general forms of the Gibbs-Thomson and Ostwald-Freundlich equations. As an example, the effect of curvature on solid-liquid equilibrium is explained quantitatively for the water/glycerol system. Considering the effect of a curved solid-liquid interface, a complete solid-liquid phase diagram is developed over a range of concentrations for the water/glycerol system (including the freezing of pure water or precipitation of pure glycerol depending on the concentration of the solution). This phase diagram is compared with the traditional phase diagram in which the assumption of a flat solid-liquid interface is made. We show the extent to which nanoscale interface curvature can affect the composition-dependent freezing and precipitating processes, as well as the change in the eutectic point temperature and concentration with interface curvature. Understanding the effect of curvature on solid-liquid equilibrium in nanoscale capillaries has applications in the food industry, soil science, cryobiology, nanoporous materials, and various nanoscience fields.

Suppressing the cellular breakdown in silicon supersaturated with titanium

NASA Astrophysics Data System (ADS)

Liu, Fang; Prucnal, S.; Hübner, R.; Yuan, Ye; Skorupa, W.; Helm, M.; Zhou, Shengqiang

2016-06-01

Hyper doping Si with up to 6 at.% Ti in solid solution was performed by ion implantation followed by pulsed laser annealing and flash lamp annealing. In both cases, the implanted Si layer can be well recrystallized by liquid phase epitaxy and solid phase epitaxy, respectively. Cross-sectional transmission electron microscopy of Ti-implanted Si after liquid phase epitaxy shows the so-called growth interface breakdown or cellular breakdown owing to the occurrence of constitutional supercooling in the melt. The appearance of cellular breakdown prevents further recrystallization. However, the out-diffusion and cellular breakdown can be effectively suppressed by solid phase epitaxy during flash lamp annealing due to the high velocity of amorphous-crystalline interface and the low diffusion velocity for Ti in the solid phase.

Comparing the catalytic oxidation of ethanol at the solid-gas and solid-liquid interfaces over size-controlled Pt nanoparticles: striking differences in kinetics and mechanism.

PubMed

Sapi, Andras; Liu, Fudong; Cai, Xiaojun; Thompson, Christopher M; Wang, Hailiang; An, Kwangjin; Krier, James M; Somorjai, Gabor A

2014-11-12

Pt nanoparticles with controlled size (2, 4, and 6 nm) are synthesized and tested in ethanol oxidation by molecular oxygen at 60 °C to acetaldehyde and carbon dioxide both in the gas and liquid phases. The turnover frequency of the reaction is ∼80 times faster, and the activation energy is ∼5 times higher at the gas-solid interface compared to the liquid-solid interface. The catalytic activity is highly dependent on the size of the Pt nanoparticles; however, the selectivity is not size sensitive. Acetaldehyde is the main product in both media, while twice as much carbon dioxide was observed in the gas phase compared to the liquid phase. Added water boosts the reaction in the liquid phase; however, it acts as an inhibitor in the gas phase. The more water vapor was added, the more carbon dioxide was formed in the gas phase, while the selectivity was not affected by the concentration of the water in the liquid phase. The differences in the reaction kinetics of the solid-gas and solid-liquid interfaces can be attributed to the molecular orientation deviation of the ethanol molecules on the Pt surface in the gas and liquid phases as evidenced by sum frequency generation vibrational spectroscopy.

Distinguishing molecular environments in supported Pt catalysts and their influences on activity and selectivity

NASA Astrophysics Data System (ADS)

Jones, Louis Chin

This thesis entails the synthesis, automated catalytic testing, and in situ molecular characterization of supported Pt and Pt-alloy nanoparticle (NP) catalysts, with emphasis on how to assess the molecular distributions of Pt environments that are affecting overall catalytic activity and selectivity. We have taken the approach of (a) manipulating nucleation and growth of NPs using oxide supports, surfactants, and inorganic complexes to create Pt NPs with uniform size, shape, and composition, (b) automating batch and continuous flow catalytic reaction tests, and (c) characterizing the molecular environments of Pt surfaces using in situ infrared (IR) spectroscopy and solid-state 195Pt NMR. The following will highlight the synthesis and characterization of Ag-doped Pt NPs and their influence on C 2H2 hydrogenation selectivity, and the implementation of advanced solid-state 195Pt NMR techniques to distinguish how distributions of molecular Pt environments vary with nanoparticle size, support, and surface composition.

Automated contact angle estimation for three-dimensional X-ray microtomography data

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

Klise, Katherine A.; Moriarty, Dylan; Yoon, Hongkyu

2015-11-10

Multiphase flow in capillary regimes is a fundamental process in a number of geoscience applications. The ability to accurately define wetting characteristics of porous media can have a large impact on numerical models. In this paper, a newly developed automated three-dimensional contact angle algorithm is described and applied to high-resolution X-ray microtomography data from multiphase bead pack experiments with varying wettability characteristics. The algorithm calculates the contact angle by finding the angle between planes fit to each solid/fluid and fluid/fluid interface in the region surrounding each solid/fluid/fluid contact point. Results show that the algorithm is able to reliably compute contactmore » angles using the experimental data. The in situ contact angles are typically larger than flat surface laboratory measurements using the same material. Furthermore, wetting characteristics in mixed-wet systems also change significantly after displacement cycles.« less

Improved ablative materials for the ASRM nozzle

NASA Technical Reports Server (NTRS)

Canfield, A.; Clinton, R. G.; Armour, W.; Koenig, J.

1992-01-01

Rayon precursor carbon-cloth phenolic was developed more than 30 years ago and is used in most nozzles today including the Poseidon, Trident, Peacekeeper, Small ICBM, Space Shuttle, and numerous tactical and space systems. Specifications and manufacturing controls were placed on these materials and, once qualified, a no-change policy was instituted. The current material is acceptable; however, prepreg variability does not always accommodate the requirements of automation. The advanced solid rocket motor requires material with less variability for automated manufacturing. An advanced solid rocket motor materials team, composed of NASA, Thiokol, Aerojet, SRI, and Lockheed specialists, along with materials suppliers ICI Fiberite/Polycarbon, BP Chemicals/Hitco, and Amoco, embarked on a program to improve the current materials. The program consisted of heat treatment studies and standard and low-density material improvements evaluation. Improvements evaluated included fiber/fabric heat treatments, weave variations, resin application methods, process controls, and monitors.

A High-Throughput Process for the Solid-Phase Purification of Synthetic DNA Sequences

PubMed Central

Grajkowski, Andrzej; Cieślak, Jacek; Beaucage, Serge L.

2017-01-01

An efficient process for the purification of synthetic phosphorothioate and native DNA sequences is presented. The process is based on the use of an aminopropylated silica gel support functionalized with aminooxyalkyl functions to enable capture of DNA sequences through an oximation reaction with the keto function of a linker conjugated to the 5′-terminus of DNA sequences. Deoxyribonucleoside phosphoramidites carrying this linker, as a 5′-hydroxyl protecting group, have been synthesized for incorporation into DNA sequences during the last coupling step of a standard solid-phase synthesis protocol executed on a controlled pore glass (CPG) support. Solid-phase capture of the nucleobase- and phosphate-deprotected DNA sequences released from the CPG support is demonstrated to proceed near quantitatively. Shorter than full-length DNA sequences are first washed away from the capture support; the solid-phase purified DNA sequences are then released from this support upon reaction with tetra-n-butylammonium fluoride in dry dimethylsulfoxide (DMSO) and precipitated in tetrahydrofuran (THF). The purity of solid-phase-purified DNA sequences exceeds 98%. The simulated high-throughput and scalability features of the solid-phase purification process are demonstrated without sacrificing purity of the DNA sequences. PMID:28628204

Nanostructured lipid carriers: effect of solid phase fraction and distribution on the release of encapsulated materials.

PubMed

Dan, Nily

2014-11-25

Emulsions, solid lipid nanoparticles (SLN), and nanostructured lipid carriers (NLC) containing a mix of liquid and solid domains are of interest as encapsulation vehicles for hydrophobic compounds. Studies of the release rate from these particles yield contradictory results: Some find that increasing the fraction of solid phase increases the rate of release and others the opposite. In this paper we study the release of encapsulated materials from lipid-based nanoparticles using Monte Carlo simulations. We find that, quite surprisingly, the release rate is largely insensitive to the size of solid domains or the fraction of solid phase. However, the distribution of the domains significantly affects the rate of release: Solid domains located at the interface with the surrounding solution inhibit transport, while nanoparticles where the solid domains are concentrated in the center enhance it. The latter can lead to release rates in NLCs that are faster than in the equivalent emulsions. We conclude that controlling the release rate from NLCs requires the ability to determine the location and distribution of the solid phase, which may be achieved through choice of the surfactants stabilizing the particles, incorporation of nucleation sites, and/or the cooling rates and temperatures.

Solid phase stability of molybdenum under compression: Sound velocity measurements and first-principles calculations

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

Zhang, Xiulu; Laboratory for Extreme Conditions Matter Properties, Southwest University of Science and Technology, 621010 Mianyang, Sichuan; Liu, Zhongli

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 themore » 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.« less

Determination of trace zinc in seawater by coupling solid phase extraction and fluorescence detection in the Lab-On-Valve format.

PubMed

Grand, Maxime M; Chocholouš, Petr; Růžička, Jarda; Solich, Petr; Measures, Christopher I

2016-06-07

By virtue of their compactness, long-term stability, minimal reagent consumption and robustness, miniaturized sequential injection instruments are well suited for automation of assays onboard research ships. However, in order to reach the sensitivity and limit of detection required for open-ocean determinations of trace elements, it is necessary to preconcentrate the analyte prior its derivatization and subsequent detection by fluorescence. In this work, a novel method for the determination of dissolved zinc (Zn) at subnanomolar levels in seawater is described. The proposed method combines, for the first time, automated matrix removal, extraction of the target element, and fluorescence detection within a miniaturized flow manifold, based on the Lab-On-Valve (LOV) concept. The key feature of the microfluidic manipulation of the sample is flow programming, designed to pass sample through a mini-column where the target analyte and other complexable cations are retained, while the seawater matrix is washed out. Next, zinc is eluted and merged with a Zn selective fluorescent probe (FluoZin-3) at the confluence point of the LOV central channel using two high-precision stepper motor driven pumps that are operated in concert. Finally, the thus formed Zn complex is transported to the LOV flow cell for selective fluorescence measurement. This work describes the characterization and optimization of the method including Solid Phase Extraction using the Toyopearl AF-Chelate-650M resin, and detailed assay protocol controlled by a commercially available software and instrument. The proposed method features a LOD of 0.02 nM, high precision (<3% at 0.1 and 2 nM Zn levels), an assay cycle of 13 min and a reagent consumption of 150 μL FluoZin-3 per sample, which makes the method highly suitable for oceanographic shipboard analysis. The accuracy of the method has been validated through the analysis of seawater reference standards and comparison with ICP-MS determinations on seawater samples collected in the upper 1300 m of the subtropical south Indian Ocean. This work confirms that integration of sample pretreatment with optical detection in the LOV format offers a widely applicable approach to trace analysis of seawater. Copyright © 2016. Published by Elsevier B.V.

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.

PubMed

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 as simplicity, automation and sensitivity, required for the monitoring programs linked to the WFD. Copyright © 2015 Elsevier B.V. All rights reserved.

Communication: phase transitions, criticality, and three-phase coexistence in constrained cell models.

PubMed

Nayhouse, Michael; Kwon, Joseph Sang-Il; Orkoulas, G

2012-05-28

In simulation studies of fluid-solid transitions, the solid phase is usually modeled as a constrained system in which each particle is confined to move in a single Wigner-Seitz cell. The constrained cell model has been used in the determination of fluid-solid coexistence via thermodynamic integration and other techniques. In the present work, the phase diagram of such a constrained system of Lennard-Jones particles is determined from constant-pressure simulations. The pressure-density isotherms exhibit inflection points which are interpreted as the mechanical stability limit of the solid phase. The phase diagram of the constrained system contains a critical and a triple point. The temperature and pressure at the critical and the triple point are both higher than those of the unconstrained system due to the reduction in the entropy caused by the single occupancy constraint.

Modeling of Shock Waves with Multiple Phase Transitions in Condensed Materials

NASA Astrophysics Data System (ADS)

Missonnier, Marc; Heuzé, Olivier

2006-07-01

When a shock wave crosses a solid material and subjects it to solid-solid or solid-liquid phase transition, related phenomena occur: shock splitting, and the corresponding released shock wave after reflection. Modelling of these phenomena raises physical and numerical issues. After shock loading, such materials can reach different kinds of states: single-phase states, binary-phase states, and triple points. The thermodynamic path can be studied and easily understood in the (V,E) or (V,S) planes. In the case of 3 phase tin (β,γ, and liquid) submitted to shock waves, seven states can occur: β,γ, liquid, β-γ, β-liquid, γ-liquid, and β-γ-liquid. After studying the thermodynamic properties with a complete 3-phase Equation of State, we show the existence of these seven states with a hydrodynamic simulation.

Optimization of the β-Elimination/Michael Addition Chemistry on Reversed-Phase Supports for Mass Spectrometry Analysis of O-Linked Protein Modifications

PubMed Central

Nika, Heinz; Nieves, Edward; Hawke, David H.; Angeletti, Ruth Hogue

2013-01-01

We previously adapted the β-elimination/Michael addition chemistry to solid-phase derivatization on reversed-phase supports, and demonstrated the utility of this reaction format to prepare phosphoseryl peptides in unfractionated protein digests for mass spectrometric identification and facile phosphorylation-site determination. Here, we have expanded the use of this technique to β-N-acetylglucosamine peptides, modified at serine/threonine, phosphothreonyl peptides, and phosphoseryl/phosphothreonyl peptides, followed in sequence by proline. The consecutive β-elimination with Michael addition was adapted to optimize the solid-phase reaction conditions for throughput and completeness of derivatization. The analyte remained intact during derivatization and was recovered efficiently from the silica-based, reversed-phase support with minimal sample loss. The general use of the solid-phase approach for enzymatic dephosphorylation was demonstrated with phosphoseryl and phosphothreonyl peptides and was used as an orthogonal method to confirm the identity of phosphopeptides in proteolytic mixtures. The solid-phase approach proved highly suitable to prepare substrates from low-level amounts of protein digests for phosphorylation-site determination by chemical-targeted proteolysis. The solid-phase protocol provides for a simple, robust, and efficient tool to prepare samples for phosphopeptide identification in MALDI mass maps of unfractionated protein digests, using standard equipment available in most biological laboratories. The use of a solid-phase analytical platform is expected to be readily expanded to prepare digest from O-glycosylated- and O-sulfonated proteins for mass spectrometry-based structural characterization. PMID:23997661

Equations of State and Phase Diagrams of Ammonia

ERIC Educational Resources Information Center

Glasser, Leslie

2009-01-01

We present equations of state relating the phases and a three-dimensional phase diagram for ammonia with its solid, liquid, and vapor phases, based on fitted authentic experimental data and including recent information on the high-pressure solid phases. This presentation follows similar articles on carbon dioxide and water published in this…

Automation of static and dynamic non-dispersive liquid phase microextraction. Part 2: Approaches based on impregnated membranes and porous supports.

PubMed

Alexovič, Michal; Horstkotte, Burkhard; Solich, Petr; Sabo, Ján

2016-02-11

A critical overview on automation of modern liquid phase microextraction (LPME) approaches based on the liquid impregnation of porous sorbents and membranes is presented. It is the continuation of part 1, in which non-dispersive LPME techniques based on the use of the extraction phase (EP) in the form of drop, plug, film, or microflow have been surveyed. Compared to the approaches described in part 1, porous materials provide an improved support for the EP. Simultaneously they allow to enlarge its contact surface and to reduce the risk of loss by incident flow or by components of surrounding matrix. Solvent-impregnated membranes or hollow fibres are further ideally suited for analyte extraction with simultaneous or subsequent back-extraction. Their use can therefore improve the procedure robustness and reproducibility as well as it "opens the door" to the new operation modes and fields of application. However, additional work and time are required for membrane replacement and renewed impregnation. Automation of porous support-based and membrane-based approaches plays an important role in the achievement of better reliability, rapidness, and reproducibility compared to manual assays. Automated renewal of the extraction solvent and coupling of sample pretreatment with the detection instrumentation can be named as examples. The different LPME methodologies using impregnated membranes and porous supports for the extraction phase and the different strategies of their automation, and their analytical applications are comprehensively described and discussed in this part. Finally, an outlook on future demands and perspectives of LPME techniques from both parts as a promising area in the field of sample pretreatment is given. Copyright © 2015 Elsevier B.V. All rights reserved.

Automating Electronic Clinical Data Capture for Quality Improvement and Research: The CERTAIN Validation Project of Real World Evidence.

PubMed

Devine, Emily Beth; Van Eaton, Erik; Zadworny, Megan E; Symons, Rebecca; Devlin, Allison; Yanez, David; Yetisgen, Meliha; Keyloun, Katelyn R; Capurro, Daniel; Alfonso-Cristancho, Rafael; Flum, David R; Tarczy-Hornoch, Peter

2018-05-22

The availability of high fidelity electronic health record (EHR) data is a hallmark of the learning health care system. Washington State's Surgical Care Outcomes and Assessment Program (SCOAP) is a network of hospitals participating in quality improvement (QI) registries wherein data are manually abstracted from EHRs. To create the Comparative Effectiveness Research and Translation Network (CERTAIN), we semi-automated SCOAP data abstraction using a centralized federated data model, created a central data repository (CDR), and assessed whether these data could be used as real world evidence for QI and research. Describe the validation processes and complexities involved and lessons learned. Investigators installed a commercial CDR to retrieve and store data from disparate EHRs. Manual and automated abstraction systems were conducted in parallel (10/2012-7/2013) and validated in three phases using the EHR as the gold standard: 1) ingestion, 2) standardization, and 3) concordance of automated versus manually abstracted cases. Information retrieval statistics were calculated. Four unaffiliated health systems provided data. Between 6 and 15 percent of data elements were abstracted: 51 to 86 percent from structured data; the remainder using natural language processing (NLP). In phase 1, data ingestion from 12 out of 20 feeds reached 95 percent accuracy. In phase 2, 55 percent of structured data elements performed with 96 to 100 percent accuracy; NLP with 89 to 91 percent accuracy. In phase 3, concordance ranged from 69 to 89 percent. Information retrieval statistics were consistently above 90 percent. Semi-automated data abstraction may be useful, although raw data collected as a byproduct of health care delivery is not immediately available for use as real world evidence. New approaches to gathering and analyzing extant data are required.

Automated delay estimation at signalized intersections : phase I concept and algorithm development.

DOT National Transportation Integrated Search

2011-07-01

Currently there are several methods to measure the performance of surface streets, but their capabilities in dynamically estimating vehicle delay are limited. The objective of this research is to develop a method to automate traffic delay estimation ...

Molecular orientation of organic thin films on dielectric solid substrates: a phase-sensitive vibrational SFG study.

PubMed

Ge, Aimin; Peng, Qiling; Qiao, Lin; Yepuri, Nageshwar R; Darwish, Tamim A; Matsusaki, Michiya; Akashi, Mitsuru; Ye, Shen

2015-07-21

Broadband phase-sensitive vibrational sum frequency generation (SFG) spectroscopy was utilized to study the molecular orientation of molecules adsorbed on dielectric solid substrates. A gold thin film was employed to generate a SFG signal as a local oscillator (LO). To simplify the phase measurement, a self-assembled monolayer (SAM) of octadecyltrichlorosilane (OTS) was used as a standard sample for phase correction of the phase-sensitive SFG measurements on the solid/air interface. It was demonstrated that the absolute orientation of molecules in the LB films on a fused quartz surface can be clearly distinguished by phase-sensitive SFG measurement. In addition, the observation on the SAM of d35-OTS reveals that the two C-H stretching modes for α-CH2 group are in opposite phase. Furthermore, by using the present phase-sensitive SFG setup, the orientation flipping of water molecules on positively and negatively charged solid/liquid interface can be distinguished.

Automation of Hubble Space Telescope Mission Operations

NASA Technical Reports Server (NTRS)

Burley, Richard; Goulet, Gregory; Slater, Mark; Huey, William; Bassford, Lynn; Dunham, Larry

2012-01-01

On June 13, 2011, after more than 21 years, 115 thousand orbits, and nearly 1 million exposures taken, the operation of the Hubble Space Telescope successfully transitioned from 24x7x365 staffing to 815 staffing. This required the automation of routine mission operations including telemetry and forward link acquisition, data dumping and solid-state recorder management, stored command loading, and health and safety monitoring of both the observatory and the HST Ground System. These changes were driven by budget reductions, and required ground system and onboard spacecraft enhancements across the entire operations spectrum, from planning and scheduling systems to payload flight software. Changes in personnel and staffing were required in order to adapt to the new roles and responsibilities required in the new automated operations era. This paper will provide a high level overview of the obstacles to automating nominal HST mission operations, both technical and cultural, and how those obstacles were overcome.

Space environments and their effects on space automation and robotics

NASA Technical Reports Server (NTRS)

Garrett, Henry B.

1990-01-01

Automated and robotic systems will be exposed to a variety of environmental anomalies as a result of adverse interactions with the space environment. As an example, the coupling of electrical transients into control systems, due to EMI from plasma interactions and solar array arcing, may cause spurious commands that could be difficult to detect and correct in time to prevent damage during critical operations. Spacecraft glow and space debris could introduce false imaging information into optical sensor systems. The presentation provides a brief overview of the primary environments (plasma, neutral atmosphere, magnetic and electric fields, and solid particulates) that cause such adverse interactions. The descriptions, while brief, are intended to provide a basis for the other papers presented at this conference which detail the key interactions with automated and robotic systems. Given the growing complexity and sensitivity of automated and robotic space systems, an understanding of adverse space environments will be crucial to mitigating their effects.

Enhancing reproducibility of ultrasonic measurements by new users

NASA Astrophysics Data System (ADS)

Pramanik, Manojit; Gupta, Madhumita; Krishnan, Kajoli Banerjee

2013-03-01

Perception of operator influences ultrasound image acquisition and processing. Lower costs are attracting new users to medical ultrasound. Anticipating an increase in this trend, we conducted a study to quantify the variability in ultrasonic measurements made by novice users and identify methods to reduce it. We designed a protocol with four presets and trained four new users to scan and manually measure the head circumference of a fetal phantom with an ultrasound scanner. In the first phase, the users followed this protocol in seven distinct sessions. They then received feedback on the quality of the scans from an expert. In the second phase, two of the users repeated the entire protocol aided by visual cues provided to them during scanning. We performed off-line measurements on all the images using a fully automated algorithm capable of measuring the head circumference from fetal phantom images. The ground truth (198.1±1.6 mm) was based on sixteen scans and measurements made by an expert. Our analysis shows that: (1) the inter-observer variability of manual measurements was 5.5 mm, whereas the inter-observer variability of automated measurements was only 0.6 mm in the first phase (2) consistency of image appearance improved and mean manual measurements was 4-5 mm closer to the ground truth in the second phase (3) automated measurements were more precise, accurate and less sensitive to different presets compared to manual measurements in both phases. Our results show that visual aids and automation can bring more reproducibility to ultrasonic measurements made by new users.

Analysis of emboli during carotid stenting with distal protection device.

PubMed

Chen, Chin-I; Iguchi, Yasuyuki; Garami, Zsolt; Malkoff, Marc D; Smalling, Richard W; Campbell, Morgan S; Alexandrov, Andrei V

2006-01-01

The newly developed multi-frequency transcranial Doppler (TCD) is able to differentiate gaseous from solid emboli. Our goal was to apply this technology to initially characterize emboli detected during carotid stenting with distal protection. Patients undergoing carotid angiography and stenting were monitored with 2-2.5 MHz TCD (Embo-Dop, DWL) over the middle cerebral artery unilateral to stent deployment. Sonographers insured optimal signal recordings during the procedures. Automated emboli detection and classification software (MultiXLab version 2.0) was applied for offline count and analysis. Monitoring using the Filter Wire EX (Boston Scientific) and ACCUNET system (Guidant Corporation) was performed. A total of 9,649 embolic signals were detected during 11 angiographic and 10 stenting procedures. An observer confirmed the signals using the International Consensus definition. Automated software classified these events into 5,900 gaseous and 3,749 solid emboli. During contrast injections without the protection device, 1,013 emboli were detected with 28% of these being solid. With deployment of the distal protection device, 8,636 emboli were found with 40% being solid (p < 0.001). During stenting and angioplasty with the protection device, 7,395 emboli with 42% solids were detected (p < 0.001). Finally injection of contrast after the procedure, with the protection device still deployed, yielded 1,241 emboli with 31% solids (NS). Only 1 patient developed transient hemiparesthesia during ballooning that reduced the flow velocity to zero for 14 s. Neither gaseous nor solid emboli resulted in a mean flow velocity decrease or clinical symptoms. Microembolization frequently occurs during stenting even with deployment of the distal protection device. More solid emboli are seen during manipulations associated with lesion crossing. Although novel TCD methods yield a high frequency of embolic signals, further validation of this technique to determine the true nature, size, and number of emboli is needed.

Automated first-principles mapping for phase-change materials.

PubMed

Esser, Marc; Maintz, Stefan; Dronskowski, Richard

2017-04-05

Plotting materials on bi-coordinate maps according to physically meaningful descriptors has a successful tradition in computational solid-state science spanning more than four decades. Equipped with new ab initio techniques introduced in this work, we generate an improved version of the treasure map for phase-change materials (PCMs) as introduced previously by Lencer et al. which, other than before, charts all industrially used PCMs correctly. Furthermore, we suggest seven new PCM candidates, namely SiSb 4 Te 7 , Si 2 Sb 2 Te 5 , SiAs 2 Te 4 , PbAs 2 Te 4 , SiSb 2 Te 4 , Sn 2 As 2 Te 5 , and PbAs 4 Te 7 , to be used as synthetic targets. To realize aforementioned maps based on orbital mixing (or "hybridization") and ionicity coordinates, structural information was first included into an ab initio numerical descriptor for sp 3 orbital mixing and then generalized beyond high-symmetry structures. In addition, a simple, yet powerful quantum-mechanical ionization measure also including structural information was introduced. Taken together, these tools allow for (automatically) generating materials maps solely relying on first-principles calculations. © 2017 Wiley Periodicals, Inc. © 2017 Wiley Periodicals, Inc.

Role of microextraction sampling procedures in forensic toxicology.

PubMed

Barroso, Mário; Moreno, Ivo; da Fonseca, Beatriz; Queiroz, João António; Gallardo, Eugenia

2012-07-01

The last two decades have provided analysts with more sensitive technology, enabling scientists from all analytical fields to see what they were not able to see just a few years ago. This increased sensitivity has allowed drug detection at very low concentrations and testing in unconventional samples (e.g., hair, oral fluid and sweat), where despite having low analyte concentrations has also led to a reduction in sample size. Along with this reduction, and as a result of the use of excessive amounts of potentially toxic organic solvents (with the subsequent environmental pollution and costs associated with their proper disposal), there has been a growing tendency to use miniaturized sampling techniques. Those sampling procedures allow reducing organic solvent consumption to a minimum and at the same time provide a rapid, simple and cost-effective approach. In addition, it is possible to get at least some degree of automation when using these techniques, which will enhance sample throughput. Those miniaturized sample preparation techniques may be roughly categorized in solid-phase and liquid-phase microextraction, depending on the nature of the analyte. This paper reviews recently published literature on the use of microextraction sampling procedures, with a special focus on the field of forensic toxicology.

Simultaneous estimation of E- and Z-isomers of guggulsterone in rabbit plasma using liquid chromatography tandem mass spectrometry and its application to pharmacokinetic study.

PubMed

Bhatta, R S; Kumar, D; Chhonker, Y S; Jain, G K

2011-09-01

A sensitive and selective liquid chromatography/tandem mass spectrometric method was developed for simultaneous determination of E- and Z-guggulsterone isomers (antihyperlipidemic drug) in rabbit plasma. Both the isomers were resolved on a Symmetry-Shield C(18) (5 µm, 4.6 × 150 mm) column, using gradient elution comprising a mobile phase of methanol, 0.5% v/v formic acid and acetonitrile. With dexamethasone as internal standard, plasma samples were extracted by an automated solid-phase extraction method using C(18) cartridges. Detection was performed by electrospray ionization in multiple reaction monitoring (MRM) in positive mode. The calibration curve was linear over the concentration range of 1.56-200 ng/mL (r(2) ≥ 0.998) for both analytes. The intra-day and inter-day accuracy and precision were within -0.96 to 4.12 (%bias) and 2.73 to 8.00 (%RSD) respectively. The analytes were stable after three freeze-thaw cycles. The method was successfully applied to study steriospecific pharmacokinetics of E- and Z-guggulsterone in NZ rabbit. Copyright © 2011 John Wiley & Sons, Ltd.

Automated Phase Segmentation for Large-Scale X-ray Diffraction Data Using a Graph-Based Phase Segmentation (GPhase) Algorithm.

PubMed

Xiong, Zheng; He, Yinyan; Hattrick-Simpers, Jason R; Hu, Jianjun

2017-03-13

The creation of composition-processing-structure relationships currently represents a key bottleneck for data analysis for high-throughput experimental (HTE) material studies. Here we propose an automated phase diagram attribution algorithm for HTE data analysis that uses a graph-based segmentation algorithm and Delaunay tessellation to create a crystal phase diagram from high throughput libraries of X-ray diffraction (XRD) patterns. We also propose the sample-pair based objective evaluation measures for the phase diagram prediction problem. Our approach was validated using 278 diffraction patterns from a Fe-Ga-Pd composition spread sample with a prediction precision of 0.934 and a Matthews Correlation Coefficient score of 0.823. The algorithm was then applied to the open Ni-Mn-Al thin-film composition spread sample to obtain the first predicted phase diagram mapping for that sample.

Phase II: Automated System for Aneuploidy Detection in Sperm Final Report CRADA No. TC-1554-98

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

Wyrobek, W. J.; Dunlay, R. T.

This was a collaborative effort between the University of California, Lawrence Livermore National Laboratory (LLNL) and Cellomics, Inc. (formerly BioDx and Biological Detection, Inc.) to develop an automated system for detecting human sperm aneuploidy. Aneuploidy (an abnormal number of chromosomes) is one of the major categories of chromosomally abnormal sperm, which results in chromosomally defective pregnancies and babies. An automated system would be used for testing the effects of toxic agents and for other research and clinical applications. This collaborated effort was funded by a National Institutes of Environmental Health Services, Phase II, Small Business Innovation Research Program (SBIR) grantmore » to Cellornics (Contract No. N44-ES-82004).« less

Numerical Computation of Flame Spread over a Thin Solid in Forced Concurrent Flow with Gas-phase Radiation

NASA Technical Reports Server (NTRS)

Jiang, Ching-Biau; T'ien, James S.

1994-01-01

Excerpts from a paper describing the numerical examination of concurrent-flow flame spread over a thin solid in purely forced flow with gas-phase radiation are presented. The computational model solves the two-dimensional, elliptic, steady, and laminar conservation equations for mass, momentum, energy, and chemical species. Gas-phase combustion is modeled via a one-step, second order finite rate Arrhenius reaction. Gas-phase radiation considering gray non-scattering medium is solved by a S-N discrete ordinates method. A simplified solid phase treatment assumes a zeroth order pyrolysis relation and includes radiative interaction between the surface and the gas phase.

Phase III gross solids removal devices pilot study, 2002-2005.

DOT National Transportation Integrated Search

2005-12-01

The objective of the Phase III Gross Solids Removal Devices (GSRDs) Pilot study was to : evaluate the performance of non-proprietary devices that can capture gross solids and that can be : incorporated into existing highway drainage systems or implem...

An alternative method for irones quantification in iris rhizomes using headspace solid-phase microextraction.

PubMed

Roger, B; Fernandez, X; Jeannot, V; Chahboun, J

2010-01-01

The essential oil obtained from iris rhizomes is one of the most precious raw materials for the perfume industry. Its fragrance is due to irones that are gradually formed by oxidative degradation of iridals during rhizome ageing. The development of an alternative method allowing irone quantification in iris rhizomes using HS-SPME-GC. The development of the method using HS-SPME-GC was achieved using the results obtained from a conventional method, i.e. a solid-liquid extraction (SLE) followed by irone quantification by CG. Among several calibration methods tested, internal calibration gave the best results and was the least sensitive to the matrix effect. The proposed method using HS-SPME-GC is as accurate and reproducible as the conventional one using SLE. These two methods were used to monitor and compare irone concentrations in iris rhizomes that had been stored for 6 months to 9 years. Irone quantification in iris rhizome can be achieved using HS-SPME-GC. This method can thus be used for the quality control of the iris rhizomes. It offers the advantage of combining extraction and analysis with an automated device and thus allows a large number of rhizome batches to be analysed and compared in a limited amount of time. Copyright © 2010 John Wiley & Sons, Ltd.

Automated CPX support system preliminary design phase

NASA Technical Reports Server (NTRS)

Bordeaux, T. A.; Carson, E. T.; Hepburn, C. D.; Shinnick, F. M.

1984-01-01

The development of the Distributed Command and Control System (DCCS) is discussed. The development of an automated C2 system stimulated the development of an automated command post exercise (CPX) support system to provide a more realistic stimulus to DCCS than could be achieved with the existing manual system. An automated CPX system to support corps-level exercise was designed. The effort comprised four tasks: (1) collecting and documenting user requirements; (2) developing a preliminary system design; (3) defining a program plan; and (4) evaluating the suitability of the TRASANA FOURCE computer model.

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

NASA Astrophysics Data System (ADS)

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.

Quick, easy, cheap, effective, rugged, and safe sample preparation approach for pesticide residue analysis using traditional detectors in chromatography: A review.

PubMed

Rahman, Md Musfiqur; Abd El-Aty, A M; Kim, Sung-Woo; Shin, Sung Chul; Shin, Ho-Chul; Shim, Jae-Han

2017-01-01

In pesticide residue analysis, relatively low-sensitivity traditional detectors, such as UV, diode array, electron-capture, flame photometric, and nitrogen-phosphorus detectors, have been used following classical sample preparation (liquid-liquid extraction and open glass column cleanup); however, the extraction method is laborious, time-consuming, and requires large volumes of toxic organic solvents. A quick, easy, cheap, effective, rugged, and safe method was introduced in 2003 and coupled with selective and sensitive mass detectors to overcome the aforementioned drawbacks. Compared to traditional detectors, mass spectrometers are still far more expensive and not available in most modestly equipped laboratories, owing to maintenance and cost-related issues. Even available, traditional detectors are still being used for analysis of residues in agricultural commodities. It is widely known that the quick, easy, cheap, effective, rugged, and safe method is incompatible with conventional detectors owing to matrix complexity and low sensitivity. Therefore, modifications using column/cartridge-based solid-phase extraction instead of dispersive solid-phase extraction for cleanup have been applied in most cases to compensate and enable the adaptation of the extraction method to conventional detectors. In gas chromatography, the matrix enhancement effect of some analytes has been observed, which lowers the limit of detection and, therefore, enables gas chromatography to be compatible with the quick, easy, cheap, effective, rugged, and safe extraction method. For liquid chromatography with a UV detector, a combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction was found to reduce the matrix interference and increase the sensitivity. A suitable double-layer column/cartridge-based solid-phase extraction might be the perfect solution, instead of a time-consuming combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction. Therefore, replacing dispersive solid-phase extraction with column/cartridge-based solid-phase extraction in the cleanup step can make the quick, easy, cheap, effective, rugged, and safe extraction method compatible with traditional detectors for more sensitive, effective, and green analysis. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Automated Power-Distribution System

NASA Technical Reports Server (NTRS)

Thomason, Cindy; Anderson, Paul M.; Martin, James A.

1990-01-01

Automated power-distribution system monitors and controls electrical power to modules in network. Handles both 208-V, 20-kHz single-phase alternating current and 120- to 150-V direct current. Power distributed to load modules from power-distribution control units (PDCU's) via subsystem distributors. Ring busses carry power to PDCU's from power source. Needs minimal attention. Detects faults and also protects against them. Potential applications include autonomous land vehicles and automated industrial process systems.

Automated high resolution full-field spatial coherence tomography for quantitative phase imaging of human red blood cells

NASA Astrophysics Data System (ADS)

Singla, Neeru; Dubey, Kavita; Srivastava, Vishal; Ahmad, Azeem; Mehta, D. S.

2018-02-01

We developed an automated high-resolution full-field spatial coherence tomography (FF-SCT) microscope for quantitative phase imaging that is based on the spatial, rather than the temporal, coherence gating. The Red and Green color laser light was used for finding the quantitative phase images of unstained human red blood cells (RBCs). This study uses morphological parameters of unstained RBCs phase images to distinguish between normal and infected cells. We recorded the single interferogram by a FF-SCT microscope for red and green color wavelength and average the two phase images to further reduced the noise artifacts. In order to characterize anemia infected from normal cells different morphological features were extracted and these features were used to train machine learning ensemble model to classify RBCs with high accuracy.

Computer aided fixture design - A case based approach

NASA Astrophysics Data System (ADS)

Tanji, Shekhar; Raiker, Saiesh; Mathew, Arun Tom

2017-11-01

Automated fixture design plays important role in process planning and integration of CAD and CAM. An automated fixture setup design system is developed where when fixturing surfaces and points are described allowing modular fixture components to get automatically select for generating fixture units and placed into position with satisfying assembled conditions. In past, various knowledge based system have been developed to implement CAFD in practice. In this paper, to obtain an acceptable automated machining fixture design, a case-based reasoning method with developed retrieval system is proposed. Visual Basic (VB) programming language is used in integrating with SolidWorks API (Application programming interface) module for better retrieval procedure reducing computational time. These properties are incorporated in numerical simulation to determine the best fit for practical use.

Fully automated segmentation of left ventricle using dual dynamic programming in cardiac cine MR images

NASA Astrophysics Data System (ADS)

Jiang, Luan; Ling, Shan; Li, Qiang

2016-03-01

Cardiovascular diseases are becoming a leading cause of death all over the world. The cardiac function could be evaluated by global and regional parameters of left ventricle (LV) of the heart. The purpose of this study is to develop and evaluate a fully automated scheme for segmentation of LV in short axis cardiac cine MR images. Our fully automated method consists of three major steps, i.e., LV localization, LV segmentation at end-diastolic phase, and LV segmentation propagation to the other phases. First, the maximum intensity projection image along the time phases of the midventricular slice, located at the center of the image, was calculated to locate the region of interest of LV. Based on the mean intensity of the roughly segmented blood pool in the midventricular slice at each phase, end-diastolic (ED) and end-systolic (ES) phases were determined. Second, the endocardial and epicardial boundaries of LV of each slice at ED phase were synchronously delineated by use of a dual dynamic programming technique. The external costs of the endocardial and epicardial boundaries were defined with the gradient values obtained from the original and enhanced images, respectively. Finally, with the advantages of the continuity of the boundaries of LV across adjacent phases, we propagated the LV segmentation from the ED phase to the other phases by use of dual dynamic programming technique. The preliminary results on 9 clinical cardiac cine MR cases show that the proposed method can obtain accurate segmentation of LV based on subjective evaluation.

SSM-based electrophysiology.

PubMed

Schulz, Patrick; Garcia-Celma, Juan J; Fendler, Klaus

2008-10-01

An assay technique for the electrical characterization of electrogenic transport proteins on solid supported membranes is presented. Membrane vesicles, proteoliposomes or membrane fragments containing the transporter are adsorbed to the solid supported membrane and are activated by providing a substrate or a ligand via a rapid solution exchange. This technique opens up new possibilities where conventional electrophysiology fails like transporters or ion channels from bacteria and from intracellular compartments. Its rugged design and potential for automation make it suitable for drug screening.

Automated Safety Warning Controller (ASWC) Phase I - Proof of Concept

DOT National Transportation Integrated Search

2010-07-07

Automated warning systems are not a new concept within the transportation community. There are several projects on the state highway that use the concept of a roadway sensor initiating some type of motorist warning. To date, all of these systems are ...

Development and validation of inexpensive, automated, dynamic flux chambers

EPA Science Inventory

We developed and validated an automated, inexpensive, and continuous multiple-species gas-flux monitoring system that can provide data for a variety of relevant atmospheric pollutants, including O3, CO2, and NOx. Validation consisted of conducting concurrent gas-phase dry deposit...

Simultaneous estimation of liquid and solid gastric emptying using radiolabelled egg and water in supine normal subjects.

PubMed

Kris, M G; Yeh, S D; Gralla, R J; Young, C W

1986-01-01

To develop an additional method for the measurement of gastric emptying in supine subjects, 10 normal subjects were given a test meal containing 99Tc-labelled scrambled egg as the "solid" phase marker and 111In in tapwater as the marker for the "liquid" phase. The mean time for emptying 50% of the "solid" phase (t1/2) was 85 min and 29 min for the "liquid" phase. Three individuals were restudied with a mean difference between the two determinations of 10.8% for the "solid" phase and 6.5% for the "liquid" phase. Twenty-six additional studies attempted have been successfully completed in symptomatic patients with advanced cancer. This method provides a simple and reproducible procedure for the determination of gastric emptying that yields results similar to those reported for other test meals and can be used in debilitated patients.

Thermal shock resistance ceramic insulator

DOEpatents

Morgan, Chester S.; Johnson, William R.

1980-01-01

Thermal shock resistant cermet insulators containing 0.1-20 volume % metal present as a dispersed phase. The insulators are prepared by a process comprising the steps of (a) providing a first solid phase mixture of a ceramic powder and a metal precursor; (b) heating the first solid phase mixture above the minimum decomposition temperature of the metal precursor for no longer than 30 minutes and to a temperature sufficiently above the decomposition temperature to cause the selective decomposition of the metal precursor to the metal to provide a second solid phase mixture comprising particles of ceramic having discrete metal particles adhering to their surfaces, said metal particles having a mean diameter no more than 1/2 the mean diameter of the ceramic particles, and (c) densifying the second solid phase mixture to provide a cermet insulator having 0.1-20 volume % metal present as a dispersed phase.

Phase IV gross solids removal devices pilot study, 2004-2005.

DOT National Transportation Integrated Search

2005-12-01

The objective of the Phase IV Gross Solids Removal Device (GSRD) Pilot study was to evaluate : the performance of one non-proprietary device that can capture gross solids and that can be : incorporated into existing highway drainage systems or implem...

Characterization of the Solid-Phase Behavior of n-Nonylammonium Tetrachlorocuprate by Fourier Transform Infrared Spectroscopy

NASA Astrophysics Data System (ADS)

Ning, Guo

1995-06-01

The solid-phase behavior of [n-C9H19NH3]2CuCl4 was investigated by infrared spectroscopy. The nature of the three solid phases (phase I, phase II, and phase III) is discussed. A temperature-dependent study of infrared spectra provides evidence for the occurrence of structural phase transitions related to the dynamics of the alkyl chains and -NH3 polar heads. The phase transition at Tc1 (22°C) arises from variation in the interaction and packing structure of the chain. The phase transition at Tc2 (34°C) is related to variation in partial conformational order-disorder at the intramolecular level. The GTG or GTG‧ and small concentration of TG structures near the CH3 group are generated in phase III (above 38°C).

Automated and sensitive method for the determination of formoterol in human plasma by high-performance liquid chromatography and electrochemical detection.

PubMed

Campestrini, J; Lecaillon, J B; Godbillon, J

1997-12-19

An automated high-performance liquid chromatography (HPLC) method for the determination of formoterol in human plasma with improved sensitivity has been developed and validated. Formoterol and CGP 47086, the internal standard, were extracted from plasma (1 ml) using a cation-exchange solid-phase extraction (SPE) cartridge. The compounds were eluted with pH 6 buffer solution-methanol (70:30, v/v) and the eluate was further diluted with water. An aliquot of the extract solution was injected and analyzed by HPLC. The extraction, dilution, injection and chromatographic analysis were combined and automated using the automate (ASPEC) system. The chromatographic separations were achieved on a 5 microm, Hypersil ODS analytical column (200 mm x 3 mm I.D.), using (pH 6 phosphate buffer, 0.035 M + 20 mg/l EDTA)-MeOH-CH3CN (70:25:5, v/v/v) as the mobile phase at a flow-rate of 0.4 ml/min. The analytes were detected with electrochemical detection at an operating potential of +0.63 V. Intra-day accuracy and precision were assessed from the relative recoveries of calibration/quality control plasma samples in the concentration range of 7.14 to 238 pmol/l of formoterol base. The accuracy over the entire concentration range varied from 81 to 105%, and the precision (C.V.) ranged from 3 to 14%. Inter-day accuracy and precision were assessed in the concentration range of 11.9 to 238 pmol/l of formoterol base in plasma. The accuracy over the entire concentration range varied from 98 to 109%, and precision ranged from 8 to 19%. At the limit of quantitation (LOQ) of 11.9 pmol/l for inter-day measurements, the recovery value was 109% and C.V. was 19%. As shown from intra-day accuracy and precision results, favorable conditions (a newly used column, a newly washed detector cell and moderate residual cell current level) allowed us to reach a LOQ of 7.14 pmol/l of formoterol base (3 pg/ml of formoterol fumarate dihydrate). Improvement of the limit of detection by a factor of about 10 was reached as compared to the previously described methods. The method has been applied for quantifying formoterol in plasma after 120 microg drug inhalation to volunteers. Formoterol was still measurable at 24 h post-dosing in most subjects and a slow elimination of formoterol from plasma beyond 6-8 h after inhalation was demonstrated for the first time thanks to the sensitivity of the method.

Role of Precursor-Conversion Chemistry in the Crystal-Phase Control of Catalytically Grown Colloidal Semiconductor Quantum Wires.

PubMed

Wang, Fudong; Buhro, William E

2017-12-26

Crystal-phase control is one of the most challenging problems in nanowire growth. We demonstrate that, in the solution-phase catalyzed growth of colloidal cadmium telluride (CdTe) quantum wires (QWs), the crystal phase can be controlled by manipulating the reaction chemistry of the Cd precursors and tri-n-octylphosphine telluride (TOPTe) to favor the production of either a CdTe solute or Te, which consequently determines the composition and (liquid or solid) state of the Bi x Cd y Te z catalyst nanoparticles. Growth of single-phase (e.g., wurtzite) QWs is achieved only from solid catalysts (y ≪ z) that enable the solution-solid-solid growth of the QWs, whereas the liquid catalysts (y ≈ z) fulfill the solution-liquid-solid growth of the polytypic QWs. Factors that affect the precursor-conversion chemistry are systematically accounted for, which are correlated with a kinetic study of the composition and state of the catalyst nanoparticles to understand the mechanism. This work reveals the role of the precursor-reaction chemistry in the crystal-phase control of catalytically grown colloidal QWs, opening the possibility of growing phase-pure QWs of other compositions.

Automated Quantitative Rare Earth Elements Mineralogy by Scanning Electron Microscopy

NASA Astrophysics Data System (ADS)

Sindern, Sven; Meyer, F. Michael

2016-09-01

Increasing industrial demand of rare earth elements (REEs) stems from the central role they play for advanced technologies and the accelerating move away from carbon-based fuels. However, REE production is often hampered by the chemical, mineralogical as well as textural complexity of the ores with a need for better understanding of their salient properties. This is not only essential for in-depth genetic interpretations but also for a robust assessment of ore quality and economic viability. The design of energy and cost-efficient processing of REE ores depends heavily on information about REE element deportment that can be made available employing automated quantitative process mineralogy. Quantitative mineralogy assigns numeric values to compositional and textural properties of mineral matter. Scanning electron microscopy (SEM) combined with a suitable software package for acquisition of backscatter electron and X-ray signals, phase assignment and image analysis is one of the most efficient tools for quantitative mineralogy. The four different SEM-based automated quantitative mineralogy systems, i.e. FEI QEMSCAN and MLA, Tescan TIMA and Zeiss Mineralogic Mining, which are commercially available, are briefly characterized. Using examples of quantitative REE mineralogy, this chapter illustrates capabilities and limitations of automated SEM-based systems. Chemical variability of REE minerals and analytical uncertainty can reduce performance of phase assignment. This is shown for the REE phases parisite and synchysite. In another example from a monazite REE deposit, the quantitative mineralogical parameters surface roughness and mineral association derived from image analysis are applied for automated discrimination of apatite formed in a breakdown reaction of monazite and apatite formed by metamorphism prior to monazite breakdown. SEM-based automated mineralogy fulfils all requirements for characterization of complex unconventional REE ores that will become increasingly important for supply of REEs in the future.

Automation of the in vitro micronucleus and chromosome aberration assay for the assessment of the genotoxicity of the particulate and gas-vapor phase of cigarette smoke.

PubMed

Roemer, Ewald; Zenzen, Volker; Conroy, Lynda L; Luedemann, Kathrin; Dempsey, Ruth; Schunck, Christian; Sticken, Edgar Trelles

2015-01-01

Total particulate matter (TPM) and the gas-vapor phase (GVP) of mainstream smoke from the Reference Cigarette 3R4F were assayed in the cytokinesis-block in vitro micronucleus (MN) assay and the in vitro chromosome aberration (CA) assay, both using V79-4 Chinese hamster lung fibroblasts exposed for up to 24 h. The Metafer image analysis platform was adapted resulting in a fully automated evaluation system of the MN assay for the detection, identification and reporting of cells with micronuclei together with the determination of the cytokinesis-block proliferation index (CBPI) to quantify the treatment-related cytotoxicity. In the CA assay, the same platform was used to identify, map and retrieve metaphases for a subsequent CA evaluation by a trained evaluator. In both the assays, TPM and GVP provoked a significant genotoxic effect: up to 6-fold more micronucleated target cells than in the negative control and up to 10-fold increases in aberrant metaphases. Data variability was lower in the automated version of the MN assay than in the non-automated. It can be estimated that two test substances that differ in their genotoxicity by approximately 30% can statistically be distinguished in the automated MN and CA assays. Time savings, based on man hours, due to the automation were approximately 70% in the MN and 25% in the CA assays. The turn-around time of the evaluation phase could be shortened by 35 and 50%, respectively. Although only cigarette smoke-derived test material has been applied, the technical improvements should be of value for other test substances.

Solid-liquid critical behavior of water in nanopores.

PubMed

Mochizuki, Kenji; Koga, Kenichiro

2015-07-07

Nanoconfined liquid water can transform into low-dimensional ices whose crystalline structures are dissimilar to any bulk ices and whose melting point may significantly rise with reducing the pore size, as revealed by computer simulation and confirmed by experiment. One of the intriguing, and as yet unresolved, questions concerns the observation that the liquid water may transform into a low-dimensional ice either via a first-order phase change or without any discontinuity in thermodynamic and dynamic properties, which suggests the existence of solid-liquid critical points in this class of nanoconfined systems. Here we explore the phase behavior of a model of water in carbon nanotubes in the temperature-pressure-diameter space by molecular dynamics simulation and provide unambiguous evidence to support solid-liquid critical phenomena of nanoconfined water. Solid-liquid first-order phase boundaries are determined by tracing spontaneous phase separation at various temperatures. All of the boundaries eventually cease to exist at the critical points and there appear loci of response function maxima, or the Widom lines, extending to the supercritical region. The finite-size scaling analysis of the density distribution supports the presence of both first-order and continuous phase changes between solid and liquid. At around the Widom line, there are microscopic domains of two phases, and continuous solid-liquid phase changes occur in such a way that the domains of one phase grow and those of the other evanesce as the thermodynamic state departs from the Widom line.

Comparison of solid-phase and eluate assays to gauge the ecotoxicological risk of organic wastes on soil organisms.

PubMed

Domene, Xavier; Alcañiz, Josep M; Andrés, Pilar

2008-02-01

Development of methodologies to assess the safety of reusing polluted organic wastes in soil is a priority in Europe. In this study, and coupled with chemical analysis, seven organic wastes were subjected to different aquatic and soil bioassays. Tests were carried out with solid-phase waste and three different waste eluates (water, methanol, and dichloromethane). Solid-phase assays were indicated as the most suitable for waste testing not only in terms of relevance for real situations, but also because toxicity in eluates was generally not representative of the chronic effects in solid-phase. No general correlations were found between toxicity and waste pollutant burden, neither in solid-phase nor in eluate assays, showing the inability of chemical methods to predict the ecotoxicological risks of wastes. On the contrary, several physicochemical parameters reflecting the degree of low organic matter stability in wastes were the main contributors to the acute toxicity seen in collembolans and daphnids.

Solid-Phase Radioimmunoassay of Total and Influenza-Specific Immunoglobulin G

PubMed Central

Daugharty, Harry; Warfield, Donna T.; Davis, Marianne L.

1972-01-01

An antigen-antibody system of polystyrene tubes coated with immunoglobulin antibody was used for quantitating immunoglobulins. A similar radioimmunoassay method was adapted for a viral antigen-antibody system. The viral system can be used for quantitating viruses and for measuring virus-specific antibodies by reacting with 125iodine-labeled anti-immunoglobulin G (IgG). Optimal conditions for coating the solid phase, specificity of the immune reaction, and other kinetics and sensitivities of the assay method were investigated. Comparison of direct and indirect methods of assaying for immunoglobulins or viral antibody indicates that the indirect method is more sensitive and can quantitate a minimum of 0.037 μg of IgG per ml. Results of solid-phase radioimmunoassay for influenza antibody correlate well with hemagglutinin antibody titers but not with complement-fixing antibody titers. Radioimmunoassay results for influenza antibody by solid phase are likewise in agreement with results by the carrier precipitate radioimmunoassay method. The simplicity, reproducibility, and versatility of the solid-phase procedure make it diagnostically useful. PMID:5062884

Molecular Simulation of the Free Energy for the Accurate Determination of Phase Transition Properties of Molecular Solids

NASA Astrophysics Data System (ADS)

Sellers, Michael; Lisal, Martin; Brennan, John

2015-06-01

Investigating the ability of a molecular model to accurately represent a real material is crucial to model development and use. When the model simulates materials in extreme conditions, one such property worth evaluating is the phase transition point. However, phase transitions are often overlooked or approximated because of difficulty or inaccuracy when simulating them. Techniques such as super-heating or super-squeezing a material to induce a phase change suffer from inherent timescale limitations leading to ``over-driving,'' and dual-phase simulations require many long-time runs to seek out what frequently results in an inexact location of phase-coexistence. We present a compilation of methods for the determination of solid-solid and solid-liquid phase transition points through the accurate calculation of the chemical potential. The methods are applied to the Smith-Bharadwaj atomistic potential's representation of cyclotrimethylene trinitramine (RDX) to accurately determine its melting point (Tm) and the alpha to gamma solid phase transition pressure. We also determine Tm for a coarse-grain model of RDX, and compare its value to experiment and atomistic counterpart. All methods are employed via the LAMMPS simulator, resulting in 60-70 simulations that total 30-50 ns. Approved for public release. Distribution is unlimited.

Phase transition thermodynamics of bisphenols.

PubMed

Costa, José C S; Dávalos, Juan Z; Santos, Luís M N B F

2014-10-16

Herein we have studied, presented, and analyzed the phase equilibria thermodynamics of a bisphenols (BP-A, BP-E, BP-F, BP-AP, and BP-S) series. In particular, the heat capacities, melting temperatures, and vapor pressures at different temperatures as well as the standard enthalpies, entropies, and Gibbs energies of phase transition (fusion and sublimation) were experimentally determined. Also, we have presented the phase diagrams of each bisphenol derivative and investigated the key parameters related to the thermodynamic stability of the condensed phases. When all the bisphenol derivatives are compared at the same conditions, solids BP-AP and BP-S present lower volatilities (higher Gibbs energy of sublimation) and high melting temperatures due to the higher stability of their solid phases. Solids BP-A and BP-F present similar stabilities, whereas BP-E is more volatile. The introduction of -CH3 groups in BP-F (giving BP-E and BP-A) leads an entropic differentiation in the solid phase, whereas in the isotropic liquids the enthalpic and entropic differentiations are negligible.

Robotics in space-age manufacturing

NASA Technical Reports Server (NTRS)

Jones, Chip

1991-01-01

Robotics technologies are developed to improve manufacturing of space hardware. The following applications of robotics are covered: (1) welding for the space shuttle and space station Freedom programs; (2) manipulation of high-pressure water for shuttle solid rocket booster refurbishment; (3) automating the application of insulation materials; (4) precision application of sealants; and (5) automation of inspection procedures. Commercial robots are used for these development programs, but they are teamed with advanced sensors, process controls, and computer simulation to form highly productive manufacturing systems. Many of the technologies are also being actively pursued in private sector manufacturing operations.

Analysis of Explosives in Soil Using Solid Phase Microextraction and Gas Chromatography: Environmental Analysis

DTIC Science & Technology

2006-01-01

ENVIRONMENTAL ANALYSIS Analysis of Explosives in Soil Using Solid Phase Microextraction and Gas Chromatography Howard T. Mayfield Air Force Research...Abstract: Current methods for the analysis of explosives in soils utilize time consuming sample preparation workups and extractions. The method detection...chromatography/mass spectrometry to provide a con- venient and sensitive analysis method for explosives in soil. Keywords: Explosives, TNT, solid phase

Binary Solid-Liquid Phase Equilibria

ERIC Educational Resources Information Center

Ellison, Herbert R.

1978-01-01

Indicates some of the information that may be obtained from a binary solid-liquid phase equilibria experiment and a method to write a computer program that will plot an ideal phase diagram to which the experimental results may be compared. (Author/CP)

Portable microfluidic platform for real-time, high sensitive detection and identification of trichloroethylene and other organochloride compounds

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

Jensen, Erik

In this successful SBIR Phase II effort, HJ Science & Technology, Inc. has designed and built a novel portable instrument capable of performing automated aqueous organochloride (chlorinated solvent) speciation analysis for environmental monitoring at DoE sites. Our technique employs performing organochloride conjugation, labeling the conjugate with an efficient fluorophore, and performing on-chip capillary electrophoresis separation with laser induced fluorescence detection. The key component of the portable instrument is a novel microfluidic chip capable of complete “end-to-end” automation of sample preparation, conjugation, labeling, and μCE separation and detection. In addition, the Phase II prototype includes key supporting instrumentation such as themore » optical module, pneumatic manifold, electronics, software, etc. As such, we have achieved all of the following 4 Phase II technical objectives: 1) Further refine and optimize the “on-chip” automation of the organochloride conjugation and labeling protocol, 2) Further improve the microfluidic chip fabrication process and the pneumatic manifold design in order to address issues related to performance consistency, product yield, performance reliability, and user friendliness, 3) Design and build the supporting components of the Phase II prototype including optical module, electronics, and software, and 4) Assemble the Phase II prototype hardware.« less

Role of lattice distortion on diffuse phase transition temperatures in Bi0.5Na0.5TiO3-BaTiO3 [BNBTO] solid solutions

NASA Astrophysics Data System (ADS)

Pradhan, Lagen Kumar; Pandey, Rabichandra; Kumar, Sunil; Supriya, Sweety; Kar, Manoranjan

2018-04-01

Effect of lattice distortion on diffuse phase transition in BNBTO solid solutions near Morphotropic phase boundary (MPB) has been investigated. Solid solutions of (Bi0.5Na0.5)1-xBaxTiO3 (with mole % of x= 0.04, 0.05, 0.06, 0.07 and 0.08) were prepared by the planetary ball mill method in ethanol medium. Rietveld refinement technique with rhombohedral (R3c) and tetragonal (P4bm) crystal symmetry has been employed for structural as well as phase analysis of the solid solutions. Both rhombohedral and tetragonal lattice distortion (c/a) tends toward the pseudo-cubic crystal symmetry with the increase of mole fraction of Ba2+ near MPB (x= 6 mole %). Also, the average crystallite size and grain size decrease with increase of mole fraction of Ba2+ in BNT ceramic are due to larger ionic radius of Ba2+ and grain boundary pinning process in the solid solutions respectively. Additionally, depolarization temperature (Td) and maximum temperature (Tm) reduces due to the lattice distortion of both the phases in BNBTO solid solutions, which is explained extensively. Significant increase of dielectric constant has been observed near MPB composition (x=6%) in BNBTO solid solutions.

Influence of calcium on microbial reduction of solid phase uranium(VI).

PubMed

Liu, Chongxuan; Jeon, Byong-Hun; Zachara, John M; Wang, Zheming

2007-08-15

The effect of calcium on the dissolution and microbial reduction of a representative solid phase uranyl [U(VI)], sodium boltwoodite (NaUO(2)SiO(3)OH . 1.5H(2)O), was investigated to evaluate the rate-limiting step of microbial reduction of the solid phase U(VI). Microbial reduction experiments were performed in a culture of a dissimilatory metal-reducing bacterium (DMRB), Shewanella oneidensis strain MR-1, in a bicarbonate medium with lactate as electron donor at pH 6.8 buffered with PIPES. Calcium increased the rate of Na-boltwoodite dissolution and U(VI) bioavailability 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) collectively revealed that microbial reduction of solid phase U(VI) was 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. Under studied experimental conditions, the overall rate of microbial reduction of solid phase U(VI) was limited by U(VI) dissolution reactions in solutions without calcium and limited by microbial reduction in solutions with calcium. Generally, the overall rate of microbial reduction of solid phase U(VI) was determined by the coupling of solid phase U(VI) dissolution, U(VI) aqueous speciation, and microbial reduction of dissolved U(VI) that were all affected by calcium. (c) 2007 Wiley Periodicals, Inc.

Development of automated testing tools for traffic control signals and devices (NTCIP and Security) phase 2.

DOT National Transportation Integrated Search

2015-02-01

Through a coordinated effort among the electrical engineering research team of the Florida State : University (FSU) and key Florida Department of Transportation (FDOT) personnel, an NTCIP-based : automated testing system for NTCIP-compliant ASC has b...

Employee Engagement Is Vital for the Successful Selection of a Total Laboratory Automation System.

PubMed

Yu, Hoi-Ying E; Wilkerson, Myra L

2017-11-08

To concretely outline a process for selecting a total laboratory automation system that connects clinical chemistry, hematology, and coagulation analyzers and to serve as a reference for other laboratories. In Phase I, a committee including the laboratory's directors and technologists conducted a review of 5 systems based on formal request for information process, site visits, and vendor presentations. We developed evaluation criteria and selected the 2 highest performing systems. In Phase II, we executed a detailed comparison of the 2 vendors based on cost, instrument layout, workflow design, and future potential. In addition to selecting a laboratory automation system, we used the process to ensure employee engagement in preparation for implementation. Selecting a total laboratory automation system is a complicated process. This paper provides practical guide in how a thorough selection process can be done with participation of key stakeholders. © American Society for Clinical Pathology, 2017. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com

Additive Construction with Mobile Emplacement (ACME) / Automated Construction of Expeditionary Structures (ACES) Materials Delivery System (MDS)

NASA Technical Reports Server (NTRS)

Mueller, R. P.; Townsend, I. I.; Tamasy, G. J.; Evers, C. J.; Sibille, L. J.; Edmunson, J. E.; Fiske, M. R.; Fikes, J. C.; Case, M.

2018-01-01

The purpose of the Automated Construction of Expeditionary Structures, Phase 3 (ACES 3) project is to incorporate the Liquid Goods Delivery System (LGDS) into the Dry Goods Delivery System (DGDS) structure to create an integrated and automated Materials Delivery System (MDS) for 3D printing structures with ordinary Portland cement (OPC) concrete. ACES 3 is a prototype for 3-D printing barracks for soldiers in forward bases, here on Earth. The LGDS supports ACES 3 by storing liquid materials, mixing recipe batches of liquid materials, and working with the Dry Goods Feed System (DGFS) previously developed for ACES 2, combining the materials that are eventually extruded out of the print nozzle. Automated Construction of Expeditionary Structures, Phase 3 (ACES 3) is a project led by the US Army Corps of Engineers (USACE) and supported by NASA. The equivalent 3D printing system for construction in space is designated Additive Construction with Mobile Emplacement (ACME) by NASA.

Evaluation of GPS position and attitude determination for automated rendezvous and docking missions. M.S. Thesis

NASA Technical Reports Server (NTRS)

Diprinzio, Marc D.; Tolson, Robert H.

1994-01-01

The use of the Global Positioning System for position and attitude determination is evaluated for an automated rendezvous and docking mission. The typical mission scenario involves the chaser docking with the target for resupply or repair purposes, and is divided into three sections. During the homing phase, the chaser utilizes coarse acquisition pseudorange data to approach the target; guidance laws for this stage are investigated. In the second phase, differential carrier phase positioning is utilized. The chaser must maintain a quasiconstant distance from the target, in order to resolve the initial integer ambiguities. Once the ambiguities are determined, the terminal phase is entered, and the rendezvous is completed with continuous carrier phase tracking. Attitude knowledge is maintained in all phases through the use of the carrier phase observable. A Kalman filter is utilized to estimate all states from the noisy measurement data. The effects of selective availability and cycle slips are also investigated.

Microfluidic multiplexing of solid-state nanopores

NASA Astrophysics Data System (ADS)

Jain, Tarun; Rasera, Benjamin C.; Guerrero, Ricardo Jose S.; Lim, Jong-Min; Karnik, Rohit

2017-12-01

Although solid-state nanopores enable electronic analysis of many clinically and biologically relevant molecular structures, there are few existing device architectures that enable high-throughput measurement of solid-state nanopores. Herein, we report a method for microfluidic integration of multiple solid-state nanopores at a high density of one nanopore per (35 µm2). By configuring microfluidic devices with microfluidic valves, the nanopores can be rinsed from a single fluid input while retaining compatibility for multichannel electrical measurements. The microfluidic valves serve the dual purpose of fluidic switching and electric switching, enabling serial multiplexing of the eight nanopores with a single pair of electrodes. Furthermore, the device architecture exhibits low noise and is compatible with electroporation-based in situ nanopore fabrication, providing a scalable platform for automated electronic measurement of a large number of integrated solid-state nanopores.

Comparison of the solid-phase fragment condensation and phase-change approaches in the synthesis of salmon I calcitonin.

PubMed

Gatos, D; Tzavara, C

2001-02-01

Salmon I calcitonin was synthesized using both phase-change and conventional solid-phase fragment condensation (SPFC) approaches, utilizing the Rink amide linker (Fmoc-amido-2,4-dimethoxybenzyl-4-phenoxyacetic acid) combined with 2-chlorotrityl resin and the Fmoc/tBu(Trt)-based protection scheme. Phase-change synthesis, performed by the selective detachment of the fully protected C-terminal 22-mer peptide-linker from the resin and subsequent condensation in solution with the N-terminal 1-10 fragment, gave a product of slightly less purity (85 vs. 92%) than the corresponding synthesis on the solid-phase. In both cases salmon I calcitonin was easily obtained in high purity.

Open-Label, Multicenter, Phase 1/2 Study of Tazemetostat (EZH2 Histone Methyl Transferase [HMT] Inhibitor) as a Single Agent in Subjects With Adv. Solid Tumors or With B-cell Lymphomas and Tazemetostat in Combination With Prednisolone in Subjects With DLBCL

ClinicalTrials.gov

2018-05-31

B-cell Lymphomas (Phase 1); Advanced Solid Tumors (Phase 1); Diffuse Large B-cell Lymphoma (Phase 2); Follicular Lymphoma (Phase 2); Transformed Follicular Lymphoma; Primary Mediastinal Large B-Cell Lymphoma

Creation of Anatomically Accurate Computer-Aided Design (CAD) Solid Models from Medical Images

NASA Technical Reports Server (NTRS)

Stewart, John E.; Graham, R. Scott; Samareh, Jamshid A.; Oberlander, Eric J.; Broaddus, William C.

1999-01-01

Most surgical instrumentation and implants used in the world today are designed with sophisticated Computer-Aided Design (CAD)/Computer-Aided Manufacturing (CAM) software. This software automates the mechanical development of a product from its conceptual design through manufacturing. CAD software also provides a means of manipulating solid models prior to Finite Element Modeling (FEM). Few surgical products are designed in conjunction with accurate CAD models of human anatomy because of the difficulty with which these models are created. We have developed a novel technique that creates anatomically accurate, patient specific CAD solids from medical images in a matter of minutes.

Pre-analytical phase: The automated ProTube device supports quality assurance in the phlebotomy process.

PubMed

Piva, Elisa; Tosato, Francesca; Plebani, Mario

2015-12-07

Most errors in laboratory medicine occur in the pre-analytical phase of the total testing process. Phlebotomy, a crucial step in the pre-analytical phase influencing laboratory results and patient outcome, calls for quality assurance procedures and automation in order to prevent errors and ensure patient safety. We compared the performance of a new small, automated device, the ProTube Inpeco, designed for use in phlebotomy with a complete traceability of the process, with a centralized automated system, BC ROBO. ProTube was used for 15,010 patients undergoing phlebotomy with 48,776 tubes being labeled. The mean time and standard deviation (SD) for blood sampling was 3:03 (min:sec; SD ± 1:24) when using ProTube, against 5:40 (min:sec; SD ± 1:57) when using BC ROBO. The mean number of patients per hour managed at each phlebotomy point was 16 ± 3 with ProTube, and 10 ± 2 with BC ROBO. No tubes were labeled erroneously or incorrectly, even if process failure occurred in 2.8% of cases when ProTube was used. Thanks to its cutting edge technology, the ProTube has many advantages over BC ROBO, above all in verifying patient identity, and in allowing a reduction in both identification error and tube mislabeling.

Analysis of nicotine and cotinine in hair by on-line in-tube solid-phase microextraction coupled with liquid chromatography-tandem mass spectrometry as biomarkers of exposure to tobacco smoke.

PubMed

Inukai, Takehito; Kaji, Sanae; Kataoka, Hiroyuki

2018-07-15

Smoking not only increases the risk of lung cancer but is strongly related to the onset of cardiovascular disease. Particularly, passive smoking due to sidestream smoke is a critical public health problem. To assess active and passive exposure to tobacco smoke, we developed a simple and sensitive method, consisting of on-line in-tube solid phase microextraction (SPME) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS), to determine nicotine and its metabolite cotinine in hair samples. These compounds were separated within 5 min using a Polar-RP80A column and detected in the positive ion mode by multiple reaction monitoring. The optimum in-tube SPME conditions were 25 draw/eject cycles of 40 μL of sample at a flow rate of 200 μL/min using a Carboxen 1006 capillary column as an extraction device. The extracted compounds in the stationary phase on the inner wall of the capillary could be dissolved easily into the mobile phase and transferred to an LC column. Using the in-tube SPME LC-MS/MS method, the calibration curves were linear in the 5-1000 pg/mL ranges for nicotine and cotinine, and the detection limits (signal to noise ratio of 3) were 0.45 and 0.13 pg/mL, respectively. The intra-day and inter-day precisions were below 3.4% and 6.0% (n = 5), respectively. This method was utilized successfully to analyze pg/mg levels of nicotine and cotinine in 1 mg of hairs without interference peaks, and good recoveries were obtained. The concentration of cotinine in hair was two orders of magnitude lower than that of nicotine, but a good positive correlation was found between the concentrations of these compounds. This method can automate the extraction, concentration and analysis of samples, and is useful for the assessment of long-term exposure to tobacco smoke. Copyright © 2018 Elsevier B.V. All rights reserved.

High-throughput determination of faropenem in human plasma and urine by on-line solid-phase extraction coupled to high-performance liquid chromatography with UV detection and its application to the pharmacokinetic study.

PubMed

Xie, Rui; Wen, Jun; Wei, Hua; Fan, Guorong; Zhang, Dabing

2010-05-01

An automated system using on-line solid-phase extraction and HPLC with UV detection was developed for the determination of faropenem in human plasma and urine. Analytical process was performed isocratically with two reversed-phase columns connected by a switching valve. After simple pretreatment for plasma and urine with acetonitrile, a volume of 100microl upper layer of the plasma or urine samples was injected for on-line SPE column switching HPLC-UV analysis. The analytes were retained on the self-made trap column (Lichrospher C(18), 4.6mmx37mm, 25microm) with the loading solvent (20mM NaH(2)PO(4) adjusted pH 3.5) at flow rate of 2mlmin(-1), and most matrix materials were removed from the column to waste. After 0.5min washing, the valve was switched to another position so that the target analytes could be eluted from trap column to analytical column in the back-flush mode by the mobile phase (acetonitrile-20mM NaH(2)PO(4) adjusted pH 3.5, 16:84, v/v) at flow rate of 1.5mlmin(-1), and then separated on the analytical column (Ultimate XB-C(18), 4.6mmx50mm, 5microm).The complete cycle of the on-line SPE preconcentration purification and HPLC separation of the analytes was 5min. Calibration curves with good linearities (r=0.9994 for plasma sample and r=0.9988 for urine sample) were obtained in the range 0.02-5microgml(-1) in plasma and 0.05-10microg ml(-1) in urine for faropenem. The optimized method showed good performance in terms of specificity, linearity, detection and quantification limits, precision and accuracy. The method was successfully utilized to quantify faropenem in human plasma and urine to support the clinical pharmacokinetic studies. Copyright 2009 Elsevier B.V. All rights reserved.

The major volume /density/ of solid oxygen in equilibrium with vapor

NASA Technical Reports Server (NTRS)

Roder, H. M.

1979-01-01

Data from the literature on the molar volume of solid oxygen have been compiled and critically analyzed. A correlated and thermodynamically consistent set of molar volumes, including the volume changes at the various solid phase transitions, is presented. Evidence for the existence of a delta-solid phase is reviewed. Uncertainties in the data and in the recommended set of values are discussed.

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

NASA Astrophysics Data System (ADS)

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.

A novel mechanical model for phase-separation in debris flows

NASA Astrophysics Data System (ADS)

Pudasaini, Shiva P.

2015-04-01

Understanding the physics of phase-separation between solid and fluid phases as a two-phase mass moves down slope is a long-standing challenge. Here, I propose a fundamentally new mechanism, called 'separation-flux', that leads to strong phase-separation in avalanche and debris flows. This new model extends the general two-phase debris flow model (Pudasaini, 2012) to include a separation-flux mechanism. The new flux separation mechanism is capable of describing and controlling the dynamically evolving phase-separation, segregation, and/or levee formation in a real two-phase, geometrically three-dimensional debris flow motion and deposition. These are often observed phenomena in natural debris flows and industrial processes that involve the transportation of particulate solid-fluid mixture material. The novel separation-flux model includes several dominant physical and mechanical aspects that result in strong phase-separation (segregation). These include pressure gradients, volume fractions of solid and fluid phases and their gradients, shear-rates, flow depth, material friction, viscosity, material densities, boundary structures, gravity and topographic constraints, grain shape, size, etc. Due to the inherent separation mechanism, as the mass moves down slope, more and more solid particles are brought to the front, resulting in a solid-rich and mechanically strong frontal surge head followed by a weak tail largely consisting of the viscous fluid. The primary frontal surge head followed by secondary surge is the consequence of the phase-separation. Such typical and dominant phase-separation phenomena are revealed here for the first time in real two-phase debris flow modeling and simulations. However, these phenomena may depend on the bulk material composition and the applied forces. Reference: Pudasaini, Shiva P. (2012): A general two-phase debris flow model. J. Geophys. Res., 117, F03010, doi: 10.1029/2011JF002186.

Impact of Implementation of an Automated Liquid Culture System on Diagnosis of Tuberculous Pleurisy.

PubMed

Lee, Byung Hee; Yoon, Seong Hoon; Yeo, Hye Ju; Kim, Dong Wan; Lee, Seung Eun; Cho, Woo Hyun; Lee, Su Jin; Kim, Yun Seong; Jeon, Doosoo

2015-07-01

This study was conducted to evaluate the impact of implementation of an automated liquid culture system on the diagnosis of tuberculous pleurisy in an HIV-uninfected patient population. We retrospectively compared the culture yield, time to positivity, and contamination rate of pleural effusion samples in the BACTEC Mycobacteria Growth Indicator Tube 960 (MGIT) and Ogawa media among patients with tuberculous pleurisy. Out of 104 effusion samples, 43 (41.3%) were culture positive on either the MGIT or the Ogawa media. The culture yield of MGIT was higher (40.4%, 42/104) than that of Ogawa media (18.3%, 19/104) (P<0.001). One of the samples was positive only on the Ogawa medium. The median time to positivity was faster in the MGIT (18 days, range 8-32 days) than in the Ogawa media (37 days, range 20-59 days) (P<0.001). No contamination or growth of nontuberculous mycobacterium was observed on either of the culture media. In conclusion, the automated liquid culture system could provide approximately twice as high yields and fast results in effusion culture, compared to solid media. Supplemental solid media may have a limited impact on maximizing sensitivity in effusion culture; however, further studies are required.

Automated Ground Umbilical Systems (AGUS) Project

NASA Technical Reports Server (NTRS)

Gosselin, Armand M.

2007-01-01

All space vehicles require ground umbilical systems for servicing. Servicing requirements can include, but are not limited to, electrical power and control, propellant loading and venting, pneumatic system supply, hazard gas detection and purging as well as systems checkout capabilities. Of the various types of umbilicals, all require several common subsystems. These typically include an alignment system, mating and locking system, fluid connectors, electrical connectors and control !checkout systems. These systems have been designed to various levels of detail based on the needs for manual and/or automation requirements. The Automated Ground Umbilical Systems (AGUS) project is a multi-phase initiative to develop design performance requirements and concepts for launch system umbilicals. The automation aspect minimizes operational time and labor in ground umbilical processing while maintaining reliability. This current phase of the project reviews the design, development, testing and operations of ground umbilicals built for the Saturn, Shuttle, X-33 and Atlas V programs. Based on the design and operations lessons learned from these systems, umbilicals can be optimized for specific applications. The product of this study is a document containing details of existing systems and requirements for future automated umbilical systems with emphasis on design-for-operations (DFO).

Estrogenic and AhR activities in dissolved phase and suspended solids from wastewater treatment plants.

PubMed

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.

Hydrothermal carbonization of food waste for nutrient recovery and reuse.

PubMed

Idowu, Ifeolu; Li, Liang; Flora, Joseph R V; Pellechia, Perry J; Darko, Samuel A; Ro, Kyoung S; Berge, Nicole D

2017-11-01

Food waste represents a rather large and currently underutilized source of potentially available and reusable nutrients. Laboratory-scale experiments evaluating the hydrothermal carbonization of food wastes collected from restaurants were conducted to understand how changes in feedstock composition and carbonization process conditions influence primary and secondary nutrient fate. Results from this work indicate that at all evaluated reaction times and temperatures, the majority of nitrogen, calcium, and magnesium remain integrated within the solid-phase, while the majority of potassium and sodium reside in the liquid-phase. The fate of phosphorus is dependent on reaction times and temperatures, with solid-phase integration increasing with higher reaction temperature and longer time. A series of leaching experiments to determine potential solid-phase nutrient availability were also conducted and indicate that, at least in the short term, nitrogen release from the solids is small, while almost all of the phosphorus present in the solids produced from carbonizing at 225 and 250°C is released. At a reaction temperature of 275°C, smaller fractions of the solid-phase total phosphorus are released as reaction times increase, likely due to increased solids incorporation. Using these data, it is estimated that up to 0.96% and 2.30% of nitrogen and phosphorus-based fertilizers, respectively, in the US can be replaced by the nutrients integrated within hydrochar and liquid-phases generated from the carbonization of currently landfilled food wastes. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effect of proximal vagotomy and Roux-en-Y diversion on gastric emptying kinetics in asymptomatic patients.

PubMed

Urbain, J L; Penninckx, F; Siegel, J A; Vandenborre, P; Van Cutsem, E; Vandenmaegdenbergh, V; De Roo, M

1990-10-01

The role of the distal stomach in gastric emptying was studied. Ten patients with proximal gastric vagotomy (PV) and 10 age-matched patients with Roux-en-Y gastro-jejunostomy (R-Y) were compared with 10 healthy controls. Gastric emptying of solids and liquids was determined by the use of Tc-99m SC scrambled eggs and In-111 DTPA. In PV, gastric emptying of both solids and liquids was delayed; the prolongation with solids was mainly accounted for by an abnormal lag phase. In R-Y patients, no lag phase was observed, and the solid emptying curve pattern was characterized by early rapid emptying followed by very slow emptying. Both the solid and liquid phases were prolonged. The lag phase is affected by proximal vagotomy and is mainly determined by the distal stomach, which appears to be essential for normal emptying.

Phase Behavior of Binary Mixture of Heptaethylene Glycol Decyl Ether and Water: Formation of Phase Compound in Solid Phase

PubMed

Nibu; Suemori; Inoue

1997-07-01

Differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FT-IR) were used to construct and characterize the phase diagram for a binary mixture of heptaethylene glycol decyl ether (C10 E7 ) and water in the temperature range from -60 to 80°C. Plots of the endothermic peak temperatures obtained by DSC measurements against compositions provided eutectic solid-liquid phase boundaries with a eutectic composition of 34 wt% of H2 O. On the other hand, heat of fusion per unit weight of the mixture changed discretely at the composition corresponding to the "eutectic" composition. Furthermore, the IR spectra obtained for the mixture in the solid phase were well reproduced as a superposition of those for the mixture of 34 wt% H2 O and pure components but were not reproduced by superimposing the spectra obtained for the solid surfactant and ice. These observations indicate that a solid phase compound is formed between C10 E7 and water with a stoichiometry of 1:14 and that the compound and pure components exist as separate phases, rather than the phases separating into surfactant and ice, which would be expected if the C10 E7 /water mixture formed a true eutectic mixture system. It is estimated from the composition corresponding to the phase compounds that two molecules of water per oxyethylene unit are bound to hydrophilic polyoxyethylene chain of C10 E7 to form a hydrated compound.

Amorphous silicon photovoltaic manufacturing technology, phase 2A

NASA Astrophysics Data System (ADS)

Duran, G.; Mackamul, K.; Metcalf, D.

1995-01-01

Utility Power Group (UPG), and its lower-tier subcontractor, Advanced Photovoltaic Systems, Inc. (APS) have conducted efforts in developing their manufacturing lines. UPG has focused on the automation of encapsulation and termination processes developed in Phase 1. APS has focused on completion of the encapsulation and module design tasks, while continuing the process and quality control and automation projects. The goal is to produce 55 watt (stabilized) EP50 modules in a new facility. In the APS Trenton EUREKA manufacturing facility, APS has: (1) Developed high throughput lamination procedures; (2) Optimized existing module designs; (3) Developed new module designs for architectural applications; (4) Developed enhanced deposition parameter control; (5) Designed equipment required to manufacture new EUREKA modules developed during Phase II; (6) Improved uniformity of thin-film materials deposition; and (7) Improved the stabilized power output of the APS EP50 EUREKA module to 55 watts. In the APS Fairfield EUREKA manufacturing facility, APS has: (1) Introduced the new products developed under Phase 1 into the APS Fairfield EUREKA module production line; (2) Increased the extent of automation in the production line; (3) Introduced Statistical Process Control to the module production line; and (4) Transferred-progress made in the APS Trenton facility into the APS Fairfield facility.

Quantification of VX Nerve Agent in Various Food Matrices by Solid-Phase Extraction Ultra-Performance Liquid ChromatographyTime-of-Flight Mass Spectrometry

DTIC Science & Technology

2016-04-01

QUANTIFICATION OF VX NERVE AGENT IN VARIOUS FOOD MATRICES BY SOLID-PHASE EXTRACTION ULTRA-PERFORMANCE...TITLE AND SUBTITLE Quantification of VX Nerve Agent in Various Food Matrices by Solid-Phase Extraction Ultra-Performance Liquid Chromatography... food matrices. The mixed-mode cation exchange (MCX) sorbent and Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) methods were used for

Implementation of a solid target production facility

NASA Astrophysics Data System (ADS)

Tochon-Danguy, H. J.; Poniger, S. S.; Sachinidis, J. I.; Panopoulos, H. P.; Scott, A. M.

2012-12-01

The desire to utilize long-lived PET isotopes in Australia has significantly increased over the years and several research projects for labelling of peptides, proteins and biomolecules, including labelling of recombinant antibodies has been restricted due to the limited availability of suitable isotopes. This need has led to the recent installation and commissioning of a new facility dedicated to fully automated solid target isotope production, including 24I, 64Cu, 89Zr and 86Y at the Austin Health Centre for PET.

Automating Phase Change Lines and Their Labels Using Microsoft Excel(R).

PubMed

Deochand, Neil

2017-09-01

Many researchers have rallied against drawn in graphical elements and offered ways to avoid them, especially regarding the insertion of phase change lines (Deochand, Costello, & Fuqua, 2015; Dubuque, 2015; Vanselow & Bourret, 2012). However, few have offered a solution to automating the phase labels, which are often utilized in behavior analytic graphical displays (Deochand et al., 2015). Despite the fact that Microsoft Excel® is extensively utilized by behavior analysts, solutions to resolve issues in our graphing practices are not always apparent or user-friendly. Considering the insertion of phase change lines and their labels constitute a repetitious and laborious endeavor, any minimization in the steps to accomplish these graphical elements could offer substantial time-savings to the field. The purpose of this report is to provide an updated way (and templates in the supplemental materials) to add phase change lines with their respective labels, which stay embedded to the graph when they are moved or updated.

Methods of Analysis by the U.S. Geological Survey Organic Geochemistry Research Group?Determination of acetamide herbicides and their degradation products in water using online solid-phase extraction and liquid chromatography/mass spectrometry

USGS Publications Warehouse

Lee, E.A.; Strahan, A.P.

2003-01-01

An analytical method for the determination of 6 acetamide herbicides (acetochlor, alachlor, dimethenamid, flufenacet, metolachlor, and propachlor) and 16 of their degradation products in natural water samples using solid-phase extraction and liquid chromatography/mass spectrometry is described in this report. Special consideration was given during the development of the method to prevent the formation of degradation products during the analysis. Filtered water samples were analyzed using octadecylsilane as the solid-phase extraction media on online automated equipment followed by liquid chromatography/mass spectrometry. The method uses only 10 milliliters of sample per injection. Three different water-sample matrices, a reagent-water, a ground-water, and a surface-water sample spiked at 0.10 and 1.0 microgram per liter, were analyzed to determine method performance. Method detection limits ranged from 0.004 to 0.051 microgram per liter for the parent acetamide herbicides and their degradation products. Mean recoveries for the acetamide compounds in the ground- and surface-water samples ranged from 62.3 to 117.4 percent. The secondary amide of acetochlor/metolachlor ethanesulfonic acid (ESA) was recovered at an average rate of 43.5 percent. The mean recoveries for propachlor and propachlor oxanilic acid (OXA) were next lowest, ranging from 62.3 to 95.5 percent. Mean recoveries from reagent-water samples ranged from 90.3 to 118.3 percent for all compounds. Overall the mean of the mean recoveries of all compounds in the three matrices spiked at 0.10 and 1.0 microgram per liter ranged from 89.9 to 100.7 percent, including the secondary amide of acetochlor/metolachlor ESA and the propachlor compounds. The acetamide herbicides and their degradation products are reported in concentrations ranging from 0.05 to 2.0 micrograms per liter. The upper concentration limit is 2.0 micrograms per liter for all compounds without dilution. With the exception of the secondary amide of acetochlor/metolachlor ESA, good precision and accuracy for the chloroacetanalide herbicides and their degradation compounds were demonstrated for the method in buffered reagent water, ground water, and surface water. The extraction method as used did not optimize the recovery of the secondary amide of acetochlor/metolachlor ESA.

A dipole-assisted solid-phase extraction microchip combined with inductively coupled plasma-mass spectrometry for online determination of trace heavy metals in natural water.

PubMed

Shih, Tsung-Ting; Hsu, I-Hsiang; Chen, Shun-Niang; Chen, Ping-Hung; Deng, Ming-Jay; Chen, Yu; Lin, Yang-Wei; Sun, Yuh-Chang

2015-01-21

We employed a polymeric material, poly(methyl methacrylate) (PMMA), for fabricating a microdevice and then implanted the chlorine (Cl)-containing solid-phase extraction (SPE) functionality into the PMMA chip to develop an innovative on-chip dipole-assisted SPE technique. Instead of the ion-ion interactions utilized in on-chip SPE techniques, the dipole-ion interactions between the highly electronegative C-Cl moieties in the channel interior and the positively charged metal ions were employed to facilitate the on-chip SPE procedures. Furthermore, to avoid labor-intensive manual manipulation, a programmable valve manifold was designed as an interface combining the dipole-assisted SPE microchip and inductively coupled plasma-mass spectrometry (ICP-MS) to achieve the fully automated operation. Under the optimized operation conditions for the established system, the detection limits for each analyte ion were obtained based on three times the standard deviation of seven measurements of the blank eluent solution. The limits ranged from 3.48 to 20.68 ng L(-1), suggesting that this technique appears uniquely suited for determining the levels of heavy metal ions in natural water. Indeed, a series of validation procedures demonstrated that the developed method could be satisfactorily applied to the determination of trace heavy metals in natural water. Remarkably, the developed device was durable enough to be reused more than 160 times without any loss in its analytical performance. To the best of our knowledge, this is the first study reporting on the combination of a dipole-assisted SPE microchip and elemental analysis instrument for the online determination of trace heavy metal ions.

A novel aptamer-based online magnetic solid phase extraction method for the selective determination of 8-hydroxy-2'-deoxyguanosine in human urine.

PubMed

Gan, Haijiao; Xu, Hui

2018-05-30

In this work, an innovative magnetic aptamer adsorbent (Fe 3 O 4 -aptamer MNPs) was synthesized for the selective extraction of 8-hydroxy-2'-deoxyguanosine (8-OHdG). Amino-functionalized-Fe 3 O 4 was crosslinked with 8-OHdG aptamer by glutaraldehyde and fixed into a steel stainless tube as the sorbent of magnetic solid phase extraction (MSPE). After selective extraction by the aptamer adsorbent, the adsorbed 8-OHdG was desorbed dynamically and online analyzed by high performance liquid chromatography-mass spectrometry (HPLC-MS). The synthesized sorbent presented outstanding features, including specific selectivity, high enrichment capacity, stability and biocompatibility. Moreover, this proposed MSPE-HPLC-MS can achieve adsorption and desorption operation integration, greatly simplify the analysis process and reduce human errors. When compared with offline MSPE, a sensitivity enhancement of 800 times was obtained for the online method. Some experimental parameters such as the amount of the sorbent, sample flow rate and sample volume, were optimized systematically. Under the optimal conditions, low limit of detection (0.01 ng mL -1 , S/N = 3), limit of quantity (0.03 ng mL -1 , S/N = 10) and wide linear range with a satisfactory correlation coefficient (R 2  ≥ 0.9992) were obtained. And the recoveries of 8-OHdG in the urine samples varied from 82% to 116%. All these results revealed that the method is simple, rapid, selective, sensitive and automated, and it could be expected to become a potential approach for the selective determination of trace 8-OHdG in complex urinary samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of needle trap micro-extraction and automatic alveolar sampling for point-of-care breath analysis.

PubMed

Trefz, Phillip; Rösner, Lisa; Hein, Dietmar; Schubert, Jochen K; Miekisch, Wolfram

2013-04-01

Needle trap devices (NTDs) have shown many advantages such as improved detection limits, reduced sampling time and volume, improved stability, and reproducibility if compared with other techniques used in breath analysis such as solid-phase extraction and solid-phase micro-extraction. Effects of sampling flow (2-30 ml/min) and volume (10-100 ml) were investigated in dry gas standards containing hydrocarbons, aldehydes, and aromatic compounds and in humid breath samples. NTDs contained (single-bed) polymer packing and (triple-bed) combinations of divinylbenzene/Carbopack X/Carboxen 1000. Substances were desorbed from the NTDs by means of thermal expansion and analyzed by gas chromatography-mass spectrometry. An automated CO2-controlled sampling device for direct alveolar sampling at the point-of-care was developed and tested in pilot experiments. Adsorption efficiency for small volatile organic compounds decreased and breakthrough increased when sampling was done with polymer needles from a water-saturated matrix (breath) instead from dry gas. Humidity did not affect analysis with triple-bed NTDs. These NTDs showed only small dependencies on sampling flow and low breakthrough from 1-5 %. The new sampling device was able to control crucial parameters such as sampling flow and volume. With triple-bed NTDs, substance amounts increased linearly with increasing sample volume when alveolar breath was pre-concentrated automatically. When compared with manual sampling, automatic sampling showed comparable or better results. Thorough control of sampling and adequate choice of adsorption material is mandatory for application of needle trap micro-extraction in vivo. The new CO2-controlled sampling device allows direct alveolar sampling at the point-of-care without the need of any additional sampling, storage, or pre-concentration steps.

High-throughput analysis of bergamot essential oil by fast solid-phase microextraction-capillary gas chromatography-flame ionization detection.

PubMed

Tranchida, Peter Quinto; Presti, Maria Lo; Costa, Rosaria; Dugo, Paola; Dugo, Giovanni; Mondello, Luigi

2006-01-20

The advantages of using a narrow-bore column in headspace solid-phase microextraction-gas chromatographic (HS-SPME-GC) analysis are investigated. An automated rapid HS-SPME-GC method for the determination of volatile compounds in a complex sample (bergamot essential oil) was developed. A low-capacity (7 microm) SPME fibre was employed, enabling a short equilibration time (15 min). The absorbed volatile compounds were then separated in 12.5 min on a 10 m x 0.1 mm I.D. capillary. The fast GC method was characterized by relatively moderate GC parameters (head pressure: 173 kPa; temperature program rate: 12 degrees C/min). The employment of the low-capacity fibre also suited the reduced sample capacity of the capillary employed, hence column overloading was avoided. Analytical repeatibility was determined in terms of retention times (maximum RSD: 0.32%) and peak areas (maximum RSD: 9.80%). The results obtained were compared to those derived from a conventional HS-SPME-GC (a 30 microm SPME fibre and 0.25 mm I.D. capillary were used) application on the same sample. In this respect, a great reduction of analytical time was obtained both with regard to the conventional SPME equilibration and GC run times, which both required 50 min. Peak resolution was altogether comparable in both applications. Although a slight loss in terms of sensitivity was observed in the rapid approach (generally within the 25-50% range), this did not impair the detection of all peaks of interest. Finally, the selectivities of the 30 and 7 microm fibres were evaluated and, as expected, these were in good agreement.

Bacterial rapid identification with matrix assisted laser desorption/ionization time-of-flight mass spectrometry: development of an 'in-house method' and comparison with Bruker Sepsityper(®) kit.

PubMed

Frédéric Ric, S; Antoine, M; Bodson, A; Lissoir, B

2015-10-01

The objective of this study was to compare an in-house matrix-assisted laser desorption ionization with time of flight (MALDI-TOF) method and a commercial MALDI-TOF kit (Sepsityper(®) kit) for direct bacterial identification in positive blood cultures. We also evaluated the time saved and the cost associated with the rapid identification techniques. We used the BACTEC(®) automated system for detecting positive blood cultures. Direct identification using Sepsityper kit and the in-house method were compared with conventional identification by MALDI-TOF using pure bacterial culture on the solid phase. We also evaluated different cut-off scores for rapid bacterial identification. In total, 127 positive blood vials were selected. The rate of rapid identification with the MALDI Sepsityper kit was 25.2% with the standard cut-off and 33.9% with the enlarged cut-off, while the results for the in-house method were 44.1 and 61.4%, respectively. Error rates with the enlarged cut-off were 6.98 (n = 3) and 2.56% (n = 2) for Sepsityper and the in-house method, respectively. Identification rates were higher for gram-negative bacteria. Direct bacterial identification succeeded in supplying rapid identification of the causative organism in cases of sepsis. The time taken to obtain a result was nearly 24  hours shorter for the direct bacterial identification methods than for conventional MALDI-TOF on solid phase culture. Compared with the Sepsityper kit, the in-house method offered better results and fewer errors, was more cost-effective and easier to use.

A validated method for rapid determination of dibenzo-p-dioxins/furans (PCDD/Fs), polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in human milk: focus on utility of tandem solid phase extraction (SPE) cleanup.

PubMed

Lin, Yuanjie; Feng, Chao; Xu, Qian; Lu, Dasheng; Qiu, Xinlei; Jin, Yu'e; Wang, Guoquan; Wang, Dongli; She, Jianwen; Zhou, Zhijun

2016-07-01

An improved method based on tandem solid phase extraction (SPE) cleanup and gas chromatography-high resolution mass spectrometry (GC-HRMS) has been validated for a rapid determination of dibenzo-p-dioxins/furans (PCDD/Fs), dioxin-like polychlorinated biphenyls (PCBs), marker polychlorinated biphenyls (M-PCBs), and polybrominated diphenyl ethers (PBDEs) using a large volume (50 mL) of human milk. This method was well validated for the measurement of these analytes in human milk from the general population with low limits of detection (LODs, 0.004-0.12 ng/g lipid), satisfactory accuracy (75-120 % of recoveries), and precision [less than 10 % of relative standard deviations (RSDs)]. To comprehensively evaluate the performance of this method, a good, presently validated and routinely used method based on an automated sample clean-up system (ASCS, based on the commercial acid multilayer silica, basic alumina, and carbon columns) was used in parallel for comparison. Compared with the ASCS method, this method presented comparable specificity. Additionally, this method, in contrast to ASCS method, highly reduced consumption of solvents (40 mL versus 500 mL), which results in much lower background in the procedural blank, reduced time, and enhanced sample pretreatment throughput. This method was also applied in a pilot study to measure a batch of human milk samples with satisfactory results. Graphical Abstract Characteristics of the application of tandem SPE cleanup for determination of PCDD/Fs, DL-PCBs,M-PCBs and PBDEs in human milk.

An improved method for the analysis of 2-aminoacetophenone in wine based on headspace solid-phase microextraction and heart-cut multidimensional gas chromatography with selective detection by tandem mass spectrometry.

PubMed

Schmarr, Hans-Georg; Keiser, Jutta; Krautwald, Susann

2016-12-16

Heart-cut multidimensional gas chromatography coupled to selective mass spectrometric detection (H/C MDGC-MS-MS) was shown to be a suitable combination for analysis of the key component for the wine off-flavor named "atypical aging off-flavor" (german: "Untypische Alterungsnote", UTA), 2-aminoacetophenone (2-AAP). Headspace solid phase microextraction (HS-SPME) was applied as an easy to automate sample preparation step suiting routine control situations. During method development two critical aspects were found, of which one is the chemical degradation of the neat substance, leading to signal reduction and a false response behavior. A second aspect is the pH stability of the deuterated isotopologue 1-(2-aminophenyl)-2,2,2-trideuterio-ethanone (2-AAP-d3) used for quantification via a stable isotope dilution assay. Despite an earlier suggestion to increase the extractable amount of 2-AAP and its isotopic standard in the headspace, alkalization of 2-AAP-d3 containing aqueous samples were found to be critical. In such a milieu a deuterium exchange can then cause erroneous quantitative results. The method proposed in our study thus uses native wine pH conditions and proved to be suitable for routine control with respect to the detection of the "atypical aging off-flavor" in wine at concentration levels below its sensory threshold of about 1μgL -1 . Good linearity was obtained in the calibrated range from 0.1-8μgL -1 (y=1,2338x+0,1029, R=0,9985) with limits of detection or quantification being 0.01 and 0.14μg/L, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry for the determination of haloanisoles in sparkling (cava and cider) and non-sparkling (wine) alcoholic beverages.

PubMed

Ruiz-Delgado, Ana; Arrebola-Liébanas, Francisco Javier; Romero-González, Roberto; López-Ruiz, Rosalía; Garrido Frenich, Antonia

2016-10-01

A highly sensitive analytical method was developed to determine 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and 2,3,4,5,6-pentachloroanisole (PCA) in sparkling alcoholic beverages. The method was based on the use of headspace solid-phase microextraction (HS-SPME) using a polydimethylsiloxane (PDMS) fibre. It was coupled to gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS/MS) for the detection and quantification of the target haloanisoles. The method was fully automated and no sample preparation was needed. The method was validated for alcoholic beverages. The influence of CO 2 on the extraction efficiency was also evaluated for the studied sparkling drinks (cava and cider). All the calibration curves showed good linearity (R 2  > 0.98) within the tested range (1-50 ng l -1 ). Recoveries were evaluated at three different levels (1, 5 and 50 ng l -1 ) and were always between 71% and 119%. Precision was expressed as relative standard deviation (RSD), and was evaluated as intra- and inter-day precisions, with values ≤ 22% in both cases. Limits of quantitation (LOQs) were ≤ 0.91 ng l -1 , which are below the sensory threshold levels for such compounds in humans. The validated method was applied to commercial samples, 10 cavas and 10 ciders, but it was also used for the analysis of nine red wines and four white wines, demonstrating the further applicability of the proposed method to non-sparkling beverages. TCA was detected in most samples at up to 0.45 ng l -1 .

Automated Solid-Phase Protein Modification with Integrated Enzymatic Digest for Reaction Validation: Application of a Compartmented Microfluidic Reactor for Rapid Optimization and Analysis of Protein Biotinylation

PubMed Central

Fraas, Regina; Diehm, Juliane; Franzreb, Matthias

2017-01-01

Protein modification by covalent coupling of small ligands or markers is an important prerequisite for the use of proteins in many applications. Well-known examples are the use of proteins with fluorescent markers in many in vivo experiments or the binding of biotinylated antibodies via biotin–streptavidin coupling in the frame of numerous bioassays. Multiple protocols were established for the coupling of the respective molecules, e.g., via the C and N-terminus, or via cysteines and lysines exposed at the protein surface. Still, in most cases the conditions of these standard protocols are only an initial guess. Optimization of the coupling parameters like reagent concentrations, pH, or temperature may strongly increase coupling yield and the biological activity of the modified protein. In order to facilitate the process of optimizing coupling conditions, a method was developed which uses a compartmented microfluidic reactor for the rapid screening of different coupling conditions. In addition, the system allows for the integration of an enzymatic digest of the modified protein directly after modification. In combination with a subsequent MALDI-TOF analysis of the resulting fragments, this gives a fast and detailed picture not only of the number and extent of the generated modifications but also of their position within the protein sequence. The described process was demonstrated for biotinylation of green fluorescent protein. Different biotin-excesses and different pH-values were tested in order to elucidate the influence on the modification extent and pattern. In addition, the results of solid-phase based modifications within the microfluidic reactor were compared to modification patterns resulting from coupling trials with unbound protein. As expected, modification patterns of immobilized proteins showed clear differences to the ones of dissolved proteins. PMID:29181376

Commercialization of a novel fermentation concept.

PubMed

Mazumdar-Shaw, Kiran; Suryanarayan, Shrikumar

2003-01-01

Fermentation is the core of biotechnology where current methodologies span across technologies based on the use of either solid or liquid substrates. Traditionally, solid substrate fermentation technologies have been the widely practiced in the Far East to manufacture fermented foods such as soya sauce, sake etc. The Western World briefly used solid substrate fermentation for the manufacture of antibiotics and enzymes but rapidly replaced this technology with submerged fermentation which proved to be a superior technology in terms of automation, containment and large volume fermentation. Biocon India developed its enzyme technology based on solid substrate fermentation as a low-cost, low-energy option for the production of specialty enzymes. However, the limitations of applying solid substrate fermentation to more sophisticated biotechnology products as well as large volume fermentations were recognized by Biocon India as early as 1990 and the company embarked on a 8 year research and development program to develop a novel bioreactor capable of conducting solid substrate fermentation with comparable levels of automation and containment as those practiced by submerged fermentation. In addition, the novel technology enabled fed-batch fermentation, in situ extraction and other enabling features that will be discussed in this article. The novel bioreactor was christened the "PlaFractor" (pronounced play-fractor). The next level of research on this novel technology is now focused on addressing large volume fermentation. This article traces the evolution of Biocon India's original solid substrate fermentation to the PlaFractor technology and provides details of the scale-up and commercialization processes that were involved therein. What is also apparent in the article is Biocon India's commercially focused research programs and the perceived need to be globally competitive through low costs of innovation that address, at all times, processes and technologies that exhibit high degrees of conformance to the international standards of regulatory and good manufacturing practice.

Process development for automated solar cell and module production. Task 4: Automated array assembly

NASA Technical Reports Server (NTRS)

Hagerty, J. J.

1981-01-01

Progress in the development of automated solar cell and module production is reported. The unimate robot is programmed for the final 35 cell pattern to be used in the fabrication of the deliverable modules. The mechanical construction of the automated lamination station and final assembly station phases are completed and the first operational testing is underway. The final controlling program is written and optimized. The glass reinforced concrete (GRC) panels to be used for testing and deliverables are in production. Test routines are grouped together and defined to produce the final control program.

The Ten Outstanding Engineering Achievements of the Past 50 Years.

ERIC Educational Resources Information Center

Hightower, George

1984-01-01

Describes the outstanding achievement in each of 10 major engineering categories. These categories include synthetic fibers, nuclear energy, computers, solid state electronics, jet aircraft, biomedical engineering, lasers, communications satellites, the United States space program, and automation and control systems. (JN)

Around Marshall

NASA Image and Video Library

1988-09-19

Marshall's fifth Center Director, James R. Thompson (1986-1989), in the control room of the Solid Rocket Booster (SRB)automated thermal protection system (TPS) removal facility. Under Dr. Thompson's leadership, the shuttle program was rekindled after the Challenger explosion. Return to Flight kept NASA 's future programs alive.

Analytical methodologies based on LC-MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge.

PubMed

Boix, C; Ibáñez, M; Fabregat-Safont, D; Morales, E; Pastor, L; Sancho, J V; Sánchez-Ramírez, J E; Hernández, F

2016-01-01

In this work, two analytical methodologies based on liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) were developed for quantification of emerging pollutants identified in sewage sludge after a previous wide-scope screening. The target list included 13 emerging contaminants (EC): thiabendazole, acesulfame, fenofibric acid, valsartan, irbesartan, salicylic acid, diclofenac, carbamazepine, 4-aminoantipyrine (4-AA), 4-acetyl aminoantipyrine (4-AAA), 4-formyl aminoantipyrine (4-FAA), venlafaxine and benzoylecgonine. The aqueous and solid phases of the sewage sludge were analyzed making use of Solid-Phase Extraction (SPE) and UltraSonic Extraction (USE) for sample treatment, respectively. The methods were validated at three concentration levels: 0.2, 2 and 20 μg L(-1) for the aqueous phase, and 50, 500 and 2000 μg kg(-1) for the solid phase of the sludge. In general, the method was satisfactorily validated, showing good recoveries (70-120%) and precision (RSD < 20%). Regarding the limit of quantification (LOQ), it was below 0.1 μg L(-1) in the aqueous phase and below 50 μg kg(-1) in the solid phase for the majority of the analytes. The method applicability was tested by analysis of samples from a wider study on degradation of emerging pollutants in sewage sludge under anaerobic digestion. The key benefits of these methodologies are: • SPE and USE are appropriate sample procedures to extract selected emerging contaminants from the aqueous phase of the sewage sludge and the solid residue. • LC-MS/MS is highly suitable for determining emerging contaminants in both sludge phases. • Up to our knowledge, the main metabolites of dipyrone had not been studied before in sewage sludge.

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

NASA Astrophysics Data System (ADS)

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.

Automated Array Assembly, Phase 2

NASA Technical Reports Server (NTRS)

Carbajal, B. G.

1979-01-01

The Automated Array Assembly Task, Phase 2 of the Low Cost Silicon Solar Array Project is a process development task. The contract provides for the fabrication of modules from large area tandem junction cells (TJC). During this quarter, effort was focused on the design of a large area, approximately 36 sq cm, TJC and process verification runs. The large area TJC design was optimized for minimum I squared R power losses. In the TJM activity, the cell-module interfaces were defined, module substrates were formed and heat treated and clad metal interconnect strips were fabricated.

Quantitative tomographic measurements of opaque multiphase flows

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

GEORGE,DARIN L.; TORCZYNSKI,JOHN R.; SHOLLENBERGER,KIM ANN

2000-03-01

An electrical-impedance tomography (EIT) system has been developed for quantitative measurements of radial phase distribution profiles in two-phase and three-phase vertical column flows. The EIT system is described along with the computer algorithm used for reconstructing phase volume fraction profiles. EIT measurements were validated by comparison with a gamma-densitometry tomography (GDT) system. The EIT system was used to accurately measure average solid volume fractions up to 0.05 in solid-liquid flows, and radial gas volume fraction profiles in gas-liquid flows with gas volume fractions up to 0.15. In both flows, average phase volume fractions and radial volume fraction profiles from GDTmore » and EIT were in good agreement. A minor modification to the formula used to relate conductivity data to phase volume fractions was found to improve agreement between the methods. GDT and EIT were then applied together to simultaneously measure the solid, liquid, and gas radial distributions within several vertical three-phase flows. For average solid volume fractions up to 0.30, the gas distribution for each gas flow rate was approximately independent of the amount of solids in the column. Measurements made with this EIT system demonstrate that EIT may be used successfully for noninvasive, quantitative measurements of dispersed multiphase flows.« less

Biofuel production utilizing a dual-phase cultivation system with filamentous cyanobacteria.

PubMed

Aoki, Jinichi; Kawamata, Toru; Kodaka, Asuka; Minakawa, Masayuki; Imamura, Nobukazu; Tsuzuki, Mikio; Asayama, Munehiko

2018-04-17

Biomass yields and biofuel production were examined in a dual (solid and liquid)-phase cultivation system (DuPHA) with the unique filamentous cyanobacteria, Pseudanabaena sp. ABRG 5-3 and Limnothrix sp. SK1-2-1. Continuous circular cultivation was driven under the indoor closed (IC) or indoor opened (IO) conditions and provided biomass yields of approximately 8 to 27 g dry cell weight (DCW) floor m -2 d -1 . Alkanes of heptadecane (C 17 H 36 ) or pentadecane (C 15 H 32 ) as liquid biofuels were also recovered from the lower liquid-phase, in which cyanobacteria were dropped from the upper solid-phase and continuously cultivated with a small amount of medium. After the main cultivation in DuPHA, the upper solid-phase of a cotton cloth on which cyanobacteria grew was dried and directly subjected to a combustion test. This resulted in the thermal power (kJ s -1 ) of the cloth with microalgae increasing approximately 20 to 50% higher than that of the cloth only, suggesting a possibility of using the solid phase with microalgae as solid biofuel. Copyright © 2018. Published by Elsevier B.V.

Biological nitrate removal from water and wastewater by solid-phase denitrification process.

PubMed

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 Elsevier Inc. All rights reserved.

Solid-State NMR Investigation of Drug-Excipient Interactions and Phase Behavior in Indomethacin-Eudragit E Amorphous Solid Dispersions.

PubMed

Lubach, Joseph W; Hau, Jonathan

2018-02-20

To investigate the nature of drug-excipient interactions between indomethacin (IMC) and methacrylate copolymer Eudragit® E (EE) in the amorphous state, and evaluate the effects on formulation and stability of these amorphous systems. Amorphous solid dispersions containing IMC and EE were spray dried with drug loadings from 20% to 90%. PXRD was used to confirm the amorphous nature of the dispersions, and DSC was used to measure glass transition temperatures (T g ). 13 C and 15 N solid-state NMR was utilized to investigate changes in local structure and protonation state, while 1 H T 1 and T 1ρ relaxation measurements were used to probe miscibility and phase behavior of the dispersions. T g values for IMC-EE solid dispersions showed significant positive deviations from predicted values in the drug loading range of 40-90%, indicating a relatively strong drug-excipient interaction. 15 N solid-state NMR exhibited a change in protonation state of the EE basic amine, with two distinct populations for the EE amine at -360.7 ppm (unprotonated) and -344.4 ppm (protonated). Additionally, 1 H relaxation measurements showed phase separation at high drug load, indicating an amorphous ionic complex and free IMC-rich phase. PXRD data showed all ASDs up to 90% drug load remained physically stable after 2 years. 15 N solid-state NMR experiments show a change in protonation state of EE, indicating that an ionic complex indeed forms between IMC and EE in amorphous solid dispersions. Phase behavior was determined to exhibit nanoscale phase separation at high drug load between the amorphous ionic complex and excess free IMC.

Further insight into the mechanism of heavy metals partitioning in stormwater runoff.

PubMed

Djukić, Aleksandar; Lekić, Branislava; Rajaković-Ognjanović, Vladana; Veljović, Djordje; Vulić, Tatjana; Djolić, Maja; Naunovic, Zorana; Despotović, Jovan; Prodanović, Dušan

2016-03-01

Various particles and materials, including pollutants, deposited on urban surfaces are washed off by stormwater runoff during rain events. The interactions between the solid and dissolved compounds in stormwater runoff are phenomena of importance for the selection and improvement of optimal stormwater management practices aimed at minimizing pollutant input to receiving waters. The objective of this research was to further investigate the mechanisms responsible for the partitioning of heavy metals (HM) between the solid and liquid phases in urban stormwater runoff. The research involved the collection of samples from urban asphalt surfaces, chemical characterization of the bulk liquid samples, solids separation, particle size distribution fractionation and chemical and physico-chemical characterization of the solid phase particles. The results revealed that a negligible fraction of HM was present in the liquid phase (less than 3% by weight), while there was a strong correlation between the total content of heavy metals and total suspended solids. Examinations of surface morphology and mineralogy revealed that the solid phase particles consist predominantly of natural macroporous materials: alpha quartz (80%), magnetite (11.4%) and silicon diphosphate (8.9%). These materials have a low surface area and do not have significant adsorptive capacity. These materials have a low surface area and do not have significant adsorptive capacity. The presence of HM on the surface of solid particles was not confirmed by scanning electron microscopy and energy dispersive X-ray microanalyses. These findings, along with the results of the liquid phase sample characterization, indicate that the partitioning of HM between the liquid and solid phases in the analyzed samples may be attributed to precipitation processes. Copyright © 2015 Elsevier Ltd. All rights reserved.

Method for removing solid particulate material from within liquid fuel injector assemblies

DOEpatents

Simandl, R.F.; Brown, J.D.; Andriulli, J.B.; Strain, P.D.

1998-09-08

A method is described for removing residual solid particulate material from the interior of liquid fuel injectors and other fluid flow control mechanisms having or being operatively associated with a flow-regulating fixed or variable orifice. The method comprises the sequential and alternate introduction of columns of a non-compressible liquid phase and columns of a compressed gas phase into the body of a fuel injector whereby the expansion of each column of the gas phase across the orifice accelerates the liquid phase in each trailing column of the liquid phase and thereby generates turbulence in each liquid phase for lifting and entraining the solid particulates for the subsequent removal thereof from the body of the fuel injector. 1 fig.

Method for removing solid particulate material from within liquid fuel injector assemblies

DOEpatents

Simandl, Ronald F.; Brown, John D.; Andriulli, John B.; Strain, Paul D.

1998-01-01

A method for removing residual solid particulate material from the interior of liquid fuel injectors and other fluid flow control mechanisms having or being operatively associated with a flow-regulating fixed or variable orifice. The method comprises the sequential and alternate introduction of columns of a non-compressible liquid phase and columns of a compressed gas phase into the body of a fuel injector whereby the expansion of each column of the gas phase across the orifice accelerates the liquid phase in each trailing column of the liquid phase and thereby generates turbulence in each liquid phase for lifting and entraining the solid particulates for the subsequent removal thereof from the body of the fuel injector.

Study on ABO and RhD blood grouping: Comparison between conventional tile method and a new solid phase method (InTec Blood Grouping Test Kit).

PubMed

Yousuf, R; Abdul Ghani, S A; Abdul Khalid, N; Leong, C F

2018-04-01

'InTec Blood Grouping Test kit' using solid-phase technology is a new method which may be used at outdoor blood donation site or at bed side as an alternative to the conventional tile method in view of its stability at room temperature and fulfilled the criteria as point of care test. This study aimed to compare the efficiency of this solid phase method (InTec Blood Grouping Test Kit) with the conventional tile method in determining the ABO and RhD blood group of healthy donors. A total of 760 voluntary donors who attended the Blood Bank, Penang Hospital or offsite blood donation campaigns from April to May 2014 were recruited. The ABO and RhD blood groups were determined by the conventional tile method and the solid phase method, in which the tube method was used as the gold standard. For ABO blood grouping, the tile method has shown 100% concordance results with the gold standard tube method, whereas the solid-phase method only showed concordance result for 754/760 samples (99.2%). Therefore, for ABO grouping, tile method has 100% sensitivity and specificity while the solid phase method has slightly lower sensitivity of 97.7% but both with good specificity of 100%. For RhD grouping, both the tile and solid phase methods have grouped one RhD positive specimen as negative each, thus giving the sensitivity and specificity of 99.9% and 100% for both methods respectively. The 'InTec Blood Grouping Test Kit' is suitable for offsite usage because of its simplicity and user friendliness. However, further improvement in adding the internal quality control may increase the test sensitivity and validity of the test results.

Massachusetts Institute of Technology Consortium Agreement

DTIC Science & Technology

1999-03-01

In this, our second progress report of the Phase Two Home Automation and Healthcare Consortium at the Brit and Alex d’Arbeloff Laboratory for...Covered here are the diverse fields of home automation and healthcare research, ranging from human modeling, patient monitoring, and diagnosis to new...sensors and actuators, physical aids, human-machine interface and home automation infrastructure. These results will be presented at the upcoming General Assembly of the Consortium held on October 27-October 30, 1998 at MIT.

Total synthesis of TMG-chitotriomycin based on an automated electrochemical assembly of a disaccharide building block.

PubMed

Isoda, Yuta; Sasaki, Norihiko; Kitamura, Kei; Takahashi, Shuji; Manmode, Sujit; Takeda-Okuda, Naoko; Tamura, Jun-Ichi; Nokami, Toshiki; Itoh, Toshiyuki

2017-01-01

The total synthesis of TMG-chitotriomycin using an automated electrochemical synthesizer for the assembly of carbohydrate building blocks is demonstrated. We have successfully prepared a precursor of TMG-chitotriomycin, which is a structurally-pure tetrasaccharide with typical protecting groups, through the methodology of automated electrochemical solution-phase synthesis developed by us. The synthesis of structurally well-defined TMG-chitotriomycin has been accomplished in 10-steps from a disaccharide building block.

Armored Family of Vehicles (AFV) Automation and Communication. Resource Management Plan (ACRMP). Phase 1. Volume 15.

DTIC Science & Technology

1987-09-01

The AFV ACRMP is the Task Force Director’s (08) tool to manage command, control, communication (C3) automation system life cycle developments for the...responsibilities, development management, acquisition strategy, testing , life cycle support, technology assessment and work group relationships. ACRMP

Phase 2 of the Array Automated Assembly Task for the Low Cost Silicon Solar Array Project

NASA Technical Reports Server (NTRS)

Wihl, M.; Torro, J.; Scheinine, A.; Anderson, J.

1978-01-01

An automated process sequence, to manufacture photovoltaic modules at a capacity of approximately 500 MW per year at a cost of approximately $0.50 per peak watt is described. Verification tests were performed and are reported along with cost predictions.

Managing Archival Collections in an Automated Environment: The Joys of Barcoding

ERIC Educational Resources Information Center

Hamburger, Susan; Charles, Jane Veronica

2006-01-01

In a desire for automated collection control, archival repositories are adopting barcoding from their library and records center colleagues. This article discusses the planning, design, and implementation phases of barcoding. The authors focus on reasons for barcoding, security benefits, in-room circulation tracking, potential for gathering…

Molecularly imprinted solid-phase extraction sorbent for the clean-up of chlorinated phenoxyacids from aqueous samples.

PubMed

Baggiani, C; Giovannoli, C; Anfossi, L; Tozzi, C

2001-12-14

A molecularly imprinted polymer (MIP) was synthesized using the herbicide 2,4,5-trichlorophenoxyacetic acid as a template, 4-vinylpyridine as an interacting monomer, ethylendimethacrylate as a cross-linker and a methanol-water mixture as a porogen. The binding properties and the selectivity of the polymer towards the template were investigated by frontal and zonal liquid chromatography. The polymer was used as a solid-phase extraction material for the clean-up of the template molecule and some related herbicides (2,4-dichlorophenoxyacetic acid, fenoprop, dichlorprop) from river water samples at a concentration level of ng/ml with quantitative recoveries comparable with those obtained with a traditional C18 reversed-phase column when analyzed by capillary electrophoresis. The results obtained show that the MIP-based approach to the solid-phase extraction is comparable with the more traditional solid-phase extraction with C18 reversed-phase columns in terms of recovery, but it is superior in terms of sample clean-up.

A Comparison Between Orion Automated and Space Shuttle Rendezvous Techniques

NASA Technical Reports Server (NTRS)

Ruiz, Jose O,; Hart, Jeremy

2010-01-01

The Orion spacecraft will replace the space shuttle and will be the first human spacecraft since the Apollo program to leave low earth orbit. This vehicle will serve as the cornerstone of a complete space transportation system with a myriad of mission requirements necessitating rendezvous to multiple vehicles in earth orbit, around the moon and eventually beyond . These goals will require a complex and robust vehicle that is, significantly different from both the space shuttle and the command module of the Apollo program. Historically, orbit operations have been accomplished with heavy reliance on ground support and manual crew reconfiguration and monitoring. One major difference with Orion is that automation will be incorporated as a key element of the man-vehicle system. The automated system will consist of software devoted to transitioning between events based on a master timeline. This effectively adds a layer of high level sequencing that moves control of the vehicle from one phase to the next. This type of automated control is not entirely new to spacecraft since the shuttle uses a version of this during ascent and entry operations. During shuttle orbit operations however many of the software modes and hardware switches must be manually configured through the use of printed procedures and instructions voiced from the ground. The goal of the automation scheme on Orion is to extend high level automation to all flight phases. The move towards automation represents a large shift from current space shuttle operations, and so these new systems will be adopted gradually via various safeguards. These include features such as authority-to-proceed, manual down modes, and functional inhibits. This paper describes the contrast between the manual and ground approach of the space shuttle and the proposed automation of the Orion vehicle. I will introduce typical orbit operations that are common to all rendezvous missions and go on to describe the current Orion automation architecture and contrast it with shuttle rendezvous techniques and circumstances. The shuttle rendezvous profile is timed to take approximately 3 days from orbit insertion to docking at the International Space Station (ISS). This process can be divided into 3 phases: far-field, mid-field and proximity operations. The far-field stage is characterized as the most quiescent phase. The spacecraft is usually too far to navigate using relative sensors and uses the Inertial Measurement Units (IMU s) to numerically solve for its position. The maneuvers are infrequent, roughly twice per day, and are larger than other burns in the profile. The shuttle uses this opportunity to take extensive ground based radar updates and keep high fidelity orbit states on the ground. This state is then periodically uplinked to the shuttle computers. The targeting solutions for burn maneuvers are also computed on the ground and uplinked. During the burn the crew is responsible for setting the shuttle attitude and configuring the propulsion system for ignition. Again this entire process is manually driven by both crew and ground activity. The only automatic processes that occur are associated with the real-time execution of the burn. The Orion automated functionality will seek to relieve the workload of both the crew and ground during this phase

Encapsulated Solid-Liquid Phase Change Nanoparticles as Thermal Barcodes for Highly Sensitive Detections of Multiple Lung Cancer Biomarkers

DTIC Science & Technology

2012-10-01

5e. TASK NUMBER LC90061 5f. WORK UNIT NUMBER 7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES) 8. PERFORMING ORGANIZATION REPORT...transduction mechanism based on solid- liquid phase change nanoparticles works for the detection of multiple proteins. A series of metal and alloy...early stage. With the support from DOD-LCRP, we have proved the new signal transduction mechanism based on solid-liquid phase change nanoparticles works

A review on solid phase extraction of actinides and lanthanides with amide based extractants.

PubMed

Ansari, Seraj A; Mohapatra, Prasanta K

2017-05-26

Solid phase extraction is gaining attention from separation scientists due to its high chromatographic utility. Though both grafted and impregnated forms of solid phase extraction resins are popular, the later is easy to make by impregnating a given organic extractant on to an inert solid support. Solid phase extraction on an impregnated support, also known as extraction chromatography, combines the advantages of liquid-liquid extraction and the ion exchange chromatography methods. On the flip side, the impregnated extraction chromatographic resins are less stable against leaching out of the organic extractant from the pores of the support material. Grafted resins, on the other hand, have a higher stability, which allows their prolong use. The goal of this article is a brief literature review on reported actinide and lanthanide separation methods based on solid phase extractants of both the types, i.e., (i) ligand impregnation on the solid support or (ii) ligand functionalized polymers (chemically bonded resins). Though the literature survey reveals an enormous volume of studies on the extraction chromatographic separation of actinides and lanthanides using several extractants, the focus of the present article is limited to the work carried out with amide based ligands, viz. monoamides, diamides and diglycolamides. The emphasis will be on reported applied experimental results rather than on data pertaining fundamental metal complexation. Copyright © 2017 Elsevier B.V. All rights reserved.

Quantitative ionspray liquid chromatographic/tandem mass spectrometric determination of reserpine in equine plasma.

PubMed

Anderson, M A; Wachs, T; Henion, J D

1997-02-01

A method based on ionspray liquid chromatography/tandem mass spectrometry (LC/MS/MS) was developed for the determination of reserpine in equine plasma. A comparison was made of the isolation of reserpine from plasma by liquid-liquid extraction and by solid-phase extraction. A structural analog, rescinnamine, was used as the internal standard. The reconstituted extracts were analyzed by ionspray LC/MS/MS in the selected reaction monitoring (SRM) mode. The calibration graph for reserpine extracted from equine plasma obtained using liquid-liquid extraction was linear from 10 to 5000 pg ml-1 and that using solid-phase extraction from 100 to 5000 pg ml-1. The lower level of quantitation (LLQ) using liquid-liquid and solid-phase extraction was 50 and 200 pg ml-1, respectively. The lower level of detection for reserpine by LC/MS/MS was 10 pg ml-1. The intra-assay accuracy did not exceed 13% for liquid-liquid and 12% for solid-phase extraction. The recoveries for the LLQ were 68% for liquid-liquid and 58% for solid-phase extraction.

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

NASA Astrophysics Data System (ADS)

Abou Mrad, Ninette; Duvernay, Fabrice; Isnard, Robin; Chiavassa, Thierry; Danger, Grégoire

2017-09-01

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 (CH3OH), binary (H2O:CH3OH, CH3OH:NH3), and ternary ice analogs (H2O:CH3OH:NH3) 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.

Melting along the Hugoniot and solid phase transition for Sn via sound velocity measurements

NASA Astrophysics Data System (ADS)

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.

Melting of Simple Solids and the Elementary Excitations of the Communal Entropy

NASA Astrophysics Data System (ADS)

Bongiorno, Angelo

2010-03-01

The melting phase transition of simple solids is addressed through the use of atomistic computer simulations. Three transition metals (Ni, Au, and Pt) and a semiconductor (Si) are considered in this study. Iso-enthalpic molecular dynamics simulations are used to compute caloric curves across the solid-to-liquid phase transition of a periodic crystalline system, to construct the free energy function of the solid and liquid phases, and thus to derive the thermodynamical limit of the melting point, latent heat and entropy of fusion of the material. The computational strategy used in this study yields accurate estimates of melting parameters, it consents to determine the superheating and supercooling temperature limits, and it gives access to the atomistic mechanisms mediating the melting process. In particular, it is found that the melting phase transition in simple solids is driven by exchange steps involving a few atoms and preserving the crystalline structure. These self-diffusion phenomena correspond to the elementary excitations of the communal entropy and, as their rate depends on the local material cohesivity, they mediate both the homogeneous and non-homogeneous melting process in simple solids.

[Determination of lead in edible salt with solid-phase extraction and GFAAS].

PubMed

Zhao, Xin; Zhou, Shuang; Ma, Lan; Yang, Dajin

2013-01-01

Establishing a method for determination of lead in salt with solid-phase extraction and GFAAS. Salt sample was diluted to a certain volume directly with ammonium acetate, then the sample solution was filtered through the solid phase extraction column which has been pre-activated. Lead ions were retained, and the sodium chloride matrix was removed. After elution, the collected lead ions was determined by graphite furnace atomic absorption spectrometry in 257.4 nm. This method can be used effectively to wipe off the sodium chloride in matrix. The limit of detection was 0.7 microg/kg and the limit of quantification was 2 microg/kg. Solid phase extraction technique can be used effectively to reduce the interference in matrix and improves the accuracy and reproducibility of detection.

Self-healing liquid/solid state battery

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

Burke, Paul J.; Chung, Brice H.V.; Phadke, Satyajit R.

A battery system that exchanges energy with an external device is provided. The battery system includes a positive electrode having a first metal or alloy, a negative electrode having a second metal or alloy, and an electrolyte including a salt of the second metal or alloy. The positive electrode, the negative electrode, and the electrolyte are in a liquid phase at an operating temperature during at least one portion of operation. The positive electrode is entirely in a liquid phase in one charged state and includes a solid phase in another charged state. The solid phase of the positive electrodemore » includes a solid intermetallic formed by the first and the second metals or alloys. Methods of storing electrical energy from an external circuit using such a battery system are also provided.« less

Flow Mapping in a Gas-Solid Riser via Computer Automated Radioactive Particle Tracking (CARPT)

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

Muthanna Al-Dahhan; Milorad P. Dudukovic; Satish Bhusarapu

2005-06-04

Statement of the Problem: Developing and disseminating a general and experimentally validated model for turbulent multiphase fluid dynamics suitable for engineering design purposes in industrial scale applications of riser reactors and pneumatic conveying, require collecting reliable data on solids trajectories, velocities ? averaged and instantaneous, solids holdup distribution and solids fluxes in the riser as a function of operating conditions. Such data are currently not available on the same system. Multiphase Fluid Dynamics Research Consortium (MFDRC) was established to address these issues on a chosen example of circulating fluidized bed (CFB) reactor, which is widely used in petroleum and chemicalmore » industry including coal combustion. This project addresses the problem of lacking reliable data to advance CFB technology. Project Objectives: The objective of this project is to advance the understanding of the solids flow pattern and mixing in a well-developed flow region of a gas-solid riser, operated at different gas flow rates and solids loading using the state-of-the-art non-intrusive measurements. This work creates an insight and reliable database for local solids fluid-dynamic quantities in a pilot-plant scale CFB, which can then be used to validate/develop phenomenological models for the riser. This study also attempts to provide benchmark data for validation of Computational Fluid Dynamic (CFD) codes and their current closures. Technical Approach: Non-Invasive Computer Automated Radioactive Particle Tracking (CARPT) technique provides complete Eulerian solids flow field (time average velocity map and various turbulence parameters such as the Reynolds stresses, turbulent kinetic energy, and eddy diffusivities). It also gives directly the Lagrangian information of solids flow and yields the true solids residence time distribution (RTD). Another radiation based technique, Computed Tomography (CT) yields detailed time averaged local holdup profiles at various planes. Together, these two techniques can provide the needed local solids flow dynamic information for the same setup under identical operating conditions, and the data obtained can be used as a benchmark for development, and refinement of the appropriate riser models. For the above reasons these two techniques were implemented in this study on a fully developed section of the riser. To derive the global mixing information in the riser, accurate solids RTD is needed and was obtained by monitoring the entry and exit of a single radioactive tracer. Other global parameters such as Cycle Time Distribution (CTD), overall solids holdup in the riser, solids recycle percentage at the bottom section of the riser were evaluated from different solids travel time distributions. Besides, to measure accurately and in-situ the overall solids mass flux, a novel method was applied.« less

Studies in Three Phase Gas-Liquid Fluidised Systems

NASA Astrophysics Data System (ADS)

Awofisayo, Joyce Ololade

1992-01-01

Available from UMI in association with The British Library. The work is a logical continuation of research started at Aston some years ago when studies were conducted on fermentations in bubble columns. The present work highlights typical design and operating problems that could arise in such systems as waste water, chemical, biochemical and petroleum operations involving three-phase, gas-liquid -solid fluidisation; such systems are in increasing use. It is believed that this is one of few studies concerned with "true" three-phase, gas-liquid-solid fluidised systems, and that this work will contribute significantly to closing some of the gaps in knowledge in this area. The research work was experimentally based and involved studies of the hydrodynamic parameters, phase holdups (gas and solid), particle mixing and segregation, and phase flow dynamics (flow regime and circulation patterns). The studies have focused particularly on the solid behaviour and the influence of properties of solids present on the above parameters in three-phase, gas-liquid-solid fluidised systems containing single particle components and those containing binary and ternary mixtures of particles. All particles were near spherical in shape and two particle sizes and total concentration levels were used. Experiments were carried out in two- and three-dimensional bubble columns. Quantitative results are presented in graphical form and are supported by qualitative results from visual studies which are also shown as schematic diagrams and in photographic form. Gas and solid holdup results are compared for air-water containing single, binary and ternary component particle mixtures. It should be noted that the criteria for selection of the materials used are very important if true three-phase fluidisation is to be achieved: this is very evident when comparing the results with those in the literature. The fluid flow and circulation patterns observed were assessed for validation of the generally accepted patterns, and the author believes that the present work provides more accurate insight into the modelling of liquid circulation in bubble columns. The characteristic bubbly flow at low gas velocity in a two-phase system is suppressed in the three-phase system. The degree of mixing within the system is found to be dependent on flow regime, liquid circulation and the ratio of solid phase physical properties.