Direct Determination of ECD in ECD Kit: A Solid Sample Quantitation Method for Active Pharmaceutical Ingredient in Drug Product

PubMed Central

Chao, Ming-Yu; Liu, Kung-Tien; Hsia, Yi-Chih; Liao, Mei-Hsiu; Shen, Lie-Hang

2011-01-01

Technetium-99m ethyl cysteinate dimer (Tc-99m-ECD) is an essential imaging agent used in evaluating the regional cerebral blood flow in patients with cerebrovascular diseases. Determination of active pharmaceutical ingredient, that is, L-Cysteine, N, N′-1,2-ethanediylbis-, diethyl ester, dihydrochloride (ECD) in ECD Kit is a relevant requirement for the pharmaceutical quality control in processes of mass fabrication. We here presented a direct solid sample determination method of ECD in ECD Kit without sample dissolution to avoid the rapid degradation of ECD. An elemental analyzer equipped with a nondispersive infrared detector and a calibration curve of coal standard was used for the quantitation of sulfur in ECD Kit. No significant matrix effect was found. The peak area of coal standard against the amount of sulfur was linear over the range of 0.03–0.10 mg, with a correlation coefficient (r) of 0.9993. Method validation parameters were achieved to demonstrate the potential of this method. PMID:21687539

Hyphenation of Raman spectroscopy with gravimetric analysis to interrogate water-solid interactions in pharmaceutical systems.

PubMed

Gift, Alan D; Taylor, Lynne S

2007-01-04

A moisture sorption gravimetric analyzer has been combined with a Raman spectrometer to better understand the various modes of water-solid interactions relevant to pharmaceutical systems. A commercial automated moisture sorption balance was modified to allow non-contact monitoring of the sample properties by interfacing a Raman probe with the sample holder. This hybrid instrument allows for gravimetric and spectroscopic changes to be monitored simultaneously. The utility of this instrument was demonstrated by investigating different types of water-solid interactions including stoichiometric and non-stoichiometric hydrate formation, deliquescence, amorphous-crystalline transformation, and capillary condensation. In each of the model systems, sulfaguanidine, cromolyn sodium, ranitidine HCl, amorphous sucrose and silica gel, spectroscopic changes were observed during the time course of the moisture sorption profile. Analysis of spectroscopic data provided information about the origin of the observed changes in moisture content as a function of relative humidity. Furthermore, multivariate data analysis techniques were employed as a means of processing the spectroscopic data. Principle components analysis was found to be useful to aid in data processing, handling and interpretation of the spectral changes that occurred during the time course of the moisture sorption profile.

On the use of ultracentrifugal devices for routine sample preparation in biomolecular magic-angle-spinning NMR

PubMed Central

Mandal, Abhishek; Boatz, Jennifer C.; Wheeler, Travis; van der Wel, Patrick C. A.

2017-01-01

A number of recent advances in the field of magic-angle-spinning (MAS) solid-state NMR have enabled its application to a range of biological systems of ever increasing complexity. To retain biological relevance, these samples are increasingly studied in a hydrated state. At the same time, experimental feasibility requires the sample preparation process to attain a high sample concentration within the final MAS rotor. We discuss these considerations, and how they have led to a number of different approaches to MAS NMR sample preparation. We describe our experience of how custom-made (or commercially available) ultracentrifugal devices can facilitate a simple, fast and reliable sample preparation process. A number of groups have since adopted such tools, in some cases to prepare samples for sedimentation-style MAS NMR experiments. Here we argue for a more widespread adoption of their use for routine MAS NMR sample preparation. PMID:28229262

Effect of modulation of the particle size distributions in the direct solid analysis by total-reflection X-ray fluorescence

NASA Astrophysics Data System (ADS)

Fernández-Ruiz, Ramón; Friedrich K., E. Josue; Redrejo, M. J.

2018-02-01

The main goal of this work was to investigate, in a systematic way, the influence of the controlled modulation of the particle size distribution of a representative solid sample with respect to the more relevant analytical parameters of the Direct Solid Analysis (DSA) by Total-reflection X-Ray Fluorescence (TXRF) quantitative method. In particular, accuracy, uncertainty, linearity and detection limits were correlated with the main parameters of their size distributions for the following elements; Al, Si, P, S, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Rb, Sr, Ba and Pb. In all cases strong correlations were finded. The main conclusion of this work can be resumed as follows; the modulation of particles shape to lower average sizes next to a minimization of the width of particle size distributions, produce a strong increment of accuracy, minimization of uncertainties and limit of detections for DSA-TXRF methodology. These achievements allow the future use of the DSA-TXRF analytical methodology for development of ISO norms and standardized protocols for the direct analysis of solids by mean of TXRF.

Nanoscale effects in the characterization of viscoelastic materials with atomic force microscopy: coupling of a quasi-three-dimensional standard linear solid model with in-plane surface interactions.

PubMed

Solares, Santiago D

2016-01-01

Significant progress has been accomplished in the development of experimental contact-mode and dynamic-mode atomic force microscopy (AFM) methods designed to measure surface material properties. However, current methods are based on one-dimensional (1D) descriptions of the tip-sample interaction forces, thus neglecting the intricacies involved in the material behavior of complex samples (such as soft viscoelastic materials) as well as the differences in material response between the surface and the bulk. In order to begin to address this gap, a computational study is presented where the sample is simulated using an enhanced version of a recently introduced model that treats the surface as a collection of standard-linear-solid viscoelastic elements. The enhanced model introduces in-plane surface elastic forces that can be approximately related to a two-dimensional (2D) Young's modulus. Relevant cases are discussed for single- and multifrequency intermittent-contact AFM imaging, with focus on the calculated surface indentation profiles and tip-sample interaction force curves, as well as their implications with regards to experimental interpretation. A variety of phenomena are examined in detail, which highlight the need for further development of more physically accurate sample models that are specifically designed for AFM simulation. A multifrequency AFM simulation tool based on the above sample model is provided as supporting information.

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.

Recent Progress in Studies of Nanostructured Impurity Helium Solids

NASA Astrophysics Data System (ADS)

Khmelenko, V. V.; Kunttu, H.; Lee, D. M.

2007-07-01

Impurity helium (Im He) solids are porous materials formed inside superfluid 4He by nanoclusters of impurities injected from the gas phase. The results of studies of these materials have relevance to soft condensed matter physics, matrix isolation of free radicals and low temperature chemistry. Recent studies by a variety of experimental techniques, including CW and pulse ESR, X-ray diffraction, ultrasound and Raman spectroscopy allow a better characterization of the properties of Im He solids. The structure of Im He solids, the trapping sites of stabilized atoms and the possible energy content of the samples are analyzed on the basis of experimental data. The kinetics of exchange tunneling reactions of hydrogen isotopes in nanoclusters and the changes of environment of the atoms during the course of these reactions are reviewed. Analysis of the ESR data shows that very large fraction of the stabilized atoms in Im He solids reside on the surfaces of impurity nanoclusters. The future directions for studying Im He solids are described. Among the most attractive are the studies of Im He solids with high concentrations of stabilized atoms at ultralow (10 20 mK) temperature for the observation of new collective quantum phenomena, the studies of practical application of Im He solids as a medium in neutron moderator for efficient production of ultracold (˜1 mK) neutrons, and the possibilities of obtaining high concentration of atomic nitrogen embedded in N2 clusters for energy storage.

Direct Measurement of the Flip-Flop Rate of Electron Spins in the Solid State

NASA Astrophysics Data System (ADS)

Dikarov, Ekaterina; Zgadzai, Oleg; Artzi, Yaron; Blank, Aharon

2016-10-01

Electron spins in solids have a central role in many current and future spin-based devices, ranging from sensitive sensors to quantum computers. Many of these apparatuses rely on the formation of well-defined spin structures (e.g., a 2D array) with controlled and well-characterized spin-spin interactions. While being essential for device operation, these interactions can also result in undesirable effects, such as decoherence. Arguably, the most important pure quantum interaction that causes decoherence is known as the "flip-flop" process, where two interacting spins interchange their quantum state. Currently, for electron spins, the rate of this process can only be estimated theoretically, or measured indirectly, under limiting assumptions and approximations, via spin-relaxation data. This work experimentally demonstrates how the flip-flop rate can be directly and accurately measured by examining spin-diffusion processes in the solid state for physically fixed spins. Under such terms, diffusion can occur only through this flip-flop-mediated quantum-state exchange and not via actual spatial motion. Our approach is implemented on two types of samples, phosphorus-doped 28Si and nitrogen vacancies in diamond, both of which are significantly relevant to quantum sensors and information processing. However, while the results for the former sample are conclusive and reveal a flip-flop rate of approximately 12.3 Hz, for the latter sample only an upper limit of approximately 0.2 Hz for this rate can be estimated.

Investigation of IRGANOX®1076 as a dosimeter for clinical X-ray, electron and proton beams and its EPR angular response

NASA Astrophysics Data System (ADS)

Smith, Clare L.; Ankers, Elizabeth; Best, Stephen P.; Gagliardi, Frank; Katahira, Kai; Tsunei, Yseu; Tominaga, Takahiro; Geso, Moshi

2017-12-01

The suitability of IRGANOX®1076 in paraffin wax as a near-tissue equivalent radiation dosimeter was investigated for various radiotherapy beam types; kV and MV X-rays, electrons and protons over clinically-relevant doses (2 -20 Gy). The radical formed upon exposure to ionising radiations was measured by Electron Paramagnetic Resonance (EPR) spectroscopy, and the single peak signal obtained for solid solutions of IRGANOX®1076 in wax is attributed to the phenoxyl radical obtained by net loss of H•. Irradiation of solid IRGANOX®1076 gives a doublet consistent with the formation of the phenol cation radical, obtained by electron loss. Solid solutions of IRGANOX®1076 in paraffin wax give a linear dose response for all types of radiations examined, which was energy independent for MV, electron and proton beams, and energy-dependent for kV X-ray irradiation. Reliable dose measurements were obtained with exposures as low as 2 Gy, and comparisons with alanine wax-pellets containing the same amount of dosimeter material (w/w) gave similar responses for all beam types investigated. Post-irradiation measurements (up to 77 days for proton irradiation for samples stored in the dark and at room temperature) indicate good signal stability with minimal signal fading (between 1.6 to 3.8%). Relative to alanine dosimeters, solid solutions of IRGANOX®1076 in wax give EPR signals with better sensitivity at low dose and do not significantly change with the orientation of the sample. Solid solutions of IRGANOX®1076 are ideal for applications in radiotherapy dosimetry for X-rays and charged particles, as IRGANOX®1076 is relatively cheap, can easily and reproducibly prepared in wax and be moulded to different shapes.

Literature review relevant to particle erosion in complex geometries

NASA Astrophysics Data System (ADS)

Volent, Eirik; Dahlhaug, Ole Gunnar

2018-06-01

Erosion is a challenge in many industries where fluid is transferred through pipe and valve arrangements. Wear can occur in a variety of systems and is often related to the presents of droplets or solid particles in the fluid stream. Solid particles are in many cases present in hydropower systems, and can cause severe damage to system components. Flow conditions, particle size and concentration vary greatly and can thus cause a vast variety of damage, ranging from manageable wear to component failure. The following paper will present a summary of literature relevant to the prediction of erosion in complex geometries. The intention of the review is to investigate the current state of the art, directly relevant to the prediction of wear due to solid particle erosion in complex geometries.

Rotary bulk solids divider

DOEpatents

Maronde, Carl P.; Killmeyer, Jr., Richard P.

1992-01-01

An apparatus for the disbursement of a bulk solid sample comprising, a gravity hopper having a top open end and a bottom discharge end, a feeder positioned beneath the gravity hopper so as to receive a bulk solid sample flowing from the bottom discharge end, and a conveyor receiving the bulk solid sample from the feeder and rotating on an axis that allows the bulk solid sample to disperse the sample to a collection station.

ROTARY BULK SOLIDS DIVIDER

DOEpatents

Maronde, Carl P.; Killmeyer JR., Richard P.

1992-03-03

An apparatus for the disbursement of a bulk solid sample comprising, a gravity hopper having a top open end and a bottom discharge end, a feeder positioned beneath the gravity hopper so as to receive a bulk solid sample flowing from the bottom discharge end, and a conveyor receiving the bulk solid sample from the feeder and rotating on an axis that allows the bulk solid sample to disperse the sample to a collection station.

Nanoscale effects in the characterization of viscoelastic materials with atomic force microscopy: Coupling of a quasi-three-dimensional standard linear solid model with in-plane surface interactions

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

Solares, Santiago D.

Significant progress has been accomplished in the development of experimental contact-mode and dynamic-mode atomic force microscopy (AFM) methods designed to measure surface material properties. However, current methods are based on one-dimensional (1D) descriptions of the tip-sample interaction forces, thus neglecting the intricacies involved in the material behavior of complex samples (such as soft viscoelastic materials) as well as the differences in material response between the surface and the bulk. In order to begin to address this gap, a computational study is presented where the sample is simulated using an enhanced version of a recently introduced model that treats the surfacemore » as a collection of standard-linear-solid viscoelastic elements. The enhanced model introduces in-plane surface elastic forces that can be approximately related to a two-dimensional (2D) Young's modulus. Relevant cases are discussed for single-and multifrequency intermittent-contact AFM imaging, with focus on the calculated surface indentation profiles and tip-sample interaction force curves, as well as their implications with regards to experimental interpretation. A variety of phenomena are examined in detail, which highlight the need for further development of more physically accurate sample models that are specifically designed for AFM simulation. As a result, a multifrequency AFM simulation tool based on the above sample model is provided as supporting information.« less

Pressurized liquid extraction using water/isopropanol coupled with solid-phase extraction cleanup for industrial and anthropogenic waste-indicator compounds in sediment

USGS Publications Warehouse

Burkhardt, M.R.; ReVello, R.C.; Smith, S.G.; Zaugg, S.D.

2005-01-01

A broad range of organic compounds is recognized as environmentally relevant for their potential adverse effects on human and ecosystem health. This method was developed to better determine the distribution of 61 compounds that are typically associated with industrial and household waste as well as some that are toxic and known (or suspected) for endocrine-disrupting potential extracted from environmental sediment samples. Pressurized liquid extraction (PLE) coupled with solid-phase extraction (SPE) was used to reduce sample preparation time, reduce solvent consumption to one-fifth of that required using dichloromethane-based Soxhlet extraction, and to minimize background interferences for full scan GC/MS analysis. Recoveries from spiked Ottawa sand, commercially available topsoil, and environmental stream sediment, fortified at 4-720 ??g per compound, averaged 76 ?? 13%. Initial method detection limits for single-component compounds ranged from 12.5 to 520 ??g/kg, based on 25 g samples. Results from 103 environmental sediment samples show that 36 out of 61 compounds (59%) were detected in at least one sample with concentrations ranging from 20 to 100,000 ??g/kg. The most frequently detected compound, beta-sitosterol, a plant sterol, was detected in 87 of the 103 (84.5%) environmental samples with a concentration range 360-100,000 ??g/kg. Results for a standard reference material using dichloromethane Soxhlet-based extraction are also compared. ?? 2004 Published by Elsevier B.V.

Nanoscale effects in the characterization of viscoelastic materials with atomic force microscopy: Coupling of a quasi-three-dimensional standard linear solid model with in-plane surface interactions

DOE PAGES

Solares, Santiago D.

2016-04-15

Significant progress has been accomplished in the development of experimental contact-mode and dynamic-mode atomic force microscopy (AFM) methods designed to measure surface material properties. However, current methods are based on one-dimensional (1D) descriptions of the tip-sample interaction forces, thus neglecting the intricacies involved in the material behavior of complex samples (such as soft viscoelastic materials) as well as the differences in material response between the surface and the bulk. In order to begin to address this gap, a computational study is presented where the sample is simulated using an enhanced version of a recently introduced model that treats the surfacemore » as a collection of standard-linear-solid viscoelastic elements. The enhanced model introduces in-plane surface elastic forces that can be approximately related to a two-dimensional (2D) Young's modulus. Relevant cases are discussed for single-and multifrequency intermittent-contact AFM imaging, with focus on the calculated surface indentation profiles and tip-sample interaction force curves, as well as their implications with regards to experimental interpretation. A variety of phenomena are examined in detail, which highlight the need for further development of more physically accurate sample models that are specifically designed for AFM simulation. As a result, a multifrequency AFM simulation tool based on the above sample model is provided as supporting information.« less

Analytical techniques for retrieval of atmospheric composition with the quadrupole mass spectrometer of the Sample Analysis at Mars instrument suite on Mars Science Laboratory

NASA Astrophysics Data System (ADS)

B. Franz, Heather; G. Trainer, Melissa; H. Wong, Michael; L. K. Manning, Heidi; C. Stern, Jennifer; R. Mahaffy, Paul; K. Atreya, Sushil; Benna, Mehdi; G. Conrad, Pamela; N. Harpold, Dan; A. Leshin, Laurie; A. Malespin, Charles; P. McKay, Christopher; Thomas Nolan, J.; Raaen, Eric

2014-06-01

The Sample Analysis at Mars (SAM) instrument suite is the largest scientific payload on the Mars Science Laboratory (MSL) Curiosity rover, which landed in Mars' Gale Crater in August 2012. As a miniature geochemical laboratory, SAM is well-equipped to address multiple aspects of MSL's primary science goal, characterizing the potential past or present habitability of Gale Crater. Atmospheric measurements support this goal through compositional investigations relevant to martian climate evolution. SAM instruments include a quadrupole mass spectrometer, a tunable laser spectrometer, and a gas chromatograph that are used to analyze martian atmospheric gases as well as volatiles released by pyrolysis of solid surface materials (Mahaffy et al., 2012). This report presents analytical methods for retrieving the chemical and isotopic composition of Mars' atmosphere from measurements obtained with SAM's quadrupole mass spectrometer. It provides empirical calibration constants for computing volume mixing ratios of the most abundant atmospheric species and analytical functions to correct for instrument artifacts and to characterize measurement uncertainties. Finally, we discuss differences in volume mixing ratios of the martian atmosphere as determined by SAM (Mahaffy et al., 2013) and Viking (Owen et al., 1977; Oyama and Berdahl, 1977) from an analytical perspective. Although the focus of this paper is atmospheric observations, much of the material concerning corrections for instrumental effects also applies to reduction of data acquired with SAM from analysis of solid samples. The Sample Analysis at Mars (SAM) instrument measures the composition of the martian atmosphere. Rigorous calibration of SAM's mass spectrometer was performed with relevant gas mixtures. Calibration included derivation of a new model to correct for electron multiplier effects. Volume mixing ratios for Ar and N2 obtained with SAM differ from those obtained with Viking. Differences between SAM and Viking volume mixing ratios are under investigation.

Storage potential and residual emissions from fresh and stabilized waste samples from a landfill simulation experiment.

PubMed

Morello, Luca; Raga, Roberto; Sgarbossa, Paolo; Rosson, Egle; Cossu, Raffaello

2018-05-01

The storage capacity and the potentially residual emissions of a stabilized waste coming from a landfill simulation experiment were evaluated. The evolution in time of the potential emissions and the mobility of some selected elements or compounds were determined, comparing the results of the stabilized waste samples with the values detected in the related fresh waste samples. Analyses were conducted for the total bulk waste and also for each identified category (under-sieve, kitchen residues, green and wooden materials, plastics, cellulosic material and textiles) to highlight the contribution of the different waste fractions in the total emission potential. The waste characterization was performed through analyses on solids and on leaching test eluates; the chemical speciation of carbon, nitrogen, chlorine and sulfur together with the partitioning of heavy metals through a SCE procedure were carried out. Results showed that the under-sieve is the most environmentally relevant fraction, hosting a consistent part of mobile compounds in fresh waste (40.7% of carbon, 44.0% of nitrogen, 47.6% of chloride and 40.0% of sulfur) and the greater part of potentially residual emissions in stabilized waste (88.4% of carbon, 90.9% of nitrogen, 98.4% of chloride and 91.1% of sulfur). Landfilled Municipal Solid Waste (MSW) proved to be an effective sink, finally storing more than 55% of carbon, 53% of nitrogen, 33% of sulfur and 90% of heavy metals (HM) which were initially present in fresh waste samples. A general decrease in leachable fractions from fresh to stabilized waste was observed for each category. Tests showed that solid waste is not a good sink for chlorine, whose residual non-mobile fraction amounts to 12.3% only. Copyright © 2018 Elsevier Ltd. All rights reserved.

Dynamic fractionation of trace metals in soil and sediment samples using rotating coiled column extraction and sequential injection microcolumn extraction: a comparative study.

PubMed

Rosende, Maria; Savonina, Elena Yu; Fedotov, Petr S; Miró, Manuel; Cerdà, Víctor; Wennrich, Rainer

2009-09-15

Dynamic fractionation has been recognized as an appealing alternative to conventional equilibrium-based sequential extraction procedures (SEPs) for partitioning of trace elements (TE) in environmental solid samples. This paper reports the first attempt for harmonization of flow-through dynamic fractionation using two novel methods, the so-called sequential injection microcolumn (SIMC) extraction and rotating coiled column (RCC) extraction. In SIMC extraction, a column packed with the solid sample is clustered in a sequential injection system, while in RCC, the particulate matter is retained under the action of centrifugal forces. In both methods, the leachants are continuously pumped through the solid substrates by the use of either peristaltic or syringe pumps. A five-step SEP was selected for partitioning of Cu, Pb and Zn in water soluble/exchangeable, acid-soluble, easily reducible, easily oxidizable and moderately reducible fractions from 0.2 to 0.5 g samples at an extractant flow rate of 1.0 mL min(-1) prior to leachate analysis by inductively coupled plasma-atomic emission spectrometry. Similarities and discrepancies between both dynamic approaches were ascertained by fractionation of TE in certified reference materials, namely, SRM 2711 Montana Soil and GBW 07311 sediment, and two real soil samples as well. Notwithstanding the different extraction conditions set by both methods, similar trends of metal distribution were in generally found. The most critical parameters for reliable assessment of mobilizable pools of TE in worse-case scenarios are the size-distribution of sample particles, the density of particles, the content of organic matter and the concentration of major elements. For reference materials and a soil rich in organic matter, the extraction in RCC results in slightly higher recoveries of environmentally relevant fractions of TE, whereas SIMC leaching is more effective for calcareous soils.

Pressurized liquid extraction using water/isopropanol coupled with solid-phase extraction cleanup for semivolatile organic compounds, polycyclic aromatic hydrocarbons (PAH), and alkylated PAH homolog groups in sediment

USGS Publications Warehouse

Burkhardt, M.R.; Zaugg, S.D.; Burbank, T.L.; Olson, M.C.; Iverson, J.L.

2005-01-01

Polycyclic aromatic hydrocarbons (PAH) are recognized as environmentally relevant for their potential adverse effects on human and ecosystem health. This paper describes a method to determine the distribution of PAH and alkylated homolog groups in sediment samples. Pressurized liquid extraction (PLE), coupled with solid-phase extraction (SPE) cleanup, was developed to decrease sample preparation time, to reduce solvent consumption, and to minimize background interferences for full-scan GC-MS analysis. Recoveries from spiked Ottawa sand, environmental stream sediment, and commercially available topsoil, fortified at 1.5-15 ??g per compound, averaged 94.6 ?? 7.8%, 90.7 ?? 5.8% and 92.8 ?? 12.8%, respectively. Initial method detection limits for single-component compounds ranged from 20 to 302 ??g/kg, based on 25 g samples. Results from 28 environmental sediment samples, excluding homologs, show 35 of 41 compounds (85.4%) were detected in at least one sample with concentrations ranging from 20 to 100,000 ??g/kg. The most frequently detected compound, 2,6-dimethylnaphthalene, was detected in 23 of the 28 (82%) environmental samples with a concentration ranging from 15 to 907 ??g/kg. The results from the 28 environmental sediment samples for the homolog series showed that 27 of 28 (96%) samples had at least one homolog series present at concentrations ranging from 20 to 89,000 ??g/kg. The most frequently detected homolog series, C2-alkylated naphthalene, was detected in 26 of the 28 (93%) environmental samples with a concentration ranging from 25 to 3900 ??g/kg. Results for a standard reference material using dichloromethane Soxhlet-based extraction also are compared. ?? 2005 Elsevier B.V. All rights reserved.

Development of a New Microextraction Fiber Combined to On-Line Sample Stacking Capillary Electrophoresis UV Detection for Acidic Drugs Determination in Real Water Samples.

PubMed

Espina-Benitez, Maria; Araujo, Lilia; Prieto, Avismelsi; Navalón, Alberto; Vílchez, José Luis; Valera, Paola; Zambrano, Ana; Dugas, Vincent

2017-07-07

A new analytical method coupling a (off-line) solid-phase microextraction with an on-line capillary electrophoresis (CE) sample enrichment technique was developed for the analysis of ketoprofen, naproxen and clofibric acid from water samples, which are known as contaminants of emerging concern in aquatic environments. New solid-phase microextraction fibers based on physical coupling of chromatographic supports onto epoxy glue coated needle were studied for the off-line preconcentration of these micropollutants. Identification and quantification of such acidic drugs were done by capillary zone electrophoresis (CZE) using ultraviolet diode array detection (DAD). Further enhancement of concentration sensitivity detection was achieved by on-line CE "acetonitrile stacking" preconcentration technique. Among the eight chromatographic supports investigated, Porapak Q sorbent showed higher extraction and preconcentration capacities. The screening of parameters that influence the microextraction process was carried out using a two-level fractional factorial. Optimization of the most relevant parameters was then done through a surface response three-factor Box-Behnken design. The limits of detection and limits of quantification for the three drugs ranged between 0.96 and 1.27 µg∙L -1 and 2.91 and 3.86 µg∙L -1 , respectively. Recovery yields of approximately 95 to 104% were measured. The developed method is simple, precise, accurate, and allows quantification of residues of these micropollutants in Genil River water samples using inexpensive fibers.

Development of a New Microextraction Fiber Combined to On-Line Sample Stacking Capillary Electrophoresis UV Detection for Acidic Drugs Determination in Real Water Samples

PubMed Central

Araujo, Lilia; Prieto, Avismelsi; Navalón, Alberto; Vílchez, José Luis; Valera, Paola; Zambrano, Ana; Dugas, Vincent

2017-01-01

A new analytical method coupling a (off-line) solid-phase microextraction with an on-line capillary electrophoresis (CE) sample enrichment technique was developed for the analysis of ketoprofen, naproxen and clofibric acid from water samples, which are known as contaminants of emerging concern in aquatic environments. New solid-phase microextraction fibers based on physical coupling of chromatographic supports onto epoxy glue coated needle were studied for the off-line preconcentration of these micropollutants. Identification and quantification of such acidic drugs were done by capillary zone electrophoresis (CZE) using ultraviolet diode array detection (DAD). Further enhancement of concentration sensitivity detection was achieved by on-line CE “acetonitrile stacking” preconcentration technique. Among the eight chromatographic supports investigated, Porapak Q sorbent showed higher extraction and preconcentration capacities. The screening of parameters that influence the microextraction process was carried out using a two-level fractional factorial. Optimization of the most relevant parameters was then done through a surface response three-factor Box-Behnken design. The limits of detection and limits of quantification for the three drugs ranged between 0.96 and 1.27 µg∙L−1 and 2.91 and 3.86 µg∙L−1, respectively. Recovery yields of approximately 95 to 104% were measured. The developed method is simple, precise, accurate, and allows quantification of residues of these micropollutants in Genil River water samples using inexpensive fibers. PMID:28686186

Thermal Regeneration of Sulfuric Acid Hydrates after Irradiation

NASA Technical Reports Server (NTRS)

Loeffler, Mark J.; Hudson, Reggie L.

2012-01-01

In an attempt to more completely understand the surface chemistry of the jovian icy satellites, we have investigated the effect of heating on two irradiated crystalline sulfuric acid hydrates, H2SO4 4H2O and H2SO4 H2O. At temperatures relevant to Europa and the warmer jovian satellites, post-irradiation heating recrystallized the amorphized samples and increased the intensities of the remaining hydrate's infrared absorptions. This thermal regeneration of the original hydrates was nearly 100% efficient, indicating that over geological times, thermally-induced phase transitions enhanced by temperature fluctuations will reform a large fraction of crystalline hydrated sulfuric acid that is destroyed by radiation processing. The work described is the first demonstration of the competition between radiation-induced amorphization and thermally-induced recrystallization in icy ionic solids relevant to the outer Solar System.

Distribution of pyrethroid insecticides in secondary wastewater effluent

PubMed Central

Parry, Emily; Young, Thomas M.

2014-01-01

Although the freely dissolved form of hydrophobic organic chemicals may best predict aquatic toxicity, differentiating between dissolved and particle bound forms is challenging at environmentally relevant concentrations for compounds with low toxicity thresholds such as pyrethroid insecticides. We investigated the distribution of pyrethroids among three forms: freely dissolved, complexed with dissolved organic carbon (DOC), and sorbed to suspended particulate matter, during a yearlong study at a secondary wastewater treatment plant. Effluent was fractionated by laboratory centrifugation to determine if sorption was driven by particle size. Linear distribution coefficients were estimated for pyrethroid sorption to suspended particulate matter (Kid) and dissolved organic carbon (Kidoc) at environmentally relevant pyrethroid concentrations. Resulting Kid values were higher than those reported for other environmental solids, and variation between sampling events correlated well with available particle surface area. Fractionation results suggest that no more than 40% of the pyrethroid remaining in secondary effluent could be removed by extending settling periods. Less than 6%of the total pyrethroid load in wastewater effluent was present in the dissolved form across all sampling events and chemicals. PMID:23939863

Dynamic X-ray diffraction observation of shocked solid iron up to 170 GPa

PubMed Central

Denoeud, Adrien; Ozaki, Norimasa; Benuzzi-Mounaix, Alessandra; Uranishi, Hiroyuki; Kondo, Yoshihiko; Kodama, Ryosuke; Brambrink, Erik; Ravasio, Alessandra; Bocoum, Maimouna; Boudenne, Jean-Michel; Harmand, Marion; Guyot, François; Mazevet, Stephane; Riley, David; Makita, Mikako; Sano, Takayoshi; Sakawa, Youichi; Inubushi, Yuichi; Gregori, Gianluca; Koenig, Michel; Morard, Guillaume

2016-01-01

Investigation of the iron phase diagram under high pressure and temperature is crucial for the determination of the composition of the cores of rocky planets and for better understanding the generation of planetary magnetic fields. Here we present X-ray diffraction results from laser-driven shock-compressed single-crystal and polycrystalline iron, indicating the presence of solid hexagonal close-packed iron up to pressure of at least 170 GPa along the principal Hugoniot, corresponding to a temperature of 4,150 K. This is confirmed by the agreement between the pressure obtained from the measurement of the iron volume in the sample and the inferred shock strength from velocimetry deductions. Results presented in this study are of the first importance regarding pure Fe phase diagram probed under dynamic compression and can be applied to study conditions that are relevant to Earth and super-Earth cores. PMID:27357672

Enhancing Entropy and Enthalpy Fluctuations to Drive Crystallization in Atomistic Simulations.

PubMed

Piaggi, Pablo M; Valsson, Omar; Parrinello, Michele

2017-07-07

Crystallization is a process of great practical relevance in which rare but crucial fluctuations lead to the formation of a solid phase starting from the liquid. As in all first order first transitions, there is an interplay between enthalpy and entropy. Based on this idea, in order to drive crystallization in molecular simulations, we introduce two collective variables, one enthalpic and the other entropic. Defined in this way, these collective variables do not prejudge the structure into which the system is going to crystallize. We show the usefulness of this approach by studying the cases of sodium and aluminum that crystallize in the bcc and fcc crystalline structures, respectively. Using these two generic collective variables, we perform variationally enhanced sampling and well tempered metadynamics simulations and find that the systems transform spontaneously and reversibly between the liquid and the solid phases.

The effect of interlayer anion on the reactivity of Mg-Al layered double hydroxides: improving and extending the customization capacity of anionic clays.

PubMed

Rojas, Ricardo; Bruna, Felipe; de Pauli, Carlos P; Ulibarri, M Ángeles; Giacomelli, Carla E

2011-07-01

Layered double hydroxides (LDHs) reactivity and interfacial behavior are closely interconnected and control particle properties relevant to the wide range of these solids' applications. Despite their importance, their relationship has been hardly described. In this work, chloride and dodecylsulfate (DDS(-)) intercalated LDHs are studied combining experimental data (electrophoretic mobility and contact angle measurements, hydroxyl and organic compounds uptake) and a simple mathematical model that includes anion-binding and acid-base reactions. This approach evidences the anion effect on LDHs interfacial behavior, reflected in the opposite particle charge and the different surface hydrophobic/hydrophilic character. LDHs reactivity are also determined by the interlayer composition, as demonstrated by the cation uptake capability of the DDS(-) intercalated sample. Consequently, the interlayer anion modifies the LDHs interfacial properties and reactivity, which in turn extends the customization capacity of these solids. Copyright © 2011 Elsevier Inc. All rights reserved.

Analysis of chemical contamination within a canal in a Mexican border colonia.

PubMed

Owens, Janel E; Niemeyer, Emily D

2006-04-01

This study examines urban pollution within Derechos Humanos, a colonia popular in Matamoros, Tamaulipas, Mexico. General water quality indicators (coliform bacteria, total dissolved solids, ecologically relevant cations and anions), heavy metals (copper, lead, nickel, zinc, iron and cadmium), and volatile organic compounds (benzene, toluene, ethylbenzene, styrene, and dichlorobenzene and xylene isomers) were quantified within a wastewater canal running adjacent to the community. Water samples were collected at multiple sites along the banks of the canal and evidence of anthropogenic emissions existed at each sampling location. Sample site 2, approximately 10 m upstream of the colonia, contained both the widest range of hazardous pollutants and the greatest number exceeding US Environmental Protection Agency surface water standards. At each sampling location, high concentrations of total coliform (> 10(4) colonies/100 mL sample), lead (ranging from 0.05 to 0.40 mg/L), nickel (levels from 0.21 to 1.45 mg/L), and benzene (up to 9.80 mg/L) were noted.

High pressure gas spheres for neutron and photon experiments

NASA Astrophysics Data System (ADS)

Rupp, G.; Petrich, D.; Käppeler, F.; Kaltenbaek, J.; Leugers, B.; Reifarth, R.

2009-09-01

High pressure gas spheres have been designed and successfully used in several nuclear physics experiments on noble gases. The pros and cons of this solution are the simple design and the high reliability versus the fact that the density is limited to 40-60% of liquid or solid gas samples. Originally produced for neutron capture studies at keV energies, the comparably small mass of the gas spheres were an important advantage, which turned out to be of relevance for other applications as well. The construction, performance, and operation of the spheres are described and examples for their use are presented.

DWPF DECON FRIT: SUMP AND SLURRY SOLIDS ANALYSIS

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

Crawford, C.; Peeler, D.; Click, D.

The Savannah River National Laboratory (SRNL) has been requested to perform analyses on samples of the Defense Waste Processing Facility (DWPF) decon frit slurry (i.e., supernate samples and sump solid samples). Four 1-L liquid slurry samples were provided to SRNL by Savannah River Remediation (SRR) from the 'front-end' decon activities. Additionally, two 1-L sump solids samples were provided to SRNL for compositional and physical analysis. In this report, the physical and chemical characterization results of the slurry solids and sump solids are reported. Crawford et al. (2010) provide the results of the supernate analysis. The results of the sump solidsmore » are reported on a mass basis given the samples were essentially dry upon receipt. The results of the slurry solids were converted to a volume basis given approximately 2.4 grams of slurry solids were obtained from the {approx}4 liters of liquid slurry sample. Although there were slight differences in the analytical results between the sump solids and slurry solids the following general summary statements can be made. Slight differences in the results are also captured for specific analysis. (1) Physical characterization - (a) SEM/EDS analysis suggested that the samples were enriched in Li and Si (B and Na not detectable using the current EDS system) which is consistent with two of the four principle oxides of Frit 418 (B{sub 2}O{sub 3}, Na{sub 2}O, Li{sub 2}O and SiO{sub 2}). (b) SEM/EDS analysis also identified impurities which were elementally consistent with stainless steel (i.e., Fe, Ni, Cr contamination). (c) XRD results indicated that the sump solids samples were amorphous which is consistent with XRD results expected for a Frit 418 based sample. (d) For the sump solids, SEM/EDS analysis indicated that the particle size of the sump solids were consistent with that of an as received Frit 418 sample from a current DWPF vendor. (e) For the slurry solids, SEM/EDS analysis indicated that the particle size range of the slurry solids was much broader than compared to the sump solids. More specifically, there were significantly more fines in the slurry solids as compared to the sump solids. (f) PSD results indicated that > 99% of both the sump and slurry solids were less than 350 microns. The PSD results also supported SEM/EDS analysis that there were significantly more fines in the slurry solids as compared to the sump solids. (2) Weight Percent Solids - Based on the measured supernate density and mass of insoluble solids (2.388 grams) filtered from the four liters of liquid slurry samples, the weight percent insoluble solids was estimated to be 0.060 wt%. This level of insoluble solids is higher than the ETP WAC limit of 100 mg/L, or 0.01 wt% which suggests a separation technology of some type would be required. (3) Chemical Analysis - (a) Elemental results from ICP-ES analysis indicated that the sump solids and slurry were very consistent with the nominal composition of Frit 418. There were other elements identified by ICP analysis which were either consistent with the presence of stainless steel (as identified by SEM/EDS analysis) or impurities that have been observed in 'as received' Frit 418 from the vendor. (b) IC anion analysis of the sump solids and slurry solids indicated all of the species were less than detection limits. (c) Radionuclide analysis of the sump solids also indicated that most of the analytes were either at or below the detection limits. (d) Organic analysis of the sump solids and slurry solids indicated all of the species were less than detection limits. It should be noted that the results of this study may not be representative of future decon frit solutions or sump/slurry solids samples. Therefore, future DWPF decisions regarding the possible disposal pathways for either the aqueous or solid portions of the Decon Frit system need to factor in the potential differences. More specifically, introduction of a different frit or changes to other DWPF flowsheet unit operations (e.g., different sludge batch or coupling with other process streams) may impact not only the results but also the conclusions regarding acceptability with respect to the ETF WAC limits or other alternative disposal options.« less

Vibrational Action Spectroscopy of Solids: New Surface-Sensitive Technique

NASA Astrophysics Data System (ADS)

Wu, Zongfang; Płucienik, Agata; Feiten, Felix E.; Naschitzki, Matthias; Wachsmann, Walter; Gewinner, Sandy; Schöllkopf, Wieland; Staemmler, Volker; Kuhlenbeck, Helmut; Freund, Hans-Joachim

2017-09-01

Vibrational action spectroscopy employing infrared radiation from a free-electron laser has been successfully used for many years to study the vibrational and structural properties of gas phase aggregates. Despite the high sensitivity of this method no relevant studies have yet been conducted for solid sample surfaces. We have set up an experiment for the application of this method to such targets, using infrared light from the free-electron laser of the Fritz Haber Institute. In this Letter, we present first results of this technique with adsorbed argon and neon atoms as messengers. We were able to detect surface-located vibrations of a thin V2O3(0 0 0 1 ) film on Au(111) as well as adsorbate vibrations, demonstrating that this method is highly surface sensitive. We consider that the dominant channel for desorption of the messenger atoms is direct inharmonic vibrational coupling, which is essentially insensitive to subsurface or bulk vibrations. Another channel is thermal desorption due to sample heating by absorption of infrared light. The high surface sensitivity of the nonthermal channel and its insensitivity to subsurface modes makes this technique an ideal tool for the study of surface-located vibrations.

Vibrational Action Spectroscopy of Solids: New Surface-Sensitive Technique.

PubMed

Wu, Zongfang; Płucienik, Agata; Feiten, Felix E; Naschitzki, Matthias; Wachsmann, Walter; Gewinner, Sandy; Schöllkopf, Wieland; Staemmler, Volker; Kuhlenbeck, Helmut; Freund, Hans-Joachim

2017-09-29

Vibrational action spectroscopy employing infrared radiation from a free-electron laser has been successfully used for many years to study the vibrational and structural properties of gas phase aggregates. Despite the high sensitivity of this method no relevant studies have yet been conducted for solid sample surfaces. We have set up an experiment for the application of this method to such targets, using infrared light from the free-electron laser of the Fritz Haber Institute. In this Letter, we present first results of this technique with adsorbed argon and neon atoms as messengers. We were able to detect surface-located vibrations of a thin V_{2}O_{3}(0001) film on Au(111) as well as adsorbate vibrations, demonstrating that this method is highly surface sensitive. We consider that the dominant channel for desorption of the messenger atoms is direct inharmonic vibrational coupling, which is essentially insensitive to subsurface or bulk vibrations. Another channel is thermal desorption due to sample heating by absorption of infrared light. The high surface sensitivity of the nonthermal channel and its insensitivity to subsurface modes makes this technique an ideal tool for the study of surface-located vibrations.

Lipidomic fingerprint of almonds (Prunus dulcis L. cv Nonpareil) using TiO₂ nanoparticle based matrix solid-phase dispersion and MALDI-TOF/MS and its potential in geographical origin verification.

PubMed

Shen, Qing; Dong, Wei; Yang, Mei; Li, Linqiu; Cheung, Hon-Yeung; Zhang, Zhifeng

2013-08-14

A matrix solid-phase dispersion (MSPD) procedure with titanium dioxide (TiO2) nanoparticles (NP) as sorbent was developed for the selective extraction of phospholipids from almond samples, and matrix-assisted laser desorption ionization-time-of-flight mass spectrometry (MALDI-TOF/MS) was employed for analysis. A remarkable increase in the signals of phospholipid accompanied by a decrease in those of triacylglycerols and diacylglycerols was observed in the relevant mass spectra. The proposed method was applied to five batches of almonds originating from four geographical areas, whereas principal component analysis (PCA) was utilized to normalize the relative amounts of the identified phospholipid species. The results indicated that the lipidomic fingerprint of almonds was successfully established by the negative ion mode spectrum, and the ratio of m/z 833.6 to 835.6 as well as m/z 821.6 could be introduced as potential markers for the differentiation of the tested almonds with different geographical origins. The whole method is of great promise for selective separation of phospholipids from nonphospholipids, especially the glycerides, and superior in fast screening and characterization of phospholipids in almond samples.

Analytical strategies for organic food packaging contaminants.

PubMed

Sanchis, Yovana; Yusà, Vicent; Coscollà, Clara

2017-03-24

In this review, we present current approaches in the analysis of food-packaging contaminants. Gas and liquid chromatography coupled to mass spectrometry detection have been widely used in the analysis of some relevant families of these compounds such as primary aromatic amines, bisphenol A, bisphenol A diglycidyl ether and related compounds, UV-ink photoinitiators, perfluorinated compounds, phthalates and non-intentionally added substances. Main applications for sample treatment and different types of food-contact material migration studies have been also discussed. Pressurized Liquid Extraction, Solid-Phase Microextraction, Focused Ultrasound Solid-Liquid Extraction and Quechers have been mainly used in the extraction of food contact material (FCM) contaminants, due to the trend of minimising solvent consumption, automatization of sample preparation and integration of extraction and clean-up steps. Recent advances in analytical methodologies have allowed unequivocal identification and confirmation of these contaminants using Liquid Chromatography coupled to High Resolution Mass Spectrometry (LC-HRMS) through mass accuracy and isotopic pattern applying. LC-HRMS has been used in the target analysis of primary aromatic amines in different plastic materials, but few studies have been carried out applying this technique in post-target and non-target analysis of FCM contaminants. Copyright © 2017 Elsevier B.V. All rights reserved.

Multiscale dispersion-state characterization of nanocomposites using optical coherence tomography

PubMed Central

Schneider, Simon; Eppler, Florian; Weber, Marco; Olowojoba, Ganiu; Weiss, Patrick; Hübner, Christof; Mikonsaari, Irma; Freude, Wolfgang; Koos, Christian

2016-01-01

Nanocomposite materials represent a success story of nanotechnology. However, development of nanomaterial fabrication still suffers from the lack of adequate analysis tools. In particular, achieving and maintaining well-dispersed particle distributions is a key challenge, both in material development and industrial production. Conventional methods like optical or electron microscopy need laborious, costly sample preparation and do not permit fast extraction of nanoscale structural information from statistically relevant sample volumes. Here we show that optical coherence tomography (OCT) represents a versatile tool for nanomaterial characterization, both in a laboratory and in a production environment. The technique does not require sample preparation and is applicable to a wide range of solid and liquid material systems. Large particle agglomerates can be directly found by OCT imaging, whereas dispersed nanoparticles are detected by model-based analysis of depth-dependent backscattering. Using a model system of polystyrene nanoparticles, we demonstrate nanoparticle sizing with high accuracy. We further prove the viability of the approach by characterizing highly relevant material systems based on nanoclays or carbon nanotubes. The technique is perfectly suited for in-line metrology in a production environment, which is demonstrated using a state-of-the-art compounding extruder. These experiments represent the first demonstration of multiscale nanomaterial characterization using OCT. PMID:27557544

Multiscale dispersion-state characterization of nanocomposites using optical coherence tomography.

PubMed

Schneider, Simon; Eppler, Florian; Weber, Marco; Olowojoba, Ganiu; Weiss, Patrick; Hübner, Christof; Mikonsaari, Irma; Freude, Wolfgang; Koos, Christian

2016-08-25

Nanocomposite materials represent a success story of nanotechnology. However, development of nanomaterial fabrication still suffers from the lack of adequate analysis tools. In particular, achieving and maintaining well-dispersed particle distributions is a key challenge, both in material development and industrial production. Conventional methods like optical or electron microscopy need laborious, costly sample preparation and do not permit fast extraction of nanoscale structural information from statistically relevant sample volumes. Here we show that optical coherence tomography (OCT) represents a versatile tool for nanomaterial characterization, both in a laboratory and in a production environment. The technique does not require sample preparation and is applicable to a wide range of solid and liquid material systems. Large particle agglomerates can be directly found by OCT imaging, whereas dispersed nanoparticles are detected by model-based analysis of depth-dependent backscattering. Using a model system of polystyrene nanoparticles, we demonstrate nanoparticle sizing with high accuracy. We further prove the viability of the approach by characterizing highly relevant material systems based on nanoclays or carbon nanotubes. The technique is perfectly suited for in-line metrology in a production environment, which is demonstrated using a state-of-the-art compounding extruder. These experiments represent the first demonstration of multiscale nanomaterial characterization using OCT.

Screening of salivary volatiles for putative breast cancer discrimination: an exploratory study involving geographically distant populations.

PubMed

Cavaco, Carina; Pereira, Jorge A M; Taunk, Khushman; Taware, Ravindra; Rapole, Srikanth; Nagarajaram, Hampapathalu; Câmara, José S

2018-05-07

Saliva is possibly the easiest biofluid to analyse and, despite its simple composition, contains relevant metabolic information. In this work, we explored the potential of the volatile composition of saliva samples as biosignatures for breast cancer (BC) non-invasive diagnosis. To achieve this, 106 saliva samples of BC patients and controls in two distinct geographic regions in Portugal and India were extracted and analysed using optimised headspace solid-phase microextraction gas chromatography mass spectrometry (HS-SPME/GC-MS, 2 mL acidified saliva containing 10% NaCl, stirred (800 rpm) for 45 min at 38 °C and using the CAR/PDMS SPME fibre) followed by multivariate statistical analysis (MVSA). Over 120 volatiles from distinct chemical classes, with significant variations among the groups, were identified. MVSA retrieved a limited number of volatiles, viz. 3-methyl-pentanoic acid, 4-methyl-pentanoic acid, phenol and p-tert-butyl-phenol (Portuguese samples) and acetic, propanoic, benzoic acids, 1,2-decanediol, 2-decanone, and decanal (Indian samples), statistically relevant for the discrimination of BC patients in the populations analysed. This work defines an experimental layout, HS-SPME/GC-MS followed by MVSA, suitable to characterise volatile fingerprints for saliva as putative biosignatures for BC non-invasive diagnosis. Here, it was applied to BC samples from geographically distant populations and good disease separation was obtained. Further studies using larger cohorts are therefore very pertinent to challenge and strengthen this proof-of-concept study. Graphical abstract ᅟ.

Theophylline-nicotinamide cocrystal formation in physical mixture during storage.

PubMed

Ervasti, Tuomas; Aaltonen, Jaakko; Ketolainen, Jarkko

2015-01-01

Pharmaceutically relevant properties, such as solubility and dissolution rate, of active pharmaceutical ingredients can be enhanced by cocrystal formation. Theophylline and nicotinamide are known to form cocrystals, for example if subjected to solid-state grinding. However, under appropriate conditions, cocrystals can also form in physical mixtures without any mechanical activation. The purpose of this work was to study whether theophylline and nicotinamide could form cocrystals spontaneously, without mechanical activation. Crystalline theophylline and nicotinamide powders were gently mixed manually in a 1:1 molar ratio and stored at different relative humidity and temperature conditions. The solid state of the samples was analyzed by differential scanning calorimetry, Raman spectroscopy and X-ray powder diffractometry. Three different variations of theophylline were used as starting materials, e.g., two size fractions of theophylline anhydrate (large 710 μm-1 mm and small 180-355 μm), and monohydrate (recrystallized from water). As a reference, anhydrous theophylline-nicotinamide cocrystals were prepared by solid-state grinding. The results of this study indicate that theophylline-nicotinamide cocrystals can form without any mechanical activation from physical mixtures of theophylline and nicotinamide during storage. For anhydrous samples, storage humidity was found to be a critical parameter for cocrystal formation. Increasing temperature was also found to have an accelerating effect on the transformation. The effect of particle size of anhydrous theophylline on the transformation rate could not be completely resolved; DSC and Raman indicated slightly faster transformation with a physical mixture prepared from large size fraction of anhydrous theophylline, but the differences were only minor. Cocrystal formation was also observed in the physical mixture prepared from theophylline monohydrate, but the rate was not as high as with samples prepared from anhydrous material. Copyright © 2015 Elsevier B.V. All rights reserved.

Ambient airborne solids concentrations including volcanic ash at Hanford, Washington sampling sites subsequent to the Mount St. Helens eruption

NASA Technical Reports Server (NTRS)

Sehmel, G. A.

1982-01-01

Airborne solids concentrations were measured on a near daily basis at two Hanford, Washington sites after the eruption of Mount St. Helens on May 18, 1980. These sites are about 211 km east of Mount St. Helens. Collected airborne solids included resuspended volcanic ash plus normal ambient solids. Average airborne solids concentrations were greater at the Hanford meteorological station sampling site which is 24 km northwest of the Horn Rapids dam sampling site. These increased concentrations reflect the sampling site proximity to greater ash fallout depths. Both sites are in low ash fallout areas although the Hanford meteorological station site is closer to the greater ash fallout areas. Airborne solids concentrations were decreased by rain, but airborne solids concentrations rapidly increased as surfaces dried. Airborne concentrations tended to become nearly the same at both sampling sites only for July 12 and 13.

Measurement of sample temperatures under magic-angle spinning from the chemical shift and spin-lattice relaxation rate of 79Br in KBr powder

PubMed Central

Thurber, Kent R.; Tycko, Robert

2009-01-01

Accurate determination of sample temperatures in solid state nuclear magnetic resonance (NMR) with magic-angle spinning (MAS) can be problematic, particularly because frictional heating and heating by radio-frequency irradiation can make the internal sample temperature significantly different from the temperature outside the MAS rotor. This paper demonstrates the use of 79Br chemical shifts and spin-lattice relaxation rates in KBr powder as temperature-dependent parameters for the determination of internal sample temperatures. Advantages of this method include high signal-to-noise, proximity of the 79Br NMR frequency to that of 13C, applicability from 20 K to 320 K or higher, and simultaneity with adjustment of the MAS axis direction. We show that spin-lattice relaxation in KBr is driven by a quadrupolar mechanism. We demonstrate a simple approach to including KBr powder in hydrated samples, such as biological membrane samples, hydrated amyloid fibrils, and hydrated microcrystalline proteins, that allows direct assessment of the effects of frictional and radio-frequency heating under experimentally relevant conditions. PMID:18930418

Measurement of sample temperatures under magic-angle spinning from the chemical shift and spin-lattice relaxation rate of 79Br in KBr powder.

PubMed

Thurber, Kent R; Tycko, Robert

2009-01-01

Accurate determination of sample temperatures in solid state nuclear magnetic resonance (NMR) with magic-angle spinning (MAS) can be problematic, particularly because frictional heating and heating by radio-frequency irradiation can make the internal sample temperature significantly different from the temperature outside the MAS rotor. This paper demonstrates the use of (79)Br chemical shifts and spin-lattice relaxation rates in KBr powder as temperature-dependent parameters for the determination of internal sample temperatures. Advantages of this method include high signal-to-noise, proximity of the (79)Br NMR frequency to that of (13)C, applicability from 20 K to 320 K or higher, and simultaneity with adjustment of the MAS axis direction. We show that spin-lattice relaxation in KBr is driven by a quadrupolar mechanism. We demonstrate a simple approach to including KBr powder in hydrated samples, such as biological membrane samples, hydrated amyloid fibrils, and hydrated microcrystalline proteins, that allows direct assessment of the effects of frictional and radio-frequency heating under experimentally relevant conditions.

Solid Waste Management: Abstracts From the Literature - 1964.

ERIC Educational Resources Information Center

Connolly, John A.; Stainback, Sandra E.

The Solid Waste Disposal Act of 1965 (Public Law 89-272, Title II) and its amending legislation, the Resource Recovery Act of 1970 (Public Law 91-512, Title I), authorize collection, storage, and retrieval of information relevant to all aspects of solid-waste management. As part of this effort, the U.S. Environmental Protection Agency's…

Natural occurrence of alternariol and alternariol monomethyl ether in soya beans.

PubMed

Oviedo, M S; Barros, G G; Chulze, S N; Ramirez, M L

2012-08-01

The natural occurrence of alternariol (AOH) and alternariol monomethyl ether (AME) in soya beans harvested in Argentina was evaluated. Both toxins were simultaneously detected by using HPLC analysis coupled with a solid phase extraction column clean-up. Characteristics of this in-house method such as accuracy, precision and detection and quantification limits were defined by means of recovery test with spiked soya bean samples. Out of 50 soya bean samples, 60% showed contamination with the mycotoxins analyzed; among them, 16% were only contaminated with AOH and 14% just with AME. Fifteen of the positive samples showed co-occurrence of both mycotoxins analyzed. AOH was detected in concentrations ranging from 25 to 211 ng/g, whereas AME was found in concentrations ranging from 62 to 1,153 ng/g. Although a limited number of samples were evaluated, this is the first report on the natural occurrence of Alternaria toxins in soya beans and is relevant from the point of view of animal public health.

Surface chemistry of carbon dioxide revisited

NASA Astrophysics Data System (ADS)

Taifan, William; Boily, Jean-François; Baltrusaitis, Jonas

2016-12-01

This review discusses modern developments in CO2 surface chemistry by focusing on the work published since the original review by H.J. Freund and M.W. Roberts two decades ago (Surface Science Reports 25 (1996) 225-273). It includes relevant fundamentals pertaining to the topics covered in that earlier review, such as conventional metal and metal oxide surfaces and CO2 interactions thereon. While UHV spectroscopy has routinely been applied for CO2 gas-solid interface analysis, the present work goes further by describing surface-CO2 interactions under elevated CO2 pressure on non-oxide surfaces, such as zeolites, sulfides, carbides and nitrides. Furthermore, it describes additional salient in situ techniques relevant to the resolution of the interfacial chemistry of CO2, notably infrared spectroscopy and state-of-the-art theoretical methods, currently used in the resolution of solid and soluble carbonate species in liquid-water vapor, liquid-solid and liquid-liquid interfaces. These techniques are directly relevant to fundamental, natural and technological settings, such as heterogeneous and environmental catalysis and CO2 sequestration.

Modified Sample Preparation Approach for the Determination of the Phenolic and Humic-Like Substances in Natural Organic Materials By the Folin Ciocalteu Method.

PubMed

Pontoni, Ludovico; Panico, Antonio; Matanò, Alessia; van Hullebusch, Eric D; Fabbricino, Massimiliano; Esposito, Giovanni; Pirozzi, Francesco

2017-12-06

A novel modification of the sample preparation procedure for the Folin-Ciocalteu colorimetric assay for the determination of total phenolic compounds in natural solid and semisolid organic materials (e.g., foods, organic solid waste, soils, plant tissues, agricultural residues, manure) is proposed. In this method, the sample is prepared by adding sodium sulfate as a solid diluting agent before homogenization. The method allows for the determination of total phenols (TP) in samples with high solids contents, and it provides good accuracy and reproducibility. Additionally, this method permits analyses of significant amounts of sample, which reduces problems related to heterogeneity. We applied this method to phenols-rich lignocellulosic and humic-like solids and semisolid samples, including rice straw (RS), peat-rich soil (PS), and food waste (FW). The TP concentrations measured with the solid dilution (SD) preparation were substantially higher (increases of 41.4%, 15.5%, and 59.4% in RS, PS and FW, respectively) than those obtained with the traditional method (solids suspended in water). These results showed that the traditional method underestimates the phenolic contents in the studied solids.

TANK 26F SUPERNATANT AND 2F EVAPORATOR EDUCTOR PUMP SAMPLE CHARACTERIZATION RESULTS

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

King, W.; Hay, M.; Coleman, C.

2011-08-23

In an effort to understand the reasons for system plugging problems in the SRS 2F evaporator, supernatant samples were retrieved from the evaporator feed tank (Tank 26F) and solids were collected from the evaporator eductor feed pump for characterization. The variable depth supernatant samples were retrieved from Tank 26F in early December of 2010 and samples were provided to SRNL and the F/H Area laboratories for analysis. Inspection and analysis of the samples at SRNL was initiated in early March of 2011. During the interim period, samples were frequently exposed to temperatures as low as 12 C with daily temperaturemore » fluctuations as high as 10 C. The temperature at the time of sample collection from the waste tank was 51 C. Upon opening the supernatant bottles at SRNL, many brown solids were observed in both of the Tank 26F supernatant samples. In contrast, no solids were observed in the supernatant samples sent to the F/H Area laboratories, where the analysis was completed within a few days after receipt. Based on these results, it is believed that the original Tank 26F supernatant samples did not contain solids, but solids formed during the interim period while samples were stored at ambient temperature in the SRNL shielded cells without direct climate control. Many insoluble solids (>11 wt. % for one sample) were observed in the Tank 26F supernatant samples after three months of storage at SRNL which would not dissolve in the supernatant solution in two days at 51 C. Characterization of these solids along with the eductor pump solids revealed the presence of sodium oxalate and clarkeite (uranyl oxyhydroxide) as major crystalline phases. Sodium nitrate was the dominant crystalline phase present in the unwashed Eductor Pump solids. Crystalline sodium nitrate may have formed during the drying of the solids after filtration or may have been formed in the Tank 26F supernatant during storage since the solution was found to be very concentrated (9-12 M Na{sup +}). Concentrated mineral acids and elevated temperature were required to dissolve all of these solids. The refractory nature of some of the solids is consistent with the presence of metal oxides such as aluminosilicates (observed as a minor phase by XRD). Characterization of the water wash solutions and the digested solids confirmed the presence of oxalate salts in both solid samples. Sulfate enrichment was also observed in the Tank 26F solids wash solution, indicating the presence of sulfate precipitates such as burkeite. OLI modeling of the Tank 26F filtered supernatant composition revealed that sodium oxalate has a very low solubility in this solution. The model predicts that the sodium oxalate solubility in the Tank 26F supernatant is only 0.0011 M at 50 C. The results indicate that the highly concentrated nature of the evaporator feed solution and the addition of oxalate anion to the waste stream each contribute to the formation of insoluble solids in the 2F evaporator system.« less

The value of mutational profiling of the cytocentrifugation supernatant fluid from fine-needle aspiration of pancreatic solid mass lesions.

PubMed

Deftereos, Georgios; Finkelstein, Sydney D; Jackson, Sara A; Ellsworth, Eric M G; Krishnamurti, Uma; Liu, Yulin; Silverman, Jan F; Binkert, Candy R; Ujevich, Beth A; Mohanty, Alok

2014-04-01

Fine-needle aspiration (FNA) of pancreatic solid masses can be significantly impacted by sampling variation. Molecular analysis of tumor DNA can be an aid for more definitive diagnosis. The aim of this study was to evaluate how molecular analysis of the cell-free cytocentrifugation supernatant DNA can help reduce sampling variability and increase diagnostic yield. Twenty-three FNA smears from pancreatic solid masses were performed. Remaining aspirates were rinsed for preparation of cytocentrifuged slides or cell blocks. DNA was extracted from supernatant fluid and assessed for DNA quantity spectrophotometrically and for amplifiability by quantitative PCR (qPCR). Supernatants with adequate DNA were analyzed for mutations using PCR/capillary electrophoresis for a broad panel of markers (KRAS point mutation by sequencing, microsatellite fragment analysis for loss of heterozygosity (LOH) of 16 markers at 1p, 3p, 5q, 9p, 10q, 17p, 17q, 21q, and 22q). In selected cases, microdissection of stained cytology smears and/or cytocentrifugation cellular slides were analyzed and compared. In all, 5/23 samples cytologically confirmed as adenocarcinoma showed detectable mutations both in the microdissected slide-based cytology cells and in the cytocentrifugation supernatant. While most mutations detected were present in both microdissected slides and supernatant fluid specimens, the latter showed additional mutations supporting greater sensitivity for detecting relevant DNA damage. Clonality for individual marker mutations was higher in the supernatant fluid than in microdissected cells. Cytocentrifugation supernatant fluid contains levels of amplifiable DNA suitable for mutation detection and characterization. The finding of additional detectable mutations at higher clonality indicates that supernatant fluid may be enriched with tumor DNA. Molecular analysis of the supernatant fluid could serve as an adjunct method to reduce sampling variability and increase diagnostic yield, especially in cases with a high clinical suspicion for malignancy and limited number of atypical cells in the smears.

Method development and validation for simultaneous quantification of 15 drugs of abuse and prescription drugs and 7 of their metabolites in whole blood relevant in the context of driving under the influence of drugs--usefulness of multi-analyte calibration.

PubMed

Steuer, Andrea E; Forss, Anna-Maria; Dally, Annika M; Kraemer, Thomas

2014-11-01

In the context of driving under the influence of drugs (DUID), not only common drugs of abuse may have an influence, but also medications with similar mechanisms of action. Simultaneous quantification of a variety of drugs and medications relevant in this context allows faster and more effective analyses. Therefore, multi-analyte approaches have gained more and more popularity in recent years. Usually, calibration curves for such procedures contain a mixture of all analytes, which might lead to mutual interferences. In this study we investigated whether the use of such mixtures leads to reliable results for authentic samples containing only one or two analytes. Five hundred microliters of whole blood were extracted by routine solid-phase extraction (SPE, HCX). Analysis was performed on an ABSciex 3200 QTrap instrument with ESI+ in scheduled MRM mode. The method was fully validated according to international guidelines including selectivity, recovery, matrix effects, accuracy and precision, stabilities, and limit of quantification. The selected SPE provided recoveries >60% for all analytes except 6-monoacetylmorphine (MAM) with coefficients of variation (CV) below 15% or 20% for quality controls (QC) LOW and HIGH, respectively. Ion suppression >30% was found for benzoylecgonine, hydrocodone, hydromorphone, MDA, oxycodone, and oxymorphone at QC LOW, however CVs were always below 10% (n=6 different whole blood samples). Accuracy and precision criteria were fulfilled for all analytes except for MAM. Systematic investigation of accuracy determined for QC MED in a multi-analyte mixture compared to samples containing only single analytes revealed no relevant differences for any analyte, indicating that a multi-analyte calibration is suitable for the presented method. Comparison of approximately 60 samples to a former GC-MS method showed good correlation. The newly validated method was successfully applied to more than 1600 routine samples and 3 proficiency tests. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Solid deuterated water in space: detection constraints from laboratory experiments

NASA Astrophysics Data System (ADS)

Urso, R. G.; Palumbo, M. E.; Baratta, G. A.; Scirè, C.; Strazzulla, G.

2018-06-01

The comparison between astronomical spectra and laboratory experiments is fundamental to spread light on the structure and composition of ices found in interstellar dense molecular clouds and in Solar System bodies. Water is among the most abundant solid-phase species observed in these environments, and several attempts have been made to investigate the presence of its solid-phase isotopologues. In particular, the detection of the O-D stretching mode band at 4.1 μm due to both D2O and HDO within icy grain mantles is still under debate, and no detection have been reported about the presence of these species within icy bodies in the Solar System yet. In the near future, an important contribution could derive from the data acquired in the O-D stretching mode spectral range by the sensitive instruments on board the James Webb Space Telescope. With this in mind, we performed several laboratory experiments to study the O-D stretching mode band in solid mixtures containing water and deuterated water deposited in the temperature range between 17 and 155 K, in order to simulate astrophysical relevant conditions. Furthermore, samples have been studied at various temperature and irradiated with energetic ions (200 keV H+) in order to study the effects induced by both thermal and energetic processing. Our results provide some constraints on the detection of the 4.1 μm band in astronomical environments.

New Mechanisms of Mercury Binding to Peat

NASA Astrophysics Data System (ADS)

Nagy, K. L.; Manceau, A.; Gasper, J. D.; Ryan, J. N.; Aiken, G. R.

2007-12-01

Mercury can be immobilized in the aquatic environment by binding to peat, a solid form of natural organic matter. Binding mechanisms can vary in strength and reversibility, and therefore will control concentrations of bioreactive mercury, may explain rates of mercury methylation, and are important for designing approaches to improve water quality using natural wetlands or engineered phytoremediation schemes. In addition, strong binding between mercury and peat is likely to result in the fixation of mercury that ultimately resides in coal. The mechanisms by which aqueous mercury at low concentrations reacts with both dissolved and solid natural organic matter remain incompletely understood, despite recent efforts. We have identified three distinct binding mechanisms of divalent cationic mercury to solid peats from the Florida Everglades using EXAFS spectroscopic data (FAME beamline, European Synchrotron Radiation Facility (ESRF)) obtained on experimental samples as compared to relevant references including mercury-bearing solids and mercury bound to various organic molecules. The proportions of the three molecular configurations vary with Hg concentration, and two new configurations that involve sulfur ligands occur at Hg concentrations up to about 4000 ppm. The binding mechanism at the lowest experimental Hg concentration (60-80 ppm) elucidates published reports on the inhibition of metacinnabar formation in the presence of Hg-bearing solutions and dissolved natural organic matter, and also, the differences in extent of mercury methylation in distinct areas of the Florida Everglades.

Stability and Solid Solutions of Hydrous Alumino-Silicates in the Earth's Mantle

NASA Astrophysics Data System (ADS)

Panero, W. R.; Caracas, R.

2017-12-01

The degree to which the Earth's mantle stores and cycles water in excess of the storage capacity of nominally anhydrous minerals is dependent upon the stability of hydrous phases under mantle-relevant pressures, temperatures, and compositions. Two hydrous phases, phase D and phase H are stable to the pressures and temperatures of the Earth's lower mantle, suggesting that the Earth's lower mantle may participate in the cycling of water. Each phase has a wide solid solution series between MgSi2O6H2-Al2SiO6H2 and MgSiO4H2-2δAlOOH-SiO2, respectively, yet most work addresses end-member compositions for analysis of stability and elastic properties. We present the results of density functional theory calculations on the stability, structure, bonding, partitioning, and elasticity of hydrous phases D and H in the Al2O3-SiO2-MgO-H2O system, addressing the solid solution series through a statistical sampling of site occupancy and calculation of the partition function from the grand canonical ensemble. We find that the addition of Al to the endmember compositions stabilizes each phase to higher temperatures through additional configurational entropy. We further find that solid solutions tend not to undergo hydrogen-bond symmetrization as is found in the end member compositions as a result of non-symmetric bonding environments.

Chemical transformation of some biologically relevant calcium phosphates in aqueous media during a steam sterilization.

PubMed

Dorozhkin, S V; Schmitt, M; Bouler, J M; Daculsi, G

2000-12-01

The purpose of this study was to investigate the effect of steam sterilization on some biologically relevant calcium phosphates: CaHPO4 . 2H2O (DCPD), calcium deficient apatite (CDA) and biphasic calcium phosphate (BCP). Suspensions of 0.2 g of each calcium phosphate compound with 5.0 ml of deionized water were prepared and steam sterilized in an autoclave (20 min at 121 degrees C). After sterilization the suspensions were filtered and the dried solids characterized with scanning electron microscopy, IR-spectroscopy and X-ray diffraction. The pH and calcium concentrations of the filtrates were determined with ion selective electrodes. Similar measurements were made with the same samples which were not sterilized. The sterilization procedure was found to result in the dehydration of DCPD and hydration of calcium oxide incorporated into the BCP. Solution pH was observed to change from 7.3 to 5.5 for the solutions in equilibrium with DCPD and from 8.5 to 10.6 for those in equilibrium with BCP. Minor changes both with the solid and liquid phases were found to occur during the steam sterilization of CDA. These results indicate that steam sterilization may have different effects on different calcium phosphate suspensions: it can result in dehydration of DCPD, fast hydration for CaO in BCP, but no significant effect on CDA. Copyright 2000 Kluwer Academic Publishers

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

Reactions of Ground State Nitrogen Atoms N(4S) with Astrochemically-Relevant Molecules on Interstellar Dusts

NASA Astrophysics Data System (ADS)

Krim, Lahouari; Nourry, Sendres

2015-06-01

In the last few years, ambitious programs were launched to probe the interstellar medium always more accurately. One of the major challenges of these missions remains the detection of prebiotic compounds and the understanding of reaction pathways leading to their formation. These complex heterogeneous reactions mainly occur on icy dust grains, and their studies require the coupling of laboratory experiments mimicking the extreme conditions of extreme cold and dilute media. For that purpose, we have developed an original experimental approach that combine the study of heterogeneous reactions (by exposing neutral molecules adsorbed on ice to non-energetic radicals H, OH, N...) and a neon matrix isolation study at very low temperatures, which is of paramount importance to isolate and characterize highly reactive reaction intermediates. Such experimental approach has already provided answers to many questions raised about some astrochemically-relevant reactions occurring in the ground state on the surface of dust grain ices in dense molecular clouds. The aim of this new present work is to show the implication of ground state atomic nitrogen on hydrogen atom abstraction reactions from some astrochemically-relevant species, at very low temperatures (3K-20K), without providing any external energy. Under cryogenic temperatures and with high barrier heights, such reactions involving N(4S) nitrogen atoms should not occur spontaneously and require an initiating energy. However, the detection of some radicals species as byproducts, in our solid samples left in the dark for hours at 10K, proves that hydrogen abstraction reactions involving ground state N(4S) nitrogen atoms may occur in solid phase at cryogenic temperatures. Our results show the efficiency of radical species formation stemming from non-energetic N-atoms and astrochemically-relevant molecules. We will then discuss how such reactions, involving nitrogen atoms in their ground states, might be the first key step towards complex organic molecules production in the interstellar medium.

Cadmium and lead in cocoa powder and chocolate products in the US Market.

PubMed

Abt, Eileen; Fong Sam, Jennifer; Gray, Patrick; Robin, Lauren Posnick

2018-06-01

Cocoa powder and chocolate products are known to sometimes contain cadmium (Cd) and lead (Pb) from environmental origins. A convenience sample of cocoa powder, dark chocolate, milk chocolate, and cocoa nib products was purchased at retail in the US and analysed using inductively coupled plasma mass spectrometry to assess Cd and Pb concentrations. Cd and Pb were evaluated in relation to the percent cocoa solids and to the reported origin of the cocoa powder and chocolate products. Cd ranged from 0.004 to 3.15 mg/kg and Pb ranged from

Nanometer-scale characterization of laser-driven compression, shocks, and phase transitions, by x-ray scattering using free electron lasers

DOE PAGES

Kluge, T.; Rödel, C.; Rödel, M.; ...

2017-10-23

In this paper, we study the feasibility of using small angle X-ray scattering (SAXS) as a new experimental diagnostic for intense laser-solid interactions. By using X-ray pulses from a hard X-ray free electron laser, we can simultaneously achieve nanometer and femtosecond resolution of laser-driven samples. This is an important new capability for the Helmholtz international beamline for extreme fields at the high energy density endstation currently built at the European X-ray free electron laser. We review the relevant SAXS theory and its application to transient processes in solid density plasmas and report on first experimental results that confirm the feasibilitymore » of the method. Finally, we present results of two test experiments where the first experiment employs ultra-short laser pulses for studying relativistic laser plasma interactions, and the second one focuses on shock compression studies with a nanosecond laser system.« less

Nanometer-scale characterization of laser-driven compression, shocks, and phase transitions, by x-ray scattering using free electron lasers

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

Kluge, T.; Rödel, C.; Rödel, M.

In this paper, we study the feasibility of using small angle X-ray scattering (SAXS) as a new experimental diagnostic for intense laser-solid interactions. By using X-ray pulses from a hard X-ray free electron laser, we can simultaneously achieve nanometer and femtosecond resolution of laser-driven samples. This is an important new capability for the Helmholtz international beamline for extreme fields at the high energy density endstation currently built at the European X-ray free electron laser. We review the relevant SAXS theory and its application to transient processes in solid density plasmas and report on first experimental results that confirm the feasibilitymore » of the method. Finally, we present results of two test experiments where the first experiment employs ultra-short laser pulses for studying relativistic laser plasma interactions, and the second one focuses on shock compression studies with a nanosecond laser system.« less

A versatile lab-on-chip test platform to characterize elementary deformation mechanisms and electromechanical couplings in nanoscopic objects

NASA Astrophysics Data System (ADS)

Pardoen, Thomas; Colla, Marie-Sthéphane; Idrissi, Hosni; Amin-Ahmadi, Behnam; Wang, Binjie; Schryvers, Dominique; Bhaskar, Umesh K.; Raskin, Jean-Pierre

2016-03-01

A nanomechanical on-chip test platform has recently been developed to deform under a variety of loading conditions freestanding thin films, ribbons and nanowires involving submicron dimensions. The lab-on-chip involves thousands of elementary test structures from which the elastic modulus, strength, strain hardening, fracture, creep properties can be extracted. The technique is amenable to in situ transmission electron microscopy (TEM) investigations to unravel the fundamental underlying deformation and fracture mechanisms that often lead to size-dependent effects in small-scale samples. The method allows addressing electrical and magnetic couplings as well in order to evaluate the impact of large mechanical stress levels on different solid-state physics phenomena. We had the chance to present this technique in details to Jacques Friedel in 2012 who, unsurprisingly, made a series of critical and very relevant suggestions. In the spirit of his legacy, the paper will address both mechanics of materials related phenomena and couplings with solids state physics issues.

System and process for dissolution of solids

DOEpatents

Liezers, Martin; Farmer, III, Orville T.

2017-10-10

A system and process are disclosed for dissolution of solids and "difficult-to-dissolve" solids. A solid sample may be ablated in an ablation device to generate nanoscale particles. Nanoparticles may then swept into a coupled plasma device operating at atmospheric pressure where the solid nanoparticles are atomized. The plasma exhaust may be delivered directly into an aqueous fluid to form a solution containing the atomized and dissolved solids. The composition of the resulting solution reflects the composition of the original solid sample.

Measuring solids concentration in stormwater runoff: comparison of analytical methods.

PubMed

Clark, Shirley E; Siu, Christina Y S

2008-01-15

Stormwater suspended solids typically are quantified using one of two methods: aliquot/subsample analysis (total suspended solids [TSS]) or whole-sample analysis (suspended solids concentration [SSC]). Interproject comparisons are difficult because of inconsistencies in the methods and in their application. To address this concern, the suspended solids content has been measured using both methodologies in many current projects, but the question remains about how to compare these values with historical water-quality data where the analytical methodology is unknown. This research was undertaken to determine the effect of analytical methodology on the relationship between these two methods of determination of the suspended solids concentration, including the effect of aliquot selection/collection method and of particle size distribution (PSD). The results showed that SSC was best able to represent the known sample concentration and that the results were independent of the sample's PSD. Correlations between the results and the known sample concentration could be established for TSS samples, but they were highly dependent on the sample's PSD and on the aliquot collection technique. These results emphasize the need to report not only the analytical method but also the particle size information on the solids in stormwater runoff.

Surface Functionalization and Targeting Strategies of Liposomes in Solid Tumor Therapy: A Review

PubMed Central

Riaz, Muhammad Kashif; Riaz, Muhammad Adil; Zhang, Xue; Lin, Congcong; Wong, Ka Hong; Chen, Xiaoyu; Lu, Aiping

2018-01-01

Surface functionalization of liposomes can play a key role in overcoming the current limitations of nanocarriers to treat solid tumors, i.e., biological barriers and physiological factors. The phospholipid vesicles (liposomes) containing anticancer agents produce fewer side effects than non-liposomal anticancer formulations, and can effectively target the solid tumors. This article reviews information about the strategies for targeting of liposomes to solid tumors along with the possible targets in cancer cells, i.e., extracellular and intracellular targets and targets in tumor microenvironment or vasculature. Targeting ligands for functionalization of liposomes with relevant surface engineering techniques have been described. Stimuli strategies for enhanced delivery of anticancer agents at requisite location using stimuli-responsive functionalized liposomes have been discussed. Recent approaches for enhanced delivery of anticancer agents at tumor site with relevant surface functionalization techniques have been reviewed. Finally, current challenges of functionalized liposomes and future perspective of smart functionalized liposomes have been discussed. PMID:29315231

Microbiome analysis of dairy cows fed pasture or total mixed ration diets.

PubMed

de Menezes, Alexandre B; Lewis, Eva; O'Donovan, Michael; O'Neill, Brendan F; Clipson, Nicholas; Doyle, Evelyn M

2011-11-01

Understanding rumen microbial ecology is essential for the development of feed systems designed to improve livestock productivity, health and for methane mitigation strategies from cattle. Although rumen microbial communities have been studied previously, few studies have applied next-generation sequencing technologies to that ecosystem. The aim of this study was to characterize changes in microbial community structure arising from feeding dairy cows two widely used diets: pasture and total mixed ration (TMR). Bacterial, archaeal and protozoal communities were characterized by terminal restriction fragment length polymorphism of the amplified SSU rRNA gene and statistical analysis showed that bacterial and archaeal communities were significantly affected by diet, whereas no effect was observed for the protozoal community. Deep amplicon sequencing of the 16S rRNA gene revealed significant differences in the bacterial communities between the diets and between rumen solid and liquid content. At the family level, some important groups of rumen bacteria were clearly associated with specific diets, including the higher abundance of the Fibrobacteraceae in TMR solid samples and members of the propionate-producing Veillonelaceae in pasture samples. This study will be relevant to the study of rumen microbial ecology and livestock feed management. © 2011 Federation of European Microbiological Societies. Published by Blackwell Publishing Ltd. All rights reserved.

Biofilm formation and potential for iron cycling in serpentinization-influenced groundwater of the Zambales and Coast Range ophiolites.

PubMed

Meyer-Dombard, D'Arcy R; Casar, Caitlin P; Simon, Alexander G; Cardace, Dawn; Schrenk, Matthew O; Arcilla, Carlo A

2018-05-01

Terrestrial serpentinizing systems harbor microbial subsurface life. Passive or active microbially mediated iron transformations at alkaline conditions in deep biosphere serpentinizing ecosystems are understudied. We explore these processes in the Zambales (Philippines) and Coast Range (CA, USA) ophiolites, and associated surface ecosystems by probing the relevance of samples acquired at the surface to in situ, subsurface ecosystems, and the nature of microbe-mineral associations in the subsurface. In this pilot study, we use microcosm experiments and batch culturing directed at iron redox transformations to confirm thermodynamically based predictions that iron transformations may be important in subsurface serpentinizing ecosystems. Biofilms formed on rock cores from the Zambales ophiolite on surface and in-pit associations, confirming that organisms from serpentinizing systems can form biofilms in subsurface environments. Analysis by XPS and FTIR confirmed that enrichment culturing utilizing ferric iron growth substrates produced reduced, magnetic solids containing siderite, spinels, and FeO minerals. Microcosms and enrichment cultures supported organisms whose near relatives participate in iron redox transformations. Further, a potential 'principal' microbial community common to solid samples in serpentinizing systems was identified. These results indicate collectively that iron redox transformations should be more thoroughly and universally considered when assessing the function of terrestrial subsurface ecosystems driven by serpentinization.

Determination of aminopolycarboxylic acids in river water by solid-phase extraction on activated charcoal cartridges and gas chromatography with mass spectrometric detection. Method performance characteristics and estimation of the uncertainty.

PubMed

Jiménez, Juan J

2013-04-03

A new sample preparation procedure to determine aminopolycarboxylic acids (ethylenediaminetetraacetic acid, EDTA, nitrilotriacetic acid, NTA, diethylenetriaminepentaacetic acid, DTPA, and cyclohexanediaminetetraacetic acid, CDTA) in river water is described. The procedure consists of the solid-phase extraction of the aminopolycaroxyllic acids on activated charcoal cartridges after increasing the ionic strength and acidifying the sample. The extract was eluted with methanol and the analytes were methylated in presence of BF3/methanol to determine them by GC with mass spectrometric detection. Recoveries were higher than 90% with good repeatabilities and inter-day precision for concentrations close to quantification limits (about 10 μg L(-1)) and higher. It has been verified that the proposed method is robust according to the Youden and Steiner test and free of matrix effects arisen from the presence of organic matter and iron(III) as deduced from statistical tests. A bottom-up approach was followed to estimate the uncertainty of the measured concentration. At concentrations close to 10 μg L(-1) the most relevant step of the method is the calculus of the interpolated concentration which has a high value of relative standard uncertainty. Copyright © 2013 Elsevier B.V. All rights reserved.

Linear and branched perfluorooctane sulfonate isomers in technical product and environmental samples by in-port derivatization-gas chromatography-mass spectrometry.

PubMed

Chu, Shaogang; Letcher, Robert J

2009-06-01

Perfluorooctane sulfonate (PFOS) is found globally as an environmental contaminant and is highly bioaccumulative in exposed biota including humans. However, there is a dearth of environmental information on the isomeric profile of PFOS, especially in biological samples, which requires suitable analysis methods for the identification and quantification of ultratrace amounts. In the present study, a novel method was developed that incorporates clean up by solid-phase extraction (SPE) WAX cartridges and in-port derivatization-gas chromatography-mass spectrometry (GC/MS) to identify and quantitatively determine linear PFOS (L-PFOS) and branched (monotrifluoromethyl and bistrifluoromethyl) isomers in PFOS technical product and in environmentally relevant biological samples. Tetrabutylammonium hydroxide (TBAH) was used for derivatization via an in situ pyrolytic alkylation reaction that occurred in the GC injector and generated butyl PFOS isomer derivatives. In addition to L-PFOS, ten branched PFOS isomers were identified in the technical product. The environmental relevance of branched PFOS isomers in addition to L-PFOS was evidenced by the presence of six branched and L-PFOS in representative herring gull and double-crested cormorant egg, and polar bear liver and plasma samples from the Great Lakes and Arctic, respectively. For all PFOS isomers in the technical product and biota samples the method demonstrated high sensitivity with the limit of detection (LOD) ranging from 0.05 to 0.25 ng/mL, with exception of L-PFOS where the LOD was 1.46 ng/mL. For the biotic samples, the method detection limits (MDLs) were slightly higher than the LODs and ranged from 0.09 to 0.46 ng/g wet weight (w.w.) with exception of L-PFOS (MDL = 6.87 ng/g w.w.).

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

USGS Publications Warehouse

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

2004-01-01

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

Real-scale comparison between simple and composite raw sewage sampling

NASA Astrophysics Data System (ADS)

Sergio Scalize, Paulo; Moraes Frazão, Juliana

2018-06-01

The present study performed a qualitative and quantitative characterization of the raw sewage collected at the entrance of the sewage treatment station of the city of Itumbiara, state of Goiás. Samples were collected every two hours over a period of seven consecutive days. Characterization of both point samples and composite samples was performed. The parameters analyzed were: temperature, pH, alkalinity, chemical oxygen demand, oil and grease, electric conductivity, total phosphorus, settleable solids, ammoniacal nitrogen, total suspended solids, volatile suspended solids, fixed suspended solids and turbidity. These results allowed us to verify that it is possible to perform the collection and analysis of a point sample, instead of a composite sample, as a way of monitoring the efficiency of a sewage treatment plant.

Reflection spectra of solids of planetary interest

NASA Technical Reports Server (NTRS)

Sill, G. T.

1973-01-01

The spectra of solids are reproduced which might be found on the surfaces of planetary bodies or as solid condensates in the upper planetary atmosphere. Among these are spectra of various iron compounds of interest in the study of the clouds of Venus. Other spectra are included of various sulfides, some at low temperature, relevant to the planet Jupiter. Meteorite and coal abstracts are also included, to illustrate dark carbon compounds.

Reflection spectra of solids of planetary interest

NASA Technical Reports Server (NTRS)

Sill, G. T.; Carm, O.

1973-01-01

This paper reproduces the spectra of solids which might be found on the surfaces of planetary bodies or as solid condensates in the upper planetary atmosphere. Among these are spectra of various iron compounds of interest in the study of the clouds of Venus. Other spectra (some at low temperature) are included for various sulfides relevant to the planet Jupiter. Meteorite and coal spectra are also included to illustrate dark carbon compounds.

Shock-transformation of whitlockite to merrillite and the implications for meteoritic phosphate

DOE PAGES

Adcock, C. T.; Tschauner, O.; Hausrath, E. M.; ...

2017-03-06

Meteorites represent the only samples available for study on Earth of a number of planetary bodies. The minerals within meteorites therefore hold the key to addressing numerous questions about our solar system. Of particular interest is the Ca-phosphate mineral merrillite, the anhydrous end-member of the merrillite-whitlockite solid solution series. For example, the anhydrous nature of merrillite in Martian meteorites has been interpreted as evidence of water-limited late-stage Martian melts. However, recent research on apatite in the same meteorites suggests higher water content in melts. One complication of using meteorites rather than direct samples is the shock compression all meteorites havemore » experienced, which can alter meteorite mineralogy. Here we show whitlockite transformation into merrillite by shock-compression levels relevant to meteorites, including Martian meteorites. The results open the possibility that at least part of meteoritic merrillite may have originally been H + -bearing whitlockite with implications for interpreting meteorites and the need for future sample return.« less

Shock-transformation of whitlockite to merrillite and the implications for meteoritic phosphate

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

Adcock, C. T.; Tschauner, O.; Hausrath, E. M.

Meteorites represent the only samples available for study on Earth of a number of planetary bodies. The minerals within meteorites therefore hold the key to addressing numerous questions about our solar system. Of particular interest is the Ca-phosphate mineral merrillite, the anhydrous end-member of the merrillite-whitlockite solid solution series. For example, the anhydrous nature of merrillite in Martian meteorites has been interpreted as evidence of water-limited late-stage Martian melts. However, recent research on apatite in the same meteorites suggests higher water content in melts. One complication of using meteorites rather than direct samples is the shock compression all meteorites havemore » experienced, which can alter meteorite mineralogy. Here we show whitlockite transformation into merrillite by shock-compression levels relevant to meteorites, including Martian meteorites. The results open the possibility that at least part of meteoritic merrillite may have originally been H + -bearing whitlockite with implications for interpreting meteorites and the need for future sample return.« less

Shock-transformation of whitlockite to merrillite and the implications for meteoritic phosphate

PubMed Central

Adcock, C. T.; Tschauner, O.; Hausrath, E. M.; Udry, A.; Luo, S. N.; Cai, Y.; Ren, M.; Lanzirotti, A.; Newville, M.; Kunz, M.; Lin, C.

2017-01-01

Meteorites represent the only samples available for study on Earth of a number of planetary bodies. The minerals within meteorites therefore hold the key to addressing numerous questions about our solar system. Of particular interest is the Ca-phosphate mineral merrillite, the anhydrous end-member of the merrillite–whitlockite solid solution series. For example, the anhydrous nature of merrillite in Martian meteorites has been interpreted as evidence of water-limited late-stage Martian melts. However, recent research on apatite in the same meteorites suggests higher water content in melts. One complication of using meteorites rather than direct samples is the shock compression all meteorites have experienced, which can alter meteorite mineralogy. Here we show whitlockite transformation into merrillite by shock-compression levels relevant to meteorites, including Martian meteorites. The results open the possibility that at least part of meteoritic merrillite may have originally been H+-bearing whitlockite with implications for interpreting meteorites and the need for future sample return. PMID:28262701

Inorganic, Radioisotopic, and Organic Analysis of 241-AP-101 Tank Waste

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

Fiskum, S.K.; Bredt, P.R.; Campbell, J.A.

2000-10-17

Battelle received five samples from Hanford waste tank 241-AP-101, taken at five different depths within the tank. No visible solids or organic layer were observed in the individual samples. Individual sample densities were measured, then the five samples were mixed together to provide a single composite. The composite was homogenized and representative sub-samples taken for inorganic, radioisotopic, and organic analysis. All analyses were performed on triplicate sub-samples of the composite material. The sample composite did not contain visible solids or an organic layer. A subsample held at 10 C for seven days formed no visible solids.

Tribology of magnetic storage systems

NASA Technical Reports Server (NTRS)

Bhushan, Bharat

1992-01-01

The construction and the materials used in different magnetic storage devices are defined. The theories of friction and adhesion, interface temperatures, wear, and solid-liquid lubrication relevant to magnetic storage systems are presented. Experimental data are presented wherever possible to support the relevant theories advanced.

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

Not Available

This volume contains the interim change notice for sample preparation methods. Covered are: acid digestion for metals analysis, fusion of Hanford tank waste solids, water leach of sludges/soils/other solids, extraction procedure toxicity (simulate leach in landfill), sample preparation for gamma spectroscopy, acid digestion for radiochemical analysis, leach preparation of solids for free cyanide analysis, aqueous leach of solids for anion analysis, microwave digestion of glasses and slurries for ICP/MS, toxicity characteristic leaching extraction for inorganics, leach/dissolution of activated metal for radiochemical analysis, extraction of single-shell tank (SST) samples for semi-VOC analysis, preparation and cleanup of hydrocarbon- containing samples for VOCmore » and semi-VOC analysis, receiving of waste tank samples in onsite transfer cask, receipt and inspection of SST samples, receipt and extrusion of core samples at 325A shielded facility, cleaning and shipping of waste tank samplers, homogenization of solutions/slurries/sludges, and test sample preparation for bioassay quality control program.« less

Electrochemical sample matrix elimination for trace-level potentiometric detection with polymeric membrane ion-selective electrodes.

PubMed

Chumbimuni-Torres, Karin Y; Calvo-Marzal, Percy; Wang, Joseph; Bakker, Eric

2008-08-01

Potentiometric sensors are today sufficiently well understood and optimized to reach ultratrace level (subnanomolar) detection limits for numerous ions. In many cases of practical relevance, however, a high electrolyte background hampers the attainable detection limits. A particularly difficult sample matrix for potentiometric detection is seawater, where the high saline concentration forms a major interfering background and reduces the activity of most trace metals by complexation. This paper describes for the first time a hyphenated system for the online electrochemically modulated preconcentration and matrix elimination of trace metals, combined with a downstream potentiometric detection with solid contact polymeric membrane ion-selective microelectrodes. Following the preconcentration at the bismuth-coated electrode, the deposited metals are oxidized and released to a medium favorable to potentiometric detection, in this case calcium nitrate. Matrix interferences arising from the saline sample medium are thus circumvented. This concept is successfully evaluated with cadmium as a model trace element and offers potentiometric detection down to low parts per billion levels in samples containing 0.5 M NaCl background electrolyte.

Electrochemical Sample Matrix Elimination for Trace Level Potentiometric Detection with Polymeric Membrane Ion-Selective Electrodes

PubMed Central

Chumbimuni-Torres, Karin Y.; Calvo-Marzal, Percy; Wang, Joseph; Bakker, Eric

2008-01-01

Potentiometric sensors are today sufficiently well understood and optimized to reach ultra-trace level (sub-nanomolar) detection limits for numerous ions. In many cases of practical relevance, however, a high electrolyte background hampers the attainable detection limits. A particularly difficult sample matrix for potentiometric detection is seawater, where the high saline concentration forms a major interfering background and reduces the activity of most trace metals by complexation. This paper describes for the first time a hyphenated system for the online electrochemically modulated preconcentration and matrix elimination (EMPM) of trace metals, combined with a downstream potentiometric detection with solid contact polymeric membrane ion-selective microelectrodes. Following the preconcentration at the bismuth coated electrodes, the deposited metals are oxidized and released to a medium favorable to potentiometric detection, in this case calcium nitrate. Matrix interferences arising from the saline sample medium are thus circumvented. This concept is successfully evaluated with cadmium as a model trace element and offers potentiometric detection down to low parts per billion levels in samples containing 0.5 M NaCl background electrolyte. PMID:18570385

Migration of bisphenol A into canned tomatoes produced in Italy: dependence on temperature and storage conditions.

PubMed

Errico, Sonia; Bianco, Mariangela; Mita, Luigi; Migliaccio, Marina; Rossi, Sergio; Nicolucci, Carla; Menale, Ciro; Portaccio, Marianna; Gallo, Pasquale; Mita, Damiano G; Diano, Nadia

2014-10-01

A method based on solid-phase extraction followed by liquid chromatography, coupled to UV-visible and fluorescence spectrophotometry, has been developed for determination of bisphenol A (BPA) in canned tomatoes. The limit of quantification (LOQ) of the procedure used is 0.03 μM (0.26 μg BPA/kg tomato). For each of three different tomato based products (peeled, cherry and concentrated paste), 16 samples belonging to six commercial brands, retailed in Italian markets, were tested for migration of BPA epoxy-coating cans. All the tomato samples exhibited migration levels below 0.4 μg/kg, while samples subjected to heating process and/or can's damage by denting, exhibited a significant increase in the migration levels. In any case, no sample contained BPA exceeding the European Union limit for migration, set at 600 μg/kg of food. By comparing the results for each brand, no relevant difference in BPA concentration was found depending on the kind of tomato products. Copyright © 2014 Elsevier Ltd. All rights reserved.

Analysis of ecologically relevant pharmaceuticals in wastewater and surface water using selective solid phase extraction and UPLC/MS/MS

EPA Science Inventory

A rapid and sensitive method has been developed for the analysis of 48 human prescription active pharmaceutical ingredients (APIs) and 6 metabolites of interest, utilizing selective solid-phase extraction (SPE) and ultra performance liquid chromatography in combination with tripl...

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

NASA Technical Reports Server (NTRS)

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

2013-01-01

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

Characterisation of the physico-mechanical parameters of MSW.

PubMed

Stoltz, Guillaume; Gourc, Jean-Pierre; Oxarango, Laurent

2010-01-01

Following the basics of soil mechanics, the physico-mechanical behaviour of municipal solid waste (MSW) can be defined through constitutive relationships which are expressed with respect to three physical parameters: the dry density, the porosity and the gravimetric liquid content. In order to take into account the complexity of MSW (grain size distribution and heterogeneity larger than for conventional soils), a special oedometer was designed to carry out laboratory experiments. This apparatus allowed a coupled measurement of physical parameters for MSW settlement under stress. The studied material was a typical sample of fresh MSW from a French landfill. The relevant physical parameters were measured using a gas pycnometer. Moreover, the compressibility of MSW was studied with respect to the initial gravimetric liquid content. Proposed methods to assess the set of three physical parameters allow a relevant understanding of the physico-mechanical behaviour of MSW under compression, specifically, the evolution of the limit liquid content. The present method can be extended to any type of MSW. 2010 Elsevier Ltd. All rights reserved.

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.

Time- and energy-efficient solution combustion synthesis of binary metal tungstate nanoparticles with enhanced photocatalytic activity.

PubMed

Thomas, Abegayl; Janáky, Csaba; Samu, Gergely F; Huda, Muhammad N; Sarker, Pranab; Liu, J Ping; van Nguyen, Vuong; Wang, Evelyn H; Schug, Kevin A; Rajeshwar, Krishnan

2015-05-22

In the search for stable and efficient photocatalysts beyond TiO2 , the tungsten-based oxide semiconductors silver tungstate (Ag2 WO4 ), copper tungstate (CuWO4 ), and zinc tungstate (ZnWO4 ) were prepared using solution combustion synthesis (SCS). The tungsten precursor's influence on the product was of particular relevance to this study, and the most significant effects are highlighted. Each sample's photocatalytic activity towards methyl orange degradation was studied and benchmarked against their respective commercial oxide sample obtained by solid-state ceramic synthesis. Based on the results herein, we conclude that SCS is a time- and energy-efficient method to synthesize crystalline binary tungstate nanomaterials even without additional excessive heat treatment. As many of these photocatalysts possess excellent photocatalytic activity, the discussed synthetic strategy may open sustainable materials chemistry avenues to solar energy conversion and environmental remediation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Recent advances in mid- and near-infrared spectroscopy with applications for research and teaching, focusing on petrochemistry and biotechnology relevant products

NASA Astrophysics Data System (ADS)

Heise, H. M.; Fritzsche, J.; Tkatsch, H.; Waag, F.; Karch, K.; Henze, K.; Delbeck, S.; Budde, J.

2013-11-01

Mid- and near-infrared spectroscopy is introduced as a versatile analytical method for characterizing liquid and solid chemicals as obtained from petrochemistry and biotechnology processes. Besides normal transmission measurements, special equipment with silver halide fiber-optic probes allowing efficient analysis based on mid-infrared attenuated total reflection, and an accessory for near-infrared diffuse reflection measurements, are presented. The latter technique can be used advantageously for powdered samples such as microalgae biomass and polysaccharides, as well as for different tissues such as meat samples. The advantages and disadvantages of both methods, which can be used for industrial process monitoring and chemical quality control applications, are discussed, and have been used in several research projects of BSc students within their degree course of bio- and nano-technologies of our University of Applied Sciences.

Single photon energy dispersive x-ray diffraction

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

Higginbotham, Andrew; Patel, Shamim; Ciricosta, Orlando

2014-03-15

With the pressure range accessible to laser driven compression experiments on solid material rising rapidly, new challenges in the diagnosis of samples in harsh laser environments are emerging. When driving to TPa pressures (conditions highly relevant to planetary interiors), traditional x-ray diffraction techniques are plagued by increased sources of background and noise, as well as a potential reduction in signal. In this paper we present a new diffraction diagnostic designed to record x-ray diffraction in low signal-to-noise environments. By utilising single photon counting techniques we demonstrate the ability to record diffraction patterns on nanosecond timescales, and subsequently separate, photon-by-photon, signalmore » from background. In doing this, we mitigate many of the issues surrounding the use of high intensity lasers to drive samples to extremes of pressure, allowing for structural information to be obtained in a regime which is currently largely unexplored.« less

Fluid/Solid Boundary Conditions in Non-Isothermal Systems

NASA Technical Reports Server (NTRS)

Rosner, Daniel E.

1999-01-01

The existing theoretical research concerned with thermal creep at fluid/solid interfaces is briefly reviewed, and the importance of microgravity-based experimental data is then discussed. It is noted that the ultimate goal of this research is a rational molecular level theory that predicts the dependence of a dimensionless thermal creep coefficient, Ctc, on relevant dimensionless parameters describing the way fluid molecules interact with the solid surface and how they interact among themselves. The discussion covers thermophoresis of isolated solid spheres and aggregates in gases; solid sphere thermophoresis in liquids and dense vapors; thermophoresis of small immiscible liquid droplets; and applications of the direct simulation Monte Carlo method.

Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry.

PubMed

Grate, Jay W; Gonzalez, Jhanis J; O'Hara, Matthew J; Kellogg, Cynthia M; Morrison, Samuel S; Koppenaal, David W; Chan, George C-Y; Mao, Xianglei; Zorba, Vassilia; Russo, Richard E

2017-09-08

Solid sampling and analysis methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), are challenged by matrix effects and calibration difficulties. Matrix-matched standards for external calibration are seldom available and it is difficult to distribute spikes evenly into a solid matrix as internal standards. While isotopic ratios of the same element can be measured to high precision, matrix-dependent effects in the sampling and analysis process frustrate accurate quantification and elemental ratio determinations. Here we introduce a potentially general solid matrix transformation approach entailing chemical reactions in molten ammonium bifluoride (ABF) salt that enables the introduction of spikes as tracers or internal standards. Proof of principle experiments show that the decomposition of uranium ore in sealed PFA fluoropolymer vials at 230 °C yields, after cooling, new solids suitable for direct solid sampling by LA. When spikes are included in the molten salt reaction, subsequent LA-ICP-MS sampling at several spots indicate that the spikes are evenly distributed, and that U-235 tracer dramatically improves reproducibility in U-238 analysis. Precisions improved from 17% relative standard deviation for U-238 signals to 0.1% for the ratio of sample U-238 to spiked U-235, a factor of over two orders of magnitude. These results introduce the concept of solid matrix transformation (SMT) using ABF, and provide proof of principle for a new method of incorporating internal standards into a solid for LA-ICP-MS. This new approach, SMT-LA-ICP-MS, provides opportunities to improve calibration and quantification in solids based analysis. Looking forward, tracer addition to transformed solids opens up LA-based methods to analytical methodologies such as standard addition, isotope dilution, preparation of matrix-matched solid standards, external calibration, and monitoring instrument drift against external calibration standards.

Assessment of Metaborate Fusion for the Rapid Dissolution of Solid Samples: Suitability with the Northstar ARSIIe

DTIC Science & Technology

2016-07-01

goal of this project was to develop a rapid dissolution methodology for solid environmental samples and a crude pre- concentration of actinides ...environmental solid samples needed to be removed from the samples prior to actinide separation on the ARSIIe system. As a result of this project, two...procedures were developed, one applicable to the pre-concentration of the actinides only and a second for the pre-concentration of both actinides and

A comparison of solids collected in sediment traps and automated water samplers

USGS Publications Warehouse

Bartsch, L.A.; Rada, R.G.; Sullivan, J.F.

1996-01-01

Sediment traps are being used in some pollution monitoring programs in the USA to sample suspended solids for contaminant analyses. This monitoring approach assumes that the characteristics of solids obtained in sediment traps are the same as those collected in whole-water sampling devices. We tested this assumption in the upper Mississippi River, based on the inorganic particle-size distribution (determined with a laser particle- analyzer) and volatile matter content of solids (a surrogate for organic matter). Cylindrical sediment traps (aspect ratio 3) were attached to a rigid mooring device and deployed in a flowing side channel in Navigation Pool 7 of the upper Mississippi River. On each side of the mooring device, a trap was situated adjacent to a port of an autosampler that collected raw water samples hourly to form 2-d composite samples. Paired samples (one trap and one raw water, composite sample) were removed from each end of the mooring device at 2-d intervals during the 30-d study period and compared. The relative particle collection efficiency of paired samplers did not vary temporally. Particle-size distributions of inorganic solids from sediment traps and water samples were not significantly different. The volatile matter content of solids was lesser in sediment traps (mean, 9.5%) than in corresponding water samples (mean, 22.7%). This bias may have been partly due to under-collection of phytoplankton (mainly cyanobacteria), which were abundant in the water column during the study. The positioning of water samplers and sediment traps in the mooring device did not influence the particle-size distribution or total solids of samples. We observed a small difference in the amount of organic matter collected by water samplers situated at opposite ends of the mooring device.

K West Basin Sand Filter Backwash Sample Analysis

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

Fiskum, Sandra K.; Smoot, Margaret R.; Coffey, Deborah S.

A sand filter is used to help maintain water clarity at the K West Basin where highly radioactive sludge is stored. Eventually that sand filter will require disposal. The radionuclide content of the solids trapped in the sand filter will affect the selection of the sand filter disposal pathway. The Pacific Northwest National Laboratory (PNNL) was contracted by the K Basin Operations & Plateau Remediation Project (operations contractor CH2M Hill) to analyze the radionuclide content of the solids collected from the backwash of the K West Basin sand filter. The radionuclide composition in the sand filter backwash solids will bemore » used by CH2M Hill to determine if the sand filter media and retained sludge solids will be designated as transuranic waste for disposal purposes or can be processed through less expensive means. On October 19, 2015, K Basin Operations & Plateau Remediation Project staff backwashed the sand filter into the North Load-Out Pit (NLOP) and immediately collected sample slurry from a sampling tube positioned 24 in. above the NLOP floor. The 764 g sand filter backwash slurry sample, KW-105 SFBW-001, was submitted to PNNL for analysis on October 20, 2015. Solids from the slurry sample were consolidated into two samples (i.e., a primary and a duplicate sample) by centrifuging and measured for mass (0.82 g combined – wet centrifuged solids basis) and volume (0.80 mL combined). The solids were a dark brown/orange color, consistent with iron oxide/hydroxide. The solids were dried; the combined dry solids mass was 0.1113 g, corresponding to 0.0146 weight percent (wt%) solids in the original submitted sample slurry. The solids were acid-digested using nitric and hydrochloric acids. Insoluble solids developed upon dilution with 0.5 M HNO 3, corresponding to an average 6.5 wt% of the initial dry solids content. The acid digestate and insoluble solids were analyzed separately by gamma spectrometry. Nominally, 7.7% of the 60Co was present in the insoluble solids; less than 1% of other gamma-emitters (i.e., 137Cs, 154/155Eu, and 241Am) were present in the insoluble solids. Aliquots of the acid digestate were analyzed directly using gamma energy analysis (GEA) and after separations for 238Pu, 239+240Pu, 237Np, and 241Am radioisotopes using alpha energy analysis (AEA). The 90Sr was measured by liquid scintillation counting (LSC) on the Sr-separated fraction. The plutonium isotopic distribution of the acid digestate was analyzed following Pu separations by thermal ionization mass spectrometry (TIMS). A table summarizes the results for the primary and duplicate samples. The 239+240Pu concentration (µCi/g dry) relative to 90Sr and to 137Cs concentrations (µCi/g dry) was examined. The K West Basin sludge has a 239+240Pu/ 90Sr ranging from 0.1 to 1.2 and the 239+240Pu/ 137Cs ratio ranging from 0.10 to 0.47. In contrast, the sand filter backwash solids 239+240Pu/ 90Sr ratio was 10.6 and the 239+240Pu/ 137Cs ratio was 2.0. The ratio differences indicate a relative enhancement of the Pu concentration in the sand filter solids relative to the 137Cs and 90Sr sludge concentrations currently in the K West Basin. A dose-to-curie radioisotope evaluation of the sand filter waste form may need to consider this dissimilarity.« less

Sample Results from MCU Solids Outage

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

Peters, T.; Washington, A.; Oji, L.

2014-09-22

Savannah River National Laboratory (SRNL) has received several solid and liquid samples from MCU in an effort to understand and recover from the system outage starting on April 6, 2014. SRNL concludes that the presence of solids in the Salt Solution Feed Tank (SSFT) is the likely root cause for the outage, based upon the following discoveries: A solids sample from the extraction contactor #1 proved to be mostly sodium oxalate; A solids sample from the scrub contactor#1 proved to be mostly sodium oxalate; A solids sample from the Salt Solution Feed Tank (SSFT) proved to be mostly sodium oxalate;more » An archived sample from Tank 49H taken last year was shown to contain a fine precipitate of sodium oxalate; A solids sample from ; A liquid sample from the SSFT was shown to have elevated levels of oxalate anion compared to the expected concentration in the feed. Visual inspection of the SSFT indicated the presence of precipitated or transferred solids, which were likely also in the Salt Solution Receipt Tank (SSRT). The presence of the solids coupled with agitation performed to maintain feed temperature resulted in oxalate solids migration through the MCU system and caused hydraulic issues that resulted in unplanned phase carryover from the extraction into the scrub, and ultimately the strip contactors. Not only did this carryover result in the Strip Effluent (SE) being pushed out of waste acceptance specification, but it resulted in the deposition of solids into several of the contactors. At the same time, extensive deposits of aluminosilicates were found in the drain tube in the extraction contactor #1. However it is not known at this time how the aluminosilicate solids are related to the oxalate solids. The solids were successfully cleaned out of the MCU system. However, future consideration must be given to the exclusion of oxalate solids into the MCU system. There were 53 recommendations for improving operations recently identified. Some additional considerations or additional details are provided below as recommendations. From this point on, IC-Anions analyses of the DSSHT should be part of the monthly routine analysis in order to spot negative trends in the oxalate leaving the MCU system. Care must be taken to monitor the oxalate content to watch for sudden precipitation of oxalate salts in the system; Conduct a study to optimize the cleaning strategy at ARP-MCU through decreasing the concentration or entirely eliminating the oxalic acid; The contents of the SSFT should remain unagitated. Routine visual observation should be maintained to ensure there is not a large buildup of solids. As water with agitation provided sufficient removal of the solids in the feed tank, it should be considered as a good means for dissolving oxalate solids if they are found in the future; Conduct a study to improve prediction of oxalate solubility in salt batch feed materials. As titanium and mercury have been found in various solids in this report, evaluate if either element plays a role in oxalate solubility during processing; Salt batch characterization focuses primarily on characterization and testing of unaltered Tank 21H material; however, non-typical feeds are developed through cleaning, washing, and/or sump transfers. As these solutions are processed through MCU, they may precipitate solids or reduce performance. Salt batch characterization and testing should be expanded to encompass a broader range of feeds that may be processed through ARPMCU.« less

Review—Practical Challenges Hindering the Development of Solid State Li Ion Batteries

DOE PAGES

Kerman, Kian; Luntz, Alan; Viswanathan, Venkatasubramanian; ...

2017-06-09

Solid state electrolyte systems boasting Li+ conductivity of >10 mS cm -1 at room temperature have opened the potential for developing a solid state battery with power and energy densities that are competitive with conventional liquid electrolyte systems. The primary focus of this review is twofold. First, differences in Li penetration resistance in solid state systems are discussed, and kinetic limitations of the solid state interface are highlighted. Second, technological challenges associated with processing such systems in relevant form factors are elucidated, and architectures needed for cell level devices in the context of product development are reviewed. Specific research vectorsmore » that provide high value to advancing solid state batteries are outlined and discussed.« less

A Critical Review on Clinical Application of Separation Techniques for Selective Recognition of Uracil and 5-Fluorouracil.

PubMed

Pandey, Khushaboo; Dubey, Rama Shankar; Prasad, Bhim Bali

2016-03-01

The most important objectives that are frequently found in bio-analytical chemistry involve applying tools to relevant medical/biological problems and refining these applications. Developing a reliable sample preparation step, for the medical and biological fields is another primary objective in analytical chemistry, in order to extract and isolate the analytes of interest from complex biological matrices. Since, main inborn errors of metabolism (IEM) diagnosable through uracil analysis and the therapeutic monitoring of toxic 5-fluoruracil (an important anti-cancerous drug) in dihydropyrimidine dehydrogenase deficient patients, require an ultra-sensitive, reproducible, selective, and accurate analytical techniques for their measurements. Therefore, keeping in view, the diagnostic value of uracil and 5-fluoruracil measurements, this article refines several analytical techniques involved in selective recognition and quantification of uracil and 5-fluoruracil from biological and pharmaceutical samples. The prospective study revealed that implementation of molecularly imprinted polymer as a solid-phase material for sample preparation and preconcentration of uracil and 5-fluoruracil had proven to be effective as it could obviates problems related to tedious separation techniques, owing to protein binding and drastic interferences, from the complex matrices in real samples such as blood plasma, serum samples.

Results of Characterization and Retrieval Testing on Tank 241-C-109 Heel Solids

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

Callaway, William S.

Eight samples of heel solids from tank 241-C-109 were delivered to the 222-S Laboratory for characterization and dissolution testing. After being drained thoroughly, one-half to two-thirds of the solids were off-white to tan solids that, visually, were fairly evenly graded in size from coarse silt (30-60 μm) to medium pebbles (8-16 mm). The remaining solids were mostly strongly cemented aggregates ranging from coarse pebbles (16-32 mm) to fine cobbles (6-15 cm) in size. Solid phase characterization and chemical analysis indicated that the air-dry heel solids contained ≈58 wt% gibbsite [Al(OH){sub 3}] and ≈37 wt% natrophosphate [Na{sub 7}F(PO{sub 4}){sub 2}·19H{sub 2}O].more » The strongly cemented aggregates were mostly fine-grained gibbsite cemented with additional gibbsite. Dissolution testing was performed on two test samples. One set of tests was performed on large pieces of aggregate solids removed from the heel solids samples. The other set of dissolution tests was performed on a composite sample prepared from well-drained, air-dry heel solids that were crushed to pass a 1/4-in. sieve. The bulk density of the composite sample was 2.04 g/mL. The dissolution tests included water dissolution followed by caustic dissolution testing. In each step of the three-step water dissolution tests, a volume of water approximately equal to 3 times the initial volume of the test solids was added. In each step, the test samples were gently but thoroughly mixed for approximately 2 days at an average ambient temperature of 25 °C. The caustic dissolution tests began with the addition of sufficient 49.6 wt% NaOH to the water dissolution residues to provide ≈3.1 moles of OH for each mole of Al estimated to have been present in the starting composite sample and ≈2.6 moles of OH for each mole of Al potentially present in the starting aggregate sample. Metathesis of gibbsite to sodium aluminate was then allowed to proceed over 10 days of gentle mixing of the test samples at temperatures ranging from 26-30 °C. The metathesized sodium aluminate was then dissolved by addition of volumes of water approximately equal to 1.3 times the volumes of caustic added to the test slurries. Aluminate dissolution was allowed to proceed for 2 days at ambient temperatures of ≈29 °C. Overall, the sequential water and caustic dissolution tests dissolved and removed 80.0 wt% of the tank 241-C-109 crushed heel solids composite test sample. The 20 wt% of solids remaining after the dissolution tests were 85-88 wt% gibbsite. If the density of the residual solids was approximately equal to that of gibbsite, they represented ≈17 vol% of the initial crushed solids composite test sample. In the water dissolution tests, addition of a volume of water ≈6.9 times the initial volume of the crushed solids composite was sufficient to dissolve and recover essentially all of the natrophosphate present. The ratio of the weight of water required to dissolve the natrophosphate solids to the estimated weight of natrophosphate present was 8.51. The Environmental Simulation Program (OLI Systems, Inc., Morris Plains, New Jersey) predicts that an 8.36 w/w ratio would be required to dissolve the estimated weight of natrophosphate present in the absence of other components of the heel solids. Only minor amounts of Al-bearing solids were removed from the composite solids in the water dissolution tests. The caustic metathesis/aluminate dissolution test sequence, executed at temperatures ranging from 27-30 °C, dissolved and recovered ≈69 wt% of the gibbsite estimated to have been present in the initial crushed heel solids composite. This level of gibbsite recovery is consistent with that measured in previous scoping tests on the dissolution of gibbsite in strong caustic solutions. Overall, the sequential water and caustic dissolution tests dissolved and removed 80.3 wt% of the tank 241-C-109 aggregate solids test sample. The residual solids were 92-95 wt% gibbsite. Only a minor portion (≈4.5 wt%) of the aggregate solids was dissolved and recovered in the water dissolution test. Other than some smoothing caused by continuous mixing, the aggregates were essentially unaffected by the water dissolution tests. During the caustic metathesis/aluminate dissolution test sequence, ≈81 wt% of the gibbsite estimated to have been present in the aggregate solids was dissolved and recovered. The pieces of aggregate were significantly reduced in size but persisted as distinct pieces of solids. The increased level of gibbsite recovery, as compared to that for the crushed heel solids composite, suggests that the way the gibbsite solids and caustic solution are mixed is a key determinant of the overall efficiency of gibbsite dissolution and recovery. The liquids recovered after the caustic dissolution tests on the crushed solids composite and the aggregate solids were observed for 170 days. No precipitation of gibbsite was observed. The distribution of particle sizes in the residual solids recovered following the dissolution tests on the crushed heel solids composite was characterized. Wet sieving indicated that 21.4 wt% of the residual solids were >710 μm in size, and laser light scattering indicated that the median equivalent spherical diameter in the <710-μm solids was 35 μm. The settling behavior of the residual solids following the large-scale dissolution tests was also studied. When dispersed at a concentration of ≈1 vol% in water, ≈24 wt% of the residual solids settled at a rate >0.43 in./s; ≈68 wt% settled at rates between 0.02 and 0.43 in./s; and ≈7 wt% settled slower than 0.02 in./s.« less

NO ICE HYDROGENATION: A SOLID PATHWAY TO NH{sub 2}OH FORMATION IN SPACE

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

Congiu, Emanuele; Dulieu, Francois; Chaabouni, Henda

2012-05-01

Icy dust grains in space act as catalytic surfaces onto which complex molecules form. These molecules are synthesized through exothermic reactions from precursor radicals and, mostly, hydrogen atom additions. Among the resulting products are species of biological relevance, such as hydroxylamine-NH{sub 2}OH-a precursor molecule in the formation of amino acids. In this Letter, laboratory experiments are described that demonstrate NH{sub 2}OH formation in interstellar ice analogs for astronomically relevant temperatures via successive hydrogenation reactions of solid nitric oxide (NO). Inclusion of the experimental results in an astrochemical gas-grain model proves the importance of a solid-state NO+H reaction channel as amore » starting point for prebiotic species in dark interstellar clouds and adds a new perspective to the way molecules of biological importance may form in space.« less

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

Aldegunde, Manuel, E-mail: M.A.Aldegunde-Rodriguez@warwick.ac.uk; Kermode, James R., E-mail: J.R.Kermode@warwick.ac.uk; Zabaras, Nicholas

This paper presents the development of a new exchange–correlation functional from the point of view of machine learning. Using atomization energies of solids and small molecules, we train a linear model for the exchange enhancement factor using a Bayesian approach which allows for the quantification of uncertainties in the predictions. A relevance vector machine is used to automatically select the most relevant terms of the model. We then test this model on atomization energies and also on bulk properties. The average model provides a mean absolute error of only 0.116 eV for the test points of the G2/97 set butmore » a larger 0.314 eV for the test solids. In terms of bulk properties, the prediction for transition metals and monovalent semiconductors has a very low test error. However, as expected, predictions for types of materials not represented in the training set such as ionic solids show much larger errors.« less

Low acetaldehyde collection efficiencies for 24-hour sampling with 2,4-dinitrophenylhydrazine (DNPH)-coated solid sorbents.

PubMed

Herrington, Jason S; Fan, Zhi-Hua Tina; Lioy, Paul J; Zhang, Junfeng Jim

2007-01-15

Airborne aldehyde and ketone (carbonyl) sampling methodologies based on derivatization with 2,4-dinitrophenylhydrazine (DNPH)-coated solid sorbents could unequivocally be considered the "gold" standard. Originally developed in the late 1970s, these methods have been extensively evaluated and developed up to the present day. However, these methods have been inadequately evaluated for the long-term (i.e., 24 h or greater) sampling collection efficiency (CE) of carbonyls other than formaldehyde. The current body of literature fails to demonstrate that DNPH-coated solid sorbent sampling methods have acceptable CEs for the long-term sampling of carbonyls other than formaldehyde. Despite this, such methods are widely used to report the concentrations of multiple carbonyls from long-term sampling, assuming approximately 100% CEs. Laboratory experiments were conducted in this study to evaluate the long-term formaldehyde and acetaldehyde sampling CEs for several commonly used DNPH-coated solid sorbents. Results from sampling known concentrations of formaldehyde and acetaldehyde generated in a dynamic atmosphere generation system demonstrate that the 24-hour formaldehyde sampling CEs ranged from 83 to 133%, confirming the findings made in previous studies. However, the 24-hour acetaldehyde sampling CEs ranged from 1 to 62%. Attempts to increase the acetaldehyde CEs by adding acid to the samples post sampling were unsuccessful. These results indicate that assuming approximately 100% CEs for 24-hour acetaldehyde sampling, as commonly done with DNPH-coated solid sorbent methods, would substantially under estimate acetaldehyde concentrations.

Nucleic acid extraction techniques and application to the microchip.

PubMed

Price, Carol W; Leslie, Daniel C; Landers, James P

2009-09-07

As recently as the early 1990s, DNA purification was time-consuming, requiring the use of toxic, hazardous reagents. The advent of solid phase extraction techniques and the availability of commercial kits for quick and reliable DNA extraction has relegated those early techniques largely to the history books. High quality DNA can now be extracted from whole blood, serum, saliva, urine, stool, cerebral spinal fluid, tissues, and cells in less time without sacrificing recovery. Having achieved such a radical change in the methodology of DNA extraction, focus has shifted to adapting these methods to a miniaturized system, or "lab-on-a-chip" (A. Manz, N. Graber and H. M. Widmer, Sens. Actuators, B, 1990, 1, 244-248). Manz et al.'s concept of a "miniaturized total chemical analysis system" (microTAS) involved a silicon chip that incorporated sample pretreatment, separation and detection. This review will focus on the first of these steps, sample pretreatment in the form of DNA purification. The intention of this review is to provide an overview of the fundamentals of nucleic acid purification and solid phase extraction (SPE) and to discuss specific microchip DNA extraction successes and challenges. In order to fully appreciate the advances in DNA purification, a brief review of the history of DNA extraction is provided so that the reader has an understanding of the impact that the development of SPE techniques have had. This review will highlight the different methods of nucleic acid extraction (Table 1), including relevant citations, but without an exhaustive summary of the literature. A recent review by Wen et al. (J. Wen, L. A. Legendre, J. M. Bienvenue and J. P. Landers, Anal. Chem., 2008, 80, 6472-6479) covers solid phase extraction methods with a greater focus on their incorporation into integrated microfluidic systems.

Construction of drug-polymer thermodynamic phase diagrams using Flory-Huggins interaction theory: identifying the relevance of temperature and drug weight fraction to phase separation within solid dispersions.

PubMed

Tian, Yiwei; Booth, Jonathan; Meehan, Elizabeth; Jones, David S; Li, Shu; Andrews, Gavin P

2013-01-07

Amorphous drug-polymer solid dispersions have the potential to enhance the dissolution performance and thus bioavailability of BCS class II drug compounds. The principle drawback of this approach is the limited physical stability of amorphous drug within the dispersion. Accurate determination of the solubility and miscibility of drug in the polymer matrix is the key to the successful design and development of such systems. In this paper, we propose a novel method, based on Flory-Huggins theory, to predict and compare the solubility and miscibility of drug in polymeric systems. The systems chosen for this study are (1) hydroxypropyl methylcellulose acetate succinate HF grade (HPMCAS-HF)-felodipine (FD) and (2) Soluplus (a graft copolymer of polyvinyl caprolactam-polyvinyl acetate-polyethylene glycol)-FD. Samples containing different drug compositions were mixed, ball milled, and then analyzed by differential scanning calorimetry (DSC). The value of the drug-polymer interaction parameter χ was calculated from the crystalline drug melting depression data and extrapolated to lower temperatures. The interaction parameter χ was also calculated at 25 °C for both systems using the van Krevelen solubility parameter method. The rank order of interaction parameters of the two systems obtained at this temperature was comparable. Diagrams of drug-polymer temperature-composition and free energy of mixing (ΔG(mix)) were constructed for both systems. The maximum crystalline drug solubility and amorphous drug miscibility may be predicted based on the phase diagrams. Hyper-DSC was used to assess the validity of constructed phase diagrams by annealing solid dispersions at specific drug loadings. Three different samples for each polymer were selected to represent different regions within the phase diagram.

Characterization of Tank 51 Sludge Slurry Samples (HTF-51-17-67, -68, -69, -74, -75, and -76) in Support of Sludge Batch 10 Processing

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

Oji, L. N.; Reboul, S. H.

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) Engineering (SRR-E) to provide sample characterization and analyses of Tank 51 sludge samples in support of Sludge Batch (SB) 10. The six Tank 51 sludge samples were sampled and delivered to SRNL in August of 2017. These six Tank 51 sludge samples, after undergoing physical characterizations which included rheology, weight percent total solid, dissolved solids and density measurements, were combined into one composite Tank 51 sample and analyzed for corrosion controls analytes, select radionuclides, chemical elements, density and weight percent total solids.

Analysis of water sorption isotherms of amorphous food materials by solution thermodynamics with relevance to glass transition: evaluation of plasticizing effect of water by the thermodynamic parameters.

PubMed

Shimazaki, Eriko; Tashiro, Akiko; Kumagai, Hitomi; Kumagai, Hitoshi

2017-04-01

Relation between the thermodynamic parameters obtained from water sorption isotherms and the degree of reduction in the glass transition temperature (T g ), accompanied by water sorption, was quantitatively studied. Two well-known glassy food materials namely, wheat gluten and maltodextrin were used as samples. The difference between the chemical potential of water in a solution and that of pure water ([Formula: see text]), the difference between the chemical potential of solid in a solution and that of a pure solid ([Formula: see text]), and the change in the integral Gibbs free energy ([Formula: see text]) were obtained by analyzing the water sorption isotherms using solution thermodynamics. The parameter [Formula: see text] correlated well with ΔT g (≡T g  - T g0 ; where T g0 is the glass transition temperature of dry material), which had been taken to be an index of plasticizing effect. This indicates that plasticizing effect of water on foods can be evaluated through the parameter [Formula: see text].

DNP-enhanced ultrawideline 207Pb solid-state NMR spectroscopy: an application to cultural heritage science

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

Kobayashi, Takeshi; Perras, Frederic A.; Murphy, Anna

Dynamic nuclear polarization (DNP) is used to enhance the (ultra)wideline 207Pb solid-state NMR spectra of lead compounds of relevance in the preservation of cultural heritage objects. The DNP SSNMR experiments enabled, for the first time, the detection of the basic lead carbonate phase of the lead white pigment by 207Pb SSNMR spectroscopy. Variable-temperature experiments revealed that the short T'2 relaxation time of the basic lead carbonate phase hinders the acquisition of the NMR signal at room temperature. We additionally observe that the DNP enhancement is twice as large for lead palmitate (a lead soap, which is a degradation product implicatedmore » in the visible deterioration of lead-based oil paintings), than it is for the basic lead carbonate. As a result, this enhancement has allowed us to detect the formation of a lead soap in an aged paint film by 207Pb SSNMR spectroscopy; which may aid in the detection of deterioration products in smaller samples removed from works of art.« less

DNP-enhanced ultrawideline 207Pb solid-state NMR spectroscopy: an application to cultural heritage science

DOE PAGES

Kobayashi, Takeshi; Perras, Frederic A.; Murphy, Anna; ...

2017-02-17

Dynamic nuclear polarization (DNP) is used to enhance the (ultra)wideline 207Pb solid-state NMR spectra of lead compounds of relevance in the preservation of cultural heritage objects. The DNP SSNMR experiments enabled, for the first time, the detection of the basic lead carbonate phase of the lead white pigment by 207Pb SSNMR spectroscopy. Variable-temperature experiments revealed that the short T'2 relaxation time of the basic lead carbonate phase hinders the acquisition of the NMR signal at room temperature. We additionally observe that the DNP enhancement is twice as large for lead palmitate (a lead soap, which is a degradation product implicatedmore » in the visible deterioration of lead-based oil paintings), than it is for the basic lead carbonate. As a result, this enhancement has allowed us to detect the formation of a lead soap in an aged paint film by 207Pb SSNMR spectroscopy; which may aid in the detection of deterioration products in smaller samples removed from works of art.« less

Modelling municipal solid waste generation: a review.

PubMed

Beigl, Peter; Lebersorger, Sandra; Salhofer, Stefan

2008-01-01

The objective of this paper is to review previously published models of municipal solid waste generation and to propose an implementation guideline which will provide a compromise between information gain and cost-efficient model development. The 45 modelling approaches identified in a systematic literature review aim at explaining or estimating the present or future waste generation using economic, socio-demographic or management-orientated data. A classification was developed in order to categorise these highly heterogeneous models according to the following criteria--the regional scale, the modelled waste streams, the hypothesised independent variables and the modelling method. A procedural practice guideline was derived from a discussion of the underlying models in order to propose beneficial design options concerning regional sampling (i.e., number and size of observed areas), waste stream definition and investigation, selection of independent variables and model validation procedures. The practical application of the findings was demonstrated with two case studies performed on different regional scales, i.e., on a household and on a city level. The findings of this review are finally summarised in the form of a relevance tree for methodology selection.

Confined-Pyrolysis as an Experimental Method for Hydrothermal Organic Synthesis

NASA Technical Reports Server (NTRS)

Leif, Roald N.; Simoneit, Bernd R. T.

1995-01-01

A closed pyrolysis system has been developed as a tool for studying the reactions of organic compounds under extreme hydrothermal conditions. Small high pressure stainless steel vessels in which the ratio of sediment or sample to water has been adjusted to eliminate the headspace at peak experimental conditions confines the organic components to the bulk solid matrix and eliminates the partitioning of the organic compounds away from the inorganic components during the experiment. Confined pyrolysis experiments were performed to simulate thermally driven catagenetic changes in sedimentary organic matter using a solids to water ratio of 3.4 to 1. The extent of alteration was measured by monitoring the steroid and triterpenoid biomarkers and polycyclic aromatic hydrocarbon distributions. These pyrolysis experiments duplicated the hydrothermal transformations observed in nature. Molecular probe experiments using alkadienes, alkenes and alkanes in H2O and D2O elucidated the isomerization and hydrogenation reactions of aliphatic and the competing oxidative reactions occurring under hydrothermal conditions. This confined pyrolysis technique is being applied to test experiments on organic synthesis of relevance to chemical evolution for the origin of life.

Organic matter-solid phase interactions are critical for predicting arsenic release and plant uptake in Bangladesh paddy soils.

PubMed

Williams, Paul N; Zhang, Hao; Davison, William; Meharg, Andrew A; Hossain, Mahmud; Norton, Gareth J; Brammer, Hugh; Islam, M Rafiqul

2011-07-15

Agroecological zones within Bangladesh with low levels of arsenic in groundwater and soils produce rice that is high in arsenic with respect to other producing regions of the globe. Little is known about arsenic cycling in these soils and the labile fractions relevant for plant uptake when flooded. Soil porewater dynamics of field soils (n = 39) were recreated under standardized laboratory conditions to investigate the mobility and interplay of arsenic, Fe, Si, C, and other elements, in relation to rice grain element composition, using the dynamic sampling technique diffusive gradients in thin films (DGT). Based on a simple model using only labile DGT measured arsenic and dissolved organic carbon (DOC), concentrations of arsenic in Aman (Monsoon season) rice grain were predicted reliably. DOC was the strongest determinant of arsenic solid-solution phase partitioning, while arsenic release to the soil porewater was shown to be decoupled from that of Fe. This study demonstrates the dual importance of organic matter (OM), in terms of enhancing arsenic release from soils, while reducing bioavailability by sequestering arsenic in solution.

Metabolic profiling for the identification of Huntington biomarkers by on-line solid-phase extraction capillary electrophoresis mass spectrometry combined with advanced data analysis tools.

PubMed

Pont, Laura; Benavente, Fernando; Jaumot, Joaquim; Tauler, Romà; Alberch, Jordi; Ginés, Silvia; Barbosa, José; Sanz-Nebot, Victoria

2016-03-01

In this work, an untargeted metabolomic approach based on sensitive analysis by on-line solid-phase extraction capillary electrophoresis mass spectrometry (SPE-CE-MS) in combination with multivariate data analysis is proposed as an efficient method for the identification of biomarkers of Huntington's disease (HD) progression in plasma. For this purpose, plasma samples from wild-type (wt) and HD (R6/1) mice of different ages (8, 12, and 30 weeks), were analyzed by C18 -SPE-CE-MS in order to obtain the characteristic electrophoretic profiles of low molecular mass compounds. Then, multivariate curve resolution alternating least squares (MCR-ALS) was applied to the multiple full scan MS datasets. This strategy permitted the resolution of a large number of metabolites being characterized by their electrophoretic peaks and their corresponding mass spectra. A total number of 29 compounds were relevant to discriminate between wt and HD plasma samples, as well as to follow-up the HD progression. The intracellular signaling was found to be the most affected metabolic pathway in HD mice after 12 weeks of birth, when mice already showed motor coordination deficiencies and cognitive decline. This fact agreed with the atrophy and dysfunction of specific neurons, loss of several types of receptors, and changed expression of neurotransmitters. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of lead in flour samples directly by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Tinas, Hande; Ozbek, Nil; Akman, Suleyman

2018-02-01

In this study, lead concentrations in various flour samples were determined by high-resolution continuum source graphite furnace atomic absorption spectrometry with solid sampling. Since samples were analyzed directly, the risks and disadvantages of sample digestion were eliminated. Solid flour samples were dried, weighed on the platforms, Pd was added as a modifier and introduced directly into a graphite tube using a manual solid sampler. Platforms and tubes were coated with Zr. The optimized pyrolysis and atomization temperatures were 800 °C and 2200 °C, respectively. The sensitivities of lead in various flour certified reference materials (CRMs) and aqueous standards were not significantly different. Therefore, aqueous standards were safely used for calibration. The absolute limit of detection and characteristic mass were 7.2 pg and 9.0 pg of lead, respectively. The lead concentrations in different types of flour samples were found in the range of 25-52 μg kg- 1. Finally, homogeneity factors representing the heterogeneity of analyte distribution for lead in flour samples were determined.

Fast identification of microplastics in complex environmental samples by a thermal degradation method.

PubMed

Dümichen, Erik; Eisentraut, Paul; Bannick, Claus Gerhard; Barthel, Anne-Kathrin; Senz, Rainer; Braun, Ulrike

2017-05-01

In order to determine the relevance of microplastic particles in various environmental media, comprehensive investigations are needed. However, no analytical method exists for fast identification and quantification. At present, optical spectroscopy methods like IR and RAMAN imaging are used. Due to their time consuming procedures and uncertain extrapolation, reliable monitoring is difficult. For analyzing polymers Py-GC-MS is a standard method. However, due to a limited sample amount of about 0.5 mg it is not suited for analysis of complex sample mixtures like environmental samples. Therefore, we developed a new thermoanalytical method as a first step for identifying microplastics in environmental samples. A sample amount of about 20 mg, which assures the homogeneity of the sample, is subjected to complete thermal decomposition. The specific degradation products of the respective polymer are adsorbed on a solid-phase adsorber and subsequently analyzed by thermal desorption gas chromatography mass spectrometry. For certain identification, the specific degradation products for the respective polymer were selected first. Afterwards real environmental samples from the aquatic (three different rivers) and the terrestrial (bio gas plant) systems were screened for microplastics. Mainly polypropylene (PP), polyethylene (PE) and polystyrene (PS) were identified for the samples from the bio gas plant and PE and PS from the rivers. However, this was only the first step and quantification measurements will follow. Copyright © 2017 Elsevier Ltd. All rights reserved.

Concept of Quantum Geometry in Optoelectronic Processes in Solids: Application to Solar Cells.

PubMed

Nagaosa, Naoto; Morimoto, Takahiro

2017-07-01

The concept of topology is becoming more and more relevant to the properties and functions of electronic materials including various transport phenomena and optical responses. A pedagogical introduction is given here to the basic ideas and their applications to optoelectronic processes in solids. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Mystery of the Cast Off Caper: 4-H Solid Waste Curriculum Guide.

ERIC Educational Resources Information Center

North Carolina Cooperative Extension Service, Raleigh.

This curriculum guide is composed of 16 lesson plans about terminology and concepts relevant to the four major methods of handling solid waste problems: (1) reuse; (2) recycling; (3) conversion of waste to energy ; and (4) landfilling. Games, investigations, a play, projects, a slide presentation, and skits are some of the teaching techniques…

Effects of Al(OH)O nanoparticle agglomerate size in epoxy resin on tension, bending, and fracture properties

NASA Astrophysics Data System (ADS)

Jux, Maximilian; Finke, Benedikt; Mahrholz, Thorsten; Sinapius, Michael; Kwade, Arno; Schilde, Carsten

2017-04-01

Several epoxy Al(OH)O (boehmite) dispersions in an epoxy resin are produced in a kneader to study the mechanistic correlation between the nanoparticle size and mechanical properties of the prepared nanocomposites. The agglomerate size is set by a targeted variation in solid content and temperature during dispersion, resulting in a different level of stress intensity and thus a different final agglomerate size during the process. The suspension viscosity was used for the estimation of stress energy in laminar shear flow. Agglomerate size measurements are executed via dynamic light scattering to ensure the quality of the produced dispersions. Furthermore, various nanocomposite samples are prepared for three-point bending, tension, and fracture toughness tests. The screening of the size effect is executed with at least seven samples per agglomerate size and test method. The variation of solid content is found to be a reliable method to adjust the agglomerate size between 138-354 nm during dispersion. The size effect on the Young's modulus and the critical stress intensity is only marginal. Nevertheless, there is a statistically relevant trend showing a linear increase with a decrease in agglomerate size. In contrast, the size effect is more dominant to the sample's strain and stress at failure. Unlike microscaled agglomerates or particles, which lead to embrittlement of the composite material, nanoscaled agglomerates or particles cause the composite elongation to be nearly of the same level as the base material. The observed effect is valid for agglomerate sizes between 138-354 nm and a particle mass fraction of 10 wt%.

Comparison of the solid-phase extraction efficiency of a bounded and an included cyclodextrin-silica microporous composite for polycyclic aromatic hydrocarbons determination in water samples.

PubMed

Mauri-Aucejo, Adela; Amorós, Pedro; Moragues, Alaina; Guillem, Carmen; Belenguer-Sapiña, Carolina

2016-08-15

Solid-phase extraction is one of the most important techniques for sample purification and concentration. A wide variety of solid phases have been used for sample preparation over time. In this work, the efficiency of a new kind of solid-phase extraction adsorbent, which is a microporous material made from modified cyclodextrin bounded to a silica network, is evaluated through an analytical method which combines solid-phase extraction with high-performance liquid chromatography to determine polycyclic aromatic hydrocarbons in water samples. Several parameters that affected the analytes recovery, such as the amount of solid phase, the nature and volume of the eluent or the sample volume and concentration influence have been evaluated. The experimental results indicate that the material possesses adsorption ability to the tested polycyclic aromatic hydrocarbons. Under the optimum conditions, the quantification limits of the method were in the range of 0.09-2.4μgL(-1) and fine linear correlations between peak height and concentration were found around 1.3-70μgL(-1). The method has good repeatability and reproducibility, with coefficients of variation under 8%. Due to the concentration results, this material may represent an alternative for trace analysis of polycyclic aromatic hydrocarbons in water trough solid-phase extraction. Copyright © 2016 Elsevier B.V. All rights reserved.

Stability of steviol glycosides in several food matrices.

PubMed

Jooken, Etienne; Amery, Ruis; Struyf, Tom; Duquenne, Barbara; Geuns, Jan; Meesschaert, Boudewijn

2012-10-24

As steviol glycosides are now allowed as a food additive in the European market, it is important to assess the stability of these steviol glycosides after they have been added to different food matrices. We analyzed and tested the stability of steviol glycosides in semiskimmed milk, soy drink, fermented milk drink, ice cream, full-fat and skimmed set yogurt, dry biscuits, and jam. The fat was removed by centrifugation from the dairy and soy drink samples. Proteins were precipitated by the addition of acetonitrile and also removed by centrifugation. Samples of jam were extracted with water. Dry biscuits were extracted with ethanol. The resulting samples were concentrated with solid-phase extraction and analyzed by high-performance liquid chromatography on a C18 stationary phase and a gradient of acetonitrile/aqueous 25 mM phosphoric acid. The accuracy was checked using a standard addition on some samples. For assessing the stability of the steviol glycosides, samples were stored in conditions relevant to each food matrix and analyzed periodically. The results indicate that steviol glycosides can be analyzed with good precision and accuracy in these food categories. The recovery was between 96 and 103%. The method was also validated by standard addition, which showed excellent agreement with the external calibration curve. No sign of decomposition of steviol glycosides was found in any of the samples.

ACCELERATED SOLVENT EXTRACTION COMBINED WITH AUTOMATED SOLID PHASE EXTRACTION-GC/MS FOR ANALYSIS OF SEMIVOLATILE COMPOUNDS IN HIGH MOISTURE CONTENT SOLID SAMPLES

EPA Science Inventory

A research project was initiated to address a recurring problem of elevated detection limits above required risk-based concentrations for the determination of semivolatile organic compounds in high moisture content solid samples. This project was initiated, in cooperation with t...

Assessment of heavy metal contamination in soil due to leachate migration from an open dumping site

NASA Astrophysics Data System (ADS)

Kanmani, S.; Gandhimathi, R.

2013-03-01

The concentration of heavy metals was studied in the soil samples collected around the municipal solid waste (MSW) open dumpsite, Ariyamangalam, Tiruchirappalli, Tamilnadu to understand the heavy metal contamination due to leachate migration from an open dumping site. The dump site receives approximately 400-470 tonnes of municipal solid waste. Solid waste characterization was carried out for the fresh and old municipal solid waste to know the basic composition of solid waste which is dumped in the dumping site. The heavy metal concentration in the municipal solid waste fine fraction and soil samples were analyzed. The heavy metal concentration in the collected soil sample was found in the following order: Mn > Pb > Cu > Cd. The presence of heavy metals in soil sample indicates that there is appreciable contamination of the soil by leachate migration from an open dumping site. However, these pollutants species will continuously migrated and attenuated through the soil strata and after certain period of time they might contaminate the groundwater system if there is no action to be taken to prevent this phenomenon.

Representation of solid and nutrient concentrations in irrigation water from tailwater recovery systems by surface water grab samples

USDA-ARS?s Scientific Manuscript database

Tailwater recovery (TWR) systems are being implemented on agricultural landscapes to create an additional source of irrigation water. Existing studies have sampled TWR systems using grab samples; however, the applicability of solids and nutrient concentrations in these samples to water being irrigat...

Fast acquisition of multidimensional NMR spectra of solids and mesophases using alternative sampling methods.

PubMed

Lesot, Philippe; Kazimierczuk, Krzysztof; Trébosc, Julien; Amoureux, Jean-Paul; Lafon, Olivier

2015-11-01

Unique information about the atom-level structure and dynamics of solids and mesophases can be obtained by the use of multidimensional nuclear magnetic resonance (NMR) experiments. Nevertheless, the acquisition of these experiments often requires long acquisition times. We review here alternative sampling methods, which have been proposed to circumvent this issue in the case of solids and mesophases. Compared to the spectra of solutions, those of solids and mesophases present some specificities because they usually display lower signal-to-noise ratios, non-Lorentzian line shapes, lower spectral resolutions and wider spectral widths. We highlight herein the advantages and limitations of these alternative sampling methods. A first route to accelerate the acquisition time of multidimensional NMR spectra consists in the use of sparse sampling schemes, such as truncated, radial or random sampling ones. These sparsely sampled datasets are generally processed by reconstruction methods differing from the Discrete Fourier Transform (DFT). A host of non-DFT methods have been applied for solids and mesophases, including the G-matrix Fourier transform, the linear least-square procedures, the covariance transform, the maximum entropy and the compressed sensing. A second class of alternative sampling consists in departing from the Jeener paradigm for multidimensional NMR experiments. These non-Jeener methods include Hadamard spectroscopy as well as spatial or orientational encoding of the evolution frequencies. The increasing number of high field NMR magnets and the development of techniques to enhance NMR sensitivity will contribute to widen the use of these alternative sampling methods for the study of solids and mesophases in the coming years. Copyright © 2015 John Wiley & Sons, Ltd.

Role of strained nano-regions in the formation of subgrains in CaCu3Ti4O12

NASA Astrophysics Data System (ADS)

Fang, Tsang-Tse; Wang, Yong-Huei; Kuo, Jui-Chao

2011-07-01

Single-phase CaCu3Ti4O12 (CCTO) was synthesized by solid-state reaction. Electron backscatter diffraction, scanning electron microscopy, and atomic force microscopy were adopted to characterize the grain orientation, microstructure, and surface morphology of the CCTO samples with or without thermal etching. Bump strained nano-regions induced by the local compositional disorder at a nano-scale have been discovered, being the origin of the formation of subgrains in CCTO. The proposed mechanism for the formation of subgrains involves the formation of etched pits and subboundaries pertaining to the strained nano-regions rather than dislocation displacement. The dielectric response inside the grains of CCTO relevant to the strained nano-regions is also discussed.

Direct determination of lead in biological samples by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) after furnace-fusion in the sample cuvette-tungsten boat furnace.

PubMed

Okamoto, Y

2000-06-01

The newly conceived electrothermal vaporization (ETV) system using a tungsten boat furnace (TBF) sample cuvette was designed for the direct analysis of solid samples with detection by inductively coupled plasma mass spectrometry (ICP-MS). Into this small sample cuvette, a solid mixture of the biological samples and diammonium hydrogenphosphate powder as a fusion flux was placed and situated on a TBF. Tetramethylammonium hydroxide solution was added to the mixture. After the on-furnace digestion had been completed, the analyte in the cuvette was vaporized and introduced into the ICP mass spectrometer. The solid samples were analyzed by using a calibration curve prepared from the aqueous standard solutions. The detection limit was estimated to be 5.1 pg of lead, which corresponds to 10.2 ng g(-1) of lead in solid samples when a prepared sample amount of 1.0 mg was applied. The relative standard deviation for 8 replicate measurements obtained with 100 pg of lead was calculated to be 6.5%. The analytical results for various biological samples are described.

AW-101 entrained solids - Solubility versus temperature

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

GJ Lumetta; RC Lettau; GF Piepel

This report describes the results of a test conducted by Battelle to assess the solubility of the solids entrained in the diluted AW-101 low-activity waste (LAW) sample. BNFL requested Battelle to dilute the AW-1-1 sample using de-ionized water to mimic expected plant operating conditions. BNFL further requested Battelle to assess the solubility of the solids present in the diluted AW-101 sample versus temperature conditions of 30, 40, and 50 C. BNFL requested these tests to assess the composition of the LAW supernatant and solids versus expected plant-operating conditions. The work was conducted according to test plan BNFL-TP-29953-7, Rev. 0, Determinationmore » of the Solubility of LAW Entrained Solids. The test went according to plan, with no deviations from the test plan.« less

Detection of multiple steroidal compounds in synthetic urine using comprehensive gas chromatography-mass spectrometry (GC×GC-MS) combined with a molecularly imprinted polymer clean-up protocol.

PubMed

Zulfiqar, Adnan; Morgan, Geraint; Turner, Nicholas W

2014-10-07

A method capable of screening for multiple steroids in urine has been developed, using a series of twelve structurally similar, and commercially relevant compounds as target analytes. A molecularly imprinted solid phase extraction clean-up step was used to make the sample suitable for injection onto a GC×GC-MS setup. Significant improvements compared to a commercially available C-18 material were observed. Each individual steroid was able to be separated and identified, using both the retention profile and diagnostic fragmentation ion monitoring abilities of the comprehensive chromatographic-mass spectrometry method. Effective LODs of between 11.7 and 27.0 pg were calculated for individual steroids, effectively equivalent to concentration levels of between 0.234 and 0.540 ng mL(-1) in urine, while the application of multiple screen was demonstrated using a 10 ng mL(-1) mixed sample. The nature of this study also removes the need for sample derivitisation which speeds up the screening process.

Bone Marrow Synoptic Reporting for Hematologic Neoplasms: Guideline From the College of American Pathologists Pathology and Laboratory Quality Center.

PubMed

Sever, Cordelia; Abbott, Charles L; de Baca, Monica E; Khoury, Joseph D; Perkins, Sherrie L; Reichard, Kaaren Kemp; Taylor, Ann; Terebelo, Howard R; Colasacco, Carol; Rumble, R Bryan; Thomas, Nicole E

2016-09-01

-There is ample evidence from the solid tumor literature that synoptic reporting improves accuracy and completeness of relevant data. No evidence-based guidelines currently exist for synoptic reporting for bone marrow samples. -To develop evidence-based recommendations to standardize the basic components of a synoptic report template for bone marrow samples. -The College of American Pathologists Pathology and Laboratory Quality Center convened a panel of experts in hematopathology to develop recommendations. A systematic evidence review was conducted to address 5 key questions. Recommendations were derived from strength of evidence, open comment feedback, and expert panel consensus. -Nine guideline statements were established to provide pathology laboratories with a framework by which to develop synoptic reporting templates for bone marrow samples. The guideline calls for specific data groups in the synoptic section of the pathology report; provides a list of evidence-based parameters for key, pertinent elements; and addresses ancillary testing. -A framework for bone marrow synoptic reporting will improve completeness of the final report in a manner that is clear, succinct, and consistent among institutions.

Petrogenesis of KREEP

NASA Technical Reports Server (NTRS)

Mckay, G. A.; Weill, D. F.

1975-01-01

Solid/liquid distribution coefficients (weight basis) were experimentally determined for a number of trace elements for olivine, orthopyroxene, plagioclase and ilmenite. Values of distribution coefficients were measured at 1200 C and a f sub O2 of 10 to the -13.0 power for liquids similar in composition to the olivine-opx-plagioclase peritectic in the pseudoternary system (Fe,Mg)2SiO4-CaAl2Si2O8-SiO2. Values were also measured at 1140 C and a f sub O2 of 10 to the -12.8 power for liquids similar in composition to high-Ti mare basalts. Major and trace element partitioning and relevant phase equilibria were used to investigate possible parent-daughter relationships between a number of highland samples and highly evolved KREEP-rich materials. Out of about 80 highlands samples tested, 33 were found to be possible parents to the KREEP-rich materials. The average composition of these samples is very similar to that of the Low-K Fra Mauro basalt (LKFM). A model is proposed to explain the production of LKFM-type material and more evolved members of the KREEP suite.

A Biophysical Basis for Mucus Solids Concentration as a Candidate Biomarker for Airways Disease

PubMed Central

Hill, David B.; Vasquez, Paula A.; Mellnik, John; McKinley, Scott A.; Vose, Aaron; Mu, Frank; Henderson, Ashley G.; Donaldson, Scott H.; Alexis, Neil E.; Boucher, Richard C.; Forest, M. Gregory

2014-01-01

In human airways diseases, including cystic fibrosis (CF) and chronic obstructive pulmonary disease (COPD), host defense is compromised and airways inflammation and infection often result. Mucus clearance and trapping of inhaled pathogens constitute key elements of host defense. Clearance rates are governed by mucus viscous and elastic moduli at physiological driving frequencies, whereas transport of trapped pathogens in mucus layers is governed by diffusivity. There is a clear need for simple and effective clinical biomarkers of airways disease that correlate with these properties. We tested the hypothesis that mucus solids concentration, indexed as weight percent solids (wt%), is such a biomarker. Passive microbead rheology was employed to determine both diffusive and viscoelastic properties of mucus harvested from human bronchial epithelial (HBE) cultures. Guided by sputum from healthy (1.5–2.5 wt%) and diseased (COPD, CF; 5 wt%) subjects, mucus samples were generated in vitro to mimic in vivo physiology, including intermediate range wt% to represent disease progression. Analyses of microbead datasets showed mucus diffusive properties and viscoelastic moduli scale robustly with wt%. Importantly, prominent changes in both biophysical properties arose at ∼4 wt%, consistent with a gel transition (from a more viscous-dominated solution to a more elastic-dominated gel). These findings have significant implications for: (1) penetration of cilia into the mucus layer and effectiveness of mucus transport; and (2) diffusion vs. immobilization of micro-scale particles relevant to mucus barrier properties. These data provide compelling evidence for mucus solids concentration as a baseline clinical biomarker of mucus barrier and clearance functions. PMID:24558372

Multiple Experimental Efforts to Understand the Structure and Dynamics of Earth's Core

NASA Astrophysics Data System (ADS)

Fei, Y.; Han, L.; Bennett, N.; Hou, M.; Kuwayama, Y.; Huang, H.

2014-12-01

It requires integration of data from different types of high-pressure experiments to understand the structure and dynamics of Earth's core. In particular, measurements of physical properties and element partitioning in systems relevant to the core provide complementary data to narrow down the range of possible core compositions. We have performed both static and dynamic compression experiments and combined results from these with literature data to establish a reliable thermal equation of state of iron. This allows us to precisely determine the density deficit in the solid inner core. The combination of density and sound velocity measurements for both solid and liquid iron and its alloys provide tight constraints on the density deficit in the liquid outer core and the amount of sulphur required to match the geophysical observations. We then conducted element-partitioning experiments between solid and liquid iron in both multi-anvil apparatus and the laser-heated diamond-anvil cell to determine the sulphur, silicon, and oxygen partitioning between the liquid outer core and solid inner core. We present newly developed high-pressure experimental and nano-scale analytical techniques that allow us to simulate the conditions of the inner core boundary (ICB) and analyze the chemical compositions of coexisting phases in the recovered samples. We have established protocols to obtain high-quality partitioning data in the laser-heating diamond-anvil cell combined with FIB/SEM crossbeam technology. The partitioning data obtained up to at least 200 GPa provide additional criteria to explain the observed density and velocity jumps at the ICB.

Solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for gold determination in geological samples after preconcentration onto carbon nanotubes

NASA Astrophysics Data System (ADS)

Dobrowolski, Ryszard; Mróz, Agnieszka; Dąbrowska, Marzena; Olszański, Piotr

2017-06-01

A novelty method for the determination of gold in geological samples by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GF AAS) after solid-phase extraction onto modified carbon nanotubes (CNT) was described. The methodology developed is based on solid phase extraction of Au(III) ions from digested samples to eliminate strong interference caused by iron compounds and problems related to inhomogeneities of the samples. The use of aqueous or solid standard for calibration was studied and the slope of calibration curve was the same for both of these modes. This statement indicates the possibility to perform the calibration of the method using aqueous standard solutions. Under optimum conditions the absolute detection limit for gold was equal to 2.24 · 10- 6 μg g- 1 while the adsorption capacity of modified carbon nanotubes was 264 mg g- 1. The proposed procedure was validated by the application of certified reference materials (CRMs) with different content of gold and different matrix, the results were in good agreement with certified values. The method was successfully applied for separation and determination of gold ions in complex geological samples, with precision generally better than 8%.

Analysis of solid uranium samples using a small mass spectrometer

NASA Astrophysics Data System (ADS)

Kahr, Michael S.; Abney, Kent D.; Olivares, José A.

2001-07-01

A mass spectrometer for isotopic analysis of solid uranium samples has been constructed and evaluated. This system employs the fluorinating agent chlorine trifluoride (ClF 3) to convert solid uranium samples into their volatile uranium hexafluorides (UF 6). The majority of unwanted gaseous byproducts and remaining ClF 3 are removed from the sample vessel by condensing the UF 6 and then pumping away the unwanted gases. The UF 6 gas is then introduced into a quadrupole mass spectrometer and ionized by electron impact ionization. The doubly charged bare metal uranium ion (U 2+) is used to determine the U 235/U 238 isotopic ratio. Precision and accuracy for several isotopic standards were found to be better than 12%, without further calibration of the system. The analysis can be completed in 25 min from sample loading, to UF 6 reaction, to mass spectral analysis. The method is amenable to uranium solid matrices, and other actinides.

Solid anaerobic digestion batch with liquid digestate recirculation and wet anaerobic digestion of organic waste: Comparison of system performances and identification of microbial guilds.

PubMed

Di Maria, Francesco; Barratta, Martino; Bianconi, Francesco; Placidi, Pisana; Passeri, Daniele

2017-01-01

Solid anaerobic digestion batch (SADB) with liquid digestate recirculation and wet anaerobic digestion of organic waste were experimentally investigated. SADB was operated at an organic loading rate (OLR) of 4.55kgVS/m 3 day, generating about 252NL CH 4 /kgVS, whereas the wet digester was operated at an OLR of 0.9kgVS/m 3 day, generating about 320NL CH 4 /kgVS. The initial total volatile fatty acids concentrations for SADB and wet digestion were about 12,500mg/L and 4500mg/L, respectively. There were higher concentrations of ammonium and COD for the SADB compared to the wet one. The genomic analysis performed by high throughput sequencing returned a number of sequences for each sample ranging from 110,619 to 373,307. More than 93% were assigned to the Bacteria domain. Seven and nine major phyla were sequenced for the SADB and wet digestion, respectively, with Bacteroidetes, Firmicutes and Proteobacteria being the dominant phyla in both digesters. Taxonomic profiles suggested a methanogenic pathway characterized by a relevant syntrophic acetate-oxidizing metabolism mainly in the liquid digestate of the SADB. This result also confirms the benefits of liquid digestate recirculation for improving the efficiency of AD performed with high solids (>30%w/w) content. Copyright © 2016 Elsevier Ltd. All rights reserved.

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.

Fungal decay and shelf life of oranges coated with chitosan and bergamot, thyme, and tea tree essential oils.

PubMed

Cháfer, M; Sánchez-González, L; González-Martínez, Ch; Chiralt, A

2012-08-01

Chitosan coatings, containing or not essential oils (bergamot, thyme and tea tree oil), were applied to oranges (cv. Navel Powell). Antifungal effect was evaluated by applying coatings before and after inoculating the fruit with Penicillium italicum CECT 2294 (10(5) spores/mL), preventive and curative treatments, respectively. The effect of coatings on the quality parameters (acidity, pH, soluble solids, juice percentage, weight loss, firmness, color parameters, and respiration rate) was controlled for the different oranges samples throughout the cold storage time. Preventive antimicrobial treatments with coatings containing tea tree oil were the most effective with a reduction of the microbial growth (expressed as the percentage of infected samples) of 50%, as compared to the uncoated samples. The coatings did not lead to any relevant changes in the development of the sample quality parameters throughout the cold storage, except for a slightly reduced loss of both weight and firmness when the coatings contained bergamot oil. Results of this study are a useful tool for the development of new environmental friendly and healthier commercial applications in the control of the main postharvest fungal decay of citrus fruits. © 2012 Institute of Food Technologists®

Trace element emissions from spontaneous combustion of gob piles in coal mines, Shanxi, China

USGS Publications Warehouse

Zhao, Y.; Zhang, Jiahua; Chou, C.-L.; Li, Y.; Wang, Z.; Ge, Y.; Zheng, C.

2008-01-01

The emissions of potentially hazardous trace elements from spontaneous combustion of gob piles from coal mining in Shanxi Province, China, have been studied. More than ninety samples of solid waste from gob piles in Shanxi were collected and the contents of twenty potentially hazardous trace elements (Be, F, V, Cr, Mn, Co, Ni, Cu, Zn, As, Se, Mo, Cd, Sn, Sb, Hg, Tl, Pb, Th, and U) in these samples were determined. Trace element contents in solid waste samples showed wide ranges. As compared with the upper continental crust, the solid waste samples are significantly enriched in Se (20x) and Tl (12x) and are moderately enriched in F, As, Mo, Sn, Sb, Hg, Th, and U (2-5x). The solid waste samples are depleted in V, Cr, Mn, Co, Ni, Cu, and Zn. The solid waste samples are enriched in F, V, Mn, Cr, Co, Ni, Cu, Zn, Sb, Th, and U as compared with the Shanxi coals. Most trace elements are higher in the clinker than in the unburnt solid waste except F, Sn, and Hg. Trace element abundances are related to the ash content and composition of the samples. The content of F is negatively correlated with the ash content, while Pb is positively correlated with the ash. The concentrations of As, Mn, Zn, and Cd are highly positively correlated with Fe2O3 in the solid waste. The As content increases with increasing sulfur content in the solid waste. The trace element emissions are calculated for mass balance. The emission factors of trace elements during the spontaneous combustion of the gobs are determined and the trace element concentrations in the flue gas from the spontaneous combustion of solid waste are calculated. More than a half of F, Se, Hg and Pb are released to the atmosphere during spontaneous combustion. Some trace element concentrations in flue gas are higher than the national emission standards. Thus, gob piles from coal mining pose a serious environmental problem. ?? 2007 Elsevier B.V. All rights reserved.

A Basic Accounting of Variation in Municipal Solid-Waste Generation at the County Level in Texas, 2006: Groundwork for Applying Metabolic-Rift Theory to Waste Generation

ERIC Educational Resources Information Center

Clement, Matthew Thomas

2009-01-01

Environmental social scientists debate whether or not modern development reduces society's impact on the biosphere. The empirical research informing the discussion has not yet adequately examined the social determinants of municipal solid-waste (MSW) generation, an increasingly relevant issue, both ecologically and sociologically. A primary…

Fluidics platform and method for sample preparation

DOEpatents

Benner, Henry W.; Dzenitis, John M.

2016-06-21

Provided herein are fluidics platforms and related methods for performing integrated sample collection and solid-phase extraction of a target component of the sample all in one tube. The fluidics platform comprises a pump, particles for solid-phase extraction and a particle-holding means. The method comprises contacting the sample with one or more reagents in a pump, coupling a particle-holding means to the pump and expelling the waste out of the pump while the particle-holding means retains the particles inside the pump. The fluidics platform and methods herein described allow solid-phase extraction without pipetting and centrifugation.

Gas-phase detection of solid-state fission product complexes for post-detonation nuclear forensic analysis

DOE PAGES

Stratz, S. Adam; Jones, Steven A.; Oldham, Colton J.; ...

2016-06-27

This study presents the first known detection of fission products commonly found in post-detonation nuclear debris samples using solid sample introduction and a uniquely coupled gas chromatography inductively-coupled plasma time-of-flight mass spectrometer. Rare earth oxides were chemically altered to incorporate a ligand that enhances the volatility of the samples. These samples were injected (as solids) into the aforementioned instrument and detected for the first time. Repeatable results indicate the validity of the methodology, and this capability, when refined, will prove to be a valuable asset for rapid post-detonation nuclear forensic analysis.

Gas-phase detection of solid-state fission product complexes for post-detonation nuclear forensic analysis

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

Stratz, S. Adam; Jones, Steven A.; Oldham, Colton J.

This study presents the first known detection of fission products commonly found in post-detonation nuclear debris samples using solid sample introduction and a uniquely coupled gas chromatography inductively-coupled plasma time-of-flight mass spectrometer. Rare earth oxides were chemically altered to incorporate a ligand that enhances the volatility of the samples. These samples were injected (as solids) into the aforementioned instrument and detected for the first time. Repeatable results indicate the validity of the methodology, and this capability, when refined, will prove to be a valuable asset for rapid post-detonation nuclear forensic analysis.

Singles correlation energy contributions in solids

NASA Astrophysics Data System (ADS)

Klimeš, Jiří; Kaltak, Merzuk; Maggio, Emanuele; Kresse, Georg

2015-09-01

The random phase approximation to the correlation energy often yields highly accurate results for condensed matter systems. However, ways how to improve its accuracy are being sought and here we explore the relevance of singles contributions for prototypical solid state systems. We set out with a derivation of the random phase approximation using the adiabatic connection and fluctuation dissipation theorem, but contrary to the most commonly used derivation, the density is allowed to vary along the coupling constant integral. This yields results closely paralleling standard perturbation theory. We re-derive the standard singles of Görling-Levy perturbation theory [A. Görling and M. Levy, Phys. Rev. A 50, 196 (1994)], highlight the analogy of our expression to the renormalized singles introduced by Ren and coworkers [Phys. Rev. Lett. 106, 153003 (2011)], and introduce a new approximation for the singles using the density matrix in the random phase approximation. We discuss the physical relevance and importance of singles alongside illustrative examples of simple weakly bonded systems, including rare gas solids (Ne, Ar, Xe), ice, adsorption of water on NaCl, and solid benzene. The effect of singles on covalently and metallically bonded systems is also discussed.

Extraction and quantitative analysis of iodine in solid and solution matrixes.

PubMed

Brown, Christopher F; Geiszler, Keith N; Vickerman, Tanya S

2005-11-01

129I is a contaminant of interest in the vadose zone and groundwater at numerous federal and privately owned facilities. Several techniques have been utilized to extract iodine from solid matrixes; however, all of them rely on two fundamental approaches: liquid extraction or chemical/heat-facilitated volatilization. While these methods are typically chosen for their ease of implementation, they do not totally dissolve the solid. We defined a method that produces complete solid dissolution and conducted laboratory tests to assess its efficacy to extract iodine from solid matrixes. Testing consisted of potassium nitrate/potassium hydroxide fusion of the sample, followed by sample dissolution in a mixture of sulfuric acid and sodium bisulfite. The fusion extraction method resulted in complete sample dissolution of all solid matrixes tested. Quantitative analysis of 127I and 129I via inductively coupled plasma mass spectrometry showed better than +/-10% accuracy for certified reference standards, with the linear operating range extending more than 3 orders of magnitude (0.005-5 microg/L). Extraction and analysis of four replicates of standard reference material containing 5 microg/g 127I resulted in an average recovery of 98% with a relative deviation of 6%. This simple and cost-effective technique can be applied to solid samples of varying matrixes with little or no adaptation.

Quality of major ion and total dissolved solids data from groundwater sampled by the National Water-Quality Assessment Program, 1992–2010

USGS Publications Warehouse

Gross, Eliza L.; Lindsey, Bruce D.; Rupert, Michael G.

2012-01-01

Field blank samples help determine the frequency and magnitude of contamination bias, and replicate samples help determine the sampling variability (error) of measured analyte concentrations. Quality control data were evaluated for calcium, magnesium, sodium, potassium, chloride, sulfate, fluoride, silica, and total dissolved solids. A 99-percent upper confidence limit is calculated from field blanks to assess the potential for contamination bias. For magnesium, potassium, chloride, sulfate, and fluoride, potential contamination in more than 95 percent of environmental samples is less than or equal to the common maximum reporting level. Contamination bias has little effect on measured concentrations greater than 4.74 mg/L (milligrams per liter) for calcium, 14.98 mg/L for silica, 4.9 mg/L for sodium, and 120 mg/L for total dissolved solids. Estimates of sampling variability are calculated for high and low ranges of concentration for major ions and total dissolved solids. Examples showing the calculation of confidence intervals and how to determine whether measured differences between two water samples are significant are presented.

Revisiting the thermal-spike concept in ion-surface interactions

NASA Astrophysics Data System (ADS)

Miotello, Antonio; Kelly, Roger

1997-02-01

In recent years many groups have advocated a thermal-spike model to explain a variety of experimental results in ion-irradiation of solids, as for example sputtering, mixing, compositional change, structural change, and track formation. The latter include crystal-to-amorphous transitions as well as track formation due to MeV/u particles. In this paper we reconsider the phenomena occurring during ion impact of solids looking at the time scale generally indicated as relevant for thermal-spike effects, namely a picosecond scale as shown by molecular dynamics. Sputtering, mixing, and track formation, however, will be analyzed in more detail. We consider first ion-beam sputtering and reiterate (as is already well-known) that yields which increase with the bulk temperature most often indicate merely the onset of normal vaporization. Indeed, only simulations appear to be capable of giving insight even if the information is sometimes tentative. In mixing, ballistic transport is important but not dominant. It is often argued that the additional transport is provided by thermal spikes but it is noted that such an assumption is normally not required by the experimental results. What is more relevant is a role for residual defects such that the total diffusion flux includes (if the defects are chemically guided) a modified Darken factor, or (if the defects are not chemically guided) simply an increased diffusivity. The time scale (min), distances (well beyond the collision cascade), temperature sensitivity (changes of as little as 75 K are relevant), and correlation with vacancy properties (thence with the solid rather than liquid state) which are relevant to these residual defects are not understandable in terms of thermal spikes. We finally consider track formation. Recent work claiming that track formation in solids, irradiated with heavy ions, may be understood in terms of thermal spikes is reconsidered to show that the thermal-spike model is utilized without considering all the relevant phenomena included in irradiation-induced heating and phase transitions. For example, a comparison of fs-laser pulse irradiation of Si with swift heavy-ion irradiation, shows that melting is possible in the first case since the excited electrons have a low and more or less restricted energy while in the case of swift ion-irradiation, the motion of the excited electrons includes a ballistic component which does not favour the localization of the thermal energy necessary to induce lattice melting. It is concluded that track formation is better understandable in a more general framework of defect-induced processes in solids.

Thermal Reactions Between Sulfur Dioxide and H202 and Their Relevance to the Jovian Icy Satellites and Other Small Bodies

NASA Technical Reports Server (NTRS)

Loefler, Mark J.; Hudson, Reggie L.

2011-01-01

Laboratory experiments have demonstrated that magnetospheric radiation in the Jovian system drives reaction chemistry in ices at temperatures relevant to Europa and other icy satellites. Here we present new results on thermally-induced reactions occurring between 50 and 130 K in solid H2O + H2O2 + SO2 samples. In our studies, we find that warming our three component mixtures induces a thermal reaction that produces SO4(2-), and this reaction appears to consume equal amounts of H2O2 and SO2. We suspect that the results may explain some of the observations related to the presence and distribution H2O2 across Europa's surface as well as the lack of H2O2 on Ganymede and Callisto. If other molecules prove to be reactive with H2O2 at these or at even lower temperatures, then it may also explain why H2O2 has been absent from surfaces of many of the small icy bodies that are known to be exposed to ionizing radiation.

Computer simulation and experimental self-assembly of irradiated glycine amino acid under magnetic fields: Its possible significance in prebiotic chemistry.

PubMed

Heredia, Alejandro; Colín-García, María; Puig, Teresa Pi I; Alba-Aldave, Leticia; Meléndez, Adriana; Cruz-Castañeda, Jorge A; Basiuk, Vladimir A; Ramos-Bernal, Sergio; Mendoza, Alicia Negrón

2017-12-01

Ionizing radiation may have played a relevant role in chemical reactions for prebiotic biomolecule formation on ancient Earth. Environmental conditions such as the presence of water and magnetic fields were possibly relevant in the formation of organic compounds such as amino acids. ATR-FTIR, Raman, EPR and X-ray spectroscopies provide valuable information about molecular organization of different glycine polymorphs under static magnetic fields. γ-glycine polymorph formation increases in irradiated samples interacting with static magnetic fields. The increase in γ-glycine polymorph agrees with the computer simulations. The AM1 semi-empirical simulations show a change in the catalyst behavior and dipole moment values in α and γ-glycine interaction with the static magnetic field. The simulated crystal lattice energy in α-glycine is also affected by the free radicals under the magnetic field, which decreases its stability. Therefore, solid α and γ-glycine containing free radicals under static magnetic fields might have affected the prebiotic scenario on ancient Earth by causing the oligomerization of glycine in prebiotic reactions. Copyright © 2017 Elsevier B.V. All rights reserved.

Superior Blends Solid Polymer Electrolyte with Integrated Hierarchical Architectures for All-Solid-State Lithium-Ion Batteries.

PubMed

Zhang, Dechao; Zhang, Long; Yang, Kun; Wang, Hongqiang; Yu, Chuang; Xu, Di; Xu, Bo; Wang, Li-Min

2017-10-25

Exploration of advanced solid electrolytes with good interfacial stability toward electrodes is a highly relevant research topic for all-solid-state batteries. Here, we report PCL/SN blends integrating with PAN-skeleton as solid polymer electrolyte prepared by a facile method. This polymer electrolyte with hierarchical architectures exhibits high ionic conductivity, large electrochemical windows, high degree flexibility, good flame-retardance ability, and thermal stability (workable at 80 °C). Additionally, it demonstrates superior compatibility and electrochemical stability toward metallic Li as well as LiFePO 4 cathode. The electrolyte/electrode interfaces are very stable even subjected to 4.5 V at charging state for long time. The LiFePO 4 /Li all-solid-state cells based on this electrolyte deliver high capacity, outstanding cycling stability, and superior rate capability better than those based on liquid electrolyte. This solid polymer electrolyte is eligible for next generation high energy density all-solid-state batteries.

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

PubMed

Mashile, Geaneth Pertunia; Nomngongo, Philiswa N

2017-03-04

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

The effect of B{sub 2}O{sub 3} flux on growth NLBCO superconductor by solid state reaction and wet-mixing methods

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

Suharta, W. G., E-mail: wgsuharta@gmail.com; Wendri, N.; Ratini, N.

The synthesis of B{sub 2}O{sub 3} flux substituted NLBCO superconductor NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂} has been done using solid state reaction and wet-mixing methods in order to obtain homogeneous crystals and single phase. From DTA/TGA characteritations showed the synthesis process by wet-mixing requires a lower temperature than the solid state reaction in growing the superconductor NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂}. Therefore, in this research NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂} sample calcinated at 650°C for wet-mixing method and 820°C for solid state reaction methods. The all samples was sintered at 950°C for ten hours. Crystallinity of the sample was confirmedmore » using X-ray techniques and generally obtained sharp peaks that indicates the sample already well crystallized. Search match analyses for diffraction data gave weight fractions of impurity phase of the solid state reaction method higher than wet-mixing method. In this research showed decreasing the price of the lattice parameter about 1% with the addition of B{sub 2}O{sub 3} flux for the both synthesis process and 2% of wet mixing process for all samples. Characterization using scanning electron microscopy (SEM) showed the distribution of crystal zise for wet-mixing method more homogeneous than solid state reaction method, with he grain size of samples is around 150–250 nm. The results of vibrating sample magnetometer (VSM) showed the paramagnetic properties for all samples.« less

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

PubMed

Shin, Sunghwan; Kang, Hani; Kim, Jun Soo; Kang, Heon

2014-11-26

We investigated the phase transformations of amorphous solid acetone under confined geometry by preparing acetone films trapped in amorphous solid water (ASW) or CCl4. Reflection absorption infrared spectroscopy (RAIRS) and temperature-programmed desorption (TPD) were used to monitor the phase changes of the acetone sample with increasing temperature. An acetone film trapped in ASW shows an abrupt change in the RAIRS features of the acetone vibrational bands during heating from 80 to 100 K, which indicates the transformation of amorphous solid acetone to a molecularly aligned crystalline phase. Further heating of the sample to 140 K produces an isotropic solid phase, and eventually a fluid phase near 157 K, at which the acetone sample is probably trapped in a pressurized, superheated condition inside the ASW matrix. Inside a CCl4 matrix, amorphous solid acetone crystallizes into a different, isotropic structure at ca. 90 K. We propose that the molecularly aligned crystalline phase formed in ASW is created by heterogeneous nucleation at the acetone-water interface, with resultant crystal growth, whereas the isotropic crystalline phase in CCl4 is formed by homogeneous crystal growth starting from the bulk region of the acetone sample.

Comparison of spray drying, electroblowing and electrospinning for preparation of Eudragit E and itraconazole solid dispersions.

PubMed

Sóti, Péter Lajos; Bocz, Katalin; Pataki, Hajnalka; Eke, Zsuzsanna; Farkas, Attila; Verreck, Geert; Kiss, Éva; Fekete, Pál; Vigh, Tamás; Wagner, István; Nagy, Zsombor K; Marosi, György

2015-10-15

Three solvent based methods: spray drying (SD), electrospinning (ES) and air-assisted electrospinning (electroblowing; EB) were used to prepare solid dispersions of itraconazole and Eudragit E. Samples with the same API/polymer ratios were prepared in order to make the three technologies comparable. The structure and morphology of solid dispersions were identified by scanning electron microscopy and solid phase analytical methods such as, X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC) and Raman chemical mapping. Moreover, the residual organic solvents of the solid products were determined by static headspace-gas chromatography/mass spectroscopy measurements and the wettability of samples was characterized by contact angle measurement. The pharmaceutical performance of the three dispersion type, evaluated by dissolution tests, proved to be very similar. According to XRPD and DSC analyses, made after the production, all the solid dispersions were free of any API crystal clusters but about 10 wt% drug crystallinity was observed after three months of storage in the case of the SD samples in contrast to the samples produced by ES and EB in which the polymer matrix preserved the API in amorphous state. Copyright © 2015 Elsevier B.V. All rights reserved.

Validation of enhanced stabilization of municipal solid waste under controlled leachate recirculation using FTIR and XRD.

PubMed

Sethi, Sapna; Kothiyal, N C; Nema, Arvind K

2012-07-01

Leachate recirculation at neutral PH accompanied with buffer/nutrients addition has been used successfully in earlier stabilization of municipal solid waste in bioreactor landfills. In the present study, efforts were made to enhance the stabilization rate of municipal solid waste (MSW) and organic solid waste (OSW) in simulated landfill bioreactors by controlling the pH of recirculated leachate towards slightly alkaline side in absence of additional buffer and nutrients addition. Enhanced stabilization in waste samples was monitored with the help of analytical tools like Fourier Transform Infrared Spectroscopy (FTIR) and X-Ray Diffraction (XRD). Predominance of bands assigned to inorganic compounds and comparatively lower intensities of bands for organic compounds in the FTIR spectra of waste samples degraded with leachate recirculation under controlled pH confirmed higher rate of biodegradation and mineralization of waste than the samples degraded without controlled leachate recirculation. XRD spectra also confirmed to a greater extent of mineralization in the waste samples degraded under leachate recirculation with controlled pH. Comparison of XRD spectra of two types of wastes pointed out higher degree of mineralization in organic solid waste as compared to municipal solid waste.

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

NASA Technical Reports Server (NTRS)

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

1973-01-01

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

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

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

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

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

Raman spectroscopic studies on bacteria

NASA Astrophysics Data System (ADS)

Maquelin, Kees; Choo-Smith, Lin-P'ing; Endtz, Hubert P.; Bruining, Hajo A.; Puppels, Gerwin J.

2000-11-01

Routine clinical microbiological identification of pathogenic micro-organisms is largely based on nutritional and biochemical tests. Laboratory results can be presented to a clinician after 2 - 3 days for most clinically relevant micro- organisms. Most of this time is required to obtain pure cultures and enough biomass for the tests to be performed. In the case of severely ill patients, this unavoidable time delay associated with such identification procedures can be fatal. A novel identification method based on confocal Raman microspectroscopy will be presented. With this method it is possible to obtain Raman spectra directly from microbial microcolonies on the solid culture medium, which have developed after only 6 hours of culturing for most commonly encountered organisms. Not only does this technique enable rapid (same day) identifications, but also preserves the sample allowing it to be double-checked with traditional tests. This, combined with the speed and minimal sample handling indicate that confocal Raman microspectroscopy has much potential as a powerful new tool in clinical diagnostic microbiology.

Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.

PubMed

Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

2013-12-20

Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including practical applications of these techniques and a critical discussion about their advantages and disadvantages. The proposed solutions fulfill the requirements resulting from the concept of sustainable development, and specifically from the implementation of green chemistry principles in analytical laboratories. Therefore, particular attention was paid to the description of possible uses of novel, selective stationary phases in extraction techniques, inter alia, polymeric ionic liquids, carbon nanotubes, and silica- and carbon-based sorbents. The methodological solutions, together with properly matched sampling devices for collecting analytes from samples with varying matrix composition, enable us to reduce the number of errors during the sample preparation prior to chromatographic analysis as well as to limit the negative impact of this analytical step on the natural environment and the health of laboratory employees. Copyright © 2013 Elsevier B.V. All rights reserved.

Contact mechanics for poroelastic, fluid-filled media, with application to cartilage.

PubMed

Persson, B N J

2016-12-21

I study a simple contact mechanics model for a poroelastic, fluid-filled solid squeezed against a rigid, randomly rough substrate. I study how the fluid is squeezed out from the interface, and how the area of contact, and the average interfacial separation, change with time. I present numerical results relevant for a human cartilage. I show that for a fluid filled poroelastic solid the probability of cavitation (and the related wear as the cavities implode), and dynamical scraping (defined below and in Hutt and Persson, J. Chem. Phys. 144, 124903 (2016)), may be suppressed by fluid flow from the poroelastic solid into the (roughness induced) interfacial gap between the solids.

Contact mechanics for poroelastic, fluid-filled media, with application to cartilage

NASA Astrophysics Data System (ADS)

Persson, B. N. J.

2016-12-01

I study a simple contact mechanics model for a poroelastic, fluid-filled solid squeezed against a rigid, randomly rough substrate. I study how the fluid is squeezed out from the interface, and how the area of contact, and the average interfacial separation, change with time. I present numerical results relevant for a human cartilage. I show that for a fluid filled poroelastic solid the probability of cavitation (and the related wear as the cavities implode), and dynamical scraping (defined below and in Hutt and Persson, J. Chem. Phys. 144, 124903 (2016)), may be suppressed by fluid flow from the poroelastic solid into the (roughness induced) interfacial gap between the solids.

Saccharose solid matrix embedded proteins: a new method for sample preparation for X-ray absorption spectroscopy.

PubMed

Ascone, I; Sabatucci, A; Bubacco, L; Di Muro, P; Salvato, B

2000-01-01

In this study, solid samples of hemoglobin and hemocyanin have been prepared by embedding the proteins into a saccharose-based matrix. These materials have been developed specifically for specimens for X-ray absorption spectroscopy (XAS). The preservation of protein conformation and active site organization was tested, making comparisons between the solid and the corresponding liquid samples, using resonance Raman, infra red, fluorescence and XAS. The XAS spectra of irradiated solid and liquid samples were then compared, and the preservation of biological activity of the proteins during both preparation procedure and X-ray irradiation was assessed. In all cases, the measurements clearly demonstrate that protein solid samples are both structurally and functionally quite well preserved, much better than those in the liquid state. The saccharose matrix provides an excellent protection against X-ray damages, allowing for longer exposure to the X-ray beam. Moreover, the demonstrated long-term stability of samples permits their preparation and storage in optimal conditions, allowing for the repetition of data collection with the same sample in several experimental sessions. The very high protein concentration that can be reached results in a significantly better signal-to-noise ratio, particularly useful for high molecular weight proteins with a low metal-to-protein ratio. On the bases of the above-mentioned results, we propose the new method as a standard procedure for the preparation of biological samples to be used for XAS spectroscopy.

Quantifying the risks of solid aerosol geoengineering: the role of fundamental material properties

NASA Astrophysics Data System (ADS)

Dykema, J. A.; Keutsch, F. N.; Keith, D.

2017-12-01

Solid aerosols have been considered as an alternative to sulfate aerosols for solar geoengineering due to their optical and chemical properties, which lead to different and possibly more attractive risk profiles. Solid aerosols can achieve higher solar scattering efficiency due to their higher refractive index, and in some cases may also be less effective absorbers of thermal infrared radiation. The optical properties of solid aerosols are however sensitive functions of the detailed physical properties of solid materials in question. The relevant details include the exact crystalline structure of the aerosols, the physical size of the particles, and interactions with background stratospheric molecular and particulate constituents. In this work, we examine the impact of these detailed physical properties on the radiative properties of calcite (CaCO3) solid aerosols. We examine how crystal morphology, size, chemical reactions, and interaction with background stratospheric aerosol may alter the scattering and absorption properties of calcite aerosols for solar and thermal infrared radiation. For example, in small particles, crystal lattice vibrations associated with the particle surface may lead to substantially different infrared absorption properties than bulk materials. We examine the wavelength dependence of absorption by the particles, which may lead to altered patterns of stratospheric radiative heating and equilibrium temperatures. Such temperature changes can lead to dynamical changes, with consequences for both stratospheric composition and tropospheric climate. We identify important uncertainties in the current state of understanding, investigate risks associated with these uncertainties, and survey potential approaches to quantitatively improving our knowledge of the relevant material properties.

Investigation of Tank 241-AN-101 Floating Solids

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

Kraft, Douglas P.; Meznarich, H. K.

Tank 241-AN-101 is the receiver tank for retrieval of several C-Farms waste tanks, including Tanks 241-C-102 and 241-C-111. Tank 241 C 111 received first-cycle decontamination waste from the bismuth phosphate process and Plutonium and Uranium Extraction cladding waste, as well as hydraulic fluid. Three grab samples, 1AN-16-01, 1AN-16-01A, and 1AN-16-01B, were collected at the surface of Tank 241-AN-101 on April 25, 2016, after Tank 241-C-111 retrieval was completed. Floating solids were observed in the three grab samples in the 11A hot cell after the samples were received at the 222-S Laboratory. Routine chemical analyses, solid phase characterization on the floatingmore » and settled solids, semivolatile organic analysis mainly on the aqueous phase for identification of degradation products of hydraulic fluids were performed. Investigation of the floating solids is reported.« less

Micropyrolyzer for chemical analysis of liquid and solid samples

DOEpatents

Mowry, Curtis D.; Morgan, Catherine H.; Manginell, Ronald P.; Frye-Mason, Gregory C.

2006-07-18

A micropyrolyzer has applications to pyrolysis, heated chemistry, and thermal desorption from liquid or solid samples. The micropyrolyzer can be fabricated from semiconductor materials and metals using standard integrated circuit technologies. The micropyrolyzer enables very small volume samples of less than 3 microliters and high sample heating rates of greater than 20.degree. C. per millisecond. A portable analyzer for the field analysis of liquid and solid samples can be realized when the micropyrolyzer is combined with a chemical preconcentrator, chemical separator, and chemical detector. Such a portable analyzer can be used in a variety of government and industrial applications, such as non-proliferation monitoring, chemical and biological warfare detection, industrial process control, water and air quality monitoring, and industrial hygiene.

Biomass Compositional Analysis Laboratory Procedures | Bioenergy | NREL

Science.gov Websites

Compositional Analysis This procedure describes methods for sample drying and size reduction, obtaining samples methods used to determine the amount of solids or moisture present in a solid or slurry biomass sample as values? We have found that neutral detergent fiber (NDF) and acid detergent fiber (ADF) methods report

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING SOLID FOOD SAMPLES FOR ANALYSIS OF POLAR ORGANIC POLLUTANTS (SOP-5.28)

EPA Science Inventory

This SOP describes the extraction and preparation of a solid food sample for analysis of acidic persistent organic pollutants such as acid herbicides, pentachlorphenol, and 3,5,6-trichloro-2-phenol. It covers the extraction, concentration and derivatization of samples that are to...

40 CFR 258.53 - Ground-water sampling and analysis requirements.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 24 2010-07-01 2010-07-01 false Ground-water sampling and analysis requirements. 258.53 Section 258.53 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES CRITERIA FOR MUNICIPAL SOLID WASTE LANDFILLS Ground-Water Monitoring and Corrective Action § 258.53 Ground-water sampling and analysi...

40 CFR 258.53 - Ground-water sampling and analysis requirements.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 26 2013-07-01 2013-07-01 false Ground-water sampling and analysis requirements. 258.53 Section 258.53 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES CRITERIA FOR MUNICIPAL SOLID WASTE LANDFILLS Ground-Water Monitoring and Corrective Action § 258.53 Ground-water sampling and analysi...

QUANTIFICATION OF 2,4-D ON SOLID-PHASE EXPOSURE SAMPLING MEDIA BY LC/MS/MS

EPA Science Inventory

Three types of solid phase chemical exposure sampling media: cellulose, polyurethane foam (PUF) and XAD-2, were analyzed for 2,4-D and the amine salts of 2,4-D. Individual samples were extracted into acidified methanol and the extracts were analyzed via LC/MS/MS using electrospra...

24-HOUR DIFFUSIVE SAMPLING OF TOXIC VOCS IN AIR ONTO CARBOPACK X SOLID ADSORBENT FOLLOWED BY THERMAL DESORPTION/GC/MS ANALYSIS - LABORATORY STUDIES

EPA Science Inventory

Diffusive sampling of a mixture of 42 volatile organic compounds (VOCs) in humidified, purified air onto the solid adsorbent Carbopack X was evaluated under controlled laboratory conditions. The evaluation included variations in sample air temperature, relative humidity, and ozon...

Geology and ground-water resources of Winkler County, Texas

USGS Publications Warehouse

Garza, Sergio; Wesselman, John B.

1963-01-01

The chemical quality of the water in the principal aquifers is generally acceptable for industry and for public supply. About two-thirds of the samples collected from fresh-water wells had a dissolved-solids content of less than 1,000 ppm (parts per million) ; however, some samples in a few areas were hard and were high in fluoride and silica. Samples from wells in polluted areas contained dissolved solids ranging from about 1,400 to 71,100 ppm. Two comprehensive analyses of water samples from the Rustler formation showed a dissolved-solids content of 18,400 ppm. and 157,000 ppm. In most of the water produced with the oil in the Hendrick oil field, the content of dissolved solids ranged from about 4,000 to about 10,000 ppm. The water produced with the oil in the rest of the oil fields in Winkler County was mainly brine.

Dynamic nuclear polarization in solid samples by electrical-discharge-induced radicals

NASA Astrophysics Data System (ADS)

Katz, Itai; Blank, Aharon

2015-12-01

Dynamic nuclear polarization (DNP) is a method for enhancing nuclear magnetic resonance (NMR) signals that has many potential applications in chemistry and medicine. Traditionally, DNP signal enhancement is achieved through the use of exogenous radicals mixed in a solution with the molecules of interest. Here we show that proton DNP signal enhancements can be obtained for solid samples without the use of solvent and exogenous radicals. Radicals are generated primarily on the surface of a solid sample using electrical discharges. These radicals are found suitable for DNP. They are stable under moderate vacuum conditions, yet readily annihilate upon compound dissolution or air exposure. This feature makes them attractive for use in medical applications, where the current variety of radicals used for DNP faces regulatory problems. In addition, this solvent-free method may be found useful for analytical NMR of solid samples which cannot tolerate solvents, such as certain pharmaceutical products.

Analysis of emerging organic contaminants in water, fish and suspended particulate matter (SPM) in the Joint Danube Survey using solid-phase extraction followed by UHPLC-MS-MS and GC-MS analysis.

PubMed

Loos, Robert; Tavazzi, Simona; Mariani, Giulio; Suurkuusk, Gert; Paracchini, Bruno; Umlauf, Gunther

2017-12-31

In the third Joint Danube Survey (JDS3), emerging organic contaminants were analysed in the dissolved water phase of samples from the Danube River and its major tributaries. Analyses were performed using solid-phase extraction (SPE) followed by ultra-high-pressure liquid chromatography triple-quadrupole mass spectrometry (UHPLC-MS-MS) and gas chromatography-mass spectrometry (GC-MS). The polar organic compounds analysed by UHPLC-MS-MS were 1H-benzotriazole, methylbenzotriazoles, carbamazepine, 10,11-dihydro-10,11-dihydroxy-carbamazepine, diclofenac, sulfamethox-azole, 2,4-D (2,4-dichlorophenoxyacetic acid), MCPA (2-methyl-4-chlorophenoxyacetic acid), metolachlor, cybutryne (irgarol), terbutryn, DEET (N,N-diethyl-m-toluamide), and several perfluoroalkyl acids (C 6 -C 9 ; C 8 =perfluorooctanoic acid (PFOA)) and perfluorooctansulfonic acid (PFOS). In addition, several organophosphorus flame retardants were analysed by GC-MS. The most relevant compounds identified in the 71 water samples, in terms of highest median and maximum concentrations, were 1H-benzotriazole, tris(1-chloro-2-propyl)phosphate (TCPP), methylbenzotriazoles, carbama-zepine and its metabolite, DEET, sulfamethoxazole, tris(isobutyl)phosphate (TiBP), tris(2-chloroethyl)phosphate (TCEP), PFOA, PFOS and diclofenac. The concentrations of these compounds in the samples were generally below the environmental quality standard (EQS) threshold values, with the exception of PFOS, the concentration of which exceeded the annual average water EQS limit of 0.65ng/L along the whole river, and also exceeded the fish biota EQS of 9.1μg/kg. In addition, the proposed EQS for diclofenac, of 0.1μg/L, was exceeded in the Arges River in Romania (255ng/L). Copyright © 2017 The Author(s). Published by Elsevier B.V. All rights reserved.

Comprehensive non-targeted analysis of contaminated groundwater of a former ammunition destruction site using 1H-NMR and HPLC-SPE-NMR/TOF-MS.

PubMed

Godejohann, Markus; Heintz, Lea; Daolio, Cristina; Berset, Jean-Daniel; Muff, Daniel

2009-09-15

The aim of the present study was to explore the capabilities of the combination of 1H NMR (proton nuclear magnetic resonance) mixture analysis and HPLC-SPE-NMR/TOF-MS (high-performance liquid chromatography coupled to solid-phase extraction and nuclear magnetic resonance and time-of-flight mass spectrometry) for the characterization of xenobiotic contaminants in groundwater samples. As an example, solid-phase extracts of two groundwater samples taken from a former ammunition destruction site in Switzerland were investigated. 1H NMR spectra of postcolumn SPE enriched compounds, together with accurate mass measurements, allowed the structural elucidation of unknowns. This untargeted approach allowed us to identify expected residues of explosives such as 2,4,6-trinitrotoluene (2,4,6-TNT), Hexogen (RDX) and Octogen (HMX), degradation products of TNT (1,3,5-trinitrobenzene (1,3,5-TNB), 2-amino-4,6-dinitrotoluene (2-A-4,6-DNT), 3,5-dinitrophenol (3,5-DNP), 3,5-dinitroaniline (3,5-DNA), 2,6-dinitroanthranite, and 2-Hydroxy-4,6-dinitrobenzonitrile), benzoic acid, Bisphenol A (a known endocrine disruptor compound), and some toxicologically relevant additives for propelling charges: Centralite I (1,3-diethyl-1,3-diphenylurea), DPU (N,N-diphenylurethane), N,N-diphenylcarbamate (Acardite II), and N-methyl-N-phenylurethane. To our knowledge, this is the first report of the presence of these additives in environmental samples. Extraction recoveries for Centralite I and DPU have been determined. Contaminants identified by our techniques were quantified based on HPLC-UV (HPLC-ultraviolet detection) and 1H NMR mixture analysis. The concentrations of the contaminants ranged between 0.1 and 48 microg/L assuming 100% recovery for the SPE step.

Analytical procedure for the determination of very volatile organic compounds (C3-C6) in indoor air.

PubMed

Schieweck, Alexandra; Gunschera, Jan; Varol, Deniz; Salthammer, Tunga

2018-05-01

The substance group of very volatile organic compounds (VVOCs) is moving into the focus of indoor air analysis, facing ongoing regulations at international and European levels targeting on indoor air quality and human health. However, there exists at present no validated analysis for the identification and quantification of VVOCs in indoor air. Therefore, the present study targeted on the development of an analytical method in order to sample the maximum possible quantity of VVOCs in indoor air on solid sorbents with subsequent analysis by thermal desorption and coupled gas chromatography/mass spectrometry (TDS-GC/MS). For this purpose, it was necessary to investigate the performance of available sorbents and to optimize the parameters of GC/MS analysis. Stainless steel tubes filled with Carbograph 5TD were applied successfully for low-volume sampling (2-4 l) with minimal breakthrough (< 1%). With the developed method, VVOCs between C 3 and C 6 of different volatility and polarity  can be detected even in trace quantities with low limits of quantitation (LOQ; 1-3 μg m -3 ). Limitations occur for low molecular weight compounds ≤C 3 , especially for polar substances, such as carboxylic acids and for some aldehydes and alcohols. Consequently, established methods for the quantification of these compounds in indoor air cannot be fully substituted yet. At least three different analytical techniques are needed to cover the large spectrum of relevant VVOCs in indoor air. In addition, unexpected reaction products might occur and need to be taken into account to avoid misinterpretation of chromatographic signals. Graphical abstract Solid sorbent sampling of VVOCs (C 3 -C 6 ) in indoor air with subsequent TDS-GC/MS analysis.

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

PubMed

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

2015-08-15

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

Speciation of metal(loid)s in environmental samples by X-ray absorption spectroscopy: a critical review.

PubMed

Gräfe, Markus; Donner, Erica; Collins, Richard N; Lombi, Enzo

2014-04-25

Element specificity is one of the key factors underlying the widespread use and acceptance of X-ray absorption spectroscopy (XAS) as a research tool in the environmental and geo-sciences. Independent of physical state (solid, liquid, gas), XAS analyses of metal(loid)s in complex environmental matrices over the past two decades have provided important information about speciation at environmentally relevant interfaces (e.g. solid-liquid) as well as in different media: plant tissues, rhizosphere, soils, sediments, ores, mineral process tailings, etc. Limited sample preparation requirements, the concomitant ability to preserve original physical and chemical states, and independence from crystallinity add to the advantages of using XAS in environmental investigations. Interpretations of XAS data are founded on sound physical and statistical models that can be applied to spectra of reference materials and mixed phases, respectively. For spectra collected directly from environmental matrices, abstract factor analysis and linear combination fitting provide the means to ascertain chemical, bonding, and crystalline states, and to extract quantitative information about their distribution within the data set. Through advances in optics, detectors, and data processing, X-ray fluorescence microprobes capable of focusing X-rays to micro- and nano-meter size have become competitive research venues for resolving the complexity of environmental samples at their inherent scale. The application of μ-XANES imaging, a new combinatorial approach of X-ray fluorescence spectrometry and XANES spectroscopy at the micron scale, is one of the latest technological advances allowing for lateral resolution of chemical states over wide areas due to vastly improved data processing and detector technology. Copyright © 2014. Published by Elsevier B.V.

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.

Dual analyzer system for surface analysis dedicated for angle-resolved photoelectron spectroscopy at liquid surfaces and interfaces

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

Niedermaier, Inga; Kolbeck, Claudia; Steinrück, Hans-Peter

The investigation of liquid surfaces and interfaces with the powerful toolbox of ultra-high vacuum (UHV)-based surface science techniques generally has to overcome the issue of liquid evaporation within the vacuum system. In the last decade, however, new classes of liquids with negligible vapor pressure at room temperature—in particular, ionic liquids (ILs)—have emerged for surface science studies. It has been demonstrated that particularly angle-resolved X-ray Photoelectron Spectroscopy (ARXPS) allows for investigating phenomena that occur at gas-liquid and liquid-solid interfaces on the molecular level. The results are not only relevant for IL systems but also for liquids in general. In all ofmore » these previous ARXPS studies, the sample holder had to be tilted in order to change the polar detection angle of emitted photoelectrons, which restricted the liquid systems to very thin viscous IL films coating a flat solid support. We now report on the concept and realization of a new and unique laboratory “Dual Analyzer System for Surface Analysis (DASSA)” which enables fast ARXPS, UV photoelectron spectroscopy, imaging XPS, and low-energy ion scattering at the horizontal surface plane of macroscopically thick non-volatile liquid samples. It comprises a UHV chamber equipped with two electron analyzers mounted for simultaneous measurements in 0° and 80° emission relative to the surface normal. The performance of DASSA on a first macroscopic liquid system will be demonstrated.« less

Quality of storm-water runoff, Mililani Town, Oahu, Hawaii, 1980-84

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

Yamane, C.M.; Lum, M.G.

1985-01-01

The data included results from analyses of 300 samples of storm water runoff. Turbidity, suspended solids, Kjeldahl nitrogen, and phosphorus concentrations exceeded the State of Hawaii Department of Health's streamwater standards in more than 50% of the samples. Mercury, lead, and fecal coliform bacteria levels exceeded the US EPAs recommended criteria for either freshwater aquatic life or shellfish harvesting waters in more than half the samples. Other constituents exceeding State or federal standards in at least one sample included pH, cadmium, nitrate plus nitrite, iron, alkalinity, manganese, chromium, copper, zinc, and the pesticides. No statistically significant relationships were found betweenmore » quantity of runoff and concentration of water quality constituents. A first flush effect was observed for chemical oxygen demand, suspended solids, lead, nitrate plus nitrite, fecal coliform bacteria, dissolved solids, and mercury. There were significant differences between the two basins for values of discharge, turbidity, specific conductance, chemical oxygen demand, suspended solids, nitrate plus nitrite, phosphorus, lead, dissolved solids, and mercury. The larger basin had higher median and maximum values, and wider ranges of values. 28 refs., 10 figs., 7 tabs.« less

Preparation of amorphous solid dispersions by rotary evaporation and KinetiSol Dispersing: approaches to enhance solubility of a poorly water-soluble gum extract.

PubMed

Bennett, Ryan C; Brough, Chris; Miller, Dave A; O'Donnell, Kevin P; Keen, Justin M; Hughey, Justin R; Williams, Robert O; McGinity, James W

2015-03-01

Acetyl-11-keto-β-boswellic acid (AKBA), a gum resin extract, possesses poor water-solubility that limits bioavailability and a high melting point making it difficult to successfully process into solid dispersions by fusion methods. The purpose of this study was to investigate solvent and thermal processing techniques for the preparation of amorphous solid dispersions (ASDs) exhibiting enhanced solubility, dissolution rates and bioavailability. Solid dispersions were successfully produced by rotary evaporation (RE) and KinetiSol® Dispersing (KSD). Solid state and chemical characterization revealed that ASD with good potency and purity were produced by both RE and KSD. Results of the RE studies demonstrated that AQOAT®-LF, AQOAT®-MF, Eudragit® L100-55 and Soluplus with the incorporation of dioctyl sulfosuccinate sodium provided substantial solubility enhancement. Non-sink dissolution analysis showed enhanced dissolution properties for KSD-processed solid dispersions in comparison to RE-processed solid dispersions. Variances in release performance were identified when different particle size fractions of KSD samples were analyzed. Selected RE samples varying in particle surface morphologies were placed under storage and exhibited crystalline growth following solid-state stability analysis at 12 months in comparison to stored KSD samples confirming amorphous instability for RE products. In vivo analysis of KSD-processed solid dispersions revealed significantly enhanced AKBA absorption in comparison to the neat, active substance.

Effects of Drying Process on an IgG1 Monoclonal Antibody Using Solid-State Hydrogen Deuterium Exchange with Mass Spectrometric Analysis (ssHDX-MS).

PubMed

Moussa, Ehab M; Wilson, Nathan E; Zhou, Qi Tony; Singh, Satish K; Nema, Sandeep; Topp, Elizabeth M

2018-01-03

Lyophilization and spray drying are widely used to manufacture solid forms of therapeutic proteins. Lyophilization is used to stabilize proteins vulnerable to degradation in solution, whereas spray drying is mainly used to prepare inhalation powders or as an alternative to freezing for storing bulk drug substance. Both processes impose stresses that may adversely affect protein structure, stability and bioactivity. Here, we compared lyophilization with and without controlled ice nucleation, and spray drying for their effects on the solid-state conformation and matrix interactions of a model IgG1 monoclonal antibody (mAb). Solid-state conformation and matrix interactions of the mAb were probed using solid-state hydrogen-deuterium exchange with mass spectrometric analysis (ssHDX-MS), and solid-state Fourier transform infrared (ssFTIR) and solid-state fluorescence spectroscopies. mAb conformation and/or matrix interactions were most perturbed in mannitol-containing samples and the distribution of states was more heterogeneous in sucrose and trehalose samples that were spray dried. The findings demonstrate the sensitivity of ssHDX-MS to changes weakly indicated by spectroscopic methods, and support the broader use of ssHDX-MS to probe formulation and process effects on proteins in solid samples.

Magnetic Resonance Imaging and Velocity Mapping in Chemical Engineering Applications.

PubMed

Gladden, Lynn F; Sederman, Andrew J

2017-06-07

This review aims to illustrate the diversity of measurements that can be made using magnetic resonance techniques, which have the potential to provide insights into chemical engineering systems that cannot readily be achieved using any other method. Perhaps the most notable advantage in using magnetic resonance methods is that both chemistry and transport can be followed in three dimensions, in optically opaque systems, and without the need for tracers to be introduced into the system. Here we focus on hydrodynamics and, in particular, applications to rheology, pipe flow, and fixed-bed and gas-solid fluidized bed reactors. With increasing development of industrially relevant sample environments and undersampling data acquisition strategies that can reduce acquisition times to <1 s, magnetic resonance is finding increasing application in chemical engineering research.

Headspace-Solid-Phase Microextraction-Gas Chromatography as Analytical Methodology for the Determination of Volatiles in Wild Mushrooms and Evaluation of Modifications Occurring during Storage

PubMed Central

Costa, Rosaria; De Grazia, Selenia; Grasso, Elisa; Trozzi, Alessandra

2015-01-01

Mushrooms are sources of food, medicines, and agricultural means. Not much is reported in the literature about wild species of the Mediterranean flora, although many of them are traditionally collected for human consumption. The knowledge of their chemical constituents could represent a valid tool for both taxonomic and physiological characterizations. In this work, a headspace-solid-phase microextraction (HS-SPME) method coupled with GC-MS and GC-FID was developed to evaluate the volatile profiles of ten wild mushroom species collected in South Italy. In addition, in order to evaluate the potential of this analytical methodology for true quantitation of volatiles, samples of the cultivated species Agaricus bisporus were analyzed. The choice of this mushroom was dictated by its ease of availability in the food market, due to the consistent amounts required for SPME method development. For calibration of the main volatile compounds, the standard addition method was chosen. Finally, the assessed volatile composition of A. bisporus was monitored in order to evaluate compositional changes occurring during storage, which represents a relevant issue for such a wide consumption edible product. PMID:25945282

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

EPA Pesticide Factsheets

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

Detection and Quantification of Nitrogen Compounds in the First Drilled Martian Solid Samples by the Sample Analysis at Mars (SAM) Instrument Suite on the Mars Science Laboratory (MSL)

NASA Technical Reports Server (NTRS)

Stern, Jennifer C.; Navarro-Gonzalez, Rafael; Freissinet, Caroline; McKay, Christopher P.; Archer, P. Douglas, Jr.; Buch, Arnaud; Coll, Patrice; Eigenbrode, Jennifer L.; Franz, Heather B.; Glavin, Daniel P.;

Laser ablation in analytical chemistry - A review

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

Russo, Richard E.; Mao, Xianglei; Liu, Haichen

Laser ablation is becoming a dominant technology for direct solid sampling in analytical chemistry. Laser ablation refers to the process in which an intense burst of energy delivered by a short laser pulse is used to sample (remove a portion of) a material. The advantages of laser ablation chemical analysis include direct characterization of solids, no chemical procedures for dissolution, reduced risk of contamination or sample loss, analysis of very small samples not separable for solution analysis, and determination of spatial distributions of elemental composition. This review describes recent research to understand and utilize laser ablation for direct solid sampling,more » with emphasis on sample introduction to an inductively coupled plasma (ICP). Current research related to contemporary experimental systems, calibration and optimization, and fractionation is discussed, with a summary of applications in several areas.« less

Wetting Properties of EMIIm & its Relevance to Electrospray Design

DTIC Science & Technology

2012-03-12

apparent surface area S Distance separating two grid apertures T Absolute temperature of the test liquid TC Critical temperature of the test liquid V...include the choice of solid materials being used as insulators, emitters or electrodes, thin film surface coatings that have a de- sired high or low...wettability, and changing the solid component surface roughness or temperature during operation.678 An electrospray thruster has been developed by

2013 Chemical reactions at surfaces. Surfaces in Energy and the Environment. Gordon Research Conference and Gordon Research Seminar (April 28 - May 3, 2013 - Les Diablerets, Switzerland)

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

Stair, Peter C.

presentations on chemistry at solid and liquid surfaces of relevance to catalysis, synthesis, photochemistry, environmental science, and tribology. Topics include: Fundamental Surface Chemistry; Catalysis; Solid Liquid and Aerosol Interfaces; Surface Photochemistry; Synthesis of Surfaces; Environmental Interfaces; Hot Topics in Surface Chemical Reactions; Tribology; Gas-Surface Scattering and Reactions; Novel Materials and Environments.

Emerging contaminants at a closed and an operating landfill in Oklahoma

USGS Publications Warehouse

Andrews, William J.; Masoner, Jason R.; Cozzarelli, Isabelle M.

2012-01-01

Landfills are the final depositories for a wide range of solid waste from both residential and commercial sources, and therefore have the potential to produce leachate containing many organic compounds found in consumer products such as pharmaceuticals, plasticizers, disinfectants, cleaning agents, fire retardants, flavorings, and preservatives, known as emerging contaminants (ECs). Landfill leachate was sampled from landfill cells of three different age ranges from two landfills in Central Oklahoma. Samples were collected from an old cell containing solid waste greater than 25 years old, an intermediate age cell with solid waste between 16 and 3 years old, and operating cell with solid waste less than 5 years old to investigate the chemical variability and persistence of selected ECs in landfill leachate of differing age sources. Twenty-eight of 69 analyzed ECs were detected in one or more samples from the three leachate sources. Detected ECs ranged in concentration from 0.11 to 114 μg/L and included 4 fecal and plant sterols, 13 household\\industrial, 7 hydrocarbon, and 4 pesticide compounds. Four ECs were solely detected in the oldest leachate sample, two ECs were solely detected in the intermediate leachate sample, and no ECs were solely detected in the youngest leachate sample. Eleven ECs were commonly detected in all three leachate samples and are an indication of the contents of solid waste deposited over several decades and the relative resistance of some ECs to natural attenuation processes in and near landfills.

Broth versus solid agar culture of swab samples of cadaveric allograft musculoskeletal tissue.

PubMed

Varettas, Kerry

2013-12-01

As part of the donor assessment protocol, bioburden assessment must be performed on allograft musculoskeletal tissue samples collected at the time of tissue retrieval. Swab samples of musculoskeletal tissue allografts from cadaveric donors are received at the microbiology department of the South Eastern Area Laboratory Services (Australia) to determine the presence of bacteria and fungi. This study will review the isolation rate of organisms from solid agar and broth culture of swab samples of cadaveric allograft musculoskeletal tissue over a 6-year period, 2006-2011. Swabs were inoculated onto horse blood agar (anaerobic, 35 °C) and chocolate agar (CO2, 35 °C) and then placed into a cooked meat broth (aerobic, 35 °C). A total of 1,912 swabs from 389 donors were received during the study period. 557 (29.1 %) swabs were culture positive with the isolation of 713 organisms, 249 (34.9 %) from solid agar culture and an additional 464 (65.1 %) from broth culture only. This study has shown that the broth culture of cadaveric allograft musculoskeletal swab samples recovered a greater amount of organisms than solid agar culture. Isolates such as Clostridium species and Staphylococcus aureus would not have been isolated from solid agar culture alone. Broth culture is an essential part of the bioburden assessment protocol of swab samples of cadaveric allograft musculoskeletal tissue in this laboratory.

Possibilities of municipal solid waste incinerator fly ash utilisation.

PubMed

Hartmann, Silvie; Koval, Lukáš; Škrobánková, Hana; Matýsek, Dalibor; Winter, Franz; Purgar, Amon

2015-08-01

Properties of the waste treatment residual fly ash generated from municipal solid waste incinerator fly ash were investigated in this study. Six different mortar blends with the addition of the municipal solid waste incinerator fly ash were evaluated. The Portland cement replacement levels of the municipal solid waste incinerator fly ash used were 25%, 30% and 50%. Both, raw and washed municipal solid waste incinerator fly ash samples were examined. According to the mineralogical composition measurements, a 22.6% increase in the pozzolanic/hydraulic properties was observed for the washed municipal solid waste incinerator fly ash sample. The maximum replacement level of 25% for the washed municipal solid waste incinerator fly ash in mortar blends was established in order to preserve the compressive strength properties. Moreover, the leaching characteristics of the crushed mortar blend was analysed in order to examine the immobilisation of its hazardous contents. © The Author(s) 2015.

Comparative Analyses of Creep Models of a Solid Propellant

NASA Astrophysics Data System (ADS)

Zhang, J. B.; Lu, B. J.; Gong, S. F.; Zhao, S. P.

2018-05-01

The creep experiments of a solid propellant samples under five different stresses are carried out at 293.15 K and 323.15 K. In order to express the creep properties of this solid propellant, the viscoelastic model i.e. three Parameters solid, three Parameters fluid, four Parameters solid, four Parameters fluid and exponential model are involved. On the basis of the principle of least squares fitting, and different stress of all the parameters for the models, the nonlinear fitting procedure can be used to analyze the creep properties. The study shows that the four Parameters solid model can best express the behavior of creep properties of the propellant samples. However, the three Parameters solid and exponential model cannot very well reflect the initial value of the creep process, while the modified four Parameters models are found to agree well with the acceleration characteristics of the creep process.

The influence of baking fuel on residues of polycyclic aromatic hydrocarbons and heavy metals in bread.

PubMed

Ahmed, M T; Abdel Hadi el-S; el-Samahy, S; Youssof, K

2000-12-30

The influence of fuel type used to bake bread on the spectrum and concentrations of some polycyclic aromatic hydrocarbons and heavy metals in baked bread was assessed. Bread samples were collected from different bakeries operated by either electricity, solar, mazot or solid waste and their residue content of PAHs and heavy metals was assessed. The total concentration of PAHs detected in mazot, solar, solid waste and electricity operated bakeries had an average of 320.6, 158.4, 317.3 and 25.5 microgkg(-1), respectively. Samples collected from mazot, solar and solid waste operated bakeries have had a wide spectrum of PAHs, in comparison to that detected in bread samples collected from electricity operated bakeries. Lead had the highest concentrations in the four groups of bread samples, followed by nickel, while the concentrations of zinc and cadmium were the least. The concentration of lead detected in bread samples produced from mazot, solar, solid waste and electricity fueled bakeries were 1375.5, 1114, 1234, and 257.3 microgkg(-1), respectively. Estimated daily intake of PAHs based on bread consumption were 48.2, 28.5, 80. 1, and 4.8 microg per person per day for bread produced in bakeries using mazot, solar, solid waste and electricity, respectively. Meanwhile, the estimated daily intake of benzo (a) pyrene were 3.69, 2.65, 8.1, and 0.81 microg per person per day for bread sample baked with mazot, solar, solid waste and electricity, respectively. The daily intake of lead, based on bread consumption was 291, 200.5, 222, and 46.31 microg per person per day for bread sample baked with mazot, solar, solid waste and electricity, respectively. The present work has indicated the comparatively high level of daily intake of benzo (a) pyrene and lead in comparison to levels reported from many other countries and those recommended by international regulatory bodies. It is probable that residues detected in bread samples are partially cereal-borne but there is strong evidence that the process of baking and the gases emitted are responsible for most of the contamination load.

Solid state SPS microwave generation and transmission study. Volume 2, phase 2: Appendices

NASA Technical Reports Server (NTRS)

Maynard, O. E.

1980-01-01

The solid state sandwich concept for SPS was further defined. The design effort concentrated on the spacetenna, but did include some system analysis for parametric comparison reasons. Basic solid state microwave devices were defined and modeled. An initial conceptual subsystems and system design was performed as well as sidelobe control and system selection. The selected system concept and parametric solid state microwave power transmission system data were assessed relevant to the SPS concept. Although device efficiency was not a goal, the sensitivities to design of this efficiency were parametrically treated. Sidelobe control consisted of various single step tapers, multistep tapers and Gaussian tapers. A hybrid concept using tubes and solid state was evaluated. Thermal analyses are included with emphasis on sensitivities to waste heat radiator form factor, emissivity, absorptivity, amplifier efficiency, material and junction temperature.

Microfluidic multiplexing of solid-state nanopores

NASA Astrophysics Data System (ADS)

Jain, Tarun; Rasera, Benjamin C.; Guerrero, Ricardo Jose S.; Lim, Jong-Min; Karnik, Rohit

2017-12-01

Although solid-state nanopores enable electronic analysis of many clinically and biologically relevant molecular structures, there are few existing device architectures that enable high-throughput measurement of solid-state nanopores. Herein, we report a method for microfluidic integration of multiple solid-state nanopores at a high density of one nanopore per (35 µm2). By configuring microfluidic devices with microfluidic valves, the nanopores can be rinsed from a single fluid input while retaining compatibility for multichannel electrical measurements. The microfluidic valves serve the dual purpose of fluidic switching and electric switching, enabling serial multiplexing of the eight nanopores with a single pair of electrodes. Furthermore, the device architecture exhibits low noise and is compatible with electroporation-based in situ nanopore fabrication, providing a scalable platform for automated electronic measurement of a large number of integrated solid-state nanopores.

Low-dose ionizing radiation increases the mortality risk of solid cancers in nuclear industry workers: A meta-analysis.

PubMed

Qu, Shu-Gen; Gao, Jin; Tang, Bo; Yu, Bo; Shen, Yue-Ping; Tu, Yu

2018-05-01

Low-dose ionizing radiation (LDIR) may increase the mortality of solid cancers in nuclear industry workers, but only few individual cohort studies exist, and the available reports have low statistical power. The aim of the present study was to focus on solid cancer mortality risk from LDIR in the nuclear industry using standard mortality ratios (SMRs) and 95% confidence intervals. A systematic literature search through the PubMed and Embase databases identified 27 studies relevant to this meta-analysis. There was statistical significance for total, solid and lung cancers, with meta-SMR values of 0.88, 0.80, and 0.89, respectively. There was evidence of stochastic effects by IR, but more definitive conclusions require additional analyses using standardized protocols to determine whether LDIR increases the risk of solid cancer-related mortality.

Detection of silver nanoparticles in parsley by solid sampling high-resolution-continuum source atomic absorption spectrometry.

PubMed

Feichtmeier, Nadine S; Leopold, Kerstin

2014-06-01

In this work, we present a fast and simple approach for detection of silver nanoparticles (AgNPs) in biological material (parsley) by solid sampling high-resolution-continuum source atomic absorption spectrometry (HR-CS AAS). A novel evaluation strategy was developed in order to distinguish AgNPs from ionic silver and for sizing of AgNPs. For this purpose, atomisation delay was introduced as significant indication of AgNPs, whereas atomisation rates allow distinction of 20-, 60-, and 80-nm AgNPs. Atomisation delays were found to be higher for samples containing silver ions than for samples containing silver nanoparticles. A maximum difference in atomisation delay normalised by the sample weight of 6.27 ± 0.96 s mg(-1) was obtained after optimisation of the furnace program of the AAS. For this purpose, a multivariate experimental design was used varying atomisation temperature, atomisation heating rate and pyrolysis temperature. Atomisation rates were calculated as the slope of the first inflection point of the absorbance signals and correlated with the size of the AgNPs in the biological sample. Hence, solid sampling HR-CS AAS was proved to be a promising tool for identifying and distinguishing silver nanoparticles from ionic silver directly in solid biological samples.

Direct determination of cadmium in foods by solid sampling electrothermal vaporization inductively coupled plasma mass spectrometry using a tungsten coil trap

NASA Astrophysics Data System (ADS)

Zhang, Ying; Mao, Xuefei; Liu, Jixin; Wang, Min; Qian, Yongzhong; Gao, Chengling; Qi, Yuehan

2016-04-01

In this work, a solid sampling device consisting of a tungsten coil trap, porous carbon vaporizer and on-line ashing furnace of a Ni-Cr coil was interfaced with inductively coupled plasma mass spectrometry (ICP-MS). A modified double gas circuit system was employed that was composed of carrier and supplemental gas lines controlled by separate gas mass flow controllers. For Cd determination in food samples using the assembled solid sampling ICP-MS, the optimal ashing and vaporization conditions, flow rate of the argon-hydrogen (Ar/H2) (v:v = 24:1) carrier gas and supplemental gas, and minimum sampling mass were investigated. Under the optimized conditions, the limit of quantification was 0.5 pg and the relative standard deviation was within a 10.0% error range (n = 10). Furthermore, the mean spiked recoveries for various food samples were 99.4%-105.9% (n = 6). The Cd concentrations measured by the proposed method were all within the certified values of the reference materials or were not significantly different (P > 0.05) from those of the microwave digestion ICP-MS method, demonstrating the good accuracy and precision of the solid sampling ICP-MS method for Cd determination in food samples.

Development of solid-state NMR techniques for the characterisation of pharmaceutical compounds

NASA Astrophysics Data System (ADS)

Tatton, Andrew S.

Structural characterisation in the solid state is an important step in understanding the physical and chemical properties of a material. Solid-state NMR techniques applied to solid delivery forms are presented as an alternative to more established structural characterisation methods. The effect of homonuclear decoupling upon heteronuclear couplings is investigated using a combination of experimental and density-matrix simulation results acquired from a 13C-1H spinecho pulse sequence, modulated by scalar couplings. It is found that third-order cross terms under MAS and homonuclear decoupling contribute to strong dephasing effects in the NMR signal. Density-matrix simulations allow access to parameters currently unattainable in experiment, and demonstrate that higher homonuclear decoupling rf nutation frequencies reduce the magnitude of third-order cross terms. 15N-1H spinecho experiments were applied to pharmaceutically relevant samples to differentiate between the number of directly attached protons. Using this method, proton transfer in an acid-base reaction is proven in pharmaceutical salts. The indirect detection of 14N lineshapes via protons obtained using 2D 14N-1H HMQC experiments is presented, where coherence transfer is achieved via heteronuclear through-space dipolar couplings. The importance of fast MAS frequencies is demonstrated, and it is found that increasing the recoupling duration reveals longer range NH proximities. The 2D 14N-1H HMQC method is used to demonstrate the presence of specific hydrogen bonding interactions, and thus aid in identifying molecular association in a cocrystal and an amorphous dispersion. In addition, hydrogen bonding motifs were identified by observing the changes in the 14N quadrupolar parameters between individual molecular components relative to the respective solid delivery form. First-principles calculations of NMR chemical shifts and quadrupolar parameters using the GIPAW method were combined with 14N-1H experimental results to assist with spectral assignment and the identification of the hydrogen bonding interactions.

Assessment of environmental policy implementation in solid waste management in Kathmandu, Nepal.

PubMed

Dangi, Mohan B; Schoenberger, Erica; Boland, John J

2017-06-01

In Nepal, full-fledged environmental legislation was rare before the democratic constitution of 1990. The first law covering the environment and sustainability was the Environment Protection Act 1997. While the Solid Waste Act was introduced in 1987, the problem of solid waste management still surfaces in Kathmandu. In order to understand the bedrock of this unrelenting failure in solid waste management, the manuscript digs deeper into policy implementation by dissecting solid waste rules, environmental legislations, relevant local laws, and solid waste management practices in Kathmandu, Nepal. A very rich field study that included surveys, interviews, site visits, and literature review provided the basis for the article. The study shows that volumes of new Nepalese rules are crafted without effective enforcement of their predecessors and there is a frequent power struggle between local government bodies and central authority in implementing the codes and allocating resources in solid waste management. The study concludes that Kathmandu does not require any new instrument to address solid waste problems; instead, it needs creation of local resources, execution of local codes, and commitment from central government to allow free exercise of these policies.

36 CFR 907.12 - Preparation of an environmental assessment.

Code of Federal Regulations, 2010 CFR

2010-07-01

...) Energy requirements and conservation; (vi) Solid waste; (vii) Transportation; (viii) Community facilities and services; (ix) Social and economic; (x) Historic and aesthetic; and (xi) Other relevant factors...

Rapid habitability assessment of Mars samples by pyrolysis-FTIR

NASA Astrophysics Data System (ADS)

Gordon, Peter R.; Sephton, Mark A.

2016-02-01

Pyrolysis Fourier transform infrared spectroscopy (pyrolysis FTIR) is a potential sample selection method for Mars Sample Return missions. FTIR spectroscopy can be performed on solid and liquid samples but also on gases following preliminary thermal extraction, pyrolysis or gasification steps. The detection of hydrocarbon and non-hydrocarbon gases can reveal information on sample mineralogy and past habitability of the environment in which the sample was created. The absorption of IR radiation at specific wavenumbers by organic functional groups can indicate the presence and type of any organic matter present. Here we assess the utility of pyrolysis-FTIR to release water, carbon dioxide, sulfur dioxide and organic matter from Mars relevant materials to enable a rapid habitability assessment of target rocks for sample return. For our assessment a range of minerals were analyzed by attenuated total reflectance FTIR. Subsequently, the mineral samples were subjected to single step pyrolysis and multi step pyrolysis and the products characterised by gas phase FTIR. Data from both single step and multi step pyrolysis-FTIR provide the ability to identify minerals that reflect habitable environments through their water and carbon dioxide responses. Multi step pyrolysis-FTIR can be used to gain more detailed information on the sources of the liberated water and carbon dioxide owing to the characteristic decomposition temperatures of different mineral phases. Habitation can be suggested when pyrolysis-FTIR indicates the presence of organic matter within the sample. Pyrolysis-FTIR, therefore, represents an effective method to assess whether Mars Sample Return target rocks represent habitable conditions and potential records of habitation and can play an important role in sample triage operations.

Municipal solid waste characterizations and management strategies for the Lower Rio Grande Valley, Texas.

PubMed

Chang, Ni-Bin; Davila, Eric

2008-01-01

The Lower Rio Grande Valley (LRGV or Valley) in Texas, facing the big waste management challenge along the US-Mexico border today, is at the crossroads as a result of the rapid population growth, the scarcity of landfill space, the bi-nation's trade impacts, and the illusive goal of environmental sustainability. This paper offers a unique municipal solid waste investigation with regard to both physical and chemical characteristics leading to illuminate the necessary management policies with greater regional relevancy. With multiple sampling campaigns conducted during the spring of 2005, this study holistically summarizes the composition of solid waste, the statistical distribution patterns of key recyclable items, and the heating value in an uncertain environment. Research findings indicate that high fractions of plastics and paper in the waste stream imply a strong potential for energy recovery. Incineration options are thus bolstered by mildly high heating values across 10 cities in this region, which may lead to save land resources required for final disposal and increase electricity generation in the long run. Additional regression analyses further identify the correlation between recyclable items and heating value, which show that current recycling programs permit no obvious negative impacts on the incineration option. Final statistical hypothesis tests for both the Brownsville-Harlingen-San Benito and the McAllen-Edinburg-Mission metropolitan regions help foster consistent management strategies across the Valley regardless of the trivial differences of waste characteristics in between.

Evaluating the ready biodegradability of two poorly water-soluble substances: comparative approach of bioavailability improvement methods (BIMs).

PubMed

Sweetlove, Cyril; Chenèble, Jean-Charles; Barthel, Yves; Boualam, Marc; L'Haridon, Jacques; Thouand, Gérald

2016-09-01

Difficulties encountered in estimating the biodegradation of poorly water-soluble substances are often linked to their limited bioavailability to microorganisms. Many original bioavailability improvement methods (BIMs) have been described, but no global approach was proposed for a standardized comparison of these. The latter would be a valuable tool as part of a wider strategy for evaluating poorly water-soluble substances. The purpose of this study was to define an evaluation strategy following the assessment of different BIMs adapted to poorly water-soluble substances with ready biodegradability tests. The study was performed with two poorly water-soluble chemicals-a solid, anthraquinone, and a liquid, isodecyl neopentanoate-and five BIMs were compared to the direct addition method (reference method), i.e., (i) ultrasonic dispersion, (ii) adsorption onto silica gel, (iii) dispersion using an emulsifier, (iv) dispersion with silicone oil, and (v) dispersion with emulsifier and silicone oil. A two-phase evaluation strategy of solid and liquid chemicals was developed involving the selection of the most relevant BIMs for enhancing the biodegradability of tested substances. A description is given of a BIM classification ratio (R BIM), which enables a comparison to be made between the different test chemical sample preparation methods used in the various tests. Thereby, using this comparison, the BIMs giving rise to the greatest biodegradability were ultrasonic dispersion and dispersion with silicone oil or with silicone oil and emulsifier for the tested solid chemical, adsorption onto silica gel, and ultrasonic dispersion for the liquid one.

33 CFR 159.126a - Suspended solids test: Type II devices.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 33 Navigation and Navigable Waters 2 2010-07-01 2010-07-01 false Suspended solids test: Type II... Suspended solids test: Type II devices. During the sewage processing test (§ 159.121) 40 effluent samples... suspended solids in accordance with 40 CFR part 136. The arithmetic mean of the total suspended solids in 38...

CHARACTERIZATION OF A PRECIPITATE REACTOR FEED TANK (PRFT) SAMPLE FROM THE DEFENSE WASTE PROCESSING FACILITY (DWPF)

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

Crawford, C.; Bannochie, C.

2014-05-12

A sample of from the Defense Waste Processing Facility (DWPF) Precipitate Reactor Feed Tank (PRFT) was pulled and sent to the Savannah River National Laboratory (SRNL) in June of 2013. The PRFT in DWPF receives Actinide Removal Process (ARP)/ Monosodium Titanate (MST) material from the 512-S Facility via the 511-S Facility. This 2.2 L sample was to be used in small-scale DWPF chemical process cell testing in the Shielded Cells Facility of SRNL. A 1L sub-sample portion was characterized to determine the physical properties such as weight percent solids, density, particle size distribution and crystalline phase identification. Further chemical analysismore » of the PRFT filtrate and dissolved slurry included metals and anions as well as carbon and base analysis. This technical report describes the characterization and analysis of the PRFT sample from DWPF. At SRNL, the 2.2 L PRFT sample was composited from eleven separate samples received from DWPF. The visible solids were observed to be relatively quick settling which allowed for the rinsing of the original shipping vials with PRFT supernate on the same day as compositing. Most analyses were performed in triplicate except for particle size distribution (PSD), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and thermogravimetric analysis (TGA). PRFT slurry samples were dissolved using a mixed HNO3/HF acid for subsequent Inductively Coupled Plasma Atomic Emission Spectroscopy (ICPAES) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) analyses performed by SRNL Analytical Development (AD). Per the task request for this work, analysis of the PRFT slurry and filtrate for metals, anions, carbon and base were primarily performed to support the planned chemical process cell testing and to provide additional component concentrations in addition to the limited data available from DWPF. Analysis of the insoluble solids portion of the PRFT slurry was aimed at detailed characterization of these solids (TGA, PSD, XRD and SEM) in support of the Salt IPT chemistry team. The overall conclusions from analyses performed in this study are that the PRFT slurry consists of 0.61 Wt.% insoluble MST solids suspended in a 0.77 M [Na+] caustic solution containing various anions such as nitrate, nitrite, sulfate, carbonate and oxalate. The corresponding measured sulfur level in the PRFT slurry, a critical element for determining how much of the PRFT slurry gets blended into the SRAT, is 0.437 Wt.% TS. The PRFT slurry does not contain insoluble oxalates nor significant quantities of high activity sludge solids. The lack of sludge solids has been alluded to by the Salt IPT chemistry team in citing that the mixing pump has been removed from Tank 49H, the feed tank to ARP-MCU, thus allowing the sludge solids to settle out. The PRFT aqueous slurry from DWPF was found to contain 5.96 Wt.% total dried solids. Of these total dried solids, relatively low levels of insoluble solids (0.61 Wt.%) were measured. The densities of both the filtrate and slurry were 1.05 g/mL. Particle size distribution of the PRFT solids in filtered caustic simulant and XRD analysis of washed/dried PRFT solids indicate that the PRFT slurry contains a bimodal distribution of particles in the range of 1 and 6 μm and that the particles contain sodium titanium oxide hydroxide Na2Ti2O4(OH)2 crystalline material as determined by XRD. These data are in excellent agreement with similar data obtained from laboratory sampling of vendor supplied MST. Scanning Electron Microscopy (SEM) combined with Energy Dispersive X-ray Spectroscopy (EDS) analysis of washed/dried PRFT solids shows the particles to be like previous MST analyses consisting of irregular shaped micron-sized solids consisting primarily of Na and Ti. Thermogravimetric analysis of the washed and unwashed PRFT solids shows that the washed solids are very similar to MST solids. The TGA mass loss signal for the unwashed solids shows similar features to TGA performed on cellulose nitrate filter paper indicating significant presence of the deteriorated filter in this unwashed sample. Neither the washed nor unwashed PRFT solids TGA traces showed any features that would indicate presence of sodium oxalate solids. The PRFT Filtrate elemental analysis shows that Na, S and Al are major soluble species with trace levels of B, Cr, Cu, K, Li, Si, Tc, Th and U present. Nitrate, nitrite, sulfate, oxalate, carbonate and hydroxide are major soluble anion species. There is good agreement between the analyzed TOC and the total carbon calculated from the sum of oxalate and minor species formate. Comparison of the amount and speciation of the carbon species between filtrate and slurry indicates no significant carbon-containing species, e.g., sodium oxalate, are present in the slurry solids. Dissolution of the PRFT slurry and subsequent analysis shows that Na, Ti, Si and U are the major elements present on a Wt.% total dried solids basis with 30, 5.8 and 0.47 and 0.11 Wt.% total dried solids, respectively. The amount of Al in the dissolved PRFT slurry is less than that calculated from the PRFT filtrate alone which suggests that the mixed acid digestion used in this work is not optimized for Al recovery. The concentrations of Ca, Fe, Hg and U are all low (at or below 0.11 wt%) and there is no detectable Mn or Ni present which indicates no significant HLW sludge solids are present in the PRFT slurry sample.« less

Specific Conductance and Dissolved-Solids Characteristics for the Green River and Muddy Creek, Wyoming, Water Years 1999-2008

USGS Publications Warehouse

Clark, Melanie L.; Davidson, Seth L.

2009-01-01

Southwestern Wyoming is an area of diverse scenery, wildlife, and natural resources that is actively undergoing energy development. The U.S. Department of the Interior's Wyoming Landscape Conservation Initiative is a long-term science-based effort to assess and enhance aquatic and terrestrial habitats at a landscape scale, while facilitating responsible energy development through local collaboration and partnerships. Water-quality monitoring has been conducted by the U.S. Geological Survey on the Green River near Green River, Wyoming, and Muddy Creek near Baggs, Wyoming. This monitoring, which is being conducted in cooperation with State and other Federal agencies and as part of the Wyoming Landscape Conservation Initiative, is in response to concerns about potentially increased dissolved solids in the Colorado River Basin as a result of energy development. Because of the need to provide real-time dissolved-solids concentrations for the Green River and Muddy Creek on the World Wide Web, the U.S. Geological Survey developed regression equations to estimate dissolved-solids concentrations on the basis of continuous specific conductance using relations between measured specific conductance and dissolved-solids concentrations. Specific conductance and dissolved-solids concentrations were less varied and generally lower for the Green River than for Muddy Creek. The median dissolved-solids concentration for the site on the Green River was 318 milligrams per liter, and the median concentration for the site on Muddy Creek was 943 milligrams per liter. Dissolved-solids concentrations ranged from 187 to 594 milligrams per liter in samples collected from the Green River during water years 1999-2008. Dissolved-solids concentrations ranged from 293 to 2,485 milligrams per liter in samples collected from Muddy Creek during water years 2006-08. The differences in dissolved-solids concentrations in samples collected from the Green River compared to samples collected from Muddy Creek reflect the different basin characteristics. Relations between specific conductance and dissolved-solids concentrations were statistically significant for the Green River (p-value less than 0.001) and Muddy Creek (p-value less than 0.001); therefore, specific conductance can be used to estimate dissolved-solids concentrations. Using continuous specific conductance values to estimate dissolved solids in real-time on the World Wide Web increases the amount and improves the timeliness of data available to water managers for assessing dissolved-solids concentrations in the Colorado River Basin.

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.

Improving the accuracy of sediment-associated constituent concentrations in whole storm water samples by wet-sieving

USGS Publications Warehouse

Selbig, W.R.; Bannerman, R.; Bowman, G.

2007-01-01

Sand-sized particles (>63 ??m) in whole storm water samples collected from urban runoff have the potential to produce data with substantial bias and/or poor precision both during sample splitting and laboratory analysis. New techniques were evaluated in an effort to overcome some of the limitations associated with sample splitting and analyzing whole storm water samples containing sand-sized particles. Wet-sieving separates sand-sized particles from a whole storm water sample. Once separated, both the sieved solids and the remaining aqueous (water suspension of particles less than 63 ??m) samples were analyzed for total recoverable metals using a modification of USEPA Method 200.7. The modified version digests the entire sample, rather than an aliquot, of the sample. Using a total recoverable acid digestion on the entire contents of the sieved solid and aqueous samples improved the accuracy of the derived sediment-associated constituent concentrations. Concentration values of sieved solid and aqueous samples can later be summed to determine an event mean concentration. ?? ASA, CSSA, SSSA.

Cross-polarization/magic-angle sample-spinning /sup 13/C NMR spectroscopic study of chlorophyll a in the solid state

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

Brown, C.E.; Spencer, R.B.; Burger, V.T.

1984-01-01

Solid-state cross-polarization/magic-angle sample-spinning /sup 13/C NMR spectra have been recorded on chlorophyll a-water aggregates, methyl pyrochlorophyllide a, and methyl pyropheophorbide a. Spectra have also been collected under a decoupling regime in which resonances of certain hydrogen-bearing carbon atoms are suppressed. These observations are used to assign the solid-state spectra. 18 references, 2 figures, 1 table.

Establishment of a cell-based wound healing assay for bio-relevant testing of wound therapeutics.

PubMed

Planz, Viktoria; Wang, Jing; Windbergs, Maike

Predictive in vitro testing of novel wound therapeutics requires adequate cell-based bio-assays. Such assays represent an integral part during preclinical development as pre-step before entering in vivo studies. Simple "scratch tests" based on defected skin cell monolayers exist, however these can solely be used for testing liquids, as cell monolayer destruction and excessive hydration limit their applicability for (semi-)solid systems like wound dressings. In this context, a cell-based wound healing assay is introduced for rapid and predictive testing of wound therapeutics independent of their physical state in a bio-relevant environment. A novel wound healing assay was established for bio-relevant and predictive testing of (semi-) solid wound therapeutics. The assay allows for physiologically relevant hydration of the tested wound therapeutics at the air-liquid interface and their removal without cell monolayer disruption. In a proof-of-concept study, the applicability and discriminative power could be demonstrated by examining unloaded and drug-loaded wound dressings with two different established wound healing actives (dexpanthenol and metyrapone) and their effect on skin cell behavior. The influence of the released drug on the cells´ healing behavior could successfully be monitored over time. Wound size assessment after 96h resulted in an eight fold smaller wound area for drug treated models compared to the ones treated with unloaded fibers and non-treated wounds. This assay provides valuable first insights towards the establishment of a valid screening and evaluation tool for preclinical wound therapeutic development from liquid to (semi-)solid systems to improve predictability in a simple, yet standardized way. Copyright © 2017 Elsevier Inc. All rights reserved.

Botanical supplements: detecting the transition from ingredients to supplements

USDA-ARS?s Scientific Manuscript database

Methods were developed using flow injection mass spectrometry (FIMS) and chemometrics for the comparison of spectral similarities and differences of 3 botanical ingredients and their supplements: Echinacea purpurea aerial samples and solid and liquid supplements, E. purpurea root samples and solid s...

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING SOLID FOOD SAMPLES FOR ANALYSIS OF PERSISTENT ORGANIC POLLUTANTS (SOP-5.20)

EPA Science Inventory

This SOP describes the procedures for homogenizing, extracting and concentrating solid food samples for persistent organic pollutants such as organochlorine compounds, organophosphate compounds, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, substituted phenols, and...

Determination of low levels of perchlorate in lettuce and spinach using ion chromatography-electrospray ionization mass spectrometry (IC-ESI-MS).

PubMed

Seyfferth, Angelia L; Parker, David R

2006-03-22

A sample preparation method was developed to quantify environmentally relevant (low micrograms per liter) concentrations of perchlorate (ClO4(-)) in leafy vegetables using IC-ESI-MS. Lettuce and spinach were macerated, centrifuged, and filtered, and the aqueous extracts were rendered water-clear using a one-step solid-phase extraction method. Total time for extraction and sample preparation was 6 h. Ion suppression was demonstrated and was likely due to unknown organics still present in the extract solution after cleanup. However, this interference was readily eliminated using a Cl(18)O4(-) internal standard at 1 microg/L in all standards and samples. Hydroponically grown perchlorate-free butterhead lettuce was spiked to either 10.3 or 37.7 microg/kg of fresh weight (FW), and recoveries were between 91 and 98% and between 93 and 101%, respectively. Five types of lettuce and spinach from a local grocery store were then analyzed; they contained from 0.6 to 6.4 microg/kg of FW. Spike recoveries using the store-bought samples ranged from 89 to 100%. The method detection limit for perchlorate in plant extracts is 40 ng/L, and the corresponding minimum reporting limit is 200 ng/L or 0.8 microg/kg of FW.

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

PubMed

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

2013-04-03

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

Water quality assessment using the AREc32 reporter gene assay indicative of the oxidative stress response pathway.

PubMed

Escher, Beate I; Dutt, Mriga; Maylin, Erin; Tang, Janet Y M; Toze, Simon; Wolf, C Roland; Lang, Matti

2012-11-01

The reporter gene assay AREc32 is based on the induction of the Nrf2 mediated oxidative stress response pathway in the human breast cancer cell line MCF7, where eight copies of the antioxidant response element (ARE) are linked to a reporter gene encoding for luciferase. The Nrf2-ARE pathway is responsive to many chemicals that cause oxidative stress, among them a large number of pesticides and skin irritants. We adopted and validated the AREc32 bioassay for water quality testing. tert-Butylhydroquinone served as the positive control, phenol as the negative control and other reactive chemicals were assessed for their specificity. An environmentally relevant reference chemical, benzo(a)pyrene was the most potent inducer of all tested chemicals. The concentration causing an induction ratio (IR) of 1.5 (EC(IR1.5)) was chosen as the effect benchmark value. The assay was applied to 21 water samples ranging from sewage to drinking water, including secondary treatment and various tertiary treatment options (ozonation, biologically activated carbon filtration, membrane filtration, reverse osmosis, advanced oxidation, chlorination, chloramination). The samples were enriched by solid phase extraction. In most samples the oxidative stress response was far more sensitive than cytotoxicity. The primary and secondary treated effluent exceeded the effect threshold IR 1.5 at a relative enrichment factor (REF) of 1, i.e., the native samples were active. All tertiary treated samples were less potent and their EC(IR1.5) lay between REF 1 and 10. The Nrf2 pathway was induced at a REF of approximately 10 for surface waters and drinking water, and above this enrichment cytotoxicity took over in most samples and quenched the induction. The blank (ultrapure water run through the sample enrichment process) was cytotoxic at an REF of 100, which is the limit of concentrations range that can be evaluated. Treatment typically decreased both the cytotoxicity and oxidative stress response apart from drinking water treatment where chlorination caused an increase in oxidative stress response, presumably due to the formation of disinfection by-products. This study demonstrates the relevance and applicability of the oxidative stress response pathway for water quality monitoring.

Quantifying suspended solids in small rivers using satellite data.

PubMed

Isidro, Celso M; McIntyre, Neil; Lechner, Alex M; Callow, Ian

2018-09-01

The management of suspended solids and associated contaminants in rivers requires knowledge of sediment sources. In-situ sampling can only describe the integrated impact of the upstream sources. Empirical models that use surface reflectance from satellite images to estimate total suspended solid (TSS) concentrations can be used to supplement measurements and provide spatially continuous maps. However, there are few examples, especially in narrow, shallow and hydrologically dynamic rivers found in mountainous areas. A case study of the Didipio catchment in Philippines was used to address these issues. Four 5-m resolution RapidEye images, from between the years 2014 and 2016, and near-simultaneous ground measurements of TSS concentrations were used to develop a power law model that approximates the relationship between TSS and reflectance for each of four spectral bands. A second dataset using two 2-m resolution Pleiades-1A and a third using a 6-m resolution SPOT-6 image along with ground-based measurements, were consistent with the model when using the red band data. Using that model, encompassing data from all three datasets, gave an R 2 value of 65% and a root mean square error of 519mgL -1 . A linear relationship between reflectance and TSS exists from 1mgL -1 to approximately 500mgL -1 . In contrast, for TSS measurements between 500mgL -1 and 3580mgL -1 reflectance increases at a generally lower and more variable rate. The results were not sensitive to changing the pixel location within the vicinity of the ground sampling location. The model was used to generate a continuous map of TSS concentration within the catchment. Further ground-based measurements including TSS concentrations that are higher than 3580mgL -1 would allow the model to be developed and applied more confidently over the full relevant range of TSS. Copyright © 2018 Elsevier B.V. All rights reserved.

An investigation into moisture barrier film coating efficacy and its relevance to drug stability in solid dosage forms.

PubMed

Mwesigwa, Enosh; Basit, Abdul W

2016-01-30

Barrier coatings are frequently employed on solid oral dosage forms under the assumption that they prevent moisture sorption into tablet cores thereby averting premature degradation of moisture-sensitive active ingredients. However, the efficacy of moisture barrier coatings remains unproven and they may actually accelerate degradation. This study aimed to investigate the barrier performance of four coating systems following application onto a low hygroscopic tablet formulation containing aspirin as a model moisture sensitive drug. Tablets were prepared by direct compaction and coated with aqueous dispersions of Eudragit(®) L30 D-55, Eudragit(®) EPO, Opadry(®) AMB and Sepifilm(®) LP at the vendors' recommended weight gains. Moisture uptake was studied by dynamic vapor sorption at 0 and 75% RH (25°C). Accelerated stability studies were undertaken at 75% RH/25°C for 90 days and HPLC assay was used to determine aspirin content. Uncoated tablet cores equilibrated rapidly and took up very little water (0.09%). The mean water uptake for coated cores was higher than for the uncoated formulation and varied as follows: 0.19% (Eudragit(®) L30 D-55), 0.35% (Opadry(®) AMB), 0.49% (Sepifilm(®) LP) and 0.76% (Eudragit(®) EPO). The level of aspirin decreased in all the samples such that by the time the study was terminated, the mean aspirin recovered was as follows: uncoated cores 80.0%; Eudragit® L30 D-55 coated cores 78.8%; Opadry(®) AMB coated cores 76.2%, Sepifilm(®) LP coated cores 76.0% and Eudragit(®) EPO coated samples 66.5%. From these results, it is concluded that the efficacy of moisture barrier polymer coatings on low hygroscopic cores is limited, and application of these coatings can, instead, enhance drug degradation in solid dosage forms. Copyright © 2015 Elsevier B.V. All rights reserved.

Multifrequency Ultra-High Resolution Miniature Scanning Microscope Using Microchannel And Solid-State Sensor Technologies And Method For Scanning Samples

NASA Technical Reports Server (NTRS)

Wang, Yu (Inventor)

2006-01-01

A miniature, ultra-high resolution, and color scanning microscope using microchannel and solid-state technology that does not require focus adjustment. One embodiment includes a source of collimated radiant energy for illuminating a sample, a plurality of narrow angle filters comprising a microchannel structure to permit the passage of only unscattered radiant energy through the microchannels with some portion of the radiant energy entering the microchannels from the sample, a solid-state sensor array attached to the microchannel structure, the microchannels being aligned with an element of the solid-state sensor array, that portion of the radiant energy entering the microchannels parallel to the microchannel walls travels to the sensor element generating an electrical signal from which an image is reconstructed by an external device, and a moving element for movement of the microchannel structure relative to the sample. Discloses a method for scanning samples whereby the sensor array elements trace parallel paths that are arbitrarily close to the parallel paths traced by other elements of the array.

Hypercrosslinked particles for the extraction of sweeteners using dispersive solid-phase extraction from environmental samples.

PubMed

Lakade, Sameer S; Zhou, Qing; Li, Aimin; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa M

2018-04-01

This work presents a new extraction material, namely, Q-100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid-phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q-100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid-phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q-100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid-phase extraction using Q-100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg/L. The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate, and sucralose) were found in both types of sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

QUANTITATION OF ESTROGENS IN GROUND WATER AND SWINE LAGOON SAMPLE USING SOLID PHASE EXTRACTION, PENTAFLUROBENZYL/TRIMETHYLSILYL DERIVATIZATIONS AND GAS CHROMATOGRAPHY NEGATIVE ION CHEMICAL IONIZATION/MASS SPECTROMETRY/MASS SPECTROMETRY

EPA Science Inventory

A method was developed for the confirmed identification and quantitation of 17B-estradiol, estrone, 17B-ethynylestrodial and 16a-hydroxy-17B-estradiol (estriol) in ground water and swine lagoon samples. Centrifuged and filtered samples were extracted using solid phase extraction...

Measurement of breast-tissue x-ray attenuation by spectral mammography: solid lesions

NASA Astrophysics Data System (ADS)

Fredenberg, Erik; Kilburn-Toppin, Fleur; Willsher, Paula; Moa, Elin; Danielsson, Mats; Dance, David R.; Young, Kenneth C.; Wallis, Matthew G.

2016-04-01

Knowledge of x-ray attenuation is essential for developing and evaluating x-ray imaging technologies. For instance, techniques to distinguish between cysts and solid tumours at mammography screening would be highly desirable to reduce recalls, but the development requires knowledge of the x-ray attenuation for cysts and tumours. We have previously measured the attenuation of cyst fluid using photon-counting spectral mammography. Data on x-ray attenuation for solid breast lesions are available in the literature, but cover a relatively wide range, likely caused by natural spread between samples, random measurement errors, and different experimental conditions. In this study, we have adapted a previously developed spectral method to measure the linear attenuation of solid breast lesions. A total of 56 malignant and 5 benign lesions were included in the study. The samples were placed in a holder that allowed for thickness measurement. Spectral (energy-resolved) images of the samples were acquired and the image signal was mapped to equivalent thicknesses of two known reference materials, which can be used to derive the x-ray attenuation as a function of energy. The spread in equivalent material thicknesses was relatively large between samples, which is likely to be caused mainly by natural variation and only to a minor extent by random measurement errors and sample inhomogeneity. No significant difference in attenuation was found between benign and malignant solid lesions. The separation between cyst-fluid and tumour attenuation was, however, significant, which suggests it may be possible to distinguish cystic from solid breast lesions, and the results lay the groundwork for a clinical trial. In addition, the study adds a relatively large sample set to the published data and may contribute to a reduction in the overall uncertainty in the literature.

A modified method for COD determination of solid waste, using a commercial COD kit and an adapted disposable weighing support.

PubMed

André, L; Pauss, A; Ribeiro, T

2017-03-01

The chemical oxygen demand (COD) is an essential parameter in waste management, particularly when monitoring wet anaerobic digestion processes. An adapted method to determine COD was developed for solid waste (total solids >15%). This method used commercial COD tubes and did not require sample dilution. A homemade plastic weighing support was used to transfer the solid sample into COD tubes. Potassium hydrogen phthalate and glucose used as standards showed an excellent repeatability. A small underestimation of the theoretical COD value (standard values around 5% lower than theoretical values) was also observed, mainly due to the intrinsic COD of the weighing support and to measurement uncertainties. The adapted COD method was tested using various solid wastes in the range of 1-8 mg COD , determining the COD of dried and ground cellulose, cattle manure, straw and a mixed-substrate sample. This new adapted method could be used to monitor and design dry anaerobic digestion processes.

The application of microwave digestion in decomposing some refractory ore samples with solid fusion agent.

PubMed

Lu, Yan; Li, Gang; Liu, Wei; Yuan, Hongyan; Xiao, Dan

2018-08-15

It is known that most of the refractory ore are the basis of national economy and widely applied in various fields, however, the complexity of the chemical composition and the diversity of the crystallinity in the mineral phases make the sample pre-treatment of refractory ore still remains a challenge. In this work, the complete decomposition of the refractory ore sample can be achieved just by exposing the solid fusion agent and the refractory ore sample in the microwave irradiation environment for a few minutes, and induced by a drop of water. A digestion time of 15 min for 3.0 g solid fusion agent mixture of sodium peroxide/sodium carbonate (Na 2 O 2 /Na 2 CO 3 ) in a corundum crucible via microwave heating is sufficient to decompose 0.1 g refractory ore sample. An excellent microwave digestion solid agent should meet the following conditions, a good decomposition ability, an outstanding ability of absorbing microwave energy and converting it into heat quickly, a higher melting point than the decomposing temperature of the ore sample. In the research, the induction effect of water plays an important role for the microwave digestion. The energy which is released by the reaction of water and the solid fusion agent (Na 2 O 2 ) is the key to decompose refractory ore samples with solid fusion agent, which replenished the total energy required for the microwave digestion and made the microwave digestion completed successfully. This microwave digestion technique has good reproducibility and precision, RSD % for Mo, Fe, Ti, Cr and W in the refractory ore samples were all better than 6, except RSD % for Be of about 8 because of the influence of matrix-effect. Meanwhile, the analysis results of the elements in the refractory ore samples provided by the microwave digestion technique were all in good agreement with the analysis results provided by the traditional fusion method except for Cr in the mixture ore samples. In the study, the non-linear dependence of the electromagnetic and thermal properties of the solid fusion agent on temperature under microwave irradiation and the selective heating of microwave are fully applied in this simple microwave technique. Comparing to the traditional fusion decomposition method, this microwave digestion technique is a simple, economical, fast and energy-saving sample pre-treatment technique. Copyright © 2018 Elsevier B.V. All rights reserved.

Assessing total and volatile solids in municipal solid waste samples.

PubMed

Peces, M; Astals, S; Mata-Alvarez, J

2014-01-01

Municipal solid waste is broadly generated in everyday activities and its treatment is a global challenge. Total solids (TS) and volatile solids (VS) are typical control parameters measured in biological treatments. In this study, the TS and VS were determined using the standard methods, as well as introducing some variants: (i) the drying temperature for the TS assays was 105°C, 70°C and 50°C and (ii) the VS were determined using different heating ramps from room tempature to 550°C. TS could be determined at either 105°C or 70°C, but oven residence time was tripled at 70°C, increasing from 48 to 144 h. The VS could be determined by smouldering the sample (where the sample is burnt without a flame), which avoids the release of fumes and odours in the laboratory. However, smouldering can generate undesired pyrolysis products as a consequence of carbonization, which leads to VS being underestimated. Carbonization can be avoided using slow heating ramps to prevent the oxygen limitation. Furthermore, crushing the sample cores decreased the time to reach constant weight and decreased the potential to underestimate VS.

"Cooking the sample": radiofrequency induced heating during solid-state NMR experiments.

PubMed

d'Espinose de Lacaillerie, Jean-Baptiste; Jarry, Benjamin; Pascui, Ovidiu; Reichert, Detlef

2005-09-01

Dissipation of radiofrequency (RF) energy as heat during continuous wave decoupling in solid-state NMR experiment was examined outside the conventional realm of such phenomena. A significant temperature increase could occur while performing dynamic NMR measurements provided the sample contains polar molecules and the sequence calls for relatively long applications of RF power. It was shown that the methyl flip motion in dimethylsulfone (DMS) is activated by the decoupling RF energy conversion to heat during a CODEX pulse sequence. This introduced a significant bias in the correlation time-temperature dependency measurement used to obtain the activation energy of the motion. By investigating the dependency of the temperature increase in hydrated lead nitrate on experimental parameters during high-power decoupling one-pulse experiments, the mechanisms for the RF energy deposition was identified. The samples were heated due to dissipation of the energy absorbed by dielectric losses, a phenomenon commonly known as "microwave" heating. It was thus established that during solid-state NMR experiments at moderate B0 fields, RF heating could lead to the heating of samples containing polar molecules such as hydrated polymers and inorganic solids. In particular, this could result in systematic errors for slow dynamics measurements by solid-state NMR.

Data for the geochemical investigation of UMTRAP designated site at Durango, Colorado

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

Markos, G.; Bush, K.J.

1983-09-01

This report contains the methods of collection and the data used in the geochemical investigation of the former tailings and raffinate pond sites at Durango, Colorado. The methods of data interpretation and results of the investigation are described in the report, ''Geochemical Investigation of UMTRAP Designated Site at Durango, Colorado''. Data are from a one-time sampling of waters and solid material from the background, the area adjacent to the site, and the site. The solid samples are water extracted to remove easily soluble salts and acid extracted to remove carbonates and hydroxides. The waters, extracts, and solid samples were analyzedmore » for selected major and trace elements. A few samples were analyzed for radioisotopes.« less

Further insight into the mechanism of heavy metals partitioning in stormwater runoff.

PubMed

Djukić, Aleksandar; Lekić, Branislava; Rajaković-Ognjanović, Vladana; Veljović, Djordje; Vulić, Tatjana; Djolić, Maja; Naunovic, Zorana; Despotović, Jovan; Prodanović, Dušan

2016-03-01

Various particles and materials, including pollutants, deposited on urban surfaces are washed off by stormwater runoff during rain events. The interactions between the solid and dissolved compounds in stormwater runoff are phenomena of importance for the selection and improvement of optimal stormwater management practices aimed at minimizing pollutant input to receiving waters. The objective of this research was to further investigate the mechanisms responsible for the partitioning of heavy metals (HM) between the solid and liquid phases in urban stormwater runoff. The research involved the collection of samples from urban asphalt surfaces, chemical characterization of the bulk liquid samples, solids separation, particle size distribution fractionation and chemical and physico-chemical characterization of the solid phase particles. The results revealed that a negligible fraction of HM was present in the liquid phase (less than 3% by weight), while there was a strong correlation between the total content of heavy metals and total suspended solids. Examinations of surface morphology and mineralogy revealed that the solid phase particles consist predominantly of natural macroporous materials: alpha quartz (80%), magnetite (11.4%) and silicon diphosphate (8.9%). These materials have a low surface area and do not have significant adsorptive capacity. These materials have a low surface area and do not have significant adsorptive capacity. The presence of HM on the surface of solid particles was not confirmed by scanning electron microscopy and energy dispersive X-ray microanalyses. These findings, along with the results of the liquid phase sample characterization, indicate that the partitioning of HM between the liquid and solid phases in the analyzed samples may be attributed to precipitation processes. Copyright © 2015 Elsevier Ltd. All rights reserved.

Organic Laboratory Experiments: Micro vs. Conventional.

ERIC Educational Resources Information Center

Chloupek-McGough, Marge

1989-01-01

Presents relevant statistics accumulated in a fall organic laboratory course. Discusses laboratory equipment setup to lower the amount of waste. Notes decreased solid wastes were produced compared to the previous semester. (MVL)

Gas sampling system for reactive gas-solid mixtures

DOEpatents

Daum, Edward D.; Downs, William; Jankura, Bryan J.; McCoury, Jr., John M.

1989-01-01

An apparatus and method for sampling a gas containing a reactive particulate solid phase flowing through a duct and for communicating a representative sample to a gas analyzer. A sample probe sheath 32 with an angular opening 34 extends vertically into a sample gas duct 30. The angular opening 34 is opposite the gas flow. A gas sampling probe 36 concentrically located within sheath 32 along with calibration probe 40 partly extend in the sheath 32. Calibration probe 40 extends further in the sheath 32 than gas sampling probe 36 for purging the probe sheath area with a calibration gas during calibration.

Gas sampling system for reactive gas-solid mixtures

DOEpatents

Daum, Edward D.; Downs, William; Jankura, Bryan J.; McCoury, Jr., John M.

1990-01-01

An apparatus and method for sampling gas containing a reactive particulate solid phase flowing through a duct and for communicating a representative sample to a gas analyzer. A sample probe sheath 32 with an angular opening 34 extends vertically into a sample gas duct 30. The angular opening 34 is opposite the gas flow. A gas sampling probe 36 concentrically located within sheath 32 along with calibration probe 40 partly extends in the sheath 32. Calibration probe 40 extends further in the sheath 32 than gas sampling probe 36 for purging the probe sheath area with a calibration gas during calibration.

EVALUATION OF SOLID ADSORBENTS FOR THE COLLECTION AND ANALYSES OF AMBIENT BIOGENIC VOLATILE ORGANICS

EPA Science Inventory

Micrometeorological flux measurements of biogenic volatile organic compounds (BVOCs) usually require that large volumes of air be collected (whole air samples) or focused during the sampling process (cryogenic trapping or gas-solid partitioning on adsorbents) in order to achiev...

40 CFR 60.51b - Definitions.

Code of Federal Regulations, 2014 CFR

2014-07-01

... gases, liquids, or solids through the heating of municipal solid waste, and the gases, liquids, or... diluent gas) for subsequent on-or off-site analysis; integrated sample(s) collected are representative of... arithmetic average flue gas temperature measured at the particulate matter control device inlet during four...

40 CFR 60.51b - Definitions.

Code of Federal Regulations, 2013 CFR

2013-07-01

... gases, liquids, or solids through the heating of municipal solid waste, and the gases, liquids, or... diluent gas) for subsequent on-or off-site analysis; integrated sample(s) collected are representative of... arithmetic average flue gas temperature measured at the particulate matter control device inlet during four...

40 CFR 60.51b - Definitions.

Code of Federal Regulations, 2012 CFR

2012-07-01

... gases, liquids, or solids through the heating of municipal solid waste, and the gases, liquids, or... diluent gas) for subsequent on-or off-site analysis; integrated sample(s) collected are representative of... arithmetic average flue gas temperature measured at the particulate matter control device inlet during four...

Isolation of breast cancer and gastric cancer circulating tumor cells by use of an anti HER2-based microfluidic device.

PubMed

Galletti, Giuseppe; Sung, Matthew S; Vahdat, Linda T; Shah, Manish A; Santana, Steven M; Altavilla, Giuseppe; Kirby, Brian J; Giannakakou, Paraskevi

2014-01-07

Circulating tumor cells (CTCs) have emerged as a reliable source of tumor cells, and their concentration has prognostic implications. CTC capture offers real-time access to cancer tissue without the need of an invasive biopsy, while their phenotypic and molecular interrogation can provide insight into the biological changes of the tumor that occur during treatment. The majority of the CTC capture methods are based on EpCAM expression as a surface marker of tumor-derived cells. However, EpCAM protein expression levels can be significantly down regulated during cancer progression as a consequence of the process of epithelial to mesenchymal transition. In this paper, we describe a novel HER2 (Human Epidermal Receptor 2)-based microfluidic device for the isolation of CTCs from peripheral blood of patients with HER2-expressing solid tumors. We selected HER2 as an alternative to EpCAM as the receptor is biologically and therapeutically relevant in several solid tumors, like breast cancer (BC), where it is overexpressed in 30% of the patients and expressed in 90%, and gastric cancer (GC), in which HER2 presence is identified in more than 60% of the cases. We tested the performance of various anti HER2 antibodies in a panel of nine different BC cell lines with varying HER2 protein expression levels, using immunoblotting, confocal microscopy, live cells imaging and flow cytometry analyses. The antibody associated with the highest capture efficiency and sensitivity for HER2 expressing cells on the microfluidic device was the one that performed best in live cells imaging and flow cytometry assays as opposed to the fixed cell analyses, suggesting that recognition of the native conformation of the HER2 extracellular epitope on living cells was essential for specificity and sensitivity of CTC capture. Next, we tested the performance of the HER2 microfluidic device using blood from metastatic breast and gastric cancer patients. The HER2 microfluidic device exhibited CTC capture in 9/9 blood samples. Thus, the described HER2-based microfluidic device can be considered as a valid clinically relevant method for CTC capture in HER2 expressing solid cancers.

Dynamics of Metabolite Induction in Fungal Co-cultures by Metabolomics at Both Volatile and Non-volatile Levels

PubMed Central

Azzollini, Antonio; Boggia, Lorenzo; Boccard, Julien; Sgorbini, Barbara; Lecoultre, Nicole; Allard, Pierre-Marie; Rubiolo, Patrizia; Rudaz, Serge; Gindro, Katia; Bicchi, Carlo; Wolfender, Jean-Luc

2018-01-01

Fungal co-cultivation has emerged as a promising way for activating cryptic biosynthetic pathways and discovering novel antimicrobial metabolites. For the success of such studies, a key element remains the development of standardized co-cultivation methods compatible with high-throughput analytical procedures. To efficiently highlight induction processes, it is crucial to acquire a holistic view of intermicrobial communication at the molecular level. To tackle this issue, a strategy was developed based on the miniaturization of fungal cultures that allows for a concomitant survey of induction phenomena in volatile and non-volatile metabolomes. Fungi were directly grown in vials, and each sample was profiled by head space solid phase microextraction gas chromatography mass spectrometry (HS-SPME-GC-MS), while the corresponding solid culture medium was analyzed by liquid chromatography high resolution mass spectrometry (LC-HRMS) after solvent extraction. This strategy was implemented for the screening of volatile and non-volatile metabolite inductions in an ecologically relevant fungal co-culture of Eutypa lata (Pers.) Tul. & C. Tul. (Diatrypaceae) and Botryosphaeria obtusa (Schwein.) Shoemaker (Botryosphaeriaceae), two wood-decaying fungi interacting in the context of esca disease of grapevine. For a comprehensive evaluation of the results, a multivariate data analysis combining Analysis of Variance and Partial Least Squares approaches, namely AMOPLS, was used to explore the complex LC-HRMS and GC-MS datasets and highlight dynamically induced compounds. A time-series study was carried out over 9 days, showing characteristic metabolite induction patterns in both volatile and non-volatile dimensions. Relevant links between the dynamics of expression of specific metabolite production were observed. In addition, the antifungal activity of 2-nonanone, a metabolite incrementally produced over time in the volatile fraction, was assessed against Eutypa lata and Botryosphaeria obtusa in an adapted bioassay set for volatile compounds. This compound has shown antifungal activity on both fungi and was found to be co-expressed with a known antifungal compound, O-methylmellein, induced in solid media. This strategy could help elucidate microbial inter- and intra-species cross-talk at various levels. Moreover, it supports the study of concerted defense/communication mechanisms for efficiently identifying original antimicrobials. PMID:29459851

Development of a depth-integrated sample arm (DISA) to reduce solids stratification bias in stormwater sampling

USGS Publications Warehouse

Selbig, William R.; ,; Roger T. Bannerman,

2011-01-01

A new depth-integrated sample arm (DISA) was developed to improve the representation of solids in stormwater, both organic and inorganic, by collecting a water quality sample from multiple points in the water column. Data from this study demonstrate the idea of vertical stratification of solids in storm sewer runoff. Concentrations of suspended sediment in runoff were statistically greater using a fixed rather than multipoint collection system. Median suspended sediment concentrations measured at the fixed location (near the pipe invert) were approximately double those collected using the DISA. In general, concentrations and size distributions of suspended sediment decreased with increasing vertical distance from the storm sewer invert. Coarser particles tended to dominate the distribution of solids near the storm sewer invert as discharge increased. In contrast to concentration and particle size, organic material, to some extent, was distributed homogenously throughout the water column, likely the result of its low specific density, which allows for thorough mixing in less turbulent water.

Development of a depth-integrated sample arm to reduce solids stratification bias in stormwater sampling.

PubMed

Selbig, William R; Bannerman, Roger T

2011-04-01

A new depth-integrated sample arm (DISA) was developed to improve the representation of solids in stormwater, both organic and inorganic, by collecting a water quality sample from multiple points in the water column. Data from this study demonstrate the idea of vertical stratification of solids in storm sewer runoff. Concentrations of suspended sediment in runoff were statistically greater using a fixed rather than multipoint collection system. Median suspended sediment concentrations measured at the fixed location (near the pipe invert) were approximately double those collected using the DISA. In general, concentrations and size distributions of suspended sediment decreased with increasing vertical distance from the storm sewer invert. Coarser particles tended to dominate the distribution of solids near the storm sewer invert as discharge increased. In contrast to concentration and particle size, organic material, to some extent, was distributed homogenously throughout the water column, likely the result of its low specific density, which allows for thorough mixing in less turbulent water.

Development of a depth-integrated sample arm to reduce solids stratification bias in stormwater sampling

USGS Publications Warehouse

Selbig, W.R.; Bannerman, R.T.

2011-01-01

A new depth-integrated sample arm (DISA) was developed to improve the representation of solids in stormwater, both organic and inorganic, by collecting a water quality sample from multiple points in the water column. Data from this study demonstrate the idea of vertical stratification of solids in storm sewer runoff. Concentrations of suspended sediment in runoff were statistically greater using a fixed rather than multipoint collection system. Median suspended sediment concentrations measured at the fixed location (near the pipe invert) were approximately double those collected using the DISA. In general, concentrations and size distributions of suspended sediment decreased with increasing vertical distance from the storm sewer invert. Coarser particles tended to dominate the distribution of solids near the storm sewer invert as discharge increased. In contrast to concentration and particle size, organic material, to some extent, was distributed homogenously throughout the water column, likely the result of its low specific density, which allows for thorough mixing in less turbulent water. ?? 2010 Publishing Technology.

Metal-organic framework based in-syringe solid-phase extraction for the on-site sampling of polycyclic aromatic hydrocarbons from environmental water samples.

PubMed

Zhang, Xiaoqiong; Wang, Peiyi; Han, Qiang; Li, Hengzhen; Wang, Tong; Ding, Mingyu

2018-04-01

In-syringe solid-phase extraction is a promising sample pretreatment method for the on-site sampling of water samples because of its outstanding advantages of portability, simple operation, short extraction time, and low cost. In this work, a novel in-syringe solid-phase extraction device using metal-organic frameworks as the adsorbent was fabricated for the on-site sampling of polycyclic aromatic hydrocarbons from environmental waters. Trace polycyclic aromatic hydrocarbons were effectively extracted through the self-made device followed by gas chromatography with mass spectrometry analysis. Owing to the excellent adsorption performance of metal-organic frameworks, the analytes could be completely adsorbed during one adsorption cycle, thus effectively shortening the extraction time. Moreover, the adsorbed analytes could remain stable on the device for at least 7 days, revealing the potential of the self-made device for on-site sampling of degradable compounds in remote regions. The limit of detection ranged from 0.20 to 1.9 ng/L under the optimum conditions. Satisfactory recoveries varying from 84.4 to 104.5% and relative standard deviations below 9.7% were obtained in real samples analysis. The results of this study promote the application of metal-organic frameworks in sample preparation and demonstrate the great potential of in-syringe solid-phase extraction for the on-site sampling of trace contaminants in environmental waters. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid versus Liquid Particle Sampling Efficiency of Three Personal Aerosol Samplers when Facing the Wind

PubMed Central

Koehler, Kirsten A.; Anthony, T. Renee; Van Dyke, Michael

2016-01-01

The objective of this study was to examine the facing-the-wind sampling efficiency of three personal aerosol samplers as a function of particle phase (solid versus liquid). Samplers examined were the IOM, Button, and a prototype personal high-flow inhalable sampler head (PHISH). The prototype PHISH was designed to interface with the 37-mm closed-face cassette and provide an inhalable sample at 10 l min−1 of flow. Increased flow rate increases the amount of mass collected during a typical work shift and helps to ensure that limits of detection are met, particularly for well-controlled but highly toxic species. Two PHISH prototypes were tested: one with a screened inlet and one with a single-pore open-face inlet. Personal aerosol samplers were tested on a bluff-body disc that was rotated along the facing-the-wind axis to reduce spatiotemporal variability associated with sampling supermicron aerosol in low-velocity wind tunnels. When compared to published data for facing-wind aspiration efficiency for a mouth-breathing mannequin, the IOM oversampled relative to mannequin facing-the-wind aspiration efficiency for all sizes and particle types (solid and liquid). The sampling efficiency of the Button sampler was closer to the mannequin facing-the-wind aspiration efficiency than the IOM for solid particles, but the screened inlet removed most liquid particles, resulting in a large underestimation compared to the mannequin facing-the-wind aspiration efficiency. The open-face PHISH results showed overestimation for solid particles and underestimation for liquid particles when compared to the mannequin facing-the-wind aspiration efficiency. Substantial (and statistically significant) differences in sampling efficiency were observed between liquid and solid particles, particularly for the Button and screened-PHISH, with a majority of aerosol mass depositing on the screened inlets of these samplers. Our results suggest that large droplets have low penetration efficiencies through screened inlets and that particle bounce, for solid particles, is an important determinant of aspiration and sampling efficiencies for samplers with screened inlets. PMID:21965462

Solid state SPS microwave generation and transmission study. Volume 1: Phase 2

NASA Technical Reports Server (NTRS)

Maynard, O. E.

1980-01-01

The solid state sandwich concept for Solar Power Station (SPS) was investigated. The design effort concentrated on the spacetenna, but did include some system analysis for parametric comparison reasons. The study specifically included definition and math modeling of basic solid state microwave devices, an initial conceptual subsystems and system design, sidelobe control and system selection, an assessment of selected system concept and parametric solid state microwave power transmission system data relevant to the SPS concept. Although device efficiency was not a goal, the sensitivities to design of this efficiency were parametrically treated. Sidelobe control consisted of various single step tapers, multistep tapers, and Gaussian tapers. A preliminary assessment of a hybrid concept using tubes and solid state is also included. There is a considerable amount of thermal analysis provided with emphasis on sensitivities to waste heat radiator form factor, emissivity, absorptivity, amplifier efficiency, material and junction temperature.

Solid-state diffusion in amorphous zirconolite

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

Yang, C.; Dove, M. T.; Trachenko, K.

2014-11-14

We discuss how structural disorder and amorphization affect solid-state diffusion, and consider zirconolite as a currently important case study. By performing extensive molecular dynamics simulations, we disentangle the effects of amorphization and density, and show that a profound increase of solid-state diffusion takes place as a result of amorphization. Importantly, this can take place at the same density as in the crystal, representing an interesting general insight regarding solid-state diffusion. We find that decreasing the density in the amorphous system increases pre-factors of diffusion constants, but does not change the activation energy in the density range considered. We also findmore » that atomic species in zirconolite are affected differently by amorphization and density change. Our microscopic insights are relevant for understanding how solid-state diffusion changes due to disorder and for building predictive models of operation of materials to be used to encapsulate nuclear waste.« less

Low-dose ionizing radiation increases the mortality risk of solid cancers in nuclear industry workers: A meta-analysis

PubMed Central

Qu, Shu-Gen; Gao, Jin; Tang, Bo; Yu, Bo; Shen, Yue-Ping; Tu, Yu

2018-01-01

Low-dose ionizing radiation (LDIR) may increase the mortality of solid cancers in nuclear industry workers, but only few individual cohort studies exist, and the available reports have low statistical power. The aim of the present study was to focus on solid cancer mortality risk from LDIR in the nuclear industry using standard mortality ratios (SMRs) and 95% confidence intervals. A systematic literature search through the PubMed and Embase databases identified 27 studies relevant to this meta-analysis. There was statistical significance for total, solid and lung cancers, with meta-SMR values of 0.88, 0.80, and 0.89, respectively. There was evidence of stochastic effects by IR, but more definitive conclusions require additional analyses using standardized protocols to determine whether LDIR increases the risk of solid cancer-related mortality. PMID:29725540

Single-Center Experience with a Targeted Next Generation Sequencing Assay for Assessment of Relevant Somatic Alterations in Solid Tumors.

PubMed

Paasinen-Sohns, Aino; Koelzer, Viktor H; Frank, Angela; Schafroth, Julian; Gisler, Aline; Sachs, Melanie; Graber, Anne; Rothschild, Sacha I; Wicki, Andreas; Cathomas, Gieri; Mertz, Kirsten D

2017-03-01

Companion diagnostics rely on genomic testing of molecular alterations to enable effective cancer treatment. Here we report the clinical application and validation of the Oncomine Focus Assay (OFA), an integrated, commercially available next-generation sequencing (NGS) assay for the rapid and simultaneous detection of single nucleotide variants, short insertions and deletions, copy number variations, and gene rearrangements in 52 cancer genes with therapeutic relevance. Two independent patient cohorts were investigated to define the workflow, turnaround times, feasibility, and reliability of OFA targeted sequencing in clinical application and using archival material. Cohort I consisted of 59 diagnostic clinical samples from the daily routine submitted for molecular testing over a 4-month time period. Cohort II consisted of 39 archival melanoma samples that were up to 15years old. Libraries were prepared from isolated nucleic acids and sequenced on the Ion Torrent PGM sequencer. Sequencing datasets were analyzed using the Ion Reporter software. Genomic alterations were identified and validated by orthogonal conventional assays including pyrosequencing and immunohistochemistry. Sequencing results of both cohorts, including archival formalin-fixed, paraffin-embedded material stored up to 15years, were consistent with published variant frequencies. A concordance of 100% between established assays and OFA targeted NGS was observed. The OFA workflow enabled a turnaround of 3½ days. Taken together, OFA was found to be a convenient tool for fast, reliable, broadly applicable and cost-effective targeted NGS of tumor samples in routine diagnostics. Thus, OFA has strong potential to become an important asset for precision oncology. Copyright © 2017 The Authors. Published by Elsevier Inc. All rights reserved.

Infrared Spectra and Thermodynamic Properties of Co2/Methanol Ices

NASA Astrophysics Data System (ADS)

Maté, Belén; Gálvez, Óscar; Herrero, Víctor J.; Escribano, Rafael

2009-01-01

Ices of mixtures of carbon dioxide and methanol have been studied in a range of temperatures relevant for star-forming regions, comets, polar caps of planets and satellites, and other solar system bodies. We have performed temperature-programmed desorption measurements and recorded IR spectra of various types of samples. The presence of two slightly different structures of CO2 is manifest. A distorted CO2 structure is characterized by bandshifts between 5 cm-1 (ν3) and 10 cm-1 (ν2) with respect to normal CO2. If the samples are heated above 130 K, the distorted CO2 sublimates and only the normal structure remains. The latter can stay trapped until the sublimation of crystalline methanol (150 K). The desorption energy (E d ~ 20 kJ mol-1) of CO2 from methanol ice, and the specific adsorption surface area (6 m2 g-1) of amorphous CH3OH ice, have been determined. CO2 does not penetrate into crystalline ice. Whereas the desorption energy is similar to that of CO2/H2O samples, the specific surface of methanol is much smaller than that of amorphous solid water (ASW). The interaction of CO2 molecules with water and methanol is similar but ices of CH3OH are much less porous than ASW. The inclusion of CO2 into previously formed ices containing these two species would take place preferentially into ASW. However, in processes of simultaneous deposition, methanol ice can admit a larger amount of CO2 than water ice. CO2/CH3OH ices formed by simultaneous deposition admit two orders of magnitude more CO2 than sequentially deposited ices. These findings can have direct relevance to the interpretation of observations from protostellar environments (e.g., RAFGL7009S) and comet nuclei.

Structure, growth kinetics, and ledge flow during vapor-solid-solid growth of copper-catalyzed silicon nanowires.

PubMed

Wen, C-Y; Reuter, M C; Tersoff, J; Stach, E A; Ross, F M

2010-02-10

We use real-time observations of the growth of copper-catalyzed silicon nanowires to determine the nanowire growth mechanism directly and to quantify the growth kinetics of individual wires. Nanowires were grown in a transmission electron microscope using chemical vapor deposition on a copper-coated Si substrate. We show that the initial reaction is the formation of a silicide, eta'-Cu(3)Si, and that this solid silicide remains on the wire tips during growth so that growth is by the vapor-solid-solid mechanism. Individual wire directions and growth rates are related to the details of orientation relation and catalyst shape, leading to a rich morphology compared to vapor-liquid-solid grown nanowires. Furthermore, growth occurs by ledge propagation at the silicide/silicon interface, and the ledge propagation kinetics suggest that the solubility of precursor atoms in the catalyst is small, which is relevant to the fabrication of abrupt heterojunctions in nanowires.

Regulation of solid waste management at Brazilian ports: analysis and proposals for Brazil in light of the European experience.

PubMed

Jaccoud, Cristiane; Magrini, Alessandra

2014-02-15

With a coastline of 8500 km, Brazil has 34 public ports and various private terminals, which together in 2012 handled 809 million tonnes of goods. The solid wastes produced (from port activities, ships and cargoes) pose a highly relevant problem, both due to the quantity and diversity, requiring a complex and integrated set of practices resulting from legal requirements and proactive initiatives. The main Brazilian law on solid waste management is recent (Law 12,305/2010) and the specific rules on solid waste in ports are badly in need of revision to meet the challenges caused by expansion of the sector and to harmonize them with the best global practices. This paper analyzes the current legal/regulatory framework for solid waste management at Brazilian ports and compares this structure with the practice in Europe. At the end, we suggest initiatives to improve the regulation of solid wastes at Brazilian ports. Copyright © 2014 Elsevier Ltd. All rights reserved.

Analysis of 100 pharmaceuticals and their degradates in water samples by liquid chromatography/quadrupole time-of-flight mass spectrometry.

PubMed

Ferrer, Imma; Thurman, E Michael

2012-10-12

A straightforward methodology for the chromatographic separation and accurate mass identification of 100 pharmaceuticals including some of their degradation products was developed using liquid chromatography/quadrupole time-of-flight mass spectrometry (LC/Q-TOF-MS). A table compiling the protonated or deprotonated exact masses for all compounds, as well as the exact mass of several fragment ions obtained by MS-MS is included. Excellent chromatographic separation was achieved by using 3.5 μm particle size columns and a slow and generic 30-min gradient. Isobaric and isomeric compounds (same nominal mass and same exact mass, respectively) were distinguished by various methods, including chromatography separation, MS-MS fragmentation, and isotopic signal identification. Method reporting limits of detection ranged from 1 to 1000 ng/L, after solid-phase extraction of 100mL aqueous samples. The methodology was successfully applied to the analysis of surface water impacted by wastewater effluent by identifying many of the pharmaceuticals and metabolites included in the list. Examples are given for some of the most unusual findings in environmental samples. This paper is meant to serve as a guide for those doing analysis of pharmaceuticals in environmental samples, by providing exact mass measurements of several well known, as well as newly identified and environmentally relevant pharmaceuticals in water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

A green analytical method using ultrasound in sample preparation for the flow injection determination of iron, manganese, and zinc in soluble solid samples by flame atomic absorption spectrometry.

PubMed

Yebra, M Carmen

2012-01-01

A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5-30 mg) at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2-4.6%) and a sample throughput of ca. 25 samples h(-1) were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee) and pharmaceutical preparations (multivitamin tablets). The ranges of concentrations found were 21.4-25.61 μg g(-1) for iron, 5.74-18.30 μg g(-1) for manganese, and 33.27-57.90 μg g(-1) for zinc in soluble solid food samples and 3.75-9.90 μg g(-1) for iron, 0.47-5.05 μg g(-1) for manganese, and 1.55-15.12 μg g(-1) for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors.

The Sample Analysis at Mars Investigation and Instrument Suite

NASA Technical Reports Server (NTRS)

Mahaffy, Paul; Webster, Chris R.; Cabane, M.; Conrad, Pamela G.; Coll, Patrice; Atreya, Sushil K.; Arvey, Robert; Barciniak, Michael; Benna, Mehdi; Bleacher, L.;

A Study of Flame Physics and Solid Propellant Rocket Physics

DTIC Science & Technology

2007-10-01

and ellipsoids, and the packing of pellets relevant to igniter modeling. Other topics are the instabilities of smolder waves, premixed flame...instabilities in narrow tubes, and flames supported by a spinning porous plug burner . Much of this work has been reported in the high-quality archival...perchlorate in fuel binder, the combustion of model propellant packs of ellipses and ellipsoids, and the packing of pellets relevant to igniter modeling

A new approach to estimate the geometrical factors, solid angle approximation, geometrical efficiency and their use in basic interaction cross section measurements

NASA Astrophysics Data System (ADS)

Rao, D. V.; Cesareo, R.; Brunetti, A.; Gigante, G. E.; Takeda, T.; Itai, Y.; Akatsuka, T.

2002-10-01

A new approach is developed to estimate the geometrical factors, solid angle approximation and geometrical efficiency for a system with experimental arrangements using X-ray tube and secondary target as an excitation source in order to produce the nearly monoenergetic Kα radiation to excite the sample. The variation of the solid angle is studied by changing the radius and length of the collimators towards and away from the source and sample. From these values the variation of the total solid angle and geometrical efficiency is deduced and the optimum value is used for the experimental work.

A visual LISP program for voxelizing AutoCAD solid models

NASA Astrophysics Data System (ADS)

Marschallinger, Robert; Jandrisevits, Carmen; Zobl, Fritz

2015-01-01

AutoCAD solid models are increasingly recognized in geological and geotechnical 3D modeling. In order to bridge the currently existing gap between AutoCAD solid models and the grid modeling realm, a Visual LISP program is presented that converts AutoCAD solid models into voxel arrays. Acad2Vox voxelizer works on a 3D-model that is made up of arbitrary non-overlapping 3D-solids. After definition of the target voxel array geometry, 3D-solids are scanned at grid positions and properties are streamed to an ASCII output file. Acad2Vox has a novel voxelization strategy that combines a hierarchical reduction of sampling dimensionality with an innovative use of AutoCAD-specific methods for a fast and memory-saving operation. Acad2Vox provides georeferenced, voxelized analogs of 3D design data that can act as regions-of-interest in later geostatistical modeling and simulation. The Supplement includes sample geological solid models with instructions for practical work with Acad2Vox.

Major- and minor-metal composition of three distinct solid material fractions associated with Juan de Fuca hydrothermal fluids (northeast Pacific), and calculation of dilution fluid samples

USGS Publications Warehouse

Hinkley, T.K.; Seeley, J.L.; Tatsumoto, M.

1988-01-01

Three distinct types of solid material are associated with each sample of the hydrothermal fluid that was collected from the vents of the Southern Juan de Fuca Ridge. The solid materials appear to be representative of deposits on ocean floors near mid-ocean ridges, and interpretation of the chemistry of the hydrothermal solutions requires understanding of them. Sr isotopic evidence indicates that at least two and probably all three of these solid materials were removed from the solution with which they are associated, by precipitation or adsorption. This occurred after the "pure" hydrothermal fluid was diluted and thoroughly mixed with ambient seawater. The three types of solid materials, are, respectively, a coarse Zn- and Fe-rich material with small amounts of Na and Ca; a finer material also rich in Zn and Fe, but with alkali and alkaline-earth metals; and a scum composed of Ba or Zn, with either considerable Fe or Si, and Sr. Mineral identification is uncertain because of uncertain anion composition. Only in the cases of Ba and Zn were metal masses greater in solid materials than in the associated fluids. For all other metals measured, masses in fluids dwarf those in solids. The fluids themselves contain greater concentrations of all metals measured, except Mg, than seawater. We discuss in detail the relative merits of two methods of determining the mixing proportions of "pure" hydrothermal solution and seawater in the fluids, one based on Sr isotopes, and another previously used method based on Mg concentrations. Comparison of solute concentrations in the several samples shows that degree of dilution of "pure" hydrothermal solutions by seawater, and amounts of original solutes that were removed from it as solid materials, are not related. There is no clear evidence that appreciable amounts of solid materials were not conserved (lost) either during or prior to sample collection. ?? 1988.

Extraction and derivatization of chemical weapons convention relevant aminoalcohols on magnetic cation-exchange resins.

PubMed

Singh, Varoon; Garg, Prabhat; Chinthakindi, Sridhar; Tak, Vijay; Dubey, Devendra Kumar

2014-02-14

Analysis and identification of nitrogen containing aminoalcohols is an integral part of the verification analysis of chemical weapons convention (CWC). This study was aimed to develop extraction and derivatization of aminoalcohols of CWC relevance by using magnetic dispersive solid-phase extraction (MDSPE) in combination with on-resin derivatization (ORD). For this purpose, sulfonated magnetic cation-exchange resins (SMRs) were prepared using magnetite nanoparticles as core, styrene and divinylbenzene as polymer coat and sulfonic acid as acidic cation exchanger. SMRs were successfully employed as extractant for targeted basic analytes. Adsorbed analytes were derivatized with hexamethyldisilazane (HMDS) on the surface of extractant. Derivatized (silylated) compounds were analyzed by GC-MS in SIM and full scan mode. The linearity of the method ranged from 5 to 200ngmL(-1). The LOD and LOQ ranged from 2 to 6ngmL(-1) and 5 to 19ngmL(-1) respectively. The relative standard deviation for intra-day repeatability and inter-day intermediate precision ranged from 5.1% to 6.6% and 0.2% to 7.6% respectively. Recoveries of analytes from spiked water samples from different sources varied from 28.4% to 89.3%. Copyright © 2014 Elsevier B.V. All rights reserved.

Surface interactions relevant to space station contamination problems

NASA Technical Reports Server (NTRS)

Dickinson, J. T.

1988-01-01

The physical and chemical processes at solid surfaces which can contribute to Space Station contamination problems are reviewed. Suggested areas for experimental studies to provide data to improve contamination modeling efforts are presented.

Spatial intratumoral heterogeneity of proliferation in immunohistochemical images of solid tumors.

PubMed

Valous, Nektarios A; Lahrmann, Bernd; Halama, Niels; Bergmann, Frank; Jäger, Dirk; Grabe, Niels

2016-06-01

The interactions of neoplastic cells with each other and the microenvironment are complex. To understand intratumoral heterogeneity, subtle differences should be quantified. Main factors contributing to heterogeneity include the gradient ischemic level within neoplasms, action of microenvironment, mechanisms of intercellular transfer of genetic information, and differential mechanisms of modifications of genetic material/proteins. This may reflect on the expression of biomarkers in the context of prognosis/stratification. Hence, a rigorous approach for assessing the spatial intratumoral heterogeneity of histological biomarker expression with accuracy and reproducibility is required, since patterns in immunohistochemical images can be challenging to identify and describe. A quantitative method that is useful for characterizing complex irregular structures is lacunarity; it is a multiscale technique that exhaustively samples the image, while the decay of its index as a function of window size follows characteristic patterns for different spatial arrangements. In histological images, lacunarity provides a useful measure for the spatial organization of a biomarker when a sampling scheme is employed and relevant features are computed. The proposed approach quantifies the segmented proliferative cells and not the textural content of the histological slide, thus providing a more realistic measure of heterogeneity within the sample space of the tumor region. The aim is to investigate in whole sections of primary pancreatic neuroendocrine neoplasms (pNENs), using whole-slide imaging and image analysis, the spatial intratumoral heterogeneity of Ki-67 immunostains. Unsupervised learning is employed to verify that the approach can partition the tissue sections according to distributional heterogeneity. The architectural complexity of histological images has shown that single measurements are often insufficient. Inhomogeneity of distribution depends not only on percentage content of proliferation phase but also on how the phase fills the space. Lacunarity curves demonstrate variations in the sampled image sections. Since the spatial distribution of proliferation in each case is different, the width of the curves changes too. Image sections that have smaller numerical variations in the computed features correspond to neoplasms with spatially homogeneous proliferation, while larger variations correspond to cases where proliferation shows various degrees of clumping. Grade 1 (uniform/nonuniform: 74%/26%) and grade 3 (uniform: 100%) pNENs demonstrate a more homogeneous proliferation with grade 1 neoplasms being more variant, while grade 2 tumor regions render a more diverse landscape (50%/50%). Hence, some cases show an increased degree of spatial heterogeneity comparing to others with similar grade. Whether this is a sign of different tumor biology and an association with a more benign/malignant clinical course needs to be investigated further. The extent and range of spatial heterogeneity has the potential to be evaluated as a prognostic marker. The association with tumor grade as well as the rationale that the methodology reflects true tumor architecture supports the technical soundness of the method. This reflects a general approach which is relevant to other solid tumors and biomarkers. Drawing upon the merits of computational biomedicine, the approach uncovers salient features for use in future studies of clinical relevance.

Sample Results From Tank 48H Samples HTF-48-14-158, -159, -169, and -170

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

Peters, T.; Hang, T.

2015-04-28

Savannah River National Laboratory (SRNL) analyzed samples from Tank 48H in support of determining the cause for the unusually high dose rates at the sampling points for this tank. A set of two samples was taken from the quiescent tank, and two additional samples were taken after the contents of the tank were mixed. The results of the analyses of all the samples show that the contents of the tank have changed very little since the analysis of the previous sample in 2012. The solids are almost exclusively composed of tetraphenylborate (TPB) salts, and there is no indication of accelerationmore » in the TPB decomposition. The filtrate composition shows a moderate increase in salt concentration and density, which is attributable to the addition of NaOH for the purposes of corrosion control. An older modeling simulation of the TPB degradation was updated, and the supernate results from a 2012 sample were run in the model. This result was compared to the results from the 2014 recent sample results reported in this document. The model indicates there is no change in the TPB degradation from 2012 to 2014. SRNL measured the buoyancy of the TPB solids in Tank 48H simulant solutions. It was determined that a solution of density 1.279 g/mL (~6.5M sodium) was capable of indefinitely suspending the TPB solids evenly throughout the solution. A solution of density 1.296 g/mL (~7M sodium) caused a significant fraction of the solids to float on the solution surface. As the experiments could not include the effect of additional buoyancy elements such as benzene or hydrogen generation, the buoyancy measurements provide an upper bound estimate of the density in Tank 48H required to float the solids.« less

Densitometry By Acoustic Levitation

NASA Technical Reports Server (NTRS)

Trinh, Eugene H.

1989-01-01

"Static" and "dynamic" methods developed for measuring mass density of acoustically levitated solid particle or liquid drop. "Static" method, unknown density of sample found by comparison with another sample of known density. "Dynamic" method practiced with or without gravitational field. Advantages over conventional density-measuring techniques: sample does not have to make contact with container or other solid surface, size and shape of samples do not affect measurement significantly, sound field does not have to be know in detail, and sample can be smaller than microliter. Detailed knowledge of acoustic field not necessary.

A Tetrazine-Labile Vinyl Ether Benzyloxycarbonyl Protecting Group (VeZ): An Orthogonal Tool for Solid-Phase Peptide Chemistry.

PubMed

Staderini, Matteo; Gambardella, Alessia; Lilienkampf, Annamaria; Bradley, Mark

2018-06-01

The vinyl ether benzyloxycarbonyl (VeZ) protecting group is selectively cleaved by treatment with tetrazines via an inverse electron-demand Diels-Alder reaction. This represents a new orthogonal protecting group for solid-phase peptide synthesis, with Fmoc-Lys(VeZ)-OH as a versatile alternative to Fmoc-Lys(Alloc)-OH and Fmoc-Lys(Dde)-OH, as demonstrated by the synthesis of two biologically relevant cyclic peptides.

Vapour-induced solid-state C-H bond activation for the clean synthesis of an organopalladium biothiol sensor.

PubMed

Monas, Andrea; Užarević, Krunoslav; Halasz, Ivan; Kulcsár, Marina Juribašić; Ćurić, Manda

2016-10-27

Room-temperature accelerated aging in the solid state has been applied for atom- and energy-efficient activation of either one or two C-H bonds of azobenzene and methyl orange by palladium(ii) acetate. Organopalladium complexes are prepared in quantitative reactions without potentially harmful side products. Dicyclopalladated methyl orange is water-soluble and is a selective chromogenic biothiol sensor at physiologically-relevant micromolar concentrations in buffered aqueous media.

Dynamics of water droplets detached from porous surfaces of relevance to PEM fuel cells.

PubMed

Theodorakakos, A; Ous, T; Gavaises, M; Nouri, J M; Nikolopoulos, N; Yanagihara, H

2006-08-15

The detachment of liquid droplets from porous material surfaces used with proton exchange membrane (PEM) fuel cells under the influence of a cross-flowing air is investigated computationally and experimentally. CCD images taken on a purpose-built transparent fuel cell have revealed that the water produced within the PEM is forming droplets on the surface of the gas-diffusion layer. These droplets are swept away if the velocity of the flowing air is above a critical value for a given droplet size. Static and dynamic contact angle measurements for three different carbon gas-diffusion layer materials obtained inside a transparent air-channel test model have been used as input to the numerical model; the latter is based on a Navier-Stokes equations flow solver incorporating the volume of fluid (VOF) two-phase flow methodology. Variable contact angle values around the gas-liquid-solid contact-line as well as their dynamic change during the droplet shape deformation process, have allowed estimation of the adhesion force between the liquid droplet and the solid surface and successful prediction of the separation line at which droplets loose their contact from the solid surface under the influence of the air stream flowing around them. Parametric studies highlight the relevant importance of various factors affecting the detachment of the liquid droplets from the solid surface.

Particle generator

DOEpatents

Hess, Wayne P.; Joly, Alan G.; Gerrity, Daniel P.; Beck, Kenneth M.; Sushko, Peter V.; Shlyuger, Alexander L.

2005-06-28

Energy tunable solid state sources of neutral particles are described. In a disclosed embodiment, a halogen particle source includes a solid halide sample, a photon source positioned to deliver photons to a surface of the halide, and a collimating means positioned to accept a spatially defined plume of hyperthermal halogen particles emitted from the sample surface.

SRB-3D Solid Rocket Booster performance prediction program. Volume 2: Sample case

NASA Technical Reports Server (NTRS)

Winkler, J. C.

1976-01-01

The sample case presented in this volume is an asymmetrical eight sector thermal gradient performance prediction for the solid rocket motor. This motor is the TC-227A-75 grain design and the initial grain geometry is assumed to be symmetrical about the motors longitudinal axis.

40 CFR 257.23 - Ground-water sampling and analysis requirements.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 26 2013-07-01 2013-07-01 false Ground-water sampling and analysis requirements. 257.23 Section 257.23 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES CRITERIA FOR CLASSIFICATION OF SOLID WASTE DISPOSAL FACILITIES AND PRACTICES Disposal Standards for the Receipt of Conditionally...

40 CFR 257.23 - Ground-water sampling and analysis requirements.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 24 2010-07-01 2010-07-01 false Ground-water sampling and analysis requirements. 257.23 Section 257.23 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES CRITERIA FOR CLASSIFICATION OF SOLID WASTE DISPOSAL FACILITIES AND PRACTICES Disposal Standards for the Receipt of Conditionally...

AUTOMATED SOLID PHASE EXTRACTION GC/MS FOR ANALYSIS OF SEMIVOLATILES IN WATER AND SEDIMENTS

EPA Science Inventory

Data is presented on the development of a new automated system combining solid phase extraction (SPE) with GC/MS spectrometry for the single-run analysis of water samples containing a broad range of organic compounds. The system uses commercially available automated in-line sampl...

Groundwater-quality characteristics for the Wyoming Groundwater-Quality Monitoring Network, November 2009 through September 2012

USGS Publications Warehouse

Boughton, Gregory K.

2014-01-01

Groundwater samples were collected from 146 shallow (less than or equal to 500 feet deep) wells for the Wyoming Groundwater-Quality Monitoring Network, from November 2009 through September 2012. Groundwater samples were analyzed for physical characteristics, major ions and dissolved solids, trace elements, nutrients and dissolved organic carbon, uranium, stable isotopes of hydrogen and oxygen, volatile organic compounds, and coliform bacteria. Selected samples also were analyzed for gross alpha radioactivity, gross beta radioactivity, radon, tritium, gasoline range organics, diesel range organics, dissolved hydrocarbon gases (methane, ethene, and ethane), and wastewater compounds. Water-quality measurements and concentrations in some samples exceeded numerous U.S. Environmental Protection Agency (EPA) drinking water standards. Physical characteristics and constituents that exceeded EPA Maximum Contaminant Levels (MCLs) in some samples were arsenic, selenium, nitrite, nitrate, gross alpha activity, and uranium. Total coliforms and Escherichia coli in some samples exceeded EPA Maximum Contaminant Level Goals. Measurements of pH and turbidity and concentrations of chloride, sulfate, fluoride, dissolved solids, aluminum, iron, and manganese exceeded EPA Secondary Maximum Contaminant Levels in some samples. Radon concentrations in some samples exceeded the alternative MCL proposed by the EPA. Molybdenum and boron concentrations in some samples exceeded EPA Health Advisory Levels. Water-quality measurements and concentrations also exceeded numerous Wyoming Department of Environmental Quality (WDEQ) groundwater standards. Physical characteristics and constituents that exceeded WDEQ Class I domestic groundwater standards in some samples were measurements of pH and concentrations of chloride, sulfate, dissolved solids, iron, manganese, boron, selenium, nitrite, and nitrate. Measurements of pH and concentrations of chloride, sulfate, dissolved solids, aluminum, iron, manganese, boron, and selenium exceeded WDEQ Class II agriculture groundwater standards in some samples. Measurements of pH and concentrations of sulfate, dissolved solids, aluminum, boron, and selenium exceeded WDEQ Class III livestock groundwater standards in some samples. The concentrations of dissolved solids in two samples exceeded the WDEQ Class IV industry groundwater standard. Measurements of pH and concentrations of dissolved solids, aluminum, iron, manganese, and selenium exceeded WDEQ Class special (A) fish and aquatic life groundwater standards in some samples. Stable isotopes of hydrogen and oxygen measured in water samples were compared to the Global Meteoric Water Line and Local Meteoric Water Lines. Results indicated that recharge to all of the wells was derived from precipitation and that the water has undergone some fractionation, possibly because of evaporation. Concentrations of organic compounds did not exceed any State or Federal water-quality standards. Few volatile organic compounds were detected in samples, whereas gasoline range organics, diesel range organics, and methane were detected most frequently. Concentrations of wastewater compounds did not exceed any State or Federal water-quality standards. The compounds N,N-diethyl-meta-toluamide (DEET), benzophenone, and phenanthrene were detected most frequently. Bacteria samples were collected, processed, incubated, and enumerated in the field or at the U.S. Geological Survey Wyoming-Montana Water Science Center. Total coliforms and Escherichia coli were detected in some samples.

Detection and Quantification of Nitrogen Compounds in the First Drilled Martian Solid Samples by the Sample Analysis at Mars (SAM) Instrument Suite on the Mars Science Laboratory (MSL)

NASA Technical Reports Server (NTRS)

Stern, J. C.; Navarro-Gonzales, R.; Freissinet, C.; McKay, C. P.; Archer, P. D., Jr.; Buch, A.; Brunner, A. E.; Coll, P.; Eigenbrode, J. L.; Franz, H. B.;

Use of itaconic acid-based polymers for solid-phase extraction of deoxynivalenol and application to pasta analysis.

PubMed

Pascale, Michelangelo; De Girolamo, Annalisa; Visconti, Angelo; Magan, Naresh; Chianella, Iva; Piletska, Elena V; Piletsky, Sergey A

2008-02-25

Molecular modelling and computational design were used to identify itaconic acid (IA) as a functional monomer with high affinity towards deoxynivalenol (DON), a Fusarium-toxin frequently occurring in cereals. IA-based polymers were photochemically synthesised in dimethyl formamide (porogen) using ethylenglycol dimethacrylate as cross-linker and 1,1'-azo-bis(cyclohexane carbonitrile) as initiator, and the relevant binding interactions with DON in solvents with different polarity were investigated. The performances of the non-imprinted IA-based polymer (blank polymer, BP) and the corresponding molecularly imprinted polymer (MIP) were compared using DON as a template. Both BP and MIP were able to bind about 90% DON either in toluene, water or water containing 5% polyethylene glycol. Non-imprinted polymers with different molar ratios of IA to cross-linker were evaluated as adsorbents for solid-phase extraction (SPE) clean-up and pre-concentration of DON from wheat and pasta samples prior to HPLC analysis. Samples were extracted with PBS/0.1M EDTA solution and cleaned up through a cartridge containing blank IA-based polymer. The column was washed with PBS (pH 9.2) and the toxin was eluted with methanol and quantified by reversed-phase HPLC with UV detector (lambda=220nm), using methanol:water:acetic acid (15:85:0.1, v/v/v) as the mobile phase. Effective removal of matrix interferences was observed only for pasta with DON recoveries higher than 70% (RSD<7%, n=3) at levels close to or higher than EU regulatory limit.

Structural analysis of geochemical samples by solid-state nuclear magnetic resonance spectrometry. Role of paramagnetic material

USGS Publications Warehouse

Vassallo, A.M.; Wilson, M.A.; Collin, P.J.; Oades, J.M.; Waters, A.G.; Malcolm, R.L.

1987-01-01

An examination of coals, coal tars, a fulvic acid, and soil fractions by solid-state 13C NMR spectrometry has demonstrated widely differing behavior regarding quantitative representation in the spectrum. Spin counting experiments on coal tars and the fulvic acid show that almost all the sample carbon is observed in both solution and solid-state NMR spectra. Similar experiments on two coals (a lignite and a bituminous coal) show that most (70-97%) of the carbon is observed; however, when the lignite is ion exchanged with 3% (w/w) Fe3+, the fraction of carbon observed drops to below 10%. In additional experiments signal intensity from soil samples is enhanced by a simple dithionite treatment. This is illustrated by 13C, 27Al, and 29Si solid-state NMR experiments on soil fractions. ?? 1987 American Chemical Society.

Concurrent Ultrasonic Tomography and Acoustic Emission in Solid Materials

NASA Astrophysics Data System (ADS)

Chow, Thomas M.

A series of experiments were performed to detect stress induced changes in the elastic properties of various solid materials. A technique was developed where these changes were monitored concurrently by two methods, ultrasonic tomography and acoustic emission monitoring. This thesis discusses some experiments in which acoustic emission (AE) and ultrasonic tomography were performed on various samples of solid materials including rocks, concrete, metals, and fibre reinforced composites. Three separate techniques were used to induce stress in these samples. Disk shaped samples were subject to stress via diametral loading using an indirect tensile test geometry. Cylindrical samples of rocks and concrete were subject to hydraulic fracture tests, and rectangular samples of fibre reinforced composite were subject to direct tensile loading. The majority of the samples were elastically anisotropic. Full waveform acoustic emission and tomographic data were collected while these samples were under load to give information concerning changes in the structure of the material as it was undergoing stress change and/or failure. Analysis of this data indicates that AE and tomographic techniques mutually compliment each other to give a view of the stress induced elastic changes in the tested samples.

Effect of highways and local activities on the quality of underground water in Ogun State, Nigeria: a case study of three districts in Ogun State, Nigeria.

PubMed

Odukoya, Olusegun O; Onianwa, Percy C; Sanusi, Olanrewaju I

2010-09-01

The effect of highways and local activities on the quality of groundwater in Ogun State, Nigeria was investigated. This was done by collecting groundwater samples from three different districts in the state, located in Southwestern Nigeria. The water samples collected at 5 m from the highway and control samples collected at 3 km from the highway were analyzed for the following physicochemical parameters: pH, conductivity, chemical oxygen demand, alkalinity, total hardness, total solid, suspended solid, dissolved solid, chloride, sulfate, phosphate, nitrate, phenol, and the metals-lead, zinc, iron, aluminum, sodium, and potassium. The levels of chromium, copper, and cadmium in the samples were below the detectable limit. The levels of the parameters show that there are significant differences between those in the samples and the controls (F test) except for phosphate and phenol. Also, anthropogenic sources (local activities) elevate the levels of different specific parameters, which are related to these activities. Good correlation was observed between traffic density and lead levels as well as between conductivity and dissolved solids. Comparisons with the World Health Organization guidelines indicate that most of the water samples are not suitable for human consumption.

Offline solid phase microextraction sampling system

DOEpatents

Harvey, Chris A.

2008-12-16

An offline solid phase microextraction (SPME) sampling apparatus for enabling SPME samples to be taken a number of times from a previously collected fluid sample (e.g. sample atmosphere) stored in a fused silica lined bottle which keeps volatile organics in the fluid sample stable for weeks at a time. The offline SPME sampling apparatus has a hollow body surrounding a sampling chamber, with multiple ports through which a portion of a previously collected fluid sample may be (a) released into the sampling chamber, (b) SPME sampled to collect analytes for subsequent GC analysis, and (c) flushed/purged using a fluidically connected vacuum source and purging fluid source to prepare the sampling chamber for additional SPME samplings of the same original fluid sample, such as may have been collected in situ from a headspace.

SOLID2: An Antibody Array-Based Life-Detector Instrument in a Mars Drilling Simulation Experiment (MARTE)

NASA Astrophysics Data System (ADS)

Parro, Víctor; Fernández-Calvo, Patricia; Rodríguez Manfredi, José A.; Moreno-Paz, Mercedes; Rivas, Luis A.; García-Villadangos, Miriam; Bonaccorsi, Rosalba; González-Pastor, José Eduardo; Prieto-Ballesteros, Olga; Schuerger, Andrew C.; Davidson, Mark; Gómez-Elvira, Javier; Stoker, Carol R.

2008-10-01

A field prototype of an antibody array-based life-detector instrument, Signs Of LIfe Detector (SOLID2), has been tested in a Mars drilling mission simulation called MARTE (Mars Astrobiology Research and Technology Experiment). As one of the analytical instruments on the MARTE robotic drilling rig, SOLID2 performed automatic sample processing and analysis of ground core samples (0.5 g) with protein microarrays that contained 157 different antibodies. Core samples from different depths (down to 5.5 m) were analyzed, and positive reactions were obtained in antibodies raised against the Gram-negative bacterium Leptospirillum ferrooxidans, a species of the genus Acidithiobacillus (both common microorganisms in the Río Tinto area), and extracts from biofilms and other natural samples from the Río Tinto area. These positive reactions were absent when the samples were previously subjected to a high-temperature treatment, which indicates the biological origin and structural dependency of the antibody-antigen reactions. We conclude that an antibody array-based life-detector instrument like SOLID2 can detect complex biological material, and it should be considered as a potential analytical instrument for future planetary missions that search for life.

SOLID2: an antibody array-based life-detector instrument in a Mars Drilling Simulation Experiment (MARTE).

PubMed

Parro, Víctor; Fernández-Calvo, Patricia; Rodríguez Manfredi, José A; Moreno-Paz, Mercedes; Rivas, Luis A; García-Villadangos, Miriam; Bonaccorsi, Rosalba; González-Pastor, José Eduardo; Prieto-Ballesteros, Olga; Schuerger, Andrew C; Davidson, Mark; Gómez-Elvira, Javier; Stoker, Carol R

2008-10-01

A field prototype of an antibody array-based life-detector instrument, Signs Of LIfe Detector (SOLID2), has been tested in a Mars drilling mission simulation called MARTE (Mars Astrobiology Research and Technology Experiment). As one of the analytical instruments on the MARTE robotic drilling rig, SOLID2 performed automatic sample processing and analysis of ground core samples (0.5 g) with protein microarrays that contained 157 different antibodies. Core samples from different depths (down to 5.5 m) were analyzed, and positive reactions were obtained in antibodies raised against the Gram-negative bacterium Leptospirillum ferrooxidans, a species of the genus Acidithiobacillus (both common microorganisms in the Río Tinto area), and extracts from biofilms and other natural samples from the Río Tinto area. These positive reactions were absent when the samples were previously subjected to a high-temperature treatment, which indicates the biological origin and structural dependency of the antibody-antigen reactions. We conclude that an antibody array-based life-detector instrument like SOLID2 can detect complex biological material, and it should be considered as a potential analytical instrument for future planetary missions that search for life.

Evaluation of Heavy Metals in Solid Waste Disposal Sites in Campinas City, Brazil Using Synchrotron Radiation Total Reflection X-Ray Fluorescence

NASA Astrophysics Data System (ADS)

de Faria, Bruna Fernanda; Moreira, Silvana

2011-12-01

The problem of solid waste in most countries is on the rise as a result of rapid population growth, urbanization, industrial development and changes in consumption habits. Amongst the various forms of waste disposals, landfills are today the most viable for the Brazilian reality, both technically and economically. Proper landfill construction practices allow minimizing the effects of the two main sources of pollution from solid waste: landfill gas and slurry. However, minimizing is not synonymous with eliminating; consequently, the landfill alone cannot resolve all the problems with solid waste disposal. The main goal of this work is to evaluate the content of trace elements in samples of groundwater, surface water and slurry arising from local solid waste disposals in the city of Campinas, SP, Brazil. Samples were collected at the Delta, Santa Barbara and Pirelli landfills. At the Delta and Santa Barbara sites, values above the maximum permitted level established by CETESB for Cr, Mn, Fe, Ni and Pb were observed in samples of groundwater, while at the Pirelli site, elements with concentrations above the permitted levels were Mn, Fe, Ba and Pb. At Delta, values above levels permitted by the CONAMA 357 legislation were still observed in surface water samples for Cr, Mn, Fe and Cu, whereas in slurry samples, values above the permitted levels were observed for Cr, Mn, Fe, Ni, Cu, Zn and Pb. Slurry samples were prepared in accordance with two extraction methodologies, EPA 3050B and EPA 200.8. Concentrations of Cr, Ni, Cu and Pb were higher than the limit established by CONAMA 357 for most samples collected at different periods (dry and rainy) and also for the two extraction methodologies employed.

Solid sampling determination of magnesium in lithium niobate crystals by graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Dravecz, Gabriella; Laczai, Nikoletta; Hajdara, Ivett; Bencs, László

2016-12-01

The vaporization/atomization processes of Mg in high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS) were investigated by evaporating solid (powder) samples of lithium niobate (LiNbO3) optical single crystals doped with various amounts of Mg in a transversally heated graphite atomizer (THGA). Optimal analytical conditions were attained by using the Mg I 215.4353 nm secondary spectral line. An optimal pyrolysis temperature of 1500 °C was found for Mg, while the compromise atomization temperature in THGAs (2400 °C) was applied for analyte vaporization. The calibration was performed against solid (powered) lithium niobate crystal standards. The standards were prepared with exactly known Mg content via solid state fusion of the oxide components of the matrix and analyte. The correlation coefficient (R value) of the linear calibration was not worse than 0.9992. The calibration curves were linear in the dopant concentration range of interest (0.74-7.25 mg/g Mg), when dosing 3-10 mg of the powder samples into the graphite sample insertion boats. The Mg content of the studied 19 samples was in the range of 1.69-4.13 mg/g. The precision of the method was better than 6.3%. The accuracy of the results was verified by means of flame atomic absorption spectrometry with solution sample introduction after digestion of several crystal samples.

Comparison of rumen bacteria distribution in original rumen digesta, rumen liquid and solid fractions in lactating Holstein cows.

PubMed

Ji, Shoukun; Zhang, Hongtao; Yan, Hui; Azarfar, Arash; Shi, Haitao; Alugongo, Gibson; Li, Shengli; Cao, Zhijun; Wang, Yajing

2017-01-01

Original rumen digesta, rumen liquid and solid fractions have been frequently used to assess the rumen bacterial community. However, bacterial profiles in rumen original digesta, liquid and solid fractions vary from each other and need to be better established. To compare bacterial profiles in each fraction, samples of rumen digesta from six cows fed either a high fiber diet (HFD) or a high energy diet (HED) were collected via rumen fistulas. Rumen digesta was then squeezed through four layers of cheesecloth to separate liquid and solid fractions. The bacterial profiles of rumen original digesta, liquid and solid fractions were analyzed with High-throughput sequencing technique. Rumen bacterial diversity was mainly affected by diet and individual cow ( P  > 0.05) rather than rumen fraction. Bias distributed bacteria were observed in solid and liquid fractions of rumen content using Venn diagram and LEfSe analysis. Fifteen out of 16 detected biomarkers (using LEfSe analysis) were found in liquid fraction, and these 15 biomarkers contributed the most to the bacterial differences among rumen content fractions. Similar results were found when using samples of original rumen digesta, rumen liquid or solid fractions to assess diversity of rumen bacteria; however, more attention should be draw onto bias distributed bacteria in different ruminal fractions, especially when liquid fraction has been used as a representative sample for rumen bacterial study.

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

PubMed

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

2015-04-15

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

Microwave assisted solid phase extraction for separation preconcentration sulfamethoxazole in wastewater using tyre based activated carbon as solid phase material prior to spectrophotometric determination

NASA Astrophysics Data System (ADS)

Mogolodi Dimpe, K.; Mpupa, Anele; Nomngongo, Philiswa N.

2018-01-01

This work was chiefly encouraged by the continuous consumption of antibiotics which eventually pose harmful effects on animals and human beings when present in water systems. In this study, the activated carbon (AC) was used as a solid phase material for the removal of sulfamethoxazole (SMX) in wastewater samples. The microwave assisted solid phase extraction (MASPE) as a sample extraction method was employed to better extract SMX in water samples and finally the analysis of SMX was done by the UV-Vis spectrophotometer. The microwave assisted solid phase extraction method was optimized using a two-level fractional factorial design by evaluating parameters such as pH, mass of adsorbent (MA), extraction time (ET), eluent ratio (ER) and microwave power (MP). Under optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) were 0.5 μg L- 1 and 1.7 μg L- 1, respectively, and intraday and interday precision expressed in terms of relative standard deviation were > 6%.The maximum adsorption capacity was 138 mg g- 1 for SMX and the adsorbent could be reused eight times. Lastly, the MASPE method was applied for the removal of SMX in wastewater samples collected from a domestic wastewater treatment plant (WWTP) and river water.

Multiplexed Colorimetric Solid-Phase Extraction

NASA Technical Reports Server (NTRS)

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

2009-01-01

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

Clinical Validation and Implementation of a Targeted Next-Generation Sequencing Assay to Detect Somatic Variants in Non-Small Cell Lung, Melanoma, and Gastrointestinal Malignancies

PubMed Central

Fisher, Kevin E.; Zhang, Linsheng; Wang, Jason; Smith, Geoffrey H.; Newman, Scott; Schneider, Thomas M.; Pillai, Rathi N.; Kudchadkar, Ragini R.; Owonikoko, Taofeek K.; Ramalingam, Suresh S.; Lawson, David H.; Delman, Keith A.; El-Rayes, Bassel F.; Wilson, Malania M.; Sullivan, H. Clifford; Morrison, Annie S.; Balci, Serdar; Adsay, N. Volkan; Gal, Anthony A.; Sica, Gabriel L.; Saxe, Debra F.; Mann, Karen P.; Hill, Charles E.; Khuri, Fadlo R.; Rossi, Michael R.

2017-01-01

We tested and clinically validated a targeted next-generation sequencing (NGS) mutation panel using 80 formalin-fixed, paraffin-embedded (FFPE) tumor samples. Forty non-small cell lung carcinoma (NSCLC), 30 melanoma, and 30 gastrointestinal (12 colonic, 10 gastric, and 8 pancreatic adenocarcinoma) FFPE samples were selected from laboratory archives. After appropriate specimen and nucleic acid quality control, 80 NGS libraries were prepared using the Illumina TruSight tumor (TST) kit and sequenced on the Illumina MiSeq. Sequence alignment, variant calling, and sequencing quality control were performed using vendor software and laboratory-developed analysis workflows. TST generated ≥500× coverage for 98.4% of the 13,952 targeted bases. Reproducible and accurate variant calling was achieved at ≥5% variant allele frequency with 8 to 12 multiplexed samples per MiSeq flow cell. TST detected 112 variants overall, and confirmed all known single-nucleotide variants (n = 27), deletions (n = 5), insertions (n = 3), and multinucleotide variants (n = 3). TST detected at least one variant in 85.0% (68/80), and two or more variants in 36.2% (29/80), of samples. TP53 was the most frequently mutated gene in NSCLC (13 variants; 13/32 samples), gastrointestinal malignancies (15 variants; 13/25 samples), and overall (30 variants; 28/80 samples). BRAF mutations were most common in melanoma (nine variants; 9/23 samples). Clinically relevant NGS data can be obtained from routine clinical FFPE solid tumor specimens using TST, benchtop instruments, and vendor-supplied bioinformatics pipelines. PMID:26801070

Method for Hot Real-Time Sampling of Gasification Products

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

Pomeroy, Marc D

The Thermochemical Process Development Unit (TCPDU) at the National Renewable Energy Laboratory (NREL) is a highly instrumented half-ton/day pilot scale plant capable of demonstrating industrially relevant thermochemical technologies from lignocellulosic biomass conversion, including gasification. Gasification creates primarily Syngas (a mixture of Hydrogen and Carbon Monoxide) that can be utilized with synthesis catalysts to form transportation fuels and other valuable chemicals. Biomass derived gasification products are a very complex mixture of chemical components that typically contain Sulfur and Nitrogen species that can act as catalysis poisons for tar reforming and synthesis catalysts. Real-time hot online sampling techniques, such as Molecular Beammore » Mass Spectrometry (MBMS), and Gas Chromatographs with Sulfur and Nitrogen specific detectors can provide real-time analysis providing operational indicators for performance. Sampling typically requires coated sampling lines to minimize trace sulfur interactions with steel surfaces. Other materials used inline have also shown conversion of sulfur species into new components and must be minimized. Sample line Residence time within the sampling lines must also be kept to a minimum to reduce further reaction chemistries. Solids from ash and char contribute to plugging and must be filtered at temperature. Experience at NREL has shown several key factors to consider when designing and installing an analytical sampling system for biomass gasification products. They include minimizing sampling distance, effective filtering as close to source as possible, proper line sizing, proper line materials or coatings, even heating of all components, minimizing pressure drops, and additional filtering or traps after pressure drops.« less

Solid state NMR: The essential technology for helical membrane protein structural characterization

PubMed Central

Cross, Timothy A.; Ekanayake, Vindana; Paulino, Joana; Wright, Anna

2014-01-01

NMR spectroscopy of helical membrane proteins has been very challenging on multiple fronts. The expression and purification of these proteins while maintaining functionality has consumed countless graduate student hours. Sample preparations have depended on whether solution or solid-state NMR spectroscopy was to be performed – neither have been easy. In recent years it has become increasingly apparent that membrane mimic environments influence the structural result. Indeed, in these recent years we have rediscovered that Nobel laureate, Christian Anfinsen, did not say that protein structure was exclusively dictated by the amino acid sequence, but rather by the sequence in a given environment (Anfinsen, 1973) [106]. The environment matters, molecular interactions with the membrane environment are significant and many examples of distorted, non-native membrane protein structures have recently been documented in the literature. However, solid-state NMR structures of helical membrane proteins in proteoliposomes and bilayers are proving to be native structures that permit a high resolution characterization of their functional states. Indeed, solid-state NMR is uniquely able to characterize helical membrane protein structures in lipid environments without detergents. Recent progress in expression, purification, reconstitution, sample preparation and in the solid-state NMR spectroscopy of both oriented samples and magic angle spinning samples has demonstrated that helical membrane protein structures can be achieved in a timely fashion. Indeed, this is a spectacular opportunity for the NMR community to have a major impact on biomedical research through the solid-state NMR spectroscopy of these proteins. PMID:24412099

Solid state NMR: The essential technology for helical membrane protein structural characterization

NASA Astrophysics Data System (ADS)

Cross, Timothy A.; Ekanayake, Vindana; Paulino, Joana; Wright, Anna

2014-02-01

NMR spectroscopy of helical membrane proteins has been very challenging on multiple fronts. The expression and purification of these proteins while maintaining functionality has consumed countless graduate student hours. Sample preparations have depended on whether solution or solid-state NMR spectroscopy was to be performed - neither have been easy. In recent years it has become increasingly apparent that membrane mimic environments influence the structural result. Indeed, in these recent years we have rediscovered that Nobel laureate, Christian Anfinsen, did not say that protein structure was exclusively dictated by the amino acid sequence, but rather by the sequence in a given environment (Anfinsen, 1973) [106]. The environment matters, molecular interactions with the membrane environment are significant and many examples of distorted, non-native membrane protein structures have recently been documented in the literature. However, solid-state NMR structures of helical membrane proteins in proteoliposomes and bilayers are proving to be native structures that permit a high resolution characterization of their functional states. Indeed, solid-state NMR is uniquely able to characterize helical membrane protein structures in lipid environments without detergents. Recent progress in expression, purification, reconstitution, sample preparation and in the solid-state NMR spectroscopy of both oriented samples and magic angle spinning samples has demonstrated that helical membrane protein structures can be achieved in a timely fashion. Indeed, this is a spectacular opportunity for the NMR community to have a major impact on biomedical research through the solid-state NMR spectroscopy of these proteins.

16S rRNA analysis of diversity of manure microbial community in dairy farm environment

PubMed Central

Miao, Max; Wang, Yi; Settles, Matthew; del Rio, Noelia Silva; Castillo, Alejandro; Souza, Alex; Pereira, Richard

2018-01-01

Dairy farms generate a considerable amount of manure, which is applied in cropland as fertilizer. While the use of manure as fertilizer reduces the application of chemical fertilizers, the main concern with regards to manure application is microbial pollution. Manure is a reservoir of a broad range of microbial populations, including pathogens, which have potential to cause contamination and pose risks to public and animal health. Despite the widespread use of manure fertilizer, the change in microbial diversity of manure under various treatment processes is still not well-understood. We hypothesize that the microbial population of animal waste changes with manure handling used in a farm environment. Consequential microbial risk caused by animal manure may depend on manure handling. In this study, a reconnaissance effort for sampling dairy manure in California Central Valley followed by 16S rRNA analysis of content and diversity was undertaken to understand the microbiome of manure after various handling processes. The microbial community analysis of manure revealed that the population in liquid manure differs from that in solid manure. For instance, the bacteria of genus Sulfuriomonas were unique in liquid samples, while the bacteria of genus Thermos were observed only in solid samples. Bacteria of genus Clostridium were present in both solid and liquid samples. The population among liquid samples was comparable, as was the population among solid samples. These findings suggest that the mode of manure application (i.e., liquid versus solid) could have a potential impact on the microbiome of cropland receiving manure as fertilizers. PMID:29304047

Comparison of the recovery of Mycobacterium bovis isolates using the BACTEC MGIT 960 system, BACTEC 460 system, and Middlebrook 7H10 and 7H11 solid media.

PubMed

Hines, Nichole; Payeur, Janet B; Hoffman, Lorraine J

2006-05-01

The BACTEC Microbacteria Growth Indicator Tube (MGIT) 960 system was evaluated to determine how it compares with the BACTEC 460 radiometric system and solid media for recovery of Mycobacterium bovis from tissue samples. A total of 506 bovine lymph node samples were collected from abattoirs in the United States and Mexico between November 2003 and September 2004. Processed samples were inoculated into an MGIT 960 tube, BACTEC 460 vial, and Middlebrook 7H10 and Middlebrook 7H11 solid media. Ziehl-Neelsen slides were prepared to check for contaminants and confirm the presence of acid-fast positive bacilli. Samples containing acid-fast bacilli were confirmed as members of the Mycobacterium tuberculosis complex by a nucleic acid assay. Niacin and nitrate biochemical tests were used to distinguish M. bovis from M. tuberculosis isolates. Statistical analyses were performed to compare recovery rate, mean time to detection, contamination rates, as well as pair-wise comparisons in each category. The results showed that the MGIT 960 system had a higher recovery rate of M. bovis (122/129) than did the BACTEC 460 (102/129) and solid media system (96/129). The average time to detection was 15.8 days for the MGIT 960 system, 28.2 days for the BACTEC 460 system, and 43.4 days for solid media. Contamination rates were 6.9% for the MGIT 960 system, 3.4% for the BACTEC 460 system, and 21.7% for solid media. These results indicate the MGIT 960 system can be used as an alternative to the BACTEC 460 system for recovering M. bovis from tissue samples.

A comparison study of rhodamine B photodegradation over nitrogen-doped lamellar niobic acid and titanic acid under visible-light irradiation.

PubMed

Li, Xiukai; Kikugawa, Naoki; Ye, Jinhua

2009-01-01

A solid-state reaction method with urea as a nitrogen precursor was used to prepare nitrogen-doped lamellar niobic and titanic solid acids (i.e., HNb(3)O(8) and H(2)Ti(4)O(9)) with different acidities for visible-light photocatalysis. The photocatalytic activities of the nitrogen-doped solid acids were evaluated for rhodamine B (RhB) degradation and the results were compared with those obtained over the corresponding nitrogen-doped potassium salts. Techniques such as XRD, BET, SEM, X-ray photoelectron spectroscopy, and UV-visible diffuse reflectance spectroscopy were adopted to explore the nature of the materials as well as the characteristics of the doped nitrogen species. It was found that the intercalation of the urea precursor helped to stabilize the layered structures of both lamellar solid acids and enabled easier nitrogen doping. The effects of urea intercalation were more significant for the more acidic HNb(3)O(8) sample than for the less acidic H(2)Ti(4)O(9). Compared with the nitrogen-doped KNb(3)O(8) and K(2)Ti(4)O(9) samples, the nitrogen-doped HNb(3)O(8) and H(2)Ti(4)O(9) solid acids absorb more visible light and exhibit a superior activity for RhB photodegradation under visible-light irradiation. The nitrogen-doped HNb(3)O(8) sample performed the best among all the samples. The results of the current study suggest that the protonic acidity of the lamellar solid-acid sample is a key factor that influences nitrogen doping and the resultant visible-light photocatalysis.

New Mechanism of Extractive Electrospray Ionization Mass Spectrometry for Heterogeneous Solid Particles.

PubMed

Kumbhani, S; Longin, T; Wingen, L M; Kidd, C; Perraud, V; Finlayson-Pitts, B J

2018-02-06

Real-time in situ mass spectrometry analysis of airborne particles is important in several applications, including exposure studies in ambient air, industrial settings, and assessing impacts on visibility and climate. However, obtaining molecular and 3D structural information is more challenging, especially for heterogeneous solid or semisolid particles. We report a study of extractive electrospray ionization mass spectrometry (EESI-MS) for the analysis of solid particles with an organic coating. The goal is to elucidate how much of the overall particle content is sampled, and determine the sensitivity of this technique to the surface layers. It is shown that, for NaNO 3 particles coated with glutaric acid (GA), very little of the solid NaNO 3 core is sampled compared to the GA coating, whereas for GA particles coated with malonic acid (MA), significant signals from both the MA coating and the GA core are observed. However, conventional ESI-MS of the same samples collected on a Teflon filter (and then extracted) detects much more core material compared to EESI-MS in both cases. These results show that, for the experimental conditions used here, EESI-MS does not sample the entire particle but, instead, is more sensitive to surface layers. Separate experiments on single-component particles of NaNO 3 , GA, or citric acid show that there must be a kinetics limitation to dissolution that is important in determining EESI-MS sensitivity. We propose a new mechanism of EESI solvent droplet interaction with solid particles that is consistent with the experimental observations. In conjunction with previous EESI-MS studies of organic particles, these results suggest that EESI does not necessarily sample the entire particle when solid, and that not only solubility but also surface energies and the kinetics of dissolution play an important role.

Direct Observation of the Phenomenology of a Solid Thermal Explosion Using Time-Resolved Proton Radiography

NASA Astrophysics Data System (ADS)

Smilowitz, L.; Henson, B. F.; Romero, J. J.; Asay, B. W.; Schwartz, C. L.; Saunders, A.; Merrill, F. E.; Morris, C. L.; Kwiatkowski, K.; Hogan, G.; Nedrow, P.; Murray, M. M.; Thompson, T. N.; McNeil, W.; Rightley, P.; Marr-Lyon, M.

2008-06-01

We present a new phenomenology for burn propagation inside a thermal explosion based on dynamic radiography. Radiographic images were obtained of an aluminum cased solid cylindrical sample of a plastic bonded formulation of octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine. The phenomenology observed is ignition followed by cracking in the solid accompanied by the propagation of a radially symmetric front of increasing proton transmission. This is followed by a further increase in transmission through the sample, ending after approximately 100μs. We show that these processes are consistent with the propagation of a convective burn front followed by consumption of the remaining solid by conductive particle burning.

Direct observation of the phenomenology of a solid thermal explosion using time-resolved proton radiography.

PubMed

Smilowitz, L; Henson, B F; Romero, J J; Asay, B W; Schwartz, C L; Saunders, A; Merrill, F E; Morris, C L; Kwiatkowski, K; Hogan, G; Nedrow, P; Murray, M M; Thompson, T N; McNeil, W; Rightley, P; Marr-Lyon, M

2008-06-06

We present a new phenomenology for burn propagation inside a thermal explosion based on dynamic radiography. Radiographic images were obtained of an aluminum cased solid cylindrical sample of a plastic bonded formulation of octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine. The phenomenology observed is ignition followed by cracking in the solid accompanied by the propagation of a radially symmetric front of increasing proton transmission. This is followed by a further increase in transmission through the sample, ending after approximately 100 micros. We show that these processes are consistent with the propagation of a convective burn front followed by consumption of the remaining solid by conductive particle burning.

A Green Analytical Method Using Ultrasound in Sample Preparation for the Flow Injection Determination of Iron, Manganese, and Zinc in Soluble Solid Samples by Flame Atomic Absorption Spectrometry

PubMed Central

Yebra, M. Carmen

2012-01-01

A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5–30 mg) at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2–4.6%) and a sample throughput of ca. 25 samples h–1 were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee) and pharmaceutical preparations (multivitamin tablets). The ranges of concentrations found were 21.4–25.61 μg g−1 for iron, 5.74–18.30 μg g−1 for manganese, and 33.27–57.90 μg g−1 for zinc in soluble solid food samples and 3.75–9.90 μg g−1 for iron, 0.47–5.05 μg g−1 for manganese, and 1.55–15.12 μg g−1 for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors. PMID:22567553

Disposable rabbit

DOEpatents

Lewis, Leroy C.; Trammell, David R.

1986-01-01

A disposable rabbit for transferring radioactive samples in a pneumatic transfer system comprises aerated plastic shaped in such a manner as to hold a radioactive sample and aerated such that dissolution of the rabbit in a solvent followed by evaporation of the solid yields solid waste material having a volume significantly smaller than the original volume of the rabbit.

Disposal rabbit

DOEpatents

Lewis, L.C.; Trammell, D.R.

1983-10-12

A disposable rabbit for transferring radioactive samples in a pneumatic transfer system comprises aerated plastic shaped in such a manner as to hold a radioactive sample and aerated such that dissolution of the rabbit in a solvent followed by evaporation of the solid yields solid waste material having a volume significantly smaller than the original volume of the rabbit.

Solid phase microextraction for active or passive sampling of methyl bromide during fumigations

USDA-ARS?s Scientific Manuscript database

The high diffusivity and volatility of methyl bromide make it an ideal compound for Solid Phase Micro Extraction (SPME)-based sampling of air prior to gas-chromatographic quantifications. SPME fibers can be used as active methyl bromide samplers, with high capacities and an equilibrium time of 1-2 m...

Structural study of the membrane protein MscL using cell-free expression and solid-state NMR

NASA Astrophysics Data System (ADS)

Abdine, Alaa; Verhoeven, Michiel A.; Park, Kyu-Ho; Ghazi, Alexandre; Guittet, Eric; Berrier, Catherine; Van Heijenoort, Carine; Warschawski, Dror E.

2010-05-01

High-resolution structures of membrane proteins have so far been obtained mostly by X-ray crystallography, on samples where the protein is surrounded by detergent. Recent developments of solid-state NMR have opened the way to a new approach for the study of integral membrane proteins inside a membrane. At the same time, the extension of cell-free expression to the production of membrane proteins allows for the production of proteins tailor made for NMR. We present here an in situ solid-state NMR study of a membrane protein selectively labeled through the use of cell-free expression. The sample consists of MscL (mechano-sensitive channel of large conductance), a 75 kDa pentameric α-helical ion channel from Escherichia coli, reconstituted in a hydrated lipid bilayer. Compared to a uniformly labeled protein sample, the spectral crowding is greatly reduced in the cell-free expressed protein sample. This approach may be a decisive step required for spectral assignment and structure determination of membrane proteins by solid-state NMR.

Effects of polymer type and storage relative humidity on the kinetics of felodipine crystallization from amorphous solid dispersions.

PubMed

Rumondor, Alfred C F; Stanford, Lindsay A; Taylor, Lynne S

2009-12-01

The objective of this study was to investigate the effects of polymer type and storage relative humidity (RH) on the crystallization kinetics of felodipine from amorphous solid dispersions. Crystallization of the model drug felodipine from amorphous solid dispersion samples containing poly(vinyl pyrrolidone) (PVP) and hypromellose acetate succinate (HPMCAS) were evaluated. Samples at three different drug-polymer weight ratios (10, 25, and 50 wt. % polymer) were prepared and stored at six different RHs (0%, 32%, 52% or 66%, 75%, 86%, and 93%). Periodically, the fraction of the drug that had crystallized from the samples was quantified using powder X-ray diffractometry (PXRD). Felodipine crystallization rates from PVP-containing dispersions were found to be very sensitive to changes in storage RH, while crystallization rates from HPMCAS-containing dispersions were not. PVP and HPMCAS were similar in terms of their ability to inhibit crystallization at low RH, but when the storage RH was increased to 75% or above, felodipine crystallization from PVP-containing solid dispersions proceeded much faster. It is hypothesized that this trend was caused by moisture-induced drug-polymer immiscibility in PVP-felodipine system. For PVP-containing solid dispersion samples stored at 75% RH and above, crystallization of the model drug felodipine seemed to approach a kinetic plateau, whereby a fraction of the drug still remained amorphous even after storage for 500 days or more. The physical stability of solid dispersions as a function of RH is highly dependent on the polymer used to form the solid dispersion, with PVP-containing dispersions being much less physically stable at high RH than HPMCAS-containing dispersions.

Low-temperature surface formation of NH3 and HNCO: hydrogenation of nitrogen atoms in CO-rich interstellar ice analogues

NASA Astrophysics Data System (ADS)

Fedoseev, G.; Ioppolo, S.; Zhao, D.; Lamberts, T.; Linnartz, H.

2015-01-01

Solid-state astrochemical reaction pathways have the potential to link the formation of small nitrogen-bearing species, like NH3 and HNCO, and prebiotic molecules, specifically amino acids. To date, the chemical origin of such small nitrogen-containing species is still not well understood, despite the fact that ammonia is an abundant constituent of interstellar ices towards young stellar objects and quiescent molecular clouds. This is mainly because of the lack of dedicated laboratory studies. The aim of this work is to experimentally investigate the formation routes of NH3 and HNCO through non-energetic surface reactions in interstellar ice analogues under fully controlled laboratory conditions and at astrochemically relevant temperatures. This study focuses on the formation of NH3 and HNCO in CO-rich (non-polar) interstellar ices that simulate the CO freeze-out stage in dark interstellar cloud regions, well before thermal and energetic processing start to become relevant. We demonstrate and discuss the surface formation of solid HNCO through the interaction of CO molecules with NH radicals - one of the intermediates in the formation of solid NH3 upon sequential hydrogenation of N atoms. The importance of HNCO for astrobiology is discussed.

A Novel Disintegration Tester for Solid Dosage Forms Enabling Adjustable Hydrodynamics.

PubMed

Kindgen, Sarah; Rach, Regine; Nawroth, Thomas; Abrahamsson, Bertil; Langguth, Peter

2016-08-01

A modified in vitro disintegration test device was designed that enables the investigation of the influence of hydrodynamic conditions on disintegration of solid oral dosage forms. The device represents an improved derivative of the compendial PhEur/USP disintegration test device. By the application of a computerized numerical control, a variety of physiologically relevant moving velocities and profiles can be applied. With the help of computational fluid dynamics, the hydrodynamic and mechanical forces present in the probe chamber were characterized for a variety of device moving speeds. Furthermore, a proof of concept study aimed at the investigation of the influence of hydrodynamic conditions on disintegration times of immediate release tablets. The experiments demonstrated the relevance of hydrodynamics for tablet disintegration, especially in media simulating the fasted state. Disintegration times increased with decreasing moving velocity. A correlation between experimentally determined disintegration times and computational fluid dynamics predicted shear stress on tablet surface was established. In conclusion, the modified disintegration test device is a valuable tool for biorelevant in vitro disintegration testing of solid oral dosage forms. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Preparation of Chemical Samples On Relevant Surfaces Using Inkjet Technology

DTIC Science & Technology

2013-04-01

PREPARATION OF CHEMICAL SAMPLES ON RELEVANT SURFACES USING INKJET TECHNOLOGY...2012 4. TITLE AND SUBTITLE 5a. CONTRACT NUMBER Preparation of Chemical Samples on Relevant Surfaces Using Inkjet Technology 5b. GRANT NUMBER...SUBJECT TERMS Surface detection Inkjet Simulant deposition 16. SECURITY CLASSIFICATION OF: 17. LIMITATION OF ABSTRACT 18. NUMBER OF

Evaluation of ultrasound-assisted in situ sorbent formation solid-phase extraction method for determination of arsenic in water, food and biological samples.

PubMed

Ezoddin, Maryam; Majidi, Behrooz; Abdi, Khosrou

2015-01-01

A simple and rapid ultrasound-assisted in situ sorbent formation solid-phase extraction (UAISFSPE) coupled with electrothermal atomic absorption spectrometry detection (ET-AAS) was developed for preconcentration and determination of arsenic (As) in various samples. A small amount of cationic surfactant is dissolved in the aqueous sample containing As ions, which were complexed by ammonium pyrrolidinedithiocarbamate After shaking, a little volume of hexafluorophosphate (NaPF6) as an ion-pairing agent was added into the solution by a microsyringe. Due to the interaction between surfactant and ion-pairing agent, solid particles are formed. The alkyl groups of the surfactant in the solid particles strongly interact with the hydrophobic groups of analytes and become bound. Sonication aids the dispersion of the sorbent into the sample solution and mass transfer of the analyte into the sorbent, thus reducing the extraction time. The solid particles are centrifuged, and the sedimented particles can be dissolved in an appropriate solvent to recover the absorbed analyte. After separation, total arsenic (As(III) and As(V)) was determined by ET-AAS. Several experimental parameters were investigated and optimized. A detection limit of 7 ng L(-1) with preconcentration factor of 100 and relative standard deviation for 10 replicate determinations of 0.1 µg L(-1) As(III) were 4.5% achieved. Consequently, the method was applied to the determination of arsenic in certified reference materials, water, food and biological samples with satisfactory results.

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

Not Available

This interim notice covers the following: extractable organic halides in solids, total organic halides, analysis by gas chromatography/Fourier transform-infrared spectroscopy, hexadecane extracts for volatile organic compounds, GC/MS analysis of VOCs, GC/MS analysis of methanol extracts of cryogenic vapor samples, screening of semivolatile organic extracts, GPC cleanup for semivolatiles, sample preparation for GC/MS for semi-VOCs, analysis for pesticides/PCBs by GC with electron capture detection, sample preparation for pesticides/PCBs in water and soil sediment, report preparation, Florisil column cleanup for pesticide/PCBs, silica gel and acid-base partition cleanup of samples for semi-VOCs, concentrate acid wash cleanup, carbon determination in solids using Coulometrics` CO{submore » 2} coulometer, determination of total carbon/total organic carbon/total inorganic carbon in radioactive liquids/soils/sludges by hot persulfate method, analysis of solids for carbonates using Coulometrics` Model 5011 coulometer, and soxhlet extraction.« less

Determining the Release of Radionuclides from Tank 18F Waste Residual Solids: FY2016 Report

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

King, William D.; Hobbs, David T.

Pore water leaching studies were conducted on actual Savannah River Site (SRS) Tank 18F residual waste solids to support Liquid Waste tank closure efforts. A test methodology was developed during previous simulant testing to produce slurries of tank residual solids and grout-representative solids in grout pore water solutions (based on SRS groundwater compositions) with pH and E h values expected during the aging of the closed waste tank. The target conditions are provided below where the initial pore water has a reducing potential and a relatively high pH (Reducing Region II). The pore water is expected to become increasingly oxidizingmore » with time (Oxidizing Region II) and during the latter stages of aging (Oxidizing Region III) the pH is expected to decrease. For the reducing case, tests were conducted with both unwashed and washed Tank 18F residual solids. For the oxidizing cases (Oxidizing Regions II and III), all samples were washed with simulated grout pore water solutions prior to testing, since it is expected that these conditions will occur after considerable pore water solution has passed through the system. For the reducing case, separate tests were conducted with representative ground grout solids and with calcium carbonate reagent, which is the grout phase believed to be controlling the pH. Ferrous sulfide (FeS) solids were also added to the reducing samples to lower the slurry E h value. Calcium carbonate solids were used as the grout-representative solid phase for each of the oxidizing cases. Air purge-gas with and without CO 2 removed was transferred through the oxidizing test samples and nitrogen purge-gas was transferred through the reducing test samples during leach testing. The target pH values were achieved to within 0.5 pH units for all samples. Leaching studies were conducted over an E h range of approximately 0.7 V. However, the highest and lowest E h values achieved of ~+0.5 V and ~-0.2 V were significantly less positive and less negative, respectively, than the target values. Achievement of more positive and more negative E h values is believed to require the addition of non-representative oxidants and reductants, respectively.« less

In-line gas chromatographic apparatus for measuring the hydrophobic micropore volume (HMV) and contaminant transformation in mineral micropores.

PubMed

Cheng, Hefa; Reinhard, Martin

2010-07-15

Desorption of hydrophobic organic compounds from micropores is characteristically slow compared to surface adsorption and partitioning. The slow-desorbing mass of a hydrophobic probe molecule can be used to calculate the hydrophobic micropore volume (HMV) of microporous solids. A gas chromatographic apparatus is described that allows characterization of the sorbed mass with respect to the desorption rate. The method is demonstrated using a dealuminated zeolite and an aquifer sand as the model and reference sorbents, respectively, and trichloroethylene (TCE) as the probe molecule. A glass column packed with the microporous sorbent is coupled directly to a gas chromatograph that is equipped with flame ionization and electron capture detectors. Sorption and desorption of TCE on the sorbent was measured by sampling the influent and effluent of the column using a combination of switching and injection valves. For geosorbents, the HMV is quantified based on Gurvitsch's rule from the mass of TCE desorbed at a rate that is characteristic for micropores. Instrumental requirements, design considerations, hardware details, detector calibration, performance, and data analysis are discussed along with applications. The method is novel and complements traditional vacuum gravimetric and piezometric techniques, which quantify the total pore volume under vacuum conditions. The HMV is more relevant than the total micropore volume for predicting the fate and transport of organic contaminants in the subsurface. Sorption in hydrophobic micropores strongly impacts the mobility of organic contaminants, and their chemical and biological transformations. The apparatus can serve as a tool for characterizing microporous solids and investigating contaminant-solid interactions. 2010 Elsevier B.V. All rights reserved.

Methods for evaluating temporal groundwater quality data and results of decadal-scale changes in chloride, dissolved solids, and nitrate concentrations in groundwater in the United States, 1988-2010

USGS Publications Warehouse

Lindsey, Bruce D.; Rupert, Michael G.

2012-01-01

Decadal-scale changes in groundwater quality were evaluated by the U.S. Geological Survey National Water-Quality Assessment (NAWQA) Program. Samples of groundwater collected from wells during 1988-2000 - a first sampling event representing the decade ending the 20th century - were compared on a pair-wise basis to samples from the same wells collected during 2001-2010 - a second sampling event representing the decade beginning the 21st century. The data set consists of samples from 1,236 wells in 56 well networks, representing major aquifers and urban and agricultural land-use areas, with analytical results for chloride, dissolved solids, and nitrate. Statistical analysis was done on a network basis rather than by individual wells. Although spanning slightly more or less than a 10-year period, the two-sample comparison between the first and second sampling events is referred to as an analysis of decadal-scale change based on a step-trend analysis. The 22 principal aquifers represented by these 56 networks account for nearly 80 percent of the estimated withdrawals of groundwater used for drinking-water supply in the Nation. Well networks where decadal-scale changes in concentrations were statistically significant were identified using the Wilcoxon-Pratt signed-rank test. For the statistical analysis of chloride, dissolved solids, and nitrate concentrations at the network level, more than half revealed no statistically significant change over the decadal period. However, for networks that had statistically significant changes, increased concentrations outnumbered decreased concentrations by a large margin. Statistically significant increases of chloride concentrations were identified for 43 percent of 56 networks. Dissolved solids concentrations increased significantly in 41 percent of the 54 networks with dissolved solids data, and nitrate concentrations increased significantly in 23 percent of 56 networks. At least one of the three - chloride, dissolved solids, or nitrate - had a statistically significant increase in concentration in 66 percent of the networks. Statistically significant decreases in concentrations were identified in 4 percent of the networks for chloride, 2 percent of the networks for dissolved solids, and 9 percent of the networks for nitrate. A larger percentage of urban land-use networks had statistically significant increases in chloride, dissolved solids, and nitrate concentrations than agricultural land-use networks. In order to assess the magnitude of statistically significant changes, the median of the differences between constituent concentrations from the first full-network sampling event and those from the second full-network sampling event was calculated using the Turnbull method. The largest median decadal increases in chloride concentrations were in networks in the Upper Illinois River Basin (67 mg/L) and in the New England Coastal Basins (34 mg/L), whereas the largest median decadal decrease in chloride concentrations was in the Upper Snake River Basin (1 mg/L). The largest median decadal increases in dissolved solids concentrations were in networks in the Rio Grande Valley (260 mg/L) and the Upper Illinois River Basin (160 mg/L). The largest median decadal decrease in dissolved solids concentrations was in the Apalachicola-Chattahoochee-Flint River Basin (6.0 mg/L). The largest median decadal increases in nitrate as nitrogen (N) concentrations were in networks in the South Platte River Basin (2.0 mg/L as N) and the San Joaquin-Tulare Basins (1.0 mg/L as N). The largest median decadal decrease in nitrate concentrations was in the Santee River Basin and Coastal Drainages (0.63 mg/L). The magnitude of change in networks with statistically significant increases typically was much larger than the magnitude of change in networks with statistically significant decreases. The magnitude of change was greatest for chloride in the urban land-use networks and greatest for dissolved solids and nitrate in the agricultural land-use networks. Analysis of data from all networks combined indicated statistically significant increases for chloride, dissolved solids, and nitrate. Although chloride, dissolved solids, and nitrate concentrations were typically less than the drinking-water standards and guidelines, a statistical test was used to determine whether or not the proportion of samples exceeding the drinking-water standard or guideline changed significantly between the first and second full-network sampling events. The proportion of samples exceeding the U.S. Environmental Protection Agency (USEPA) Secondary Maximum Contaminant Level for dissolved solids (500 milligrams per liter) increased significantly between the first and second full-network sampling events when evaluating all networks combined at the national level. Also, for all networks combined, the proportion of samples exceeding the USEPA Maximum Contaminant Level (MCL) of 10 mg/L as N for nitrate increased significantly. One network in the Delmarva Peninsula had a significant increase in the proportion of samples exceeding the MCL for nitrate. A subset of 261 wells was sampled every other year (biennially) to evaluate decadal-scale changes using a time-series analysis. The analysis of the biennial data set showed that changes were generally similar to the findings from the analysis of decadal-scale change that was based on a step-trend analysis. Because of the small number of wells in a network with biennial data (typically 4-5 wells), the time-series analysis is more useful for understanding water-quality responses to changes in site-specific conditions rather than as an indicator of the change for the entire network.

Residents' concerns and attitudes toward a municipal solid waste landfill: integrating a questionnaire survey and GIS techniques.

PubMed

Che, Yue; Yang, Kai; Jin, Yan; Zhang, Weiqian; Shang, Zhaoyi; Tai, Jun

2013-12-01

The ever-growing industry of municipal solid waste (MSW) disposal appeals to the growing need for disposal facilities, and MSW treatment facilities are increasingly an environmental and public health concern. Residents living near MSW management facilities are confronted with various risk perceptions, especially odour. In this study, in an effort to assist responsible decision-makers in better planning and managing such a project, a structured questionnaire was designed and distributed to assess the nearby residents' concerns and attitudes surrounding the Laogang Landfill in Shanghai. Geographic information system techniques and relevance analysis were employed to conduct the spatial analysis of physical perceptions, especially odour annoyance. The findings of the research indicate that a significant percentage of the responding sample was aware of the negative impacts of landfills on the environment and public health, and residents in close proximity preferred to live farther from the landfill. The results from the spatial analysis demonstrated a definite degree of correlation between odour annoyance and distance to the facility and proved that the benefits of the socially disadvantaged have been neglected. The research findings also direct attention to the important role of public participation, information disclosure, transparency in management, and mutual communication to avoid conflicts and build social trust.

Fe1-xZnxS ternary solid solution as an efficient Fenton-like catalyst for ultrafast degradation of phenol.

PubMed

Gao, Jing; Liu, Yutang; Xia, Xinnian; Wang, Longlu; Dong, Wanyue

2018-07-05

Heterogeneous Fenton-like system has been proved to be an promising alternative to Fenton system due to its easy separation. However, it's a challenge to design heterogeneous Fenton-like catalysts with high activity and great durability. Here, ternary solid solution Fe 1-x Zn x S were prepared via hydrothermal synthesis as heterogeneous Fenton-like catalysts. The Fe 0.7 Zn 0.3 S sample exhibited state of the art activity for yielding OH by H 2 O 2 decomposition, and the ultrafast degradation of phenol was achieved in 4 min at initial acidic condition under room temperature. The phenol degradation rate constant of Fe 0.7 Zn 0.3 S was 99 and 70 times of ZnS and FeS, respectively. Further, we show that the unique structural configuration of iron atoms, the formation of FeS 2 -pyrite with (200) plane, are responsible for the excellent activity. The intermediate products were identified by LC-MS and a possible pathway was accordingly proposed to elucidate the mechanism of phenol degradation by OH. Overall, this work provides an idea for the rational design of the relevant heterogeneous Fenton-like catalysts. Copyright © 2018 Elsevier B.V. All rights reserved.

Dietary Sodium and Other Nutrient Intakes among Patients Undergoing Hemodialysis in New Zealand.

PubMed

Xie, Zhengxiu; McLean, Rachael; Marshall, Mark

2018-04-18

This study describes baseline intakes of sodium and other nutrients in a multi-ethnic sample of hemodialysis patients in New Zealand participating in the SoLID Trial between May/2013 to May/2016. Baseline 3-day weighed food record collections were analyzed using Foodworks 8 Professional food composition database, supplemented by other sources of nutrient information. Intakes of dietary sodium and other nutrients were compared with relevant guidelines and clinical recommendations. Eighty-five participants completed a 3-day weighed food record. The mean (SD) sodium intake was 2502 (957) mg/day at and more than half of the participants exceeded recommended intake levels. Sodium intake was positively associated with energy intake. Only 5% of participants met the recommended calorie density; nine percent of participants ate the recommended minimum of 1.2 g/kg of protein per day; 68% of participants were consuming inadequate fiber at baseline. A high proportion of dialysis patients in SoLID Trial did not meet current renal-specific dietary recommendations. The data show excess sodium intake. It is also evident that there was poor adherence to dietary guidelines for a range of other nutrients. A total diet approach is needed to lower sodium intake and improve total diet quality among hemodialysis patients in New Zealand.

High pressure effects on the structural functionality of condensed globular-protein matrices.

PubMed

Savadkoohi, Sobhan; Kasapis, Stefan

2016-07-01

High pressure technology is the outcome of consumer demand for better quality control of processed foods. There is great potential to apply HPP to condensed systems of globular proteins for the generation of industry-relevant biomaterials with advanced techno- and biofunctionality. To this end, research demonstrates that application of high hydrostatic pressure generates a coherent structure and preserves the native conformation in condensed globular proteins, which is an entirely unexpected but interesting outcome on both scientific and technological grounds. In microbiological challenge tests, high pressure at conventional commercial conditions, demonstrated to effectively reduce the concentration of typical Gram negative or Gram positive foodborne pathogens, and proteolytic enzymes in high-solid protein samples. This may have industrial significance in relation to the formulation and stabilisation of "functional food" products as well as in protein ingredients and concentrates by replacing spray dried powders with condensed HPP-treated pastes that maintain structure and bioactivity. Fundamental concepts and structural functionality of condensed matrices of globular proteins are the primary interest in this mini-review, which may lead to opportunities for industrial exploitation, but earlier work on low-solid systems is also summarised presently to put recent developments in context of this rapidly growing field. Copyright © 2016. Published by Elsevier B.V.

Dietary Sodium and Other Nutrient Intakes among Patients Undergoing Hemodialysis in New Zealand

PubMed Central

Xie, Zhengxiu; Marshall, Mark

2018-01-01

This study describes baseline intakes of sodium and other nutrients in a multi-ethnic sample of hemodialysis patients in New Zealand participating in the SoLID Trial between May/2013 to May/2016. Baseline 3-day weighed food record collections were analyzed using Foodworks 8 Professional food composition database, supplemented by other sources of nutrient information. Intakes of dietary sodium and other nutrients were compared with relevant guidelines and clinical recommendations. Eighty-five participants completed a 3-day weighed food record. The mean (SD) sodium intake was 2502 (957) mg/day at and more than half of the participants exceeded recommended intake levels. Sodium intake was positively associated with energy intake. Only 5% of participants met the recommended calorie density; nine percent of participants ate the recommended minimum of 1.2 g/kg of protein per day; 68% of participants were consuming inadequate fiber at baseline. A high proportion of dialysis patients in SoLID Trial did not meet current renal-specific dietary recommendations. The data show excess sodium intake. It is also evident that there was poor adherence to dietary guidelines for a range of other nutrients. A total diet approach is needed to lower sodium intake and improve total diet quality among hemodialysis patients in New Zealand. PMID:29670030

Thermoacoustics of solids: A pathway to solid state engines and refrigerators

NASA Astrophysics Data System (ADS)

Hao, Haitian; Scalo, Carlo; Sen, Mihir; Semperlotti, Fabio

2018-01-01

Thermoacoustic oscillations have been one of the most exciting discoveries of the physics of fluids in the 19th century. Since its inception, scientists have formulated a comprehensive theoretical explanation of the basic phenomenon which has later found several practical applications to engineering devices. To date, all studies have concentrated on the thermoacoustics of fluid media where this fascinating mechanism was exclusively believed to exist. Our study shows theoretical and numerical evidence of the existence of thermoacoustic instabilities in solid media. Although the underlying physical mechanism exhibits some interesting similarities with its counterpart in fluids, the theoretical framework highlights relevant differences that have important implications on the ability to trigger and sustain the thermoacoustic response. This mechanism could pave the way to the development of highly robust and reliable solid-state thermoacoustic engines and refrigerators.

Facile synthesis and microwave absorbability of C@Ni–NiO core–shell hybrid solid sphere and multi-shelled NiO hollow sphere

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

Wu, Hongjing, E-mail: wuhongjing@mail.nwpu.edu.cn; Wu, Guanglei, E-mail: wuguanglei@mail.xjtu.edu.cn; Wu, Qiaofeng

2014-11-15

We reported the preparation of C@Ni–NiO core–shell hybrid solid spheres or multi-shelled NiO hollow spheres by combining a facile hydrothermal route with a calcination process in H{sub 2} or air atmosphere, respectively. The synthesized C@Ni–NiO core–shell solid spheres with diameters of approximately 2–6 μm were in fact built from dense NiO nanoparticles coated by random two-dimensional metal Ni nanosheets without any visible pores. The multi-shelled NiO hollow spheres were built from particle-like ligaments and there are a lot of pores with size of several nanometers on the surface. Combined Raman spectra with X-ray photoelectron spectra (XPS), it suggested that themore » defects in the samples play a limited role in the dielectric loss. Compared with the other samples, the permeability of the samples calcined in H{sub 2} and air was increased slightly and the natural resonance frequency shifted to higher frequency (7, 11 and 14 GHz, respectively), leading to an enhancement of microwave absorption property. For the sample calcined in H{sub 2}, an optimal reflection loss less than − 10 was obtained at 7 GHz with a matching thickness of 5.0 mm. Our study demonstrated the potential application of C@Ni–NiO core–shell hybrid solid sphere or multi-shelled NiO hollow sphere as a more efficient electromagnetic (EM) wave absorber. - Highlights: • C@Ni–NiO core–shell hybrid solid sphere was synthesized by a facile method. • Multi-shelled NiO hollow sphere was synthesized by a facile method. • It suggested that the defects in the samples play a limited role in dielectric loss. • The permeability of the samples calcined in H{sub 2} and air was increased. • Microwave absorbability of C@Ni–NiO core–shell hybrid solid sphere was investigated.« less

Role of adsorption in liquid lubrication

NASA Technical Reports Server (NTRS)

Groszek, A. J.

1973-01-01

Changes at solid-liquid interfaces caused by adsorption from solution are discussed paying attention to the following aspects: (1) stability of adsorbed films and the structure of metal-additive-film-liquid interface and effect of adsorbate orientation. (2) chemical versus physical adsorption, (3) heat of adsorption, (4) adsorption of additives, (5) activated adsorption, effect of activating adsorbates, (6) displacement phenomena at solid-liquid interfaces, (7) competition of antiwear additives, their solvents, and water, (8) effect of adsorption on the orientation of liquid in the interfacial region, and (9) relation between the chemical nature of solid surfaces and their interaction with liquid lubricants. The relevance of the above adsorption phenomena to lubrication is discussed, referring where possible to specific examples.

Electric shielding films for biased TEM samples and their application to in situ electron holography.

PubMed

Nomura, Yuki; Yamamoto, Kazuo; Hirayama, Tsukasa; Saitoh, Koh

2018-06-01

We developed a novel sample preparation method for transmission electron microscopy (TEM) to suppress superfluous electric fields leaked from biased TEM samples. In this method, a thin TEM sample is first coated with an insulating amorphous aluminum oxide (AlOx) film with a thickness of about 20 nm. Then, the sample is coated with a conductive amorphous carbon film with a thickness of about 10 nm, and the film is grounded. This technique was applied to a model sample of a metal electrode/Li-ion-conductive-solid-electrolyte/metal electrode for biasing electron holography. We found that AlOx film with a thickness of 10 nm has a large withstand voltage of about 8 V and that double layers of AlOx and carbon act as a 'nano-shield' to suppress 99% of the electric fields outside of the sample. We also found an asymmetry potential distribution between high and low potential electrodes in biased solid-electrolyte, indicating different accumulation behaviors of lithium-ions (Li+) and lithium-ion vacancies (VLi-) in the biased solid-electrolyte.

The Sample Analysis at Mars Investigation and Instrument Suite

NASA Technical Reports Server (NTRS)

Mahaffy, Paul; Webster, Christopher R.; Conrad, Pamela G.; Arvey, Robert; Bleacher, Lora; Brinckerhoff, William B.; Eigenbrode, Jennifer L.; Chalmers, Robert A.; Dworkin, Jason P.; Errigo, Therese;

Electrochemical pesticide detection with AutoDip--a portable platform for automation of crude sample analyses.

PubMed

Drechsel, Lisa; Schulz, Martin; von Stetten, Felix; Moldovan, Carmen; Zengerle, Roland; Paust, Nils

2015-02-07

Lab-on-a-chip devices hold promise for automation of complex workflows from sample to answer with minimal consumption of reagents in portable devices. However, complex, inhomogeneous samples as they occur in environmental or food analysis may block microchannels and thus often cause malfunction of the system. Here we present the novel AutoDip platform which is based on the movement of a solid phase through the reagents and sample instead of transporting a sequence of reagents through a fixed solid phase. A ball-pen mechanism operated by an external actuator automates unit operations such as incubation and washing by consecutively dipping the solid phase into the corresponding liquids. The platform is applied to electrochemical detection of organophosphorus pesticides in real food samples using an acetylcholinesterase (AChE) biosensor. Minimal sample preparation and an integrated reagent pre-storage module hold promise for easy handling of the assay. Detection of the pesticide chlorpyrifos-oxon (CPO) spiked into apple samples at concentrations of 10(-7) M has been demonstrated. This concentration is below the maximum residue level for chlorpyrifos in apples defined by the European Commission.

Solid sampling determination of total fluorine in baby food samples by high-resolution continuum source graphite furnace molecular absorption spectrometry.

PubMed

Ozbek, Nil; Akman, Suleyman

2016-11-15

This study describes the applicability of solid sampling technique for the determination of fluorine in various baby foods via molecular absorption of calcium monofluoride generated in a graphite furnace of high-resolution continuum source atomic absorption spectrometry. Fluorine was determined at CaF wavelength, 606.440nm in a graphite tube applying a pyrolysis temperature of 1000°C and a molecule forming temperature of 2200°C. The limit of detection and characteristic mass of the method were 0.20ng and 0.17ng of fluorine, respectively. The fluorine concentrations determined in standard reference sample (bush branches and leaves) were in good agreement with the certified values. By applying the optimized parameters, the concentration of fluorine in various baby foods were determined. The fluorine concentrations were ranged from

Optical Measurements on Solid Specimens of Solid Rocket Motor Exhaust and Solid Rocket Motor Slag

NASA Technical Reports Server (NTRS)

Roberts, F. E., III

1991-01-01

Samples of aluminum slag were investigated to aid the Earth Science and Applications Division at the Marshall Space Flight Center (MSFC). Alumina from space motor propellant exhaust and space motor propellant slag was examined as a component of space refuse. Thermal emittance and solar absorptivity measurements were taken to support their comparison with reflectance measurements derived from actual debris. To determine the similarity between the samples and space motor exhaust or space motor slag, emittance and absorbance results were correlated with an examination of specimen morphology.

Space Shuttle solid rocket motor exposure monitoring

NASA Technical Reports Server (NTRS)

Brown, S. W.

1993-01-01

During the processing of the Space Shuttle Solid Rocket Booster (SRB), segments at the Kennedy Space Center, an odor was detected around the solid propellant. An Industrial Hygiene survey was conducted to determine the chemical identity of the SRB offgassing constituents. Air samples were collected inside a forward SRB segment and analyzed to determine chemical composition. Specific chemical analysis for suspected offgassing constituents of the propellant indicated ammonia to be present. A gas chromatograph mass spectroscopy (GC/MS) analysis of the air samples detected numerous high molecular weight hydrocarbons.

The potential of household solid waste reduction in Sukomanunggal District, Surabaya

NASA Astrophysics Data System (ADS)

Warmadewanthi, I. D. A. A.; Kurniawati, S.

2018-01-01

The rapid population growth affects the amount of waste generated. Sukomanunggal Subdistrict is the densest area in West Surabaya which has a population of 100,602 inhabitants with a total area of 11.2 km2. The population growth significantly affects the problem of limited land for landfill facilities (final processing sites). According to the prevailing regulations, solid waste management solutions include the solid waste reduction and management. This study aims to determine the potential reduction of household solid waste at the sources. Household solid waste samplings were performed for eight consecutive days. The samples were then analyzed to obtain the generation rate, density, and composition so that the household solid waste reduction potential for the next 20 years could be devised. Results of the analysis showed that the value of waste is 0.27 kg/person/day, while the total household solid waste generation amounted to 27,162.58 kg/day or 187.70 m3/day. Concerning the technical aspects, the current solid waste reduction in Sukomanunggal Subdistrict has reached 2.1% through the application of waste bank, composting, and scavenging activities at the dumping sites by the garbage collectors. In the year of 2036, the potential reduction of household solid waste in Sukomanunggal Subdistrict has been estimated to reach 28.0%.

Visualizing the shape of soft solid and fluid contacts between two surfaces

NASA Astrophysics Data System (ADS)

Pham, Jonathan; Schellenberger, Frank; Kappl, Michael; Vollmer, Doris; Butt, Hans-Jürgen

The soft contact between two surfaces is fundamentally interesting for soft materials and fluid mechanics and relevant for friction and wear. The deformation of soft solid interfaces has received much interest because it interestingly reveals similarities to fluid wetting. We present an experimental route towards visualizing the three-dimensional contact geometry of either liquid-solid (i.e., oil and glass) or solid-solid (i.e., elastomer and glass) interfaces using a home-built combination of confocal microscopy and atomic force microscopy. We monitor the shape of a fluid capillary bridge and the depth of indentation in 3D while simultaneously measuring the force. In agreement with theoretical predictions, the height of the capillary bridge depends on the interfacial tensions. By using a slowly evaporating solvent, we quantify the temporal evolution of the capillary bridge and visualized the influence of pinning points on its shape. The position dependence of the advancing and receding contact angle along the three-phase contact line, particle-liquid-air, is resolved. Extending our system, we explore the contact deformation of soft solids where elasticity, in addition to surface tension, becomes an important factor.

Processing of solid solution, mixed uranium/refractory metal carbides for advanced space nuclear power and propulsion systems

NASA Astrophysics Data System (ADS)

Knight, Travis Warren

Nuclear thermal propulsion (NTP) and space nuclear power are two enabling technologies for the manned exploration of space and the development of research outposts in space and on other planets such as Mars. Advanced carbide nuclear fuels have been proposed for application in space nuclear power and propulsion systems. This study examined the processing technologies and optimal parameters necessary to fabricate samples of single phase, solid solution, mixed uranium/refractory metal carbides. In particular, the pseudo-ternary carbide, UC-ZrC-NbC, system was examined with uranium metal mole fractions of 5% and 10% and corresponding uranium densities of 0.8 to 1.8 gU/cc. Efforts were directed to those methods that could produce simple geometry fuel elements or wafers such as those used to fabricate a Square Lattice Honeycomb (SLHC) fuel element and reactor core. Methods of cold uniaxial pressing, sintering by induction heating, and hot pressing by self-resistance heating were investigated. Solid solution, high density (low porosity) samples greater than 95% TD were processed by cold pressing at 150 MPa and sintering above 2600 K for times longer than 90 min. Some impurity oxide phases were noted in some samples attributed to residual gases in the furnace during processing. Also, some samples noted secondary phases of carbon and UC2 due to some hyperstoichiometric powder mixtures having carbon-to-metal ratios greater than one. In all, 33 mixed carbide samples were processed and analyzed with half bearing uranium as ternary carbides of UC-ZrC-NbC. Scanning electron microscopy, x-ray diffraction, and density measurements were used to characterize samples. Samples were processed from powders of the refractory mono-carbides and UC/UC 2 or from powders of uranium hydride (UH3), graphite, and refractory metal carbides to produce hypostoichiometric mixed carbides. Samples processed from the constituent carbide powders and sintered at temperatures above the melting point of UC showed signs of liquid phase sintering and were shown to be largely solid solutions. Pre-compaction of mixed carbide powders prior to sintering was shown to be necessary to achieve high densities. Hypostoichiometric, samples processed at 2500 K exhibited only the initial stage of sintering and solid solution formation. Based on these findings, a suggested processing methodology is proposed for producing high density, solid solution, mixed carbide fuels. Pseudo-binary, refractory carbide samples hot pressed at 3100 K and 6 MPa showed comparable densities (approximately 85% of the theoretical value) to samples processed by cold pressing and sintering at temperatures of 2800 K.

234U/238U isotope data from groundwater and solid-phase leachate samples near Tuba City Open Dump, Tuba City, Arizona

USGS Publications Warehouse

Johnson, Raymond H.; Horton, Robert J.; Otton, James K.; Ketterer, Michael K.

2012-01-01

This report releases 234U/238U isotope data, expressed as activity ratios, and uranium concentration data from analyses completed at Northern Arizona University for groundwater and solid-phase leachate samples that were collected in and around Tuba City Open Dump, Tuba City, Arizona, in 2008.

Evolution of structural, electronic and magneto-transport properties of Sr2Ir1-xTixO4 5d based oxide

NASA Astrophysics Data System (ADS)

Bhatti, Imtiaz Noor; Pramanik, A. K.

2018-05-01

To investigate the effect of chemical doping on structural and transport properties in Sr2IrO4, in this study we have doped Ti4+ (3d0) at Ir4+ (5d5) site. Thus Ti doping introduces hole in the electronic band moreover, it also weaken the spin orbital coupling (SOC) and enhance electronic correlation (U). We have prepared the polycrystalline samples of Sr2Ir1-xTixO4 with x = 0.0 0.05 and 0.10 with solid state reaction method. Single phase and chemically pure samples were obtained. All samples crystalizes in tetragonal structure and I41/acd symmetry. The structural analysis shows the evolution of lattice parameter with doping. The temperature dependent resistivity is measured using four probe technique down in the temperature range 5 K-300 K. The resistivity increases with Ti doping. Temperature dependency of resistivity is explained by thermal activated 2-dimensional Mott Variable Hopping range model. To further understand the transport behavior both temperature and field dependent magneto-resistance is also studied. Negative magneto-resistance (MR) has been observed for all samples at 50 K. The MR shows quadratic field dependence at high field, implies a relevance of a quantum interference effect in this spin orbital coupled insulator.

Comparison of solid-phase and eluate assays to gauge the ecotoxicological risk of organic wastes on soil organisms.

PubMed

Domene, Xavier; Alcañiz, Josep M; Andrés, Pilar

2008-02-01

Development of methodologies to assess the safety of reusing polluted organic wastes in soil is a priority in Europe. In this study, and coupled with chemical analysis, seven organic wastes were subjected to different aquatic and soil bioassays. Tests were carried out with solid-phase waste and three different waste eluates (water, methanol, and dichloromethane). Solid-phase assays were indicated as the most suitable for waste testing not only in terms of relevance for real situations, but also because toxicity in eluates was generally not representative of the chronic effects in solid-phase. No general correlations were found between toxicity and waste pollutant burden, neither in solid-phase nor in eluate assays, showing the inability of chemical methods to predict the ecotoxicological risks of wastes. On the contrary, several physicochemical parameters reflecting the degree of low organic matter stability in wastes were the main contributors to the acute toxicity seen in collembolans and daphnids.

Distinct ice patterns on solid surfaces with various wettabilities

PubMed Central

Liu, Jie; Zhu, Chongqin; Liu, Kai; Jiang, Ying; Song, Yanlin; Francisco, Joseph S.; Zeng, Xiao Cheng; Wang, Jianjun

2017-01-01

No relationship has been established between surface wettability and ice growth patterns, although ice often forms on top of solid surfaces. Here, we report experimental observations obtained using a process specially designed to avoid the influence of nucleation and describe the wettability-dependent ice morphology on solid surfaces under atmospheric conditions and the discovery of two growth modes of ice crystals: along-surface and off-surface growth modes. Using atomistic molecular dynamics simulation analysis, we show that these distinct ice growth phenomena are attributable to the presence (or absence) of bilayer ice on solid surfaces with different wettability; that is, the formation of bilayer ice on hydrophilic surface can dictate the along-surface growth mode due to the structural match between the bilayer hexagonal ice and the basal face of hexagonal ice (ice Ih), thereby promoting rapid growth of nonbasal faces along the hydrophilic surface. The dramatically different growth patterns of ice on solid surfaces are of crucial relevance to ice repellency surfaces. PMID:29073045

Distinct ice patterns on solid surfaces with various wettabilities.

PubMed

Liu, Jie; Zhu, Chongqin; Liu, Kai; Jiang, Ying; Song, Yanlin; Francisco, Joseph S; Zeng, Xiao Cheng; Wang, Jianjun

2017-10-24

No relationship has been established between surface wettability and ice growth patterns, although ice often forms on top of solid surfaces. Here, we report experimental observations obtained using a process specially designed to avoid the influence of nucleation and describe the wettability-dependent ice morphology on solid surfaces under atmospheric conditions and the discovery of two growth modes of ice crystals: along-surface and off-surface growth modes. Using atomistic molecular dynamics simulation analysis, we show that these distinct ice growth phenomena are attributable to the presence (or absence) of bilayer ice on solid surfaces with different wettability; that is, the formation of bilayer ice on hydrophilic surface can dictate the along-surface growth mode due to the structural match between the bilayer hexagonal ice and the basal face of hexagonal ice (ice I h ), thereby promoting rapid growth of nonbasal faces along the hydrophilic surface. The dramatically different growth patterns of ice on solid surfaces are of crucial relevance to ice repellency surfaces. Published under the PNAS license.

Effect of air confinement on thermal contact resistance in nanoscale heat transfer

NASA Astrophysics Data System (ADS)

Pratap, Dheeraj; Islam, Rakibul; Al-Alam, Patricia; Randrianalisoa, Jaona; Trannoy, Nathalie

2018-03-01

Here, we report a detailed analysis of thermal contact resistance (R c) of nano-size contact formed between a Wollaston wire thermal probe and the used samples (fused silica and titanium) as a function of air pressure (from 1 Pa to 105 Pa). Moreover, we suggest an analytical model using experimental data to extract R c. We found that for both samples, the thermal contact resistance decreases with increasing air pressure. We also showed that R c strongly depends on the thermal conductivity of materials keeping other parameters the same, such as roughness of the probe and samples, as well as the contact force. We provide a physical explanation of the R c trend with pressure and thermal conductivity of the materials: R c is ascribed to the heat transfer through solid-solid (probe-sample) contact and confined air at nanoscale cavities, due to the rough nature of the materials in contact. The contribution of confined air on heat transfer through the probe sample contact is significant at atmospheric pressure but decreases as the pressure decreases. In vacuum, only the solid-solid contact contributes to R c. In addition, theoretical calculations using the well-known acoustic and diffuse mismatch models showed a high thermal conductivity material that exhibits high heat transmission and consequently low R c, supporting our findings.

Noncontact technique for measuring the electrical resistivity and magnetic susceptibility of electrostatically levitated materials

NASA Astrophysics Data System (ADS)

Rustan, G. E.; Spyrison, N. S.; Kreyssig, A.; Prozorov, R.; Goldman, A. I.

2012-10-01

We describe the development of a new method for measuring the electrical resistivity and magnetic susceptibility of high temperature liquids and solids. The technique combines a tunnel diode oscillator with an electrostatic levitation furnace to perform noncontact measurements on spherical samples 2-3 mm in diameter. The tank circuit of the oscillator is inductively coupled to the sample, and measurements of the oscillator frequency as a function of sample temperature can be translated into changes in the sample's electrical resistivity and magnetic susceptibility. Particular emphasis is given on the need to improve the positional stability of the levitated samples, as well as the need to stabilize the temperature of the measurement coil. To demonstrate the validity of the technique, measurements have been performed on solid spheres of pure zirconium and low-carbon steel. In the case of zirconium, while absolute values of the resistivity were not determined, the temperature dependence of the resistivity was measured over the range of 640-1770 K and found to be in good agreement with literature data. In the case of low-carbon steel, the ferromagnetic-paramagnetic transition was clearly observable and, when combined with thermal data, appears to occur simultaneously with the solid-solid structural transition.

Characterization of rhamnolipids by liquid chromatography/mass spectrometry after solid-phase extraction.

PubMed

Behrens, Beate; Engelen, Jeannine; Tiso, Till; Blank, Lars Mathias; Hayen, Heiko

2016-04-01

Rhamnolipids are surface-active agents with a broad application potential that are produced in complex mixtures by bacteria of the genus Pseudomonas. Analysis from fermentation broth is often characterized by laborious sample preparation and requires hyphenated analytical techniques like liquid chromatography coupled to mass spectrometry (LC-MS) to obtain detailed information about sample composition. In this study, an analytical procedure based on chromatographic method development and characterization of rhamnolipid sample material by LC-MS as well as a comparison of two sample preparation methods, i.e., liquid-liquid extraction and solid-phase extraction, is presented. Efficient separation was achieved under reversed-phase conditions using a mixed propylphenyl and octadecylsilyl-modified silica gel stationary phase. LC-MS/MS analysis of a supernatant from Pseudomonas putida strain KT2440 pVLT33_rhlABC grown on glucose as sole carbon source and purified by solid-phase extraction revealed a total of 20 congeners of di-rhamnolipids, mono-rhamnolipids, and their biosynthetic precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) with different carbon chain lengths from C8 to C14, including three rhamnolipids with uncommon C9 and C11 fatty acid residues. LC-MS and the orcinol assay were used to evaluate the developed solid-phase extraction method in comparison with the established liquid-liquid extraction. Solid-phase extraction exhibited higher yields and reproducibility as well as lower experimental effort.

Microwave assisted solid phase extraction for separation preconcentration sulfamethoxazole in wastewater using tyre based activated carbon as solid phase material prior to spectrophotometric determination.

PubMed

Mogolodi Dimpe, K; Mpupa, Anele; Nomngongo, Philiswa N

2018-01-05

This work was chiefly encouraged by the continuous consumption of antibiotics which eventually pose harmful effects on animals and human beings when present in water systems. In this study, the activated carbon (AC) was used as a solid phase material for the removal of sulfamethoxazole (SMX) in wastewater samples. The microwave assisted solid phase extraction (MASPE) as a sample extraction method was employed to better extract SMX in water samples and finally the analysis of SMX was done by the UV-Vis spectrophotometer. The microwave assisted solid phase extraction method was optimized using a two-level fractional factorial design by evaluating parameters such as pH, mass of adsorbent (MA), extraction time (ET), eluent ratio (ER) and microwave power (MP). Under optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) were 0.5μgL -1 and 1.7μgL -1 , respectively, and intraday and interday precision expressed in terms of relative standard deviation were >6%.The maximum adsorption capacity was 138mgg -1 for SMX and the adsorbent could be reused eight times. Lastly, the MASPE method was applied for the removal of SMX in wastewater samples collected from a domestic wastewater treatment plant (WWTP) and river water. Copyright © 2017 Elsevier B.V. All rights reserved.

Molecularly imprinted polymer/cryogel composites for solid-phase extraction of bisphenol A from river water and wine.

PubMed

Baggiani, Claudio; Baravalle, Patrizia; Giovannoli, Cristina; Anfossi, Laura; Giraudi, Gianfranco

2010-05-01

Superporous monolithic hydrogels (cryogel monoliths) are elastic, sponge-like materials that can be prepared in an aqueous medium through a cryotropic gelation technique. These monoliths show interesting properties for the development of high-throughput solid-phase extraction supports to treat large volumes of aqueous samples. In this work, a cryogel-supported molecularly imprinted solid-phase extraction approach for the endocrine disruptor bisphenol A (BPA) from river water and wine samples is presented. An imprinted polymer with molecular recognition properties for BPA was prepared in acetonitrile by thermal polymerization of a mixture of 4,4'-dihydroxy-2,2-diphenyl-1,1,1,3,3,3-trifluoropropane as a mimic template of BPA, 4-vinylpyridine and trimethylolpropane trimethacrylate in a molar ratio of 1 + 6 + 6. Fine imprinted particles (<10 microm) were embedded in a poly-acrylamide-co-N,N'-methylenbisacrylamide cryogel obtained by ammonium persulfate-induced cryopolymerization at -18 degrees C. The resulting monolithic gel was evaluated for its use as a sorbent support in an off-line solid-phase extraction approach to recover BPA from dilute aqueous samples with minimum pre-loading work-up. The optimized extraction protocol resulted in a reliable MISPE method suitable to selectively extract and preconcentrate BPA from river water and red wine samples, demonstrating the practical feasibility of cryogel-trapped imprinted polymers as solid-phase extraction materials.

Probe Heating Method for the Analysis of Solid Samples Using a Portable Mass Spectrometer

PubMed Central

Kumano, Shun; Sugiyama, Masuyuki; Yamada, Masuyoshi; Nishimura, Kazushige; Hasegawa, Hideki; Morokuma, Hidetoshi; Inoue, Hiroyuki; Hashimoto, Yuichiro

2015-01-01

We previously reported on the development of a portable mass spectrometer for the onsite screening of illicit drugs, but our previous sampling system could only be used for liquid samples. In this study, we report on an attempt to develop a probe heating method that also permits solid samples to be analyzed using a portable mass spectrometer. An aluminum rod is used as the sampling probe. The powdered sample is affixed to the sampling probe or a droplet of sample solution is placed on the tip of the probe and dried. The probe is then placed on a heater to vaporize the sample. The vapor is then introduced into the portable mass spectrometer and analyzed. With the heater temperature set to 130°C, the developed system detected 1 ng of methamphetamine, 1 ng of amphetamine, 3 ng of 3,4-methylenedioxymethamphetamine, 1 ng of 3,4-methylenedioxyamphetamine, and 0.3 ng of cocaine. Even from mixtures consisting of clove powder and methamphetamine powder, methamphetamine ions were detected by tandem mass spectrometry. The developed probe heating method provides a simple method for the analysis of solid samples. A portable mass spectrometer incorporating this method would thus be useful for the onsite screening of illicit drugs. PMID:26819909

Phenomenological study of decoherence in solid-state spin qubits due to nuclear spin diffusion

NASA Astrophysics Data System (ADS)

Biercuk, Michael J.; Bluhm, Hendrik

2011-06-01

We present a study of the prospects for coherence preservation in solid-state spin qubits using dynamical decoupling protocols. Recent experiments have provided the first demonstrations of multipulse dynamical decoupling sequences in this qubit system, but quantitative analyses of potential coherence improvements have been hampered by a lack of concrete knowledge of the relevant noise processes. We present calculations of qubit coherence under the application of arbitrary dynamical decoupling pulse sequences based on an experimentally validated semiclassical model. This phenomenological approach bundles the details of underlying noise processes into a single experimentally relevant noise power spectral density. Our results show that the dominant features of experimental measurements in a two-electron singlet-triplet spin qubit can be replicated using a 1/ω2 noise power spectrum associated with nuclear spin flips in the host material. Beginning with this validation, we address the effects of nuclear programming, high-frequency nuclear spin dynamics, and other high-frequency classical noise sources, with conjectures supported by physical arguments and microscopic calculations where relevant. Our results provide expected performance bounds and identify diagnostic metrics that can be measured experimentally in order to better elucidate the underlying nuclear spin dynamics.

13C and 1H NMR (Nuclear Magnetic Resonance) studies of solid polyolefines

NASA Technical Reports Server (NTRS)

Cudby, M. E. A.; Harris, R. K.; Metcalfe, K.; Packer, K. J.; Smith, P. W. R.

1983-01-01

The basis of H-1 and C-13 high-resolution NMR investigations of solid polymers is outlined. The C-13 NMR spectra of solid syndiotactic and isotactic polypropene are discussed and their interpretation in terms of conformation and chain-packing effects are reviewed. The effects of decreasing temperature on the C-13 high-resolution spectrum of an annealed sample of isotactic polypropene is described and interpreted in terms of the crystal structure. The question of the proportion of the sample giving rise to C-13 signals is addressed and some results reported. The main cause for observing only part of the total sample is shown to be the H-1 rotating frame spin-lattice relaxation behavior. The H-1 spin-lattice relaxation and spectral characteristics of a number of polyolefin samples are summarized and the role of spin-diffusion discussed.

Investigation of Tank 241-AW-104 Composite Floating Layer

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

Meznarich, H. K.; Bolling, S. D.; Lachut, J. S.

Seven grab samples and one field blank were taken from Tank 241-AW-104 (AW-104) on June 2, 2017, and received at 222-S Laboratory on June 5, 2017. A visible layer with brown solids was observed floating on the top of two surface tank waste samples (4AW-17-02 and 4AW 17 02DUP). The floating layer from both samples was collected, composited, and submitted for chemical analyses and solid phase characterization in order to understand the composition of the floating layer. Tributyl phosphate and tridecane were higher in the floating layer than in the aqueous phase. Density in the floating layer was slightly lowermore » than the mean density of all grab samples. Sodium nitrate and sodium carbonate were major components with a trace of gibbsite and very small size agglomerates were present in the solids of the floating layer. The supernate consisted of organics, soluble salt, and particulates.« less

Nonthermal effects in photostimulated solid state reaction of Mn doped SrTiO3

NASA Astrophysics Data System (ADS)

Daraselia, D.; Japaridze, D.; Jibuti, Z.; Shengelaya, A.; Müller, K. A.

2017-04-01

The effect of a photostimulated solid state reaction was investigated in Mn doped SrTiO3 samples. Light irradiation was performed by either halogen or UV lamps in order to study the effect of the spectral composition, and the results were compared with samples prepared at the same temperatures in a conventional furnace. The obtained samples were studied by X-ray diffraction for structural characterization and by Electron Paramagnetic Resonance, which provides microscopic information about the local environment as well as the valence state of Mn ions. It was found that light irradiation significantly enhances the solid state reaction rate compared to synthesis in the conventional furnace. Moreover, it was observed that UV lamp irradiation is much more effective compared to halogen lamps. This indicates that the absorption of light with energy larger than the materials band gap plays an important role and points towards the nonthermal mechanism of the photostimulated solid state reaction.

Polymorphs of Theophylline Characterized by DNP Enhanced Solid-State NMR

PubMed Central

2015-01-01

We show how dynamic nuclear polarization (DNP) enhanced solid-state NMR spectroscopy can be used to characterize polymorphs and solvates of organic solids. We applied DNP to three polymorphs and one hydrated form of the asthma drug molecule theophylline. For some forms of theophylline, sample grinding and impregnation with the radical-containing solution, which are necessary to prepare the samples for DNP, were found to induce polymorphic transitions or desolvation between some forms. We present protocols for sample preparation for solid-state magic-angle spinning (MAS) DNP experiments that avoid the polymorphic phase transitions in theophylline. These protocols include cryogrinding, grinding under inert atmosphere, and the appropriate choice of the impregnating liquid. By applying these procedures, we subsequently demonstrate that two-dimensional correlation experiments, such as 1H–13C and 1H–15N HETCOR or 13C–13C INADEQUATE, can be obtained at natural isotopic abundance in reasonable times, thus enabling more advanced structural characterization of polymorphs. PMID:26393368

Molecularly imprinted solid-phase extraction sorbent for the clean-up of chlorinated phenoxyacids from aqueous samples.

PubMed

Baggiani, C; Giovannoli, C; Anfossi, L; Tozzi, C

2001-12-14

A molecularly imprinted polymer (MIP) was synthesized using the herbicide 2,4,5-trichlorophenoxyacetic acid as a template, 4-vinylpyridine as an interacting monomer, ethylendimethacrylate as a cross-linker and a methanol-water mixture as a porogen. The binding properties and the selectivity of the polymer towards the template were investigated by frontal and zonal liquid chromatography. The polymer was used as a solid-phase extraction material for the clean-up of the template molecule and some related herbicides (2,4-dichlorophenoxyacetic acid, fenoprop, dichlorprop) from river water samples at a concentration level of ng/ml with quantitative recoveries comparable with those obtained with a traditional C18 reversed-phase column when analyzed by capillary electrophoresis. The results obtained show that the MIP-based approach to the solid-phase extraction is comparable with the more traditional solid-phase extraction with C18 reversed-phase columns in terms of recovery, but it is superior in terms of sample clean-up.

Characterization of acid-base properties of two gibbsite samples in the context of literature results.

PubMed

Adekola, F; Fédoroff, M; Geckeis, H; Kupcik, T; Lefèvre, G; Lützenkirchen, J; Plaschke, M; Preocanin, T; Rabung, T; Schild, D

2011-02-01

Two different gibbsites, one commercial and one synthesized according to a frequently applied recipe, were studied in an interlaboratory attempt to gain insight into the origin of widely differing reports on gibbsite acid-base surface properties. In addition to a thorough characterization of the two solids, several methods relevant to the interfacial charging were applied to the two samples: potentiometric titrations to obtain the "apparent" proton related surface charge density, zeta-potential measurements characterizing the potential at the plane of shear, and Attenuated Total Reflection Infrared Spectroscopy (ATR-IR) to obtain information on the variation of counter-ion adsorption with pH (using nitrate as a probe). Values of the IEP at 9-10 and 11.2-11.3 were found for the commercial and synthesized sample, respectively. The experimental observations revealed huge differences in the charging behavior between the two samples. Such differences also appeared in the titration kinetics. A detailed literature review revealed similar disparity with no apparent systematic trend. While previously the waiting time between additions had been advocated to explain such differences among synthesized samples, our results do not support such a conclusion. Instead, we find that the amount of titrant added in each aliquot appears to have a significant influence on the titration curves. While we can relate a number of observations to others, a number of open questions and contradictions remain. We suggest various processes, which can explain the observed behavior. Copyright © 2010 Elsevier Inc. All rights reserved.

Assessment of a combined gas chromatography mass spectrometer sensor (GC-MSS) system for detecting biologically relevant volatile compounds (VCs).

PubMed

Gould, Oliver; Wieczorek, Tomas; de Lacy Costello, Ben P J; Persad, Raj; Ratcliffe, Norman

2017-09-26

There have been a number of studies in which metal oxide sensors (MOS) have replaced conventional analytical detectors in gas chromatography systems. However, despite the use of these instruments in a range of applications including breath research the sensor responses (i.e. resistance changes w.r.t. concentration of VCs) remain largely unreported. This paper addresses that issue by comparing the response of a metal oxide sensor directly with a mass spectrometer (MS), whereby both detectors are interfaced to the same GC column using an s-swafer. It was demonstrated that the sensitivity of an in-house fabricated ZnO/ SnO2 thick film MOS was superior to a modern MS for the detection of a wide range of volatile compounds (VCs) of different functionalities and masses. Better techniques for detection and quantification of these VCs is valuable, as many of these compounds are commonly reported throughout the scientific literature. This is also the first published report of a combined GC-MS sensor system. These 2 different detector technologies when combined, should enhance discriminatory abilities to aid disease diagnoses using volatiles from e.g. breath, and bodily fluids. 29 chemical standards have been tested using solid phase micro-extraction; 25 of these compounds are found on human breath. In all but 2 instances the sensor exhibited the same or superior limit of detection compared to the MS. 12 stool samples from healthy participants were analysed, the sensor detected, on average 1.6 peaks more per sample than the MS. Similarly analysing the headspace of E. coli broth cultures the sensor detected 6.9 more peaks per sample versus the MS. This greater sensitivity is primarily a function of the superior limits of detection of the metal oxide sensor. This shows that systems based on the combination of chromatography systems with solid state sensors shows promise for a range of applications. © 2017 IOP Publishing Ltd.

Assessment of a combined gas chromatography mass spectrometer sensor system for detecting biologically relevant volatile compounds.

PubMed

Gould, Oliver; Wieczorek, Tom; de Lacy Costello, Ben; Persad, Raj; Ratcliffe, Norman

2017-12-06

There have been a number of studies in which metal oxide sensors (MOS) have replaced conventional analytical detectors in gas chromatography systems. However, despite the use of these instruments in a range of applications including breath research the sensor responses (i.e. resistance changes w.r.t. concentration of VCs) remain largely unreported. This paper addresses that issue by comparing the response of a metal oxide sensor directly with a mass spectrometer (MS), whereby both detectors are interfaced to the same GC column using an s-swafer. It was demonstrated that the sensitivity of an in-house fabricated ZnO/SnO 2 thick film MOS was superior to a modern MS for the detection of a wide range of volatile compounds (VCs) of different functionalities and masses. Better techniques for detection and quantification of these VCs is valuable, as many of these compounds are commonly reported throughout the scientific literature. This is also the first published report of a combined GC-MS sensor system. These two different detector technologies when combined, should enhance discriminatory abilities to aid disease diagnoses using volatiles from e.g. breath, and bodily fluids. Twenty-nine chemical standards have been tested using solid phase micro-extraction; 25 of these compounds are found on human breath. In all but two instances the sensor exhibited the same or superior limit of detection compared to the MS. Twelve stool samples from healthy participants were analysed; the sensor detected, on average 1.6 peaks more per sample than the MS. Similarly, analysing the headspace of E. coli broth cultures the sensor detected 6.9 more peaks per sample versus the MS. This greater sensitivity is primarily a function of the superior limits of detection of the metal oxide sensor. This shows that systems based on the combination of chromatography systems with solid state sensors shows promise for a range of applications.

A solid-state dedicated circularly polarized luminescence spectrophotometer: Development and application.

PubMed

Harada, Takunori; Hayakawa, Hiroshi; Watanabe, Masayuki; Takamoto, Makoto

2016-07-01

A new solid-state dedicated circularly polarized luminescence (CPL) instrument (CPL-200CD) was successfully developed for measuring true CPL spectra for optically anisotropic samples on the basis of the Stokes-Mueller matrix approach. Electric components newly installed in the CPL-200CD include a pulse motor-driven sample rotation holder and a 100 kHz lock-in amplifier to achieve the linearly polarized luminescence measurement, which is essential for obtaining the true CPL signal for optically anisotropic samples. An acquisition approach devised for solid-state CPL analysis reduces the measurement times for a data set by ca. 98% compared with the time required in our previous method. As a result, the developed approach is very effective for samples susceptible to light-induced degradation. The theory and implementation of the method are described, and examples of its application to a CPL sample with macroscopic anisotropies are provided. An important advantage of the developed instrument is its ability to obtain molecular information for both excited and ground states because circular dichroism measurements can be performed by switching the monochromatic light to white light without rearrangement of the sample.

Solid-Phase Extraction (SPE): Principles and Applications in Food Samples.

PubMed

Ötles, Semih; Kartal, Canan

2016-01-01

Solid-Phase Extraction (SPE) is a sample preparation method that is practised on numerous application fields due to its many advantages compared to other traditional methods. SPE was invented as an alternative to liquid/liquid extraction and eliminated multiple disadvantages, such as usage of large amount of solvent, extended operation time/procedure steps, potential sources of error, and high cost. Moreover, SPE can be plied to the samples combined with other analytical methods and sample preparation techniques optionally. SPE technique is a useful tool for many purposes through its versatility. Isolation, concentration, purification and clean-up are the main approaches in the practices of this method. Food structures represent a complicated matrix and can be formed into different physical stages, such as solid, viscous or liquid. Therefore, sample preparation step particularly has an important role for the determination of specific compounds in foods. SPE offers many opportunities not only for analysis of a large diversity of food samples but also for optimization and advances. This review aims to provide a comprehensive overview on basic principles of SPE and its applications for many analytes in food matrix.

Radiative characteristics of a thin solid fuel at discrete levels of pyrolysis: Angular, spectral, and thermal dependencies

NASA Astrophysics Data System (ADS)

Pettegrew, Richard Dale

Numerical models of solid fuel combustion rely on accurate radiative property values to properly account for radiative heat transfer to and from the surface. The spectral properties can change significantly over the temperature range from ambient to burnout temperature. The variations of these properties are due to mass loss (as the sample pyrolyzes), chemical changes, and surface finish changes. In addition, band-integrated properties can vary due to the shift in the peak of the Planck curve as the temperature increases, which results in differing weightings of the spectral values. These effects were quantified for a thin cellulosic fuel commonly used in microgravity combustion studies (KimWipesRTM). Pyrolytic effects were simulated by heat-treating the samples in a constant temperature oven for varying times. Spectral data was acquired using a Fourier Transform Infrared (FTIR) spectrometer, along with an integrating sphere. Data was acquired at different incidence angles by mounting the samples at different angles inside the sphere. Comparisons of samples of similar area density created using different heat-treatment regimens showed that thermal history of the samples was irrelevant in virtually all spectral regions, with overall results correlating well with changes in area density. Spectral, angular, and thermal dependencies were determined for a representative data set, showing that the spectral absorptance decreases as the temperature increases, and decreases as the incidence angle varies from normal. Changes in absorptance are primarily offset by corresponding changes in transmittances, with reflectance values shown to be low over the tested spectral region of 2.50 mum to 24.93 mum. Band-integrated values were calculated as a function of temperature for the entire tested spectral region, as well as limited bands relevant for thermal imaging applications. This data was used to demonstrate the significant error that is likely if incorrect emittance values are used in heat transfer calculations. The pyrolyzed samples were also used to determine the activation energy and pre-exponential factor needed in the zeroth-order Arrhenius reaction, sometimes used to model the mass loss from the surface in numerical models. The values determined were used to calculate an estimated peak surface temperature, which agrees well with experimentally determined values.

Analysis of the contaminants released from municipal solid waste landfill site: A case study.

PubMed

Samadder, S R; Prabhakar, R; Khan, D; Kishan, D; Chauhan, M S

2017-02-15

Release and transport of leachate from municipal solid waste landfills pose a potential hazard to both surrounding ecosystems and human populations. In the present study, soil, groundwater, and surface water samples were collected from the periphery of a municipal solid waste landfill (located at Ranital of Jabalpur, Madhya Pradesh, India) for laboratory analysis to understand the release of contaminants. The landfill does not receive any solid wastes for dumping now as the same is under a landfill closure plan. Groundwater and soil samples were collected from the bore holes of 15m deep drilled along the periphery of the landfill and the surface water samples were collected from the existing surface water courses near the landfill. The landfill had neither any bottom liner nor any leachate collection and treatment system. Thus the leachate generated from the landfills finds paths into the groundwater and surrounding surface water courses. Concentrations of various physico-chemical parameters including some toxic metals (in collected groundwater, soil, and surface water samples) and microbiological parameters (in surface water samples) were determined. The analyzed data were integrated into ArcGIS environment and the spatial distribution of the metals and other physic- chemical parameter across the landfill was extrapolated to observe the distribution. The statistical analysis and spatial variations indicated the leaching of metals from the landfill to the groundwater aquifer system. The study will help the readers and the municipal engineers to understand the release of contaminants from landfills for better management of municipal solid wastes. Copyright © 2016 Elsevier B.V. All rights reserved.

Heat Management Strategies for Solid-state NMR of Functional Proteins

PubMed Central

Fowler, Daniel J.; Harris, Michael J.; Thompson, Lynmarie K.

2012-01-01

Modern solid-state NMR methods can acquire high-resolution protein spectra for structure determination. However, these methods use rapid sample spinning and intense decoupling fields that can heat and denature the protein being studied. Here we present a strategy to avoid destroying valuable samples. We advocate first creating a sacrificial sample, which contains unlabeled protein (or no protein) in buffer conditions similar to the intended sample. This sample is then doped with the chemical shift thermometer Sm2Sn2O7. We introduce a pulse scheme called TCUP (for Temperature Calibration Under Pulseload) that can characterize the heating of this sacrificial sample rapidly, under a variety of experimental conditions, and with high temporal resolution. Sample heating is discussed with respect to different instrumental variables such as spinning speed, decoupling strength and duration, and cooling gas flow rate. The effects of different sample preparation variables are also discussed, including ionic strength, the inclusion of cryoprotectants, and the physical state of the sample (i.e. liquid, solid, or slurry). Lastly, we discuss probe detuning as a measure of sample thawing that does not require retuning the probe or using chemical shift thermometer compounds. Use of detuning tests and chemical shift thermometers with representative sample conditions makes it possible to maximize the efficiency of the NMR experiment while retaining a functional sample. PMID:22868258

Application of solid phase extraction procedures for rare earth elements determination in environmental samples.

PubMed

Pyrzynska, Krystyna; Kubiak, Anna; Wysocka, Irena

2016-07-01

Determination of rare earth elements in environmental samples requires often pre-concentration and separation step due to a low metal content and high concentration of the interfering matrix components. A solid phase extraction technique with different kind of solid sorbents offers a high enrichment factor, rapid phase separation and the possibility of its combination with various detection techniques used either in on-line or off-line mode. The recent developments in this area published over the last five years are presented and discussed in this paper. Copyright © 2016 Elsevier B.V. All rights reserved.

Mutation spectrum and differential gene expression in cystic and solid vestibular schwannoma.

PubMed

Zhang, Zhihua; Wang, Zhaoyan; Sun, Lianhua; Li, Xiaohua; Huang, Qi; Yang, Tao; Wu, Hao

2014-03-01

We sought to characterize the mutation spectrum of NF2 and the differential gene expression in cystic and solid vestibular schwannomas. We collected tumor tissue and blood samples of 31 cystic vestibular schwannomas and 114 solid vestibular schwannomas. Mutation screening of NF2 was performed in both tumor and blood DNA samples of all patients. cDNA microarray was used to analyze the differential gene expression between 11 cystic vestibular schwannomas and 6 solid vestibular schwannomas. Expression levels of top candidate genes were verified by quantitative reverse transcription PCR. NF2 mutations were identified in 34.5% of sporadic vestibular schwannomas, with all mutations being exclusively somatic. No significant difference was found between the mutation detection rates of cystic vestibular schwannoma (35.5%) and solid vestibular schwannoma (34.2%). cDNA microarray analysis detected a total of 46 differentially expressed genes between the cystic vestibular schwannoma and solid vestibular schwannoma samples. The significantly decreased expression of four top candidate genes, C1orf130, CNTF, COL4A3, and COL4A4, was verified by quantitative reverse transcription PCR. NF2 mutations are not directly involved in the cystic formation of vestibular schwannoma. In addition, the differential gene expression of cystic vestibular schwannoma reported in our study may provide useful insights into the molecular mechanism underlying this process.

Revisiting the elemental composition and the calorific value of the organic fraction of municipal solid wastes.

PubMed

Komilis, Dimitrios; Evangelou, Alexandros; Giannakis, Georgios; Lymperis, Constantinos

2012-03-01

In this work, the elemental content (C, N, H, S, O), the organic matter content and the calorific value of various organic components that are commonly found in the municipal solid waste stream were measured. The objective of this work was to develop an empirical equation to describe the calorific value of the organic fraction of municipal solid waste as a function of its elemental composition. The MSW components were grouped into paper wastes, food wastes, yard wastes and plastics. Sample sizes ranged from 0.2 to 0.5 kg. In addition to the above individual components, commingled municipal solid wastes were sampled from a bio-drying facility located in Crete (sample sizes ranged from 8 to 15 kg) and were analyzed for the same parameters. Based on the results of this work, an improved empirical model was developed that revealed that carbon, hydrogen and oxygen were the only statistically significant predictors of calorific value. Total organic carbon was statistically similar to total carbon for most materials in this work. The carbon to organic matter ratio of 26 municipal solid waste substrates and of 18 organic composts varied from 0.40 to 0.99. An approximate chemical empirical formula calculated for the organic fraction of commingled municipal solid wastes was C(32)NH(55)O(16). Copyright © 2011 Elsevier Ltd. All rights reserved.

Systemic Inflammation-Based Biomarkers and Survival in HIV-Positive Subject With Solid Cancer in an Italian Multicenter Study.

PubMed

Raffetti, Elena; Donato, Francesco; Pezzoli, Chiara; Digiambenedetto, Simona; Bandera, Alessandra; Di Pietro, Massimo; Di Filippo, Elisa; Maggiolo, Franco; Sighinolfi, Laura; Fornabaio, Chiara; Castelnuovo, Filippo; Ladisa, Nicoletta; Castelli, Francesco; Quiros Roldan, Eugenia

2015-08-15

Recently, some systemic inflammation-based biomarkers have been demonstrated useful for predicting risk of death in patients with solid cancer independently of tumor characteristics. This study aimed to investigate the prognostic role of systemic inflammation-based biomarkers in HIV-infected patients with solid tumors and to propose a risk score for mortality in these subjects. Clinical and pathological data on solid AIDS-defining cancer (ADC) and non-AIDS-defining cancer (NADC), diagnosed between 1998 and 2012 in an Italian cohort, were analyzed. To evaluate the prognostic role of systemic inflammation- and nutrition-based markers, univariate and multivariable Cox regression models were applied. To compute the risk score equation, the patients were randomly assigned to a derivation and a validation sample. A total of 573 patients (76.3% males) with a mean age of 46.2 years (SD = 10.3) were enrolled. 178 patients died during a median of 3.2 years of follow-up. For solid NADCs, elevated Glasgow Prognostic Score, modified Glasgow Prognostic Score, neutrophil/lymphocyte ratio, platelet/lymphocyte ratio, and Prognostic Nutritional Index were independently associated with risk of death; for solid ADCs, none of these markers was associated with risk of death. For solid NADCs, we computed a mortality risk score on the basis of age at cancer diagnosis, intravenous drug use, and Prognostic Nutritional Index. The areas under the receiver operating characteristic curve were 0.67 (95% confidence interval: 0.58 to 0.75) in the derivation sample and 0.66 (95% confidence interval: 0.54 to 0.79) in the validation sample. Inflammatory biomarkers were associated with risk of death in HIV-infected patients with solid NADCs but not with ADCs.

The effects of solid rocket motor effluents on selected surfaces and solid particle size, distribution, and composition for simulated shuttle booster separation motors

NASA Technical Reports Server (NTRS)

Jex, D. W.; Linton, R. C.; Russell, W. M.; Trenkle, J. J.; Wilkes, D. R.

1976-01-01

A series of three tests was conducted using solid rocket propellants to determine the effects a solid rocket plume would have on thermal protective surfaces (TPS). The surfaces tested were those which are baselined for the shuttle vehicle. The propellants used were to simulate the separation solid rocket motors (SSRM) that separate the solid rocket boosters (SRB) from the shuttle launch vehicle. Data cover: (1) the optical effects of the plume environment on spacecraft related surfaces, and (2) the solid particle size, distribution, and composition at TPS sample locations.

Solid phase extraction of 2,4-D from human urine.

PubMed

Thompson, T S; Treble, R G

1996-10-01

A method for determining urinary concentrations of 2,4-D in samples collected from non-occupationally, environmentally exposed individuals was developed. The 2,4-D was extracted from fortified human urine samples using octadecylsilane solid phase extraction cartridges. The average percent recovery for urine samples spiked at 2 and 20 ng/mL was 100% and 93%, respectively. The method detection limit was estimated to be 0.75 ng of 2,4-D per mL of urine based on a 10 mL sample size. The potential use of 2,4-dichlorophenylacetic acid as a surrogate standard was also investigated.

Quality of water on the Prairie Band Potawatomi Reservation, northeastern Kansas, May 2001 through August 2003

USGS Publications Warehouse

Ross Schmidt, Heather C.

2004-01-01

Water-quality samples were collected from 20 surface-water sites and 11 ground-water sites on the Prairie Band Potawatomi Reservation in northeastern Kansas in an effort to describe existing water-quality conditions on the reservation and to compare water-quality conditions to results from previous reports published as part of a multiyear cooperative study with the Prairie Band Potawatomi Nation. Water is a valuable resource to the Prairie Band Potawatomi Nation as tribal members use the streams draining the reservation, Soldier, Little Soldier, and South Cedar Creeks, to fulfill subsistence hunting and fishing needs and as the tribe develops an economic base on the reservation. Samples were collected once at 20 surface-water monitoring sites during June 2001, and quarterly samples were collected at 5 of the 20 monitoring sites from May 2001 through August 2003. Ground-water-quality samples were collected once from seven wells and twice from four wells during April through May 2003 and in August 2003. Surface-water-quality samples collected from May through August 2001 were analyzed for physical properties, nutrients, pesticides, fecal indicator bacteria, and total suspended solids. In November 2001, an additional analysis for dissolved solids, major ions, trace elements, and suspended-sediment concentration was added for surface-water samples. Ground-water samples were analyzed for physical properties, dissolved solids, major ions, nutrients, trace elements, pesticides, and fecal indicator bacteria. Chemical oxygen demand and volatile organic compounds were analyzed in a sample from one monitoring well located near a construction and demolition landfill on the reservation. Previous reports published as a part of this ongoing study identified total phosphorus, triazine herbicides, and fecal coliform bacteria as exceeding their respective water-quality criteria in surface water on the reservation. Previous ground-water assessments identified occasional sample concentrations of dissolved solids, sodium, sulfate, boron, iron, and manganese as exceeding their respective water-quality criteria. Forty percent of the 65 surface-water samples analyzed for total phosphorus exceeded the aquatic-life goal of 0.1 mg/L (milligrams per liter) established by the U.S. Environmental Protection Agency (USEPA). Concentrations of dissolved solids and sodium occasionally exceeded USEPA Secondary Drinking-Water Regulations and Drinking-Water Advisory Levels, respectively. One of the 20 samples analyzed for atrazine concentrations exceeded the Maximum Contaminant Level (MCL) of 3.0 ?g/L (micrograms per liter) as an annual average established for drinking water by USEPA. A triazine herbicide screen was used on 63 surface-water samples, and triazine compounds were frequently detected. Triazine herbicides and their degradates are listed on the USEPA Contaminant Candidate List. Nitrite plus nitrate concentrations in two ground-water samples from one monitoring well exceeded the MCL of 10 mg/L established by USEPA for drinking water. Arsenic concentrations in two samples from one monitoring well also exceeded the proposed MCL of 10 ?g/L established by the USEPA for drinking water. Concentrations of dissolved solids and sulfate in some ground-water samples exceeded their respective Secondary Drinking-Water Regulations, and concentrations exceeded the taste threshold of the USEPA?s Drinking-Water Advisory Level for sodium. Consequently, in the event that ground water on the reservation is to be used as a drinking-water source, additional treatment may be necessary to remove excess dissolved solids, sulfate, and sodium.

Direct determination of chromium in infant formulas employing high-resolution continuum source electrothermal atomic absorption spectrometry and solid sample analysis.

PubMed

Silva, Arlene S; Brandao, Geovani C; Matos, Geraldo D; Ferreira, Sergio L C

2015-11-01

The present work proposed an analytical method for the direct determination of chromium in infant formulas employing the high-resolution continuum source electrothermal atomic absorption spectrometry combined with the solid sample analysis (SS-HR-CS ET AAS). Sample masses up to 2.0mg were directly weighted on a solid sampling platform and introduced into the graphite tube. In order to minimize the formation of carbonaceous residues and to improve the contact of the modifier solution with the solid sample, a volume of 10 µL of a solution containing 6% (v/v) H2O2, 20% (v/v) ethanol and 1% (v/v) HNO3 was added. The pyrolysis and atomization temperatures established were 1600 and 2400 °C, respectively, using magnesium as chemical modifier. The calibration technique was evaluated by comparing the slopes of calibration curves established using aqueous and solid standards. This test revealed that chromium can be determined employing the external calibration technique using aqueous standards. Under these conditions, the method developed allows the direct determination of chromium with limit of quantification of 11.5 ng g(-1), precision expressed as relative standard deviation (RSD) in the range of 4.0-17.9% (n=3) and a characteristic mass of 1.2 pg of chromium. The accuracy was confirmed by analysis of a certified reference material of tomato leaves furnished by National Institute of Standards and Technology. The method proposed was applied for the determination of chromium in five different infant formula samples. The chromium content found varied in the range of 33.9-58.1 ng g(-1) (n=3). These samples were also analyzed employing ICP-MS. A statistical test demonstrated that there is no significant difference between the results found by two methods. The chromium concentrations achieved are lower than the maximum limit permissible for chromium in foods by Brazilian Legislation. Copyright © 2015. Published by Elsevier B.V.

An efficient method and device for transfer of semisolid materials into solid-state NMR spectroscopy rotors.

PubMed

Hisao, Grant S; Harland, Michael A; Brown, Robert A; Berthold, Deborah A; Wilson, Thomas E; Rienstra, Chad M

2016-04-01

The study of mass-limited biological samples by magic angle spinning (MAS) solid-state NMR spectroscopy critically relies upon the high-yield transfer of material from a biological preparation into the MAS rotor. This issue is particularly important for maintaining biological activity and hydration of semi-solid samples such as membrane proteins in lipid bilayers, pharmaceutical formulations, microcrystalline proteins and protein fibrils. Here we present protocols and designs for rotor-packing devices specifically suited for packing hydrated samples into Pencil-style 1.6 mm, 3.2 mm standard, and 3.2 mm limited speed MAS rotors. The devices are modular and therefore readily adaptable to other rotor and/or ultracentrifugation tube geometries. Copyright © 2016 Elsevier Inc. All rights reserved.

Risk element sorption/desorption characteristics of dry olive residue: a technique for the potential immobilization of risk elements in contaminated soils.

PubMed

Hovorka, Miloš; Száková, Jiřina; García-Sánchez, Mercedes; Acebal, Mercedes Blanc; García-Romera, Inmaculada; Tlustoš, Pavel

2016-11-01

Olive oil production is one of the most relevant agroindustrial activities in the Mediterranean region and generates a huge amount of both solid and semi-solid wastes, the uncontrolled disposal of which might lead to serious environmental problems. Due to its organic matter and mineral nutrient content, the waste material can be applied to agricultural soil as a fertilizer. However, due to its high organic matter content, dry olive residue (DOR), commonly called "alperujo," has the potential to immobilize risk elements in contaminated soils. The main objective of this study was to assess the possible effect of DOR on sorption of risk elements such as cadmium (Cd), lead (Pb), and zinc (Zn) in the soil. A set of batch sorption experiments were carried out to assess the ability of DOR to adsorb Cd, Pb, and Zn where the effect of the preceding biotransformation of DOR by four species of fungi: Penicillium chrysogenum, Coriolopsis floccosa, Bjerkhandera adusta, and Chondrostereum purpureum was compared. The Freundlich and Langmuir sorption isotherms were calculated to assess the sorption characteristics of both transformed and non-transformed DOR. The results showed good potential sorption capacity of DOR, especially for Pb and to a lesser extent for Cd and Zn. Better sorption characteristics were reported for the biotransformed DOR samples, which are expected to show higher humification of the organic matter. However, the desorption experiments showed weakness and instability of the DOR-bound elements, especially in the case of Zn. Thus, future research should aim to verify the DOR sorption pattern in contaminated soil as well as the potential stabilization of the DOR element bounds where the increase of the pH levels of the DOR samples needs to be taken into account.

Recurrent patterns of DNA methylation in the ZNF154, CASP8, and VHL promoters across a wide spectrum of human solid epithelial tumors and cancer cell lines

PubMed Central

Sánchez-Vega, Francisco; Gotea, Valer; Petrykowska, Hanna M; Margolin, Gennady; Krivak, Thomas C; DeLoia, Julie A; Bell, Daphne W; Elnitski, Laura

2013-01-01

The study of aberrant DNA methylation in cancer holds the key to the discovery of novel biological markers for diagnostics and can help to delineate important mechanisms of disease. We have identified 12 loci that are differentially methylated in serous ovarian cancers and endometrioid ovarian and endometrial cancers with respect to normal control samples. The strongest signal showed hypermethylation in tumors at a CpG island within the ZNF154 promoter. We show that hypermethylation of this locus is recurrent across solid human epithelial tumor samples for 15 of 16 distinct cancer types from TCGA. Furthermore, ZNF154 hypermethylation is strikingly present across a diverse panel of ENCODE cell lines, but only in those derived from tumor cells. By extending our analysis from the Illumina 27K Infinium platform to the 450K platform, to sequencing of PCR amplicons from bisulfite treated DNA, we demonstrate that hypermethylation extends across the breadth of the ZNF154 CpG island. We have also identified recurrent hypomethylation in two genomic regions associated with CASP8 and VHL. These three genes exhibit significant negative correlation between methylation and gene expression across many cancer types, as well as patterns of DNaseI hypersensitivity and histone marks that reflect different chromatin accessibility in cancer vs. normal cell lines. Our findings emphasize hypermethylation of ZNF154 as a biological marker of relevance for tumor identification. Epigenetic modifications affecting the promoters of ZNF154, CASP8, and VHL are shared across a vast array of tumor types and may therefore be important for understanding the genomic landscape of cancer. PMID:24149212

Recurrent patterns of DNA methylation in the ZNF154, CASP8, and VHL promoters across a wide spectrum of human solid epithelial tumors and cancer cell lines.

PubMed

Sánchez-Vega, Francisco; Gotea, Valer; Petrykowska, Hanna M; Margolin, Gennady; Krivak, Thomas C; DeLoia, Julie A; Bell, Daphne W; Elnitski, Laura

2013-12-01

The study of aberrant DNA methylation in cancer holds the key to the discovery of novel biological markers for diagnostics and can help to delineate important mechanisms of disease. We have identified 12 loci that are differentially methylated in serous ovarian cancers and endometrioid ovarian and endometrial cancers with respect to normal control samples. The strongest signal showed hypermethylation in tumors at a CpG island within the ZNF154 promoter. We show that hypermethylation of this locus is recurrent across solid human epithelial tumor samples for 15 of 16 distinct cancer types from TCGA. Furthermore, ZNF154 hypermethylation is strikingly present across a diverse panel of ENCODE cell lines, but only in those derived from tumor cells. By extending our analysis from the Illumina 27K Infinium platform to the 450K platform, to sequencing of PCR amplicons from bisulfite treated DNA, we demonstrate that hypermethylation extends across the breadth of the ZNF154 CpG island. We have also identified recurrent hypomethylation in two genomic regions associated with CASP8 and VHL. These three genes exhibit significant negative correlation between methylation and gene expression across many cancer types, as well as patterns of DNaseI hypersensitivity and histone marks that reflect different chromatin accessibility in cancer vs. normal cell lines. Our findings emphasize hypermethylation of ZNF154 as a biological marker of relevance for tumor identification. Epigenetic modifications affecting the promoters of ZNF154, CASP8, and VHL are shared across a vast array of tumor types and may therefore be important for understanding the genomic landscape of cancer.

[Determination of lead in edible salt with solid-phase extraction and GFAAS].

PubMed

Zhao, Xin; Zhou, Shuang; Ma, Lan; Yang, Dajin

2013-01-01

Establishing a method for determination of lead in salt with solid-phase extraction and GFAAS. Salt sample was diluted to a certain volume directly with ammonium acetate, then the sample solution was filtered through the solid phase extraction column which has been pre-activated. Lead ions were retained, and the sodium chloride matrix was removed. After elution, the collected lead ions was determined by graphite furnace atomic absorption spectrometry in 257.4 nm. This method can be used effectively to wipe off the sodium chloride in matrix. The limit of detection was 0.7 microg/kg and the limit of quantification was 2 microg/kg. Solid phase extraction technique can be used effectively to reduce the interference in matrix and improves the accuracy and reproducibility of detection.

Extraction tools for identification of chemical contaminants in estuarine and coastal waters to determine toxic pressure on primary producers.

PubMed

Booij, Petra; Sjollema, Sascha B; Leonards, Pim E G; de Voogt, Pim; Stroomberg, Gerard J; Vethaak, A Dick; Lamoree, Marja H

2013-09-01

The extent to which chemical stressors affect primary producers in estuarine and coastal waters is largely unknown. However, given the large number of legacy pollutants and chemicals of emerging concern present in the environment, this is an important and relevant issue that requires further study. The purpose of our study was to extract and identify compounds which are inhibitors of photosystem II activity in microalgae from estuarine and coastal waters. Field sampling was conducted in the Western Scheldt estuary (Hansweert, The Netherlands). We compared four different commonly used extraction methods: passive sampling with silicone rubber sheets, polar organic integrative samplers (POCIS) and spot water sampling using two different solid phase extraction (SPE) cartridges. Toxic effects of extracts prepared from spot water samples and passive samplers were determined in the Pulse Amplitude Modulation (PAM) fluorometry bioassay. With target chemical analysis using LC-MS and GC-MS, a set of PAHs, PCBs and pesticides was determined in field samples. These compound classes are listed as priority substances for the marine environment by the OSPAR convention. In addition, recovery experiments with both SPE cartridges were performed to evaluate the extraction suitability of these methods. Passive sampling using silicone rubber sheets and POCIS can be applied to determine compounds with different structures and polarities for further identification and determination of toxic pressure on primary producers. The added value of SPE lies in its suitability for quantitative analysis; calibration of passive samplers still needs further investigation for quantification of field concentrations of contaminants. Copyright © 2013 Elsevier Ltd. All rights reserved.

Temporal and spatial variability of chemical and isotopic composition of soil solutions from cambisols - field study and experiments.

PubMed

Schön, Walter; Mittermayr, Florian; Leis, Albrecht; Mischak, Irene; Dietzel, Martin

2016-12-01

The chemical and isotopic composition of soil solutions is highly relevant for environmental and forensic tasks. We investigated interstitial solutions from soil horizons of three cambisols in Styria (Austria). The soils consisted mainly of quartz, feldspar and clay minerals with a vertical variability. Two soil solution fractions from meso-, macro- and micropores (m) and micropores only (μ) were extracted at two subsequent hydraulic pressure steps corresponding to matrix potentials of up to pF 5.43 and from 5.43 to 5.73, respectively. While solute concentrations indicated diverse distribution in soil solution fractions m and μ, heavy stable hydrogen and oxygen isotopes of H 2 O (-92.5‰<δ 2 H<-34.4‰; -11.9‰<δ 18 O<-4.0‰, VSMOW) are clearly enriched in the μ versus m fractions. Principal component analysis on the hydrochemical data set indicates that the intensity of the overall silicate weathering is higher in autumn versus spring, whereas the anthropogenic impact on weathering behaves inversely. The anthropogenic impact is related to seasonal variability of nitrification of N-fertilizers. In consequence of evaluated signals for overall silicate weathering about three-fourths of the soil solutions sampled in autumn indicated elevated total dissolved solid concentration vs. those in spring accompanied with washing out solutes from the soil cover following precipitation events in autumn before sampling. Isotopic shift of soil solutions from the local meteoric water line in spring obviously followed an evaporation trend because of less precipitation and high evaporation before sampling. Experimentally simulated evaporation of soil samples confirmed the observed isotopic evaporation trend. Wetting experiments indicated the infiltration of water within minutes into the micropores of the soils. Exchange of water molecules between micro-, meso- and macropores is an almost instantaneous process and soil solutions in micropores are not as isolated from the soil water system as it was formerly suggested, e.g. for plant uptake. Highly dynamic and complex mechanisms in the gas-water-solid system of soils have to be considered for the application of elemental and isotope proxies related to environmental, forensic and agricultural tasks. Copyright © 2016 Elsevier B.V. All rights reserved.

Improved quantification of livestock associated odorous volatile organic compounds in a standard flow-through system using solid-phase microextraction and gas chromatography-mass spectrometry.

PubMed

Yang, Xiuyan; Zhu, Wenda; Koziel, Jacek A; Cai, Lingshuang; Jenks, William S; Laor, Yael; Leeuwen, J Hans van; Hoff, Steven J

2015-10-02

Aerial emissions of odorous volatile organic compounds (VOCs) are an important nuisance factor from livestock production systems. Reliable air sampling and analysis methods are needed to develop and test odor mitigation technologies. Quantification of VOCs responsible for livestock odor remains an analytical challenge due to physicochemical properties of VOCs and the requirement for low detection thresholds. A new air sampling and analysis method was developed for testing of odor/VOCs mitigation in simulated livestock emissions system. A flow-through standard gas generating system simulating odorous VOCs in livestock barn emissions was built on laboratory scale and tested to continuously generate ten odorous VOCs commonly defining livestock odor. Standard VOCs included sulfur VOCs (S-VOCs), volatile fatty acids (VFAs), and p-cresol. Solid-phase microextraction (SPME) was optimized for sampling of diluted odorous gas mixtures in the moving air followed by gas chromatography-mass spectrometry (GC-MS) analysis. CAR/PDMS 85μm fiber was shown to have the best sensitivity for the target odorous VOCs. A practical 5-min sampling time was selected to ensure optimal extraction of VFAs and p-cresol, as well as minimum displacement of S-VOCs. Method detection limits ranged from 0.39 to 2.64ppbv for S-VOCs, 0.23 to 0.77ppbv for VFAs, and 0.31ppbv for p-cresol. The method developed was applied to quantify VOCs and odorous VOC mitigation with UV light treatment. The measured concentrations ranged from 20.1 to 815ppbv for S-VOCs, 10.3 to 315ppbv for VFAs, and 4.73 to 417ppbv for p-cresol. Relative standard deviations between replicates ranged from 0.67% to 12.9%, 0.50% to 11.4%, 0.83% to 5.14% for S-VOCs, VFAs, and p-cresol, respectively. This research shows that a simple manual SPME sampler could be used successfully for quantification of important classes of odorous VOCs at concentrations relevant for real aerial emissions from livestock operations. Copyright © 2015 Elsevier B.V. All rights reserved.

Comparability of suspended-sediment concentration and total suspended-solids data for two sites on the L'Anguille River, Arkansas, 2001 to 2003

USGS Publications Warehouse

Galloway, Joel M.; Evans, Dennis A.; Green, W. Reed

2005-01-01

Suspended-sediment concentration and total suspended solids data collected with automatic pumping samplers at the L'Anguille River near Colt and the L'Anguille River at Palestine, Arkansas, August 2001 to October 2003 were compared using ordinary least squares regression analyses to determine the relation between the two datasets for each of the two sites. The purpose of this report is to describe the suspended-sediment concentration and total suspended-solids data and examine the comparability of the two datasets for each site. Suspended-sediment concentration and total suspended solids data for the L'Anguille River varied spatially and temporally from August 2001 to October 2003. The site at the L'Anguille River at Palestine represents a larger portion of the L'Anguille River Basin than the site near Colt, and generally had higher median suspended-sediment concentration and total suspended solids and greater ranges in values. The differences between suspended-sediment concentration and total suspended solids data for the L'Anguille River near Colt appeared inversely related to streamflow and not related to time. The relation between suspended-sediment concentration and total suspended solids at the L'Anguille River at Palestine was more variable than at Colt and did not appear to have a relation with flow or time. The relation between suspended-sediment concentration and total suspended solids for the L'Anguille River near Colt shows that total suspended solids increased proportionally as suspended-sediment concentration increased. However, the relation between suspended-sediment concentration and total suspended solids for the L'Anguille River at Palestine showed total suspended solids increased less proportionally as suspended-sediment concentration increased compared to the L'Anguille River near Colt. Differences between the two analytical methods may partially explain differences between the suspended-sediment concentration and total suspended solids data at the two sites. Total suspended solids are analyzed by removing an aliquot of the original sample for further analysis, and suspended-sediment concentrations are analyzed using all sediment and the total mass of the sample. At the L'Anguille River at Palestine another source of variability in the two data sets could have been the location of the automatic pumping sampler intake. The intake was located at a point in the stream cross-section that was subject to sedimentation, which may have resulted in positive sample bias.

Geometric confinement effects on the metal-insulator transition temperature and stress relaxation in VO2 thin films grown on silicon

NASA Astrophysics Data System (ADS)

Viswanath, Changhyun Ko, B.; Yang, Zheng; Ramanathan, Shriram

2011-03-01

VO2 undergoes a sharp metal-insulator transition at ˜67 °C with several orders of change in conductivity and optical transmittance. Understanding and control of the properties of vanadium oxide layers grown on technologically relevant substrates such as Si (100) single crystals is therefore of great interest. In this work, we show tunability of metal-insulator transition temperature as well as recoverable stress in VO2 thin films grown on Si substrate by introducing nanoscale atomic layer deposited HfO2 interfacial layers with no degradation in the resistance ratio. For a confined VO2 film, the metal-insulator transition temperature is suppressed by ˜16 °C and the recoverable stress is 150 MPa, compared to 400 MPa for a bare film. These observations are further correlated with in situ variable temperature measurement of stress changes occurring during the phase transition. Structural and microstructural studies on the various samples have been carried out by x ray diffraction and cross-sectional transmission electron microscopy. The strategy of tuning the metal-insulator transition characteristics by nanoscale interfacial dielectrics is of broader relevance in design of programmable materials and integration into solid state devices for electronics.

Spin-lattice relaxation study of the methyl proton dynamics in solid 9,10-dimethyltriptycene (DMT).

PubMed

Piślewski, N; Tritt-Goc, J; Bielejewski, M; Rachocki, A; Ratajczyk, T; Szymański, S

2009-06-01

Proton spin-lattice relaxation studies are performed for powder samples of 9,10-dimethyltriptycene (DMT) and its isotopomer DMT-d(12) in which all the non-methyl protons in the molecule are replaced by deuterons. The relaxation data are interpreted in terms of the conventional relaxation theory based on the random jump model in which the Pauli correlations between the relevant spin and torsional states are discarded. The Arrhenius activation energies, obtained from the relaxation data, 25.3 and 24.8 kJ mol(-1) for DMT and DMT-d(12), respectively, are very high as for the methyl groups. The validity of the jump model in the present case is considered from the perspective of Haupt theory in which the Pauli principle is explicitly invoked. To this purpose, the dynamic quantities entering the Haupt model are reinterpreted in the spirit of the damped quantum rotation (DQR) approach introduced recently for the purpose of NMR lineshape studies of hindered molecular rotators. Theoretical modelling of the relevant methyl group dynamics, based on the DQR theory, was performed. From these calculations it is inferred that direct assessments of the torsional barrier heights, based on the Arrhenius activation energies extracted from relaxation data, should be treated with caution.

Urokinase-receptor (u-PAR): an essential player in multiple games of cancer: a review on its role in tumor progression, invasion, metastasis, proliferation/dormancy, clinical outcome and minimal residual disease.

PubMed

Laufs, Stephanie; Schumacher, Jens; Allgayer, Heike

2006-08-01

The relevance of the u-PA system in mediating tumor-associated proteolysis, invasion and metastasis, amongst other phenomena associated with tumor progression, has been clearly demonstrated in diverse cancer entities. This review will update on the biological and clinical relevance of the urokinase-receptor (u-PAR). Specifically, the article focuses on the potential importance of u-PAR for the development of minimal residual disease in solid cancer, and in this context reviews the biological relevance of the u-PAR for tumor cell dormancy. Furthermore, transcriptional mechanisms regulating u-PAR in vitro and in vivo, and their potential clinical and therapeutic relevance in gastrointestinal cancers, are elucidated.

Mars Solar Balloon Landed Gas Chromatograph Mass Spectrometer

NASA Technical Reports Server (NTRS)

Mahaffy, P.; Harpold, D.; Niemann, H.; Atreya, S.; Gorevan, S.; Israel, G.; Bertaux, J. L.; Jones, J.; Owen, T.; Raulin, F.

1999-01-01

A Mars surface lander Gas Chromatograph Mass Spectrometer (GCMS) is described to measure the chemical composition of abundant and trace volatile species and isotope ratios for noble gases and other elements. These measurements are relevant to the study of atmospheric evolution and past climatic conditions. A Micromission plan is under study where a surface package including a miniaturized GCMS would be delivered to the surface by a solar heated hot air balloon based system. The balloon system would be deployed about 8 km above the surface of Mars, wherein it would rapidly fill with Martian atmosphere and be heated quickly by the sun. The combined buoyancy and parachuting effects of the solar balloon result in a surface package impact of about 5 m/sec. After delivery of the package to the surface, the balloon would ascend to about 4 km altitude, with imaging and magnetometry data being taken for the remainder of the daylight hours as the balloon is blown with the Martian winds. Total atmospheric entry mass of this mission is estimated to be approximately 50 kg, and it can fit as an Ariane 5 piggyback payload. The GCMS would obtain samples directly from the atmosphere at the surface and also from gases evolved from solid phase material collected from well below the surface with a Sample Acquisition and Transport Mechanism (SATM). The experiment envisioned in the Mars Micromission described would obtain samples from a much greater depth of up to one meter below the surface, and would search for organic molecules trapped in ancient stratified layers well below the oxidized surface. Insitu instruments on upcoming NASA missions working in concert with remote sensing measurement techniques have the potential to provide a more detailed investigation of mineralogy and the extent of simple volatiles such as CO2 and H2O in surface and subsurface solid phase materials. Within the context of subsequent mission opportunities such as those provided by the Ariane 5 piggyback payload based Micromissions, it is essential to implement an even broader chemical analysis and to enable a significant extension of previous isotope measurements. Such a development would enhance the presently very active study of questions of atmospheric evolution and loss and past climatic conditions. The method selected to implement this program can be based on well-established mass spectrometry techniques. Sampled gas is chemically and physically processed to separate the gas mixture into components using gas chromatograph and related enrichment techniques. This allows trace species to be identified and reveals isotopic distributions in many cases with improved precision. Samples of interest, such as organic molecules, may lie deep below the highly oxidized surface layer and the suggested program includes enhanced sampling techniques to measure volatiles preserved in solid phase material deep below the surface as well as gas from the well mixed atmosphere.

Determination of fossil carbon content in Swedish waste fuel by four different methods.

PubMed

Jones, Frida C; Blomqvist, Evalena W; Bisaillon, Mattias; Lindberg, Daniel K; Hupa, Mikko

2013-10-01

This study aimed to determine the content of fossil carbon in waste combusted in Sweden by using four different methods at seven geographically spread combustion plants. In total, the measurement campaign included 42 solid samples, 21 flue gas samples, 3 sorting analyses and 2 investigations using the balance method. The fossil carbon content in the solid samples and in the flue gas samples was determined using (14)C-analysis. From the analyses it was concluded that about a third of the carbon in mixed Swedish waste (municipal solid waste and industrial waste collected at Swedish industry sites) is fossil. The two other methods (the balance method and calculations from sorting analyses), based on assumptions and calculations, gave similar results in the plants in which they were used. Furthermore, the results indicate that the difference between samples containing as much as 80% industrial waste and samples consisting of solely municipal solid waste was not as large as expected. Besides investigating the fossil content of the waste, the project was also established to investigate the usability of various methods. However, it is difficult to directly compare the different methods used in this project because besides the estimation of emitted fossil carbon the methods provide other information, which is valuable to the plant owner. Therefore, the choice of method can also be controlled by factors other than direct determination of the fossil fuel emissions when considering implementation in the combustion plants.

Nickel Nanocatalyst Ex-Solution from Ceria-Nickel Oxide Solid Solution for Low Temperature CO Oxidation.

PubMed

Singhania, Amit; Gupta, Shipra Mital

2018-07-01

In this work, in situ growth of Ni nanocatalysts to attach onto the ceria (CeO2) surface through direct Ni ex-solution from the NiO-CeO2 solid solution in a reducing atmosphere at high temperatures with an aim to improve the catalytic activity, and stability for low temperature carbon monoxide (CO) oxidation reaction have been reported. The NiO-CeO2 solid solutions were prepared by solution combustion method, and the results of XRD and RAMAN showed that doping of Ni increases the oxygen vacancies due to charge compensation. Ni is clearly visible in XRD and TEM of Ni ex-solved sample (R-UCe5Ni10) after reduction of NiO-CeO2 (UCe5Ni10) sample by 5% H2/Ar reduction at 1000 °C. TEM analysis revealed a size of 9.2 nm of Ni nanoparticle that is ex-solved on the surface CeO2. This ex-solved sample showed very high catalytic activity (T50 ~ 110 °C), and stability (100 h) for CO oxidation reaction as compared to prepared solid solution samples. This is due to the highly active metallic nano-phase which is ex-solved on the surface of CeO2 and strongly adherent to the support. The apparent activation energy Ni ex-solved sample is found out to be 48.4 kJ mol-1. Thus, the above Ni ex-solved sample shows a practical applicability for the CO reaction.

Determination of triazine herbicides in seaweeds: development of a sample preparation method based on Matrix Solid Phase Dispersion and Solid Phase Extraction Clean-up.

PubMed

Rodríguez-González, N; González-Castro, M J; Beceiro-González, E; Muniategui-Lorenzo, S; Prada-Rodríguez, D

2014-04-01

A method using dual process columns of Matrix Solid Phase Dispersion (MSPD) and Solid Phase Extraction (SPE) has been developed for extracting and cleaning-up of nine triazine herbicides (ametryn, atrazine, cyanazine, prometryn, propazine, simazine, simetryn, terbuthylazine and terbutryn) in seaweed samples. Under optimized conditions, samples were blended with 2g of octasilyl-derivatized silica (C8) and transferred into an SPE cartridge containing ENVI-Carb II/PSA (0.5/0.5 g) as a clean up co-sorbent. Then the dispersed sample was washed with 10 mL of n-hexane and triazines were eluted with 20 mL ethyl acetate and 5 mL acetonitrile. Finally the extract was concentrated to dryness, re-constituted with 1 mL methanol:water (1:1) and injected into the HPLC-DAD system. The linearity of the calibration curves was excellent in matrix matched standards, and yielded the coefficients of determination>0.995 for all the target analytes. The recoveries ranged from 75% to 100% with relative standard deviations lower than 7%. The achieved LOQs (<10 µg kg(-1)) for all triazines under study permits to ensure proper determination at the maximum allowed residue levels set in the European Union Legislation. Samples of three seaweeds were subjected to the procedure proving the suitability of MSPD method for the analysis of triazines in different seaweeds samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Variables controlling the recovery of ignitable liquid residues from simulated fire debris samples using solid-phase microextraction/gas chromatography

NASA Astrophysics Data System (ADS)

Furton, Kenneth G.; Almirall, Jose R.; Wang, Jing

1999-02-01

In this paper, we present data comparing a variety of different conditions for extracting ignitable liquid residues from simulated fire debris samples in order to optimize the conditions for using Solid Phase Microextraction. A simulated accelerant mixture containing 30 components, including those from light petroleum distillates, medium petroleum distillates and heavy petroleum distillates were used to study the important variables controlling Solid Phase Microextraction (SPME) recoveries. SPME is an inexpensive, rapid and sensitive method for the analysis of volatile residues from the headspace over solid debris samples in a container or directly from aqueous samples followed by GC. The relative effects of controllable variables, including fiber chemistry, adsorption and desorption temperature, extraction time, and desorption time, have been optimized. The addition of water and ethanol to simulated debris samples in a can was shown to increase the sensitivity when using headspace SPME extraction. The relative enhancement of sensitivity has been compared as a function of the hydrocarbon chain length, sample temperature, time, and added ethanol concentrations. The technique has also been optimized to the extraction of accelerants directly from water added to the fire debris samples. The optimum adsorption time for the low molecular weight components was found to be approximately 25 minutes. The high molecular weight components were found at a higher concentration the longer the fiber was exposed to the headspace (up to 1 hr). The higher molecular weight components were also found in higher concentrations in the headspace when water and/or ethanol was added to the debris.

Effect of somatic cell count and mastitis pathogens on milk composition in Gyr cows

PubMed Central

2013-01-01

Background Gyr cows are well adapted to tropical conditions, resistant to some tropical diseases and have satisfactory milk production. However, Gyr dairy herds have a high prevalence of subclinical mastitis, which negatively affects their milk yield and composition. The objectives of this study were (i) to evaluate the effects of seasonality, mammary quarter location (rear x front), mastitis-causing pathogen species, and somatic cell count (SCC) on milk composition in Gyr cows with mammary quarters as the experimental units and (ii) to evaluate the effects of seasonality and somatic cell count (SCC) on milk composition in Gyr cows with cows as the experimental units. A total of 221 lactating Gyr cows from three commercial dairy farms were selected for this study. Individual foremilk quarter samples and composite milk samples were collected once a month over one year from all lactating cows for analysis of SCC, milk composition, and bacteriological culture. Results Subclinical mastitis reduced lactose, nonfat solids and total solids content, but no difference was found in the protein and fat content between infected and uninfected quarters. Seasonality influenced milk composition both in mammary quarters and composite milk samples. Nevertheless, there was no effect of mammary quarter position on milk composition. Mastitis-causing pathogens affected protein, lactose, nonfat solids, and total solids content, but not milk fat content. Somatic cell count levels affected milk composition in both mammary quarters and composite samples of milk. Conclusions Intramammary infections in Gyr cows alter milk composition; however, the degree of change depends on the mastitis-causing pathogen. Somatic cell count is negatively associated with reduced lactose and nonfat solids content in milk. Seasonality significantly affects milk composition, in which the concentration of lactose, fat, protein, nonfat solids and total solids differs between dry and wet seasons in Gyr cows. PMID:23566405

AUTOMATED ANALYSIS OF AQUEOUS SAMPLES CONTAINING PESTICIDES, ACIDIC/BASIC/NEUTRAL SEMIVOLATILES AND VOLATILE ORGANIC COMPOUNDS BY SOLID PHASE EXTRACTION COUPLED IN-LINE TO LARGE VOLUME INJECTION GC/MS

EPA Science Inventory

Data is presented on the development of a new automated system combining solid phase extraction (SPE) with GC/MS spectrometry for the single-run analysis of water samples containing a broad range of organic compounds. The system uses commercially available automated in-line 10-m...

Streamlined sample cleanup using combined dispersive solid-phase extraction and in-vial filtration for analysis of pesticides and environmental pollutants in shrimp

USDA-ARS?s Scientific Manuscript database

A new method of sample preparation was developed and is reported for the first time. The approach combines in-vial filtration with dispersive solid-phase extraction (d-SPE) in a fast and convenient cleanup of QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts. The method was appli...

Comprehensive multiphase NMR spectroscopy: Basic experimental approaches to differentiate phases in heterogeneous samples

NASA Astrophysics Data System (ADS)

Courtier-Murias, Denis; Farooq, Hashim; Masoom, Hussain; Botana, Adolfo; Soong, Ronald; Longstaffe, James G.; Simpson, Myrna J.; Maas, Werner E.; Fey, Michael; Andrew, Brian; Struppe, Jochem; Hutchins, Howard; Krishnamurthy, Sridevi; Kumar, Rajeev; Monette, Martine; Stronks, Henry J.; Hume, Alan; Simpson, André J.

2012-04-01

Heterogeneous samples, such as soils, sediments, plants, tissues, foods and organisms, often contain liquid-, gel- and solid-like phases and it is the synergism between these phases that determine their environmental and biological properties. Studying each phase separately can perturb the sample, removing important structural information such as chemical interactions at the gel-solid interface, kinetics across boundaries and conformation in the natural state. In order to overcome these limitations a Comprehensive Multiphase-Nuclear Magnetic Resonance (CMP-NMR) probe has been developed, and is introduced here, that permits all bonds in all phases to be studied and differentiated in whole unaltered natural samples. The CMP-NMR probe is built with high power circuitry, Magic Angle Spinning (MAS), is fitted with a lock channel, pulse field gradients, and is fully susceptibility matched. Consequently, this novel NMR probe has to cover all HR-MAS aspects without compromising power handling to permit the full range of solution-, gel- and solid-state experiments available today. Using this technology, both structures and interactions can be studied independently in each phase as well as transfer/interactions between phases within a heterogeneous sample. This paper outlines some basic experimental approaches using a model heterogeneous multiphase sample containing liquid-, gel- and solid-like components in water, yielding separate 1H and 13C spectra for the different phases. In addition, 19F performance is also addressed. To illustrate the capability of 19F NMR soil samples, containing two different contaminants, are used, demonstrating a preliminary, but real-world application of this technology. This novel NMR approach possesses a great potential for the in situ study of natural samples in their native state.

Simultaneous determination of the endocrine disrupting compounds nonylphenol, nonylphenol ethoxylates, triclosan and bisphenol A in wastewater and sewage sludge by gas chromatography-mass spectrometry.

PubMed

Gatidou, Georgia; Thomaidis, Nikolaos S; Stasinakis, Athanasios S; Lekkas, Themistokles D

2007-01-05

An integrated analytical method for the simultaneous determination of 4-n-nonylphenol (4-n-NP), nonylphenol monoethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), bisphenol A (BPA) and triclosan (TCS) in wastewater (dissolved and particulate phase) and sewage sludge was developed based on gas chromatography-mass spectrometry. Chromatographic analysis was achieved after derivatization with bis(trimethylsilyl)trifluoroacetamide (BSTFA). Extraction from water samples was performed by solid-phase extraction (SPE). The optimization of SPE procedure included the type of sorbent and the type of the organic solvent used for the elution. Referred to solid samples, the target compounds were extracted by sonication. In this case the optimization of the extraction procedure included the variation of the amount of the extracted biomass, the duration and the temperature of sonication and the type of the extraction organic solvent. The developed extraction procedures resulted in good repeatability and reproducibility with relative standard deviations (RSDs) less than 13% for all the tested compounds for both types of samples. Satisfactory recoveries were obtained (>60%) for all the compounds in both liquid and solid samples, except for 4-n-NP, which gave recoveries up to 35% in wastewater samples and up to 63% in sludge samples. The limits of detection (LODs) of the target compounds varied from 0.03 (4-n-NP) to 0.41 microg l(-1) (NP2EO) and from 0.04 (4-n-NP) to 0.96 microg kg(-1) (NP2EO) for liquid and solid samples, respectively. The developed methods were successfully applied to the analysis of the target compounds in real samples.

Comprehensive multiphase NMR spectroscopy: basic experimental approaches to differentiate phases in heterogeneous samples.

PubMed

Courtier-Murias, Denis; Farooq, Hashim; Masoom, Hussain; Botana, Adolfo; Soong, Ronald; Longstaffe, James G; Simpson, Myrna J; Maas, Werner E; Fey, Michael; Andrew, Brian; Struppe, Jochem; Hutchins, Howard; Krishnamurthy, Sridevi; Kumar, Rajeev; Monette, Martine; Stronks, Henry J; Hume, Alan; Simpson, André J

2012-04-01

Heterogeneous samples, such as soils, sediments, plants, tissues, foods and organisms, often contain liquid-, gel- and solid-like phases and it is the synergism between these phases that determine their environmental and biological properties. Studying each phase separately can perturb the sample, removing important structural information such as chemical interactions at the gel-solid interface, kinetics across boundaries and conformation in the natural state. In order to overcome these limitations a Comprehensive Multiphase-Nuclear Magnetic Resonance (CMP-NMR) probe has been developed, and is introduced here, that permits all bonds in all phases to be studied and differentiated in whole unaltered natural samples. The CMP-NMR probe is built with high power circuitry, Magic Angle Spinning (MAS), is fitted with a lock channel, pulse field gradients, and is fully susceptibility matched. Consequently, this novel NMR probe has to cover all HR-MAS aspects without compromising power handling to permit the full range of solution-, gel- and solid-state experiments available today. Using this technology, both structures and interactions can be studied independently in each phase as well as transfer/interactions between phases within a heterogeneous sample. This paper outlines some basic experimental approaches using a model heterogeneous multiphase sample containing liquid-, gel- and solid-like components in water, yielding separate (1)H and (13)C spectra for the different phases. In addition, (19)F performance is also addressed. To illustrate the capability of (19)F NMR soil samples, containing two different contaminants, are used, demonstrating a preliminary, but real-world application of this technology. This novel NMR approach possesses a great potential for the in situ study of natural samples in their native state. Copyright © 2012 Elsevier Inc. All rights reserved.

Determinations of rare earth element abundance and U-Pb age of zircons using multispot laser ablation-inductively coupled plasma mass spectrometry.

PubMed

Yokoyama, Takaomi D; Suzuki, Toshihiro; Kon, Yoshiaki; Hirata, Takafumi

2011-12-01

We have developed a new calibration technique for multielement determination and U-Pb dating of zircon samples using laser ablation-inductively coupled plasma mass spectrometry (ICPMS) coupled with galvanometric optics. With the galvanometric optics, laser ablation of two or more sample materials could be achieved in very short time intervals (~10 ms). The resulting sample aerosols released from different ablation pits or different solid samples were mixed and homogenized within the sample cell and then transported into the ICP ion source. Multiple spot laser ablation enables spiking of analytes or internal standard elements directly into the solid samples, and therefore the standard addition calibration method can be applied for the determination of trace elements in solid samples. In this study, we have measured the rare earth element (REE) abundances of two zircon samples (Nancy 91500 and Prešovice) based on the standard addition technique, using a direct spiking of analytes through a multispot laser ablation of the glass standard material (NIST SRM612). The resulting REE abundance data show good agreement with previously reported values within analytical uncertainties achieved in this study (10% for most elements). Our experiments demonstrated that nonspectroscopic interferences on 14 REEs could be significantly reduced by the standard addition technique employed here. Another advantage of galvanometric devices is the accumulation of sample aerosol released from multiple spots. In this study we have measured the U-Pb age of a zircon sample (LMR) using an accumulation of sample aerosols released from 10 separate ablation pits of low diameters (~8 μm). The resulting (238)U-(206)Pb age data for the LMR zircons was 369 ± 64 Ma, which is in good agreement with previously reported age data (367.6 ± 1.5 Ma). (1) The data obtained here clearly demonstrate that the multiple spot laser ablation-ICPMS technique can become a powerful approach for elemental and isotopic ratio measurements in solid materials.

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

NASA Astrophysics Data System (ADS)

Krawczyk-Coda, Magdalena

2017-03-01

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

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.

Efficient sample preparation method based on solvent-assisted dispersive solid-phase extraction for the trace detection of butachlor in urine and waste water samples.

PubMed

Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

2016-10-01

In this work, an efficient sample preparation method termed solvent-assisted dispersive solid-phase extraction was applied. The used sample preparation method was based on the dispersion of the sorbent (benzophenone) into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the butachlor, the cloudy solution was centrifuged and butachlor in the sediment phase dissolved in ethanol and determined by gas chromatography with flame ionization detection. Under the optimized conditions (solution pH = 7.0, sorbent: benzophenone, 2%, disperser solvent: ethanol, 500 μL, centrifuged at 4000 rpm for 3 min), the method detection limit for butachlor was 2, 3 and 3 μg/L for distilled water, waste water, and urine sample, respectively. Furthermore, the preconcentration factor was 198.8, 175.0, and 174.2 in distilled water, waste water, and urine sample, respectively. Solvent-assisted dispersive solid-phase extraction was successfully used for the trace monitoring of butachlor in urine and waste water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Application of Acoustic and Optic Methods for Estimating Suspended-Solids Concentrations in the St. Lucie River Estuary, Florida

USGS Publications Warehouse

Patino, Eduardo; Byrne, Michael J.

2004-01-01

Acoustic and optic methods were applied to estimate suspended-solids concentrations in the St. Lucie River Estuary, southeastern Florida. Acoustic Doppler velocity meters were installed at the North Fork, Speedy Point, and Steele Point sites within the estuary. These sites provide varying flow, salinity, water-quality, and channel cross-sectional characteristics. The monitoring site at Steele Point was not used in the analyses because repeated instrument relocations (due to bridge construction) prevented a sufficient number of samples from being collected at the various locations. Acoustic and optic instruments were installed to collect water velocity, acoustic backscatter strength (ABS), and turbidity data that were used to assess the feasibility of estimating suspended-solids concentrations in the estuary. Other data collected at the monitoring sites include tidal stage, salinity, temperature, and periodic discharge measurements. Regression analyses were used to determine the relations of suspended-solids concentration to ABS and suspended-solids concentration to turbidity at the North Fork and Speedy Point sites. For samples used in regression analyses, measured suspended-solids concentrations at the North Fork and Speedy Point sites ranged from 3 to 37 milligrams per liter, and organic content ranged from 50 to 83 percent. Corresponding salinity for these samples ranged from 0.12 to 22.7 parts per thousand, and corresponding temperature ranged from 19.4 to 31.8 ?C. Relations determined using this technique are site specific and only describe suspended-solids concentrations at locations where data were collected. The suspended-solids concentration to ABS relation resulted in correlation coefficients of 0.78 and 0.63 at the North Fork and Speedy Point sites, respectively. The suspended-solids concentration to turbidity relation resulted in correlation coefficients of 0.73 and 0.89 at the North Fork and Speedy Point sites, respectively. The adequacy of the empirical equations seems to be limited by the number and distribution of suspended-solids samples collected throughout the expected concentration range at the North Fork and Speedy Point sites. Additionally, the ABS relations for both sites seem to overestimate at the low end and underestimate at the high end of the concentration range. Based on the sensitivity analysis, temperature had a greater effect than salinity on estimated suspended-solids concentrations. Temperature also appeared to affect ABS data, perhaps by changing the absorptive and reflective characteristics of the suspended material. Salinity and temperature had no observed effects on the turbidity relation at the North Fork and Speedy Point sites. Estimates of suspended-solids concentrations using ABS data were less 'erratic' than estimates using turbidity data. Combining ABS and turbidity data into one equation did not improve the accuracy of results, and therefore, was not considered.

Performance and completion assessment of an in-situ aerated municipal solid waste landfill - Final scientific documentation of an Austrian case study.

PubMed

Hrad, Marlies; Huber-Humer, Marion

2017-05-01

By converting anaerobic landfills into a biologically stabilized state through accelerating aerobic organic matter degradation, the effort and duration necessary for post-closure procedures can be shortened. In Austria, the first full-scale application of in-situ landfill aeration by means of low pressure air injection with simultaneous off-gas collection and treatment was implemented on an old MSW-landfill and operated between 2007 and 2013. Besides complementary laboratory investigations, which included waste sampling from the landfill site prior to aeration start, a comprehensive field monitoring program was conducted to assess the influence of the aeration measure on the emission behavior of the landfilled waste during the aeration period as well as after aeration completion. Although the initial waste material was described as rather stable, the lab-scale aeration tests indicated a significant improvement of the leachate quality and even the biological solid waste stability. However, the aeration success was less pronounced for the application at the landfill site, mainly due to technical limitations in the full-scale operation. In this paper main performance data of the field investigation are compared to four other scientifically documented case studies along with stability indicators for solid waste and leachate characteristics in order to evaluate the success of aeration as well as the progress of a landfill towards completion and end of post-closure care. A number of quantitative benchmarks and relevant context information for the performance assessment of the five hitherto conducted international aeration projects are proposed aiming to support the systematization and harmonization of available results from diverse field studies and full-scale applications in future. Copyright © 2016 Elsevier Ltd. All rights reserved.

Can currently available advanced combustion biomass cook-stoves provide health relevant exposure reductions? Results from initial assessment of select commercial models in India.

PubMed

Sambandam, Sankar; Balakrishnan, Kalpana; Ghosh, Santu; Sadasivam, Arulselvan; Madhav, Satish; Ramasamy, Rengaraj; Samanta, Maitreya; Mukhopadhyay, Krishnendu; Rehman, Hafeez; Ramanathan, Veerabhadran

2015-03-01

Household air pollution from use of solid fuels is a major contributor to the national burden of disease in India. Currently available models of advanced combustion biomass cook-stoves (ACS) report significantly higher efficiencies and lower emissions in the laboratory when compared to traditional cook-stoves, but relatively little is known about household level exposure reductions, achieved under routine conditions of use. We report results from initial field assessments of six commercial ACS models from the states of Tamil Nadu and Uttar Pradesh in India. We monitored 72 households (divided into six arms to each receive an ACS model) for 24-h kitchen area concentrations of PM2.5 and CO before and (1-6 months) after installation of the new stove together with detailed information on fixed and time-varying household characteristics. Detailed surveys collected information on user perceptions regarding acceptability for routine use. While the median percent reductions in 24-h PM2.5 and CO concentrations ranged from 2 to 71% and 10-66%, respectively, concentrations consistently exceeded WHO air quality guideline values across all models raising questions regarding the health relevance of such reductions. Most models were perceived to be sub-optimally designed for routine use often resulting in inappropriate and inadequate levels of use. Household concentration reductions also run the risk of being compromised by high ambient backgrounds from community level solid-fuel use and contributions from surrounding fossil fuel sources. Results indicate that achieving health relevant exposure reductions in solid-fuel using households will require integration of emissions reductions with ease of use and adoption at community scale, in cook-stove technologies. Imminent efforts are also needed to accelerate the progress towards cleaner fuels.

Detection of HLA Antibodies in Organ Transplant Recipients – Triumphs and Challenges of the Solid Phase Bead Assay

PubMed Central

Tait, Brian D.

2016-01-01

This review outlines the development of human leukocyte antigen (HLA) antibody detection assays and their use in organ transplantation in both antibody screening and crossmatching. The development of sensitive solid phase assays such as the enzyme-linked immunosorbent assay technique, and in particular the bead-based technology has revolutionized this field over the last 10–15 years. This revolution however has created a new paradigm in clinical decision making with respect to the detection of low level pretransplant HLA sensitization and its clinical relevance. The relative sensitivities of the assays used are discussed and the relevance of conflicting inter-assay results. Each assay has its advantages and disadvantages and these are discussed. Over the last decade, the bead-based assay utilizing the Luminex® fluorocytometer instrument has become established as the “gold standard” for HLA antibody testing. However, there are still unresolved issues surrounding this technique, such as the presence of denatured HLA molecules on the beads which reveal cryptic epitopes and the issue of appropriate fluorescence cut off values for positivity. The assay has been modified to detect complement binding (CB) in addition to non-complement binding (NCB) HLA antibodies although the clinical relevance of the CB and NCB IgG isotypes is not fully resolved. The increase sensitivity of the Luminex® bead assay over the complement-dependent cytotoxicity crossmatch has permitted the concept of the “virtual crossmatch” whereby the crossmatch is predicted to a high degree of accuracy based on the HLA antibody specificities detected by the solid phase assay. Dialog between clinicians and laboratory staff on an individual patient basis is essential for correct clinical decision making based on HLA antibody results obtained by the various techniques. PMID:28018342

Sample processor for the automatic extraction of families of compounds from liquid samples and/or homogenized solid samples suspended in a liquid

NASA Technical Reports Server (NTRS)

Jahnsen, Vilhelm J. (Inventor); Campen, Jr., Charles F. (Inventor)

1980-01-01

A sample processor and method for the automatic extraction of families of compounds, known as extracts, from liquid and/or homogenized solid samples are disclosed. The sample processor includes a tube support structure which supports a plurality of extraction tubes, each containing a sample from which families of compounds are to be extracted. The support structure is moveable automatically with respect to one or more extraction stations, so that as each tube is at each station a solvent system, consisting of a solvent and reagents, is introduced therein. As a result an extract is automatically extracted from the tube. The sample processor includes an arrangement for directing the different extracts from each tube to different containers, or to direct similar extracts from different tubes to the same utilization device.

Effect of Compression on the Molecular Arrangement of Itraconazole-Soluplus Solid Dispersions: Induction of Liquid Crystals or Exacerbation of Phase Separation?

PubMed

Singh, Abhishek; Bharati, Avanish; Frederiks, Pauline; Verkinderen, Olivier; Goderis, Bart; Cardinaels, Ruth; Moldenaers, Paula; Van Humbeeck, Jan; Van den Mooter, Guy

2016-06-06

Predensification and compression are unit operations imperative to the manufacture of tablets and capsules. Such stress-inducing steps can cause destabilization of solid dispersions which can alter their molecular arrangement and ultimately affect dissolution rate and bioavailability. In this study, itraconazole-Soluplus solid dispersions with 50% (w/w) drug loading prepared by hot-melt extrusion (HME) were investigated. Compression was performed at both pharmaceutically relevant and extreme compression pressures and dwell times. The starting materials, powder, and compressed solid dispersions were analyzed using modulated differential scanning calorimetry (MDSC), X-ray diffraction (XRD), small- and wide-angle X-ray scattering (SWAXS), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), and broadband dielectric spectroscopy (BDS). MDSC analysis revealed that compression promotes phase separation of solid dispersions as indicated by an increase in glass transition width, occurrence of a peak in the nonreversing heat flow signal, and an increase in the net heat of fusion indicating crystallinity in the systems. SWAXS analysis ruled out the presence of mesophases. BDS measurements elucidated an increase in the Soluplus-rich regions of the solid dispersion upon compression. FTIR indicated changes in the spatiotemporal architecture of the solid dispersions mediated via disruption in hydrogen bonding and ultimately altered dynamics. These changes can have significant consequences on the final stability and performance of the solid dispersions.

Discussion of and reply to ``The search for an accurate and practical means for testing residue from combustion of municipal solid waste for percent combustibles and energy content``

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

Eppich, J.D.; Hecklinger, R.S.

1995-11-01

This paper by Roger S. Hecklinger is a good contribution to the understanding of municipal solid waste combustion. The traditional test methods used on residue testing were summarized in a clear manner. Mr. Hecklinger describes sampling problems using coal and coke ash testing methods, which are similar to those experienced in testing the solid waste itself for its fuel content. The author gives several comments regarding the importance of the sampling program. This article also contains the original author`s reply to the comments and questions.

X-ray photoelectron spectroscopy and paramagnetic resonance evidence for shock-induced intramolecular bond breaking in some energetic solids

NASA Astrophysics Data System (ADS)

Owens, F. J.; Sharma, J.

1980-03-01

Solid samples of 1,3,5, trinitro 1,3,5, triazacyclohexane (RDX), trinitrotoluene (TNT), and ammonium nitrate were subjected to shock pulses of strength and duration less than the threshold to cause detonation. The recovered shocked samples were studied by x-ray photoelectron spectroscopy (XPS) and electron paramagnetic resonance (EPR). The results of these measurements indicate that the shock pulse either broke or altered the internal bonds of the molecules of the solid. The results of the shock decomposition are compared with measurements of the uv and slow thermal decomposition of these materials using the same experimental techniques.

First Detection of Non-Chlorinated Organic Molecules Indigenous to a Martian Sample

NASA Technical Reports Server (NTRS)

Freissinet, C.; Glavin, D. P.; Buch, A.; Szopa, C.; Summons, R. E.; Eigenbrode, J. L.; Archer, P. D., Jr.; Brinckerhoff, W. B.; Brunner, A. E.; Cabane, M.;

Assessment of nonpoint source chemical loading potential to watersheds containing uranium waste dumps and human health hazards associated with uranium exploration and mining, Red, White, and Fry Canyons, southeastern Utah, 2007

USGS Publications Warehouse

Beisner, Kimberly R.; Marston, Thomas M.; Naftz, David L.; Snyder, Terry; Freeman, Michael L.

2010-01-01

During May, June, and July 2007, 58 solid-phase samples were collected from abandoned uranium mine waste dumps, background sites, and adjacent streambeds in Red, White, and Fry Canyons in southeastern Utah. The objectives of this sampling program were to (1) assess the nonpoint-source chemical loading potential to ephemeral and perennial drainage basins from uranium waste dumps and (2) assess potential effects on human health due to recreational activities on and around uranium waste dumps on Bureau of Land Management property. Uranium waste-dump samples were collected using solid-phase sampling protocols. After collection, solid-phase samples were homogenized and extracted in the laboratory using a leaching procedure. Filtered (0.45 micron) water samples were obtained from the field leaching procedure and were analyzed for major and trace elements at the Inductively Coupled Plasma-Mass Spectrometry Metals Analysis Laboratory at the University of Utah. A subset of the solid-phase samples also were digested with strong acids and analyzed for major ions and trace elements at the U.S. Geological Survey Geologic Division Laboratory in Denver, Colorado. For the initial ranking of chemical loading potential for uranium waste dumps, results of leachate analyses were compared with existing aquatic-life and drinking-water-quality standards. To assess potential effects on human health, solid-phase digestion values for uranium were compared to soil screening levels (SSL) computed using the computer model RESRAD 6.5 for a probable concentration of radium. One or more chemical constituents exceeded aquatic life and drinking-water-quality standards in approximately 64 percent (29/45) of the leachate samples extracted from uranium waste dumps. Most of the uranium waste dump sites with elevated trace-element concentrations in leachates were located in Red Canyon. Approximately 69 percent (31/45) of the strong acid digestible soil concentration values were greater than a calculated SSL. Uranium waste dump sites with elevated leachate and total digestible concentrations may need to be further investigated to determine the most appropriate remediation method.

The profile of the bending mode band in solid CO2

NASA Astrophysics Data System (ADS)

Baratta, G. A.; Palumbo, M. E.

2017-12-01

Context. Solid carbon dioxide (CO2) is one of the most abundant species detected in icy grain mantles in dense molecular clouds. Its identification is based on the comparison between astronomical and laboratory spectra. In the past 30 yr the profile of solid CO2 infrared absorption bands has been extensively studied experimentally, however, the debate on the structure (amorphous versus crystalline) of CO2 samples obtained in laboratory by the thin-film technique is still open. Aims: The aim of this work is to investigate if the presence of the double peak feature in the profile of the CO2 bending mode band is related to the crystalline or amorphous structure of the sample. Methods: We performed new laboratory experiments depositing CO2 under ultra high vacuum (UHV) conditions at 17 K. We investigated, using infrared transmission spectroscopy, the influence of various experimental parameters on the profile of the CO2 bands, namely deposition rate, sample thickness, annealing, and presence of H2O, CH3OH or CO co-deposited with CO2. Results: We found that, within experimental uncertainties, under UHV conditions the profile of the CO2 bands in pure solid samples does not depend on the deposition rate or the sample thickness in the ranges investigated. In all cases the bending mode band profile shows a double peak (at 660 and 655 cm-1). The spectra also show the Fermi resonance features that cannot be active in crystalline samples. On the other hand, when a small fraction of H2O or CH3OH is co-deposited with CO2 the double peak is not observed while it is observed when a CO2:CO mixture is considered. Furthermore, we measured the density of solid CO2 and the refractive index (at 543.5 nm) at 17 K and at 70 K: ρ(17 K)= 1.17 g cm-3, ρ(70K)= 1.49 g cm-3, n(17K)= 1.285, and n(70K)= 1.372. Conclusions: Our experimental results indicate that the presence of the double peak in the profile of the bending mode band is not an indication of a crystalline structure of the sample and they do not exclude the presence of amorphous solid CO2 in space.

Identification And Characterization Of The Solids Found In Extraction Contactor SEP-401 In June 2012

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

Fondeur, F. F.; Fink, S. D.

2012-12-10

The Modular Caustic-Side Solvent Extraction Unit (MCU) recently conducted an outage that included maintenance on the centrifugal contactors. Operations personnel observed solids or deposits in two contactors and attempted to collect samples for analyses by Savannah River National Laboratory (SRNL). The residues found in Extraction Contactor SEP-401 are a mixture of amorphous silica, aluminosilicate, titanium, and debris from low alloy steel. The solids contain low concentrations of plutonium and strontium. These isotopes are associated with the titanium that came from the monosodium titanate (MST) added in the Actinide Removal Process (ARP) most likely as leached Ti from the MST thatmore » precipitated subsequently in MCU. An attempt was also made to obtain samples from the contents of Wash Contactor SEP-702. However, sampling provide ineffective.« less

Watershed characteristics and water-quality trends and loads in 12 watersheds in Gwinnett County, Georgia

USGS Publications Warehouse

Joiner, John K.; Aulenbach, Brent T.; Landers, Mark N.

2014-01-01

The U.S. Geological Survey, in cooperation with Gwinnett County Department of Water Resources, established a Long-Term Trend Monitoring (LTTM) program in 1996. The LTTM program is a comprehensive, long-term, water-quantity and water-quality monitoring program designed to document and analyze the hydrologic and water-quality conditions of selected watersheds of Gwinnett County, Georgia. Water-quality monitoring initially began in six watersheds and was expanded to another six watersheds in 2001. As part of the LTTM program, streamflow, precipitation, water temperature, specific conductance, and turbidity were measured continuously at the 12 watershed monitoring stations for water years 2004–09. In addition, discrete water-quality samples were collected seasonally from May through October (summer) and November through April (winter), including one base-flow and three stormflow event composite samples, during the study period. Samples were analyzed for nutrients (nitrogen and phosphorus), total organic carbon, trace elements (total lead and total zinc), total dissolved solids, and total suspended sediment (total suspended solids and suspended-sediment concentrations). The sampling scheme was designed to identify variations in water quality both hydrologically and seasonally. The 12 watersheds were characterized for basin slope, population density, land use for 2009, and the percentage of impervious area from 2000 to 2009. Precipitation in water years 2004–09 was about 18 percent below average, and the county experienced exceptional drought conditions and below average runoff in water years 2007 and 2008. Watershed water yields, the percentage of precipitation that results in runoff, typically are lower in low precipitation years and are higher for watersheds with the highest percentages of impervious areas. A comparison of base-flow and stormflow water-quality samples indicates that turbidity and concentrations of total ammonia plus organic nitrogen, total nitrogen, total phosphorus, total organic carbon, total lead, total zinc, total suspended solids, and suspended-sediment concentrations increased with increasing discharge at all watersheds. Specific conductance, however, decreased during stormflow at all watersheds, and total dissolved solids concentrations decreased during stormflow at a few of the watersheds. Total suspended solids and suspended-sediment concentrations typically were two orders of magnitude higher in stormflow samples, turbidities were about 1.5 orders of magnitude higher, total phosphorus and total zinc were about one order of magnitude higher, and total ammonia plus organic nitrogen, total nitrogen, total organic carbon, and total lead were about twofold higher than in base-flow samples. Seasonal patterns and long-term trends in flow-adjusted water-quality concentrations were identified for five representative constituents—total nitrogen, total phosphorus, total zinc, total dissolved solids, and total suspended solids. Seasonal patterns for all five constituents were fairly similar, with higher concentrations in the summer and lower concentrations in the winter. Significant linear long-term trends in stormflow composite concentrations were identified for 36 of the 60 constituent-watershed combinations (5 constituents multiplied by 12 watersheds) for the period of record through water year 2011. Significant trends typically were decreasing for total nitrogen, total phosphorus, total suspended solids, and total zinc and increasing for total dissolved solids. Total dissolved solids and total suspended solids trends had the largest magnitude changes per year. Stream water loads were estimated for 10 water-quality constituents. These estimates represent the cumulative effects of watershed characteristics, hydrologic processes, biogeochemical processes, climatic variability, and human influences on watershed water quality. Yields, in load per unit area, were used to compare loads from watersheds with different sizes. A load estimation approach developed for the Gwinnett County LTTM program that incorporates storm-event composited samples was used with some minor modifications. This approach employs the commonly used regression-model method. Concentrations were modeled as a function of discharge, time, season, and turbidity to improve model predictions and reduce errors in load estimates. Total suspended solids annual loads have been identified in Gwinnett County’s Watershed Protection Plan for target performance criterion. The amount of annual runoff is the primary factor in determining the amount of annual constituent loads. Below average runoff during water years 2004–09, especially during water years 2006–08, resulted in corresponding below average loads. Variations in constituent yields between watersheds appeared to be related to various watershed characteristics. Suspended sediment (total suspended solids and suspended-sediment concentrations) along with constituents transported predominately in solid phase (total phosphorus, total organic carbon, total lead, and total zinc) and total dissolved solids typically had higher yields from watersheds that had high percentages of impervious areas or high basin slope. High total nitrogen yields were also associated with watersheds with high percentages of impervious areas. Low total nitrogen, total suspended solids, total lead, and total zinc yields appear to be associated with watersheds that have a low percentage of high-density development. Total suspended solids yields were lower in drought years, water years 2007–08, from the combined effects of less runoff and the result of fewer, lower magnitude storms, which likely resulted in less surface erosion and lower stream sediment transport.

Waste diminution in Construction projects: Environmental Predicaments

NASA Astrophysics Data System (ADS)

Gharehbaghi, Koorosh; Scott-Young, Christina

2018-03-01

Waste diminution in construction projects is not only a behavioural issue, but also an energy consumption and reduction concern. With construction waste equating to the significant amount of exhausted energy together with increased pollution, this contributes to a series of environmental predicaments. The overall goal of construction solid Waste Management is to collect, treat and dispose of solid wastes generated by project activities in an environmentally and socially satisfactory manner, using the most economical means available. As cities expand, their construction activities and consumption patterns further drive up the solid waste quantities. Governments are usually authorized to have responsibility for providing solid Waste Management services, and various administrative laws give them exclusive ownership over the waste produced. In addition, construction waste processing can be further controlled and minimized according to specialized authorities such as Environmental Protection Agencies (EPA) and their relevant acts and regulations. Moreover, a Construction Environmental Management Plan (CEMP) can further control the treatment of waste and therefore, reduce the amount produced. Key elements of a CEMP not only include complying with relevant legislation, standards and guidance from the EPA; however, also to ensuring that there are systems in place to resolve any potential problems associated with site activities. Accordingly, as a part of energy consumption and lessening strategies, this paper will discuss various effective waste reduction methods for construction projects. Finally, this paper will also examine tactics to further improve energy efficiency through innovative construction Waste Management strategies (including desirability rating of most favourable options) to promote the lessening of overall CO2production.

Arsenic uptake by gypsum and calcite: Modelling and probing by neutron and X-ray scattering

NASA Astrophysics Data System (ADS)

Fernández-Martínez, A.; Román-Ross, G.; Cuello, G. J.; Turrillas, X.; Charlet, L.; Johnson, M. R.; Bardelli, F.

2006-11-01

Uptaking of contaminants by solid phases is relevant to many issues in environmental science as this process can remove them from solutions and retard their transport into the hydrosphere. Here we report on two structural studies performed on As-doped gypsum (CaSO 4 2H 2O) and calcite (CaCO 3), using neutron (D20-ILL) and X-ray (ID11-ESRF) diffraction data and EXAFS (BM8-ESRF). The aim of this study is to determine whether As gets into the bulk of gypsum and calcite structures or is simply adsorbed on the surface. Different mechanisms of substitution are used as hypotheses. The combined Rietveld analysis of neutron and X-ray diffraction data shows an expansion of the unit cell volume proportional to the As concentration within the samples. DFT-based simulations confirm the increase of the unit cell volume proportional to the amount of carbonate or sulphate groups substituted. Interpolation of the experimental Rietveld data allows us to distinguish As substituted within the structure from that adsorbed on the surface of both minerals. Results obtained by EXAFS analysis from calcite samples show good agreement with the hypothesis of replacement of As into the C crystallographic site.

Supercritical fluid chromatography applied to the highly selective isolation of urinary steroid hormones prior to GC/MS analysis.

PubMed

Doué, Mickael; West, Caroline; Bichon, Emmanuelle; Le Bizec, Bruno; Lesellier, Eric

2018-06-01

To assess the presence of prohibited anabolic substances used to promote growth in livestock, calf urine is the most relevant matrix. However, the sample preparation methods (required to remove unwanted matrix components and fractionate isobaric species that may be unresolved by gas chromatography- mass spectrometry GC/MS) are long and complex. In this context, semi-preparative supercritical fluid chromatography (SFC) was considered to possibly simplify the sample preparation in reducing the number of procedures. Fifteen stationary phases were screened with SFC combined with UV and evaporative light-scattering detection (ELSD), among which two columns (Cosmosil π-NAP and Princeton DIOL) were retained for their ability to isolate steroid hormones from other matrix components and, for the second column, for the additional possibility to fractionate steroid hormones into different families (estrogens, mono-hydroxylated and di-hydroxylated androgens). The fractions were further analysed with GC/MS showing the benefit of class fractionation. The final method allows for significant time, solvent and money savings compared to the previously widely used method (solid-phase extraction combined with semi-preparative high-performance liquid chromatography). Copyright © 2018 Elsevier B.V. All rights reserved.

Children's Sleep Comic: development of a new diagnostic tool for children with sleep disorders.

PubMed

Schwerdtle, Barbara; Kanis, Julia; Kahl, Lena; Kübler, Andrea; Schlarb, Angelika A

2012-01-01

A solid diagnosis of sleep disorders in children should include both self-ratings and parent ratings. However, there are few standardized self-assessment instruments to meet this need. The Children's Sleep Comic is an adapted version of the unpublished German questionnaire "Freiburger Kinderschlafcomic" and provides pictures for items and responses. Because the drawings were outdated and allowed only for qualitative analysis, we revised the comic, tested its applicability in a target sample, and suggest a procedure for quantitative analysis. All items were updated and pictures were newly drawn. We used a sample of 201 children aged 5-10 years to test the applicability of the Children's Sleep Comic in young children and to run a preliminary analysis. The Children's Sleep Comic comprises 37 items covering relevant aspects of sleep disorders in children. Application took on average 30 minutes. The procedure was well accepted by the children, as reflected by the absence of any dropouts. First comparisons with established questionnaires indicated moderate correlations. The Children's Sleep Comic is appropriate for screening sleep behavior and sleep problems in children. The interactive procedure can foster a good relationship between the investigator and the child, and thus establish the basis for successful intervention if necessary.

Acoustic Streaming and Heat and Mass Transfer Enhancement

NASA Technical Reports Server (NTRS)

Trinh, E. H.; Gopinath, A.

1996-01-01

A second order effect associated with high intensity sound field, acoustic streaming has been historically investigated to gain a fundamental understanding of its controlling mechanisms and to apply it to practical aspects of heat and mass transfer enhancement. The objectives of this new research project are to utilize a unique experimental technique implementing ultrasonic standing waves in closed cavities to study the details of the generation of the steady-state convective streaming flows and of their interaction with the boundary of ultrasonically levitated near-spherical solid objects. The goals are to further extend the existing theoretical studies of streaming flows and sample interactions to higher streaming Reynolds number values, for larger sample size relative to the wavelength, and for a Prandtl and Nusselt numbers parameter range characteristic of both gaseous and liquid host media. Experimental studies will be conducted in support to the theoretical developments, and the crucial impact of microgravity will be to allow the neglect of natural thermal buoyancy. The direct application to heat and mass transfer in the absence of gravity will be emphasized in order to investigate a space-based experiment, but both existing and novel ground-based scientific and technological relevance will also be pursued.

Manganese ore tailing: optimization of acid leaching conditions and recovery of soluble manganese.

PubMed

Santos, Olívia de Souza Heleno; Carvalho, Cornélio de Freitas; Silva, Gilmare Antônia da; Santos, Cláudio Gouvêa Dos

2015-01-01

Manganese recovery from industrial ore processing waste by means of leaching with sulfuric acid was the objective of this study. Experimental conditions were optimized by multivariate experimental design approaches. In order to study the factors affecting leaching, a screening step was used involving a full factorial design with central point for three variables in two levels (2(3)). The three variables studied were leaching time, concentration of sulfuric acid and sample amount. The three factors screened were shown to be relevant and therefore a Doehlert design was applied to determine the best working conditions for leaching and to build the response surface. By applying the best leaching conditions, the concentrations of 12.80 and 13.64 %w/w of manganese for the global sample and for the fraction -44 + 37 μm, respectively, were found. Microbeads of chitosan were tested for removal of leachate acidity and recovering of soluble manganese. Manganese recovery from the leachate was 95.4%. Upon drying the leachate, a solid containing mostly manganese sulfate was obtained, showing that the proposed optimized method is efficient for manganese recovery from ore tailings. Copyright © 2014 Elsevier Ltd. All rights reserved.

Insights into the discrepant luminescence for BaSiO3 :Eu2+ phosphors prepared by solid-state reaction and precipitation reaction methods.

PubMed

Xu, Jiao; Zhao, Yang; Chen, Jingjing; Mao, Zhiyong; Yang, Yanfang; Wang, Dajian

2017-09-01

Two synthesis routes, solid-state reaction and precipitation reaction, were employed to prepare BaSiO 3 :Eu 2+ phosphors in this study. Discrepancies in the luminescence green emission at 505 nm for the solid-state reaction method sample and in the yellow emission at 570 nm for the sample prepared by the precipitation reaction method, were observed respectively. A detail investigation about the discrepant luminescence of BaSiO 3 :Eu 2+ phosphors was performed by evaluation of X-ray diffraction (XRD), photoluminescence (PL)/photoluminescence excitation (PLE), decay time and thermal quenching properties. The results showed that the yellow emission was generated from the BaSiO 3 :Eu 2+ phosphor, while the green emission was ascribed to a small amount of Ba 2 SiO 4 :Eu 2+ compound that was present in the solid-state reaction sample. This work clarifies the luminescence properties of Eu 2+ ions in BaSiO 3 and Ba 2 SiO 4 hosts. Copyright © 2017 John Wiley & Sons, Ltd.

Solid-substrate fermentation of alfalfa for enhanced protein recovery

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

Bajracharya, R.; Madgett, R.E.

1979-04-01

Solid-substrate fermentations for extraction of protein from pressed alfalfa residues with Aspergillus Sp. QM 9994, Aspergillus niger QM 877, and Rhizopus nigricans QM 387 were conducted in shake flasks. Upon reimbibing and second pressing, total protein recovery from alfalfa was increased from 47.2% for control samples and up to 64.5% for fermented samples. Analysis of juice from fermented samples indicated the presence of cellulase as well as pectinase activities. Dialysis cultures of cellulase-producing fungi showed that total biomass production and solids consumption were much higher than those of a mutant strain lacking the ability to produce cellulase, indicating significant utilizationmore » of cellulosic materials in alfalfa. The biomass yields in the former case ranged from 39-47% based on total solids consumption. Since some of the cellulosic and other carbohydrate constituents in alfalfa may be converted into fungal protein, final alfalfa residues following protein extraction in a commercial process would be less bulky for storage and handling and would be more digestible as a nonruminant animal feed.« less

Split Flow Online Solid-Phase Extraction Coupled with Inductively Coupled Plasma Mass Spectrometry System for One-Shot Data Acquisition of Quantification and Recovery Efficiency.

PubMed

Furukawa, Makoto; Takagai, Yoshitaka

2016-10-04

Online solid-phase extraction (SPE) coupled with inductively coupled plasma mass spectrometry (ICPMS) is a useful tool in automatic sequential analysis. However, it cannot simultaneously quantify the analytical targets and their recovery percentages (R%) in one-shot samples. We propose a system that simultaneously acquires both data in a single sample injection. The main flowline of the online solid-phase extraction is divided into main and split flows. The split flow line (i.e., bypass line), which circumvents the SPE column, was placed on the main flow line. Under program-controlled switching of the automatic valve, the ICPMS sequentially measures the targets in a sample before and after column preconcentration and determines the target concentrations and the R% on the SPE column. This paper describes the system development and two demonstrations to exhibit the analytical significance, i.e., the ultratrace amounts of radioactive strontium ( 90 Sr) using commercial Sr-trap resin and multielement adsorbability on the SPE column. This system is applicable to other flow analyses and detectors in online solid phase extraction.

Molecularly imprinted polymer online solid-phase extraction coupled with high-performance liquid chromatography-UV for the determination of three sulfonamides in pork and chicken.

PubMed

He, Jinxing; Wang, Shuo; Fang, Guozhen; Zhu, Huaping; Zhang, Yan

2008-05-14

A selective imprinted amino-functionalized silica gel sorbent was prepared by combining a surface molecular imprinting technique with a sol-gel process for online solid-phase extraction-HPLC determination of three trace sulfonamides in pork and chicken muscle. The imprinted functionalized silica gel sorbent exhibited selectivity and fast kinetics for the adsorption and desorption of sulfonamides. With a sample loading flow rate of 4 mL min (-1) for 12.5 min, enhancement factors and detection limits for three sulfonamides ( S/ N = 3) were achieved. The precision (RSD) for nine replicate online sorbent extractions of 5 microg L (-1) sulfonamides was less than 4.5%. The sorbent also offered good linearity ( r (2) > 0.99) for online solid-phase extraction of trace levels of sulfonamides. The method was applied to the determination of sulfonamides in pork and chicken muscle samples. The prepared polymer sorbent shows promise for online solid-phase extraction for HPLC determination of trace levels of sulfonamides in pork and chicken samples.

Solid and Gaseous Fuels.

ERIC Educational Resources Information Center

Schultz, Hyman; And Others

1989-01-01

This review covers methods of sampling, analyzing, and testing coal, coke, and coal-derived solids and methods for the chemical, physical, and instrumental analyses of gaseous fuels. The review covers from October 1986, to September 1988. (MVL)

Measuring Sulfur Isotope Ratios from Solid Samples with the Sample Analysis at Mars Instrument and the Effects of Dead Time Corrections

NASA Technical Reports Server (NTRS)

Franz, H. B.; Mahaffy, P. R.; Kasprzak, W.; Lyness, E.; Raaen, E.

2011-01-01

The Sample Analysis at Mars (SAM) instrument suite comprises the largest science payload on the Mars Science Laboratory (MSL) "Curiosity" rover. SAM will perform chemical and isotopic analysis of volatile compounds from atmospheric and solid samples to address questions pertaining to habitability and geochemical processes on Mars. Sulfur is a key element of interest in this regard, as sulfur compounds have been detected on the Martian surface by both in situ and remote sensing techniques. Their chemical and isotopic composition can belp constrain environmental conditions and mechanisms at the time of formation. A previous study examined the capability of the SAM quadrupole mass spectrometer (QMS) to determine sulfur isotope ratios of SO2 gas from a statistical perspective. Here we discuss the development of a method for determining sulfur isotope ratios with the QMS by sampling SO2 generated from heating of solid sulfate samples in SAM's pyrolysis oven. This analysis, which was performed with the SAM breadboard system, also required development of a novel treatment of the QMS dead time to accommodate the characteristics of an aging detector.

Dynamics of Re(2,2'-bipyridine)(CO)3Cl MLCT formation and decay after picosecond pulsed X-ray excitation and femtosecond UV excitation.

PubMed

Zhao, Liyan; Odaka, Hideho; Ono, Hiroshi; Kajimoto, Shinji; Hatanaka, Koji; Hobley, Jonathan; Fukumura, Hiroshi

2005-01-01

The dynamics of Re(2,2'-bipyridine)(CO)3Cl MLCT state formation and decay were determined after femtosecond UV laser excitation and picosecond pulsed X-ray excitation, in an N,N-dimethylformamide (DMF) solution as well as in its solid form. At room temperature, after UV excitation, this MLCT excited state emits both in DMF solution and in the solid form. Transient absorption spectra were measured in solution at various delay times following excitation by a 160 fs, 390 nm laser pulse. There was a prompt absorption increase at around 460 nm occurring within the pump probe convolution (<1 ps), which was assigned to the formation of the 3MLCT state. This transient absorbance was constant over 100 ps. In contrast to the solution state, in the solid state, the emission maximum slightly red-shifts with increasing time after laser excitation. In both solid and solution the emission rises within the system response time. The solid sample exhibited a 1.4 ns emission decay that was not observed for the solution sample. The emission rise from a solid sample after 20 ps pulsed X-ray excitation was significantly slower than the system's time resolution. It is proposed that kinetically energetic electrons are ejected following X-ray induced ionisation, creating ionised tracks in which energetic cations and electrons take time to recombine yielding delayed 3MLCT states that emit.

Role of Dynamically Frustrated Bond Disorder in a Li + Superionic Solid Electrolyte

DOE PAGES

Adelstein, Nicole; Wood, Brandon C.

2016-09-16

Inorganic lithium solid electrolytes are critical components in next-generation solid-state batteries, yet the fundamental nature of the cation-anion interactions and their relevance for ionic conductivity in these materials remains enigmatic. Here, we employ first-principles molecular dynamics simulations to explore the interplay between chemistry, structure, and functionality of a highly conductive Li + solid electrolyte, Li3InBr6. Using local-orbital projections to dynamically track the evolution of the electronic charge density, the simulations reveal rapid, correlated fluctuations between cation-anion interactions with different degrees of directional covalent character. These chemical bond dynamics are shown to correlate with Li + mobility, and are enabled thermallymore » by intrinsic frustration between the preferred geometries of chemical bonding and lattice symmetry. We suggest that the fluctuating chemical environment from the polarizable anions functions similar to a solvent, contributing to the superionic behavior of Li 3InBr 6 by temporarily stabilizing configurations favorable for migrating Li +. The generality of these conclusions for understanding solid electrolytes and key factors governing the superionic phase transition is discussed.« less

Solid Sampling with a Diode Laser for Portable Ambient Mass Spectrometry

PubMed Central

2017-01-01

A hand-held diode laser is implemented for solid sampling in portable ambient mass spectrometry (MS). Specifically, a pseudocontinuous wave battery-powered surgical laser diode is employed for portable laser diode thermal desorption (LDTD) at 940 nm and compared with nanosecond pulsed laser ablation at 2940 nm. Postionization is achieved in both cases using atmospheric pressure photoionization (APPI). The laser ablation atmospheric pressure photoionization (LAAPPI) and LDTD-APPI mass spectra of sage leaves (Salvia officinalis) using a field-deployable quadrupole ion trap MS display many similar ion peaks, as do the mass spectra of membrane grown biofilms of Pseudomonas aeruginosa. These results indicate that LDTD-APPI method should be useful for in-field sampling of plant and microbial communities, for example, by portable ambient MS. The feasibility of many portable MS applications is facilitated by the availability of relatively low cost, portable, battery-powered diode lasers. LDTD could also be coupled with plasma- or electrospray-based ionization for the analysis of a variety of solid samples. PMID:28632988

Solid Sampling with a Diode Laser for Portable Ambient Mass Spectrometry.

PubMed

Yung, Yeni P; Wickramasinghe, Raveendra; Vaikkinen, Anu; Kauppila, Tiina J; Veryovkin, Igor V; Hanley, Luke

2017-07-18

A hand-held diode laser is implemented for solid sampling in portable ambient mass spectrometry (MS). Specifically, a pseudocontinuous wave battery-powered surgical laser diode is employed for portable laser diode thermal desorption (LDTD) at 940 nm and compared with nanosecond pulsed laser ablation at 2940 nm. Postionization is achieved in both cases using atmospheric pressure photoionization (APPI). The laser ablation atmospheric pressure photoionization (LAAPPI) and LDTD-APPI mass spectra of sage leaves (Salvia officinalis) using a field-deployable quadrupole ion trap MS display many similar ion peaks, as do the mass spectra of membrane grown biofilms of Pseudomonas aeruginosa. These results indicate that LDTD-APPI method should be useful for in-field sampling of plant and microbial communities, for example, by portable ambient MS. The feasibility of many portable MS applications is facilitated by the availability of relatively low cost, portable, battery-powered diode lasers. LDTD could also be coupled with plasma- or electrospray-based ionization for the analysis of a variety of solid samples.

Comparison of polycyclic aromatic hydrocarbons level between suspended solid and sediment samples of Pengkalan Chepa River, Kelantan state, Malaysia

NASA Astrophysics Data System (ADS)

Muslim, Noor Zuhartini Md; Babaheidari, Seyedreza Hashemi; Zakaria, Mohamad Pauzi

2015-09-01

Sixteen type of common Polycyclic Aromatic Hydrocarbons (PAHs) which consist of naphthalene, acenaphthene, acenaphthylene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, benzo[ghi]-perylene, indeno[1,2,3-cd]-pyrene and dibenz[a,h]-anthracene in suspended solid and sediment samples of Pengkalan Chepa River, Kelantan state, Malaysia were investigated. The analysis samples were taken from six different sites of Pengkalan Chepa River during sunny day. The samples were subjected to a series of pre-treatment before the level of PAHs can be determined. A Gas Chromatography-Mass Spectrometry (GC-MS) was the prime method for the analysis of PAHs level. A total of 16 PAHs concentration in suspended solid of the whole Pengkalan Chepa River was found to be 2144.6 ng/g dry weights. This concentration was about eight times more than 16 PAHs concentration in sediment which found to be 266.5 ng/g dry weights.

Platform construction and extraction mechanism study of magnetic mixed hemimicelles solid-phase extraction

NASA Astrophysics Data System (ADS)

Xiao, Deli; Zhang, Chan; He, Jia; Zeng, Rong; Chen, Rong; He, Hua

2016-12-01

Simple, accurate and high-throughput pretreatment method would facilitate large-scale studies of trace analysis in complex samples. Magnetic mixed hemimicelles solid-phase extraction has the power to become a key pretreatment method in biological, environmental and clinical research. However, lacking of experimental predictability and unsharpness of extraction mechanism limit the development of this promising method. Herein, this work tries to establish theoretical-based experimental designs for extraction of trace analytes from complex samples using magnetic mixed hemimicelles solid-phase extraction. We selected three categories and six sub-types of compounds for systematic comparative study of extraction mechanism, and comprehensively illustrated the roles of different force (hydrophobic interaction, π-π stacking interactions, hydrogen-bonding interaction, electrostatic interaction) for the first time. What’s more, the application guidelines for supporting materials, surfactants and sample matrix were also summarized. The extraction mechanism and platform established in the study render its future promising for foreseeable and efficient pretreatment under theoretical based experimental design for trace analytes from environmental, biological and clinical samples.

Magnetic dummy molecularly imprinted polymers based on multi-walled carbon nanotubes for rapid selective solid-phase extraction of 4-nonylphenol in aqueous samples.

PubMed

Rao, Wei; Cai, Rong; Yin, Yuli; Long, Fang; Zhang, Zhaohui

2014-10-01

In this paper, a highly selective sample clean-up procedure combining magnetic dummy molecular imprinting with solid-phase extraction was developed for rapid separation and determination of 4-nonylphenol (NP) in the environmental water samples. The magnetic dummy molecularly imprinted polymers (mag-DMIPs) based on multi-walled carbon nanotubes were successfully synthesized with a surface molecular imprinting technique using 4-tert-octylphenol as the dummy template and tetraethylorthosilicate as the cross-linker. The maximum adsorption capacity of the mag-DMIPs for NP was 52.4 mg g(-1) and it took about 20 min to achieve the adsorption equilibrium. The mag-DMIPs exhibited the specific selective adsorption toward NP. Coupled with high performance liquid chromatography analysis, the mag-DMIPs were used to extract solid-phase and detect NP in real water samples successfully with the recoveries of 88.6-98.1%. Copyright © 2014 Elsevier B.V. All rights reserved.

Correcting sensitivity drift during long-term multi-element signal measurements by solid sampling-ETV-ICP-MS.

PubMed

Martin-Esteban, A; Slowikowski, B; Grobecker, K H

2004-06-17

Solid sampling-electrothermal vaporisation-inductively coupled plasma-mass spectrometry (SS-ETV-ICP-MS) is an attractive technique for the direct simultaneous determination of trace elements in solid samples and especially in long-term studies (i.e. assessment of the homogeneity of reference materials). However, during these studies a downward drift in the instrument sensitivity has been observed due likely to deposits on the sampling and skimmer cones and on the ion lens of the mass spectrometer. Accordingly, in this paper, several means of correcting and/or suppressing sensitivity drift are proposed and evaluated for the monitoring of Cd, Cu, Hg, Mn, Pb, Sb, Se, Sn, Tl, U and V in different reference materials of inorganic and organic (biological) origin. From that studies, the combination of the use of the argon dimer as internal standard together with a modification in the ETV-ICP connection tube seems to be the best mean of getting stable sensitivity during at least 60 consecutive ETV runs.

A Synopsis of Technical Issues for Monitoring Sediment in Highway and Urban Runoff

USGS Publications Warehouse

Bent, Gardner C.; Gray, John R.; Smith, Kirk P.; Glysson, G. Douglas

2000-01-01

Accurate and representative sediment data are critical for assessing the potential effects of highway and urban runoff on receiving waters. The U.S. Environmental Protection Agency identified sediment as the most widespread pollutant in the Nation's rivers and streams, affecting aquatic habitat, drinking water treatment processes, and recreational uses of rivers, lakes, and estuaries. Representative sediment data are also necessary for quantifying and interpreting concentrations, loads, and effects of trace elements and organic constituents associated with highway and urban runoff. Many technical issues associated with the collecting, processing, and analyzing of samples must be addressed to produce valid (useful for intended purposes), current, complete, and technically defensible data for local, regional, and national information needs. All aspects of sediment data-collection programs need to be evaluated, and adequate quality-control data must be collected and documented so that the comparability and representativeness of data obtained for highway- and urban-runoff studies may be assessed. Collection of representative samples for the measurement of sediment in highway and urban runoff involves a number of interrelated issues. Temporal and spatial variability in runoff result from a combination of factors, including volume and intensity of precipitation, rate of snowmelt, and features of the drainage basin such as area, slope, infiltration capacity, channel roughness, and storage characteristics. In small drainage basins such as those found in many highway and urban settings, automatic samplers are often the most suitable method for collecting samples of runoff for a variety of reasons. Indirect sediment-measurement methods are also useful as supplementary and(or) surrogate means for monitoring sediment in runoff. All of these methods have limitations in addition to benefits, which must be identified and quantified to produce representative data. Methods for processing raw sediment samples (including homogenization and subsampling) for subsequent analysis for total suspended solids or suspended-sediment concentration often increase variance and may introduce bias. Processing artifacts can be substantial if the methods used are not appropriate for the concentrations and particle-size distributions present in the samples collected. Analytical methods for determining sediment concentrations include the suspended-sediment concentration and the total suspended solids methods. Although the terms suspended-sediment concentration and total suspended solids are often used interchangeably to describe the total concentration of suspended solid-phase material, the analytical methods differ and can produce substantially different results. The total suspended solids method, which commonly is used to produce highway- and urban-runoff sediment data, may not be valid for studies of runoff water quality. Studies of fluvial and highway-runoff sediment data indicate that analyses of samples by the total suspended solids method tends to under represent the true sediment concentration, and that relations between total suspended solids and suspended-sediment concentration are not transferable from site to site even when grain-size distribution information is available. Total suspended solids data used to calculate suspended-sediment loads in highways and urban runoff may be fundamentally unreliable. Consequently, use of total suspended solids data may have adverse consequences for the assessment, design, and maintenance of sediment-removal best management practices. Therefore, it may be necessary to analyze water samples using the suspended-sediment concentration method. Data quality, comparability, and utility are important considerations in collection, processing, and analysis of sediment samples and interpretation of sediment data for highway- and urban-runoff studies. Results from sediment studies must be comparable and readily transf

Rheology and TIC/TOC results of ORNL tank samples

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

Pareizs, J. M.; Hansen, E. K.

2013-04-26

The Savannah River National Laboratory (SRNL)) was requested by Oak Ridge National Laboratory (ORNL) to perform total inorganic carbon (TIC), total organic carbon (TOC), and rheological measurements for several Oak Ridge tank samples. As received slurry samples were diluted and submitted to SRNL-Analytical for TIC and TOC analyses. Settled solids yield stress (also known as settled shear strength) of the as received settled sludge samples were determined using the vane method and these measurements were obtained 24 hours after the samples were allowed to settled undisturbed. Rheological or flow properties (Bingham Plastic viscosity and Bingham Plastic yield stress) were determinedmore » from flow curves of the homogenized or well mixed samples. Other targeted total suspended solids (TSS) concentrations samples were also analyzed for flow properties and these samples were obtained by diluting the as-received sample with de-ionized (DI) water.« less

40 CFR 60.2770 - What information must I include in my annual report?

Code of Federal Regulations, 2014 CFR

2014-07-01

... (CONTINUED) AIR PROGRAMS (CONTINUED) STANDARDS OF PERFORMANCE FOR NEW STATIONARY SOURCES Emissions Guidelines and Compliance Times for Commercial and Industrial Solid Waste Incineration Units Model Rule... calibration drift specification in the applicable performance specification or in the relevant standard. (2...

40 CFR 60.2770 - What information must I include in my annual report?

Code of Federal Regulations, 2013 CFR

2013-07-01

... (CONTINUED) AIR PROGRAMS (CONTINUED) STANDARDS OF PERFORMANCE FOR NEW STATIONARY SOURCES Emissions Guidelines and Compliance Times for Commercial and Industrial Solid Waste Incineration Units Model Rule... calibration drift specification in the applicable performance specification or in the relevant standard. (2...

C sbnd H…F hydrogen bonds as the organising force in F-substituted α-phenyl cinnamic acid aggregates studied by the combination of FTIR spectroscopy and computations

NASA Astrophysics Data System (ADS)

Tolnai, B.; Kiss, J. T.; Felföldi, K.; Pálinkó, I.

2009-04-01

Various F-substituted E-2,3-diphenyl propenoic acid molecules were synthesised and their aggregation behaviour was studied by experimental (FT-IR spectroscopy) and computational (semiempirical and DFT) methods. Experimental approach embraced the identification of potential hydrogen bonding sites through finding the relevant IR bands and monitoring their shifts upon increasing the acid concentration and on going to the solid state. It was found that fluorine engaged in C sbnd H…F hydrogen bonding easily, where the carbon atom could be of any kind available in the molecule (aromatic, aliphatic or olefinic). Shifts were found even in moderately concentrated solutions and in the solid state too. Hydrogen bonding sites could be assigned and relevant aggregate models could be built. Molecular modelling allowed obtaining good estimates for hydrogen bond lengths and angles and visualisation of the geometric arrangements even of extended networks also became feasible.

A target development program for beamhole spallation neutron sources in the megawatt range

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

Bauer, G.S.; Atchison, F.

1995-10-01

Spallation sources as an alternative to fission neutron sources have been operating successfully up to 160 kW of beam power. With the next generation of these facilities aiming at the medium power range between 0.5 and 5 MW, loads on the targets will be high enough to make present experience of little relevance. With the 0.6 MW continuous facility SINQ under construction, and a 5 MW pulsed facility (ESS) under study in Europe, a research and development program is about to be started which aimes at assessing the limits of stationary and moving solid targets and the feasibility and potentialmore » benefits of flowing liquid metal targets. Apart from theoretical work and examination of existing irradiated material, including used targets from ISIS, it is intended to take advantage of the SINQ solid rod target design to improve the relevant data base by building the target in such a way that individual rods can be equipped as irradiation capsules.« less

Bi2MoxW1-xO6 solid solutions with tunable band structure and enhanced visible-light photocatalytic activities

NASA Astrophysics Data System (ADS)

Li, Wenqi; Ding, Xingeng; Wu, Huating; Yang, Hui

2018-07-01

Semiconductor photocatalysis is an effective green way to combat water pollution. For the first time, this study reports a novel method to develop Bi2MoxW1-xO6 solid solution with microsphere structure through anion-exchange method. All Bi2MoxW1-xO6 samples exhibit an Aurivillius-type crystal structure without any secondary phase, confirming that in complete solid solutions as the value of x increases, the band gap energy of Bi2MoxW1-xO6 solid solutions decreases, while the optical absorption edge moves to longer wavelength. The Raman spectra research shows an increase in orthorhombic distortion with progressive replacement of W sites in Bi2WO6 with Mo6+ ions. Compared to Bi2MoO6 and Bi2WO6 samples, Bi2Mo0.4W0.6O6 sample displayed best photocatalytic activity and cycling stability for degradation of RhB dye. The enhanced photocatalytic activity of Bi2Mo0.4W0.6O6 sample can be synergetically linked to hierarchical hollow structure, enhanced light absorbance, and high carrier-separation efficiency. Additionally, the hollow Bi2MoxW1-xO6 microspheres formation can be attributed to the Kirkendall effect.

Application of a thiourea-containing task-specific ionic liquid for the solid-phase extraction cleanup of lead ions from red lipstick, pine leaves, and water samples.

PubMed

Saljooqi, Asma; Shamspur, Tayebeh; Mohamadi, Maryam; Mostafavi, Ali

2014-07-01

Here, task-specific ionic liquid solid-phase extraction is proposed for the first time. In this approach, a thiourea-functionalized ionic liquid is immobilized on the solid sorbent, multiwalled carbon nanotubes. These modified nanotubes packed into a solid-phase extraction column are used for the selective extraction and preconcentration of ultra-trace amounts of lead(II) from aqueous samples prior to electrothermal atomic absorption spectroscopy determination. The thiourea functional groups act as chelating agents for lead ions retaining them and so, give the selectivity to the sorbent. Elution of the retained ions can be performed using an acidic thiourea solution. The effects of experimental parameters including pH of the aqueous solution, type and amount of eluent, and the flow rates of sample and eluent solutions on the separation efficiency are investigated. The linear dependence of absorbance of lead on its concentration in the initial solution is in the range of 0.5-40.0 ng/mL with the detection limit of 0.13 ng/mL (3(Sb)/m, n = 10). The proposed method is applicable to the analysis of red lipstick, pine leaves, and water samples for their lead contents. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid film lubricants and thermal control coatings flown aboard the EOIM-3 MDA sub-experiment

NASA Technical Reports Server (NTRS)

Murphy, Taylor J.; David, Kaia E.; Babel, Hank W.

1995-01-01

Additional experimental data were desired to support the selection of candidate thermal control coatings and solid film lubricants for the McDonnell Douglas Aerospace (MDA) Space Station hardware. The third Evaluation of Oxygen Interactions With Materials Mission (EOIM-3) flight experiment presented an opportunity to study the effects of the low Earth orbit environment on thermal control coatings and solid film lubricants. MDA provided five solid film lubricants and two anodic thermal control coatings for EOIM-3. The lubricant sample set consisted of three solid film lubricants with organic binders one solid film lubricant with an inorganic binder, and one solid film lubricant with no binder. The anodize coating sample set consisted of undyed sulfuric acid anodize and cobalt sulfide dyed sulfuric acid anodize, each on two different substrate aluminum alloys. The organic and inorganic binders in the solid film lubricants experienced erosion, and the lubricating pigments experienced oxidation. MDA is continuing to assess the effect of exposure to the low Earth orbit environment on the life and friction properties of the lubricants. Results to date support the design practice of shielding solid film lubricants from the low Earth orbit environment. Post-flight optical property analysis of the anodized specimens indicated that there were limited contamination effects and some atomic oxygen and ultraviolet radiation effects. These effects appeared to be within the values predicted by simulated ground testing and analysis of these materials, and they were different for each coating and substrate.

A phase I and pharmacokinetic study of the quinoxaline antitumour Agent R(+)XK469 in patients with advanced solid tumours

PubMed Central

Undevia, Samir D.; Innocenti, Federico; Ramirez, Jacqueline; House, Larry; Desai, Apurva A.; Skoog, Linda A.; Singh, Deepti A.; Karrison, Theodore; Kindler, Hedy L.; Ratain, Mark J.

2009-01-01

Purpose To investigate the safety and pharmacokinetics of R(+)XK469, a quinoxaline analogue, in patients with advanced refractory solid tumours. Preclinical studies suggested that efficacy was independent of schedule but that toxicity was decreased by dividing the dose. Methods R(+)XK469 was initially administered as a 30 min intravenous infusion on days 1–5 of a 21-d cycle. Based on the demonstration of a long half-life, the dosing schedule was subsequently amended to infusion on days 1, 3 and 5 of a 21-d cycle. An alternate single-dose schedule of once every 21 d was also explored. Blood samples were collected for pharmaco-kinetic studies. Results Dose-limiting toxicity (DLT) was neutropaenia. There was significant interindividual variability in clearance as evidenced by a coefficient of variation of 46%. A flat-dosing scheme (not based on body surface area) was justified by the absence of correlation between clearance and body surface area. A partial response was observed in a patient with nasopharyngeal carcinoma. Conclusions The recommended phase II doses are 850–1100 mg/d on days 1, 3 and 5 of a 21-d cycle and 2500 mg on day 1 of a 21-d cycle. The observed interpatient pharmacokinetic variability should prompt investigation into the presence of genetic polymorphism in relevant metabolizing enzymes. PMID:18650079

Isolation of clinically relevant fungal species from solid waste and environment of dental health services.

PubMed

Vieira, C D; de Carvalho, M A R; de Resende, M A; de Menezes Cussiol, N A; Alvarez-Leite, M E; dos Santos, S G; de Oliveira, M B; de Magalhães, T F F; Silva, M X; Nicoli, J R; de Macêdo Farias, L

2010-10-01

This study was undertaken to detect, identify and determine antifungal susceptibility of yeast strains isolated from dental solid waste and to evaluate airborne fungi in the Brazilian dental health care environment and in the waste storage room. A group of 17 yeast strains were identified by macroscopic and microscopic characteristics, API 20C Aux system and Multiplex PCR. All 104 airborne fungal colonies were identified by macroscopic and microscopic morphology. The CLSI broth microdilution method was utilized as the susceptibility test. Candida parapsilosis was the prevailing yeast species recovered from waste, followed by Rhodotorula glutinis. Three strains of Candida guilliermondii presented minimal inhibitory concentration values considered to be susceptible dose dependent (2 μg ml(-1)) to voriconazole. Of all airborne fungal species, 69% were recovered from the waste storage room and 31% were recovered from the clinical/surgical environment. Most of them were identified as Cladosporium spp. These findings reinforce the potential risk of waste handling and point out the need for safe management to minimize the spread of these agents to the environment. Filamentous fungi isolation in almost all sampled environments indicates that a periodic monitoring of airborne microbiota in the dental health care service environment is required. The survival of yeast strains for 48 h suggests that dental waste should be carefully controlled and monitored. © 2010 The Authors. Journal compilation © 2010 The Society for Applied Microbiology.

Early Passage Dependence of Mesenchymal Stem Cell Mechanics Influences Cellular Invasion and Migration.

PubMed

Spagnol, Stephen T; Lin, Wei-Chun; Booth, Elizabeth A; Ladoux, Benoit; Lazarus, Hillard M; Dahl, Kris Noel

2016-07-01

The cellular structures and mechanical properties of human mesenchymal stem cells (hMSCs) vary significantly during culture and with differentiation. Previously, studies to measure mechanics have provided divergent results using different quantitative parameters and mechanical models of deformation. Here, we examine hMSCs prepared for clinical use and subject them to mechanical testing conducive to the relevant deformability associated with clinical injection procedures. Micropipette aspiration of hMSCs shows deformation as a viscoelastic fluid, with little variation from cell to cell within a population. After two passages, hMSCs deform as viscoelastic solids. Further, for clinical applicability during stem cell migration in vivo, we investigated the ability of hMSCs to invade into micropillar arrays of increasing confinement from 12 to 8 μm spacing between adjacent micropillars. We find that hMSC samples with reduced deformability and cells that are more solid-like with passage are more easily able to enter the micropillar arrays. Increased cell fluidity is an advantage for injection procedures and optimization of cell selection based on mechanical properties may enhance efficacy of injected hMSC populations. However, the ability to invade and migrate within tight interstitial spaces appears to be increased with a more solidified cytoskeleton, likely from increased force generation and contractility. Thus, there may be a balance between optimal injection survival and in situ tissue invasion.

Simultaneous determination of mushroom toxins α-amanitin, β-amanitin and muscarine in human urine by solid-phase extraction and ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry.

PubMed

Tomková, Jana; Ondra, Peter; Válka, Ivo

2015-06-01

This paper presents a method for the simultaneous determination of α-amanitin, β-amanitin and muscarine in human urine by solid-phase extraction (SPE) and ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry. The method can be used for a diagnostics of mushroom poisonings. Different SPE cartridges were tested for sample preparation, namely hydrophilic modified reversed-phase (Oasis HLB) and polymeric weak cation phase (Strata X-CW). The latter gave better results and therefore it was chosen for the subsequent method optimization and partial validation. In the course of validation, limits of detection, linearity, intraday and interday precisions and recoveries were evaluated. The obtained LOD values of α-amanitin and β-amanitin were 1ng/mL and of muscarine 0.09ng/mL. The intraday and interday precisions of human urine spiked with α-amanitin (10ng/mL), β-amanitin (10ng/mL) and muscarine (1ng/mL) ranged from 6% to 10% and from 7% to 13%, respectively. The developed method was proved to be a relevant tool for the simultaneous determination of the studied mushroom toxins in human urine after mushroom poisoning. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

Monitoring carbonate dissolution using spatially resolved under-sampled NMR propagators and MRI

NASA Astrophysics Data System (ADS)

Sederman, A. J.; Colbourne, A.; Mantle, M. D.; Gladden, L. F.; Oliveira, R.; Bijeljic, B.; Blunt, M. J.

2017-12-01

The dissolution of a porous rock matrix by an acidic flow causes a change in the pore structure and consequently the pattern of fluid flow and rock permeability. This process is relevant to many areas of practical relevance such as enhanced oil recovery, water contaminant migration and sequestration of supercritical CO2. The most important governing factors for the type of change in the pore space are related by the Péclet (Pe) and Damköhler (Da) dimensionless numbers; these compare the transport properties of the fluid in the porous medium with the reactive properties of the solid matrix and the incident fluid respectively. Variation in Pe and Da can cause very different evolution regimes of the pore space and flow can occur, ranging from a uniform dissolution through different "wormholing" regimes (shown on the left hand side of figure 1) to face dissolution. NMR has a unique capability of measuring both the flow and structural changes during such dissolution whilst the characteristics of flow in the highly heterogeneous matrix that is formed can be predicted by the CTRW modelling approach. Here, NMR measurements of displacement probability distributions, or propagators, have been used to monitor the evolution of fluid flow during a reactive dissolution rock core floods. Developments in the NMR method by undersampling the acquisition data enable spatially resolved measurements of the propagators to be done at sufficient displacement resolution and in a timescale that is short enough to capture the changes in structure and flow. The highly under-sampled (4%) data, which typically reduces the acquisition time from 2 hours to 6 minutes, has been shown to produce equivalent propagator results to the fully sampled experiment. Combining these propagator measurements with quantitative and fast imaging techniques a full time-resolved picture of the dissolution reaction is built up. Experiments have been done for both Ketton and Estaillades carbonate rock cores, which exhibit very different dissolution behaviours, and for which experiments and model comparisons will be shown.

Persistence of perfluoroalkyl acid precursors in AFFF-impacted groundwater and soil.

PubMed

Houtz, Erika F; Higgins, Christopher P; Field, Jennifer A; Sedlak, David L

2013-08-06

Several classes of polyfluorinated chemicals that are potential precursors to the perfluorinated carboxylates and sulfonates are present in aqueous film-forming foams (AFFF). To assess the persistence of these AFFF-derived precursors, groundwater, soil, and aquifer solids were obtained in 2011 from an unlined firefighter training area at a U.S. Air Force Base where AFFF was regularly used between 1970 and 1990. To measure the total concentration of perfluorinated carboxylate and sulfonate precursors in archived AFFF formulations and AFFF-impacted environmental samples, a previously developed assay that uses hydroxyl radical to oxidize precursors to perfluorinated carboxylates was adapted for these media. This assay was employed along with direct measurement of 22 precursors found in AFFF and a suite of other poly- and perfluoroalkyl substances (PFASs). On a molar basis, precursors accounted for 41-100% of the total concentration of PFASs in archived AFFF formulations. In the training area, precursors measured by the oxidation assay accounted for an average of 23% and 28% of total PFASs (i.e., precursors and perfluorinated carboxylates and sulfonates) in groundwater and solids samples, respectively. One precursor in AFFF, perfluorohexane sulfonamide amine, was observed on several highly contaminated soil and aquifer solids samples, but no other precursors present in AFFF formulations were detected in any samples at this field site. Suspected intermediate transformation products of precursors in AFFF that were directly measured accounted for approximately half of the total precursor concentration in samples from the training site. The fraction of PFASs consisting of perfluorinated carboxylates and sulfonates was greater in groundwater and solid samples than in any archived AFFF formulations, suggesting that much of the mass of precursors released at the site was converted to perfluorinated carboxylates and sulfonates. The precursors that have persisted at this site may generate significant amounts of additional perfluorinated carboxylates and sulfonates upon remediation of contaminated groundwater or aquifer solids.

The acoustic radiation force on a small thermoviscous or thermoelastic particle suspended in a viscous and heat-conducting fluid

NASA Astrophysics Data System (ADS)

Karlsen, Jonas; Bruus, Henrik

2015-11-01

We present a theoretical analysis (arxiv.org/abs/1507.01043) of the acoustic radiation force on a single small particle, either a thermoviscous fluid droplet or a thermoelastic solid particle, suspended in a viscous and heat-conducting fluid. Our analysis places no restrictions on the viscous and thermal boundary layer thicknesses relative to the particle radius, but it assumes the particle to be small in comparison to the acoustic wavelength. This is the limit relevant to scattering of ultrasound waves from sub-micrometer particles. For particle sizes smaller than the boundary layer widths, our theory leads to profound consequences for the acoustic radiation force. For example, for liquid droplets and solid particles suspended in gasses we predict forces orders of magnitude larger than expected from ideal-fluid theory. Moreover, for certain relevant choices of materials, we find a sign change in the acoustic radiation force on different-sized but otherwise identical particles. These findings lead to the concept of a particle-size-dependent acoustophoretic contrast factor, highly relevant to applications in acoustic levitation or separation of micro-particles in gases, as well as to handling of μm- and nm-sized particles such as bacteria and vira in lab-on-a-chip systems.

Clinical Relevance of Nontuberculous Mycobacteria Isolated from Sputum in a Gold Mining Workforce in South Africa: An Observational, Clinical Study.

PubMed

van Halsema, Clare L; Chihota, Violet N; Gey van Pittius, Nicolaas C; Fielding, Katherine L; Lewis, James J; van Helden, Paul D; Churchyard, Gavin J; Grant, Alison D

2015-01-01

The clinical relevance of nontuberculous mycobacteria (NTM), detected by liquid more than solid culture in sputum specimens from a South African mining workforce, is uncertain. We aimed to describe the current spectrum and relevance of NTM in this population. An observational study including individuals with sputum NTM isolates, recruited at workforce tuberculosis screening and routine clinics. Symptom questionnaires were administered at the time of sputum collection and clinical records and chest radiographs reviewed retrospectively. Of 232 individuals included (228 (98%) male, median age 44 years), M. gordonae (60 individuals), M. kansasii (50), and M. avium complex (MAC: 38) were the commonest species. Of 38 MAC isolates, only 2 (5.3%) were from smear-positive sputum specimens and 30/38 grew in liquid but not solid culture. MAC was especially prevalent among symptomatic, HIV-positive individuals. HIV prevalence was high: 57/74 (77%) among those tested. No differences were found in probability of death or medical separation by NTM species. M. gordonae, M. kansasii, and MAC were the commonest NTM among miners with suspected tuberculosis, with most MAC from smear-negative specimens in liquid culture only. HIV testing and identification of key pathogenic NTM in this setting are essential to ensure optimal treatment.

Clinical Relevance of Nontuberculous Mycobacteria Isolated from Sputum in a Gold Mining Workforce in South Africa: An Observational, Clinical Study

PubMed Central

van Halsema, Clare L.; Chihota, Violet N.; Gey van Pittius, Nicolaas C.; Fielding, Katherine L.; Lewis, James J.; van Helden, Paul D.; Churchyard, Gavin J.; Grant, Alison D.

2015-01-01

Background. The clinical relevance of nontuberculous mycobacteria (NTM), detected by liquid more than solid culture in sputum specimens from a South African mining workforce, is uncertain. We aimed to describe the current spectrum and relevance of NTM in this population. Methods. An observational study including individuals with sputum NTM isolates, recruited at workforce tuberculosis screening and routine clinics. Symptom questionnaires were administered at the time of sputum collection and clinical records and chest radiographs reviewed retrospectively. Results. Of 232 individuals included (228 (98%) male, median age 44 years), M. gordonae (60 individuals), M. kansasii (50), and M. avium complex (MAC: 38) were the commonest species. Of 38 MAC isolates, only 2 (5.3%) were from smear-positive sputum specimens and 30/38 grew in liquid but not solid culture. MAC was especially prevalent among symptomatic, HIV-positive individuals. HIV prevalence was high: 57/74 (77%) among those tested. No differences were found in probability of death or medical separation by NTM species. Conclusions. M. gordonae, M. kansasii, and MAC were the commonest NTM among miners with suspected tuberculosis, with most MAC from smear-negative specimens in liquid culture only. HIV testing and identification of key pathogenic NTM in this setting are essential to ensure optimal treatment. PMID:26180817

HPLC-MS/MS methods for the determination of 52 perfluoroalkyl and polyfluoroalkyl substances in aqueous samples.

PubMed

Gremmel, Christoph; Frömel, Tobias; Knepper, Thomas P

2017-02-01

Two quantitative methods using high-performance liquid chromatography (HPLC) combined with triple quadrupole tandem mass spectrometry (MS/MS) were developed to determine perfluoroalkyl and polyfluoroalkyl substances (PFASs) in aqueous samples. The first HPLC-MS/MS method was applied to 47 PFASs of 12 different substance classes with acidic characteristics such as perfluoroalkyl carboxylic acids (PFCAs) and perfluoroalkane sulfonic acids (PFSAs), as well as precursor substances and biotransformation intermediates (e.g., unsaturated fluorotelomer carboxylic acids). In addition, 25 13 C-, 18 O-, and 2 H-labeled PFASs were used as internal standards in this method. The second HPLC-MS/MS method was applied to fluorotelomer alcohols (FTOHs) and perfluorooctane sulfonamidoethanols as these compounds have physicochemical properties different from those of the previous ones. Accuracy between 82% and 110% and a standard deviation in the range from 2% to 22% depending on the substances were determined during the evaluation of repeatability and precision. The method quantification limit after solid-phase extraction ranged from 0.3 to 199 ng/L depending on the analyte and matrix. The HPLC-MS/MS methods developed were suitable for the determination of PFASs in aqueous samples (e.g., wastewater treatment plant effluents or influents after solid-phase extraction). These methods will be helpful in monitoring campaigns to evaluate the relevance of precursor substances as indirect sources of perfluorinated substances in the environment. In one exemplary application in an industrial wastewater treatment plant, FTOHs were found to be the major substance class in the influent; in particular, 6:2-FTOH was the predominant compound in the industrial samples and accounted for 74% of the total PFAS concentration. The increase in the concentration of the transformation products of FTOHs in the corresponding effluent, such as fluorotelomer carboxylic acids, unsaturated fluorotelomer carboxylic acids, n:3 polyfluorinated saturated carboxylic acids (n indicates the number of nonfluorinated carbon atoms), and PFCAs, indicated biotransformation of FTOHs or their derivatives during wastewater treatment. However, only 33 mol% of the total amount of PFASs present in the influent was quantified in the corresponding effluent. Graphical abstract Method development of an HPLC-MS/MS multi-method for the determination of PFASs in aqueos samples.

Design and optimization of reverse-transcription quantitative PCR experiments.

PubMed

Tichopad, Ales; Kitchen, Rob; Riedmaier, Irmgard; Becker, Christiane; Ståhlberg, Anders; Kubista, Mikael

2009-10-01

Quantitative PCR (qPCR) is a valuable technique for accurately and reliably profiling and quantifying gene expression. Typically, samples obtained from the organism of study have to be processed via several preparative steps before qPCR. We estimated the errors of sample withdrawal and extraction, reverse transcription (RT), and qPCR that are introduced into measurements of mRNA concentrations. We performed hierarchically arranged experiments with 3 animals, 3 samples, 3 RT reactions, and 3 qPCRs and quantified the expression of several genes in solid tissue, blood, cell culture, and single cells. A nested ANOVA design was used to model the experiments, and relative and absolute errors were calculated with this model for each processing level in the hierarchical design. We found that intersubject differences became easily confounded by sample heterogeneity for single cells and solid tissue. In cell cultures and blood, the noise from the RT and qPCR steps contributed substantially to the overall error because the sampling noise was less pronounced. We recommend the use of sample replicates preferentially to any other replicates when working with solid tissue, cell cultures, and single cells, and we recommend the use of RT replicates when working with blood. We show how an optimal sampling plan can be calculated for a limited budget. .

Application of binomial-edited CPMG to shale characterization

USGS Publications Warehouse

Washburn, Kathryn E.; Birdwell, Justin E.

2014-01-01

Unconventional shale resources may contain a significant amount of hydrogen in organic solids such as kerogen, but it is not possible to directly detect these solids with many NMR systems. Binomial-edited pulse sequences capitalize on magnetization transfer between solids, semi-solids, and liquids to provide an indirect method of detecting solid organic materials in shales. When the organic solids can be directly measured, binomial-editing helps distinguish between different phases. We applied a binomial-edited CPMG pulse sequence to a range of natural and experimentally-altered shale samples. The most substantial signal loss is seen in shales rich in organic solids while fluids associated with inorganic pores seem essentially unaffected. This suggests that binomial-editing is a potential method for determining fluid locations, solid organic content, and kerogen–bitumen discrimination.

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

Faria, Bruna Fernanda de; Moreira, Silvana

The problem of solid waste in most countries is on the rise as a result of rapid population growth, urbanization, industrial development and changes in consumption habits. Amongst the various forms of waste disposals, landfills are today the most viable for the Brazilian reality, both technically and economically. Proper landfill construction practices allow minimizing the effects of the two main sources of pollution from solid waste: landfill gas and slurry. However, minimizing is not synonymous with eliminating; consequently, the landfill alone cannot resolve all the problems with solid waste disposal. The main goal of this work is to evaluate themore » content of trace elements in samples of groundwater, surface water and slurry arising from local solid waste disposals in the city of Campinas, SP, Brazil. Samples were collected at the Delta, Santa Barbara and Pirelli landfills. At the Delta and Santa Barbara sites, values above the maximum permitted level established by CETESB for Cr, Mn, Fe, Ni and Pb were observed in samples of groundwater, while at the Pirelli site, elements with concentrations above the permitted levels were Mn, Fe, Ba and Pb. At Delta, values above levels permitted by the CONAMA 357 legislation were still observed in surface water samples for Cr, Mn, Fe and Cu, whereas in slurry samples, values above the permitted levels were observed for Cr, Mn, Fe, Ni, Cu, Zn and Pb. Slurry samples were prepared in accordance with two extraction methodologies, EPA 3050B and EPA 200.8. Concentrations of Cr, Ni, Cu and Pb were higher than the limit established by CONAMA 357 for most samples collected at different periods (dry and rainy) and also for the two extraction methodologies employed.« less

Understanding Cryptic Pocket Formation in Protein Targets by Enhanced Sampling Simulations.

PubMed

Oleinikovas, Vladimiras; Saladino, Giorgio; Cossins, Benjamin P; Gervasio, Francesco L

2016-11-02

Cryptic pockets, that is, sites on protein targets that only become apparent when drugs bind, provide a promising alternative to classical binding sites for drug development. Here, we investigate the nature and dynamical properties of cryptic sites in four pharmacologically relevant targets, while comparing the efficacy of various simulation-based approaches in discovering them. We find that the studied cryptic sites do not correspond to local minima in the computed conformational free energy landscape of the unliganded proteins. They thus promptly close in all of the molecular dynamics simulations performed, irrespective of the force-field used. Temperature-based enhanced sampling approaches, such as Parallel Tempering, do not improve the situation, as the entropic term does not help in the opening of the sites. The use of fragment probes helps, as in long simulations occasionally it leads to the opening and binding to the cryptic sites. Our observed mechanism of cryptic site formation is suggestive of an interplay between two classical mechanisms: induced-fit and conformational selection. Employing this insight, we developed a novel Hamiltonian Replica Exchange-based method "SWISH" (Sampling Water Interfaces through Scaled Hamiltonians), which combined with probes resulted in a promising general approach for cryptic site discovery. We also addressed the issue of "false-positives" and propose a simple approach to distinguish them from druggable cryptic pockets. Our simulations, whose cumulative sampling time was more than 200 μs, help in clarifying the molecular mechanism of pocket formation, providing a solid basis for the choice of an efficient computational method.

Elastic moduli in nano-size samples of amorphous solids: System size dependence

NASA Astrophysics Data System (ADS)

Cohen, Yossi; Procaccia, Itamar

2012-08-01

This letter is motivated by some recent experiments on pan-cake-shaped nano-samples of metallic glass that indicate a decline in the measured shear modulus upon decreasing the sample radius. Similar measurements on crystalline samples of the same dimensions showed a much more modest change. In this letter we offer a theory of this phenomenon; we argue that such results are generically expected for any amorphous solid, with the main effect being related to the increased contribution of surfaces with respect to the bulk when the samples get smaller. We employ exact relations between the shear modulus and the eigenvalues of the system's Hessian matrix to explore the role of surface modes in affecting the elastic moduli.

Pesticide-sampling equipment, sample-collection and processing procedures, and water-quality data at Chicod Creek, North Carolina, 1992

USGS Publications Warehouse

Manning, T.K.; Smith, K.E.; Wood, C.D.; Williams, J.B.

1994-01-01

Water-quality samples were collected from Chicod Creek in the Coastal Plain Province of North Carolina during the summer of 1992 as part of the U.S. Geological Survey's National Water-Quality Assessment Program. Chicod Creek is in the Albemarle-Pamlico drainage area, one of four study units designated to test equipment and procedures for collecting and processing samples for the solid-phase extraction of selected pesticides, The equipment and procedures were used to isolate 47 pesticides, including organonitrogen, carbamate, organochlorine, organophosphate, and other compounds, targeted to be analyzed by gas chromatography/mass spectrometry. Sample-collection and processing equipment equipment cleaning and set-up procedures, methods pertaining to collecting, splitting, and solid-phase extraction of samples, and water-quality data resulting from the field test are presented in this report Most problems encountered during this intensive sampling exercise were operational difficulties relating to equipment used to process samples.

Exploration of the Habitability of Mars with the SAM Suite Investigation on the 2009 Mars Science Laboratory

NASA Technical Reports Server (NTRS)

Mahaffy, P. R.; Cabane, M.; Webster, C. R.

2008-01-01

The 2009 Mars Science Laboratory (MSL) with a substantially larger payload capability that any other Mars rover, to date, is designed to quantitatively assess a local region on Mars as a potential habitat for present or past life. Its goals are (1) to assess past or present biological potential of a target environment, (2) to characterize geology and geochemistry at the MSL landing site, and (3) to investigate planetary processes that influence habitability. The Sample Analysis at Mars (SAM) Suite, in its final stages of integration and test, enables a sensitive search for organic molecules and chemical and isotopic analysis of martian volatiles. MSL contact and remote surface and subsurface survey Instruments establish context for these measurements and facilitate sample identification and selection. The SAM instruments are a gas chromatograph (GC), a mass spectrometer (MS), and a tunable laser spectrometer (TLS). These together with supporting sample manipulation and gas processing devices are designed to analyze either the atmospheric composition or gases extracted from solid phase samples such as rocks and fines. For example, one of the core SAM experiment sequences heats a small powdered sample of a Mars rock or soil from ambient to -1300 K in a controlled manner while continuously monitoring evolved gases. This is followed by GCMS analysis of released organics. The general chemical survey is complemented by a specific search for molecular classes that may be relevant to life including atmospheric methane and its carbon isotope with the TLS and biomarkers with the GCMS.

Electrical field-induced extraction and separation techniques: promising trends in analytical chemistry--a review.

PubMed

Yamini, Yadollah; Seidi, Shahram; Rezazadeh, Maryam

2014-03-03

Sample preparation is an important issue in analytical chemistry, and is often a bottleneck in chemical analysis. So, the major incentive for the recent research has been to attain faster, simpler, less expensive, and more environmentally friendly sample preparation methods. The use of auxiliary energies, such as heat, ultrasound, and microwave, is one of the strategies that have been employed in sample preparation to reach the above purposes. Application of electrical driving force is the current state-of-the-art, which presents new possibilities for simplifying and shortening the sample preparation process as well as enhancing its selectivity. The electrical driving force has scarcely been utilized in comparison with other auxiliary energies. In this review, the different roles of electrical driving force (as a powerful auxiliary energy) in various extraction techniques, including liquid-, solid-, and membrane-based methods, have been taken into consideration. Also, the references have been made available, relevant to the developments in separation techniques and Lab-on-a-Chip (LOC) systems. All aspects of electrical driving force in extraction and separation methods are too specific to be treated in this contribution. However, the main aim of this review is to provide a brief knowledge about the different fields of analytical chemistry, with an emphasis on the latest efforts put into the electrically assisted membrane-based sample preparation systems. The advantages and disadvantages of these approaches as well as the new achievements in these areas have been discussed, which might be helpful for further progress in the future. Copyright © 2013 Elsevier B.V. All rights reserved.

A Device for Comparing Callus Growth Rates in Vitro

PubMed Central

Krul, William R.; Combs, Michael

1975-01-01

A device to compare the kinetics of callus growth in vitro is described. Changes in volumes of callus grown in scintillation vials were monitored photometrically without removing the sample from the solid support and medium. It is shown that a fiberglass-paper solid support is superior to a plastic foam solid support for the growth of American chestnut callus. PMID:16659126

Determination of Total Solids and Ash in Algal Biomass: Laboratory Analytical Procedure (LAP)

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

Van Wychen, Stefanie; Laurens, Lieve M. L.

2016-01-13

This procedure describes the methods used to determine the amount of moisture or total solids present in a freeze-dried algal biomass sample, as well as the ash content. A traditional convection oven drying procedure is covered for total solids content, and a dry oxidation method at 575 deg. C is covered for ash content.

Stability of Molecules of Biological Importance to Ionizing Radiation: Relevance in Astrobiology

NASA Astrophysics Data System (ADS)

Meléndez-López, A. L.; Negrón-Mendoza, A.; Ramos-Bernal, S.; Colín-García, M.; Heredia, A.

2017-11-01

Our aim is to study the stability of amino acids in conditions that probably existed in the primitive environments. We study aspartic acid and glutamic acid, in solid state and aqueous solution, against high doses of gamma radiation at 298 and 77 K.

Product formulation for ohmic heating: blanching as a pretreatment method to improve uniformity in heating of solid-liquid food mixtures.

PubMed

Sarang, S; Sastry, S K; Gaines, J; Yang, T C S; Dunne, P

2007-06-01

The electrical conductivity of food components is critical to ohmic heating. Food components of different electrical conductivities heat at different rates. While equal electrical conductivities of all phases are desirable, real food products may behave differently. In the present study involving chicken chow mein consisting of a sauce and different solid components, celery, water chestnuts, mushrooms, bean sprouts, and chicken, it was observed that the sauce was more conductive than all solid components over the measured temperature range. To improve heating uniformity, a blanching method was developed to increase the ionic content of the solid components. By blanching different solid components in a highly conductive sauce at 100 degrees C for different lengths of time, it was possible to adjust their conductivity to that of the sauce. Chicken chow mein samples containing blanched particulates were compared with untreated samples with respect to ohmic heating uniformity at 60 Hz up to 140 degrees C. All components of the treated product containing blanched solids heated more uniformly than untreated product. In sensory tests, 3 different formulations of the blanched product showed good quality attributes and overall acceptability, demonstrating the practical feasibility of the blanching protocol.

Disappearing Polymorphs Revisited

PubMed Central

Bučar, Dejan-Krešimir; Lancaster, Robert W; Bernstein, Joel

2015-01-01

Nearly twenty years ago, Dunitz and Bernstein described a selection of intriguing cases of polymorphs that disappear. The inability to obtain a crystal form that has previously been prepared is indeed a frustrating and potentially serious problem for solid-state scientists. This Review discusses recent occurrences and examples of disappearing polymorphs (as well as the emergence of elusive crystal forms) to demonstrate the enduring relevance of this troublesome, but always captivating, phenomenon in solid-state research. A number of these instances have been central issues in patent litigations. This Review, therefore, also highlights the complex relationship between crystal chemistry and the law. PMID:26031248

Solid Lubrication Fundamentals and Applications. Chapter 2

NASA Technical Reports Server (NTRS)

Miyoshi, Kazuhisa

1998-01-01

This chapter describes powerful analytical techniques capable of sampling tribological surfaces and solid-film lubricants. Some of these techniques may also be used to determine the locus of failure in a bonded structure or coated substrate; such information is important when seeking improved adhesion between a solid-film lubricant and a substrate and when seeking improved performance and long life expectancy of solid lubricants. Many examples are given here and through-out the book on the nature and character of solid surfaces and their significance in lubrication, friction, and wear. The analytical techniques used include the late spectroscopic methods.

Rapid wide-scope screening of drugs of abuse, prescription drugs with potential for abuse and their metabolites in influent and effluent urban wastewater by ultrahigh pressure liquid chromatography-quadrupole-time-of-flight-mass spectrometry.

PubMed

Hernández, Félix; Bijlsma, Lubertus; Sancho, Juan V; Díaz, Ramon; Ibáñez, María

2011-01-17

This work illustrates the potential of hybrid quadrupole-time-of-flight mass spectrometry (QTOF MS) coupled to ultrahigh pressure liquid chromatography (UHPLC) to investigate the presence of drugs of abuse in wastewater. After solid-phase extraction with Oasis MCX cartridges, seventy-six illicit drugs, prescription drugs with potential for abuse, and metabolites were investigated in the samples by TOF MS using electrospray interface under positive ionization mode, with MS data acquired over an m/z range of 50-1000Da. For 11 compounds, reference standards were available, and experimental data (e.g., retention time and fragmentation data) could be obtained, facilitating a more confident identification. The use of a QTOF instrument enabled the simultaneous application of two acquisition functions with different collision energies: a low energy (LE) function, where none or poor fragmentation took place, and a high energy (HE) function, where fragmentation in the collision cell was promoted. This approach, known as MS(E), enabled the simultaneous acquisition of full-spectrum accurate mass data of both protonated molecules and fragment ions in a single injection, providing relevant information that facilitates the rapid detection and reliable identification of these emerging contaminants in the sample matrices analyzed. In addition, isomeric compounds, like the opiates, morphine and norcodeine, could be discriminated by their specific fragments observed in HE TOF MS spectra, without the need of reference standards. UHPLC-QTOF MS was proven to be a powerful and efficient technique for rapid wide-scope screening and identification of many relevant drugs in complex matrices, such as influent and effluent urban wastewater. Copyright © 2010 Elsevier B.V. All rights reserved.

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

Bass, Jay D.

This project is aimed at experimental characterization of the sound velocities, equations of state (EOS), and derived physical and chemical properties of aqueous solutions and carbon dioxide at extreme pressure and temperature conditions relevant to processes occurring in the interior of the Earth. Chemical transport, phase changes (including melting), fluid-solid reactions, and formation of magmatic liquids at convergent plat boundaries are a key motivation for this project. Research in this area has long been limited by the extreme experimental challenges and lack of data under the appropriate pressure-temperature (P-T) conditions. The vast majority of studies of aqueous geochemistry relevant tomore » terrestrial problems of fluid-rock interactions have been conducted at 0.3 GPa or less, and the widely used Helgeson-Kirkham-Flowers equation of state for aqueous species is applicable only at ~ < 0.5 GPa. These limits are unfortunate because fluid flow and reactions plays a central role in many deeper environments. Recent efforts including our own, have resulted in new experimental techniques that now make it possible to investigate properties of homogeneous and heterogeneous equilibria involving aqueous species and minerals over a much broader range of pressure and temperature appropriate for deep crustal and upper mantle processes involving water-rich fluids. We carried out 1) Brillouin scattering measurements of the equations of state and molar volume of water and carbon dioxide to over 10 GPa and 870K using precise resistance heating of samples under pressure in the diamond anvil cell, and 2) the phase diagrams of the water and CO2, and 3) Exploring new experimental approaches, including CO2 laser heating of samples in a diamond cell, to measurements of sound velocities, EOS, and phase relations by Brillouin scattering to far greater pressures and temperatures.« less

Quantitative secondary electron detection

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

Agrawal, Jyoti; Joy, David C.; Nayak, Subuhadarshi

Quantitative Secondary Electron Detection (QSED) using the array of solid state devices (SSD) based electron-counters enable critical dimension metrology measurements in materials such as semiconductors, nanomaterials, and biological samples (FIG. 3). Methods and devices effect a quantitative detection of secondary electrons with the array of solid state detectors comprising a number of solid state detectors. An array senses the number of secondary electrons with a plurality of solid state detectors, counting the number of secondary electrons with a time to digital converter circuit in counter mode.

A contribution to the knowledge of HMX decomposition and application of results. [at atmospheric pressure

NASA Technical Reports Server (NTRS)

Kraeutle, K. J.

1980-01-01

The decomposition of cyclotramethylenetetranitramine (HMX) in the solid and liquid phase was studied by isothermal and nonisothermal heating at atmospheric pressure. Decomposition rates of solid HMX changed with sample size and gaseous environment. Kinetic parameters were obtained from weight loss measurements in the temperature range 229 C - 269 C. These tests also yielded highly porous solid residues. Qualitative aspects of solid and liquid phase decomposition of HMX with additives were also investigated in isothermal and nonisothermal tests.

Using large volume samplers for the monitoring of particle bound micro pollutants in rivers

NASA Astrophysics Data System (ADS)

Kittlaus, Steffen; Fuchs, Stephan

2015-04-01

The requirements of the WFD as well as substance emission modelling at the river basin scale require stable monitoring data for micro pollutants. The monitoring concepts applied by the local authorities as well as by many scientists use single sampling techniques. Samples from water bodies are usually taken in volumes of about one litre and depending on predetermined time steps or through discharge thresholds. For predominantly particle bound micro pollutants the small sample size of about one litre results in a very small amount of suspended particles. To measure micro pollutant concentrations in these samples is demanding and results in a high uncertainty of the measured concentrations, if the concentration is above the detection limit in the first place. In many monitoring programs most of the measured values were below the detection limit. This results in a high uncertainty if river loads were calculated from these data sets. The authors propose a different approach to gain stable concentration values for particle bound micro pollutants from river monitoring: A mixed sample of about 1000 L was pumped in a tank with a dirty-water pump. The sampling usually is done discharge dependant by using a gauge signal as input for the control unit. After the discharge event is over or the tank is fully filled, the suspended solids settle in the tank for 2 days. After this time a clear separation of water and solids can be shown. A sample (1 L) from the water phase and the total mass of the settled solids (about 10 L) are taken to the laboratory for analysis. While the micro pollutants can't hardly be detected in the water phase, the signal from the sediment is high above the detection limit, thus certain and very stable. From the pollutant concentration in the solid phase and the total tank volume the initial pollutant concentration in the sample can be calculated. If the concentration in the water phase is detectable, it can be used to correct the total load. This relatively low cost approach (less costs for analysis because of small sample number) allows to quantify the pollutant load, to derive dissolved-solid partition coefficients and to quantify the pollutant load in different particle size classes.

Nutrient, suspended-sediment, and total suspended-solids data for surface water in the Great Salt Lake basins study unit, Utah, Idaho, and Wyoming, 1980-95

USGS Publications Warehouse

Hadley, Heidi K.

2000-01-01

Selected nitrogen and phosphorus (nutrient), suspended-sediment and total suspended-solids surface-water data were compiled from January 1980 through December 1995 within the Great Salt Lake Basins National Water-Quality Assessment study unit, which extends from southeastern Idaho to west-central Utah and from Great Salt Lake to the Wasatch and western Uinta Mountains. The data were retrieved from the U.S. Geological Survey National Water Information System and the State of Utah, Department of Environmental Quality, Division of Water Quality database. The Division of Water Quality database includes data that are submitted to the U.S. Environmental Protection Agency STOrage and RETrieval system. Water-quality data included in this report were selected for surface-water sites (rivers, streams, and canals) that had three or more nutrient, suspended-sediment, or total suspended-solids analyses. Also, 33 percent or more of the measurements at a site had to include discharge, and, for non-U.S. Geological Survey sites, there had to be 2 or more years of data. Ancillary data for parameters such as water temperature, pH, specific conductance, streamflow (discharge), dissolved oxygen, biochemical oxygen demand, alkalinity, and turbidity also were compiled, as available. The compiled nutrient database contains 13,511 samples from 191 selected sites. The compiled suspended-sediment and total suspended-solids database contains 11,642 samples from 142 selected sites. For the nutrient database, the median (50th percentile) sample period for individual sites is 6 years, and the 75th percentile is 14 years. The median number of samples per site is 52 and the 75th percentile is 110 samples. For the suspended-sediment and total suspended-solids database, the median sample period for individual sites is 9 years, and the 75th percentile is 14 years. The median number of samples per site is 76 and the 75th percentile is 120 samples. The compiled historical data are being used in the basinwide sampling strategy to characterize the broad-scale geographic and seasonal water-quality conditions in relation to major contaminant sources and background conditions. Data for this report are stored on a compact disc.

A METHOD FOR AUTOMATED ANALYSIS OF 10 ML WATER SAMPLES CONTAINING ACIDIC, BASIC, AND NEUTRAL SEMIVOLATILE COMPOUNDS LISTED IN USEPA METHOD 8270 BY SOLID PHASE EXTRACTION COUPLED IN-LINE TO LARGE VOLUME INJECTION GAS CHROMATOGRAPHY/MASS SPECTROMETRY

EPA Science Inventory

Data is presented showing the progress made towards the development of a new automated system combining solid phase extraction (SPE) with gas chromatography/mass spectrometry for the single run analysis of water samples containing a broad range of acid, base and neutral compounds...

A sol-gel based solid phase microextraction fiber for the analysis of aliphatic alcohols in apple juices.

PubMed

Farhadi, Khalil; Maleki, Ramin; Tahmasebi, Raheleh

2010-01-01

A new fiber based on titania-chitin sol-gel coated on a silver wire for the headspace solid phase microextraction of aliphatic alcohols from apple juice samples was developed. The influences of fiber coating composition and microextraction conditions (extraction temperature, extraction time, and ionic strength of the sample matrix) on the fiber performance were investigated. Also, the influence of temperature and time on desorption of analytes from fiber were studied. Under the optimized conditions, a porous fiber with a high extraction capacity and good thermal stability (up to 250 degrees C) was obtained. The proposed headspace solid-phase microextraction-GC method was successfully used for the analysis of aliphatic alcohols in apple juice and concentrate samples. The recovery values were from 92.8 to 98.6%. The RSD (n=5) for all analytes were below 7.8%.

Experimental and computational studies on molecularly imprinted solid-phase extraction for gonyautoxins 2,3 from dinoflagellate Alexandrium minutum.

PubMed

Lian, Ziru; Li, Hai-Bei; Wang, Jiangtao

2016-08-01

An innovative and effective extraction procedure based on molecularly imprinted solid-phase extraction (MISPE) was developed for the isolation of gonyautoxins 2,3 (GTX2,3) from Alexandrium minutum sample. Molecularly imprinted polymer microspheres were prepared by suspension polymerization and and were employed as sorbents for the solid-phase extraction of GTX2,3. An off-line MISPE protocol was optimized. Subsequently, the extract samples from A. minutum were analyzed. The results showed that the interference matrices in the extract were obviously cleaned up by MISPE procedures. This outcome enabled the direct extraction of GTX2,3 in A. minutum samples with extraction efficiency as high as 83 %, rather significantly, without any need for a cleanup step prior to the extraction. Furthermore, computational approach also provided direct evidences of the high selective isolation of GTX2,3 from the microalgal extracts.

Effect of decompression drying treatment on physical properties of solid foods.

PubMed

Morikawa, Takuya; Takada, Norihisa; Miura, Makoto

2017-04-01

This study used a decompression drying instrument to investigate the effects of a drying treatment on the physical properties of solid foods. Commercial tofu was used as a model food and was treated at different temperature and pressure conditions in a drying chamber. Overall, high temperatures resulted in better drying. Additionally, pressure in the chamber influenced the drying conditions of samples. Differences in physical properties, such as food texture, shrinkage, and color were observed among some samples, even with similar moisture content. This was caused by differences in moisture distribution in the food, which seems to have manifested as a thin, dried film on the surfaces of samples. It caused inefficient drying and changes in physical properties. Control of the drying conditions (i.e. pressure and heat supply) has relations with not only physical properties, but also the drying efficiency of solid foods.

The SOLID (Signs Of LIfe Detector) instrument concept: an antibody microarray-based biosensor for life detection in astrobiology

NASA Astrophysics Data System (ADS)

Parro, V.; Rivas, L. A.; Rodríguez-Manfredi, J. A.; Blanco, Y.; de Diego-Castilla, G.; Cruz-Gil, P.; Moreno-Paz, M.; García-Villadangos, M.; Compostizo, C.; Herrero, P. L.

2009-04-01

Immunosensors have been extensively used since many years for environmental monitoring. Different technological platforms allow new biosensor designs and implementations. We have reported (Rivas et al., 2008) a shotgun approach for antibody production for biomarker detection in astrobiology and environmental monitoring, the production of 150 new polyclonal antibodies against microbial strains and environmental extracts, and the construction and validation of an antibody microarray (LDCHIP200, for "Life Detector Chip") containing 200 different antibodies. We have successfully used the LDCHIP200 for the detection of biological polymers in extreme environments in different parts of the world (e.g., a deep South African mine, Antarctica's Dry valleys, Yellowstone, Iceland, and Rio Tinto). Clustering analysis associated similar immunopatterns to samples from apparently very different environments, indicating that they indeed share similar universal biomarkers. A redundancy in the number of antibodies against different target biomarkers apart of revealing the presence of certain biomolecules, it renders a sample-specific immuno-profile, an "immnuno-fingerprint", which may constitute by itself an indirect biosignature. We will present a case study of immunoprofiling different iron-sulfur as well as phylosilicates rich samples along the Rio Tinto river banks. Based on protein microarray technology, we designed and built the concept instrument called SOLID (for "Signs Of LIfe Detector"; Parro et al., 2005; 2008a, b; http://cab.inta.es/solid) for automatic in situ analysis of soil samples and molecular biomarkers detection. A field prototype, SOLID2, was successfully tested for the analysis of grinded core samples during the 2005 "MARTE" campaign of a Mars drilling simulation experiment by a sandwich microarray immunoassay (Parro et al., 2008b). We will show the new version of the instrument (SOLID3) which is able to perform both sandwich and competitive immunoassays. SOLID3 consists of two separate functional units: a Sample Preparation Unit (SPU), for ten different extractions by ultrasonication, and a Sample Analysis Unit (SAU), for fluorescent immunoassays. The SAU consists of ten different flow cells each of one allocate one antibody microarray (up to 2000 spots), and is equipped with an unique designed optical package for fluorescent detection. We demonstrate the performance of SOLID3 for the detection of a broad range of molecular size compounds, from the amino acid size, peptides, proteins, to whole cells and spores, with sensitivities at the ppb level. References Parro, V., et al., 2005. Planetary and Space Science 53: 729-737. Parro, V., et al., 2008a. Space Science Reviews 135: 293-311 Parro, V., et al., 2008b. Astrobiology 8:987-99 Rivas, L. A., et al., 2008. Analytical Chemistry 80: 7970-7979

Chemical ageing and transformation of diffusivity in semi-solid multi-component organic aerosol particles

NASA Astrophysics Data System (ADS)

Pfrang, C.; Shiraiwa, M.; Pöschl, U.

2011-04-01

Recent experimental evidence underlines the importance of reduced diffusivity in amorphous semi-solid or glassy atmospheric aerosols. This paper investigates the impact of diffusivity on the ageing of multi-component reactive organic particles representative of atmospheric cooking aerosols. We apply and extend the recently developed KM-SUB model in a study of a 12-component mixture containing oleic and palmitoleic acids. We demonstrate that changes in the diffusivity may explain the evolution of chemical loss rates in ageing semi-solid particles, and we resolve surface and bulk processes under transient reaction conditions considering diffusivities altered by oligomerisation. This new model treatment allows prediction of the ageing of mixed organic multi-component aerosols over atmospherically relevant time scales and conditions. We illustrate the impact of changing diffusivity on the chemical half-life of reactive components in semi-solid particles, and we demonstrate how solidification and crust formation at the particle surface can affect the chemical transformation of organic aerosols.

Chemical ageing and transformation of diffusivity in semi-solid multi-component organic aerosol particles

NASA Astrophysics Data System (ADS)

Pfrang, C.; Shiraiwa, M.; Pöschl, U.

2011-07-01

Recent experimental evidence underlines the importance of reduced diffusivity in amorphous semi-solid or glassy atmospheric aerosols. This paper investigates the impact of diffusivity on the ageing of multi-component reactive organic particles approximating atmospheric cooking aerosols. We apply and extend the recently developed KM-SUB model in a study of a 12-component mixture containing oleic and palmitoleic acids. We demonstrate that changes in the diffusivity may explain the evolution of chemical loss rates in ageing semi-solid particles, and we resolve surface and bulk processes under transient reaction conditions considering diffusivities altered by oligomerisation. This new model treatment allows prediction of the ageing of mixed organic multi-component aerosols over atmospherically relevant timescales and conditions. We illustrate the impact of changing diffusivity on the chemical half-life of reactive components in semi-solid particles, and we demonstrate how solidification and crust formation at the particle surface can affect the chemical transformation of organic aerosols.

Sewer solids separation by sedimentation--the problem of modeling, validation and transferability.

PubMed

Kutzner, R; Brombach, H; Geiger, W F

2007-01-01

Sedimentation of sewer solids in tanks, ponds and similar devices is the most relevant process for the treatment of stormwater and combined sewer overflows in urban collecting systems. In the past a lot of research work was done to develop deterministic models for the description of this separation process. But these modern models are not commonly accepted in Germany until today. Water Authorities are sceptical with regard to model validation and transferability. Within this paper it is checked whether this scepticism is reasonable. A framework-proposal for the validation of mathematical models with zero or one dimensional spatial resolution for particle separation processes for stormwater and combined sewer overflow treatment is presented. This proposal was applied to publications of repute on sewer solids separation by sedimentation. The result was that none of the investigated models described in literature passed the validation entirely. There is an urgent need for future research in sewer solids sedimentation and remobilization!

EVALUATION OF SOLID PHASE MICROEXTRACTION FOR THE ANALYSIS OF HYDROPHILIC COMPOUNDS

EPA Science Inventory

Two commercially available solid phase microextractions (SPME) fibers, polyacrylate and carboxem/polydimethylsiloxane (PDMS), were evaluated for their ability to extract hydrophilic compounds from drinking water. Conditions, such as desorption time, desorption temperature, sample...

Experimental research results of solid particle erosion resistance of blade steel with protective coating

NASA Astrophysics Data System (ADS)

Kachalin, G. V.; Mednikov, A. F.; Tkhabisimov, A. B.; Seleznev, L. I.

2017-11-01

The paper presents the results of metallographic studies and solid particle erosion tests of uncoated blade steel 20kH13 samples and samples with a protective coating based on chromium carbide (Cr-CrC) at a flow (air) velocity CA = 180 m/s, flow temperature tA = 25 °C, attack angle α = 30° and consumption of solid abrasive particles GP = 5·10-4 kg/s. It was found that the coating has a granular structure, a thickness is about 11 μm, the microhardness of the surface is 1520 ± 50 HV0.05. Processing of the obtained data by statistical analysis methods showed that the protective coating based on Cr-CrC increases the solid particle erosion resistance of the blade steel 20kH13 by the incubation-transitional period duration more than 2.5 times.

Assessment of Bacterial Spores in Solid Materials: Curriculum Improvements Partnership Award for the Integration of Research (CIPAIR)

NASA Technical Reports Server (NTRS)

Lavallee, Richard J.

2012-01-01

This summer, we quantified the release, by cryogenic grinding at liquid nitrogen temperatures, of microbes present in 4 different spacecraft solids: epoxy 9309, epoxy 9394, epoxy 9396, and a silicone coating. Three different samples of each material were prepared: aseptically prepared solid material, powdered material inoculated with a known spore count of Bacillus atrophaeus, and solid material artificially embedded with a known spore count of Bacillus atrophaeus. Samples were cryogenically ground as needed, and the powders were directly cultured to determine the number of microbial survivors per gram of material. Recovery rates were found to be highly material-dependent, varying from 0.2 to 50% for inoculated material surfaces and 0.002 to 0.5% for embedded spores. A study of the spore survival rate versus total grinding time was also performed, with results indicating that longer grinding time decreases recovery rates of viable spores.

Gravitational Role in Liquid Phase Sintering

NASA Technical Reports Server (NTRS)

Upadhyaya, Anish; Iacocca, Ronald G.; German, Randall M.

1998-01-01

To comprehensively understand the gravitational effects on the evolution of both the microstructure and the macrostructure during liquid phase sintering, W-Ni-Fe alloys with W content varying from 35 to 98 wt.% were sintered in microgravity. Compositions that slump during ground-based sintering also distort when sintered under microgravity. In ground-based sintering, low solid content alloys distort with a typical elephant-foot profile, while in microgravity, the compacts tend to spheroidize. This study shows that microstructural segregation occurs in both ground-based as well as microgravity sintering. In ground-based experiments, because of the density difference between the solid and the liquid phase, the solid content increases from top to the bottom of the sample. In microgravity, the solid content increases from periphery to the center of the samples. This study also shows that the pores during microgravity sintering act as a stable phase and attain anomalous shapes.

Radioactivity concentration in liquid and solid phases of scale and sludge generated in the petroleum industry.

PubMed

Paranhos Gazineu, Maria Helena; de Araújo, Andressa Arruda; Brandão, Yana Batista; Hazin, Clovis Abrahão; de O Godoy, José Marcos

2005-01-01

Scales and sludge generated during oil extraction and production can contain uranium, thorium, radium and other natural radionuclides, which can cause exposure of maintenance personnel. This work shows how the oil content can influence the results of measurements of radionuclide concentration in scale and sludge. Samples were taken from a PETROBRAS unit in Northeast Brazil. They were collected directly from the inner surface of water pipes or from barrels stored in the waste storage area of the E&P unit. The oil was separated from the solids with a Soxhlet extractor by using aguarras at 90+/-5 degrees C as solvent. Concentrations of 226Ra and 228Ra in the samples were determined before and after oil extraction by using an HPGe gamma spectrometric system. The results showed an increase in the radionuclide concentration in the solid (dry) phase, indicating that the above radionuclides concentrate mostly in the solid material.

Isotope Labeling for Solution and Solid-State NMR Spectroscopy of Membrane Proteins

PubMed Central

Verardi, Raffaello; Traaseth, Nathaniel J.; Masterson, Larry R.; Vostrikov, Vitaly V.; Veglia, Gianluigi

2013-01-01

In this chapter, we summarize the isotopic labeling strategies used to obtain high-quality solution and solid-state NMR spectra of biological samples, with emphasis on integral membrane proteins (IMPs). While solution NMR is used to study IMPs under fast tumbling conditions, such as in the presence of detergent micelles or isotropic bicelles, solid-state NMR is used to study the structure and orientation of IMPs in lipid vesicles and bilayers. In spite of the tremendous progress in biomolecular NMR spectroscopy, the homogeneity and overall quality of the sample is still a substantial obstacle to overcome. Isotopic labeling is a major avenue to simplify overlapped spectra by either diluting the NMR active nuclei or allowing the resonances to be separated in multiple dimensions. In the following we will discuss isotopic labeling approaches that have been successfully used in the study of IMPs by solution and solid-state NMR spectroscopy. PMID:23076578

Experimental validation of Swy-2 clay standard's PHREEQC model

NASA Astrophysics Data System (ADS)

Szabó, Zsuzsanna; Hegyfalvi, Csaba; Freiler, Ágnes; Udvardi, Beatrix; Kónya, Péter; Székely, Edit; Falus, György

2017-04-01

One of the challenges of the present century is to limit the greenhouse gas emissions for the mitigation of climate change which is possible for example by a transitional technology, CCS (Carbon Capture and Storage) and, among others, by the increase of nuclear proportion in the energy mix. Clay minerals are considered to be responsible for the low permeability and sealing capacity of caprocks sealing off stored CO2 and they are also the main constituents of bentonite in high level radioactive waste disposal facilities. The understanding of clay behaviour in these deep geological environments is possible through laboratory batch experiments of well-known standards and coupled geochemical models. Such experimentally validated models are scarce even though they allow deriving more precise long-term predictions of mineral reactions and rock and bentonite degradation underground and, therefore, ensuring the safety of the above technologies and increase their public acceptance. This ongoing work aims to create a kinetic geochemical model of Na-montmorillonite standard Swy-2 in the widely used PHREEQC code, supported by solution and mineral composition results from batch experiments. Several four days experiments have been carried out in 1:35 rock:water ratio at atmospheric conditions, and with inert and CO2 supercritical phase at 100 bar and 80 ⁰C relevant for the potential Hungarian CO2 reservoir complex. Solution samples have been taken during and after experiments and their compositions were measured by ICP-OES. The treated solid phase has been analysed by XRD and ATR-FTIR and compared to in-parallel measured references (dried Swy-2). Kinetic geochemical modelling of the experimental conditions has been performed by PHREEQC version 3 using equations and kinetic rate parameters from the USGS report of Palandri and Kharaka (2004). The visualization of experimental and numerous modelling results has been automatized by R. Experiments and models show very fast reactions under the studied conditions and increased reactivity in presence of scCO2. A model sensitivity analysis has pointed out that the continuously changing solution composition results cannot be described by the change of the uncertain reactive surface area of mineral phases in the model and still several orders of magnitude different ion-concentrations are predicted. However, by considering the clay standard's cation exchange capacity divided proportionally among interlayer cations of Na-montmorillonite, the measured variation can be described on an order of magnitude level. It is furthermore indicated that not only the interlayer cations take part in this process but a minor proportion of other, structural ions as well, differently in the reference and scCO2 environments. Experimental methodological aspects of the work, such as solution sampling, solid sample post-experimental treatment, solution and solid sample analysis sensitivity, expected experimental by-products etc. are also to be addressed.

Heat Transfer in High Temperature Multilayer Insulation

NASA Technical Reports Server (NTRS)

Daryabeigi, Kamran; Miller, Steve D.; Cunnington, George R.

2007-01-01

High temperature multilayer insulations have been investigated as an effective component of thermal-protection systems for atmospheric re-entry of reusable launch vehicles. Heat transfer in multilayer insulations consisting of thin, gold-coated, ceramic reflective foils and Saffil(TradeMark) fibrous insulation spacers was studied both numerically and experimentally. A finite volume numerical thermal model using combined conduction (gaseous and solid) and radiation in porous media was developed. A two-flux model with anisotropic scattering was used for radiation heat transfer in the fibrous insulation spacers between the reflective foils. The thermal model was validated by comparison with effective thermal conductivity measurements in an apparatus based on ASTM standard C201. Measurements were performed at environmental pressures in the range from 1x10(exp -4) to 760 torr over the temperature range from 300 to 1300 K. Four multilayer samples with nominal densities of 48 kg/cu m were tested. The first sample was 13.3 mm thick and had four evenly spaced reflective foils. The other three samples were 26.6 mm thick and utilized either one, two, or four reflective foils, located near the hot boundary with nominal foil spacing of 1.7 mm. The validated thermal model was then used to study relevant design parameters, such as reflective foil spacing and location in the stack-up and coating of one or both sides of foils.

On the coherent rotation of diffuse matter in numerical simulations of clusters of galaxies

NASA Astrophysics Data System (ADS)

Baldi, Anna Silvia; De Petris, Marco; Sembolini, Federico; Yepes, Gustavo; Lamagna, Luca; Rasia, Elena

2017-03-01

We present a study on the coherent rotation of the intracluster medium and dark matter components of simulated galaxy clusters extracted from a volume-limited sample of the MUSIC project. The set is re-simulated with three different recipes for the gas physics: (I) non-radiative, (II) radiative without active galactic nuclei (AGN) feedback and (III) radiative with AGN feedback. Our analysis is based on the 146 most massive clusters identified as relaxed, 57 per cent of the total sample. We classify these objects as rotating and non-rotating according to the gas spin parameter, a quantity that can be related to cluster observations. We find that 4 per cent of the relaxed sample is rotating according to our criterion. By looking at the radial profiles of their specific angular momentum vector, we find that the solid body model is not a suitable description of rotational motions. The radial profiles of the velocity of the dark matter show a prevalence of the random velocity dispersion. Instead, the intracluster medium profiles are characterized by a comparable contribution from the tangential velocity and the dispersion. In general, the dark matter component dominates the dynamics of the clusters, as suggested by the correlation between its angular momentum and the gas one, and by the lack of relevant differences among the three sets of simulations.

Development of Millimeter-Wave Velocimetry and Acoustic Time-of-Flight Tomography for Measurements in Densely Loaded Gas-Solid Riser Flow

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

Fort, James A.; Pfund, David M.; Sheen, David M.

2007-04-01

The MFDRC was formed in 1998 to advance the state-of-the-art in simulating multiphase turbulent flows by developing advanced computational models for gas-solid flows that are experimentally validated over a wide range of industrially relevant conditions. The goal was to transfer the resulting validated models to interested US commercial CFD software vendors, who would then propagate the models as part of new code versions to their customers in the US chemical industry. Since the lack of detailed data sets at industrially relevant conditions is the major roadblock to developing and validating multiphase turbulence models, a significant component of the work involvedmore » flow measurements on an industrial-scale riser contributed by Westinghouse, which was subsequently installed at SNL. Model comparisons were performed against these datasets by LANL. A parallel Office of Industrial Technology (OIT) project within the consortium made similar comparisons between riser measurements and models at NETL. Measured flow quantities of interest included volume fraction, velocity, and velocity-fluctuation profiles for both gas and solid phases at various locations in the riser. Some additional techniques were required for these measurements beyond what was currently available. PNNL’s role on the project was to work with the SNL experimental team to develop and test two new measurement techniques, acoustic tomography and millimeter-wave velocimetry. Acoustic tomography is a promising technique for gas-solid flow measurements in risers and PNNL has substantial related experience in this area. PNNL is also active in developing millimeter wave imaging techniques, and this technology presents an additional approach to make desired measurements. PNNL supported the advanced diagnostics development part of this project by evaluating these techniques and then by adapting and developing the selected technology to bulk gas-solids flows and by implementing them for testing in the SNL riser testbed.« less

PAHs contamination in urban soils from Lisbon: spatial variability and potential risks

NASA Astrophysics Data System (ADS)

Cachada, Anabela; Pereira, Ruth; Ferreira da Silva, Eduardo; Duarte, Armando

2015-04-01

Polycyclic Aromatic hydrocarbons (PAHs) can become major contaminants in urban and industrial areas, due to the existence of a plethora of diffuse and point sources. Particularly diffuse pollution, which is normally characterized by continuous and long-term emission of contaminants below risk levels, can be a major problem in urban areas. Since PAHs are persistent and tend to accumulate in soils, levels are often above the recommended guidelines indicating that ecological functions of soils may be affected. Moreover, due to the lipophilic nature, hydrophobicity and low chemical and biological degradation rates of PAHs, which leads to their bioconcentration and bioamplification, they may reach toxicological relevant concentrations in organisms. The importance and interest of studying this group of contaminants is magnified due to their carcinogenic, mutagenic and endocrine disrupting effects. In this study, a risk assessment framework has been followed in order to evaluate the potential hazards posed by the presence of PAHs in Lisbon urban soils. Hence, the first step consisted in screening the total concentrations of PAHs followed by the calculation of risks based on existing models. Considering these models several samples were identified as representing a potential risk when comparing with the guidelines for soil protection. Moreover, it was found that for 38% of samples more than 50% of species can be potentially affected by the mixture of PAHs. The use of geostatistical methods allowed to visualize the predicted distribution of PAHs in Lisbon area and identify the areas where possible risk to the environment are likely occurring However, it is known that total concentration may not allow a direct prediction of environmental risk, since in general only a fraction of total concentration is available for partitioning between soil and solution and thus to be uptake or transformed by organisms (bioacessible or bioavailable) or to be leached to groundwater. The reason is that once PAHs reach the soils, they can be incorporated into more stable solid phases over time, for instance, they can be retained in the organic phase, and this process known as aging, can be virtually irreversible. This phenomenon can be particularly relevant in urban soils since the highest levels are normally found in historical sites, suggesting a long-term accumulation as observed in the present study. The estimation of this fraction is traditionally performed by using bioassays (bioavailability), yet chemical methods can also be used (chemical availability). Following a higher tier of the risk assessment framework, some selected samples previously identified as representing a potential hazard were tested for their bioavailability (earthworm bioaccumulation assay, OECD test n° 317) and chemical availability (solid phase extraction with Tenax® and water). Results showed that in spite of the very high levels found in some samples, the risks can be negligible, since both the bioavailable and water soluble fractions were very low. The relationship between available fraction and soil properties is not clear, and differences observed between samples are probably related to the age of contamination since lower available fractions were observed in the most contaminated soils.

Effectiveness of catch basins equipped with hoods in retaining gross solids and hydrocarbons in highway runoff, Southeast Expressway, Boston, Massachusetts, 2008-09

USGS Publications Warehouse

Smith, Kirk P.

2011-01-01

Stormwater mobilizes litter and other debris along the roadway where it is transported to the highway drainage systems. Initial treatment for stormwater runoff typically is provided by catch basins in highway settings. Modification of catch basins to include hoods that cover the catch-basin outlet is intended to enhance catch-basin performance by retaining floatable debris and various hydrophobic organic compounds that tend to float on the water surface within the sump of the catch basin. The effectiveness of six deep-sump off-line catch basins equipped with hoods in reducing the mass of gross solids greater than 0.25 inches in diameter and concentrations of oil and grease (OG) and total petroleum hydrocarbons (TPH) was examined along the Southeast Expressway, in Boston, Massachusetts. Two deep-sump catch basins were equipped with cast-iron hoods. Three were equipped with molded plastic hoods, known as an Eliminator, and a single catch basin was equipped with a fiberglass anti-siphoning hood, known as a Snout. Samples of gross solids greater than 0.25 inches in diameter, excluding gravel and metallic materials, were routinely collected for a 6-month period from a collection structure mounted at the end of each catch-basin outlet pipe. After about 6 months, all floatable, saturated low-density and high-density solids were removed from each catch basin. In addition to the collection of samples of gross solids, samples of sump water from five catch basins and flow-weighted composite samples of stormwater from the outlet of one catch basin were collected and analyzed for concentrations of OG and TPH. A mass balance approach was used to assess the effectiveness of each catch basin equipped with a hood in retaining gross solids. The effectiveness of the deep-sump catch basins fitted with one of three types of hoods in retaining gross solids ranged from 27 to 52 percent. From 45 to 90 percent of the gross solids collected from the catch-basin sumps were composed of materials made of high-density plastics that did not float in water, and as a result, the effect that the catch-basin hoods had on these materials likely was marginal. The effectiveness for the deep-sump hooded catch basins, excluding the mass of high-density materials identified in the solids collected from the outlet pipe and the sump of the catch basins, ranged from 13 to 38 percent. The effectiveness for each catch basin, based solely on the material that remained floating at the end of the monitoring period, was less than 11 percent; however, these values likely underestimate the effectiveness of the hooded catch basins because much of the low-density material collected from the sumps may have been retained as floatable material before it was saturated and settled during non-storm conditions. The effectiveness of the catch basins equipped with hoods in reducing gross solids was not greatly different among the three types of hoods tested in this study. Concentrations of OG and TPH collected from the water surface of the catch-basins varied from catch basin to catch basin and were similar to concentrations of flow-weighted composite samples collected during storms. Comparisons indicate concentrations of OG and TPH in flow-weighted composite samples collected at the outlet of a catch basin equipped with an Eliminator hood were not substantially different from concentrations of the respective constituents in flow-weighted composite samples collected during a previous study from catch basins containing cast-iron hoods in the same study area. The similarity between these flow-weighted concentrations and the concentrations of the respective constituents in a vertical profile sample collected from the catch-basin sump indicates that OG and TPH are emulsified in the sump of each catch basin during storms and circumvent the hoods.

Apparatus and method for measuring electrostatic polarization

DOEpatents

Hahn, Erwin L.; Clarke, John; Sloater, Tycho; Hilbert, Claude; Heaney, Michael B.

1989-01-01

An apparatus and method for measuring the electric properties of solid matter which provides data for determining the polarizability of the electron distributions contained therein is disclosed. A sample of the solid to be studied is placed between the plates of a capacitor where it acts as a dielectric. The sample is excited by the interaction of electromagnetic radiation with an atomic species contained in the sample. The voltage induced across the capacitor is then measured as a function of time with the aid of a high Q circuit tuned to a frequency related to the frequency of the applied electromagnetic energy.

Thermal Design, Analysis, and Testing of the Quench Module Insert Bread Board

NASA Technical Reports Server (NTRS)

Breeding Shawn; Khodabandeh, Julia; Turner, Larry D. (Technical Monitor)

2001-01-01

The science requirements for materials processing is to provide the desired PI requirements of thermal gradient, solid/liquid interface front velocity for a given processing temperature desired by the PI. Processing is performed by translating the furnace with the sample in a stationary position to minimize any disturbances to the solid/liquid interface front during steady state processing. Typical sample materials for this metals and alloys furnace are lead-tin alloys, lead-antimony alloys, and aluminum alloys. Samples must be safe to process and therefore typically are contained with hermetically sealed cartridge tubes (gas tight) with inner ceramic liners (liquid tight) to prevent contamination and/or reaction of the sample material with the cartridge tube.

Identifying marker genes in transcription profiling data using a mixture of feature relevance experts.

PubMed

Chow, M L; Moler, E J; Mian, I S

2001-03-08

Transcription profiling experiments permit the expression levels of many genes to be measured simultaneously. Given profiling data from two types of samples, genes that most distinguish the samples (marker genes) are good candidates for subsequent in-depth experimental studies and developing decision support systems for diagnosis, prognosis, and monitoring. This work proposes a mixture of feature relevance experts as a method for identifying marker genes and illustrates the idea using published data from samples labeled as acute lymphoblastic and myeloid leukemia (ALL, AML). A feature relevance expert implements an algorithm that calculates how well a gene distinguishes samples, reorders genes according to this relevance measure, and uses a supervised learning method [here, support vector machines (SVMs)] to determine the generalization performances of different nested gene subsets. The mixture of three feature relevance experts examined implement two existing and one novel feature relevance measures. For each expert, a gene subset consisting of the top 50 genes distinguished ALL from AML samples as completely as all 7,070 genes. The 125 genes at the union of the top 50s are plausible markers for a prototype decision support system. Chromosomal aberration and other data support the prediction that the three genes at the intersection of the top 50s, cystatin C, azurocidin, and adipsin, are good targets for investigating the basic biology of ALL/AML. The same data were employed to identify markers that distinguish samples based on their labels of T cell/B cell, peripheral blood/bone marrow, and male/female. Selenoprotein W may discriminate T cells from B cells. Results from analysis of transcription profiling data from tumor/nontumor colon adenocarcinoma samples support the general utility of the aforementioned approach. Theoretical issues such as choosing SVM kernels and their parameters, training and evaluating feature relevance experts, and the impact of potentially mislabeled samples on marker identification (feature selection) are discussed.

Sewage sludge solubilization by high-pressure homogenization.

PubMed

Zhang, Yuxuan; Zhang, Panyue; Guo, Jianbin; Ma, Weifang; Fang, Wei; Ma, Boqiang; Xu, Xiangzhe

2013-01-01

The behavior of sludge solubilization using high-pressure homogenization (HPH) treatment was examined by investigating the sludge solid reduction and organics solubilization. The sludge volatile suspended solids (VSS) decreased from 10.58 to 6.67 g/L for the sludge sample with a total solids content (TS) of 1.49% after HPH treatment at a homogenization pressure of 80 MPa with four homogenization cycles; total suspended solids (TSS) correspondingly decreased from 14.26 to 9.91 g/L. About 86.15% of the TSS reduction was attributed to the VSS reduction. The increase of homogenization pressure from 20 to 80 MPa or homogenization cycle number from 1 to 4 was favorable to the sludge organics solubilization, and the protein and polysaccharide solubilization linearly increased with the soluble chemical oxygen demand (SCOD) solubilization. More proteins were solubilized than polysaccharides. The linear relationship between SCOD solubilization and VSS reduction had no significant change under different homogenization pressures, homogenization cycles and sludge solid contents. The SCOD of 1.65 g/L was solubilized for the VSS reduction of 1.00 g/L for the three experimental sludge samples with a TS of 1.00, 1.49 and 2.48% under all HPH operating conditions. The energy efficiency results showed that the HPH treatment at a homogenization pressure of 30 MPa with a single homogenization cycle for the sludge sample with a TS of 2.48% was the most energy efficient.

Effect of ultrasound and centrifugal force on carambola (Averrhoa carambola L.) slices during osmotic dehydration.

PubMed

Barman, Nirmali; Badwaik, Laxmikant S

2017-01-01

Osmotic dehydration (OD) of carambola slices were carried out using glucose, sucrose, fructose and glycerol as osmotic agents with 70°Bx solute concentration, 50°C of temperature and for time of 180min. Glycerol and sucrose were selected on the basis of their higher water loss, weight reduction and lowers solid gain. Further the optimization of OD of carambola slices (5mm thick) were carried out under different process conditions of temperature (40-60°C), concentration of sucrose and glycerol (50-70°Bx), time (180min) and fruit to solution ratio (1:10) against various responses viz. water loss, solid gain, texture, rehydration ratio and sensory score according to a composite design. The optimized value for temperature, concentration of sucrose and glycerol has been found to be 50°C, 66°Bx and 66°Bx respectively. Under optimized conditions the effect of ultrasound for 10, 20, 30min and centrifugal force (2800rpm) for 15, 30, 45 and 60min on OD of carambola slices were checked. The controlled samples showed 68.14% water loss and 13.05% solid gain in carambola slices. While, the sample having 30min ultrasonic treatment showed 73.76% water loss and 9.79% solid gain; and the sample treated with centrifugal force for 60min showed 75.65% water loss and 6.76% solid gain. The results showed that with increasing in treatment time the water loss, rehydration ratio were increased and solid gain, texture were decreased. Copyright © 2016 Elsevier B.V. All rights reserved.

Millimeter-Wave Spectroscopy for Analytical Chemistry: Thermal Evolution of Low Volatility Impurities and Detection with a Fourier Transform Molecular Rotational Resonance Spectrometer (tev Ft-Mrr

NASA Astrophysics Data System (ADS)

Harris, Brent; Fields, Shelby S.; Neill, Justin L.; Pulliam, Robin; Muckle, Matt; Pate, Brooks

2016-06-01

Recent advances in Fourier transform millimeter-wave spectroscopy techniques have renewed the application reach of molecular rotational spectroscopy for analytical chemistry. We present a sampling method for sub ppm analysis of low volatility impurities by thermal evolution from solid powders using a millimeter-wave Fourier transform molecular rotational resonance (FT-MRR) spectrometer for detection. This application of FT-MRR is relevant to the manufacturing of safe oral pharmaceuticals. Low volatility impurities can be challenging to detect at 1 ppm levels with chromatographic techniques. One such example of a potentially mutagenic impurity is acetamide (v.p. 1 Torr at 40 C, m.p. 80 C). We measured the pure reference spectrum of acetamide by flowing the sublimated vapor pressure of acetamide crystals through the FT-MRR spectrometer. The spectrometer lower detection level (LDL) for a broadband (> 20 GHz, 10 min.) spectrum is 300 nTorr, 30 pmol, or 2 ng. For a 50 mg powder, perfect sample transfer efficiency can yield a w/w % detection limit of 35 ppb. We extended the sampling method for the acetamide reference measurement to an acetaminophen sample spiked with 5000 ppm acetamide in order to test the sample transfer efficiency when liberated from an pharmaceutical powder. A spectral reference matching algorithm detected the presence of several impurities including acetaldehyde, acetic acid, and acetonitrile that evolved at the melting point of acetaminophen, demonstrating the capability of FT-MRR for identification without a routine chemical standard. The method detection limit (MDL) without further development is less than 10 ppm w/w %. Resolved FT-MRR mixture spectra will be presented with a description of sampling methods.

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

PubMed

Verplaetse, Ruth; Henion, Jack

2016-01-01

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

The self-absorption correction factors for 210Pb concentration in mining waste and influence on environmental radiation risk assessment.

PubMed

Bonczyk, Michal; Michalik, Boguslaw; Chmielewska, Izabela

2017-03-01

The radioactive lead isotope 210 Pb occurs in waste originating from metal smelting and refining industry, gas and oil extraction and sometimes from underground coal mines, which are deposited in natural environment very often. Radiation risk assessment requires accurate knowledge about the concentration of 210 Pb in such materials. Laboratory measurements seem to be the only reliable method applicable in environmental 210 Pb monitoring. One of the methods is gamma-ray spectrometry, which is a very fast and cost-effective method to determine 210 Pb concentration. On the other hand, the self-attenuation of gamma ray from 210 Pb (46.5 keV) in a sample is significant as it does not depend only on sample density but also on sample chemical composition (sample matrix). This phenomenon is responsible for the under-estimation of the 210 Pb activity concentration level often when gamma spectrometry is applied with no regard to relevant corrections. Finally, the corresponding radiation risk can be also improperly evaluated. Sixty samples of coal mining solid tailings (sediments created from underground mining water) were analysed. Slightly modified and adapted to the existing laboratory condition, a transmission method has been applied for the accurate measurement of 210 Pb concentration . The observed concentrations of 210 Pb range between 42.2 ÷ 11,700 Bq·kg -1 of dry mass. Experimentally obtained correction factors related to a sample density and elemental composition range between 1.11 and 6.97. Neglecting this factor can cause a significant error or underestimations in radiological risk assessment. The obtained results have been used for environmental radiation risk assessment performed by use of the ERICA tool assuming exposure conditions typical for the final destination of such kind of waste.

Modelling solid solutions with cluster expansion, special quasirandom structures, and thermodynamic approaches

NASA Astrophysics Data System (ADS)

Saltas, V.; Horlait, D.; Sgourou, E. N.; Vallianatos, F.; Chroneos, A.

2017-12-01

Modelling solid solutions is fundamental in understanding the properties of numerous materials which are important for a range of applications in various fields including nanoelectronics and energy materials such as fuel cells, nuclear materials, and batteries, as the systematic understanding throughout the composition range of solid solutions for a range of conditions can be challenging from an experimental viewpoint. The main motivation of this review is to contribute to the discussion in the community of the applicability of methods that constitute the investigation of solid solutions computationally tractable. This is important as computational modelling is required to calculate numerous defect properties and to act synergistically with experiment to understand these materials. This review will examine in detail two examples: silicon germanium alloys and MAX phase solid solutions. Silicon germanium alloys are technologically important in nanoelectronic devices and are also relevant considering the recent advances in ternary and quaternary groups IV and III-V semiconductor alloys. MAX phase solid solutions display a palette of ceramic and metallic properties and it is anticipated that via their tuning they can have applications ranging from nuclear to aerospace industries as well as being precursors for particular MXenes. In the final part, a brief summary assesses the limitations and possibilities of the methodologies discussed, whereas there is discussion on the future directions and examples of solid solution systems that should prove fruitful to consider.