The first liquid biopsy test approved. Is it a new era of mutation testing for non-small cell lung cancer?

PubMed Central

2017-01-01

Specific mutations in epidermal growth factor receptor (EGFR) gene are predictive for response to the EGFR tyrosine kinase inhibitors (TKIs) in non-small cell lung cancer patients (NSCLC). According to international guidelines, the molecular testing in patients with advanced NSCLC of a non-squamous subtype is recommended. However, obtain a tissue sample could be challenging. Liquid biopsy allows to determine patients suitable for EGFR-targeted therapy by analysis of circulating-free tumor DNA (cfDNA) in peripheral blood samples and might replace tissue biopsy. It allows to acquire a material in convenient minimally invasive manner, is easily repeatable, could be used for molecular identification and molecular changes monitoring. Many studies show a high concordance rate between tissue and plasma samples testing. When U.S. Food and Drug Administration (FDA) approved the first liquid biopsy test, analysis of driver gene mutation from cfDNA becomes a reality in clinical practice for patients with NSCLC. PMID:28251125

A micro-rheological method for determination of blood type.

PubMed

Makulska, Sylwia; Jakiela, Slawomir; Garstecki, Piotr

2013-07-21

The measurement of time and distance can be used for determining agglutination in small (nL) samples of liquid. We demonstrate the use of this new scheme of detection in typing and subtyping blood in a simple microfluidic system that monitors the speed of flow of microdroplets. The system (i) accepts small samples of liquids deposited directly onto the chip, (ii) forms droplets on demand from these samples, (iii) merges the droplets, and (iv) measures their speed in a microchannel. A sequence of measurements on different combinations of blood and antibodies can thus be used to determine blood type with the estimated probability of mistyping being less than 1 in a million tests. In addition, in the agglutinated samples, red blood cells concentrate at the rear of the droplets yielding an additional vista for detection and suggesting a possible mechanism for separations.

Cavity ring-down spectroscopy in the liquid phase

NASA Astrophysics Data System (ADS)

Xu, Shucheng; Sha, Guohe; Xie, Jinchun

2002-02-01

A new application for cavity ring-down spectroscopic (CRDS) technique using a pulsed polarized light source has been developed in the absorption measurement of liquids for "colorless" organic compounds using both a single sample cell and double sample cells inserted in an optical cavity at Brewster angle. At present an experimental capability of measuring absorption coefficients as small as 2-5×10-7 cm-1 has been demonstrated by measurement of the absorption baselines. The first spectra for CRDS in the liquid phase, the C-H stretching fifth vibrational overtones of benzene in the pure liquid and hexane solution are obtained. The optical absorption length for liquids in both a single sample cell and double sample cells of 1 cm length is up to 900 cm due to multipass of light within an optical cavity. Compared to the thermal lens and optoacoustic spectroscopic techniques, the sensitivity for CRDS mainly depends on the optical absorption path of the sample (single passing path of the sample times multipass times), is not determined by the laser power and the length of the sample cell. The absolute absorption coefficient and band intensity for the sample are determined directly by the spectroscopy.

Chemical Characterization of an Envelope B/D Sample from Hanford Tank 241-AZ-102

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

Hay, M.S.

2000-08-23

A sample from Hanford waste tank 241-AZ-102 was received at the Savannah River Technology Center (SRTC) and chemically characterized. The sample containing supernate and a small amount of sludge solids was analyzed as-received. The filtered supernatant liquid, the total dried solids of the sample, and the washed insoluble solids obtained from filtration of the sample were analyzed. A mass balance calculation of the three fractions of the sample analyzed indicate the analytical results appear relatively self-consistent for major components of the sample. However, some inconsistency was observed between results were more than one method of determination was employed and formore » species present in low concentrations. The actinides isotopes, plutonium, americium, and curium, present analytical challenges due to the low concentration of these species and the potential for introduction of small amounts of contamination during sampling handling resulting in large uncertainties. A direct comparison to previous analyses of material from tank 241-AZ-102 showed good agreement with the filtered supernatant liquid. However, the comparison of solids data showed poor agreement. The poor agreement shown between the current results for the solids samples and previous analyses most likely results from the uncertainties associated with obtaining small solids samples from a large non-homogenized waste tank.« less

Highly efficient and ultra-small volume separation by pressure-driven liquid chromatography in extended nanochannels.

PubMed

Ishibashi, Ryo; Mawatari, Kazuma; Kitamori, Takehiko

2012-04-23

The rapidly developing interest in nanofluidic analysis, which is used to examine liquids ranging in amounts from the attoliter to the femtoliter scale, correlates with the recent interest in decreased sample amounts, such as in the field of single-cell analysis. For general nanofluidic analysis, the fact that a pressure-driven flow does not limit the choice of solvents (aqueous or organic) is important. This study shows the first pressure-driven liquid chromatography technique that enables separation of atto- to femtoliter sample volumes, with a high separation efficiency within a few seconds. The apparent diffusion coefficient measurement of the unretentive sample suggests that there is no increase in the viscosity of toluene in the extended nanospace, unlike in aqueous solvents. Evaluation of the normal phase separation, therefore, should involve only the examination of the effect of the small size of the extended nanospace. Compared to a conventionally packed high-performance liquid chromatography column, the separation here results in a faster separation (4 s) by 2 orders of magnitude, a smaller injection volume (10(0) fL) by 9 orders, and a higher separation efficiency (440,000 plates/m) by 1 order. Moreover, the separation behavior agrees with the theory showing that this high efficiency was due to the small and controlled size of the separation channel, where the diffusion through the channel depth direction is fast enough to be neglected. Our chip-based platform should allow direct and real-time analysis or screening of ultralow volume of sample. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Gas bubble detector

NASA Technical Reports Server (NTRS)

Mount, Bruce E. (Inventor); Burchfield, David E. (Inventor); Hagey, John M. (Inventor)

1995-01-01

A gas bubble detector having a modulated IR source focused through a bandpass filter onto a venturi, formed in a sample tube, to illuminate the venturi with modulated filtered IR to detect the presence of gas bubbles as small as 0.01 cm or about 0.004 in diameter in liquid flowing through the venturi. Means are provided to determine the size of any detected bubble and to provide an alarm in the absence of liquid in the sample tube.

Ultrasonic characterization of single drops of liquids

DOEpatents

Sinha, Dipen N.

1998-01-01

Ultrasonic characterization of single drops of liquids. The present invention includes the use of two closely spaced transducers, or one transducer and a closely spaced reflector plate, to form an interferometer suitable for ultrasonic characterization of droplet-size and smaller samples without the need for a container. The droplet is held between the interferometer elements, whose distance apart may be adjusted, by surface tension. The surfaces of the interferometer elements may be readily cleansed by a stream of solvent followed by purified air when it is desired to change samples. A single drop of liquid is sufficient for high-quality measurement. Examples of samples which may be investigated using the apparatus and method of the present invention include biological specimens (tear drops; blood and other body fluid samples; samples from tumors, tissues, and organs; secretions from tissues and organs; snake and bee venom, etc.) for diagnostic evaluation, samples in forensic investigations, and detection of drugs in small quantities.

Ultrasonic sensor and method of use

DOEpatents

Condreva, Kenneth J.

2001-01-01

An ultrasonic sensor system and method of use for measuring transit time though a liquid sample, using one ultrasonic transducer coupled to a precision time interval counter. The timing circuit captures changes in transit time, representing small changes in the velocity of sound transmitted, over necessarily small time intervals (nanoseconds) and uses the transit time changes to identify the presence of non-conforming constituents in the sample.

An assessment of the potential of laser-induced breakdown spectroscopy (LIBS) for the analysis of cesium in liquid samples of biological origin.

PubMed

Metzinger, Anikó; Kovács-Széles, Eva; Almási, István; Galbács, Gábor

2014-01-01

The present study describes the development of an analytical method for the determination of cesium in biological fluid samples (human urine and blood samples) by laser-induced breakdown spectroscopy (LIBS). The developed method is based on sample presentation by liquid-to-solid conversion, enhancing the emission signal by drying the liquid into small "pockets" created in a metal support (zinc plate), and allows the analysis to be carried out on as little as 1 μL of sample volume, in a closed sample cell. Absolute detection limits on the Cs I 852.1 nm spectral line were calculated by the IUPAC 3σ method to be 6 ng in the urine sample and 27 ng in the blood serum sample. It is estimated that LIBS may be used to detect highly elevated concentration levels of Cs in fluid samples taken from people potentially exposed to surges of Cs from non-natural sources.

[Determination of four phenolic endocrine disruptors in environmental water samples by high performance liquid chromatography-fluorescence detection using dispersive liquid-liquid microextraction coupled with derivatization].

PubMed

Wang, Xiaoyan; Qi, Weimei; Zhao, Xian'en; Lü, Tao; Wang, Xiya; Zheng, Longfang; Yan, Yehao; You, Jinmao

2014-06-01

To achieve accurate, fast and sensitive detection of phenolic endocrine disruptors in small volume of environmental water samples, a method of dispersive liquid-liquid microextraction (DLLME) coupled with fluorescent derivatization was developed for the determination of bisphenol A, nonylphenol, octylphenol and 4-tert-octylphenol in environmental water samples by high performance liquid chromatography-fluorescence detection (HPLC-FLD). The DLLME and derivatization conditions were investigated, and the optimized DLLME conditions for small volume of environmental water samples (pH 4.0) at room temperature were as follows: 70 microL chloroform as extraction solvent, 400 microL acetonitrile as dispersing solvent, vortex mixing for 3 min, and then high-speed centrifugation for 2 min. Using 2-[2-(7H-dibenzo [a, g] carbazol-7-yl)-ethoxy] ethyl chloroformate (DBCEC-Cl) as precolumn derivatization reagent, the stable derivatives of the four phenolic endocrine disruptors were obtained in pH 10.5 Na2CO3-NaHCO3 buffer/acetonitrile at 50 degrees C for 3 min, and then separated within 10 min by HPLC-FLD. The limits of detection (LODs) were in the range of 0.9-1.6 ng/L, and the limits of quantification (LOQs) were in the range of 3.8-7.1 ng/L. This method had perfect linearity, precision and recovery results, and showed obvious advantages and practicality comparing to the previously reported methods. It is a convenient and validated method for the routine analysis of phenolic endocrine disruptors in waste water of paper mill, lake water, domestic wastewater, tap water, etc.

Simultaneous extraction and clean-up of polychlorinated biphenyls and their metabolites from small tissue samples using pressurized liquid extraction

PubMed Central

Kania-Korwel, Izabela; Zhao, Hongxia; Norstrom, Karin; Li, Xueshu; Hornbuckle, Keri C.; Lehmler, Hans-Joachim

2008-01-01

A pressurized liquid extraction-based method for the simultaneous extraction and in situ clean-up of polychlorinated biphenyls (PCBs), hydroxylated (OH)-PCBs and methylsulfonyl (MeSO2)-PCBs from small (< 0.5 gram) tissue samples was developed and validated. Extraction of a laboratory reference material with hexane:dichloromethane:methanol (48:43:9, v/v) and Florisil as fat retainer allowed an efficient recovery of PCBs (78–112%; RSD: 13–37%), OH-PCBs (46±2%; RSD: 4%) and MeSO2-PCBs (89±21%; RSD: 24%). Comparable results were obtained with an established analysis method for PCBs, OH-PCBs and MeSO2-PCBs. PMID:19019378

Highly concentrated, ring-shaped phase conversion laser-induced breakdown spectroscopy technology for liquid sample analysis.

PubMed

Lin, Qingyu; Wei, Zhimei; Guo, Hongli; Wang, Shuai; Guo, Guangmeng; Zhang, Zhi; Duan, Yixiang

2017-06-10

A highly concentrated, ring-shaped phase conversion (RSPC) method was developed for liquid sample analysis using the laser-induced breakdown spectroscopy (LIBS) technique. In this work, test samples were prepared by mixing the metal particles with polyvinyl alcohol (PVA) supporter in liquid phase. With heat, the PVA solution solidified inside a modified glass petri dish, forming a metal-enriched polymer ring film. Distinguished from other traditional liquid-to-solid conversing methods, the proposed new method takes advantage of enhanced homogeneity for the target elements inside the ring film. The modified glass petri dish was used to control the ring-shaped concentration. Due to the specially designed circular groove at the bottom of this dish, where the PVA solution and liquid sample mixture accumulated, the target elements were concentrated in this small ring, which is beneficial for enhancing and stabilizing the plasma signals compared to the direct liquid sample analysis using LIBS. The limits of detection for Ag, Cu, Cr, and Ba obtained with the RSPC-LIBS technology were 0.098  μg·mL -1 , 0.18  μg·mL -1 , 0.83  μg·mL -1 , and 0.046  μg·mL -1 , respectively, which provided greater improvement than the direct bulk liquid analysis using LIBS.

Rapid analysis of aflatoxins B1, B2, and ochratoxin A in rice samples using dispersive liquid-liquid microextraction combined with HPLC.

PubMed

Lai, Xian-Wen; Sun, Dai-Li; Ruan, Chun-Qiang; Zhang, He; Liu, Cheng-Lan

2014-01-01

A novel, simple, and rapid method is presented for the analysis of aflatoxin B1, aflatoxin B2, and ochratoxin A in rice samples by dispersive liquid-liquid microextraction combined with LC and fluorescence detection. After extraction of the rice samples with a mixture of acetonitrile/water/acetic acid, mycotoxins were rapidly partitioned into a small volume of organic solvent (chloroform) by dispersive liquid-liquid microextraction. The three mycotoxins were simultaneously determined by LC with fluorescence detection after precolumn derivatization for aflatoxin B1 and B2. Parameters affecting both extraction and dispersive liquid-liquid microextraction procedures, including the extraction solvent, the type and volume of extractant, the volume of dispersive solvent, the addition of salt, the pH and the extraction time, were optimized. The optimized protocol provided an enrichment factor of approximately 1.25 and with detection of limits (0.06-0.5 μg/kg) below the maximum levels imposed by current regulations for aflatoxins and ochratoxin A. The mean recovery of three mycotoxins ranged from 82.9-112%, with a RSD less than 7.9% in all cases. The method was successfully applied to measure mycotoxins in commercial rice samples collected from local supermarkets in China. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Entropic Description of Gas Hydrate Ice-Liquid Equilibrium via Enhanced Sampling of Coexisting Phases

NASA Astrophysics Data System (ADS)

Małolepsza, Edyta; Kim, Jaegil; Keyes, Tom

2015-05-01

Metastable β ice holds small guest molecules in stable gas hydrates, so its solid-liquid equilibrium is of interest. However, aqueous crystal-liquid transitions are very difficult to simulate. A new molecular dynamics algorithm generates trajectories in a generalized N P T ensemble and equilibrates states of coexisting phases with a selectable enthalpy. With replicas spanning the range between β ice and liquid water, we find the statistical temperature from the enthalpy histograms and characterize the transition by the entropy, introducing a general computational procedure for first-order transitions.

Entropic description of gas hydrate ice/liquid equilibrium via enhanced sampling of coexisting phases

DOE PAGES

Malolepsza, Edyta; Kim, Jaegil; Keyes, Tom

2015-04-28

Metastable β ice holds small guest molecules in stable gas hydrates, so its solid/liquid equilibrium is of interest. However, aqueous crystal/liquid transitions are very difficult to simulate. A new MD algorithm generates trajectories in a generalized NPT ensemble and equilibrates states of coexisting phases with a selectable enthalpy. Furthermore, with replicas spanning the range between β ice and liquid water we find the statistical temperature from the enthalpy histograms and characterize the transition by the entropy, introducing a general computational procedure for first-order transitions.

Ultrasonic characterization of single drops of liquids

DOEpatents

Sinha, D.N.

1998-04-14

Ultrasonic characterization of single drops of liquids is disclosed. The present invention includes the use of two closely spaced transducers, or one transducer and a closely spaced reflector plate, to form an interferometer suitable for ultrasonic characterization of droplet-size and smaller samples without the need for a container. The droplet is held between the interferometer elements, whose distance apart may be adjusted, by surface tension. The surfaces of the interferometer elements may be readily cleansed by a stream of solvent followed by purified air when it is desired to change samples. A single drop of liquid is sufficient for high-quality measurement. Examples of samples which may be investigated using the apparatus and method of the present invention include biological specimens (tear drops; blood and other body fluid samples; samples from tumors, tissues, and organs; secretions from tissues and organs; snake and bee venom, etc.) for diagnostic evaluation, samples in forensic investigations, and detection of drugs in small quantities. 5 figs.

Ultrasonic characterization of single drops of liquids

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

Sinha, D.N.

Ultrasonic characterization of single drops of liquids is disclosed. The present invention includes the use of two closely spaced transducers, or one transducer and a closely spaced reflector plate, to form an interferometer suitable for ultrasonic characterization of droplet-size and smaller samples without the need for a container. The droplet is held between the interferometer elements, whose distance apart may be adjusted, by surface tension. The surfaces of the interferometer elements may be readily cleansed by a stream of solvent followed by purified air when it is desired to change samples. A single drop of liquid is sufficient for high-qualitymore » measurement. Examples of samples which may be investigated using the apparatus and method of the present invention include biological specimens (tear drops; blood and other body fluid samples; samples from tumors, tissues, and organs; secretions from tissues and organs; snake and bee venom, etc.) for diagnostic evaluation, samples in forensic investigations, and detection of drugs in small quantities. 5 figs.« less

Method for digital measurement of phase-frequency characteristics for a fixed-length ultrasonic spectrometer

NASA Astrophysics Data System (ADS)

Astashev, M. E.; Belosludtsev, K. N.; Kharakoz, D. P.

2014-05-01

One of the most accurate methods for measuring the compressibility of liquids is resonance measurement of sound velocity in a fixed-length interferometer. This method combines high sensitivity, accuracy, and small sample volume of the test liquid. The measuring principle is to study the resonance properties of a composite resonator that contains a test liquid sample. Ealier, the phase-locked loop (PLL) scheme was used for this. In this paper, we propose an alternative measurement scheme based on digital analysis of harmonic signals, describe the implementation of this scheme using commercially available data acquisition modules, and give examples of test measurements with accuracy evaluations of the results.

Next generation sequencing techniques in liquid biopsy: focus on non-small cell lung cancer patients.

PubMed

Malapelle, Umberto; Pisapia, Pasquale; Rocco, Danilo; Smeraglio, Riccardo; di Spirito, Maria; Bellevicine, Claudio; Troncone, Giancarlo

2016-10-01

The advent of genomic based personalized medicine has led to multiple advances in the molecular characterization of many tumor types, such as non-small cell lung cancer (NSCLC). NSCLC is diagnosed in most cases on small tissue samples that may be not always sufficient for EGFR mutational assessment to select patients for first and second generations' tyrosine kinase inhibitors (TKIs) therapy. In patients without tissue availability at presentation, the analysis of cell free DNA (cfDNA) derived from liquid biopsy samples, in particular from plasma, represent an established alternative to provide EGFR mutational testing for treatment decision making. In addition, a new paradigm for TKIs resistance management was recently approved by Food and Drug Administration, supporting the liquid biopsy based genotyping prior to tissue based genotyping for the detection of T790M mutation to select patients for third generation TKIs. In these settings, real time PCR (RT-PCR) and digital PCR 'targeted' methods, which detect known mutations by specific probes, have extensively been adopted. Taking into account the restricted reference range and the limited multiplexing power of these targeted methods, the performance of liquid biopsy analyses may be further improved by next generation sequencing (NGS). While most tissue based NGS genotyping is well established, liquid biopsy NGS application is challenging, requiring a careful validation of the whole process, from blood collection to variant calling. Here we review this evolving field, highlighting those methodological points that are crucial to accurately select NSCLC patients for TKIs treatment administration by NGS on cfDNA.

Combination of saponification and dispersive liquid-liquid microextraction for the determination of tocopherols and tocotrienols in cereals by reversed-phase high-performance liquid chromatography.

PubMed

Shammugasamy, Balakrishnan; Ramakrishnan, Yogeshini; Ghazali, Hasanah M; Muhammad, Kharidah

2013-07-26

A simple sample preparation technique coupled with reversed-phase high-performance liquid chromatography was developed for the determination of tocopherols and tocotrienols in cereals. The sample preparation procedure involved a small-scale hydrolysis of 0.5g cereal sample by saponification, followed by the extraction and concentration of tocopherols and tocotrienols from saponified extract using dispersive liquid-liquid microextraction (DLLME). Parameters affecting the DLLME performance were optimized to achieve the highest extraction efficiency and the performance of the developed DLLME method was evaluated. Good linearity was observed over the range assayed (0.031-4.0μg/mL) with regression coefficients greater than 0.9989 for all tocopherols and tocotrienols. Limits of detection and enrichment factors ranged from 0.01 to 0.11μg/mL and 50 to 73, respectively. Intra- and inter-day precision were lower than 8.9% and the recoveries were around 85.5-116.6% for all tocopherols and tocotrienols. The developed DLLME method was successfully applied to cereals: rice, barley, oat, wheat, corn and millet. This new sample preparation approach represents an inexpensive, rapid, simple and precise sample cleanup and concentration method for the determination of tocopherols and tocotrienols in cereals. Copyright © 2013 Elsevier B.V. All rights reserved.

Accurate high-speed liquid handling of very small biological samples.

PubMed

Schober, A; Günther, R; Schwienhorst, A; Döring, M; Lindemann, B F

1993-08-01

Molecular biology techniques require the accurate pipetting of buffers and solutions with volumes in the microliter range. Traditionally, hand-held pipetting devices are used to fulfill these requirements, but many laboratories have also introduced robotic workstations for the handling of liquids. Piston-operated pumps are commonly used in manually as well as automatically operated pipettors. These devices cannot meet the demands for extremely accurate pipetting of very small volumes at the high speed that would be necessary for certain applications (e.g., in sequencing projects with high throughput). In this paper we describe a technique for the accurate microdispensation of biochemically relevant solutions and suspensions with the aid of a piezoelectric transducer. It is suitable for liquids of a viscosity between 0.5 and 500 milliPascals. The obtainable drop sizes range from 5 picoliters to a few nanoliters with up to 10,000 drops per second. Liquids can be dispensed in single or accumulated drops to handle a wide volume range. The system proved to be excellently suitable for the handling of biological samples. It did not show any detectable negative impact on the biological function of dissolved or suspended molecules or particles.

Determination of polycyclic aromatic hydrocarbons in drinking water samples by solid-phase nanoextraction and high-performance liquid chromatography.

PubMed

Wang, Huiyong; Campiglia, Andres D

2008-11-01

A novel alternative is presented for the extraction and preconcentration of polycyclic aromatic hydrocarbons (PAH) from water samples. The new approachwhich we have named solid-phase nanoextraction (SPNE)takes advantage of the strong affinity that exists between PAH and gold nanoparticles. Carefully optimization of experimental parameters has led to a high-performance liquid chromatography method with excellent analytical figures of merit. Its most striking feature correlates to the small volume of water sample (500 microL) for complete PAH analyses. The limits of detection ranged from 0.9 (anthracene) to 58 ng.L (-1) (fluorene). The relative standard deviations at medium calibration concentrations vary from 3.2 (acenaphthene) to 9.1% (naphthalene). The analytical recoveries from tap water samples of the six regulated PAH varied from 83.3 +/- 2.4 (benzo[ k]fluoranthene) to 95.7 +/- 4.1% (benzo[ g,h,i]perylene). The entire extraction procedure consumes less than 100 microL of organic solvents per sample, which makes it environmentally friendly. The small volume of extracting solution makes SPNE a relatively inexpensive extraction approach.

Chrysotile in water

PubMed Central

Speil, Sidney

1974-01-01

The problems of quantitating chrysotile in water by fiber count techniques are reviewed briefly and the use of mass quantitation is suggested as a preferable measure. Chrysotile fiber has been found in almost every sample of natural water examined, but generally transmission electron miscroscopy (TEM) is required because of the small diameters involved. The extreme extrapolation required in mathematically converting a few fibers or fiber fragments under the TEM to the fiber content of a liquid sample casts considerable doubt on the validity of numbers used to compare chrysotile contents of different liquids. PMID:4470930

Gas pressure assisted microliquid-liquid extraction coupled online to direct infusion mass spectrometry: a new automated screening platform for bioanalysis.

PubMed

Raterink, Robert-Jan; Witkam, Yoeri; Vreeken, Rob J; Ramautar, Rawi; Hankemeier, Thomas

2014-10-21

In the field of bioanalysis, there is an increasing demand for miniaturized, automated, robust sample pretreatment procedures that can be easily connected to direct-infusion mass spectrometry (DI-MS) in order to allow the high-throughput screening of drugs and/or their metabolites in complex body fluids like plasma. Liquid-Liquid extraction (LLE) is a common sample pretreatment technique often used for complex aqueous samples in bioanalysis. Despite significant developments that have been made in automated and miniaturized LLE procedures, fully automated LLE techniques allowing high-throughput bioanalytical studies on small-volume samples using direct infusion mass spectrometry, have not been matured yet. Here, we introduce a new fully automated micro-LLE technique based on gas-pressure assisted mixing followed by passive phase separation, coupled online to nanoelectrospray-DI-MS. Our method was characterized by varying the gas flow and its duration through the solvent mixture. For evaluation of the analytical performance, four drugs were spiked to human plasma, resulting in highly acceptable precision (RSD down to 9%) and linearity (R(2) ranging from 0.990 to 0.998). We demonstrate that our new method does not only allow the reliable extraction of analytes from small sample volumes of a few microliters in an automated and high-throughput manner, but also performs comparable or better than conventional offline LLE, in which the handling of small volumes remains challenging. Finally, we demonstrate the applicability of our method for drug screening on dried blood spots showing excellent linearity (R(2) of 0.998) and precision (RSD of 9%). In conclusion, we present the proof of principe of a new high-throughput screening platform for bioanalysis based on a new automated microLLE method, coupled online to a commercially available nano-ESI-DI-MS.

High-field dynamic nuclear polarization in aqueous solutions.

PubMed

Prandolini, M J; Denysenkov, V P; Gafurov, M; Endeward, B; Prisner, T F

2009-05-06

Unexpected high DNP enhancements of more than 10 have been achieved in liquid water samples at room temperature and magnetic fields of 9.2 T (corresponding to 400 MHz (1)H NMR frequency and 260 GHz EPR frequency). The liquid samples were polarized in situ using a double-resonance structure, which allows simultaneous excitation of NMR and EPR transitions and achieves significant DNP enhancements at very low incident microwave power of only 45 mW. These results demonstrate the first important step toward the application of DNP to high-resolution NMR, increasing the sensitivity on biomolecules with small sample volumes and at physiologically low concentrations.

Liquid chromatography-mass spectrometry in metabolomics research: mass analyzers in ultra high pressure liquid chromatography coupling.

PubMed

Forcisi, Sara; Moritz, Franco; Kanawati, Basem; Tziotis, Dimitrios; Lehmann, Rainer; Schmitt-Kopplin, Philippe

2013-05-31

The present review gives an introduction into the concept of metabolomics and provides an overview of the analytical tools applied in non-targeted metabolomics with a focus on liquid chromatography (LC). LC is a powerful analytical tool in the study of complex sample matrices. A further development and configuration employing Ultra-High Pressure Liquid Chromatography (UHPLC) is optimized to provide the largest known liquid chromatographic resolution and peak capacity. Reasonably UHPLC plays an important role in separation and consequent metabolite identification of complex molecular mixtures such as bio-fluids. The most sensitive detectors for these purposes are mass spectrometers. Almost any mass analyzer can be optimized to identify and quantify small pre-defined sets of targets; however, the number of analytes in metabolomics is far greater. Optimized protocols for quantification of large sets of targets may be rendered inapplicable. Results on small target set analyses on different sample matrices are easily comparable with each other. In non-targeted metabolomics there is almost no analytical method which is applicable to all different matrices due to limitations pertaining to mass analyzers and chromatographic tools. The specifications of the most important interfaces and mass analyzers are discussed. We additionally provide an exemplary application in order to demonstrate the level of complexity which remains intractable up to date. The potential of coupling a high field Fourier Transform Ion Cyclotron Resonance Mass Spectrometer (ICR-FT/MS), the mass analyzer with the largest known mass resolving power, to UHPLC is given with an example of one human pre-treated plasma sample. This experimental example illustrates one way of overcoming the necessity of faster scanning rates in the coupling with UHPLC. The experiment enabled the extraction of thousands of features (analytical signals). A small subset of this compositional space could be mapped into a mass difference network whose topology shows specificity toward putative metabolite classes and retention time. Copyright © 2013 Elsevier B.V. All rights reserved.

Sub-nanometer Resolution Imaging with Amplitude-modulation Atomic Force Microscopy in Liquid

PubMed Central

Farokh Payam, Amir; Piantanida, Luca; Cafolla, Clodomiro; Voïtchovsky, Kislon

2016-01-01

Atomic force microscopy (AFM) has become a well-established technique for nanoscale imaging of samples in air and in liquid. Recent studies have shown that when operated in amplitude-modulation (tapping) mode, atomic or molecular-level resolution images can be achieved over a wide range of soft and hard samples in liquid. In these situations, small oscillation amplitudes (SAM-AFM) enhance the resolution by exploiting the solvated liquid at the surface of the sample. Although the technique has been successfully applied across fields as diverse as materials science, biology and biophysics and surface chemistry, obtaining high-resolution images in liquid can still remain challenging for novice users. This is partly due to the large number of variables to control and optimize such as the choice of cantilever, the sample preparation, and the correct manipulation of the imaging parameters. Here, we present a protocol for achieving high-resolution images of hard and soft samples in fluid using SAM-AFM on a commercial instrument. Our goal is to provide a step-by-step practical guide to achieving high-resolution images, including the cleaning and preparation of the apparatus and the sample, the choice of cantilever and optimization of the imaging parameters. For each step, we explain the scientific rationale behind our choices to facilitate the adaptation of the methodology to every user's specific system. PMID:28060262

A Compact Microwave Microfluidic Sensor Using a Re-Entrant Cavity.

PubMed

Hamzah, Hayder; Abduljabar, Ali; Lees, Jonathan; Porch, Adrian

2018-03-19

A miniaturized 2.4 GHz re-entrant cavity has been designed, manufactured and tested as a sensor for microfluidic compositional analysis. It has been fully evaluated experimentally with water and common solvents, namely methanol, ethanol, and chloroform, with excellent agreement with the expected behaviour predicted by the Debye model. The sensor's performance has also been assessed for analysis of segmented flow using water and oil. The samples' interaction with the electric field in the gap region has been maximized by aligning the sample tube parallel to the electric field in this region, and the small width of the gap (typically 1 mm) result in a highly localised complex permittivity measurement. The re-entrant cavity has simple mechanical geometry, small size, high quality factor, and due to the high concentration of electric field in the gap region, a very small mode volume. These factors combine to result in a highly sensitive, compact sensor for both pure liquids and liquid mixtures in capillary or microfluidic environments.

Absorbance and fluorometric sensing with capillary wells microplates.

PubMed

Tan, Han Yen; Cheong, Brandon Huey-Ping; Neild, Adrian; Liew, Oi Wah; Ng, Tuck Wah

2010-12-01

Detection and readout from small volume assays in microplates are a challenge. The capillary wells microplate approach [Ng et al., Appl. Phys. Lett. 93, 174105 (2008)] offers strong advantages in small liquid volume management. An adapted design is described and shown here to be able to detect, in a nonimaging manner, fluorescence and absorbance assays minus the error often associated with meniscus forming at the air-liquid interface. The presence of bubbles in liquid samples residing in microplate wells can cause inaccuracies. Pipetting errors, if not adequately managed, can result in misleading data and wrong interpretations of assay results; particularly in the context of high throughput screening. We show that the adapted design is also able to detect for bubbles and pipetting errors during actual assay runs to ensure accuracy in screening.

Effective screening length of isotropic liquid samples submitted to an applied voltage.

PubMed

Zola, R S; Evangelista, L R; Barbero, G

2006-05-25

A cell of isotropic liquid in the shape of a slab of thickness d and containing ionic impurities is considered. It is shown that the screening effect produced by the ionic charges on the external field is characterized by an effective surface length, lambda(S)(U), depending on the applied voltage U. The analysis indicates that lambda(S)(U)) < lambda(D) when the applied voltage is very large, and lambda(S)(U) --> lambda(D) for very small values of the applied voltage, where lambda(D) is the Debye screening length. The presence of the ions is responsible also for a counterpotential, v, that for small U is such to cancel the effective electric field in the sample, whereas in the opposite limit it is inversely proportional to the applied difference of potential.

Propulsion engineering study for small-scale Mars missions

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

Whitehead, J.

1995-09-12

Rocket propulsion options for small-scale Mars missions are presented and compared, particularly for the terminal landing maneuver and for sample return. Mars landing has a low propulsive {Delta}v requirement on a {approximately}1-minute time scale, but at a high acceleration. High thrust/weight liquid rocket technologies, or advanced pulse-capable solids, developed during the past decade for missile defense, are therefore more appropriate for small Mars landers than are conventional space propulsion technologies. The advanced liquid systems are characterize by compact lightweight thrusters having high chamber pressures and short lifetimes. Blowdown or regulated pressure-fed operation can satisfy the Mars landing requirement, but hardwaremore » mass can be reduced by using pumps. Aggressive terminal landing propulsion designs can enable post-landing hop maneuvers for some surface mobility. The Mars sample return mission requires a small high performance launcher having either solid motors or miniature pump-fed engines. Terminal propulsion for 100 kg Mars landers is within the realm of flight-proven thruster designs, but custom tankage is desirable. Landers on a 10 kg scale also are feasible, using technology that has been demonstrated but not previously flown in space. The number of sources and the selection of components are extremely limited on this smallest scale, so some customized hardware is required. A key characteristic of kilogram-scale propulsion is that gas jets are much lighter than liquid thrusters for reaction control. The mass and volume of tanks for inert gas can be eliminated by systems which generate gas as needed from a liquid or a solid, but these have virtually no space flight history. Mars return propulsion is a major engineering challenge; earth launch is the only previously-solved propulsion problem requiring similar or greater performance.« less

High-throughput liquid-absorption air-sampling apparatus and methods

DOEpatents

Zaromb, Solomon

2000-01-01

A portable high-throughput liquid-absorption air sampler [PHTLAAS] has an asymmetric air inlet through which air is drawn upward by a small and light-weight centrifugal fan driven by a direct current motor that can be powered by a battery. The air inlet is so configured as to impart both rotational and downward components of motion to the sampled air near said inlet. The PHTLAAS comprises a glass tube of relatively small size through which air passes at a high rate in a swirling, highly turbulent motion, which facilitates rapid transfer of vapors and particulates to a liquid film covering the inner walls of the tube. The pressure drop through the glass tube is <10 cm of water, usually <5 cm of water. The sampler's collection efficiency is usually >20% for vapors or airborne particulates in the 2-3.mu. range and >50% for particles larger than 4.mu.. In conjunction with various analyzers, the PHTLAAS can serve to monitor a variety of hazardous or illicit airborne substances, such as lead-containing particulates, tritiated water vapor, biological aerosols, or traces of concealed drugs or explosives.

Method to determine 226Ra in small sediment samples by ultralow background liquid scintillation.

PubMed

Sanchez-Cabeza, Joan-Albert; Kwong, Laval Liong Wee; Betti, Maria

2010-08-15

(210)Pb dating of sediment cores is a widely used tool to reconstruct ecosystem evolution and historical pollution during the last century. Although (226)Ra can be determined by gamma spectrometry, this method shows severe limitations which are, among others, sample size requirements and counting times. In this work, we propose a new strategy based on the analysis of (210)Pb through (210)Po in equilibrium by alpha spectrometry, followed by the determination of (226)Ra (base or supported (210)Pb) without any further chemical purification by liquid scintillation and with a higher sample throughput. Although gamma spectrometry might still be required to determine (137)Cs as an independent tracer, the effort can then be focused only on those sections dated around 1963, when maximum activities are expected. In this work, we optimized the counting conditions, calibrated the system for changing quenching, and described the new method to determine (226)Ra in small sediment samples, after (210)Po determination, allowing a more precise determination of excess (210)Pb ((210)Pb(ex)). The method was validated with reference materials IAEA-384, IAEA-385, and IAEA-313.

Field-controlled structures in ferromagnetic cholesteric liquid crystals.

PubMed

Medle Rupnik, Peter; Lisjak, Darja; Čopič, Martin; Čopar, Simon; Mertelj, Alenka

2017-10-01

One of the advantages of anisotropic soft materials is that their structures and, consequently, their properties can be controlled by moderate external fields. Whereas the control of materials with uniform orientational order is straightforward, manipulation of systems with complex orientational order is challenging. We show that a variety of structures of an interesting liquid material, which combine chiral orientational order with ferromagnetic one, can be controlled by a combination of small magnetic and electric fields. In the suspensions of magnetic nanoplatelets in chiral nematic liquid crystals, the platelet's magnetic moments orient along the orientation of the liquid crystal and, consequently, the material exhibits linear response to small magnetic fields. In the absence of external fields, orientations of the liquid crystal and magnetization have wound structure, which can be either homogeneously helical, disordered, or ordered in complex patterns, depending on the boundary condition at the surfaces and the history of the sample. We demonstrate that by using different combinations of small magnetic and electric fields, it is possible to control reversibly the formation of the structures in a layer of the material. In such a way, different periodic structures can be explored and some of them may be suitable for photonic applications. The material is also a convenient model system to study chiral magnetic structures, because it is a unique liquid analog of a solid helimagnet.

Pesticide extraction from table grapes and plums using ionic liquid based dispersive liquid-liquid microextraction.

PubMed

Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Herrera-Herrera, Antonio V; Rodríguez-Delgado, Miguel Angel

2009-12-01

Room temperature ionic liquids (RTILs) have been used as extraction solvents in dispersive liquid-liquid microextraction (DLLME) for the determination of eight multi-class pesticides (i.e. thiophanate-methyl, carbofuran, carbaryl, tebuconazole, iprodione, oxyfluorfen, hexythiazox, and fenazaquin) in table grapes and plums. The developed method involves the combination of DLLME and high-performance liquid chromatography with diode array detection. Samples were first homogenized and extracted with acetonitrile. After evaporation and reconstitution of the extract in water containing sodium chloride, a quick DLLME procedure that used the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]) and methanol was developed. The RTIL dissolved in a very small volume of acetonitrile was directed injected in the chromatographic system. The comparison between the calibration curves obtained from standards and from spiked sample extracts (matrix-matched calibration) showed the existence of a strong matrix effect for most of the analyzed pesticides. A recovery study was also developed with five consecutive extractions of the two types of fruits spiked at three concentration levels. Mean recovery values were in the range of 72-100% for table grapes and 66-105% for plum samples (except for thiophanate-methyl and carbofuran, which were 64-75% and 58-66%, respectively). Limits of detection (LODs) were in the range 0.651-5.44 microg/kg for table grapes and 0.902-6.33 microg/kg for plums, representing LODs below the maximum residue limits (MRLs) established by the European Union in these fruits. The potential of the method was demonstrated by analyzing 12 commercial fruit samples (six of each type).

Controllable picoliter pipetting using hydrophobic microfluidic valves

NASA Astrophysics Data System (ADS)

Zhang, M.; Huang, J.; Qian, X.; Mi, S.; Wang, X.

2017-06-01

A picoliter pipetting technique using the microfluidic method is presented. Utilizing the hydrophobic self-assembled monolayer films patterned in microchannels as pressure-controlled valves, a small volume of liquid can be separated by a designed channel trap and then ejected from the channel end at a higher pressure. The liquid trap section is composed of a T-shaped channel junction and a hydrophobic patch. The liquid volume can be precisely controlled by varying the distance of the hydrophobic patch from the T-junction. By this means, liquid less than 100 pl can be separated and pipetted. The developed device is potentially useful for sample dispensing in biological, medical, and chemical applications.

Agreement between experimental and theoretical effects of nitrogen gas flowrate on liquid jet atomization

NASA Technical Reports Server (NTRS)

Ingebo, Robert D.

1987-01-01

Two-phase flows were investigated by using high velocity nitrogen gas streams to atomize small-diameter liquid jets. Tests were conducted primarily in the acceleration-wave regime for liquid jet atomization, where it was found that the loss of droplets due to vaporization had a marked effect on drop size measurements. In addition, four identically designed two-fluid atomizers were fabricated and tested for similarity of spray profiles. A scattered-light scanner was used to measure a characteristic drop diameter, which was correlated with nitrogen gas flowrate. The exponent of 1.33 for nitrogen gas flowrate is identical to that predicted by atomization theory for liquid jet breakup in the acceleration-wave regime. This is higher than the value of 1.2 which was previously obtained at a sampling distance of 4.4 cm downstream of the atomizer. The difference is attributed to the fact that drop-size measurements obtained at a 2.2 cm sampling distance are less effected by vaporization and dispersion of small droplets and therefore should give better agreement with atomization theory. Profiles of characteristic drop diameters were also obtained by making at least five line-of-sight measurements across the spray at several horizontal positions above and below the center line of the spray.

Absorbance and fluorometric sensing with capillary wells microplates

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

Tan, Han Yen; Cheong, Brandon Huey-Ping; Neild, Adrian

2010-12-15

Detection and readout from small volume assays in microplates are a challenge. The capillary wells microplate approach [Ng et al., Appl. Phys. Lett. 93, 174105 (2008)] offers strong advantages in small liquid volume management. An adapted design is described and shown here to be able to detect, in a nonimaging manner, fluorescence and absorbance assays minus the error often associated with meniscus forming at the air-liquid interface. The presence of bubbles in liquid samples residing in microplate wells can cause inaccuracies. Pipetting errors, if not adequately managed, can result in misleading data and wrong interpretations of assay results; particularly inmore » the context of high throughput screening. We show that the adapted design is also able to detect for bubbles and pipetting errors during actual assay runs to ensure accuracy in screening.« less

Refractive index dependence of Papilio Ulysses butterfly wings reflectance spectra

NASA Astrophysics Data System (ADS)

Isnaeni, Muslimin, Ahmad Novi; Birowosuto, Muhammad Danang

2016-02-01

We have observed and utilized butterfly wings of Papilio Ulysses for refractive index sensor. We noticed this butterfly wings have photonic crystal structure, which causes blue color appearance on the wings. The photonic crystal structure, which consists of cuticle and air void, is approximated as one dimensional photonic crystal structure. This photonic crystal structure opens potential to several optical devices application, such as refractive index sensor. We have utilized small piece of Papilio Ulysses butterfly wings to characterize refractive index of several liquid base on reflectance spectrum of butterfly wings in the presence of sample liquid. For comparison, we simulated reflectance spectrum of one dimensional photonic crystal structure having material parameter based on real structure of butterfly wings. We found that reflectance spectrum peaks shifted as refractive index of sample changes. Although there is a slight difference in reflectance spectrum peaks between measured spectrum and calculated spectrum, the trend of reflectance spectrum peaks as function of sample's refractive index is the similar. We assume that during the measurement, the air void that filled by sample liquid is expanded due to liquid pressure. This change of void shape causes non-similarity between measured spectrum and calculated spectrum.

Plastic waste to liquid oil through catalytic pyrolysis using natural and synthetic zeolite catalysts.

PubMed

Miandad, R; Barakat, M A; Rehan, M; Aburiazaiza, A S; Ismail, I M I; Nizami, A S

2017-11-01

This study aims to examine the catalytic pyrolysis of various plastic wastes in the presence of natural and synthetic zeolite catalysts. A small pilot scale reactor was commissioned to carry out the catalytic pyrolysis of polystyrene (PS), polypropylene (PP), polyethylene (PE) and their mixtures in different ratios at 450°C and 75min. PS plastic waste resulted in the highest liquid oil yield of 54% using natural zeolite and 50% using synthetic zeolite catalysts. Mixing of PS with other plastic wastes lowered the liquid oil yield whereas all mixtures of PP and PE resulted in higher liquid oil yield than the individual plastic feedstocks using both catalysts. The GC-MS analysis revealed that the pyrolysis liquid oils from all samples mainly consisted of aromatic hydrocarbons with a few aliphatic hydrocarbon compounds. The types and amounts of different compounds present in liquid oils vary with some common compounds such as styrene, ethylbenzene, benzene, azulene, naphthalene, and toluene. The FT-IR data also confirmed that liquid oil contained mostly aromatic compounds with some alkanes, alkenes and small amounts of phenol group. The produced liquid oils have high heating values (HHV) of 40.2-45MJ/kg, which are similar to conventional diesel. The liquid oil has potential to be used as an alternative source of energy or fuel production. Copyright © 2017 Elsevier Ltd. All rights reserved.

Electrostatic levitation facility optimized for neutron diffraction studies of high temperature liquids at a spallation neutron source

DOE PAGES

Mauro, N. A.; Vogt, A. J.; Derendorf, K. S.; ...

2016-01-01

Neutron diffraction studies of metallic liquids provide valuable information about inherent topological and chemical ordering on multiple length scales as well as insight into dynamical processes at the level of a few atoms. But, there exist very few facilities in the world that allow such studies to be made of reactive metallic liquids in a containerless environment, and these are designed for use at reactor-based neutron sources. We present an electrostatic levitation facility, NESL (for Neutron ElectroStatic Levitator), which takes advantage of the enhanced capabilities and increased neutron flux available at spallation neutron sources (SNSs). NESL enables high quality elasticmore » and inelastic neutron scattering experiments to be made of reactive metallic and other liquids in the equilibrium and supercooled temperature regime. The apparatus is comprised of a high vacuum chamber, external and internal neutron collimation optics, and a sample exchange mechanism that allows up to 30 samples to be processed between chamber openings. Two heating lasers allow excellent sample temperature homogeneity, even for samples approaching 500 mg, and an automated temperature control system allows isothermal measurements to be conducted for times approaching 2 h in the liquid state, with variations in the average sample temperature of less than 0.5%. Furthermore, to demonstrate the capabilities of the facility for elastic scattering studies of liquids, a high quality total structure factor for Zr 64Ni 36 measured slightly above the liquidus temperature is presented from experiments conducted on the nanoscale-ordered materials diffractometer (NOMAD) beam line at the SNS after only 30 min of acquisition time for a small sample ( 100 mg).« less

Electrostatic levitation facility optimized for neutron diffraction studies of high temperature liquids at a spallation neutron source

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

Mauro, N. A., E-mail: namauro@noctrl.edu; Vogt, A. J.; Derendorf, K. S.

2016-01-15

Neutron diffraction studies of metallic liquids provide valuable information about inherent topological and chemical ordering on multiple length scales as well as insight into dynamical processes at the level of a few atoms. However, there exist very few facilities in the world that allow such studies to be made of reactive metallic liquids in a containerless environment, and these are designed for use at reactor-based neutron sources. We present an electrostatic levitation facility, NESL (for Neutron ElectroStatic Levitator), which takes advantage of the enhanced capabilities and increased neutron flux available at spallation neutron sources (SNSs). NESL enables high quality elasticmore » and inelastic neutron scattering experiments to be made of reactive metallic and other liquids in the equilibrium and supercooled temperature regime. The apparatus is comprised of a high vacuum chamber, external and internal neutron collimation optics, and a sample exchange mechanism that allows up to 30 samples to be processed between chamber openings. Two heating lasers allow excellent sample temperature homogeneity, even for samples approaching 500 mg, and an automated temperature control system allows isothermal measurements to be conducted for times approaching 2 h in the liquid state, with variations in the average sample temperature of less than 0.5%. To demonstrate the capabilities of the facility for elastic scattering studies of liquids, a high quality total structure factor for Zr{sub 64}Ni{sub 36} measured slightly above the liquidus temperature is presented from experiments conducted on the nanoscale-ordered materials diffractometer (NOMAD) beam line at the SNS after only 30 min of acquisition time for a small sample (∼100 mg)« less

Further development of a robust workup process for solution-phase high-throughput library synthesis to address environmental and sample tracking issues.

PubMed

Kuroda, Noritaka; Hird, Nick; Cork, David G

2006-01-01

During further improvement of a high-throughput, solution-phase synthesis system, new workup tools and apparatus for parallel liquid-liquid extraction and evaporation have been developed. A combination of in-house design and collaboration with external manufacturers has been used to address (1) environmental issues concerning solvent emissions and (2) sample tracking errors arising from manual intervention. A parallel liquid-liquid extraction unit, containing miniature high-speed magnetic stirrers for efficient mixing of organic and aqueous phases, has been developed for use on a multichannel liquid handler. Separation of the phases is achieved by dispensing them into a newly patented filter tube containing a vertical hydrophobic porous membrane, which allows only the organic phase to pass into collection vials positioned below. The vertical positioning of the membrane overcomes the hitherto dependence on the use of heavier-than-water, bottom-phase, organic solvents such as dichloromethane, which are restricted due to environmental concerns. Both small (6-mL) and large (60-mL) filter tubes were developed for parallel phase separation in library and template synthesis, respectively. In addition, an apparatus for parallel solvent evaporation was developed to (1) remove solvent from the above samples with highly efficient recovery and (2) avoid the movement of individual samples between their collection on a liquid handler and registration to prevent sample identification errors. The apparatus uses a diaphragm pump to achieve a dynamic circulating closed system with a heating block for the rack of 96 sample vials and an efficient condenser to trap the solvents. Solvent recovery is typically >98%, and convenient operation and monitoring has made the apparatus the first choice for removal of volatile solvents.

Combination of solid phase extraction and dispersive liquid-liquid microextraction for separation/preconcentration of ultra trace amounts of uranium prior to its fiber optic-linear array spectrophotometry determination.

PubMed

Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji; Shakerian, Farid; Shiralian Esfahani, Golnaz

2013-12-15

A simple and sensitive method for the separation and preconcentration of the ultra trace amounts of uranium and its determination by spectrophotometry was developed. The method is based on the combination of solid phase extraction and dispersive liquid-liquid microextraction. Thus, by passing the sample through the basic alumina column, the uranyl ion and some cations are separated from the sample matrix. The retained uranyl ion along with the cations are eluted with 5 mL of nitric acid (2 mol L(-1)) and after neutralization of the eluent, the extracted uranyl ion is converted to its anionic benzoate complex and is separated from other cations by extraction of its ion pair with malachite green into small volume of chloroform using dispersive liquid-liquid microextraction. The amount of uranium is then determined by the absorption measurement of the extracted ion pair at 621 nm using flow injection spectrophotometry. Under the optimum conditions, with 500 mL of the sample, a preconcentration factor of 1980, a detection limit of 40 ng L(-1), and a relative standard deviation of 4.1% (n=6) at 400 ng L(-1) were obtained. The method was successfully applied to the determination of uranium in mineral water, river water, well water, spring water and sea water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Simultaneous determination of atorvastatin and valsartan in human plasma by solid-based disperser liquid-liquid microextraction followed by high-performance liquid chromatography-diode array detection.

PubMed

Farajzadeh, Mir Ali; Khorram, Parisa; Pazhohan, Azar

2016-04-01

A simple, sensitive, and efficient method has been developed for simultaneous estimation of valsartan and atorvastatin in human plasma by combination of solid-based dispersive liquid-liquid microextraction and high performance liquid chromatography-diode array detection. In the proposed method, 1,2-dibromoethane (extraction solvent) is added on a sugar cube (as a solid disperser) and it is introduced into plasma sample containing the analytes. After manual shaking and centrifugation, the resultant sedimented phase is subjected to back extraction into a small volume of sodium hydrogen carbonate solution using air-assisted liquid-liquid microextraction. Then the cloudy solution is centrifuged and the obtained aqueous phase is transferred into a microtube and analyzed by the separation system. Under the optimal conditions, extraction recoveries are obtained in the range of 81-90%. Calibration curves plotted in drug-free plasma sample are linear in the ranges of 5-5000μgL(-1) for valsartan and 10-5000μgL(-1) for atorvastatin with the coefficients of determination higher than 0.997. Limits of detection and quantification of the studied analytes in plasma sample are 0.30-2.6 and 1.0-8.2μgL(-1), respectively. Intra-day (n=6) and inter-days (n=4) precisions of the method are satisfactory with relative standard deviations less than 7.4% (at three levels of 10, 500, and 2000μgL(-1), each analyte). These data suggest that the method can be successfully applied to determine trace amounts of valsartan and atorvastatin in human plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Piezo- and solenoid valve-based liquid dispensing for miniaturized assays.

PubMed

Niles, Walter D; Coassin, Peter J

2005-04-01

Miniaturization of biological assays requires dispensing liquids in the submicroliter range of volumes. Accuracy and reproducibility of dispensing this range depend on both the dispenser and the receptacle in which the assay is constructed. Miniaturization technologies developed by Aurora Discovery, Inc. (San Diego, CA) include high-density multiwell plates for assay samples and reagent storage, as well as piezo-based and solenoid valve-based liquid dispensers. Some basic principles of small-volume dispensing by jetting are described to provide context for dispenser design and function. Performance of the latest instruments incorporating these dispensing devices is presented.

Compact air scrubber

DOEpatents

Bentley, Bill F.; Jett, James H.; Martin, John C.; Saunders, George C.

1992-01-01

Method and apparatus for removing material from a gas. A mist created by a piezoelectric ultrasonic transducer is contacted with the gas and both gas and mist are passed through baffled separators. Liquid effluent from the separators contains solid material removed from the gas and gaseous material which reacted with the liquid or was absorbed by the liquid. The invention is useful for collecting a sample of material in a gas, such as a vapor in the atmosphere, and in cleaning a gas. A relatively concentrated solution of a material present in a gas in a very small concentration can be obtained.

Transdiaphragmatic transport of tracer albumin from peritoneal to pleural liquid measured in rats.

PubMed

Lai-Fook, Stephen J; Houtz, Pamela K; Jones, Philip D

2005-12-01

In conscious Wistar-Kyoto rats, we studied the uptake of radioactive tracer (125)I-albumin into the pleural space and circulation after intraperitoneal (IP) injections with 1 or 5 ml of Ringer solution (3 g/dl albumin). Postmortem, we sampled pleural liquid, peritoneal liquid, and blood plasma 2-48 h after IP injection and measured their radioactivity and protein concentration. Tracer concentration was greater in pleural liquid than in plasma approximately 3 h after injection with both IP injection volumes. This behavior indicated transport of tracer through the diaphragm into the pleural space. A dynamic analysis of the tracer uptake with 5-ml IP injections showed that at least 50% of the total pleural flow was via the diaphragm. A similar estimate was derived from an analysis of total protein concentrations. Both estimates were based on restricted pleural capillary filtration and unrestricted transdiaphragmatic transport. The 5-ml IP injections did not change plasma protein concentration but increased pleural and peritoneal protein concentrations from control values by 22 and 30%, respectively. These changes were consistent with a small (approximately 8%) increase in capillary filtration and a small (approximately 20%) reduction in transdiaphragmatic flow from control values, consistent with the small (3%) decrease in hydration measured in diaphragm muscle. Thus the pleural uptake of tracer via the diaphragm with the IP injections occurred by the near-normal transport of liquid and protein.

METHOD OF PREPARATION OF MATERIAL FOR NEUTRON BOMBARDMENT

DOEpatents

Ura, C.L.; Sisman, O.; Briggs, R.B.

1959-02-01

A method is presented for forming slugs or cartridges of sample material to be proeessed in a neutronic reactor. Aceording to this invention, the sample material is originally in the fcrm of powder. The powder is placed within a tube formed of a metallic foil. The material encased in the foil is then placed in a die and compressed under sufficient pressure to form a rigid cartridge. The cartridge is then sealed in a metallic can. As a result of this process, crumbling of the compact during handling is eliminated and it is not necessary to clean ana relubricate the die after compression of each cartridge. ~ A method is presented for producing small spherical shot-type pellets from ceramic or refractory materials. According to this process the material to be pelletized is first formed into a powder. The powdered material is then suspended in a liquid carrier or vehicle. Small drops of the suspension, produced by a capillary-drop apparatus, are deposited on the surfacc of a liquid repellent powder, which causes the drops to assume a spherical shape. The liquid is then evaporated from the spherical pellets and tbe pellets are collected and fired to produce the finished product.

High-Field Liquid-State Dynamic Nuclear Polarization in Microliter Samples.

PubMed

Yoon, Dongyoung; Dimitriadis, Alexandros I; Soundararajan, Murari; Caspers, Christian; Genoud, Jeremy; Alberti, Stefano; de Rijk, Emile; Ansermet, Jean-Philippe

2018-05-01

Nuclear hyperpolarization in the liquid state by dynamic nuclear polarization (DNP) has been of great interest because of its potential use in NMR spectroscopy of small samples of biological and chemical compounds in aqueous media. Liquid state DNP generally requires microwave resonators in order to generate an alternating magnetic field strong enough to saturate electron spins in the solution. As a consequence, the sample size is limited to dimensions of the order of the wavelength, and this restricts the sample volume to less than 100 nL for DNP at 9 T (∼260 GHz). We show here a new approach that overcomes this sample size limitation. Large saturation of electron spins was obtained with a high-power (∼150 W) gyrotron without microwave resonators. Since high power microwaves can cause serious dielectric heating in polar solutions, we designed a planar probe which effectively alleviates dielectric heating. A thin liquid sample of 100 μm of thickness is placed on a block of high thermal conductivity aluminum nitride, with a gold coating that serves both as a ground plane and as a heat sink. A meander or a coil were used for NMR. We performed 1 H DNP at 9.2 T (∼260 GHz) and at room temperature with 10 μL of water, a volume that is more than 100× larger than reported so far. The 1 H NMR signal is enhanced by a factor of about -10 with 70 W of microwave power. We also demonstrated the liquid state of 31 P DNP in fluorobenzene containing triphenylphosphine and obtained an enhancement of ∼200.

Additional band broadening of peptides in the first size-exclusion chromatographic dimension of an automated stop-flow two-dimensional high performance liquid chromatography.

PubMed

Xu, Jucai; Sun-Waterhouse, Dongxiao; Qiu, Chaoying; Zhao, Mouming; Sun, Baoguo; Lin, Lianzhu; Su, Guowan

2017-10-27

The need to improve the peak capacity of liquid chromatography motivates the development of two-dimensional analysis systems. This paper presented a fully automated stop-flow two-dimensional liquid chromatography system with size exclusion chromatography followed by reversed phase liquid chromatography (SEC×RPLC) to efficiently separate peptides. The effects of different stop-flow operational parameters (stop-flow time, peak parking position, number of stop-flow periods and column temperature) on band broadening in the first dimension (1 st D) SEC column were quantitatively evaluated by using commercial small proteins and peptides. Results showed that the effects of peak parking position and the number of stop-flow periods on band broadening were relatively small. Unlike stop-flow analysis of large molecules with a long running time, additional band broadening was evidently observed for small molecule analytes due to the relatively high effective diffusion coefficient (D eff ). Therefore, shorter analysis time and lower 1 st D column temperature were suggested for analyzing small molecules. The stop-flow two-dimensional liquid chromatography (2D-LC) system was further tested on peanut peptides and an evidently improved resolution was observed for both stop-flow heart-cutting and comprehensive 2D-LC analysis (in spite of additional band broadening in SEC). The stop-flow SEC×RPLC, especially heart-cutting analysis with shorter analysis time and higher 1 st D resolution for selected fractions, offers a promising approach for efficient analysis of complex samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Centrifugeless dispersive liquid-liquid microextraction based on salting-out phenomenon followed by high performance liquid chromatography for determination of Sudan dyes in different species.

PubMed

Bazregar, Mohammad; Rajabi, Maryam; Yamini, Yadollah; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

2018-04-01

In this work, a novel method, namely centrifugeless dispersive liquid-liquid microextraction, is introduced for the efficient extraction of banned Sudan dyes from foodstuff and water samples. In this method, which is based upon the salting-out phenomenon, in order to accelerate the extraction process, the extraction solvent (1-undecanol, 75 μL) is dispersed into the sample solution. Then the mixture is passed through a small column filled with 5 g sodium chloride, used as a separating reagent. In this condition, fine droplets of the extraction solvent are floated on the mixture, and the phase separation is simply achieved. This method is environmentally friendly, simple, and very fast, so that the overall extraction time is only 7 min. Under the optimal experimental conditions, the preconcentration factors in the range of 90-121 were obtained for the analytes. Also good linearities were obtained in the range of 2.5-1200 ng mL -1 (r 2  ≥ 0.993). Copyright © 2017 Elsevier Ltd. All rights reserved.

Sub-μL measurements of the thermal conductivity and heat capacity of liquids.

PubMed

López-Bueno, C; Bugallo, D; Leborán, V; Rivadulla, F

2018-03-07

We present the analysis of the thermal conductivity, κ, and heat capacity, C p , of a wide variety of liquids, covering organic molecular solvents, ionic liquids and water-polymer mixtures. These data were obtained from ≈0.6 μL samples, using an experimental development based on the 3ω method, capable of the simultaneous measurement of κ and C p . In spite of the different type and strength of interactions, expected in a priori so different systems, the ratio of κ to the sound velocity is approximately constant for all of them. This is the consequence of a similar atomic density for all these liquids, notwithstanding their different molecular structures. This was corroborated experimentally by the observation of a C p /V ≈ 1.89 × 10 6 J K -1 m -3 (≈3R/2 per atom), for all liquids studied in this work. Finally, the very small volume of the sample required in this experimental method is an important advantage for the characterization of systems like nanofluids, in which having a large amount of the dispersed phase is sometimes extremely challenging.

Nondisruptive Dissolution of Hyperpolarized 129 Xe into Viscous Aqueous and Organic Liquid Crystalline Environments

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

Truxal, Ashley E.; Slack, Clancy C.; Gomes, Muller D.

2016-03-08

Studies of hyperpolarized xenon-129 in media such as liquid crystals and cell suspensions are in demand for applications ranging from biomedical imaging to materials engineering but have been hindered by the inability to bubble Xe through the desired media as a result of viscosity or perturbations caused by bubbles. This research reports on a device that can be reliably used to dissolve hp- 129 Xe into viscous aqueous and organic samples without bubbling. This method is robust, requires small sample volumes ( < 60 μL), is compatible with existing NMR hardware, and is made from readily available materials. Experiments showmore » that Xe can be introduced into viscous and aligned media without disrupting molecular order. We detected dissolved xenon in an aqueous liquid crystal that is disrupted by the shear forces of bubbling, and we observed liquid-crystal phase transitions in (MBBA). This tool allows an entirely new class of samples to be investigated by hyperpolarized-gas NMR spectroscopy. Blending into the crowd: A new device that facilitates the direct dissolution of hyperpolarized 129 Xe into viscous liquid-crystalline media is presented. 129 Xe and 2 H NMR spectra show the nondisruptive dissolution of xenon, the presence of ordered phases, and, in the case of the thermotropic liquid crystal N-(4-methoxybenzylidene)-4-butylaniline, a nematic-isotropic phase transition.« less

Permeability of cork for water and ethanol.

PubMed

Fonseca, Ana Luisa; Brazinha, Carla; Pereira, Helena; Crespo, Joao G; Teodoro, Orlando M N D

2013-10-09

Transport properties of natural (noncompressed) cork were evaluated for water and ethanol in both vapor and liquid phases. The permeability for these permeants has been measured, as well as the sorption and diffusion coefficients. This paper focuses on the differences between the transport of gases' relevant vapors and their liquids (water and ethanol) through cork. A transport mechanism of vapors and liquids is proposed. Experimental evidence shows that both vapors and liquids permeate not only through the small channels across the cells (plasmodesmata), as in the permeation of gases, but also through the walls of cork cells by sorption and diffusion as in dense membranes. The present study also shows that cork permeability for gases was irreversibly and drastically decreased after cork samples were exposed to ethanol or water in liquid phase.

Exploring the dynamics of phase separation in colloid-polymer mixtures with long range attraction.

PubMed

Sabin, Juan; Bailey, Arthur E; Frisken, Barbara J

2016-06-28

We have studied the kinetics of phase separation and gel formation in a low-dispersity colloid - non-adsorbing polymer system with long range attraction using small-angle light scattering. This system exhibits two-phase and three-phase coexistence of gas, liquid and crystal phases when the strength of attraction is between 2 and 4kBT and gel phases when the strength of attraction is increased. For those samples that undergo macroscopic phase separation, whether to gas-crystal, gas-liquid or gas-liquid-crystal coexistence, we observe dynamic scaling of the structure factor and growth of a characteristic length scale that behaves as expected for phase separation in fluids. In samples that gel, the power law associated with the growth of the dominant length scale is not equal to 1/3, but appears to depend mainly on the strength of attraction, decreasing from 1/3 for samples near the coexistence region to 1/27 at 8kBT, over a wide range of colloid and polymer concentrations.

Current status and future prospects of an automated sample exchange system PAM for protein crystallography

NASA Astrophysics Data System (ADS)

Hiraki, M.; Yamada, Y.; Chavas, L. M. G.; Matsugaki, N.; Igarashi, N.; Wakatsuki, S.

2013-03-01

To achieve fully-automated and/or remote data collection in high-throughput X-ray experiments, the Structural Biology Research Centre at the Photon Factory (PF) has installed PF automated mounting system (PAM) for sample exchange robots at PF macromolecular crystallography beamlines BL-1A, BL-5A, BL-17A, AR-NW12A and AR-NE3A. We are upgrading the experimental systems, including the PAM for stable and efficient operation. To prevent human error in automated data collection, we installed a two-dimensional barcode reader for identification of the cassettes and sample pins. Because no liquid nitrogen pipeline in the PF experimental hutch is installed, the users commonly add liquid nitrogen using a small Dewar. To address this issue, an automated liquid nitrogen filling system that links a 100-liter tank to the robot Dewar has been installed on the PF macromolecular beamline. Here we describe this new implementation, as well as future prospects.

Ultra-high-pressure liquid chromatography-tandem mass spectrometry method for the determination of alkylphenols in soil.

PubMed

Wang, Jing; Pan, Hefang; Liu, Zhengzheng; Ge, Fei

2009-03-20

A novel method has been developed for the determination of alkylphenols in soil by ultra-high-pressure liquid chromatography employing small particle sizes, combined with tandem mass spectrometry. Soil samples were extracted with pressurized liquid extraction (PLE) and then cleaned with solid-phase extraction (SPE). The extracts were separated on C18 column (1.7 microm, 50 mm x 2.1mm) with a gradient elution and a mobile phase consisting of water and acetonitrile, and then detected by an electrospray ionization tandem mass spectrometry in negative ion mode with multiple reaction monitoring (MRM). Compared with traditional liquid chromatography, it took ultra-high-pressure liquid chromatography much less time to analyze alkylphenols. Additionally, the ultra-high-pressure liquid chromatography/tandem mass spectrometry method produces satisfactory reliability, sensitivity, and accuracy. The average recoveries of the three target analytes were 74.0-103.4%, with the RSD<15%. The calibration curves for alkylphenols were linear within the range of 0.01-0.4 microg/ml, with the correlation coefficients greater than 0.99. When 10 g soil sample was used for analysis, the limits of quantification (LOQs) of the three alkylphenols were all 1.0 microg/kg.

Flexible packaging of solid-state integrated circuit chips with elastomeric microfluidics

PubMed Central

Zhang, Bowei; Dong, Quan; Korman, Can E.; Li, Zhenyu; Zaghloul, Mona E.

2013-01-01

A flexible technology is proposed to integrate smart electronics and microfluidics all embedded in an elastomer package. The microfluidic channels are used to deliver both liquid samples and liquid metals to the integrated circuits (ICs). The liquid metals are used to realize electrical interconnects to the IC chip. This avoids the traditional IC packaging challenges, such as wire-bonding and flip-chip bonding, which are not compatible with current microfluidic technologies. As a demonstration we integrated a CMOS magnetic sensor chip and associate microfluidic channels on a polydimethylsiloxane (PDMS) substrate that allows precise delivery of small liquid samples to the sensor. Furthermore, the packaged system is fully functional under bending curvature radius of one centimetre and uniaxial strain of 15%. The flexible integration of solid-state ICs with microfluidics enables compact flexible electronic and lab-on-a-chip systems, which hold great potential for wearable health monitoring, point-of-care diagnostics and environmental sensing among many other applications.

Integration of Ion Mobility MSE after Fully Automated, Online, High-Resolution Liquid Extraction Surface Analysis Micro-Liquid Chromatography

PubMed Central

2017-01-01

Direct analysis by mass spectrometry (imaging) has become increasingly deployed in preclinical and clinical research due to its rapid and accurate readouts. However, when it comes to biomarker discovery or histopathological diagnostics, more sensitive and in-depth profiling from localized areas is required. We developed a comprehensive, fully automated online platform for high-resolution liquid extraction surface analysis (HR-LESA) followed by micro–liquid chromatography (LC) separation and a data-independent acquisition strategy for untargeted and low abundant analyte identification directly from tissue sections. Applied to tissue sections of rat pituitary, the platform demonstrated improved spatial resolution, allowing sample areas as small as 400 μm to be studied, a major advantage over conventional LESA. The platform integrates an online buffer exchange and washing step for removal of salts and other endogenous contamination that originates from local tissue extraction. Our carry over–free platform showed high reproducibility, with an interextraction variability below 30%. Another strength of the platform is the additional selectivity provided by a postsampling gas-phase ion mobility separation. This allowed distinguishing coeluted isobaric compounds without requiring additional separation time. Furthermore, we identified untargeted and low-abundance analytes, including neuropeptides deriving from the pro-opiomelanocortin precursor protein and localized a specific area of the pituitary gland (i.e., adenohypophysis) known to secrete neuropeptides and other small metabolites related to development, growth, and metabolism. This platform can thus be applied for the in-depth study of small samples of complex tissues with histologic features of ∼400 μm or more, including potential neuropeptide markers involved in many diseases such as neurodegenerative diseases, obesity, bulimia, and anorexia nervosa. PMID:28945354

Thorough small-angle X-ray scattering analysis of the instability of liquid micro-jets in air.

PubMed

Marmiroli, Benedetta; Cacho-Nerin, Fernando; Sartori, Barbara; Pérez, Javier; Amenitsch, Heinz

2014-01-01

Liquid jets are of interest, both for their industrial relevance and for scientific applications (more important, in particular for X-rays, after the advent of free-electron lasers that require liquid jets as sample carrier). Instability mechanisms have been described theoretically and by numerical simulation, but confirmed by few experimental techniques. In fact, these are mainly based on cameras, which is limited by the imaging resolution, and on light scattering, which is hindered by absorption, reflection, Mie scattering and multiple scattering due to complex air/liquid interfaces during jet break-up. In this communication it is demonstrated that synchrotron small-angle X-ray scattering (SAXS) can give quantitative information on liquid jet dynamics at the nanoscale, by detecting time-dependent morphology and break-up length. Jets ejected from circular tubes of different diameters (100-450 µm) and speeds (0.7-21 m s(-1)) have been explored to cover the Rayleigh and first wind-induced regimes. Various solvents (water, ethanol, 2-propanol) and their mixtures have been examined. The determination of the liquid jet behaviour becomes essential, as it provides background data in subsequent studies of chemical and biological reactions using SAXS or X-ray diffraction based on synchrotron radiation and free-electron lasers.

Magnetic particles as liquid carriers in the microfluidic lab-in-tube approach to detect phase change.

PubMed

Blumenschein, Nicholas A; Han, Daewoo; Caggioni, Marco; Steckl, Andrew J

2014-06-11

Magnetic beads (MBs) with ∼1.9 μm average diameter were used to transport specific microliter-scale volumes of liquids between adjacent reservoirs within a closed tube under the influence of a magnetic field. The tube's inner surface is coated with a hydrophobic layer, enabling the formation of a surface tension valve by inserting an air gap between reservoirs. This transfer process was implemented by keeping the MBs stationary with a fixed external magnet while the liquid reservoirs were translated by a computer-controlled syringe pump system. The magnet induces the aggregation of MBs in a loosely packed cluster (void volume ∼90-95%) against the tube's inner wall. The liquid trapped in the MB cluster is transported across the air gap between reservoirs. Fluorescence intensity from a dye placed in one reservoir is used to measure the volume of liquid transferred between reservoirs. The carry-over liquid volume is controlled by the mass of the MBs within the device. The typical volume of liquid carried by the MB cluster is ∼2 to 3 μL/mg of beads, allowing the use of small samples. This technique can be used to study the effect of small compositional variation on the properties of fluid mixtures. The feasibility of this "lab-in-tube" approach for binary phase diagram determination in a water-surfactant (C12E5) system was demonstrated.

Fast automated dual-syringe based dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry for the determination of polycyclic aromatic hydrocarbons in environmental water samples.

PubMed

Guo, Liang; Tan, Shufang; Li, Xiao; Lee, Hian Kee

2016-03-18

An automated procedure, combining low density solvent based solvent demulsification dispersive liquid-liquid microextraction (DLLME) with gas chromatography-mass spectrometry analysis, was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. Capitalizing on a two-rail commercial autosampler, fast solvent transfer using a large volume syringe dedicated to the DLLME process, and convenient extract collection using a small volume microsyringe for better GC performance were enabled. Extraction parameters including the type and volume of extraction solvent, the type and volume of dispersive solvent and demulsification solvent, extraction and demulsification time, and the speed of solvent injection were investigated and optimized. Under the optimized conditions, the linearity ranged from 0.1 to 50 μg/L, 0.2 to 50 μg/L, and 0.5 to 50 μg/L, depending on the analytes. Limits of detection were determined to be between 0.023 and 0.058 μg/L. The method was applied to determine PAHs in environmental water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Characterization of white poplar and eucalyptus after ionic liquid pretreatment as a function of biomass loading using X-ray diffraction and small angle neutron scattering

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

Yuan, Xueming; Duan, Yonghao; He, Lilin

A systematic study was done to understand interactions among biomass loading during ionic liquid (IL) pretreatment, biomass type and biomass structures. White poplar and eucalyptus samples were pretreated using 1-ethyl-3-methylimidazolium acetate (EmimOAc) at 110 °C for 3 h at biomass loadings of 5, 10, 15, 20 and 25 wt%. All of the samples were chemically characterized and tested for enzymatic hydrolysis. Physical structures including biomass crystallinity and porosity were measured by X-ray diffraction (XRD) and small angle neutron scattering (SANS), respectively. SANS detected pores of radii ranging from ~25 to 625 Å, enabling assessment of contributions of pores with different sizes to increased porositymore » after pretreatment. Contrasting dependences of sugar conversion on white poplar and eucalyptus as a function of biomass loading were observed and cellulose crystalline structure was found to play an important role.« less

Characterization of white poplar and eucalyptus after ionic liquid pretreatment as a function of biomass loading using X-ray diffraction and small angle neutron scattering.

PubMed

Yuan, Xueming; Duan, Yonghao; He, Lilin; Singh, Seema; Simmons, Blake; Cheng, Gang

2017-05-01

A systematic study was performed to understand interactions among biomass loading during ionic liquid (IL) pretreatment, biomass type and biomass structures. White poplar and eucalyptus samples were pretreated using 1-ethyl-3-methylimidazolium acetate (EmimOAc) at 110°C for 3h at biomass loadings of 5, 10, 15, 20 and 25wt%. All of the samples were chemically characterized and tested for enzymatic hydrolysis. Physical structures including biomass crystallinity and porosity were measured by X-ray diffraction (XRD) and small angle neutron scattering (SANS), respectively. SANS detected pores of radii ranging from ∼25 to 625Å, enabling assessment of contributions of pores with different sizes to increased porosity after pretreatment. Contrasting dependences of sugar conversion on white poplar and eucalyptus as a function of biomass loading were observed and cellulose crystalline structure was found to play an important role. Copyright © 2017 Elsevier Ltd. All rights reserved.

Characterization of a Hybrid Optical Microscopy/Laser Ablation Liquid Vortex Capture/Electrospray Ionization System for Mass Spectrometry Imaging

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

Cahill, John F.; Kertesz, Vilmos; Van Berkel, Gary J.

Herein, a commercial optical microscope, laser microdissection instrument was coupled with an electrospray ionization mass spectrometer via a low profile liquid vortex capture probe to yield a hybrid optical microscopy/mass spectrometry imaging system. The instrument has bright-field and fluorescence microscopy capabilities in addition to a highly focused UV laser beam that is utilized for laser ablation of samples. With this system, material laser ablated from a sample using the microscope was caught by a liquid vortex capture probe and transported in solution for analysis by electrospray ionization mass spectrometry. Both lane scanning and spot sampling mass spectral imaging modes weremore » used. The smallest area the system was able to ablate was ~0.544 μm × ~0.544 μm, achieved by oversampling of the smallest laser ablation spot size that could be obtained (~1.9 μm). With use of a model photoresist surface, known features as small as ~1.5 μm were resolved. The capabilities of the system with real world samples were demonstrated first with a blended polymer thin film containing poly(2-vinylpyridine) and poly(N-vinylcarbazole). Using spot sampling imaging, sub-micrometer sized features (0.62, 0.86, and 0.98 μm) visible by optical microscopy were clearly distinguished in the mass spectral images. A second real world example showed the imaging of trace amounts of cocaine in mouse brain thin tissue sections. Lastly, with use of a lane scanning mode with ~6 μm × ~6 μm data pixels, features in the tissue as small as 15 μm in size could be distinguished in both the mass spectral and optical images.« less

Characterization of a Hybrid Optical Microscopy/Laser Ablation Liquid Vortex Capture/Electrospray Ionization System for Mass Spectrometry Imaging

DOE PAGES

Cahill, John F.; Kertesz, Vilmos; Van Berkel, Gary J.

2015-10-22

Herein, a commercial optical microscope, laser microdissection instrument was coupled with an electrospray ionization mass spectrometer via a low profile liquid vortex capture probe to yield a hybrid optical microscopy/mass spectrometry imaging system. The instrument has bright-field and fluorescence microscopy capabilities in addition to a highly focused UV laser beam that is utilized for laser ablation of samples. With this system, material laser ablated from a sample using the microscope was caught by a liquid vortex capture probe and transported in solution for analysis by electrospray ionization mass spectrometry. Both lane scanning and spot sampling mass spectral imaging modes weremore » used. The smallest area the system was able to ablate was ~0.544 μm × ~0.544 μm, achieved by oversampling of the smallest laser ablation spot size that could be obtained (~1.9 μm). With use of a model photoresist surface, known features as small as ~1.5 μm were resolved. The capabilities of the system with real world samples were demonstrated first with a blended polymer thin film containing poly(2-vinylpyridine) and poly(N-vinylcarbazole). Using spot sampling imaging, sub-micrometer sized features (0.62, 0.86, and 0.98 μm) visible by optical microscopy were clearly distinguished in the mass spectral images. A second real world example showed the imaging of trace amounts of cocaine in mouse brain thin tissue sections. Lastly, with use of a lane scanning mode with ~6 μm × ~6 μm data pixels, features in the tissue as small as 15 μm in size could be distinguished in both the mass spectral and optical images.« less

Urinary metabolomic study of non-small cell lung carcinoma based on ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

PubMed

Wu, Qian; Wang, Yan; Gu, Xue; Zhou, Junyi; Zhang, Huiping; Lv, Wang; Chen, Zhe; Yan, Chao

2014-07-01

Metabolic profiles from human urine reveal the significant difference of carnitine and acylcarnitines levels between non-small cell lung carcinoma patients and healthy controls. Urine samples from cancer patients and healthy individuals were assayed in this metabolomic study using ultra high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry. The data were normalized by the sum of all intensities and creatinine calibration, respectively, before orthogonal partial least squares discriminant analysis. Twenty differential metabolites were identified based on standard compounds or tandem mass spectrometry fragments. Among them, some medium-/long-chain acylcarnitines, for example, cis-3,4-methylene heptanoylcarnitine, were found to be downregulated while carnitine was upregulated in urine samples from the cancer group compared to the control group. Receiver operating characteristic analysis of the two groups showed that the area under curve for the combination of carnitine and 11 selected acylcarnitines was 0.958. This study suggests that the developed carnitine and acylcarnitines profiling method has the potential to be used for screening non-small cell lung carcinoma. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Polymerization speed and diffractive experiments in polymer network LC test cells

NASA Astrophysics Data System (ADS)

Braun, Larissa; Gong, Zhen; Habibpourmoghadam, Atefeh; Schafforz, Samuel L.; Wolfram, Lukas; Lorenz, Alexander

2018-02-01

Polymer-network liquid crystals (LCs), where the response properties of a LC can be enhanced by the presence of a porous polymer network, are investigated. In the reported experiments, liquid crystals were doped with a small amount (< 10%) of photo-curable acrylate monomers. Samples with surface grafted photoinitiators, dissolvable photoinitiators, and samples with both kinds of photoinitiators were prepared. Both conventional (planar electrodes) and diffractive (interdigitated electrodes) test cells were used. These samples were exposed with a UV light source and changes of their capacitance were investigated with an LCR meter during exposure. Due to the presence of the in-situ generated polymer network, the electro-optic response properties of photo cured samples were enhanced. For example, their continuous phase modulation properties led to more localized responses in samples with interdigitated electrodes, which caused suppression of selected diffraction orders in the diffraction patterns recorded in polymer network LC samples. Moreover, capacitance changes were investigated during photopolymerization of a blue phase LC.

Sampling and analysis for radon-222 dissolved in ground water and surface water

USGS Publications Warehouse

DeWayne, Cecil L.; Gesell, T.F.

1992-01-01

Radon-222 is a naturally occurring radioactive gas in the uranium-238 decay series that has traditionally been called, simply, radon. The lung cancer risks associated with the inhalation of radon decay products have been well documented by epidemiological studies on populations of uranium miners. The realization that radon is a public health hazard has raised the need for sampling and analytical guidelines for field personnel. Several sampling and analytical methods are being used to document radon concentrations in ground water and surface water worldwide but no convenient, single set of guidelines is available. Three different sampling and analytical methods - bubbler, liquid scintillation, and field screening - are discussed in this paper. The bubbler and liquid scintillation methods have high accuracy and precision, and small analytical method detection limits of 0.2 and 10 pCi/l (picocuries per liter), respectively. The field screening method generally is used as a qualitative reconnaissance tool.

Determination of alkylphenols and bisphenol A in seawater samples by dispersive liquid-liquid microextraction and liquid chromatography tandem mass spectrometry for compliance with environmental quality standards (Directive 2008/105/EC).

PubMed

Salgueiro-González, N; Concha-Graña, E; Turnes-Carou, I; Muniategui-Lorenzo, S; López-Mahía, P; Prada-Rodríguez, D

2012-02-03

A fast, simple, sensitive and green analytical chemistry method for the simultaneous determination of alkylphenols (4-tert-octylphenol, 4-octylphenol, 4-n-nonylphenol, nonylphenol) and bisphenol A in seawater was developed and validated. The procedure was based on a dispersive liquid-liquid microextraction (DLLME) of a small volume of seawater sample (30 mL) using only 100 μL of 1-octanol, combined with liquid chromatography-electrospray ionization tandem mass spectrometry in negative mode (LC-ESI-MS/MS). The matrix effect was studied and compensated using deuterated labelled standards as surrogate standards for the quantitation of target compounds. The analytical features of the proposed method were satisfactory: repeatability and intermediate precision were <10% and recoveries were around 84-104% for all compounds. Uncertainty assessment of measurement was estimated on the basis of an in-house validation according to EURACHEM/CITAC guide. Quantitation limits of the method (MQL) ranged between 0.005 and 0.03 μg L⁻¹, therefore the levels established in the Directive 2008/105/EC were achieved. The applicability of the proposed method was demonstrated analyzing seawater samples from different sites of A Coruña (Northwest of Spain). The analyses showed the presence of all compounds at levels between 0.035 (bisphenol A) and 0.14 μg L⁻¹ (nonylphenol). Copyright © 2011 Elsevier B.V. All rights reserved.

Binary Solvents Dispersive Liquid-Liquid Microextraction (BS-DLLME) Method for Determination of Tramadol in Urine Using High-Performance Liquid Chromatography.

PubMed

Kiarostami, Vahid; Rouini, Mohamad-Reza; Mohammadian, Razieh; Lavasani, Hoda; Ghazaghi, Mehri

2014-02-03

Tramadol is an opioid, synthetic analog of codeine and has been used for the treatment of acute or chronic pain may be abused. In this work, a developed Dispersive liquid liquid microextraction (DLLME) as binary solvents-based dispersive liquid-liquid microextraction (BS-DLLME) combined with high performance liquid chromatography (HPLC) with fluorescence detection (FD) was employed for determination of tramadol in the urine samples. This procedure involves the use of an appropriate mixture of binary extraction solvents (70 μL CHCl3 and 30 μL ethyl acetate) and disperser solvent (600 μL acetone) for the formation of cloudy solution in 5 ml urine sample comprising tramadol and NaCl (7.5%, w/v). After centrifuging, the small droplets of extraction solvents were precipitated. In the final step, the HPLC with fluorescence detection was used for determination of tramadol in the precipitated phase. Various factors on the efficiency of the proposed procedure were investigated and optimized. The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 μg/L, respectively. The relative standard deviations (RSD) for the extraction of 30 μg L of tramadol was found 4.1% (n = 6). The relative recoveries of tramadol from urine samples at spiking levels of 10, 30 and 60 μg/L were in the range of 95.6 - 99.6%. Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories.

Analysis of small droplets with a new detector for liquid chromatography based on laser-induced breakdown spectroscopy

NASA Astrophysics Data System (ADS)

Janzen, Christoph; Fleige, Rüdiger; Noll, Reinhard; Schwenke, Heinrich; Lahmann, Wilhelm; Knoth, Joachim; Beaven, Peter; Jantzen, Eckard; Oest, Andreas; Koke, Peter

2005-08-01

The miniaturization of analytical techniques is a general trend in speciation analytics. We have developed a new analytical technique combining high pressure liquid chromatography (HPLC) with laser-induced breakdown spectroscopy (LIBS). This enables a molecule-specific separation followed by an element-specific analysis of smallest amounts of complex samples. The liquid flow coming from a HPLC pump is transformed into a continuous stream of small droplets (diameter 50-100 μm, volume 65-500 pl) using a piezoelectric pulsed nozzle. After the detection of single droplets with a droplet detector, a Q-switched Nd:YAG Laser is triggered to emit a synchronized laser pulse that irradiates a single droplet. The droplets are evaporated and transformed to the plasma state. The spectrum emitted from the plasma is collected by a spherical mirror and directed through the entrance slit of a Paschen-Runge spectrometer equipped with channel photomultipliers. The spectrometer detects 31 elements simultaneously covering a spectral range from 120 to 589 nm. Purging the measurement chamber with argon enables the detection of vacuum-UV lines. Since the sample is transferred to the plasma state without dilution, very low flow rates in the sub-μl/min range can be realised.

Effect of gas mass flux on cryogenic liquid jet breakup

NASA Technical Reports Server (NTRS)

Ingebo, R. D.

1992-01-01

A scattered-light scanning instrument developed at NASA Lewis Research Center was used to measure the characteristic drop size of clouds of liquid nitrogen droplets. The instrument was calibrated with suspensions of monosized polystyrene spheres. In this investigation of the mechanism of liquid nitrogen jet disintegration in a high-velocity gas flow, the Sauter mean diameter, D32, was found to vary inversely with the nitrogen gas mass flux raised to the power 1.33. Values of D32 varied from 5 to 25 microns and the mass flux exponent of 1.33 agrees well with theory for liquid jet breakup in high-velocity gas flows. The loss of very small droplets due to the high vaporization rate of liquid nitrogen was avoided by sampling the spray very close to the atomizer, i.e., 1.3 cm downstream of the nozzle orifice. The presence of high velocity and thermal gradients in the gas phase also made sampling of the particles difficult. As a result, it was necessary to correct the measurements for background noise produced by both highly turbulent gas flows and thermally induced density gradients in the gas phase.

Heat capacity measurements of sub-nanoliter volumes of liquids using bimaterial microchannel cantilevers

NASA Astrophysics Data System (ADS)

Khan, M. F.; Miriyala, N.; Lee, J.; Hassanpourfard, M.; Kumar, A.; Thundat, T.

2016-05-01

Lab-on-a-Chip compatible techniques for thermal characterization of miniaturized volumes of liquid analytes are necessary in applications such as protein blotting, DNA melting, and drug development, where samples are either rare or volume-limited. We developed a closed-chamber calorimeter based on a bimaterial microchannel cantilever (BMC) for sub-nanoliter level thermal analysis. When the liquid-filled BMC is irradiated with infrared (IR) light at a specific wavelength, the IR absorption by the liquid analyte results in localized heat generation and the subsequent deflection of the BMC, due to a thermal expansion mismatch between the constituent materials. The time constant of the deflection, which is dependent upon the heat capacity of the liquid analyte, can be directly measured by recording the time-dependent bending of the BMC. We have used the BMC to quantitatively measure the heat capacity of five volatile organic compounds. With a deflection noise level of ˜10 nm and a signal-to-noise ratio of 68:1, the BMC offers a sensitivity of 30.5 ms/(J g-1 K-1) and a resolution of 23 mJ/(g K) for ˜150 pl liquid for heat capacity measurements. This technique can be used for small-scale thermal characterization of different chemical and biological samples.

Monitoring xenon purity in the LUX detector with a mass spectrometry system

NASA Astrophysics Data System (ADS)

Balajthy, Jon; LUX Experiment Collaboration

2015-04-01

The LUX dark matter search experiment is a 350 kg two-phase liquid/gas xenon time projection chamber located at the 4850 ft level of the Sanford Underground Research Facility in Lead, SD. To monitor for radioactive impurities such as krypton and impurities which limit charge yield such as oxygen, LUX uses a xenon sampling system consisting of a mass spectrometer and a liquid nitrogen cold trap. The cold trap separates the gaseous impurities from a small sample of xenon and allows them to pass to the mass spectrometer for analysis. We report here on results from the LUX xenon sampling program. We also report on methods to enhance the sensitivity of the cold trap technique in preparation for the next-generation LUX-ZEPLIN experiment which will have even more stringent purity requirements.

Compact dry chemistry instruments.

PubMed

Terashima, K; Tatsumi, N

1999-01-01

Compact dry chemistry instruments are designed for use in point-of-care-testing (POCT). These instruments have a number of advantages, including light weight, compactness, ease of operation, and the ability to provide accurate results in a short time with a very small sample volume. On the other hand, reagent costs are high compared to liquid method. Moreover, differences in accuracy have been found between dry chemistry and the liquid method in external quality assessment scheme. This report examines reagent costs and shows how the total running costs associated with dry chemistry are actually lower than those associated with the liquid method. This report also describes methods for minimizing differences in accuracy between dry chemistry and the liquid method. Use of these measures is expected to increase the effectiveness of compact dry chemistry instruments in POCT applications.

Binary Colloidal Alloy Test-5: Aspheres

NASA Technical Reports Server (NTRS)

Chaikin, Paul M.; Hollingsworth, Andrew D.

2008-01-01

The Binary Colloidal Alloy Test - 5: Aspheres (BCAT-5-Aspheres) experiment photographs initially randomized colloidal samples (tiny nanoscale spheres suspended in liquid) in microgravity to determine their resulting structure over time. BCAT-5-Aspheres will study the properties of concentrated systems of small particles when they are identical, but not spherical in microgravity..

Comparison of Internal Energy Distributions of Ions Created by Electrospray Ionization and Laser Ablation-Liquid Vortex Capture-Electrospray Ionization

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

Cahill, John F.; Kertesz, Vilmos; Ovchinnikova, Olga S.

2015-06-27

Recently a number of techniques have combined laser ablation with liquid capture for mass spectrometry spot sampling and imaging applications. The newly developed non-contact liquid-vortex capture probe has been used to efficiently collect 355 nm UV laser ablated material in a continuous flow solvent stream in which the captured material dissolves and then undergoes electrospray ionization. This sampling and ionization approach has produced what appear to be classic electrospray ionization spectra; however, the softness of this sampling/ionization process versus simple electrospray ionization has not been definitely determined. A series of benzlypyridinium salts, known as thermometer ions, were used to comparemore » internal energy distributions between electrospray ionization and the UV laser ablation liquid-vortex capture probe electrospray combination. Measured internal energy distributions were identical between the two techniques, even with differences in laser fluence (0.7-3.1 J cm-2) and when using UV-absorbing or non-UV-absorbing sample substrates. This data indicates ions formed directly by UV laser ablation, if any, are likely an extremely small constituent of the total ion signal observed. Instead, neutral molecules, clusters or particulates ejected from the surface during laser ablation, subsequently captured and dissolved in the flowing solvent stream then electrosprayed are the predominant source of ion signal observed. The electrospray ionization process used controls the softness of the technique.« less

Microvolume trace environmental analysis using peak-focusing online solid-phase extraction-nano-liquid chromatography-high-resolution mass spectrometry.

PubMed

Stravs, Michael A; Mechelke, Jonas; Ferguson, P Lee; Singer, Heinz; Hollender, Juliane

2016-03-01

Online solid-phase extraction was combined with nano-liquid chromatography coupled to high-resolution mass spectrometry (HRMS) for the analysis of micropollutants in environmental samples from small volumes. The method was validated in surface water, Microcystis aeruginosa cell lysate, and spent Microcystis growth medium. For 41 analytes, quantification limits of 0.1-28 ng/L (surface water) and 0.1-32 ng/L (growth medium) were obtained from only 88 μL of sample. In cell lysate, quantification limits ranged from 0.1-143 ng/L or 0.33-476 ng/g dry weight from a sample of 88 μL, or 26 μg dry weight, respectively. The method matches the sensitivity of established online and offline solid-phase extraction-liquid chromatography-mass spectrometry methods but requires only a fraction of the sample used by those techniques, and is among the first applications of nano-LC-MS for environmental analysis. The method was applied to the determination of bioconcentration in Microcystis aeruginosa in a laboratory experiment, and the benefit of coupling to HRMS was demonstrated in a transformation product screening.

Liquid chromatography/Fourier transform IR spectrometry interface flow cell

DOEpatents

Johnson, Charles C.; Taylor, Larry T.

1986-01-01

A zero dead volume (ZDV) microbore high performance liquid chromatography (.mu.HPLC)/Fourier transform infrared (FTIR) interface flow cell includes an IR transparent crystal having a small diameter bore therein through which a sample liquid is passed. The interface flow cell further includes a metal holder in combination with a pair of inner, compressible seals for directly coupling the thus configured spectrometric flow cell to the outlet of a .mu.HPLC column end fitting to minimize the transfer volume of the effluents exiting the .mu.HPLC column which exhibit excellent flow characteristics due to the essentially unencumbered, open-flow design. The IR beam passes transverse to the sample flow through the circular bore within the IR transparent crystal, which is preferably comprised of potassium bromide (KBr) or calcium fluoride (CaF.sub.2), so as to minimize interference patterns and vignetting encountered in conventional parallel-plate IR cells. The long IR beam pathlength and lensing effect of the circular cross-section of the sample volume in combination with the refractive index differences between the solvent and the transparent crystal serve to focus the IR beam in enhancing sample detection sensitivity by an order of magnitude.

Liquid chromatography/Fourier transform IR spectrometry interface flow cell

DOEpatents

Johnson, C.C.; Taylor, L.T.

1985-01-04

A zero dead volume (ZDV) microbore high performance liquid chromatography (..mu.. HPLC)/Fourier transform infrared (FTIR) interface flow cell includes an IR transparent crystal having a small diameter bore therein through which a sample liquid is passed. The interface flow cell further includes a metal holder in combination with a pair of inner, compressible seals for directly coupling the thus configured spectrometric flow cell to the outlet of a ..mu.. HPLC column end fitting to minimize the transfer volume of the effluents exiting the ..mu.. HPLC column which exhibit excellent flow characteristics due to the essentially unencumbered, open-flow design. The IR beam passes transverse to the sample flow through the circular bore within the IR transparent crystal, which is preferably comprised of potassium bromide (KBr) or calcium fluoride (CaF/sub 2/), so as to minimize interference patterns and vignetting encountered in conventional parallel-plate IR cells. The long IR beam pathlength and lensing effect of the circular cross-section of the sample volume in combination with the refractive index differences between the solvent and the transparent crystal serve to focus the IR beam in enhancing sample detection sensitivity by an order of magnitude.

Meteorite heat capacities: Results to date

NASA Astrophysics Data System (ADS)

Consolmagno, G.; Macke, R.; Britt, D.

2014-07-01

Heat capacity is an essential thermal property for modeling asteroid internal metamorphism or differentiation, and dynamical effects like YORP or Yarkovsky perturbations. We have developed a rapid, inexpensive, and non-destructive method for measuring the heat capacity of meteorites at low temperature [1]. A sample is introduced into a dewar of liquid nitrogen and an electronic scale measures the amount of nitrogen boiled away as the sample is cooled from the room temperature to the liquid nitrogen temperature; given the heat of vaporization of liquid nitrogen, one can then calculate the heat lost from the sample during the cooling process. Note that heat capacity in this temperature range is a strong function of temperature, but this functional relation is essentially the same for all materials; the values we determine are equivalent to the heat capacity of the sample at 175 K. To correct for systematic errors, samples of laboratory-grade quartz are measured along with the meteorite samples. To date, more than 70 samples of more than 50 different meteorites have been measured in this way, including ordinary chondrites [1], irons [2], basaltic achondrites [3], and a limited number of carbonaceous chondrites [1]. In general, one can draw a number of important conclusions from these results. First, the heat capacity of a meteorite is a function of its mineral composition, independent of shock, metamorphism, or other physical state. Second, given this relation, heat capacity can be strongly altered by terrestrial weathering. Third, the measurement of heat capacity in small (less than 1 g) samples as done typically by commercial systems runs a serious risk of giving misleading results for samples that are heterogeneous on scales of tens of grams or more. Finally, we demonstrate that heat capacity is a useful tool for determining and classifying a sample, especially if used in conjunction with other intrinsic variables such as grain density and magnetic susceptibility. We will present an updated list of our results, incorporating our latest corrections for a variety of small but measurable systematic errors, and new results for meteorites and meteorite types not previously measured or reported.

Isotropic-nematic phase transition in aqueous sepiolite suspensions.

PubMed

Woolston, Phillip; van Duijneveldt, Jeroen S

2015-01-01

Aqueous suspensions of sepiolite clay rods in water tend to form gels on increase of concentration. Here it is shown how addition of a small amount (0.1% of the clay mass) of a common stabiliser for clay suspensions, sodium polyacrylate, can allow the observation of an isotropic-nematic liquid crystal phase transition. This transition was found to move to higher clay concentrations upon adding NaCl, with samples containing 10(-3) M salt or above only displaying a gel phase. Even samples that initially formed liquid crystals had a tendency to form gels after several weeks, possibly due to Mg(2+) ions leaching from the clay mineral. Copyright © 2014 The Authors. Published by Elsevier Inc. All rights reserved.

Quantitative Analysis of Urine Vapor and Breath by Gas-Liquid Partition Chromatography

PubMed Central

Pauling, Linus; Robinson, Arthur B.; Teranishi, Roy; Cary, Paul

1971-01-01

When a human being is placed for several days on a completely defined diet, consisting almost entirely of small molecules that are absorbed from the stomach into the blood, intestinal flora disappear because of lack of nutrition. By this technique, the composition of body fluids can be made constant (standard deviation about 10%) after a few days, permitting significant quantitative analyses to be performed. A method of temperature-programmed gas-liquid partition chromatography has been developed for this purpose. It permits the quantitative determination of about 250 substances in a sample of breath, and of about 280 substances in a sample of urine vapor. The technique should be useful in the application of the principles of orthomolecular medicine. PMID:5289873

Quantitative analysis of urine vapor and breath by gas-liquid partition chromatography.

PubMed

Pauling, L; Robinson, A B; Teranishi, R; Cary, P

1971-10-01

When a human being is placed for several days on a completely defined diet, consisting almost entirely of small molecules that are absorbed from the stomach into the blood, intestinal flora disappear because of lack of nutrition. By this technique, the composition of body fluids can be made constant (standard deviation about 10%) after a few days, permitting significant quantitative analyses to be performed. A method of temperature-programmed gas-liquid partition chromatography has been developed for this purpose. It permits the quantitative determination of about 250 substances in a sample of breath, and of about 280 substances in a sample of urine vapor. The technique should be useful in the application of the principles of orthomolecular medicine.

OASIS: Organics Analyzer for Sampling Icy Surfaces

NASA Technical Reports Server (NTRS)

Getty, S. A.; Dworkin, J. P.; Glavin, D. P.; Martin, M.; Zheng, Y.; Balvin, M.; Southard, A. E.; Ferrance, J.; Malespin, C.

2012-01-01

Liquid chromatography mass spectrometry (LC-MS) is a well established laboratory technique for detecting and analyzing organic molecules. This approach has been especially fruitful in the analysis of nucleobases, amino acids, and establishing chirol ratios [1 -3]. We are developing OASIS, Organics Analyzer for Sampling Icy Surfaces, for future in situ landed missions to astrochemically important icy bodies, such as asteroids, comets, and icy moons. The OASIS design employs a microfabricated, on-chip analytical column to chromatographically separate liquid ana1ytes using known LC stationary phase chemistries. The elution products are then interfaced through electrospray ionization (ESI) and analyzed by a time-of-flight mass spectrometer (TOF-MS). A particular advantage of this design is its suitability for microgravity environments, such as for a primitive small body.

Design and development of a highly sensitive, field portable plasma source instrument for on-line liquid stream monitoring and real-time sample analysis

NASA Astrophysics Data System (ADS)

Duan, Yixiang; Su, Yongxuan; Jin, Zhe; Abeln, Stephen P.

2000-03-01

The development of a highly sensitive, field portable, low-powered instrument for on-site, real-time liquid waste stream monitoring is described in this article. A series of factors such as system sensitivity and portability, plasma source, sample introduction, desolvation system, power supply, and the instrument configuration, were carefully considered in the design of the portable instrument. A newly designed, miniature, modified microwave plasma source was selected as the emission source for spectroscopy measurement, and an integrated small spectrometer with a charge-coupled device detector was installed for signal processing and detection. An innovative beam collection system with optical fibers was designed and used for emission signal collection. Microwave plasma can be sustained with various gases at relatively low power, and it possesses high detection capabilities for both metal and nonmetal pollutants, making it desirable to use for on-site, real-time, liquid waste stream monitoring. An effective in situ sampling system was coupled with a high efficiency desolvation device for direct-sampling liquid samples into the plasma. A portable computer control system is used for data processing. The new, integrated instrument can be easily used for on-site, real-time monitoring in the field. The system possesses a series of advantages, including high sensitivity for metal and nonmetal elements; in situ sampling; compact structure; low cost; and ease of operation and handling. These advantages will significantly overcome the limitations of previous monitoring techniques and make great contributions to environmental restoration and monitoring.

Thermodynamic and Neutron Scattering Study of the Spin-1/2 Kagome Antiferromagnet ZnCu3(OH)6Cl2: A Quantum Spin Liquid System

NASA Astrophysics Data System (ADS)

Han, Tianheng

New physics, such as a quantum spin liquid, can emerge in systems where quantum fluctuations are enhanced due to reduced dimensionality and strong frustration . The realization of a quantum spin liquid in two-dimensions would represent a new state of matter. It is believed that spin liquid physics plays a role in the phenomenon of high-Tc superconductivity, and the topological properties of the spin liquid state may have applications in the field of quantum information. The Zn-paratacamite family, ZnxCu4-- x(OH)6Cl2 for x > 0.33, is an ideal system to look for such an exotic state in the form of antiferromagnetic Cu 2 + kagome planes. The x = 1 end member, named herbertsmithite, has shown promising spin liquid properties from prior studies on powder samples. Here we show a new synthesis by which high-quality centimeter-sized single crystals of Znparatacamite have been produced for the first time. Neutron and synchrotron xray diffraction experiments indicate no structural transition down to T = 2 K. The magnetic susceptibility both perpendicular and parallel to the kagome plane has been measured for the x = 1 sample. A small, temperature-dependent anisotropy has been observed, where chi z / chip > 1 at high temperatures and chiz / chip < 1 at low temperatures. Fits of the high-temperature data to a Curie-Weiss model also reveal anisotropies for thetacw's and g-factors. By comparing with theoretical calculations, the presence of a small easy-axis exchange anisotropy can be deduced as a primary perturbation to the dominant Heisenberg nearest neighbor interaction. These results have great bearing on the interpretation of theoretical calculations based on the kagome Heisenberg antiferromagnet model to the experiments on ZnCu3(OH) 6Cl2. Specific heat measurements down to dilution temperatures and under strong applied magnetic fields show a superlinear temperature dependence with a finite linear term. Most importantly, we present neutron scattering measurements of the spin excitations on a large deuterated single crystal sample of herbertsmithite. Our observation of a spinon continuum in a two-dimensional magnet is unprecedented. The sresults serve as a a key fingerprint of the quantum spin liquid state in herbertsmithite. (Copies available exclusively from MIT Libraries, libraries.mit.edu/docs - docs mit.edu)

A High-Q AFM Sensor Using a Balanced Trolling Quartz Tuning Fork in the Liquid

PubMed Central

Li, Yingzi; Song, Zihang; Lin, Rui; Chen, Yifu; Qian, Jianqiang

2018-01-01

A quartz tuning fork (QTF) has been widely used as a force sensor of the frequency modulation atomic force microscope due to its ultrahigh stiffness, high quality factor and self-sensing nature. However, due to the bulky structure and exposed surface electrode arrangement, its application is limited, especially in liquid imaging of in situ biological samples, ionic liquids, electrochemical reaction, etc. Although the complication can be resolved by coating insulating materials on the QTF surface and then immersing the whole QTF into the liquid, it would result in a sharp drop of the quality factor, which will reduce the sensitivity of the QTF. To solve the problem, a novel method, called the balanced trolling quartz tuning fork (BT-QTF), is introduced here. In this method, two same probes are glued on both prongs of the QTF separately while only one probe immersed in the liquid. With the method, the hydrodynamic interaction can be reduced, thus the BT-QTF can retain a high quality factor and constant resonance frequency. The stable small vibration of the BT-QTF can be achieved in the liquid. Initially, a theoretical model is presented to analyze the sensing performance of the BT-QTF in the liquid. Then, the sensing performance analysis experiments of the BT-QTF have been performed. At last, the proposed method is applied to atomic force microscope imaging different samples in the liquid, which proves its feasibility. PMID:29783740

Rapid and sensitive analysis of 27 underivatized free amino acids, dipeptides, and tripeptides in fruits of Siraitia grosvenorii Swingle using HILIC-UHPLC-QTRAP(®)/MS (2) combined with chemometrics methods.

PubMed

Zhou, Guisheng; Wang, Mengyue; Li, Yang; Peng, Ying; Li, Xiaobo

2015-08-01

In the present study, a new strategy based on chemical analysis and chemometrics methods was proposed for the comprehensive analysis and profiling of underivatized free amino acids (FAAs) and small peptides among various Luo-Han-Guo (LHG) samples. Firstly, the ultrasound-assisted extraction (UAE) parameters were optimized using Plackett-Burman (PB) screening and Box-Behnken designs (BBD), and the following optimal UAE conditions were obtained: ultrasound power of 280 W, extraction time of 43 min, and the solid-liquid ratio of 302 mL/g. Secondly, a rapid and sensitive analytical method was developed for simultaneous quantification of 24 FAAs and 3 active small peptides in LHG at trace levels using hydrophilic interaction ultra-performance liquid chromatography coupled with triple-quadrupole linear ion-trap tandem mass spectrometry (HILIC-UHPLC-QTRAP(®)/MS(2)). The analytical method was validated by matrix effects, linearity, LODs, LOQs, precision, repeatability, stability, and recovery. Thirdly, the proposed optimal UAE conditions and analytical methods were applied to measurement of LHG samples. It was shown that LHG was rich in essential amino acids, which were beneficial nutrient substances for human health. Finally, based on the contents of the 27 analytes, the chemometrics methods of unsupervised principal component analysis (PCA) and supervised counter propagation artificial neural network (CP-ANN) were applied to differentiate and classify the 40 batches of LHG samples from different cultivated forms, regions, and varieties. As a result, these samples were mainly clustered into three clusters, which illustrated the cultivating disparity among the samples. In summary, the presented strategy had potential for the investigation of edible plants and agricultural products containing FAAs and small peptides.

Liquid microjunction surface sampling of acetaminophen, terfenadine and their metabolites in thin tissue sections

DOE PAGES

Kertesz, Vilmos; Paranthaman, Nithya; Moench, Paul; ...

2014-10-01

The aim of this paper was to evaluate the analytical performance of a fully automated droplet-based surface-sampling system for determining the distribution of the drugs acetaminophen and terfenadine, and their metabolites, in rat thin tissue sections. The following are the results: The rank order of acetaminophen concentration observed in tissues was stomach > small intestine > liver, while the concentrations of its glucuronide and sulfate metabolites were greatest in the liver and small intestine. Terfenadine was most concentrated in the liver and kidney, while its major metabolite, fexofenadine, was found in the liver and small intestine. In conclusion, the spatialmore » distributions of both drugs and their respective metabolites observed in this work were consistent with previous studies using radiolabeled drugs.« less

Sensitive analysis of steroid estrogens and bisphenol a in small volumes of water using isotope-dilution ultra-performance liquid chromatography-tandem mass spectrometry.

PubMed

Chang, Hong; Shen, Xiaoyan; Shao, Bing; Wu, Fengchang

2018-04-01

An isotope-dilution ultra-performance liquid chromatography-electrospray tandem mass spectrometry method combined with dansylation was established to sensitively quantify four steroid estrogens (estrone, 17α-estradiol, 17β-estradiol and 17α-ethynylestradiol) and bisphenol A in sewage influent and effluent. A simple hexane extraction was performed from a small volume (10 mL), followed by dansyl chloride derivatization and purification with a silica cartridge. The method effectively reduced the matrix effects in sample extract and permitted the selective and sensitive determination of target compounds from complicated matrices. The detection limits of the method for steroid estrogens were 0.20-0.90 ng L -1 in influent and 0.10-0.20 ng L -1 in effluent samples. For bisphenol A, the limits detection of the method were 20 and 0.80 for influent and effluent samples, respectively. Recoveries of 85%-96% were observed in all matrices. The method was applied to analyze residual estrogens and bisphenol A in sewage influent and effluent samples from Beijing, China. The concentrations of bisphenol A (636-1200 ng L -1 ) were up to 250 times higher than those of steroid estrogens. Estrone was the dominant estrogen in influent and effluent samples, while similar concentrations of 17α-estradiol and 17β-estradiol were detected in all samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

Sample mounts for microcrystal crystallography

NASA Technical Reports Server (NTRS)

Thorne, Robert E. (Inventor); Kmetko, Jan (Inventor); Stum, Zachary (Inventor); O'Neill, Kevin (Inventor)

2007-01-01

Sample mounts (10) for mounting microcrystals of biological macromolecules for X-ray crystallography are prepared by using patterned thin polyimide films (12) that have curvature imparted thereto, for example, by being attached to a curved outer surface of a small metal rod (16). The patterned film (12) preferably includes a tapered tip end (24) for holding a crystal. Preferably, a small sample aperture is disposed in the film for reception of the crystal. A second, larger aperture can also be provided that is connected to the sample aperture by a drainage channel, allowing removal of excess liquid and easier manipulation in viscous solutions. The curvature imparted to the film (12) increases the film's rigidity and allows a convenient scoop-like action for retrieving crystals. The polyimide contributes minimally to background and absorption, and can be treated to obtain desired hydrophobicity or hydrophilicity.

Sample mounts for microcrystal crystallography

NASA Technical Reports Server (NTRS)

O'Neill, Kevin (Inventor); Kmetko, Jan (Inventor); Thorne, Robert E. (Inventor); Stum, Zachary (Inventor)

2009-01-01

Sample mounts (10) for mounting microcrystals of biological macromolecules for X-ray crystallography are prepared by using patterned thin polyimide films (12) that have curvature imparted thereto, for example, by being attached to a curved outer surface of a small metal rod (16). The patterned film (12) preferably includes a tip end (24) for holding a crystal. Preferably, a small sample aperture is disposed in the film for reception of the crystal. A second, larger aperture can also be provided that is connected to the sample aperture by a drainage channel, allowing removal of excess liquid and easier manipulation in viscous solutions. The curvature imparted to the film (12) increases the film's rigidity and allows a convenient scoop-like action for retrieving crystals. The polyimide contributes minimally to background and absorption, and can be treated to obtain desired hydrophobicity or hydrophilicity.

Comprehensive quantitative analysis of Chinese patent drug YinHuang drop pill by ultra high-performance liquid chromatography quadrupole time of flight mass spectrometry.

PubMed

Wong, Tin-Long; An, Ya-Qi; Yan, Bing-Chao; Yue, Rui-Qi; Zhang, Tian-Bo; Ho, Hing-Man; Ren, Tian-Jing; Fung, Hau-Yee; Ma, Dik-Lung; Leung, Chung-Hang; Liu, Zhong-Liang; Pu, Jian-Xin; Han, Quan-Bin; Sun, Han-Dong

2016-06-05

YinHuang drop pill (YHDP) is a new preparation, derived from the traditional YinHuang (YH) decoction. Since drop pills are one of the newly developed forms of Chinese patent drugs, not much research has been done regarding the quality and efficacy. This study aims to establish a comprehensive quantitative analysis of the chemical profile of YHDP. ultra high-performance liquid chromatography quadrupole time of flight mass spectrometry (UHPLC-Q-TOF-MS/MS) was used to identify 34 non-sugar small molecules including 15 flavonoids, 9 phenolic acids, 5 saponins, 1 iridoid, and 4 iridoid glycosides in YHDP samples, and 26 of them were quantitatively determined. Sugar composition of YHDP in terms of fructose, glucose and sucrose was examined via a high performance liquid chromatography-evaporative light scattering detector on an amide column (HPLC-NH2P-ELSD). Macromolecules were examined by high performance gel permeation chromatography coupled with ELSD (HPGPC-ELSD). The content of the drop pill's skeleton component PEG-4000 was also quantified via ultra-high performance liquid chromatography coupled with charged aerosol detector (UHPLC-CAD). The results showed that up to 73% (w/w) of YHDP could be quantitatively determined. Small molecules accounted for approximately 5%, PEG-4000 represented 68%, while no sugars or macromolecules were found. Furthermore, YHDP showed no significant differences in terms of daily dosage, compared to YinHuang granules and YinHuang oral liquid; however, it has a higher small molecules content compared to YinHuang lozenge. Copyright © 2016 Elsevier B.V. All rights reserved.

Development of a novel ultrasound-assisted headspace liquid-phase microextraction and its application to the analysis of chlorophenols in real aqueous samples.

PubMed

Xu, Hui; Liao, Ying; Yao, Jinrong

2007-10-05

A new sample pretreatment technique, ultrasound-assisted headspace liquid-phase microextraction was developed as mentioned in this paper. In the technique, the volatile analytes were headspace extracted into a small drop of solvent, which suspended on the bottom of a cone-shaped PCR tube instead of the needle tip of a microsyringe. More solvent could be suspended in the PCR tube than microsyringe due to the larger interfacial tension, thus the analysis sensitivity was significantly improved with the increase of the extractant volume. Moreover, ultrasound-assisted extraction and independent controlling temperature of the extractant and the sample were performed to enhance the extraction efficiency. Following the extraction, the solvent-loaded sample was analyzed by high-performance liquid chromatography. Chlorophenols (2-chlorophenol, 2,4-dichlorophenol and 2,6-dichlorophenol) were chosen as model analytes to investigate the feasibility of the method. The experimental conditions related to the extraction efficiency were systematically studied. Under the optimum experimental conditions, the detection limit (S/N=3), intra- and inter-day RSD were 6 ng mL(-1), 4.6%, 3.9% for 2-chlorophenol, 12 ng mL(-1), 2.4%, 8.8% for 2,4-dichlorophenol and 23 ng mL(-1), 3.3%, 5.3% for 2,6-dichlorophenol, respectively. The proposed method was successfully applied to determine chlorophenols in real aqueous samples. Good recoveries ranging from 84.6% to 100.7% were obtained. In addition, the extraction efficiency of our method and the conventional headspace liquid-phase microextraction were compared; the extraction efficiency of the former was about 21 times higher than that of the latter. The results demonstrated that the proposed method is a promising sample pretreatment approach, its advantages over the conventional headspace liquid-phase microextraction include simple setup, ease of operation, rapidness, sensitivity, precision and no cross-contamination. The method is very suitable for the analysis of trace volatile and semivolatile pollutants in real aqueous sample.

A simple high-performance liquid chromatography for the determination of linezolid in human plasma and saliva.

PubMed

Hara, Shuuji; Uchiyama, Masanobu; Yoshinari, Masami; Matsumoto, Taichi; Jimi, Shiro; Togawa, Atsushi; Takata, Tohru; Takamatsu, Yasushi

2015-09-01

Linezolid is an antimicrobial agent for the treatment of multiresistant Gram-positive infections. A practical high-performance liquid chromatography method was developed for the determination of linezolid in human plasma and saliva. Linezolid and an internal standard (o-ethoxybenzamide) were extracted from plasma and saliva with ethyl acetate and analyzed on a Capcell Pak C18 MG column with UV detection at 254 nm. The calibration curve was linear through the range 0.5-50 µg/mL using a 200 μL sample volume. The intra- and interday precisions were all <6.44% for plasma and 5.60% for saliva. The accuracies ranged from 98.8 to 110% for both matrices. The mean recoveries of linezolid were 80.8% for plasma and 79.0% for saliva. This method was used to determine the plasma and saliva concentrations of linezolid in healthy volunteers who were orally administered a 600 mg dose of linezolid. Our liquid-liquid extraction procedure is easy and requires a small volume of plasma or saliva (200 μL). This small volume can be advantageous in clinical pharmacokinetic studies, especially if children participate. Copyright © 2015 John Wiley & Sons, Ltd.

Binary Solvents Dispersive Liquid—Liquid Microextraction (BS-DLLME) Method for Determination of Tramadol in Urine Using High-Performance Liquid Chromatography

PubMed Central

2014-01-01

Background Tramadol is an opioid, synthetic analog of codeine and has been used for the treatment of acute or chronic pain may be abused. In this work, a developed Dispersive liquid liquid microextraction (DLLME) as binary solvents-based dispersive liquid-liquid microextraction (BS-DLLME) combined with high performance liquid chromatography (HPLC) with fluorescence detection (FD) was employed for determination of tramadol in the urine samples. This procedure involves the use of an appropriate mixture of binary extraction solvents (70 μL CHCl3 and 30 μL ethyl acetate) and disperser solvent (600 μL acetone) for the formation of cloudy solution in 5 ml urine sample comprising tramadol and NaCl (7.5%, w/v). After centrifuging, the small droplets of extraction solvents were precipitated. In the final step, the HPLC with fluorescence detection was used for determination of tramadol in the precipitated phase. Results Various factors on the efficiency of the proposed procedure were investigated and optimized. The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 μg/L, respectively. The relative standard deviations (RSD) for the extraction of 30 μg L of tramadol was found 4.1% (n = 6). The relative recoveries of tramadol from urine samples at spiking levels of 10, 30 and 60 μg/L were in the range of 95.6 – 99.6%. Conclusions Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories. PMID:24495475

Incorporation of ionic liquid into porous polymer monoliths to enhance the separation of small molecules in reversed-phase high-performance liquid chromatography.

PubMed

Wang, Jiafei; Bai, Ligai; Wei, Zhen; Qin, Junxiao; Ma, Yamin; Liu, Haiyan

2015-06-01

An ionic liquid was incorporated into the porous polymer monoliths to afford stationary phases with enhanced chromatographic performance for small molecules in reversed-phase high-performance liquid chromatography. The effect of the ionic liquid in the polymerization mixture on the performance of the monoliths was studied in detail. While monoliths without ionic liquid exhibited poor resolution and low efficiency, the addition of ionic liquid to the polymerization mixture provides highly increased resolution and high efficiency. The chromatographic performances of the monoliths were demonstrated by the separations of various small molecules including aromatic hydrocarbons, isomers, and homologues using a binary polar mobile phase. The present column efficiency reached 27 000 plates/m, which showed that the ionic liquid monoliths are alternative stationary phases in the separation of small molecules by high-performance liquid chromatography. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A rapid high-performance liquid-chromatographic method for simultaneously determining the concentrations of TFM and Bayer 73 in water during lampricide treatments

USGS Publications Warehouse

Dawson, V.K.

1982-01-01

The high-performance liquid-chromatography (HPLC) procedure requires only minutes per sample, is specific, and is relatively sensitive (limit of detection 18 disposable cartridge. The cartridge adsorbs and retains both the lampricides and the internal standard. The quantitative elution of the three chemicals from the cartridge with a small volume of methanol effectively concentrates the sample and provides sample cleanup. The methanol extract is then analyzed directly by HPLC on an MCH 10 reverse phase column by using a methanol:0.01 mol/L acetate buffer (87:13, v:v) as the mobile phase at 2 mL/min and detected by ultraviolet spectrophotometry at 330 (or 254) nm. A microprocessor data system further facilitates the procedure by quantifying off-scale peaks and yielding results directly in units of concentration (mg/L).

Rapid sample classification using an open port sampling interface coupled with liquid introduction atmospheric pressure ionization mass spectrometry

DOE PAGES

Van Berkel, Gary J.; Kertesz, Vilmos

2016-11-15

An “Open Access”-like mass spectrometric platform to fully utilize the simplicity of the manual open port sampling interface for rapid characterization of unprocessed samples by liquid introduction atmospheric pressure ionization mass spectrometry has been lacking. The in-house developed integrated software with a simple, small and relatively low-cost mass spectrometry system introduced here fills this void. Software was developed to operate the mass spectrometer, to collect and process mass spectrometric data files, to build a database and to classify samples using such a database. These tasks were accomplished via the vendorprovided software libraries. Sample classification based on spectral comparison utilized themore » spectral contrast angle method. As a result, using the developed software platform near real-time sample classification is exemplified using a series of commercially available blue ink rollerball pens and vegetable oils. In the case of the inks, full scan positive and negative ion ESI mass spectra were both used for database generation and sample classification. For the vegetable oils, full scan positive ion mode APCI mass spectra were recorded. The overall accuracy of the employed spectral contrast angle statistical model was 95.3% and 98% in case of the inks and oils, respectively, using leave-one-out cross-validation. In conclusion, this work illustrates that an open port sampling interface/mass spectrometer combination, with appropriate instrument control and data processing software, is a viable direct liquid extraction sampling and analysis system suitable for the non-expert user and near real-time sample classification via database matching.« less

Rapid sample classification using an open port sampling interface coupled with liquid introduction atmospheric pressure ionization mass spectrometry

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

Van Berkel, Gary J.; Kertesz, Vilmos

An “Open Access”-like mass spectrometric platform to fully utilize the simplicity of the manual open port sampling interface for rapid characterization of unprocessed samples by liquid introduction atmospheric pressure ionization mass spectrometry has been lacking. The in-house developed integrated software with a simple, small and relatively low-cost mass spectrometry system introduced here fills this void. Software was developed to operate the mass spectrometer, to collect and process mass spectrometric data files, to build a database and to classify samples using such a database. These tasks were accomplished via the vendorprovided software libraries. Sample classification based on spectral comparison utilized themore » spectral contrast angle method. As a result, using the developed software platform near real-time sample classification is exemplified using a series of commercially available blue ink rollerball pens and vegetable oils. In the case of the inks, full scan positive and negative ion ESI mass spectra were both used for database generation and sample classification. For the vegetable oils, full scan positive ion mode APCI mass spectra were recorded. The overall accuracy of the employed spectral contrast angle statistical model was 95.3% and 98% in case of the inks and oils, respectively, using leave-one-out cross-validation. In conclusion, this work illustrates that an open port sampling interface/mass spectrometer combination, with appropriate instrument control and data processing software, is a viable direct liquid extraction sampling and analysis system suitable for the non-expert user and near real-time sample classification via database matching.« less

Electron paramagnetic resonance study of alinement induced by magnetic fields in two smectic-A liquid crystals not exhibiting nematic phases

NASA Technical Reports Server (NTRS)

Fryburg, G. C.; Gelerinter, E.

1972-01-01

Using vanadyl acetylacetonate (VAAC) as a paramagnetic probe, the molecular ordering in two smectic-A liquid crystals that do not display nematic phases were studied. Reproducible alinement was attained by slow cooling throughout the isotropic smectic-A transition in dc magnetic fields of 1.1 and 2.15 teslas. The degree of order attained is small for a smectic-A liquid crystal. Measurements were made of the variation of the average hyperfine splitting of the alined samples as a function of orientation relative to the dc magnetic field of the spectrometer. This functional dependence is in agreement with the theoretical prediction except where the viscosity of the liquid crystal becomes large enough to slow the tumbling of the VAAC, as indicated by asymmetry in the end lines of the spectrum.

Preparation of well-controlled three-dimensional skeletal hybrid monoliths via thiol-epoxy click polymerization for highly efficient separation of small molecules in capillary liquid chromatography.

PubMed

Lin, Hui; Chen, Lianfang; Ou, Junjie; Liu, Zhongshan; Wang, Hongwei; Dong, Jing; Zou, Hanfa

2015-10-16

Two kinds of hybrid monoliths were first prepared via thiol-epoxy click polymerization using a multi-epoxy monomer, octaglycidyldimethylsilyl POSS (POSS-epoxy), and two multi-thiols, trimethylolpropanetris(3-mercaptopropionate) (TPTM) and pentaerythritoltetrakis(3-mercaptopropionate) (PTM), respectively, as the precursors. The resulting two hybrid monoliths (assigned as POSS-epoxy-TPTM and POSS-epoxy-PTM) not only possessed high thermal, mechanical and chemical stabilities, but also exhibited well-controlled 3D skeletal microstructure and high efficiency in capillary liquid chromatography (cLC) separation of small molecules. The highest column efficiency reached 182,700N/m (for butylbenzene) on the monolith POSS-epoxy-PTM at the velocity of 0.75mm/s. Furthermore, the hybrid monolith POSS-epoxy-PTM was successfully applied for cLC separations of various samples, not only standard compounds such as alkylbenzenes, PAHs, phenols and dipeptides, as well as intact proteins, but also complex samples of EPA 610 and BSA digest. Copyright © 2015 Elsevier B.V. All rights reserved.

Micro Linear Pump with Electromagnetic Actuator

NASA Astrophysics Data System (ADS)

Suzumori, Koichi; Furusawa, Hiroaki; Kanda, Takefumi; Yamada, Yoshiaki; Nagata, Takashi

In recent years, research and development of the micro-fluid systems have been activated in the field of chemical technology and biotechnology. Micro-fluid systems are realized by micromachine technology and MEMS technology. Micro pump is an essential element for miniaturization of chemical analysis reaction systems. The aim of this research is development of a micro linear pump which will be built into micro-fluid systems. This pump aims to take a sample of very-small-quantity of liquids. Taking a sample of very-small-quantity of liquids reduce the amount used and waste fluid of a reagent. Full length and diameter of this pump are 32.5mm and 6mm respectively. The features of this pump are (1) the pump is built with actuator, (2) the gap of 7μm between piston and cylinder is achieved through fine machining process, and (3) micro check-valves of 2mm diameter made of stainless-steel film are fabricated and integrated. In this paper, the structure and the characteristics of this pump were shown. And the characteristics after improvement of micro check-valves were shown.

Quantitative evaluation of analyte transport on microfluidic paper-based analytical devices (μPADs).

PubMed

Ota, Riki; Yamada, Kentaro; Suzuki, Koji; Citterio, Daniel

2018-02-07

The transport efficiency during capillary flow-driven sample transport on microfluidic paper-based analytical devices (μPADs) made from filter paper has been investigated for a selection of model analytes (Ni 2+ , Zn 2+ , Cu 2+ , PO 4 3- , bovine serum albumin, sulforhodamine B, amaranth) representing metal cations, complex anions, proteins and anionic molecules. For the first time, the transport of the analytical target compounds rather than the sample liquid, has been quantitatively evaluated by means of colorimetry and absorption spectrometry-based methods. The experiments have revealed that small paperfluidic channel dimensions, additional user operation steps (e.g. control of sample volume, sample dilution, washing step) as well as the introduction of sample liquid wicking areas allow to increase analyte transport efficiency. It is also shown that the interaction of analytes with the negatively charged cellulosic paper substrate surface is strongly influenced by the physico-chemical properties of the model analyte and can in some cases (Cu 2+ ) result in nearly complete analyte depletion during sample transport. The quantitative information gained through these experiments is expected to contribute to the development of more sensitive μPADs.

Preventive doping control screening analysis of prohibited substances in human urine using rapid-resolution liquid chromatography/high-resolution time-of-flight mass spectrometry.

PubMed

Vonaparti, A; Lyris, E; Angelis, Y S; Panderi, I; Koupparis, M; Tsantili-Kakoulidou, A; Peters, R J B; Nielen, M W F; Georgakopoulos, C

2010-06-15

Unification of the screening protocols for a wide range of doping agents has become an important issue for doping control laboratories. This study presents the development and validation of a generic liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) screening method of 241 small molecule analytes from various categories of prohibited substances (stimulants, narcotics, diuretics, beta(2)-agonists, beta-blockers, hormone antagonists and modulators, glucocorticosteroids and anabolic agents). It is based on a single-step liquid-liquid extraction of hydrolyzed urine and the use of a rapid-resolution liquid chromatography/high-resolution time-of-flight mass spectrometric system acquiring continuous full scan data. Electrospray ionization in the positive mode was used. Validation parameters consisted of identification capability, limit of detection, specificity, ion suppression, extraction recovery, repeatability and mass accuracy. Detection criteria were established on the basis of retention time reproducibility and mass accuracy. The suitability of the methodology for doping control was demonstrated with positive urine samples. The preventive role of the method was proved by the case where full scan acquisition with accurate mass measurement allowed the retrospective reprocessing of acquired data from past doping control samples for the detection of a designer drug, the stimulant 4-methyl-2-hexanamine, which resulted in re-reporting a number of stored samples as positives for this particular substance, when, initially, they had been reported as negatives. Copyright (c) 2010 John Wiley & Sons, Ltd.

Improved 3-omega measurement of thermal conductivity in liquid, gases, and powders using a metal-coated optical fiber.

PubMed

Schiffres, Scott N; Malen, Jonathan A

2011-06-01

A novel 3ω thermal conductivity measurement technique called metal-coated 3ω is introduced for use with liquids, gases, powders, and aerogels. This technique employs a micron-scale metal-coated glass fiber as a heater/thermometer that is suspended within the sample. Metal-coated 3ω exceeds alternate 3ω based fluid sensing techniques in a number of key metrics enabling rapid measurements of small samples of materials with very low thermal effusivity (gases), using smaller temperature oscillations with lower parasitic conduction losses. Its advantages relative to existing fluid measurement techniques, including transient hot-wire, steady-state methods, and solid-wire 3ω are discussed. A generalized n-layer concentric cylindrical periodic heating solution that accounts for thermal boundary resistance is presented. Improved sensitivity to boundary conductance is recognized through this model. Metal-coated 3ω was successfully validated through a benchmark study of gases and liquids spanning two-orders of magnitude in thermal conductivity. © 2011 American Institute of Physics

48 CFR 19.705-7 - Liquidated damages.

Code of Federal Regulations, 2014 CFR

2014-10-01

... SOCIOECONOMIC PROGRAMS SMALL BUSINESS PROGRAMS The Small Business Subcontracting Program 19.705-7 Liquidated damages. (a) Maximum practicable utilization of small business, veteran-owned small business, service-disabled veteran-owned small business, HUBZone small business, small disadvantaged business and women-owned...

48 CFR 19.705-7 - Liquidated damages.

Code of Federal Regulations, 2011 CFR

2011-10-01

... SOCIOECONOMIC PROGRAMS SMALL BUSINESS PROGRAMS The Small Business Subcontracting Program 19.705-7 Liquidated damages. (a) Maximum practicable utilization of small business, veteran-owned small business, service-disabled veteran-owned small business, HUBZone small business, small disadvantaged business and women-owned...

48 CFR 19.705-7 - Liquidated damages.

Code of Federal Regulations, 2010 CFR

2010-10-01

... SOCIOECONOMIC PROGRAMS SMALL BUSINESS PROGRAMS The Small Business Subcontracting Program 19.705-7 Liquidated damages. (a) Maximum practicable utilization of small business, veteran-owned small business, service-disabled veteran-owned small business, HUBZone small business, small disadvantaged business and women-owned...

48 CFR 19.705-7 - Liquidated damages.

Code of Federal Regulations, 2012 CFR

2012-10-01

... SOCIOECONOMIC PROGRAMS SMALL BUSINESS PROGRAMS The Small Business Subcontracting Program 19.705-7 Liquidated damages. (a) Maximum practicable utilization of small business, veteran-owned small business, service-disabled veteran-owned small business, HUBZone small business, small disadvantaged business and women-owned...

Externally pressurized porous cylinder for multiple surface aerosol generation and method of generation

DOEpatents

Apel, Charles T.; Layman, Lawrence R.; Gallimore, David L.

1988-01-01

A nebulizer for generating aerosol having small droplet sizes and high efficiency at low sample introduction rates. The nebulizer has a cylindrical gas permeable active surface. A sleeve is disposed around the cylinder and gas is provided from the sleeve to the interior of the cylinder formed by the active surface. In operation, a liquid is provided to the inside of the gas permeable surface. The gas contacts the wetted surface and forms small bubbles which burst to form an aerosol. Those bubbles which are large are carried by momentum to another part of the cylinder where they are renebulized. This process continues until the entire sample is nebulized into aerosol sized droplets.

The composition of liquid atmospheric pressure matrix-assisted laser desorption/ionization matrices and its effect on ionization in mass spectrometry.

PubMed

Ryumin, Pavel; Cramer, Rainer

2018-07-12

New liquid atmospheric pressure (AP) matrix-assisted laser desorption/ionization (MALDI) matrices that produce predominantly multiply charged ions have been developed and evaluated with respect to their performance for peptide and protein analysis by mass spectrometry (MS). Both the chromophore and the viscous support liquid in these matrices were optimized for highest MS signal intensity, S/N values and maximum charge state. The best performance in both protein and peptide analysis was achieved employing light diols as matrix support liquids (e.g. ethylene glycol and propylene glycol). Investigating the influence of the chromophore, it was found that 2,5-dihydroxybenzoic acid resulted in a higher analyte ion signal intensity for the analysis of small peptides; however, larger molecules (>17 kDa) were undetectable. For larger molecules, a sample preparation based on α-cyano-4-hydroxycinnammic acid as the chromophore was developed and multiply protonated analytes with charge states of more than 50 were detected. Thus, for the first time it was possible to detect with MALDI MS proteins as large as ∼80 kDa with a high number of charge states, i.e. m/z values below 2000. Systematic investigations of various matrix support liquids have revealed a linear dependency between laser threshold energy and surface tension of the liquid MALDI sample. Copyright © 2018 Elsevier B.V. All rights reserved.

Heat capacity measurements of sub-nanoliter volumes of liquids using bimaterial microchannel cantilevers

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

Khan, M. F.; Miriyala, N.; Hassanpourfard, M.

Lab-on-a-Chip compatible techniques for thermal characterization of miniaturized volumes of liquid analytes are necessary in applications such as protein blotting, DNA melting, and drug development, where samples are either rare or volume-limited. We developed a closed-chamber calorimeter based on a bimaterial microchannel cantilever (BMC) for sub-nanoliter level thermal analysis. When the liquid-filled BMC is irradiated with infrared (IR) light at a specific wavelength, the IR absorption by the liquid analyte results in localized heat generation and the subsequent deflection of the BMC, due to a thermal expansion mismatch between the constituent materials. The time constant of the deflection, which ismore » dependent upon the heat capacity of the liquid analyte, can be directly measured by recording the time-dependent bending of the BMC. We have used the BMC to quantitatively measure the heat capacity of five volatile organic compounds. With a deflection noise level of ∼10 nm and a signal-to-noise ratio of 68:1, the BMC offers a sensitivity of 30.5 ms/(J g{sup −1 }K{sup −1}) and a resolution of 23 mJ/(g K) for ∼150 pl liquid for heat capacity measurements. This technique can be used for small-scale thermal characterization of different chemical and biological samples.« less

Sensitive trace enrichment of environmental andiandrogen vinclozolin from natural waters and sediment samples using hollow-fiber liquid-phase microextraction.

PubMed

Lambropoulou, Dimitra A; Albanis, Triantafyllos A

2004-12-17

The presence of vinclozolin in the environment as far as the endocrine disruption effects in biota are concerned has raised interest in the environmental fate of this compound. In this respect, the present study attempts to investigate the feasibility of applying a novel quantitative method, liquid-phase microextraction (LPME), so as to determine this environmental andiandrogen in environmental samples such as water and sediment samples. The technique involved the use of a small amount (3 microL) of organic solvent impregnated in a hollow fiber membrane, which was attached to the needle of a conventional GC syringe. The extracted samples were analyzed by gas chromatography coupled with electron-capture detection. Experimental LPME conditions such as extraction solvent, stirring rate, content of NaCl and pH were tested. Once LPME was optimized, the performance of the proposed technique was evaluated for the determination of vinclozolin in different types of natural water samples. The recovery of spiked water samples was from 80 to 99%. The procedure was adequate for quantification of vinclozolin in waters at levels of 0.010 to 50 microg/L (r> 0.994) with a detection limit of 0.001 microg/L (S/N= 3). Natural sediment samples from the Aliakmonas River area (Macedonia, Greece) spiked with the target andiandrogen compound were liquid-liquid extracted and analyzed by the methodology developed in this work. No significant interferences from the samples matrix were noticed, indicating that the reported methodology is an innovative tactic for sample preparation in sediment analysis, with a considerable improvement in the achieved detection limits. The results demonstrated that apart from analyte enrichment, the proposed LPME procedure also serves as clean-up method and could be successfully performed to determine trace amounts of vinclozolin in water and sediment samples.

AFM fluid delivery/liquid extraction surface sampling/electrostatic spray cantilever probe

DOEpatents

Van Berkel, Gary J.

2015-06-23

An electrospray system comprises a liquid extraction surface sampling probe. The probe comprises a probe body having a liquid inlet and a liquid outlet, and having a liquid extraction tip. A solvent delivery conduit is provided for receiving solvent liquid from the liquid inlet and delivering the solvent liquid to the liquid extraction tip. An open liquid extraction channel extends across an exterior surface of the probe body from the liquid extraction tip to the liquid outlet. An electrospray emitter tip is in liquid communication with the liquid outlet of the liquid extraction surface sampling probe. A system for analyzing samples, a liquid junction surface sampling system, and a method of analyzing samples are also disclosed.

A Liquid-Handling Robot for Automated Attachment of Biomolecules to Microbeads.

PubMed

Enten, Aaron; Yang, Yujia; Ye, Zihan; Chu, Ryan; Van, Tam; Rothschild, Ben; Gonzalez, Francisco; Sulchek, Todd

2016-08-01

Diagnostics, drug delivery, and other biomedical industries rely on cross-linking ligands to microbead surfaces. Microbead functionalization requires multiple steps of liquid exchange, incubation, and mixing, which are laborious and time intensive. Although automated systems exist, they are expensive and cumbersome, limiting their routine use in biomedical laboratories. We present a small, bench-top robotic system that automates microparticle functionalization and streamlines sample preparation. The robot uses a programmable microcontroller to regulate liquid exchange, incubation, and mixing functions. Filters with a pore diameter smaller than the minimum bead diameter are used to prevent bead loss during liquid exchange. The robot uses three liquid reagents and processes up to 10(7) microbeads per batch. The effectiveness of microbead functionalization was compared with a manual covalent coupling process and evaluated via flow cytometry and fluorescent imaging. The mean percentages of successfully functionalized beads were 91% and 92% for the robot and manual methods, respectively, with less than 5% bead loss. Although the two methods share similar qualities, the automated approach required approximately 10 min of active labor, compared with 3 h for the manual approach. These results suggest that a low-cost, automated microbead functionalization system can streamline sample preparation with minimal operator intervention. © 2015 Society for Laboratory Automation and Screening.

DREAMing: a simple and ultrasensitive method for assessing intratumor epigenetic heterogeneity directly from liquid biopsies

PubMed Central

Pisanic, Thomas R.; Athamanolap, Pornpat; Poh, Weijie; Chen, Chen; Hulbert, Alicia; Brock, Malcolm V.; Herman, James G.; Wang, Tza-Huei

2015-01-01

Many cancers comprise heterogeneous populations of cells at primary and metastatic sites throughout the body. The presence or emergence of distinct subclones with drug-resistant genetic and epigenetic phenotypes within these populations can greatly complicate therapeutic intervention. Liquid biopsies of peripheral blood from cancer patients have been suggested as an ideal means of sampling intratumor genetic and epigenetic heterogeneity for diagnostics, monitoring and therapeutic guidance. However, current molecular diagnostic and sequencing methods are not well suited to the routine assessment of epigenetic heterogeneity in difficult samples such as liquid biopsies that contain intrinsically low fractional concentrations of circulating tumor DNA (ctDNA) and rare epigenetic subclonal populations. Here we report an alternative approach, deemed DREAMing (Discrimination of Rare EpiAlleles by Melt), which uses semi-limiting dilution and precise melt curve analysis to distinguish and enumerate individual copies of epiallelic species at single-CpG-site resolution in fractions as low as 0.005%, providing facile and inexpensive ultrasensitive assessment of locus-specific epigenetic heterogeneity directly from liquid biopsies. The technique is demonstrated here for the evaluation of epigenetic heterogeneity at p14ARF and BRCA1 gene-promoter loci in liquid biopsies obtained from patients in association with non-small cell lung cancer (NSCLC) and myelodysplastic/myeloproliferative neoplasms (MDS/MPN), respectively. PMID:26304549

Liquid crystal-based Mueller matrix spectral imaging polarimetry for parameterizing mineral structural organization.

PubMed

Gladish, James C; Duncan, Donald D

2017-01-20

Herein, we discuss the remote assessment of the subwavelength organizational structure of a medium. Specifically, we use spectral imaging polarimetry, as the vector nature of polarized light enables it to interact with optical anisotropies within a medium, while the spectral aspect of polarization is sensitive to small-scale structure. The ability to image these effects allows for inference of spatial structural organization parameters. This work describes a methodology for revealing structural organization by exploiting the Stokes/Mueller formalism and by utilizing measurements from a spectral imaging polarimeter constructed from liquid crystal variable retarders and a liquid crystal tunable filter. We provide results to validate the system and then show results from measurements on a mineral sample.

Use of high-resolution mass spectrometry to investigate a metabolite interference during liquid chromatography/tandem mass spectrometric quantification of a small molecule in toxicokinetic study samples.

PubMed

Furlong, Michael; Bessire, Andrew; Song, Wei; Huntington, Christopher; Groeber, Elizabeth

2010-07-15

During routine liquid chromatography/tandem mass spectrometric (LC/MS/MS) bioanalysis of a small molecule analyte in rat serum samples from a toxicokinetic study, an unexpected interfering peak was observed in the extracted ion chromatogram of the internal standard. No interfering peaks were observed in the extracted ion chromatogram of the analyte. The dose-dependent peak area response and peak area response versus time profiles of the interfering peak suggested that it might have been related to a metabolite of the dosed compound. Further investigation using high-resolution mass spectrometry led to unequivocal identification of the interfering peak as an N-desmethyl metabolite of the parent analyte. High-resolution mass spectrometry (HRMS) was also used to demonstrate that the interfering response of the metabolite in the multiple reaction monitoring (MRM) channel of the internal standard was due to an isobaric relationship between the (13)C-isotope of the metabolite and the internal standard (i.e., common precursor ion mass), coupled with a metabolite product ion with identical mass to the product ion used in the MRM transition of the internal standard. These results emphasize (1) the need to carefully evaluate internal standard candidates with regard to potential interferences from metabolites during LC/MS/MS method development, validation and bioanalysis of small molecule analytes in biological matrices; (2) the value of HRMS as a tool to investigate unexpected interferences encountered during LC/MS/MS analysis of small molecules in biological matrices; and (3) the potential for interference regardless of choice of IS and therefore the importance of conducting assay robustness on incurred in vitro or in vivo study samples. Copyright 2010 John Wiley & Sons, Ltd.

Combination of acoustic levitation with small angle scattering techniques and synchrotron radiation circular dichroism. Application to the study of protein solutions.

PubMed

Cristiglio, Viviana; Grillo, Isabelle; Fomina, Margarita; Wien, Frank; Shalaev, Evgenyi; Novikov, Alexey; Brassamin, Séverine; Réfrégiers, Matthieu; Pérez, Javier; Hennet, Louis

2017-01-01

The acoustic levitation technique is a useful sample handling method for small solid and liquids samples, suspended in air by means of an ultrasonic field. This method was previously used at synchrotron sources for studying pharmaceutical liquids and protein solutions using x-ray diffraction and small angle x-ray scattering (SAXS). In this work we combined for the first time this containerless method with small angle neutron scattering (SANS) and synchrotron radiation circular dichroism (SRCD) to study the structural behavior of proteins in solutions during the water evaporation. SANS results are also compared with SAXS experiments. The aggregation behavior of 45μl droplets of lysozyme protein diluted in water was followed during the continuous increase of the sample concentration by evaporating the solvent. The evaporation kinetics was followed at different drying stage by SANS and SAXS with a good data quality. In a prospective work using SRCD, we also studied the evolution of the secondary structure of the myoglobin protein in water solution in the same evaporation conditions. Acoustic levitation was applied for the first time with SANS and the high performances of the used neutron instruments made it possible to monitor fast container-less reactions in situ. A preliminary work using SRCD shows the potentiality of its combination with acoustic levitation for studying the evolution of the protein structure with time. This multi-techniques approach could give novel insights into crystallization and self-assembly phenomena of biological compound with promising potential applications in pharmaceutical, food and cosmetics industry. This article is part of a Special Issue entitled "Science for Life" Guest Editor: Dr. Austen Angell, Dr. Salvatore Magazù and Dr. Federica Migliardo. Copyright © 2016 Elsevier B.V. All rights reserved.

Syringe needle-based sampling coupled with liquid-phase extraction for determination of the three-dimensional distribution of l-ascorbic acid in apples.

PubMed

Tang, Sheng; Lee, Hian Kee

2016-05-15

A novel syringe needle-based sampling approach coupled with liquid-phase extraction (NBS-LPE) was developed and applied to the extraction of l-ascorbic acid (AsA) in apple. In NBS-LPE, only a small amount of apple flesh (ca. 10mg) was sampled directly using a syringe needle and placed in a glass insert for liquid extraction of AsA by 80 μL oxalic acid-acetic acid. The extract was then directly analyzed by liquid chromatography. This new procedure is simple, convenient, almost organic solvent free, and causes far less damage to the fruit. To demonstrate the applicability of NBS-LPE, AsA levels at different sampling points in a single apple were determined to reveal the spatial distribution of the analyte in a three-dimensional model. The results also showed that this method had good sensitivity (limit of detection of 0.0097 mg/100g; limit of quantification of 0.0323 mg/100g), acceptable reproducibility (relative standard deviation of 5.01% (n=6)), a wide linear range of between 0.05 and 50mg/100g, and good linearity (r(2)=0.9921). This interesting extraction technique and modeling approach can be used to measure and monitor a wide range of compounds in various parts of different soft-matrix fruits and vegetables, including single specimens. Copyright © 2015 Elsevier Ltd. All rights reserved.

Segmental analysis of amphetamines in hair using a sensitive UHPLC-MS/MS method.

PubMed

Jakobsson, Gerd; Kronstrand, Robert

2014-06-01

A sensitive and robust ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated for quantification of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine and 3,4-methylenedioxy methamphetamine in hair samples. Segmented hair (10 mg) was incubated in 2M sodium hydroxide (80°C, 10 min) before liquid-liquid extraction with isooctane followed by centrifugation and evaporation of the organic phase to dryness. The residue was reconstituted in methanol:formate buffer pH 3 (20:80). The total run time was 4 min and after optimization of UHPLC-MS/MS-parameters validation included selectivity, matrix effects, recovery, process efficiency, calibration model and range, lower limit of quantification, precision and bias. The calibration curve ranged from 0.02 to 12.5 ng/mg, and the recovery was between 62 and 83%. During validation the bias was less than ±7% and the imprecision was less than 5% for all analytes. In routine analysis, fortified control samples demonstrated an imprecision <13% and control samples made from authentic hair demonstrated an imprecision <26%. The method was applied to samples from a controlled study of amphetamine intake as well as forensic hair samples previously analyzed with an ultra high performance liquid chromatography time of flight mass spectrometry (UHPLC-TOF-MS) screening method. The proposed method was suitable for quantification of these drugs in forensic cases including violent crimes, autopsy cases, drug testing and re-granting of driving licences. This study also demonstrated that if hair samples are divided into several short segments, the time point for intake of a small dose of amphetamine can be estimated, which might be useful when drug facilitated crimes are investigated. Copyright © 2014 John Wiley & Sons, Ltd.

Development of OSL system using two high-density blue LEDs equipped with liquid light guides

NASA Astrophysics Data System (ADS)

Choi, J. H.; Kim, M. J.; Cheong, C. S.; Hong, D. G.

2014-03-01

In recent years, considerable developments in optically stimulated luminescence (OSL) have been made in the fields of radiation dosimetry, age determination, and medical applications. A compact and economical OSL system comprising a precision x-y-z stage for loading 12 samples, a small X-ray generator for radiation dosing, and two powerful blue light emitting diodes (LEDs) for optical stimulation equipped with VIS liquid light guides (VIS-LLGs) has been developed. This paper describes the principal features of the system along with the examples of measurements performed by the system.

ICSH recommendations for assessing automated high-performance liquid chromatography and capillary electrophoresis equipment for the quantitation of HbA2.

PubMed

Stephens, A D; Colah, R; Fucharoen, S; Hoyer, J; Keren, D; McFarlane, A; Perrett, D; Wild, B J

2015-10-01

Automated high performance liquid chromatography and Capillary electrophoresis are used to quantitate the proportion of Hemoglobin A2 (HbA2 ) in blood samples order to enable screening and diagnosis of carriers of β-thalassemia. Since there is only a very small difference in HbA2 levels between people who are carriers and people who are not carriers such analyses need to be both precise and accurate. This paper examines the different parameters of such equipment and discusses how they should be assessed. © 2015 John Wiley & Sons Ltd.

Characterization of Extracellular Vesicles by Size-Exclusion High-Performance Liquid Chromatography (HPLC).

PubMed

Huang, Tao; He, Jiang

2017-01-01

Extracellular vesicles (EVs) have recently attracted substantial attention due to the potential diagnostic and therapeutic relevance. Although a variety of techniques have been used to isolate and analyze EVs, it is still far away from satisfaction. Size-exclusion chromatography (SEC), which separates subjects by size, has been widely applied in protein purification and analysis. The purpose of this chapter is to show the applications of size-exclusion high-performance liquid chromatography (HPLC) as methods for EV characterization of impurities or contaminants of small size, and thus for quality assay for the purity of the samples of EVs.

Liquid biopsy based biomarkers in non-small cell lung cancer for diagnosis and treatment monitoring.

PubMed

Pérez-Callejo, David; Romero, Atocha; Provencio, Mariano; Torrente, María

2016-10-01

Advances in the knowledge of the biology of non-small cell lung cancer (NSCLC) have revealed molecular information used for systemic cancer therapy targeting metastatic disease, with an important impact on patients overall survival (OS) and quality of life. However, a biopsy of overt metastases is an invasive procedure limited to certain locations and not easily acceptable in the clinic. Moreover, a single biopsy cannot reflect the clonal heterogeneity of the tumor. The analysis of peripheral blood samples of cancer patients represents a new source of cancer-derived material, known as liquid biopsy, and its components can be obtained from almost all body fluids. These components have shown to reflect characteristics of the status of both the primary and metastatic diseases, helping the clinicians to move towards a personalized medicine. The present review focuses on the liquid biopsy components: circulating tumor cells (CTCS), circulating free DNA (cfDNA), exosomes and tumor-educated platelets (TEP); the isolation technologies used and their potential use for non-invasive screening, early diagnosis, prognosis, response to treatment and real time monitoring of the disease, in NSCLC patients.

Liquid biopsy based biomarkers in non-small cell lung cancer for diagnosis and treatment monitoring

PubMed Central

Pérez-Callejo, David; Provencio, Mariano

2016-01-01

Advances in the knowledge of the biology of non-small cell lung cancer (NSCLC) have revealed molecular information used for systemic cancer therapy targeting metastatic disease, with an important impact on patients overall survival (OS) and quality of life. However, a biopsy of overt metastases is an invasive procedure limited to certain locations and not easily acceptable in the clinic. Moreover, a single biopsy cannot reflect the clonal heterogeneity of the tumor. The analysis of peripheral blood samples of cancer patients represents a new source of cancer-derived material, known as liquid biopsy, and its components can be obtained from almost all body fluids. These components have shown to reflect characteristics of the status of both the primary and metastatic diseases, helping the clinicians to move towards a personalized medicine. The present review focuses on the liquid biopsy components: circulating tumor cells (CTCS), circulating free DNA (cfDNA), exosomes and tumor-educated platelets (TEP); the isolation technologies used and their potential use for non-invasive screening, early diagnosis, prognosis, response to treatment and real time monitoring of the disease, in NSCLC patients. PMID:27826527

A Microwave Method for Dielectric Characterization Measurement of Small Liquids Using a Metamaterial-Based Sensor.

PubMed

Liu, Weina; Sun, Haoran; Xu, Lei

2018-05-05

We present a microwave method for the dielectric characterization of small liquids based on a metamaterial-based sensor The proposed sensor consists of a micro-strip line and a double split-ring resonator (SRR). A large electric field is observed on the two splits of the double SRRs at the resonance frequency (1.9 GHz). The dielectric property data of the samples under test (SUTs) were obtained with two measurements. One is with the sensor loaded with the reference liquid (REF) and the other is with the sensor loaded with the SUTs. Additionally, the principle of extracting permittivity from measured changes of resonance characteristics changes of the sensor loaded with REF and SUTs is given. Some measurements were carried out at 1.9 GHz, and the calculated results of methanol⁻water mixtures with different molar fractions agree well with the time-domain reflectometry method. Moreover, the proposed sensor is compact and highly sensitive for use of sub-wavelength resonance. In comparison with literature data, relative errors are less than 3% for the real parts and 2% for the imaginary parts of complex permittivity.

Milk fat globules: fatty acid composition, size and in vivo regulation of fat liquidity.

PubMed

Timmen, H; Patton, S

1988-07-01

Populations of large and small milk fat globules were isolated and analyzed to determine differences in fatty acid composition. Globule samples were obtained by centrifugation from milks of a herd and of individual animals produced under both pasture and barn feeding. Triacylglycerols of total globule lipids were prepared by thin layer chromatography and analyzed for fatty acid composition by gas chromatography. Using content of the acids in large globules as 100%, small globules contained fewer short-chain acids, -5.9%, less stearic acid, -22.7%, and more oleic acids, +4.6%, mean values for five trials. These differences are consistent with alternative use of short-chain acids or oleic acid converted from stearic acid to maintain liquidity at body temperature of milk fat globules and their precursors, intracellular lipid droplets. Stearyl-CoA desaturase (EC 1.14.99.5), which maintains fluidity of cellular endoplasmic reticulum membrane, is suggested to play a key role in regulating globule fat liquidity. Possible origins of differences between individual globules in fatty acid composition of their triacylglycerols are discussed.

Loss of the ability to generate large burst-forming unit-like megakaryocytic colonies from thawed cord blood in semisolid cultures after short term suspension culture.

PubMed

Eskola, M; Bäckman, S; Möttönen, S; Kekomäki, R

2015-04-01

Total colony-forming cells from thawed cord blood units (CBUs) include megakaryocytic colony-forming units (CFU-Mks), which survive the freezing process. The aim of this study was to evaluate whether different megakaryocytic progenitors from unseparated CBUs survive the freezing process and a short-term liquid culture. Thawed samples of CBUs were cultured in liquid medium. During the cultures, serial samples were drawn to assess the growth of different megakaryocytic progenitors in a semisolid collagen medium with identical cytokines as in the liquid medium. Megakaryocytic cells were detected using immunohistochemistry and flow cytometry. In suspension culture, the megakaryocytic progenitors almost completely lost the ability to generate large (burst-forming unit-like, BFU-like) megakaryocytic colonies in semisolid cultures (large colonies, median count per chamber d0: 7.25 vs. d7: 1.5; P < 0.0001), whereas the number of small colonies (median count per chamber d0: 7.25 vs. d7: 16.0; P = 0.0505) peaked at day seven. Further 7-day culture in suspension resulted in the decline of small colonies as well (d7: 16.0 vs. d14: 5.75; P = 0.0088). Total CFU-Mk count declined from 23.3 (range 12.5-34.0) at d0 to 7.25 (range 1.0-13.5) at d14 (P < 0.0001). Immediately post-thaw, CBUs possess an ability to generate large BFU-like megakaryocytic colonies, whereas the colonies were not detectable in most CBUs in semisolid culture after a short suspension culture. Small CFU-Mks were observed throughout the cultures. It may be that the BFU-Mk colonies matured and acquired CFU-Mk behaviour. © 2014 International Society of Blood Transfusion.

Compact, Automated Centrifugal Slide-Staining System

NASA Technical Reports Server (NTRS)

Feeback, Daniel L.; Clarke, Mark S. F.

2004-01-01

The Directional Acceleration Vector-Driven Displacement of Fluids (DAVD-DOF) system, under development at the time of reporting the information for this article, would be a relatively compact, automated, centrifugally actuated system for staining blood smears and other microbiological samples on glass microscope slides in either a microgravitational or a normal Earth gravitational environment. The DAVD-DOF concept is a successor to the centrifuge-operated slide stainer (COSS) concept, which was reported in Slide-Staining System for Microgravity or Gravity (MSC-22949), NASA Tech Briefs, Vol. 25, No. 1 (January, 2001), page 64. The COSS includes reservoirs and a staining chamber that contains a microscope slide to which a biological sample is affixed. The staining chamber is sequentially filled with and drained of staining and related liquids from the reservoirs by use of a weighted plunger to force liquid from one reservoir to another at a constant level of hypergravity maintained in a standard swing-bucket centrifuge. In the DAVD-DOF system, a staining chamber containing a sample would also be sequentially filled and emptied, but with important differences. Instead of a simple microscope slide, one would use a special microscope slide on which would be fabricated a network of very small reservoirs and narrow channels connected to a staining chamber (see figure). Unlike in the COSS, displacement of liquid would be effected by use of the weight of the liquid itself, rather than the weight of a plunger.

Electron transparent graphene windows for environmental scanning electron microscopy in liquids and dense gases.

PubMed

Stoll, Joshua D; Kolmakov, Andrei

2012-12-21

Due to its ultrahigh electron transmissivity in a wide electron energy range, molecular impermeability, high electrical conductivity and excellent mechanical stiffness, suspended graphene membranes appear to be a nearly ideal window material for in situ (in vivo) environmental electron microscopy of nano- and mesoscopic objects (including bio-medical samples) immersed in liquids and/or in dense gaseous media. In this paper, taking advantage of a small modification of the graphene transfer protocol onto metallic and SiN supporting orifices, reusable environmental cells with exchangeable graphene windows have been designed. Using colloidal gold nanoparticles (50 nm) dispersed in water as model objects for scanning electron microscopy in liquids as proof of concept, different conditions for imaging through the graphene membrane were tested. Limiting factors for electron microscopy in liquids, such as electron beam induced water radiolysis and damage of the graphene membrane at high electron doses, are discussed.

An online monitor of the oxidative capacity of aerosols (o-MOCA)

NASA Astrophysics Data System (ADS)

Eiguren-Fernandez, Arantzazu; Kreisberg, Nathan; Hering, Susanne

2017-02-01

The capacity of airborne particulate matter to generate reactive oxygen species (ROS) has been correlated with the generation of oxidative stress both in vitro and in vivo. The cellular damage from oxidative stress, and by implication with ROS, is associated with several common diseases, such as asthma and chronic obstructive pulmonary disease (COPD), and some neurological diseases. Yet currently available chemical and in vitro assays to determine the oxidative capacity of ambient particles require large samples, analyses are typically done offline, and the results are not immediate.Here we report the development of an online monitor of the oxidative capacity of aerosols (o-MOCA) to provide online, time-resolved assessment of the capacity of airborne particles to generate ROS. Our approach combines the Liquid Spot Sampler (LSS), which collects particles directly into small volumes of liquid, and a chemical module optimized for online measurement of the oxidative capacity of aerosol using the dithiothreitol (DTT) assay. The LSS uses a three-stage, laminar-flow water condensation approach to enable the collection of particles as small as 5 nm into liquid. The DTT assay has been improved to allow the online, time-resolved analysis of samples collected with the LSS but could be adapted to other collection methods or offline analysis of liquid extracts.The o-MOCA was optimized and its performance evaluated using the 9,10-phenanthraquinone (PQ) as a standard redox-active compound. Laboratory testing shows minimum interferences or carryover between consecutive samples, low blanks, and a reproducible, linear response between the DTT consumption rate (nmol min-1) and PQ concentration (µM). The calculated limit of detection for o-MOCA was 0.15 nmol min-1. The system was validated with a diesel exhaust particle (DEP) extract, previously characterized and used for the development, improvement, and validation of the standard DTT analysis. The DTT consumption rates (nmol min-1) obtained with the o-MOCA were within experimental uncertainties of those previously reported for these DEP samples. In ambient air testing, the fully automated o-MOCA was run unattended for 3 days with 3 h time resolution and showed a diurnal and daily variability in the measured consumption rates (nmol min-1 m-3).

Rapid sample classification using an open port sampling interface coupled with liquid introduction atmospheric pressure ionization mass spectrometry.

PubMed

Van Berkel, Gary J; Kertesz, Vilmos

2017-02-15

An "Open Access"-like mass spectrometric platform to fully utilize the simplicity of the manual open port sampling interface for rapid characterization of unprocessed samples by liquid introduction atmospheric pressure ionization mass spectrometry has been lacking. The in-house developed integrated software with a simple, small and relatively low-cost mass spectrometry system introduced here fills this void. Software was developed to operate the mass spectrometer, to collect and process mass spectrometric data files, to build a database and to classify samples using such a database. These tasks were accomplished via the vendor-provided software libraries. Sample classification based on spectral comparison utilized the spectral contrast angle method. Using the developed software platform near real-time sample classification is exemplified using a series of commercially available blue ink rollerball pens and vegetable oils. In the case of the inks, full scan positive and negative ion ESI mass spectra were both used for database generation and sample classification. For the vegetable oils, full scan positive ion mode APCI mass spectra were recorded. The overall accuracy of the employed spectral contrast angle statistical model was 95.3% and 98% in case of the inks and oils, respectively, using leave-one-out cross-validation. This work illustrates that an open port sampling interface/mass spectrometer combination, with appropriate instrument control and data processing software, is a viable direct liquid extraction sampling and analysis system suitable for the non-expert user and near real-time sample classification via database matching. Published in 2016. This article is a U.S. Government work and is in the public domain in the USA. Published in 2016. This article is a U.S. Government work and is in the public domain in the USA.

Agreement between experimental and theoretical effects of nitrogen gas flowrate on liquid jet atomization

NASA Technical Reports Server (NTRS)

Ingebo, Robert D.

1987-01-01

Two-phase flows were investigated by using high velocity nitrogen gas streams to atomize small-diameter liquid jets. Tests were conducted primarily in the acceleration-wave regime for liquid jet atomization, where it was found that the loss of droplets due to vaporization had a marked effect on drop-size measurements. In addition, four identically designed two-fluid atomizers were fabricated and tested for similarity of spray profiles. A scattered-light scanner was used to measure a characteristic drop diameter, which was correlated with nitrogen gas flowrate. The exponent of 1.33 for nitrogen gas flowrate is identical to that predicted by atomization theory for liquid jet breakup in the acceleration-wave regime. This is higher than the value of 1.2 which was previously obtained at a smapling distance of 4.4 cm downstream of the atomizer. The difference is attributed to the fact that drop-size measurements obtained at a 2.2 cm sampling distance are less affected by vaporization and dispersion of small droplets and therefore should give better agreement with atomization theory. Profiles of characteristic drop diameters were also obtained by making at least five line-of-sight measurements across the spray at several horizontal positions above and below the center line of the spray.

Simultaneous determination of 12 pharmaceuticals in water samples by ultrasound-assisted dispersive liquid-liquid microextraction coupled with ultra-high performance liquid chromatography with tandem mass spectrometry.

PubMed

Guan, Jin; Zhang, Chi; Wang, Yang; Guo, Yiguang; Huang, Peiting; Zhao, Longshan

2016-11-01

A new analytical method was developed for simultaneous determination of 12 pharmaceuticals using ultrasound-assisted dispersive liquid-liquid microextraction (DLLME) followed by ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS). Six nonsteroidal anti-inflammatory drugs (NSAIDs, ketoprofen, mefenamic acid, tolfenamic acid, naproxen, sulindac, and piroxicam) and six antibiotics (tinidazole, cefuroxime axetil, ciprofloxacin, sulfamethoxazole, sulfadiazine, and chloramphenicol) were extracted by ultrasound-assisted DLLME using dichloromethane (800 μL) and methanol/acetonitrile (1:1, v/v, 1200 μL) as the extraction and dispersive solvents, respectively. The factors affecting the extraction efficiency, such as the type and volume of extraction and dispersive solvent, vortex and ultrasonic time, sample pH, and ionic strength, were optimized. The ultrasound-assisted process was applied to accelerate the formation of the fine cloudy solution by using a small volume of dispersive solvent, which increased the extraction efficiency and reduced the equilibrium time. Under the optimal conditions, the calibration curves showed good linearity in the range of 0.04-20 ng mL -1 (ciprofloxacin and sulfadiazine), 0.2-100 ng mL -1 (ketoprofen, tinidazole, cefuroxime axetil, naproxen, sulfamethoxazole, and sulindac), and 1-200 ng mL -1 (mefenamic acid, tolfenamic acid, piroxicam, and chloramphenicol). The LODs and LOQs of the method were in the range of 0.006-0.091 and 0.018-0.281 ng mL -1 , respectively. The relative recoveries of the target analytes were in the range from 76.77 to 99.97 % with RSDs between 1.6 and 8.8 %. The developed method was successfully applied to the extraction and analysis of 12 pharmaceuticals in five kinds of water samples (drinking water, running water, river water, influent and effluent wastewater) with satisfactory results. Graphical Abstract Twelve pharmaceuticals in water samples analyted by UHPLC-MS/MS using ultrasound-assisted DLLME.

Coarsening in Solid-Liquid Mixtures Studied on the Space Shuttle

NASA Technical Reports Server (NTRS)

Caruso, John J.

1999-01-01

Ostwald ripening, or coarsening, is a process in which large particles in a two-phase mixture grow at the expense of small particles. It is a ubiquitous natural phenomena occurring in the late stages of virtually all phase separation processes. In addition, a large number of commercially important alloys undergo coarsening because they are composed of particles embedded in a matrix. Many of them, such as high-temperature superalloys used for turbine blade materials and low-temperature aluminum alloys, coarsen in the solid state. In addition, many alloys, such as the tungsten-heavy metal systems, coarsen in the solid-liquid state during liquid phase sintering. Numerous theories have been proposed that predict the rate at which the coarsening process occurs and the shape of the particle size distribution. Unfortunately, these theories have never been tested using a system that satisfies all the assumptions of the theory. In an effort to test these theories, NASA studied the coarsening process in a solid-liquid mixture composed of solid tin particles in a liquid lead-tin matrix. On Earth, the solid tin particles float to the surface of the sample, like ice in water. In contrast, in a microgravity environment this does not occur. The microstructures in the ground- and space-processed samples (see the photos) show clearly the effects of gravity on the coarsening process. The STS-83-processed sample (right image) shows nearly spherical uniformly dispersed solid tin particles. In contrast, the identically processed, ground-based sample (left image) shows significant density-driven, nonspherical particles, and because of the higher effective solid volume fraction, a larger particle size after the same coarsening time. The "Coarsening in Solid-Liquid Mixtures" (CSLM) experiment was conducted in the Middeck Glovebox facility (MGBX) flown aboard the shuttle in the Microgravity Science Laboratory (MSL-1/1R) on STS-83/94. The primary objective of CSLM is to measure the temporal evolution of the solid particles during coarsening.

Externally pressurized porous cylinder for multiple surface aerosol generation and method of generation

DOEpatents

Apel, C.T.; Layman, L.R.; Gallimore, D.L.

1988-05-10

A nebulizer is described for generating aerosol having small droplet sizes and high efficiency at low sample introduction rates. The nebulizer has a cylindrical gas permeable active surface. A sleeve is disposed around the cylinder and gas is provided from the sleeve to the interior of the cylinder formed by the active surface. In operation, a liquid is provided to the inside of the gas permeable surface. The gas contacts the wetted surface and forms small bubbles which burst to form an aerosol. Those bubbles which are large are carried by momentum to another part of the cylinder where they are renebulized. This process continues until the entire sample is nebulized into aerosol sized droplets. 2 figs.

Sensitive determination of phenolic acids in extra-virgin olive oil by capillary zone electrophoresis.

PubMed

Carrasco Pancorbo, Alegría; Cruces-Blanco, Carmen; Segura Carretero, Antonio; Fernández Gutiérrez, Alberto

2004-11-03

A sensitive, rapid, efficient, and reliable method for the separation and determination of phenolic acids by capillary zone electrophoresis has been carried out. A detailed method optimization was carried out to separate 14 different compounds by studying parameters such as pH, type and concentration of buffer, applied voltage, and injection time. The separation was performed within 16 min, using a 25 mM sodium borate buffer (pH 9.6) at 25 kV with 8 s of hydrodynamic injection. With this method and using a liquid-liquid extraction system, with recovery values around 95%, it has been possible to detect small quantities of phenolic acids in olive oil samples. This is apparently the first paper showing the quantification of this specific family of phenolic compounds in virgin olive oil samples.

Measurement of particulates

NASA Technical Reports Server (NTRS)

Woods, D.

1980-01-01

The size distributions of particles in the exhaust plumes from the Titan rockets launched in August and September 1977 were determined from in situ measurements made from a small sampling aircraft that flew through the plumes. Two different sampling instruments were employed, a quartz crystal microbalance (QCM) cascade impactor and a forward scattering spectrometer probe (FSSP). The QCM measured the nonvolatile component of the aerosols in the plume covering an aerodynamic size ranging from 0.05 to 25 micrometers diameter. The FSSP, flown outside the aircraft under the nose section, measured both the liquid droplets and the solid particles over a size range from 0.5 to 7.5 micrometers in diameter. The particles were counted and classified into 15 size intervals. The presence of a large number of liquid droplets in the exhaust clouds is discussed and data are plotted for each launch and compared.

LIFE: Enceladus Sample Return Mission Concept for Searching Evidence of Life

NASA Technical Reports Server (NTRS)

Tsou, P.; Brownlee, D. E.; McKay, C. P.; Beegle, L. W.; Spilker, L.; Kanik, I.

2011-01-01

One of the most promising targets for the search for life other than Mars in our Solar System is the tiny Saturn moon Enceladus. The Cassini mission to the Saturian system detected an active region on Enceladus where small water particles and gas containing organic materials were being flung into space from a region near the south pole known as the tiger stripes. This discovery indicated that there is very likely a liquid subsurface ocean heated through tidal interactions as Enceladus orbits Saturn. On Earth, whenever there is an energy source, liquid water and organics, there is life; this makes Enceladus one of the prime candidates for a search for life missions. In this presentation, we describe LIFE (Life Investigation For Enceladus) sample return concept from Enceladus in the search for evidence of life.

Small-scale enzymatic digestion of glycoproteins and proteoglycans for analysis of oligosaccharides by LC-MS and FACE gel electrophoresis.

PubMed

Estrella, Ruby P; Whitelock, John M; Roubin, Rebecca H; Packer, Nicolle H; Karlsson, Niclas G

2009-01-01

Structural characterization of oligosaccharides from proteoglycans and other glycoproteins is greatly enhanced through the use of mass spectrometry and gel electrophoresis. Sample preparation for these sensitive techniques often requires enzymatic treatments to produce oligosaccharide sequences for subsequent analysis. This chapter describes several small-scale methods for in-gel, on-blot, and in-solution enzymatic digestions in preparation for graphitized carbon liquid chromatography-mass spectrometry (LC-MS) analysis, with specific applications indicated for glycosaminoglycans (GAGs) and N-linked oligosaccharides. In addition, accompanying procedures for oligosaccharide reduction by sodium borohydride, sample desalting via carbon microcolumn, desialylation by sialidase enzyme treatment, and small-scale oligosaccharide species fractionation are included. Fluorophore-assisted carbohydrate electrophoresis (FACE) is another useful method to isolate derivatized oligosaccharides. Overall, the modularity of these techniques provides ease and flexibility for use in conjunction with mass spectrometric and electrophoretic tools for glycomic research studies.

Toward reliable biomarker signatures in the age of liquid biopsies - how to standardize the small RNA-Seq workflow

PubMed Central

Buschmann, Dominik; Haberberger, Anna; Kirchner, Benedikt; Spornraft, Melanie; Riedmaier, Irmgard; Schelling, Gustav; Pfaffl, Michael W.

2016-01-01

Small RNA-Seq has emerged as a powerful tool in transcriptomics, gene expression profiling and biomarker discovery. Sequencing cell-free nucleic acids, particularly microRNA (miRNA), from liquid biopsies additionally provides exciting possibilities for molecular diagnostics, and might help establish disease-specific biomarker signatures. The complexity of the small RNA-Seq workflow, however, bears challenges and biases that researchers need to be aware of in order to generate high-quality data. Rigorous standardization and extensive validation are required to guarantee reliability, reproducibility and comparability of research findings. Hypotheses based on flawed experimental conditions can be inconsistent and even misleading. Comparable to the well-established MIQE guidelines for qPCR experiments, this work aims at establishing guidelines for experimental design and pre-analytical sample processing, standardization of library preparation and sequencing reactions, as well as facilitating data analysis. We highlight bottlenecks in small RNA-Seq experiments, point out the importance of stringent quality control and validation, and provide a primer for differential expression analysis and biomarker discovery. Following our recommendations will encourage better sequencing practice, increase experimental transparency and lead to more reproducible small RNA-Seq results. This will ultimately enhance the validity of biomarker signatures, and allow reliable and robust clinical predictions. PMID:27317696

13 CFR 107.880 - Assets acquired in liquidation of Portfolio securities.

Code of Federal Regulations, 2010 CFR

2010-01-01

... Portfolio securities. 107.880 Section 107.880 Business Credit and Assistance SMALL BUSINESS ADMINISTRATION... liquidation of Portfolio securities. You may acquire assets in full or partial liquidation of a Small Business... assets. You must dispose of assets acquired in liquidation of a Portfolio security within a reasonable...

The absence of lithium isotope fractionation during basalt differentiation: New measurements by multicollector sector ICP-MS

USGS Publications Warehouse

Tomascak, P.B.; Tera, F.; Helz, R.T.; Walker, R.J.

1999-01-01

We report measurements of the isotopic composition of lithium in basalts using a multicollector magnetic sector plasma-source mass spectrometer (MC-ICP-MS). This is the first application of this analytical technique to Li isotope determination. External precision of multiple replicate and duplicate measurements for a variety of sample types averages ??1.1??? (2?? population). The method allows for the rapid (???8 min/sample) analysis of small samples (???40 ng Li) relative to commonly used thermal ionization methods. The technique has been applied to a suite of samples from Kilauea Iki lava lake, Hawaii. The samples range from olivine-rich cumulitic lava to SiO2 - and K2O-enriched differentiated liquids, and have ??7Li (per mil deviation of sample 7Li/6Li relative to the L-SVEC standard) of +3.0 to +4.8. The data indicate a lack of per mil-level Li isotope fractionation as a result of crystal-liquid fractionation at temperatures greater than 1050??C. This conclusion has been tacitly assumed but never demonstrated, and is important to the interpretation of Li isotope results from such geochemically complex environments as island arcs. Copyright ?? 1999 Elsevier Science Ltd.

Sensitive and rapid determination of pyrethroids in human blood by gas chromatography-tandem mass spectrometry with ultrasound-assisted dispersive liquid-liquid microextraction.

PubMed

Gao, Xue; Guo, Hao; Wang, Junwei; Zhao, Qingbiao

2018-01-19

In this study, a sensitive and fast procedure of ultrasonic-assisted dispersive liquid-liquid microextraction (UADLLME) coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) for the determination of major pyrethroid pesticides (permethrin, tetramethrin, bifenthrin, fenvalerate, flucythrinate, fluvalinate, fenpropathrin, deltamethrin, and cyhalothrin) in blood samples was developed. Response surface methodology (RSM) combined with Box-Behnken design (BBD) and ANOVA function was used to optimize key factors affecting the extraction efficiency of UADLLME procedure. Target compounds were analyzed by GC-MS/MS. Under the optimal conditions, good linearity (R 2 >0.99) was achieved for all the analytes in the concentration range of 0.5 to 100 μg L -1 . The recoveries for spiked samples at 3 concentration levels were between 70.2 and 91.8%, with relative standard deviations (RSD) lower than 10%. Very low limits of detection (LODs) and limits of quantification (LOQs) ranging from 0.01 to 0.1 μg L -1 and from 0.03 to 0.3 μg L -1 were achieved. This method was successfully applied to the determination of low concentration of pyrethroids in blood samples from real forensic cases. High sensitivity, fast determination, simplicity in operation, small sample volume, and low usage of organic solvents are the advantages of this method. This methodology is of important value for sensitive and quick determination of residue pesticides and metabolites, study of residue pesticides behavior in human body, as well as application in real forensic cases. Copyright © 2018 John Wiley & Sons, Ltd.

Magnetic levitation of condensed hydrogen

NASA Technical Reports Server (NTRS)

Paine, C. G.; Seidel, G. M.

1991-01-01

Liquid and solid molecular hydrogen has been levitated using a pair of small superconducting solenoids. The hydrogen samples, up to 3 mm in dimension, were trapped in a magnetic potential having either a discrete minimum or a minimum in the form of a ring 1 cm in diameter. The hydrogen could be moved about in the magnetic trap by applying an electric field.

Pseudolinear gradient ultrahigh-pressure liquid chromatography using an injection valve assembly.

PubMed

Xiang, Yanqiao; Liu, Yansheng; Stearns, Stanley D; Plistil, Alex; Brisbin, Martin P; Lee, Milton L

2006-02-01

The use of ultrahigh pressures in liquid chromatography (UHPLC) imposes stringent requirements on hardware such as pumps, valves, injectors, connecting tubing, and columns. One of the most difficult components of the UHPLC system to develop has been the sample injector. Static-split injection, which can be performed at pressures up to 6900 bar (100,000 psi), consumes a large sample volume and is very irreproducible. A pressure-balanced injection valve provided better reproducibility, shorter injection time, reduced sample consumption, and greater ease of use; however, it could only withstand pressures up to approximately 1000 bar (15,000 psi). In this study, a new injection valve assembly that can operate at pressures as high as 2070 bar (30,000 psi) was evaluated for UHPLC. This assembly contains six miniature electronically controlled needle valves to provide accurate and precise volumes for introduction into the capillary LC column. It was found that sample volumes as small as several tenths of a nanoliter can be injected, which are comparable to the results obtained from the static-split injector. The reproducibilities of retention time, efficiency, and peak area were investigated, and the results showed that the relative standard deviations of these parameters were small enough for quantitative analyses. Separation experiments using the UHPLC system with this new injection valve assembly showed that this new injector is suitable for both isocratic and gradient operation modes. A newly designed capillary connector was used at a pressure as high as 2070 bar (30,000 psi).

Uncertainty budgets for liquid waveguide CDOM absorption measurements.

PubMed

Lefering, Ina; Röttgers, Rüdiger; Utschig, Christian; McKee, David

2017-08-01

Long path length liquid waveguide capillary cell (LWCC) systems using simple spectrometers to determine the spectral absorption by colored dissolved organic matter (CDOM) have previously been shown to have better measurement sensitivity compared to high-end spectrophotometers using 10 cm cuvettes. Information on the magnitude of measurement uncertainties for LWCC systems, however, has remained scarce. Cross-comparison of three different LWCC systems with three different path lengths (50, 100, and 250 cm) and two different cladding materials enabled quantification of measurement precision and accuracy, revealing strong wavelength dependency in both parameters. Stable pumping of the sample through the capillary cell was found to improve measurement precision over measurements made with the sample kept stationary. Results from the 50 and 100 cm LWCC systems, with higher refractive index cladding, showed systematic artifacts including small but unphysical negative offsets and high-frequency spectral perturbations due to limited performance of the salinity correction. In comparison, the newer 250 cm LWCC with lower refractive index cladding returned small positive offsets that may be physically correct. After null correction of measurements at 700 nm, overall agreement of CDOM absorption data at 440 nm was found to be within 5% root mean square percentage error.

Simultaneous viscosity and density measurement of small volumes of liquids using a vibrating microcantilever† †Electronic supplementary information (ESI) available. See DOI: 10.1039/c6an02674e Click here for additional data file.

PubMed Central

Payam, A. F.; Trewby, W.

2017-01-01

Many industrial and technological applications require precise determination of the viscosity and density of liquids. Such measurements can be time consuming and often require sampling substantial amounts of the liquid. These problems can partly be overcome with the use of microcantilevers but most existing methods depend on the specific geometry and properties of the cantilever, which renders simple, accurate measurement difficult. Here we present a new approach able to simultaneously quantify both the density and the viscosity of microliters of liquids. The method, based solely on the measurement of two characteristic frequencies of an immersed microcantilever, is completely independent of the choice of a cantilever. We derive analytical expressions for the liquid's density and viscosity and validate our approach with several simple liquids and different cantilevers. Application of our model to non-Newtonian fluids shows that the calculated viscosities are remarkably robust when compared to measurements obtained from a standard rheometer. However, the results become increasingly dependent on the cantilever geometry as the frequency-dependent nature of the liquid's viscosity becomes more significant. PMID:28352874

Spray-loading: A cryogenic deposition method for diamond anvil cell

NASA Astrophysics Data System (ADS)

Scelta, Demetrio; Ceppatelli, Matteo; Ballerini, Riccardo; Hajeb, Ahmed; Peruzzini, Maurizio; Bini, Roberto

2018-05-01

An efficient loading technique has been developed for flammable, toxic, or explosive gases which can be condensed at liquid nitrogen temperature and ambient pressure in membrane diamond anvil cells (DACs). This cryogenic technique consists in a deposition of small quantities of the desired gas directly into the sample chamber. The deposition is performed using a capillary that reaches the space between the diamond anvils. The DAC is kept under inert gas overpressure during the whole process, in order to avoid contamination from atmospheric O2, CO2, and H2O. This technique provides significant advantages over standard cryo-loading and gas-loading when the condensation of dangerous samples at liquid nitrogen temperature raises safety concerns because it allows dealing with minimum quantities of condensed gases. The whole procedure is particularly fast and efficient. The "spray-loading" has been successfully used in our laboratory to load several samples including acetylene, ammonia, ethylene, and carbon dioxide/water or red phosphorus/NH3 mixtures.

Analysis of lipoprotein profiles of healthy cats by gel-permeation high-performance liquid chromatography

PubMed Central

MIZUTANI, Hisashi; SAKO, Toshinori; OKUDA, Hiroko; ARAI, Nobuaki; KURIYAMA, Koji; MORI, Akihiro; YOSHIMURA, Itaru; KOYAMA, Hidekazu

2016-01-01

Density gradient ultracentrifugation (DGUC) and gel electrophoresis are conventionally used to obtain lipoprotein profiles of animals. We recently applied high-performance liquid chromatography with a gel permeation column (GP-HPLC) and an on-line dual enzymatic system to dogs for lipoprotein profile analysis. We compared the GP-HPLC with DGUC as a method to obtain a feline lipoprotein profile. The lipoprotein profiles showed large and small peaks, which corresponded to high-density lipoprotein (HDL) and low-density lipoprotein (LDL), respectively, whereas very low-density lipoprotein (VLDL) and chylomicron (CM) were only marginally detected. This profile was very similar to that of dogs reported previously. Healthy cats also had a small amount of cholesterol-rich particles distinct from the normal LDL or HDL profile. There was no difference in lipoprotein profiles between the sexes, but males had a significantly larger LDL particle size (P=0.015). This study shows the feasibility of GP-HPLC for obtaining accurate lipoprotein profiles with small sample volumes and provides valuable reference data for healthy cats that should facilitate diagnoses. PMID:27170431

Robotic liquid handling and automation in epigenetics.

PubMed

Gaisford, Wendy

2012-10-01

Automated liquid-handling robots and high-throughput screening (HTS) are widely used in the pharmaceutical industry for the screening of large compound libraries, small molecules for activity against disease-relevant target pathways, or proteins. HTS robots capable of low-volume dispensing reduce assay setup times and provide highly accurate and reproducible dispensing, minimizing variation between sample replicates and eliminating the potential for manual error. Low-volume automated nanoliter dispensers ensure accuracy of pipetting within volume ranges that are difficult to achieve manually. In addition, they have the ability to potentially expand the range of screening conditions from often limited amounts of valuable sample, as well as reduce the usage of expensive reagents. The ability to accurately dispense lower volumes provides the potential to achieve a greater amount of information than could be otherwise achieved using manual dispensing technology. With the emergence of the field of epigenetics, an increasing number of drug discovery companies are beginning to screen compound libraries against a range of epigenetic targets. This review discusses the potential for the use of low-volume liquid handling robots, for molecular biological applications such as quantitative PCR and epigenetics.

Dark field imaging system for size characterization of magnetic micromarkers

NASA Astrophysics Data System (ADS)

Malec, A.; Haiden, C.; Kokkinis, G.; Keplinger, F.; Giouroudi, I.

2017-05-01

In this paper we demonstrate a dark field video imaging system for the detection and size characterization of individual magnetic micromarkers suspended in liquid and the detection of pathogens utilizing magnetically labelled E.coli. The system follows dynamic processes and interactions of moving micro/nano objects close to or below the optical resolution limit, and is especially suitable for small sample volumes ( 10 μl). The developed detection method can be used to obtain clinical information about liquid contents when an additional biological protocol is provided, i.e., binding of microorganisms (e.g. E.coli) to specific magnetic markers. Some of the major advantages of our method are the increased sizing precision in the micro- and nano-range as well as the setup's simplicity making it a perfect candidate for miniaturized devices. Measurements can thus be carried out in a quick, inexpensive, and compact manner. A minor limitation is that the concentration range of micromarkers in a liquid sample needs to be adjusted in such a manner that the number of individual particles in the microscope's field of view is sufficient.

A method for the direct measurement of surface tension of collected atmospherically relevant aerosol particles using atomic force microscopy

NASA Astrophysics Data System (ADS)

Hritz, Andrew D.; Raymond, Timothy M.; Dutcher, Dabrina D.

2016-08-01

Accurate estimates of particle surface tension are required for models concerning atmospheric aerosol nucleation and activation. However, it is difficult to collect the volumes of atmospheric aerosol required by typical instruments that measure surface tension, such as goniometers or Wilhelmy plates. In this work, a method that measures, ex situ, the surface tension of collected liquid nanoparticles using atomic force microscopy is presented. A film of particles is collected via impaction and is probed using nanoneedle tips with the atomic force microscope. This micro-Wilhelmy method allows for direct measurements of the surface tension of small amounts of sample. This method was verified using liquids, whose surface tensions were known. Particles of ozone oxidized α-pinene, a well-characterized system, were then produced, collected, and analyzed using this method to demonstrate its applicability for liquid aerosol samples. It was determined that oxidized α-pinene particles formed in dry conditions have a surface tension similar to that of pure α-pinene, and oxidized α-pinene particles formed in more humid conditions have a surface tension that is significantly higher.

Simple and portable low frequency lock-in amplifier designed for photoacoustic measurements and its application to thermal effusivity determination in liquids

NASA Astrophysics Data System (ADS)

Ortega-Robles, Emmanuel; Cruz-Orea, Alfredo; Elías-Viñas, David

2018-03-01

The lock-in amplifier is a very useful instrument for observing very small signals under adverse signal-to-noise conditions. In this work, we describe a simple and portable lock-in amplifier designed to be used in photoacoustic measurements. The device was used to measure the thermal effusivity of eight different liquid samples (distilled water, glycerol, acetone, ethanol, 2-propanol, chloroform, hexane, and methanol), as well as the effusivity of acetone in aqueous solution at distinct concentrations, giving good results. The instrument has a bandwidth of 10 Hz-10 kHz and a sensitivity of 1 μV.

Attenuation of the Acoustic Signal Propagating Through a Bubbly Liquid Layer

NASA Astrophysics Data System (ADS)

Gubaidullin, D. A.; Nikiforov, A. A.

2018-01-01

The acoustic signal dynamics in a five-layer medium containing two liquid layers with polydisperse gas bubbles has been investigated. Calculations have been made for the interaction between the pulse perturbation of smallamplitude pressure and a multilayer sample containing two layers of industrial gel with polydisperse air bubbles. It has been shown that a small content of bubbles (about 0.1 vol. %) in a thin gel layer decreases tenfold or more the amplitude of acoustic waves with frequencies close to the resonance frequency of natural oscillations of bubbles. There are frequency ranges thereby where the influence of the bubbly layer is insignificant.

In situ SAXS study on cationic and non-ionic surfactant liquid crystals using synchrotron radiation.

PubMed

Fritscher, C; Hüsing, N; Bernstorff, S; Brandhuber, D; Koch, T; Seidler, S; Lichtenegger, H C

2005-11-01

In situ synchrotron small-angle X-ray scattering was used to investigate various surfactant/water systems with hexagonal and lamellar structures regarding their structural behaviour upon heating and cooling. Measurements of the non-ionic surfactant Triton X-45 (polyethylene glycol 4-tert-octylphenyl ether) at different surfactant concentrations show an alignment of the lamellar liquid-crystalline structure close to the wall of the glass capillaries and also a decrease in d-spacing following subsequent heating/cooling cycles. Additionally, samples were subjected to a weak magnetic field (0.3-0.7 T) during heating and cooling, but no influence of the magnetic field was observed.

A novel approach to the simultaneous extraction and non-targeted analysis of the small molecules metabolome and lipidome using 96-well solid phase extraction plates with column-switching technology.

PubMed

Li, Yubo; Zhang, Zhenzhu; Liu, Xinyu; Li, Aizhu; Hou, Zhiguo; Wang, Yuming; Zhang, Yanjun

2015-08-28

This study combines solid phase extraction (SPE) using 96-well plates with column-switching technology to construct a rapid and high-throughput method for the simultaneous extraction and non-targeted analysis of small molecules metabolome and lipidome based on ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry. This study first investigated the columns and analytical conditions for small molecules metabolome and lipidome, separated by an HSS T3 and BEH C18 columns, respectively. Next, the loading capacity and actuation duration of SPE were further optimized. Subsequently, SPE and column switching were used together to rapidly and comprehensively analyze the biological samples. The experimental results showed that the new analytical procedure had good precision and maintained sample stability (RSD<15%). The method was then satisfactorily applied to more widely analyze the small molecules metabolome and lipidome to test the throughput. The resulting method represents a new analytical approach for biological samples, and a highly useful tool for researches in metabolomics and lipidomics. Copyright © 2015 Elsevier B.V. All rights reserved.

Crystallization of hard spheres revisited. II. Thermodynamic modeling, nucleation work, and the surface of tension.

PubMed

Richard, David; Speck, Thomas

2018-06-14

Combining three numerical methods (forward flux sampling, seeding of droplets, and finite-size droplets), we probe the crystallization of hard spheres over the full range from close to coexistence to the spinodal regime. We show that all three methods allow us to sample different regimes and agree perfectly in the ranges where they overlap. By combining the nucleation work calculated from forward flux sampling of small droplets and the nucleation theorem, we show how to compute the nucleation work spanning three orders of magnitude. Using a variation of the nucleation theorem, we show how to extract the pressure difference between the solid droplet and ambient liquid. Moreover, combining the nucleation work with the pressure difference allows us to calculate the interfacial tension of small droplets. Our results demonstrate that employing bulk quantities yields inaccurate results for the nucleation rate.

Quantification of myo-inositol, 1,5-anhydro-D-sorbitol, and D-chiro-inositol using high-performance liquid chromatography with electrochemical detection in very small volume clinical samples

PubMed Central

Schimpf, Karen J.; Meek, Claudia C.; Leff, Richard D.; Phelps, Dale L.; Schmitz, Daniel J.; Cordle, Christopher T.

2015-01-01

Inositol is a six-carbon sugar alcohol and is one of nine biologically significant isomers of hexahydroxycyclohexane. Myo-inositol is the primary biologically active form and is present in higher concentrations in the fetus and newborn than in adults. It is currently being examined for the prevention of retinopathy of prematurity in newborn preterm infants. A robust method for quantifying myo-inositol (MI), D-chiro-inositol (DCI) and 1,5-anhydro-D-sorbitol (ADS) in very small-volume (25 μL) urine, blood serum and/or plasma samples was developed. Using a multiple-column, multiple mobile phase liquid chromatographic system with electrochemical detection, the method was validated with respect to (a) selectivity, (b) accuracy/recovery, (c) precision/reproducibility, (d) sensitivity, (e) stability and (f) ruggedness. The standard curve was linear and ranged from 0.5 to 30 mg/L for each of the three analytes. Above-mentioned performance measures were within acceptable limits described in the Food and Drug Administration’s Guidance for Industry: Bioanalytical Method Validation. The method was validated using blood serum and plasma collected using four common anticoagulants, and also by quantifying the accuracy and sensitivity of MI measured in simulated urine samples recovered from preterm infant diaper systems. The method performs satisfactorily measuring the three most common inositol isomers on 25 μL clinical samples of serum, plasma milk, and/or urine. Similar performance is seen testing larger volume samples of infant formulas and infant formula ingredients. MI, ADS and DCI may be accurately tested in urine samples collected from five different preterm infant diapers if the urine volume is greater than 2–5 mL. PMID:26010453

A Survey on Aflatoxin M1 Content in Sheep and Goat Milk Produced in Sardinia Region, Italy (2005-2013).

PubMed

Virdis, Salvatore; Scarano, Christian; Spanu, Vincenzo; Murittu, Gavino; Spanu, Carlo; Ibba, Ignazio; De Santis, Enrico Pietro Luigi

2014-12-09

In the present work the results of a survey conducted in Sardinia Region on Aflatoxin M 1 (AFM 1 ) contamination in milk of small ruminants from 2005 to 2013 are reported. A total of 517 sheep and 88 goat milk samples from bulk tank, tank trucks and silo tank milk were collected. Analyses were performed by the Regional Farmers Association laboratory using high-performance liquid chromatography following the ISO 14501:1998 standard. None of the sheep milk samples analysed during 2005-2012 showed AFM 1 contamination. In sheep milk samples collected in 2013, 8 out of 172 (4.6%) were contaminated by AFM 1 with a concentration (mean±SD) of 12.59±14.05 ng/L. In one bulk tank milk sample 58.82 ng/L AFM 1 was detected, exceeding the EU limit. In none of goat milk samples analysed from 2010 to 2012 AFM 1 was detected. In 2013, 9 out of 66 goat milk samples (13.6%) showed an AFM 1 concentration of 47.21±19.58 ng/L. Two of these samples exceeded the EU limit, with concentrations of 62.09 and 138.6 ng/L. Higher contamination frequency and concentration rates were detected in bulk tank milk samples collected at farm than in bulk milk truck or silo samples, showing a dilution effect on AFM 1 milk content along small ruminants supply chain. The rate and levels of AFM 1 contamination in sheep and goat milk samples were lower than other countries. However, the small number of milk samples analysed for AFM 1 in Sardinia Region in 2005-2013 give evidence that food business operators check programmes should be improved to ensure an adequate monitoring of AFM 1 contamination in small ruminant dairy chain.

DESIGN OF A SIMPLE SLOW COOLING DEVICE FOR CRYOPRESERVATION OF SMALL BIOLOGICAL SAMPLES.

PubMed

de Paz, Leonardo Juan; Robert, Maria Celeste; Graf, Daniel Adolfo; Guibert, Edgardo Elvio; Rodriguez, Joaquin Valentin

2015-01-01

Slow cooling is a cryopreservation methodology where samples are cooled to its storage temperature at controlled cooling rates. Design, construction and evaluation of a simple and low cost device for slow cooling of small biological samples. The device was constructed based on Pye's freezer idea. A Dewar flask filled with liquid nitrogen was used as heat sink and a methanol bath containing the sample was cooled at constant rates using copper bars as heat conductor. Sample temperature may be lowered at controlled cooling rate (ranging from 0.4°C/min to 6.0°C/min) down to ~-60°C, where it could be conserved at lower temperatures. An example involving the cryopreservation of Neuro-2A cell line showed a marked influence of cooling rate over post preservation cell viability with optimal values between 2.6 and 4.6°C/min. The cooling device proved to be a valuable alternative to more expensive systems allowing the assessment of different cooling rates to evaluate the optimal condition for cryopreservation of such samples.

Triacylglycerol Analysis in Human Milk and Other Mammalian Species: Small-Scale Sample Preparation, Characterization, and Statistical Classification Using HPLC-ELSD Profiles.

PubMed

Ten-Doménech, Isabel; Beltrán-Iturat, Eduardo; Herrero-Martínez, José Manuel; Sancho-Llopis, Juan Vicente; Simó-Alfonso, Ernesto Francisco

2015-06-24

In this work, a method for the separation of triacylglycerols (TAGs) present in human milk and from other mammalian species by reversed-phase high-performance liquid chromatography using a core-shell particle packed column with UV and evaporative light-scattering detectors is described. Under optimal conditions, a mobile phase containing acetonitrile/n-pentanol at 10 °C gave an excellent resolution among more than 50 TAG peaks. A small-scale method for fat extraction in these milks (particularly of interest for human milk samples) using minimal amounts of sample and reagents was also developed. The proposed extraction protocol and the traditional method were compared, giving similar results, with respect to the total fat and relative TAG contents. Finally, a statistical study based on linear discriminant analysis on the TAG composition of different types of milks (human, cow, sheep, and goat) was carried out to differentiate the samples according to their mammalian origin.

Rapid ionic liquid-based ultrasound assisted dual magnetic microextraction to preconcentrate and separate cadmium-4-(2-thiazolylazo)-resorcinol complex from environmental and biological samples.

PubMed

Khan, Sumaira; Kazi, Tasneem Gul; Soylak, Mustafa

2014-04-05

A rapid and innovative microextraction technique named as, ionic liquid-based ultrasound-assisted dual magnetic microextraction (IL-UA-DMME) was developed for the preconcentration and extraction of trace cadmium from environmental and biological samples, prior to analyzed by flame atomic absorption spectrometry (FAAS). The proposed method has many obvious advantages, including evading the use of organic solvents and achieved high extraction yields by the combination of dispersive liquid-liquid microextraction (DLLME) and magnetic mediated-solid phase extraction (MM-SPE). In this approach ionic liquid (IL) 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6] play an important role to extract the cadmium-4-(2-thiazolylazo)-resorcinol (Cd-TAR) complex from acid digested sample solutions and ultrasonic irradiation was applied to assist emulsification. After then, dispersed small amount of Fe3O4 magnetic nanoparticles (MNPs) in sample solutions to salvaged the IL and complete phase separation was attained. Some analytical parameters that influencing the efficiency of proposed (IL-UA-DMME) method, such as pH, volume of IL, ligand concentration, ultra-sonication time, amount of Fe3O4 MNPs, sample volume and matrix effect were optimized. Limit of detection (LOD) and enrichment factor (EF) of the method under optimal experimental conditions were found to be 0.40μgL(-1) and 100, respectively. The relative standard deviation (RSD) of 50μgL(-1) Cd was 4.29%. The validity and accuracy of proposed method, was assessed to analyzed certified reference materials of fortified lake water TMDA-54.4, SPS-WW2 waste water, spinach leaves 1570a and also checked by standard addition method. The obtained values showed good agreement with the certified values and sufficiently high recovery were found in the range of 98.1-101% for Cd. The proposed method was facile, rapid and successfully applied for the determination of Cd in environmental and different biological samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Open port sampling interface

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

Van Berkel, Gary J

A system for sampling a sample material includes a probe which can have an outer probe housing with an open end. A liquid supply conduit within the housing has an outlet positioned to deliver liquid to the open end of the housing. The liquid supply conduit can be connectable to a liquid supply for delivering liquid at a first volumetric flow rate to the open end of the housing. A liquid exhaust conduit within the housing is provided for removing liquid from the open end of the housing. A liquid exhaust system can be provided for removing liquid from themore » liquid exhaust conduit at a second volumetric flow rate, the first volumetric flow rate exceeding the second volumetric flow rate, wherein liquid at the open end will receive sample, liquid containing sample material will be drawn into and through the liquid exhaust conduit, and liquid will overflow from the open end.« less

Apparatus and method for detecting gamma radiation

DOEpatents

Sigg, Raymond A.

1994-01-01

A high efficiency radiation detector for measuring X-ray and gamma radiation from small-volume, low-activity liquid samples with an overall uncertainty better than 0.7% (one sigma SD). The radiation detector includes a hyperpure germanium well detector, a collimator, and a reference source. The well detector monitors gamma radiation emitted by the reference source and a radioactive isotope or isotopes in a sample source. The radiation from the reference source is collimated to avoid attenuation of reference source gamma radiation by the sample. Signals from the well detector are processed and stored, and the stored data is analyzed to determine the radioactive isotope(s) content of the sample. Minor self-attenuation corrections are calculated from chemical composition data.

Fabrication of electron beam deposited tip for atomic-scale atomic force microscopy in liquid.

PubMed

Miyazawa, K; Izumi, H; Watanabe-Nakayama, T; Asakawa, H; Fukuma, T

2015-03-13

Recently, possibilities of improving operation speed and force sensitivity in atomic-scale atomic force microscopy (AFM) in liquid using a small cantilever with an electron beam deposited (EBD) tip have been intensively explored. However, the structure and properties of an EBD tip suitable for such an application have not been well-understood and hence its fabrication process has not been established. In this study, we perform atomic-scale AFM measurements with a small cantilever and clarify two major problems: contaminations from a cantilever and tip surface, and insufficient mechanical strength of an EBD tip having a high aspect ratio. To solve these problems, here we propose a fabrication process of an EBD tip, where we attach a 2 μm silica bead at the cantilever end and fabricate a 500-700 nm EBD tip on the bead. The bead height ensures sufficient cantilever-sample distance and enables to suppress long-range interaction between them even with a short EBD tip having high mechanical strength. After the tip fabrication, we coat the whole cantilever and tip surface with Si (30 nm) to prevent the generation of contamination. We perform atomic-scale AFM imaging and hydration force measurements at a mica-water interface using the fabricated tip and demonstrate its applicability to such an atomic-scale application. With a repeated use of the proposed process, we can reuse a small cantilever for atomic-scale measurements for several times. Therefore, the proposed method solves the two major problems and enables the practical use of a small cantilever in atomic-scale studies on various solid-liquid interfacial phenomena.

Liquid-chromatographic analysis for cyclosporine with use of a microbore column and small sample volume.

PubMed

Annesley, T; Matz, K; Balogh, L; Clayton, L; Giacherio, D

1986-07-01

This liquid-chromatographic assay requires 0.2 to 0.5 mL of whole blood, avoids the use of diethyl ether, and consumes only 10 to 20% of the solvents used in prior methods. Sample preparation involves an acidic extraction with methyl-t-butyl ether, performed in a 13 X 100 mm disposable glass tube, then a short second extraction of the organic phase with sodium hydroxide. After evaporation of the methyl-t-butyl ether, chromatography is performed on an "Astec" 2.0-mm (i.d.) octyl column. We compared results by this procedure with those by use of earlier larger-scale extractions and their respective 4.6-mm (i.d.) columns; analytical recoveries of cyclosporins A and D were comparable with previous findings and results for patients' specimens were equivalent, but the microbore columns provided greatly increased resolution and sensitivity.

Dependence of Liquid Supercooling on Liquid Overheating Levels of Al Small Particles

PubMed Central

Mei, Qingsong; Li, Juying

2015-01-01

The liquid thermal history effect on liquid supercooling behavior has been found in various metals and alloys; typically the degree of liquid supercooling (ΔT−) increases with the increase of liquid overheating (ΔT+) up to several to tens of degrees above the equilibrium melting point (T0). Here we report quantitative experimental measurements on the ΔT−-ΔT+ relationship of Al small particles encapsulated in Al2O3 shells by using a differential scanning calorimeter. We find a remarkable dependence of ΔT− on ΔT+ of Al small particles, extending to at least 340 °C above T0 of Al (~1.36T0), which indicates the existence of temperature-dependent crystallization centers in liquid Al up to very high liquid overheating levels. Our results demonstrate quantitatively the significant effect of liquid thermal history on the supercooling behavior of Al and its alloys, and raise new considerations about the dependence of ΔT− on ΔT+ at very high ΔT+ levels. PMID:28787806

Hydrophilic interaction liquid chromatography/positive ion electrospray ionization mass spectrometry method for the quantification of alprazolam and α-hydroxy-alprazolam in human plasma.

PubMed

Kalogria, Eleni; Pistos, Constantinos; Panderi, Irene

2013-12-30

A hydrophilic interaction liquid chromatography/positive ion electrospray-mass spectrometry (HILIC-ESI/MS) has been developed and fully validated for the quantification of alprazolam and its main metabolite, α-hydroxy-alprazolam, in human plasma. The assay is based on 50μL plasma samples, following liquid-liquid extraction. All analytes and the internal standard (tiamulin) were separated by hydrophilic interaction liquid chromatography using an X-Bridge-HILIC analytical column (150.0mm×2.1mm i.d., particle size 3.5μm) under isoscratic elution. The mobile phase was composed of a 7% 10mM ammonium formate water solution in acetonitrile and pumped at a flow rate of 0.20mLmin(-1). Running in positive electrospray ionization and selected ion monitoring (SIM) the mass spectrometer was set to analyze the protonated molecules [M+H](+) at m/z 309, 325 and 494 for alprazolam, α-hydroxy-alprazolam and tiamulin (ISTD) respectively. The assay was linear over the concentration range of 2.5-250ngmL(-1) for alprazolam and 2.5-50ngmL(-1) for α-hydroxy alprazolam. Intermediate precision was less than 4.1% over the tested concentration ranges. The method is the first reported application of HILIC in the analysis benzodiazepines in human plasma. With a small sample size (50μL human plasma) and a run time less than 10.0min for each sample the method can be used to support a wide range of clinical studies concerning alprazolam quantification. Copyright © 2013 Elsevier B.V. All rights reserved.

A new laser pain threshold model detects a faster onset of action from a liquid formulation of 1 g paracetamol than an equivalent tablet formulation

PubMed Central

Sutton, J A; Gillin, W P; Grattan, T J; Clarke, G D; Kilminster, S G

2002-01-01

Aims To discover whether a new infra-red laser method could detect a change in pain threshold after as mild an analgesic as paracetamol and whether an effervescent liquid formulation produced a faster onset of action than tablets. Methods This double-blind, placebo controlled randomized study used a portable, infra-red laser to measure ‘first pain’ thresholds on the nondominant forearm in 12 normal volunteers before and after 1 g of paracetamol or placebo. The mean of six recordings was determined three times before dosing, the first being used as a familiarization procedure, and 14 times after dosing. Results We detected a small (2%), statistically significant difference in pain threshold between a liquid formulation of paracetamol and placebo at 30 and 60 min (P = 0.004 and P = 0.001), but not between tablets and placebo. Liquid also increased the threshold significantly compared with tablets at 60 min (P = 0.01). Conclusions To detect such a small increase in pain threshold requires a highly consistent measure and the coefficient of variation was 2% for the study overall, surprisingly low for a subjective phenomenon. The reasons for this include minimizing reflectance by blacking the skin, using a nonhairy site, averaging six data points at each sample time and controlling closely the ambient conditions and the subjects’ preparation for studies. PMID:11849194

Microfluidic interconnects

DOEpatents

Benett, William J.; Krulevitch, Peter A.

2001-01-01

A miniature connector for introducing microliter quantities of solutions into microfabricated fluidic devices. The fluidic connector, for example, joins standard high pressure liquid chromatography (HPLC) tubing to 1 mm diameter holes in silicon or glass, enabling ml-sized volumes of sample solutions to be merged with .mu.l-sized devices. The connector has many features, including ease of connect and disconnect; a small footprint which enables numerous connectors to be located in a small area; low dead volume; helium leak-tight; and tubing does not twist during connection. Thus the connector enables easy and effective change of microfluidic devices and introduction of different solutions in the devices.

Gusev Crater on Mars: Wet and Dry

NASA Technical Reports Server (NTRS)

Yen, Albert; Gellert, Ralf; Morris, Richard

2008-01-01

The Mars Exploration Rover Spirit has traversed over 7.5 km in 1470 sols of operations at the Gusev Crater landing site. Chemical and mineralogical evidence from approximately 200 in-situ samples indicate various degrees of exposure to liquid water, from wet and saturated to dry and unaltered. (1) Six samples with concentrations of amorphous silica between 60 and 95 wt% were discovered in a small valley less than 50 meters in length. Associated enrichments in titanium oxide, relatively insoluble at low pH, suggest that these silica deposits formed as a result of acidic leaching processes. Liquid water interactions with these surface materials were necessary to remove cations solubilized in the low pH environment or to concentrate silica in solution prior to precipitation. (2) Hydrated ferric sulfates are found in subsurface deposits which have the unmistakable chemical signatures of nearby rocks. The movement of hydrothermal fluids and/or fumarolic vapors through local rocks prior to precipitation of these materials is suggested by these observations. (3) Goethite (alpha-FeOOH), a mineral phase which requires water to form, represents 20% to 35% of the iron in numerous rock samples (Clovis Class) on the West Spur of the Columbia Hills. Alteration of iron under aqueous conditions is clearly indicated by this presence of goethite. (4) Nearly isochemical signatures are found in elemental analyses of over ten distinct samples (Wishstone/Watchtower class rocks), yet the ratio of ferric iron to total iron varies from 0.4 to 0.95. Small quantities of water, insufficient to flush cations from the samples, were likely responsible for this weathering. (5) Bromine, a trace element readily mobilized by water, is found in high concentrations in certain rock interiors and is enhanced in subsurface soils, consistent with transport to localized cold traps by water thin-films. (6) Also relevant to the characterizing the role of liquid water is the discovery of an areally extensive ultramafic sequence of rocks where over 70% of the iron is in unaltered olivine and the ferric to total iron ratio is 0.1. This result indicates that certain materials at the martian surface have been protected from aqueous alteration.

Efficacy of Thickened Liquids for Eliminating Aspiration in Head and Neck Cancer: A Systematic Review

PubMed Central

Barbon, Carly E.A.; Steele, Catriona M.

2015-01-01

Objective To appraise the current videofluoroscopic evidence on the reduction of aspiration using thickened liquids in the head and neck cancer population. Data Sources Search terms relating to deglutition or dysphagia or swallow and neoplasms and oncology or head and neck cancer and viscosity or texture and apira or residu* were combined with honey or nectar, xerostomia, respiratory aspiration using Boolean operators. Review Methods A multi-engine literature search identified 337 non-duplicate articles of which 6 were judged to be relevant. These underwent detailed review for study quality and qualitative synthesis. Results The articles reviewed in detail predominantly described heterogeneous study samples with small sample sizes, making for difficult interpretation and generalization of results. Rates of aspiration were typically not reported by bolus consistency, despite the fact that a variety of stimulus consistencies was used during VFSS. Studies confirmed that aspiration is a major concern in the head and neck cancer population and reported a trend towards more frequent aspiration post-(chemo)radiotherapy. Conclusion Overall, the literature on thickened liquids as an intervention to eliminate aspiration in the head and neck cancer population is limited. Because aspiration is known to be prevalent in the head and neck cancer population and thickened liquids are known to eliminate aspiration in other populations, it is important to determine the effectiveness of thickened liquids for reducing aspiration in the head and neck cancer population. PMID:25358345

Performance of a Small Gas Generator Using Liquid Hydrogen and Liquid Oxygen

NASA Technical Reports Server (NTRS)

Acker, Loren W.; Fenn, David B.; Dietrich, Marshall W.

1961-01-01

The performance and operating problems of a small hot-gas generator burning liquid hydrogen with liquid oxygen are presented. Two methods of ignition are discussed. Injector and combustion chamber design details based on rocket design criteria are also given. A carefully fabricated showerhead injector of simple design provided a gas generator that yielded combustion efficiencies of 93 and 96 percent.

Liquid scintillation counting for /sup 14/C uptake of single algal cells isolated from natural samples

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

Rivkin, R.B.; Seliger, H.H.

1981-07-01

Short term rates of /sup 14/C uptake for single cells and small numbers of isolated algal cells of five phytoplankton species from natural populations were measured by liquid scintillation counting. Regression analysis of uptake rates per cell for cells isolated from unialgal cultures of seven species of dinoflagellates, ranging in volume from ca. 10/sup 3/ to 10/sup 7/ ..mu..m/sup 3/, gave results identical to uptake rates per cell measured by conventional /sup 14/C techniques. Relative standard errors or regression coefficients ranged between 3 and 10%, indicating that for any species there was little variation in photosynthesis per cell.

Estimation of the curvature of the solid liquid interface during Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Barat, Catherine; Duffar, Thierry; Garandet, Jean-Paul

1998-11-01

An approximate solution for the solid/liquid interface curvature due to the crucible effect in crystal growth is derived from simple heat flux considerations. The numerical modelling of the problem carried out with the help of the finite element code FIDAP supports the predictions of our analytical expression and allows to identify its range of validity. Experimental interface curvatures, measured in gallium antimonide samples grown by the vertical Bridgman method, are seen to compare satisfactorily to analytical and numerical results. Other literature data are also in fair agreement with the predictions of our models in the case where the amount of heat carried by the crucible is small compared to the overall heat flux.

Velocimetry of fast microscopic liquid jets by nanosecond dual-pulse laser illumination for megahertz X-ray free-electron lasers.

PubMed

Grünbein, Marie Luise; Shoeman, Robert L; Doak, R Bruce

2018-03-19

To conduct X-ray Free-Electron Laser (XFEL) measurements at megahertz (MHz) repetition rates, sample solution must be delivered in a micron-sized liquid free-jet moving at up to 100 m/s. This exceeds by over a factor of two the jet speeds measurable with current high-speed camera techniques. Accordingly we have developed and describe herein an alternative jet velocimetry based on dual-pulse nanosecond laser illumination. Three separate implementations are described, including a small laser-diode system that is inexpensive and highly portable. We have also developed and describe analysis techniques to automatically and rapidly extract jet speed from dual-pulse images.

IASLC Statement Paper: Liquid Biopsy for Advanced Non-Small Cell Lung Cancer (NSCLC).

PubMed

Rolfo, Christian; Mack, Philip C; Scagliotti, Giorgio V; Baas, Paul; Barlesi, Fabrice; Bivona, Trever G; Herbst, Roy S; Mok, Tony S; Peled, Nir; Pirker, Robert; Raez, Luis E; Reck, Martin; Riess, Jonathan W; Sequist, Lecia V; Shepherd, Frances A; Sholl, Lynette M; Tan, Daniel Sw; Wakelee, Heather A; Wistuba, Ignacio I; Wynes, Murry W; Carbone, David P; Hirsch, Fred R; Gandara, David R

2018-06-06

The isolation of circulating cell-free tumoral DNA (ctDNA) in plasma and its subsequent molecular analysis is a powerful tool that can help improve clinical outcomes across multiple cancer types, including non-small cell lung cancer (NSCLC). Assays of this nature that utilize blood as opposed to tumor samples are frequently referred to as liquid biopsies. An increasing number of new platforms have been recently developed that improve not only the fidelity of the molecular analysis of the liquid biopsy but also the number of tests performed on a single specimen. ctDNA assays for detection of both epidermal growth factor receptor (EGFR) sensitizing and resistance mutations have already entered clinical practice and many other molecular tests - such as resistance mutations for ALK rearrangements - are likely to do so in the near future. Due to an abundance of new evidence, an appraisal was warranted to review strengths and weaknesses, to describe what is already in clinical practice and what has yet to be implemented, and to highlight areas in need of further investigation. A multidisciplinary panel of experts in the field of thoracic oncology with interest and expertise in liquid biopsy and molecular pathology, was convened by the International Association for the Study of Lung Cancer (IASLC) to evaluate current available evidence with the aim of producing a set of recommendations for the use of liquid biopsy for molecular analysis in in guiding the clinical management of advanced NSCLC patients as well as identifying unmet needs. Copyright © 2018. Published by Elsevier Inc.

Biobriefcase aerosol collector

DOEpatents

Bell, Perry M [Tracy, CA; Christian, Allen T [Madison, WI; Bailey, Christopher G [Pleasanton, CA; Willis, Ladona [Manteca, CA; Masquelier, Donald A [Tracy, CA; Nasarabadi, Shanavaz L [Livermore, CA

2009-09-22

A system for sampling air and collecting particles entrained in the air that potentially include bioagents. The system comprises providing a receiving surface, directing a liquid to the receiving surface and producing a liquid surface. Collecting samples of the air and directing the samples of air so that the samples of air with particles entrained in the air impact the liquid surface. The particles potentially including bioagents become captured in the liquid. The air with particles entrained in the air impacts the liquid surface with sufficient velocity to entrain the particles into the liquid but cause minor turbulence. The liquid surface has a surface tension and the collector samples the air and directs the air to the liquid surface so that the air with particles entrained in the air impacts the liquid surface with sufficient velocity to entrain the particles into the liquid, but cause minor turbulence on the surface resulting in insignificant evaporation of the liquid.

In-flow detection of ultra-small magnetic particles by an integrated giant magnetic impedance sensor

NASA Astrophysics Data System (ADS)

Fodil, K.; Denoual, M.; Dolabdjian, C.; Treizebre, A.; Senez, V.

2016-04-01

We have designed and fabricated a microfluidic system made of glass and polydimethylsiloxane. A micro-magnetometer has been integrated to the system. This sensor is made of a giant magneto-impedance wire known to have very high magnetic sensitivity at room temperature. A liquid-liquid segmented multiphase flow was generated in the channel using a Y-shaped inlet junction. The dispersed phase plugs contained superparamagnetic iron oxide (20 nm) nanoparticles at a molar concentration of 230 mmol/l. We have shown both theoretically and experimentally that in-flow detection of these nanoparticles is performed by the microsystem for concentration as small as 5.47 × 10-9 mol. These performances show that it is conceivable to use this system for ex-vivo analysis of blood samples where superparamagnetic iron oxide nanoparticles, initially used as magnetic contrast agents, could be functionalized for biomarkers fishing. It opens new perspectives in the context of personalized medicine.

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.

Measuring the Coefficient of Friction of a Small Floating Liquid Marble

PubMed Central

Ooi, Chin Hong; Nguyen, Anh Van; Evans, Geoffrey M.; Dao, Dzung Viet; Nguyen, Nam-Trung

2016-01-01

This paper investigates the friction coefficient of a moving liquid marble, a small liquid droplet coated with hydrophobic powder and floating on another liquid surface. A floating marble can easily move across water surface due to the low friction, allowing for the transport of aqueous solutions with minimal energy input. However, the motion of a floating marble has yet to be systematically characterised due to the lack of insight into key parameters such as the coefficient of friction between the floating marble and the carrier liquid. We measured the coefficient of friction of a small floating marble using a novel experimental setup that exploits the non-wetting properties of a liquid marble. A floating liquid marble pair containing a minute amount magnetite particles were immobilised and then released in a controlled manner using permanent magnets. The capillarity-driven motion was analysed to determine the coefficient of friction of the liquid marbles. The “capillary charge” model was used to fit the experimental results. We varied the marble content and carrier liquid to establish a relationship between the friction correction factor and the meniscus angle. PMID:27910916

Method of forming calthrate ice

DOEpatents

Hino, T.; Gorski, A.J.

1985-09-30

A method of forming clathrate ice in a supercooled water-based liquid contained in a vessel is disclosed. Initially, an oscillator device is located in the liquid in the vessel. The oscillator device is then oscillated ultransonically so that small crystals are formed in the liquid. Thes small crystals serve as seed crystals for ice formation in the liquid and thereby prevent supercooling of the liquid. Preferably, the oscillating device is controlled by a thermostat which initiates operation of the oscillator device when the temperature of the liquid is lowered to the freezing point. Thereafter, the operation of the oscillator device is terminated when ice is sensed in the liquid by an ice sensor.

Method of forming clathrate ice

DOEpatents

Hino, Toshiyuki; Gorski, Anthony J.

1987-01-01

A method of forming clathrate ice in a supercooled water-based liquid contained in a vessel is disclosed. Initially, an oscillator device is located in the liquid in the vessel. The oscillator device is then oscillated ultrasonically so that small crystals are formed in the liquid. These small crystals serve as seed crystals for ice formation in the liquid and thereby prevent supercooling of the liquid. Preferably, the oscillating device is controlled by a thermostat which initiates operation of the oscillator device when the temperature of the liquid is lowered to the freezing point. Thereafter, the operation of the oscillator device is terminated when ice is sensed in the liquid by an ice sensor.

β2-Adrenergic receptors and G-protein-coupled receptor kinase 2 in rabbit pleural mesothelium.

PubMed

Sironi, Chiara; Bodega, Francesca; Armilli, Marta; Porta, Cristina; Zocchi, Luciano; Agostoni, Emilio

2010-09-30

Former studies on net rate of liquid absorption from small Ringer or 1% albumin-Ringer hydrothoraces in rabbits indicated that Na+ transport and solute-coupled liquid absorption by mesothelium is increased by pleural liquid dilution, and stimulation of β2-adrenoreceptors (β2AR). In this research we tried to provide molecular evidence for β2AR in visceral and parietal mesothelium of rabbit pleura. Moreover, because prolonged stimulation of β2AR may lead to desensitization mediated by G-protein-coupled receptor kinase 2 (GRK2), we also checked whether GRK2 is expressed in pleural mesothelium. To this end we performed immunoblot assays on total protein extracts from scraped visceral and parietal mesothelium, and from cultured pleural mesothelial cells of rabbits. All three samples showed β2AR and GRK2 specific bands. Copyright 2010 Elsevier B.V. All rights reserved.

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

Van Berkel, Gary J.

A system for sampling a sample material includes a probe which can have an outer probe housing with an open end. A liquid supply conduit within the housing has an outlet positioned to deliver liquid to the open end of the housing. The liquid supply conduit can be connectable to a liquid supply for delivering liquid at a first volumetric flow rate to the open end of the housing. A liquid exhaust conduit within the housing is provided for removing liquid from the open end of the housing. A liquid exhaust system can be provided for removing liquid from themore » liquid exhaust conduit at a second volumetric flow rate, the first volumetric flow rate exceeding the second volumetric flow rate, wherein liquid at the open end will receive sample, liquid containing sample material will be drawn into and through the liquid exhaust conduit, and liquid will overflow from the open end.« less

Capillary liquid chromatography combined with pressurized liquid extraction and dispersive liquid-liquid microextraction for the determination of vitamin E in cosmetic products.

PubMed

Viñas, Pilar; Pastor-Belda, Marta; Campillo, Natalia; Bravo-Bravo, María; Hernández-Córdoba, Manuel

2014-06-01

Capillary liquid chromatography (LC) is used for the determination of tocopherols and tocotrienols in cosmetic products. Dispersive liquid-liquid microextraction (DLLME) allows the analytes to be preconcentrated into a very small volume of organic solvent which is then injected into the chromatograph running at a very low flow rate. Pressurized liquid extraction (PLE) at a high temperature and pressure was used to isolate vitamin E forms from cosmetics. The Taguchi experimental method was used to optimize the factors affecting DLLME. The parameters selected were 2mL of acetonitrile (disperser solvent), 100μL carbon tetrachloride (extraction solvent) and 10mL aqueous solution. A volume of 5μL of the organic phase was injected into the reversed-phase capillary LC system equipped with a diode array detector and using an isocratic mobile phase composed of an 95:5 (v/v) methanol:water mixture at a flow-rate of 20μLmin(-1). Quantification was carried out using aqueous standards and detection limits were in the range 0.1-0.5ngmL(-1), corresponding to 3-15ngg(-1) in the cosmetic sample. The recoveries were in the 87-105% range, with RSDs lower than 7.8%. The method was validated according to international guidelines and using a certified reference material. Copyright © 2014 Elsevier B.V. All rights reserved.

Changes to Serum Sample Tube and Processing Methodology Does Not Cause Inter-Individual Variation in Automated Whole Serum N-Glycan Profiling in Health and Disease

PubMed Central

Shubhakar, Archana; Kalla, Rahul; Nimmo, Elaine R.; Fernandes, Daryl L.; Satsangi, Jack; Spencer, Daniel I. R.

2015-01-01

Introduction Serum N-glycans have been identified as putative biomarkers for numerous diseases. The impact of different serum sample tubes and processing methods on N-glycan analysis has received relatively little attention. This study aimed to determine the effect of different sample tubes and processing methods on the whole serum N-glycan profile in both health and disease. A secondary objective was to describe a robot automated N-glycan release, labeling and cleanup process for use in a biomarker discovery system. Methods 25 patients with active and quiescent inflammatory bowel disease and controls had three different serum sample tubes taken at the same draw. Two different processing methods were used for three types of tube (with and without gel-separation medium). Samples were randomised and processed in a blinded fashion. Whole serum N-glycan release, 2-aminobenzamide labeling and cleanup was automated using a Hamilton Microlab STARlet Liquid Handling robot. Samples were analysed using a hydrophilic interaction liquid chromatography/ethylene bridged hybrid(BEH) column on an ultra-high performance liquid chromatography instrument. Data were analysed quantitatively by pairwise correlation and hierarchical clustering using the area under each chromatogram peak. Qualitatively, a blinded assessor attempted to match chromatograms to each individual. Results There was small intra-individual variation in serum N-glycan profiles from samples collected using different sample processing methods. Intra-individual correlation coefficients were between 0.99 and 1. Unsupervised hierarchical clustering and principal coordinate analyses accurately matched samples from the same individual. Qualitative analysis demonstrated good chromatogram overlay and a blinded assessor was able to accurately match individuals based on chromatogram profile, regardless of disease status. Conclusions The three different serum sample tubes processed using the described methods cause minimal inter-individual variation in serum whole N-glycan profile when processed using an automated workstream. This has important implications for N-glycan biomarker discovery studies using different serum processing standard operating procedures. PMID:25831126

Changes to serum sample tube and processing methodology does not cause Intra-Individual [corrected] variation in automated whole serum N-glycan profiling in health and disease.

PubMed

Ventham, Nicholas T; Gardner, Richard A; Kennedy, Nicholas A; Shubhakar, Archana; Kalla, Rahul; Nimmo, Elaine R; Fernandes, Daryl L; Satsangi, Jack; Spencer, Daniel I R

2015-01-01

Serum N-glycans have been identified as putative biomarkers for numerous diseases. The impact of different serum sample tubes and processing methods on N-glycan analysis has received relatively little attention. This study aimed to determine the effect of different sample tubes and processing methods on the whole serum N-glycan profile in both health and disease. A secondary objective was to describe a robot automated N-glycan release, labeling and cleanup process for use in a biomarker discovery system. 25 patients with active and quiescent inflammatory bowel disease and controls had three different serum sample tubes taken at the same draw. Two different processing methods were used for three types of tube (with and without gel-separation medium). Samples were randomised and processed in a blinded fashion. Whole serum N-glycan release, 2-aminobenzamide labeling and cleanup was automated using a Hamilton Microlab STARlet Liquid Handling robot. Samples were analysed using a hydrophilic interaction liquid chromatography/ethylene bridged hybrid(BEH) column on an ultra-high performance liquid chromatography instrument. Data were analysed quantitatively by pairwise correlation and hierarchical clustering using the area under each chromatogram peak. Qualitatively, a blinded assessor attempted to match chromatograms to each individual. There was small intra-individual variation in serum N-glycan profiles from samples collected using different sample processing methods. Intra-individual correlation coefficients were between 0.99 and 1. Unsupervised hierarchical clustering and principal coordinate analyses accurately matched samples from the same individual. Qualitative analysis demonstrated good chromatogram overlay and a blinded assessor was able to accurately match individuals based on chromatogram profile, regardless of disease status. The three different serum sample tubes processed using the described methods cause minimal inter-individual variation in serum whole N-glycan profile when processed using an automated workstream. This has important implications for N-glycan biomarker discovery studies using different serum processing standard operating procedures.

Concentration methods for high-resolution THz spectroscopy of nucleic-acid biomolecules and crystals

NASA Astrophysics Data System (ADS)

Brown, E. R.; Zhang, W.; Mendoza, E. A.; Kuznetsova, Y.; Brueck, S. R. J.; Rahman, M.; Norton, M. L.

2012-03-01

Biomolecules can exhibit low-lying vibrational modes in the THz region which are detectable in transmission given a strong molecular dipole moment and optical depth, and a spectrometer of adequate sensitivity. The nucleic acids are particularly interesting because of applications such as label-free gene assay, bio-agent detection, etc. However for nucleic acids, sample preparation and THz coupling are of paramount importance because of the strong absorption by liquid water and the small concentration of molecules present in physiological solutions. Concentration methods become necessary to make the THz vibrational modes detectable, either by concentrating the nucleic-acid sample itself in a small volume but large area, or by concentrating the THz radiation down to the volume of the sample. This paper summarizes one type of the first method: nanofluidic channel arrays for biological nucleic acids; and two types of the second method: (1) a circular-waveguide pinhole, and (2) a circular-waveguide, conical-horn coupling structure, both for DNA crystals. The first method has been demonstrated on a very short artificial nucleic acid [small-interfering (si) RNA (17-to-25 bp)] and a much longer, biological molecule [Lambda-phage DNA (48.5 kbp)]. The second method has been demonstrated on small (~100 micron) single crystals of DNA grown by the sitting-drop method.

POTENTIAL IMPACT OF TANK F FLUSH SOLUTION ON H-CANYON EVAPORATOR OPERATION

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

Kyser, E.; Fondeur, F.; Fink, S.

2010-09-13

Previous chemical analysis of a sample from the liquid heel found in Tank F of the High Activity Drain (HAD) system in F/H laboratory revealed the presence of n-paraffin, tributyl phosphate (TBP), Modifier from the Modular Caustic-Side Solvent Extraction Unit (MCU) process and a vinyl ester resin that is very similar to the protective lining on Tank F. Subsequent analyses detected the presence of a small amount of diisopropylnaphthalene (DIN) (major component of Ultima Gold{trademark} AB liquid scintillation cocktail). Indications are that both vinyl ester resin and DIN are present in small amounts in the flush solution. The flush solutionmore » currently in the LR-56S trailer likely has an emulsion which is believed to contain a mixture of the reported organic species dominated by TBP. An acid treatment similar to that proposed to clear the HAD tank heel in F/H laboratory was found to allow separation of an organic phase from the cloudy sample tested by SRNL. Mixing of that clear sample did re-introduce some cloudiness that did not immediately clear but that cloudiness is attributed to the DIN in the matrix. An organic phase does quickly separate from the cloudy matrix allowing separation by a box decanter in H-Canyon prior to transfer to the evaporator feed tank. This separation should proceed normally as long as the emulsion is broken-up by acidification.« less

Analysis of catecholamines in urine by unique LC/MS suitable ion-pairing chromatography.

PubMed

Bergmann, Marianne L; Sadjadi, Seyed; Schmedes, Anne

2017-07-01

The catecholamines, epinephrine (E) and norepinephrine (NE) are small polar, hydrophilic molecules, posing significant challenges to liquid chromatography - tandem mass spectrometry (LC-MS/MS) method development. Specifically, these compounds show little retention on conventional reversed-phase liquid chromatography columns. This work presents development and validation of an LC-MS/MS method for determining catecholamines in urine, based on a new approach to ion-pairing chromatography (IPC), in which the ion-pairing reagent (IPR), 1-Heptane Sulfonic Acid (HSA), is added to the extracted samples instead of the mobile phases. A Hamilton STARlet workstation carried out the solid phase extraction of urine samples. The extracted samples were diluted with 60mmol/L HSA and injected on a Kinetex core-shell biphenyl column with conventional LC-MS/MS suitable mobile phases. Chromatographic separation of E and NE was achieved successfully with very stable retention times (RT). In 484 injections, the RTs were steady with a CV of less than ±4%. Furthermore, HSA was separated from E and NE, allowing HSA to be diverted to waste instead of entering the mass spectrometer ion chamber. The method was validated with good analytical performance, and even though the analysis for urinary catecholamines is increasingly being replaced by plasma free metanephrines in diagnosing pheochromocytomas, this work represents the application of a new analytical technique that can be transferred to other small polar molecules, that are difficult to chromatograph on traditional reversed phase columns. Copyright © 2017 Elsevier B.V. All rights reserved.

Measuring the structure factor of simple fluids under extreme conditions

NASA Astrophysics Data System (ADS)

Weck, Gunnar

2013-06-01

The structure and dynamics of fluids, although a long standing matter of investigations, is still far from being well established. In particular, with the existence of a first order liquid-liquid phase transition (LLT) discovered in liquid phosphorus at 0.9 GPa and 1300 K it is now recognized that the fluid state could present complex structural changes. At present, very few examples of LLTs have been clearly evidenced, which may mean that a larger range of densities must be probed. First order transitions between a molecular and a polymeric liquid have been recently predicted by first principles calculations in liquid nitrogen at 88 GPa and 2000 K and in liquid CO2 at 45 GPa and 1850 K. The only device capable of reaching these extreme conditions is the diamond anvil cell (DAC), in which, the sample is sandwiched between two diamond anvils of thickness 100 times larger. Consequently, the diffracted signal from the sample is very weak compared to the Compton signal of the anvils, and becomes hardly measurable for pressures above ~20 GPa. A similar problem has been faced by the high pressure community using large volume press so as to drastically reduce the x-ray background from the sample environment. In the angle-dispersive diffraction configuration, it was proposed to use a multichannel collimator (MCC). This solution has been implemented to fit the constraints of the Paris-Edimburg (PE) large volume press and it is now routinely used on beamline ID27 of the European Synchrotron Radiation Facility. In this contribution, we present our adaptation of the MCC device accessible at ID27 for the DAC experiment. Because of the small sample volume a careful alignment procedure between the MCC slits and the DAC had to be implemented. The data analysis procedure initially developed by Eggert et al. has also been completed in order to take into account the complex contribution of the MCC slits. A large reduction of the Compton diffusion from the diamond anvils is obtained enabling quantitative structure factor measurement, even for the weakest x-ray scatterer liquid. Experimental results on fluid hydrogen will be presented to test the limits of this new setup. In collaboration with Gaston Garbarino, ESRF, France; Frederic Datchi, Sandra Ninet, Université Pierre et Marie Curie-Paris VI, France; Dylan Spaulding, Paul Loubeyre, CEA, DAM, DIF, France; and Mohamed Mezouar, ESRF, France.

Plasma serotonin in horses undergoing surgery for small intestinal colic

PubMed Central

Torfs, Sara C.; Maes, An A.; Delesalle, Catherine J.; Pardon, Bart; Croubels, Siska M.; Deprez, Piet

2015-01-01

This study compared serotonin concentrations in platelet poor plasma (PPP) from healthy horses and horses with surgical small intestinal (SI) colic, and evaluated their association with postoperative ileus, strangulation and non-survival. Plasma samples (with EDTA) from 33 horses with surgical SI colic were collected at several pre- and post-operative time points. Serotonin concentrations were determined using liquid-chromatography tandem mass spectrometry. Results were compared with those for 24 healthy control animals. The serotonin concentrations in PPP were significantly lower (P < 0.01) in pre- and post-operative samples from surgical SI colic horses compared to controls. However, no association with postoperative ileus or non-survival could be demonstrated at any time point. In this clinical study, plasma serotonin was not a suitable prognostic factor in horses with SI surgical colic. PMID:25694668

Apparatus and method for detecting gamma radiation

DOEpatents

Sigg, R.A.

1994-12-13

A high efficiency radiation detector is disclosed for measuring X-ray and gamma radiation from small-volume, low-activity liquid samples with an overall uncertainty better than 0.7% (one sigma SD). The radiation detector includes a hyperpure germanium well detector, a collimator, and a reference source. The well detector monitors gamma radiation emitted by the reference source and a radioactive isotope or isotopes in a sample source. The radiation from the reference source is collimated to avoid attenuation of reference source gamma radiation by the sample. Signals from the well detector are processed and stored, and the stored data is analyzed to determine the radioactive isotope(s) content of the sample. Minor self-attenuation corrections are calculated from chemical composition data. 4 figures.

Uranium determination in natural water by the fissiontrack technique

USGS Publications Warehouse

Reimer, G.M.

1975-01-01

The fission track technique, utilizing the neutron-induced fission of uranium-235, provides a versatile analytical method for the routine analysis of uranium in liquid samples of natural water. A detector is immersed in the sample and both are irradiated. The fission track density observed in the detector is directly proportional to the uranium concentration. The specific advantages of this technique are: (1) only a small quantity of sample, typically 0.1-1 ml, is needed; (2) no sample concentration is necessary; (3) it is capable of providing analyses with a lower reporting limit of 1 ??g per liter; and (4) the actual time spent on an analysis can be only a few minutes. This paper discusses and describes the method. ?? 1975.

Rapid determination of tafenoquine in small volume human plasma samples by high-performance liquid chromatography-tandem mass spectrometry.

PubMed

Doyle, E; Fowles, S E; Summerfield, S; White, T J

2002-03-25

A method was developed for the determination of tafenoquine (I) in human plasma using high-performance liquid chromatography-tandem mass spectrometry. Prior to analysis, the protein in plasma samples was precipitated with methanol containing [2H3(15N)]tafenoquine (II) to act as an internal standard. The supernatant was injected onto a Genesis-C18 column without any further clean-up. The mass spectrometer was operated in the positive ion mode, employing a heat assisted nebulisation, electrospray interface. Ions were detected in multiple reaction monitoring mode. The assay required 50 microl of plasma and was precise and accurate within the range 2 to 500 ng/ml. The average within-run and between-run relative standard deviations were < 7% at 2 ng/ml and greater concentrations. The average accuracy of validation standards was generally within +/- 4% of the nominal concentration. There was no evidence of instability of I in human plasma following three complete freeze-thaw cycles and samples can safely be stored for at least 8 months at approximately -70 degrees C. The method was very robust and has been successfully applied to the analysis of clinical samples from patients and healthy volunteers dosed with I.

The simultaneous separation and determination of chloropropanols in soy sauce and other flavoring with gas chromatography-mass spectrometry in negative chemical and electron impact ionization modes.

PubMed

Xu, Xiaomin; Ren, Yiping; Wu, Pinggu; Han, Jianlong; Shen, Xianghong

2006-02-01

Both gas chromatography-mass spectrometry in electron ionization (GC-MS-EI) and negative chemical ionization (GC-MS-NCI) modes are reported in this paper for the simultaneous determination of 1,3-dichloropropan-2-ol (1,3-DCP), 2,3-dichloropropan-1-ol (2,3-DCP), 3-chloropropane-1,2-diol (3-MCPD) and 2-chloropropane-1,3-diol (2-MCPD) in soy sauce and other flavoring. D(5)-3-MCPD (for 3-MCPD and 2-MCPD) and d(5)-1,3-DCP (for 1,3-DCP and 2,3-DCP) were used as the deuterium isotopic labelled internal standards. The feasibility of using heptafluorobutyric anhydride modified with triethylamine (HFBA-Et(3)N) as a new derivatization reagent to replace heptafluorobutyrylimidazole (HFBI) is proposed. Liquid/liquid extraction with hexane was introduced for high lipid content samples. A small survey was carried out of soy sauces (103 samples) and instant noodles (45 samples) and the applicability of GC-MS-NCI and GC-MS-EI was assessed in these different matrices.

Rotor for processing liquids using movable capillary tubes

DOEpatents

Johnson, Wayne F.; Burtis, Carl A.; Walker, William A.

1989-01-01

A rotor assembly for processing liquids, especially whole blood samples, is disclosed. The assembly includes apparatus for separating non-liquid components of whole blood samples from liquid components, apparatus for diluting the separated liquid component with a diluent and apparatus for transferring the diluted sample to an external apparatus for analysis. The rotor assembly employs several movable capillary tubes to handle the sample and diluents. A method for using the rotor assembly to process liquids is also described.

Rotor for processing liquids using movable capillary tubes

DOEpatents

Johnson, Wayne F [Loudon, TN; Burtis, Carl A [Oak Ridge, TN; Walker, William A [Knoxville, TN

1989-05-30

A rotor assembly for processing liquids, especially whole blood samples, is disclosed. The assembly includes apparatus for separating non-liquid components of whole blood samples from liquid components, apparatus for diluting the separated liquid component with a diluent and apparatus for transferring the diluted sample to an external apparatus for analysis. The rotor assembly employs several movable capillary tubes to handle the sample and diluents. A method for using the rotor assembly to process liquids is also described.

Systems and methods for analyzing liquids under vacuum

DOEpatents

Yu, Xiao-Ying; Yang, Li; Cowin, James P.; Iedema, Martin J.; Zhu, Zihua

2013-10-15

Systems and methods for supporting a liquid against a vacuum pressure in a chamber can enable analysis of the liquid surface using vacuum-based chemical analysis instruments. No electrical or fluid connections are required to pass through the chamber walls. The systems can include a reservoir, a pump, and a liquid flow path. The reservoir contains a liquid-phase sample. The pump drives flow of the sample from the reservoir, through the liquid flow path, and back to the reservoir. The flow of the sample is not substantially driven by a differential between pressures inside and outside of the liquid flow path. An aperture in the liquid flow path exposes a stable portion of the liquid-phase sample to the vacuum pressure within the chamber. The radius, or size, of the aperture is less than or equal to a critical value required to support a meniscus of the liquid-phase sample by surface tension.

Principal component analysis of TOF-SIMS spectra, images and depth profiles: an industrial perspective

NASA Astrophysics Data System (ADS)

Pacholski, Michaeleen L.

2004-06-01

Principal component analysis (PCA) has been successfully applied to time-of-flight secondary ion mass spectrometry (TOF-SIMS) spectra, images and depth profiles. Although SIMS spectral data sets can be small (in comparison to datasets typically discussed in literature from other analytical techniques such as gas or liquid chromatography), each spectrum has thousands of ions resulting in what can be a difficult comparison of samples. Analysis of industrially-derived samples means the identity of most surface species are unknown a priori and samples must be analyzed rapidly to satisfy customer demands. PCA enables rapid assessment of spectral differences (or lack there of) between samples and identification of chemically different areas on sample surfaces for images. Depth profile analysis helps define interfaces and identify low-level components in the system.

Ionic liquid ultrasound-assisted dispersive liquid-liquid microextraction based on solidification of the aqueous phase for preconcentration of heavy metals ions prior to determination by LC-UV.

PubMed

Werner, Justyna

2018-05-15

Ionic liquid ultrasound-assisted dispersive liquid-liquid microextraction based on solidification of the aqueous phase was used for preconcentration of Ni 2+ , Co 2+ , Cd 2+ , Cu 2+ , Pb 2+ in natural water samples prior to liquid chromatography with UV detection. In the proposed method, the ammonium pyrrolidinedithiocarbamate was used as a complexing agent and the phosphonium ionic liquid trihexyl(tetradecyl)phosphonium bis[(2,4,4-trimethyl)pentyl]phosphinate (Cyphos IL 104) was used as an extractant. Ultrasound energy was used to disperse the extractant in the aqueous phase. After microextraction, the ionic liquid and aqueous phases were separated by centrifugation. Then the aqueous phase was frozen and the lighter than water ionic liquid phase containing metal ions complexes with pyrrolidinedithiocarbamate was separated and dissolved in a small volume of methanol prior to injection into the liquid chromatograph. Several parameters including the volume of extractant, the pH of the sample, the concentration of complexing agent, the time of ultrasound energy treatment, the time and speed of centrifugation and the effect of ionic strength were optimized. Under the optimized conditions (10 µL of Cyphos IL 104, pH = 5, 0.3% w/v ammonium pyrrolidinedithiocarbamate, 60 s of ultrasound use, 5 min/5000 rpm (2516×g) of centrifugation, 2.0 mg of NaCl), preconcentration factors were 211, 210, 209, 207 and 211 for Ni 2+ , Co 2+ , Cd 2+ , Cu 2+ and Pb 2+ respectively. Linearity was observed in the ranges 0.2-75.0 µg L -1 for Pb 2+ , Cd 2+ , Co 2+ and 0.5-100.0 µg L -1 for Cu 2+ , Ni 2+ . The limits of detection were 0.03 µg L -1 for Ni 2+ , 0.03 µg L -1 for Co 2+ , 0.03 µg L -1 for Cd 2+ , 0.02 µg L -1 for Cu 2+ , 0.02 µg L -1 for Pb 2+ , respectively. The accuracy of this method was evaluated by preconcentration and determination of Ni 2+ , Co 2+ , Cd 2+ , Cu 2+ , Pb 2+ in certified reference materials (TMRAIN-04 and NIST 1643e) with the recovery values in the range of 97-102%. The presented method has been successfully applied for the determination of analytes in natural water samples (river and lake waters). Copyright © 2018 Elsevier B.V. All rights reserved.

Mixed hemimicelles solid-phase extraction based on ionic liquid-coated Fe3O4/SiO2 nanoparticles for the determination of flavonoids in bio-matrix samples coupled with high performance liquid chromatography.

PubMed

He, Huan; Yuan, Danhua; Gao, Zhanqi; Xiao, Deli; He, Hua; Dai, Hao; Peng, Jun; Li, Nan

2014-01-10

A novel magnetic solid-phase extraction (MSPE) method based on mixed hemimicelles of room temperature ionic liquids (RTILs) coated Fe3O4/SiO2 nanoparticles (NPs) was developed for simultaneous extraction of trace amounts of flavonoids in bio-matrix samples. A comparative study on the use of RTILs (C16mimBr) and CTAB-coated Fe3O4/SiO2 NPs as sorbents was presented. Owing to bigger adsorption amounts for analytes, RTILs-coated Fe3O4/SiO2 NPs was selected as MSPE materials and three analytes luteolin, quercetin and kaempferol can be quantitatively extracted and simultaneously determined coupled with high performance liquid chromatography (HPLC) in urine samples. No interferences were caused by proteins or endogenous compounds. Good linearity (R(2)>0.9993) for all calibration curves was obtained, and the limits of detection (LOD) for luteolin, quercetin and kaempferol were 0.10 ng/mL, 0.50 ng/mL and 0.20 ng/mL in urine samples, respectively. Satisfactory recoveries (93.5-97.6%, 90.1-95.4% and 93.3-96.6% for luteolin, quercetin and kaempferol) in biological matrices were achieved. It was notable that while using a small amount of Fe3O4/SiO2 NPs (4.0 mg) and C16mimBr (1.0 mg), satisfactory preconcentration factors and extraction recoveries for the three flavonoids were obtained. To the best of our knowledge, this is the first time a mixed hemimicelles MSPE method based on RTILs and Fe3O4/SiO2 NPs magnetic separation has ever been used for pretreatment of complex biological samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Enhanced electrocatalytic activity of reduced graphene oxide-Os nanoparticle hybrid films obtained at a liquid/liquid interface

NASA Astrophysics Data System (ADS)

Bramhaiah, K.; Pandey, Indu; Singh, Vidya N.; Kavitha, C.; John, Neena S.

2018-03-01

Hybrid films of reduced graphene oxide-osmium nanoparticles (rGO-Os NPs) synthesized at a liquid/liquid interface are explored for their electrocatalytic activity towards the oxidation of rhodamine B (RhB), a popular colourant found in textile industry effluents and a non-permitted food colour. The free-standing nature of the films enables them to be lifted directly on to electrodes without the aid of any binders. The films consist of aggregates of ultra-small Os NPs interspersed with rGO layers. The hybrid film exhibits enhanced RhB oxidation when compared to its constituents arising from the synergic effect between rGO and Os NPs, Os contributing to electrocatalysis and rGO contributing to high surface area and conductance as well as stabilization of Os nanoparticles. The electrochemical sensor based on rGO-Os NP hybrid film on pencil graphite electrode shows a remarkable performance for the quantitative detection of RhB with a linear variation in a wide range of concentrations, 4-1300 ppb (8.3 nM-2.71 μM). The modified electrode presents good stability over more than 6 months, reproducibility and anti-interference capability. The use of developed sensor for adequate detection of RhB in real samples such as food samples and pen markers is also demonstrated.

Ultrasound-assisted dispersive liquid-liquid microextraction for the determination of seven recreational drugs in human whole blood using gas chromatography-mass spectrometry.

PubMed

Lin, Zebin; Li, Jiaolun; Zhang, Xinyu; Qiu, Meihong; Huang, Zhibin; Rao, Yulan

2017-03-01

Recreational drugs have large impact on public health and security, and to monitor them is of urgent demand. In the present study, ultrasound-assisted dispersive liquid-liquid microextraction combined with the detection of gas chromatography-mass spectrometry was applied to the determination of seven common recreational drugs, including amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, meperidine, methadone and ketamine in 200μL of human whole blood. A series of factors which would affect the extraction efficiency were systematically investigated, including the nature and the volume of extraction and dispersing solvents, ultrasonication time, salting-out effect and pH value. The method consumed small amount of sample. The limits of detection and limits of quantification for each analyte were 10 and 40ng/mL, respectively, and the linearity was in the range of 0.04-25μg/mL (R 2 higher than 0.99). Good specificity, precision (1.5-8.2% for the intra-day study and 2.6-12.8% for the inter-day study), satisfactory accuracy (85.0-117.1%) and extraction recovery (77.0-92.4%) were obtained, which makes it a high performance method for the determination of recreational drugs in human whole blood samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Cancer Liquid Biopsy: Is It Ready for Clinic?

PubMed

Pan, Ying; Ji, John S; Jin, Jason Gang; Kuo, Winston Patrick; Kang, Hongjun

2017-01-01

The management of cancer relies on a combination of imaging and tissue biopsy for diagnosis, monitoring, and molecular classification-based patient stratification to ensure appropriate treatment. Conventional tissue biopsy harvests tumor samples with invasive procedures, which are often difficult for patients with advanced disease. Given the well-recognized intratumor genetic heterogeneity [1], the biopsy of small tumor fragments does not necessarily represent all the genetic aberrations in the tumor, but sampling the entire tumor in each patient is not realistic. Moreover, tumors evolve all the time from local to advanced disease and by adapting to selective pressure from treatment.

Procedure for Uranium-Molybdenum Density Measurements and Porosity Determination

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

Prabhakaran, Ramprashad; Devaraj, Arun; Joshi, Vineet V.

2016-08-13

The purpose of this document is to provide guidelines for preparing uranium-molybdenum (U-Mo) specimens, performing density measurements, and computing sample porosity. Typical specimens (solids) will be sheared to small rectangular foils, disks, or pieces of metal. A mass balance, solid density determination kit, and a liquid of known density will be used to determine the density of U-Mo specimens using the Archimedes principle. A standard test weight of known density would be used to verify proper operation of the system. By measuring the density of a U-Mo sample, it is possible to determine its porosity.

Temperature Gradients on the Cell Wall in the Critical Viscosity Experiment

NASA Technical Reports Server (NTRS)

Berg, Robert F.; Moldover, Michael R.

1993-01-01

Because of the diverging susceptibility delta rho/delta Tau near the liquid-vapor critical point, temperature gradients must be kept small to maintain adequate sample homogeneity. In our Science Requirements Document we paid particular attention to radial density gradients caused by equilibration of the xenon sample. Axial density gradients were addressed through the requirement that the cell's copper wall have a gradient less than 22 microK/m. This report re-examines the cell wall's temperature distribution in more detail by estimating all known significant contributions to temperature differences on the cell's wall.

Blister pouches for effective reagent storage and release for low cost point-of-care diagnostic applications

NASA Astrophysics Data System (ADS)

Smith, Suzanne; Sewart, Rene; Land, Kevin; Roux, Pieter; Gärtner, Claudia; Becker, Holger

2016-03-01

Lab-on-a-chip devices are often applied to point-of-care diagnostic solutions as they are low-cost, compact, disposable, and require only small sample volumes. For such devices, various reagents are required for sample preparation and analysis and, for an integrated solution to be realized, on-chip reagent storage and automated introduction are required. This work describes the implementation and characterization of effective liquid reagent storage and release mechanisms utilizing blister pouches applied to various point-of-care diagnostic device applications. The manufacturing aspects as well as performance parameters are evaluated.

Airborne chemistry: acoustic levitation in chemical analysis.

PubMed

Santesson, Sabina; Nilsson, Staffan

2004-04-01

This review with 60 references describes a unique path to miniaturisation, that is, the use of acoustic levitation in analytical and bioanalytical chemistry applications. Levitation of small volumes of sample by means of a levitation technique can be used as a way to avoid solid walls around the sample, thus circumventing the main problem of miniaturisation, the unfavourable surface-to-volume ratio. Different techniques for sample levitation have been developed and improved. Of the levitation techniques described, acoustic or ultrasonic levitation fulfils all requirements for analytical chemistry applications. This technique has previously been used to study properties of molten materials and the equilibrium shape()and stability of liquid drops. Temperature and mass transfer in levitated drops have also been described, as have crystallisation and microgravity applications. The airborne analytical system described here is equipped with different and exchangeable remote detection systems. The levitated drops are normally in the 100 nL-2 microL volume range and additions to the levitated drop can be made in the pL-volume range. The use of levitated drops in analytical and bioanalytical chemistry offers several benefits. Several remote detection systems are compatible with acoustic levitation, including fluorescence imaging detection, right angle light scattering, Raman spectroscopy, and X-ray diffraction. Applications include liquid/liquid extractions, solvent exchange, analyte enrichment, single-cell analysis, cell-cell communication studies, precipitation screening of proteins to establish nucleation conditions, and crystallisation of proteins and pharmaceuticals.

Rotor for processing liquids using movable capillary tubes

DOEpatents

Johnson, W.F.; Burtis, C.A.; Walker, W.A.

1987-07-17

A rotor assembly for processing liquids, especially whole blood samples, is disclosed. The assembly includes apparatus for separating non-liquid components of whole blood samples from liquid components, apparatus for diluting the separated liquid component with a diluent and apparatus for transferring the diluted sample to an external apparatus for analysis. The rotor assembly employs several movable capillary tubes to handle the sample and diluents. A method for using the rotor assembly to process liquids is also described. 5 figs.

Design and performance of a new continuous-flow sample-introduction system for flame infrared-emission spectrometry: Applications in process analysis, flow injection analysis, and ion-exchange high-performance liquid chromatography.

PubMed

Lam, C K; Zhang, Y; Busch, M A; Busch, K W

1993-06-01

A new sample introduction system for the analysis of continuously flowing liquid streams by flame infrared-emission (FIRE) spectrometry has been developed. The system uses a specially designed purge cell to strip dissolved CO(2) from solution into a hydrogen gas stream that serves as the fuel for a hydrogen/air flame. Vibrationally excited CO(2) molecules present in the flame are monitored with a simple infrared filter (4.4 mum) photometer. The new system can be used to introduce analytes as a continuous liquid stream (process analysis mode) or on a discrete basis by sample injection (flow injection analysis mode). The key to the success of the method is the new purge-cell design. The small internal volume of the cell minimizes problems associated with purge-cell clean-out and produces sharp, reproducible signals. Spent analytical solution is continuously drained from the cell, making cell disconnection and cleaning between samples unnecessary. Under the conditions employed in this study, samples could be analyzed at a maximum rate of approximately 60/h. The new sample introduction system was successfully tested in both a process analysis- and a flow injection analysis mode for the determination of total inorganic carbon in Waco tap water. For the first time, flame infrared-emission spectrometry was successfully extended to non-volatile organic compounds by using chemical pretreatment with peroxydisulfate in the presence of silver ion to convert the analytes into dissolved carbon dioxide, prior to purging and detection by the FIRE radiometer. A test of the peroxydisulfate/Ag(+) reaction using six organic acids and five sugars indicated that all 11 compounds were oxidized to nearly the same extent. Finally, the new sample introduction system was used in conjunction with a simple filter FIRE radiometer as a detection system in ion-exchange high-performance liquid chromatography. Ion-exchange chromatograms are shown for two aqueous mixtures, one containing six organic acids and the second containing six mono-, di-, and trisaccharides.

Capillary pumping independent of the liquid surface energy and viscosity

NASA Astrophysics Data System (ADS)

Guo, Weijin; Hansson, Jonas; van der Wijngaart, Wouter

2018-03-01

Capillary pumping is an attractive means of liquid actuation because it is a passive mechanism, i.e., it does not rely on an external energy supply during operation. The capillary flow rate generally depends on the liquid sample viscosity and surface energy. This poses a problem for capillary-driven systems that rely on a predictable flow rate and for which the sample viscosity or surface energy are not precisely known. Here, we introduce the capillary pumping of sample liquids with a flow rate that is constant in time and independent of the sample viscosity and sample surface energy. These features are enabled by a design in which a well-characterized pump liquid is capillarily imbibed into the downstream section of the pump and thereby pulls the unknown sample liquid into the upstream pump section. The downstream pump geometry is designed to exert a Laplace pressure and fluidic resistance that are substantially larger than those exerted by the upstream pump geometry on the sample liquid. Hence, the influence of the unknown sample liquid on the flow rate is negligible. We experimentally tested pumps of the new design with a variety of sample liquids, including water, different samples of whole blood, different samples of urine, isopropanol, mineral oil, and glycerol. The capillary filling speeds of these liquids vary by more than a factor 1000 when imbibed to a standard constant cross-section glass capillary. In our new pump design, 20 filling tests involving these liquid samples with vastly different properties resulted in a constant volumetric flow rate in the range of 20.96-24.76 μL/min. We expect this novel capillary design to have immediate applications in lab-on-a-chip systems and diagnostic devices.

Superconducting Quantum Interferometers for Nondestructive Evaluation

PubMed Central

Kostyurina, E. A.; Kalashnikov, K. V.; Maslennikov, Yu. V.; Koshelets, V. P.

2017-01-01

We review stationary and mobile systems that are used for the nondestructive evaluation of room temperature objects and are based on superconducting quantum interference devices (SQUIDs). The systems are optimized for samples whose dimensions are between 10 micrometers and several meters. Stray magnetic fields from small samples (10 µm–10 cm) are studied using a SQUID microscope equipped with a magnetic flux antenna, which is fed through the walls of liquid nitrogen cryostat and a hole in the SQUID’s pick-up loop and returned sidewards from the SQUID back to the sample. The SQUID microscope does not disturb the magnetization of the sample during image recording due to the decoupling of the magnetic flux antenna from the modulation and feedback coil. For larger samples, we use a hand-held mobile liquid nitrogen minicryostat with a first order planar gradiometric SQUID sensor. Low-Tc DC SQUID systems that are designed for NDE measurements of bio-objects are able to operate with sufficient resolution in a magnetically unshielded environment. High-Tc DC SQUID magnetometers that are operated in a magnetic shield demonstrate a magnetic field resolution of ~4 fT/√Hz at 77 K. This sensitivity is improved to ~2 fT/√Hz at 77 K by using a soft magnetic flux antenna. PMID:29210980

Quantification of the xenoestrogens 4-tert.-octylphenol and bisphenol A in water and in fish tissue based on microwave assisted extraction, solid-phase extraction and liquid chromatography-mass spectrometry.

PubMed

Pedersen, S N; Lindholst, C

1999-12-09

Extraction methods were developed for quantification of the xenoestrogens 4-tert.-octylphenol (tOP) and bisphenol A (BPA) in water and in liver and muscle tissue from the rainbow trout (Oncorhynchus mykiss). The extraction of tOP and BPA from tissue samples was carried out using microwave-assisted solvent extraction (MASE) followed by solid-phase extraction (SPE). Water samples were extracted using only SPE. For the quantification of tOP and BPA, liquid chromatography mass spectrometry (LC-MS) equipped with an atmospheric pressure chemical ionisation interface (APCI) was applied. The combined methods for tissue extraction allow the use of small sample amounts of liver or muscle (typically 1 g), low volumes of solvent (20 ml), and short extraction times (25 min). Limits of quantification of tOP in tissue samples were found to be approximately 10 ng/g in muscle and 50 ng/g in liver (both based on 1 g of fresh tissue). The corresponding values for BPA were approximately 50 ng/g in both muscle and liver tissue. In water, the limit of quantification for tOP and BPA was approximately 0.1 microg/l (based on 100 ml sample size).

An improved analytical strategy combining microextraction by packed sorbent combined with ultra high pressure liquid chromatography for the determination of fluoxetine, clomipramine and their active metabolites in human urine.

PubMed

Alves, Vera; Gonçalves, João; Conceição, Carlota; Teixeira, Helena M; Câmara, José S

2015-08-21

A powerful and sensitive method, by microextraction packed sorbent (MEPS), and ultra-high performance liquid chromatography (UHPLC) with a photodiode array (PDA) detection, is described for the determination of fluoxetine, clomipramine and their active metabolites in human urine samples. The MEPS variables, such as sample volume, pH, number of extraction cycles (draw-eject), and desorption conditions (solvent and solvent volume of elution) were optimized. The analysis were carried out using small sample volumes (500μL) and in a short time period (5min for the entire sample preparation step). Good linearity was obtained for all antidepressants with the correlation coefficients (R(2)) above 0.9965. The limits of detection (LOD) ranged from 0.068 to 0.087μgmL(-1). The recoveries were from 93% to 98%, with relative standard deviations less than 6%. The inter-day precision, expressed as the relative standard deviation, varied between 3.8% and 8.5% while the intra-day precision between 3.0% and 7.1%. In order to evaluate the proposed method for clinical use, the MEPS/UHPLC-PDA method was applied to analysis of urine samples from depressed patients. Copyright © 2015 Elsevier B.V. All rights reserved.

In vivo microsampling to capture the elusive exposome

NASA Astrophysics Data System (ADS)

Bessonneau, Vincent; Ings, Jennifer; McMaster, Mark; Smith, Richard; Bragg, Leslie; Servos, Mark; Pawliszyn, Janusz

2017-03-01

Loss and/or degradation of small molecules during sampling, sample transportation and storage can adversely impact biological interpretation of metabolomics data. In this study, we performed in vivo sampling using solid-phase microextraction (SPME) in combination with non-targeted liquid chromatography and high-resolution tandem mass spectrometry (LC-MS/MS) to capture the fish tissue exposome using molecular networking analysis, and the results were contrasted with molecular differences obtained with ex vivo SPME sampling. Based on 494 MS/MS spectra comparisons, we demonstrated that in vivo SPME sampling provided better extraction and stabilization of highly reactive molecules, such as 1-oleoyl-sn-glycero-3-phosphocholine and 1-palmitoleoyl-glycero-3-phosphocholine, from fish tissue samples. This sampling approach, that minimizes sample handling and preparation, offers the opportunity to perform longitudinal monitoring of the exposome in biological systems and improve the reliability of exposure-measurement in exposome-wide association studies.

In vivo microsampling to capture the elusive exposome

PubMed Central

Bessonneau, Vincent; Ings, Jennifer; McMaster, Mark; Smith, Richard; Bragg, Leslie; Servos, Mark; Pawliszyn, Janusz

2017-01-01

Loss and/or degradation of small molecules during sampling, sample transportation and storage can adversely impact biological interpretation of metabolomics data. In this study, we performed in vivo sampling using solid-phase microextraction (SPME) in combination with non-targeted liquid chromatography and high-resolution tandem mass spectrometry (LC-MS/MS) to capture the fish tissue exposome using molecular networking analysis, and the results were contrasted with molecular differences obtained with ex vivo SPME sampling. Based on 494 MS/MS spectra comparisons, we demonstrated that in vivo SPME sampling provided better extraction and stabilization of highly reactive molecules, such as 1-oleoyl-sn-glycero-3-phosphocholine and 1-palmitoleoyl-glycero-3-phosphocholine, from fish tissue samples. This sampling approach, that minimizes sample handling and preparation, offers the opportunity to perform longitudinal monitoring of the exposome in biological systems and improve the reliability of exposure-measurement in exposome-wide association studies. PMID:28266605

Delivery of Formulated Industrial Enzymes with Acoustic Technology.

PubMed

Hwang, Jennifer Dorcas; Ortiz-Maldonado, Mariliz; Paramonov, Sergey

2016-02-01

Industrial enzymes are instrumental in many applications, including carbohydrate processing, fabric and household care, biofuels, food, and animal nutrition, among others. Enzymes have to be active and stable not only in harsh application conditions, but also during shipment and storage. In protein stability studies, formulated concentrated enzyme solutions are frequently diluted gravimetrically prior to enzyme activity measurements, making it challenging to move toward more high-throughput techniques using conventional robotic equipment. Current assay methods pose difficulties when measuring highly concentrated proteins. For example, plastic pipette tips can introduce error because proteins adsorb to the tip surface, despite the presence of detergents, decreasing precision and overall efficiency of protein activity assays. Acoustic liquid handling technology, frequently used for various dilute small-molecule assays, may overcome such problems. Originally shown to effectively deliver dilute solutions of small molecules, this technology is used here as an effective alternative to the aforementioned challenge with viscous concentrated protein solutions. Because the acoustic liquid handler transfers nanoliter quantities of liquids without using pipette tips and without sample loss, it rapidly and uniformly prepares assay plates for enzyme activity measurements within minutes. This increased efficiency transforms the nature of enzyme stability studies toward high precision and throughput. © 2015 Society for Laboratory Automation and Screening.

Performance evaluation of laser induced breakdown spectroscopy in the measurement of liquid and solid samples

NASA Astrophysics Data System (ADS)

Bilge, Gonca; Sezer, Banu; Boyaci, Ismail Hakki; Eseller, Kemal Efe; Berberoglu, Halil

2018-07-01

Liquid analysis by using LIBS is a complicated process due to difficulties encountered during the collection of light and formation of plasma in liquid. To avoid these, some applications are performed such as aerosol formation and transforming liquid into solid state. However, performance of LIBS in liquid samples still remains a challenging issue. In this study, performance evaluation of LIBS and parameter optimizations in liquid and solid phase samples were performed. For this purpose, milk was chosen as model sample; milk powder was used as solid sample, and milk was used as liquid sample in the experiments. Different experimental setups have been constructed for each sampling technique, and optimizations were performed to determine suitable parameters such as delay time, laser energy, repetition rate and speed of rotary table for solid sampling technique, and flow rate of carrier gas for liquid sampling technique. Target element was determined as Ca, which is a critically important element in milk for determining its nutritional value and Ca addition. In optimum parameters, limit of detection (LOD), limit of quantification (LOQ) and relative standard deviation (RSD) values were calculated as 0.11%, 0.36% and 8.29% respectively for milk powders samples; while LOD, LOQ and RSD values were calculated as 0.24%, 0.81%, and 10.93% respectively for milk samples. It can be said that LIBS is an applicable method in both liquid and solid samples with suitable systems and parameters. However, liquid analysis requires much more developed systems for more accurate results.

Real Space Imaging of Nanoparticle Assembly at Liquid-Liquid Interfaces with Nanoscale Resolution.

PubMed

Costa, Luca; Li-Destri, Giovanni; Thomson, Neil H; Konovalov, Oleg; Pontoni, Diego

2016-09-14

Bottom up self-assembly of functional materials at liquid-liquid interfaces has recently emerged as method to design and produce novel two-dimensional (2D) nanostructured membranes and devices with tailored properties. Liquid-liquid interfaces can be seen as a "factory floor" for nanoparticle (NP) self-assembly, because NPs are driven there by a reduction of interfacial energy. Such 2D assembly can be characterized by reciprocal space techniques, namely X-ray and neutron scattering or reflectivity. These techniques have drawbacks, however, as the structural information is averaged over the finite size of the radiation beam and nonperiodic isolated assemblies in 3D or defects may not be easily detected. Real-space in situ imaging methods are more appropriate in this context, but they often suffer from limited resolution and underperform or fail when applied to challenging liquid-liquid interfaces. Here, we study the surfactant-induced assembly of SiO2 nanoparticle monolayers at a water-oil interface using in situ atomic force microscopy (AFM) achieving nanoscale resolved imaging capabilities. Hitherto, AFM imaging has been restricted to solid-liquid interfaces because applications to liquid interfaces have been hindered by their softness and intrinsic dynamics, requiring accurate sample preparation methods and nonconventional AFM operational schemes. Comparing both AFM and grazing incidence X-ray small angle scattering data, we unambiguously demonstrate correlation between real and reciprocal space structure determination showing that the average interfacial NP density is found to vary with surfactant concentration. Additionally, the interaction between the tip and the interface can be exploited to locally determine the acting interfacial interactions. This work opens up the way to studying complex nanostructure formation and phase behavior in a range of liquid-liquid and complex liquid interfaces.

Sample types applied for molecular diagnosis of therapeutic management of advanced non-small cell lung cancer in the precision medicine.

PubMed

Han, Yanxi; Li, Jinming

2017-10-26

In this era of precision medicine, molecular biology is becoming increasingly significant for the diagnosis and therapeutic management of non-small cell lung cancer. The specimen as the primary element of the whole testing flow is particularly important for maintaining the accuracy of gene alteration testing. Presently, the main sample types applied in routine diagnosis are tissue and cytology biopsies. Liquid biopsies are considered as the most promising alternatives when tissue and cytology samples are not available. Each sample type possesses its own strengths and weaknesses, pertaining to the disparity of sampling, preparation and preservation procedures, the heterogeneity of inter- or intratumors, the tumor cellularity (percentage and number of tumor cells) of specimens, etc., and none of them can individually be a "one size to fit all". Therefore, in this review, we summarized the strengths and weaknesses of different sample types that are widely used in clinical practice, offered solutions to reduce the negative impact of the samples and proposed an optimized strategy for choice of samples during the entire diagnostic course. We hope to provide valuable information to laboratories for choosing optimal clinical specimens to achieve comprehensive functional genomic landscapes and formulate individually tailored treatment plans for NSCLC patients that are in advanced stages.

Adiabatic Compression Sensitivity of Liquid Fuels and Monopropellants

NASA Technical Reports Server (NTRS)

Ismail, Ismail M. K.; Hawkins, Tom W.

2000-01-01

Liquid rocket propellants can be sensitive to rapid compression. Such liquids may undergo decomposition and their handling may be accompanied with risk. Decomposition produces small gas bubbles in the liquid, which upon rapid compression may cause catastrophic explosions. The rapid compression can result from mechanical shocks applied on the tank containing the liquid or from rapid closure of the valves installed on the lines. It is desirable to determine the conditions that may promote explosive reactions. At Air Force Research Laboratory (AFRL), we constructed an apparatus and established a safe procedure for estimating the sensitivity of propellant materials towards mechanical shocks (Adiabatic Compression Tester). A sample is placed on a stainless steel U-tube, held isothermally at a temperature between 20 and 150 C then exposed to an abrupt mechanical shock of nitrogen gas at a pressure between 6.9 and 20.7 MPa (1000 to 3000 psi). The apparatus is computer interfaced and is driven with LABTECH NOTEBOOK-pro (registered) Software. In this presentation, the design of the apparatus is shown, the operating procedure is outlined, and the safety issues are addressed. The results obtained on different energetic materials are presented.

A study of the acoustic-optic effect in nematics

NASA Astrophysics Data System (ADS)

Hayes, C. F.

1980-12-01

The program of this contract has been to study the acousto-optic effect which occurs in nematic liquid crystals when excited by acoustic waves. Both theory and practical application are presented. Hydrodynamic equations were solved which govern the streaming and obtained a solution for the magnitude of the fluid speed and flow pattern for a small disc shaped liquid crystal. A sample, doped with grains, was used to test the solution experimentally. A series of cells was constructed and tested which, in fact, showed that an acoustic wavefront pattern can be visualized with this technique. During the second year of the contract we developed and tested a mathematical model which prescribes how a cell should be constructed in terms of: the densities of the cell walls, liquid crystal, and surrounding fluids; the thickness of the cell walls and liquid crystal layer; the acoustic speeds in cell wall (shear and longitudinal), liquid crystal, and surrounding fluids; acoustic frequency; and the incident acoustic bean angle. Cells were also constructed and tested in which an electric field could be applied simultaneously with the acoustic wave in such a way that the sensitivity of the cell to the acoustic field could be adjusted.

40 CFR 761.269 - Sampling liquid PCB remediation waste.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Sampling liquid PCB remediation waste..., AND USE PROHIBITIONS Cleanup Site Characterization Sampling for PCB Remediation Waste in Accordance with § 761.61(a)(2) § 761.269 Sampling liquid PCB remediation waste. (a) If the liquid is single phase...

Determination of Total Soy Isoflavones in Dietary Supplements, Supplement Ingredients, and Soy Foods by High-Performance Liquid Chromatography with Ultraviolet Detection: Collaborative Study

PubMed Central

Collison, Mark W.

2008-01-01

An interlaboratory study was conducted to evaluate a method for determining total soy isoflavones in dietary supplements, dietary supplement ingredients, and soy foods. Isoflavones were extracted using aqueous acetonitrile containing a small amount of dimethylsulfoxide (DMSO) and all 12 of the naturally occuring isoflavones in soy were determined by high-performance liquid Chromatography (HPLC) with UV detection using apigenin as an internal standard. Fifteen samples (6 pairs of blind duplicates plus 3 additional samples) of soy isoflavone ingredients, soy isoflavone dietary supplements, soy flour, and soy protein products were successfully analyzed by 13 collaborating laboratories in 6 countries. For repeatability, the relative standard deviations (RSDr) ranged from 1.07 for samples containing over 400 mg/g total isoflavones to 3.31 for samples containing 0.87 mg/g total isoflavones, and for reproducibility the RSDR values ranged from 2.29 for samples containing over 400 mg/g total isoflavones to 9.36 for samples containing 0.87 mg/g total isoflavones. HorRat values ranged from 1.00 to 1.62 for all samples containing at least 0.8 mg/g total isoflavones. One sample, containing very low total isoflavones (<0.05 mg/g), gave RSDR values of 175 and a HorRat value of 17.6. This sample was deemed to be below the usable range of the method. The method provides accurate and precise results for analysis of soy isoflavones in dietary supplements and soy foods. PMID:18567292

Determination of total soy isoflavones in dietary supplements, supplement ingredients, and soy foods by high-performance liquid chromatography with ultraviolet detection: collaborative study.

PubMed

Collison, Mark W

2008-01-01

An interlaboratory study was conducted to evaluate a method for determining total soy isoflavones in dietary supplements, dietary supplement ingredients, and soy foods. Isoflavones were extracted using aqueous acetonitrile containing a small amount of dimethylsulfoxide (DMSO) and all 12 of the naturally occuring isoflavones in soy were determined by high-performance liquid chromatography (HPLC) with UV detection using apigenin as an internal standard. Fifteen samples (6 pairs of blind duplicates plus 3 additional samples) of soy isoflavone ingredients, soy isoflavone dietary supplements, soy flour, and soy protein products were successfully analyzed by 13 collaborating laboratories in 6 countries. For repeatability, the relative standard deviations (RSDr) ranged from 1.07 for samples containing over 400 mglg total isoflavones to 3.31 for samples containing 0.87 mg/g total isoflavones, and for reproducibility the RSDR values ranged from 2.29 for samples containing over 400 mg/g total isoflavones to 9.36 for samples containing 0.87 mg/g total isoflavones. HorRat values ranged from 1.00 to 1.62 for all samples containing at least 0.8 mg/g total isoflavones. One sample, containing very low total isoflavones (< 0.05 mg/g), gave RSDR values of 175 and a HorRat value of 17.6. This sample was deemed to be below the usable range of the method. The method provides accurate and precise results for analysis of soy isoflavones in dietary supplements and soy foods.

Drying regimes in homogeneous porous media from macro- to nanoscale

NASA Astrophysics Data System (ADS)

Thiery, J.; Rodts, S.; Weitz, D. A.; Coussot, P.

2017-07-01

Magnetic resonance imaging visualization down to nanometric liquid films in model porous media with pore sizes from micro- to nanometers enables one to fully characterize the physical mechanisms of drying. For pore size larger than a few tens of nanometers, we identify an initial constant drying rate period, probing homogeneous desaturation, followed by a falling drying rate period. This second period is associated with the development of a gradient in saturation underneath the sample free surface that initiates the inward recession of the contact line. During this latter stage, the drying rate varies in accordance with vapor diffusion through the dry porous region, possibly affected by the Knudsen effect for small pore size. However, we show that for sufficiently small pore size and/or saturation the drying rate is increasingly reduced by the Kelvin effect. Subsequently, we demonstrate that this effect governs the kinetics of evaporation in nanopores as a homogeneous desaturation occurs. Eventually, under our experimental conditions, we show that the saturation unceasingly decreases in a homogeneous manner throughout the wet regions of the medium regardless of pore size or drying regime considered. This finding suggests the existence of continuous liquid flow towards the interface of higher evaporation, down to very low saturation or very small pore size. Paradoxically, even if this net flow is unidirectional and capillary driven, it corresponds to a series of diffused local capillary equilibrations over the full height of the sample, which might explain that a simple Darcy's law model does not predict the effect of scaling of the net flow rate on the pore size observed in our tests.

Instability in radiatively melted silicon films

NASA Astrophysics Data System (ADS)

Jackson, K. A.; Kurtze, Douglas A.

1985-04-01

Bosch and Lemons [Phys. Rev. Letters 47 (1981) 1151] were first to report that on heating of silicon with a laser, the heated area can break up into small regions of solid and liquid. Thus phenomenon produces undesirable surface roughness on silicon which has been melted using irradiation from a laser or heat lamps. It is due to the higher reflectivity of liquid silicon so that radiative heating produces small regions of superheated solid in contact with small regions of supercooled liquid. In this paper, the instabilities resulting from this unusual thermal situation have been analyzed. It is shown that a stable pattern can develop provided that the spacing between the solid and liquid is small enough. For a 1/2 μm thick layer of polysilicon on silica, the calculated stable spacing is less than about 10 μm, in accord with experiment.

Physical Properties of Liquid Fe-S Alloys at High Pressure

NASA Astrophysics Data System (ADS)

Antonangeli, D.; Morard, G.; Marret, A.; Prescher, C.; Boulard, E.; Mezouar, M.; Rivoldini, A.

2016-12-01

Sulfur is classically considered the dominant light element alloyed to iron in the core of small telluric planets such as Mercury and Mars. The expected pressure (P) and temperature (T) conditions are: P between 6 and 40 GPa and T between 1300 and 2300 K for Mercury's core and P between 24 and 42 GPa and T between 1800 and 2600 K for Mars'core. The presence of an internally generated magnetic field and the amplitude of its 88d libration support the liquid nature of a portion of Merury's core, and various independent lines of evident suggest that Mars's core has been liquid throughout its history. However, as only few experiments, mostly based on sink/float methods studied liquid Fe-S alloys, little is known about the physical properties at these P-T conditions, greatly limiting our capability to produce accurate planetary models. Here we present results of in-situ x-ray diffraction experiments on Fe-S liquids compressed in laser heated diamond anvil cell and of ex-situ electron microcopy analysis of the recovered samples. Our data allowed us to determine the evolution of the eutectic composition with pressure and to establish the eutectic melting curve up to 50 GPa. The x-ray diffuse signal from the liquid is analyzed to derive the density and compressibility of the Fe-S liquid alloys as a function of the S content.

A smartphone controlled handheld microfluidic liquid handling system.

PubMed

Li, Baichen; Li, Lin; Guan, Allan; Dong, Quan; Ruan, Kangcheng; Hu, Ronggui; Li, Zhenyu

2014-10-21

Microfluidics and lab-on-a-chip technologies have made it possible to manipulate small volume liquids with unprecedented resolution, automation and integration. However, most current microfluidic systems still rely on bulky off-chip infrastructures such as compressed pressure sources, syringe pumps and computers to achieve complex liquid manipulation functions. Here, we present a handheld automated microfluidic liquid handling system controlled by a smartphone, which is enabled by combining elastomeric on-chip valves and a compact pneumatic system. As a demonstration, we show that the system can automatically perform all the liquid handling steps of a bead-based HIV1 p24 sandwich immunoassay on a multi-layer PDMS chip without any human intervention. The footprint of the system is 6 × 10.5 × 16.5 cm, and the total weight is 829 g including battery. Powered by a 12.8 V 1500 mAh Li battery, the system consumed 2.2 W on average during the immunoassay and lasted for 8.7 h. This handheld microfluidic liquid handling platform is generally applicable to many biochemical and cell-based assays requiring complex liquid manipulation and sample preparation steps such as FISH, PCR, flow cytometry and nucleic acid sequencing. In particular, the integration of this technology with read-out biosensors may help enable the realization of the long-sought Tricorder-like handheld in vitro diagnostic (IVD) systems.

ALK status testing in non-small-cell lung carcinoma by FISH on ThinPrep slides with cytology material.

PubMed

Minca, Eugen C; Lanigan, Christopher P; Reynolds, Jordan P; Wang, Zhen; Ma, Patrick C; Cicenia, Joseph; Almeida, Francisco A; Pennell, Nathan A; Tubbs, Raymond R

2014-04-01

Oncogenic anaplastic lymphoma kinase (ALK) gene rearrangements in non-small-cell lung carcinomas (NSCLC) provide the basis for targeted therapy with crizotinib and other specific ALK inhibitors. Treatment eligibility is conventionally determined by the Food and Drug Administration-approved companion diagnostic fluorescence in situ hybridization (FISH) assay on paraffin-embedded tissue (PET). On limited samples such as fine needle aspiration-derived cytoblocks, FISH for ALK is often uninformative. FISH performed on liquid-based ThinPrep slides (ThinPrep-FISH) may represent a robust alternative. Two hundred thirty cytology samples from 217 patients with advanced NSCLC, including a consecutive series of 179 specimens, were used to generate matched ThinPrep slides and paraffin cytoblocks. The same ThinPrep slides used for cytologic diagnosis were assessed by standard ALK break-apart two-color probe FISH, after etching of tumor areas. Ultrasensitive ALK immunohistochemistry (IHC) on corresponding cytoblocks [D5F3 antibody, OptiView signal amplification] served as the reference data set. ThinPrep-FISH ALK signals were robust in 228 of 230 cases and not compromised by nuclear truncation inherent in paraffin-embedded tissue-FISH; only two samples displayed no signals. Nine of 178 informative cases (5%) in the consecutive series and 18 of 228 informative cases (7.8%) overall were ALK rearranged by ThinPrep-FISH. In 154 informative matched ThinPrep-FISH and cytoblock-IHC samples, 152 were concordant (10, 6.5% ALK status positive; 142, 92.2% ALK status negative), and two (1.3%) were ThinPrep-FISH positive but IHC negative (sensitivity 100%, specificity 98.6%, overall agreement 98.7%). Detection of ALK gene rearrangements in liquid cytology ThinPrep slides derived from patients with NSCLC can be confidently used for clinical ALK molecular testing.

Sequential Injection Chromatography with an Ultra-short Monolithic Column for the Low-Pressure Separation of α-Tocopherol and γ-Oryzanol in Vegetable Oils and Nutrition Supplements.

PubMed

Thaithet, Sujitra; Kradtap Hartwell, Supaporn; Lapanantnoppakhun, Somchai

2017-01-01

A low-pressure separation procedure of α-tocopherol and γ-oryzanol was developed based on a sequential injection chromatography (SIC) system coupled with an ultra-short (5 mm) C-18 monolithic column, as a lower cost and more compact alternative to the HPLC system. A green sample preparation, dilution with a small amount of hexane followed by liquid-liquid extraction with 80% ethanol, was proposed. Very good separation resolution (R s = 3.26), a satisfactory separation time (10 min) and a total run time including column equilibration (16 min) were achieved. The linear working range was found to be 0.4 - 40 μg with R 2 being more than 0.99. The detection limits of both analytes were 0.28 μg with the repeatability within 5% RSD (n = 7). Quantitative analyses of the two analytes in vegetable oil and nutrition supplement samples, using the proposed SIC method, agree well with the results from HPLC.

Immunological detection of small organic molecules in the presence of perchlorates: relevance to the life marker chip and life detection on Mars.

PubMed

Rix, Catherine S; Sims, Mark R; Cullen, David C

2011-11-01

The proposed ExoMars mission, due to launch in 2018, aims to look for evidence of extant and extinct life in martian rocks and regolith. Previous attempts to detect organic molecules of biological or abiotic origin on Mars have been unsuccessful, which may be attributable to destruction of these molecules by perchlorate salts during pyrolysis sample extraction techniques. Organic molecules can also be extracted and measured with solvent-based systems. The ExoMars payload includes the Life Marker Chip (LMC) instrument, capable of detecting biomarker molecules of extant and extinct Earth-like life in liquid extracts of martian samples with an antibody microarray assay. The aim of the work reported here was to investigate whether the presence of perchlorate salts, at levels similar to those at the NASA Phoenix landing site, would compromise the LMC extraction and detection method. To test this, we implemented an LMC-representative sample extraction process with an LMC-representative antibody assay and used these to extract and analyze a model sample that consisted of a Mars analog sample matrix (JSC Mars-1) spiked with a representative organic molecular target (pyrene, an example of abiotic meteoritic infall targets) in the presence of perchlorate salts. We found no significant change in immunoassay function when using pyrene standards with added perchlorate salts. When model samples spiked with perchlorate salts were subjected to an LMC-representative liquid extraction, immunoassays functioned in a liquid extract and detected extracted pyrene. For the same model sample matrix without perchlorate salts, we observed anomalous assay signals that coincided with yellow coloration of the extracts. This unexpected observation is being studied further. This initial study indicates that the presence of perchlorate salts, at levels similar to those detected at the NASA Phoenix landing site, is unlikely to prevent the LMC from extracting and detecting organic molecules from martian samples.

Electrofluidic Circuit-Based Microfluidic Viscometer for Analysis of Newtonian and Non-Newtonian Liquids under Different Temperatures.

PubMed

Lee, Tse-Ang; Liao, Wei-Hao; Wu, Yi-Fan; Chen, Yeng-Long; Tung, Yi-Chung

2018-02-06

This paper reports a microfluidic viscometer with an integrated pressure sensor based on electrofluidic circuits, which are electrical circuits constructed by ionic liquid-filled microfluidic channels. The electrofluidic circuit provides a pressure-sensing scheme with great long-term and thermal stability. The viscosity of the tested fluidic sample is estimated by its flow resistance, which is a function of pressure drop, flow rate, and the geometry of the microfluidic channel. The viscometer can be exploited to measure viscosity of either Newtonian or non-Newtonian power-law fluid under various shear rates (3-500 1/s) and temperatures (4-70 °C) with small sample volume (less than 400 μL). The developed sensor-integrated microfluidic viscometer is made of poly(dimethylsiloxane) (PDMS) with transparent electrofluidic circuit, which makes it feasible to simultaneously image samples under tests. In addition, the entire device is disposable to prevent cross-contamination between samples, which is desired for various chemical and biomedical applications. In the experiments, viscosities of Newtonian fluids, glycerol water solutions with different concentrations and a mixture of pyrogallol and sodium hydroxide (NaOH), and non-Newtonian fluids, xanthan gum solutions and human blood samples, have been characterized. The results demonstrate that the developed microfluidic viscometer provides a convenient and useful platform for practical viscosity characterization of fluidic samples for a wide variety of applications.

Best-Matched Internal Standard Normalization in Liquid Chromatography-Mass Spectrometry Metabolomics Applied to Environmental Samples.

PubMed

Boysen, Angela K; Heal, Katherine R; Carlson, Laura T; Ingalls, Anitra E

2018-01-16

The goal of metabolomics is to measure the entire range of small organic molecules in biological samples. In liquid chromatography-mass spectrometry-based metabolomics, formidable analytical challenges remain in removing the nonbiological factors that affect chromatographic peak areas. These factors include sample matrix-induced ion suppression, chromatographic quality, and analytical drift. The combination of these factors is referred to as obscuring variation. Some metabolomics samples can exhibit intense obscuring variation due to matrix-induced ion suppression, rendering large amounts of data unreliable and difficult to interpret. Existing normalization techniques have limited applicability to these sample types. Here we present a data normalization method to minimize the effects of obscuring variation. We normalize peak areas using a batch-specific normalization process, which matches measured metabolites with isotope-labeled internal standards that behave similarly during the analysis. This method, called best-matched internal standard (B-MIS) normalization, can be applied to targeted or untargeted metabolomics data sets and yields relative concentrations. We evaluate and demonstrate the utility of B-MIS normalization using marine environmental samples and laboratory grown cultures of phytoplankton. In untargeted analyses, B-MIS normalization allowed for inclusion of mass features in downstream analyses that would have been considered unreliable without normalization due to obscuring variation. B-MIS normalization for targeted or untargeted metabolomics is freely available at https://github.com/IngallsLabUW/B-MIS-normalization .

Accelerated solvent extraction combined with dispersive liquid-liquid microextraction before gas chromatography with mass spectrometry for the sensitive determination of phenols in soil samples.

PubMed

Xing, Han-Zhu; Wang, Xia; Chen, Xiang-Feng; Wang, Ming-Lin; Zhao, Ru-Song

2015-05-01

A method combining accelerated solvent extraction with dispersive liquid-liquid microextraction was developed for the first time as a sample pretreatment for the rapid analysis of phenols (including phenol, m-cresol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol) in soil samples. In the accelerated solvent extraction procedure, water was used as an extraction solvent, and phenols were extracted from soil samples into water. The dispersive liquid-liquid microextraction technique was then performed on the obtained aqueous solution. Important accelerated solvent extraction and dispersive liquid-liquid microextraction parameters were investigated and optimized. Under optimized conditions, the new method provided wide linearity (6.1-3080 ng/g), low limits of detection (0.06-1.83 ng/g), and excellent reproducibility (<10%) for phenols. Four real soil samples were analyzed by the proposed method to assess its applicability. Experimental results showed that the soil samples were free of our target compounds, and average recoveries were in the range of 87.9-110%. These findings indicate that accelerated solvent extraction with dispersive liquid-liquid microextraction as a sample pretreatment procedure coupled with gas chromatography and mass spectrometry is an excellent method for the rapid analysis of trace levels of phenols in environmental soil samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Cation effect on small phosphonium based ionic liquid electrolytes with high concentrations of lithium salt

NASA Astrophysics Data System (ADS)

Chen, Fangfang; Kerr, Robert; Forsyth, Maria

2018-05-01

Ionic liquid electrolytes with high alkali salt concentrations have displayed some excellent electrochemical properties, thus opening up the field for further improvements to liquid electrolytes for lithium or sodium batteries. Fundamental computational investigations into these high concentration systems are required in order to gain a better understanding of these systems, yet they remain lacking. Small phosphonium-based ionic liquids with high concentrations of alkali metal ions have recently shown many promising results in experimental studies, thereby prompting us to conduct further theoretical exploration of these materials. Here, we conducted a molecular dynamics simulation on four small phosphonium-based ionic liquids with 50 mol. % LiFSI salt, focusing on the effect of cation structure on local structuring and ion diffusional and rotational dynamics—which are closely related to the electrochemical properties of these materials.

Thorium Fuel Utilization Analysis on Small Long Life Reactor for Different Coolant Types

NASA Astrophysics Data System (ADS)

Permana, Sidik

2017-07-01

A small power reactor and long operation which can be deployed for less population and remote area has been proposed by the IAEA as a small and medium reactor (SMR) program. Beside uranium utilization, it can be used also thorium fuel resources for SMR as a part of optimalization of nuclear fuel as a “partner” fuel with uranium fuel. A small long-life reactor based on thorium fuel cycle for several reactor coolant types and several power output has been evaluated in the present study for 10 years period of reactor operation. Several key parameters are used to evaluate its effect to the reactor performances such as reactor criticality, excess reactivity, reactor burnup achievement and power density profile. Water-cooled types give higher criticality than liquid metal coolants. Liquid metal coolant for fast reactor system gives less criticality especially at beginning of cycle (BOC), which shows liquid metal coolant system obtains almost stable criticality condition. Liquid metal coolants are relatively less excess reactivity to maintain longer reactor operation than water coolants. In addition, liquid metal coolant gives higher achievable burnup than water coolant types as well as higher power density for liquid metal coolants.

Piezoelectric sensors based on molecular imprinted polymers for detection of low molecular mass analytes.

PubMed

Uludağ, Yildiz; Piletsky, Sergey A; Turner, Anthony P F; Cooper, Matthew A

2007-11-01

Biomimetic recognition elements employed for the detection of analytes are commonly based on proteinaceous affibodies, immunoglobulins, single-chain and single-domain antibody fragments or aptamers. The alternative supra-molecular approach using a molecularly imprinted polymer now has proven utility in numerous applications ranging from liquid chromatography to bioassays. Despite inherent advantages compared with biochemical/biological recognition (which include robustness, storage endurance and lower costs) there are few contributions that describe quantitative analytical applications of molecularly imprinted polymers for relevant small molecular mass compounds in real-world samples. There is, however, significant literature describing the use of low-power, portable piezoelectric transducers to detect analytes in environmental monitoring and other application areas. Here we review the combination of molecularly imprinted polymers as recognition elements with piezoelectric biosensors for quantitative detection of small molecules. Analytes are classified by type and sample matrix presentation and various molecularly imprinted polymer synthetic fabrication strategies are also reviewed.

Interface for the rapid analysis of liquid samples by accelerator mass spectrometry

DOEpatents

Turteltaub, Kenneth; Ognibene, Ted; Thomas, Avi; Daley, Paul F; Salazar Quintero, Gary A; Bench, Graham

2014-02-04

An interface for the analysis of liquid sample having carbon content by an accelerator mass spectrometer including a wire, defects on the wire, a system for moving the wire, a droplet maker for producing droplets of the liquid sample and placing the droplets of the liquid sample on the wire in the defects, a system that converts the carbon content of the droplets of the liquid sample to carbon dioxide gas in a helium stream, and a gas-accepting ion source connected to the accelerator mass spectrometer that receives the carbon dioxide gas of the sample in a helium stream and introduces the carbon dioxide gas of the sample into the accelerator mass spectrometer.

Reactor for in situ measurements of spatially resolved kinetic data in heterogeneous catalysis

NASA Astrophysics Data System (ADS)

Horn, R.; Korup, O.; Geske, M.; Zavyalova, U.; Oprea, I.; Schlögl, R.

2010-06-01

The present work describes a reactor that allows in situ measurements of spatially resolved kinetic data in heterogeneous catalysis. The reactor design allows measurements up to temperatures of 1300 °C and 45 bar pressure, i.e., conditions of industrial relevance. The reactor involves reactants flowing through a solid catalyst bed containing a sampling capillary with a side sampling orifice through which a small fraction of the reacting fluid (gas or liquid) is transferred into an analytical device (e.g., mass spectrometer, gas chromatograph, high pressure liquid chromatograph) for quantitative analysis. The sampling capillary can be moved with μm resolution in or against flow direction to measure species profiles through the catalyst bed. Rotation of the sampling capillary allows averaging over several scan lines. The position of the sampling orifice is such that the capillary channel through the catalyst bed remains always occupied by the capillary preventing flow disturbance and fluid bypassing. The second function of the sampling capillary is to provide a well which can accommodate temperature probes such as a thermocouple or a pyrometer fiber. If a thermocouple is inserted in the sampling capillary and aligned with the sampling orifice fluid temperature profiles can be measured. A pyrometer fiber can be used to measure the temperature profile of the solid catalyst bed. Spatial profile measurements are demonstrated for methane oxidation on Pt and methane oxidative coupling on Li/MgO, both catalysts supported on reticulated α -Al2O3 foam supports.

Advanced sampling techniques for hand-held FT-IR instrumentation

NASA Astrophysics Data System (ADS)

Arnó, Josep; Frunzi, Michael; Weber, Chris; Levy, Dustin

2013-05-01

FT-IR spectroscopy is the technology of choice to identify solid and liquid phase unknown samples. The challenging ConOps in emergency response and military field applications require a significant redesign of the stationary FT-IR bench-top instruments typically used in laboratories. Specifically, field portable units require high levels of resistance against mechanical shock and chemical attack, ease of use in restrictive gear, extreme reliability, quick and easy interpretation of results, and reduced size. In the last 20 years, FT-IR instruments have been re-engineered to fit in small suitcases for field portable use and recently further miniaturized for handheld operation. This article introduces the HazMatID™ Elite, a FT-IR instrument designed to balance the portability advantages of a handheld device with the performance challenges associated with miniaturization. In this paper, special focus will be given to the HazMatID Elite's sampling interfaces optimized to collect and interrogate different types of samples: accumulated material using the on-board ATR press, dispersed powders using the ClearSampler™ tool, and the touch-to-sample sensor for direct liquid sampling. The application of the novel sample swipe accessory (ClearSampler) to collect material from surfaces will be discussed in some detail. The accessory was tested and evaluated for the detection of explosive residues before and after detonation. Experimental results derived from these investigations will be described in an effort to outline the advantages of this technology over existing sampling methods.

Simulation of the planetary interior differentiation processes in the laboratory.

PubMed

Fei, Yingwei

2013-11-15

A planetary interior is under high-pressure and high-temperature conditions and it has a layered structure. There are two important processes that led to that layered structure, (1) percolation of liquid metal in a solid silicate matrix by planet differentiation, and (2) inner core crystallization by subsequent planet cooling. We conduct high-pressure and high-temperature experiments to simulate both processes in the laboratory. Formation of percolative planetary core depends on the efficiency of melt percolation, which is controlled by the dihedral (wetting) angle. The percolation simulation includes heating the sample at high pressure to a target temperature at which iron-sulfur alloy is molten while the silicate remains solid, and then determining the true dihedral angle to evaluate the style of liquid migration in a crystalline matrix by 3D visualization. The 3D volume rendering is achieved by slicing the recovered sample with a focused ion beam (FIB) and taking SEM image of each slice with a FIB/SEM crossbeam instrument. The second set of experiments is designed to understand the inner core crystallization and element distribution between the liquid outer core and solid inner core by determining the melting temperature and element partitioning at high pressure. The melting experiments are conducted in the multi-anvil apparatus up to 27 GPa and extended to higher pressure in the diamond-anvil cell with laser-heating. We have developed techniques to recover small heated samples by precision FIB milling and obtain high-resolution images of the laser-heated spot that show melting texture at high pressure. By analyzing the chemical compositions of the coexisting liquid and solid phases, we precisely determine the liquidus curve, providing necessary data to understand the inner core crystallization process.

Simulation of the Planetary Interior Differentiation Processes in the Laboratory

PubMed Central

Fei, Yingwei

2013-01-01

A planetary interior is under high-pressure and high-temperature conditions and it has a layered structure. There are two important processes that led to that layered structure, (1) percolation of liquid metal in a solid silicate matrix by planet differentiation, and (2) inner core crystallization by subsequent planet cooling. We conduct high-pressure and high-temperature experiments to simulate both processes in the laboratory. Formation of percolative planetary core depends on the efficiency of melt percolation, which is controlled by the dihedral (wetting) angle. The percolation simulation includes heating the sample at high pressure to a target temperature at which iron-sulfur alloy is molten while the silicate remains solid, and then determining the true dihedral angle to evaluate the style of liquid migration in a crystalline matrix by 3D visualization. The 3D volume rendering is achieved by slicing the recovered sample with a focused ion beam (FIB) and taking SEM image of each slice with a FIB/SEM crossbeam instrument. The second set of experiments is designed to understand the inner core crystallization and element distribution between the liquid outer core and solid inner core by determining the melting temperature and element partitioning at high pressure. The melting experiments are conducted in the multi-anvil apparatus up to 27 GPa and extended to higher pressure in the diamond-anvil cell with laser-heating. We have developed techniques to recover small heated samples by precision FIB milling and obtain high-resolution images of the laser-heated spot that show melting texture at high pressure. By analyzing the chemical compositions of the coexisting liquid and solid phases, we precisely determine the liquidus curve, providing necessary data to understand the inner core crystallization process. PMID:24326245

[Determination of seven phenoxyacid herbicides in environmental water by high performance liquid chromatography coupled with three phase hollow fiber liquid phase microextraction].

PubMed

Peng, Xiaojun; Pang, Jinshan; Deng, Aihua

2011-12-01

A novel method for the simultaneous determination of seven phenoxyacid herbicides such as dicamba, fluroxypyr, 4-chlorophenoxyacetic acid (4-CPA), 2-methyl-4-chlorophenoxyacetic acid (MCPA), 2, 4-dichlorophenoxyacetic acid (2,4-D), 2,4-dichlorophenoxybutyric acid (2,4-DB) and 4-(2-methyl-4-chlorophenoxy) butyric acid (MCPB) in environmental water by three phase hollow fiber liquid phase microextraction (HF-LPME) coupled with high performance liquid chromatography (HPLC) was developed. In order to optimize the experimental conditions, the orthogonal test has been used. The effects of extraction solvent, pH of the donor phase and acceptor phase, extraction time, stirring speed and salt concentration on the detection were investigated. The optimal experimental conditions were as follows: octanol as organic solvent, pH 3 of donor phase, pH 12 of acceptor phase, extraction time of 30 min, stirring speed of 400 r/min. The results showed that the proposed method provided a wide linear range for 7 phenoxyacid herbicides with correlation coefficients of 0.995 3 - 0.998 8. The detection limits ranged from 0.2 to 1.0 microg/L. The enrichment factors were in the range of 76.7 - 121. The recoveries were in the range of 68% - 104% and the relative standard deviations (RSDs) were less than 8.1% for the environmental water samples. The method has the advantages of sensitivity, simplicity, fastness and the use of very small amounts of organic solvent. The method can meet the requirements of the determination of trace phenoxyacid herbicides in the environmental water samples, and the study provided a useful method for the analysis of trace substances in water samples.

Novel method of realizing metal freezing points by induced solidification

NASA Astrophysics Data System (ADS)

Ma, C. K.

1997-07-01

The freezing point of a pure metal, tf, is the temperature at which the solid and liquid phases are in equilibrium. The purest metal available is actually a dilute alloy. Normally, the liquidus point of a sample, tl, at which the amount of the solid phase in equilibrium with the liquid phase is minute, provides the closest approximation to tf. Thus the experimental realization of tf is a matter of realizing tl. The common method is to cool a molten sample continuously so that it supercools and recalesces. The highest temperature after recalescence is normally the best experimental value of tl. In the realization, supercooling of the sample at the sample container and the thermometer well is desirable for the formation of dual solid-liquid interfaces to thermally isolate the sample and the thermometer. However, the subsequent recalescence of the supercooled sample requires the formation of a certain amount of solid, which is not minute. Obviously, the plateau temperature is not the liquidus point. In this article we describe a method that minimizes supercooling. The condition that provides tl is closely approached so that the latter may be measured. As the temperature of the molten sample approaches the anticipated value of tl, a small solid of the same alloy is introduced into the sample to induce solidification. In general, solidification does not occur as long as the temperature is above or at tl, and occurs as soon as the sample supercools minutely. Thus tl can be obtained, in principle, by observing the temperature at which induced solidification begins. In case the solid is introduced after the sample has supercooled slightly, a slight recalescence results and the subsequent maximum temperature is a close approximation to tl. We demonstrate that the principle of induced solidification is indeed applicable to freezing point measurements by applying it to the design of a copper-freezing-point cell for industrial applications, in which a supercooled sample is reheated and then induced to solidify by the solidification of an auxiliary sample. Further experimental studies are necessary to assess the practical advantages and disadvantages of the induction method.

Primary resistance to osimertinib due to SCLC transformation: Issue of T790M determination on liquid re-biopsy.

PubMed

Minari, R; Bordi, P; Del Re, M; Facchinetti, F; Mazzoni, F; Barbieri, F; Camerini, A; Comin, C E; Gnetti, L; Azzoni, C; Nizzoli, R; Bortesi, B; Rofi, E; Petreni, P; Campanini, N; Rossi, G; Danesi, R; Tiseo, M

2018-01-01

EGFR T790M mutation is the most common mechanism of resistance to first-/second-generation EGFR tyrosine kinase inhibitors (TKIs) in non-small cell lung cancer (NSCLC) and could be overcome by third-generation EGFR-TKIs, such as osimertinib. Liquid biopsy, a non-invasive technique used to test the presence of the resistant mutation, may help avoiding tissue re-biopsy. However, analysing only circulating-free DNA, information about other less frequent and coexisting resistance mechanisms may remain unrevealed. All patients reported in this series participated in the ASTRIS trial, a real world treatment study testing the efficacy of osimertinib (80mg os die) in advanced T790M-positive NSCLC progressed to prior EGFR-TKI. Patients were considered eligible to osimertinib if T790M positive on tissue or plasma samples. In our patients, EGFR molecular testing on blood sample was conducted with digital droplet PCR (ddPCR). We report our experience of five patients treated with osimertinib after T790M detection on liquid biopsy that presented a disease progression at first tumor assessment mediated by SCLC transformation, as evidenced at tissue re-biopsies. All patients showed low ratio T790M/activating mutation in the blood before osimertinib (lower than 0.03). For three patients, EGFR mutational analysis was T790M-negative when re-assessed by using a less sensitive method (therascreen ® ) on the same liquid biopsy sample analysed by ddPCR before osimertinib therapy. Although liquid biopsy is a relevant tool to diagnose T790M presence in NSCLC patients resistant to EGFR-TKI, in case of a low ratio T790M/activating mutation, tissue biopsy should be considered to exclude the presence of SCLC transformation and/or other concomitant resistance mechanisms. Copyright © 2017 Elsevier B.V. All rights reserved.

Sensitive Determination of Cd in Small-Volume Samples by Miniaturized Liquid Drop Anode Atmospheric Pressure Glow Discharge Optical Emission Spectrometry.

PubMed

Jamroz, Piotr; Greda, Krzysztof; Dzimitrowicz, Anna; Swiderski, Krzysztof; Pohl, Pawel

2017-06-06

A novel liquid drop anode (LDA) direct current atmospheric pressure glow discharge (dc-APGD) system was applied for direct determination of Cd in liquid microsamples (50 μL) by optical emission spectrometry (OES). The microdischarge was generated in open-to-air atmosphere between a solid pin type tungsten cathode and a liquid drop placed on a graphite disk anode. The arrangement of the graphite disk placed on a PTFE chip platform as well as the solid pin type cathode was simple and robust. The limit of detection (LOD) of Cd for the developed LDA-APGD-OES method was 0.20-0.40 μg L -1 , while precision (as the relative standard deviation for the repeated measurements) was within 2-5%. By using the liquid drop of 50 μL, the linearity range of 1-1000 μg L -1 was achieved. The effect of addition of the low-molecular weight (LMW) organic compounds, easily ionized elements (EIEs), i.e., Ca, K, Mg, and Na, as well as the foreign ions (Al, Cu, Fe, Mn, Zn) to the solution on the in situ atomization and excitation processes occurred during operation of the LDA-APGD system, and the response of Cd was studied. Validation of the proposed method was demonstrated by analysis of Lobster hepatopancreas (TORT-2), pig kidney (ERM-BB186), and groundwater (ERM-CA615) certified reference materials (CRMs) and recoveries of Cd from water samples spiked with 25 μg L -1 of Cd. Very good agreement between the found and certified values of Cd in the CRMs (the recoveries were within the range of 96.3-99.6%) indicated trueness of the method and its reliability for determination of traces of Cd. In the case of the spiked water samples, the recoveries obtained were in the range from 95.2 to 99.5%.

Maximal liquid bridges between horizontal cylinders

NASA Astrophysics Data System (ADS)

Cooray, Himantha; Huppert, Herbert E.; Neufeld, Jerome A.

2016-08-01

We investigate two-dimensional liquid bridges trapped between pairs of identical horizontal cylinders. The cylinders support forces owing to surface tension and hydrostatic pressure that balance the weight of the liquid. The shape of the liquid bridge is determined by analytically solving the nonlinear Laplace-Young equation. Parameters that maximize the trapping capacity (defined as the cross-sectional area of the liquid bridge) are then determined. The results show that these parameters can be approximated with simple relationships when the radius of the cylinders is small compared with the capillary length. For such small cylinders, liquid bridges with the largest cross-sectional area occur when the centre-to-centre distance between the cylinders is approximately twice the capillary length. The maximum trapping capacity for a pair of cylinders at a given separation is linearly related to the separation when it is small compared with the capillary length. The meniscus slope angle of the largest liquid bridge produced in this regime is also a linear function of the separation. We additionally derive approximate solutions for the profile of a liquid bridge, using the linearized Laplace-Young equation. These solutions analytically verify the above-mentioned relationships obtained for the maximization of the trapping capacity.

Fluid Mechanics and Heat Transfer of Liquid Precursor Droplets Injected into High-Temperature Plasmas

NASA Astrophysics Data System (ADS)

Basu, Saptarshi; Jordan, Eric H.; Cetegen, Baki M.

2008-03-01

Thermo-physical processes in liquid ceramic precursor droplets in plasma were modeled. Models include aerodynamic droplet break-up, droplet transport, as well as heat and mass transfer within individual droplets. Droplet size, solute concentration, and plasma temperature effects are studied. Results are discussed with the perspective of selecting processing conditions and injection parameters to obtain certain types of coating microstructures. Small droplets (<5 microns) are found to undergo volumetric precipitation and coating deposition with small unpyrolized material. Droplets can be made to undergo shear break-up by reducing surface tension and small droplets promote volumetric precipitation. Small particles reach substrate as molten splats resulting in denser coatings. Model predicts that larger droplets (>5 microns) tend to surface precipitate-forming shells with liquid core. They may be subjected to internal pressurization leading to shattering of shells and secondary atomization of liquid within. They arrive at the substrate as broken shells and unpyrolized material.

Lysimeter apparatus

DOEpatents

Clark, Don T.; Erickson, Eugene E.; Casper, William L.; Everett, David M.; Hubbell, Joel M.; Sisson, James B.

2005-09-06

A suction lysimeter for sampling subsurface liquids includes a lysimeter casing having a drive portion, a reservoir portion, and a tip portion, the tip portion including a membrane through which subsurface liquids may be sampled; a fluid conduit coupled in fluid flowing relation relative to the membrane, and which in operation facilitates the delivery of the sampled subsurface liquids from the membrane to the reservoir portion; and a plurality of tubes coupled in fluid flowing relation relative to the reservoir portion, the tubes in operation facilitating delivery of the sampled subsurface liquids from the reservoir portion for testing. A method of sampling subsurface liquids comprises using this lysimeter.

Emissions of C&D refuse in landfills: a European case.

PubMed

López, Ana; Lobo, Amaya

2014-08-01

A field study was developed in a new landfill for refuse from construction and demolition (C&D) material recovery plants of small size (4 Ha.) in Europe, with the aim of evaluating the liquid and gas emissions in this type of facility at a large scale. It included characterization of the materials, monitoring leachate and gas quantity and composition. Besides thermometers, piezometers and sampling ports were placed in several points within the waste. This paper presents the data obtained for five years of the landfill life. The materials disposed were mainly made up of wood and concrete, similar to other C&D debris sites, but the amount of gypsum drywall (below 3% of the waste) was significantly smaller than other available studies, where percentages above 20% had been reported. Leachate contained typical C&D pollutants, such as different inorganic ions and metals, some of which exceeded other values reported in the literature (conductivity, ammonium, lead and arsenic). The small net precipitation in the area and the leachate recirculation into the landfill surface help explain these higher concentrations, thus highlighting the impact of liquid to solid (L/S) ratio on leachate characteristics. In contrast to previous studies, neither odor nuisances nor significant landfill gas over the surface were detected. However, gas samples taken from the landfill inside revealed sulfate reducing and methanogenic activity. Copyright © 2014 Elsevier Ltd. All rights reserved.

[Multi-residue method for screening of pesticides in crops by liquid chromatography with tandem mass spectrometry].

PubMed

Tanizawa, Haruna; Shima, Mikie; Ikehara, Chieko; Kobata, Masakazu; Sato, Motoaki

2005-10-01

A simple and rapid method was developed for the screening of 82 pesticides/metabolites in a wide variety of crops, using solid-phase extraction and liquid chromatography with tandem mass spectrometry (LC/MS/MS). After extraction with methanol, the filtered extracts were made up to 100 mL and a 2 mL aliquot was subjected to solid-phase extraction. Co-extractives were removed with a C18 mini-column, while pesticides were retained on 3 kinds of mini-columns (HLB, SAX, activated carbon), and then eluted with acetonitrile. Analysis was performed by LC/MS/MS, and MS acquisition parameters were established in positive and negative ESI modes. The utility of the method was demonstrated by the analysis of 6 crops (carrot, cabbage, onion, spinach, lemon, brown rice) and one mixed vegetable juice. Of 82 compounds tested, 75 in carrot and 62 in lemon were obtained with recoveries ranging from 70-120%. For all samples tested, 75 compounds could be obtained with recoveries of over 50%, and the detection limits of most compounds were lower than 0.01 microg/g. This method provides acceptable performance for analysis of these 75 compounds. Further, by using aliquots of the extracts with small-scale mini-columns, purified samples could be obtained. This proposed method with small matrix effects, is effective and suitable for screening of multiple residual pesticides by using LC/MS/MS.

Portable capillary electrophoresis-system for on-site food analysis with lab-on-a-chip based contactless conductivity detection

NASA Astrophysics Data System (ADS)

Gärtner, Claudia; Sewart, René; Klemm, Richard; Becker, Holger

2014-06-01

A portable analytical system for the characterization of liquid environmental samples and beverages in food control was realized. The key element is the implementation of contactless conductivity detection on lab-on-a-chip basis ensuring the system to be operated in a label free mode. Typical target molecules such as small ionic species like Li+, Na+, K+, SO4 2- or NO3-, organic acids in wine whose concentration and ratio to each other documents the wine quality, or caffeine or phosphate in coke were detected. Results from sample matrices like various beverages as water, cola, tea, wine and milk, water from heaters, environmental samples and blood will be presented.

Measurement of lumefantrine and its metabolite in plasma by high performance liquid chromatography with ultraviolet detection.

PubMed

Khalil, Insaf F; Abildrup, Ulla; Alifrangis, Lene H; Maiga, Deogratius; Alifrangis, Michael; Hoegberg, Lotte; Vestergaard, Lasse S; Persson, Ola Per-Eric; Nyagonde, Nyagonde; Lemnge, Martha M; Theander, Thor G; Bygbjerg, Ib C

2011-01-05

Artemether-lumefantrine (ARM-LUM) has in recent years become the first-line treatment for uncomplicated malaria in many Sub-Saharan African countries. Vigorous monitoring of the therapeutic efficacy of this treatment is needed. This requires high-quality studies following standard protocols; ideally, such studies should incorporate measurement of drug levels in the study patients to exclude the possibility that insufficient drug levels explain an observed treatment failure. Several methods for measuring lumefantrine (LUM) in plasma by HPLC are available; however, several of these methods have some limitations in terms of high costs and limited feasibility arising from large required sample volumes and demanding sample preparation. Therefore, we set out to develop a simpler reversed phase high performance liquid chromatography (RP-HPLC) method based on UV detection for simultaneous measurement of LUM and its major metabolite the desbutyl LUM (DL) in plasma. Halofantrine was used as an internal standard. Liquid-liquid extraction of samples was carried out using hexane-ethyl acetate (70:30, v/v). Chromatographic separation was carried out on a Synergi Polar-RP column (250 mm × 300 mm, particle size 4 μm). The mobile phase consisted of acetonitrile-0.1M ammonium acetate buffer adjusted to pH 4.9 (85:15%, v/v). Absorbance of the compounds was monitored at 335 nm using a reference wavelength of 360 nm. Absolute extraction recovery for LUM and DL were 88% and 90%, respectively. Inter- and intraday coefficients of variation for LUM and DL were ≤ 10%. The lower limits of quantification for LUM and DL were 12.5 and 6.5 ng/ml, respectively. After validation, the methodology was transferred to a local laboratory in Tanga Tanzania and samples from a small subset of malaria patients were analysed for LUM. The method appears to be applicable in settings with limited facilities. Copyright © 2010 Elsevier B.V. All rights reserved.

Simultaneous and rapid determination of gefitinib, erlotinib and afatinib plasma levels using liquid chromatography/tandem mass spectrometry in patients with non-small-cell lung cancer.

PubMed

Hayashi, Hideki; Kita, Yutaro; Iihara, Hirotoshi; Yanase, Koumei; Ohno, Yasushi; Hirose, Chiemi; Yamada, Maya; Todoroki, Kenichiro; Kitaichi, Kiyoyuki; Minatoguchi, Shinya; Itoh, Yoshinori; Sugiyama, Tadashi

2016-07-01

A simultaneous, selective, sensitive and rapid liquid chromatography/tandem mass spectrometry method was developed and validated for the quantification of gefitinib, erlotinib and afatinib in 250 μL samples of human blood plasma. Diluted plasma samples were extracted using a liquid-phase extraction procedure with tert-butyl methyl ether. The three drugs were separated by high-performance liquid chromatography using a C18 column and an isocratic mobile phase running at a flow rate of 0.2 mL/min for 5 min. The drugs were detected using a tandem mass spectrometer with electrospray ionization using imatinib as an internal standard. Calibration curves were generated over the linear concentration range of 0.05-100 nm in plasma with a lower limit of quantification of 0.01 or 0.05 nm for all compounds. Finally, the validated method was applied to a clinical pharmacokinetic study in patients with nonsmall-cell lung cancer (NSCLC) following the oral administration of afatinib. These results indicate that this method is suitable for assessing the risks and benefits of chemotherapy in patients with NSCLC and is useful for therapeutic drug monitoring for NSCLC treatment. As far as we know, this is the first report on LC-MS/MS method for the simultaneous quantification of NSCLC tyrosine kinase inhibitor plasma concentrations including afatinib. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

Recent approaches for bridging the pressure gap in photoelectron microspectroscopy

PubMed Central

Kolmakov, Andrei; Gregoratti, Luca; Kiskinova, Maya; Günther, Sebastian

2016-01-01

Ambient-pressure photoelectron spectroscopy (APPES) and microscopy are at the frontier of modern chemical analysis at liquid-gas, solid-liquid and solid-gas interfaces, bridging science and engineering of functional materials. Complementing the current state-of-the art of the instruments, we survey in this short review several alternative APPES approaches, developed recently in the scanning photoelectron microscope (SPEM) at the Elettra laboratory. In particular, we report on experimental setups for dynamic near-ambient pressure environment, using pulsed-gas injection in the vicinity of samples or reaction cells with very small apertures, allowing for experiments without introducing additional differential pumping stages. The major part of the review is dedicated to the construction and performance of novel environmental cells using ultrathin electron-transparent but molecularly impermeable membranes to isolate the gas or liquid ambient from the electron detector operating in ultra-high vacuum (UHV). We demonstrate that two dimensional materials, such as graphene and derivatives, are mechanically robust to withstand atmospheric - UHV pressure differences and are sufficiently transparent for the photoelectrons emitted from samples immersed in the liquid or gaseous media. There are many unique opportunities for APPES using X-rays over a wide energy range. We show representative results that illustrate the potential of these ‘ambient-pressure’ approaches. Combined with the ca 100 nm lateral resolution of SPEM, they can overcome the pressure gap challenges and address the evolution of chemical composition and electronic structure at surface and interfaces under realistic operation conditions with unprecedented lateral and spectral resolution. PMID:28008215

Improved procedure for determination of flucytosine in human blood plasma by high-pressure liquid chromatography.

PubMed Central

Schwertschlag, U; Nakata, L M; Gal, J

1984-01-01

Several high-pressure liquid chromatography procedures for the determination of flucytosine in serum or plasma have appeared. Some of these suffer from significant disadvantages, and none was applicable in our routine clinical therapeutic-drug-monitoring laboratory. A new high-pressure liquid chromatography assay for flucytosine was therefore developed. A 100-microliter sample of plasma was treated with an aqueous 5-iodocytosine internal-standard solution, and the mixture was deproteinized with trichloroacetic acid. A portion of the protein-free supernatant was diluted with 0.1 M ammonium phosphate, and an aliquot of the resulting solution was injected into the high-pressure liquid chromatography system. Chromatography was performed on a strong-cation-exchange column with a mobile phase containing aqueous ammonium phosphate, phosphoric acid, methanol, and acetonitrile. Detection was at 254 nm. The assay was shown to be linear in the 10 to 200-micrograms/ml drug-concentration range. Forty other drugs were tested for potential interference with the assay, and none was found. For routine use, a single-point working standard containing 75 micrograms of flucytosine per ml was used, giving intraassay coefficients of variation at 50 and 150 micrograms/ml of 1.8 and 2.3% respectively, whereas the day-to-day coefficient of variation at 50 micrograms/ml was 10.0%. Advantages of the procedure include the small sample size, the use of a convenient and reliable internal standard, speed, and simplicity. The assay is highly suitable for routine clinical drug-analysis laboratories. PMID:6508261

Determination of antibacterial agent tilmicosin in pig plasma by LC/MS/MS and its application to pharmacokinetics.

PubMed

Li, Bing; Gong, Shi-Yue; Zhou, Xu-Zheng; Yang, Ya-Jun; Li, Jian-Yong; Wei, Xiao-Juan; Cheng, Fu-Sheng; Niu, Jian-Rong; Liu, Xi-Wang; Zhang, Ji-Yu

2017-03-01

A rapid and sensitive high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated to quantify tilmicosin in pig plasma. Plasma samples were prepared by liquid-liquid extraction. Chromatographic separation was achieved on a C 18 column (2.1 × 30 mm, 3.5 μm) using acetonitrile-water (90:10, v/v; water included 0.1% formic acid) as the mobile phase. Mass detection was carried out using positive electrospray ionization in multiple reaction monitoring mode. The calibration curve was linear from 0.5 to 2000 ng/mL (r 2  = 0.9998). The intra- and inter-day accuracy and precision were within the acceptable limits of ±10% for all tilmicosin concentrations. The recoveries ranged from 95 to 99% for the three tested concentrations. The LC-MS/MS method described herein was simple, fast and less laborious than other methods, achieved high sensitivity using a small sample volume, and was successfully applied to pharmacokinetic studies of tilmicosin enteric granules after oral delivery to pigs. In comparison with tilmicosin premix, tilmicosin enteric granules slowed the elimination rate of tilmicosin, prolonged its period of action and significantly improved its bioavailability. Copyright © 2016 John Wiley & Sons, Ltd.

Comprehensive Study of the Flow Control Strategy in a Wirelessly Charged Centrifugal Microfluidic Platform with Two Rotation Axes.

PubMed

Zhu, Yunzeng; Chen, Yiqi; Meng, Xiangrui; Wang, Jing; Lu, Ying; Xu, Youchun; Cheng, Jing

2017-09-05

Centrifugal microfluidics has been widely applied in the sample-in-answer-out systems for the analyses of nucleic acids, proteins, and small molecules. However, the inherent characteristic of unidirectional fluid propulsion limits the flexibility of these fluidic chips. Providing an extra degree of freedom to allow the unconstrained and reversible pumping of liquid is an effective strategy to address this limitation. In this study, a wirelessly charged centrifugal microfluidic platform with two rotation axes has been constructed and the flow control strategy in such platform with two degrees of freedom was comprehensively studied for the first time. Inductively coupled coils are installed on the platform to achieve wireless power transfer to the spinning stage. A micro servo motor is mounted on both sides of the stage to alter the orientation of the device around a secondary rotation axis on demand during stage rotation. The basic liquid operations on this platform, including directional transport of liquid, valving, metering, and mixing, are comprehensively studied and realized. Finally, a chip for the simultaneous determination of hexavalent chromium [Cr(VI)] and methanal in water samples is designed and tested based on the strategy presented in this paper, demonstrating the potential use of this platform for on-site environmental monitoring, food safety testing, and other life science applications.

Demagnetization Treatment of Remanent Composite Microspheres Studied by Alternating Current Susceptibility Measurements

PubMed Central

van Berkum, Susanne; Erné, Ben H.

2013-01-01

The magnetic remanence of silica microspheres with a low concentration of embedded cobalt ferrite nanoparticles is studied after demagnetization and remagnetization treatments. When the microspheres are dispersed in a liquid, alternating current (AC) magnetic susceptibility spectra reveal a constant characteristic frequency, corresponding to the rotational diffusion of the microparticles; this depends only on particle size and liquid viscosity, making the particles suitable as a rheological probe and indicating that interactions between the microspheres are weak. On the macroscopic scale, a sample with the dry microparticles is magnetically remanent after treatment in a saturating field, and after a demagnetization treatment, the remanence goes down to zero. The AC susceptibility of a liquid dispersion, however, characterizes the remanence on the scale of the individual microparticles, which does not become zero after demagnetization. The reason is that an individual microparticle contains only a relatively small number of magnetic units, so that even if they can be reoriented magnetically at random, the average vector sum of the nanoparticle dipoles is not negligible on the scale of the microparticle. In contrast, on the macroscopic scale, the demagnetization procedure randomizes the orientations of a macroscopic number of magnetic units, resulting in a remanent magnetization that is negligible compared to the saturation magnetization of the entire sample. PMID:24009021

A prototypic small molecule database for bronchoalveolar lavage-based metabolomics

NASA Astrophysics Data System (ADS)

Walmsley, Scott; Cruickshank-Quinn, Charmion; Quinn, Kevin; Zhang, Xing; Petrache, Irina; Bowler, Russell P.; Reisdorph, Richard; Reisdorph, Nichole

2018-04-01

The analysis of bronchoalveolar lavage fluid (BALF) using mass spectrometry-based metabolomics can provide insight into lung diseases, such as asthma. However, the important step of compound identification is hindered by the lack of a small molecule database that is specific for BALF. Here we describe prototypic, small molecule databases derived from human BALF samples (n=117). Human BALF was extracted into lipid and aqueous fractions and analyzed using liquid chromatography mass spectrometry. Following filtering to reduce contaminants and artifacts, the resulting BALF databases (BALF-DBs) contain 11,736 lipid and 658 aqueous compounds. Over 10% of these were found in 100% of samples. Testing the BALF-DBs using nested test sets produced a 99% match rate for lipids and 47% match rate for aqueous molecules. Searching an independent dataset resulted in 45% matching to the lipid BALF-DB compared to<25% when general databases are searched. The BALF-DBs are available for download from MetaboLights. Overall, the BALF-DBs can reduce false positives and improve confidence in compound identification compared to when general databases are used.

A small-angle x-ray scattering system with a vertical layout.

PubMed

Wang, Zhen; Chen, Xiaowei; Meng, Lingpu; Cui, Kunpeng; Wu, Lihui; Li, Liangbin

2014-12-01

A small-angle x-ray scattering (SAXS) system with a vertical layout (V-SAXS) has been designed and constructed for in situ detection on nanostructures, which is well suitable for in situ study on self-assembly of nanoparticles at liquid interface and polymer processing. A steel-tower frame on a reinforced basement is built as the supporting skeleton for scattering beam path and detector platform, ensuring the system a high working stability and a high operating accuracy. A micro-focus x-ray source combining parabolic three-dimensional multi-layer mirror and scatteringless collimation system provides a highly parallel beam, which allows us to detect the very small angle range. With a sample-to-detector distance of 7 m, the largest measurable length scale is 420 nm in real space. With a large sample zone, it is possible to install different experimental setups such as film stretching machine, which makes the system perfect to follow the microstructures evolution of materials during processing. The capability of the V-SAXS on in situ study is tested with a drying experiment of a free latex droplet, which confirms our initial design.

A comparison of two cloudwater/fogwater collectors: The rotating arm collector and the caltech active strand cloudwater collector

NASA Astrophysics Data System (ADS)

Collett, Jeffrey L.; Daube, Bruce C.; Munger, J. William; Hoffmann, Michael R.

A side-by-side comparison of the Rotating Arm Collector (RAC) and the Caltech Active Strand Cloudwater Collector (CASCC) was conducted at an elevated coastal site near the eastern end of the Santa Barbara Channel in southern California. The CASCC was observed to collect cloudwater at rates of up to 8.5 ml min -1. The ratio of cloudwater collection rates was found to be close to the theoretical prediction of 4.2:1 (CASCC:RAC) over a wide range of liquid water contents (LWC). At low LWC, however, this ratio climbed rapidly, possibly reflecting a predominance of small droplets under these conditions, coupled with a greater collection efficiency of small droplets by the CASCC. Cloudwater samples collected by the RAC had significantly higher concentrations of Na +, Ca 2+, Mg 2+ and Cl - than those collected by the CASCC. These higher concentrations may be due to differences in the chemical composition of large vs small droplets. No significant differences were observed in concentrations of NO 3-, SO 42- or NH 4+ in samples collected by the two instruments.

Microparticle sampling by electrowetting-actuated droplet sweeping.

PubMed

Zhao, Yuejun; Cho, Sung Kwon

2006-01-01

This paper describes a new microparticle sampler where particles can be efficiently swept from a solid surface and sampled into a liquid medium using moving droplets actuated by the electrowetting principle. We successfully demonstrate that super hydrophilic (2 microm and 7.9 microm diameter glass beads of about 14 degrees contact angle), intermediate hydrophilic (7.5 microm diameter polystyrene beads of about 70 degrees contact angle), and super hydrophobic (7.9 microm diameter Teflon-coated glass beads and 3 microm size PTFE particles of over 110 degrees contact angles) particles on a solid surface are picked up by electrowetting-actuated moving droplets. For the glass beads as well as the polystyrene beads, the sampling efficiencies are over 93%, in particular over 98% for the 7.9 microm glass beads. For the PTFE particles, however, the sampling efficiency is measured at around 70%, relatively lower than that of the glass and polystyrene beads. This is due mainly to the non-uniformity in particle size and the particle hydrophobicity. In this case, the collected particles staying (adsorbing) on the air-to-water interface hinder the droplet from advancing. This particle sampler requires an extremely small amount of liquid volume (about 500 nanoliters) and will thus be highly compatible and easily integrated with lab-on-a-chip systems for follow-up biological/chemical analyses.

Extraction of 3,4,4'-Trichlorocarbanilide from Rat Fecal Samples for Determination by High Pressure Liquid Chromatography-Tandem Mass Spectrometry.

PubMed

Kennedy, Rebekah C; Fling, Russell R; Terry, Paul D; Menn, Fu-Min; Chen, Jiangang; Borman, Christopher J

2015-07-15

Triclocarban (3,4,4'-Trichlorocarbanilide; TCC) in the environment has been well documented. Methods have been developed to monitor TCC levels from various matrices including water, sediment, biosolids, plants, blood and urine; however, no method has been developed to document the concentration of TCC in fecal content after oral exposure in animal studies. In the present study, we developed and validated a method that uses liquid extraction coupled with HPLC-MS/MS determination to measure TCC in feces. The limit of detection and limit of quantitation in control rats without TCC exposure was 69.0 ng/g and 92.9 ng/g of feces, respectively. The base levels of TCC in feces were lower than LOD. At 12 days of treatment, the fecal TCC concentration increased to 2220 µg/g among 0.2% w/w exposed animals. The concentration in fecal samples decreased over the washout period in 0.2% w/w treated animals to 0.399 µ/g feces after exposure was removed for 28 days. This method required a small amount of sample (0.1 g) with simple sample preparation. Given its sensitivity and efficiency, this method may be useful for monitoring TCC exposure in toxicological studies of animals.

Department of Homeland Security (DHS) Proficiency Testing on Small-Scale Safety and Thermal Testing of Improvised Explosives

NASA Astrophysics Data System (ADS)

Reynolds, John; Sandstrom, Mary; Brown, Geoffrey; Warner, Kirstin; Phillips, Jason; Shelley, Timothy; Reyes, Jose; Hsu, Peter

2013-06-01

One of the first steps in establishing safe handling procedures for explosives is small-scale safety and thermal (SSST) testing. To better understand the response of improvised materials or HMEs to SSST testing, 18 HME materials were compared to 3 standard military explosives in a proficiency-type round robin study among five laboratories--2 DoD and 3 DOE--sponsored by DHS. The testing matrix has been designed to address problems encountered with improvised materials--powder mixtures, liquid suspensions, partially wetted solids, immiscible liquids, and reactive materials. Over 30 issues have been identified that indicate standard test methods may require modification when applied to HMEs to derive accurate sensitivity assessments needed for development safe handling and storage practices. This presentation will discuss experimental difficulties encountered when testing these problematic samples, show inter-laboratory testing results, show some statistical interpretation of the results, and highlight some of the testing issues. Some of the work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344. LLNL-ABS-617519 (721812).

Steroid Profiling by Gas Chromatography–Mass Spectrometry and High Performance Liquid Chromatography–Mass Spectrometry for Adrenal Diseases

PubMed Central

McDonald, Jeffrey G.; Matthew, Susan

2012-01-01

The ability to measure steroid hormone concentrations in blood and urine specimens is central to the diagnosis and proper treatment of adrenal diseases. The traditional approach has been to assay each steroid hormone, precursor, or metabolite using individual aliquots of serum, each with a separate immunoassay. For complex diseases, such as congenital adrenal hyperplasia and adrenocortical cancer, in which the assay of several steroids is essential for management, this approach is time consuming and costly, in addition to using large amounts of serum. Gas chromatography/mass spectrometry profiling of steroid metabolites in urine has been employed for many years but only in a small number of specialized laboratories and suffers from slow throughput. The advent of commercial high-performance liquid chromatography instruments coupled to tandem mass spectrometers offers the potential for medium- to high-throughput profiling of serum steroids using small quantities of sample. Here, we review the physical principles of mass spectrometry, the instrumentation used for these techniques, the terminology used in this field and applications to steroid analysis. PMID:22170384

The quantitative impact of the mesopore size on the mass transfer mechanism of the new 1.9μm fully porous Titan-C18 particles. I: analysis of small molecules.

PubMed

Gritti, Fabrice; Guiochon, Georges

2015-03-06

Previous data have shown that could deliver a minimum reduced plate height as small as 1.7. Additionally, the reduction of the mesopore size after C18 derivatization and the subsequent restriction for sample diffusivity across the Titan-C18 particles were found responsible for the unusually small value of the experimental optimum reduced velocity (5 versus 10 for conventional particles) and for the large values of the average reduced solid-liquid mass transfer resistance coefficients (0.032 versus 0.016) measured for a series of seven n-alkanophenones. The improvements in column efficiency made by increasing the average mesopore size of the Titan silica from 80 to 120Å are investigated from a quantitative viewpoint based on the accurate measurements of the reduced coefficients (longitudinal diffusion, trans-particle mass transfer resistance, and eddy diffusion) and of the intra-particle diffusivity, pore, and surface diffusion for the same series of n-alkanophenone compounds. The experimental results reveal an increase (from 0% to 30%) of the longitudinal diffusion coefficients for the same sample concentration distribution (from 0.25 to 4) between the particle volume and the external volume of the column, a 40% increase of the intra-particle diffusivity for the same sample distribution (from 1 to 7) between the particle skeleton volume and the bulk phase, and a 15-30% decrease of the solid-liquid mass transfer coefficient for the n-alkanophenone compounds. Pore and surface diffusion are increased by 60% and 20%, respectively. The eddy dispersion term and the maximum column efficiency (295000plates/m) remain virtually unchanged. The rate of increase of the total plate height with increasing the chromatographic speed is reduced by 20% and it is mostly controlled (75% and 70% for 80 and 120Å pore size) by the flow rate dependence of the eddy dispersion term. Copyright © 2015 Elsevier B.V. All rights reserved.

Simple and quick determination of analgesics and other contaminants of emerging concern in environmental waters by on-line solid phase extraction coupled to liquid chromatography-tandem mass spectrometry.

PubMed

Ferrer-Aguirre, Alejandra; Romero-González, Roberto; Vidal, J L Martínez; Frenich, Antonia Garrido

2016-05-13

A simple and quick analytical method has been developed for the determination of pharmaceutical compounds in water. An on-line solid-phase extraction (SPE) coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been optimized to determine 7 contaminants of emerging concern in environmental waters at ngL(-1) levels. This procedure requires minimal sample handling and small sample volume (900μL) with a total running time of 18min. Several SPE parameters were evaluated and optimized in order to achieve a high sample throughput. Therefore sample volume, carryover and reusability of the cartridges were evaluated. Performance characteristics were evaluated and good linearity was obtained (R(2)>0.98). Recoveries were evaluated in spiked samples at three concentrations and the values ranged from 71 to 104%. Intra and inter-day precision was lower than 10 and 13% respectively. Limits of quantification were equal to or lower than 10ngL(-1), except for 1,7-dimethylxanthine (20ngL(-1)) and ibuprofen (50ngL(-1)). The method was applied to 20 environmental water samples, and ibuprofen was the compound most widely detected at concentrations up to 42.06μgL(-1), whereas the other compounds were detected in fewer samples at lower concentrations (up to 15.99μgL(-1)). Copyright © 2016 Elsevier B.V. All rights reserved.

Development of a rapid and sensitive method for the determination of aluminum by reverse-phase high-performance liquid chromatography using a fluorescence detector.

PubMed

Heena; Kumar, Rajesh; Rani, Susheela; Malik, Ashok Kumar

2015-01-01

This study represents a new analytical high-performance liquid chromatography-fluorescence detector method for the determination of Al(III) as Al(III) complex with 8-hydroxyquinoline-5-sulfonic acid in a tap water sample and a coke sample. A micellar liquid chromatographic method is proposed for the determination of aluminum metal in the presence of cetyltrimethylammonium bromide, a cationic surfactant (0.05 M) used for the solubilization of the aluminum complex. The influence of pH and ligand concentration on the formation of the complex was studied by adding a small amount of 0.1 M sodium hydroxide. The metal chelate was detected at λEx 410 nm and λEm 510 nm. This method eliminates the need for addition of reagent or organic modifier to the mobile phase. The complex was analyzed using an Ascentis Express C18 column and a mobile phase consisting of acetonitrile, methanol and water (55 : 30 : 15). Under the optimized conditions, the linear range was 1-200 µg L(-1) and the limit of detection was 0.05 µg L(-1). The method showed a good detector response over the range of interest and was successfully applied for the determination of trace Al(III) in canned coke and water samples containing excess of Mg(II), Ca(II) and other matrices. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Determination of benzodiazepines in beverages using green extraction methods and capillary HPLC-UV detection.

PubMed

Piergiovanni, Maurizio; Cappiello, Achille; Famiglini, Giorgio; Termopoli, Veronica; Palma, Pierangela

2018-05-30

Dispersive liquid-liquid microextraction with and without ultrasound assistance (DLLME, UA-DLLME) and microextraction with packed sorbent (MEPS) methods for the extraction and determination of eight different benzodiazepines (BDZ) (chlordiazepoxide, flurazepam, bromazepam, oxazepam, lorazepam, clobazam, clonazepam, and flunitrazepam) in three commercial non-alcoholic and light alcoholic beverages were optimized and compared. Benzodiazepines are frequently used for their extensive diffusion and strong numbing effect in drug-facilitated crimes (DFC). The tiny small amount of sample required for DLLME and MEPS extraction makes them very suitable for specimens collected at the crime scene of DFCs. Microextraction techniques are of increasing interest thanks to their accordance to green analytical chemistry (GAC) guidelines providing good recovery values. Ultrasound assistance (UA-DLLME) was used to investigate whether this type of energy can improve the recoveries of the analytes. Analyses of the extracts were performed with reverse-phase capillary high-performance liquid chromatography with UV detection (HPLC - UV), thanks to low environmental impact, robustness, diffusion, and affordability. Recovery percentages at three different concentrations in the three beverages were between 14.30% and 103.28% with intraday and interday RSD lower than ±2.78%. The same samples were extracted using a MEPS protocol, and the results were compared with those obtained with DLLME. MEPS gave recoveries between 20.90% and 101.88% for all matrices showing a better performance than DLLME at higher concentrations, though lower recoveries were observed with diluted samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Preservation of Liquid Biological Samples

NASA Technical Reports Server (NTRS)

Putcha, Lakshmi (Inventor); Nimmagudda, Ramalingeshwara R. (Inventor)

2000-01-01

The present invention provides a method of preserving a liquid biological sample, comprising the step of: contacting said liquid biological sample with a preservative comprising, sodium benzoate in an amount of at least about 0.15% of the sample (weight/volume) and citric acid in an amount of at least about 0.025% of the sample (weight/volume).

Critical issues in the clinical application of liquid biopsy in non-small cell lung cancer.

PubMed

Manicone, Mariangela; Poggiana, Cristina; Facchinetti, Antonella; Zamarchi, Rita

2017-10-01

Current therapeutic options for non-small cell lung cancer (NSCLC) patients are chemotherapy and targeted therapy directed mainly against epidermal growth factor receptor (EGFR) mutations and anaplastic lymphoma kinase (ALK) rearrangements. Targeted therapy relies on the availability of tumor biopsies for molecular profiling at diagnosis and to longitudinally monitor treatment response and resistance development. Unfortunately, tumor biopsy might be invasive, recover poor material of suboptimal quality, and cause sample bias due to tumor heterogeneity. Many studies have illustrated the potential of liquid biopsy as minimal invasive approach to respond to the urgent need for real time monitoring, stratification, and personalized optimized treatment in NSCLC patients. In principle, the liquid biopsy could provide the genetic landscape of primary and metastatic cancerous lesions, detecting "druggable" genomic alterations or associated with treatment resistance. Moreover, it would guarantee the prognostic/predictive biomarkers evaluation in patients for whom biopsies are inaccessible or difficult to repeat. At this regard, the prognostic value of circulating tumor cells (CTCs) in NSCLC patients has been largely investigated, but still their clinical utility as tumor biomarker is hampered by the lack of a consensus on the criteria necessary and sufficient to define them and on the standard operating procedures (SOPs) for their assessment. This review will summarize current developments on liquid biopsy in NSCLC, addressing the technology issues that contribute to the poor ability to track CTCs in the blood of NSCLC patients, thus limiting their extensive use in the clinical practice, and analyzing the solutions adopted to overcome such limits, on the road towards the clinical validation.

The application of supported liquid extraction in the analysis of benzodiazepines using surface enhanced Raman spectroscopy.

PubMed

Doctor, Erika L; McCord, Bruce

2015-11-01

Benzodiazepines are among the most frequently prescribed medicines for anxiety disorders and are present in many toxicological screens. These drugs are often administered in the commission of drug facilitated sexual assaults due their effects on the central nervous system. Due to the potency of the drugs, only small amounts are usually given to victims; therefore, the target detection limit for these compounds in biological samples has been set at 50 ng/mL. Currently the standard screening method for detection of this class of drug is the immunoassay; however, screening methods that are more sensitive and selective than immunoassays are needed to encompass the wide range of structural variants of this class of compounds. Surface enhanced Raman spectroscopy (SERS) can be highly sensitive and has been shown to permit analysis of various benzodiazepines with limits of detection as low as 6 ng/mL. This technique permits analytical results in less than 2 min when used on pure drug samples. For biological samples, a key issue for analysis by SERS is removal of exogenous salts and matrix components. In this paper we examine supported liquid extraction as a useful preparation technique for SERS detection. Supported liquid extraction has many of the benefits of liquid-liquid extraction along with the ability to be automated. This technique provides a fast and clean extraction for benzodiazepines from urine at a pH of 5.0, and does not produce large quantities of solvent waste. To validate this procedure we have determined figures of merit and examined simulated urine samples prepared with commonly appearing interferences. It was shown that at a pH 5.0 many drugs that are prevalent in urine samples can be removed, permitting a selective detection of the benzodiazepine of interest. This technique has been shown to provide rapid (less than 20 min), sensitive, and specific detection of benzodiazepines with limits of detection between 32 and 600 ng/mL and dynamic range of 32-25,000 ng/mL. It provides the forensic community with a sensitive and specific screening technique for the detection of benzodiazepines in drug facilitated assault cases. Copyright © 2015 Elsevier B.V. All rights reserved.

Measurement of Gas-Liquid Two-Phase Flow in Micro-Pipes by a Capacitance Sensor

PubMed Central

Ji, Haifeng; Li, Huajun; Huang, Zhiyao; Wang, Baoliang; Li, Haiqing

2014-01-01

A capacitance measurement system is developed for the measurement of gas-liquid two-phase flow in glass micro-pipes with inner diameters of 3.96, 2.65 and 1.56 mm, respectively. As a typical flow regime in a micro-pipe two-phase flow system, slug flow is chosen for this investigation. A capacitance sensor is designed and a high-resolution and high-speed capacitance measurement circuit is used to measure the small capacitance signals based on the differential sampling method. The performance and feasibility of the capacitance method are investigated and discussed. The capacitance signal is analyzed, which can reflect the voidage variation of two-phase flow. The gas slug velocity is determined through a cross-correlation technique using two identical capacitance sensors. The simulation and experimental results show that the presented capacitance measurement system is successful. Research work also verifies that the capacitance sensor is an effective method for the measurement of gas liquid two-phase flow parameters in micro-pipes. PMID:25587879

Measurement of gas-liquid two-phase flow in micro-pipes by a capacitance sensor.

PubMed

Ji, Haifeng; Li, Huajun; Huang, Zhiyao; Wang, Baoliang; Li, Haiqing

2014-11-26

A capacitance measurement system is developed for the measurement of gas-liquid two-phase flow in glass micro-pipes with inner diameters of 3.96, 2.65 and 1.56 mm, respectively. As a typical flow regime in a micro-pipe two-phase flow system, slug flow is chosen for this investigation. A capacitance sensor is designed and a high-resolution and high-speed capacitance measurement circuit is used to measure the small capacitance signals based on the differential sampling method. The performance and feasibility of the capacitance method are investigated and discussed. The capacitance signal is analyzed, which can reflect the voidage variation of two-phase flow. The gas slug velocity is determined through a cross-correlation technique using two identical capacitance sensors. The simulation and experimental results show that the presented capacitance measurement system is successful. Research work also verifies that the capacitance sensor is an effective method for the measurement of gas liquid two-phase flow parameters in micro-pipes.

Portable system and method combining chromatography and array of electrochemical sensors

DOEpatents

Zaromb, Solomon; Stetter, Joseph R.

1989-01-01

A portable system for analyzing a fluid sample includes a small, portable, low-pressure and low-power chromatographic analyzer and a chemical parameter spectrometry monitor including an array of sensors for detecting, identifying and measuring the concentrations of a variety of components in the eluent from the chromatographic analyzer. The monitor includes one or more operating condition controllers which may be used to change one or more of the operating conditions during exposure of the sensors to the eluent from the chromatography analyzer to form a response pattern which is then compared with a library of previously established patterns. Gas and liquid chromatographic embodiments are disclosed. In the gas embodiment, the operating condition controllers include heated filaments which may convert electrochemically inactive components to electrochemically active products. In the liquid chromatography embodiment, low-power, liquid-phase equivalents of heated filaments are used with appropriate sensors. The library response patterns may be divided into subsets and the formed pattern may be assigned for comparison only with the patterns of a particular subset.

Coarsening Experiment Prepared for Flight

NASA Technical Reports Server (NTRS)

Hickman, J. Mark

2003-01-01

The Coarsening in Solid-Liquid Mixtures-2 (CSLM-2) experiment is a materials science spaceflight experiment whose purpose is to investigate the kinetics of competitive particle growth within a liquid matrix. During coarsening, small particles shrink by losing atoms to larger particles, causing the larger particles to grow. In this experiment, solid particles of tin will grow (coarsen) within a liquid lead-tin eutectic matrix. The following figures show the coarsening of tin particles in a lead-tin (Pb-Sn) eutectic as a function of time. By conducting this experiment in a microgravity environment, we can study a greater range of solid volume fractions, and the effects of sedimentation present in terrestrial experiments will be negligible. The CSLM-2 experiment flew November 2002 on space shuttle flight STS-113 for operation on the International Space Station, but it could not be run because of problems with the Microgravity Science Glovebox in the U.S. Laboratory module. Additional samples will be sent to ISS on subsequent shuttle flights.

First application of liquid-metal-jet sources for small-animal imaging: high-resolution CT and phase-contrast tumor demarcation.

PubMed

Larsson, Daniel H; Lundström, Ulf; Westermark, Ulrica K; Arsenian Henriksson, Marie; Burvall, Anna; Hertz, Hans M

2013-02-01

Small-animal studies require images with high spatial resolution and high contrast due to the small scale of the structures. X-ray imaging systems for small animals are often limited by the microfocus source. Here, the authors investigate the applicability of liquid-metal-jet x-ray sources for such high-resolution small-animal imaging, both in tomography based on absorption and in soft-tissue tumor imaging based on in-line phase contrast. The experimental arrangement consists of a liquid-metal-jet x-ray source, the small-animal object on a rotating stage, and an imaging detector. The source-to-object and object-to-detector distances are adjusted for the preferred contrast mechanism. Two different liquid-metal-jet sources are used, one circulating a Ga∕In∕Sn alloy and the other an In∕Ga alloy for higher penetration through thick tissue. Both sources are operated at 40-50 W electron-beam power with ∼7 μm x-ray spots, providing high spatial resolution in absorption imaging and high spatial coherence for the phase-contrast imaging. High-resolution absorption imaging is demonstrated on mice with CT, showing 50 μm bone details in the reconstructed slices. High-resolution phase-contrast soft-tissue imaging shows clear demarcation of mm-sized tumors at much lower dose than is required in absorption. This is the first application of liquid-metal-jet x-ray sources for whole-body small-animal x-ray imaging. In absorption, the method allows high-resolution tomographic skeletal imaging with potential for significantly shorter exposure times due to the power scalability of liquid-metal-jet sources. In phase contrast, the authors use a simple in-line arrangement to show distinct tumor demarcation of few-mm-sized tumors. This is, to their knowledge, the first small-animal tumor visualization with a laboratory phase-contrast system.

Lysimeter methods and apparatus

DOEpatents

Clark, Don T.; Erickson, Eugene E.; Casper, William L.; Everett, David M.; Hubbell, Joel M.; Sisson, James B.

2004-12-07

A suction lysimeter for sampling subsurface liquids includes a lysimeter casing having a drive portion, a reservoir portion, and a tip portion, the tip portion including a membrane through which subsurface liquids may be sampled; a fluid conduit coupled in fluid flowing relation relative to the membrane, and which in operation facilitates the delivery of the sampled subsurface liquids from the membrane to the reservoir portion; and a plurality of tubes coupled in fluid flowing relation relative to the reservoir portion, the tubes in operation facilitating delivery of the sampled subsurface liquids from the reservoir portion for testing. A method of sampling subsurface liquids comprises using this lysimeter.

Determination of sulfonamides in butter samples by ionic liquid magnetic bar liquid-phase microextraction high-performance liquid chromatography.

PubMed

Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

2015-01-01

A novel, simple, and environmentally friendly pretreatment method, ionic liquid magnetic bar liquid-phase microextraction, was developed for the determination of sulfonamides in butter samples by high-performance liquid chromatography. The ionic liquid magnetic bar was prepared by inserting a stainless steel wire into the hollow of a hollow fiber and immobilizing ionic liquid in the micropores of the hollow fiber. In the extraction process, the ionic liquid magnetic bars were used to stir the mixture of sample and extraction solvent and enrich the sulfonamides in the mixture. After extraction, the analyte-adsorbed ionic liquid magnetic bars were readily isolated with a magnet from the extraction system. It is notable that the present method was environmentally friendly since water and only several microliters of ionic liquid were used in the whole extraction process. Several parameters affecting the extraction efficiency were investigated and optimized, including the type of ionic liquid, sample-to-extraction solvent ratio, the number of ionic liquid magnetic bars, extraction temperature, extraction time, salt concentration, stirring speed, pH of the extraction solvent, and desorption conditions. The recoveries were in the range of 73.25-103.85 % and the relative standard deviations were lower than 6.84 %. The experiment results indicated that the present method was effective for the extraction of sulfonamides in high-fat content samples.

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.

Analysis of PBDEs in soil, dust, spiked lake water, and human serum samples by hollow fiber-liquid phase microextraction combined with GC-ICP-MS.

PubMed

Xiao, Qin; Hu, Bin; Duan, Jiankun; He, Man; Zu, Wanqing

2007-10-01

A novel method for the analysis of four polybrominated diphenyl ethers (PBDEs) in environmental and human serum samples based on hollow fiber-liquid phase microextraction (HF-LPME) followed by gas chromatography-inductively coupled plasma mass spectrometric (GC-ICP-MS) detection has been developed. The organic solvent in the porous hollow fiber was first dipped into the sample for extraction at a given time, and the retracted organic phase was introduced into the GC-ICP-MS for analysis. The addition of methanol has a strong effect on the HF-LPME extraction efficiency. Other significant parameters affecting the extraction efficiency of HF-LPME were also studied. HF-LPME was effective to isolate the analytes from the complex matrix. Under the optimized conditions, the detection limits of the proposed method varied from 15.2 to 40.5 ng/L. In general, the relative standard deviations (RSDs) were less than 10%. Good linearity was obtained with the correlation coefficients all better than 0.999. The proposed method is simple, quick, few microliters of organic solvent required, and is especially suitable for the analysis of the real sample with small amount available. The overall process of HF-LPME with GC-ICP-MS was applied successfully for the determination of polybrominated diphenyl ethers (PBDEs) in environmental and spiked human serum samples, and the results were satisfactory.

Microfluidics, Chromatography, and Atomic-Force Microscopy

NASA Technical Reports Server (NTRS)

Anderson, Mark

2008-01-01

A Raman-and-atomic-force microscope (RAFM) has been shown to be capable of performing several liquid-transfer and sensory functions essential for the operation of a microfluidic laboratory on a chip that would be used to perform rapid, sensitive chromatographic and spectro-chemical analyses of unprecedentedly small quantities of liquids. The most novel aspect of this development lies in the exploitation of capillary and shear effects at the atomic-force-microscope (AFM) tip to produce shear-driven flow of liquids along open microchannels of a microfluidic device. The RAFM can also be used to perform such functions as imaging liquids in microchannels; removing liquid samples from channels for very sensitive, tip-localized spectrochemical analyses; measuring a quantity of liquid adhering to the tip; and dip-pen deposition from a chromatographic device. A commercial Raman-spectroscopy system and a commercial AFM were integrated to make the RAFM so as to be able to perform simultaneous topographical AFM imaging and surface-enhanced Raman spectroscopy (SERS) at the AFM tip. The Raman-spectroscopy system includes a Raman microprobe attached to an optical microscope, the translation stage of which is modified to accommodate the AFM head. The Raman laser excitation beam, which is aimed at the AFM tip, has a wavelength of 785 nm and a diameter of about 5 m, and its power is adjustable up to 10 mW. The AFM is coated with gold to enable tip-localized SERS.

Methodological considerations for measuring glucocorticoid metabolites in feathers

PubMed Central

Berk, Sara A.; McGettrick, Julie R.; Hansen, Warren K.; Breuner, Creagh W.

2016-01-01

In recent years, researchers have begun to use corticosteroid metabolites in feathers (fCORT) as a metric of stress physiology in birds. However, there remain substantial questions about how to measure fCORT most accurately. Notably, small samples contain artificially high amounts of fCORT per millimetre of feather (the small sample artefact). Furthermore, it appears that fCORT is correlated with circulating plasma corticosterone only when levels are artificially elevated by the use of corticosterone implants. Here, we used several approaches to address current methodological issues with the measurement of fCORT. First, we verified that the small sample artefact exists across species and feather types. Second, we attempted to correct for this effect by increasing the amount of methanol relative to the amount of feather during extraction. We consistently detected more fCORT per millimetre or per milligram of feather in small samples than in large samples even when we adjusted methanol:feather concentrations. We also used high-performance liquid chromatography to identify hormone metabolites present in feathers and measured the reactivity of these metabolites against the most commonly used antibody for measuring fCORT. We verified that our antibody is mainly identifying corticosterone (CORT) in feathers, but other metabolites have significant cross-reactivity. Lastly, we measured faecal glucocorticoid metabolites in house sparrows and correlated these measurements with corticosteroid metabolites deposited in concurrently grown feathers; we found no correlation between faecal glucocorticoid metabolites and fCORT. We suggest that researchers should be cautious in their interpretation of fCORT in wild birds and should seek alternative validation methods to examine species-specific relationships between environmental challenges and fCORT. PMID:27335650

Apparatus and method for quantitative measurement of small differences in optical absorptivity between two samples using differential interferometry and the thermooptic effect

DOEpatents

Cremers, David A.; Keller, Richard A.

1984-01-01

An apparatus and method for the measurement of small differences in optical absorptivity of weakly absorbing solutions using differential interferometry and the thermooptic effect has been developed. Two sample cells are placed in each arm of an interferometer and are traversed by colinear probe and heating laser beams. The interrogation probe beams are recombined forming a fringe pattern, the intensity of which can be related to changes in optical pathlength of these laser beams through the cells. This in turn can be related to small differences in optical absorptivity which results in different amounts of sample heating when the heating laser beams are turned on, by the fact that the index of refraction of a liquid is temperature dependent. A critical feature of this invention is the stabilization of the optical path of the probe beams against drift. Background (solvent) absorption can then be suppressed by a factor of approximately 400. Solute absorptivities of about 10.sup.-5 cm.sup.-1 can then be determined in the presence of background absorptions in excess of 10.sup.-3 cm.sup.-1. In addition, the smallest absorption measured with the instant apparatus and method is about 5.times. 10.sup.-6 cm.sup.-1.

Apparatus and method for quantitative measurement of small differences in optical absorptivity between two samples using differential interferometry and the thermooptic effect

DOEpatents

Cremers, D.A.; Keller, R.A.

1982-06-08

An apparatus and method for the measurement of small differences in optical absorptivity of weakly absorbing solutions using differential interferometry and the thermooptic effect has been developed. Two sample cells are placed in each arm of an interferometer and are traversed by colinear probe and heating laser beams. The interrogation probe beams are recombined forming a fringe pattern, the intensity of which can be related to changes in optical pathlength of these laser beams through the cells. This in turn can be related to small differences in optical absorptivity which results in different amounts of sample heating when the heating laser beams are turned on, by the fact that the index of refraction of a liquid is temperature dependent. A critical feature of this invention is the stabilization of the optical path of the probe beams against drift. Background (solvent) absorption can then be suppressed by a factor of approximately 400. Solute absorptivities of about 10/sup -5/ cm/sup -1/ can then be determined in the presence of background absorptions in excess of 10/sup -3/ cm/sup -1/. In addition, the smallest absorption measured with the instant apparatus and method is about 5 x 10/sup -6/ cm/sup -1/.

24th International Symposium on Ballistics

DTIC Science & Technology

2008-09-26

production Samples dimensions were 0.3x0.05 m. Test set up Gas gun 5.5 mm diameter steel spheres and sabot Velocity measuring  systems High speed rate...Oilwell perforators – small caliber shaped charges – create the pathway for oil or gas to flow from the reservoir rock into the wellbore  Deep, clean ...overburden, tectonic) – Pore fluid pressure – Pore fluid type ( liquid vs. gas ) Background  Geomechanics considerations: – In-situ stresses (“total

Multifunctional Composites with Applications to Energy Performance and Efficiency

DTIC Science & Technology

2011-08-01

surface for comparing the effects of processing. Parylene/ Teflon AF adhesion was measured using a modified tape test. Samples were razor cut (3-6...lines, 2 mm spacing ) at 0 and 90 degrees to the tape -pull direction. SEMicro CHT tape (synthetic rubber adhesive, 12 to 25 mm wide x 75 mm long) was...surface, a thin layer of Teflon AF (~200 nm) is spin- coated for hydrophobicity. Small drops of ionic liquids in contact with a conductive probe are

A compact tritium enrichment unit for large sample volumes with automated re-filling and higher enrichment factor.

PubMed

Kumar, B; Han, L-F; Wassenaar, L I; Klaus, P M; Kainz, G G; Hillegonds, D; Brummer, D; Ahmad, M; Belachew, D L; Araguás, L; Aggarwal, P

2016-12-01

Tritium ( 3 H) in natural waters is a powerful tracer of hydrological processes, but its low concentrations require electrolytic enrichment before precise measurements can be made with a liquid scintillation counter. Here, we describe a newly developed, compact tritium enrichment unit which can be used to enrich up to 2L of a water sample. This allows a high enrichment factor (>100) for measuring low 3 H contents of <0.05TU. The TEU uses a small cell (250mL) with automated re-filling and a CO 2 bubbling technique to neutralize the high alkalinity of enriched samples. The enriched residual sample is retrieved from the cell under vacuum by cryogenic distillation at -20°C and the tritium enrichment factor for each sample is accurately determined by measuring pre- and post- enrichment 2 H concentrations with laser spectrometry. Copyright © 2016. Published by Elsevier Ltd.

System and method for liquid extraction electrospray-assisted sample transfer to solution for chemical analysis

DOEpatents

Kertesz, Vilmos; Van Berkel, Gary J.

2016-07-12

A system for sampling a surface includes a surface sampling probe comprising a solvent liquid supply conduit and a distal end, and a sample collector for suspending a sample collection liquid adjacent to the distal end of the probe. A first electrode provides a first voltage to solvent liquid at the distal end of the probe. The first voltage produces a field sufficient to generate electrospray plume at the distal end of the probe. A second electrode provides a second voltage and is positioned to produce a plume-directing field sufficient to direct the electrospray droplets and ions to the suspended sample collection liquid. The second voltage is less than the first voltage in absolute value. A voltage supply system supplies the voltages to the first electrode and the second electrode. The first electrode can apply the first voltage directly to the solvent liquid. A method for sampling for a surface is also disclosed.

30 CFR 57.4460 - Storage of flammable liquids underground.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 30 Mineral Resources 1 2011-07-01 2011-07-01 false Storage of flammable liquids underground. 57... Fire Prevention and Control Flammable and Combustible Liquids and Gases § 57.4460 Storage of flammable liquids underground. (a) Flammable liquids shall not be stored underground, except— (1) Small quantities...

30 CFR 57.4460 - Storage of flammable liquids underground.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 30 Mineral Resources 1 2012-07-01 2012-07-01 false Storage of flammable liquids underground. 57... Fire Prevention and Control Flammable and Combustible Liquids and Gases § 57.4460 Storage of flammable liquids underground. (a) Flammable liquids shall not be stored underground, except— (1) Small quantities...

30 CFR 57.4460 - Storage of flammable liquids underground.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 30 Mineral Resources 1 2014-07-01 2014-07-01 false Storage of flammable liquids underground. 57... Fire Prevention and Control Flammable and Combustible Liquids and Gases § 57.4460 Storage of flammable liquids underground. (a) Flammable liquids shall not be stored underground, except— (1) Small quantities...

30 CFR 57.4460 - Storage of flammable liquids underground.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 30 Mineral Resources 1 2013-07-01 2013-07-01 false Storage of flammable liquids underground. 57... Fire Prevention and Control Flammable and Combustible Liquids and Gases § 57.4460 Storage of flammable liquids underground. (a) Flammable liquids shall not be stored underground, except— (1) Small quantities...

Microextraction techniques combined with capillary electrophoresis in bioanalysis.

PubMed

Kohler, Isabelle; Schappler, Julie; Rudaz, Serge

2013-01-01

Over the past two decades, many environmentally sustainable sample-preparation techniques have been proposed, with the objective of reducing the use of toxic organic solvents or substituting these with environmentally friendly alternatives. Microextraction techniques (MEs), in which only a small amount of organic solvent is used, have several advantages, including reduced sample volume, analysis time, and operating costs. Thus, MEs are well adapted in bioanalysis, in which sample preparation is mandatory because of the complexity of a sample that is available in small quantities (mL or even μL only). Capillary electrophoresis (CE) is a powerful and efficient separation technique in which no organic solvents are required for analysis. Combination of CE with MEs is regarded as a very attractive environmentally sustainable analytical tool, and numerous applications have been reported over the last few decades for bioanalysis of low-molecular-weight compounds or for peptide analysis. In this paper we review the use of MEs combined with CE in bioanalysis. The review is divided into two sections: liquid and solid-based MEs. A brief practical and theoretical description of each ME is given, and the techniques are illustrated by relevant applications.

Method of foaming a liquid metal

DOEpatents

Fischer, Albert K.; Johnson, Carl E.

1980-01-01

The addition of a small quantity of barium to liquid metal NaK or sodium has been found to promote foam formation and improve bubble retention in the liquid metal. A stable liquid metal foam will provide a more homogeneous liquid metal flow through the channel of a two-phase liquid metal MHD power generator to improve operating efficiency.

Actualistic models of mantle metasomatism documented in a composite xenolith from Dish Hill, California

USGS Publications Warehouse

Nielson, J.E.; Budahn, J.R.; Unruh, D.M.; Wilshire, H.G.

1993-01-01

Major and trace-element whole rock and mineral variations in composite hornblendite-peridotite xenolith Ba-2-1, from Dish Hill, CA, are due to a single event of metasomatism in the mantle. The hornblendite is the crystallized selvage of a dike conduit charged with incompatible-element-enriched hydrous mafic magma. The magma infiltrated the refractory peridotite wallrock, reacted with its constituent minerals, and simultaneously deposited amphibole. The systematic data from this study show considerable variation in isotopic values and trace elements. These data provide insight into a mantle process that was defined previously from samples without context, lacking evidence about the number or source of metasomatic events. In the contact zone of Ba-2-1, peridotite is enriched in Fe, Ti, CO2) and H2O; clinopyroxene and amphibole also are enriched in Fe and Ti, but clinopyroxene appears slightly depleted in CaO. Compared to chondrites, peridotite, clinopyroxene, and probably amphibole are enriched in light rare earth (LREEcn) and other incompatible trace elements. Values of 87Sr 86Sr and 143Nd 144Nd in the contact zone are close to isotopic equilibrium with the dike. Whole rock and constituent clinopyroxene compositions change to those of refractory peridotite with distance from the contact. These compositional variations were modelled using Gresens' equation for whole-rock major and minor elements, and calculations for isotopic ratios and REEs, which emulate the effects of Chromatographic fractionation. The choice of endmembers was restricted to compositions actually present in mantle samples from Dish Hill. Model results indicate that: 1. (1) the variations can be explained as the result of a single metasomatic event, probably a single pulse of previously fractionated liquid; 2. (2) the ratio of total interacting liquid to peridotite was at least 1:3 by weight in the contact zone; and 3. (3) the composition of the metasomatic liquid changed progressively as it infiltrated beyond that zone. The small distance over which variations occur is due to the small amount of liquid that infiltrated. Only in the contact zone was peridotite wallrock saturated by a liquid composition similar to the dike. Comparison of the Ba-2-1 data with those of another xenolith from Dish Hill suggests that the compositional variations of mantle metasomatism result from both the compositional contrast between the metasomatizing liquid and wallrock and the relative abundances of each. Compositional and volumetric variations of mantle partial melts and their fractionates, and repeated events of melting and reaction in contiguous mantle, can create broad ranges of metasomatic "signatures" from the same process. ?? 1993.

Rational approach to solvent system selection for liquid-liquid extraction-assisted sample pretreatment in counter-current chromatography.

PubMed

Wang, Jiajia; Gu, Dongyu; Wang, Miao; Guo, Xinfeng; Li, Haoquan; Dong, Yue; Guo, Hong; Wang, Yi; Fan, Mengqi; Yang, Yi

2017-05-15

A rational liquid-liquid extraction approach was established to pre-treat samples for high-speed counter-current chromatography (HSCCC). n-Hexane-ethyl acetate-methanol-water (4:5:4:5, v/v) and (1:5:1:5, v/v) were selected as solvent systems for liquid-liquid extraction by systematically screening K of target compounds to remove low- and high-polarity impurities in the sample, respectively. After liquid-liquid extraction was performed, 1.4g of crude sample II was obtained from 18.5g of crude sample I which was extracted from the flowers of Robinia pseudoacacia L., and then separated with HSCCC by using a solvent system composed of n-hexane-ethyl acetate-methanol-water (1:2:1:2, v/v). As a result, 31mg of robinin and 37mg of kaempferol 7-O-α-l-rhamnopyranoside were isolated from 200mg of crude sample II in a single run of HSCCC. A scale-up separation was also performed, and 160mg of robinin with 95% purity and 188mg of kaempferol 7-O-α-l-rhamnopyranoside with 97% purity were produced from 1.2g of crude sample II. Copyright © 2017 Elsevier B.V. All rights reserved.

Liquid sampling system

DOEpatents

Larson, L.L.

1984-09-17

A conduit extends from a reservoir through a sampling station and back to the reservoir in a closed loop. A jet ejector in the conduit establishes suction for withdrawing liquid from the reservoir. The conduit has a self-healing septum therein upstream of the jet ejector for receiving one end of a double-ended cannula, the other end of which is received in a serum bottle for sample collection. Gas is introduced into the conduit at a gas bleed between the sample collection bottle and the reservoir. The jet ejector evacuates gas from the conduit and the bottle and aspirates a column of liquid from the reservoir at a high rate. When the withdrawn liquid reaches the jet ejector the rate of flow therethrough reduces substantially and the gas bleed increases the pressure in the conduit for driving liquid into the sample bottle, the gas bleed forming a column of gas behind the withdrawn liquid column and interrupting the withdrawal of liquid from the reservoir. In the case of hazardous and toxic liquids, the sample bottle and the jet ejector may be isolated from the reservoir and may be further isolated from a control station containing remote manipulation means for the sample bottle and control valves for the jet ejector and gas bleed. 5 figs.

Liquid sampling system

DOEpatents

Larson, Loren L.

1987-01-01

A conduit extends from a reservoir through a sampling station and back to the reservoir in a closed loop. A jet ejector in the conduit establishes suction for withdrawing liquid from the reservoir. The conduit has a self-healing septum therein upstream of the jet ejector for receiving one end of a double-ended cannula, the other end of which is received in a serum bottle for sample collection. Gas is introduced into the conduit at a gas bleed between the sample collection bottle and the reservoir. The jet ejector evacuates gas from the conduit and the bottle and aspirates a column of liquid from the reservoir at a high rate. When the withdrawn liquid reaches the jet ejector the rate of flow therethrough reduces substantially and the gas bleed increases the pressure in the conduit for driving liquid into the sample bottle, the gas bleed forming a column of gas behind the withdrawn liquid column and interrupting the withdrawal of liquid from the reservoir. In the case of hazardous and toxic liquids, the sample bottle and the jet ejector may be isolated from the reservoir and may be further isolated from a control station containing remote manipulation means for the sample bottle and control valves for the jet ejector and gas bleed.

[Advances in Liquid Biopsy and its Clinical Application in the Diagnosis 
and Treatment of Non-small Cell Lung Cancer].

PubMed

Zheng, Difan; Chen, Haiquan

2016-06-20

With the advances of technology, great progresses have been made in liquid biopsy in recent years. Liquid biopsy is currently playing a more and more important role in early diagnosis and treatment of cancer. Compared with traditional tissue biopsy, liquid biopsy is more popular in clinical practice due to its non-invasiveness, convenience and high repeatability. It has huge potential in the future. This review introduces circulating tumor cells (CTCs) and circulating tumor DNA (ctDNA) as the most important objects in liquid biopsy, mainly focusing on their history, biological characteristics, detection technologies, limitations and applications in non-small cell lung cancer.

Ionic Liquid Dispersive Liquid-Liquid Microextraction Method for the Determination of Irinotecan, an Anticancer Drug, in Water and Urine Samples Using UV-Vis Spectrophotometry.

PubMed

Uysal, Deniz; Karadaş, Cennet; Kara, Derya

2017-05-01

A new, simple, efficient, and environmentally friendly ionic liquid dispersive liquid-liquid microextraction method was developed for the determination of irinotecan, an anticancer drug, in water and urine samples using UV-Vis spectrophotometry. The ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate was used as the extraction solvent, and ethanol was used as the disperser solvent. The main parameters affecting the extraction efficiency, including sample pH, volume of the ionic liquid, choice of the dispersive solvent and its volume, concentration of NaCl, and extraction and centrifugation times, were investigated and optimized. The effect of interfering species on the recovery of irinotecan was also examined. Under optimal conditions, the LOD (3σ) was 48.7 μg/L without any preconcentration. Because the urine sample was diluted 10-fold, the LOD for urine would be 487 μg/L. However, this could be improved 16-fold if preconcentration using a 40 mL aliquot of the sample is used. The proposed method was successfully applied to the determination of irinotecan in tap water, river water, and urine samples spiked with 10.20 mg/L for the water samples and 8.32 mg/L for the urine sample. The average recovery values of irinotecan determined were 99.1% for tap water, 109.4% for river water, and 96.1% for urine.

Effect of pressure on viscosity of liquid Fe-alloys up to 16 GPa

NASA Astrophysics Data System (ADS)

Terasaki, H.; Ohtani, E.; Suzuki, A.; Nishida, K.; Sakamaki, T.; Shindo, S.; Funakoshi, K.

2005-12-01

Viscosity of liquid Fe-alloy is closely related to a convection behavior of the Earth's liquid outer core and also time scale of planetary core formation. In previous studies, viscosity of liquid Fe-S has been measured up to 7 GPa using X-ray radiography falling sphere method [Terasaki et al. 2001]. However, some technical problems, such as chemical reaction between the metal marker sphere and the Fe-alloy sample and insufficient image recording time for less viscous material, have been suggested. In this study, we have measured the viscosity of Fe-S and Fe-C liquids without those problems by using novel techniques combined with in situ X-ray radiography falling sphere method and extended the pressure range to 16 GPa. Falling sphere viscometry was carried out under high pressure and temperature using high speed CCD camera with 1500 ton Kawai-type multi-anvil device at BL04B1, SPring-8 in Japan. Starting compositions of Fe-alloy were Fe78S22 and Fe86C14 which correspond to near eutectic compositions at the experimental pressures. Viscosity marker sphere, which was made of Re or Pt, was coated by alumina in order to prevent the reaction between the sphere and the Fe-alloy sample. Falling sphere images were obtained with recording rate of 50 - 125 frame/second. Viscosity of liquid Fe-S was measured up to 16.1 GPa and 1763 K. Measured viscosity coefficients were in the range of 8.8 - 9.2 mPa-s which indicates that the activation volume of viscous flow is approximately a half of the previous estimations (1.5 cm3/mol). Viscosity of liquid Fe-C was measured up to 5 GPa and 1843 K. Viscosity coefficients are 4.7 - 4.9 mPa-s. Activation volume of Fe-C liquid is estimated to be 0.8 cm3/mol. This pressure dependence is consistent with the result of Lucas (1964) measured at ambient pressure. Consequently, viscosity of Fe-alloy liquids are likely to stay small in the Earth's interior and there is no large difference in viscosity coefficient and activation volume between Fe-S and Fe-C eutectic liquids in the range of measurements.

13 CFR 107.1505 - Liquidity requirements for Licensees issuing Participating Securities.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false Liquidity requirements for Licensees issuing Participating Securities. 107.1505 Section 107.1505 Business Credit and Assistance SMALL BUSINESS ADMINISTRATION SMALL BUSINESS INVESTMENT COMPANIES SBA Financial Assistance for Licensees...

Open tubular lab-on-column/mass spectrometry for targeted proteomics of nanogram sample amounts.

PubMed

Hustoft, Hanne Kolsrud; Vehus, Tore; Brandtzaeg, Ole Kristian; Krauss, Stefan; Greibrokk, Tyge; Wilson, Steven Ray; Lundanes, Elsa

2014-01-01

A novel open tubular nanoproteomic platform featuring accelerated on-line protein digestion and high-resolution nano liquid chromatography mass spectrometry (LC-MS) has been developed. The platform features very narrow open tubular columns, and is hence particularly suited for limited sample amounts. For enzymatic digestion of proteins, samples are passed through a 20 µm inner diameter (ID) trypsin + endoproteinase Lys-C immobilized open tubular enzyme reactor (OTER). Resulting peptides are subsequently trapped on a monolithic pre-column and transferred on-line to a 10 µm ID porous layer open tubular (PLOT) liquid chromatography LC separation column. Wnt/ß-catenein signaling pathway (Wnt-pathway) proteins of potentially diagnostic value were digested+detected in targeted-MS/MS mode in small cell samples and tumor tissues within 120 minutes. For example, a potential biomarker Axin1 was identifiable in just 10 ng of sample (protein extract of ∼1,000 HCT15 colon cancer cells). In comprehensive mode, the current OTER-PLOT set-up could be used to identify approximately 1500 proteins in HCT15 cells using a relatively short digestion+detection cycle (240 minutes), outperforming previously reported on-line digestion/separation systems. The platform is fully automated utilizing common commercial instrumentation and parts, while the reactor and columns are simple to produce and have low carry-over. These initial results point to automated solutions for fast and very sensitive MS based proteomics, especially for samples of limited size.

Feasibility study of mid-infrared absorption spectroscopy using electrospray ionization

NASA Astrophysics Data System (ADS)

Ahmed, Tahsin; Foster, Erick; Bohn, Paul; Howard, Scott

2016-09-01

Precise detection of trace amount of molecules, such as the disease biomarkers present in biofluids or explosive residues, requires high sensitivity detection. electrospray ionization-mass spectrometry (ESI-MS) is a common and effective technique for sensitive trace molecular detection in small-volume liquid samples. In ESI-MS, nano-liter volume samples are ionized and aerosolized by ESI, and fed into MS for mass analysis. ESI-MS has proven to be a reliable ionization technique for coupling liquid phase separations like liquid chromatography (LC) and capillary zone electrophoresis (CE) with the highly specific resolving power of MS. While CE and ESI can be performed on a microfluidic chip having a footprint of a few cm2, MS is typically at least 100 times bigger in size than a micro-chip. A reduced size, weight, and power profile would enable semi-portable applications in forensics, environmental monitoring, defense, and biological/pharmaceutical applications. To achieve this goal, we present an initial study evaluating the use of mid-infrared absorption spectroscopy (MIRAS) in place of MS to create a ESI-MIRAS system. To establish feasibility, we perform ESI-MIRAS on phospholipid samples, which have been previously demonstrated to be separable by CE. Phospholipids are biomarkers of degenerative neurological, kidney, and bone diseases and can be found in biofluids such as blood, urine and cerebrospinal fluid. To establish sensitivity limits, calibration samples of 100 μM concentration are electrospray deposited on to a grounded Si wafer for different times (1 minutes to 4 minutes with a 1 minute step). The minimum detectable concentration-time product, where a FTIR globar is used as the MIR source, is found 200 μM·s.

Plasma capric acid concentrations in healthy subjects determined by high-performance liquid chromatography.

PubMed

Shrestha, Rojeet; Hui, Shu-Ping; Imai, Hiromitsu; Hashimoto, Satoru; Uemura, Naoto; Takeda, Seiji; Fuda, Hirotoshi; Suzuki, Akira; Yamaguchi, Satoshi; Hirano, Ken-Ichi; Chiba, Hitoshi

2015-09-01

Capric acid (FA10:0, decanoic acid) is a medium-chain fatty acid abundant in tropical oils such as coconut oil, whereas small amounts are present in milk of goat, cow, and human. Orally ingested FA10:0 is transported to the liver and quickly burnt within it. Only few reports are available for FA10:0 concentrations in human plasma. Fasting (n = 5, male/female = 3/2, age 31 ± 9.3 years old) and non-fasting (n = 106, male/female = 44/62, age 21.9 ± 3.2 years old) blood samples were collected from apparently healthy Japanese volunteers. The total FA10:0 in the plasma were measured by high-performance liquid chromatography after derivatization with 2-nitrophenylhydrazine followed by UV detection. Inter and intra-assay coefficient of variation of FA10:0 assay at three different concentrations ranged in 1.7-3.9 and 1.3-5.4%, respectively, with an analytical recovery of 95.2-104.0%. FA10:0 concentration was below detection limit (0.1 µmol/L) in each fasting human plasma. FA10:0 was not detected in 50 (47.2%) of 106 non-fasting blood samples, while 29 (27.4%) plasma samples contained FA10:0 less than or equal to 0.5 µmol/L (0.4 ± 0.1), and 27 (25.5%) contained it at more than 0.5 µmol/L (0.9 ± 0.3). A half of the non-fasting plasma samples contained detectable FA10:0. This simple, precise, and accurate high-performance liquid chromatography method might be useful for monitoring plasma FA10:0 during medium-chain triglycerides therapy. © The Author(s) 2015.

Concomitant ion effects on isotope ratio measurements with liquid sampling – atmospheric pressure glow discharge ion source Orbitrap mass spectrometry

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

Hoegg, Edward D.; Marcus, R. Kenneth; Hager, George J.

RATIONALE: The field of highly accurate and precise isotope ratio (IR) analysis has been dominated by inductively coupled plasma and thermal ionization mass spectrometers. While these instruments are considered the gold standard for IR analysis, the International Atomic Energy Agency desires a field deployable instrument capable of accurately and precisely measuring U isotope ratios. METHODS: The proposed system interfaces the liquid sampling – atmospheric pressure glow discharge (LS-APGD) ion source with a high resolution Exactive Orbitrap mass spectrometer. With this experimental setup certified U isotope standards and unknown samples were analyzed. The accuracy and precision of the system were thenmore » determined. RESULTS: The LS-APGD /Exactive instrument measures a certified reference material of natural U (235U/238U = 0.007258) as 0.007041 with a relative standard deviation of 0.158% meeting the International Target Values for Uncertainty for the destructive analysis of U. Additionally, when three unknowns measured and compared to the results from an ICP multi collector instrument, there is no statistical difference between the two instruments.CONCLUSIONS: The LS-APGD / Orbitrap system, while still in the preliminary stages of development, offers highly accurate and precise IR analysis that suggest a paradigm shift in the world of IR analysis. Furthermore, the portability of the LS-APGD as an elemental ion source combined with the low overhead and small size of the Orbitrap suggest that the instrumentation is capable of being field deployable.With liquid sampling glow discharge-Orbitrap MS, isotope ratio and precision performance improves with rejection of concomitant ion species.« less

Effects of dry brining, liquid smoking and high-pressure treatment on the physical properties of aquacultured King salmon (Oncorhynchus tshawytscha) during refrigerated storage.

PubMed

Kong, Kelvin Jia Wey; Alçiçek, Zayde; Balaban, Murat O

2015-03-15

Aquacultured King salmon (Oncorhynchus tshawytscha) pieces were dry brined with a salt/brown sugar mix, dipped in liquid smoke for 3 min, vacuum packed, high hydrostatic pressure (HHP) treated at 600 or 200 MPa for 5 min and stored at 4 °C for up to 40 days. The surface redness (average a*) of the samples increased after dry brining, then decreased after liquid smoke treatment. HHP did not change the outside color of liquid-smoked samples. However, the inside color changed depending on pressure. HHP-treated control samples without dry brining and liquid smoking changed to a pale pink color. HHP at 600 MPa resulted in a significant increase in hardness. Compared with fresh samples, dry-brined samples had reduced water activity, while samples dipped in liquid smoke had lower pH values. Dry brining and liquid smoking protect the outside color of salmon against changes caused by HHP. The increase in hardness may counteract the softening of the smoked salmon tissue over time. © 2014 Society of Chemical Industry.

Fixation and chemical analysis of single fog and rain droplets

NASA Astrophysics Data System (ADS)

Kasahara, M.; Akashi, S.; Ma, C.-J.; Tohno, S.

Last decade, the importance of global environmental problems has been recognized worldwide. Acid rain is one of the most important global environmental problems as well as the global warming. The grasp of physical and chemical properties of fog and rain droplets is essential to make clear the physical and chemical processes of acid rain and also their effects on forests, materials and ecosystems. We examined the physical and chemical properties of single fog and raindrops by applying fixation technique. The sampling method and treatment procedure to fix the liquid droplets as a solid particle were investigated. Small liquid particles like fog droplet could be easily fixed within few minutes by exposure to cyanoacrylate vapor. The large liquid particles like raindrops were also fixed successively, but some of them were not perfect. Freezing method was applied to fix the large raindrops. Frozen liquid particles existed stably by exposure to cyanoacrylate vapor after freezing. The particle size measurement and the elemental analysis of the fixed particle were performed in individual base using microscope, and SEX-EDX, particle-induced X-ray emission (PIXE) and micro-PIXE analyses, respectively. The concentration in raindrops was dependent upon the droplet size and the elapsed time from the beginning of rainfall.

High resolution full scan liquid chromatography mass spectrometry comprehensive screening in sports antidoping urine analysis.

PubMed

Abushareeda, Wadha; Vonaparti, Ariadni; Saad, Khadija Al; Almansoori, Moneera; Meloug, Mbarka; Saleh, Amal; Aguilera, Rodrigo; Angelis, Yiannis; Horvatovich, Peter L; Lommen, Arjen; Alsayrafi, Mohammed; Georgakopoulos, Costas

2018-03-20

The aim of this paper is to present the development and validation of a high-resolution full scan (HR-FS) electrospray ionization (ESI) liquid chromatography coupled to quadrupole Orbitrap mass spectrometer (LC/Q/Orbitrap MS) platform for the screening of prohibited substances in human urine according to World Antidoping Agency (WADA) requirements. The method was also validated for quantitative analysis of six endogenous steroids (epitestosterone, testosterone, 5α-dihydrotestosterone, dehydroepiandrosterone, androsterone and etiocholanolone) in their intact sulfates form. The sample preparation comprised a combination of a hydrolyzed urine liquid-liquid extraction and the dilute & shoot addition of original urine in the extracted aliquot. The HR-FS MS acquisition mode with Polarity Switching was applied in combination of the Quadrupole-Orbitrap mass filter. The HR-FS acquisition of analytical signal, for known and unknown small molecules, allows the inclusion of all analytes detectable with LC-MS for antidoping investigations to identify the use of known or novel prohibited substances and metabolites after electronic data files' reprocessing. The method has been validated to be fit-for-purpose for the antidoping analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Studying Dynamic Processes of Nano-sized Objects in Liquid using Scanning Transmission Electron Microscopy.

PubMed

Hermannsdörfer, Justus; de Jonge, Niels

2017-02-05

Samples fully embedded in liquid can be studied at a nanoscale spatial resolution with Scanning Transmission Electron Microscopy (STEM) using a microfluidic chamber assembled in the specimen holder for Transmission Electron Microscopy (TEM) and STEM. The microfluidic system consists of two silicon microchips supporting thin Silicon Nitride (SiN) membrane windows. This article describes the basic steps of sample loading and data acquisition. Most important of all is to ensure that the liquid compartment is correctly assembled, thus providing a thin liquid layer and a vacuum seal. This protocol also includes a number of tests necessary to perform during sample loading in order to ensure correct assembly. Once the sample is loaded in the electron microscope, the liquid thickness needs to be measured. Incorrect assembly may result in a too-thick liquid, while a too-thin liquid may indicate the absence of liquid, such as when a bubble is formed. Finally, the protocol explains how images are taken and how dynamic processes can be studied. A sample containing AuNPs is imaged both in pure water and in saline.

Studying Dynamic Processes of Nano-sized Objects in Liquid using Scanning Transmission Electron Microscopy

PubMed Central

Hermannsdörfer, Justus; de Jonge, Niels

2017-01-01

Samples fully embedded in liquid can be studied at a nanoscale spatial resolution with Scanning Transmission Electron Microscopy (STEM) using a microfluidic chamber assembled in the specimen holder for Transmission Electron Microscopy (TEM) and STEM. The microfluidic system consists of two silicon microchips supporting thin Silicon Nitride (SiN) membrane windows. This article describes the basic steps of sample loading and data acquisition. Most important of all is to ensure that the liquid compartment is correctly assembled, thus providing a thin liquid layer and a vacuum seal. This protocol also includes a number of tests necessary to perform during sample loading in order to ensure correct assembly. Once the sample is loaded in the electron microscope, the liquid thickness needs to be measured. Incorrect assembly may result in a too-thick liquid, while a too-thin liquid may indicate the absence of liquid, such as when a bubble is formed. Finally, the protocol explains how images are taken and how dynamic processes can be studied. A sample containing AuNPs is imaged both in pure water and in saline. PMID:28190028

A simple and selective method for determination of phthalate biomarkers in vegetable samples by high pressure liquid chromatography-electrospray ionization-tandem mass spectrometry.

PubMed

Zhou, Xi; Cui, Kunyan; Zeng, Feng; Li, Shoucong; Zeng, Zunxiang

2016-06-01

In the present study, solid-phase extraction cartridges including silica reversed-phase Isolute C18, polymeric reversed-phase Oasis HLB and mixed-mode anion-exchange Oasis MAX, and liquid-liquid extractions with ethyl acetate, n-hexane, dichloromethane and its mixtures were compared for clean-up of phthalate monoesters from vegetable samples. Best recoveries and minimised matrix effects were achieved using ethyl acetate/n-hexane liquid-liquid extraction for these target compounds. A simple and selective method, based on sample preparation by ultrasonic extraction and liquid-liquid extraction clean-up, for the determination of phthalate monoesters in vegetable samples by liquid chromatography/electrospray ionisation-tandem mass spectrometry was developed. The method detection limits for phthalate monoesters ranged from 0.013 to 0.120 ng g(-1). Good linearity (r(2)>0.991) between MQLs and 1000× MQLs was achieved. The intra- and inter-day relative standard deviation values were less than 11.8%. The method was successfully used to determine phthalate monoester metabolites in the vegetable samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction for the separation and determination of estrogens in water samples by high-performance liquid chromatography with fluorescence detection.

PubMed

Zhang, Rui; Wang, Chuanliu; Yue, Qiaohong; Zhou, Tiecheng; Li, Na; Zhang, Hanqi; Hao, Xiaoke

2014-11-01

An ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction method was proposed for the extraction and concentration of 17-α-estradiol, 17-β-estradiol-benzoate, and quinestrol in environmental water samples by high-performance liquid chromatography with fluorescence detection. 1-Hexyl-3-methylimidazolium tetrafluoroborate was applied as foaming agent in the foam flotation process and dispersive solvent in microextraction. The introduction of the ion-pairing and salting-out agent NH4 PF6 was beneficial to the improvement of recoveries for the hydrophobic ionic liquid phase and analytes. Parameters of the proposed method including concentration of 1-hexyl-3-methylimidazolium tetrafluoroborate, flow rate of carrier gas, floatation time, types and concentration of ionic liquids, salt concentration in samples, extraction time, and centrifugation time were evaluated. The recoveries were between 98 and 105% with relative standard deviations lower than 7% for lake water and well water samples. The isolation of the target compounds from the water was found to be efficient, and the enrichment factors ranged from 4445 to 4632. This developing method is free of volatile organic solvents compared with regular extraction. Based on the unique properties of ionic liquids, the application of foam floatation, and dispersive liquid-liquid microextraction was widened. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of triazine herbicides in juice samples by microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography.

PubMed

Su, Rui; Li, Dan; Wu, Lijie; Han, Jing; Lian, Wenhui; Wang, Keren; Yang, Hongmei

2017-07-01

A novel microextraction method, termed microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction, has been developed for the rapid enrichment and analysis of triazine herbicides in fruit juice samples by high-performance liquid chromatography. Instead of using hazardous organic solvents, two kinds of ionic liquids, a hydrophobic ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate) and a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate), were used as the extraction solvent and dispersion agent, respectively, in this method. The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of 1-hexyl-3-methylimidazolium hexafluorophosphate dispersed entirely into sample solution with the help of 1-butyl-3-methylimidazolium tetrafluoroborate. In addition, an ion-pairing agent (NH 4 PF 6 ) was introduced to improve recoveries of the ionic liquid phase. Several experimental parameters that might affect the extraction efficiency were investigated. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 5.00-250.00 μg/L, with the correlation coefficients of 0.9982-0.9997. The practical application of this effective and green method is demonstrated by the successful analysis of triazine herbicides in four juice samples, with satisfactory recoveries (76.7-105.7%) and relative standard deviations (lower than 6.6%). In general, this method is fast, effective, and robust to determine triazine herbicides in juice samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

48 CFR 19.705-7 - Liquidated damages.

Code of Federal Regulations, 2013 CFR

2013-10-01

...-disabled veteran-owned small business, HUBZone small business, small disadvantaged business and women-owned... veteran-owned small business, HUBZone small business, small disadvantaged business and women-owned small... small business, HUBZone small business, small disadvantaged business or women-owned small business...

Quantitative and Qualitative Aspects of Gas-Metal-Oxide Mass Transfer in High-Temperature Confocal Scanning Laser Microscopy

NASA Astrophysics Data System (ADS)

Piva, Stephano P. T.; Pistorius, P. Chris; Webler, Bryan A.

2018-05-01

During high-temperature confocal scanning laser microscopy (HT-CSLM) of liquid steel samples, thermal Marangoni flow and rapid mass transfer between the sample and its surroundings occur due to the relatively small sample size (diameter around 5 mm) and large temperature gradients. The resulting evaporation and steel-slag reactions tend to change the chemical composition in the metal. Such mass transfer effects can change observed nonmetallic inclusions. This work quantifies oxide-metal-gas mass transfer of solutes during HT-CSLM experiments using computational simulations and experimental data for (1) dissolution of MgO inclusions in the presence and absence of slag and (2) Ca, Mg-silicate inclusion changes upon exposure of a Si-Mn-killed steel to an oxidizing gas atmosphere.

Petrology and geochemistry of lithic fragments separated from the Apollo 15 deep-drill core

NASA Technical Reports Server (NTRS)

Lindstrom, M. M.; Nielsen, R. L.; Drake, M. J.

1977-01-01

Petrological and geochemical analysis of lithic fragments separated from the Apollo 15 deep-drill core showed these fragments to fall into the essentially the same range of rock types as observed in surface soil samples and large rock samples. Three particles are singled out as being of special interest. One sample is a mare basalt containing extremely evolved phases. The particle may represent small-scale imperfect crystal/liquid separation in a lava flow. A green glass particle is not the ultramafic emerald green glass described from the Apollo 15 site, but rather an ANT-like light green color, and has a quite different chemical composition from the ultramafic variety. One mare basalt displays a positive Eu anomaly and is enriched in plagioclase relative to olivine plus pyroxene.

Rapid method for measuring rotenone in water at piscicidal concentrations

USGS Publications Warehouse

Dawson, V.K.; Harman, P.D.; Schultz, D.P.; Allen, J.L.

1983-01-01

A high-performance liquid chromatography (HPLC) procedure that is rapid, specific, and sensitive (limit of detection <0.005 mg/liter) was developed for monitoring application and degradation rates of rotenone. For analysis, a water sample is buffered to pH 5 and injected through a Sep Pak(R) C18 disposable cartridge. The cartridge adsorbs and retains the rotenone which then can be eluted quantitatively from the cartridge with a small volume of methanol. This step effectively concentrates the sample and provides sample cleanup. The methanol extract is analyzed directly by HPLC on an MCH 10 reverse-phase column; methanol: water (75:25, volume : volume) is the mobile phase and flow rate is 1.5 ml/minute. The rotenone is detected by ultraviolet spectrophotometry at a wavelength of 295 nm.

Effect of Genetic Database Comprehensiveness on Fractional Proteomics of Escherichia coli O157:H7

DTIC Science & Technology

2014-01-01

proteins would be observed in the extracellular fraction. 15. SUBJECT TERMS Escherichia coli O157:H7 Liquid chromatography Mass spectrometry...Preparation ...............1 2.2 Liquid Chromatography /Mass Spectrometry Sample Preparation ....................2 2.3 Liquid Chromatography /Mass... Chromatography /Mass Spectrometry Sample Preparation. Samples were prepared for liquid chromatography tandem mass spectrometry (LC-MS/MS) in a similar

Possible overestimation of surface disinfection efficiency by assessment methods based on liquid sampling procedures as demonstrated by in situ quantification of spore viability.

PubMed

Grand, I; Bellon-Fontaine, M-N; Herry, J-M; Hilaire, D; Moriconi, F-X; Naïtali, M

2011-09-01

The standard test methods used to assess the efficiency of a disinfectant applied to surfaces are often based on counting the microbial survivors sampled in a liquid, but total cell removal from surfaces is seldom achieved. One might therefore wonder whether evaluations of microbial survivors in liquid-sampled cells are representative of the levels of survivors in whole populations. The present study was thus designed to determine the "damaged/undamaged" status induced by a peracetic acid disinfection for Bacillus atrophaeus spores deposited on glass coupons directly on this substrate and to compare it to the status of spores collected in liquid by a sampling procedure. The method utilized to assess the viability of both surface-associated and liquid-sampled spores included fluorescence labeling with a combination of Syto 61 and Chemchrome V6 dyes and quantifications by analyzing the images acquired by confocal laser scanning microscopy. The principal result of the study was that the viability of spores sampled in the liquid was found to be poorer than that of surface-associated spores. For example, after 2 min of peracetic acid disinfection, less than 17% ± 5% of viable cells were detected among liquid-sampled cells compared to 79% ± 5% or 47% ± 4%, respectively, when the viability was evaluated on the surface after or without the sampling procedure. Moreover, assessments of the survivors collected in the liquid phase, evaluated using the microscopic method and standard plate counts, were well correlated. Evaluations based on the determination of survivors among the liquid-sampled cells can thus overestimate the efficiency of surface disinfection procedures.

Possible Overestimation of Surface Disinfection Efficiency by Assessment Methods Based on Liquid Sampling Procedures as Demonstrated by In Situ Quantification of Spore Viability ▿

PubMed Central

Grand, I.; Bellon-Fontaine, M.-N.; Herry, J.-M.; Hilaire, D.; Moriconi, F.-X.; Naïtali, M.

2011-01-01

The standard test methods used to assess the efficiency of a disinfectant applied to surfaces are often based on counting the microbial survivors sampled in a liquid, but total cell removal from surfaces is seldom achieved. One might therefore wonder whether evaluations of microbial survivors in liquid-sampled cells are representative of the levels of survivors in whole populations. The present study was thus designed to determine the “damaged/undamaged” status induced by a peracetic acid disinfection for Bacillus atrophaeus spores deposited on glass coupons directly on this substrate and to compare it to the status of spores collected in liquid by a sampling procedure. The method utilized to assess the viability of both surface-associated and liquid-sampled spores included fluorescence labeling with a combination of Syto 61 and Chemchrome V6 dyes and quantifications by analyzing the images acquired by confocal laser scanning microscopy. The principal result of the study was that the viability of spores sampled in the liquid was found to be poorer than that of surface-associated spores. For example, after 2 min of peracetic acid disinfection, less than 17% ± 5% of viable cells were detected among liquid-sampled cells compared to 79% ± 5% or 47% ± 4%, respectively, when the viability was evaluated on the surface after or without the sampling procedure. Moreover, assessments of the survivors collected in the liquid phase, evaluated using the microscopic method and standard plate counts, were well correlated. Evaluations based on the determination of survivors among the liquid-sampled cells can thus overestimate the efficiency of surface disinfection procedures. PMID:21742922

Proposal of ultrasonic-assisted mid-infrared spectroscopy for incorporating into daily life like smart-toilet and non-invasive blood glucose sensor

NASA Astrophysics Data System (ADS)

Kitazaki, Tomoya; Mori, Keita; Yamamoto, Naoyuki; Wang, Congtao; Kawashima, Natsumi; Ishimaru, Ichiro

2017-07-01

We proposed the extremely compact beans-size snap-shot mid-infrared spectroscopy that will be able to be built in smartphones. And also the easy preparation method of thin-film samples generated by ultrasonic standing wave is proposed. Mid-infrared spectroscopy is able to identify material components and estimate component concentrations quantitatively from absorption spectra. But conventional spectral instruments were very large-size and too expensive to incorporate into daily life. And preparations of thin-film sample were very troublesome task. Because water absorption in mid-infrared lights is very strong, moisture-containing-sample thickness should be less than 100[μm]. Thus, midinfrared spectroscopy has been utilized only by analytical experts in their laboratories. Because ultrasonic standing wave is compressional wave, we can generate periodical refractive-index distributions inside of samples. A high refractiveindex plane is correspond to a reflection boundary. When we use a several MHz ultrasonic transducer, the distance between sample surface and generated first node become to be several ten μm. Thus, the double path of this distance is correspond to sample thickness. By combining these two proposed methods, as for liquid samples, urinary albumin and glucose concentrations will be able to be measured inside of toilet. And as for solid samples, by attaching these apparatus to earlobes, the enhancement of reflection lights from near skin surface will create a new path to realize the non-invasive blood glucose sensor. Using the small ultrasonic-transducer whose diameter was 10[mm] and applied voltage 8[V], we detected the internal reflection lights from colored water as liquid sample and acrylic board as solid sample.

Advances in the analysis of biological samples using ionic liquids.

PubMed

Clark, Kevin D; Trujillo-Rodríguez, María J; Anderson, Jared L

2018-02-12

Ionic liquids are a class of solvents and materials that hold great promise in bioanalytical chemistry. Task-specific ionic liquids have recently been designed for the selective extraction, separation, and detection of proteins, peptides, nucleic acids, and other physiologically relevant analytes from complex biological samples. To facilitate rapid bioanalysis, ionic liquids have been integrated in miniaturized and automated procedures. Bioanalytical separations have also benefited from the modification of nonspecific magnetic materials with ionic liquids or the implementation of ionic liquids with inherent magnetic properties. Furthermore, the direct detection of the extracted molecules in the analytical instrument has been demonstrated with structurally tuned ionic liquids and magnetic ionic liquids, providing a significant advantage in the analysis of low-abundance analytes. This article gives an overview of these advances that involve the application of ionic liquids and derivatives in bioanalysis. Graphical abstract Ionic liquids, magnetic ionic liquids, and ionic liquid-based sorbents are increasing the speed, selectivity, and sensitivity in the analysis of biological samples.

A novel percussion type droplet-on-demand generator

NASA Astrophysics Data System (ADS)

Hussain, Taaha; Patel, Priyesh; Balachandran, Ramanarayanan; Ladommatos, Nicos

2015-01-01

Numerous engineering applications require generation of droplets on demand which are of high uniformity and constant size. The common method to produce droplets is to drive liquid at high pressure through a small orifice/nozzle. The liquid stream disintegrates into small droplets. However this method normally requires large volumes of liquid and is not suitable for applications where single droplets of constant size is required. Such applications require droplet-on-demand generators which commonly employ piezoelectric or pneumatic actuation. It is well known that piezoelectric generators are hard to employ at high pressure and, high temperature applications, and the pneumatic generators often produce satellite (secondary) droplets. This paper describes the development of a novel percussion type droplet-on-demand generator, which overcomes some of the above difficulties and is capable of producing single droplets on demand. The generator consists of a cylindrical liquid filled chamber with a small orifice at the bottom. The top of the chamber is covered with a thin flexible metal disc. A small metal pin is employed to hammer/impact the top metal surface to generate a pressure pulse inside the liquid chamber. The movement and the momentum of the metal pin are controlled using a solenoid device. The pressure pulse generated overcomes the surface tension of the liquid meniscus at the exit of the orifice and ejects a single droplet. The work presented in this paper will demonstrate the capabilities of the droplet generator.

Semi-automated 96-well liquid-liquid extraction for quantitation of drugs in biological fluids.

PubMed

Zhang, N; Hoffman, K L; Li, W; Rossi, D T

2000-02-01

A semi-automated liquid-liquid extraction (LLE) technique for biological fluid sample preparation was introduced for the quantitation of four drugs in rat plasma. All liquid transferring during the sample preparation was automated using a Tomtec Quadra 96 Model 320 liquid handling robot, which processed up to 96 samples in parallel. The samples were either in 96-deep-well plate or tube-rack format. One plate of samples can be prepared in approximately 1.5 h, and the 96-well plate is directly compatible with the autosampler of an LC/MS system. Selection of organic solvents and recoveries are discussed. Also, precision, relative error, linearity and quantitation of the semi automated LLE method are estimated for four example drugs using LC/MS/MS with a multiple reaction monitoring (MRM) approach. The applicability of this method and future directions are evaluated.

Matrix Effect Compensation in Small-Molecule Profiling for an LC-TOF Platform Using Multicomponent Postcolumn Infusion.

PubMed

González, Oskar; van Vliet, Michael; Damen, Carola W N; van der Kloet, Frans M; Vreeken, Rob J; Hankemeier, Thomas

2015-06-16

The possible presence of matrix effect is one of the main concerns in liquid chromatography-mass spectrometry (LC-MS)-driven bioanalysis due to its impact on the reliability of the obtained quantitative results. Here we propose an approach to correct for the matrix effect in LC-MS with electrospray ionization using postcolumn infusion of eight internal standards (PCI-IS). We applied this approach to a generic ultraperformance liquid chromatography-time-of-flight (UHPLC-TOF) platform developed for small-molecule profiling with a main focus on drugs. Different urine samples were spiked with 19 drugs with different physicochemical properties and analyzed in order to study matrix effect (in absolute and relative terms). Furthermore, calibration curves for each analyte were constructed and quality control samples at different concentration levels were analyzed to check the applicability of this approach in quantitative analysis. The matrix effect profiles of the PCI-ISs were different: this confirms that the matrix effect is compound-dependent, and therefore the most suitable PCI-IS has to be chosen for each analyte. Chromatograms were reconstructed using analyte and PCI-IS responses, which were used to develop an optimized method which compensates for variation in ionization efficiency. The approach presented here improved the results in terms of matrix effect dramatically. Furthermore, calibration curves of higher quality are obtained, dynamic range is enhanced, and accuracy and precision of QC samples is increased. The use of PCI-ISs is a very promising step toward an analytical platform free of matrix effect, which can make LC-MS analysis even more successful, adding a higher reliability in quantification to its intrinsic high sensitivity and selectivity.

Surface treatment of polypropylene (PP) film by 50 Hz dielectric barrier discharge produced in air and argon/air mixture at atmospheric pressure

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

Joshi, Ujjwal Man, E-mail: umjoshi@gmail.com; Subedi, Deepak Prasad, E-mail: deepaksubedi2001@yahoo.com

Thin films of polypropylene (PP) are treated for improving hydrophilicity using non-thermal plasma generated by 50 Hz line frequency dielectric barrier discharge produced in air and argon/air mixture at atmospheric pressure. PP samples before and after the treatments are studied using contact angle measurements, surface free energy calculations and scanning electron microscopy (SEM). Distilled water (H{sub 2}O), glycerol (C{sub 3}H{sub 8}O{sub 3}) and diiodomethane (CH{sub 2}I{sub 2}) are used as test liquids. The contact angle measurements between test liquids and PP samples are used to determine total surface free energy using sessile drop technique. PP films show a remarkable increase inmore » surface free energy after plasma treatment. SEM analysis of the plasma-treated PP films shows that plasma treatment introduces greater roughness on the surface leading to the increased surface free energy. Furthermore, it is found that introducing a small quantity of argon can enhance the surface treatment remarkably.« less

Laser-desorption tandem time-of-flight mass spectrometry with continuous liquid introduction

NASA Astrophysics Data System (ADS)

Williams, Evan R.; Jones, Glenn C., Jr.; Fang, LiLing; Nagata, Takeshi; Zare, Richard N.

1992-05-01

A new method to combine aqueous sample introduction with matrix assisted laser desorption mass spectrometry (MS) for interfacing liquid-chromatographic techniques, such as capillary electrophoresis, to MS is described. Aqueous sample solution is introduced directly into the ion source of a time-of-. flight (TOF) mass spectrometer through a fused silica capillary; evaporative cooling results in ice formation at the end of the capillary. The ice can be made to extrude continuously by using localized resistive heating. With direct laser desorption, molecular ions from proteins as large as bovine insulin (5734 Da) can be produced. Two-step desorption/photoionization with a variety of wavelengths is demonstrated, and has the advantages of improved resolution and shot-to-shot reproducibility. Ion structural information is obtained using surface-induced dissociation with an in-line collision device in the reflectron mirror of the TOF instrument. Product ion resolution of ~70 is obtained at m/z77. Extensive fragmentation can be produced with dissociation efficiencies between 7-15% obtained for molecular ions of small organic molecules. Efficiencies approaching 30% are obtained for larger peptide ions.

Peculiar phase diagram with isolated superconducting regions in ThFeAsN1‑x O x

NASA Astrophysics Data System (ADS)

Li, Bai-Zhuo; Wang, Zhi-Cheng; Wang, Jia-Lu; Zhang, Fu-Xiang; Wang, Dong-Ze; Zhang, Feng-Yuan; Sun, Yu-Ping; Jing, Qiang; Zhang, Hua-Fu; Tan, Shu-Gang; Li, Yu-Ke; Feng, Chun-Mu; Mei, Yu-Xue; Wang, Cao; Cao, Guang-Han

2018-06-01

ThFeAsN1‑x O x () system with heavy electron doping has been studied by the measurements of x-ray diffraction, electrical resistivity, magnetic susceptibility and specific heat. The non-doped compound exhibits superconductivity at K, which is possibly due to an internal uniaxial chemical pressure that is manifested by the extremely small value of As height with respect to the Fe plane. With the oxygen substitution, the T c value decreases rapidly to below 2 K for , and surprisingly, superconductivity re-appears in the range of with a maximum of 17.5 K at x  =  0.3. For the normal-state resistivity, while the samples in intermediate non-superconducting interval exhibit Fermi liquid behavior, those in other regions show a non-Fermi-liquid behavior. The specific heat jump for the superconducting sample of x  =  0.4 is , which is discussed in terms of anisotropic superconducting gap. The peculiar phase diagram in ThFeAsN1‑x O x presents additional ingredients for understanding the superconducting mechanism in iron-based superconductors.

Tests of PMT signal read-out of liquid argon scintillation with a new fast waveform digitizer

NASA Astrophysics Data System (ADS)

Acciarri, R.; Canci, N.; Cavanna, F.; Cortopassi, A.; D'Incecco, M.; Mini, G.; Pietropaolo, F.; Romboli, A.; Segreto, E.; Szelc, A. M.

2012-07-01

The CAEN V1751 is a new generation of Waveform Digitizer recently introduced by CAEN SpA. It features 8 Channels per board, 10 bit, 1 GS/s using Flash ADCs Waveform Digitizers (or 4 channels at 2 GS/s in Dual Edge Sampling mode) with threshold and Auto-Trigger capabilities. This provides a good basis for data acquisition in Dark Matter searches using PMTs to detect scintillation light in liquid argon, as it matches the requirements for measuring the fast scintillation component. The board was tested by operating it in real experimental conditions and by comparing it with a state of the art digital oscilloscope. We find that the sampling at 1 or 2 GS/s is appropriate for the reconstruction of the fast component of the scintillation light in argon (characteristic time of about 6-7 ns) and the extended dynamic range, after a small customization, allows for the detection of signals in the range of energy needed. The bandwidth is found to be adequate and the intrinsic noise is very low.

Liquid microjunction surface sampling coupled with high-pressure liquid chromatography-electrospray ionization-mass spectrometry for analysis of drugs and metabolites in whole-body thin tissue sections.

PubMed

Kertesz, Vilmos; Van Berkel, Gary J

2010-07-15

In this work, a commercially available autosampler was adapted to perform direct liquid microjunction (LMJ) surface sampling followed by a high-pressure liquid chromatography (HPLC) separation of the extract components and detection with electrospray ionization mass spectrometry (ESI-MS). To illustrate the utility of coupling a separation with this direct liquid extraction based surface sampling approach, four different organs (brain, lung, kidney, and liver) from whole-body thin tissue sections of propranolol dosed and control mice were examined. The parent drug was observed in the chromatograms of the surface sampling extracts from all the organs of the dosed mouse examined. In addition, two isomeric phase II metabolites of propranolol (an aliphatic and an aromatic hydroxypropranolol glucuronide) were observed in the chromatograms of the extracts from lung, kidney, and liver. Confirming the presence of one or the other or both of these glucuronides in the extract from the various organs was not possible without the separation. These drug and metabolite data obtained using the LMJ surface sampling/HPLC-MS method and the results achieved by analyzing similar samples by conventional extraction of the tissues and subsequent HPLC-MS analysis were consistent. The ability to directly and efficiently sample from thin tissue sections via a liquid extraction and then perform a subsequent liquid phase separation increases the utility of this liquid extraction surface sampling approach.

Metabolomics: A Primer.

PubMed

Liu, Xiaojing; Locasale, Jason W

2017-04-01

Metabolomics generates a profile of small molecules that are derived from cellular metabolism and can directly reflect the outcome of complex networks of biochemical reactions, thus providing insights into multiple aspects of cellular physiology. Technological advances have enabled rapid and increasingly expansive data acquisition with samples as small as single cells; however, substantial challenges in the field remain. In this primer we provide an overview of metabolomics, especially mass spectrometry (MS)-based metabolomics, which uses liquid chromatography (LC) for separation, and discuss its utilities and limitations. We identify and discuss several areas at the frontier of metabolomics. Our goal is to give the reader a sense of what might be accomplished when conducting a metabolomics experiment, now and in the near future. Copyright © 2017 Elsevier Ltd. All rights reserved.

Re-electrospraying splash-landed proteins and nanoparticles.

PubMed

Benner, W Henry; Lewis, Gregory S; Hering, Susanne V; Selgelke, Brent; Corzett, Michelle; Evans, James E; Lightstone, Felice C

2012-03-06

FITC-albumin, Lsr-F, or fluorescent polystyrene latex particles were electrosprayed from aqueous buffer and subjected to dispersion by differential electrical mobility at atmospheric pressure. A resulting narrow size cut of singly charged molecular ions or particles was passed through a condensation growth tube collector to create a flow stream of small water droplets, each carrying a single ion or particle. The droplets were splash landed (impacted) onto a solid or liquid temperature controlled surface. Small pools of droplets containing size-selected particles, FITC-albumin, or Lsr-F were recovered, re-electrosprayed, and, when analyzed a second time by differential electrical mobility, showed increased homogeneity. Transmission electron microscopy (TEM) analysis of the size-selected Lsr-F sample corroborated the mobility observation.

Dynamics and structure of an aging binary colloidal glass

NASA Astrophysics Data System (ADS)

Lynch, Jennifer M.; Cianci, Gianguido C.; Weeks, Eric R.

2008-09-01

We study aging in a colloidal suspension consisting of micron-sized particles in a liquid. This system is made glassy by increasing the particle concentration. We observe samples composed of particles of two sizes, with a size ratio of 1:2.1 and a volume fraction ratio 1:6, using fast laser scanning confocal microscopy. This technique yields real-time, three-dimensional movies deep inside the colloidal glass. Specifically, we look at how the size, motion, and structural organization of the particles relate to the overall aging of the glass. Particles move in spatially heterogeneous cooperative groups. These mobile regions tend to be richer in small particles, and these small particles facilitate the motion of nearby particles of both sizes.

Solubility of structurally complicated materials: 3. Hair.

PubMed

Horvath, Ari L

2009-04-27

Hair is composed of proteins, lipids, water, and small amounts of trace elements. All proteins in animal and human bodies are built from permutations of amino acid molecules in a polypeptide string. The polypeptide chains of protein keratin are organized into filaments in hair cells. Hair is one of the most difficult proteins to digest or solubilize. Among the most common dissolving procedures for hair are acidic, alkaline, and enzymatic hydrolysis. For the analysis of hair, the solid samples are transferred by solubilization via digestion into a liquid phase. Small molecular solvents and molecules with hydrophobic groups appear to have higher affinity for hair. A good solvent attacks the disulfide bonds between cystine molecules and hydrates the hair shaft. Consequently, the hair becomes a jelly-like mass.

Microfluidic interconnects

DOEpatents

Benett, William J.; Krulevitch, Peter A.

2001-01-01

A miniature connector for introducing microliter quantities of solutions into microfabricated fluidic devices, and which incorporates a molded ring or seal set into a ferrule cartridge, with or without a compression screw. The fluidic connector, for example, joins standard high pressure liquid chromatography (HPLC) tubing to 1 mm diameter holes in silicon or glass, enabling ml-sized volumes of sample solutions to be merged with .mu.l-sized devices. The connector has many features, including ease of connect and disconnect; a small footprint which enables numerous connectors to be located in a small area; low dead volume; helium leak-tight; and tubing does not twist during connection. Thus the connector enables easy and effective change of microfluidic devices and introduction of different solutions in the devices.

Description and evaluation of a peracetic acid air sampling and analysis method.

PubMed

Nordling, John; Kinsky, Owen R; Osorio, Magdalena; Pechacek, Nathan

2017-12-01

Peracetic acid (PAA) is a corrosive chemical with a pungent odor, which is extensively used in occupational settings and causes various health hazards in exposed workers. Currently, there is no US government agency recommended method that could be applied universally for the sampling and analysis of PAA. Legacy methods for determining airborne PAA vapor levels frequently suffered from cross-reactivity with other chemicals, particularly hydrogen peroxide (H 2 O 2 ). Therefore, to remove the confounding factor of cross-reactivity, a new viable, sensitive method was developed for assessment of PAA exposure levels, based on the differential reaction kinetics of PAA with methyl p-tolylsulfide (MTS), relative to H 2 O 2 , to preferentially derive methyl p-tolysulfoxide (MTSO). By quantifying MTSO concentration produced in the liquid capture solution from an air sampler, using an internal standard, and utilizing the reaction stoichiometry of PAA and MTS, the original airborne concentration of PAA is determined. After refining this liquid trap high-performance liquid chromatography (HPLC) method in the laboratory, it was tested in five workplace settings where PAA products were used. PAA levels ranged from the detection limit of 0.013 parts per million (ppm) to 0.4 ppm. The results indicate a viable and potentially dependable method to assess the concentrations of PAA vapors under occupational exposure scenarios, though only a small number of field measurements were taken while field testing this method. However, the low limit of detection and precision offered by this method makes it a strong candidate for further testing and validation to expand the uses of this liquid trap HPLC method.

Measurement of activity coefficients of mixtures by head-space gas chromatography: general procedure.

PubMed

Luis, Patricia; Wouters, Christine; Van der Bruggen, Bart; Sandler, Stanley I

2013-08-09

Head-space gas chromatography (HS-GC) is an applicable method to perform vapor-liquid equilibrium measurements and determine activity coefficients. However, the reproducibility of the data may be conditioned by the experimental procedure concerning to the automated pressure-balanced system. The study developed in this work shows that a minimum volume of liquid in the vial is necessary to ensure the reliability of the activity coefficients since it may become a parameter that influences the magnitude of the peak areas: the helium introduced during the pressurization step may produce significant variations of the results when too small volume of liquid is selected. The minimum volume required should thus be evaluated prior to obtain experimentally the concentration in the vapor phase and the activity coefficients. In this work, the mixture acetonitrile-toluene is taken as example, requiring a sample volume of more than 5mL (about more than 25% of the vial volume). The vapor-liquid equilibrium and activity coefficients of mixtures at different concentrations (0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 molar fraction) and four temperatures (35, 45, 55 and 70°C) have been determined. Relative standard deviations (RSD) lower than 5% have been obtained, indicating the good reproducibility of the method when a sample volume larger than 5mL is used. Finally, a general procedure to measure activity coefficients by means of pressure-balanced head-space gas chromatography is proposed. Copyright © 2013 Elsevier B.V. All rights reserved.

Effective hydrogen generator testing for on-site small engine

NASA Astrophysics Data System (ADS)

Chaiwongsa, Praitoon; Pornsuwancharoen, Nithiroth; Yupapin, Preecha P.

2009-07-01

We propose a new concept of hydrogen generator testing for on-site small engine. In general, there is a trade-off between simpler vehicle design and infrastructure issues, for instance, liquid fuels such as gasoline and methanol for small engine use. In this article we compare the hydrogen gases combination the gasoline between normal systems (gasoline only) for small engine. The advantage of the hydrogen combines gasoline for small engine saving the gasoline 25%. Furthermore, the new concept of hydrogen combination for diesel engine, bio-diesel engine, liquid petroleum gas (LPG), natural gas vehicle (NGV), which is discussed in details.

Characteristics of acoustic emissions from shearing of granular media

NASA Astrophysics Data System (ADS)

Michlmayr, Gernot; Cohen, Denis; Or, Dani

2010-05-01

Deformation and abrupt formation of small failure cracks on hillslopes often precede sudden release of shallow landslides. The associated frictional sliding, breakage of cementing agents and rupture of embedded biological fibers or liquid bonds between grain contacts are associated with measurable acoustic emissions (AE). The aim of this study was to characterize small scale shear induced failure events (as models of precursors prior to a landslide) by capturing elastic body waves emitted from such events. We conducted a series of experiments with a specially-designed shear frame to measure and characterize high frequency (kHz range) acoustic emissions under different conditions using piezoelectric sensors. Tests were performed at different shear rates ranging from 0.01mm/sec to 2mm/sec with different dry and wet granular materials. In addition to acoustic emissions the setup allows to measure forces and deformations in both horizontal and vertical directions. Results provide means to define characteristic AE signature for different failure events. We observed an increase in AE activity during dilation of granular samples. In wet material AE signals were attributed to the snap-off of liquid bridges between single gains. Acoustic emissions clearly provide an experimental tool for exploring micro-mechanical processes in dry and wet material. Moreover, high sampling rates found in most AE systems coupled with waveguides to overcome signal attenuation offer a promise for field applications as an early warning method for observing the progressive development of slip planes prior to the onset of a landslide.

Clinical evaluation of human papillomavirus detection by careHPV™ test on physician-samples and self-samples using the indicating FTA Elute® card.

PubMed

Wang, Shao-Ming; Hu, Shang-Ying; Chen, Feng; Chen, Wen; Zhao, Fang-Hui; Zhang, Yu-Qing; Ma, Xin-Ming; Qiao, You-Lin

2014-01-01

To make the clinical evaluation of a solid-state human papillomavirus (HPV) sampling medium in combination with an economical HPV testing method (careHPV™) for cervical cancer screening. 396 women aged 25-65 years were enrolled for cervical cancer screening, and four samples were collected. Two samples were collected by woman themselves, among which one was stored in DCM preservative solution (called "liquid sample") and the other was applied on the Whatman Indicating FTA Elute® card (FTA card). Another two samples were collected by physician and stored in DCM preservative solution and FTA card, respectively. All the samples were detected by careHPV™ test. All the women were administered a colposcopy examination, and biopsies were taken for pathological confirmation if necessary. FTA card demonstrated a comparable sensitivity of detecting high grade Cervical Intraepithelial Neoplasia (CIN) with the liquid sample carrier for self and physician-sampling, but showed a higher specificity than that of liquid sample carrier for self-sampling (FTA vs Liquid: 79.0% vs 71.6%, p=0.02). Generally, the FTA card had a comparable accuracy with that of Liquid-based medium by different sampling operators, with an area under the curve of 0.807 for physician and FTA, 0.781 for physician and Liquid, 0.728 for self and FTA, and 0.733 for self and Liquid (p>0.05). FTA card is a promising sample carrier for cervical cancer screening. With appropriate education programmes and further optimization of the experimental workflow, FTA card based self-collection in combination with centralized careHPV™ testing can help expand the coverage of cervical cancer screening in low-resource areas.

Demonstrating Paramagnetism Using Liquid Nitrogen.

ERIC Educational Resources Information Center

Simmonds, Ray; And Others

1994-01-01

Describes how liquid nitrogen is attracted to the poles of neodymium magnets. Nitrogen is not paramagnetic, so the attraction suggests that the liquid nitrogen contains a small amount of oxygen, which causes the paramagnetism. (MVL)

Microanalysis of the antiretroviral nevirapine in human hair from HIV-infected patients by liquid chromatography-tandem mass spectrometry

PubMed Central

Huang, Yong; Yang, Qiyun; Yoon, Kwangchae; Lei, Yovnne; Shi, Robert; Gee, Winnie; Lin, Emil T.; Greenblatt, Ruth M.; Gandhi, Monica

2012-01-01

Sufficient drug exposure is crucial for maintaining durable responses to HIV treatments. However, monitoring drug exposure using single blood samples only provides short-term information and is highly subject to intra-individual pharmacokinetic variation. Drugs can accumulate in hair over a long period of time, so hair drug levels can provide drug exposure information over prolonged periods. We now report on a specific, sensitive and reproducible LC-MS/MS method for measuring nevirapine (NVP), a widely used antiretroviral drug, levels in human hair using even a single short strand of hair. Hair samples are cut into small segments and drug is extracted in methanol/trifluoroacetic acid (v/v, 9:1) shaken at 37°C in a water bath overnight, followed by liquid-liquid extraction under alkaline conditions. The extracted samples are then separated on a BDS-C18 column with mobile phase composed as 50% acetonitrile containing 0.15% acetic acid and 4 mM ammonium acetate with an isocratic elution for a total run time of 3 min. and detected by triple quadrupole electrospray multiple reaction mode at precursor/product ion at 267.0>225.9 m/z. Deuterated nevirapine-d5 was used as internal standard. This method was validated from 0.25 to 100 ng/mg using 2 mg hair samples. The accuracies for spiked NVP hair control samples were 98–106% with coefficients of variation (CV) less than 10%. The CV for incurred hair control samples was less than 7%. The extraction efficiency for incurred control hair samples was estimated at more than 95% by repeated extractions. This method has been successfully applied to analyze more than 1000 hair samples from participants in a large ongoing cohort study of HIV-infected participants. We also showed that nevirapine in human hair can easily be detected in a single short strand of hair. This method will allow us to identify drug non-adherence using even a single strand of hair. PMID:21847531

Effect of Yifukang oral liquid on gastric emptying and intestinal peristalsis in mice

NASA Astrophysics Data System (ADS)

Sun, Jianhua; Li, Jun; Li, Xianyu; Hao, Shaojun; Guo, Junyi; Ma, Zhenzhen; Zhang, Zhengchen

2018-04-01

To observe the effect of Yifukang oral liquid on gastric emptying and intestinal peristalsis in mice. Methods: 60 mice were randomly divided into 5 groups. The suspension of Baohe Pill and the same volume of normal saline group were given once a day for 7 days. After the last administration for 30 minutes, 0.25 ml of 0.04% phenolic red solution was administered by stomach. After 20 minutes, the animals were killed, the stomach was removed, the gastric contents were cleaned, and the lotion 5ml was centrifuged. The absorbance of the supernatant was measured by TU-1901 ultraviolet spectrophotometer at the wavelength of 560nm. The residual rate of gastric phenolic red was calculated. Rate was used to evaluate gastric emptying velocity.60 mice were randomly divided into five groups: group 5, large, medium, small Yifukang oral liquid dosage group, pill suspension and the same volume normal saline. After 20 min after the last dose of carbon powder suspension, the mice were sacrificed, the abdominal cavity was cut open, the intestine of the ileocecum was cut off, the intestinal mesentery was separated, the total length of the small intestine (cm) was measured, and the distance (cm) in the small intestine was measured, and the end-of-carbon propulsion rate was calculated. Compared with the blank group, small dose of Yi Fu Kang group and Baohe Pill group could significantly promote the ability of gastric emptying in mice. Compared with the blank group, small dose group and rehabilitation benefits Baohewan group can significantly promote the gastric emptying ability of mice (P<0.01), high dose group had no obvious benefit rehabilitation ability to promote gastric emptying in mice. Yi Fu Kang oral liquid group could significantly increase the percentage of small intestine carbon powder(P<0.01), Large, medium-dose Yifukang oral liquid and Baofuwan group could significantly increase the percentage of small intestinal carbon in mice (P<0.05). Yi Fukang oral liquid has the effect of promoting gastric emptying and small intestinal peristalsis.

Ionic liquid-based air-assisted liquid-liquid microextraction followed by high performance liquid chromatography for the determination of five fungicides in juice samples.

PubMed

You, Xiangwei; Chen, Xiaochu; Liu, Fengmao; Hou, Fan; Li, Yiqiang

2018-01-15

A novel and simple ionic liquid-based air-assisted liquid-liquid microextraction technique combined with high performance liquid chromatography was developed to analyze five fungicides in juice samples. In this method, ionic liquid was used instead of a volatile organic solvent as the extraction solvent. The emulsion was formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent repeatedly using a 10mL glass syringe. No organic dispersive solvent was required. Under the optimized conditions, the limits of detection (LODs) were 0.4-1.8μgL -1 at a signal-to-noise ratio of 3. The limits of quantification (LOQs) set as the lowest spiking levels with acceptable recovery in juices were 10μgL -1 , except for fludioxonil whose LOQ was 20μgL -1 . The proposed method was applied to determine the target fungicides in juice samples, and acceptable recoveries ranging from 74.9% to 115.4% were achieved. Copyright © 2017. Published by Elsevier Ltd.

Development of New Supramolecular Lyotropic Liquid Crystals and Their Application as Alignment Media for Organic Compounds.

PubMed

Leyendecker, Martin; Meyer, Nils-Christopher; Thiele, Christina M

2017-09-11

Most alignment media for the residual dipolar coupling (RDC) based molecular structure determination of small organic compounds consist of rod-like polymers dissolved in organic solvents or of swollen cross-linked polymer gels. Thus far, the synthesis of polymer-based alignment media has been a challenging process, which is often followed by a time-consuming sample preparation. We herein propose the use of non-polymeric alignment media based on benzenetricarboxamides (BTAs), which self-assemble into rod-like supramolecules. Our newly found supramolecular lyotropic liquid crystals (LLCs) are studied in terms of their LLC properties and their suitability as alignment media in NMR spectroscopy. Scalable enantiodifferentiating properties are introduced through a sergeant-and-soldier principle by blending achiral with chiral substituted BTAs. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of sulfonamides in swine muscle after salting-out assisted liquid extraction with acetonitrile coupled with back-extraction by a water/acetonitrile/dichloromethane ternary component system prior to high-performance liquid chromatography.

PubMed

Tsai, Wen-Hsien; Huang, Tzou-Chi; Chen, Ho-Hsien; Wu, Yuh-Wern; Huang, Joh-Jong; Chuang, Hung-Yi

2010-01-15

A salting-out assisted liquid extraction coupled with back-extraction by a water/acetonitrile/dichloromethane ternary component system combined with high-performance liquid chromatography with diode-array detection (HPLC-DAD) was developed for the extraction and determination of sulfonamides in solid tissue samples. After the homogenization of the swine muscle with acetonitrile and salt-promoted partitioning, an aliquot of 1 mL of the acetonitrile extract containing a small amount of dichloromethane (250-400 microL) was alkalinized with diethylamine. The clear organic extract obtained by centrifugation was used as a donor phase and then a small amount of water (40-55 microL) could be used as an acceptor phase to back-extract the analytes in the water/acetonitrile/dichloromethane ternary component system. In the back-extraction procedure, after mixing and centrifuging, the sedimented phase would be water and could be withdrawn easily into a microsyringe and directly injected into the HPLC system. Under the optimal conditions, recoveries were determined for swine muscle fortified at 10 ng/g and quantification was achieved by matrix-matched calibration. The calibration curves of five sulfonamides showed linearity with the coefficient of estimation above 0.998. Relative recoveries for the analytes were all from 96.5 to 109.2% with relative standard deviation of 2.7-4.0%. Preconcentration factors ranged from 16.8 to 30.6 for 1 mL of the acetonitrile extract. Limits of detection ranged from 0.2 to 1.0 ng/g. 2009 Elsevier B.V. All rights reserved.

Quantitative determination of risperidone, paliperidone and olanzapine in human serum by liquid chromatography-tandem mass spectrometry coupled with on-line solid-phase extraction.

PubMed

Ruan, Can-Jun; Guo, Wei; Zhou, Miao; Guo, Gui-Xin; Wang, Chuan-Yue; Li, Wen-Biao; de Leon, Jose

2018-07-01

A recent guideline recommends therapeutic drug monitoring for risperidone, paliperidone and olanzapine, which are frequently used second-generation antipsychotics. We developed a simple high-performance liquid chromatography-tandem mass spectrometry coupled with an online solid-phase extraction method that can be used to measure risperidone, paliperidone and olanzapine using small (40 μL) samples. The analytes were extracted from serum samples automatically pre-concentrated and purified by C 8 (5 μm, 2.1 × 30 mm) solid-phase extraction cartridges, then chromatographed on an Xbidge™ C 18 column (3.5 μm, 100 × 2.1 mm) thermostatted at 30°C with a mobile phase consisting of 70% acetonitrile and 30% ammonium hydroxide 1% solution at an isocratic flow rate of 0.3 mL/min, and detected with tandem mass spectrometry. The assay was validated in the concentration range from 2.5 to 160 ng/mL. Intra- and inter-day precision for all analytes was between 1.1 and 8.2%; method accuracy was between 6.6 and 7.6%. The risperidone and paliperidone assay was compared with a high-performance liquid chromatography-ultraviolet assay currently used in our hospital for risperidone and paliperidone therapeutic drug monitoring, and the results of weighted Deming regression analysis showed good agreement. For the olanzapine assay, we compared 20 samples in separate re-assays on different days; all the relative errors were within the 20% recommended limit. Copyright © 2018 John Wiley & Sons, Ltd.

Liquid/Gas Flow Mixers

NASA Technical Reports Server (NTRS)

Fabris, Gracio

1994-01-01

Improved devices mix gases and liquids into bubbly or foamy flows. Generates flowing, homogeneous foams or homogeneous dispersions of small, noncoalescing bubbles entrained in flowing liquids. Mixers useful in liquid-metal magnetohydrodynamic electric-power generator, froth flotation in mining industry, wastewater treatment, aerobic digestion, and stripping hydrocarbon contaminants from ground water.

Crystallization in Micellar Cores: confinement effects and dynamics

NASA Astrophysics Data System (ADS)

Lund, Reidar; Zinn, Thomas; Willner, Lutz; Department of Chemistry, University of Oslo Team; Forschungszentrum Jülich Collaboration

It is well known that liquids confined to small nanoscopic pores and droplets exhibit thermal behavior very different from bulk samples. Here we demonstrate that n-alkanes forming 2-3 nm small micellar cores are considerably affected by confinement in analogue with hard confined systems. We study micelles form by self-assembly of a series of well-defined n-Alkyl-PEO polymers in aqueous solutions. By using small-angle X-ray scattering (SAXS), densiometry and differential scanning calorimetry (DSC), we show that n-alkane exhibit a first-order phase transition i.e. melting. Correlating the structural and thermodynamic data, we find that a melting depression can be accurately described by the Gibbs-Thomson equation. ∖f1 The effect of core crystallinity on the molecular exchange kinetics is investigated using time-resolved small-angle neutron scattering (TR-SANS). We show that there are considerable entropic and enthalpic contributions from the chain packing that affect the kinetic stability of micelles. ∖pard

Zoonotic Agents in Small Ruminants Kept on City Farms in Southern Germany

PubMed Central

Schilling, Anna-Katarina; Hotzel, Helmut; Methner, Ulrich; Sprague, Lisa D.; Schmoock, Gernot; El-Adawy, Hosny; Ehricht, Ralf; Wöhr, Anna-Caroline; Erhard, Michael

2012-01-01

Sheep and goats are popular examples of livestock kept on city farms. In these settings, close contacts between humans and animals frequently occur. Although it is widely accepted that small ruminants can carry numerous zoonotic agents, it is unknown which of these agents actually occur in sheep and goats on city farms in Germany. We sampled feces and nasal liquid of 48 animals (28 goats, 20 sheep) distributed in 7 city farms and on one activity playground in southern Germany. We found that 100% of the sampled sheep and 89.3% of the goats carried Shiga toxin-producing Escherichia coli (STEC). The presence of Staphylococcus spp. in 75% of both sheep and goats could be demonstrated. Campylobacter spp. were detected in 25% and 14.3% of the sheep and goats, respectively. Neither Salmonella spp. nor Coxiella burnetii was found. On the basis of these data, we propose a reasonable hygiene scheme to prevent transmission of zoonotic agents during city farm visits. PMID:22447607

Optical determination of crystal phase in semiconductor nanocrystals

PubMed Central

Lim, Sung Jun; Schleife, André; Smith, Andrew M.

2017-01-01

Optical, electronic and structural properties of nanocrystals fundamentally derive from crystal phase. This is especially important for polymorphic II–VI, III–V and I-III-VI2 semiconductor materials such as cadmium selenide, which exist as two stable phases, cubic and hexagonal, each with distinct properties. However, standard crystallographic characterization through diffraction yields ambiguous phase signatures when nanocrystals are small or polytypic. Moreover, diffraction methods are low-throughput, incompatible with solution samples and require large sample quantities. Here we report the identification of unambiguous optical signatures of cubic and hexagonal phases in II–VI nanocrystals using absorption spectroscopy and first-principles electronic-structure theory. High-energy spectral features allow rapid identification of phase, even in small nanocrystals (∼2 nm), and may help predict polytypic nanocrystals from differential phase contributions. These theoretical and experimental insights provide simple and accurate optical crystallographic analysis for liquid-dispersed nanomaterials, to improve the precision of nanocrystal engineering and improve our understanding of nanocrystal reactions. PMID:28513577

Liquid chromatography of polymers under limiting conditions of desorption II. Tandem injection and quantitative molar mass determination.

PubMed

Snauko, Marián; Berek, Dusan

2005-11-11

Liquid chromatography under limiting conditions of desorption (LC LCD) is a method which allows molar mass independent elution of various synthetic polymers. A narrow, slowly moving zone of small molecules, which promotes full adsorption of one kind of polymer species within column (an adsorli) acts as an impermeable barrier for the fast moving macromolecules. The latter accumulate on the barrier edge and elute nearly in total volume of liquid within column. At the same time, transport of less adsorptive macromolecules is not hampered so that these are eluted in the size exclusion (SEC) mode. As result, polymers differing in their polarity and adsorptivity can be easily separated without molar mass interference. Three methods of barrier creation are discussed and compared. It is shown that a fraction of sample may elute unretained if the adsorli sample solvent is used as a barrier in connection with a narrow-pore column packing. One part of excluded macromolecules likely breaks-out from the adsorli zone and this results in partial loss of sample and distortion of the LC LCD peaks. This problem can be avoided if the adsorli zone is injected immediately before sample solution. Applicability of the LC LCD method for polymer separation has been demonstrated with a model mixture of poly(methyl methacrylate) (adsorbing polymer) and polystyrene (non adsorbing polymer) using bare silica gel as a column packing with a combination of tetrahydrofuran (a desorption promoting liquid -a desorli) and toluene (adsorli). It has been shown that the LC LCD procedure with tandem injection allows simple and fast discrimination of polymer blend components with good repeatability and high sample recovery. For quantitative determination of molar masses of both LC LCD and SEC eluted polymers, an additional size exclusion chromatographic column can be applied either in a conventional way or in combination with a multi-angle light scattering detector. A single eluent is used in the latter column, which separates the mixed mobile phase, system peaks and the desorli zone from the polymer peaks so that measurements are free from disturbances caused by the changing eluent composition. The resulting LC LCD x SEC procedure has been successfully applied to poly(methyl methacrylate) samples.

Liquid film on a circular plate formed by a droplet train impingement

NASA Astrophysics Data System (ADS)

Sanada, Toshiyuki; Yamamoto, Shoya

2017-11-01

Droplet impingement phenomena are found in the wide variety of industrial processes, however the detail of liquid film structure formed by the continuous impact of droplets is not clarified. In this study, we experimentally investigated behavior of liquid film which was formed by a droplet train impact. Especially, we focus on the diameter of hydraulic jump formed on a circular plate. The effects of nozzle diameter, liquid surface tension and liquid flow rate on the jump diameter were investigated. In addition, we compared the liquid film by the droplet train impact with that by a liquid column impact. As a result, the hydraulic jump was observed under the smaller water flow rate condition compare to the liquid column impact. And the jump diameters for the case of droplet train impact were greater than that of liquid column impact. However, the jump diameters for the small surface tension liquid for the case of droplet train impact were smaller than that of liquid column impact. We consider that this phenomenon is related to both high speed lateral flow after droplet impact and splash formation. In addition, the liquid film heights after hydraulic jump on a small circular plate were sensitive to either the droplet train impact or liquid column impact.

A fast passive and planar liquid sample micromixer.

PubMed

Melin, Jessica; Gimenéz, Guillem; Roxhed, Niclas; van der Wijngaart, Wouter; Stemme, Göran

2004-06-01

A novel microdevice for passively mixing liquid samples based on surface tension and a geometrical mixing chamber is presented. Due to the laminar flow regime on the microscale, mixing becomes difficult if not impossible. We present a micromixer where a constantly changing time dependent flow pattern inside a two sample liquid plug is created as the plug simply passes through the planar mixer chamber. The device requires no actuation during mixing and is fabricated using a single etch process. The effective mixing of two coloured liquid samples is demonstrated.

Tidal sampler

DOEpatents

Hayes, David W.

1978-01-01

An apparatus for pumping a sample of water or other liquid that uses the energy generated from the rise and fall of the liquid level to force a sample of the liquid into a collection vessel. A suction vessel and booster vessel with interconnecting tubing and check valves are responsive to an oscillating liquid level to pump a portion of said liquid into a collection vessel.

Microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid for the determination of sulfonamides in environmental water samples.

PubMed

Song, Ying; Wu, Lijie; Lu, Chunmei; Li, Na; Hu, Mingzhu; Wang, Ziming

2014-12-01

An easy, quick, and green method, microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid, was first developed and applied to the extraction of sulfonamides in environmental water samples. 1-Ethy-3-methylimidazolium hexafluorophosphate, which is a solid-state ionic liquid at room temperature, was used as extraction solvent in the present method. After microwave irradiation for 90 s, the solid-state ionic liquid was melted into liquid phase and used to finish the extraction of the analytes. The ionic liquid and sample matrix can be separated by freezing and centrifuging. Several experimental parameters, including amount of extraction solvent, microwave power and irradiation time, pH of sample solution, and ionic strength, were investigated and optimized. Under the optimum experimental conditions, good linearity was observed in the range of 2.00-400.00 μg/L with the correlation coefficients ranging from 0.9995 to 0.9999. The limits of detection for sulfathiazole, sulfachlorpyridazine, sulfamethoxazole, and sulfaphenazole were 0.39, 0.33, 0.62, and 0.85 μg/L, respectively. When the present method was applied to the analysis of environmental water samples, the recoveries of the analytes ranged from 75.09 to 115.78% and relative standard deviations were lower than 11.89%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Small-scale experimental study of vaporization flux of liquid nitrogen released on water.

PubMed

Gopalaswami, Nirupama; Olewski, Tomasz; Véchot, Luc N; Mannan, M Sam

2015-10-30

A small-scale experimental study was conducted using liquid nitrogen to investigate the convective heat transfer behavior of cryogenic liquids released on water. The experiment was performed by spilling five different amounts of liquid nitrogen at different release rates and initial water temperatures. The vaporization mass fluxes of liquid nitrogen were determined directly from the mass loss measured during the experiment. A variation of initial vaporization fluxes and a subsequent shift in heat transfer mechanism were observed with changes in initial water temperature. The initial vaporization fluxes were directly dependent on the liquid nitrogen spill rate. The heat flux from water to liquid nitrogen determined from experimental data was validated with two theoretical correlations for convective boiling. It was also observed from validation with correlations that liquid nitrogen was found to be predominantly in the film boiling regime. The substantial results provide a suitable procedure for predicting the heat flux from water to cryogenic liquids that is required for source term modeling. Copyright © 2015 Elsevier B.V. All rights reserved.

Online reverse phase-high-performance liquid chromatography-fluorescence detection-electrospray ionization-mass spectrometry separation and characterization of heparan sulfate, heparin, and low-molecular weight-heparin disaccharides derivatized with 2-aminoacridone.

PubMed

Galeotti, Fabio; Volpi, Nicola

2011-09-01

A high-resolution online reverse-phase-high-performance liquid chromatography (RP-HPLC)-fluorescence detector (Fd)-electrospray ionization-mass spectrometry (ESI-MS) separation and structural characterization of disaccharides prepared from heparin (Hep), heparan sulfate (HS), and various low-molecular-weight (LMW)-Hep using heparin lyases and derivatization with 2-aminoacridone (AMAC) are described. A total of 12 commercially available Hep/HS-derived unsaturated disaccharides were separated and unambiguously identified on the basis of their retention times and mass spectra. The constituent disaccharides of various samples, including unfractionated Hep/HS, fast-moving and slow-moving Hep components, and several marketed products, were characterized. Furthermore, for the first time, the saturated trisulfated disaccharide belonging to the nonreducing end of Heps was detected as being approximately 2% in unfractionated samples and ~15-21% in LMW-Heps prepared by nitrous acid depolymerization. No desalting of the commercial products prior to enzymatic digestion or prepurification steps to eliminate any excess of AMAC reagent or interference from proteins, peptides, and other sample impurities before RP-HPLC-Fd-ESI-MS injection were necessary. This method has applicability for the rapid differentiation of pharmaceutical Heps and LMW-Heps prepared by means of different depolymerization processes and for compositional analysis of small amounts of samples derived from biological sources by using the highly sensitive fluorescence detector.

Effects of laser fluence and liquid media on preparation of small Ag nanoparticles by laser ablation in liquid

NASA Astrophysics Data System (ADS)

Moura, Caroline Gomes; Pereira, Rafael Santiago Floriani; Andritschky, Martin; Lopes, Augusto Luís Barros; Grilo, João Paulo de Freitas; Nascimento, Rubens Maribondo do; Silva, Filipe Samuel

2017-12-01

This study aims to assess a method for preparation of small and highly stable Ag nanoparticles by nanosecond laser ablation in liquid. Effect of liquid medium and laser fluence on the size, morphology and structure of produced nanoparticles has been studied experimentally. Pulses of a Nd:YAG laser of 1064 nm wavelength at 35 ns pulse width at different fluences were employed to irradiate the silver target in different environments (water, ethanol and acetone). The UV-Visible absorption spectra of nanoparticles exhibit surface plasmon resonance absorption peak in the UV region. STEM and TEM micrographs were used to evaluate the size and shape of nanoparticles. The stability of silver colloids in terms of oxidation at different liquid media was analyzed by SAED patterns. The results showed that characteristics of Ag nanoparticles and their production rate were strongly influenced by varying laser fluence and liquid medium. Particles from 2 to 80 nm of diameter were produced using different conditions and no oxidation was found in ethanol and acetone media. This work puts in evidence a promising approach to produce small nanoparticles by using high laser fluence energy.

Structure-Antibacterial Activity Relationships of Imidazolium-Type Ionic Liquid Monomers, Poly(ionic liquids) and Poly(ionic liquid) Membranes: Effect of Alkyl Chain Length and Cations.

PubMed

Zheng, Zhiqiang; Xu, Qiming; Guo, Jiangna; Qin, Jing; Mao, Hailei; Wang, Bin; Yan, Feng

2016-05-25

The structure-antibacterial activity relationship between the small molecular compounds and polymers are still elusive. Here, imidazolium-type ionic liquid (IL) monomers and their corresponding poly(ionic liquids) (PILs) and poly(ionic liquid) membranes were synthesized. The effect of chemical structure, including carbon chain length of substitution at the N3 position and charge density of cations (mono- or bis-imidazolium) on the antimicrobial activities against both Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus) was investigated by determination of minimum inhibitory concentration (MIC). The antibacterial activities of both ILs and PILs were improved with the increase of the alkyl chain length and higher charge density (bis-cations) of imidazolium cations. Moreover, PILs exhibited lower MIC values relative to the IL monomers. However, the antibacterial activities of PIL membranes showed no correlation to those of their analogous small molecule IL monomers and PILs, which increased with the charge density (bis-cations) while decreasing with the increase of alkyl chain length. The results indicated that antibacterial property studies on small molecules and homopolymers may not provide a solid basis for evaluating that in corresponding polymer membranes.

Preconcentration and determination of ceftazidime in real samples using dispersive liquid-liquid microextraction and high-performance liquid chromatography with the aid of experimental design.

PubMed

Razmi, Rasoul; Shahpari, Behrouz; Pourbasheer, Eslam; Boustanifar, Mohammad Hasan; Azari, Zhila; Ebadi, Amin

2016-11-01

A rapid and simple method for the extraction and preconcentration of ceftazidime in aqueous samples has been developed using dispersive liquid-liquid microextraction followed by high-performance liquid chromatography analysis. The extraction parameters, such as the volume of extraction solvent and disperser solvent, salt effect, sample volume, centrifuge rate, centrifuge time, extraction time, and temperature in the dispersive liquid-liquid microextraction process, were studied and optimized with the experimental design methods. Firstly, for the preliminary screening of the parameters the taguchi design was used and then, the fractional factorial design was used for significant factors optimization. At the optimum conditions, the calibration curves for ceftazidime indicated good linearity over the range of 0.001-10 μg/mL with correlation coefficients higher than the 0.98, and the limits of detection were 0.13 and 0.17 ng/mL, for water and urine samples, respectively. The proposed method successfully employed to determine ceftazidime in water and urine samples and good agreement between the experimental data and predictive values has been achieved. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and characterization of mesoporous ZnS with narrow size distribution of small pores

NASA Astrophysics Data System (ADS)

Nistor, L. C.; Mateescu, C. D.; Birjega, R.; Nistor, S. V.

2008-08-01

Pure, nanocrystalline cubic ZnS forming a stable mesoporous structure was synthesized at room temperature by a non-toxic surfactant-assisted liquid liquid reaction, in the 9.5 10.5 pH range of values. The appearance of an X-ray diffraction (XRD) peak in the region of very small angles (˜ 2°) reveals the presence of a porous material with a narrow pore size distribution, but with an irregular arrangement of the pores, a so-called worm hole or sponge-like material. The analysis of the wide angle XRD diffractograms shows the building blocks to be ZnS nanocrystals with cubic structure and average diameter of 2 nm. Transmission electron microscopy (TEM) investigations confirm the XRD results; ZnS crystallites of 2.5 nm with cubic (blende) structure are the building blocks of the pore walls with pore sizes from 1.9 to 2.5 nm, and a broader size distribution for samples with smaller pores. Textural measurements (N2 adsorption desorption isotherms) confirm the presence of mesoporous ZnS with a narrow range of small pore sizes. The relatively lower surface area of around 100 m2/g is attributed to some remaining organic molecules, which are filling the smallest pores. Their presence, confirmed by IR spectroscopy, seems to be responsible for the high stability of the resulting mesoporous ZnS as well.

A magnetic resonance (MR) microscopy system using a microfluidically cryo-cooled planar coil.

PubMed

Koo, Chiwan; Godley, Richard F; Park, Jaewon; McDougall, Mary P; Wright, Steven M; Han, Arum

2011-07-07

We present the development of a microfluidically cryo-cooled planar coil for magnetic resonance (MR) microscopy. Cryogenically cooling radiofrequency (RF) coils for magnetic resonance imaging (MRI) can improve the signal to noise ratio (SNR) of the experiment. Conventional cryostats typically use a vacuum gap to keep samples to be imaged, especially biological samples, at or near room temperature during cryo-cooling. This limits how close a cryo-cooled coil can be placed to the sample. At the same time, a small coil-to-sample distance significantly improves the MR imaging capability due to the limited imaging depth of planar MR microcoils. These two conflicting requirements pose challenges to the use of cryo-cooling in MR microcoils. The use of a microfluidic based cryostat for localized cryo-cooling of MR microcoils is a step towards eliminating these constraints. The system presented here consists of planar receive-only coils with integrated cryo-cooling microfluidic channels underneath, and an imaging surface on top of the planar coils separated by a thin nitrogen gas gap. Polymer microfluidic channel structures fabricated through soft lithography processes were used to flow liquid nitrogen under the coils in order to cryo-cool the planar coils to liquid nitrogen temperature (-196 °C). Two unique features of the cryo-cooling system minimize the distance between the coil and the sample: (1) the small dimension of the polymer microfluidic channel enables localized cooling of the planar coils, while minimizing thermal effects on the nearby imaging surface. (2) The imaging surface is separated from the cryo-cooled planar coil by a thin gap through which nitrogen gas flows to thermally insulate the imaging surface, keeping it above 0 °C and preventing potential damage to biological samples. The localized cooling effect was validated by simulations, bench testing, and MR imaging experiments. Using this cryo-cooled planar coil system inside a 4.7 Tesla MR system resulted in an average image SNR enhancement of 1.47 ± 0.11 times relative to similar room-temperature coils. This journal is © The Royal Society of Chemistry 2011

A Magnetic Resonance (MR) Microscopy System using a Microfluidically Cryo-Cooled Planar Coil

PubMed Central

Koo, Chiwan; Godley, Richard F.; Park, Jaewon; McDougall, Mary P.; Wright, Steven M.; Han, Arum

2011-01-01

We present the development of a microfluidically cryo-cooled planar coil for magnetic resonance (MR) microscopy. Cryogenically cooling radiofrequency (RF) coils for magnetic resonance imaging (MRI) can improve the signal to noise ratio (SNR) of the experiment. Conventional cryostats typically use a vacuum gap to keep samples to be imaged, especially biological samples, at or near room temperature during cryo-cooling. This limits how close a cryo-cooled coil can be placed to the sample. At the same time, a small coil-to-sample distance significantly improves the MR imaging capability due to the limited imaging depth of planar MR microcoils. These two conflicting requirements pose challenges to the use of cryo-cooling in MR microcoils. The use of a microfluidic based cryostat for localized cryo-cooling of MR microcoils is a step towards eliminating these constraints. The system presented here consists of planar receive-only coils with integrated cryo-cooling microfluidic channels underneath, and an imaging surface on top of the planar coils separated by a thin nitrogen gas gap. Polymer microfluidic channel structures fabricated through soft lithography processes were used to flow liquid nitrogen under the coils in order to cryo-cool the planar coils to liquid nitrogen temperature (−196°C). Two unique features of the cryo-cooling system minimize the distance between the coil and the sample: 1) The small dimension of the polymer microfluidic channel enables localized cooling of the planar coils, while minimizing thermal effects on the nearby imaging surface. 2) The imaging surface is separated from the cryo-cooled planar coil by a thin gap through which nitrogen gas flows to thermally insulate the imaging surface, keeping it above 0°C and preventing potential damage to biological samples. The localized cooling effect was validated by simulations, bench testing, and MR imaging experiments. Using this cryo-cooled planar coil system inside a 4.7 Tesla MR system resulted in an average image SNR enhancement of 1.47 ± 0.11 times relative to similar room-temperature coils. PMID:21603723

Solid-phase extraction of small biologically active peptides on cartridges and microelution 96-well plates from human urine.

PubMed

Semenistaya, Ekaterina; Zvereva, Irina; Krotov, Grigory; Rodchenkov, Grigory

2016-09-01

Currently liquid chromatography - mass spectrometry (LC-MS) analysis after solid-phase extraction (SPE) on weak cation-exchange cartridges is a method of choice for anti-doping analysis of small bioactive peptides such as growth hormone releasing peptides (GHRPs), desmoporessin, LHRH, and TB-500 short fragment. Dilution of urine samples with phosphate buffer for pH adjustment and SPE on weak cation exchange microelution plates was tested as a means to increase throughput of this analysis. Dilution using 200 mM phosphate buffer provides good buffering capacity without affecting the peptides recoveries. SPE on microelution plates was performed on Waters Positive Pressure-96 Processor with subsequent evaporation of eluates in nitrogen flow. Though the use of smaller sample volume decreases the pre-concentration factor and increases the limits of detection of 5 out of 17 detected peptides, the recovery, linearity, and reproducibility of the microelution extraction were comparable with cartridge SPE. The effectiveness of protocols was confirmed by analysis of urine samples containing ipamorelin, and GHRP-6 and its metabolites. SPE after urine sample dilution with buffer can be used for faster sample preparation. The use of microelution plates decreases consumption of solvents and allows processing of up to 96 samples simultaneously. Cartridge SPE with manual рН adjustment remains the best option for confirmation. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

Application of an ultrasonic focusing radiator for acoustic levitation of submillimeter samples

NASA Technical Reports Server (NTRS)

Lee, M. C.

1981-01-01

An acoustic apparatus has been specifically developed to handle samples of submillimeter size in a gaseous medium. This apparatus consists of an acoustic levitation device, deployment devices for small liquid and solid samples, heat sources for sample heat treatment, acoustic alignment devices, a cooling system and data-acquisition instrumentation. The levitation device includes a spherical aluminum dish of 12 in. diameter and 0.6 in. thickness, 130 pieces of PZT transducers attached to the back side of the dish and a spherical concave reflector situated in the vicinity of the center of curvature of the dish. The three lowest operating frequencies for the focusing-radiator levitation device are 75, 105 and 163 kHz, respectively. In comparison with other levitation apparatus, it possesses a large radiation pressure and a high lateral positional stability. This apparatus can be used most advantageously in the study of droplets and spherical shell systems, for instance, for fusion target applications.

Biobriefcase aerosol collector heater

DOEpatents

Bell, Perry M [Tracy, CA; Christian, Allen T [Madison, WI; Bailey, Christopher G [Pleasanton, CA; Willis, Ladona [Manteca, CA; Masquelier, Donald A [Tracy, CA; Nasarabadi, Shanavaz L [Livermore, CA

2009-03-17

A system for sampling air and collecting particles potentially including bioagents entrained in the air for detection. The system comprises collecting a sample of the air with the particles entrained in the air, directing the sample to a receiving surface, directing a liquid to the receiving surface thereby producing a liquid surface, wherein the particles potentially including bioagents become captured in the liquid, and heating the liquid wherein the particles potentially including bioagents become heated to lysis the bioagents.

Gas-liquid chromatographic and gas-liquid-mass spectometric determination of fenvalerate and permethrin residues in grasshoppers and duck tissue samples

USGS Publications Warehouse

Reichel, W.L.; Kolbe, E.J.; Stafford, C.J.

1981-01-01

A procedure is described for determining fenvalerate and permethrin residues in grasshoppers and duck tissues. Samples are Soxhlet-extracted with hexane and cleaned up by gel permeation chromatography with an in-line alumina column. Samples are analyzed by gas-liquid chromatography with electron capture detection, and confirmed by gas-liquid chromatography-mass spectrometry. The average recovery from fortified tissues was 97%.

Science Using an Electrostatic Levitation Furnace in the MUCAT Sector at the APS

NASA Technical Reports Server (NTRS)

Goldman, A.; Kelton, K. F.; Rogers, J. R.

2004-01-01

The original motivation for the construction of the BESL prototype was to obtain the first proof of a 50-year-old hypothesis regarding the solidification of liquid metals. Since the 1950s it has been known that under proper conditions liquid metals can be cooled below their melting temperature (undercooled) without crystallizing to the stable solid phase. In 1952 Frank proposed that this was because the atoms in the metallic liquid were arranged with the symmetry of an icosahedron, a Platonic solid consisting of 20 tetrahedra (4-sided pyramid-shaped polyhedra) arranged around a common center. Since this local atomic order is incompatible with the long-range translational periodicity of crystal phases, a barrier is formed to the formation of small regions of the crystal phase, the nucleation barrier. A proof of Frank's hypothesis required a direct correlation between measured icosahedral order in the undercooled liquid and the nucleation barrier. The tendency of sample containers to catalyze nucleation obscured this relation, requiring containerless techniques. Combining containerless processing techniques for electrostatically levitated droplets (ESL) with x-ray synchrotron methods, a team from Washington University, St. Louis, MO, NASA Marshall Space Flight Center, and MUCAT at the APS demonstrated an increasing icosahedral order in TiZrNi liquids with decreasing temperature below the melting temperature. The increased icosahedral order caused the transformation of the liquid to a metastable icosahedral quasicrystal phase, instead of the stable tetrahedrally-coordinated crystal intermetallic, giving the first clear demonstration of the connection between the nucleation barrier and the local structure of the liquid, verifying Frank's hypothesis for this alloy.

Determination of Meteorite Porosity Using Liquid Nitrogen

NASA Technical Reports Server (NTRS)

Kohout, T.; Kletetschka, G.; Pesonen, L. J.; Wasilewski, P. J.

2005-01-01

We introduce a new harmless method for porosity measurement suitable for meteorite samples. The method is a modification of the traditional Archimedean method based on immersion of the samples in a liquid medium like water or organic liquids. In our case we used liquid nitrogen for its chemically inert characteristics.

Colloidal mode of transport in the Potomac River watershed

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

Maher, I.L.; Foster, G.D.

1995-12-31

Similarly to the particulate phase the colloidal phase may play an important role in the organic contaminant transport downstream the river. The colloidal phase consisting of microparticles and micromolecules which are small enough to be mobile and large enough to attract pollutants can absorb nonpolar organic compounds similarly as do soil and sediment particles. To test the hypothesis three river water samples have been analyzed for PAH content in the dissolved, the colloidal, and the particulate phase. The first sample was collected at the Blue Ridge province of Potomac River watershed, at Point of Rocks, the second one in themore » Pidmont province, at Riverbend Park, and the third sample at Coastal Plane, at Dyke Marsh (Belle Heven marina). In the laboratory environment each water sample was prefiltered to separate the particulate phase form the dissolved and colloidal phase. One part of the prefiltered water sample was ultrafiltered to separate colloids while the second part of the water was Goulden extracted. The separated colloidal phase was liquid-liquid extracted (LLE) while filters containing the suspended solids were Soxhlet extracted. The extracts of the particulate phase, the colloidal phase, and the dissolved plus colloidal phase were analyzed for selected PAHs via GC/MS. It is planned that concentrations of selected PAHs in three phases will be used for calculations of the partition coefficients, the colloid/dissolved partition coefficient and the particle/dissolved partition coefficient. Both partition coefficients will be compared to define the significance of organic contaminant transport by aquatic colloids.« less

Development of gas chromatography-flame ionization detection system with a single column and liquid nitrogen-free for measuring atmospheric C2-C12 hydrocarbons.

PubMed

Liu, Chengtang; Mu, Yujing; Zhang, Chenglong; Zhang, Zhibo; Zhang, Yuanyuan; Liu, Junfeng; Sheng, Jiujiang; Quan, Jiannong

2016-01-04

A liquid nitrogen-free GC-FID system equipped with a single column has been developed for measuring atmospheric C2-C12 hydrocarbons. The system is consisted of a cooling unit, a sampling unit and a separation unit. The cooling unit is used to meet the temperature needs of the sampling unit and the separation unit. The sampling unit includes a dehydration tube and an enrichment tube. No breakthrough of the hydrocarbons was detected when the temperature of the enrichment tube was kept at -90 °C and sampling volume was 400 mL. The separation unit is a small round oven attached on the cooling column. A single capillary column (OV-1, 30 m × 0.32 mm I.D.) was used to separate the hydrocarbons. An optimal program temperature (-60 ∼ 170 °C) of the oven was achieved to efficiently separate C2-C12 hydrocarbons. There were good linear correlations (R(2)=0.993-0.999) between the signals of the hydrocarbons and the enrichment amount of hydrocarbons, and the relative standard deviation (RSD) was less than 5%, and the method detection limits (MDLs) for the hydrocarbons were in the range of 0.02-0.10 ppbv for sampling volume of 400 mL. Field measurements were also conducted and more than 50 hydrocarbons from C2 to C12 were detected in Beijing city. Copyright © 2015 Elsevier B.V. All rights reserved.

Qualitative analysis of Pb liquid sample using laser-induced breakdown spectroscopy (LIBS)

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

Suyanto, Hery; Rupiasih, Ni Nyoman; Winardi, T. B.

2013-09-03

Qualitative analysis of liquid sample containing 1,000 ppm of Pb was performed by using LIBS technique. In order to avoid splashing off of the liquid sample during laser irradiation, a sample pretreatment was done, namely the liquid sample was absorbed by using commercial available stomach medicine. Two kinds of absorbent materials were chosen in this experiment, first containing 125 mg activated carbon and second 600 mg activated attapulgite. These absorbent materials were used since carbon sample gives better absorption of infrared laser irradiation used in this experiment. In order to characterize the absorption process, three treatments were conducted in thismore » experiment; first, without heating the sample but varying the absorption time before laser irradiation; second by varying the heating temperature after certain time of absorption process and third by varying the temperature only. The maximum emission intensity of Pb I 405.7 nm was found in the second treatment of heating the sample till 85°C after 30 minutes absorption of the liquid sample in both absorbent materials.« less

A small-angle x-ray scattering system with a vertical layout

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

Wang, Zhen; Chen, Xiaowei; Meng, Lingpu

A small-angle x-ray scattering (SAXS) system with a vertical layout (V-SAXS) has been designed and constructed for in situ detection on nanostructures, which is well suitable for in situ study on self-assembly of nanoparticles at liquid interface and polymer processing. A steel-tower frame on a reinforced basement is built as the supporting skeleton for scattering beam path and detector platform, ensuring the system a high working stability and a high operating accuracy. A micro-focus x-ray source combining parabolic three-dimensional multi-layer mirror and scatteringless collimation system provides a highly parallel beam, which allows us to detect the very small angle range.more » With a sample-to-detector distance of 7 m, the largest measurable length scale is 420 nm in real space. With a large sample zone, it is possible to install different experimental setups such as film stretching machine, which makes the system perfect to follow the microstructures evolution of materials during processing. The capability of the V-SAXS on in situ study is tested with a drying experiment of a free latex droplet, which confirms our initial design.« less

Ion Formation Resulting from Freezing, Thawing, and Collisional Processes in Plumes Emitted from Planetary Bodies: Implications for Plume Chemistry and the Detection of Trace Organics Present in Enceladus Geysers

NASA Astrophysics Data System (ADS)

Beauchamp, J. L.; Wiley, J. S.; Thomas, D. A.

2014-12-01

Icy plumes emitted into space from Enceladus and other planetary bodies offer the intriguing possibility of sampling the composition of subsurface liquid reservoirs that may comprise habitable zones of particular astrobiological significance in our solar system. Mass spectrometric sampling of plume materials enables the detection of molecules that facilitate an assessment of the extent of chemical and biological evolution that may have occurred in a subsurface sea. In laboratory experiments we have investigated the physical and chemical processes that occur in the complex plume environment that lead to ionization of trace organic constituents, both as a result of the freezing of liquid droplets and the thawing of icy particles. We also demonstrate that collisions between icy particles lead to triboelectric charging. Subsequent discharges between oppositely charged particles result not only in the ionization of trace organics but to chemical reactions between molecular components present in the particles. For example, nitriles react with water to form amides and acids. In particular, icy particles doped with small amounts of aminoacetonitrile and water lead to the formation of the simplest amino acid glycine. The implications which these observations may have for sampling plume composition from orbit in a future mission to Enceladus will be discussed.

Drop size distributions and related properties of fog for five locations measured from aircraft

NASA Technical Reports Server (NTRS)

Zak, J. Allen

1994-01-01

Fog drop size distributions were collected from aircraft as part of the Synthetic Vision Technology Demonstration Program. Three west coast marine advection fogs, one frontal fog, and a radiation fog were sampled from the top of the cloud to the bottom as the aircraft descended on a 3-degree glideslope. Drop size versus altitude versus concentration are shown in three dimensional plots for each 10-meter altitude interval from 1-minute samples. Also shown are median volume radius and liquid water content. Advection fogs contained the largest drops with median volume radius of 5-8 micrometers, although the drop sizes in the radiation fog were also large just above the runway surface. Liquid water content increased with height, and the total number of drops generally increased with time. Multimodal variations in number density and particle size were noted in most samples where there was a peak concentration of small drops (2-5 micrometers) at low altitudes, midaltitude peak of drops 5-11 micrometers, and high-altitude peak of the larger drops (11-15 micrometers and above). These observations are compared with others and corroborate previous results in fog gross properties, although there is considerable variation with time and altitude even in the same type of fog.

Morphological transitions of brain sphingomyelin are determined by the hydration protocol: ripples re-arrange in plane, and sponge-like networks disintegrate into small vesicles.

PubMed

Meyer, H W; Bunjes, H; Ulrich, A S

1999-06-01

The phase transition of hydrated brain sphingomyelin occurs at around 35 degrees C, which is close to the physiological temperature. Freeze-fracture electron microscopy is used to characterize different gel state morphologies in terms of solid-ordered and liquid-ordered phase states, according to the occurrence of ripples and other higher-dimensional bilayer deformations. Evidently, the natural mixed-chain sphingomyelin does not assume the flat L beta, phase but instead the rippled P beta, phase, with symmetric and asymmetric ripples as well as macroripples and an egg-carton pattern, depending on the incubation conditions. An unexpected difference was observed between samples that are hydrated above and below the phase transition temperature. When the lipid is hydrated at low temperature, a sponge-like network of bilayers is formed in the gel state, next to some normal lamellae. The network loses its ripples during cold-incubation, which indicates the formation of a liquid-ordered (lo) gel phase. Ripples re-appear upon warming and the sponge-like network disintegrates spontaneously and irreversibly into small vesicles above the phase transition.

An integrated scheme for the simultaneous determination of biogenic amines, precursor amino acids, and related metabolites by liquid chromatography with electrochemical detection.

PubMed

Oka, K; Kojima, K; Togari, A; Nagatsu, T; Kiss, B

1984-06-08

A new method using high-performance liquid chromatography with electrochemical detection (HPLC-ED) for the simultaneous determination of monoamines, their precursor amino acids, and related major metabolites in small samples of brain tissue weighing from 0.5 to 50 mg is described. The method is based on the preliminary isolation of monoamines (dopamine, norepinephrine, epinephrine, and serotonin), their precursor amino acids (tyrosine, 3,4-dihydroxyphenylalanine, tryptophan and 5-hydroxytryptophan), and their major metabolites (3-methoxytyramine, normetanephrine, 3,4-dihydroxyphenylacetic acid, homovanillic acid, vanillylmandelic acid, 3-methoxy-4-hydroxyphenylethyleneglycol, and 5-hydroxyindoleacetic acid) by chromatography on small columns of Amberlite CG-50 and Dowex 50W, and by ethyl acetate extraction. All the compounds in the four isolated fractions were measured by HPLC-ED on a reversed-phase column under four different conditions. The sensitivity was from 0.1 to 40 pmol, depending on the substances analysed. This newly established method was applied to the study of the effects of an aromatic L-amino acid decarboxylase inhibitor (NSD-1015) and a monoamine oxidase inhibitor (pargyline) on the levels of monoamines, their precursor amino acids and their major metabolites in brain regions of mice.

Neutron diffraction study of aqueous Laponite suspensions at the NIMROD diffractometer.

PubMed

Tudisca, V; Bruni, F; Scoppola, E; Angelini, R; Ruzicka, B; Zulian, L; Soper, A K; Ricci, M A

2014-09-01

The process of dynamical arrest, leading to formation of different arrested states such as glasses and gels, along with the closely related process of aging, is central for both basic research and technology. Here we report on a study of the time-dependent structural evolution of two aqueous Laponite clay suspensions at different weight concentrations. Neutron diffraction experiments have been performed with the near and intermediate range order diffractometer (NIMROD) that allows studies of the structure of liquids and disordered materials over a continuous length scale ranging from 1 to 300 Å, i.e., from the atomistic to the mesoscopic scales. NIMROD is presently a unique diffractometer, bridging the length scales traditionally investigated by small angle neutron scattering or small angle x-ray scattering with that accessible by traditional diffractometers for liquids. Interestingly, we have unveiled a signature of aging of both suspensions in the length scale region of NIMROD. This phenomenon, ascribed to sporadic contacts between Laponite platelets at long times, has been observed with the sample arrested as gel or as repulsive glass. Moreover, water molecules within the layers closest to Laponite platelets surface show orientational and translational order, which maps into the crystalline structure of Laponite.

Assessment of external heat transfer coefficient during oocyte vitrification in liquid and slush nitrogen using numerical simulations to determine cooling rates.

PubMed

Santos, M V; Sansinena, M; Zaritzky, N; Chirife, J

2012-01-01

In oocyte vitrification, plunging directly into liquid nitrogen favor film boiling and strong nitrogen vaporization. A survey of literature values of heat transfer coefficients (h) for film boiling of small metal objects with different geometries plunged in liquid nitrogen revealed values between 125 to 1000 W per per square m per K. These h values were used in a numerical simulation of cooling rates of two oocyte vitrification devices (open-pulled straw and Cryotop), plunged in liquid and slush nitrogen conditions. Heat conduction equation with convective boundary condition was considered a linear mathematical problem and was solved using the finite element method applying the variational formulation. COMSOL Multiphysics was used to simulate the cooling process of the systems. Predicted cooling rates for OPS and Cryotop when cooled at -196 degree C (liquid nitrogen) or -207 degree C (average for slush nitrogen) for heat transfer coefficients estimated to be representative of film boiling, indicated lowering the cooling temperature produces only a maximum 10 percent increase in cooling rates; confirming the main benefit of plunging in slush over liquid nitrogen does not arise from their temperature difference. Numerical simulations also demonstrated that a hypothetical four-fold increase in the cooling rate of vitrification devices when plunging in slush nitrogen would be explained by an increase in heat transfer coefficient. This improvement in heat transfer (i.e., high cooling rates) in slush nitrogen is attributed to less or null film boiling when a sample is placed in slush (mixture of liquid and solid nitrogen) because it first melts the solid nitrogen before causing the liquid to boil and form a film.

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

Lorenz, Matthias; Ovchinnikova, Olga S; Van Berkel, Gary J

RATIONALE: Laser ablation provides for the possibility of sampling a large variety of surfaces with high spatial resolution. This type of sampling when employed in conjunction with liquid capture followed by nanoelectrospray ionization provides the opportunity for sensitive and prolonged interrogation of samples by mass spectrometry as well as the ability to analyze surfaces not amenable to direct liquid extraction. METHODS: A fully automated, reflection geometry, laser ablation liquid capture spot sampling system was achieved by incorporating appropriate laser fiber optics and a focusing lens into a commercially available, liquid extraction surface analysis (LESA ) ready Advion TriVersa NanoMate system.more » RESULTS: Under optimized conditions about 10% of laser ablated material could be captured in a droplet positioned vertically over the ablation region using the NanoMate robot controlled pipette. The sampling spot size area with this laser ablation liquid capture surface analysis (LA/LCSA) mode of operation (typically about 120 m x 160 m) was approximately 50 times smaller than that achievable by direct liquid extraction using LESA (ca. 1 mm diameter liquid extraction spot). The set-up was successfully applied for the analysis of ink on glass and paper as well as the endogenous components in Alstroemeria Yellow King flower petals. In a second mode of operation with a comparable sampling spot size, termed laser ablation/LESA , the laser system was used to drill through, penetrate, or otherwise expose material beneath a solvent resistant surface. Once drilled, LESA was effective in sampling soluble material exposed at that location on the surface. CONCLUSIONS: Incorporating the capability for different laser ablation liquid capture spot sampling modes of operation into a LESA ready Advion TriVersa NanoMate enhanced the spot sampling spatial resolution of this device and broadened the surface types amenable to analysis to include absorbent and solvent resistant materials.« less

Investigation of the Matrix Effect on the Accuracy of Quantitative Analysis of Trace Metals in Liquids Using Laser-Induced Breakdown Spectroscopy with Solid Substrates.

PubMed

Xiu, Junshan; Dong, Lili; Qin, Hua; Liu, Yunyan; Yu, Jin

2016-12-01

The detection limit of trace metals in liquids has been improved greatly by laser-induced breakdown spectroscopy (LIBS) using solid substrate. A paper substrate and a metallic substrate were used as a solid substrate for the detection of trace metals in aqueous solutions and viscous liquids (lubricating oils) respectively. The matrix effect on quantitative analysis of trace metals in two types of liquids was investigated. For trace metals in aqueous solutions using paper substrate, the calibration curves established for pure solutions and mixed solutions samples presented large variation on both the slope and the intercept for the Cu, Cd, and Cr. The matrix effects among the different elements in mixed solutions were observed. However, good agreement was obtained between the measured and known values in real wastewater. For trace metals in lubricating oils, the matrix effect between the different oils is relatively small and reasonably negligible under the conditions of our experiment. A universal calibration curve can be established for trace metals in different types of oils. The two approaches are verified that it is possible to develop a feasible and sensitive method with accuracy results for rapid detection of trace metals in industrial wastewater and viscous liquids by laser-induced breakdown spectroscopy. © The Author(s) 2016.

Determination of chlorophenols in honey samples using in-situ ionic liquid-dispersive liquid-liquid microextraction as a pretreatment method followed by high-performance liquid chromatography.

PubMed

Fan, Chen; Li, Nai; Cao, Xueli

2015-05-01

In-situ ionic liquid-dispersive liquid-liquid microextraction (IL-DLLME) method was developed as a pretreatment method for the detection of six chlorophenols (CPs) in honey samples. The hydrophobic ionic liquid [C4MIM][NTf2], formed in-situ by the hydrophilic ionic liquid [C4MIM][BF4] and the ion exchange reagent LiNTf2 was used as the microextractant solvent of CPs from honey sample. Then the enriched analytes were back-extracted into 40 μL of 0.14 M NaOH solution and finally subjected to analysis by high-performance liquid chromatography. The method showed low limit of detection of CPs, 0.8-3.2 μg/L and high enrichment factor, 34-65 with the recoveries range from 91.60% to 114.33%. The method is simple, rapid, environmentally friendly and with high extraction efficiency. Copyright © 2014 The Authors. Published by Elsevier Ltd.. All rights reserved.

Ionic imbalance induced self-propulsion of liquid metals

PubMed Central

Zavabeti, Ali; Daeneke, Torben; Chrimes, Adam F.; O'Mullane, Anthony P.; Zhen Ou, Jian; Mitchell, Arnan; Khoshmanesh, Khashayar; Kalantar-zadeh, Kourosh

2016-01-01

Components with self-propelling abilities are important building blocks of small autonomous systems and the characteristics of liquid metals are capable of fulfilling self-propulsion criteria. To date, there has been no exploration regarding the effect of electrolyte ionic content surrounding a liquid metal for symmetry breaking that generates motion. Here we show the controlled actuation of liquid metal droplets using only the ionic properties of the aqueous electrolyte. We demonstrate that pH or ionic concentration gradients across a liquid metal droplet induce both deformation and surface Marangoni flow. We show that the Lippmann dominated deformation results in maximum velocity for the self-propulsion of liquid metal droplets and illustrate several key applications, which take advantage of such electrolyte-induced motion. With this finding, it is possible to conceive the propulsion of small entities that are constructed and controlled entirely with fluids, progressing towards more advanced soft systems. PMID:27488954

Liquid metal enabled pump

PubMed Central

Tang, Shi-Yang; Khoshmanesh, Khashayar; Sivan, Vijay; Petersen, Phred; O’Mullane, Anthony P.; Abbott, Derek; Mitchell, Arnan; Kalantar-zadeh, Kourosh

2014-01-01

Small-scale pumps will be the heartbeat of many future micro/nanoscale platforms. However, the integration of small-scale pumps is presently hampered by limited flow rate with respect to the input power, and their rather complicated fabrication processes. These issues arise as many conventional pumping effects require intricate moving elements. Here, we demonstrate a system that we call the liquid metal enabled pump, for driving a range of liquids without mechanical moving parts, upon the application of modest electric field. This pump incorporates a droplet of liquid metal, which induces liquid flow at high flow rates, yet with exceptionally low power consumption by electrowetting/deelectrowetting at the metal surface. We present theory explaining this pumping mechanism and show that the operation is fundamentally different from other existing pumps. The presented liquid metal enabled pump is both efficient and simple, and thus has the potential to fundamentally advance the field of microfluidics. PMID:24550485

Ionic imbalance induced self-propulsion of liquid metals.

PubMed

Zavabeti, Ali; Daeneke, Torben; Chrimes, Adam F; O'Mullane, Anthony P; Zhen Ou, Jian; Mitchell, Arnan; Khoshmanesh, Khashayar; Kalantar-Zadeh, Kourosh

2016-08-04

Components with self-propelling abilities are important building blocks of small autonomous systems and the characteristics of liquid metals are capable of fulfilling self-propulsion criteria. To date, there has been no exploration regarding the effect of electrolyte ionic content surrounding a liquid metal for symmetry breaking that generates motion. Here we show the controlled actuation of liquid metal droplets using only the ionic properties of the aqueous electrolyte. We demonstrate that pH or ionic concentration gradients across a liquid metal droplet induce both deformation and surface Marangoni flow. We show that the Lippmann dominated deformation results in maximum velocity for the self-propulsion of liquid metal droplets and illustrate several key applications, which take advantage of such electrolyte-induced motion. With this finding, it is possible to conceive the propulsion of small entities that are constructed and controlled entirely with fluids, progressing towards more advanced soft systems.

Ionic imbalance induced self-propulsion of liquid metals

NASA Astrophysics Data System (ADS)

Zavabeti, Ali; Daeneke, Torben; Chrimes, Adam F.; O'Mullane, Anthony P.; Zhen Ou, Jian; Mitchell, Arnan; Khoshmanesh, Khashayar; Kalantar-Zadeh, Kourosh

2016-08-01

Components with self-propelling abilities are important building blocks of small autonomous systems and the characteristics of liquid metals are capable of fulfilling self-propulsion criteria. To date, there has been no exploration regarding the effect of electrolyte ionic content surrounding a liquid metal for symmetry breaking that generates motion. Here we show the controlled actuation of liquid metal droplets using only the ionic properties of the aqueous electrolyte. We demonstrate that pH or ionic concentration gradients across a liquid metal droplet induce both deformation and surface Marangoni flow. We show that the Lippmann dominated deformation results in maximum velocity for the self-propulsion of liquid metal droplets and illustrate several key applications, which take advantage of such electrolyte-induced motion. With this finding, it is possible to conceive the propulsion of small entities that are constructed and controlled entirely with fluids, progressing towards more advanced soft systems.

A variable conductance gas switch for intermediate temperature operation of liquid He/liquid N2 cryostats

NASA Technical Reports Server (NTRS)

Rayner, J. T.; Chuter, T. C.; Mclean, I. S.; Radostitz, J. V.; Nolt, I. G.

1988-01-01

A technique for establishing a stable intermediate temperature stage in liquid He/liquid N2 double vessel cryostats is described. The tertiary cold stage, which can be tuned to any temperature between 10 and 60 K, is ideal for cooling IR sensors for use in astronomy and physics applications. The device is called a variable-conductance gas switch. It is essentially a small chamber, located between the cold stage and liquid helium cold-face, whose thermal conductance may be controlled by varying the pressure of helium gas within the chamber. A key feature of this device is the large range of temperature control achieved with a very small (less than 10 mW) heat input from the cryogenic temperature control switch.

Mixed cryogen cooling systems for HTS power applications: A status report of progress in Korea University

NASA Astrophysics Data System (ADS)

Song, Jung-Bin; Lee, Haigun

2012-12-01

A cooling system employing a solid cryogen (SC), such as solid nitrogen (SN2), was recently reported for high-temperature superconducting (HTS) applications. However, thermal contact between the SC and the HTS can be degraded by repeated overcurrent runs, resulting in 'thermal dry-out'. Novel cryogens, SC with small amounts of liquid cryogen, have been suggested to overcome this problem. Such cooling systems rely on the small amount of liquid cryogen to facilitate heat exchange so as to fully exploit the heat capacity of the solid cryogen. This paper presents a description and summary of recent activities at Korea University related to cooling systems employing mixed cryogens of solid-liquid nitrogen, solid argon-liquid nitrogen, and solid nitrogen-liquid neon.

Sensitive assay for measurement of volatile borneol, isoborneol, and the metabolite camphor in rat pharmacokinetic study of Borneolum (Bingpian) and Borneolum syntheticum (synthetic Bingpian)

PubMed Central

Cheng, Chen; Liu, Xin-wei; Du, Fei-fei; Li, Mei-juan; Xu, Fang; Wang, Feng-qing; Liu, Yang; Li, Chuan; Sun, Yan

2013-01-01

Aim: Both Borneolum (Chinese name Bingpian; dextrorotatory borneol) and Borneolum syntheticum (synthetic Bingpian; a mixture of optically inactive borneol and isoborneol) have been used for medicinal purposes in Chinese traditional medicine. The aim of this study was to develop a sensitive assay for measuring volatile ingredients borneol, isoborneol, and their metabolite camphor in pharmacokinetic study of Bingpian. Methods: Rat plasma samples were prepared using liquid-liquid microextraction: 70 μL of plasma sample (containing 125 nmol/L naphthalene as the internal standard) was extracted with 35 μL of n-hexane. The resulting n-hexane extract (20 μL) was introduced into a gas chromatography/mass spectrometry system using programmable temperature vaporizing-based large-volume injection. The assay was validated to demonstrate its reliability for the intended use. Using this assay, pharmacokinetic studies of Bingpian, synthetic Bingpian, and Fufang-Danshen tablets (containing synthetic Bingpian) were conducted in rats. Results: The extraction efficiency for the analytes and the internal standard from plasma was almost constant with decrease in n-hexane-to-plasma volume ratio, thus enabling a small volume of extracting solvent to be used for sample preparation, and enhancing the assay sensitivity. The lower quantification limit for measuring borneol, isoborneol, and camphor in plasma was 0.98 nmol/L, which was 33–330 times more sensitive than those reported earlier for Bingpian and synthetic Bingpian. The applicability of the miniaturized liquid-liquid extraction technique could be extended to measure other volatile and nonvolatile medicinal compounds in biomatrices, which can be predicted according to the analytes' octanol/water distribution coefficient (logD) and acid dissociation constant (pKa). Conclusion: This assay is sensitive, accurate and free of matrix effects, and can be applied to pharmacokinetic studies of Bingpian, synthetic Bingpian, and Bingpian-containing herbal products. PMID:23974515

Solvent sensitivity of smart 3D-printed nanocomposite liquid sensor

NASA Astrophysics Data System (ADS)

Aliheidari, Nahal; Ameli, Amir; Pötschke, Petra

2018-03-01

Fused deposition modeling (FDM) is one of the 3D printing methods that has attracted significant attention. In this method, small and complex samples with nearly no limitation in geometry can be fabricated layer by layer to form end-use parts. This work investigates the liquid sensing behavior of FDM printed flexible thermoplastic polyurethane, TPU filled with multiwalled carbon nanotubes, MWCNTs. The sensing capability of printed TPU-MWCNT was studied as a function of MWCNT content and infill density in response to different solvents, i.e., ethanol, acetone and toluene. The solvents were selected based on their widespread use and importance in medical and industrial applications. U-shaped liquid sensors with 2, 3 and 4wt.% MWCNT content were printed at three different infill densities of 50, 75 and 100%. Solvent sensitivity was then characterized by immersing the sensors in the solvents and measuring the resistance evolution over 25s. The results indicated a sensitivity order of acetone > toluene > ethanol, which was in agreement with the predictions of FloryHiggins solubility equation. For all the solvents, the sensitivity was enhanced as the infill density of the printed samples was decreased. This was attributed to the increased surface area to volume ratio and shortened diffusion paths. The MWCNT content was also observed to have a profound effect on the sensitivity; in samples with partial infill, the sensitivity was found to be inversely proportional to the MWCNT content, such that the highest resistance change was obtained for nanocomposites with the lowest MWCNT content of 2wt.%. For instance, a resistance increase of more than 10 times was obtained in 25 s once TPU-2wt.%MWCNT with 50% infill was tested against acetone. The results of this work reveals that highly sensitive liquid sensors can be fabricated with the aid of 3D printing without the need for complex processing methods.

Chromatographic behavior of small organic compounds in low-temperature high-performance liquid chromatography using liquid carbon dioxide as the mobile phase.

PubMed

Motono, Tomohiro; Nagai, Takashi; Kitagawa, Shinya; Ohtani, Hajime

2015-07-01

Low-temperature high-performance liquid chromatography, in which a loop injector, column, and detection cell were refrigerated at -35ºC, using liquid carbon dioxide as the mobile phase was developed. Small organic compounds (polyaromatic hydrocarbons, alkylbenzenes, and quinones) were separated by low-temperature high-performance liquid chromatography at temperatures from -35 to -5ºC. The combination of liquid carbon dioxide mobile phase with an octadecyl-silica (C18 ) column provided reversed phase mode separation, and a bare silica-gel column resulted in normal phase mode separation. In both the cases, nonlinear behavior at approximately -15ºC was found in the relationship between the temperature and the retention factors of the analytes (van't Hoff plots). In contrast to general trends in high-performance liquid chromatography, the decrease in temperature enhanced the separation efficiency of both the columns. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Measuring the Densities of Aqueous Glasses at Cryogenic Temperatures.

PubMed

Shen, Chen; Julius, Ethan F; Tyree, Timothy J; Dan, Ritwik; Moreau, David W; Thorne, Robert

2017-06-28

We demonstrate a method for determining the vitreous phase cryogenic temperature densities of aqueous mixtures, and other samples that require rapid cooling, to prepare the desired cryogenic temperature phase. Microliter to picoliter size drops are cooled by projection into a liquid nitrogen-argon (N2-Ar) mixture. The cryogenic temperature phase of the drop is evaluated using a visual assay that correlates with X-ray diffraction measurements. The density of the liquid N2-Ar mixture is adjusted by adding N2 or Ar until the drop becomes neutrally buoyant. The density of this mixture and thus of the drop is determined using a test mass and Archimedes principle. With appropriate care in drop preparation, management of gas above the liquid cryogen mixture to minimize icing, and regular mixing of the cryogenic mixture to prevent density stratification and phase separation, densities accurate to <0.5% of drops as small as 50 pL can readily be determined. Measurements on aqueous cryoprotectant mixtures provide insight into cryoprotectant action, and provide quantitative data to facilitate thermal contraction matching in biological cryopreservation.

Experiments on Lunar Core Composition: Phase Equilibrium Analysis of A Multi-Element (Fe-Ni-S-C) System

NASA Technical Reports Server (NTRS)

Go, B. M.; Righter, K.; Danielson, L.; Pando, K.

2015-01-01

Previous geochemical and geophysical experiments have proposed the presence of a small, metallic lunar core, but its composition is still being investigated. Knowledge of core composition can have a significant effect on understanding the thermal history of the Moon, the conditions surrounding the liquid-solid or liquid-liquid field, and siderophile element partitioning between mantle and core. However, experiments on complex bulk core compositions are very limited. One limitation comes from numerous studies that have only considered two or three element systems such as Fe-S or Fe-C, which do not supply a comprehensive understanding for complex systems such as Fe-Ni-S-Si-C. Recent geophysical data suggests the presence of up to 6% lighter elements. Reassessments of Apollo seismological analyses and samples have also shown the need to acquire more data for a broader range of pressures, temperatures, and compositions. This study considers a complex multi-element system (Fe-Ni-S-C) for a relevant pressure and temperature range to the Moon's core conditions.

Development of a fast and simple test system for the semiquantitative protein detection in cerebrospinal liquids based on gold nanoparticles.

PubMed

Göbel, Gero; Lange, Robert; Hollidt, Jörg-Michael; Lisdat, Fred

2016-01-01

The fast and simple detection of increased protein concentrations in cerebrospinal liquids is preferable in the emergency medicine and it can help to avoid unnecessary laboratory work by an early classification of neurological diseases. Here a test system is developed which is based on the electrostatic interaction between negatively charged gold nanoparticles and proteins at pH values around 5. The test system can be adjusted in such a way that protein/nanoparticles aggregates are formed leading to a red-shift in the absorption spectrum of the nanoparticles suspension. At concentrations above 500 mg/l the color of the suspension changes from red via violet toward blue in a rather small concentration range from 500 to 1000 mg/l. Furthermore the influence of various parameters such as gold nanoparticle concentration, pH value and varying ion concentration in the sample on the test system is examined. Finally cerebrospinal liquids of a larger number of patients have been analyzed. Copyright © 2015 Elsevier B.V. All rights reserved.

Liquid-Liquid Extraction of Insecticides from Juice: An Analytical Chemistry Laboratory Experiment

ERIC Educational Resources Information Center

Radford, Samantha A.; Hunter, Ronald E., Jr.; Barr, Dana Boyd; Ryan, P. Barry

2013-01-01

A laboratory experiment was developed to target analytical chemistry students and to teach them about insecticides in food, sample extraction, and cleanup. Micro concentrations (sub-microgram/mL levels) of 12 insecticides spiked into apple juice samples are extracted using liquid-liquid extraction and cleaned up using either a primary-secondary…

Apparatus and method for quantitative measurement of small differences in optical absorptivity between two samples using differential interferometry and the thermooptic effect

DOEpatents

Cremers, D.A.; Keller, R.A.

1984-05-08

An apparatus and method for the measurement of small differences in optical absorptivity of weakly absorbing solutions using differential interferometry and the thermooptic effect have been developed. Two sample cells are placed in each arm of an interferometer and are traversed by colinear probe and heating laser beams. The interrogation probe beams are recombined forming a fringe pattern, the intensity of which can be related to changes in optical path length of these laser beams through the cells. This in turn can be related to small differences in optical absorptivity which results in different amounts of sample heating when the heating laser beams are turned on, by the fact that the index of refraction of a liquid is temperature dependent. A critical feature of this invention is the stabilization of the optical path of the probe beams against drift. Background (solvent) absorption can then be suppressed by a factor of approximately 400. Solute absorptivities of about 10[sup [minus]5] cm[sup [minus]1] can then be determined in the presence of background absorptions in excess of 10[sup [minus]3] cm[sup [minus]1]. In addition, the smallest absorption measured with the instant apparatus and method is about 5 [times] 10[sup [minus]6] cm[sup [minus]1]. 6 figs.

Chirality sensing with stereodynamic biphenolate zinc complexes.

PubMed

Bentley, Keith W; de Los Santos, Zeus A; Weiss, Mary J; Wolf, Christian

2015-10-01

Two bidentate ligands consisting of a fluxional polyarylacetylene framework with terminal phenol groups were synthesized. Reaction with diethylzinc gives stereodynamic complexes that undergo distinct asymmetric transformation of the first kind upon binding of chiral amines and amino alcohols. The substrate-to-ligand chirality imprinting at the zinc coordination sphere results in characteristic circular dichroism signals that can be used for direct enantiomeric excess (ee) analysis. This chemosensing approach bears potential for high-throughput ee screening with small sample amounts and reduced solvent waste compared to traditional high-performance liquid chromatography methods. © 2015 Wiley Periodicals, Inc.

Chemical Sensing Using Fiber Cavity Ring-Down Spectroscopy

PubMed Central

Waechter, Helen; Litman, Jessica; Cheung, Adrienne H.; Barnes, Jack A.; Loock, Hans-Peter

2010-01-01

Waveguide-based cavity ring-down spectroscopy (CRD) can be used for quantitative measurements of chemical concentrations in small amounts of liquid, in gases or in films. The change in ring-down time can be correlated to analyte concentration when using fiber optic sensing elements that change their attenuation in dependence of either sample absorption or refractive index. Two types of fiber cavities, i.e., fiber loops and fiber strands containing reflective elements, are distinguished. Both types of cavities were coupled to a variety of chemical sensor elements, which are discussed and compared. PMID:22294895

Rapid analysis of ultraviolet filters using dispersive liquid-liquid microextraction coupled to headspace gas chromatography and mass spectrometry.

PubMed

Pierson, Stephen A; Trujillo-Rodríguez, María J; Anderson, Jared L

2018-05-29

An ionic-liquid-based in situ dispersive liquid-liquid microextraction method coupled to headspace gas chromatography and mass spectrometry was developed for the rapid analysis of ultraviolet filters. The chemical structures of five ionic liquids were specifically designed to incorporate various functional groups for the favorable extraction of the target analytes. Extraction parameters including ionic liquid mass, molar ratio of ionic liquid to metathesis reagent, vortex time, ionic strength, pH, and total sample volume were studied and optimized. The effect of the headspace temperature and volume during the headspace sampling step was also evaluated to increase the sensitivity of the method. The optimized procedure is fast as it only required ∼7-10 min per extraction and allowed for multiple extractions to be performed simultaneously. In addition, the method exhibited high precision, good linearity, and low limits of detection for six ultraviolet filters in aqueous samples. The developed method was applied to both pool and lake water samples attaining acceptable relative recovery values. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evaluation of two-dimensional electrophoresis and liquid chromatography – tandem mass spectrometry for tissue-specific protein profiling of laser-microdissected plant samples

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

Schad, Martina; Lipton, Mary S.; Giavalisco, Patrick

2005-07-14

Laser microdissection (LM) allows the collection of homogeneous tissue- and cell specific plant samples. The employment of this technique with subsequent protein analysis has thus far not been reported for plant tissues, probably due to the difficulties associated with defining a reasonable cellular morphology and, in parallel, allowing efficient protein extraction from tissue samples. The relatively large sample amount needed for successful proteome analysis is an additional issue that complicates protein profiling on a tissue- or even cell-specific level. In contrast to transcript profiling that can be performed from very small sample amounts due to efficient amplification strategies, there ismore » as yet no amplification procedure for proteins available. In the current study, we compared different tissue preparation techniques prior to LM/laser pressure catapulting (LMPC) with respect to their suitability for protein retrieval. Cryosectioning was identified as the best compromise between tissue morphology and effective protein extraction. After collection of vascular bundles from Arabidopsis thaliana stem tissue by LMPC, proteins were extracted and subjected to protein analysis, either by classical two-dimensional gel electrophoresis (2-DE), or by high-efficiency liquid chromatography (LC) in conjunction with tandem mass spectrometry (MS/MS). Our results demonstrate that both methods can be used with LMPC collected plant material. But because of the significantly lower sample amount required for LC-MS/MS than for 2-DE, the combination of LMPC and LC-MS/MS has a higher potential to promote comprehensive proteome analysis of specific plant tissues.« less

Simultaneous determination of the quantity and isotopic signature of dissolved organic matter from soil water using high-performance liquid chromatography/isotope ratio mass spectrometry.

PubMed

Scheibe, Andrea; Krantz, Lars; Gleixner, Gerd

2012-01-30

We assessed the accuracy and utility of a modified high-performance liquid chromatography/isotope ratio mass spectrometry (HPLC/IRMS) system for measuring the amount and stable carbon isotope signature of dissolved organic matter (DOM) <1 µm. Using a range of standard compounds as well as soil solutions sampled in the field, we compared the results of the HPLC/IRMS analysis with those from other methods for determining carbon and (13)C content. The conversion efficiency of the in-line wet oxidation of the HPLC/IRMS averaged 99.3% for a range of standard compounds. The agreement between HPLC/IRMS and other methods in the amount and isotopic signature of both standard compounds and soil water samples was excellent. For DOM concentrations below 10 mg C L(-1) (250 ng C total) pre-concentration or large volume injections are recommended in order to prevent background interferences. We were able to detect large differences in the (13)C signatures of soil solution DOM sampled in 10 cm depth of plots with either C3 or C4 vegetation and in two different parent materials. These measurements also demonstrated changes in the (13)C signature that demonstrate rapid loss of plant-derived C with depth. Overall the modified HLPC/IRMS system has the advantages of rapid sample preparation, small required sample volume and high sample throughput, while showing comparable performance with other methods for measuring the amount and isotopic signature of DOM. Copyright © 2011 John Wiley & Sons, Ltd.

Optimizing "self-wicking" nanowire grids.

PubMed

Wei, Hui; Dandey, Venkata P; Zhang, Zhening; Raczkowski, Ashleigh; Rice, Willam J; Carragher, Bridget; Potter, Clinton S

2018-05-01

We have developed a self-blotting TEM grid for use with a novel instrument for vitrifying samples for cryo-electron microscopy (cryoEM). Nanowires are grown on the copper surface of the grid using a simple chemical reaction and the opposite smooth side is used to adhere to a holey sample substrate support, for example carbon or gold. When small volumes of sample are applied to the nanowire grids the wires effectively act as blotting paper to rapidly wick away the liquid, leaving behind a thin film. In this technical note, we present a detailed description of how we make these grids using a variety of substrates fenestrated with either lacey or regularly spaced holes. We explain how we characterize the quality of the grids and we describe their behavior under a variety of conditions. Copyright © 2018 Elsevier Inc. All rights reserved.

Displacement-dispersive liquid-liquid microextraction based on solidification of floating organic drop of trace amounts of palladium in water and road dust samples prior to graphite furnace atomic absorption spectrometry determination.

PubMed

Ghanbarian, Maryam; Afzali, Daryoush; Mostafavi, Ali; Fathirad, Fariba

2013-01-01

A new displacement-dispersive liquid-liquid microextraction method based on the solidification of floating organic drop was developed for separation and preconcentration of Pd(ll) in road dust and aqueous samples. This method involves two steps of dispersive liquid-liquid microextraction based on solidification. In Step 1, Cu ions react with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which is extracted by dispersive liquid-liquid microextraction based on a solidification procedure using 1-undecanol (extraction solvent) and ethanol (dispersive solvent). In Step 2, the extracted complex is first dispersed using ethanol in a sample solution containing Pd ions, then a dispersive liquid-liquid microextraction based on a solidification procedure is performed creating an organic drop. In this step, Pd(ll) replaces Cu(ll) from the pre-extracted Cu-DDTC complex and goes into the extraction solvent phase. Finally, the Pd(ll)-containing drop is introduced into a graphite furnace using a microsyringe, and Pd(ll) is determined using atomic absorption spectrometry. Several factors that influence the extraction efficiency of Pd and its subsequent determination, such as extraction and dispersive solvent type and volume, pH of sample solution, centrifugation time, and concentration of DDTC, are optimized.

System and method for assaying radiation

DOEpatents

DiPrete, David P; Whiteside, Tad; Pak, Donald J; DiPrete, Cecilia C

2013-11-12

A system for assaying radiation includes a sample holder configured to hold a liquid scintillation solution. A photomultiplier receives light from the liquid scintillation solution and generates a signal reflective of the light. A control circuit biases the photomultiplier and receives the signal from the photomultiplier reflective of the light. A light impermeable casing surrounds the sample holder, photomultiplier, and control circuit. A method for assaying radiation includes placing a sample in a liquid scintillation solution, placing the liquid scintillation solution in a sample holder, and placing the sample holder inside a light impermeable casing. The method further includes positioning a photomultiplier inside the light impermeable casing and supplying power to a control circuit inside the light impermeable casing.

Apparatus and method for spraying liquid materials

DOEpatents

Alvarez, J.L.; Watson, L.D.

1988-01-21

A method for spraying liquids involving a flow of gas which shears the liquid. A flow of gas is introduced in a converging-diverging nozzle where it meets and shears the liquid into small particles which are of a size and uniformity which can be controlled through adjustment of pressures and gas velocity. 5 figs.

Apparatus and method for spraying liquid materials

DOEpatents

Alvarez, Joseph L.; Watson, Lloyd D.

1990-01-01

A method for spraying liquids involving a flow of gas which shears the liquid. A flow of gas is introduced in a converging-diverging nozzle where it meets and shears the liquid into small particles which are of a size and uniformity which can be controlled through adjustment of pressures and gas velocity.

Fuel Injector With Shear Atomizer

NASA Technical Reports Server (NTRS)

Beal, George W.; Mills, Virgil L.; Smith, Durward B., II; Beacom, William F.

1995-01-01

Atomizer for injecting liquid fuel into combustion chamber uses impact and swirl to break incoming stream of fuel into small, more combustible droplets. Slanted holes direct flow of liquid fuel to stepped cylindrical wall. Impact on wall atomizes liquid. Air flowing past vanes entrains droplets of liquid in swirling flow. Fuel injected at pressure lower than customarily needed.

Experimental tobacco marketplace: substitutability of e-cigarette liquid for cigarettes as a function of nicotine strength.

PubMed

Pope, Derek A; Poe, Lindsey; Stein, Jeffrey S; Kaplan, Brent A; Heckman, Bryan W; Epstein, Leonard H; Bickel, Warren K

2018-04-18

The experimental tobacco marketplace (ETM) provides a method to estimate, prior to implementation, the effects of new products or policies on purchasing across various products in a complex tobacco marketplace. We used the ETM to examine the relationship between nicotine strength and substitutability of alternative products for cigarettes to contribute to the literature on regulation of e-liquid nicotine strength. The present study contained four sampling and four ETM purchasing sessions. During sampling sessions, participants were provided 1 of 4 e-liquid strengths (randomised) to sample for 2 days followed by an ETM purchasing session. The nicotine strength sampled in the 2 days prior to an ETM session was the same strength available for purchase in the next ETM. Each participant sampled and could purchase 0 mg/mL, 6 mg/mL, 12 mg/mL and 24 mg/mL e-liquid, among other products, during the study. Cigarette demand was unaltered across e-liquid strength. E-liquid was the only product to substitute for cigarettes across more than one e-liquid strength. Substitutability increased as a function of e-liquid strength, with the 24 mg/mL displaying the greatest substitutability of all products. The present study found that e-liquid substitutability increased with nicotine strength, at least up to 24 mg/mL e-liquid. However, the effects of e-liquid nicotine strength on cigarette purchasing were marginal and total nicotine purchased increased as e-liquid nicotine strength increased. © Article author(s) (or their employer(s) unless otherwise stated in the text of the article) 2018. All rights reserved. No commercial use is permitted unless otherwise expressly granted.

Determination of ten pyrethroids in various fruit juices: comparison of dispersive liquid-liquid microextraction sample preparation and QuEChERS method combined with dispersive liquid-liquid microextraction.

PubMed

Zhang, Yaohai; Zhang, Xuelian; Jiao, Bining

2014-09-15

Dispersive liquid-liquid microextraction (DLLME) sample preparation and the quick, easy, cheap, effective, rugged and safe (QuEChERS) method combined with DLLME were developed and compared for the analysis of ten pyrethroids in various fruit juices using gas chromatography-electron capture detection (GC-ECD). QuEChERS-DLLME method has found its widespread applications to all the fruit juices including those samples with more complex matrices (orange, lemon, kiwi and mango) while DLLME was confined to the fruit juices with simpler matrices (apple, pear, grape and peach). The two methods provided acceptable recoveries and repeatability. In addition, the applicabilities of two methods were demonstrated with the real samples and further confirmed by gas chromatography-mass spectrometry (GC-MS). Copyright © 2014. Published by Elsevier Ltd.

Laboratory-based x-ray phase-contrast tomography enables 3D virtual histology

NASA Astrophysics Data System (ADS)

Töpperwien, Mareike; Krenkel, Martin; Quade, Felix; Salditt, Tim

2016-09-01

Due to the large penetration depth and small wavelength hard x-rays offer a unique potential for 3D biomedical and biological imaging, combining capabilities of high resolution and large sample volume. However, in classical absorption-based computed tomography, soft tissue only shows a weak contrast, limiting the actual resolution. With the advent of phase-contrast methods, the much stronger phase shift induced by the sample can now be exploited. For high resolution, free space propagation behind the sample is particularly well suited to make the phase shift visible. Contrast formation is based on the self-interference of the transmitted beam, resulting in object-induced intensity modulations in the detector plane. As this method requires a sufficiently high degree of spatial coherence, it was since long perceived as a synchrotron-based imaging technique. In this contribution we show that by combination of high brightness liquid-metal jet microfocus sources and suitable sample preparation techniques, as well as optimized geometry, detection and phase retrieval, excellent three-dimensional image quality can be obtained, revealing the anatomy of a cobweb spider in high detail. This opens up new opportunities for 3D virtual histology of small organisms. Importantly, the image quality is finally augmented to a level accessible to automatic 3D segmentation.

DMSO Assisted Electrospray Ionization for the Detection of Small Peptide Hormones in Urine by Dilute-and-Shoot-Liquid-Chromatography-High Resolution Mass Spectrometry

NASA Astrophysics Data System (ADS)

Judák, Péter; Grainger, Janelle; Goebel, Catrin; Van Eenoo, Peter; Deventer, Koen

2017-08-01

The mobile phase additive (DMSO) has been described as a useful tool to enhance electrospray ionization (ESI) of peptides and proteins. So far, this technique has mainly been used in proteomic/peptide research, and its applicability in a routine clinical laboratory setting (i.e., doping control analysis) has not been described yet. This work provides a simple, easy to implement screening method for the detection of doping relevant small peptides (GHRPs, GnRHs, GHS, and vasopressin-analogues) with molecular weight less than 2 kDa applying DMSO in the mobile phase. The gain in sensitivity was sufficient to inject the urine samples after a 2-fold dilution step omitting a time consuming sample preparation. The employed analytical procedure was validated for the qualitative determination of 36 compounds, including 13 metabolites. The detection limits (LODs) ranged between 50 and 1000 pg/mL and were compliant with the 2 ng/mL minimum detection level required by the World Anti-Doping Agency (WADA) for all the target peptides. To demonstrate the feasibility of the work, urine samples obtained from patients who have been treated with desmopressin or leuprolide and urine samples that have been declared as adverse analytical findings were analyzed.

[Role of emotional stress in development of somatic injuries in liquidators of the Chernobyl power plant accident irradiated with small doses].

PubMed

Moroz, B B; Deshevoĭ, Iu B

1999-01-01

In the light of modern beliefs about emotional stress are considered available in the literature given on changing a picture of health beside persons, taken part in liquidations of consequences of damage on Chernobil atomic stations. Results of psychological, psychophysiological and endocrinological examinations point to that beside significant numbers of liquidators of damage was developed chronic emotional stress. Expected presence of feedforward between the emotional stress and development beside liquidators of psychic frustrations, cardiovascular pathology, peptic ulcer of stomach and duodenum. Is discussed problem of combining action on the organism of ionizing radiating in small doses and long emotional stress.

Determination of sudan dyes in red wine and fruit juice using ionic liquid-based liquid-liquid microextraction and high-performance liquid chromatography.

PubMed

Sun, Shuo; Wang, Ying; Yu, Wenzhi; Zhao, Tianqi; Gao, Shiqian; Kang, Mingqin; Zhang, Yupu; Zhang, Hanqi; Yu, Yong

2011-07-01

The liquid-liquid microextraction (LLME) was developed for extracting sudan dyes from red wine and fruit juice. Room temperature ionic liquid was used as the extraction solvent. The target analytes were determined by high-performance liquid chromatography. The extraction parameters were optimized. The optimal conditions are as follows: volume of [C(6)MIM][PF(6)] 50 μL; the extraction time 10 min; pH value of the sample solution 7.0; NaCl concentration in sample solution 5%. The extraction recoveries for the analytes in red wine and fruit samples are 86.79-108.28 and 68.54-85.66%, whereas RSDs are 1.42-5.12 and 1.43-6.19%, respectively. The limits of detection and quantification were 0.428 and 1.426 ng/mL for sudan I, 0.938 and 3.127 ng/mL for sudan II, 1.334 and 4.445 ng/mL for sudan III, 1.454 and 4.846 ng/mL for sudan IV, respectively. Compared with conventional liquid-liquid extraction (CLLE) and ultrasonic extraction (UE), when LLME was applied, the sample amount was less (LLME: 4 mL; CLLE: 10 mL; UE: 10 mL), the extraction time was shorter (LLME: 15 min; CLLE: 110 min; UE: 50 min) and the extraction solvent amount was less (LLME: 0.05 mL IL; CLLE: 15 mL hexane; UE: 20 mL hexane). The proposed method offers a simple, rapid and efficient sample preparation for determining sudan dyes in red wine and fruit juice samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Qualitative Analysis of E-Liquid Emissions as a Function of Flavor Additives Using Two Aerosol Capture Methods.

PubMed

Eddingsaas, Nathan; Pagano, Todd; Cummings, Cody; Rahman, Irfan; Robinson, Risa; Hensel, Edward

2018-02-13

This work investigates emissions sampling methods employed for qualitative identification of compounds in e-liquids and their resultant aerosols to assess what capture methods may be sufficient to identify harmful and potentially harmful constituents present. Three popular e-liquid flavors (cinnamon, mango, vanilla) were analyzed using qualitative gas chromatography-mass spectrometry (GC-MS) in the un-puffed state. Each liquid was also machine-puffed under realistic-use flow rate conditions and emissions were captured using two techniques: filter pads and methanol impingers. GC-MS analysis was conducted on the emissions captured using both techniques from all three e-liquids. The e-liquid GC-MS analysis resulted in positive identification of 13 compounds from the cinnamon flavor e-liquid, 31 from mango, and 19 from vanilla, including a number of compounds observed in all e-liquid experiments. Nineteen compounds were observed in emissions which were not present in the un-puffed e-liquid. Qualitative GC-MS analysis of the emissions samples identify compounds observed in all three samples: e-liquid, impinge, and filter pads, and each subset thereof. A limited number of compounds were observed in emissions captured with impingers, but were not observed in emissions captured using filter pads; a larger number of compounds were observed on emissions collected from the filter pads, but not those captured with impingers. It is demonstrated that sampling methods have different sampling efficiencies and some compounds might be missed using only one method. It is recommended to investigate filter pads, impingers, thermal desorption tubes, and solvent extraction resins to establish robust sampling methods for emissions testing of e-cigarette emissions.

Qualitative Analysis of E-Liquid Emissions as a Function of Flavor Additives Using Two Aerosol Capture Methods

PubMed Central

Eddingsaas, Nathan; Pagano, Todd; Cummings, Cody; Rahman, Irfan; Robinson, Risa

2018-01-01

This work investigates emissions sampling methods employed for qualitative identification of compounds in e-liquids and their resultant aerosols to assess what capture methods may be sufficient to identify harmful and potentially harmful constituents present. Three popular e-liquid flavors (cinnamon, mango, vanilla) were analyzed using qualitative gas chromatography-mass spectrometry (GC-MS) in the un-puffed state. Each liquid was also machine-puffed under realistic-use flow rate conditions and emissions were captured using two techniques: filter pads and methanol impingers. GC-MS analysis was conducted on the emissions captured using both techniques from all three e-liquids. The e-liquid GC-MS analysis resulted in positive identification of 13 compounds from the cinnamon flavor e-liquid, 31 from mango, and 19 from vanilla, including a number of compounds observed in all e-liquid experiments. Nineteen compounds were observed in emissions which were not present in the un-puffed e-liquid. Qualitative GC-MS analysis of the emissions samples identify compounds observed in all three samples: e-liquid, impinge, and filter pads, and each subset thereof. A limited number of compounds were observed in emissions captured with impingers, but were not observed in emissions captured using filter pads; a larger number of compounds were observed on emissions collected from the filter pads, but not those captured with impingers. It is demonstrated that sampling methods have different sampling efficiencies and some compounds might be missed using only one method. It is recommended to investigate filter pads, impingers, thermal desorption tubes, and solvent extraction resins to establish robust sampling methods for emissions testing of e-cigarette emissions. PMID:29438289

Thermal Degradation of Small Molecules: A Global Metabolomic Investigation.

PubMed

Fang, Mingliang; Ivanisevic, Julijana; Benton, H Paul; Johnson, Caroline H; Patti, Gary J; Hoang, Linh T; Uritboonthai, Winnie; Kurczy, Michael E; Siuzdak, Gary

2015-11-03

Thermal processes are widely used in small molecule chemical analysis and metabolomics for derivatization, vaporization, chromatography, and ionization, especially in gas chromatography mass spectrometry (GC/MS). In this study the effect of heating was examined on a set of 64 small molecule standards and, separately, on human plasma metabolite extracts. The samples, either derivatized or underivatized, were heated at three different temperatures (60, 100, and 250 °C) at different exposure times (30 s, 60 s, and 300 s). All the samples were analyzed by liquid chromatography coupled to electrospray ionization mass spectrometry (LC/MS) and the data processed by XCMS Online ( xcmsonline.scripps.edu ). The results showed that heating at an elevated temperature of 100 °C had an appreciable effect on both the underivatized and derivatized molecules, and heating at 250 °C created substantial changes in the profile. For example, over 40% of the molecular peaks were altered in the plasma metabolite analysis after heating (250 °C, 300s) with a significant formation of degradation and transformation products. The analysis of 64 small molecule standards validated the temperature-induced changes observed on the plasma metabolites, where most of the small molecules degraded at elevated temperatures even after minimal exposure times (30 s). For example, tri- and diorganophosphates (e.g., adenosine triphosphate and adenosine diphosphate) were readily degraded into a mono-organophosphate (e.g., adenosine monophosphate) during heating. Nucleosides and nucleotides (e.g., inosine and inosine monophosphate) were also found to be transformed into purine derivatives (e.g., hypoxanthine). A newly formed transformation product, oleoyl ethyl amide, was identified in both the underivatized and derivatized forms of the plasma extracts and small molecule standard mixture, and was likely generated from oleic acid. Overall these analyses show that small molecules and metabolites undergo significant time-sensitive alterations when exposed to elevated temperatures, especially those conditions that mimic sample preparation and analysis in GC/MS experiments.

Cryogenic Liquid Sample Acquisition System for Remote Space Applications

NASA Technical Reports Server (NTRS)

Mahaffy, Paul; Trainer, Melissa; Wegel, Don; Hawk, Douglas; Melek, Tony; Johnson, Christopher; Amato, Michael; Galloway, John

2013-01-01

There is a need to acquire autonomously cryogenic hydrocarbon liquid sample from remote planetary locations such as the lakes of Titan for instruments such as mass spectrometers. There are several problems that had to be solved relative to collecting the right amount of cryogenic liquid sample into a warmer spacecraft, such as not allowing the sample to boil off or fractionate too early; controlling the intermediate and final pressures within carefully designed volumes; designing for various particulates and viscosities; designing to thermal, mass, and power-limited spacecraft interfaces; and reducing risk. Prior art inlets for similar instruments in spaceflight were designed primarily for atmospheric gas sampling and are not useful for this front-end application. These cryogenic liquid sample acquisition system designs for remote space applications allow for remote, autonomous, controlled sample collections of a range of challenging cryogenic sample types. The design can control the size of the sample, prevent fractionation, control pressures at various stages, and allow for various liquid sample levels. It is capable of collecting repeated samples autonomously in difficult lowtemperature conditions often found in planetary missions. It is capable of collecting samples for use by instruments from difficult sample types such as cryogenic hydrocarbon (methane, ethane, and propane) mixtures with solid particulates such as found on Titan. The design with a warm actuated valve is compatible with various spacecraft thermal and structural interfaces. The design uses controlled volumes, heaters, inlet and vent tubes, a cryogenic valve seat, inlet screens, temperature and cryogenic liquid sensors, seals, and vents to accomplish its task.

Experimental research on rock fracture failure characteristics under liquid nitrogen cooling conditions

NASA Astrophysics Data System (ADS)

Gao, Feng; Cai, Chengzheng; Yang, Yugui

2018-06-01

As liquid nitrogen is injected into a wellbore as fracturing fluid, it can rapidly absorb heat from warmer rock and generate cryogenic condition in downhole region. This will alter the physical conditions of reservoir rocks and further affect rock failure characteristics. To investigate rock fracture failure characteristics under liquid nitrogen cooling conditions, the fracture features of four types of sandstones and one type of marble were tested on original samples (the sample without any treatment) and cryogenic samples (the samples just taken out from the liquid nitrogen), respectively. The differences between original samples and cryogenic samples in load-displacement curves, fracture toughness, energy evolution and the crack density of ruptured samples were compared and analyzed. The results showed that at elastic deformation stage, cryogenic samples presented less plastic deformation and more obvious brittle failure characteristics than original ones. The average fracture toughness of cryogenic samples was 10.47%-158.33% greater than that of original ones, indicating that the mechanical strength of rocks used were enhanced under cooling conditions. When the samples ruptured, the cryogenic ones were required to absorb more energy and reserve more elastic energy. In general, the fracture degree of cryogenic samples was higher than that of original ones. As the samples were entirely fractured, the crack density of cryogenic samples was about 536.67% at most larger than that of original ones. This indicated that under liquid nitrogen cooling conditions, the stimulation reservoir volume is expected to be improved during fracturing. This work could provide a reference to the research on the mechanical properties and fracture failure of rock during liquid nitrogen fracturing.

Grab and passive sampling applied to pesticide analysis in the São Lourenço river headwater in Campo Verde - MT, Brazil.

PubMed

Berton, André; Brugnera, Michelle F; Dores, Eliana F G C

2018-04-03

In this study, the quality of surface water in the headwaters of São Lourenço River in Mato Grosso, Brazil, was evaluated in relation to contamination by pesticides. For this purpose, samples were collected between December 2015 and June 2016 by grab sampling and by passive sampling using an integrative polar organic compound sampler installed in the field during four 14-day cycles between March and June 2016. The analyses were performed by gas chromatography (CG/MS) and by liquid chromatography (UPLC-MS/MS). The results showed the detection of two pesticides (atrazine and pyraclostrobin) of the five analyzed by passive sampling and eight active principles among the 20 analyzed (malathion, diuron, carbofuran, carbendazim, trifluralin, imidacloprid, metolachlor, and acetamiprid) by grab sampling. The detection of 10 pesticides, even almost a decade after the beginning of a recovery process of the ciliary forest, confirms the headwaters' vulnerability to these contaminants and passive sampling proved to be an important tool in capturing small concentrations of pesticides constituting an interesting complement to grab sampling.

Liquid crystals in micron-scale droplets, shells and fibers

NASA Astrophysics Data System (ADS)

Urbanski, Martin; Reyes, Catherine G.; Noh, JungHyun; Sharma, Anshul; Geng, Yong; Subba Rao Jampani, Venkata; Lagerwall, Jan P. F.

2017-04-01

The extraordinary responsiveness and large diversity of self-assembled structures of liquid crystals are well documented and they have been extensively used in devices like displays. For long, this application route strongly influenced academic research, which frequently focused on the performance of liquid crystals in display-like geometries, typically between flat, rigid substrates of glass or similar solids. Today a new trend is clearly visible, where liquid crystals confined within curved, often soft and flexible, interfaces are in focus. Innovation in microfluidic technology has opened for high-throughput production of liquid crystal droplets or shells with exquisite monodispersity, and modern characterization methods allow detailed analysis of complex director arrangements. The introduction of electrospinning in liquid crystal research has enabled encapsulation in optically transparent polymeric cylinders with very small radius, allowing studies of confinement effects that were not easily accessible before. It also opened the prospect of functionalizing textile fibers with liquid crystals in the core, triggering activities that target wearable devices with true textile form factor for seamless integration in clothing. Together, these developments have brought issues center stage that might previously have been considered esoteric, like the interaction of topological defects on spherical surfaces, saddle-splay curvature-induced spontaneous chiral symmetry breaking, or the non-trivial shape changes of curved liquid crystal elastomers with non-uniform director fields that undergo a phase transition to an isotropic state. The new research thrusts are motivated equally by the intriguing soft matter physics showcased by liquid crystals in these unconventional geometries, and by the many novel application opportunities that arise when we can reproducibly manufacture these systems on a commercial scale. This review attempts to summarize the current understanding of liquid crystals in spherical and cylindrical geometry, the state of the art of producing such samples, as well as the perspectives for innovative applications that have been put forward.

Homogeneous nucleation of ethanol and n-propanol in a shock tube

NASA Technical Reports Server (NTRS)

Peters, F.

1982-01-01

The condensation by homogeneous nucleation of ethanol (200 proof) and of n-propanol (99.98%) carried at small mole fraction in dry air (99.995%) was studied in the unsteady, isentropic expansion of a shock tube. Samples of the vapor at different partial pressures in dry air at room temperature were expanded into the liquid coexistence regime of the condensing species. A Kristler pressure transducer and Rayleigh light scattering were used to measure the pressure in the expansion and the onset of condensation. Condensation was observed at different locations between 0.15 and 1 m upstream of the diaphragm location, which correspond to different cooling rates of of the vapor samples about 50 to 10 C/ms.

Fluidics cube for biosensor miniaturization

NASA Technical Reports Server (NTRS)

Dodson, J. M.; Feldstein, M. J.; Leatzow, D. M.; Flack, L. K.; Golden, J. P.; Ligler, F. S.

2001-01-01

To create a small, portable, fully automated biosensor, a compact means of fluid handling is required. We designed, manufactured, and tested a "fluidics cube" for such a purpose. This cube, made of thermoplastic, contains reservoirs and channels for liquid samples and reagents and operates without the use of any internal valves or meters; it is a passive fluid circuit that relies on pressure relief vents to control fluid movement. We demonstrate the ability of pressure relief vents to control fluid movement and show how to simply manufacture or modify the cube. Combined with the planar array biosensor developed at the Naval Research Laboratory, it brings us one step closer to realizing our goal of a handheld biosensor capable of analyzing multiple samples for multiple analytes.

Development and Applications of Liquid Sample Desorption Electrospray Ionization Mass Spectrometry

NASA Astrophysics Data System (ADS)

Zheng, Qiuling; Chen, Hao

2016-06-01

Desorption electrospray ionization mass spectrometry (DESI-MS) is a recent advance in the field of analytical chemistry. This review surveys the development of liquid sample DESI-MS (LS-DESI-MS), a variant form of DESI-MS that focuses on fast analysis of liquid samples, and its novel analy-tical applications in bioanalysis, proteomics, and reaction kinetics. Due to the capability of directly ionizing liquid samples, liquid sample DESI (LS-DESI) has been successfully used to couple MS with various analytical techniques, such as microfluidics, microextraction, electrochemistry, and chromatography. This review also covers these hyphenated techniques. In addition, several closely related ionization methods, including transmission mode DESI, thermally assisted DESI, and continuous flow-extractive DESI, are briefly discussed. The capabilities of LS-DESI extend and/or complement the utilities of traditional DESI and electrospray ionization and will find extensive and valuable analytical application in the future.

Genotoxicity of wastewaters used for irrigation of food crops.

PubMed

Ansari, Mohd Ikram; Malik, Abdul

2009-04-01

In most towns of India, wastewater coming from both industrial and domestic sources and without any treatment is used to irrigate the agricultural crops. This practice has been polluting the soil, and pollutants could possibly reach the food chain. For the above reasons, the wastewaters of Ghaziabad City (India), which is used for irrigation, were sampled (at two different sites) and monitored for the presence of genotoxic agents from January 2005 to June 2007. Gas chromatographic analysis showed the presence of certain OC (DDE, DDT, Dieldrin, Aldrin, and Endosulfan) and OP (Dimethoate, Malathion, Methlyparathion, and Chlorpyrifos) pesticides in both the sampling sites. Wastewater samples were concentrated using XAD resins (XAD-4 and XAD-8) and liquid-liquid extraction procedures, and the extracts were assayed for genotoxic potential by Ames Salmonella/microsome test, DNA repair defective mutants, and bacteriophage lambda systems. The test samples exhibited significant mutagenicity with TA98, TA97a, and TA100 strains with the probable role of contaminating pesticides in the wastewater. However, XAD-concentrated samples were more mutagenic in both sites as compared to liquid-liquid-extracted samples. The damage in the DNA repair defective mutants in the presence of XAD-concentrated water samples were also found to be higher to that of liquid-liquid-extracted water samples at the dose level of 20 muL/mL culture. All the mutants invariably exhibited significant decline in their colony-forming units as compared to their isogenic wild-type counterparts. The survival was decreased by 81.7 and 75.5% in polA(-) strain in site I, and 76.0 and 73.5% in site II in polA(-) under the same experimental conditions after 6 h of treatment with XAD-concentrated and liquid-liquid-extracted samples, respectively. A significant decrease in the survival of bacteriophage lambda was also observed when treated with the test samples. Copyright 2008 Wiley Periodicals, Inc.

Solubility of Structurally Complicated Materials: 3. Hair

PubMed Central

Horvath, Ari L.

2009-01-01

Hair is composed of proteins, lipids, water, and small amounts of trace elements. All proteins in animal and human bodies are built from permutations of amino acid molecules in a polypeptide string. The polypeptide chains of protein keratin are organized into filaments in hair cells. Hair is one of the most difficult proteins to digest or solubilize. Among the most common dissolving procedures for hair are acidic, alkaline, and enzymatic hydrolysis. For the analysis of hair, the solid samples are transferred by solubilization via digestion into a liquid phase. Small molecular solvents and molecules with hydrophobic groups appear to have higher affinity for hair. A good solvent attacks the disulfide bonds between cystine molecules and hydrates the hair shaft. Consequently, the hair becomes a jelly-like mass. PMID:19412554

Test plan for Geo-Cleanse{reg_sign} demonstration (in situ destruction of dense non-aqueous phase liquid (DNAPL))

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

Jerome, K.M.; Looney, B.B.; Accorsi, F.

1996-09-01

Soils and groundwater beneath an abandoned process sewer line in the A/M Area of the Savannah River Site (SRS) contain elevated levels of volatile organic compounds, specifically trichloroethylene (TCE) and tetrachloroethylene (PCE), two common chlorinated solvents. These compounds have low aqueous solubilities, thus when released to the subsurface in sufficient quantity, tend to exist as immiscible fluids or nonaqueous phase liquids (NAPLs). Because chlorinated solvents are also denser than water, they are referred to by the acronym DNAPLs, or dense non-aqueous phase liquids. Technologies targeted at the efficient characterization or removal of DNAPL are not currently proven. For example, mostmore » DNAPL studies rely on traditional soil and water sampling and the fortuitous observation of immiscible solvent. Once DNAPL is identified, soil excavation (which is only applicable to small contained spill sites) is the only proven cleanup method. New cleanup approaches based on destruction of DNAPL either in situ or ex situ have been proposed and tested at the pilot scale. The proposed demonstration, as described in this report will evaluate the applicability to DNAPL plumes of a technology proven for in situ destruction of light non-aqueous phase liquids (LNAPLs) such as oils.« less

Cadmium accumulation in zebrafish (Danio rerio) eggs is modulated by dissolved organic matter (DOM).

PubMed

Burnison, B Kent; Meinelt, Thomas; Playle, Richard; Pietrock, Michael; Wienke, Andreas; Steinberg, Christian E W

2006-08-23

Experiments were conducted to investigate factors influencing the accumulation of cadmium (Cd(2+)) into zebrafish (Danio rerio) eggs. The accumulation of (109)Cd was affected by: (1) concentration, (2) time, (3) presence of dissolved organic material (DOM), (4) different origin of DOM and (5) different parts of fish eggs. Over a 5-h exposure, zebrafish eggs showed a steady increase in Cd-accumulation. DOM-concentrations over 15ppm carbon (C) decreased Cd-uptake significantly. Both samples of DOM, brown water marsh (LM) and a eutrophic pond (SP), at 16.9ppmC, reduced the Cd-accumulation in the chorion, perivitelline liquid and the embryo. Cd was mainly accumulated in the egg's outer shell chorion (61%) and only small amounts passed through the chorion into the perivitelline liquid (38%) and embryo (1%). In the presence of LM-DOM, the accumulation of Cd into the egg components was decreased by 43% (chorion), 52% (perivitelline liquid) and 52% (embryo), respectively, compared with the control group. Similarly, the presence of SP-DOM reduced the Cd-accumulation by 29% (chorion), 61% (perivitelline liquid) and 60% (embryo), respectively, compared with the controls. DOM-concentration should be taken into consideration when determining ecotoxicological effects of Cd on fish populations.

Fluid sampling system

DOEpatents

Houck, Edward D.

1994-01-01

An fluid sampling system allows sampling of radioactive liquid without spillage. A feed tank is connected to a liquid transfer jet powered by a pumping chamber pressurized by compressed air. The liquid is pumped upwardly into a sampling jet of a venturi design having a lumen with an inlet, an outlet, a constricted middle portion, and a port located above the constricted middle portion. The liquid is passed under pressure through the constricted portion causing its velocity to increase and its pressure to decreased, thereby preventing liquid from escaping. A septum sealing the port can be pierced by a two pointed hollow needle leading into a sample bottle also sealed by a pierceable septum affixed to one end. The bottle is evacuated by flow through the sample jet, cyclic variation in the sampler jet pressure periodically leaves the evacuated bottle with lower pressure than that of the port, thus causing solution to pass into the bottle. The remaining solution in the system is returned to the feed tank via a holding tank.

Fluid sampling system

DOEpatents

Houck, E.D.

1994-10-11

An fluid sampling system allows sampling of radioactive liquid without spillage. A feed tank is connected to a liquid transfer jet powered by a pumping chamber pressurized by compressed air. The liquid is pumped upwardly into a sampling jet of a venturi design having a lumen with an inlet, an outlet, a constricted middle portion, and a port located above the constricted middle portion. The liquid is passed under pressure through the constricted portion causing its velocity to increase and its pressure to be decreased, thereby preventing liquid from escaping. A septum sealing the port can be pierced by a two pointed hollow needle leading into a sample bottle also sealed by a pierceable septum affixed to one end. The bottle is evacuated by flow through the sample jet, cyclic variation in the sampler jet pressure periodically leaves the evacuated bottle with lower pressure than that of the port, thus causing solution to pass into the bottle. The remaining solution in the system is returned to the feed tank via a holding tank. 4 figs.

Hexavalent chromium monitor

DOEpatents

Tao, Shiquan; Winstead, Christopher B.

2005-04-12

A monitor is provided for use in measuring the concentration of hexavalent chromium in a liquid, such as water. The monitor includes a sample cell, a light source, and a photodetector. The sample cell is in the form of a liquid-core waveguide, the sample cell defining an interior core and acting as a receiver for the liquid to be analyzed, the interior surface of the sample cell having a refractive index of less than 1.33. The light source is in communication with a first end of the sample cell for emitting radiation having a wavelength of about and between 350 to 390 nm into the interior core of the waveguide. The photodetector is in communication with a second end of the waveguide for measuring the absorption of the radiation emitted by the light source by the liquid in the sample cell. The monitor may also include a processor electronically coupled to the photodetector for receipt of an absorption signal to determine the concentration of hexavalent chromium in the liquid.

Development of a new extraction method based on counter current salting-out homogenous liquid-liquid extraction followed by dispersive liquid-liquid microextraction: Application for the extraction and preconcentration of widely used pesticides from fruit juices.

PubMed

Farajzadeh, Mir Ali; Feriduni, Behruz; Mogaddam, Mohammad Reza Afshar

2016-01-01

In this paper, a new extraction method based on counter current salting-out homogenous liquid-liquid extraction (CCSHLLE) followed by dispersive liquid-liquid microextraction (DLLME) has been developed for the extraction and preconcentration of widely used pesticides in fruit juice samples prior to their analysis by gas chromatography-flame ionization detection (GC-FID). In this method, initially, sodium chloride as a separation reagent is filled into a small column and a mixture of water (or fruit juice) and acetonitrile is passed through the column. By passing the mixture sodium chloride is dissolved and the fine droplets of acetonitrile are formed due to salting-out effect. The produced droplets go up through the remained mixture and collect as a separated layer. Then, the collected organic phase (acetonitrile) is removed with a syringe and mixed with 1,1,2,2-tetrachloroethane (extraction solvent at µL level). In the second step, for further enrichment of the analytes the above mixture is injected into 5 mL de-ionized water placed in a test tube with conical bottom in order to dissolve acetonitrile into water and to achieve a sedimented phase at µL-level volume containing the enriched analytes. Under the optimal extraction conditions (extraction solvent, 1.5 mL acetonitrile; pH, 7; flow rate, 0.5 mL min(-1); preconcentration solvent, 20 µL 1,1,2,2-tetrachloroethane; NaCl concentration; 5%, w/w; and centrifugation rate and time, 5000 rpm and 5 min, respectively), the extraction recoveries and enrichment factors ranged from 87% to 96% and 544 to 600, respectively. Repeatability of the proposed method, expressed as relative standard deviations, ranged from 2% to 6% for intra-day (n=6, C=250 or 500 µg L(-1)) and inter-days (n=4, C=250 or 500 µg L(-1)) precisions. Limits of detection are obtained between 2 and 12 µg L(-1). Finally, the proposed method is applied for the determination of the target pesticide residues in the juice samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Heat Capacity of Hydrous Silicate Melts

NASA Astrophysics Data System (ADS)

Robert, G.; Whittington, A. G.; Stechern, A.; Behrens, H.

2015-12-01

We determined the heat capacities of four series of glasses and liquids of basaltic and basaltic andesite compositions including two natural remelts from Fuego volcano, Guatemala, and two Fe-free analogs. The samples are low-alkali, Ca- and Mg-rich aluminosilicates with non-bridging oxygen to tetrahedrally-coordinated cation ratios (NBO/T) ranging between 0.33 and 0.67. Differential scanning calorimetry measurements were performed at atmospheric pressure between room temperature and ≈100 K above the glass transition for hydrous samples and up to ≈1800 K for dry samples. The water contents investigated range up to 5.34 wt.% (16.4 mol%). Water does not measurably affect the heat capacity of glasses (T

Isolation of anticancer drug TAXOL from Pestalotiopsis breviseta with apoptosis and B-Cell lymphoma protein docking studies.

PubMed

Kathiravan, G; Sureban, Sripathi M; Sree, Harsha N; Bhuvaneshwari, V; Kramony, Evelin

2012-12-01

Extraction and investigation of TAXOL from Pestalotiopsis breviseta (Sacc.) using protein docking, which is a computational technique that samples conformations of small molecules in protein-binding sites. Scoring functions are used to assess which of these conformations best complements the protein binding site and active site prediction. Coelomycetous fungi P. breviseta (Sacc.) Steyaert was screened for the production of TAXOL, an anticancer drug. TAXOL PRODUCTION WAS CONFIRMED BY THE FOLLOWING METHODS: Ultraviolet (UV) spectroscopic analysis, Infrared analysis, High performance liquid chromatography analysis (HPLC), and Liquid chromatography mass spectrum (LC-MASS). TAXOL produced by the fungi was compared with authentic TAXOL, and protein docking studies were performed. The BCL2 protein of human origin showed a higher affinity toward the compound paclitaxel. It has the binding energy value of -13.0061 (KJ/Mol) with four hydrogen bonds.

Isolation of anticancer drug TAXOL from Pestalotiopsis breviseta with apoptosis and B-Cell lymphoma protein docking studies

PubMed Central

Kathiravan, G.; Sureban, Sripathi M.; Sree, Harsha N.; Bhuvaneshwari, V.; Kramony, Evelin

2012-01-01

Background: Extraction and investigation of TAXOL from Pestalotiopsis breviseta (Sacc.) using protein docking, which is a computational technique that samples conformations of small molecules in protein-binding sites. Scoring functions are used to assess which of these conformations best complements the protein binding site and active site prediction. Materials and Methods: Coelomycetous fungi P. breviseta (Sacc.) Steyaert was screened for the production of TAXOL, an anticancer drug. Results: TAXOL production was confirmed by the following methods: Ultraviolet (UV) spectroscopic analysis, Infrared analysis, High performance liquid chromatography analysis (HPLC), and Liquid chromatography mass spectrum (LC-MASS). TAXOL produced by the fungi was compared with authentic TAXOL, and protein docking studies were performed. Conclusion: The BCL2 protein of human origin showed a higher affinity toward the compound paclitaxel. It has the binding energy value of −13.0061 (KJ/Mol) with four hydrogen bonds. PMID:24808664

A simplified computer program for the prediction of the linear stability behavior of liquid propellant combustors

NASA Technical Reports Server (NTRS)

Mitchell, C. E.; Eckert, K.

1979-01-01

A program for predicting the linear stability of liquid propellant rocket engines is presented. The underlying model assumptions and analytical steps necessary for understanding the program and its input and output are also given. The rocket engine is modeled as a right circular cylinder with an injector with a concentrated combustion zone, a nozzle, finite mean flow, and an acoustic admittance, or the sensitive time lag theory. The resulting partial differential equations are combined into two governing integral equations by the use of the Green's function method. These equations are solved using a successive approximation technique for the small amplitude (linear) case. The computational method used as well as the various user options available are discussed. Finally, a flow diagram, sample input and output for a typical application and a complete program listing for program MODULE are presented.

Targeted profiling of hydrophilic constituents of royal jelly by hydrophilic interaction liquid chromatography-tandem mass spectrometry.

PubMed

Pina, Athanasia; Begou, Olga; Kanelis, Dimitris; Gika, Helen; Kalogiannis, Stavros; Tananaki, Chrysoula; Theodoridis, Georgios; Zotou, Anastasia

2018-01-05

In the present work a Hydrophilic Interaction Liquid Chromatography-tandem Mass Spectrometry (HILIC-MS/MS) method was developed for the efficient separation and quantification of a large number of small polar bioactive molecules in Royal Jelly. The method was validated and provided satisfactory detection sensitivity for 88 components. Quantification was proven to be precise for 64 components exhibiting good linearity, recoveries R% >90% for the majority of analytes and intra- and inter-day precision from 0.14 to 20% RSD. Analysis of 125 fresh royal jelly samples of Greek origin provided useful information on royal jelly's hydrophilic bioactive components revealing lysine, ribose, proline, melezitose and glutamic acid to be in high abundance. In addition the occurrence of 18 hydrophilic nutrients which have not been reported previously as royal jelly constituents is shown. Copyright © 2017 Elsevier B.V. All rights reserved.

Acoustic levitation of liquid drops: Dynamics, manipulation and phase transitions.

PubMed

Zang, Duyang; Yu, Yinkai; Chen, Zhen; Li, Xiaoguang; Wu, Hongjing; Geng, Xingguo

2017-05-01

The technique of acoustic levitation normally produces a standing wave and the potential well of the sound field can be used to trap small objects. Since no solid surface is involved it has been widely applied for the study of fluid physics, nucleation, bio/chemical processes, and various forms of soft matter. In this article, we survey the works on drop dynamics in acoustic levitation, focus on how the dynamic behavior is related to the rheological properties and discuss the possibility to develop a novel rheometer based on this technique. We review the methods and applications of acoustic levitation for the manipulation of both liquid and solid samples and emphasize the important progress made in the study of phase transitions and bio-chemical analysis. We also highlight the possible open areas for future research. Copyright © 2017 Elsevier B.V. All rights reserved.

Spectral properties of thermal fluctuations on simple liquid surfaces below shot-noise levels.

PubMed

Aoki, Kenichiro; Mitsui, Takahisa

2012-07-01

We study the spectral properties of thermal fluctuations on simple liquid surfaces, sometimes called ripplons. Analytical properties of the spectral function are investigated and are shown to be composed of regions with simple analytic behavior with respect to the frequency or the wave number. The derived expressions are compared to spectral measurements performed orders of magnitude below shot-noise levels, which is achieved using a novel noise reduction method. The agreement between the theory of thermal surface fluctuations and the experiment is found to be excellent, elucidating the spectral properties of the surface fluctuations. The measurement method requires relatively only a small sample both spatially (few μm) and temporally (~20 s). The method also requires relatively weak light power (~0.5 mW) so that it has a broad range of applicability, including local measurements, investigations of time-dependent phenomena, and noninvasive measurements.

Liquid chromatography/electrospray ionization tandem mass spectrometry analysis of octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX).

PubMed

Pan, Xiaoping; Zhang, Baohong; Tian, Kang; Jones, Lindsey E; Liu, Jun; Anderson, Todd A; Wang, Jia-Sheng; Cobb, George P

2006-01-01

A quantitative liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) method was developed for the analysis of the explosive, octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX). In negative ionization mode, HMX forms an acetate adduct ion [M + CH(3)COO](-), m/z 355, in the presence of a small amount of acetic acid in the mobile phase. The ESI collision-induced dissociation (CID) spectrum of m/z 355 was acquired and the transitions m/z 355 --> 147 and m/z 355 --> 174 were chosen for the determination of HMX in samples. Using this quantification technique, the method detection limit was 1.57 microg/L and good linearity was achieved in the range 5-500 microg/L. This method will help to unambiguously analyze environmentally relevant concentrations of HMX. Copyright (c) 2006 John Wiley & Sons, Ltd.

Determination of nonylphenol and nonylphenol ethoxylates in environmental solid samples by ultrasonic-assisted extraction and high performance liquid chromatography-fluorescence detection.

PubMed

Núñez, L; Turiel, E; Tadeo, J L

2007-04-06

A simple and rapid analytical method for the determination of nonylphenol (NP) and nonylphenol ethoxylates (NPEOx) in solid environmental samples has been developed. This method combines an ultrasonic-assisted extraction procedure in small columns and an enrichment step onto C(18) solid-phase extraction cartridges prior to separation using HPLC with fluorescence detection. Method optimization was carried out using soil samples fortified at different concentration levels (from 0.1 to 100 microg/g). Under optimum conditions, 2g of soil was placed in small glass columns and extraction was performed assisted by sonication (SAESC) at 45 degrees C in two consecutive steps of 15 min using a mixture of H(2)O/MeOH (30/70). The obtained extracts were collected, loaded onto 500 mg C(18) cartridges, and analytes were eluted with 3 x 1 ml of methanol and 1 ml of acetonitrile. Finally, sample extracts were evaporated under a nitrogen stream, redissolved in 500 microl H(2)O/AcN (50/50), and passed though a 0.45 microm nylon filter before final determination by HPLC-FL. The developed procedure allowed to achieve quantitative recoveries for NP and NPEOx, and was properly validated. Finally, the method was applied to the determination of these compounds in soils and other environmental solid samples such as sediments, compost and sludge.

Solid surface wetting and the deployment of drops in microgravity

NASA Technical Reports Server (NTRS)

Trinh, E. H.; Depew, J.

1994-01-01

The complete or partial deployment of liquid samples in low gravity is primarily influenced by the interfacial properties of the specific liquid and solid materials used because the overwhelming bias of the Earth gravitational acceleration is removed. This study addresses the engineering aspects of injecting and deploying drops of prescribed volume into an acoustic positioning chamber in microgravity. The specific problems of interest are the design, testing, and implementation of injector tips to be used in a simultaneously retracting dual-injector system in the Drop Physics Module microgravity experiment facility. Prior to release, the liquid to be deployed must be retained within a restricted area at the very end of the injectors under dynamic stimuli from the continuous injection flow as well as from the stepped motion of the injectors. The final released drop must have a well determined volume and negligible residual linear or angular momentum. The outcome of Earth-based short-duration low gravity experiments had been the selection of two types of injector tips which were flown as back-up parts. They were successfully utilized during the USML-1 Spacelab mission as the primary tips. The combination of a larger contact surface, liquid pinning with a sharp edge, and selective coating of strategic tip surfaces with a non-wetting compound has allowed a significant increase in the success rate of deployment of simple and compound drops of aqueous solutions of glycerol and silicone oil. The diameter of the samples studied in the Drop Physics Module range between 0.3 and 2.7 cm. The tests conducted on-orbit with a manually operated small device have allowed the calibration of the volume deployed for a few drop sizes. The design for improved tips to be used during the next USML flight is based on these results.

Solid Surface Wetting and the Deployment of Drops in Microgravity

NASA Technical Reports Server (NTRS)

Trinh, E. H.; Depew, J.

1994-01-01

The complete or partial deployment of liquid samples in low gravity is primarily influenced by the interfacial properties of the specific liquid and solid materials used because the overwhelming bias of the Earth gravitational acceleration is removed. This study addresses the engineering aspects of injecting and deploying drops of prescribed volume into an acoustic positioning chamber in microgravity. The specific problems of interest are the design, testing, and implementation of injector tips to be used in a simuttaneously retracting dual-injector system used in the Drop Physics Module microgravity experiment facility. Prior to release, the liquid to be deployed must be retained within a restricted area at the very end of the injectors even under dynamic stimuli due to continuous injection flow as well as to the stepped motion of the injectors, and the final released drop must have a well determined volume as well as negligible residual linear or angular momentum from the deployment process. The outcome of Earthbased short-duration low gravity experiments had been the selection of two types of injector tips which were flown as back-up parts and were successfully utilized during the USML-1 Spacelab mission. The combination of a larger contact surface, liquid pinning with a sharp edge, and selective coating of strategic tip surfaces with a non-wetting compound has allowed a significant increase in the success rate of deployment of simple and compound drops of aqueous solutions of glycerol and silicone oil. The diameter of the samples studied in the Drop Physics Module ranged between 0.3 and 2.7 cm. The tests conducted onsrbit with a manually operated small device have allowed the calibration of the volume deployed for a few drop sizes. The design for improved tips to be used during the next USML flight is based on these results.

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

Larsson, Daniel H.; Lundstroem, Ulf; Burvall, Anna

Purpose: Small-animal studies require images with high spatial resolution and high contrast due to the small scale of the structures. X-ray imaging systems for small animals are often limited by the microfocus source. Here, the authors investigate the applicability of liquid-metal-jet x-ray sources for such high-resolution small-animal imaging, both in tomography based on absorption and in soft-tissue tumor imaging based on in-line phase contrast. Methods: The experimental arrangement consists of a liquid-metal-jet x-ray source, the small-animal object on a rotating stage, and an imaging detector. The source-to-object and object-to-detector distances are adjusted for the preferred contrast mechanism. Two different liquid-metal-jetmore » sources are used, one circulating a Ga/In/Sn alloy and the other an In/Ga alloy for higher penetration through thick tissue. Both sources are operated at 40-50 W electron-beam power with {approx}7 {mu}m x-ray spots, providing high spatial resolution in absorption imaging and high spatial coherence for the phase-contrast imaging. Results: High-resolution absorption imaging is demonstrated on mice with CT, showing 50 {mu}m bone details in the reconstructed slices. High-resolution phase-contrast soft-tissue imaging shows clear demarcation of mm-sized tumors at much lower dose than is required in absorption. Conclusions: This is the first application of liquid-metal-jet x-ray sources for whole-body small-animal x-ray imaging. In absorption, the method allows high-resolution tomographic skeletal imaging with potential for significantly shorter exposure times due to the power scalability of liquid-metal-jet sources. In phase contrast, the authors use a simple in-line arrangement to show distinct tumor demarcation of few-mm-sized tumors. This is, to their knowledge, the first small-animal tumor visualization with a laboratory phase-contrast system.« less

A simple, rapid and novel method based on salting-out assisted liquid-liquid extraction for ochratoxin A determination in beer samples prior to ultra-high performance liquid chromatography coupled to tandem mass spectrometry.

PubMed

Mariño-Repizo, Leonardo; Goicoechea, Hector; Raba, Julio; Cerutti, Soledad

2018-06-07

A novel, simple, easy and cheap sample treatment strategy based on salting-out assisted liquid-liquid extraction (SALLE) for ochratoxin A (OTA) ultra-trace analysis in beer samples using ultra-high performance liquid chromatography-tandem mass spectrometry determination was developed. The factors involved in the efficiency of pretreatment were studied employing factorial design in the screening phase and the optimal conditions of the significant variables on the analytical response were evaluated using a central composite face-centred design (CCF). Consequently, the amount of salt ((NH 4 ) 2 SO 4 ), together with the volumes of sample, hydrophilic (acetone) and nonpolar (toluene) solvents, and times of vortexing and centrifugation were optimized. Under optimized conditions, the limits of detection (LOD) and quantification (LOQ) were 0.02 µg l -1 and 0.08 µg l -1 respectively. OTA extraction recovery by SALLE was approximately 90% (0.2 µg l -1 ). Furthermore, the methodology was in agreement with EU Directive requirements and was successfully applied for analysis of beer samples.

Fast, simple and efficient salting-out assisted liquid-liquid extraction of naringenin from fruit juice samples prior to their enantioselective determination by liquid chromatography.

PubMed

Magiera, Sylwia; Kwietniowska, Ewelina

2016-11-15

In this study, an easy, simple and efficient method for the determination of naringenin enantiomers in fruit juices after salting-out-assisted liquid-liquid extraction (SALLE) and high-performance liquid chromatography (HPLC) with diode-array detection (DAD) was developed. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. After extraction, juice samples were incubated with hydrochloric acid in order to achieve hydrolysis of naringin to naringenin. The hydrolysis parameters were optimized by using a half-fraction factorial central composite design (CCD). After sample preparation, chromatographic separation was obtained on a Chiralcel® OJ-RH column using the mobile phase consisting of 10mM aqueous ammonium acetate:methanol:acetonitrile (50:30:20; v/v/v) with detection at 288nm. The average recovery of the analyzed compounds ranged from 85.6 to 97.1%. The proposed method was satisfactorily used for the determination of naringenin enantiomers in various fruit juices samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

An ultrasound-based liquid pressure measurement method in small diameter pipelines considering the installation and temperature.

PubMed

Li, Xue; Song, Zhengxiang

2015-04-09

Liquid pressure is a key parameter for detecting and judging faults in hydraulic mechanisms, but traditional measurement methods have many deficiencies. An effective non-intrusive method using an ultrasound-based technique to measure liquid pressure in small diameter (less than 15 mm) pipelines is presented in this paper. The proposed method is based on the principle that the transmission speed of an ultrasonic wave in a Kneser liquid correlates with liquid pressure. Liquid pressure was calculated using the variation of ultrasonic propagation time in a liquid under different pressures: 0 Pa and X Pa. In this research the time difference was obtained by an electrical processing approach and was accurately measured to the nanosecond level through a high-resolution time measurement module. Because installation differences and liquid temperatures could influence the measurement accuracy, a special type of circuit called automatic gain control (AGC) circuit and a new back propagation network (BPN) model accounting for liquid temperature were employed to improve the measurement results. The corresponding pressure values were finally obtained by utilizing the relationship between time difference, transient temperature and liquid pressure. An experimental pressure measurement platform was built and the experimental results confirm that the proposed method has good measurement accuracy.

Scuffing Characteristics of High-Load Rolling/Sliding Contacts Operating in Liquid Oxygen: Effects of Materials and Surface Roughness

NASA Technical Reports Server (NTRS)

Chang, L.; Hall, P. B.; Thom, R.

1996-01-01

This research reports on an experimental study of the effects of materials and surface roughness on the scuffing characteristics of rolling/sliding contacts cooled and lubricated with liquid oxygen. Experiments were carried out under heavy loading with a Hertzian pressure in the range of 2.0 GPa to 3.0 GPa and with a high rolling velocity of up to 48 m/s. For contacts between AISI 440 C stainless-steel elements, the results showed that the scuffing behavior of the system was fairly consistent under a wide range of rolling velocity. Scuffing commenced at a small slide-to-roll ratio of around 0.02, and the scuffing behavior of the contact was not sensitive to surface roughness for the test-sample RMS roughness ranging from 0.02 microns to 0.10 microns. For contacts between 440 C and Si3N4 elements, on the other hand, the scuffing behavior of the system was not very consistent and somewhat unpredictable. The results were sensitive to surface roughness particularly that of the Si3N4 test sample. With well polished test samples, consistent results were obtained; the level of traction was lower than that with a 440 C toroid and scuffing did not take place up to a slide-to-roll ratio of near 0.03. The results strongly suggest that significant hydrodynamic effect can be generated by liquid oxygen under heavy loading and high velocity conditions. The results also suggest that the hydrodynamic action is likely generated by the conventional viscous mechanism as it can be largely destroyed by a narrow circumferential surface scratch running through the central region of the contact.

Determining aromatic and aliphatic carboxylic acids in biomass-derived oil samples using 2,4-dinitrophenylhydrazine and liquid chromatography-electrospray injection-mass spectrometry/mass spectrometry

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

Lewis, Sr., Samuel A.; Connatser, Raynella M.; Olarte, Mariefel V.

Here, converting biomass to a useful fuel commonly incorporates the pyrolysis of the biomass feed stock. The base liquid fraction usually contains high concentrations of ketones, aldehydes and carboxylic acids, of which each can cause detrimental issues related to the storage and upgrading process. Knowing the carbonyl species and the concentration of each will provide value information to the pyrolysis researchers, specifically as that community branches into more targeted end-products such as jet fuel or biogenic-derived oxygenate-containing fuel products. The analysis of aldehydes, ketones and small alkyl carboxylic acids using 2,4-dinitrophenylhydrazine (DNPH) derivation method has been well documented and themore » method is commonly used the analytical community. By using liquid chromatograph coupled to tandem mass spectrometry, biomass sample analysis can be complete with identification of most carbonyl species. The issue of identifying isobaric ketone and aldehyde compounds can be resolved by utilizing differences in retention time or characteristic fragment ions of ketones and aldehydes. One issue which could not resolved using published methods was identifying aromatic or large non-aromatic carboxylic acids from their corresponding hydroxyl aldehyde or ketone analogs. By modifying the current method for determining carbonyls in biomass samples, carboxylic and hydroxyl-carbonyl can be determined. A careful adjustment of the pH during the extraction procedure and extended heating time of the DNPH solution allowed for the successful derivation of aromatic carboxylic acids. Like other dinitrophenylhydrazones, carboxylic acid derivatives also produce a unique secondary ion pattern, which was useful to distinguish these species from the non-acid analogs.« less

Determining aromatic and aliphatic carboxylic acids in biomass-derived oil samples using 2,4-dinitrophenylhydrazine and liquid chromatography-electrospray injection-mass spectrometry/mass spectrometry

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

Lewis, Samuel A.; Connatser, Raynella M.; Olarte, Mariefel V.

Converting biomass to a useful fuel commonly incorporates the pyrolysis of the biomass feed stock. The base liquid fraction usually contains high concentrations of ketones, aldehydes and carboxylic acids, of which each can cause detrimental issues related to the storage and upgrading process. Knowing the carbonyl species and the concentration of each will provide value information to the pyrolysis researchers, specifically as that community branches into more targeted end-products such as jet fuel or biogenic-derived oxygenate-containing fuel products. The analysis of aldehydes, ketones and small alkyl carboxylic acids using 2,4-dinitrophenylhydrazine (DNPH) derivation method has been well documented and the methodmore » is commonly used the analytical community. By using liquid chromatograph coupled to tandem mass spectrometry, biomass sample analysis can be complete with identification of most carbonyl species. The issue of identifying isobaric ketone and aldehyde compounds can be resolved by utilizing differences in retention time or characteristic fragment ions of ketones and aldehydes. One issue which could not resolved using published methods was identifying aromatic or large non-aromatic carboxylic acids from their corresponding hydroxyl aldehyde or ketone analogs. By modifying the current method for determining carbonyls in biomass samples, carboxylic and hydroxyl-carbonyl can be determined. A careful adjustment of the pH during the extraction procedure and extended heating time of the DNPH solution allowed for the successful derivation of aromatic carboxylic acids. Like other dinitrophenylhydrazones, carboxylic acid derivatives also produce a unique secondary ion pattern, which was useful to distinguish these species from the non-acid analogs.« less

Determining aromatic and aliphatic carboxylic acids in biomass-derived oil samples using 2,4-dinitrophenylhydrazine and liquid chromatography-electrospray injection-mass spectrometry/mass spectrometry

DOE PAGES

Lewis, Sr., Samuel A.; Connatser, Raynella M.; Olarte, Mariefel V.; ...

2017-11-22

Here, converting biomass to a useful fuel commonly incorporates the pyrolysis of the biomass feed stock. The base liquid fraction usually contains high concentrations of ketones, aldehydes and carboxylic acids, of which each can cause detrimental issues related to the storage and upgrading process. Knowing the carbonyl species and the concentration of each will provide value information to the pyrolysis researchers, specifically as that community branches into more targeted end-products such as jet fuel or biogenic-derived oxygenate-containing fuel products. The analysis of aldehydes, ketones and small alkyl carboxylic acids using 2,4-dinitrophenylhydrazine (DNPH) derivation method has been well documented and themore » method is commonly used the analytical community. By using liquid chromatograph coupled to tandem mass spectrometry, biomass sample analysis can be complete with identification of most carbonyl species. The issue of identifying isobaric ketone and aldehyde compounds can be resolved by utilizing differences in retention time or characteristic fragment ions of ketones and aldehydes. One issue which could not resolved using published methods was identifying aromatic or large non-aromatic carboxylic acids from their corresponding hydroxyl aldehyde or ketone analogs. By modifying the current method for determining carbonyls in biomass samples, carboxylic and hydroxyl-carbonyl can be determined. A careful adjustment of the pH during the extraction procedure and extended heating time of the DNPH solution allowed for the successful derivation of aromatic carboxylic acids. Like other dinitrophenylhydrazones, carboxylic acid derivatives also produce a unique secondary ion pattern, which was useful to distinguish these species from the non-acid analogs.« less

Ionic liquid-based microwave-assisted dispersive liquid-liquid microextraction and derivatization of sulfonamides in river water, honey, milk, and animal plasma.

PubMed

Xu, Xu; Su, Rui; Zhao, Xin; Liu, Zhuang; Zhang, Yupu; Li, Dan; Li, Xueyuan; Zhang, Hanqi; Wang, Ziming

2011-11-30

The ionic liquid-based microwave-assisted dispersive liquid-liquid microextraction (IL-based MADLLME) and derivatization was applied for the pretreatment of six sulfonamides (SAs) prior to the determination by high-performance liquid chromatography (HPLC). By adding methanol (disperser), fluorescamine solution (derivatization reagent) and ionic liquid (extraction solvent) into sample, extraction, derivatization, and preconcentration were continuously performed. Several experimental parameters, such as the type and volume of extraction solvent, the type and volume of disperser, amount of derivatization reagent, microwave power, microwave irradiation time, pH of sample solution, and ionic strength were investigated and optimized. When the microwave power was 240 W, the analytes could be derivatized and extracted simultaneously within 90 s. The proposed method was applied to the analysis of river water, honey, milk, and pig plasma samples, and the recoveries of analytes obtained were in the range of 95.0-110.8, 95.4-106.3, 95.0-108.3, and 95.7-107.7, respectively. The relative standard deviations varied between 1.5% and 7.3% (n=5). The results showed that the proposed method was a rapid, convenient and feasible method for the determination of SAs in liquid samples. Copyright © 2011 Elsevier B.V. All rights reserved.

Combining Laser Ablation/Liquid Phase Collection Surface Sampling and High-Performance Liquid Chromatography Electrospray Ionization Mass Spectrometry

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

Ovchinnikova, Olga S; Kertesz, Vilmos; Van Berkel, Gary J

This paper describes the coupling of ambient pressure transmission geometry laser ablation with a liquid phase sample collection method for surface sampling and ionization with subsequent mass spectral analysis. A commercially available autosampler was adapted to produce a liquid droplet at the end of the syringe injection needle while in close proximity to the surface to collect the sample plume produced by laser ablation. The sample collection was followed by either flow injection or a high performance liquid chromatography (HPLC) separation of the extracted components and detection with electrospray ionization mass spectrometry (ESI-MS). To illustrate the analytical utility of thismore » coupling, thin films of a commercial ink sample containing rhodamine 6G and of mixed isobaric rhodamine B and 6G dyes on glass microscope slides were analyzed. The flow injection and HPLC/ESI-MS analysis revealed successful laser ablation, capture and, with HPLC, the separation of the two compounds. The ablated circular area was about 70 m in diameter for these experiments. The spatial sampling resolution afforded by the laser ablation, as well as the ability to use sample processing methods like HPLC between the sample collection and ionization steps, makes this combined surface sampling/ionization technique a highly versatile analytical tool.« less

Suicide attempt with a mix of synthetic cannabinoids and synthetic cathinones: Case report of non-fatal intoxication with AB-CHMINACA, AB-FUBINACA, alpha-PHP, alpha-PVP and 4-CMC.

PubMed

Klavž, Janez; Gorenjak, Maksimiljan; Marinšek, Martin

2016-08-01

We report on a case of intoxication with a mix of new psychoactive substances. A 38-year-old male was brought to the emergency department (ED) following the ingestion of an unknown drug in a suicide attempt. During the transport, he became progressively more somnolent and unresponsive to painful stimuli. Urine and stomach content were collected on admission to be screened for drugs of abuse and medicinal drugs. After admission, the patient's next of kin presented five small grip seal plastic bags containing different powders/crystals, and they were sent for analysis along with urine and stomach content to the toxicology laboratory. An easy and rapid sample preparation technique was applied for the extraction of urine and stomach content. Samples were extracted with liquid-liquid extraction (LLE) technique and analysed using gas chromatography-mass spectrometry (GC-MS). A small amount of powder material from the bags was diluted in methanol and injected directly into the GC-MS instrument. Obtained spectra (EI) were evaluated against SWGDRUG library. Five different designer drugs were identified in the powder material, including synthetic cannabinoids (AB-CHMINACA, AB-FUBINACA) and synthetic cathinones (alpha-PHP, alpha-PVP and 4-CMC). With the exception of 4-CMC, all of these substances were also detected in the stomach content along with the prescription drugs. This is the first time that a positive identification of these five drugs has been made by a clinical laboratory in Slovenia. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Occurrence of Campylobacter in commercially broken liquid egg in Japan.

PubMed

Sato, Miki; Sashihara, Nobuhiro

2010-03-01

Samples of unpasteurized liquid egg (whole egg, egg yolk, and egg white) and pasteurized liquid whole egg were collected from egg-breaking facilities in Japan and were tested for the presence of Campylobacter. Isolates recovered were tested for freeze-thaw response, sensitivity to antimicrobials, and heat resistance. Campylobacter was isolated from 27.9% of unpasteurized liquid whole egg samples and 36.0% of unpasteurized liquid egg yolk samples. No Campylobacter was isolated from unpasteurized liquid egg white or pasteurized liquid whole egg samples. The contamination levels of Campylobacter ranged from <3 to 240/100 ml. Freeze-thaw response was tested by freezing and thawing liquid whole egg and egg yolk to examine whether those conditions influenced the survival rate. It was shown that freezing and thawing reduced Campylobacter counts. Sensitivity to all antimicrobials used in this study was observed in 47.6% of the isolates. The most predominant antibiotic resistance profile was similar to that of isolates from chicken. D(55 degrees C)-values of 0.16 to 0.38 min and 0.47 to 0.84 min were determined for Campylobacter isolates in liquid whole egg and egg yolk, respectively. These values were lower than those reported for Salmonella. The very weak heat tolerance of Campylobacter indicated that it could be eliminated at the current legal pasteurization condition. There is no safety concern for commercially broken pasteurized liquid egg pertaining to Campylobacter contamination.

[Sample preparation and bioanalysis in mass spectrometry].

PubMed

Bourgogne, Emmanuel; Wagner, Michel

2015-01-01

The quantitative analysis of compounds of clinical interest of low molecular weight (<1000 Da) in biological fluids is currently in most cases performed by liquid chromatography-mass spectrometry (LC-MS). Analysis of these compounds in biological fluids (plasma, urine, saliva, hair...) is a difficult task requiring a sample preparation. Sample preparation is a crucial part of chemical/biological analysis and in a sense is considered the bottleneck of the whole analytical process. The main objectives of sample preparation are the removal of potential interferences, analyte preconcentration, and converting (if needed) the analyte into a more suitable form for detection or separation. Without chromatographic separation, endogenous compounds, co-eluted products may affect a quantitative method in mass spectrometry performance. This work focuses on three distinct parts. First, quantitative bioanalysis will be defined, different matrices and sample preparation techniques currently used in bioanalysis by mass spectrometry of/for small molecules of clinical interest in biological fluids. In a second step the goals of sample preparation will be described. Finally, in a third step, sample preparation strategies will be made either directly ("dilute and shoot") or after precipitation.

Extending the solvent-free MALDI sample preparation method.

PubMed

Hanton, Scott D; Parees, David M

2005-01-01

Matrix-assisted laser desorption/ionization (MALDI) mass spectrometry is an important technique to characterize many different materials, including synthetic polymers. MALDI mass spectral data can be used to determine the polymer average molecular weights, repeat units, and end groups. One of the key issues in traditional MALDI sample preparation is making good solutions of the analyte and the matrix. Solvent-free sample preparation methods have been developed to address these issues. Previous results of solvent-free or dry prepared samples show some advantages over traditional wet sample preparation methods. Although the results of the published solvent-free sample preparation methods produced excellent mass spectra, we found the method to be very time-consuming, with significant tool cleaning, which presents a significant possibility of cross contamination. To address these issues, we developed an extension of the solvent-free method that replaces the mortar and pestle grinding with ball milling the sample in a glass vial with two small steel balls. This new method generates mass spectra with equal quality of the previous methods, but has significant advantages in productivity, eliminates cross contamination, and is applicable to liquid and soft or waxy analytes.

Parameterizing Size Distribution in Ice Clouds

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

DeSlover, Daniel; Mitchell, David L.

2009-09-25

PARAMETERIZING SIZE DISTRIBUTIONS IN ICE CLOUDS David L. Mitchell and Daniel H. DeSlover ABSTRACT An outstanding problem that contributes considerable uncertainty to Global Climate Model (GCM) predictions of future climate is the characterization of ice particle sizes in cirrus clouds. Recent parameterizations of ice cloud effective diameter differ by a factor of three, which, for overcast conditions, often translate to changes in outgoing longwave radiation (OLR) of 55 W m-2 or more. Much of this uncertainty in cirrus particle sizes is related to the problem of ice particle shattering during in situ sampling of the ice particle size distribution (PSD).more » Ice particles often shatter into many smaller ice fragments upon collision with the rim of the probe inlet tube. These small ice artifacts are counted as real ice crystals, resulting in anomalously high concentrations of small ice crystals (D < 100 µm) and underestimates of the mean and effective size of the PSD. Half of the cirrus cloud optical depth calculated from these in situ measurements can be due to this shattering phenomenon. Another challenge is the determination of ice and liquid water amounts in mixed phase clouds. Mixed phase clouds in the Arctic contain mostly liquid water, and the presence of ice is important for determining their lifecycle. Colder high clouds between -20 and -36 oC may also be mixed phase but in this case their condensate is mostly ice with low levels of liquid water. Rather than affecting their lifecycle, the presence of liquid dramatically affects the cloud optical properties, which affects cloud-climate feedback processes in GCMs. This project has made advancements in solving both of these problems. Regarding the first problem, PSD in ice clouds are uncertain due to the inability to reliably measure the concentrations of the smallest crystals (D < 100 µm), known as the “small mode”. Rather than using in situ probe measurements aboard aircraft, we employed a treatment of ice cloud optical properties formulated in terms of PSD parameters in combination with remote measurements of thermal radiances to characterize the small mode. This is possible since the absorption efficiency (Qabs) of small mode crystals is larger at 12 µm wavelength relative to 11 µm wavelength due to the process of wave resonance or photon tunneling more active at 12 µm. This makes the 12/11 µm absorption optical depth ratio (or equivalently the 12/11 µm Qabs ratio) a means for detecting the relative concentration of small ice particles in cirrus. Using this principle, this project tested and developed PSD schemes that can help characterize cirrus clouds at each of the three ARM sites: SGP, NSA and TWP. This was the main effort of this project. These PSD schemes and ice sedimentation velocities predicted from them have been used to test the new cirrus microphysics parameterization in the GCM known as the Community Climate Systems Model (CCSM) as part of an ongoing collaboration with NCAR. Regarding the second problem, we developed and did preliminary testing on a passive thermal method for retrieving the total water path (TWP) of Arctic mixed phase clouds where TWPs are often in the range of 20 to 130 g m-2 (difficult for microwave radiometers to accurately measure). We also developed a new radar method for retrieving the cloud ice water content (IWC), which can be vertically integrated to yield the ice water path (IWP). These techniques were combined to determine the IWP and liquid water path (LWP) in Arctic clouds, and hence the fraction of ice and liquid water. We have tested this approach using a case study from the ARM field campaign called M-PACE (Mixed-Phase Arctic Cloud Experiment). This research led to a new satellite remote sensing method that appears promising for detecting low levels of liquid water in high clouds typically between -20 and -36 oC. We hope to develop this method in future research.« less

Do-It-Yourself Device for Recovery of Cryopreserved Samples Accidentally Dropped into Cryogenic Storage Tanks

PubMed Central

Mehta, Rohini; Baranova, Ancha; Birerdinc, Aybike

2012-01-01

Liquid nitrogen is colorless, odorless, extremely cold (-196 °C) liquid kept under pressure. It is commonly used as a cryogenic fluid for long term storage of biological materials such as blood, cells and tissues 1,2. The cryogenic nature of liquid nitrogen, while ideal for sample preservation, can cause rapid freezing of live tissues on contact - known as 'cryogenic burn'2, which may lead to severe frostbite in persons closely involved in storage and retrieval of samples from Dewars. Additionally, as liquid nitrogen evaporates it reduces the oxygen concentration in the air and might cause asphyxia, especially in confined spaces2. In laboratories, biological samples are often stored in cryovials or cryoboxes stacked in stainless steel racks within the Dewar tanks1. These storage racks are provided with a long shaft to prevent boxes from slipping out from the racks and into the bottom of Dewars during routine handling. All too often, however, boxes or vials with precious samples slip out and sink to the bottom of liquid nitrogen filled tank. In such cases, samples could be tediously retrieved after transferring the liquid nitrogen into a spare container or discarding it. The boxes and vials can then be relatively safely recovered from emptied Dewar. However, the cryogenic nature of liquid nitrogen and its expansion rate makes sunken sample retrieval hazardous. It is commonly recommended by Safety Offices that sample retrieval be never carried out by a single person. Another alternative is to use commercially available cool grabbers or tongs to pull out the vials3. However, limited visibility within the dark liquid filled Dewars poses a major limitation in their use. In this article, we describe the construction of a Cryotolerant DIY retrieval device, which makes sample retrieval from Dewar containing cryogenic fluids both safe and easy. PMID:22617806

Do-It-Yourself device for recovery of cryopreserved samples accidentally dropped into cryogenic storage tanks.

PubMed

Mehta, Rohini; Baranova, Ancha; Birerdinc, Aybike

2012-05-11

Liquid nitrogen is colorless, odorless, extremely cold (-196 °C) liquid kept under pressure. It is commonly used as a cryogenic fluid for long term storage of biological materials such as blood, cells and tissues (1,2). The cryogenic nature of liquid nitrogen, while ideal for sample preservation, can cause rapid freezing of live tissues on contact - known as 'cryogenic burn' (2), which may lead to severe frostbite in persons closely involved in storage and retrieval of samples from Dewars. Additionally, as liquid nitrogen evaporates it reduces the oxygen concentration in the air and might cause asphyxia, especially in confined spaces (2). In laboratories, biological samples are often stored in cryovials or cryoboxes stacked in stainless steel racks within the Dewar tanks (1). These storage racks are provided with a long shaft to prevent boxes from slipping out from the racks and into the bottom of Dewars during routine handling. All too often, however, boxes or vials with precious samples slip out and sink to the bottom of liquid nitrogen filled tank. In such cases, samples could be tediously retrieved after transferring the liquid nitrogen into a spare container or discarding it. The boxes and vials can then be relatively safely recovered from emptied Dewar. However, the cryogenic nature of liquid nitrogen and its expansion rate makes sunken sample retrieval hazardous. It is commonly recommended by Safety Offices that sample retrieval be never carried out by a single person. Another alternative is to use commercially available cool grabbers or tongs to pull out the vials (3). However, limited visibility within the dark liquid filled Dewars poses a major limitation in their use. In this article, we describe the construction of a Cryotolerant DIY retrieval device, which makes sample retrieval from Dewar containing cryogenic fluids both safe and easy.

Recent progress of task-specific ionic liquids in chiral resolution and extraction of biological samples and metal ions.

PubMed

Wu, Datong; Cai, Pengfei; Zhao, Xiaoyong; Kong, Yong; Pan, Yuanjiang

2018-01-01

Ionic liquids have been functionalized for modern applications. The functional ionic liquids are also called task-specific ionic liquids. Various task-specific ionic liquids with certain groups have been constructed and exploited widely in the field of separation. To take advantage of their properties in separation science, task-specific ionic liquids are generally used in techniques such as liquid-liquid extraction, solid-phase extraction, gas chromatography, high-performance liquid chromatography, and capillary electrophoresis. This review mainly covers original research papers published in the last five years, and we will focus on task-specific ionic liquids as the chiral selectors in chiral resolution and as extractant or sensor for biological samples and metal ion purification. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The distribution of saturated clusters in wetted granular materials

NASA Astrophysics Data System (ADS)

Li, Shuoqi; Hanaor, Dorian; Gan, Yixiang

2017-06-01

The hydro-mechanical behaviour of partially saturated granular materials is greatly influenced by the spatial and temporal distribution of liquid within the media. The aim of this paper is to characterise the distribution of saturated clusters in granular materials using an optical imaging method under different water drainage conditions. A saturated cluster is formed when a liquid phase fully occupies the pore space between solid grains in a localized region. The samples considered here were prepared by vibrating mono-sized glass beads to form closely packed assemblies in a rectangular container. A range of drainage conditions were applied to the specimen by tilting the container and employing different flow rates, and the liquid pressure was recorded at different positions in the experimental cell. The formation of saturated clusters during the liquid withdrawal processes is governed by three competing mechanisms arising from viscous, capillary, and gravitational forces. When the flow rate is sufficiently large and the gravity component is sufficiently small, the viscous force tends to destabilize the liquid front leading to the formation of narrow fingers of saturated material. As the water channels along these liquid fingers break, saturated clusters are formed inside the specimen. Subsequently, a spatial and temporal distribution of saturated clusters can be observed. We investigated the resulting saturated cluster distribution as a function of flow rate and gravity to achieve a fundamental understanding of the formation and evolution of such clusters in partially saturated granular materials. This study serves as a bridge between pore-scale behavior and the overall hydro-mechanical characteristics in partially saturated soils.

Finite-size radiation force correction for inviscid spheres in standing waves.

PubMed

Marston, Philip L

2017-09-01

Yosioka and Kawasima gave a widely used approximation for the acoustic radiation force on small liquid spheres surrounded by an immiscible liquid in 1955. Considering the liquids to be inviscid with negligible thermal dissipation, in their approximation the force on the sphere is proportional to the sphere's volume and the levitation position in a vertical standing wave becomes independent of the size. The analysis given here introduces a small correction term proportional to the square of the sphere's radius relative to the aforementioned small-sphere force. The significance of this term also depends on the relative density and sound velocity of the sphere. The improved approximation is supported by comparison with the exact partial-wave-series based radiation force for ideal fluid spheres in ideal fluids.

Quantitative determination of atmospheric hydroperoxyl radical

DOEpatents

Springston, Stephen R.; Lloyd, Judith; Zheng, Jun

2007-10-23

A method for the quantitative determination of atmospheric hydroperoxyl radical comprising: (a) contacting a liquid phase atmospheric sample with a chemiluminescent compound which luminesces on contact with hydroperoxyl radical; (b) determining luminescence intensity from the liquid phase atmospheric sample; and (c) comparing said luminescence intensity from the liquid phase atmospheric sample to a standard luminescence intensity for hydroperoxyl radical. An apparatus for automating the method is also included.

MEMS-based liquid lens for capsule endoscope

NASA Astrophysics Data System (ADS)

Seo, S. W.; Han, S.; Seo, J. H.; Kim, Y. M.; Kang, M. S.; Min, N. G.; Choi, W. B.; Sung, M. Y.

2008-03-01

The capsule endoscope, a new application area of digital imaging, is growing rapidly but needs the versatile imaging capabilities such as auto-focusing and zoom-in to be an active diagnostic tool. The liquid lens based on MEMS technology can be a strong candidate because it is able to be small enough. In this paper, a cylinder-type liquid lens was designed based on Young-Lippmann model and then fabricated with MEMS technology combining the silicon thin-film process and the wafer bonding process. The focal length of the lens module including the fabricated liquid lens was changed reproducibly as a function of the applied voltage. With the change of 30V in the applied bias, the focal length of the constructed lens module could be tuned in the range of about 42cm. The fabricated liquid lens was also proven to be small enough to be adopted in the capsule endoscope, which means the liquid lens can be utilized for the imaging capability improvement of the capsule endoscope.

Peculiar phase diagram with isolated superconducting regions in ThFeAsN1-x O x.

PubMed

Li, Bai-Zhuo; Wang, Zhi-Cheng; Wang, Jia-Lu; Zhang, Fu-Xiang; Wang, Dong-Ze; Zhang, Feng-Yuan; Sun, Yu-Ping; Jing, Qiang; Zhang, Hua-Fu; Tan, Shu-Gang; Li, Yu-Ke; Feng, Chun-Mu; Mei, Yu-Xue; Wang, Cao; Cao, Guang-Han

2018-06-27

ThFeAsN 1-x O x ([Formula: see text]) system with heavy electron doping has been studied by the measurements of x-ray diffraction, electrical resistivity, magnetic susceptibility and specific heat. The non-doped compound exhibits superconductivity at [Formula: see text] K, which is possibly due to an internal uniaxial chemical pressure that is manifested by the extremely small value of As height with respect to the Fe plane. With the oxygen substitution, the T c value decreases rapidly to below 2 K for [Formula: see text], and surprisingly, superconductivity re-appears in the range of [Formula: see text] with a maximum [Formula: see text] of 17.5 K at x  =  0.3. For the normal-state resistivity, while the samples in intermediate non-superconducting interval exhibit Fermi liquid behavior, those in other regions show a non-Fermi-liquid behavior. The specific heat jump for the superconducting sample of x  =  0.4 is [Formula: see text], which is discussed in terms of anisotropic superconducting gap. The peculiar phase diagram in ThFeAsN 1-x O x presents additional ingredients for understanding the superconducting mechanism in iron-based superconductors.

Acrylamide analysis in food by liquid chromatographic and gas chromatographic methods.

PubMed

Elbashir, Abdalla A; Omar, Mei M Ali; Ibrahim, Wan Aini Wan; Schmitz, Oliver J; Aboul-Enein, Hassan Y

2014-01-01

Acrylamide (AA) is a compound classified as carcinogenic to humans by the International Agency for Research on Cancer. It was first discovered to be present in certain heated processed food by the Swedish National Food Administration (SNFA) and University of Stockholm in early 2002. The major pathway for AA formation in food is the Maillard reaction between reducing sugar and the amino acid asparagine at high temperature. Since the discovery of AA's presence in food, many analytical methods have been developed for determination of AA contents in different food matrices. Also, several studies have been conducted to develop extraction procedures for AA from difficult food matrices. AA is a small, highly polar molecule, which makes its extraction and analysis challenging. Many articles and reviews have been published dealing with AA in food. The aim of the review is to discuss AA formation in food, the factors affecting AA formation and removal, AA exposure assessment, AA extraction and cleanup from food samples, and analytical methods used in AA determination, such as high-performance liquid chromatography (HPLC) and gas chromatography (GC). Special attention is given to sample extraction and cleanup procedures and analytical techniques used for AA determination.

Study of density distribution in a near-critical simple fluid (19-IML-1)

NASA Technical Reports Server (NTRS)

Michels, Teun

1992-01-01

This experiment uses visual observation, interferometry, and light scattering techniques to observe and analyze the density distribution in SF6 above and below the critical temperature. Below the critical temperature, the fluid system is split up into two coexisting phases, liquid and vapor. The spatial separation of these phases on earth, liquid below and vapor above, is not an intrinsic property of the fluid system; it is merely an effect of the action of the gravity field. At a fixed temperature, the density of each of the coexisting phases is in principle fixed. However, near T sub c where the fluid is strongly compressible, gravity induced hydrostatic forces will result in a gradual decrease in density with increasing height in the sample container. This hydrostatic density profile is even more pronounced in the one phase fluid at temperatures slightly above T sub c. The experiment is set up to study the intrinsic density distributions and equilibration rates of a critical sample in a small container. Interferometry will be used to determine local density and thickness of surface and interface layers. The light scattering data will reveal the size of the density fluctuations on a microscopic scale.