Hydrodynamic injection with pneumatic valving for microchip electrophoresis with total analyte utilization

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

Sun, Xuefei; Kelly, Ryan T.; Danielson, William F.

2011-04-26

A novel hydrodynamic injector that is directly controlled by a pneumatic valve has been developed for reproducible microchip capillary electrophoresis (CE) separations. The poly(dimethylsiloxane) (PDMS) devices used for evaluation comprise a separation channel, a side channel for sample introduction, and a pneumatic valve aligned at the intersection of the channels. A low pressure (≤ 3 psi) applied to the sample reservoir is sufficient to drive sample into the separation channel. The rapidly actuated pneumatic valve enables injection of discrete sample plugs as small as ~100 pL for CE separation. The injection volume can be easily controlled by adjusting the intersectionmore » geometry, the solution back pressure and the valve actuation time. Sample injection could be reliably operated at different frequencies (< 0.1 Hz to >2 Hz) with good reproducibility (peak height relative standard deviation ≤ 3.6%) and no sampling biases associated with the conventional electrokinetic injections. The separation channel was dynamically coated with a cationic polymer, and FITC-labeled amino acids were employed to evaluate the CE separation. Highly efficient (≥ 7.0 × 103 theoretical plates for the ~2.4 cm long channel) and reproducible CE separations were obtained. The demonstrated method has numerous advantages compared with the conventional techniques, including repeatable and unbiased injections, no sample waste, high duty cycle, controllable injected sample volume, and fewer electrodes with no need for voltage switching. The prospects of implementing this injection method for coupling multidimensional separations, for multiplexing CE separations and for sample-limited bioanalyses are discussed.« less

Droplet-based microfluidic flow injection system with large-scale concentration gradient by a single nanoliter-scale injection for enzyme inhibition assay.

PubMed

Cai, Long-Fei; Zhu, Ying; Du, Guan-Sheng; Fang, Qun

2012-01-03

We described a microfluidic chip-based system capable of generating droplet array with a large scale concentration gradient by coupling flow injection gradient technique with droplet-based microfluidics. Multiple modules including sample injection, sample dispersion, gradient generation, droplet formation, mixing of sample and reagents, and online reaction within the droplets were integrated into the microchip. In the system, nanoliter-scale sample solution was automatically injected into the chip under valveless flow injection analysis mode. The sample zone was first dispersed in the microchannel to form a concentration gradient along the axial direction of the microchannel and then segmented into a linear array of droplets by immiscible oil phase. With the segmentation and protection of the oil phase, the concentration gradient profile of the sample was preserved in the droplet array with high fidelity. With a single injection of 16 nL of sample solution, an array of droplets with concentration gradient spanning 3-4 orders of magnitude could be generated. The present system was applied in the enzyme inhibition assay of β-galactosidase to preliminarily demonstrate its potential in high throughput drug screening. With a single injection of 16 nL of inhibitor solution, more than 240 in-droplet enzyme inhibition reactions with different inhibitor concentrations could be performed with an analysis time of 2.5 min. Compared with multiwell plate-based screening systems, the inhibitor consumption was reduced 1000-fold. © 2011 American Chemical Society

Dark Current Characterization of SW HgCdTe IRFPAs Detectors on Si Substrate with Long Time Integration

NASA Astrophysics Data System (ADS)

Song, P. Y.; Ye, Z. H.; Huang, A. B.; Chen, H. L.; Hu, X. N.; Ding, R. J.; He, L.

2016-09-01

The dark currents of two short wave (SW) HgCdTe infrared focal plane arrays (IRFPA) detectors hybridized with direct injection (DI) readout and capacitance transimpedance amplifier (CTIA) with long time integration were investigated. The cutoff wavelength of the two SW IRFPAs is about 2.6 μm at 84 K. The dark current densities of DI and CTIA samples are approximately 8.0 × 10-12 A/cm2 and 7.2 × 10-10 A/cm2 at 110 K, respectively. The large divergence of the dark current density might arise from the injection efficiency difference of the two readouts. The low injection efficiency of the DI readout, compared with the high injection efficiency of the CTIA readout at low temperature, makes the dark current density of the DI sample much lower than that of the CTIA sample. The experimental value of injection efficiency of the DI sample was evaluated as 1.1% which is consistent with its theoretical value.

Determination of low molecular weight alcohols including fusel oil in various samples by diethyl ether extraction and capillary gas chromatography.

PubMed

Woo, Kang-Lyung

2005-01-01

Low molecular weight alcohols including fusel oil were determined using diethyl ether extraction and capillary gas chromatography. Twelve kinds of alcohols were successfully resolved on the HP-FFAP (polyethylene glycol) capillary column. The diethyl ether extraction method was very useful for the analysis of alcohols in alcoholic beverages and biological samples with excellent cleanliness of the resulting chromatograms and high sensitivity compared to the direct injection method. Calibration graphs for all standard alcohols showed good linearity in the concentration range used, 0.001-2% (w/v) for all alcohols. Salting out effects were significant (p < 0.01) for the low molecular weight alcohols methanol, isopropanol, propanol, 2-butanol, n-butanol and ethanol, but not for the relatively high molecular weight alcohols amyl alcohol, isoamyl alcohol, and heptanol. The coefficients of variation of the relative molar responses were less than 5% for all of the alcohols. The limits of detection and quantitation were 1-5 and 10-60 microg/L for the diethyl ether extraction method, and 10-50 and 100-350 microg/L for the direct injection method, respectively. The retention times and relative retention times of standard alcohols were significantly shifted in the direct injection method when the injection volumes were changed, even with the same analysis conditions, but they were not influenced in the diethyl ether extraction method. The recoveries by the diethyl ether extraction method were greater than 95% for all samples and greater than 97% for biological samples.

Anisotropic mechanical behavior of an injection molded short fiber reinforced thermoplastic

NASA Astrophysics Data System (ADS)

Lopez, Delphine; Thuillier, Sandrine; Bessières, Nicolas; Grohens, Yves

2016-10-01

A short fiber reinforced thermoplastic was injected into a rectangular mold, in order to prepare samples to characterize the mechanical behavior of the material. The injection process was simulated with Moldflow and a cutting pattern was deduced from the predicted fiber orientation, leading to samples with several well-defined orientations with respect to the injection direction. Monotonic tensile tests up to rupture, as well as complex cycles made of loading steps followed by relaxation steps at different strain levels were performed, in order to check the reproducibility for a given orientation. Moreover, the fiber orientation in the central part of the tensile samples was also analyzed with X-ray tomography. The results show that the mechanical behavior for each orientation (among 6) was rather reproducible, thus validating the cutting pattern.

Skin sterility after application of ethyl chloride spray.

PubMed

Polishchuk, Daniil; Gehrmann, Robin; Tan, Virak

2012-01-18

Ethyl chloride topical anesthetic spray is labeled as nonsterile, yet it is widely used during injection procedures performed in an outpatient setting. The purpose of this study was to investigate the sterility of ethyl chloride topical anesthetic spray applied before an injection. Our a priori hypothesis was that application of the spray after the skin has been prepared would not alter the sterility of the injection site. We conducted a prospective, blinded, controlled study to assess the effect of ethyl chloride spray on skin sterility. Fifteen healthy adult subjects (age, twenty-three to sixty-one years) were prepared for mock injections into both shoulders and both knees, although no injection was actually performed. Three culture samples were obtained from each site on the skin: one before skin preparation with isopropyl alcohol, one after skin preparation and before application of ethyl chloride, and one after ethyl chloride had been sprayed on the site. In addition, the sterility of the ethyl chloride was tested directly by inoculating cultures with spray from the bottles. Growth occurred in 70% of the samples obtained before skin preparation, 3% of the samples obtained after skin preparation but before application of ethyl chloride, and 5% of the samples obtained after the injection site had been sprayed with ethyl chloride. The percentage of positive cultures did not increase significantly after application of ethyl chloride (p = 0.65). Spraying of ethyl chloride directly on agar plates resulted in growth on 13% of these plates compared with 11% of the control plates; this difference was also not significant (p = 0.80). Although ethyl chloride spray is not sterile, its application did not alter the sterility of the injection sites in the shoulder and knee.

The effect of CNC and manual laser machining on electrical resistance of HDPE/MWCNT composite

NASA Astrophysics Data System (ADS)

Mohammadi, Fatemeh; Farshbaf Zinati, Reza; Fattahi, A. M.

2018-05-01

In this study, electrical conductivity of high-density polyethylene (HDPE)/multi-walled carbon nanotube (MWCNT) composite was investigated after laser machining. To this end, produced using plastic injection process, nano-composite samples were laser machined with various combinations of input parameters such as feed rate (35, 45, and 55 mm/min), feed angle with injection flow direction (0°, 45°, and 90°), and MWCNT content (0.5, 1, and 1.5 wt%). The angle between laser feed and injected flow direction was set via either of two different methods: CNC programming and manual setting. The results showed that the parameters of angle between laser line and melt flow direction and feed rate were both found to have statistically significance and physical impacts on electrical resistance of the samples in manual setting. Also, maximum conductivity was seen when the angle between laser line and melt flow direction was set to 90° in manual setting, and maximum conductivity was seen at feed rate of 55 mm/min in both of CNC programming and manual setting.

Fast batch injection analysis system for on-site determination of ethanol in gasohol and fuel ethanol.

PubMed

Pereira, Polyana F; Marra, Mariana C; Munoz, Rodrigo A A; Richter, Eduardo M

2012-02-15

A simple, accurate and fast (180 injections h(-1)) batch injection analysis (BIA) system with multiple-pulse amperometric detection has been developed for selective determination of ethanol in gasohol and fuel ethanol. A sample aliquot (100 μL) was directly injected onto a gold electrode immersed in 0.5 mol L(-1) NaOH solution (unique reagent). The proposed BIA method requires minimal sample manipulation and can be easily used for on-site analysis. The results obtained with the BIA method were compared to those obtained by gas-chromatography and similar results were obtained (at 95% of confidence level). Published by Elsevier B.V.

Gene delivery by direct injection (microinjection) using a controlled-flow system.

PubMed

Dean, David A

2006-12-01

INTRODUCTIONThis protocol describes a method for constant-flow microinjection using the Pneumatic PicoPump (World Precision Instruments). This type of system is very simple and can be assembled on a relatively low budget. In this method, a constant flow of sample is delivered from the tip of the pipette, and the amount of sample injected into the cell is determined by how long the pipette remains in the cell. A typical system is composed of a pressure regulator that can be adjusted for two pressures (back pressure and injection pressure), a capillary holder, and a coarse and fine micromanipulator.

40 CFR 147.3013 - Information to be considered for Class I wells.

Code of Federal Regulations, 2012 CFR

2012-07-01

... (CONTINUED) WATER PROGRAMS (CONTINUED) STATE, TRIBAL, AND EPA-ADMINISTERED UNDERGROUND INJECTION CONTROL... pressure changes, native fluid displacement, and direction of movement of the injected fluid; and (2) Methods to be used for sampling, and for measurement and calculation of flow. (b) In addition to the...

40 CFR 147.3013 - Information to be considered for Class I wells.

Code of Federal Regulations, 2013 CFR

2013-07-01

... (CONTINUED) WATER PROGRAMS (CONTINUED) STATE, TRIBAL, AND EPA-ADMINISTERED UNDERGROUND INJECTION CONTROL... pressure changes, native fluid displacement, and direction of movement of the injected fluid; and (2) Methods to be used for sampling, and for measurement and calculation of flow. (b) In addition to the...

40 CFR 147.3013 - Information to be considered for Class I wells.

Code of Federal Regulations, 2014 CFR

2014-07-01

... (CONTINUED) WATER PROGRAMS (CONTINUED) STATE, TRIBAL, AND EPA-ADMINISTERED UNDERGROUND INJECTION CONTROL... pressure changes, native fluid displacement, and direction of movement of the injected fluid; and (2) Methods to be used for sampling, and for measurement and calculation of flow. (b) In addition to the...

40 CFR 147.3013 - Information to be considered for Class I wells.

Code of Federal Regulations, 2011 CFR

2011-07-01

... (CONTINUED) WATER PROGRAMS (CONTINUED) STATE, TRIBAL, AND EPA-ADMINISTERED UNDERGROUND INJECTION CONTROL... pressure changes, native fluid displacement, and direction of movement of the injected fluid; and (2) Methods to be used for sampling, and for measurement and calculation of flow. (b) In addition to the...

Determination of benzylpenicillin in pharmaceuticals by capillary zone electrophoresis

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

Hoyt, A.M. Jr.; Sepaniak, M.J.

A rapid and direct method is described for the determination of benzylpenicillin (penicillin G) in pharmaceutical preparations. The method involves very little sample preparation and total analysis time for duplicate results is less 30 minutes per sample. The method takes advantage of the speed and separating power of capillary zone electrophoresis (CZE). Detection of penicillin is by absorption at 228 nm. An internal standard is employed to reduce sample injection error. The method was applied successfully to both tablets and injectable preparations. 14 refs., 5 figs., 3 tabs.

In vivo induction of interferon gamma expression in grey horses with metastatic melanoma resulting from direct injection of plasmid DNA coding for equine interleukin 12.

PubMed

Müller, J-M V; Wissemann, J; Meli, M L; Dasen, G; Lutz, H; Heinzerling, L; Feige, K

2011-11-01

Whole blood pharmacokinetics of intratumourally injected naked plasmid DNA coding for equine Interleukin 12 (IL-12) was assessed as a means of in vivo gene transfer in the treatment of melanoma in grey horses. The expression of induced interferon gamma (IFN-g) was evaluated in order to determine the pharmacodynamic properties of in vivo gene transduction. Seven grey horses bearing melanoma were injected intratumourally with 250 µg naked plasmid DNA coding for IL-12. Peripheral blood and biopsies from the injection site were taken at 13 time points until day 14 post injection (p.i.). Samples were analysed using quantitative real-time PCR. Plasmid DNA was quantified in blood samples and mRNA expression for IFN-g in tissue samples. Plasmid DNA showed fast elimination kinetics with more than 99 % of the plasmid disappearing within 36 hours. IFN-g expression increased quickly after IL-12 plasmid injection, but varied between individual horses. Intratumoural injection of plasmid DNA is a feasible method for inducing transgene expression in vivo. Biological activity of the transgene IL-12 was confirmed by measuring expression of IFN-g.

Determination of acrylamide in drinking water by large-volume direct injection and ion-exclusion chromatography-mass spectrometry.

PubMed

Cavalli, S; Polesello, S; Saccani, G

2004-06-11

Acrylamide, a known neurotoxin and putative human carcinogen, has been included among the substances to be monitored in drinking water according to the European Union Directive 98/83 on potable water. This paper reports a new method based on the combination of ion-exclusion chromatographic separation and MS detection. Samples of drinking water have been directly injected in the microbore ICE-AS1 column and detected in the selected-ion monitoring mode by a single quadrupole system with electrospray ionization. Chromatographic conditions, such as eluent composition and flow rate, have been optimized by a central composite design experiment. Statistical analysis of data showed that the amount of acetonitrile fraction in the eluent mixture, composed by acetonitrile and formic acid solution, is the variable that most influences retention of the acrylamide peak. After optimization of MS detection parameters, this method has been validated for spiked drinking water samples. The effect of large-volume injection (up to 500 microl) has been also explored. Linearity was evaluated from 0.5 to 5 microg l(-1). Repeatability, expressed as R.S.D., was 16 and 12% at 0.5 and 1 microg l(-1) respectively. The limit of detection was 0.20 ppb with 500 microl injection volume.

Micellar electrokinetic chromatography and capillary electrochromatography of nitroaromatic explosives in seawater.

PubMed

Giordano, Braden C; Copper, Christine L; Collins, Greg E

2006-02-01

The ability to separate nitroaromatic and nitramine explosives in seawater sample matrices is demonstrated using both MEKC and CEC. While several capillary-based separations exist for explosives, none address direct sampling from seawater, a sample matrix of particular interest in the detection of undersea mines. Direct comparisons are made between MEKC and CEC in terms of sensitivity and separation efficiency for the analysis of 14 explosives and explosive degradation products in seawater and diluted seawater. The use of high-salt stacking with MEKC results, on average, in a three-fold increase in the number of theoretical plates, and nearly double resolution for samples prepared in 25% seawater. By taking advantage of long injection times in conjunction with stacking, detection limits down to sub mg/L levels are attainable; however, resolution is sacrificed. CEC of explosive mixtures using sol-gels prepared from methyltrimethoxysilane does not perform as well as MEKC in terms of resolving power, but does permit extended injection times for concentrating analyte onto the head of the separation column with little or no subsequent loss in resolution. Electrokinetic injections of 8 min at high voltage allow for detection limits of explosives below 100 microg/L.

New Cost-Effective Method for Long-Term Groundwater Monitoring Programs

DTIC Science & Technology

2013-05-01

with a small-volume, gas -tight syringe (< 1 mL) and injected directly into the field-portable GC. Alternatively, the well headspace sample can be...according to manufacturers’ protocols. Isobutylene was used as the calibration standard for the PID. The standard gas mixtures were used for 3-point...monitoring wells are being evaluated: 1) direct headspace sampling, 2) sampling tube with gas permeable membrane, and 3) gas -filled passive vapor

Comprehensive evaluation of direct injection mass spectrometry for the quantitative profiling of volatiles in food samples

PubMed Central

2016-01-01

Although qualitative strategies based on direct injection mass spectrometry (DIMS) have recently emerged as an alternative for the rapid classification of food samples, the potential of these approaches in quantitative tasks has scarcely been addressed to date. In this paper, the applicability of different multivariate regression procedures to data collected by DIMS from simulated mixtures has been evaluated. The most relevant factors affecting quantitation, such as random noise, the number of calibration samples, type of validation, mixture complexity and similarity of mass spectra, were also considered and comprehensively discussed. Based on the conclusions drawn from simulated data, and as an example of application, experimental mass spectral fingerprints collected by direct thermal desorption coupled to mass spectrometry were used for the quantitation of major volatiles in Thymus zygis subsp. zygis chemotypes. The results obtained, validated with the direct thermal desorption coupled to gas chromatography–mass spectrometry method here used as a reference, show the potential of DIMS approaches for the fast and precise quantitative profiling of volatiles in foods. This article is part of the themed issue ‘Quantitative mass spectrometry’. PMID:27644978

Detection of recombinant EPO in blood and urine samples with EPO WGA MAIIA, IEF and SAR-PAGE after microdose injections.

PubMed

Dehnes, Yvette; Shalina, Alexandra; Myrvold, Linda

2013-01-01

The misuse of microdoses of performance enhancing drugs like erythropoietin (EPO) constitutes a major challenge in doping analysis. When injected intravenously, the half-life of recombinant human EPO (rhEPO) like epoetin alfa, beta, and zeta is only a few hours and hence, the window for direct detection of rhEPO in urine is small. In order to investigate the detection window for rhEPO directly in blood and urine with a combined affinity chromatography and lateral flow immunoassay (EPO WGA MAIIA), we recruited nine healthy people who each received six intravenously injected microdoses (7.5 IU/kg) of NeoRecormon (epoetin beta) over a period of three weeks. Blood and urine samples were collected in the days following the injections and analyzed with EPO WGA MAIIA as well as the current validated methods for rhEPO; isoelectric focusing (IEF) and sarcosyl polyacrylamide gel electrophoresis (SAR-PAGE). For samples collected 18 h after a microdose, the sensitivity of the EPO WGA MAIIA assay was 100% in plasma and 87.5% in urine samples at the respective 98% specificity threshold levels. In comparison, the sensitivity in plasma and urine was 75% and 100%, respectively, with IEF, and 87.5% in plasma and 100% in urine when analyzed with SAR-PAGE. We conclude that EPO WGA MAIIA is a sensitive assay for the detection of rhEPO, with the potential of being a fast, supplemental screening assay for use in doping analysis.

Application of direct-injection detector integrated with the multi-pumping flow system to chemiluminescence determination of the total polyphenol index.

PubMed

Nalewajko-Sieliwoniuk, Edyta; Iwanowicz, Magdalena; Kalinowski, Sławomir; Kojło, Anatol

2016-03-10

In this work, we present a novel chemiluminescence (CL) method based on direct-injection detector (DID) integrated with the multi-pumping flow system (MPFS) to chemiluminescence determination of the total polyphenol index. In this flow system, the sample and the reagents are injected directly into the cone-shaped detection cell placed in front of the photomultiplier window. Such construction of the detection chamber allows for fast measurement of the CL signal in stopped-flow conditions immediately after mixing the reagents. The proposed DID-CL-MPFS method is based on the chemiluminescence of nanocolloidal manganese(IV)-hexametaphosphate-ethanol system. The application of ethanol as a sensitizer, eliminated the use of carcinogenic formaldehyde. Under the optimized experimental conditions, the chemiluminescence intensities are proportional to the concentration of gallic acid in the range from 5 to 350 ng mL(-1). The DID-CL-MPFS method offers a number of advantages, including low limit of detection (0.80 ng mL(-1)), high precision (RSD = 3.3%) and high sample throughput (144 samples h(-1)) as well as low consumption of reagents, energy and low waste generation. The proposed method has been successfully applied to determine the total polyphenol index (expressed as gallic acid equivalent) in a variety of plant-derived food samples (wine, tea, coffee, fruit and vegetable juices, herbs, spices). Copyright © 2016 Elsevier B.V. All rights reserved.

Simultaneous enantioselective quantification of fluoxetine and norfluoxetine in human milk by direct sample injection using 2-dimensional liquid chromatography-tandem mass spectrometry.

PubMed

Alvim, Joel; Lopes, Bianca Rebelo; Cass, Quezia Bezerra

2016-06-17

A two-dimensional liquid chromatography system coupled to triple quadrupole tandem mass spectrometer (2D LC-MS/MS) was employed for the simultaneously quantification of fluoxetine (FLX) and norfluoxetine (NFLX) enantiomers in human milk by direct injection of samples. A restricted access media of bovine serum albumin octadecyl column (RAM-BSAC18) was used in the first dimension for the milk proteins depletion, while an antibiotic-based chiral column was used in the second dimension. The results herein described show good selectivity, extraction efficiency, accuracy, and precision with limits of quantification in the order of 7.5ngmL(-1)for the FLX enantiomers and 10.0ngmL(-1) for NFLX enantiomers. Furthermore, it represents a practical tool in terms of sustainability for the sample preparation of such a difficult matrix. Copyright © 2016 Elsevier B.V. All rights reserved.

Geohydrologic reconnaissance of drainage wells in Florida; an interim report

USGS Publications Warehouse

Kimrey, Joel O.; Fayard, Larry D.

1982-01-01

Drainage wells are used to inject surface waters directly into an aquifer, or shallow ground waters directly into a deeper aquifer, primarily by gravity. Such wells in Florida may be grouped into two broad types: (1) Surface-water injection wells, and (2) interaquifer connector wells. Surface-water injection wells are commonly used to supplement drainage for urban areas in karst terranes of central and north Florida. Data are available for 25 wells in the Ocala, Live Oak, and Orlando areas that allow comparison of the quality of water samples from these Floridan aquifer drainage wells with allowable contaminant levels. Comparison indicates that maximum contaminant levels for turbidity, color, and iron, manganese, and lead concentrations are equaled or exceeded in some drainage-well samples, and relatively high counts for coliform bacteria are present in most wells. Interaquifer connector wells are used in the phosphate mining areas of Polk and Hillsborough Counties, to drain mining operations and recharge the Floridan aquifer. Water-quality data available from 13 connector wells indicate that samples from most of these wells exceed standards values for iron concentration and turbidity. One well yielded a highly mineralized water, and samples from 6 of the other 12 wells exceed standards values for gross alpha concentrations. (USGS)

Method to make accurate concentration and isotopic measurements for small gas samples

NASA Astrophysics Data System (ADS)

Palmer, M. R.; Wahl, E.; Cunningham, K. L.

2013-12-01

Carbon isotopic ratio measurements of CO2 and CH4 provide valuable insight into carbon cycle processes. However, many of these studies, like soil gas, soil flux, and water head space experiments, provide very small gas sample volumes, too small for direct measurement by current constant-flow Cavity Ring-Down (CRDS) isotopic analyzers. Previously, we addressed this issue by developing a sample introduction module which enabled the isotopic ratio measurement of 40ml samples or smaller. However, the system, called the Small Sample Isotope Module (SSIM), does dilute the sample during the delivery with inert carrier gas which causes a ~5% reduction in concentration. The isotopic ratio measurements are not affected by this small dilution, but researchers are naturally interested accurate concentration measurements. We present the accuracy and precision of a new method of using this delivery module which we call 'double injection.' Two portions of the 40ml of the sample (20ml each) are introduced to the analyzer, the first injection of which flushes out the diluting gas and the second injection is measured. The accuracy of this new method is demonstrated by comparing the concentration and isotopic ratio measurements for a gas sampled directly and that same gas measured through the SSIM. The data show that the CO2 concentration measurements were the same within instrument precision. The isotopic ratio precision (1σ) of repeated measurements was 0.16 permil for CO2 and 1.15 permil for CH4 at ambient concentrations. This new method provides a significant enhancement in the information provided by small samples.

How Do Deep Saline Aquifer Microbial Communities Respond to Supercritical CO2 Injection?

NASA Astrophysics Data System (ADS)

Mu, A.; Billman-Jacobe, H.; Boreham, C.; Schacht, U.; Moreau, J. W.

2011-12-01

Carbon Capture and Storage (CCS) is currently seen as a viable strategy for mitigating anthropogenic carbon dioxide pollution. The Cooperative Research Centre for Greenhouse Gas Technologies (CO2CRC) is currently conducting a field experiment in the Otway Basin (Australia) studying residual gas saturation in the water-saturated reservoir of the Paaratte Formation. As part of this study, a suite of pre-CO2 injection water samples were collected from approximately 1400 meters depth (60°C, 13.8 MPa) via an in situ sampling system. The in situ sampling system isolates aquifer water from sources of contamination while maintaining the formation pressure. Whole community DNA was extracted from these samples to investigate the prokaryotic biodiversity of the saline Paaratte aquifer (EC = 1509.6 uS/cm). Bioinformatic analysis of preliminary 16S ribosomal gene data revealed Thermincola, Acinetobacter, Sphingobium, and Dechloromonas amongst the closest related genera to environmental clone sequences obtained from a subset of pre-CO2 injection groundwater samples. Epifluorescent microscopy with 4',6-diamidino-2-phenylindole (DAPI) highlighted an abundance of filamentous cells ranging from 5 to 45 μM. Efforts are currently directed towards utilising a high throughput sequencing approach to capture an exhaustive profile of the microbial diversity of the Paaratte aquifer CO2 injection site, and to understand better the response of in situ microbial populations to the injection of large volumes (e.g. many kilotonnes) of supercritical CO2 (sc-CO2). Sequencing results will be used to direct cultivation efforts towards enrichment of a CO2-tolerant microorganism. Understanding the microbial response to sc-CO2 is an integral aspect of carbon dioxide storage, for which very little information exists in the literature. This study aims to elucidate molecular mechanisms, through genomic and cultivation-based methods, for CO2 tolerance with the prospect of engineering biofilms to enhance trapping of CO2 in saline aquifers.

Optimizations of packed sorbent and inlet temperature for large volume-direct aqueous injection-gas chromatography to determine high boiling volatile organic compounds in water.

PubMed

Yu, Bofan; Song, Yonghui; Han, Lu; Yu, Huibin; Liu, Yang; Liu, Hongliang

2014-08-22

For the expanded application area, fast trace analysis of certain high boiling point (i.e., 150-250 °C) volatile organic compounds (HVOCs) in water, a large volume-direct aqueous injection-gas chromatography (LV-DAI-GC) method was optimized for the following parameters: packed sorbent for sample on-line pretreatment, inlet temperature and detectors configuration. Using the composite packed sorbent self-prepared with lithium chloride and a type of diatomite, the method enabled safe injection of an approximately 50-100 μL sample at an inlet temperature of 150 °C in the splitless mode and separated HVOCs from water matrix in 2 min. Coupled with a flame ionization detector (FID), an electron capture detector (ECD) and a flame photometric detector (FPD), the method could simultaneously quantify 27 HVOCs that belong to seven subclasses (i.e., halogenated aliphatic hydrocarbons, chlorobenzenes, nitrobenzenes, anilines, phenols, polycyclic aromatic hydrocarbons and organic sulfides) in 26 min. Injecting a 50 μL sample without any enrichment step, such as cryotrap focusing, the limits of quantification (LOQs) for the 27 HVOCs was 0.01-3 μg/L. Replicate analyses of the 27 HVOCs spiked source and river water samples exhibited good precision (relative standard deviations ≤ 11.3%) and accuracy (relative errors ≤ 17.6%). The optimized LV-DAI-GC was robust and applicable for fast determination and automated continuous monitoring of HVOCs in surface water. Copyright © 2014 Elsevier B.V. All rights reserved.

Time-domain measurement of terahertz frequency magnetoplasmon resonances in a two-dimensional electron system by the direct injection of picosecond pulsed currents

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

Wu, Jingbo; Mayorov, Alexander S.; Wood, Christopher D.

2016-02-29

We have investigated terahertz (THz) frequency magnetoplasmon resonances in a two-dimensional electron system through the direct injection of picosecond duration current pulses. The evolution of the time-domain signals was measured as a function of magnetic field, and the results were found to be in agreement with calculations using a mode-matching approach for four modes observed in the frequency range above 0.1 THz. This introduces a generic technique suitable for sampling ultrafast carrier dynamics in low-dimensional semiconductor nanostructures at THz frequencies.

Techniques for the inorganic analysis in a controlled ecological life support system

NASA Technical Reports Server (NTRS)

1983-01-01

Sample preparation, instrumental analysis, a direct injection device for IC/ICP interfacing, a hydraulic jet bend impaction device, monodisperse aerosol generator, and low gravity environments are discussed.

Combined Falling Drop/Open Port Sampling Interface System for Automated Flow Injection Mass Spectrometry

DOE PAGES

Van Berkel, Gary J.; Kertesz, Vilmos; Orcutt, Matt; ...

2017-11-07

The aim of this work was to demonstrate and to evaluate the analytical performance of a combined falling drop/open port sampling interface (OPSI) system as a simple noncontact, no-carryover, automated system for flow injection analysis with mass spectrometry. The falling sample drops were introduced into the OPSI using a widely available autosampler platform utilizing low cost disposable pipet tips and conventional disposable microtiter well plates. The volume of the drops that fell onto the OPSI was in the 7–15 μL range with an injected sample volume of several hundred nanoliters. Sample drop height, positioning of the internal capillary on themore » sampling end of the probe, and carrier solvent flow rate were optimized for maximum signal. Sample throughput, signal reproducibility, matrix effects, and quantitative analysis capability of the system were established using the drug molecule propranolol and its isotope labeled internal standard in water, unprocessed river water and two commercially available buffer matrices. A sample-to-sample throughput of ~45 s with a ~4.5 s base-to-base flow injection peak profile was obtained in these experiments. In addition, quantitation with minimally processed rat plasma samples was demonstrated with three different statin drugs (atorvastatin, rosuvastatin, and fluvastatin). Direct characterization capability of unprocessed samples was demonstrated by the analysis of neat vegetable oils. Employing the autosampler system for spatially resolved liquid extraction surface sampling exemplified by the analysis of propranolol and its hydroxypropranolol glucuronide phase II metabolites from a rat thin tissue section was also illustrated.« less

Combined Falling Drop/Open Port Sampling Interface System for Automated Flow Injection Mass Spectrometry

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

Van Berkel, Gary J.; Kertesz, Vilmos; Orcutt, Matt

The aim of this work was to demonstrate and to evaluate the analytical performance of a combined falling drop/open port sampling interface (OPSI) system as a simple noncontact, no-carryover, automated system for flow injection analysis with mass spectrometry. The falling sample drops were introduced into the OPSI using a widely available autosampler platform utilizing low cost disposable pipet tips and conventional disposable microtiter well plates. The volume of the drops that fell onto the OPSI was in the 7–15 μL range with an injected sample volume of several hundred nanoliters. Sample drop height, positioning of the internal capillary on themore » sampling end of the probe, and carrier solvent flow rate were optimized for maximum signal. Sample throughput, signal reproducibility, matrix effects, and quantitative analysis capability of the system were established using the drug molecule propranolol and its isotope labeled internal standard in water, unprocessed river water and two commercially available buffer matrices. A sample-to-sample throughput of ~45 s with a ~4.5 s base-to-base flow injection peak profile was obtained in these experiments. In addition, quantitation with minimally processed rat plasma samples was demonstrated with three different statin drugs (atorvastatin, rosuvastatin, and fluvastatin). Direct characterization capability of unprocessed samples was demonstrated by the analysis of neat vegetable oils. Employing the autosampler system for spatially resolved liquid extraction surface sampling exemplified by the analysis of propranolol and its hydroxypropranolol glucuronide phase II metabolites from a rat thin tissue section was also illustrated.« less

Direct-injection chemiluminescence detector. Properties and potential applications in flow analysis.

PubMed

Koronkiewicz, Stanislawa; Kalinowski, Slawomir

2015-02-01

We present a novel chemiluminescence detector, with a cone-shaped detection chamber where the analytical reaction takes place. The sample and appropriate reagents are injected directly into the chamber in countercurrent using solenoid-operated pulse micro-pumps. The proposed detector allows for fast measurement of the chemiluminescence signal in stop-flow conditions from the moment of reagents mixing. To evaluate potential applications of the detector the Fenton-like reaction with a luminol-H2O2 system and several transition metal ions (Co(2+), Cu(2+), Cr(3+), Fe(3+)) as a catalyst were investigated. The results demonstrate suitability of the proposed detector for quantitative analysis and for investigations of reaction kinetics, particularly rapid reactions. A multi-pumping flow system was designed and optimized. The developed methodology demonstrated that the shape of the analytical signals strongly depends on the type and concentration of the metal ions. The application of the detector in quantitative analysis was assessed for determination of Fe(III). The direct-injection chemiluminescence detector allows for a sensitive and repeatable (R.S.D. 2%) determination. The intensity of chemiluminescence increased linearly in the range from about 0.5 to 10 mg L(-1) Fe(III) with the detection limit of 0.025 mg L(-1). The time of analysis depended mainly on reaction kinetics. It is possible to achieve the high sampling rate of 144 samples per hour. Copyright © 2014 Elsevier B.V. All rights reserved.

Evaluation of a direct injection nebulizer interface for flow injection analysis and high performance liquid chromatography with inductively coupled plasma-atomic emission spectroscopic detection

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

LaFreniere, K.E.

A direct injection nebulizer (DIN) was designed, developed and evaluated to determine its potential utilization as an effective interface for flow injection analysis (FIA) and high performance liquid chromatography (HPLC) coupled with inductively coupled plasma-atomic emission spectroscopic detection. The analytical figures of merit for the DIN when used as an interface for FIA-ICP-AES were found to be comparable to or better than those obtained with conventional pneumatic nebulization in terms of limits of detection (LODs), reproducibility, linearity, and interelement effects. In the HPLC mode, the LODDs were found to be comparable to those obtained by continuous-flow sample introduction into themore » ICP, or inferior by up to only a factor of four. Stable plasma operation was maintained for the DIN sample introduction of a variety of pure organic solvents, including acetonitrile, methanol, methyl-isobutylketone, and pyridine. The HPLC-DIN-ICP-AES facility was specifically applied for the speciation of inorganic and organo-metallic species contained in synthetic mixtures, vanilla extracts and a variety of energy-related materials, such as shale oil process water, coal extracts, shale oil, crude oil, and an SRC II. Suggestions for future research are also considered.« less

Redesigning flow injection after 40 years of development: Flow programming.

PubMed

Ruzicka, Jaromir Jarda

2018-01-01

Automation of reagent based assays, by means of Flow Injection (FI), is based on sample processing, in which a sample flows continuously towards and through a detector for quantification of the target analyte. The Achilles heel of this methodology, the legacy of Auto Analyzer®, is continuous reagent consumption, and continuous generation of chemical waste. However, flow programming, assisted by recent advances in precise pumping, combined with the lab-on-valve technique, allows the FI manifold to be designed around a single confluence point through which sample and reagents are sequentially directed by means of a series of flow reversals. This approach results in sample/reagent mixing analogous to the traditional FI, reduces sample and reagent consumption, and uses the stop flow technique for enhancement of the yield of chemical reactions. The feasibility of programmable Flow Injection (pFI) is documented by example of commonly used spectrophotometric assays of, phosphate, nitrate, nitrite and glucose. Experimental details and additional information are available in online tutorial http://www.flowinjectiontutorial.com/. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of Flow-Injection Tandem Mass Spectrometry for Rapid and High-Throughput Quantitative Determination of B-Vitamins in Nutritional Supplements

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

Bhandari, Deepak; Van Berkel, Gary J

2012-01-01

The use of flow-injection electrospray ionization tandem mass spectrometry for rapid and high-throughput mass spectral analysis of selected B-vitamins, viz. B1, B2, B3, B5, and B6, in nutritional formulations was demonstrated. A simple and rapid (~5 min) in-tube sample preparation was performed by adding extraction solvent to a powdered sample aliquot followed by agitation, centrifugation, and filtration to recover an extract for analysis. Automated flow injection introduced 1 L of the extracts directly into the mass spectrometer ion source without chromatographic separation. Sample-to-sample analysis time was 60 s representing significant improvement over conventional liquid chromatography approaches which typically require 25-45more » min, and often require more significant sample preparation procedures. Quantitative capabilities of the flow-injection analysis were tested using the method of standard additions and NIST standard reference material (SRM 3280) multivitamin/multielement tablets. The quantity determined for each B-vitamin in SRM 3280 was within the statistical range provided for the respective certified values. The same sample preparation and analysis approach was also applied to two different commercial vitamin supplement tablets and proved to be successful in the quantification of the selected B-vitamins as evidenced by an agreement with the labels values and the results obtained using isotope dilution liquid chromatography/mass spectrometry.« less

Capabilities of Direct Sample Introduction - Comprehensive Two-Dimensional Gas Chromatgraphy-Time-of-Flight Mass Spectrometry to Analyze Organic Chemicals of Interest in Fish Oils

USDA-ARS?s Scientific Manuscript database

Most analytical methods for persistent organic pollutants (POPs) focus on targeted analytes. Therefore, analysis of multiple classes of POPs typically entails several sample preparations, fractionations, and injections, whereas other chemicals of possible interest are neglected. To analyze a wider...

Mass discharge in a tracer plume: Evaluation of the Theissen Polygon Method

PubMed Central

Mackay, Douglas M.; Einarson, Murray D.; Kaiser, Phil M.; Nozawa-Inoue, Mamie; Goyal, Sham; Chakraborty, Irina; Rasa, Ehsan; Scow, Kate M.

2013-01-01

A tracer plume was created within a thin aquifer by injection for 299 days of two adjacent “sub-plumes” to represent one type of plume heterogeneity encountered in practice. The plume was monitored by snapshot sampling of transects of fully screened wells. The mass injection rate and total mass injected were known. Using all wells in each transect (0.77 m well spacing, 1.4 points/m2 sampling density), the Theissen Polygon Method (TPM) yielded apparently accurate mass discharge (Md) estimates at 3 transects for 12 snapshots. When applied to hypothetical sparser transects using subsets of the wells with average spacing and sampling density from 1.55 to 5.39 m and 0.70 to 0.20 points/m2, respectively, the TPM accuracy depended on well spacing and location of the wells in the hypothesized transect with respect to the sub-plumes. Potential error was relatively low when the well spacing was less than the widths of the sub-plumes (> 0.35 points/m2). Potential error increased for well spacing similar to or greater than the sub-plume widths, or when less than 1% of the plume area was sampled. For low density sampling of laterally heterogeneous plumes, small changes in groundwater flow direction can lead to wide fluctuations in Md estimates by the TPM. However, sampling conducted when flow is known or likely to be in a preferred direction can potentially allow more useful comparisons of Md over multiyear time frames, such as required for performance evaluation of natural attenuation or engineered remediation systems. PMID:22324777

Soft Ionization of Saturated Hydrocarbons, Alcohols and Nonpolar Compounds by Negative-Ion Direct Analysis in Real-Time Mass Spectrometry

NASA Astrophysics Data System (ADS)

Cody, Robert B.; Dane, A. John

2013-03-01

Large polarizable n-alkanes (approximately C18 and larger), alcohols, and other nonpolar compounds can be detected as negative ions when sample solutions are injected directly into the sampling orifice of the atmospheric pressure interface of the time-of-flight mass spectrometer with the direct analysis in real time (DART) ion source operating in negative-ion mode. The mass spectra are dominated by peaks corresponding to [M + O2]‾•. No fragmentation is observed, making this a very soft ionization technique for samples that are otherwise difficult to analyze by DART. Detection limits for cholesterol were determined to be in the low nanogram range.

Soft ionization of saturated hydrocarbons, alcohols and nonpolar compounds by negative-ion direct analysis in real-time mass spectrometry.

PubMed

Cody, Robert B; Dane, A John

2013-03-01

Large polarizable n-alkanes (approximately C18 and larger), alcohols, and other nonpolar compounds can be detected as negative ions when sample solutions are injected directly into the sampling orifice of the atmospheric pressure interface of the time-of-flight mass spectrometer with the direct analysis in real time (DART) ion source operating in negative-ion mode. The mass spectra are dominated by peaks corresponding to [M + O2]‾(•). No fragmentation is observed, making this a very soft ionization technique for samples that are otherwise difficult to analyze by DART. Detection limits for cholesterol were determined to be in the low nanogram range.

Applicability of the direct injection liquid chromatographic tandem mass spectrometric analytical approach to the sub-ngL-1 determination of perfluoro-alkyl acids in waste, surface, ground and drinking water samples.

PubMed

Ciofi, Lorenzo; Renai, Lapo; Rossini, Daniele; Ancillotti, Claudia; Falai, Alida; Fibbi, Donatella; Bruzzoniti, Maria Concetta; Santana-Rodriguez, José Juan; Orlandini, Serena; Del Bubba, Massimo

2018-01-01

The applicability of a direct injection UHPLC-MS/MS method for the analysis of several perfluoroalkyl acids (PFAAs) in a wide range of water matrices was investigated. The method is based on the direct injection of 100µL of centrifuged water sample, without any other sample treatment. Very good method detection limits (0.014-0.44ngL -1 ) and excellent intra and inter-day precision (RSD% values in the range 1.8-4.4% and 2.7-5.7%, respectively) were achieved, with a total analysis time of 20min per sample. A high number of samples - i.e. 8 drinking waters (DW), 12 ground waters (GW), 13 surface waters (SW), 8 influents and 11 effluents of wastewater treatment plants (WWTP IN and WWTP OUT ) were processed and the extent of matrix effect (ME) was calculated, highlighting the strong prevalence of |ME| < 20%. The occurrence of |ME| > 50% was occasionally observed only for perfluorooctanesulphonic and perfluorodecanoic acids. Linear discriminant analysis highlighted the great contribution of the sample origin (i.e. DW, GW, SW, WWTP IN and WWTP OUT ) to the ME. Partial least square regression (PLS) and leave-one-out cross-validation were performed in order to interpret and predict the signal suppression or enhancement phenomena as a function of physicochemical parameters of water samples (i.e. conductivity, hardness and chemical oxygen demand) and background chromatographic area. The PLS approach resulted only in an approximate screening, due to the low prediction power of the PLS models. However, for most analytes in most samples, the fitted and cross-validated values were such as to correctly distinguish between | ME | higher than 20% or below this limit. PFAAs in the aforementioned water samples were quantified by means of the standard addition method, highlighting their occurrence mainly in WWTP influents and effluents, at concentrations as high as one hundred of µgL -1 . Copyright © 2017 Elsevier B.V. All rights reserved.

Comparative studies on the performance and emissions of a direct injection diesel engine fueled with neem oil and pumpkin seed oil biodiesel with and without fuel preheater.

PubMed

Ramakrishnan, Muneeswaran; Rathinam, Thansekhar Maruthu; Viswanathan, Karthickeyan

2018-02-01

In the present experimental analysis, two non-edible oils namely neem oil and pumpkin seed oil were considered. They are converted into respective biodiesels namely neem oil methyl ester (B1) and pumpkin seed oil methyl ester (B2) through transesterification process and their physical and chemical properties were examined using ASTM standards. Diesel was used as a baseline fuel in Kirloskar TV1 model direct injection four stroke diesel engine. A fuel preheater was designed and fabricated to operate at various temperatures (60, 70, and 80 °C). Diesel showed higher brake thermal efficiency (BTE) than biodiesel samples. Lower brake specific fuel consumption (BSFC) was obtained with diesel than B1 sample. B1 exhibited lower BSFC than B2 sample without preheating process. High preheating temperature (80 °C) results in lower fuel consumption for B1 sample. The engine emission characteristics like carbon monoxide (CO), hydrocarbon (HC), and smoke were found lower with B1 sample than diesel and B2 except oxides of nitrogen (NOx) emission. In preheating of fuel, B1 sample with high preheating temperature showed lower CO, HC, and smoke emission (except NOx) than B2 sample.

Large-volume injection of sample diluents not miscible with the mobile phase as an alternative approach in sample preparation for bioanalysis: an application for fenspiride bioequivalence.

PubMed

Medvedovici, Andrei; Udrescu, Stefan; Albu, Florin; Tache, Florentin; David, Victor

2011-09-01

Liquid-liquid extraction of target compounds from biological matrices followed by the injection of a large volume from the organic layer into the chromatographic column operated under reversed-phase (RP) conditions would successfully combine the selectivity and the straightforward character of the procedure in order to enhance sensitivity, compared with the usual approach of involving solvent evaporation and residue re-dissolution. Large-volume injection of samples in diluents that are not miscible with the mobile phase was recently introduced in chromatographic practice. The risk of random errors produced during the manipulation of samples is also substantially reduced. A bioanalytical method designed for the bioequivalence of fenspiride containing pharmaceutical formulations was based on a sample preparation procedure involving extraction of the target analyte and the internal standard (trimetazidine) from alkalinized plasma samples in 1-octanol. A volume of 75 µl from the octanol layer was directly injected on a Zorbax SB C18 Rapid Resolution, 50 mm length × 4.6 mm internal diameter × 1.8 µm particle size column, with the RP separation being carried out under gradient elution conditions. Detection was made through positive ESI and MS/MS. Aspects related to method development and validation are discussed. The bioanalytical method was successfully applied to assess bioequivalence of a modified release pharmaceutical formulation containing 80 mg fenspiride hydrochloride during two different studies carried out as single-dose administration under fasting and fed conditions (four arms), and multiple doses administration, respectively. The quality attributes assigned to the bioanalytical method, as resulting from its application to the bioequivalence studies, are highlighted and fully demonstrate that sample preparation based on large-volume injection of immiscible diluents has an increased potential for application in bioanalysis.

Validated ¹H and 13C Nuclear Magnetic Resonance Methods for the Quantitative Determination of Glycerol in Drug Injections.

PubMed

Lu, Jiaxi; Wang, Pengli; Wang, Qiuying; Wang, Yanan; Jiang, Miaomiao

2018-05-15

In the current study, we employed high-resolution proton and carbon nuclear magnetic resonance spectroscopy (¹H and 13 C NMR) for quantitative analysis of glycerol in drug injections without any complex pre-treatment or derivatization on samples. The established methods were validated with good specificity, linearity, accuracy, precision, stability, and repeatability. Our results revealed that the contents of glycerol were convenient to calculate directly via the integration ratios of peak areas with an internal standard in ¹H NMR spectra, while the integration of peak heights were proper for 13 C NMR in combination with an external calibration of glycerol. The developed methods were both successfully applied in drug injections. Quantitative NMR methods showed an extensive prospect for glycerol determination in various liquid samples.

A timed solenoid injector for flow analysis.

PubMed

Rothwell, S D; Woolf, A A

1985-05-01

Samples can be reproducibly injected into flow-streams by timed switching of a sample stream with a miniature solenoid valve and timer circuit. The device is simpler to assemble and use than the standard rotary valve and a direct comparison under the same operating conditions shows that the solenoid valve is an adequate replacement for the rotary valve.

Determination of mercury in agroindustrial samples by flow-injection cold vapor atomic absorption spectrometry using ion exchange and reductive elution.

PubMed

Gomes Neto, J A; Zara, L F; Rocha, J C; Santos, A; Dakuzaku, C S; Nóbrega, J A

2000-03-06

A flow-injection system with a Chelite-S(R) cationic resin packed minicolumn is proposed for the determination of trace levels of mercury in agroindustrial samples by cold vapor atomic absorption spectrometry. Improved sensitivity and selectivity are attained since mercuric ions are on-line concentrated whereas other potential interferents are discarded. With on-line reductive elution procedure, concentrated hydrochloric acid could be replaced by 10% w/v SnCl(2), in 6 M HCl as eluent. The reversed-intermittent stream either carries the atomic mercury to the flow cell in the forward direction or removes the residue from reactor/gas-liquid separator to a discarding flask in the opposite direction. Concentration and volume of reagent, acidity, flow rates, commutation times and potential interfering species were investigated. For 120 s preconcentration time, the proposed system handles about 25 samples h(-1) (50.0-500 ng l(-1)), consuming about 10 ml sample and 5 mg SnCl(2) per determination. The detection limit is 0.8 ng l(-1) and the relative standard deviation (RSD) (n=12) of a 76.7 ng l(-1) sample is about 5%. Results are in agreement with certified value of standard materials at 95% confidence level and good recoveries (97-128%) of spiked samples were found.

Automation of flow injection gas diffusion-ion chromatography for the nanomolar determination of methylamines and ammonia in seawater and atmospheric samples

PubMed Central

Gibb, Stuart W.; Wood, John W.; Fauzi, R.; Mantoura, C.

1995-01-01

The automation and improved design and performance of Flow Injection Gas Diffusion-Ion Chromatography (FIGD-IC), a novel technique for the simultaneous analysis of trace ammonia (NH3) and methylamines (MAs) in aqueous media, is presented. Automated Flow Injection Gas Diffusion (FIGD) promotes the selective transmembrane diffusion of MAs and NH3 from aqueous sample under strongly alkaline (pH > 12, NaOH), chelated (EDTA) conditions into a recycled acidic acceptor stream. The acceptor is then injected onto an ion chromatograph where NH3 and the MAs are fully resolved as their cations and detected conductimetrically. A versatile PC interfaced control unit and data capture unit (DCU) are employed in series to direct the selonoid valve switching sequence, IC operation and collection of data. Automation, together with other modifications improved both linearily (R2 > 0.99 MAs 0-100 nM, NH3 0-1000 nM) and precision (<8%) of FIGD-IC at nanomolar concentrations, compared with the manual procedure. The system was successfully applied to the determination of MAs and NH3 in seawater and in trapped particulate and gaseous atmospheric samples during an oceanographic research cruise. PMID:18925047

Simultaneous determination of fluoroquinolones in environmental water by liquid chromatography-tandem mass spectrometry with direct injection: A green approach.

PubMed

Denadai, Marina; Cass, Quezia Bezerra

2015-10-30

This work describes an on-line multi-residue method for simultaneous quantification of ciprofloxacin, enrofloxacin, gemifloxacin, moxifloxacin, norfloxacin and ofloxacin in superficial and wastewater samples. For that, an octyl restricted-access media bovine serum albumin column (RAM-BSA C8) was used for sample clean-up, enrichment and analysis with quantitation carried out by tandem mass spectrometry. For water samples volumes of only 500μL the method provided good selectivity, extraction efficiency, accuracy, and precision with quantification limits in the order of 20-150ngL(-1). Out of the six fluoroquinolones only ciprofloxacin (195ngL(-1)) and norfloxacin (270ngL(-1)) were quantified in an influent sample of the wastewater treatment plant (WWTP) of São Carlos (SP, Brazil). None were found in the superficial water samples analyzed. The capability of injecting native sample in an automated mode provides high productivity and represents a greener approach in environmental sample analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

Rapid and direct determination of glyphosate, glufosinate, and aminophosphonic acid by online preconcentration CE with contactless conductivity detection.

PubMed

See, Hong Heng; Hauser, Peter C; Ibrahim, Wan Aini Wan; Sanagi, Mohd Marsin

2010-01-01

Rapid and direct online preconcentration followed by CE with capacitively coupled contactless conductivity detection (CE-C(4)D) is evaluated as a new approach for the determination of glyphosate, glufosinate (GLUF), and aminophosphonic acid (AMPA) in drinking water. Two online preconcentration techniques, namely large volume sample stacking without polarity switching and field-enhanced sample injection, coupled with CE-C(4)D were successfully developed and optimized. Under optimized conditions, LODs in the range of 0.01-0.1 microM (1.7-11.1 microg/L) and sensitivity enhancements of 48- to 53-fold were achieved with the large volume sample stacking-CE-C(4)D method. By performing the field-enhanced sample injection-CE-C(4)D procedure, excellent LODs down to 0.0005-0.02 microM (0.1-2.2 microg/L) as well as sensitivity enhancements of up to 245- to 1002-fold were obtained. Both techniques showed satisfactory reproducibility with RSDs of peak height of better than 10%. The newly established approaches were successfully applied to the analysis of glyphosate, glufosinate, and aminophosphonic acid in spiked tap drinking water.

Intracerebral Injections and Ultrastructural Analysis of High-Pressure Frozen Brain Tissue.

PubMed

Weil, Marie-Theres; Ruhwedel, Torben; Möbius, Wiebke; Simons, Mikael

2017-01-03

Intracerebral injections are an invasive method to bypass the blood brain barrier and are widely used to study molecular and cellular mechanisms of the central nervous system. The administered substances are injected directly at the site of interest, executing their effect locally. By combining injections in the rat brain with state-of-the-art electron microscopy, subtle changes in ultrastructure of the nervous tissue can be detected prior to overt damage or disease. The protocol presented here involves stereotactic injection into the corpus callosum of Lewis rats and the cryopreparation of freshly dissected tissue for electron microscopy. The localization of the injection site in tissue sections during the sample preparation for transmission electron microscopy is explained and possible artifacts of the method are indicated. With the help of this powerful combination of injections and electron microscopy, subtle effects of the applied substances on the biology of neural cells can be identified and monitored over time. © 2017 by John Wiley & Sons, Inc. Copyright © 2017 John Wiley & Sons, Inc.

T-load microchannel array and fabrication method

DOEpatents

Swierkowski, Stefan P.

2000-01-01

A three-dimensional (3-D) T-load for planar microchannel arrays for electrophoresis, for example, which enables sample injection directly onto a plane perpendicular to the microchannels' axis, at their ends. This is accomplished by forming input wells that extend beyond the ends of the microchannel thereby eliminating the right angle connection from the input well into the end of the microchannel. In addition, the T-load input well eases the placement of electrode in or adjacent the well and thus enables very efficient reproducible electrokinetic (ek) injection. The T-load input well eliminates the prior input well/microchannel alignment concerns, since the input well can be drilled after the top and bottom microchannel plates are bonded together. The T-load input well may extend partially or entirely through the bottom microchannel plate which enables more efficient gel and solution flushing, and also enables placement of multiple electrodes to assist in the ek sample injection.

Accuracy of MRI-compatible contrast media injectors.

PubMed

Saake, M; Wuest, W; Becker, S; Uder, M; Janka, R

2014-03-01

To analyze the exactness of MRI-compatible contrast media (CM) injectors in an experimental setup and clinical use. Ejected fluid volumes and amounts of CM were quantified for single and double piston injections. The focus was on small volumes, as used in pediatric examination and test-bolus measurements. Samples were collected before and after clinical MRI scans and amounts of CM were measured. For single piston injections the volume differences were minimal (mean difference 0.01  ml). For double piston injections the volume of the first injection was decreased (mean 20.74  ml, target 21.00  ml, p < 0.01). After a position change of the Y-piece of the injection system, the amount of CM differed significantly from the target value (mean 1.23  mmol and 0.83  mmol at 1  ml/s flow rate, target 1.00  mmol, p < 0.01), independently of the wait time. The clinical samples confirmed these findings. The pistons of modern CM injectors work exactly. However, for small CM volumes the injected amount of CM can differ significantly from the target value in both directions. Influence factors are an incomplete elimination of air and exchange processes between the CM and saline chaser in the injection system. • In MRI examinations of children and test-bolus measurements, small amounts of CM are used. • The accuracy of single piston injections is high. • In double piston injections the injected amount of CM can differ significantly from the target value. © Georg Thieme Verlag KG Stuttgart · New York.

A method for the direct injection and analysis of small volume human blood spots and plasma extracts containing high concentrations of organic solvents using revered-phase 2D UPLC/MS.

PubMed

Rainville, Paul D; Simeone, Jennifer L; Root, Dan S; Mallet, Claude R; Wilson, Ian D; Plumb, Robert S

2015-03-21

The emergence of micro sampling techniques holds great potential to improve pharmacokinetic data quality, reduce animal usage, and save costs in safety assessment studies. The analysis of these samples presents new challenges for bioanalytical scientists, both in terms of sample processing and analytical sensitivity. The use of two dimensional LC/MS with, at-column-dilution for the direct analysis of highly organic extracts prepared from biological fluids such as dried blood spots and plasma is demonstrated. This technique negated the need to dry down and reconstitute, or dilute samples with water/aqueous buffer solutions, prior to injection onto a reversed-phase LC system. A mixture of model drugs, including bromhexine, triprolidine, enrofloxacin, and procaine were used to test the feasibility of the method. Finally an LC/MS assay for the probe pharmaceutical rosuvastatin was developed from dried blood spots and protein-precipitated plasma. The assays showed acceptable recovery, accuracy and precision according to US FDA guidelines. The resulting analytical method showed an increase in assay sensitivity of up to forty fold as compared to conventional methods by maximizing the amount loaded onto the system and the MS response for the probe pharmaceutical rosuvastatin from small volume samples.

Evaluation of a direct injection nebulizer interface for flow injection analysis and high performance liquid chromatography with inductively coupled plasma-atomic emission spectroscopic detection

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

LaFreniere, K.E.

A direct injection nebulizer (DIN) was designed, developed, and evaluated to determine its potential utilization as an effective interface for flow injection analysis (FIA) and high performance liquid chromatography (HPLC) coupled with inductively coupled plasma-atomic emission spectroscopic detection. The analytical figures of merit for the DIN when used as an interface for FIA-ICP-AES were found to be comparable to or better than those obtained with conventional pneumatic nebulization in terms of limits of detection (LODs), reproducibility, linearity, and interelement effects. Stable plasma operation was maintained for the DIN sample introduction of a variety of pure organic solvents, including acetonitrile, methanol,more » methylisobutylketone, and pyridine. The HPLC-DIN-ICP-AES facility was specifically applied for the speciation of inorganic and organometallic species contained in synthetic mixtures, vanilla extracts, and a variety of energy-related materials, such as shale oil process water, coal extracts, shale oil, crude oil, and an SRC II. Suggestions for future research are also considered. 227 refs., 44 figs., 15 tabs.« less

Analytical instrument with apparatus and method for sample concentrating

DOEpatents

Zaromb, S.

1986-08-04

A system for analysis of trace concentrations of contaminants in air includes a portable liquid chromatograph and a preconcentrator for the contaminants to be analyzed. The preconcentrator includes a sample bag having an inlet valve and an outlet valve for collecting an air sample. When the sample is collected the sample bag is connected in series with a sorbing apparatus in a recirculation loop. The sorbing apparatus has an inner gas-permeable container containing a sorbent material and an outer gas-impermeable container. The sample is circulated through the outer container and around the inner container for trapping and preconcentrating the contaminants in the sorbent material. The sorbent material may be a liquid having the same composition as the mobile phase of the chromatograph for direct injection thereinto. Alternatively, the sorbent material may be a porous, solid body, to which mobile phase liquid is added after preconcentration of the contaminants for dissolving the contaminants, the liquid solution then being withdrawn for injection into the chromatograph.

Analytical instrument with apparatus for sample concentrating

DOEpatents

Zaromb, Solomon

1989-01-01

A system for analysis of trace concentrations of contaminants in air includes a portable liquid chromatograph and a preconcentrator for the contaminants to be analyzed. The preconcentrator includes a sample bag having an inlet valve and an outlet valve for collecting an air sample. When the sample is collected the sample bag is connected in series with a sorbing apparatus in a recirculation loop. The sorbing apparatus has an inner gas-permeable container containing a sorbent material and an outer gas-impermeable container. The sample is circulated through the outer container and around the inner container for trapping and preconcentrating the contaminants in the sorbent material. The sorbent material may be a liquid having the same composition as the mobile phase of the chromatograph for direct injection thereinto. Alternatively, the sorbent material may be a porous, solid body, to which mobile phase liquid is added after preconcentration of the contaminants for dissolving the contaminants, the liquid solution then being withdrawn for injection into the chromatograph.

Method for preconcentrating a sample for subsequent analysis

DOEpatents

Zaromb, Solomon

1990-01-01

A system for analysis of trace concentration of contaminants in air includes a portable liquid chromatograph and a preconcentrator for the contaminants to be analyzed. The preconcentrator includes a sample bag having an inlet valve and an outlet valve for collecting an air sample. When the sample is collected the sample bag is connected in series with a sorbing apparatus in a recirculation loop. The sorbing apparatus has an inner gas-permeable container containing a sorbent material and an outer gas-impermeable container. The sample is circulated through the outer container and around the inner container for trapping and preconcentrating the contaminants in the sorbent material. The sorbent material may be a liquid having the same composition as the mobile phase of the chromatograph for direct injection thereinto. Alternatively, the sorbent material may be a porous, solid body, to which mobile phase liquid is added after preconcentration of the contaminants for dissolving the contaminants, the liquid solution then being withdrawn for injection into the chromatograph.

Simulation of a Single-Element Lean-Direct Injection Combustor Using Arbitrary Polyhedral Mesh

NASA Technical Reports Server (NTRS)

Wey, Thomas; Liu, Nan-Suey

2012-01-01

This paper summarizes procedures of generating the arbitrary polyhedral mesh as well as presents sample results from its application to the numerical solution of a single-element LDI combustor using a preliminary version of the new OpenNCC.

Mapping of local argon impingement on a virtual surface: an insight for gas injection during FEBID

NASA Astrophysics Data System (ADS)

Wanzenboeck, H. D.; Hochleitner, G.; Mika, J.; Shawrav, M. M.; Gavagnin, M.; Bertagnolli, E.

2014-12-01

During the last decades, focused electron beam induced deposition (FEBID) has become a successful approach for direct-write fabrication of nanodevices. Such a deposition technique relies on the precursor supply to the sample surface which is typically accomplished by a gas injection system using a tube-shaped injector nozzle. This precursor injection strategy implies a position-dependent concentration gradient on the surface, which affects the geometry and chemistry of the final nanodeposit. Although simulations already proposed the local distribution of nozzle-borne gas molecules impinging on the surface, this isolated step in the FEBID process has never been experimentally measured yet. This work experimentally investigates the local distribution of impinging gas molecules on the sample plane, isolating the direct impingement component from surface diffusion or precursor depletion by deposition. The experimental setup used in this work maps and quantifies the local impinging rate of argon gas over the sample plane. This setup simulates the identical conditions for a precursor molecule during FEBID. Argon gas was locally collected with a sniffer tube, which is directly connected to a residual gas analyzer for quantification. The measured distribution of impinging gas molecules showed a strong position dependence. Indeed, a 300-µm shift of the deposition area to a position further away from the impingement center spot resulted in a 50 % decrease in the precursor impinging rate on the surface area. With the same parameters, the precursor distribution was also simulated by a Monte Carlo software by Friedli and Utke and showed a good correlation between the empirical and the simulated precursor distribution. The results hereby presented underline the importance of controlling the local precursor flux conditions in order to obtain reproducible and comparable deposition results in FEBID.

THE DETERMINATION OF MERCURY SPECIES AND MULTIPLE METALS IN COAL COMBUSTION EMISSIONS USING IODINE-BASED IMPINGERS AND DIRECT INJECTION NEBULIZATION - INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY ANALYSIS

EPA Science Inventory

Mercury (Hg) emissions from coal utilities are difficult to control. Hg eludes capture by most air pollution control devices (APCDs). To determine the gaseous Hg species in stack gases, U.S. EPA Method 5 type sampling is used. In this type of sampling a hole is drilled into th...

Flow injection gas chromatography with sulfur chemiluminescence detection for the analysis of total sulfur in complex hydrocarbon matrixes.

PubMed

Hua, Yujuan; Hawryluk, Myron; Gras, Ronda; Shearer, Randall; Luong, Jim

2018-01-01

A fast and reliable analytical technique for the determination of total sulfur levels in complex hydrocarbon matrices is introduced. The method employed flow injection technique using a gas chromatograph as a sample introduction device and a gas phase dual-plasma sulfur chemiluminescence detector for sulfur quantification. Using the technique described, total sulfur measurement in challenging hydrocarbon matrices can be achieved in less than 10 s with sample-to-sample time <2 min. The high degree of selectivity and sensitivity toward sulfur compounds of the detector offers the ability to measure low sulfur levels with a detection limit in the range of 20 ppb w/w S. The equimolar response characteristic of the detector allows the quantitation of unknown sulfur compounds and simplifies the calibration process. Response is linear over a concentration range of five orders of magnitude, with a high degree of repeatability. The detector's lack of response to hydrocarbons enables direct analysis without the need for time-consuming sample preparation and chromatographic separation processes. This flow injection-based sulfur chemiluminescence detection technique is ideal for fast analysis or trace sulfur analysis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microfluidic system for the identification of bacterial pathogens causing urinary tract infections

NASA Astrophysics Data System (ADS)

Becker, Holger; Hlawatsch, Nadine; Haraldsson, Tommy; van der Wijngaart, Wouter; Lind, Anders; Malhotra-Kumar, Surbi; Turlej-Rogacka, Agata; Goossens, Herman

2015-03-01

Urinary tract infections (UTIs) are among the most common bacterial infections and pose a significant healthcare burden. The growing trend in antibiotic resistance makes it mandatory to develop diagnostic kits which allow not only the determination of a pathogen but also the antibiotic resistances. We have developed a microfluidic cartridge which takes a direct urine sample, extracts the DNA, performs an amplification using batch-PCR and flows the sample over a microarray which is printed into a microchannel for fluorescence detection. The cartridge is injection-molded out of COP and contains a set of two-component injection-molded rotary valves to switch between input and to isolate the PCR chamber during thermocycling. The hybridization probes were spotted directly onto a functionalized section of the outlet microchannel. We have been able to successfully perform PCR of E.coli in urine in this chip and perform a fluorescence detection of PCR products. An upgraded design of the cartridge contains the buffers and reagents in blisters stored on the chip.

Microfluidic direct injection method for analysis of urinary 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) using molecularly imprinted polymers coupled on-line with LC-MS/MS.

PubMed

Shah, Kumar A; Peoples, Michael C; Halquist, Matthew S; Rutan, Sarah C; Karnes, H Thomas

2011-01-25

The work described in this paper involves development of a high-throughput on-line microfluidic sample extraction method using capillary micro-columns packed with MIP beads coupled with tandem mass spectrometry for the analysis of urinary NNAL. The method was optimized and matrix effects were evaluated and resolved. The method enabled low sample volume (200 μL) and rapid analysis of urinary NNAL by direct injection onto the microfluidic column packed with molecularly imprinted beads engineered to NNAL. The method was validated according to the FDA bioanalytical method validation guidance. The dynamic range extended from 20.0 to 2500.0 pg/mL with a percent relative error of ±5.9% and a run time of 7.00 min. The lower limit of quantitation was 20.0 pg/mL. The method was used for the analysis of NNAL and NNAL-Gluc concentrations in smokers' urine. Copyright © 2010 Elsevier B.V. All rights reserved.

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

PubMed

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

2015-08-21

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

Rapid determination of piracetam in human plasma and cerebrospinal fluid by micellar electrokinetic chromatography with sample direct injection.

PubMed

Yeh, Hsin-Hua; Yang, Yuan-Han; Ko, Ju-Yun; Chen, Su-Hwei

2006-07-07

A simple micellar electrokinetic chromatography (MEKC) method with UV detection at 200 nm for analysis of piracetam in plasma and in cerebrospinal fluid (CSF) by direct injection without any sample pretreatment is described. The separation of piracetam from biological matrix was performed at 25 degrees C using a background electrolyte consisting of Tris buffer with sodium dodecyl sulfate (SDS) as the electrolyte solution. Several parameters affecting the separation of the drug from biological matrix were studied, including the pH and concentrations of the Tris buffer and SDS. Under optimal MEKC condition, good separation with high efficiency and short analyses time is achieved. Using imidazole as an internal standard (IS), the linear ranges of the method for the determination of piracetam in plasma and in CSF were all between 5 and 500 microg/mL; the detection limit of the drug in plasma and in CSF (signal-to-noise ratio=3; injection 0.5 psi, 5s) was 1.0 microg/mL. The applicability of the proposed method for determination of piracetam in plasma and CSF collected after intravenous administration of 3g piracetam every 6h and oral administration 1.2g every 6h in encephalopathy patients with aphasia was demonstrated.

Double-cross hydrostatic pressure sample injection for chip CE: variable sample plug volume and minimum number of electrodes.

PubMed

Luo, Yong; Wu, Dapeng; Zeng, Shaojiang; Gai, Hongwei; Long, Zhicheng; Shen, Zheng; Dai, Zhongpeng; Qin, Jianhua; Lin, Bingcheng

2006-09-01

A novel sample injection method for chip CE was presented. This injection method uses hydrostatic pressure, generated by emptying the sample waste reservoir, for sample loading and electrokinetic force for dispensing. The injection was performed on a double-cross microchip. One cross, created by the sample and separation channels, is used for formation of a sample plug. Another cross, formed by the sample and controlling channels, is used for plug control. By varying the electric field in the controlling channel, the sample plug volume can be linearly adjusted. Hydrostatic pressure takes advantage of its ease of generation on a microfluidic chip, without any electrode or external pressure pump, thus allowing a sample injection with a minimum number of electrodes. The potential of this injection method was demonstrated by a four-separation-channel chip CE system. In this system, parallel sample separation can be achieved with only two electrodes, which is otherwise impossible with conventional injection methods. Hydrostatic pressure maintains the sample composition during the sample loading, allowing the injection to be free of injection bias.

Automated fluid analysis apparatus and techniques

DOEpatents

Szecsody, James E.

2004-03-16

An automated device that couples a pair of differently sized sample loops with a syringe pump and a source of degassed water. A fluid sample is mounted at an inlet port and delivered to the sample loops. A selected sample from the sample loops is diluted in the syringe pump with the degassed water and fed to a flow through detector for analysis. The sample inlet is also directly connected to the syringe pump to selectively perform analysis without dilution. The device is airtight and used to detect oxygen-sensitive species, such as dithionite in groundwater following a remedial injection to treat soil contamination.

Three-dimensional printed sample load/inject valves enabling online monitoring of extracellular calcium and zinc ions in living rat brains.

PubMed

Su, Cheng-Kuan; Hsia, Sheng-Chieh; Sun, Yuh-Chang

2014-08-01

We have developed a simple and low-cost flow injection system coupled to a quadruple ICP-MS for the direct and continuous determination of multi-element in microdialysates. To interface microdialysis sampling to an inductively coupled plasma mass spectrometer (ICP-MS), we employed 3D printing to manufacture an as-designed sample load/inject valve featuring an in-valve sample loop for precise handling of microliter samples with a dissolved solids content of 0.9% NaCl (w/v). To demonstrate the practicality of our developed on-line system, we applied the 3D printed valve equipped a 5-μL sample loop to minimize the occurrence of salt matrix effects and facilitate an online dynamic monitoring of extracellular calcium and zinc ions in living rat brains. Under the practical condition (temporal resolution: 10h(-1)), dynamic profiling of these two metal ions in living rat brain extracellular fluid after probe implantation (the basal values for Ca and Zn were 12.11±0.10mg L(-1) and 1.87±0.05μg L(-1), respectively) and real-time monitoring of the physiological response to excitotoxic stress elicited upon perfusing a solution of 2.5mM N-methyl-d-aspartate were performed. Copyright © 2014 Elsevier B.V. All rights reserved.

Evaluation of an ODS column modified with zwitterionic/nonionic mixed surfactants and its application to direct injection determination of inorganic anions.

PubMed

Hasegawa, Takuya; Umemura, Tomonari; Koide, Akira; Chiba, Koichi; Ueki, Yuji; Tsunoda, Kin-ichi; Haraguchi, Hiroki

2005-08-01

An octadecylsilica (ODS) column modified with zwitterionic/nonionic mixed surfactants was evaluated for the direct injection determination of inorganic anions in biological fluids by ion chromatography. A zwitterionic surfactant (sulfobetaine-type) and a nonionic surfactant (polyoxyethylene-type) were used for a stationary-phase modification. When aqueous electrolyte solutions with concentrations of sub-mM to several mM were used as a mobile phase, the zwitterionic surfactant coated on the ODS surface exhibited unique separation selectivity for ionic species, while the nonionic surfactant coated on the ODS might have formed a hydrophilic network over the ODS surface and restricted matrix proteins from adsorbing on the stationary phase. Consequently, the mixed surfactant-modified column system allowed an efficient ion chromatographic separation of inorganic anions as well as a size-exclusive removal of column-fouling proteins. This separation system was applied to the direct injection determination of UV-absorbing anions in human saliva. The detection limits for nitrite, nitrate, iodide and thiocyanate were 3.1, 2.7, 4.5 and 25 microM, respectively, with UV detection at 210 nm (injection volume; 20 microl), and their relative standard deviations for 5 replicate measurements of saliva samples spiked with 100 microM each of those anions were 1.4, 0.9, 2.2 and 5.5%, respectively.

Evaluation of injection methods for fast, high peak capacity separations with low thermal mass gas chromatography.

PubMed

Fitz, Brian D; Mannion, Brandyn C; To, Khang; Hoac, Trinh; Synovec, Robert E

2015-05-01

Low thermal mass gas chromatography (LTM-GC) was evaluated for rapid, high peak capacity separations with three injection methods: liquid, headspace solid phase micro-extraction (HS-SPME), and direct vapor. An Agilent LTM equipped with a short microbore capillary column was operated at a column heating rate of 250 °C/min to produce a 60s separation. Two sets of experiments were conducted in parallel to characterize the instrumental platform. First, the three injection methods were performed in conjunction with in-house built high-speed cryo-focusing injection (HSCFI) to cryogenically trap and re-inject the analytes onto the LTM-GC column in a narrower band. Next, the three injection methods were performed natively with LTM-GC. Using HSCFI, the peak capacity of a separation of 50 nl of a 73 component liquid test mixture was 270, which was 23% higher than without HSCFI. Similar peak capacity gains were obtained when using the HSCFI with HS-SPME (25%), and even greater with vapor injection (56%). For the 100 μl vapor sample injected without HSCFI, the preconcentration factor, defined as the ratio of the maximum concentration of the detected analyte peak relative to the analyte concentration injected with the syringe, was determined to be 11 for the earliest eluting peak (most volatile analyte). In contrast, the preconcentration factor for the earliest eluting peak using HSCFI was 103. Therefore, LTM-GC is demonstrated to natively provide in situ analyte trapping, although not to as great an extent as with HSCFI. We also report the use of LTM-GC applied with time-of-flight mass spectrometry (TOFMS) detection for rapid, high peak capacity separations from SPME sampled banana peel headspace. Copyright © 2015 Elsevier B.V. All rights reserved.

EPA Method 538: Determination of Selected Organic Contaminants in Drinking Water by Direct Aqueous Injection-Liquid Chromatography/Tandem Mass Spectrometry (DAI-LC/MS/MS)

EPA Pesticide Factsheets

EPA’s Selected Analytical Methods for Environmental Remediation and Recovery (SAM) lists this method for preparation and analysis of drinking water samples to detect and measure acephate, diisopropyl methylphosphonate (DIMP), methamidophos and thiofanox.

Construction of a Direct Water-Injected Two-Stroke Engine for Phased Direct Fuel Injection-High Pressure Charging Investigations

NASA Technical Reports Server (NTRS)

Somsel, James P.

1998-01-01

The development of a water injected Orbital Combustion Process (OCP) engine was conducted to assess the viability of using the powerplant for high altitude NASA aircraft and General Aviation (GA) applications. An OCP direct fuel injected, 1.2 liter, three cylinder, two-stroke engine has been enhanced to independently inject water directly into the combustion chamber. The engine currently demonstrates low brake specific fuel consumption capability and an excellent power to weight ratio. With direct water injection, significant improvements can be made to engine power, to knock limits/ignition advance timing, and to engine NO(x) emissions. The principal aim of the testing was to validate a cyclic model developed by the Systems Analysis Branch at NASA Ames Research Center. The work is a continuation of Ames' investigations into a Phased Direct Fuel Injection Engine with High Pressure Charging (PDFI-ITPC).

Simple and clean determination of tetracyclines by flow injection analysis

NASA Astrophysics Data System (ADS)

Rodríguez, Michael Pérez; Pezza, Helena Redigolo; Pezza, Leonardo

2016-01-01

An environmentally reliable analytical methodology was developed for direct quantification of tetracycline (TC) and oxytetracycline (OTC) using continuous flow injection analysis with spectrophotometric detection. The method is based on the diazo coupling reaction between the tetracyclines and diazotized sulfanilic acid in a basic medium, resulting in the formation of an intense orange azo compound that presents maximum absorption at 434 nm. Experimental design was used to optimize the analytical conditions. The proposed technique was validated over the concentration range of 1 to 40 μg mL- 1, and was successfully applied to samples of commercial veterinary pharmaceuticals. The detection (LOD) and quantification (LOQ) limits were 0.40 and 1.35 μg mL- 1, respectively. The samples were also analyzed by an HPLC method, and the results showed agreement with the proposed technique. The new flow injection method can be immediately used for quality control purposes in the pharmaceutical industry, facilitating monitoring in real time during the production processes of tetracycline formulations for veterinary use.

Acupuncture injection for field amplified sample stacking and glass microchip-based capillary gel electrophoresis.

PubMed

Ha, Ji Won; Hahn, Jong Hoon

2017-02-01

Acupuncture sample injection is a simple method to deliver well-defined nanoliter-scale sample plugs in PDMS microfluidic channels. This acupuncture injection method in microchip CE has several advantages, including minimization of sample consumption, the capability of serial injections of different sample solutions into the same microchannel, and the capability of injecting sample plugs into any desired position of a microchannel. Herein, we demonstrate that the simple and cost-effective acupuncture sample injection method can be used for PDMS microchip-based field amplified sample stacking in the most simplified straight channel by applying a single potential. We achieved the increase in electropherogram signals for the case of sample stacking. Furthermore, we present that microchip CGE of ΦX174 DNA-HaeⅢ digest can be performed with the acupuncture injection method on a glass microchip while minimizing sample loss and voltage control hardware. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-accuracy measurements of N2O concentration and site-specific nitrogen isotopes in small or high concentration samples

NASA Astrophysics Data System (ADS)

Palmer, M. R.; Arata, C.; Huang, K.

2014-12-01

Nitrous oxide (N2O) gas is among the major contributors to global warming and ozone depletion in stratosphere. Quantitative estimate of N­2O production in various pathways and N­2O fluxes across different reservoirs is the key to understanding the role of N­2O in the global change. To achieve this goal, accurate and concurrent measurement of both N2O concentration ([N2O]) and its site-specific isotopic composition (SP-δ15N), namely δ15Nα and δ15Nβ, is desired. Recent developments in Cavity Ring-Down Spectroscopy (CRDS) have enabled high precision measurements of [N2O] and SP-δ15N of a continuous gas flow. However, many N­­2O samples are discrete with limited volume (< 500 ml), and/or high [N2O] (> 2 ppm), and are not suitable for direct measurements by CRDS. Here we present results of a Small Sample Isotope Module 2 (SSIM2) which is coupled to and automatically coordinated with a Picarro isotopic N2O CRDS analyzer to handle and measure high concentration and/or small volume samples. The SSIM2 requires 20 ml of sample per analysis, and transfers the sample to the CRDS for high precision measurement. When the sample injection is < 20 ml, a zero gas is optionally filled to make up the volume. We used the SSIM2 to dilute high [N2O] samples and < 20 ml samples, and tested the effect of dilution on the measured SP-δ15N. In addition, we employed and tested a newly developed double injection method for samples adequate for two 20 ml injections. After the SSIM2 and the CRDS cavity was primed with the first injection, the second injection, which has negligible dilution of the sample, can be accurately measured for both [N2O] and SP-δ15N. Results of these experiments indicate that the precision of SSIM2-CRDS is similar to that of the continuous measurements using the CRDS alone, and that dilution has minimal effect on SP-δ15N, as along as the [N2O] is > 300 ppb after dilution. Overall, the precision of SP-δ15N measured using the SSIM2 is < 0.5 ‰.

Hot flue-gas spiking and recovery study for tetrachlorodibenzodioxins (TCDD) using Modified Method 5 and SASS (Source Assessment Sampling System) sampling with a simulated incinerator. Final report, May 1981-February 1982

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

Cooke, M.; DeRoos, F.; Rising, B.

1984-10-01

The report gives results of an evaluation of the sampling and analysis of ultratrace levels of dibenzodioxins using EPA's recommended source sampling procedures (Modified Method 5 (MM5) train and the Source Assessment Sampling System--SASS). A gas-fired combustion system was used to simulate incineration flue gas, and a precision liquid injection system was designed for the program. The precision liquid injector was used to administer dilute solutions of 1,2,3,4-tetrachlorodibenzo-p-dioxin (1,2,3,4-TCDD) directly into a hot--260C (500F)--flue gas stream. Injections occurred continuously during the sampling episode so that very low gas-phase concentrations of 1,2,3,4-TCDD were continuously mixed with the flue gases. Recoveries weremore » measured for eight burn experiments. For all but one, the recoveries could be considered quantitative, demonstrating efficient collection by the EPA sampling systems. In one study, the components and connecting lines from a sampling device were analyzed separately to show where the 1,2,3,4-TCDD deposited in the train.« less

Determination of stream reaeration coefficients by use of tracers

USGS Publications Warehouse

Kilpatrick, F.A.; Rathbun, R.E.; Yotsukura, N.; Parker, G.W.; DeLong, L.L.

1987-01-01

Stream reaeration is the physical absorption of oxygen from the atmosphere by a flowing stream. This is the primary process by which a stream replenishes the oxygen consumed in the biodegradation of organic wastes.Prior to 1965, reaeration rate coefficients could be estimated only by indirect methods. In 1965, a direct method of measuring stream reaeration coefficients was developed in which a radioactive tracer gas was injected into a stream--the tracer gas being desorbed from the stream inversely to how oxygen would be absorbed. The technique has since been modified by substituting hydrocarbon gases for the radioactive tracer gas.This manual describes the slug-injection and constant-rate injection methods of performing gas-tracer desorption measurements. Emphasis is on the use of rhodamine WT dye as a relatively conservative tracer and propane as the nonconservative gas tracer, on planning field tests, methods of injection, sampling and analysis, and computational techniques to compute desorption and reaeration coefficients.

Internal validation of the GlobalFiler™ Express PCR Amplification Kit for the direct amplification of reference DNA samples on a high-throughput automated workflow.

PubMed

Flores, Shahida; Sun, Jie; King, Jonathan; Budowle, Bruce

2014-05-01

The GlobalFiler™ Express PCR Amplification Kit uses 6-dye fluorescent chemistry to enable multiplexing of 21 autosomal STRs, 1 Y-STR, 1 Y-indel and the sex-determining marker amelogenin. The kit is specifically designed for processing reference DNA samples in a high throughput manner. Validation studies were conducted to assess the performance and define the limitations of this direct amplification kit for typing blood and buccal reference DNA samples on various punchable collection media. Studies included thermal cycling sensitivity, reproducibility, precision, sensitivity of detection, minimum detection threshold, system contamination, stochastic threshold and concordance. Results showed that optimal amplification and injection parameters for a 1.2mm punch from blood and buccal samples were 27 and 28 cycles, respectively, combined with a 12s injection on an ABI 3500xL Genetic Analyzer. Minimum detection thresholds were set at 100 and 120RFUs for 27 and 28 cycles, respectively, and it was suggested that data from positive amplification controls provided a better threshold representation. Stochastic thresholds were set at 250 and 400RFUs for 27 and 28 cycles, respectively, as stochastic effects increased with cycle number. The minimum amount of input DNA resulting in a full profile was 0.5ng, however, the optimum range determined was 2.5-10ng. Profile quality from the GlobalFiler™ Express Kit and the previously validated AmpFlSTR(®) Identifiler(®) Direct Kit was comparable. The validation data support that reliable DNA typing results from reference DNA samples can be obtained using the GlobalFiler™ Express PCR Amplification Kit. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Study of pore pressure reaction on hydraulic fracturing

NASA Astrophysics Data System (ADS)

Trimonova, Mariia; Baryshnikov, Nikolay; Turuntaev, Sergey; Zenchenko, Evgeniy; Zenchenko, Petr

2017-04-01

We represent the results of the experimental study of the hydraulic fracture propagation influence on the fluid pore pressure. Initial pore pressure was induced by injection and production wells. The experiments were carried out according to scaling analysis based on the radial model of the fracture. All required geomechanical and hydrodynamical properties of a sample were derived from the scaling laws. So, gypsum was chosen as a sample material and vacuum oil as a fracturing fluid. The laboratory setup allows us to investigate the samples of cylindrical shape. It can be considered as an advantage in comparison with standard cubic samples, because we shouldn't consider the stress field inhomogeneity induced by the corners. Moreover, we can set 3D-loading by this setting. Also the sample diameter is big enough (43cm) for placing several wells: the fracturing well in the center and injection and production wells on two opposite sides of the central well. The experiment consisted of several stages: a) applying the horizontal pressure; b) applying the vertical pressure; c) water solution injection in the injection well with a constant pressure; d) the steady state obtaining; e) the oil injection in the central well with a constant rate. The pore pressure was recorded in the 15 points along bottom side of the sample during the whole experiment. We observe the pore pressure change during all the time of the experiment. First, the pore pressure changed due to water injection. Then we began to inject oil in the central well. We compared the obtained experimental data on the pore pressure changes with the solution of the 2D single-phase equation of pore-elasticity, and we found significant difference. The variation of the equation parameters couldn't help to resolve the discrepancy. After the experiment, we found that oil penetrated into the sample before and after the fracture initiation. This fact encouraged us to consider another physical process - the oil-water displacement. Have taken into account the phenomenon, we could find the parameter values for the best matching the experimental data with the analytical one. After such a comparison, we could estimate the permeability variation in the different directions due to changes in the pore pressure during fracturing. Thus it was found that for the correct solution of hydrodynamic problems in relation with hydraulic fracturing (for example, to estimate the production rate of the fractured well) one should take into account the change of the permeability in the vicinity of the fracture and solve nonlinear pore-elasticity problem.

Experimental study of switching in a rho-i(MQW)-eta vertical coupler

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

Cavailles, J.A.; Erman, M.; Woodbridge, K.

1989-11-01

Electrically controlled switching in a vertically arranged directional coupler with GaAs/GaAIAs multiple quantum well waveguides is demonstrated. Coupling lengths and extinction parameters are determined by using a sample processed in such a way that injection conditions are well defined and that the coupler length can be varied continuously.

Reaction-space analysis of homogeneous charge compression ignition combustion with varying levels of fuel stratification under positive and negative valve overlap conditions

DOE PAGES

Kodavasal, Janardhan; Lavoie, George A.; Assanis, Dennis N.; ...

2015-10-26

Full-cycle computational fluid dynamics simulations with gasoline chemical kinetics were performed to determine the impact of breathing and fuel injection strategies on thermal and compositional stratification, combustion and emissions during homogeneous charge compression ignition combustion. The simulations examined positive valve overlap and negative valve overlap strategies, along with fueling by port fuel injection and direct injection. The resulting charge mass distributions were analyzed prior to ignition using ignition delay as a reactivity metric. The reactivity stratification arising from differences in the distributions of fuel–oxygen equivalence ratio (Φ FO), oxygen molar fraction (χ O2) and temperature (T) was determined for threemore » parametric studies. In the first study, the reactivity stratification and burn duration for positive valve overlap valve events with port fuel injection and early direct injection were nearly identical and were dominated by wall-driven thermal stratification. nitrogen oxide (NO) and carbon monoxide (CO) emissions were negligible for both injection strategies. In the second study, which examined negative valve overlap valve events with direct injection and port fuel injection, reactivity stratification increased for direct injection as the Φ FO and T distributions associated with direct fuel injection into the hot residual gas were positively correlated; however, the latent heat absorbed from the hot residual gas by the evaporating direct injection fuel jet reduced the overall thermal and reactivity stratification. These stratification effects were offsetting, resulting in similar reactivity stratification and burn durations for the two injection strategies. The higher local burned gas temperatures with direct injection resulted in an order of magnitude increase in NO, while incomplete combustion of locally over-lean regions led to a sevenfold increase in CO emissions compared to port fuel injection. The final study evaluated positive valve overlap and negative valve overlap valve events with direct injection. Furthermore, relative to positive valve overlap, the negative valve overlap condition had a wider reactivity stratification, a longer burn duration and higher NO and CO emissions associated with reduced fuel–air mixing.« less

Fast determination of phosphorus in honey, milk and infant formulas by electrothermal atomic absorption spectrometry using a slurry sampling procedure

NASA Astrophysics Data System (ADS)

López-García, I.; Viñas, P.; Romero-Romero, R.; Hernández-Córdoba, M.

2007-01-01

A procedure for the electrothermal atomic absorption spectrometric determination of phosphorus in honey, milk and infant formulas using slurried samples is described. Suspensions prepared in a medium containing 50% v/v concentrated hydrogen peroxide, 1% v/v concentrated nitric acid, 10% m/v glucose, 5% m/v sucrose and 100 mg l - 1 of potassium were introduced directly into the furnace. For the honey samples, multiple injection of the sample was necessary. The modifier selected was a mixture of 20 μg palladium and 5 μg magnesium nitrate, which was injected after the sample and before proceeding with the drying and calcination steps. Calibration was performed using aqueous standards prepared in the same suspension medium and the graph was linear between 5 and 80 mg l - 1 of phosphorus. The reliability of the procedure was checked by comparing the results obtained by the new developed method with those found when using a reference spectrophotometric method after a mineralization step, and by analyzing several certified reference materials.

Quality of groundwater at and near an aquifer storage and recovery site, Bexar, Atascosa, and Wilson Counties, Texas, June 2004-August 2008

USGS Publications Warehouse

Otero, Cassi L.; Petri, Brian L.

2010-01-01

The U.S. Geological Survey, in cooperation with the San Antonio Water System, did a study during 2004-08 to characterize the quality of native groundwater from the Edwards aquifer and pre- and post-injection water from the Carrizo aquifer at and near an aquifer storage and recovery (ASR) site in Bexar, Atascosa, and Wilson Counties, Texas. Groundwater samples were collected and analyzed for selected physical properties and constituents to characterize the quality of native groundwater from the Edwards aquifer and pre- and post-injection water from the Carrizo aquifer at and near the ASR site. Geochemical and isotope data indicated no substantial changes in major-ion, trace-element, and isotope chemistry occurred as the water from the Edwards aquifer was transferred through a 38-mile pipeline to the aquifer storage and recovery site. The samples collected from the four ASR recovery wells were similar in major-ion and stable isotope chemistry compared to the samples collected from the Edwards aquifer source wells and the ASR injection well. The similarity could indicate that as Edwards aquifer water was injected, it displaced native Carrizo aquifer water, or, alternatively, if mixing of Edwards and Carrizo aquifer waters was occurring, the major-ion and stable isotope signatures for the Carrizo aquifer water might have been obscured by the signatures of the injected Edwards aquifer water. Differences in the dissolved iron and dissolved manganese concentrations indicate that either minor amounts of mixing occurred between the waters from the two aquifers, or as Edwards aquifer water displaced Carrizo aquifer water it dissolved the iron and manganese directly from the Carrizo Sand. Concentrations of radium-226 in the samples collected at the ASR recovery wells were smaller than the concentrations in samples collected from the Edwards aquifer source wells and from the ASR injection well. The smaller radium-226 concentrations in the samples collected from the ASR recovery wells likely indicate some degree of mixing of the two waters occurred rather than continued decay of radium-226 in the injected water. Geochemical and isotope data measured in samples collected in May 2005 from two Carrizo aquifer monitoring wells and in July 2008 from the three ASR production-only wells in the northern section of the ASR site indicate that injected Edwards aquifer water had not migrated to these five sites. Geochemical and isotope data measured in samples collected from Carrizo aquifer wells in 2004, 2005, and 2008 were graphically analyzed to determine if changes in chemistry could be detected. Major-ion, trace element, and isotope chemistry varied spatially in the samples collected from the Carrizo aquifer. With the exception of a few samples, major-ion concentrations measured in samples collected in Carrizo aquifer wells in 2004, 2005, and 2008 were similar. A slightly larger sulfate con-centration and a slightly smaller bicarbonate concentration were measured in samples collected in 2005 and 2008 from well NC1 compared to samples collected at well NC1 in 2004. Larger sodium concentrations and smaller calcium, magnesium, bicarbonate, and sulfate concentrations were measured in samples collected in 2008 from well WC1 than in samples collected at this well in 2004 and 2005. Larger calcium and magnesium concentrations and a smaller sodium concentration were measured in the samples collected in 2008 at well EC2 compared to samples collected at this well in 2004 and 2005. While in some cases the computed percent differences (compared to concentrations from June 2004) in dissolved iron and dissolved manganese concentrations in 11 wells sampled in the Carrizo aquifer in 2005 and 2008 were quite large, no trends that might have been caused by migration of injected Edwards aquifer water were observed. Because of the natural variation in geochemical data in the Carrizo aquifer and the small data set collected for this study, differences in major-ion and

Quantitative Detection of Trace Explosive Vapors by Programmed Temperature Desorption Gas Chromatography-Electron Capture Detector

PubMed Central

Field, Christopher R.; Lubrano, Adam; Woytowitz, Morgan; Giordano, Braden C.; Rose-Pehrsson, Susan L.

2014-01-01

The direct liquid deposition of solution standards onto sorbent-filled thermal desorption tubes is used for the quantitative analysis of trace explosive vapor samples. The direct liquid deposition method yields a higher fidelity between the analysis of vapor samples and the analysis of solution standards than using separate injection methods for vapors and solutions, i.e., samples collected on vapor collection tubes and standards prepared in solution vials. Additionally, the method can account for instrumentation losses, which makes it ideal for minimizing variability and quantitative trace chemical detection. Gas chromatography with an electron capture detector is an instrumentation configuration sensitive to nitro-energetics, such as TNT and RDX, due to their relatively high electron affinity. However, vapor quantitation of these compounds is difficult without viable vapor standards. Thus, we eliminate the requirement for vapor standards by combining the sensitivity of the instrumentation with a direct liquid deposition protocol to analyze trace explosive vapor samples. PMID:25145416

Quantitative detection of trace explosive vapors by programmed temperature desorption gas chromatography-electron capture detector.

PubMed

Field, Christopher R; Lubrano, Adam; Woytowitz, Morgan; Giordano, Braden C; Rose-Pehrsson, Susan L

2014-07-25

The direct liquid deposition of solution standards onto sorbent-filled thermal desorption tubes is used for the quantitative analysis of trace explosive vapor samples. The direct liquid deposition method yields a higher fidelity between the analysis of vapor samples and the analysis of solution standards than using separate injection methods for vapors and solutions, i.e., samples collected on vapor collection tubes and standards prepared in solution vials. Additionally, the method can account for instrumentation losses, which makes it ideal for minimizing variability and quantitative trace chemical detection. Gas chromatography with an electron capture detector is an instrumentation configuration sensitive to nitro-energetics, such as TNT and RDX, due to their relatively high electron affinity. However, vapor quantitation of these compounds is difficult without viable vapor standards. Thus, we eliminate the requirement for vapor standards by combining the sensitivity of the instrumentation with a direct liquid deposition protocol to analyze trace explosive vapor samples.

Lean direct wall fuel injection method and devices

NASA Technical Reports Server (NTRS)

Choi, Kyung J. (Inventor); Tacina, Robert (Inventor)

2000-01-01

A fuel combustion chamber, and a method of and a nozzle for mixing liquid fuel and air in the fuel combustion chamber in lean direct injection combustion for advanced gas turbine engines, including aircraft engines. Liquid fuel in a form of jet is injected directly into a cylindrical combustion chamber from the combustion chamber wall surface in a direction opposite to the direction of the swirling air at an angle of from about 50.degree. to about 60.degree. with respect to a tangential line of the cylindrical combustion chamber and at a fuel-lean condition, with a liquid droplet momentum to air momentum ratio in the range of from about 0.05 to about 0.12. Advanced gas turbines benefit from lean direct wall injection combustion. The lean direct wall injection technique of the present invention provides fast, uniform, well-stirred mixing of fuel and air. In addition, in order to further improve combustion, the fuel can be injected at a venturi located in the combustion chamber at a point adjacent the air swirler.

Improved hydrostatic pressure sample injection by tilting the microchip towards the disposable miniaturized CE device.

PubMed

Wang, Wei; Zhou, Fang; Zhao, Liang; Zhang, Jian-Rong; Zhu, Jun-Jie

2008-02-01

A simple method of hydrostatic pressure sample injection towards a disposable microchip CE device was developed. The liquid level in the sample reservoir was higher than that in the sample waste reservoir (SWR) by tilting microchip and hydrostatic pressure was generated, the sample was driven to pass through injection channel into SWR. After sample loading, the microchip was levelled for separation under applied high separation voltage. Effects of tilted angle, initial liquid height and injection duration on electrophoresis were investigated. With enough injection duration, the injection result was little affected by tilted angle and initial liquid heights in the reservoirs. Injection duration for obtaining a stable sample plug was mainly dependent on the tilted angle rather than the initial height of liquid. Experimental results were consistent with theoretical prediction. Fluorescence observation and electrochemical detection of dopamine and catechol were employed to verify the feasibility of tilted microchip hydrostatic pressure injection. Good reproducibility of this injection method was obtained. Because the instrumentation was simplified and no additional hardware was needed in this technology, the proposed method would be potentially useful in disposable devices.

Do flexible inter-injection intervals improve the effects of botulinum toxin A treatment in reducing impairment and disability in patients with spasticity?

PubMed

Trompetto, Carlo; Marinelli, Lucio; Mori, Laura; Puce, Luca; Pelosin, Elisa; Serrati, Carlo; Fattapposta, Francesco; Rinalduzzi, Steno; Abbruzzese, Giovanni; Currà, Antonio

2017-05-01

In patients treated with botulinum toxin-A (BoNT-A), toxin-directed antibody formation was related to the dosage and frequency of injections, leading to the empirical adoption of minimum time intervals between injections of 3months or longer. However, recent data suggest that low immunogenicity of current BoNT-A preparations could allow more frequent injections. Our hypothesis is that a short time interval between injections may be safe and effective in reducing upper limb spasticity and related disability. IncobotulinumtoxinA was injected under ultrasound guidance in spastic muscles of 11 subjects, who were evaluated just before BoNT-A injection (T0), and 1month (T1), 2months (T2) and 4months (T3) after injecting. At T1, in the case of persistent disability related to spasticity interfering with normal activities, patients received an additional toxin dose. Seven subjects received the additional dose at T1 because of persistent disability; 4 of them had a decrease of disability 1month later (T2). Rethinking the injection scheme for BoNT-A treatment may have a major impact in the management of spasticity and related disability. Future studies with larger sample sizes are warranted to confirm that injection schedules with short time intervals should no longer be discouraged in clinical practice. Copyright © 2017 Elsevier Ltd. All rights reserved.

Quantification of polychlorinated dibenzo-p-dioxins and dibenzofurans by direct injection of sample extract into the comprehensive multidimensional gas chromatograph/high-resolution time-of-flight mass spectrometer.

PubMed

Shunji, Hashimoto; Yoshikatsu, Takazawa; Akihiro, Fushimi; Hiroyasu, Ito; Kiyoshi, Tanabe; Yasuyuki, Shibata; Masa-aki, Ubukata; Akihiko, Kusai; Kazuo, Tanaka; Hideyuki, Otsuka; Katsunori, Anezaki

2008-01-18

Polychlorinated dibenzo-p-dioxins and dibenzofurans in crude extracts of fly ash and flue gas from municipal waste incinerators were quantified using a comprehensive multidimensional gas chromatograph (GC x GC) coupled to a high-resolution time-of-flight mass spectrometer (HR-TOFMS). For identification and quantification, we developed our own program to prepare 3D chromatograms of selected mass numbers from the data of the GC x GC/HR-TOFMS. Isolation of all congeners with a TCDD toxic equivalency factor from the other isomers by only one injection was confirmed. The instrumental detection limit of TCDD on the GC x GC/HR-TOFMS was 0.9 pg by the relative calibration method. Quantification of these substances in the crude extracts was achieved by direct injection to the GC x GC/HR-TOFMS. The results agree with the values obtained using a generic gas chromatography/high-resolution mass spectrometry (GC/HRMS) system. It was confirmed that measurement by high-resolution TOFMS and GC x GC effectively reduces interference from other chemicals.

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

Zelenyuk, Alla; Reitz, Paul; Stewart, Mark L.

Gasoline Compression Ignition (GCI) engines have the potential to achieve high fuel efficiency and to significantly reduce both NOx and particulate matter (PM) emissions by operating under dilute partially-premixed conditions. This low temperature combustion strategy is dependent upon direct-injection of gasoline during the compression stroke and potentially near top dead center (TDC). The timing and duration of the in-cylinder injections can be tailored based on speed and load to create optimized conditions that result in a stable combustion. We present the results of advanced aerosol analysis methods that have been used for detailed real-time characterization of PM emitted from amore » single-cylinder GCI engine operated at different speed, load, timing, and number and duration of near-TDC fuel injections. PM characterization included 28 measurements of size and composition of individual particles sampled directly from the exhaust and after mass and/or mobility classification. We use these data to calculate particle effective density, fractal dimension, dynamic shape factors in free-molecular and transition flow regimes, average diameter of primary spherules, number of spherules, and void fraction of soot agglomerates.« less

Automation and integration of multiplexed on-line sample preparation with capillary electrophoresis for DNA sequencing

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

Tan, H.

1999-03-31

The purpose of this research is to develop a multiplexed sample processing system in conjunction with multiplexed capillary electrophoresis for high-throughput DNA sequencing. The concept from DNA template to called bases was first demonstrated with a manually operated single capillary system. Later, an automated microfluidic system with 8 channels based on the same principle was successfully constructed. The instrument automatically processes 8 templates through reaction, purification, denaturation, pre-concentration, injection, separation and detection in a parallel fashion. A multiplexed freeze/thaw switching principle and a distribution network were implemented to manage flow direction and sample transportation. Dye-labeled terminator cycle-sequencing reactions are performedmore » in an 8-capillary array in a hot air thermal cycler. Subsequently, the sequencing ladders are directly loaded into a corresponding size-exclusion chromatographic column operated at {approximately} 60 C for purification. On-line denaturation and stacking injection for capillary electrophoresis is simultaneously accomplished at a cross assembly set at {approximately} 70 C. Not only the separation capillary array but also the reaction capillary array and purification columns can be regenerated after every run. DNA sequencing data from this system allow base calling up to 460 bases with accuracy of 98%.« less

[Rapid screening the alkaloids of poppy shell in hot pot condiment, beef noodle soup and seasoning by direct analysis in real time-tandem mass spectrometry].

PubMed

Zhang, Baile; Gao, Lihong; Xie, Yingshuang; Zhou, Wei; Chen, Xiaofeng; Lei, Chunni; Zhang, Huan

2017-07-08

A direct analysis in real time tandem mass spectrometry (DART-MS/MS) method was established for quickly screening five illegally added alkaloids of poppy shell from the hot pot condiment, beef noodle soup and seasoning. The samples were extracted and purified by acetonitrile, and then injected under the conditions of ionization temperature of 300℃, grid electrode voltage of 150 V and sampling rate of 0.8 mm/s using DART in the positive ion mode. The determination was conducted by tandem mass spectrometry in positive ESI mode under multiple reaction monitoring (MRM) mode. The method is simple and rapid, and can meet the requirement of rapid screening and analysis of large quantities of samples.

In-situ droplet monitoring for self-tuning spectrometers

DOEpatents

Montaser, Akbar; Jorabchi, Kaveh; Kahen, Kaveh

2010-09-28

A laser scattering based imaging technique is utilized in order to visualize the aerosol droplets in an inductively coupled plasma (ICP) torch from an aerosol source to the site of analytical measurements. The resulting snapshots provide key information about the spatial distribution of the aerosol introduced by direct and indirect injection devices: 1) a direct injection high efficiency nebulizer (DIHEN); 2) a large-bore DIHEN (LB-DIHEN); and 3) a PFA microflow nebulizer with a PFA Scott-type spray chamber. Moreover, particle image velocimetry (PIV) is used to study the in-situ behavior of the aerosol before interaction with, for example, plasma, while the individual surviving droplets are explored by particle tracking velocimetry (PTV). Further, the velocity distribution of the surviving droplets demonstrates the importance of the initial droplet velocities in complete desolvation of the aerosol for optimum analytical performance in ICP spectrometries. These new observations are important in the design of the next-generation direct injection devices for lower sample consumption, higher sensitivity, lower noise levels, suppressed matrix effects, and for developing smart spectrometers. For example, a controller can be provided to control the output of the aerosol source by controlling the configuration of the source or the gas flow rate via feedback information concerning the aerosol.

The influence of technological parameters on the dynamic behavior of "liquid wood" samples obtained by injection molding

NASA Astrophysics Data System (ADS)

Plavanescu Mazurchevici, Simona; Carausu, Constantin; Comaneci, Radu; Nedelcu, Dumitru

2017-10-01

The plastic products contribute to environmental pollution. Replacing the plastic materials with biodegradable materials with superior properties is an absolute necessity and important research direction for the near future. The first steps in this regard were the creation of composite materials containing natural fibers with positive effects on the environment that have penetrated in different fields. The bioplastics and biocomposites made from natural fibers is a topical solution. The next step was made towards obtaining biodegradable and recyclable materials based on cellulose, lignin and no carcinogens. In this category fall the "liquid wood" with a use up to five times without affecting the mechanical properties. "Liquid wood" is a high quality thermoplastic biocomposite. "Liquid wood" is a biopolymer composite divided in three categories, ARBOFORM®, ARBOBLEND® and ARBOFILL®, which have differed composition in terms of lignin percentage, being delivered by Tecnaro, as granules, [1]. The paper's research was focus on Arboform L V3 Nature and Arboform L V3 Nature reinforced with aramid fiber. In the experimental plan were taken into account six parameters (Dinj - direction of injection [°]; Ttop - melting temperature [°C]; Pinj - injection pressure [MPa] Ss - speed [m/min]; tinj - injection time [s] and tc - cooling time [s]) each with two levels, research carried on by Taguchi methodology. Processing Taguchi method allowed both Taguchi setting work parameters influence on storage modulus and damping as the size and influence their ranking. Experimental research concerning the influence technological parameters on storage modulus of samples obtained by injection from Arboform L V3 Nature yielded an average of 6055MPa and descending order as follows: Trac, Ss, Pinj, Dinj and Ttop. The average of model for reinforced material was 6419MPa and descending order of parameters influence such as: Dinj, Trac, Ttop, tinj, Ss and Pinj.

Analysis of chlorophenoxy acid herbicides in water by large-volume on-line derivatization and gas chromatography-mass spectrometry.

PubMed

Ding, W H; Liu, C H; Yeh, S P

2000-10-27

This work presents a modified method to analyze chlorophenoxy acid herbicides in water samples. The herbicides 2,4-D (2,4-dichlorophenoxyacetic acid). Silvex (2,4,5-trichlorophenoxypropionic acid) and 2,4,5-T (2,4,5-trichlorophenoxyacetic acid) were used to evaluate the method. The method involves extraction of samples by a graphitized carbon black cartridge, and on-line derivatization in the GC injection port using a large-volume (10-20 microl) direct sample introduction (DSI) device with tetraalkylammonium salts. The analytes were then identified and quantitated by ion-trap gas chromatography-mass spectrometry. The large-volume DSI injection-port derivatization technique provides sensitivity, fast and reproducible results for chlorophenoxy acid herbicides residues, to quantitation at 0.1 to 0.2 microg/l in 500-ml water samples. An enhanced characteristic mass chromatogram of molecular ions of butylated chlorophenoxy acid herbicides with a significant chlorine isotope pattern by electron impact ionization MS allows us to determine herbicides residues at trace levels in aqueous samples. Recovery of the herbicide residues in spiked various water samples ranged from 70 to 99% while RSDs ranged from 1 to 13%.

EVALUATION OF IODINE BASED IMPINGER SOLUTIONS FOR THE EFFICIENT CAPTURE OF HG USING DIRECT INJECTION NEBULIZATION INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY (DIN-ICP/MS) ANALYSIS

EPA Science Inventory

Currently there are no EPA reference sampling methods that have been promulgated for measuring stack emissions of Hg from coal combustion sources, however, EPA Method 29 is most commonly applied. The draft ASTM Ontario Hydro Method for measuring oxidized, elemental, particulate-b...

IMPINGER SOLUTIONS FOR THE EFFICIENT CAPTURE OF GASEOUS MERCURY SPECIES USING DIRECT INJECTION NEBULIZATION INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY (DIN-ICP/MS) ANALYSIS

EPA Science Inventory

Currently there are no EPA reference sampling mehtods that have been promulgated for measuring Hg from coal combustion sources. EPA Method 29 is most commonly applied. The ASTM Ontario Hydro Draft Method for measuring oxidized, elemental, particulate-bound and total Hg is now und...

Process control of apple winemaking by low-resolution gas-phase Fourier-transform infrared spectroscopy.

PubMed

Ahro, M; Hakala, M; Kauppinen, J; Kallio, H

2001-10-01

Four apple wine fermentation processes have been observed by means of direct-inlet gas-phase FTIR spectroscopy. The apple juice concentrates were each fermented by two species of Saccharomyces cerevisiae starters, and the experiment was repeated. The development of the concentrations of 1-propanol, 4-methylpyridine, acetaldehyde, acetic acid, and ethyl acetate was monitored. Two different sampling methods were used--static headspace and direct injection of the must. The performance of the FTIR method is limited by the high ethanol concentration. It can be mathematically proven that the amount of sample can be selected so that any distortion due to ethanol is minimized. Headspace GC-MS was used for preliminary compound identification.

Effects of Pre and Post-Rigor Marinade Injection on Some Quality Parameters of Longissimus Dorsi Muscles

PubMed Central

Fadıloğlu, Eylem Ezgi; Serdaroğlu, Meltem

2018-01-01

Abstract This study was conducted to evaluate the effects of pre and post-rigor marinade injections on some quality parameters of Longissimus dorsi (LD) muscles. Three marinade formulations were prepared with 2% NaCl, 2% NaCl+0.5 M lactic acid and 2% NaCl+0.5 M sodium lactate. In this study marinade uptake, pH, free water, cooking loss, drip loss and color properties were analyzed. Injection time had significant effect on marinade uptake levels of samples. Regardless of marinate formulation, marinade uptake of pre-rigor samples injected with marinade solutions were higher than post rigor samples. Injection of sodium lactate increased pH values of samples whereas lactic acid injection decreased pH. Marinade treatment and storage period had significant effect on cooking loss. At each evaluation period interaction between marinade treatment and injection time showed different effect on free water content. Storage period and marinade application had significant effect on drip loss values. Drip loss in all samples increased during the storage. During all storage days, lowest CIE L* value was found in pre-rigor samples injected with sodium lactate. Lactic acid injection caused color fade in pre-rigor and post-rigor samples. Interaction between marinade treatment and storage period was found statistically significant (p<0.05). At day 0 and 3, the lowest CIE b* values obtained pre-rigor samples injected with sodium lactate and there were no differences were found in other samples. At day 6, no significant differences were found in CIE b* values of all samples. PMID:29805282

Effects of Pre and Post-Rigor Marinade Injection on Some Quality Parameters of Longissimus Dorsi Muscles.

PubMed

Fadıloğlu, Eylem Ezgi; Serdaroğlu, Meltem

2018-04-01

This study was conducted to evaluate the effects of pre and post-rigor marinade injections on some quality parameters of Longissimus dorsi (LD) muscles. Three marinade formulations were prepared with 2% NaCl, 2% NaCl+0.5 M lactic acid and 2% NaCl+0.5 M sodium lactate. In this study marinade uptake, pH, free water, cooking loss, drip loss and color properties were analyzed. Injection time had significant effect on marinade uptake levels of samples. Regardless of marinate formulation, marinade uptake of pre-rigor samples injected with marinade solutions were higher than post rigor samples. Injection of sodium lactate increased pH values of samples whereas lactic acid injection decreased pH. Marinade treatment and storage period had significant effect on cooking loss. At each evaluation period interaction between marinade treatment and injection time showed different effect on free water content. Storage period and marinade application had significant effect on drip loss values. Drip loss in all samples increased during the storage. During all storage days, lowest CIE L* value was found in pre-rigor samples injected with sodium lactate. Lactic acid injection caused color fade in pre-rigor and post-rigor samples. Interaction between marinade treatment and storage period was found statistically significant ( p <0.05). At day 0 and 3, the lowest CIE b* values obtained pre-rigor samples injected with sodium lactate and there were no differences were found in other samples. At day 6, no significant differences were found in CIE b* values of all samples.

A centrifugal direct recombinase polymerase amplification (direct-RPA) microdevice for multiplex and real-time identification of food poisoning bacteria.

PubMed

Choi, Goro; Jung, Jae Hwan; Park, Byung Hyun; Oh, Seung Jun; Seo, Ji Hyun; Choi, Jong Seob; Kim, Do Hyun; Seo, Tae Seok

2016-06-21

In this study, we developed a centrifugal direct recombinase polymerase amplification (direct-RPA) microdevice for multiplex and real-time identification of food poisoning bacteria contaminated milk samples. The microdevice was designed to contain identical triplicate functional units and each unit has four reaction chambers, thereby making it possible to perform twelve direct-RPA reactions simultaneously. The integrated microdevice consisted of two layers: RPA reagents were injected in the top layer, while spiked milk samples with food poisoning bacteria were loaded into sample reservoirs in the bottom layer. For multiplex bacterial detection, the target gene-specific primers and probes were dried in each reaction chamber. The introduced samples and reagents could be equally aliquoted and dispensed into each reaction chamber by centrifugal force, and then the multiplex direct-RPA reaction was executed. The target genes of bacteria spiked in milk could be amplified at 39 °C without a DNA extraction step by using the direct-RPA cocktails, which were a combination of a direct PCR buffer and RPA enzymes. As the target gene amplification proceeded, the increased fluorescence signals coming from the reaction chambers were recorded in real-time at an interval of 2 min. The entire process, including the sample distribution, the direct-RPA reaction, and the real-time analysis, was accomplished with a custom-made portable genetic analyzer and a miniaturized optical detector. Monoplex, duplex, and triplex food poisoning bacteria (Salmonella enterica, Escherichia coli O157:H7, and Vibrio parahaemolyticus) detection was successfully performed with a detection sensitivity of 4 cells per 3.2 μL of milk samples within 30 min. By implementing the direct-PRA on the miniaturized centrifugal microsystem, the on-site food poisoning bacteria analysis would be feasible with high speed, sensitivity, and multiplicity.

Surface time-lapse electrical resistivity tomography (TLERT) monitoring of an SRS injection and associated biogeochemical processes, Oak Ridge National Laboratory, Tennessee USA

NASA Astrophysics Data System (ADS)

Baker, G. S.; Wu, Y.; Hubbard, S. S.; Wu, W.; Gaines, D. P.; Pratt, J. C.; Modi, A. L.; Watson, D.; Jardine, P.

2009-05-01

We present results from surface time-lapse electrical resistivity tomography (TLERT) data collected within a uranium-contaminated unconfined aquifer underlying the Oak Ridge Field Research Center (ORFRC) located at the Oak Ridge National Laboratory (ORNL) in Tennessee. As part of an Integrated Field Research Challenge (IFRC) project supported by the DOE Environmental Remediation Sciences Program (ERSP), bioreduction of U(VI) to U(IV) with ethanol as an electron donor has been tested during the last four years. Low U concentration (below US EPA MCL of 0.03 mg/L) can be achieved by frequent injection of electron donor. To reduce the costs and improve the sustainability for remediation and site maintenance, our IFRC team is exploring the effectiveness of a slowly degrading substrate such as commercial emulsified vegetable oil substrate (EVO) as alternative electron donor sources. Laboratory batch and flow-through column experiments were carried out to investigate the sensitivity of various physical properties (e.g., electrical conductivity) to EVO injection to test the applicability of geophysics as a monitoring tool at the field scale. Results revealed increased electrical conductivity during both EVO injection and subsequent degradation of surfactant with an overall increase in conductivity of ˜35%; thus, surface TLERT was selected as a monitoring tool to supplement well fluid samples. The field stimulation test began at Area 2 during early February 2009. Prior to the injection of the EVO, preliminary characterization completed, including a geochemical survey of the ground water from ˜50 wells, microbial samples of groundwater and sediment collected from selected wells, and site hydrology characterized by bromide tracer test and surface ERT methods. On February 9, 2009, diluted EVO solution (20% concentration, 900 gal vol) was injected into three injection wells within 1.5 hours. Distribution of the injected EVO and accompanying biogeochemical processes has been monitored since injection through analysis of numerous well fluid samples and TLERT data from 2 profiles. Initial TLERT data were collected at the 2 profiles over a two-week period at 12 different time steps. The surface profiles, situated parallel to and perpendicular to the major flow direction (as delineated by tracer tests), are each 40 m long and consist of 52 electrodes spaced at 0.75 m. Initial analysis indicate good correlation between well fluid samples and TLERT data and allow for improved extrapolation of well data to the field scale. Long-term monitoring is in place to track the continuing hydrologic dynamics and reduction duration in this test area throughout Spring 2009.

Direct Measurement of Trace Elemental Mercury in Hydrocarbon Matrices by Gas Chromatography with Ultraviolet Photometric Detection.

PubMed

Gras, Ronda; Luong, Jim; Shellie, Robert A

2015-11-17

We introduce a technique for the direct measurement of elemental mercury in light hydrocarbons such as natural gas. We determined elemental mercury at the parts-per-trillion level with high precision [<3% RSD (n = 20 manual injection)] using gas chromatography with ultraviolet photometric detection (GC-UV) at 254 nm. Our approach requires a small sample volume (1 mL) and does not rely on any form of sample preconcentration. The GC-UV separation employs an inert divinylbenzene porous layer open tubular column set to separate mercury from other components in the sample matrix. We incorporated a 10-port gas-sampling valve in the GC-UV system, which enables automated sampling, as well as back flushing capability to enhance system cleanliness and sample throughput. Total analysis time is <2 min, and the procedure is linear over a range of 2-83 μg/m(3) [correlation coefficient of R(2) = 0.998] with a measured recovery of >98% over this range.

Rapid determination of benzodiazepines, zolpidem and their metabolites in urine using direct injection liquid chromatography-tandem mass spectrometry.

PubMed

Jeong, Yu-Dong; Kim, Min Kyung; Suh, Sung Ill; In, Moon Kyo; Kim, Jin Young; Paeng, Ki-Jung

2015-12-01

Benzodiazepines and zolpidem are generally prescribed as sedative, hypnotics, anxiolytics or anticonvulsants. These drugs, however, are frequently misused in drug-facilitated crime. Therefore, a rapid and simple liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed for identification and quantification of benzodiazepines, zolpidem and their metabolites in urine using deuterium labeled internal standards (IS). Urine samples (120 μL) mixed with 80 μL of the IS solution were centrifuged. An aliquot (5 μL) of the sample solution was directly injected into the LC-MS/MS system for analysis. The mobile phases consisted of water and acetonitrile containing 2mM ammonium trifluoroacetate and 0.2% acetic acid. The analytical column was a Zorbax SB-C18 (100 mm × 2.1 mm i.d., 3.5 μm, Agilent). The separation and detection of 18 analytes were achieved within 10 min. Calibration curves were linear over the concentration ranges of 0.5-20 ng/mL (zolpidem), 1.0-40 ng/mL (flurazepam and temazepam), 2.5-100 ng/mL (7-aminoclonazepam, 1-hydroxymidazolam, midazolam, flunitrazepam and alprazolam), 5.0-200 ng/mL (zolpidem phenyl-4-carboxylic acid, α-hydroxyalprazolam, oxazepam, nordiazepam, triazolam, diazepam and α-hydroxytriazolam), 10-400 ng/mL (lorazepam and desalkylflurazepam) and 10-100 ng/mL (N-desmethylflunitrazepam) with the coefficients of determination (r(2)) above 0.9971. The dilution integrity of the analytes was examined for supplementation of short linear range. Dilution precision and accuracy were tested using two, four and ten-folds dilutions and they ranged from 3.7 to 14.4% and -12.8 to 12.5%, respectively. The process efficiency for this method was 63.0-104.6%. Intra- and inter-day precisions were less than 11.8% and 9.1%, while intra- and inter-day accuracies were less than -10.0 to 8.2%, respectively. The lower limits of quantification were lower than 10 ng/mL for each analyte. The applicability of the developed method was successfully verified with human urine samples from drug users (n=21). Direct urine sample injection and optimized mobile phases were introduced for simple sample preparation and high-sensitivity with the desired separation. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

Automated system for on-line determination of dimethylarsinic and inorganic arsenic by hydride generation-atomic fluorescence spectrometry.

PubMed

Chaparro, L L; Ferrer, L; Cerdà, V; Leal, L O

2012-09-01

A multisyringe flow-injection approach has been coupled to hydride generation-atomic fluorescence spectrometry (HG-AFS) with UV photo-oxidation for dimethylarsinic (DMA), inorganic As and total As determination, depending on the pre-treatment given to the sample (extraction or digestion). The implementation of a UV lamp allows on-line photo-oxidation of DMA and the following arsenic detection, whereas a bypass leads the flow directly to the HG-AFS system, performing inorganic arsenic determination. DMA concentration is calculated by the difference of total inorganic arsenic and measurement of the photo-oxidation step. The detection limits for DMA and inorganic arsenic were 0.09 and 0.47 μg L(-1), respectively. The repeatability values accomplished were of 2.4 and 1.8%, whereas the injection frequencies were 24 and 28 injections per hour for DMA and inorganic arsenic, respectively. This method was validated by means of a solid reference material BCR-627 (muscle of tuna) with good agreement with the certified values. Satisfactory results for DMA and inorganic arsenic determination were obtained in several water matrices. The proposed method offers several advantages, such as increasing the sampling frequency, low detection limits and decreasing reagents and sample consumption, which leads to lower waste generation.

A microchip-based flow injection-amperometry system with mercaptopropionic acid modified electroless gold microelectrode for the selective determination of dopamine.

PubMed

Wang, Yi; Luo, Jie; Chen, Hengwu; He, Qiaohong; Gan, Nin; Li, Tianhua

2008-09-12

A novel chip-based flow injection analysis (FIA) system has been developed for automatic, rapid and selective determination of dopamine (DA) in the presence of ascorbic acid (AA). The system is composed of a polycarbonate (PC) microfluidic chip with an electrochemical detector (ED), a gravity pump, and an automatic sample loading and injection unit. The selectivity of the ED was improved by modification of the gold working microelectrode, which was fabricated on the PC chip by UV-directed electroless gold plating, with a self-assembled monolayer (SAM) of 3-mercaptopropionic acid (MPA). Postplating treatment methods for cleaning the surface of electroless gold microelectrodes were investigated to ensure the formation of high quality SAMs. The effects of detection potential, flow rate, and sampling volume on the performance of the chip-based FIA system were studied. Under optimum conditions, a detection limit of 74 nmol L(-1) for DA was achieved at the sample throughput rate of 180 h(-1). A RSD of 0.9% for peak heights was observed for 19 runs of a 100 micromol L(-1) DA solution. Interference-free determination of DA could be conducted if the concentration ratio of AA-DA was no more than 10.

Development of an Ethanol Blend Two-Stroke Direct-Injection Snowmobile for Use in the Clean Snowmobile Challenge and National Parks

DOT National Transportation Integrated Search

2010-09-01

The University of Idaho's entry into the 2010 SAE Clean Snowmobile Challenge (CSC) was a direct-injection (DI) two-stroke powered snowmobile modified to use blended ethanol fuel. The modulated and battery-less direct-injection system used to decrease...

Strength and Deformation Behaviour of Cap Rocks Above the CO2SINK-Reservoir

NASA Astrophysics Data System (ADS)

Mutschler, T.; Triantafyllidis, T.; Balthasar, K.; Norden, B.

2009-04-01

The cap-rock of the CO2SINK storage site close to Ketzin consists of clay rich rocks which are typical for cap rock formations above CO2 storage reservoirs. The strength and deformation behaviour of such claystone samples are therefore of fundamental importance for the characterization of secure geological storage of CO2. The elastic and anelastic deformation behaviour limits the maximum injection pressure during CO2-injection and is part of the security measures for the long term storage of CO2. The laboratory experiments where performed on samples gathered from the injection well of the Ketzin pilot test site in Germany and are compared with the elastic and anelastic behaviour of samples from the same Keuper formation in a near-surface outcrop in the Southwest of Germany showing a similar lithology. The samples from the outcrop allowed drilling of samples with a standard size of 100 mm diameter and 200 mm height as well as large samples with a diameter of 550 mm and a height of 1200 mm. The investigations have a special emphasis on the viscous behaviour of the clay stones and its scaling behaviour. A special triaxial testing procedure is applied both on standard and large size samples allowing the determination of the strength, stiffness and viscosity behaviour of the rock in one experimental run. Multi-stage technique (stepwise variation of the confining pressure) gives the strength behaviour of each single sample while applying a constant deformation rate. Stepwise varied deformation rates on the other hand lead to steps in the stress-strain-curve from which the viscosity index is determined. The viscosity index is directly used in the Norton's constitutive relations for viscoplastic simulations. The combination of tests allows for the determination of a broad range of elastic and anelastic properties. The comparison of results - both for elastic and anelastic behaviour - from standard and large samples shows that for the examined rocks a scale effect is negligible. Transition from cataclastic to non-cataclastic behaviour - the transition limit - occurs in a similar range of applied levels of pressure and deformation rates even at room temperature. The obtained transition limit is very important for the judgment of the sealing capacity and integrity of the cap rock. The deformation rates predicted for the pressure and temperature conditions of the caprock at Ketzin test site are far beneath the determined transition limit during the injection and after stop of injection. As a 0° friction angle is used for pressure and deformation limit at Ketzin, the measured elastic and anelastic behaviour of the real caprock act as additional safety margin during injection and in the post injection phase. As the examined rocks are typical for many possible storage sites, the discussed results are of importance beyond the Ketzin Pilot Experiment CO2SINK.

Multiplexed detection of nitrate and nitrite for capillary electrophoresis with an automated device for high injection efficiency.

PubMed

Gao, Leyi; Patterson, Eric E; Shippy, Scott A

2006-02-01

A simple automated nanoliter scale injection device which allows for reproducible 5 nL sample injections from samples with a volume of <1 microL is successfully used for conventional capillary electrophoresis (CE) and Hadamard transform (HT) CE detection. Two standard fused silica capillaries are assembled axially through the device to function as an injection and a separation capillary. Sample solution is supplied to the injection capillary using pressure controlled with a solenoid valve. Buffer solution flows gravimetrically by the junction of the injection and separation capillaries and is also gated with a solenoid valve. Plugs of sample are pushed into the space between the injection and separation capillaries for electrokinectic injection. To evaluate the performance of the injection device, several optimizations are performed including the influence of flow rates, the injected sample volume and the control of the buffer transverse flow on the overall sensitivity. The system was then applied to HT-CE-UV detection for the signal-to-noise ratio (S/N) improvement of the nitric oxide (NO) metabolites, nitrite and nitrate. In addition, signal averaging was performed to explore the possibility of greater sensitivity enhancements compared to single injections.

Focal plane infrared readout circuit with automatic background suppression

NASA Technical Reports Server (NTRS)

Pain, Bedabrata (Inventor); Yang, Guang (Inventor); Sun, Chao (Inventor); Shaw, Timothy J. (Inventor); Wrigley, Chris J. (Inventor)

2002-01-01

A circuit for reading out a signal from an infrared detector includes a current-mode background-signal subtracting circuit having a current memory which can be enabled to sample and store a dark level signal from the infrared detector during a calibration phase. The signal stored by the current memory is subtracted from a signal received from the infrared detector during an imaging phase. The circuit also includes a buffered direct injection input circuit and a differential voltage readout section. By performing most of the background signal estimation and subtraction in a current mode, a low gain can be provided by the buffered direct injection input circuit to keep the gain of the background signal relatively small, while a higher gain is provided by the differential voltage readout circuit. An array of such readout circuits can be used in an imager having an array of infrared detectors. The readout circuits can provide a high effective handling capacity.

Identification of polar volatile organic compounds in consumer products and common microenvironments

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

Wallace, L.A.; Nelson, W.C.; Pellizzari, E.

1991-03-01

Polar volatile organic compounds were identified in the headspace of 31 fragrance products such as perfumes, colognes and soaps. About 150 different chemicals were identified in a semiquantitative fashion, using two methods to analyze the headspace: direct injection into a gas chromatograph and collection by an evacuated canister, each followed by GC-MS analysis. The canister method displayed low recoveries for most of the 25 polar chemical standards tested. However, reconstructed ion chromatograms (RICs) from the canister showed good agreement with RICs from the direct injection method except for some high boiling point compounds. Canister samples collected in 15 microenvironments expectedmore » to contain the fragrance products tested (potpourri stores, fragrance sections of department stores, etc.) showed relatively low concentrations of most of these polar chemicals compared with certain common nonpolar chemicals. The results presented will be useful for models of personal exposure and indoor air quality.« less

Recent Development in Optical Chemical Sensors Coupling with Flow Injection Analysis

PubMed Central

Ojeda, Catalina Bosch; Rojas, Fuensanta Sánchez

2006-01-01

Optical techniques for chemical analysis are well established and sensors based on these techniques are now attracting considerable attention because of their importance in applications such as environmental monitoring, biomedical sensing, and industrial process control. On the other hand, flow injection analysis (FIA) is advisable for the rapid analysis of microliter volume samples and can be interfaced directly to the chemical process. The FIA has become a widespread automatic analytical method for more reasons; mainly due to the simplicity and low cost of the setups, their versatility, and ease of assembling. In this paper, an overview of flow injection determinations by using optical chemical sensors is provided, and instrumentation, sensor design, and applications are discussed. This work summarizes the most relevant manuscripts from 1980 to date referred to analysis using optical chemical sensors in FIA.

Miniaturized flow injection analysis system

DOEpatents

Folta, James A.

1997-01-01

A chemical analysis technique known as flow injection analysis, wherein small quantities of chemical reagents and sample are intermixed and reacted within a capillary flow system and the reaction products are detected optically, electrochemically, or by other means. A highly miniaturized version of a flow injection analysis system has been fabricated utilizing microfabrication techniques common to the microelectronics industry. The microflow system uses flow capillaries formed by etching microchannels in a silicon or glass wafer followed by bonding to another wafer, commercially available microvalves bonded directly to the microflow channels, and an optical absorption detector cell formed near the capillary outlet, with light being both delivered and collected with fiber optics. The microflow system is designed mainly for analysis of liquids and currently measures 38.times.25.times.3 mm, but can be designed for gas analysis and be substantially smaller in construction.

Use of an injection port for thermochemolysis-gas chromatography/mass spectrometry: rapid profiling of biomaterials.

PubMed

Shadkami, Farzad; Helleur, Robert

2009-07-31

A simple and direct approach was developed for thermochemolytic analysis of a wide range of biomolecules present in plant materials using an injection port of a gas chromatograph/mass spectrometer (GC/MS) and a novel solids injector consisting of a coiled stainless steel wire placed inside a modified needle syringe. Optimum thermochemolysis (or Thermally Assisted Hydrolysis/Methylation) was achieved by using a suitable methanolic solution of trimethylsulfonium hydroxide (TMSH) or tetramethylammonium hydroxide (TMAH) with an injection port temperature of 350 degrees C. Intact, methylated flavonoids, saccharides, phenolic and fatty acids, lignin dimers and diterpene resin acids were identified. Samples include tea leaves, hemicelluloses, lignin isolates and herbal medicines. Unexpected chromatographic results using TMAH reagent revealed the presence of intact methylated trisaccharides (658 Da) and structurally informative dimer lignin markers.

Determination of stream reaeration coefficients by use of tracers

USGS Publications Warehouse

Kilpatrick, F.A.; Rathbun, R.E.; Yotsukura, Nobuhiro; Parker, G.W.; DeLong, L.L.

1989-01-01

Stream reaeration is the physical absorption of oxygen from the atmosphere by a flowing stream. This is the primary process by which a stream replenishes the oxygen consumed in the biodegradation of organic wastes. Prior to 1965, reaeration rate coefficients could be estimated only by indirect methods. In 1965, a direct method of measuring stream reaeration coefficients was developed whereby a radioactive tracer gas was injected into a stream-the principle being that the tracer gas would be desorbed from the stream inversely to how oxygen would be absorbed. The technique has since been modified by substituting hydrocarbon gases for the radioactive tracer gas. This manual describes the slug-injection and constant-rate-injection methods of measuring gas-tracer desorption. Emphasis is on the use of rhodamine WT dye as a relatively conservative tracer and propane as the nonconservative gas tracer, on planning field tests, on methods of injection, sampling, and analysis, and on techniques for computing desorption and reaeration coefficients.

Field-scale demonstration of induced biogeochemical reductive dechlorination at Dover Air Force Base, Dover, Delaware

NASA Astrophysics Data System (ADS)

Kennedy, Lonnie G.; Everett, Jess W.; Becvar, Erica; DeFeo, Donald

2006-11-01

Biogeochemical reductive dechlorination (BiRD) is a new remediation approach for chlorinated aliphatic hydrocarbons (CAHs). The approach stimulates common sulfate-reducing soil bacteria, facilitating the geochemical conversion of native iron minerals into iron sulfides. Iron sulfides have the ability to chemically reduce many common CAH compounds including PCE, TCE, DCE, similar to zero valent iron (Fe 0). Results of a field test at Dover Air Force Base, Dover, Delaware, are given in this paper. BiRD was stimulated by direct injection of Epson salt (MgSO 4·7H 2O) and sodium (L) lactate (NaC 3H 5O 3) in five injection wells. Sediment was sampled before and 8 months after injection. Significant iron sulfide minerals developed in the sandy aquifer matrix. From ground water analyses, treatment began a few weeks after injection with up to 95% reduction in PCE, TCE, and cDCE in less than 1 year. More complete CAH treatment is likely at a larger scale than this demonstration.

Geohydrologic reconnaissance of drainage wells in Florida

USGS Publications Warehouse

Kimrey, J.O.; Fayard, L.D.

1984-01-01

Drainage wells are used to inject surface waters directly into an aquifer, or shallow ground waters directly into a deeper aquifer, primarily by gravity. Such wells in Florida may be grouped into two broad types: (1) surface-water injection wells, and (2) interaquifer connector wells. Drainage wells of the first type are further categorized as either Floridan aquifer drainage wells or Biscayne aquifer drainage wells. Floridan aquifer drainage wells are commonly used to supplement drainage for urban areas in karst terranes of central and north Florida. Data are available for 25 wells in the Ocala, Live Oak, and Orlando areas that allow comparison of the quality of water samples from these Floridan aquifer drainage wells with allowable contaminant levels. Comparison indicates that maximum contaminant levels for turbidity, color, and iron, manganese, and lead concentrations are equaled or exceeded in some drainage-well samples, and relatively high counts for coliform bacteria are present in most wells. Biscayne aquifer drainage wells are used locally to dispose of stormwater runoff and other surplus water in southeast Florida, where large numbers of these wells have been permitted in Dade and Broward Counties. The majority of these wells are used to dispose of water from swimming pools or to dispose of heated water from air-conditioning units. The use of Biscayne aquifer drainage wells may have minimal effect on aquifer potability so long as injection of runoff and industrial wates is restricted to zones where chloride concentrations exceed 1,500 milligrams per liter. Interaquifer connector wells are used in the phosphate mining areas of Polk and Hillsborough Counties, to drain mines and recharge the Floridan aquifer. Water-quality data available from 13 connector wells indicate that samples from most of these wells exceed standards values for iron concentration and turbidity. One well yielded a highly mineralized water, and samples from 6 of the other 12 wells exceed standards values for gross alpha concentrations. (USGS)

Transport of fluorobenzoate tracers in a vegetated hydrologic control volume: 1. Experimental results

NASA Astrophysics Data System (ADS)

Queloz, Pierre; Bertuzzo, Enrico; Carraro, Luca; Botter, Gianluca; Miglietta, Franco; Rao, P. S. C.; Rinaldo, Andrea

2015-04-01

This paper reports about the experimental evidence collected on the transport of five fluorobenzoate tracers injected under controlled conditions in a vegetated hydrologic volume, a large lysimeter (fitted with load cells, sampling ports, and an underground chamber) where two willows prompting large evapotranspiration fluxes had been grown. The relevance of the study lies in the direct and indirect measures of the ways in which hydrologic fluxes, in this case, evapotranspiration from the upper surface and discharge from the bottom drainage, sample water and solutes in storage at different times under variable hydrologic forcings. Methods involve the accurate control of hydrologic inputs and outputs and a large number of suitable chemical analyses of water samples in discharge waters. Mass extraction from biomass has also been performed ex post. The results of the 2 year long experiment established that our initial premises on the tracers' behavior, known to be sorption-free under saturated conditions which we verified in column leaching tests, were unsuitable as large differences in mass recovery appeared. Issues on reactivity thus arose and were addressed in the paper, in this case attributed to microbial degradation and solute plant uptake. Our results suggest previously unknown features of fluorobenzoate compounds as hydrologic tracers, potentially interesting for catchment studies owing to their suitability for distinguishable multiple injections, and an outlook on direct experimental closures of mass balance in hydrologic transport volumes involving fluxes that are likely to sample differently stored water and solutes.

Petrophysical characterization of first ever drilled core samples from an active CO2 storage site, the German Ketzin Pilot Site - Comparison with long term experiments

NASA Astrophysics Data System (ADS)

Zemke, Kornelia; Liebscher, Axel

2014-05-01

Petrophysical properties like porosity and permeability are key parameters for a safe long-term storage of CO2 but also for the injection operation itself. These parameters may change during and/or after the CO2 injection due to geochemical reactions in the reservoir system that are triggered by the injected CO2. Here we present petrophysical data of first ever drilled cores from a newly drilled well at the active CO2 storage site - the Ketzin pilot site in the Federal State of Brandenburg, Germany. By comparison with pre-injection baseline data from core samples recovered prior to injection, the new samples provide the unique opportunity to evaluate the impact of CO2 on pore size related properties of reservoir and cap rocks at a real injection site under in-situ reservoir conditions. After injection of 61 000 tons CO2, an additional well was drilled and new rock cores were recovered. In total 100 core samples from the reservoir and the overlaying caprock were investigated by NMR relaxation. Permeability of 20 core samples was estimated by nitrogen and porosity by helium pycnometry. The determined data are comparable between pre-injection and post-injection core samples. The lower part of the reservoir sandstone is unaffected by the injected CO2. The upper part of the reservoir sandstone shows consistently slightly lower NMR porosity and permeability values in the post-injection samples when compared to the pre-injection data. This upper sandstone part is above the fluid level and CO2 present as a free gas phase and a possible residual gas saturation of the cores distorted the NMR results. The potash-containing drilling fluid can also influence these results: NMR investigation of twin samples from inner and outer parts of the cores show a reduced fraction of larger pores for the outer core samples together with lower porosities and T2 times. The drill mud penetration depth can be controlled by the added fluorescent tracer. Due to the heterogeneous character of the Stuttgart Formation it is difficult to estimate definite CO2 induced changes from petrophysical measurements. The observed changes are only minor. Several batch experiments on Ketzin samples drilled prior injection confirm the results from investigation of the in-situ rock cores. Core samples of the pre-injection wells were exposed to CO2 and brine in autoclaves over various time periods. Samples were characterized prior to and after the experiments by NMR and Mercury Injection Porosimetry (MIP). The results are consistent with the logging data and show only minor change. Unfortunately, also in these experiments observed mineralogical and petrophysical changes were within the natural heterogeneity of the Ketzin reservoir and precluded unequivocal conclusions. However, given the only minor differences between post-injection well and pre-injection well, it is reasonable to assume that the potential dissolution-precipitation processes appear to have no severe consequences on reservoir and cap rock integrity or on the injection behaviour. This is also in line with the continuously recorded injection operation parameter. These do not point to any changes in reservoir injectivity.|

Bi-directionally draining pore fluid extraction vessel

DOEpatents

Prizio, Joseph; Ritt, Alexander; Mower, Timothy E.; Rodine, Lonn

1991-01-01

The invention is used to extract pore fluid from porous solids through a combination of mechanical compression and inert-gas injection and comprises a piston for axially compressing samples to force water out, and top and bottom drainage plates for capturing the exuded water and using inert gas to force water to exit when the limits of mechanical compression have been reached.

The gas chromatographic determination of volatile fatty acids in wastewater samples: evaluation of experimental biases in direct injection method against thermal desorption method.

PubMed

Ullah, Md Ahsan; Kim, Ki-Hyun; Szulejko, Jan E; Cho, Jinwoo

2014-04-11

The production of short-chained volatile fatty acids (VFAs) by the anaerobic bacterial digestion of sewage (wastewater) affords an excellent opportunity to alternative greener viable bio-energy fuels (i.e., microbial fuel cell). VFAs in wastewater (sewage) samples are commonly quantified through direct injection (DI) into a gas chromatograph with a flame ionization detector (GC-FID). In this study, the reliability of VFA analysis by the DI-GC method has been examined against a thermal desorption (TD-GC) method. The results indicate that the VFA concentrations determined from an aliquot from each wastewater sample by the DI-GC method were generally underestimated, e.g., reductions of 7% (acetic acid) to 93.4% (hexanoic acid) relative to the TD-GC method. The observed differences between the two methods suggest the possibly important role of the matrix effect to give rise to the negative biases in DI-GC analysis. To further explore this possibility, an ancillary experiment was performed to examine bias patterns of three DI-GC approaches. For instance, the results of the standard addition (SA) method confirm the definite role of matrix effect when analyzing wastewater samples by DI-GC. More importantly, their biases tend to increase systematically with increasing molecular weight and decreasing VFA concentrations. As such, the use of DI-GC method, if applied for the analysis of samples with a complicated matrix, needs a thorough validation to improve the reliability in data acquisition. Copyright © 2014 Elsevier B.V. All rights reserved.

Respondent-driven sampling and the recruitment of people with small injecting networks.

PubMed

Paquette, Dana; Bryant, Joanne; de Wit, John

2012-05-01

Respondent-driven sampling (RDS) is a form of chain-referral sampling, similar to snowball sampling, which was developed to reach hidden populations such as people who inject drugs (PWID). RDS is said to reach members of a hidden population that may not be accessible through other sampling methods. However, less attention has been paid as to whether there are segments of the population that are more likely to be missed by RDS. This study examined the ability of RDS to capture people with small injecting networks. A study of PWID, using RDS, was conducted in 2009 in Sydney, Australia. The size of participants' injecting networks was examined by recruitment chain and wave. Participants' injecting network characteristics were compared to those of participants from a separate pharmacy-based study. A logistic regression analysis was conducted to examine the characteristics independently associated with having small injecting networks, using the combined RDS and pharmacy-based samples. In comparison with the pharmacy-recruited participants, RDS participants were almost 80% less likely to have small injecting networks, after adjusting for other variables. RDS participants were also more likely to have their injecting networks form a larger proportion of those in their social networks, and to have acquaintances as part of their injecting networks. Compared to those with larger injecting networks, individuals with small injecting networks were equally likely to engage in receptive sharing of injecting equipment, but less likely to have had contact with prevention services. These findings suggest that those with small injecting networks are an important group to recruit, and that RDS is less likely to capture these individuals.

Rock samples analysis with the pyrolysis system of the Mars Organic Molecule Analyzer (MOMA)

NASA Astrophysics Data System (ADS)

Steininger, H.; Goetz, W.; Goesmann, F.

2012-12-01

The Mars Organic Molecule Analyzer (MOMA) is a combined pyrolysis gas chromatograph mass spectrometer (GC-MS) and laser desorption mass spectrometer (LD-MS). It will be the key instrument of the ESA/Roscosmos ExoMars 2018 mission to search for extinct and extant life. Additionally the instrument will be able to detect the organic background which has possibly been delivered to Mars by meteorites. Several samples containing a wide range of organic molecules have been tested with a flight analog injection system. The results of the tests were compared to results obtained by a commercial pyrolysis system, the Pyrola pyrolysis unit. The first experimental setup (Pyrola unit) consists of a small quartz tube with an electrically heated platinum filament. A constant helium flow transports the volatilized compounds through an injection needle directly into the injector of the GC. The whole system is heated to 175°C. The second experimental setup (flight analog injection system) consists of a 6 mm diameter platinum oven connected to a microvalve plate to route the gas from the oven to the GC. The microvalves can be switched electrically. The volatiles are subsequently trapped in a cold trap consisting of a Tenax filed tube. Heating this tube releases the volatiles and injects them through an injection needle into the GC. A Varian 4000 GC-MS with RTX-5 column was used to separate and analyze the volatiles generated from both experimental setups. During the experiments several natural rock samples with a broad content of organic material have been analyzed. The sample material was crushed and ground. To obtain comparable results the same amount of sample was used in both setups. Lower temperatures were used in the flight analog injection system due to restrictions of the reusable oven. Lower temperatures normally lead to only a slight decrease in the very heavy and non-volatile compounds but do not change the overall appearance of the chromatogram. Significant differences in the amount and composition of organic compounds have been found in the GC traces. In the flight like configuration an increase of the light volatile compounds was observed especially for benzene and toluene. We want to acknowledge the support by DLR (FKZ 50QX1001).

Automated centrifugal-microfluidic platform for DNA purification using laser burst valve and coriolis effect.

PubMed

Choi, Min-Seong; Yoo, Jae-Chern

2015-04-01

We report a fully automated DNA purification platform with a micropored membrane in the channel utilizing centrifugal microfluidics on a lab-on-a-disc (LOD). The microfluidic flow in the LOD, into which the reagents are injected for DNA purification, is controlled by a single motor and laser burst valve. The sample and reagents pass successively through the micropored membrane in the channel when each laser burst valve is opened. The Coriolis effect is used by rotating the LOD bi-directionally to increase the purity of the DNA, thereby preventing the mixing of the waste and elution solutions. The total process from the lysed sample injection into the LOD to obtaining the purified DNA was finished within 7 min with only one manual step. The experimental result for Salmonella shows that the proposed microfluidic platform is comparable to the existing devices in terms of the purity and yield of DNA.

Aerosol mobility size spectrometer

DOEpatents

Wang, Jian; Kulkarni, Pramod

2007-11-20

A device for measuring aerosol size distribution within a sample containing aerosol particles. The device generally includes a spectrometer housing defining an interior chamber and a camera for recording aerosol size streams exiting the chamber. The housing includes an inlet for introducing a flow medium into the chamber in a flow direction, an aerosol injection port adjacent the inlet for introducing a charged aerosol sample into the chamber, a separation section for applying an electric field to the aerosol sample across the flow direction and an outlet opposite the inlet. In the separation section, the aerosol sample becomes entrained in the flow medium and the aerosol particles within the aerosol sample are separated by size into a plurality of aerosol flow streams under the influence of the electric field. The camera is disposed adjacent the housing outlet for optically detecting a relative position of at least one aerosol flow stream exiting the outlet and for optically detecting the number of aerosol particles within the at least one aerosol flow stream.

Characterization of Reactivity Controlled Compression Ignition (RCCI) Using Premixed Gasoline and Direct-Injected Gasoline with a Cetane Improver on a Multi-Cylinder Engine

DOE PAGES

Dempsey, Adam B.; Curran, Scott; Reitz, Rolf D.

2015-04-14

The focus of the present paper was to characterize Reactivity Controlled Compression Ignition (RCCI) using a single-fuel approach of gasoline and gasoline mixed with a commercially available cetane improver on a multi-cylinder engine. RCCI was achieved by port-injecting a certification grade 96 research octane gasoline and direct-injecting the same gasoline mixed with various levels of a cetane improver, 2-ethylhexyl nitrate (EHN). The EHN volume percentages investigated in the direct-injected fuel were 10, 5, and 2.5%. The combustion phasing controllability and emissions of the different fueling combinations were characterized at 2300 rpm and 4.2 bar brake mean effective pressure over amore » variety of parametric investigations including direct injection timing, premixed gasoline percentage, and intake temperature. Comparisons were made to gasoline/diesel RCCI operation on the same engine platform at nominally the same operating condition. The experiments were conducted on a modern four cylinder light-duty diesel engine that was modified with a port-fuel injection system while maintaining the stock direct injection fuel system. The pistons were modified for highly premixed operation and feature an open shallow bowl design. The results indicate that the authority to control the combustion phasing through the fuel delivery strategy (e.g., direct injection timing or premixed gasoline percentage) is not a strong function of the EHN concentration in the direct-injected fuel. It was also observed that NOx emissions are a strong function of the global EHN concentration in-cylinder and the combustion phasing. Finally, in general, NOx emissions are significantly elevated for gasoline/gasoline+EHN operation compared with gasoline/diesel RCCI operation at a given operating condition.« less

Electrokinetic focusing injection methods on microfluidic devices.

PubMed

Fu, Lung-Ming; Yang, Ruey-Jen; Lee, Gwo-Bin

2003-04-15

This paper presents an experimental and numerical investigation into electrokinetic focusing injection on microfluidic chips. The valving characteristics on microfluidic devices are controlled through appropriate manipulations of the electric potential strengths during the sample loading and dispensing steps. The present study also addresses the design and testing of various injection systems used to deliver a sample plug. A novel double-cross injection microfluidic chip is fabricated, which employs electrokinetic focusing to deliver sample plugs of variable volume. The proposed design combines several functions of traditional sample plug injection systems on a single microfluidic chip. The injection technique uses an unique sequence of loading steps with different electric potential distributions and magnitudes within the various channels to effectuate a virtual valve.

High-throughput microcoil NMR of compound libraries using zero-dispersion segmented flow analysis.

PubMed

Kautz, Roger A; Goetzinger, Wolfgang K; Karger, Barry L

2005-01-01

An automated system for loading samples into a microcoil NMR probe has been developed using segmented flow analysis. This approach enhanced 2-fold the throughput of the published direct injection and flow injection methods, improved sample utilization 3-fold, and was applicable to high-field NMR facilities with long transfer lines between the sample handler and NMR magnet. Sample volumes of 2 microL (10-30 mM, approximately 10 microg) were drawn from a 96-well microtiter plate by a sample handler, then pumped to a 0.5-microL microcoil NMR probe as a queue of closely spaced "plugs" separated by an immiscible fluorocarbon fluid. Individual sample plugs were detected by their NMR signal and automatically positioned for stopped-flow data acquisition. The sample in the NMR coil could be changed within 35 s by advancing the queue. The fluorocarbon liquid wetted the wall of the Teflon transfer line, preventing the DMSO samples from contacting the capillary wall and thus reducing sample losses to below 5% after passage through the 3-m transfer line. With a wash plug of solvent between samples, sample-to-sample carryover was <1%. Significantly, the samples did not disperse into the carrier liquid during loading or during acquisitions of several days for trace analysis. For automated high-throughput analysis using a 16-second acquisition time, spectra were recorded at a rate of 1.5 min/sample and total deuterated solvent consumption was <0.5 mL (1 US dollar) per 96-well plate.

Hydro-geophysical responses to the injection of CO2 in core plugs of Berea sandstone

NASA Astrophysics Data System (ADS)

Song, I.; Park, K. G.

2017-12-01

We have built a laboratory-scale core flooding system to measure the relative permeability of a core sample and the acoustic response to the CO2 saturation degree at in situ condition of pressure and temperature down to a few kilometer depths. The system consisted of an acoustic velocity core holder (AVC model from the Core Laboratories) between upstream where CO2 and H2O were injected separately and downstream where the mixed fluids came out of a core sample. Core samples with 4 cm in diameter and 5 cm in length of Berea sandstone were in turn placed in the core holder for confining and axial pressures. The flooding operations of the multiphase fluids were conducted through the sample at 40ºC in temperature and 8 MPa in backpressure. CO2 and H2O in the physical condition were injected separately into a sample at constant rate with various ratios. The two phases were mixed during flowing through the sample. The mixed fluids out of the sample were separated again by their different densities in a chamber equipped with a level gauge of the interface. From the level change of the water in the separator, we measured the volume of water coming out of the sample for each test with a constant ratio of the injection rates. Then it was possible to calculate the saturation degree of CO2 from the difference between input volume and output volume of water. The differential pressure between upstream and downstream was directly measured to calculate the relative permeability as a function of the CO2 saturation degree. We also conducted ultrasonic measurements using piezoelectric sensors on the end plugs. An electric pulse was given to a sensor on one end of sample, and then ultrasonic waves were recorded from the other end. The various ratios of injection rate of CO2 and H2O into Berea sandstone yielded a range of 0.1-0.7 in CO2 saturation degree. The relative permeability was obtained at the condition of steady-state flow for given stages from the velocity of each phase and the pressure gradient. The arrival time of P-wave became retarded and its amplitude became smaller as the degree of CO2 saturation increases. However no change was observed in S-wave in both characters. According to our results, time-lapse measurements of P-wave signals can be a monitoring tool of the subsurface migration of CO2, thus of detecting even its leakage.

The use of laser-induced fluorescence or ultraviolet detectors for sensitive and selective analysis of tobramycin or erythropoietin in complex samples

NASA Astrophysics Data System (ADS)

Ahmed, Hytham M.; Ebeid, Wael B.

2015-05-01

Complex samples analysis is a challenge in pharmaceutical and biopharmaceutical analysis. In this work, tobramycin (TOB) analysis in human urine samples and recombinant human erythropoietin (rhEPO) analysis in the presence of similar protein were selected as representative examples of such samples analysis. Assays of TOB in urine samples are difficult because of poor detectability. Therefore laser induced fluorescence detector (LIF) was combined with a separation technique, micellar electrokinetic chromatography (MEKC), to determine TOB through derivatization with fluorescein isothiocyanate (FITC). Borate was used as background electrolyte (BGE) with negative-charged mixed micelles as additive. The method was successively applied to urine samples. The LOD and LOQ for Tobramycin in urine were 90 and 200 ng/ml respectively and recovery was >98% (n = 5). All urine samples were analyzed by direct injection without sample pre-treatment. Another use of hyphenated analytical technique, capillary zone electrophoresis (CZE) connected to ultraviolet (UV) detector was also used for sensitive analysis of rhEPO at low levels (2000 IU) in the presence of large amount of human serum albumin (HSA). Analysis of rhEPO was achieved by the use of the electrokinetic injection (EI) with discontinuous buffers. Phosphate buffer was used as BGE with metal ions as additive. The proposed method can be used for the estimation of large number of quality control rhEPO samples in a short period.

An in vitro and in vivo investigation of the biological behavior of a ferrimagnetic cement for highly focalized thermotherapy.

PubMed

Portela, Ana; Vasconcelos, Mário; Branco, Rogério; Gartner, Fátima; Faria, Miguel; Cavalheiro, José

2010-08-01

The cancer treatment by local hyperthermia, using a high frequency electromagnetic field is an extensively studied subject. For this propose it was developed a ferrimagnetic cement (FC) to be injected directly into the tumor. In this study it was determined the FC injectability, its capability to generate heat when placed within a magnetic field and its interaction with a modified simulated body fluid using SEM/EDS and XRD. The FC biological response was assessed by the intramuscular implantation in rats and histological analysis of the surrounding tissues. The results suggest that FC can be injected directly into the tumor, its temperature can be increased when exposed to a magnetic field and the surface of the immersed samples quickly becomes coated with precipitate denoting its ionic change with the surrounding medium. The histological analysis revealed a transient local inflammatory reaction, similar to the control material, only slightly more abundant during the first weeks, with a gradual decrease over the implantation time. Based on these results, we concluded that FC might be useful for highly focalized thermotherapy, with a good potential for clinical use.

Simulation of elution profiles in liquid chromatography - II: Investigation of injection volume overload under gradient elution conditions applied to second dimension separations in two-dimensional liquid chromatography.

PubMed

Stoll, Dwight R; Sajulga, Ray W; Voigt, Bryan N; Larson, Eli J; Jeong, Lena N; Rutan, Sarah C

2017-11-10

An important research direction in the continued development of two-dimensional liquid chromatography (2D-LC) is to improve the detection sensitivity of the method. This is especially important in applications where injection of large volumes of effluent from the first dimension ( 1 D) column into the second dimension ( 2 D) column leads to severe 2 D peak broadening and peak shape distortion. For example, this is common when coupling two reversed-phase columns and the organic solvent content of the 1 D mobile phase overwhelms the 2 D column with each injection of 1 D effluent, leading to low resolution in the second dimension. In a previous study we validated a simulation approach based on the Craig distribution model and adapted from the work of Czok and Guiochon [1] that enabled accurate simulation of simple isocratic and gradient separations with very small injection volumes, and isocratic separations with mismatched injection and mobile phase solvents [2]. In the present study we have extended this simulation approach to simulate separations relevant to 2D-LC. Specifically, we have focused on simulating 2 D separations where gradient elution conditions are used, there is mismatch between the sample solvent and the starting point in the gradient elution program, injection volumes approach or even exceed the dead volume of the 2 D column, and the extent of sample loop filling is varied. To validate this simulation we have compared results from simulations and experiments for 101 different conditions, including variation in injection volume (0.4-80μL), loop filling level (25-100%), and degree of mismatch between sample organic solvent and the starting point in the gradient elution program (-20 to +20% ACN). We find that that the simulation is accurate enough (median errors in retention time and peak width of -1.0 and -4.9%, without corrections for extra-column dispersion) to be useful in guiding optimization of 2D-LC separations. However, this requires that real injection profiles obtained from 2D-LC interface valves are used to simulate the introduction of samples into the 2 D column. These profiles are highly asymmetric - simulation using simple rectangular pulses leads to peak widths that are far too narrow under many conditions. We believe the simulation approach developed here will be useful for addressing practical questions in the development of 2D-LC methods. Copyright © 2017 Elsevier B.V. All rights reserved.

Optimization of throughput in semipreparative chiral liquid chromatography using stacked injection.

PubMed

Taheri, Mohammadreza; Fotovati, Mohsen; Hosseini, Seyed-Kiumars; Ghassempour, Alireza

2017-10-01

An interesting mode of chromatography for preparation of pure enantiomers from pure samples is the method of stacked injection as a pseudocontinuous procedure. Maximum throughput and minimal production costs can be achieved by the use of total chiral column length in this mode of chromatography. To maximize sample loading, often touching bands of the two enantiomers is automatically achieved. Conventional equations show direct correlation between touching-band loadability and the selectivity factor of two enantiomers. The important question for one who wants to obtain the highest throughput is "How to optimize different factors including selectivity, resolution, run time, and loading of the sample in order to save time without missing the touching-band resolution?" To answer this question, tramadol and propranolol were separated on cellulose 3,5-dimethyl phenyl carbamate, as two pure racemic mixtures with low and high solubilities in mobile phase, respectively. The mobile phase composition consisted of n-hexane solvent with alcohol modifier and diethylamine as the additive. A response surface methodology based on central composite design was used to optimize separation factors against the main responses. According to the stacked injection properties, two processes were investigated for maximizing throughput: one with a poorly soluble and another with a highly soluble racemic mixture. For each case, different optimization possibilities were inspected. It was revealed that resolution is a crucial response for separations of this kind. Peak area and run time are two critical parameters in optimization of stacked injection for binary mixtures which have low solubility in the mobile phase. © 2017 Wiley Periodicals, Inc.

Pushing quantitation limits in micro UHPLC-MS/MS analysis of steroid hormones by sample dilution using high volume injection.

PubMed

Márta, Zoltán; Bobály, Balázs; Fekete, Jenő; Magda, Balázs; Imre, Tímea; Mészáros, Katalin Viola; Szabó, Pál Tamás

2016-09-10

Ultratrace analysis of sample components requires excellent analytical performance in terms of limits of quantitation (LoQ). Micro UHPLC coupling with sensitive tandem mass spectrometry provides state of the art solutions for such analytical problems. Decreased column volume in micro LC limits the injectable sample volume. However, if analyte concentration is extremely low, it might be necessary to inject high sample volumes. This is particularly critical for strong sample solvents and weakly retained analytes, which are often the case when preparing biological samples (protein precipitation, sample extraction, etc.). In that case, high injection volumes may cause band broadening, peak distortion or even elution in dead volume. In this study, we evaluated possibilities of high volume injection onto microbore RP-LC columns, when sample solvent is diluted. The presented micro RP-LC-MS/MS method was optimized for the analysis of steroid hormones from human plasma after protein precipitation with organic solvents. A proper sample dilution procedure helps to increase the injection volume without compromising peak shapes. Finally, due to increased injection volume, the limit of quantitation can be decreased by a factor of 2-5, depending on the analytes and the experimental conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

Sampling and analytical methods of stable isotopes and dissolved inorganic carbon from CO2 injection sites

NASA Astrophysics Data System (ADS)

van Geldern, Robert; Myrttinen, Anssi; Becker, Veith; Barth, Johannes A. C.

2010-05-01

The isotopic composition (δ13C) of dissolved inorganic carbon (DIC), in combination with DIC concentration measurements, can be used to quantify geochemical trapping of CO2 in water. This is of great importance in monitoring the fate of CO2 in the subsurface in CO2 injection projects. When CO2 mixes with water, a shift in the δ13C values, as well as an increase in DIC concentrations is observed in the CO2-H2O system. However, when using standard on-site titration methods, it is often challenging to determining accurate in-situ DIC concentrations. This may be due to CO2 degassing and CO2-exchange between the sample and the atmosphere during titration, causing a change in the pH value or due to other unfavourable conditions such as turbid water samples or limited availability of fluid samples. A way to resolve this problem is by simultaneously determining the DIC concentration and carbon isotopic composition using a standard continuous flow Isotope Ratio Mass Spectrometry (CF-IRMS) setup with a Gasbench II coupled to Delta plusXP mass spectrometer. During sampling, in order to avoid atmospheric contact, water samples taken from the borehole-fluid-sampler should be directly transferred into a suitable container, such as a gasbag. Also, to avoid isotope fractionation due to biological activity in the sample, it is recommended to stabilize the gasbags prior to sampling with HgCl2 for the subsequent stable isotope analysis. The DIC concentration of the samples can be determined from the area of the sample peaks in a chromatogram from a CF-IRMS analysis, since it is directly proportional to the CO2 generated by the reaction of the water with H3PO4. A set of standards with known DIC concentrations should be prepared by mixing NaHCO3 with DIC free water. Since the DIC concentrations of samples taken from CO2 injection sites are expected to be exceptionally high due to the additional high amounts of added CO2, the DIC concentration range of the standards should be set high enough to cover the sample concentrations. In order to assure methodological reproducibility, this 'calibration set' should be included in every sequence analysed with the Gasbench CF-IRMS system. The standards, therefore, should also be treated in the same way as the samples. For accurate determination, it is essential to know the exact amount of water in the vial and the density of the sample. This requires weighing of each vial before and after injection of the water sample. For stable isotope analysis, the required signal height can be adjusted by the sample amount. Therefore this method is suitable for analysing samples with highly differing DIC concentrations. Reproducibility and accuracy of the quantitative analysis of the dissolved inorganic carbon need to be verified by independent control standards, treated as samples. This study was conducted as a part of the R&D programme CLEAN, which is funded by the German Federal Ministry of Education in the framework of the programme GEOTECHNOLOGIEN. We would like to thank GDF SUEZ for permitting us to conduct sampling campaigns at their site.

Injection Drug Users’ Involvement In Drug Economy: Dynamics of Sociometric and Egocentric Social Networks

PubMed Central

Yang, Cui; Latkin, Carl; Muth, Stephen Q.; Rudolph, Abby

2014-01-01

The purpose of this analysis was to examine the effect of social network cohesiveness on drug economy involvement, and to test whether this relationship is mediated by drug support network size in a sample of active injection drug users. Involvement in the drug economy was defined by self-report of participation in at least one of the following activities: selling drugs, holding drugs or money for drugs, providing street security for drug sellers, cutting/packaging/cooking drugs, selling or renting drug paraphernalia (e.g., pipes, tools, rigs), and injecting drugs in others’ veins. The sample consists of 273 active injection drug users in Baltimore, Maryland who reported having injected drugs in the last 6 months and were recruited through either street outreach or by their network members. Egocentric drug support networks were assessed through a social network inventory at baseline. Sociometric networks were built upon the linkages by selected matching characteristics, and k-plex rank was used to characterize the level of cohesiveness of the individual to others in the social network. Although no direct effect was observed, structural equation modeling indicated k-plex rank was indirectly associated with drug economy involvement through drug support network size. These findings suggest the effects of large-scale sociometric networks on injectors’ drug economy involvement may occur through their immediate egocentric networks. Future harm reduction programs for injection drug users (IDUs) should consider providing programs coupled with economic opportunities to those drug users within a cohesive network subgroup. Moreover, individuals with a high connectivity to others in their network may be optimal individuals to train for diffusing HIV prevention messages. PMID:25309015

Theoretical studies on a new pattern of laser-driven systems: towards elucidation of direct photo-injection in dye-sensitized solar cells

NASA Astrophysics Data System (ADS)

Mishima, Kenji; Yamashita, Koichi

2011-03-01

We theoretically and numerically investigated a new type of analytically solvable laser-driven systems inspired by electron-injection dynamics in dye-sensitized solar cells. The simple analytical expressions were found to be useful for understanding the difference between dye excitation and direct photo-injection occurring between dye molecule and semiconductor nanoparticles. More importantly, we propose a method for discriminating experimentally dye excitation and direct photo-injection by using time-dependent fluorescence. We found that dye excitation shows no significant quantum beat whereas the direct photo-injection shows a significant quantum beat. This work was supported by Funding Program for World-Leading Innovative R&D on Science and Technology (FIRST) ``Development of Organic Photovoltaics toward a Low-Carbon Society,'' Cabinet Office, Japan.

Dry low NOx combustion system with pre-mixed direct-injection secondary fuel nozzle

DOEpatents

Zuo, Baifang; Johnson, Thomas; Ziminsky, Willy; Khan, Abdul

2013-12-17

A combustion system includes a first combustion chamber and a second combustion chamber. The second combustion chamber is positioned downstream of the first combustion chamber. The combustion system also includes a pre-mixed, direct-injection secondary fuel nozzle. The pre-mixed, direct-injection secondary fuel nozzle extends through the first combustion chamber into the second combustion chamber.

Miniaturized flow injection analysis system

DOEpatents

Folta, J.A.

1997-07-01

A chemical analysis technique known as flow injection analysis is described, wherein small quantities of chemical reagents and sample are intermixed and reacted within a capillary flow system and the reaction products are detected optically, electrochemically, or by other means. A highly miniaturized version of a flow injection analysis system has been fabricated utilizing microfabrication techniques common to the microelectronics industry. The microflow system uses flow capillaries formed by etching microchannels in a silicon or glass wafer followed by bonding to another wafer, commercially available microvalves bonded directly to the microflow channels, and an optical absorption detector cell formed near the capillary outlet, with light being both delivered and collected with fiber optics. The microflow system is designed mainly for analysis of liquids and currently measures 38{times}25{times}3 mm, but can be designed for gas analysis and be substantially smaller in construction. 9 figs.

Direct chemiluminescence of carbon dots induced by potassium ferricyanide and its analytical application

NASA Astrophysics Data System (ADS)

Amjadi, Mohammad; Manzoori, Jamshid L.; Hallaj, Tooba; Sorouraddin, Mohammad H.

2014-03-01

The chemiluminescence (CL) of water-soluble fluorescent carbon dots (C-dots) induced by direct chemical oxidation was investigated. C-dots were prepared by solvothermal method and characterized by fluorescence spectra and transmission electron microscopy. It was found that K3Fe(CN)6 could directly oxidize C-dots to produce a relatively intense CL emission. The mechanism of CL generation was investigated based on the fluorescence and CL emission spectra and the effect of radical scavengers on the CL intensity. The inhibitive effect of some metal ions and biologically important molecules on the CL intensity of the system was examined and the potential of the system for the determination of these species at trace levels was studied. In order to evaluate the capability of method to real sample analysis, it was applied to the determination of Cr(VI) and adrenaline in water and injection samples, respectively.

Polyion selective polymeric membrane-based pulstrode as a detector in flow-injection analysis.

PubMed

Bell-Vlasov, Andrea K; Zajda, Joanna; Eldourghamy, Ayman; Malinowska, Elzbieta; Meyerhoff, Mark E

2014-04-15

A method for the detection of polyions using fully reversible polyion selective polymeric membrane type pulstrodes as detectors in a flow-injection analysis (FIA) system is examined. The detection electrode consists of a plasticized polymeric membrane doped with 10 wt % of tridodecylmethylammonium-dinonylnaphthalene sulfonate (TDMA/DNNS) ion-exchanger salt. The pulse sequence used involves a short (1 s) galvanostatic pulse, an open-circuit pulse (0.5 s) during which the EMF of the cell is measured, and a longer (15 s) potentiostatic pulse to return the membrane to its original chemical composition. It is shown that total pulse sequence times can be optimized to yield reproducible real-time detection of injected samples of protamine and heparin at up to 20 samples/h. Further, it is shown that the same membrane detector can be employed for FIA detection of both polycations at levels ≥10 μg/mL and polyanions at levels of ≥40 μg/mL by changing the direction of the galvanostatic pulse. The methodology described may also be applicable in the detection of polyionic species at low levels in other flowing configurations, such as in liquid chromatography and capillary electrophoresis.

Evaluating outcome-correlated recruitment and geographic recruitment bias in a respondent-driven sample of people who inject drugs in Tijuana, Mexico.

PubMed

Rudolph, Abby E; Gaines, Tommi L; Lozada, Remedios; Vera, Alicia; Brouwer, Kimberly C

2014-12-01

Respondent-driven sampling's (RDS) widespread use and reliance on untested assumptions suggests a need for new exploratory/diagnostic tests. We assessed geographic recruitment bias and outcome-correlated recruitment among 1,048 RDS-recruited people who inject drugs (Tijuana, Mexico). Surveys gathered demographics, drug/sex behaviors, activity locations, and recruiter-recruit pairs. Simulations assessed geographic and network clustering of active syphilis (RPR titers ≥1:8). Gender-specific predicted probabilities were estimated using logistic regression with GEE and robust standard errors. Active syphilis prevalence was 7 % (crude: men = 5.7 % and women = 16.6 %; RDS-adjusted: men = 6.7 % and women = 7.6 %). Syphilis clustered in the Zona Norte, a neighborhood known for drug and sex markets. Network simulations revealed geographic recruitment bias and non-random recruitment by syphilis status. Gender-specific prevalence estimates accounting for clustering were highest among those living/working/injecting/buying drugs in the Zona Norte and directly/indirectly connected to syphilis cases (men: 15.9 %, women: 25.6 %) and lowest among those with neither exposure (men: 3.0 %, women: 6.1 %). Future RDS analyses should assess/account for network and spatial dependencies.

Effect of suppressor current intensity on the determination of glyphosate and aminomethylphosphonic acid by suppressed conductivity ion chromatography.

PubMed

Dimitrakopoulos, Ioannis K; Thomaidis, Nikolaos S; Megoulas, Nikolaos C; Koupparis, Michael A

2010-05-28

This paper presents the application of ion chromatography with electrolytic eluent generation and mobile phase suppression for the direct conductimetric detection of glyphosate and its degradation product aminomethylphosphonic acid (AMPA). The compounds were separated on a Dionex AS18 anion exchange column with a 12-40 mM KOH step gradient from 9 to 9.5 min. The effect of the suppressor current intensity on the electrostatic interaction of these amphoteric compounds with the suppressor cation exchange membranes was evaluated. A suppressor current gradient technique was proposed for the limitation of peak broadening and baseline noise, in order to improve method sensitivity and detectability. It was observed that residual sample carbonates co-eluted with AMPA when a large injection loop was installed for the low level determination of both compounds in natural waters. For this reason, glyphosate was isocratically eluted using 33 mM KOH in order to decrease analysis time within 10 min and a column clean up step using 100 mM KOH was used to ensure retention time reproducibility. The developed method was applied to the analysis of drinking and natural water and it was further successfully applied to orange samples with slight modifications. Instrumental LOD for glyphosate was 0.24 microg/L, while method LOD was 0.54 microg/L for spring waters and 0.01 mg/kg for oranges using a 1000 microL direct loop injection of the sample. Intra-day and inter-day precision (as %RSD) for water samples was 4.6% and 12% at a spiking level of 2 microg/L, and the recovery ranged from 64% to 88% depending on sample conductivity. For orange samples, the inter-day precision was 1.4% at a spiking level of 4.4 mg/kg, while overall recovery was 103%. The developed method is direct, fast, sensitive and relatively inexpensive, and could be used as an ideal fast screening tool for the monitoring of glyphosate residues in water and fruit samples. Copyright 2010 Elsevier B.V. All rights reserved.

Direct Gallbladder Indocyanine Green Injection Fluorescence Cholangiography During Laparoscopic Cholecystectomy.

PubMed

Graves, Claire; Ely, Sora; Idowu, Olajire; Newton, Christopher; Kim, Sunghoon

2017-10-01

Intravenous injection of indocyanine green (ICG) is used to illuminate extrahepatic biliary anatomy. Fluorescence of biliary structures may lower surgical complications that can arise due to inadvertent injury to the common bile duct. We describe a method of injecting ICG directly into the gallbladder to define the cystic duct and common bile duct anatomy. A standard laparoscopic cholecystectomy was performed using a laparoscope with near-infrared imaging capability. Before dissection, the gallbladder was punctured with a cholangiogram catheter or a pigtail catheter to aspirate the bile within the gallbladder. The aspirated bile is mixed with ICG solution, which is reinjected into the gallbladder to fluoresce the gallbladder, cystic duct, and common bile duct structures. Eleven patients underwent direct gallbladder ICG injection for fluorescence cholangiography during cholecystectomy. Direct gallbladder ICG injection clearly defined the extrahepatic biliary anatomy, including the cystic duct-common bile duct junction, by fluorescence. In addition, the dissection plane between the gallbladder and the liver is highlighted with the gallbladder ICG fluorescence. Direct gallbladder ICG injection provides immediate visualization of extrahepatic biliary structures and clarifies the dissection plane between the gallbladder and the liver bed.

Characterization of quantum interference control of injected currents in LT-GaAs for carrier-envelope phase measurements.

PubMed

Roos, Peter; Quraishi, Qudsia; Cundiff, Steven; Bhat, Ravi; Sipe, J

2003-08-25

We use two mutually coherent, harmonically related pulse trains to experimentally characterize quantum interference control (QIC) of injected currents in low-temperature-grown gallium arsenide. We observe real-time QIC interference fringes, optimize the QIC signal fidelity, uncover critical signal dependences regarding beam spatial position on the sample, measure signal dependences on the fundamental and second harmonic average optical powers, and demonstrate signal characteristics that depend on the focused beam spot sizes. Following directly from our motivation for this study, we propose an initial experiment to measure and ultimately control the carrier-envelope phase evolution of a single octave-spanning pulse train using the QIC phenomenon.

Updates to Simulation of a Single-Element Lean-Direct Injection Combustor Using a Polyhedral Mesh Derived From Hanging-Node Elements

NASA Technical Reports Server (NTRS)

Wey, Changju Thomas; Liu, Nan-Suey

2014-01-01

This paper summarizes the procedures of inserting a thin-layer mesh to existing inviscid polyhedral mesh either with or without hanging-node elements as well as presents sample results from its applications to the numerical solution of a single-element LDI combustor using a releasable edition of the National Combustion Code (NCC).

Updates to Simulation of a Single-Element Lean-Direct Injection Combustor Using a Polyhedral Mesh Derived from Hanging-Node Elements

NASA Technical Reports Server (NTRS)

Wey, Thomas; Liu, Nan-Suey

2014-01-01

This paper summarizes the procedures of inserting a thin-layer mesh to existing inviscid polyhedral mesh either with or without hanging-node elements as well as presents sample results from its applications to the numerical solution of a single-element LDI combustor using a releasable edition of the National Combustion Code (NCC).

Analysis of volatile organic compounds. [trace amounts of organic volatiles in gas samples

NASA Technical Reports Server (NTRS)

Zlatkis, A. (Inventor)

1977-01-01

An apparatus and method are described for reproducibly analyzing trace amounts of a large number of organic volatiles existing in a gas sample. Direct injection of the trapped volatiles into a cryogenic percolum provides a sharply defined plug. Applications of the method include: (1) analyzing the headspace gas of body fluids and comparing a profile of the organic volatiles with standard profiles for the detection and monitoring of disease; (2) analyzing the headspace gas of foods and beverages and comparing the profile with standard profiles to monitor and control flavor and aroma; and (3) analyses for determining the organic pollutants in air or water samples.

The assesment of effectiveness of plasmonic resonance photothermal therapy in tumor-bearing rats after multiple intravenous administration of gold nanorods

NASA Astrophysics Data System (ADS)

Bucharskaya, Alla B.; Maslyakova, Galina N.; Navolokin, Nikita A.; Terentyuk, Georgy S.; Khlebtsov, Boris N.; Khlebtsov, Nikolai G.; Bashkatov, Alexey N.; Genina, Elina A.; Tuchin, V. V.

2017-03-01

To assess the effectiveness of plasmonic photothermal therapy (PPT) multiple intravenous strategy of gold nanorods (GNRs) administration was used before laser exposure. The model of alveolar liver cancer PC-1 was used in male outbred albino rats, which were intravenously administrated by single and multiple injections of GNRs and then were treated by PPT. The gold dosage was 400 μg (single injection group), 800 μg (double injection group), 1200 μg (triple injection group), and absorption maximum of gold nanorods suspension was at the wavelength of 808 nm. 24 hours after last injection the tumors were irradiated by the 808-nm diode laser during 15 min at power density 2.3 W/cm2. Temperature control of the tumor heating was provided by IR imager. 24 hours after the PPT the half of animals from each group was withdrawn from the experiments and the sampling tumor tissue for morphological study was performed. In survived animals the growth of tumors was evaluated during 21 days after the PPT. The antitumor effects of PPT after triple intravenous injection were comparable with those obtained at direct intratumoral administration of similar total dose of GNRs. The effectiveness of PPT depended on gold accumulation in tumor, probably, due to sufficient vascularization of tumor tissue.

Paraffin wax removal from metal injection moulded cocrmo alloy compact by solvent debinding process

NASA Astrophysics Data System (ADS)

Dandang, N. A. N.; Harun, W. S. W.; Khalil, N. Z.; Ahmad, A. H.; Romlay, F. R. M.; Johari, N. A.

2017-10-01

One of the most crucial and time consuming phase in metal injection moulding (MIM) process is “debinding”. These days, in metal injection moulding process, they had recounted that first debinding practice was depend on thermal binder degradation, which demanding more than 200 hours for complete removal of binder. Fortunately, these days world had introduced multi-stage debinding techniques to simplified the debinding time process. This research study variables for solvent debinding which are temperature and soaking time for samples made by MIM CoCrMo powder. Since wax as the key principal in the binder origination, paraffin wax will be removed together with stearic acid from the green bodies. Then, debinding process is conducted at 50, 60 and 70°C for 30-240 minutes. It is carried out in n-heptane solution. Percentage weight loss of the binder were measured. Lastly, scanning electron microscope (SEM) analysis and visual inspection were observed for the surface of brown compact. From the results, samples debound at 70°C exhibited a significant amount of binder loss; nevertheless, sample collapse, brittle surface and cracks were detected. But, at 60°C temperature and time of 4 hours proven finest results as it shows sufficient binder loss, nonappearance of surface cracks and easy to handle. Overall, binder loss is directly related to solvent debinding temperature and time.

Ducted fuel injection: A new approach for lowering soot emissions from direct-injection engines

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

Mueller, Charles J.; Nilsen, Christopher W.; Ruth, Daniel J.

Designers of direct-injection compression-ignition engines use a variety of strategies to improve the fuel/charge-gas mixture within the combustion chamber for increased efficiency and reduced pollutant emissions. Strategies include the use of high fuel-injection pressures, multiple injections, small injector orifices, flow swirl, long-ignition-delay conditions, and oxygenated fuels. This is the first journal publication paper on a new mixing-enhancement strategy for emissions reduction: ducted fuel injection. The concept involves injecting fuel along the axis of a small cylindrical duct within the combustion chamber, to enhance the mixture in the autoignition zone relative to a conventional free-spray configuration (i.e., a fuel spray thatmore » is not surrounded by a duct). Finally, the results described herein, from initial proof-of-concept experiments conducted in a constant-volume combustion vessel, show dramatically lower soot incandescence from ducted fuel injection than from free sprays over a range of charge-gas conditions that are representative of those in modern direct-injection compression-ignition engines.« less

Ducted fuel injection: A new approach for lowering soot emissions from direct-injection engines

DOE PAGES

Mueller, Charles J.; Nilsen, Christopher W.; Ruth, Daniel J.; ...

2017-07-18

Designers of direct-injection compression-ignition engines use a variety of strategies to improve the fuel/charge-gas mixture within the combustion chamber for increased efficiency and reduced pollutant emissions. Strategies include the use of high fuel-injection pressures, multiple injections, small injector orifices, flow swirl, long-ignition-delay conditions, and oxygenated fuels. This is the first journal publication paper on a new mixing-enhancement strategy for emissions reduction: ducted fuel injection. The concept involves injecting fuel along the axis of a small cylindrical duct within the combustion chamber, to enhance the mixture in the autoignition zone relative to a conventional free-spray configuration (i.e., a fuel spray thatmore » is not surrounded by a duct). Finally, the results described herein, from initial proof-of-concept experiments conducted in a constant-volume combustion vessel, show dramatically lower soot incandescence from ducted fuel injection than from free sprays over a range of charge-gas conditions that are representative of those in modern direct-injection compression-ignition engines.« less

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

Dempsey, Adam B.; Curran, Scott; Reitz, Rolf D.

The focus of the present paper was to characterize Reactivity Controlled Compression Ignition (RCCI) using a single-fuel approach of gasoline and gasoline mixed with a commercially available cetane improver on a multi-cylinder engine. RCCI was achieved by port-injecting a certification grade 96 research octane gasoline and direct-injecting the same gasoline mixed with various levels of a cetane improver, 2-ethylhexyl nitrate (EHN). The EHN volume percentages investigated in the direct-injected fuel were 10, 5, and 2.5%. The combustion phasing controllability and emissions of the different fueling combinations were characterized at 2300 rpm and 4.2 bar brake mean effective pressure over amore » variety of parametric investigations including direct injection timing, premixed gasoline percentage, and intake temperature. Comparisons were made to gasoline/diesel RCCI operation on the same engine platform at nominally the same operating condition. The experiments were conducted on a modern four cylinder light-duty diesel engine that was modified with a port-fuel injection system while maintaining the stock direct injection fuel system. The pistons were modified for highly premixed operation and feature an open shallow bowl design. The results indicate that the authority to control the combustion phasing through the fuel delivery strategy (e.g., direct injection timing or premixed gasoline percentage) is not a strong function of the EHN concentration in the direct-injected fuel. It was also observed that NOx emissions are a strong function of the global EHN concentration in-cylinder and the combustion phasing. Finally, in general, NOx emissions are significantly elevated for gasoline/gasoline+EHN operation compared with gasoline/diesel RCCI operation at a given operating condition.« less

Legionnaires' Disease Bacteria in power plant cooling systems: downtime report. Final report

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

Tyndall, R.L.; Solomon, J.A.; Christensen, S.W.

1985-04-01

Legionnaires' Disease Bacteria (Legionella) are a normal part of the aquatic community that, when aerosolized, can be pathogenic to man. The downtime study was designed to determine the degree to which Legionella populations are aerosolized during cleaning and maintenance operations in a closed-cycle steam-electric power plant. Both high-volume and impinger air samples were collected prior to and during downtime operations. Emphasis was placed on sampling inside or adjacent to water boxes, condensers, and cooling towers. Control air samples were taken upwind from the plant site. Water and sludge samples were also collected at various locations. In the laboratory, the concentrationsmore » of Groups A, B, and C Legionella were determined using the direct fluorescent antibody method. All positive air samples, and other selected air samples, were injected into guinea pigs to detect infectious Legionella. Legionella could be detected in only 12 of the 126 air samples collected. These were predominantly Group A Legionella (L. pneumophila, serogroups 1 to 6). All 12 positive samples had been collected in the vicinity of water boxes, condensers, detention ponds, and cooling towers during downtime operations where aerosolization of Legionella populations would be expected. None of the air samples yielded infectious Legionella when injected into guinea pigs. Detection of Legionella in air samples taken during downtime was significantly more likely than detection during normal operating conditions (p <0.01). 13 refs., 4 figs., 10 tabs.« less

Liquid chromatography-tandem mass spectrometry direct injection analysis of organophosphorus flame retardants in Ontario surface water and wastewater effluent.

PubMed

Hao, Chunyan; Helm, Paul A; Morse, David; Reiner, Eric J

2018-01-01

Organophosphorus flame retardants (OPFRs) started to be used in plastics, electronics and furnishings back in the 1960s and became popular again last decade. They are now widely present in the environment and regarded as "new" emerging organic pollutants. An effective liquid chromatography-tandem mass spectrometry (LC-MS/MS) direct injection analysis (DIA) method was developed to monitor OPFR levels in aquatic environment. The removal of sample extraction and concentration steps not only improved operation efficiency, but also reduced the potential contamination commonly observed during the sample preparation process before. Positive background signals from the analytical instrument were eliminated by employing a "trap" column in front of the sample injector while an ACE C18 and an ACE C18-PFP column were compared for the separation of OPFRs. Nineteen OPFR related compounds were evaluated and rapid signal drops were observed for seven of them including TOTP, TMTP, TPTP, TEHP, T35DMPP, T2iPPP and EHDP, due to their low water solubility. The other twelve compounds, TMP, TEP, TPrP, TiPP, TBP, TCEP, TCPP, TDCPP, TPP, TBEP, BDCP and BEHP, were included for the measurement of OPFRs in drinking water, surface water, ground water and wastewater effluent samples. The instrumental detection limits of these twelve OPFRs at signal-to-noise ≥3 were in the 1.5-30 ng/L range. The method was applied for the determination of OPFRs in surface water and wastewater samples in Ontario, Canada, and BEHP, TBEP, TBP, TCEP, TCPP, TDCPP, and TEP were commonly detected. Crown Copyright © 2017. Published by Elsevier Ltd. All rights reserved.

Reservoir fluid and gas chemistry during CO2 injection at the Cranfield field, Mississippi, USA

NASA Astrophysics Data System (ADS)

Lu, J.; Kharaka, Y. K.; Cole, D. R.; Horita, J.; Hovorka, S.

2009-12-01

At Cranfield field, Mississippi, USA, a monitored CO2-EOR project provides a unique opportunity to understand geochemical interactions of injected CO2 within the reservoir. Cranfield field, discovered in 1943, is a simple anticlinal four-way closure and had a large gas cap surrounded by an oil ring (Mississippi Oil and Gas Board, 1966). The field was abandoned in 1966. The reservoir returned to original reservoir pressure (hydrostatic pressure) by a strong aquifer drive by 2008. The reservoir is in the lower Tuscaloosa Formation at depths of more than 3000 m. It is composed of stacked and incised channel fills and is highly heterogeneous vertically and horizontally. A variable thickness (5 to 15 m) of terrestrial mudstone directly overlies the basal sandstone providing the primary seal, isolating the injection interval from a series of fluvial sand bodies occurring in the overlying 30 m of section. Above these fluvial channels, the marine mudstone of the Middle Tuscaloosa forms a continuous secondary confining system of approximately 75 m. The sandstones of the injection interval are rich in iron, containing abundant diagenetic chamosite (ferroan chlorite), hematite and pyrite. Geochemical modeling suggests that the iron-bearing minerals will be dissolved in the face of high CO2 and provide iron for siderite precipitation. CO2 injection by Denbury Resources Inc. begun in mid-July 2008 on the north side of the field with rates at ~500,000 tones per year. Water and gas samples were taken from seven production wells after eight months of CO2 injection. Gas analyses from three wells show high CO2 concentrations (up to 90 %) and heavy carbon isotopic signatures similar to injected CO2, whereas the other wells show original gas composition and isotope. The mixing ratio between original and injected CO2 is calculated based on its concentration and carbon isotope. However, there is little variation in fluid samples between the wells which have seen various levels of CO2. Comparison between preinjection and postinjection fluid analyses also shows little difference. It suggests that CO2 injection has not induced significant mineral-water reactions to change water chemistry. In October 2009, CO2 will be injected into the down-dip, non-productive Tuscaloosa Formation on the east side of the same field. In-situ fluid and gas samples will be collected using downhole U-tube. Fluid chemistry data through time will reveal mineral reactions during and after injection and confine timescales of the interactions. This project was funded thought the National Energy Technology Laboratory Regional Carbon Sequestration Partnership Program as part of the Southeast Regional Carbon Sequestration Partnership.

QUANTITATIVE ANALYSIS OF 68 POLAR COMPOUNDS FROM TEN CHEMICAL CLASSES BY DIRECT AQUEOUS INJECTION GAS CHROMATOGRAPHY

EPA Science Inventory

Porous polymer packings have been used successfully in many applications of direct aqueous injection gas chromatography. The authors have expanded the use of aqueous injection to the quantitative analysis of 68 alcohols, acetates, ketones, ethers, sulfides, aldehydes, diols, dion...

Chemical and sensorial aroma characterization of freshly distilled Calvados. 1. Evaluation of quality and defects on the basis of key odorants by olfactometry and sensory analysis.

PubMed

Guichard, Hugues; Lemesle, Stéphane; Ledauphin, Jérôme; Barillier, Daniel; Picoche, Bernard

2003-01-15

Eight freshly distilled samples of Calvados, a fermented and distilled apple juice, were analyzed by sensory evaluation and direct injection GC to determine the composition of higher alcohols, esters, and aldehydes. The composition determined by direct injection was tentatively related to sensory descriptors. Esters have a probable maximum level around 500 g/hl of pure alcohol (PA). This level also corresponds to the threshold of the main ester constituent, ethyl acetate. A high ratio of esters to ethyl acetate seems to be of prime importance for good quality. Total aldehydes, with a maximum level between 8 and 11 g/hl of PA and mainly comprising acetal (maximum between 5 and 9 g/hl of PA), were related to a "green" descriptor. Higher alcohols do not have a direct impact on quality, but other volatile compounds with a positive impact on flavor should probably be present at a high level. As overall quality was not well related to sensory quality, it was necessary to perform more a precise analysis to determine the key odorants. The Calvados samples were thus extracted using pentane. Gas chromatography, employing both a flame ionization detector and an olfactometry port, was used to analyze the obtained extracts. Seventy-one odors were detected and distributed according to Calvados quality determined by sensory evaluation. Nineteen odors common to all Calvados samples constituted the "skeleton" of the aroma. Twenty-eight odors were specific to a quality class: 6 for good quality, 4 for neutral, and 18 for defective. Twenty-four other odors had either too low an odor impact or no evident specificity.

Needle Tip Position and Bevel Direction Have No Effect in the Fluoroscopic Epidural Spreading Pattern in Caudal Epidural Injections: A Randomized Trial

PubMed Central

Kwon, Won Kyoung; Kim, Ah Na; Lee, Pil Moo; Park, Cheol Hwan; Kim, Jae Hun

2016-01-01

Background. Caudal epidural steroid injections (CESIs) are an effective treatment for pain. If the injection spreads in a specific pattern depending on the needle position or bevel direction, it would be possible to inject the agent into a specific and desired area. Objectives. We conducted a prospective randomized trial to determine if the needle position and bevel direction have any effect on the epidural spreading pattern in CESI. Methods. Demographic data of the patient were collected. During CESI, the needle position (middle or lateral) and direction (ventral or dorsal) were randomly allocated. Following fluoroscope-guided injection of 4 mL contrast media and 10 mL of injectates, the epidural spreading patterns (ventral or dorsal, bilateral or lateral) were imaged. Results. In the 210 CESIs performed, the needle tip position and bevel direction did not influence the epidural spreading patterns at L4-5 and L5-S1 disc levels. A history of Lumbar spine surgery was associated with a significantly limited spread to each disc level. A midline needle tip position was more effective than the lateral position in spreading to the distant disc levels. Conclusions. Neither the needle tip position nor the bevel direction affected the epidural drug spreading pattern during CESI. PMID:27445609

Integrated on-line system for DNA sequencing by capillary electrophoresis: From template to called bases

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

Ton, H.; Yeung, E.S.

1997-02-15

An integrated on-line prototype for coupling a microreactor to capillary electrophoresis for DNA sequencing has been demonstrated. A dye-labeled terminator cycle-sequencing reaction is performed in a fused-silica capillary. Subsequently, the sequencing ladder is directly injected into a size-exclusion chromatographic column operated at nearly 95{degree}C for purification. On-line injection to a capillary for electrophoresis is accomplished at a junction set at nearly 70{degree}C. High temperature at the purification column and injection junction prevents the renaturation of DNA fragments during on-line transfer without affecting the separation. The high solubility of DNA in and the relatively low ionic strength of 1 x TEmore » buffer permit both effective purification and electrokinetic injection of the DNA sample. The system is compatible with highly efficient separations by a replaceable poly(ethylene oxide) polymer solution in uncoated capillary tubes. Future automation and adaptation to a multiple-capillary array system should allow high-speed, high-throughput DNA sequencing from templates to called bases in one step. 32 refs., 5 figs.« less

Injection molding of iPP samples in controlled conditions and resulting morphology

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

Sessa, Nino, E-mail: ninosessa.ns@gmail.com; De Santis, Felice, E-mail: fedesantis@unisa.it; Pantani, Roberto, E-mail: rpantani@unisa.it

2015-12-17

Injection molded parts are driven down in size and weight especially for electronic applications. In this work, an investigation was carried out on the process of injection molding of thin iPP samples and on the morphology of these parts. Melt flow in the mold cavity was analyzed and described with a mathematical model. Influence of mold temperature and injection pressure was analyzed. Samples orientation was studied using optical microscopy.

Electrical imaging of subsurface nanoparticle propagation for in-situ groundwater remediation

NASA Astrophysics Data System (ADS)

Flores Orozco, Adrián; Gallistl, Jakob; Schmid, Doris; Micic Batka, Vesna; Bücker, Matthias; Hofmann, Thilo

2017-04-01

Application of nanoparticles has emerged as a promising in situ remediation technology for the remediation of contaminated groundwater, particularly for areas difficult to access by other remediation techniques. The performance of nanoparticle injections, as a foremost step within this technology, is usually assessed through the geochemical analysis of soil and groundwater samples. This approach is not well suited for a real-time monitoring, and often suffers from a poor spatio-temporal resolution and only provides information from areas close to the sampling points. To overcome these limitations we propose the application of non-invasive Induced Polarization (IP) imaging, a geophysical method that provides information on the electrical properties of the subsurface. The analysis of temporal changes in the electrical images allows tracking the propagation of the injected nanoparticle suspension and detection of the induced bio-geochemical changes in the subsurface. Here, we present IP monitoring results for data collected during the injection of Nano-Goethite particles (NGP) used for simulation of biodegradation of a BTEX plume (i.e., benzene, toluene, ethylbenzene, and xylene) at the Spolchemie II site, CZ. Frequency-domain IP measurements were collected parallel to the groundwater flow direction and centred on the NGP injection point. Pre-injection imaging results revealed high electrical conductivities (> 10 S/m) and negligible polarization effects in the BTEX-contaminated part of the saturated zone (below 5 m depth). The apparently contradictory observation - BTEX compounds are poor electrical conductors - can be explained by the release of carbonic acids (a metabolic by-product of the biodegradation of hydrocarbons), which leads to an increase of the electrical conductivity. Post-injection images revealed a significant decrease (> 50%) of the electrical conductivity, with even larger changes in the proximity of the injection points, most likely due to the relatively high resistivity of the NGP suspension. This is in line with geochemical data from both the injected NGP suspension and the groundwater samples. Furthermore, temporal changes in the IP images are consistent with variations in total iron concentration in groundwater (a proxy for the NGP concentration) as well as in situ groundwater parameters, such as pH and oxidation-reduction potential. Our results demonstrate the applicability of IP imaging for the real-time monitoring of nanoparticle injection, as well as of the accompanying geochemical changes. Part of this research is funded by the European Union's Seventh Framework Programme for research, technological development and demonstration under grant agreement no 309517.

Quantification of γ-Aminobutyric Acid in Cerebrospinal Fluid Using Liquid Chromatography-Electrospray Tandem Mass Spectrometry.

PubMed

Arning, Erland; Bottiglieri, Teodoro

2016-01-01

We describe a simple stable isotope dilution method for accurate and precise measurement of γ-aminobutyric acid (GABA), a major inhibitory neurotransmitter in human cerebrospinal fluid (CSF) as a clinical diagnostic test. Determination of GABA in CSF (50 μL) was performed utilizing high performance liquid chromatography coupled with electrospray positive ionization tandem mass spectrometry (HPLC-ESI-MS/MS). Analysis of free and total GABA requires two individual sample preparations and mass spectrometry analyses. Free GABA in CSF is determined by a 1:2 dilution with internal standard (GABA-D2) and injected directly onto the HPLC-ESI-MS/MS system. Determination of total GABA in CSF requires additional sample preparation in order to hydrolyze all the bound GABA in the sample to the free form. This requires hydrolyzing the sample by boiling in acidic conditions (hydrochloric acid) for 4 h. The sample is then further diluted 1:10 with a 90 % acetonitrile/0.1 % formic acid solution and injected into the HPLC-ESI-MS/MS system. Each assay is quantified using a five-point standard curve and is linear from 6 nM to 1000 nM and 0.63 μM to 80 μM for free and total GABA, respectively.

Investigation on the Characteristics of Pellet Ablation in a Toroidal Plasma

NASA Astrophysics Data System (ADS)

Sato, K. N.; Sakakita, H.; Fujita, H.

2003-06-01

Characteristics of a cloud ablated from an ice pellet has been investigated in detail in the JIPP T-IIU tokamak plasma by utilizing a new scheme of pellet injection system, "the injection-angle controllable system". A long "helical tail" of ablation light has been observed using CCD cameras and a high speed framing photograph in the case of on-axis and off-axis injection with the injection angle smaller than a certain value. The direction of the helical tail is found to be independent to that of the total magnetic field lines of the torus. From the experiments with the combination of two toroildal filed directions and two plasma current directions, it is considered that the tail seems to rotate, in most cases, to the electron diamagnetic direction poloidally, and to the opposite to the plasma current direction toroidally. Consideration on various cross sections including charge exchange, ionization and elastic collisions leads us to the conclusion that the tail-shaped phenomena may come from the situation of charge exchange equilibrium of hydrogen ions and neutrals at extremely high density regime in the cloud. The relation of ablation behavior with plasma potential and rotation has also been studied. Potential measurements of pellet-injected plasmas using heavy ion beam probe (HIBP) method were carried out for the first time. In the case of an injection angle to be anti-parallel to the electron diamagnetic direction in the poloidal plane, the result shows that the direction of potential change is negative, and consequently the potential after the injection should be negative because it has been measured to be negative in usual ohmic plasmas without pellet injection. Thus, the direction of the "tail" structure seems to be consistent to that of the plasma potential measured, if it is considered that tail structure may be caused by the effect of the plasma potential and the rotation.

Numerical investigation of liver radioembolization via computational particle-hemodynamics: The role of the microcatheter distal direction and microsphere injection point and velocity.

PubMed

Aramburu, Jorge; Antón, Raúl; Rivas, Alejandro; Ramos, Juan Carlos; Sangro, Bruno; Bilbao, José Ignacio

2016-11-07

Liver radioembolization is a treatment option for patients with primary and secondary liver cancer. The procedure consists of injecting radiation-emitting microspheres via an intra-arterially placed microcatheter, enabling the deposition of the microspheres in the tumoral bed. The microcatheter location and the particle injection rate are determined during a pretreatment work-up. The purpose of this study was to numerically study the effects of the injection characteristics during the first stage of microsphere travel through the bloodstream in a patient-specific hepatic artery (i.e., the near-tip particle-hemodynamics and the segment-to-segment particle distribution). Specifically, the influence of the distal direction of an end-hole microcatheter and particle injection point and velocity were analyzed. Results showed that the procedure targeted the right lobe when injecting from two of the three injection points under study and the remaining injection point primarily targeted the left lobe. Changes in microcatheter direction and injection velocity resulted in an absolute difference in exiting particle percentage for a given liver segment of up to 20% and 30%, respectively. It can be concluded that even though microcatheter placement is presumably reproduced in the treatment session relative to the pretreatment angiography, the treatment may result in undesired segment-to-segment particle distribution and therefore undesired treatment outcomes due to modifications of any of the parameters studied, i.e., microcatheter direction and particle injection point and velocity. Copyright © 2016 Elsevier Ltd. All rights reserved.

Mechanical Weakening during Fluid Injection in Critically Stressed Sandstones with Acoustic Monitoring

NASA Astrophysics Data System (ADS)

David, C.; Dautriat, J. D.; Sarout, J.; Macault, R.; Bertauld, D.

2014-12-01

Water weakening is a well-known phenomenon which can lead to subsidence during the production of hydrocarbon reservoirs. The example of the Ekofisk oil field in the North Sea has been well documented for years. In order to assess water weakening effects in reservoir rocks, previous studies have focused on changes in the failure envelopes derived from mechanical tests conducted on rocks saturated either with water or with inert fluids. However, little attention has been paid so far on the mechanical behaviour during the fluid injection stage, like in enhanced oil recovery operations. We studied the effect of fluid injection on the mechanical behaviour of Sherwood sandstone, a weakly-consolidated sandstone sampled at Ladram Bay in UK. In order to highlight possible weakening effects, water and inert oil have been injected into critically-loaded samples to assess their effect on strength and elastic properties and to derive the acoustic signature of the saturation front for each fluid. The specimens were instrumented with 16 ultrasonic P-wave transducers for both passive and active acoustic monitoring during fluid injection and loading. After conducting standard triaxial tests on three samples saturated with air, water and oil respectively, mechanical creep tests were conducted on dry samples loaded at 80% of the compressive strength of the dry rock. While these conditions are kept constant, a fluid is injected at the bottom end of the sample with a low back pressure (0.5 MPa) to minimize effective stress variations during injection. Both water and oil were used as the injected pore fluid in two experiments. As soon as the fluids start to flow into the samples, creep is taking place with a much higher strain rate for water injection compared to oil injection. A transition from secondary creep to tertiary creep is observed in the water injection test whereas in the oil injection test no significant creep acceleration is observed after one pore volume of oil was injected. The most remarkable difference is that water injection induces mechanical instability and failure, whereas oil injection does not. This was confirmed by the analysis of acoustic emissions activity and post-mortem sample imaging using CT scan. Contrasting evolutions of the P wave velocity during the fluid front propagation were also observed in both experiments.

Helium ionization detection apparatus

NASA Technical Reports Server (NTRS)

Nagai, R.

1984-01-01

In a gas chromatograph apparatus comprising a gas supply (He carrier gas), a sample injection apparatus, a chromatograph column, a He ion detector, and connecting tubes, a foreign gas (other than He) injection apparatus is installed between the sample injection apparatus and the detector. Mixing of the sample gas and foreign gas takes place readily, the sample gas is always maintained at a stable concentrator range, and accurate measurements are possible, especially at low sample gas concentrations.

Updates to Simulation of a Single-Element Lean-Direct Injection Combustor Using Arbitary Polyhedral Meshes

NASA Technical Reports Server (NTRS)

Wey, Thomas; Liu, Nan-Suey

2015-01-01

This paper summarizes the procedures of (1) generating control volumes anchored at the nodes of a mesh; and (2) generating staggered control volumes via mesh reconstructions, in terms of either mesh realignment or mesh refinement, as well as presents sample results from their applications to the numerical solution of a single-element LDI combustor using a releasable edition of the National Combustion Code (NCC).

Ultrasound extracted flavonoids from four varieties of Portuguese red grape skins determined by reverse-phase high-performance liquid chromatography with electrochemical detection.

PubMed

Novak, Ivana; Janeiro, Patricia; Seruga, Marijan; Oliveira-Brett, Ana Maria

2008-12-23

Several flavonoids present in red grape skins from four varieties of Portuguese grapes were determined by reverse-phase high-performance liquid chromatography (RP-HPLC) with electrochemical detection (ECD). Extraction of flavonoids from red grape skins was performed by ultrasonication, and hydrochloric acid in methanol was used as extraction solvent. The developed RP-HPLC method used combined isocratic and gradient elution with amperometric detection with a glassy carbon-working electrode. Good peak resolution was obtained following direct injection of a sample of red grape extract in a pH 2.20 mobile phase. Eleven different flavonoids: cyanidin-3-O-glucoside (kuromanin), delphinidin-3-O-glucoside (myrtillin), petunidin-3-O-glucoside, peonidin-3-O-glucoside, malvidin-3-O-glucoside (oenin), (+)-catechin, rutin, fisetin, myricetin, morin and quercetin, can be separated in a single run by direct injection of sample solution. The limit of detection obtained for these compounds by ECD was 20-90 pg/L, 1000 times lower when compared with photodiode array (PDA) limit of detection of 12-55 ng/L. RP-HPLC-ECD was characterized by an excellent sensitivity and selectivity, and appropriate for the simultaneous determination of these electroactive phenolic compounds present in red grape skins.

Bulk derivatization and direct injection of human cerebrospinal fluid for trace-level quantification of endogenous estrogens using trap-and-elute liquid chromatography with tandem mass spectrometry.

PubMed

Fan, Hui; Papouskova, Barbora; Lemr, Karel; Wigginton, Jane G; Schug, Kevin A

2014-08-01

Although there are existing methods for determining estrogen in human bodily fluids including blood plasma and serum, very little information is available regarding estrogen levels in human cerebrospinal fluid (CSF), which is critical to assess in studies of neuroprotective functions and diffusion of neuroprotective estrogens across the blood-brain barrier. To address this problem, a liquid chromatography with tandem mass spectrometry method for the simultaneous quantification of four endogenous estrogens (estrone, 17α-estradiol, 17β-estradiol, and estriol) in human CSF was developed. An aliquot (300 μL) of human CSF was bulk derivatized using dansyl chloride in the sample and 10 μL was directly injected onto a restricted-access media trap column for protein removal. No off-line sample extraction or cleanup was needed. The limits of detection of estrone, 17α-estradiol, 17β-estradiol, and estriol were 17, 28, 13, and 30 pg/mL, respectively, which is in the parts-per-trillion regime. The method was then applied to human CSF collected from ischemic trauma patients. Endogenous estrogens were detected and quantified, demonstrating the effectiveness of this method. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of available phosphorus in soils by using a new extraction procedure and a flow injection amperometric system.

PubMed

Jakmunee, Jaroon; Junsomboon, Jaroon

2009-09-15

A new extraction procedure based on an off-line extraction column was proposed for extracting of available phosphorus from soils. The column was fabricated from a plastic syringe fitted at the bottom with a cotton wool and a piece of filter paper to support a soil sample. An aliquot (50 mL) of extracting solution (0.05 M HCl+0.0125 M H(2)SO(4)) was used to extract the sample under gravity flow and the eluate was collected in a polyethylene bottle. The extract was then analyzed for phosphorus contents by a simple flow injection amperometric system, employing a set of three-way solenoid valves as an injection valve. The method is based on the electrochemical reduction of 12-molybdophosphate which is produced on-line by the reaction of orthophosphate with acidic molybdate and the electrical current produced was directly proportional to the concentration of phosphate in range of 0.1-10.0 mg L(-1) PO(4)-P, with a detection limit of 0.02 mg L(-1). Relative standard for 11 replicate injections of 5 mg L(-1) PO(4)-P was 0.5%. A sample through put of 35 h(-1) was achieved, with consumption of 14 mg KCl, 10mg ammonium molybdate and 0.05 mL H(2)SO(4) per analysis. The detection system does not suffer from the interferences that are encountered in the photometric method such as colored substances, colloids, metal ions, silicate and refractive index effect (Schlieren effect). The results obtained by the column extraction procedure were well correlated with those obtained by the steady-state extraction procedure, but showed slightly higher extraction efficiency.

The use of laser-induced fluorescence or ultraviolet detectors for sensitive and selective analysis of tobramycin or erythropoietin in complex samples.

PubMed

Ahmed, Hytham M; Ebeid, Wael B

2015-05-15

Complex samples analysis is a challenge in pharmaceutical and biopharmaceutical analysis. In this work, tobramycin (TOB) analysis in human urine samples and recombinant human erythropoietin (rhEPO) analysis in the presence of similar protein were selected as representative examples of such samples analysis. Assays of TOB in urine samples are difficult because of poor detectability. Therefore laser induced fluorescence detector (LIF) was combined with a separation technique, micellar electrokinetic chromatography (MEKC), to determine TOB through derivatization with fluorescein isothiocyanate (FITC). Borate was used as background electrolyte (BGE) with negative-charged mixed micelles as additive. The method was successively applied to urine samples. The LOD and LOQ for Tobramycin in urine were 90 and 200ng/ml respectively and recovery was >98% (n=5). All urine samples were analyzed by direct injection without sample pre-treatment. Another use of hyphenated analytical technique, capillary zone electrophoresis (CZE) connected to ultraviolet (UV) detector was also used for sensitive analysis of rhEPO at low levels (2000IU) in the presence of large amount of human serum albumin (HSA). Analysis of rhEPO was achieved by the use of the electrokinetic injection (EI) with discontinuous buffers. Phosphate buffer was used as BGE with metal ions as additive. The proposed method can be used for the estimation of large number of quality control rhEPO samples in a short period. Copyright © 2015 Elsevier B.V. All rights reserved.

Perilymph Kinetics of FITC-Dextran Reveals Homeostasis Dominated by the Cochlear Aqueduct and Cerebrospinal Fluid.

PubMed

Salt, A N; Gill, R M; Hartsock, J J

2015-06-01

Understanding how drugs are distributed in perilymph following local applications is important as local drug therapies are increasingly used to treat disorders of the inner ear. The potential contribution of cerebrospinal fluid (CSF) entry to perilymph homeostasis has been controversial for over half a century, largely due to artifactual contamination of collected perilymph samples with CSF. Measures of perilymph flow and of drug distribution following round window niche applications have both suggested a slow, apically directed flow occurs along scala tympani (ST) in the normal, sealed cochlea. In the present study, we have used fluorescein isothiocyanate-dextran as a marker to study perilymph kinetics in guinea pigs. Dextran is lost from perilymph more slowly than other substances so far quantified. Dextran solutions were injected from pipettes sealed into the lateral semicircular canal (SCC), the cochlear apex, or the basal turn of ST. After varying delays, sequential perilymph samples were taken from the cochlear apex or lateral SCC, allowing dextran distribution along the perilymphatic spaces to be quantified. Variability was low and findings were consistent with the injection procedure driving volume flow towards the cochlear aqueduct, and with volume flow during perilymph sampling driven by CSF entry at the aqueduct. The decline of dextran with time in the period between injection and sampling was consistent with both a slow volume influx of CSF (~30 nL/min) entering the basal turn of ST at the cochlear aqueduct and a CSF-perilymph exchange driven by pressure-driven fluid oscillation across the cochlear aqueduct. Sample data also allowed contributions of other processes, such as communications with adjacent compartments, to be quantified. The study demonstrates that drug kinetics in the basal turn of ST is complex and is influenced by a considerable number of interacting processes.

Dioctyl sulfosuccinate analysis in near-shore Gulf of Mexico water by direct-injection liquid chromatography-tandem mass spectrometry.

PubMed

Mathew, Johnson; Schroeder, David L; Zintek, Lawrence B; Schupp, Caitlin R; Kosempa, Michael G; Zachary, Adam M; Schupp, George C; Wesolowski, Dennis J

2012-03-30

Dioctyl sulfosuccinate (DOSS) was a major component of the dispersants most used in the 2010 Deepwater Horizon Oil Spill incident response. This analytical method quantifies salt water DOSS concentrations to a reporting limit of 20 μg/L, which was below the United States Environmental Protection Agency's (U.S. EPA) 40 μg/L DOSS Aquatic Life Benchmark. DOSS in Gulf of Mexico water samples were analyzed by direct-injection reversed-phase liquid chromatography-tandem mass spectrometry (LC-MS/MS). Sample preparation with 50% acetonitrile (ACN) enabled quantitative transfer of DOSS and increased DOSS response 20-fold by reducing aggregation. This increased sensitivity enabled the detection of a confirmatory transition over the calibration range of 10-200 μg/L. U.S. EPA Region 5 and Region 6 laboratories analyzed hundreds of near-shore surface Gulf of Mexico water samples, none contained more than the 20 ppb reporting limit. The matrix spike DOSS/deuterated surrogate (DOSS-D34) correlation of determination varied with mobile phase modifier (ammonium formate R(2)=0.95 and formic acid R(2)=0.27). Using ammonium formate, DOSS-D34 accurately measured DOSS matrix effect. The near-shore sodium concentrations varied more than 10,000-fold, but were not strongly correlated with DOSS recovery. DOSS detection by LC-MS/MS enabled rapid analysis which was valuable in guiding incident response. Published by Elsevier B.V.

The contribution of lubricant to the formation of particulate matter with reactivity controlled compression ignition in light-duty diesel engines

DOE PAGES

Storey, John Morse; Curran, Scott; Dempsey, Adam B.; ...

2014-12-25

Reactivity controlled compression ignition (RCCI) has been shown in single- and multi-cylinder engine research to achieve high thermal efficiencies with ultra-low NO X and soot emissions. The nature of the particulate matter (PM) produced by RCCI operation has been shown in recent research to be different than that of conventional diesel combustion and even diesel low-temperature combustion. Previous research has shown that the PM from RCCI operation contains a large amount of organic material that is volatile and semi-volatile. However, it is unclear if the organic compounds are stemming from fuel or lubricant oil. The PM emissions from dual-fuel RCCImore » were investigated in this study using two engine platforms, with an emphasis on the potential contribution of lubricant. Both engine platforms used the same base General Motors (GM) 1.9-L diesel engine geometry. The first study was conducted on a single-cylinder research engine with primary reference fuels (PRFs), n-heptane, and iso-octane. The second study was conducted on a four-cylinder GM 1.9-L ZDTH engine which was modified with a port fuel injection (PFI) system while maintaining the stock direct injection fuel system. Multi-cylinder RCCI experiments were run with PFI gasoline and direct injection of 2-ethylhexyl nitrate (EHN) mixed with gasoline at 5 % EHN by volume. In addition, comparison cases of conventional diesel combustion (CDC) were performed. Particulate size distributions were measured, and PM filter samples were collected for analysis of lube oil components. Triplicate PM filter samples (i.e., three individual filter samples) for both gas chromatography-mass spectroscopy (GC-MS; organic) analysis and X-ray fluorescence (XRF; metals) were obtained at each operating point and queued for analysis of both organic species and lubricant metals. Here, the results give a clear indication that lubricants do not contribute significantly to the formation of RCCI PM.« less

Orthogonal ion injection apparatus and process

DOEpatents

Kurulugama, Ruwan T; Belov, Mikhail E

2014-04-15

An orthogonal ion injection apparatus and process are described in which ions are directly injected into an ion guide orthogonal to the ion guide axis through an inlet opening located on a side of the ion guide. The end of the heated capillary is placed inside the ion guide such that the ions are directly injected into DC and RF fields inside the ion guide, which efficiently confines ions inside the ion guide. Liquid droplets created by the ionization source that are carried through the capillary into the ion guide are removed from the ion guide by a strong directional gas flow through an inlet opening on the opposite side of the ion guide. Strong DC and RF fields divert ions into the ion guide. In-guide orthogonal injection yields a noise level that is a factor of 1.5 to 2 lower than conventional inline injection known in the art. Signal intensities for low m/z ions are greater compared to convention inline injection under the same processing conditions.

A line source tracer test - a better method for assessing high groundwater velocity

NASA Astrophysics Data System (ADS)

Magal, E.; Weisbrod, N.; Yakirevich, A.; Kurtzman, D.; Yechieli, Y.

2009-12-01

A line source injection is suggested as an effective method for assessing groundwater velocities and flow directions in subsurface characterized by high water fluxes. Modifying the common techniques of injecting a tracer into a well was necessary after frequently-used methods of natural and forced gradient tracer tests ended with no reliable information on the local groundwater flow. In a field experiment, tracers were injected into 8-m long line injection system constructed below the water table almost perpendicular to the assumed flow direction. The injection system was divided to four separate segments (each 2 m long) enabling the injection of four different tracers along the line source. An array of five boreholes located in an area of 10x10 m downstream was used for monitoring the tracers' transport. Two dye tracers (Uranine and Na Naphthionate) were injected in a long pulse of several hours into two of the injection pipe segments and two tracers (Rhenium oxide and Gd-DTPA) were instantaneously injected to the other two segments. The tracers were detected 0.7 to 2.3 hours after injection in four of the five observation wells, located 2.3 to 10 m from the injection system, respectively. Groundwater velocities were calculated directly from the tracers' arrival times and by fitting the observed breakthrough curves to simulations with one and two dimensions analytical solutions for conservative tracer transport. The groundwater velocity was determined to be ~100 m/d. The longitudinal dispersivity value, generated from fitting the tracer breakthrough curves, was in a range of 0.2-3m. The groundwater flow direction was derived based on the arrival of the tracers and was found to be consistent with the apparent direction of the hydraulic gradient. The hydraulic conductivity derived from the groundwater velocity was ~1200 m/d, which is in the upper range of gravel sediment.

Further improvement of hydrostatic pressure sample injection for microchip electrophoresis.

PubMed

Luo, Yong; Zhang, Qingquan; Qin, Jianhua; Lin, Bingcheng

2007-12-01

Hydrostatic pressure sample injection method is able to minimize the number of electrodes needed for a microchip electrophoresis process; however, it neither can be applied for electrophoretic DNA sizing, nor can be implemented on the widely used single-cross microchip. This paper presents an injector design that makes the hydrostatic pressure sample injection method suitable for DNA sizing. By introducing an assistant channel into the normal double-cross injector, a rugged DNA sample plug suitable for sizing can be successfully formed within the cross area during the sample loading. This paper also demonstrates that the hydrostatic pressure sample injection can be performed in the single-cross microchip by controlling the radial position of the detection point in the separation channel. Rhodamine 123 and its derivative as model sample were successfully separated.

Injection of Super-Critical CO2 in Brine Saturated Sandstone:

NASA Astrophysics Data System (ADS)

Ott, Holger; de Kloe, Kees; Taberner, Conxita; Marcelis, Fons; Makurat, Axel

2010-05-01

Presently, large-scale geological sequestration of CO2, originating from sources like fossil-fueled power plants and contaminated gas production, is seen as an option to reduce anthropogenic emission of greenhouse gases to the atmosphere. Deep saline aquifers and depleted oil and gas fields are potential subsurface deposits for CO2. Injected CO2, however, interacts physically and chemically with the formation leading to uncertainties for CCS projects. One of these uncertainties is related to a dry-out zone that is likely to form around the well bore owing to the injection of dry CO2. Precipitation of salt (mainly halite) that is associated with that drying out of a saline formation has the potential to impair injectivity, and could even lead to the loss of a well. If dry (or under-saturated), super-critical (SC) CO2 is injected into water-bearing geological formations like saline aquifers, water is removed by either advection of the aqueous phase or by evaporation of water and subsequent advection in the injected CO2-rich phase. Both mechanisms act in parallel, however while advection of the aqueous phase decreases with increasing CO2 saturation (diminished mobility), evaporation becomes increasingly important as the aqueous phase becomes immobile. Below residual water saturation, only evaporation takes place and the formation dries out if no additional source of water is available. If water evaporates, the salts originally present in the water are left behind. In case of highly saline formations, the amount of salt that potentially precipitates per unit volume can be quite substantial. It depends on salinity, the solubility limit of water in the CO2 rich phase, and on the ratio of advection and evaporation rates. Since saturations and flow rates cover a large range as functions of space and time close to the well bore, there is no easy answer to the questions whether, where and how salt precipitation impacts injectivity. The present paper presents results of core-flood experiments that were performed to investigate the spatial and temporal precipitation of salt due to the injection of dry CO2 and to understand the underlying mechanisms; super-critical CO2 was injected into brine-saturated sandstone (Berea) samples under realistic pressure and temperature conditions and at high injection rate. To match flow rates that are realistic for the near well-bore area, the experiments were performed on small-scale samples with a cross section of less than 1 cm2. Density profiles were measured by mCT (micro computer tomography) scanning during injection. Reference scans and brine doping with a contrast agent allow the distinction between the CO2-rich phase, the aqueous phase and precipitated solid salt even on pore scale. By means of mCT scanning, spatial and time evolution of halite precipitation in rock samples have been observed under sequestration conditions. Pattern formation of solid salt along the main flow direction as well as a cross-sectional pattern formation has been found. However, while there are areas of high local solid salt accumulation, permeability remained unaffected, which might be a result of the precipitation pattern. The results were complemented by (ex-situ) eSEM/EDAX measurements to study where and how salt precipitates on the microscopic scale. The SEM results cannot be directly translated to in-situ conditions, as salt migrates post-experiment at ambient conditions, but give valuable insight into microscopic processes controlling deposition. Numerical simulations have been performed for a qualitative understanding of principle mechanisms and show a dependency of the observed profile on injection rate and capillary pressure.

Method and Apparatus for Concentrating Vapors for Analysis

DOEpatents

Grate, Jay W.; Baldwin, David L.; Anheier, Jr., Norman C.

2008-10-07

An apparatus and method are disclosed for pre-concentrating gaseous vapors for analysis. The invention finds application in conjunction with, e.g., analytical instruments where low detection limits for gaseous vapors are desirable. Vapors sorbed and concentrated within the bed of the apparatus can be thermally desorbed achieving at least partial separation of vapor mixtures. The apparatus is suitable, e.g., for preconcentration and sample injection, and provides greater resolution of peaks for vapors within vapor mixtures, yielding detection levels that are 10-10,000 times better than for direct sampling and analysis systems. Features are particularly useful for continuous unattended monitoring applications.

Borehole geophysical monitoring of amendment emplacement and geochemical changes during vegetable oil biostimulation, Anoka County Riverfront Park, Fridley, Minnesota

USGS Publications Warehouse

Lane, John W.; Day-Lewis, Frederick D.; Johnson, Carole D.; Joesten, Peter K.; Kochiss, Christopher S.

2007-01-01

Based on the geophysical data, conceptual models of the distributions of emulsified vegetable oil and ground water with altered chemistry were developed. The field data indicate that, in several cases, the plume of ground water with altered chemistry would not be detected by direct chemical sampling given the construction of monitoring wells; hence the geophysical data provide valuable site-specific insights for the interpretation of water samples and monitoring of biostimulation projects. Application of geophysical methods to data from the ACP demonstrated the utility of radar for monitoring biostimulation injections.

In-line characterization of nanostructured mass-produced polymer components using scatterometry

NASA Astrophysics Data System (ADS)

Skovlund Madsen, Jonas; Højlund Thamdrup, Lasse; Czolkos, Ilja; Hansen, Poul Erik; Johansson, Alicia; Garnaes, Jørgen; Nygård, Jesper; Hannibal Madsen, Morten

2017-08-01

Scatterometry is used as an in-line metrology solution for injection molded nanostructures to evaluate the pattern replication fidelity. The method is used to give direct feedback to an operator when testing new molding parameters and for continuous quality control. A compact scatterometer has been built and tested at a fabrication facility. The scatterometry measurements, including data analysis and handling of the samples, are much faster than the injection molding cycle time, and thus, characterization does not slow down the production rate. Fabrication and characterization of 160 plastic parts with line gratings are presented here, and the optimal molding temperatures for replication of nanostructures are found for two polymers. Scatterometry results are compared to state of the art metrology solutions: atomic force and scanning electron microscopy. It is demonstrated that the scatterometer can determine the structural parameters of the samples with an accuracy of a few nanometers in less than a second, thereby enabling in-line characterization.

Rapid control of mold temperature during injection molding process

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

Liparoti, Sara; Titomanlio, Giuseppe; Hunag, Tsang Min

2015-05-22

The control of mold surface temperature is an important factor that determines surface morphology and its dimension in thickness direction. It can also affect the frozen molecular orientation and the mold surface replicability in injection molded products. In this work, thin thermally active films were used to quickly control the mold surface temperature. In particular, an active high electrical conductivity carbon black loaded polyimide composites sandwiched between two insulating thin polymeric layers was used to condition the mold surface. By controlling the heating time, it was possible to control precisely the temporal variation of the mold temperature surface during themore » entire cycle. The surface heating rate was about 40°C/s and upon contact with the polymer the surface temperature decreased back to 40°C within about 5 s; the overall cycle time increased only slightly. The effect on cross section sample morphology of samples of iPP were analyzed and discussed on the basis of the recorded temperature evolution.« less

Evaluation of the antioxidant power of honey, propolis and royal jelly by amperometric flow injection analysis.

PubMed

Buratti, S; Benedetti, S; Cosio, M S

2007-02-28

In this paper is described the applicability of a flow injection system, operating with an amperometric detector, for measurement in rapid and simple way the antioxidant power of honey, propolis and royal jelly. The proposed method evaluates the reducing power of selected antioxidant compounds and does not require the use of free radicals or oxidants. Twelve honey, 12 propolis and 4 royal jelly samples of different botanical and geographical origin were evaluated by the electrochemical method and the data were compared with those obtained by the DPPH assay. Since a good correlation was found (R(2)=0.92) the proposed electrochemical method can be successfully employed for the direct, rapid and simple monitoring of the antioxidant power of honeybee products. Furthermore, the total phenolic content of samples was determined by the Folin-Ciocalteau procedure and the characteristic antioxidant activities showed a good correlation with phenolics (R(2)=0.96 for propolis and 0.90 for honey).

Magnetic Remanence and Anisotropy of Magnetic Susceptibility of Dikes From Super-Fast Spread Crust Exposed At Pito Deep Rift

NASA Astrophysics Data System (ADS)

Horst, A.; Varga, R. J.; Gee, J. S.; Karson, J. A.

2006-12-01

The tectonic window at the Pito Deep Rift exposes super-fast spread (>140mm/yr) oceanic crust created at the East Pacific Rise (EPR). Observations and investigations of well-exposed cross sections into modern ocean crust, such as Pito Deep, provide essential insights into ridge crest dynamics. Paleomagnetic analysis provides a quantitative means for assessing both magnitude and style of structural rotations of oceanic crust. The Pito Cruise 2005 collected 69 fully oriented samples [67 dikes, 2 gabbros] during several ALVIN and JASON II dives. These samples were all oriented in situ using the Geocompass. Along the escarpment of Pito Deep, dike orientations have consistant NE strikes and SE dips. These dikes are all formed roughly 3 million years ago at the EPR located to the west of their present position. We determined magnetic remanence for a subset of 34 oriented blocks. A majority of dikes in this subset have normal polarity and many are clockwise rotated from expected orientations. To assess possible orientation errors during collection, we sampled multiple dikes from relatively small areas. On ALVIN dive 4081, for example, we collected 14 samples from a well-exposed, subparallel series of dikes. These dikes provide stable and consistently oriented remanence directions suggesting that errors in the collection process are small. Remanence data collected to date verify tectonic models that suggest clockwise rotation of the Easter microplate, consistent with current models. In addition to magnetic remanence, we determined the anisotropy of magnetic susceptibility (AMS) of the 34 dike samples. AMS studies have proven their utility in a wide range of geological studies and have been shown to determine flow direction within dikes in a variety of settings. In most Pito Deep samples, two of three AMS eigenvectors lie close to dike plane orientations. Kmin generally lies perpendicular to dike planes while, in most samples, Kmax is shallow indicating dominantly subhorizontal magma flow. Steep Kmax in a few samples indicates vertical flow directions suggestive of primary flow or of gravitational back-flow during the waning stages of dike injection. Primarily horizontal magma flow in dikes might indicate injection of magma from a centralized magma chamber toward a plate segment boundary.

Portable device and method for determining permeability characteristics of earth formations

DOEpatents

Shuck, Lowell Z.

1977-01-01

The invention is directed to a device which is used for determining permeability characteristics of earth formations at the surface thereof. The determination of the maximum permeability direction and the magnitude of permeability are achieved by employing a device comprising a housing having a central fluid-injection port surrounded by a plurality of spaced-apart fluid flow and pressure monitoring ports radially extending from the central injection port. With the housing resting on the earth formation in a relatively fluid-tight manner as provided by an elastomeric pad disposed therebetween, fluid is injected through the central port into the earth formation and into registry with the fluid-monitoring ports disposed about the injection port. The fluid-monitoring ports are selectively opened and the flow of the fluid through the various fluid ports is measured so as to provide a measurement of flow rates and pressure distribution about the center hole which is indicative on the earth formation permeability direction and magnitude. For example, the azimuthal direction of the fluid-monitoring ports in the direction through which the greatest amount of injected fluid flows as determined by the lowest pressure distribution corresponds to the direction of maximum permeability in the earth formation.

Non-fatal overdose among adult prisoners with a history of injecting drug use in two Australian states.

PubMed

Moore, Elizabeth; Winter, Rebecca; Indig, Devon; Greenberg, David; Kinner, Stuart A

2013-11-01

Recently released prisoners are at markedly increased risk of death and drug-related causes predominate. Non-fatal overdose (NFOD) is considerably more common than fatal overdose, but has received relatively little research attention and most studies of NFOD in this population have suffered from small samples of unknown representativeness. This study aimed to estimate the prevalence and correlates of lifetime NFOD among prisoners in NSW and Queensland. Cross-sectional surveys of adult prisoners in two Australian states: New South Wales (n=972) and Queensland (n=1316). Use of similar measures and methods in the two states made direct comparison of findings possible. In both NSW and Queensland, 23% of participants reported a lifetime history of NFOD and prisoners with a history of injecting drug use were significantly more likely to report lifetime NFOD. The lifetime prevalence of NFOD among prisoners with a history of injecting drug use was significantly higher in NSW than in Queensland (44% vs. 35%; p<0.01). Independent correlates of lifetime NFOD were similar across the two states and included ever attempting suicide, ever injecting heroin, and ever injecting opioids. The risk of NFOD among prisoners with a history of injecting drug use is high. An understanding of the risk factors for NFOD in this population can inform targeted, evidence-based interventions to reduce this risk. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Efficient optical injection locking of electronic oscillators

NASA Astrophysics Data System (ADS)

Cochran, S. R.; Wang, S. Y.

1989-05-01

The paper presents techniques for direct optical injection locking of electronic oscillators and analyzes the problem of direct optical injection locking of a common-source FET oscillator using a high impedance optoelectronic transducer. A figure-of-merit for optically injection locked oscillators is defined, and an experimental oscillator based on the design criteria was fabricated. The oscillator achieved efficient, high power operation and moderate locking bandwidth with small locking signal magnitude. The experimental results are consistent with the theoretical model.

The stimulation of central kappa opioid receptors decreases male sexual behavior and locomotor activity.

PubMed

Leyton, M; Stewart, J

1992-10-23

Systemic injections of the kappa (kappa) opioid receptor agonist U-50,488H decreased male sexual behavior, locomotor activity, body temperature and bodily grooming, and induced body flattening. The U-50,488H-induced inhibitions of male sexual behavior were prevented by systemic injections of naloxone and by intra-cranial injections of the kappa opioid antagonist nor-binaltorphimine (NBNI). Injections of NBNI to either the ventral tegmental area (VTA) or the nucleus accumbens septi (NAS) increased female-directed behavior, and prevented the U-50,488H-induced decreases in female-directed behavior. Intra-VTA NBNI prevented U-50,488H-induced decreases in the mean number of ejaculations, intra-NAS NBNI prevented U-50,488H-induced increases in copulation latencies. Intra-medial preoptic area (mPOA) injections of NBNI increased female-directed behavior, and attenuated U-50,488H-induced decreases in female-directed behavior as well as U-50,488H-induced increases in both copulation and ejaculation latencies. Injections of NBNI dorsal to the mPOA were ineffective. Two of 26 days following the central injection of NBNI, systemic injections of U-50,488H remained behaviorally ineffective, leaving both sexual behavior and locomotor activity undiminished. These results suggest that the stimulation of central kappa opioid receptors inhibits sexual behavior in the male rat; perhaps endogenous kappa opioid agonists induce sexual refractory periods.

Water-level altitudes and continuous and discrete water quality at and near an aquifer storage and recovery site, Bexar, Atascosa, and Wilson Counties, Texas, June 2004-September 2011

USGS Publications Warehouse

Crow, Cassi L.

2012-01-01

The U.S. Geological Survey (USGS), in cooperation with the San Antonio Water System (SAWS), collected data during 2004–11 to characterize the quality of native groundwater from the San Antonio segment of the Edwards aquifer (hereinafter, Edwards aquifer) and preinjection and postinjection water from the Carrizo aquifer (informal name commonly applied to the upper part of the Carrizo-Wilcox aquifer in the area) at and near an aquifer storage and recovery (ASR) site in Bexar, Atascosa, and Wilson Counties, Texas. Daily mean water-level altitude, water temperature, and specific conductance were measured continuously in a monitoring well on the ASR site to determine how injection and withdrawal at the ASR site might affect local groundwater. Groundwater samples were collected and analyzed for selected physical properties and constituents to characterize the quality of native groundwater from the Edwards aquifer and preinjection and postinjection water from the Carrizo aquifer near the ASR site to provide a better understanding of possible changes in the quality of groundwater near an active ASR site that might result from the mixing of water from different aquifers. During injection periods, the water-level altitude in the monitoring well generally increased as the amount of water being injected into all wells at the ASR site increased and decreased as the amount of water being injected into all wells at the ASR site decreased. During withdrawal periods, the water-level altitude in the monitoring well generally increased as the total volume of water being withdrawn from all wells at the ASR site decreased and generally decreased as the total volume of water being withdrawn from all wells increased. Daily mean water temperature fluctuated by less than 1 degree Celsius and was determined to be independent of injection or withdrawal conditions at the ASR site. Changes in daily mean specific-conductance values measured at four depths in the monitoring well at the ASR site occurred without regard to total ASR site injection or withdrawal volumes. No substantial differences were measured over time in major-ion, trace-element, or isotope chemistry of water samples collected from the wells that supplied water from the Edwards aquifer. Little variation in water chemistry was detected in the samples collected from four wells designed to inject and withdraw water at the ASR site, regardless of whether the ASR site was injecting or withdrawing water. The similarity of major-ion and isotope chemistry between the Edwards aquifer source wells and the four ASR wells indicates that little, if any, migration of injected water away from the ASR wells has occurred. In a well located closest to the ASR site in the direction of regional flow for the Carrizo aquifer, a greater alkalinity value and a smaller concentration of chloride were measured in the most recent sample than in all other samples collected at this well. Substantial increases in dissolved iron and manganese concentrations also were observed in this well. The increased alkalinity value and dissolved iron and manganese concentrations and the decreased chloride concentration in the well could indicate that the injected water from the Edwards aquifer had begun to move into at least a part of the strata supplying these wells and might be causing iron and manganese mobilization in the Carrizo aquifer.

78 FR 32081 - Airworthiness Directives; Aircraft Industries a.s. Airplanes

Federal Register 2010, 2011, 2012, 2013, 2014

2013-05-29

... Injection System WATER INJECTION circuit ON breakter. TCL TQ=min. 60% WATER INJECTION/ON push- Push and hold till amber button. WATER INJECTION signal comes on (on the front control panel) Before throttling back power: WATER INJECTION/OFF push- Push and check amber button. WATER INJECTION signal extinguishes...

New drostanolone metabolites in human urine by liquid chromatography time-of-flight tandem mass spectrometry and their application for doping control.

PubMed

Liu, Yang; Lu, Jianghai; Yang, Sheng; Zhang, Qingying; Xu, Youxuan

2016-04-01

Drostanolone is one of the most frequently detected anabolic androgenic steroids in doping control analysis. Here, we studied drostanolone urinary metabolic profiles using liquid chromatography quadruple time of flight mass spectrometry (LC-QTOF-MS) in full scan and targeted MS/MS modes with accurate mass measurement. The drug was administered to one healthy male volunteer and liquid-liquid extraction along with direct-injection were used to analyze urine samples. Chromatographic peaks for potential metabolites were identified with the theoretical [M-H](-) as a target ion in a full scan experiment and actual deprotonated ions were analyzed in targeted MS/MS mode. Eleven metabolites including five new sulfates, five glucuronide conjugates, and one free metabolite were confirmed for drostanolone. Due to the absence of useful fragment ions to illustrate the steroid ring structure of drostanolone phase II metabolites, gas chromatography mass spectrometry (GC-MS) was used to obtain structural details of the trimethylsilylated phase I metabolite released after enzymatic hydrolysis and a potential structure was proposed using a combined MS approach. Metabolite detection times were recorded and S4 (2α-methyl-5α-androstan-17-one-6β-ol-3α-sulfate) and G1 (2α-methyl-5α-androstan-17-one-3α-glucuronide) were thought to be new potential biomarkers for drostanolone misuse which can be detected up to 24days by liquid-liquid extraction and 7days by direct-injection analysis after intramuscular injection. S4 and G1 were also detected in two drostanolone-positive routine urine samples. Copyright © 2016 Elsevier Inc. All rights reserved.

The Incidence of Intravascular Needle Entrance during Inferior Alveolar Nerve Block Injection.

PubMed

Taghavi Zenouz, Ali; Ebrahimi, Hooman; Mahdipour, Masoumeh; Pourshahidi, Sara; Amini, Parisa; Vatankhah, Mahdi

2008-01-01

Dentists administer thousands of local anesthetic injections every day. Injection to a highly vascular area such as pterygomandibular space during an inferior alveolar nerve block has a high risk of intravascular needle entrance. Accidental intravascular injection of local anesthetic agent with vasoconstrictor may result in cardiovascular and central nervous system toxicity, as well as tachycardia and hypertension. There are reports that indicate aspiration is not performed in every injection. The aim of the present study was to assess the incidence of intravascular needle entrance in inferior alveolar nerve block injections. Three experienced oral and maxillofacial surgeons performed 359 inferior alveolar nerve block injections using direct or indirect techniques, and reported the results of aspiration. Aspirable syringes and 27 gauge long needles were used, and the method of aspiration was similar in all cases. Data were analyzed using t-test. 15.3% of inferior alveolar nerve block injections were aspiration positive. Intravascular needle entrance was seen in 14.2% of cases using direct and 23.3% of cases using indirect block injection techniques. Of all injections, 15.8% were intravascular on the right side and 14.8% were intravascular on the left. There were no statistically significant differences between direct or indirect block injection techniques (P = 0.127) and between right and left injection sites (P = 0.778). According to our findings, the incidence of intravascular needle entrance during inferior alveolar nerve block injection was relatively high. It seems that technique and maneuver of injection have no considerable effect in incidence of intravascular needle entrance.

The Incidence of Intravascular Needle Entrance during Inferior Alveolar Nerve Block Injection

PubMed Central

Taghavi Zenouz, Ali; Ebrahimi, Hooman; Mahdipour, Masoumeh; Pourshahidi, Sara; Amini, Parisa; Vatankhah, Mahdi

2008-01-01

Background and aims Dentists administer thousands of local anesthetic injections every day. Injection to a highly vascular area such as pterygomandibular space during an inferior alveolar nerve block has a high risk of intravascular needle entrance. Accidental intravascular injection of local anesthetic agent with vasoconstrictor may result in cardiovascular and central nervous system toxicity, as well as tachycardia and hypertension. There are reports that indicate aspiration is not performed in every injection. The aim of the present study was to assess the incidence of intravascular needle entrance in inferior alveolar nerve block injections. Materials and methods Three experienced oral and maxillofacial surgeons performed 359 inferior alveolar nerve block injections using direct or indirect techniques, and reported the results of aspiration. Aspirable syringes and 27 gauge long needles were used, and the method of aspiration was similar in all cases. Data were analyzed using t-test. Results 15.3% of inferior alveolar nerve block injections were aspiration positive. Intravascular needle entrance was seen in 14.2% of cases using direct and 23.3% of cases using indirect block injection techniques. Of all injections, 15.8% were intravascular on the right side and 14.8% were intravascular on the left. There were no statistically significant differences between direct or indirect block injection techniques (P = 0.127) and between right and left injection sites (P = 0.778). Conclusion According to our findings, the incidence of intravascular needle entrance during inferior alveolar nerve block injection was relatively high. It seems that technique and maneuver of injection have no considerable effect in incidence of intravascular needle entrance. PMID:23285329

XFM demonstrates preferential accumulation of a vanadyl-based MRI contrast agent in murine colonic tumors

PubMed Central

Mustafi, Devkumar; Ward, Jesse; Dougherty, Urszula; Bissonnette, Marc; Hart, John; Vogt, Stefan; Karczmar, Gregory S.

2016-01-01

Contrast agents that specifically enhance cancers on MRI would allow earlier detection. Vanadyl-based chelates (VCs) selectively enhance rodent cancers on MRI, suggesting selective uptake of VCs by cancers. Here we report X-ray fluorescence microscopy (XFM) of VC uptake by murine colon cancer. Colonic tumors in mice treated with azoxymethane/dextran sulfate sodium were identified by MRI. Then a gadolinium-based contrast agent and a VC were injected I.V.; mice were sacrificed and colons sectioned. VC distribution was sampled at 120 minutes after injection to evaluate the long term accumulation. Gadolinium distribution was sampled at 10 minutes after injection due to its rapid washout. XFM was performed on 72 regions of normal and cancerous colon from 5 normal mice and 4 cancer-bearing mice. XFM showed that all gadolinium was extracellular with similar concentrations in colon cancers and normal colon. In contrast, the average VC concentration was 2-fold higher in cancers vs. normal tissue (p<0.002). Cancers also contained numerous ‘hot spots’ with intracellular VC concentrations 6-fold higher than the concentration in normal colon (p<0.0001). No ‘hot spots’ were detected in normal colon. This is the first direct demonstration that VCs selectively accumulate in cancer cells, and thus may improve cancer detection. PMID:25813904

Pilot-Scale Demonstration of In-Situ Chemical Oxidation ...

EPA Pesticide Factsheets

A pilot-scale in situ chemical oxidation (ISCO) demonstration, involving subsurface injections of sodium permanganate (NaMnO4), was performed at the US Marine Corp Recruit Depot (MCRD), site 45 (Parris Island (PI), SC). The ground water was originally contaminated with perchloroethylene (PCE) (also known as tetrachloroethylene), a chlorinated solvent used in dry cleaner operations. High resolution site characterization involved multiple iterations of soil core sampling and analysis. Nested micro-wells and conventional wells were also used to sample and analyze ground water for PCE and decomposition products (i.e., trichloroethyelene (TCE), dichloroethylene (c-DCE, t-DCE), and vinyl chloride (VC)), collectively referred to as chlorinated volatile organic compounds (CVOC). This characterization methodology was used to develop and refine the conceptual site model and the ISCO design, not only by identifying CVOC contamination but also by eliminating uncontaminated portions of the aquifer from further ISCO consideration. Direct-push injection was selected as the main method of NaMnO4 delivery due to its flexibility and low initial capital cost. Site impediments to ISCO activities in the source area involved subsurface utilities, including a high pressure water main, a high voltage power line, a communication line, and sanitary and stormwater sewer lines. Utility markings were used in conjunction with careful planning and judicious selection of injection locations. A

GRIN: "GRoup versus INdividual physiotherapy following lower limb intra-muscular Botulinum Toxin-A injections for ambulant children with cerebral palsy: an assessor-masked randomised comparison trial": study protocol.

PubMed

Thomas, Rachel E; Johnston, Leanne M; Boyd, Roslyn N; Sakzewski, Leanne; Kentish, Megan J

2014-02-07

Cerebral palsy is the most common cause of physical disability in childhood. Spasticity is a significant contributor to the secondary impairments impacting functional performance and participation. The most common lower limb spasticity management is focal intramuscular injections of Botulinum Toxin-Type A accompanied by individually-delivered (one on one) physiotherapy rehabilitation. With increasing emphasis on improving goal-directed functional activity and participation within a family-centred framework, it is timely to explore whether physiotherapy provided in a group could achieve comparable outcomes, encouraging providers to offer flexible models of physiotherapy delivery. This study aims to compare individual to group-based physiotherapy following intramuscular Botulinum Toxin-A injections to the lower limbs for ambulant children with cerebral palsy aged four to fourteen years. An assessor-masked, block randomised comparison trial will be conducted with random allocation to either group-based or individual physiotherapy. A sample size of 30 (15 in each study arm) will be recruited. Both groups will receive six hours of direct therapy following Botulinum Toxin-A injections in either an individual or group format with additional home programme activities (three exercises to be performed three times a week). Study groups will be compared at baseline (T1), then at 10 weeks (T2, efficacy) and 26 weeks (T3, retention) post Botulinum Toxin-A injections. Primary outcomes will be caregiver/s perception of and satisfaction with their child's occupational performance goals (Canadian Occupational Performance Measure) and quality of gait (Edinburgh Visual Gait Score) with a range of secondary outcomes across domains of the International Classification of Disability, Functioning and Health. This paper outlines the study protocol including theoretical basis, study hypotheses and outcome measures for this assessor-masked, randomised comparison trial comparing group versus individual models of physiotherapy following intramuscular injections of Botulinum Toxin-A to the lower limbs for ambulant children with cerebral palsy. ACTRN12611000454976.

Electrokinetic Sample Preconcentration and Hydrodynamic Sample Injection for Microchip Electrophoresis Using a Pneumatic Microvalve

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

Cong, Yongzheng; Katipamula, Shanta; Geng, Tao

2016-02-01

A microfluidic platform was developed to perform online electrokinetic sample preconcentration and rapid hydrodynamic sample injection for electrophoresis using a single microvalve. The PDMS microchip consists of a separation channel, a side channel for sample introduction, and a control channel which is used as a pneumatic microvalve aligned at the intersection of the two flow channels. The closed microvalve, created by multilayer soft lithography, can serve as a preconcentrator under an applied electric potential, enabling current to pass through while blocking bulk flow. Once analytes are concentrated, the valve is briefly opened and the stacked sample is pressure injected intomore » the separation channel for electrophoretic separation. Fluorescently labeled peptides were enriched by a factor of ~450 in 230 s. The performance of the platform was validated by the online preconcentration, injection and electrophoretic separation of fluorescently labeled peptides. This method enables both rapid analyte concentration and controlled injection volume for high sensitivity, high resolution capillary electrophoresis.« less

Effect of the Ethanol Injection Moment During Compression Stroke on the Combustion of Ethanol - Diesel Dual Direct Injection Engine

NASA Astrophysics Data System (ADS)

Liang, Yu; Zhou, Liying; Huang, Haomin; Xu, Mingfei; Guo, Mei; Chen, Xin

2018-01-01

A set of GDI system is installed on a F188 single-cylinder, air-cooled and direct injection diesel engine, which is used for ethanol injection, with the injection time controlled by the crank angle signal collected by AVL angle encoder. The injection of ethanol amounts to half of the thermal equivalent of an original diesel fuel. A 3D combustion model is established for the ethanol - diesel dual direct injection engine. Diesel was injected from the original fuel injection system, with a fuel supply advance angle of 20°CA. The ethanol was injected into the cylinder during compression process. Diesel injection began after the completion of ethanol injection. Ethanol injection starting point of 240°CA, 260°CA, 280°CA, 300°CA and 319.4°CA were simulated and analyzed. Due to the different timing of ethanol injection, the ignition of the ethanol mixture when diesel fires, results in non-uniform ignition distribution and flame propagation rate, since the distribution and concentration gradients of the ethanol mixture in the cylinder are different, thus affecting the combustion process. The results show that, when ethanol is injected at 319.4°CA, the combustion heat release rate and the pressure rise rate during the initial stage are the highest. Also, the maximum combustion pressure, with a relatively advance phase, is the highest. In case of later initial ethanol injection, the average temperature in the cylinder during the initial combustion period will have a faster rise. In case of initial injection at 319.4°CA, the average temperature in the cylinder is the highest, followed by 240°CA ethanol injection. In the post-combustion stage, the earlier ethanol injection will result in higher average temperature in the cylinder and more complete fuel combustion. The injection of ethanol at 319.4°CA produces earlier and highest NOX emissions.

Insights on the injection mechanisms inferred from AMS fabrics of sand injectites in a turbiditic system, the exemple of Bevon area of the SE Basin (France).

NASA Astrophysics Data System (ADS)

Robion, Philippe; Mehl, Caroline

2016-04-01

We propose to investigate the set up mechanisms of sands injection in the case of dykes injected in host marls of Aptian-Albian age in the Vocontian basin (SE France). Several models have been proposed for a downward injection of the dyke in the Bevons area and we guess that AMS fabric investigations can be used to infer the flow direction. 144 drill cores distributed on 14 sites were sampled, among which 8 sites in the injectites and 6 sites in the host rocks. The studied dykes are generally of a few decimeters thick and are setting up in both in vertical or oblique position with respect to the subhorizontal bedding of the host rocks. There were sampled from one side to the other in order to track the flow direction by identification of imbricated fabric. Magnetic mineralogy, i.e. unblocking temperature inferred from IRM 3 axes demagnetization, indicates that the ferromagnetics s.l. mineralogy is dominated by an assemblage of magnetite (unblocking temperature Tub=580°C) and pyrrhotite (Tub=325°C). Magnetic susceptibility is low, typical for siliciclastic rocks, ranging from 4x10-5 up to 1.7x10-4 SI. Degree of magnetic anisotropy is likely representative of AMS measurements in sedimentary rocks with weak values, below than 5 %. In marly host rocks magnetic mineralogy is dominated by pyrrhotite associated with magnetite and both the magnetic susceptibility and degree of anisotropy are slightly lower than for injectites. Regarding magnetic fabric axes distribution, despite some dispersion, the results show that minimum axes of AMS (K3) are parallel to the dyke plane, and maximum axes (K1) are roughly in horizontal position. In marly host rocks, the magnetic fabric is related to tectonic shortening. We interpret that the host rocks have recorded the regional tectonic imprint while the magnetic fabric of the injectites are related to early sedimentary processes. The mechanism of set up proposed to explain the magnetic fabric in the Bevon injectites is a step-by-step process of filling the pre-existing fractures with highly fluidized sand and a compaction direction parallel to dyke plane. A late diagenetic cementation affecting the injectites network prevents any further deformation during tectonic inversion.

Does opioid substitution treatment in prisons reduce injecting-related HIV risk behaviours? A systematic review.

PubMed

Larney, Sarah

2010-02-01

To review systematically the evidence on opioid substitution treatment (OST) in prisons in reducing injecting-related human immunodeficiency virus (HIV) risk behaviours. Systematic review in accordance with guidelines of the Cochrane Collaboration. Electronic databases were searched to identify studies of prison-based opioid substitution treatment programmes that included assessment of effects of prison OST on injecting drug use, sharing of needles and syringes and HIV incidence. Published data were used to calculate risk ratios for outcomes of interest. Risk ratios were not pooled due to the low number of studies and differences in study designs. Five studies were included in the review. Poor follow-up rates were reported in two studies, and representativeness of the sample was uncertain in the remaining three studies. Compared to inmates in control conditions, for treated inmates the risk of injecting drug use was reduced by 55-75% and risk of needle and syringe sharing was reduced by 47-73%. No study reported a direct effect of prison OST on HIV incidence. There may be a role for OST in preventing HIV transmission in prisons, but methodologically rigorous research addressing this question specifically is required. OST should be implemented in prisons as part of comprehensive HIV prevention programmes that also provide condoms and sterile injecting and tattooing equipment.

Effect of cavitation in high-pressure direct injection

NASA Astrophysics Data System (ADS)

Aboulhasanzadeh, Bahman; Johnsen, Eric

2015-11-01

As we move toward higher pressures for Gasoline Direct Injection and Diesel Direct Injection, cavitation has become an important issue. To better understand the effect of cavitation on the nozzle flow and primary atomization, we use a high-order accurate Discontinuous Galerkin approach using multi-GPU parallelism to simulate the compressible flow inside and outside the nozzle. Phase change is included using the six-equations model. We investigate the effect of nozzle geometry on cavitation inside the injector and on primary atomization outside the nozzle.

Experimental feasibility study of radial injection cooling of three-pad radial air foil bearings

NASA Astrophysics Data System (ADS)

Shrestha, Suman K.

Air foil bearings use ambient air as a lubricant allowing environment-friendly operation. When they are designed, installed, and operated properly, air foil bearings are very cost effective and reliable solution to oil-free turbomachinery. Because air is used as a lubricant, there are no mechanical contacts between the rotor and bearings and when the rotor is lifted off the bearing, near frictionless quiet operation is possible. However, due to the high speed operation, thermal management is one of the very important design factors to consider. Most widely accepted practice of the cooling method is axial cooling, which uses cooling air passing through heat exchange channels formed underneath the bearing pad. Advantage is no hardware modification to implement the axial cooling because elastic foundation structure of foil bearing serves as a heat exchange channels. Disadvantage is axial temperature gradient on the journal shaft and bearing. This work presents the experimental feasibility study of alternative cooling method using radial injection of cooling air directly on the rotor shaft. The injection speeds, number of nozzles, location of nozzles, total air flow rate are important factors determining the effectiveness of the radial injection cooling method. Effectiveness of the radial injection cooling was compared with traditional axial cooling method. A previously constructed test rig was modified to accommodate a new motor with higher torque and radial injection cooling. The radial injection cooling utilizes the direct air injection to the inlet region of air film from three locations at 120° from one another with each location having three axially separated holes. In axial cooling, a certain axial pressure gradient is applied across the bearing to induce axial cooling air through bump foil channels. For the comparison of the two methods, the same amount of cooling air flow rate was used for both axial cooling and radial injection. Cooling air flow rate was referenced to the rotor surface speed for radial injection cooling. The mass flow rates for the radial injection were 0.032, 0.0432, 0.054 and 0.068 Kg/min, which result in average injection speed of 150, 200, 250 and 300% of rotor surface speed. Several thermocouples were attached at various circumferential directions of the bearing sleeve, two plenums, bearing holder and ball bearing housings to collect the temperature data of the bearing at 30krpm under 10lb of load. Both axial cooling and radial injection are effective cooling mechanism and effectiveness of both cooling methods is directly proportional to the total mass flow rates. However, axial cooling is slightly more efficient in controlling the average temperature of the bearing sleeve, but results in higher thermal gradient of the shaft along the axial direction and also higher thermal gradient of the bearing sleeve along the circumferential direction compared to the radial injection cooling. The smaller thermal gradient of the radial injection cooling is due to the direct cooling effect of the shaft by impinging jets. While the axial cooling has an effect on only the bearing, the radial injection has a cooling effect on both the bearing sleeve and shaft. It is considered the radial injection cooling needs to be further optimized in terms of number of injection holes and their locations.

Sample flow switching techniques on microfluidic chips.

PubMed

Pan, Yu-Jen; Lin, Jin-Jie; Luo, Win-Jet; Yang, Ruey-Jen

2006-02-15

This paper presents an experimental investigation into electrokinetically focused flow injection for bio-analytical applications. A novel microfluidic device for microfluidic sample handling is presented. The microfluidic chip is fabricated on glass substrates using conventional photolithographic and chemical etching processes and is bonded using a high-temperature fusion method. The proposed valve-less device is capable not only of directing a single sample flow to a specified output port, but also of driving multiple samples to separate outlet channels or even to a single outlet to facilitate sample mixing. The experimental results confirm that the sample flow can be electrokinetically pre-focused into a narrow stream and guided to the desired outlet port by means of a simple control voltage model. The microchip presented within this paper has considerable potential for use in a variety of applications, including high-throughput chemical analysis, cell fusion, fraction collection, sample mixing, and many other applications within the micro-total-analysis systems field.

Sensitive flow-injection spectrophotometric analysis of bromopride

NASA Astrophysics Data System (ADS)

Lima, Liliane Spazzapam; Weinert, Patrícia Los; Pezza, Leonardo; Pezza, Helena Redigolo

2014-12-01

A flow injection spectrophotometric procedure employing merging zones is proposed for direct bromopride determination in pharmaceutical formulations and biological fluids. The proposed method is based on the reaction between bromopride and p-dimethylaminocinnamaldehyde (p-DAC) in acid medium, in the presence of sodium dodecyl sulfate (SDS), resulting in formation of a violet product (λmax = 565 nm). Experimental design methodologies were used to optimize the experimental conditions. The Beer-Lambert law was obeyed in a bromopride concentration range of 3.63 × 10-7 to 2.90 × 10-5 mol L-1, with a correlation coefficient (r) of 0.9999. The limits of detection and quantification were 1.07 × 10-7 and 3.57 × 10-7 mol L-1, respectively. The proposed method was successfully applied to the determination of bromopride in pharmaceuticals and human urine, and recoveries of the drug from these media were in the ranges 99.6-101.2% and 98.6-102.1%, respectively. This new flow injection procedure does not require any sample pretreatment steps.

Rapid non-invasive quality control of semi-finished products for the food industry by direct injection mass spectrometry headspace analysis: the case of milk powder, whey powder and anhydrous milk fat.

PubMed

Makhoul, Salim; Yener, Sine; Khomenko, Iuliia; Capozzi, Vittorio; Cappellin, Luca; Aprea, Eugenio; Scampicchio, Matteo; Gasperi, Flavia; Biasioli, Franco

2016-09-01

In this study, we demonstrated the suitability of direct injection mass spectrometry headspace analysis for rapid non-invasive quality control of semi-finished dairy ingredients, such as skim milk powder (SMP), whole milk powder (WMP), whey powder (WP) and anhydrous milk fat (AMF), which are widely used as ingredients in the food industry. In this work, for the first time, we applied proton transfer reaction-mass spectrometry (PTR-MS) with a time-of-flight (ToF) analyzer for the rapid and non-invasive analysis of volatile compounds in different samples of SMP, WMP, WP and AMF. We selected different dairy ingredients in various concrete situations (e.g. same producer and different expiration times, different producers and same days of storage, different producers) based on their sensory evaluation. PTR-ToF-MS allowed the separation and characterization of different samples based on the volatile organic compound (VOC) profiles. Statistically significant differences in VOC content were generally coherent with differences in sensory evaluation, particularly for SMP, WMP and WP. The good separation of SMP samples from WMP samples suggested the possible application of PTR-ToF-MS to detect possible cases of adulteration of dairy ingredients for the food industry. Our findings demonstrate the efficient and rapid differentiation of dairy ingredients on the basis of the released VOCs via PTR-ToF-MS analysis and suggest this method as a versatile tool (1) for the facilitation/optimization of the selection of dairy ingredients in the food industry and (2) and for the prompt innovation in the production of dairy ingredients. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Measuring oxygen yields of a thermal conversion/elemental analyzer-isotope ratio mass spectrometer for organic and inorganic materials through injection of CO.

PubMed

Yin, Xijie; Chen, Zhigang

2014-12-01

The thermal conversion/elemental analyzer-isotope ratio mass spectrometer (TC/EA-IRMS) is widely used to measure the δ(18) O value of various substances. A premise for accurate δ(18) O measurement is that the oxygen in the sample can be converted into carbon monoxide (CO) quantitatively or at least proportionally. Therefore, a precise method to determine the oxygen yield of TC/EA-IRMS measurements is needed. Most studies have used the CO peak area obtained from a known amount of a solid reference material (for example, benzoic acid) to calibrate the oxygen yield of the sample. Although it was assumed that the oxygen yield of the solid reference material is 100%, no direct evidence has been provided. As CO is the analyte gas for δ(18) O measurement by IRMS, in this study, we use a six-port valve to inject CO gas into the TC/EA. The CO is carried to the IRMS by the He carrier gas and the CO peak area is measured by the IRMS. The CO peak area thus obtained from a known amount of the injected CO is used to calibrate the oxygen yield of the sample. The oxygen yields of commonly used organic and inorganic reference materials such as benzoic acid (C6 H5 COOH), silver phosphate (Ag3 PO4 ), calcium carbonate (CaCO3 ) and silicon dioxide (SiO2 ) are investigated at different reactor temperatures and sample sizes. We obtained excellent linear correlation between the peak area for the injected CO and its oxygen atom amount. C6 H5 COOH has the highest oxygen yield, followed by Ag3 PO4 , CaCO3 and SiO2 . The oxygen yields of TC/EA-IRMS are less than 100% for both organic and inorganic substances, but the yields are relatively stable at the specified reactor temperature and for a given quantity of sample. Copyright © 2014 John Wiley & Sons, Ltd.

Simultaneous analysis of seven oligopeptides in microbial fuel cell by micro-fluidic chip with reflux injection mode.

PubMed

Wang, Wei; Wang, Zijian; Lin, Xiuli; Wang, ZongWen; Fu, FengFu

2012-10-15

In this work, a reflux injection mode for the cross form micro-fluidic chip was studied. This injection mode could flexibly control the length of sample plug from less than one channel width (<83 μm) to tens of channel widths (millimeter-sized) by adjusting the injection time. Namely, the separation resolution or sample detection sensitivity could be selectively improved by changing injection time. Composed of four steps, the reflux injection mode alleviated the electrophoretic sampling bias and prevented sample leakage successfully. On a micro-fluidic chip coupled with laser induced fluorescence (LIF) detector, the injection mode was applied to separate seven oligopeptides, namely GG, GL, RPP, KPV, VKK, WYD and YWS. All analytes were completely separated and detected within 12 min with detection limits of 25-625 nmol/L. At last, the proposed method had been successfully applied to detect oligopeptides consumed by bacillus licheniformis in anode chamber of microbial fuel cell (MFC) to study the effect of oligopeptides on the MFC running. Copyright © 2012 Elsevier B.V. All rights reserved.

Direct Analysis of Low-Volatile Molecular Marker Extract from Airborne Particulate Matter Using Sensitivity Correction Method

PubMed Central

Irei, Satoshi

2016-01-01

Molecular marker analysis of environmental samples often requires time consuming preseparation steps. Here, analysis of low-volatile nonpolar molecular markers (5-6 ring polycyclic aromatic hydrocarbons or PAHs, hopanoids, and n-alkanes) without the preseparation procedure is presented. Analysis of artificial sample extracts was directly conducted by gas chromatography-mass spectrometry (GC-MS). After every sample injection, a standard mixture was also analyzed to make a correction on the variation of instrumental sensitivity caused by the unfavorable matrix contained in the extract. The method was further validated for the PAHs using the NIST standard reference materials (SRMs) and then applied to airborne particulate matter samples. Tests with the SRMs showed that overall our methodology was validated with the uncertainty of ~30%. The measurement results of airborne particulate matter (PM) filter samples showed a strong correlation between the PAHs, implying the contributions from the same emission source. Analysis of size-segregated PM filter samples showed that their size distributions were found to be in the PM smaller than 0.4 μm aerodynamic diameter. The observations were consistent with our expectation of their possible sources. Thus, the method was found to be useful for molecular marker studies. PMID:27127511

Influence of high-conductivity buffer composition on field-enhanced sample injection coupled to sweeping in CE.

PubMed

Anres, Philippe; Delaunay, Nathalie; Vial, Jérôme; Thormann, Wolfgang; Gareil, Pierre

2013-02-01

The aim of this work was to clarify the mechanism taking place in field-enhanced sample injection coupled to sweeping and micellar EKC (FESI-Sweep-MEKC), with the utilization of two acidic high-conductivity buffers (HCBs), phosphoric acid or sodium phosphate buffer, in view of maximizing sensitivity enhancements. Using cationic model compounds in acidic media, a chemometric approach and simulations with SIMUL5 were implemented. Experimental design first enabled to identify the significant factors and their potential interactions. Simulation demonstrates the formation of moving boundaries during sample injection, which originate at the initial sample/HCB and HCB/buffer discontinuities and gradually change the compositions of HCB and BGE. With sodium phosphate buffer, the HCB conductivity increased during the injection, leading to a more efficient preconcentration by staking (about 1.6 times) than with phosphoric acid alone, for which conductivity decreased during injection. For the same injection time at constant voltage, however, a lower amount of analytes was injected with sodium phosphate buffer than with phosphoric acid. Consequently sensitivity enhancements were lower for the whole FESI-Sweep-MEKC process. This is why, in order to maximize sensitivity enhancements, it is proposed to work with sodium phosphate buffer as HCB and to use constant current during sample injection. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous detection of antibacterial sulfonamides in a microfluidic device with amperometry.

PubMed

Won, So-Young; Chandra, Pranjal; Hee, Tak Seong; Shim, Yoon-Bo

2013-01-15

A highly sensitive and robust method for simultaneous detection of five sulfonamide drugs is developed by integrating the preconcentration and separation steps in a microfluidic device. An ampetrometry is performed for the selective detection of sulfonamides using an aluminum oxide-gold nanoparticle (Al(2)O(3)-AuNPs) modified carbon paste (CP) electrode at the end of separation channel. The preconcentration capacity of the channel is enhanced by using the field amplified sample stacking and the field amplified sample injection techniques. The experimental parameters affecting the analytical performances, such as pH, % of Al(2)O(3), volume of AuNPs, buffer concentration, and water plug length are optimized. A reproducible response is observed during the multiple injections of samples with RSDs<4%. The calibration plots are linear with the correlation coefficient between 0.991 and 0.997 over the range between 0.01 and 2025pM. The detection limits of five drugs are determined to be between 0.91 (±0.03) and 2.21 (±0.09)fM. The interference effects of common biological compounds are also investigated and the applicability of the method to the direct analysis of sulfonamides in real meat samples is successfully demonstrated. Long term stability of the modified electrode was also investigated. Copyright © 2012 Elsevier B.V. All rights reserved.

Thermal analysis in the rat glioma model during directly multipoint injection hyperthermia incorporating magnetic nanoparticles.

PubMed

Liu, Lianke; Ni, Fang; Zhang, Jianchao; Wang, Chunyu; Lu, Xiang; Guo, Zhirui; Yao, Shaowei; Shu, Yongqian; Xu, Ruizhi

2011-12-01

Hyperthermia incorporating magnetic nanoparticles (MNPs) is a hopeful therapy to cancers and steps into clinical tests at present. However, the clinical plan of MNPs deposition in tumors, especially applied for directly multipoint injection hyperthermia (DMIH), and the information of temperature rise in tumors by DMIH is lack of studied. In this paper, we mainly discussed thermal distributions induced by MNPs in the rat brain tumors during DMIH. Due to limited experimental measurement for detecting thermal dose of tumors, and in order to acquire optimized results of temperature distributions clinically needed, we designed the thermal model in which three types of MNPs injection for hyperthermia treatments were simulated. The simulated results showed that MNPs injection plan played an important role in determining thermal distribution, as well as the overall dose of MNPs injected. We found that as injected points enhanced, the difference of temperature in the whole tumor volume decreased. Moreover, from temperature detecting data by Fiber Optic Temperature Sensors (FOTSs) in glioma bearing rats during MNPs hyperthermia, we found the temperature errors by FOTSs reduced as the number of points injected enhanced. Finally, the results showed that the simulations are preferable and the optimized plans of the numbers and spatial positions of MNPs points injected are essential during direct injection hyperthermia.

A volumetric flow sensor for automotive injection systems

NASA Astrophysics Data System (ADS)

Schmid, U.; Krötz, G.; Schmitt-Landsiedel, D.

2008-04-01

For further optimization of the automotive power train of diesel engines, advanced combustion processes require a highly flexible injection system, provided e.g. by the common rail (CR) injection technique. In the past, the feasibility to implement injection nozzle volumetric flow sensors based on the thermo-resistive measurement principle has been demonstrated up to injection pressures of 135 MPa (1350 bar). To evaluate the transient behaviour of the system-integrated flow sensors as well as an injection amount indicator used as a reference method, hydraulic simulations on the system level are performed for a CR injection system. Experimentally determined injection timings were found to be in good agreement with calculated values, especially for the novel sensing element which is directly implemented into the hydraulic system. For the first time pressure oscillations occurring after termination of the injection pulse, predicted theoretically, could be verified directly in the nozzle. In addition, the injected amount of fuel is monitored with the highest resolution ever reported in the literature.

A method for direct, semi-quantitative analysis of gas phase samples using gas chromatography-inductively coupled plasma-mass spectrometry

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

Carter, Kimberly E; Gerdes, Kirk

2013-07-01

A new and complete GC–ICP-MS method is described for direct analysis of trace metals in a gas phase process stream. The proposed method is derived from standard analytical procedures developed for ICP-MS, which are regularly exercised in standard ICP-MS laboratories. In order to implement the method, a series of empirical factors were generated to calibrate detector response with respect to a known concentration of an internal standard analyte. Calibrated responses are ultimately used to determine the concentration of metal analytes in a gas stream using a semi-quantitative algorithm. The method was verified using a traditional gas injection from a GCmore » sampling valve and a standard gas mixture containing either a 1 ppm Xe + Kr mix with helium balance or 100 ppm Xe with helium balance. Data collected for Xe and Kr gas analytes revealed that agreement of 6–20% with the actual concentration can be expected for various experimental conditions. To demonstrate the method using a relevant “unknown” gas mixture, experiments were performed for continuous 4 and 7 hour periods using a Hg-containing sample gas that was co-introduced into the GC sample loop with the xenon gas standard. System performance and detector response to the dilute concentration of the internal standard were pre-determined, which allowed semi-quantitative evaluation of the analyte. The calculated analyte concentrations varied during the course of the 4 hour experiment, particularly during the first hour of the analysis where the actual Hg concentration was under predicted by up to 72%. Calculated concentration improved to within 30–60% for data collected after the first hour of the experiment. Similar results were seen during the 7 hour test with the deviation from the actual concentration being 11–81% during the first hour and then decreasing for the remaining period. The method detection limit (MDL) was determined for the mercury by injecting the sample gas into the system following a period of equilibration. The MDL for Hg was calculated as 6.8 μg · m -3. This work describes the first complete GC–ICP-MS method to directly analyze gas phase samples, and detailed sample calculations and comparisons to conventional ICP-MS methods are provided.« less

University of Idaho's low-speed flex fuel direct-injected 797cc two-stroke rear drive snowmobile.

DOT National Transportation Integrated Search

2012-06-01

The University of Idahos entry into the 2012 SAE Clean Snowmobile Challenge uses a Ski-Doo XP chassis with a low-speed 797 cc direct-injection two-stroke powered snowmobile modified for flex fuel use on blended ethanol fuel. A battery-less direct ...

Analysis of Androgenic Steroids in Environmental Waters by Large-volume Injection Liquid Chromatography Tandem Mass Spectrometry

PubMed Central

Backe, Will J.; Ort, Christoph; Brewer, Alex J.; Field, Jennifer A.

2014-01-01

A new method was developed for the analysis of natural and synthetic androgenic steroids and their selected metabolites in aquatic environmental matrices using direct large-volume injection (LVI) high performance liquid chromatography (HPLC) tandem mass spectrometry (MS/MS). Method accuracy ranged from 88 to 108% for analytes with well-matched internal standards. Precision, quantified by relative standard deviation (RSD), was less than 12%. Detection limits for the method ranged from 1.2 to 360 ng/L. The method was demonstrated on a series of 1-hr composite wastewater influent samples collected over a day with the purpose of assessing temporal profiles of androgen loads in wastewater. Testosterone, androstenedione, boldenone, and nandrolone were detected in the sample series at concentrations up to 290 ng/L and loads up to 535 mg. Boldenone, a synthetic androgen, had a temporal profile that was strongly correlated to testosterone, a natural human androgen, suggesting its source may be endogenous. An analysis of the sample particulate fraction revealed detectable amounts of sorbed testosterone and androstenedione. Androstenedione sorbed to the particulate fraction accounted for an estimated five to seven percent of the total androstenedione mass. PMID:21391574

Analysis of androgenic steroids in environmental waters by large-volume injection liquid chromatography tandem mass spectrometry.

PubMed

Backe, Will J; Ort, Christoph; Brewer, Alex J; Field, Jennifer A

2011-04-01

A new method was developed for the analysis of natural and synthetic androgenic steroids and their selected metabolites in aquatic environmental matrixes using direct large-volume injection (LVI) high-performance liquid chromatography (HPLC) tandem mass spectrometry (MS/MS). Method accuracy ranged from 87.6 to 108% for analytes with well-matched internal standards. Precision, quantified by relative standard deviation (RSD), was less than 12%. Detection limits for the method ranged from 1.2 to 360 ng/L. The method was demonstrated on a series of 1 h composite wastewater influent samples collected over a day with the purpose of assessing temporal profiles of androgen loads in wastewater. Testosterone, androstenedione, boldenone, and nandrolone were detected in the sample series at concentrations up to 290 ng/L and loads up to 535 mg/h. Boldenone, a synthetic androgen, had a temporal profile that was strongly correlated to testosterone, a natural human androgen, suggesting its source may be endogenous. An analysis of the sample particulate fraction revealed detectable amounts of sorbed testosterone and androstenedione. Androstenedione sorbed to the particulate fraction accounted for an estimated 5 to 7% of the total androstenedione mass.

Micro-injector for capillary electrophoresis.

PubMed

Sáiz, Jorge; Koenka, Israel Joel; García-Ruiz, Carmen; Müller, Beat; Chwalek, Thomas; Hauser, Peter C

2015-08-01

A novel micro-injector for capillary electrophoresis for the handling of samples with volumes down to as little as 300 nL was designed and built in our laboratory for analyses in which the available volume is a limitation. The sample is placed into a small cavity located directly in front of the separation capillary, and the injection is then carried out automatically by controlled pressurization of the chamber with compressed air. The system also allows automated flushing of the injection chamber as well as of the capillary. In a trial with a capillary electrophoresis system with contactless conductivity detector, employing a capillary of 25 μm diameter, the results showed good stability of migration times and peak areas. To illustrate the technique, the fast separation of five inorganic cations (Na(+) , K(+) , NH4 (+) , Ca(2+) , and Mg(2+) ) was set up. This could be achieved in less than 3 min, with good limits of detection (10 μM) and linear ranges (between about 10 and 1000 μM). The system was demonstrated for the determination of the inorganic cations in porewater samples of a lake sediment core. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Staged direct injection diesel engine

DOEpatents

Baker, Quentin A.

1985-01-01

A diesel engine having staged injection for using lower cetane number fuels than No. 2 diesel fuel. The engine includes a main fuel injector and a pilot fuel injector. Pilot and main fuel may be the same fuel. The pilot injector injects from five to fifteen percent of the total fuel at timings from 20.degree. to 180.degree. BTDC depending upon the quantity of pilot fuel injected, the fuel cetane number and speed and load. The pilot fuel injector is directed toward the centerline of the diesel cylinder and at an angle toward the top of the piston, avoiding the walls of the cylinder. Stratification of the early injected pilot fuel is needed to reduce the fuel-air mixing rate, prevent loss of pilot fuel to quench zones, and keep the fuel-air mixture from becoming too fuel lean to become effective. In one embodiment, the pilot fuel injector includes a single hole for injection of the fuel and is directed at approximately 48.degree. below the head of the cylinder.

Stability considerations of aspartame in the direct analysis of artificial sweeteners in water samples using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).

PubMed

Berset, Jean-Daniel; Ochsenbein, Nicole

2012-07-01

A HPLC-MS/MS method is presented for the simultaneous determination of frequently used artificial sweeteners (ASs) and the main metabolite of aspartame (ASP), diketopiperazine (DKP), in environmental water samples using the direct-injection (DI) technique, thereby achieving limits of quantification (LOQ) of 10 ng L(-1). For a reliable quantification of ASP pH should be adjusted to 4.3 to prevent formation of the metabolite. Acesulfame (ACE), saccharin (SAC), cyclamate (CYC) and sucralose (SUC) were ubiquitously found in water samples. Highest concentrations up to 61 μg L(-1) of ACE were found in wastewater effluents, followed by surface water with concentrations up to 7 μg L(-1), lakes up to 600 ng L(-1) and groundwater and tap water up to 70 ng L(-1). The metabolite DKP was only detected in wastewater up to 200 ng L(-1) and at low detection frequencies. Copyright © 2012 Elsevier Ltd. All rights reserved.

Determination of residual solvents in pharmaceuticals by thermal desorption-GC/MS.

PubMed

Hashimoto, K; Urakami, K; Fujiwara, Y; Terada, S; Watanabe, C

2001-05-01

A novel method for the determination of residual solvents in pharmaceuticals by thermal desorption (TD)-GC/MS has been established. A programmed temperature pyrolyzer (double shot pyrolyzer) is applied for the TD. This method does not require any sample pretreatment and allows very small amounts of the sample. Directly desorbed solvents from intact pharmaceuticals (ca. 1 mg) in the desorption cup (5 mm x 3.8 mm i.d.) were cryofocused at the head of a capillary column prior to a GC/MS analysis. The desorption temperature was set at a point about 20 degrees C higher than the melting point of each sample individually, and held for 3 min. The analytical results using 7 different pharmaceuticals were in agreement with those obtained by direct injection (DI) of the solution, followed by USP XXIII. This proposed TD-GC/MS method was demonstrated to be very useful for the identification and quantification of residual solvents. Furthermore, this method was simple, allowed rapid analysis and gave good repeatability.

Determination of Aniline and Its Derivatives in Environmental Water by Capillary Electrophoresis with On-Line Concentration

PubMed Central

Liu, Shuhui; Wang, Wenjun; Chen, Jie; Sun, Jianzhi

2012-01-01

This paper describes a simple, sensitive and environmentally benign method for the direct determination of aniline and its derivatives in environmental water samples by capillary zone electrophoresis (CZE) with field-enhanced sample injection. The parameters that influenced the enhancement and separation efficiencies were investigated. Surprisingly, under the optimized conditions, two linear ranges for the calibration plot, 1–50 ng/mL and 50–1000 ng/mL (R > 0.998), were obtained. The detection limit was in the range of 0.29–0.43 ng/mL. To eliminate the effect of the real sample matrix on the stacking efficiency, the standard addition method was applied to the analysis of water samples from local rivers. PMID:22837668

A micro-fluidic sub-microliter sample introduction system for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry using external aqueous calibration

NASA Astrophysics Data System (ADS)

Cheng, Heyong; Liu, Jinhua; Xu, Zigang; Yin, Xuefeng

2012-07-01

A microfluidic sub-microliter sample introducing system was developed for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry (ICP-MS). It consisted of a microfluidic chip integrating variable-volume sampling channels (0.1-0.8 μL), an eight-way multi-functional valve used in flow injection analysis (FIA), a syringe pump and a peristaltic pump of the Ar ICP-MS instrument. Three solutions, i.e., 15, 40 and 100 g L- 1 glucose in 20% ethanol were used to simulate Chinese rice wine of the dry type, the semidry type and the semisweet type, each. The effects of their volume introduced into ICP-MS on the plasma stability and ICP-MS intensities were studied. The experimental results showed that neither alteration of plasma stability nor carbon deposition was observed when the sampling volume of 20% ethanol containing 100 g L- 1 glucose was downscaled to 0.8 μL. Further reducing the sampling volume to 0.4 μL, no significant difference between the intensities of multi-element standard prepared in three simulated Chinese rice wine matrices and those in aqueous solution was observed. It indicated no negative effect of Chinese rice wine matrix on the ICP-MS intensities. A sampling volume of 0.4 μL was considered to be a good compromise between sensitivity and matrix effect. The flow rate of the carrier was chosen as 20 μL min- 1 for obtaining peaks with the highest peak height within the shortest time. Based on these observations, a microflow injection (μFI) method for the direct determination of cadmium and lead in Chinese rice wine by ICP-MS using an external aqueous calibration was developed. The sample throughput was 45 h- 1 with the detection limit of 19.8 and 10.4 ng L- 1 for Cd and Pb, respectively. The contents of Cd and Pb in 10 Chinese rice wine samples were measured. The results agreed well with those determined by ICP-MS with the conventional sampling system after microwave assisted digestion. The recoveries of three Chinese rice wine samples ranged between 95.5 and 102.8%. Furthermore, the determined contents of Cd and Pb in a certified reference material of red wine (GBW 10031) and a quality control test material of wine (FAPAS T07163QC) by the proposed method were in fairly good accordance with the certified/assigned values. All results verified the accuracy of our method.

A High-Performance Liquid Chromatography-Based Screening Method for the Analysis of Atrazine, Alachlor, and Ten of Their Transformation Products

USGS Publications Warehouse

Schroyer, B.R.; Capel, P.D.

1996-01-01

A high-performance liquid Chromatography (HPLC) method is presented for the for the fast, quantitative analysis of the target analytes in water and in low organic-carbon, sandy soils that are known to be contaminated with the parent herbicides. Speed and ease of sample preparation was prioritized above minimizing detection limits. Soil samples were extracted using 80:20 methanol:water (volume:volume). Water samples (50 ??L) were injected directly into the HPLC without prior preparation. Method quantification limits for soil samples (10 g dry weight) and water samples ranged from 20 to 110 ng/g and from 20 to 110 ??g/L for atrazine and its transformation products and from 80 to 320 ng/g and from 80 to 320 ??g/L for alachlor and its transformation products, respectively.

Percutaneous Direct Needle Puncture and Transcatheter N-butyl Cyanoacrylate Injection Techniques for the Embolization of Pseudoaneurysms and Aneurysms of Arteries Supplying the Hepato-pancreato-biliary System and Gastrointestinal Tract

PubMed Central

Yadav, Rajanikant R; Boruah, Deb K; Bhattacharyya, Vishwaroop; Prasad, Raghunandan; Kumar, Sheo; Saraswat, V A; Kapoor, V K; Saxena, Rajan

2016-01-01

Aims: The aim of this study was to evaluate the safety and clinical efficacy of percutaneous direct needle puncture and transcatheter N-butyl cyanoacrylate (NBCA) injection techniques for the embolization of pseudoaneurysms and aneurysms of arteries supplying the hepato-pancreato-biliary (HPB) system and gastrointestinal (GI) tract. Subjects and Methods: A hospital-based cross-sectional retrospective study was conducted, where the study group comprised 11 patients with pseudoaneurysms/aneurysms of arteries supplying the HPB system and GI tract presenting to a tertiary care center from January 2015 to June 2016. Four patients (36.4%) underwent percutaneous direct needle puncture of pseudoaneurysms with NBCA injection, 3 patients (27.3%) underwent transcatheter embolization with NBCA as sole embolic agent, and in 4 patients (36.4%), transcatheter NBCA injection was done along with coil embolization. Results: This retrospective study comprised 11 patients (8 males and 3 females) with mean age of 35.8 years ± 1.6 (standard deviation [SD]). The mean volume of NBCA: ethiodized oil (lipiodol) mixture injected by percutaneous direct needle puncture was 0.62 ml ± 0.25 (SD) (range = 0.5–1 ml), and by transcatheter injection, it was 0.62 ml ± 0.37 (SD) (range = 0.3–1.4 ml). Embolization with NBCA was technically and clinically successful in all patients (100%). No recurrence of bleeding or recurrence of pseudoaneurysm/aneurysm was noted in our study. Conclusions: Percutaneous direct needle puncture of visceral artery pseudoaneurysms and NBCA glue injection and transcatheter NBCA injection for embolization of visceral artery pseudoaneurysms and aneurysms are cost-effective techniques that can be used when coil embolization is not feasible or has failed. PMID:28123838

Concurrent Lactic and Volatile Fatty Acid Analysis of Microbial Fermentation Samples by Gas Chromatography with Heat Pre-treatment.

PubMed

Darwin; WipaCharles; Cord-Ruwisch, Ralf

2018-01-01

Organic acid analysis of fermentation samples can be readily achieved by gas chromatography (GC), which detects volatile organic acids. However, lactic acid, a key fermentation acid is non-volatile and can hence not be quantified by regular GC analysis. However the addition of periodic acid to organic acid samples has been shown to enable lactic acid analysis by GC, as periodic acid oxidizes lactic acid to the volatile acetaldehyde. Direct GC injection of lactic acid standards and periodic acid generated inconsistent and irreproducible peaks, possibly due to incomplete lactic acid oxidation to acetaldehyde. The described method is developed to improve lactic acid analysis by GC by using a heat treated derivatization pre-treatment, such that it becomes independent of the retention time and temperature selection of the GC injector. Samples containing lactic acid were amended by periodic acid and heated in a sealed test tube at 100°C for at least 45 min before injecting it to the GC. Reproducible and consistent peaks of acetaldehyde were obtained. Simultaneous determination of lactic acid, acetone, ethanol, butanol, volatile fatty acids could also be accomplished by applying this GC method, enabling precise and convenient organic acid analysis of biological samples such as anaerobic digestion and fermentation processes. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Accuracy of palpation-directed intra-articular glenohumeral injection confirmed by magnetic resonance arthrography.

PubMed

Powell, Scott E; Davis, Shane M; Lee, Emily H; Lee, Robert K; Sung, Ryan M; McGroder, Claire; Kouk, Shalen; Lee, Christopher S

2015-02-01

The aim of this study was to determine the accuracy of anatomic palpation-directed injections in the office setting. Two hundred twenty-six shoulders in 208 patients were studied using a 0.2-Tesla extremity scanner after the injection of gadolinium-diethylene triamine pentaacetic acid-saline. All patients were injected in a sterile fashion by a single board-certified shoulder surgeon using an anterior approach by palpating the rotator interval anterior to the acromioclavicular joint and angling the needle 45° lateral and 45° caudad. All injections, successful or otherwise, were single injections. Magnetic resonance (MR) arthrograms were retrospectively read by 2 musculoskeletal fellowship-trained, board certified radiologists to determine whether the injection was in the glenohumeral joint. Two hundred one of the 226 injections were successful (88.9%). Of the 25 unsuccessful injections, the contrast material extravasated out of the capsule in 5 cases and into the subscapularis tendon in 10 cases. The contrast material was injected into the subacromial space in 9 cases, into the rotator interval fat in 9 cases, and into extracapsular tissue in 6 cases. There was insufficient volume of contrast material in 10 cases. The accuracy rate was 88.9%. There were no complications. The palpation-directed rotator interval anterior approach technique for intra-articular glenohumeral MR arthrogram injections performed by a single surgeon was 88.9% accurate. Level IV, therapeutic case series. Copyright © 2015 Arthroscopy Association of North America. Published by Elsevier Inc. All rights reserved.

Monitoring population exposure to pesticides based on liquid chromatography-tandem mass spectrometry measurement of their urinary metabolites in urban wastewater: A novel biomonitoring approach.

PubMed

Rousis, Nikolaos I; Zuccato, Ettore; Castiglioni, Sara

2016-11-15

Biomonitoring studies have documented the high exposure of the population to pesticides which are widely used for crop protection, industrial and household purposes. This is the first study which has measured human urinary metabolites of pesticides in urban wastewater as biomarkers of population exposure. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed to measure fifteen urinary metabolites selected from the major classes of pesticides. Raw wastewater samples were processed by solid phase extraction (SPE) or direct injection into the LC-MS/MS system. Recoveries ranged from 75 to 115% and the limits of quantification were 1-15ng/L for the SPE method and 40-800ng/L for direct injection. The method was employed for the analysis of 44 composite 24-h wastewater samples collected in seven Italian cities. Most of the target substances were detected at concentrations ranging from 1.1ng/L to 1.6μg/L. The highest concentrations were for some common metabolites of alkyl phosphates and pyrethroids and the specific metabolite of chlorpyrifos and chlorpyrifos-methyl (3,5,6-trichloro-2-pyridinol). The frequency of detection and abundance of most of the measured metabolites were in line with the profiles reported in urine biomonitoring studies. This method is therefore proposed as a novel "biomonitoring approach" for obtaining objective, direct information on the levels of exposure of a specific population to pesticides, and current research is addressed to validate the method identifying the most reliable biomarkers. Copyright © 2016 Elsevier B.V. All rights reserved.

Modified HS-SPME for determination of quantitative relations between low-molecular oxygen compounds in various matrices.

PubMed

Dawidowicz, Andrzej L; Szewczyk, Joanna; Dybowski, Michal P

2016-09-07

Similar quantitative relations between individual constituents of the liquid sample established by its direct injection can be obtained applying Polydimethylsiloxane (PDMS) fiber in the headspace solid phase microextraction (HS-SPME) system containing the examined sample suspended in methyl silica oil. This paper proves that the analogous system composed of sample suspension/emulsion in polyethylene glycol (PEG) and Carbowax fiber allows to get similar quantitative relations between components of the mixture as those established by its direct analysis, but only for polar constituents. It is demonstrated for essential oil (EO) components of savory, sage, mint and thyme, and of artificial liquid mixture of polar constituents. The observed differences in quantitative relations between polar constituents estimated by both applied procedures are insignificant (Fexp < Fcrit). The presented results indicates that wider applicability of the system composed of a sample suspended in the oil of the same physicochemical character as that of used SPME fiber coating strongly depends on the character of interactions between analytes-suspending liquid and analytes-fiber coating. Copyright © 2016 Elsevier B.V. All rights reserved.

Direct analysis of six antibiotics in wastewater samples using rapid high-performance liquid chromatography coupled with diode array detector: a chemometric study towards green analytical chemistry.

PubMed

Vosough, Maryam; Rashvand, Masoumeh; Esfahani, Hadi M; Kargosha, Kazem; Salemi, Amir

2015-04-01

In this work, a rapid HPLC-DAD method has been developed for the analysis of six antibiotics (amoxicillin, metronidazole, sulfamethoxazole, ofloxacine, sulfadiazine and sulfamerazine) in the sewage treatment plant influent and effluent samples. Decreasing the chromatographic run time to less than 4 min as well as lowering the cost per analysis, were achieved through direct injection of the samples into the HPLC system followed by chemometric analysis. The problem of the complete separation of the analytes from each other and/or from the matrix ingredients was resolved as a posteriori. The performance of MCR/ALS and U-PLS/RBL, as second-order algorithms, was studied and comparable results were obtained from implication of these modeling methods. It was demonstrated that the proposed methods could be used promisingly as green analytical strategies for detection and quantification of the targeted pollutants in wastewater samples while avoiding the more complicated high cost instrumentations. Copyright © 2014 Elsevier B.V. All rights reserved.

Occupational hazards of traditional healers: repeated unprotected blood exposures risk infectious disease transmission.

PubMed

Audet, Carolyn M; Salato, José; Blevins, Meridith; Silva, Wilson; González-Calvo, Lázaro; Vermund, Sten H; Gaspar, Felisbela

2016-11-01

Healers provide support for acute and chronic illnesses in rural Mozambique, such as socially acceptable traditional 'vaccinations' (subcutaneous cuts in the skin to rub herbs directly into the bloody lesion). We aimed to document the frequency of blood exposure by traditional practitioners in Mozambique. We conducted surveys with a simple random sample of 236 traditional healers in Zambézia province. Chi-square and Wilcoxon rank-sum tests were used to compare 'injection' behaviours across districts. Healers treated a median of eight patients in the past month (IQR: 4-15). About 75% conducted 'injections'. These healers 'injected' a median of four patients (IQR: 1-8), used a new razor a median of three times (IQR: 1-8), and almost never used gloves. Lifetime blood exposures among those who provided 'injections' during treatments were estimated to be 1758 over a healer's career. The majority of healers are exposed repeatedly to patient blood. Given the high prevalence of HIV, hepatitis B and C virus, and other blood-borne agents, specific healer practices are an occupational hazard and reuse of razors is risky for their clients. © 2016 John Wiley & Sons Ltd.

Use of and access to oral and injectable contraceptives in Brazil

PubMed Central

Farias, Mareni Rocha; Leite, Silvana Nair; Tavares, Noemia Urruth Leão; Oliveira, Maria Auxiliadora; Arrais, Paulo Sergio Dourado; Bertoldi, Andréa Dâmaso; Pizzol, Tatiane da Silva Dal; Luiza, Vera Lucia; Ramos, Luiz Roberto; Mengue, Sotero Serrate

2016-01-01

ABSTRACT OBJECTIVE To analyze the prevalence of current use of oral and injectable contraceptives by Brazilian women, according to demographic and socioeconomic variables and issues related to access to those medicines. METHODS A cross-sectional, population-based analytical study with probability sampling based on data from the Pesquisa Nacional sobre Acesso, Utilização e Promoção do Uso Racional de Medicamentos (PNAUM – National Survey on Access, Use and Promotion of Rational Use of Medicines), carried out between September 2013 and February 2014 in 20,404 Brazilian urban households. Prevalence was calculated based on reports from non-pregnant women aged 15-49 on the use of oral or injectable contraceptives. The independent variables were gender, age, level of education, socioeconomic class, Brazilian region and marital status. Also analyzed were access, means of payment, sources, and reported medicines. Statistical analyses considered 95% confidence intervals (95%CI) and Pearson Chi-square test to evaluate the statistical significance of differences between groups, considering a 5% significance level. RESULTS Prevalence of use was 28.2% for oral contraceptives (OC) and 4.5% for injectable contraceptives (IC). The highest prevalence of oral contraceptives was in the South region (37.5%) and the lowest in the North region (15.7%). For injectable contraceptives there was no difference between regions. Access was higher for oral contraceptive users (90.7%) than injectable contraceptives users (81.2%), as was direct payment (OC 78.1%, IC 58.0%). Users who paid for contraceptives acquired them at retail pharmacies (OC 95.0% and IC 86.6%) and at Farmácia Popular (Popular Pharmacy Program) (OC 4.8% and IC 12.7%). Free of charge contraceptives were mostly obtained from the Brazilian Unified Health System – SUS (OC 86.7%; IC 96.0%). Free samples were reported by 10.4% of users who did not pay for oral contraceptives. Most of paying users did not try to obtain contraceptives from SUS. Monophasic combined oral contraceptives were the most frequently reported (71.6%) and low-level levonorgestrel + ethinylestradiol combination accounted for 38.7% of them. The most frequently reported medicines are included in the Relação Nacional de Medicamentos Essenciais (RENAME – National List of Essential Medicines. CONCLUSIONS Most women aged 15 to 49 who reported using contraceptives had access to the medicine and use monophasic combined oral contraceptives of appropriate efficiency and safety purchased by direct payment, mainly from retail pharmacies. PMID:27982384

Direct laboratory observation of fluid distribution and its influence on acoustic properties of patchy saturated rocks

NASA Astrophysics Data System (ADS)

Lebedev, M.; Clennell, B.; Pervukhina, M.; Shulakova, V.; Mueller, T.; Gurevich, B.

2009-04-01

Porous rocks in hydrocarbon reservoirs are often saturated with a mixture of two or more fluids. Interpretation of exploration seismograms requires understanding of the relationship between distribution of the fluids patches and acoustic properties of rocks. The sizes of patches as well as their distribution affect significantly the seismic response. If the size of the fluid patch is smaller than the diffusion wavelength then pressure equilibration is achieved and the bulk modulus of the rock saturated with a mixture is defined by the Gassmann equations (Gassmann, 1951) with the saturation-weighted average of the fluid bulk modulus given by Wood's law (Wood, 1955, Mavko et al., 1998). If the fluid patch size is much larger than the diffusion wavelength then there is no pressure communication between different patches. In this case, fluid-flow effects can be neglected and the overall rock may be considered equivalent to an elastic composite material consisting of homogeneous parts whose properties are given by Gassmann theory with Hill's equation for the bulk modulus (Hill, 1963, Mavko et al., 1998). At intermediate values of fluid saturation the velocity-saturation relationship is significantly affected by the fluid patch distribution. In order to get an improved understanding of factors influencing the patch distribution and the resulting seismic wave response we performed simultaneous measurements of P-wave velocities and rock sample CT imaging. The CT imaging allows us to map the fluid distribution inside rock sample during saturation (water imbibition). We compare the experimental results with theoretical predictions. In this paper we will present results of simultaneous measurements of longitudinal wave velocities and imaging mapping of fluid distribution inside rock sample during sample saturation. We will report results of two kinds of experiments: "dynamic" and "quasi static" saturation. In both experiments Casino Cores Otway Basin sandstone, Australia core samples (38 mm in diameter, approximately 60 mm long) were dried in oven under reduced pressure. In dynamic saturation experiments, samples were jacketed in the experimental cell, made from transparent for X-radiation material (PMMA). Distillate water was injected into the sample from the one side. Fluid distribution in such "dynamic" experiment: both spatial and time dependant was measured using X-ray Computer Tomograph (CT) with resolution 0.2 x 0.2 x 1 mm3. Velocities (Vp, and Vs) at ultrasonic frequency of 1 MHz, were measured in the direction perpendicular to initial direction of the fluid flow injection. Sample saturation was estimated from the CT results. In "quasi static" experiments samples were saturated during long period of time (over 2 weeks) to achieve uniform distribution of liquid inside the sample. Saturation was determined by measurement of the weight of water fraction. All experiments were performed at laboratory environments at temperature 25 C. Ultrasonic velocities and fluid saturations were measured simultaneously during water injection into sandstone core samples. The experimental results obtained on low-permeability samples show that at low saturation values the velocity-saturation dependence can be described by the Gassmann-Wood relationship. However, with increasing saturation a sharp increase of P-wave velocity is observed, eventually approaching the Gassmann-Hill relationship. We connect the characteristics of the transition behavior of the velocity-saturation relationships to the increasing size of the patches inside the rock sample. In particular, we show that for relatively large fluid injection rate this transition occurs at smaller degrees of saturation as compared with high injection rate. We model the experimental data using the so-called White model (Toms 2007) that assumes fluid patch distribution as a periodic assemblage of concentric spheres. We can observe reasonable agreement between experimental results and theoretical predictions of White's model. The results illustrate the non-unique relationships between saturation and velocity in sandstones dependent on texture and fluid displacement history: fuller understanding of these phenomena is needed for accurate assessment of time lapse seismic measurements, be they for oil and gas recovery or for CO2 disposal purposes. Gassmann, F., 1951, Elastic waves through a packing of spheres. Geophysics 16, 673-685; Mavko, G., T. Mukerji, and J. Dvorkin, 1998, The Rock Physics Handbook: Tools for seismic analysis in porous media: Cambridge University Press. Wood, A. W., 1955, A Textbook of Sound, The MacMillan Co., New York, 360 pp. Hill, R., 1963, Elastic properties of reinforced solids: some theoretical principles. J. Mech. Phys. Solids, 11, 357-372. Hill, R., 1952, The elastic behavior of crystalline aggregates. Proc. Physical Soc., London, A65, 349-354. J. Toms, T.M. Mueller, B. Gurevich, 2007 Seismic attenuation in porous rocks with random patchy saturation. Geophysical Prospecting, 55, 671-678.

Design and development of an automated flow injection instrument for the determination of arsenic species in natural waters.

PubMed

Hanrahan, Grady; Fan, Tina K; Kantor, Melanie; Clark, Keith; Cardenas, Steven; Guillaume, Darrell W; Khachikian, Crist S

2009-10-01

The design and development of an automated flow injection instrument for the determination of arsenite [As(III)] and arsenate [As(V)] in natural waters is described. The instrument incorporates solenoid activated self-priming micropumps and electronic switching valves for controlling the fluidics of the system and a miniature charge-coupled device spectrometer operating in a graphical programming environment. The limits of detection were found to be 0.79 and 0.98 microM for As(III) and As(V), respectively, with linear range of 1-50 microM. Spiked ultrapure water samples were analyzed and recoveries were found to be 97%-101% for As(III) and 95%-99% for As(V), respectively. Future directions in terms of automation, optimization, and field deployment are discussed.

Pharmacokinetic-pharmacodynamic study of subcutaneous injection of depot nandrolone decanoate using dried blood spots sampling coupled with ultrapressure liquid chromatography tandem mass spectrometry assays.

PubMed

Singh, Gurmeet K S; Turner, Leo; Desai, Reena; Jimenez, Mark; Handelsman, David J

2014-07-01

Testosterone (T) and nandrolone (N) esters require deep im injections by medical personnel but these often deposit injectate into sc fat so that more convenient sc self-administration may be feasible. To investigate the feasibility and pharmacology of sc injection of N decanoate in healthy men using dried blood spot (DBS) for frequent blood sampling without clinic visits. Healthy male volunteers received 100 mg N decanoate by a single sc injection. Finger-prick capillary blood was spotted onto filter paper before injection daily at home for 21 d and stored at room temperature. Venous whole blood was also spotted onto filter paper before and weekly for 3 wk after injection. DBS were extracted for assay of N and T by liquid chromatography tandem mass spectrometry in a single batch with serum concentrations estimated with adjustment for capillary blood sample volume and hematocrit to define peak (N) or nadir (T) time and concentration from individual daily measurements. Daily serum N peaked 2.50 ± 0.25 (SEM) ng/mL at a median (range) of 6 (4-13) days causing a reduction in serum T from 3.50 ± 0.57 ng/mL at baseline to a nadir of 0.38 ± 0.13 (SEM) ng/mL (89 ± 3% suppression) at a median (range) of 8 (5-16) days. Simultaneously sampled capillary, venous whole blood, and serum gave almost identical results for serum T and N. Finger-pricks and sc injections were well tolerated. This study demonstrates that A) DBS sampling with liquid chromatography mass spectrometry steroid analysis achieves frequent time sampling in the community without requiring clinic visits, venesection, or frozen serum storage, and B) androgen esters in an oil vehicle can be delivered effectively by sc injection, thus avoiding the need for medically supervised deep-im injections.

Results of ground-water tracer tests using tritiated water at Oak Ridge National Laboratory, Tennessee

USGS Publications Warehouse

Webster, D.A.

1996-01-01

Ground-water tracer test were conducted at two sites in the radioactive-waste disposal area of Oak Ridge National Laboratory from 1977 to 1982. The purpose of the tests was to determine if the regolith beds had weathered sufficiently to permit the substantial flow of water across them. About 50 curies of tritium dissolved in water were used as the tracer in one site, and about 100 curies at the other. Results demonstrated that ground water is able to flow through joints in the weathered bedding and that the direction of the water-table gradient is the primary factor governint flow direction. Nevertheless, the substantial lateral spread of the plume as it developed showed that bedding-plane openings can still exert a significant secondary influence on flow direction in weathered rock. About 3,500 water samples from the injection and observation wells were analyzed for tritium during the test period. Concentrations detected spanned 11 orders of magnitude. Measurable concentrations were still present in the two injection wells and most observation wells 5 years after the tracer was introduced. Matrix diffusion may have played a significant role in these tests. The process would account for the sustained concentrations of tritium at many of the observation wells, the long-term residual concentrations at the injection and observation wells, and the apparent slow movement of the centers of mass across the two well fields. The process also would have implications regarding aquifer remediation. Other tracer tests have been conducted in the regolith of the Conasauga Group. Results differ from the results described in this report.

Thermally Stratified Compression Ignition: A new advanced low temperature combustion mode with load flexibility

DOE PAGES

Lawler, Benjamin; Splitter, Derek; Szybist, James; ...

2017-03-01

We introduce a new advanced combustion mode, called Thermally Stratified Compression Ignition (TSCI), which uses direct water injection to control both the average temperature and the temperature distribution prior to ignition, thereby providing cycle-to-cycle control over the start and rate of heat release in Low Temperature Combustion (LTC). Experiments were conducted to fundamentally understand the effects of water injection on heat release in LTC. Our results show that water injection retards the start of combustion due to the latent heat of vaporization of the injected water. Furthermore, for start of water injection timings between 20 and 70 degrees before topmore » dead center, combustion is significantly elongated compared to without water injection. The 10–90% burn duration with 6.6 and 9.0 mg of water per cycle was 77% and 146% longer than without water injection, respectively. Forced thermal stratification result from a direct water injection which reduces the heat release rate by local evaporative cooling. Finally, the load limits with and without water injection were determined experimentally. Without water injection, the load range was 2.3–3.6 bar gross IMEP. By using water injection to control heat release, the load range in TSCI was 2.3–8.4 bar gross IMEP, which is a range expansion of over 350%. These results demonstrate that direct water injection can provide significant improvements to both controllability and the range of operability of LTC, thereby resolving the major challenges associated with HCCI.« less

Thermally Stratified Compression Ignition: A new advanced low temperature combustion mode with load flexibility

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

Lawler, Benjamin; Splitter, Derek; Szybist, James

We introduce a new advanced combustion mode, called Thermally Stratified Compression Ignition (TSCI), which uses direct water injection to control both the average temperature and the temperature distribution prior to ignition, thereby providing cycle-to-cycle control over the start and rate of heat release in Low Temperature Combustion (LTC). Experiments were conducted to fundamentally understand the effects of water injection on heat release in LTC. Our results show that water injection retards the start of combustion due to the latent heat of vaporization of the injected water. Furthermore, for start of water injection timings between 20 and 70 degrees before topmore » dead center, combustion is significantly elongated compared to without water injection. The 10–90% burn duration with 6.6 and 9.0 mg of water per cycle was 77% and 146% longer than without water injection, respectively. Forced thermal stratification result from a direct water injection which reduces the heat release rate by local evaporative cooling. Finally, the load limits with and without water injection were determined experimentally. Without water injection, the load range was 2.3–3.6 bar gross IMEP. By using water injection to control heat release, the load range in TSCI was 2.3–8.4 bar gross IMEP, which is a range expansion of over 350%. These results demonstrate that direct water injection can provide significant improvements to both controllability and the range of operability of LTC, thereby resolving the major challenges associated with HCCI.« less

Determination of residual solvents in bulk pharmaceuticals by thermal desorption/gas chromatography/mass spectrometry.

PubMed

Urakami, K; Saito, Y; Fujiwara, Y; Watanabe, C; Umemoto, K; Godo, M; Hashimoto, K

2000-12-01

Thermal desorption (TD) techniques followed by capillary GC/MS were applied for the analysis of residual solvents in bulk pharmaceuticals. Solvents desorbed from samples by heating were cryofocused at the head of a capillary column prior to GC/MS analysis. This method requires a very small amount of sample and no sample pretreatment. Desorption temperature was set at the point about 20 degrees C higher than the melting point of each sample individually. The relative standard deviations of this method tested by performing six consecutive analyses of 8 different samples were 1.1 to 3.1%, and analytical results of residual solvents were in agreement with those obtained by direct injection of N,N-dimethylformamide solution of the samples into the GC. This novel TD/GC/MS method was demonstrated to be very useful for the identification and quantification of residual solvents in bulk pharmaceuticals.

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

DTIC Science & Technology

2012-04-01

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

Immunological techniques as tools to characterize the subsurface microbial community at a trichloroethylene contaminated site

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

Fliermans, C.B.; Dougherty, J.M.; Franck, M.M.

Effective in situ bioremediation strategies require an understanding of the effects pollutants and remediation techniques have on subsurface microbial communities. Therefore, detailed characterization of a site`s microbial communities is important. Subsurface sediment borings and water samples were collected from a trichloroethylene (TCE) contaminated site, before and after horizontal well in situ air stripping and bioventing, as well as during methane injection for stimulation of methane-utilizing microorganisms. Subsamples were processed for heterotrophic plate counts, acridine orange direct counts (AODC), community diversity, direct fluorescent antibodies (DFA) enumeration for several nitrogen-transforming bacteria, and Biolog {reg_sign} evaluation of enzyme activity in collected water samples.more » Plate counts were higher in near-surface depths than in the vadose zone sediment samples. During the in situ air stripping and bioventing, counts increased at or near the saturated zone, remained elevated throughout the aquifer, but did not change significantly after the air stripping. Sporadic increases in plate counts at different depths as well as increased diversity appeared to be linked to differing lithologies. AODCs were orders of magnitude higher than plate counts and remained relatively constant with depth except for slight increases near the surface depths and the capillary fringe. Nitrogen-transforming bacteria, as measured by serospecific DFA, were greatly affected both by the in situ air stripping and the methane injection. Biolog{reg_sign} activity appeared to increase with subsurface stimulation both by air and methane. The complexity of subsurface systems makes the use of selective monitoring tools imperative.« less

Direct sample introduction gas chromatography and mass spectrometry for the determination of phthalate esters in cleaning products.

PubMed

Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

2015-02-06

A method using direct sample introduction (DSI) coupled to gas chromatography-mass spectrometry (GC-MS) is developed for the determination of six phthalate esters (dimethyl, diethyl, dibutyl, butylbenzyl, diethylhexyl and dioctyl phthalate) in cleaning products. The different variables involved in the DSI step, including venting time and temperature, vaporisation time and temperature, injector heating temperature and gas flow rate and pressure, were evaluated and optimised using Taguchi orthogonal arrays. The proposed method, using calibration against methanolic standards, showed good linearity in the 0.05-15 μg g(-1) range and good repeatability, with RSD values ranging from 3.5% to 5.7%. Quantification limits between 0.010 and 0.041 μg g(-1), depending on the compound, were attained, while recovery assays provided values from 83% to 115%. Twenty-seven cleaning products were analysed using the DSI-GC-MS method, being four phthalates (dimethyl, diethyl, dibutyl and diethylhexyl phthalate) found in fourteen of them at concentration levels in the 0.1-21 μg g(-1) range. Compared with the most common GC injection technique, which uses the split/splitless injector, the proposed DSI procedure provided larger peak areas and lower detection limits, as result of the greater injected volume and reduction in noise. Copyright © 2014 Elsevier B.V. All rights reserved.

Pre-injection brine production for managing pressure in compartmentalized CO₂ storage reservoirs

DOE PAGES

Buscheck, Thomas A.; White, Joshua A.; Chen, Mingjie; ...

2014-12-31

We present a reservoir management approach for geologic CO₂ storage that combines CO₂ injection with brine extraction. In our approach, dual-mode wells are initially used to extract formation brine and subsequently used to inject CO₂. These wells can also be used to monitor the subsurface during pre-injection brine extraction so that key data is acquired and analyzed prior to CO₂ injection. The relationship between pressure drawdown during pre-injection brine extraction and pressure buildup during CO₂ injection directly informs reservoir managers about CO₂ storage capacity. These data facilitate proactive reservoir management, and thus reduce costs and risks. The brine may bemore » used directly as make-up brine for nearby reservoir operations; it can also be desalinated and/or treated for a variety of beneficial uses.« less

Quality investigation of hydroxyprogesterone caproate active pharmaceutical ingredient and injection

PubMed Central

Chollet, John L.; Jozwiakowski, Michael J.

2012-01-01

The purpose of this study was to investigate the quality of hydroxyprogesterone caproate (HPC) active pharmaceutical ingredient (API) sources that may be used by compounding pharmacies, compared to the FDA-approved source of the API; and to investigate the quality of HPC injection samples obtained from compounding pharmacies in the US, compared to the FDA-approved product (Makena®). Samples of API were obtained from every source confirmed to be an original manufacturer of the drug for human use, which were all companies in China that were not registered with FDA. Eight of the ten API samples (80%) did not meet the impurity specifications required by FDA for the API used in the approved product. One API sample was found to not be HPC at all; additional laboratory testing showed that it was glucose. Thirty samples of HPC injection obtained from com pounding pharmacies throughout the US were also tested, and eight of these samples (27%) failed to meet the potency requirement listed in the USP monograph for HPC injection and/or the HPLC assay. Sixteen of the thirty injection samples (53%) exceeded the impurity limit setforthe FDA-approved drug product. These results confirm the inconsistency of compounded HPC Injections and suggest that the risk-benefit ratio of using an unapproved compounded preparation, when an FDA-approved drug product is available, is not favorable. PMID:22329865

Real-time ultrasound image classification for spine anesthesia using local directional Hadamard features.

PubMed

Pesteie, Mehran; Abolmaesumi, Purang; Ashab, Hussam Al-Deen; Lessoway, Victoria A; Massey, Simon; Gunka, Vit; Rohling, Robert N

2015-06-01

Injection therapy is a commonly used solution for back pain management. This procedure typically involves percutaneous insertion of a needle between or around the vertebrae, to deliver anesthetics near nerve bundles. Most frequently, spinal injections are performed either blindly using palpation or under the guidance of fluoroscopy or computed tomography. Recently, due to the drawbacks of the ionizing radiation of such imaging modalities, there has been a growing interest in using ultrasound imaging as an alternative. However, the complex spinal anatomy with different wave-like structures, affected by speckle noise, makes the accurate identification of the appropriate injection plane difficult. The aim of this study was to propose an automated system that can identify the optimal plane for epidural steroid injections and facet joint injections. A multi-scale and multi-directional feature extraction system to provide automated identification of the appropriate plane is proposed. Local Hadamard coefficients are obtained using the sequency-ordered Hadamard transform at multiple scales. Directional features are extracted from local coefficients which correspond to different regions in the ultrasound images. An artificial neural network is trained based on the local directional Hadamard features for classification. The proposed method yields distinctive features for classification which successfully classified 1032 images out of 1090 for epidural steroid injection and 990 images out of 1052 for facet joint injection. In order to validate the proposed method, a leave-one-out cross-validation was performed. The average classification accuracy for leave-one-out validation was 94 % for epidural and 90 % for facet joint targets. Also, the feature extraction time for the proposed method was 20 ms for a native 2D ultrasound image. A real-time machine learning system based on the local directional Hadamard features extracted by the sequency-ordered Hadamard transform for detecting the laminae and facet joints in ultrasound images has been proposed. The system has the potential to assist the anesthesiologists in quickly finding the target plane for epidural steroid injections and facet joint injections.

Supercritical fluid extraction and direct fluid injection mass spectrometry for the determination of trichothecene mycotoxins in wheat samples

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

Kalinoski, H.T.; Udseth, H.R.; Wright, B.W.

1986-10-01

The application of on-line supercritical fluid extraction with chemical ionization mass spectrometry and collision induced dissociation tandem mass spectrometry for the rapid identification of parts-per-million levels of several trichothecene mycotoxins is demonstrated. Supercritical carbon dioxide is shown to allow identification of mycotoxins with minimum sample handling in complex natural matrices (e.g., wheat). Tandem mass spectrometry techniques are employed for unambiguous identification of compounds of varying polarity, and false positives from isobaric compounds are avoided. Capillary column supercritical fluid chromatography-mass spectrometry of a supercritical fluid extract of the same sample was also performed and detection limits in the parts-per-billion range appearmore » feasible.« less

Method and apparatus for concentrating vapors for analysis

DOEpatents

Grate, Jay W [West Richland, WA; Baldwin, David L [Kennewick, WA; Anheier, Jr., Norman C.

2012-06-05

A pre-concentration device and a method are disclosed for concentrating gaseous vapors for analysis. Vapors sorbed and concentrated within the bed of the pre-concentration device are thermally desorbed, achieving at least partial separation of the vapor mixtures. The pre-concentration device is suitable, e.g., for pre-concentration and sample injection, and provides greater resolution of peaks for vapors within vapor mixtures, yielding detection levels that are 10-10,000 times better than direct sampling and analysis systems. Features are particularly useful for continuous unattended monitoring applications. The invention finds application in conjunction with, e.g., analytical instruments where low detection limits for gaseous vapors are desirable.

Pressurized feed-injection spray-forming apparatus

DOEpatents

Berry, R.A.; Fincke, J.R.; McHugh, K.M.

1995-08-29

A spray apparatus and method are disclosed for injecting a heated, pressurized liquid in a first predetermined direction into a pressurized gas flow that is flowing in a second predetermined direction, to provide for atomizing and admixing the liquid with the gas to form a two-phase mixture. A valve is also disposed within the injected liquid conduit to provide for a pulsed injection of the liquid and timed deposit of the atomized gas phase. Preferred embodiments include multiple liquid feed ports and reservoirs to provide for multiphase mixtures of metals, ceramics, and polymers. 22 figs.

Pressurized feed-injection spray-forming apparatus

DOEpatents

Berry, Ray A.; Fincke, James R.; McHugh, Kevin M.

1995-01-01

A spray apparatus and method for injecting a heated, pressurized liquid in a first predetermined direction into a pressurized gas flow that is flowing in a second predetermined direction, to provide for atomizing and admixing the liquid with the gas to form a two-phase mixture. A valve is also disposed within the injected liquid conduit to provide for a pulsed injection of the liquid and timed deposit of the atomized gas phase. Preferred embodiments include multiple liquid feed ports and reservoirs to provide for multiphase mixtures of metals, ceramics, and polymers.

BEVACIZUMAB LEVELS IN BREAST MILK AFTER LONG-TERM INTRAVITREAL INJECTIONS.

PubMed

McFarland, Trevor J; Rhoads, Andrew D; Hartzell, Matthew; Emerson, Geoffrey G; Bhavsar, Abdhish R; Stout, J Timothy

2015-08-01

The purpose of this study is to determine whether bevacizumab is detectable in the breast milk of nursing mothers. Breast milk samples were collected from 2 patients receiving monthly intravitreal bevacizumab injections for choroidal neovascularization over the course of 16 months. Enzyme-linked immunosorbent assay and Western blot analysis was used to determine the levels of bevacizumab in the milk samples. An enzyme-linked immunosorbent assay was developed using antibodies specific to bevacizumab in which the sensitivity threshold was 3 ng/mL. All breast milk samples assayed from the two patients actively undergoing treatment did not have detectable levels of bevacizumab. Samples collected 1.5 hours and 7 hours after an injection and 2 randomly chosen samples were negative by Western blot analysis. A sensitive assay to detect bevacizumab in breast milk samples assayed suggests that intravitreal injections do not result in detectable bevacizumab in breast milk.

Electrokinetic sample preconcentration and hydrodynamic sample injection for microchip electrophoresis using a pneumatic microvalve.

PubMed

Cong, Yongzheng; Katipamula, Shanta; Geng, Tao; Prost, Spencer A; Tang, Keqi; Kelly, Ryan T

2016-02-01

A microfluidic platform was developed to perform online electrokinetic sample preconcentration and rapid hydrodynamic sample injection for zone electrophoresis using a single microvalve. The polydimethylsiloxane microchip comprises a separation channel, a side channel for sample introduction, and a control channel which is used as a pneumatic microvalve aligned at the intersection of the two flow channels. The closed microvalve, created by multilayer soft lithography, serves as a nanochannel preconcentrator under an applied electric potential, enabling current to pass through while preventing bulk flow. Once analytes are concentrated, the valve is briefly opened and the stacked sample is pressure injected into the separation channel for electrophoretic separation. Fluorescently labeled peptides were enriched by a factor of ∼450 in 230 s. This method enables both rapid analyte concentration and controlled injection volume for high sensitivity, high-resolution CE. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A study for characterization of IgE-mediated cutaneous immediate and late-phase reactions in non-allergic domestic cats.

PubMed

Seals, Shanna L; Kearney, Michael; Del Piero, Fabio; Hammerberg, Bruce; Pucheu-Haston, Cherie M

2014-05-15

Immunoglobulin-E (IgE) mediated reactions can be induced by intradermal injection of anti-IgE antibodies in both humans and dogs. These reactions grossly and histologically mimic changes seen in naturally occurring allergic dermatitis in these species. Similar studies have not been conducted in the cat. Purified polyclonal rabbit-origin IgG specific for canine IgE (anti-IgE) and rabbit immunoglobulin G (IgG) were injected intradermally in 7 non-allergic laboratory colony cats. Wheal measurements were obtained and biopsies collected before injection and at injection sites after 20 min, 6, 24, and 48 h. Injection of anti-IgE induced an immediate wheal response which was significantly larger than that seen after injection of rabbit IgG. Anti-IgE injected skin was also significantly thicker than IgG-injected skin. This corresponded with a significant increase in number of visibly degranulated mast cells in anti-IgE samples when compared to IgG samples. Injection of anti-IgE was associated with the rapid recruitment of inflammatory cells to the injected dermis. The number of inflammatory cells and mononuclear cells were significantly elevated after the injection of anti-IgE when compared to IgG-injected skin. Both eosinophils and neutrophils were significantly increased in anti-IgE samples relative to IgG, although neutrophils were only transiently increased. The high eosinophil and relatively low neutrophil cell counts in these samples were consistent with previously documented histologic features of naturally occurring feline allergic skin disease. Immunohistochemistry identified a significantly overall increased CD1a(+) cells after the intradermal injection of anti-IgE when compared to IgG and non-injected skin. CD3(+), CD8(+) and CD4(+) were also significantly increased overall in anti-IgE injected skin relative to IgG injected skin. These data document the gross and cellular response to injection of anti-IgE in the skin of healthy, non-allergic cats and support a possible role for IgE in the development of feline allergic dermatitis. Copyright © 2014 Elsevier B.V. All rights reserved.

Comparison of long-term voice outcomes after vocal fold augmentation using autologous fat injection by direct microlaryngoscopy versus office-based calcium hydroxylapatite injection.

PubMed

Zeleník, Karol; Walderová, Radana; Kučová, Hana; Jančatová, Debora; Komínek, Pavel

2017-08-01

The objective is to compare the long-term voice outcomes of vocal fold augmentation (VFA) using autologous fat injection via direct microlaryngoscopy versus office-based calcium hydroxylapatite (CaHA) injection. Patients with glottal insufficiency and a gap no greater than 3 mm caused by unilateral vocal fold paralysis or vocal fold atrophy were prospectively recruited to the study from September 2012 to September 2015. From September 2012 to May 2014, VFA was only performed using autologous fat via direct microlaryngoscopy under general anesthesia (N = 14). From May 2014 to September 2015, VFA was performed as an office-based procedure using a transoral approach to inject CaHA (N = 17). Videolaryngostroboscopic evaluation, subjective satisfaction with voice, voice handicap index (VHI), and maximal phonation time (MPT) were analyzed pre-injection and 12 months after VFA. A total of 31 patients were analyzed. One year after VFA, 67.8% of the patients were satisfied with their voice, with no significant difference between groups (P = 0.247). The mean improvement in VHI in the autologous fat group was 31.6 ± 16.82 versus 35 ± 27.24 in the CaHA group (P = 0.664). MPT improvement was also similar in the two groups: 5.5 ± 2.52 for the autologous fat group versus 6.0 ± 3.98 for the CaHA group (P = 0.823). Both autologous fat injection via direct microlaryngoscopy and office-based CaHA injection have good long-term results. There were no differences in the treatment results of the two procedures 1 year after injection.

Automated in-line gel filtration for native state mass spectrometry.

PubMed

Waitt, Greg M; Xu, Robert; Wisely, G Bruce; Williams, Jon D

2008-02-01

Characterization of protein-ligand complexes by nondenaturing mass spectrometry provides direct evidence of drug-like molecules binding with potential therapeutic targets. Typically, protein-ligand complexes to be analyzed contain buffer salts, detergents, and other additives to enhance protein solubility, all of which make the sample unable to be analyzed directly by electrospray ionization mass spectrometry. This work describes an in-line gel-filtration method that has been automated and optimized. Automation was achieved using commercial HPLC equipment. Gel column parameters that were optimized include: column dimensions, flow rate, packing material type, particle size, and molecular weight cut-off. Under optimal conditions, desalted protein ions are detected 4 min after injection and the analysis is completed in 20 min. The gel column retains good performance even after >200 injections. A demonstration for using the in-line gel-filtration system is shown for monitoring the exchange of fatty acids from the pocket of a nuclear hormone receptor, peroxisome proliferator activator-delta (PPARdelta) with a tool compound. Additional utilities of in-line gel-filtration mass spectrometry system will also be discussed.

Micromechanical modeling of short glass-fiber reinforced thermoplastics-Isotropic damage of pseudograins

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

Kammoun, S.; Brassart, L.; Doghri, I.

A micromechanical damage modeling approach is presented to predict the overall elasto-plastic behavior and damage evolution in short fiber reinforced composite materials. The practical use of the approach is for injection molded thermoplastic parts reinforced with short glass fibers. The modeling is proceeded as follows. The representative volume element is decomposed into a set of pseudograins, the damage of which affects progressively the overall stiffness and strength up to total failure. Each pseudograin is a two-phase composite with aligned inclusions having same aspect ratio. A two-step mean-field homogenization procedure is adopted. In the first step, the pseudograins are homogenized individuallymore » according to the Mori-Tanaka scheme. The second step consists in a self-consistent homogenization of homogenized pseudograins. An isotropic damage model is applied at the pseudograin level. The model is implemented as a UMAT in the finite element code ABAQUS. Model is shown to reproduce the strength and the anisotropy (Lankford coefficient) during uniaxial tensile tests on samples cut under different directions relative to the injection flow direction.« less

Direct-injection HPLC method of measuring micafungin in human plasma using a novel hydrophobic/hydrophilic hybrid ODS column.

PubMed

Uranishi, Hiroaki; Nakamura, Mitsuhiro; Nakamura, Hiroki; Ikeda, Yukari; Otsuka, Mayuko; Kato, Zenichiro; Tsuchiya, Teruo

2011-04-15

A direct-injection HPLC-based method has been developed for determining amounts of micafungin in human plasma using a novel hydrophobic/hydrophilic hybrid ODS column. The method is easy to perform and requires only 10 μL of a filtered plasma sample. The chromatographic separations were carried out with a gradient mode. The fluorescence detection wavelengths of excitation and emission were set at 273 nm and 464 nm, respectively. Retention times for micafungin and IS were 22.4 and 23.7 min, respectively. Micafungin and FR195743 (IS) peaks were completely separated with little tailing, and no interference was observed. The calibration curve of micafungin showed good linearity in the range of 0.5-20.0 μg/mL (r(2)=1.00). The intra-day accuracy ranged from -4.5 to 5.3%. The inter-day accuracy ranged from -9.8 to 1.5%. The precisions were less than 10%. This method is useful for the determination of micafungin in human plasma. Copyright © 2011 Elsevier B.V. All rights reserved.

Micromechanical modeling of short glass-fiber reinforced thermoplastics-Isotropic damage of pseudograins

NASA Astrophysics Data System (ADS)

Kammoun, S.; Brassart, L.; Robert, G.; Doghri, I.; Delannay, L.

2011-05-01

A micromechanical damage modeling approach is presented to predict the overall elasto-plastic behavior and damage evolution in short fiber reinforced composite materials. The practical use of the approach is for injection molded thermoplastic parts reinforced with short glass fibers. The modeling is proceeded as follows. The representative volume element is decomposed into a set of pseudograins, the damage of which affects progressively the overall stiffness and strength up to total failure. Each pseudograin is a two-phase composite with aligned inclusions having same aspect ratio. A two-step mean-field homogenization procedure is adopted. In the first step, the pseudograins are homogenized individually according to the Mori-Tanaka scheme. The second step consists in a self-consistent homogenization of homogenized pseudograins. An isotropic damage model is applied at the pseudograin level. The model is implemented as a UMAT in the finite element code ABAQUS. Model is shown to reproduce the strength and the anisotropy (Lankford coefficient) during uniaxial tensile tests on samples cut under different directions relative to the injection flow direction.

Ultrafast gas chromatography method with direct injection for the quantitative determination of benzene, toluene, ethylbenzene, and xylenes in commercial gasoline.

PubMed

Miranda, Nahieh Toscano; Sequinel, Rodrigo; Hatanaka, Rafael Rodrigues; de Oliveira, José Eduardo; Flumignan, Danilo Luiz

2017-04-01

Benzene, toluene, ethylbenzene, and xylenes are some of the most hazardous constituents found in commercial gasoline samples; therefore, these components must be monitored to avoid toxicological problems. We propose a new routine method of ultrafast gas chromatography coupled to flame ionization detection for the direct determination of benzene, toluene, ethylbenzene, and xylenes in commercial gasoline. This method is based on external standard calibration to quantify each compound, including the validation step of the study of linearity, detection and quantification limits, precision, and accuracy. The time of analysis was less than 3.2 min, with quantitative statements regarding the separation and quantification of all compounds in commercial gasoline samples. Ultrafast gas chromatography is a promising alternative method to official analytical techniques. Government laboratories could consider using this method for quality control. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Data on subsurface storage of liquid waste near Pensacola, Florida, 1963-1980

USGS Publications Warehouse

Hull, R.W.; Martin, J.B.

1982-01-01

Since 1963, when industrial waste was first injected into the subsurface in northwest Florida, considerable data have been collected relating to the geochemistry of subsurface waste storage. This report presents hydrogeologic data on two subsurface waste storage. This report presents hydrogeologic data on two subsurface storage systems near Pensacola, Fla., which inject liquid industrial waste through deep wells into a saline aquifer. Injection sites are described giving a history of well construction, injection, and testing; geologic data from cores and grab samples; hydrographs of injection rates, volume, pressure, and water levels; and chemical and physical data from water-quality samples collected from injection and monitor wells. (USGS)

Stability of penicillin G sodium diluted with 0.9% sodium chloride injection or 5% dextrose injection and stored in polyvinyl chloride bag containers and elastomeric pump containers.

PubMed

Hossain, Mirza Akram; Friciu, Mihaela; Aubin, Sebastien; Leclair, Grégoire

2014-04-15

The stability of penicillin G sodium solutions stored in polyvinyl chloride (PVC) bags or elastomeric pump containers was studied. Test samples were prepared by diluting powdered penicillin G sodium (10 million units/10-mL vial) to solutions of 2,500 or 50,000 units/mL with 0.9% sodium chloride injection or 5% dextrose injection. The preparations were transferred to 250-mL PVC bags and elastomeric pump containers. All samples were prepared in triplicate and stored at 5°C. Chemical stability was measured by a stability-indicating high-performance liquid chromatographic (HPLC) assay and by pH evaluation. Particulate matter was evaluated according to compendial standards using a light-obscuration particle count test. Preparations were visually examined throughout the study. After 21 days of storage, all test samples remained chemically stable, with an HPLC assay recovery value of more than 90% of the initial value. After 28 days, all samples prepared with either diluent and stored in PVC bags, as well as the samples diluted to 2,500 units/mL with sodium chloride injection and stored in elastomeric pump containers, did not meet the recovery acceptance limit. For all test samples, the mean pH consistently decreased during storage, from about 6.4 to about 5.5. Particle counts remained acceptable throughout the study, and no change in appearance was observed. Penicillin G for injection (2,500 and 50,000 units/mL) diluted in 0.9% sodium chloride injection or 5% dextrose injection and stored at 5°C in PVC containers or elastomeric pump containers was physically and chemically stable for a period of at least 21 days.

Enhancing resolution of free-flow zone electrophoresis via a simple sheath-flow sample injection.

PubMed

Yang, Ying; Kong, Fan-Zhi; Liu, Ji; Li, Jun-Min; Liu, Xiao-Ping; Li, Guo-Qing; Wang, Ju-Fang; Xiao, Hua; Fan, Liu-Yin; Cao, Cheng-Xi; Li, Shan

2016-07-01

In this work, a simple and novel sheath-flow sample injection method (SFSIM) is introduced to reduce the band broadening of free-flow zone electrophoresis separation in newly developed self-balance free-flow electrophoresis instrument. A needle injector was placed in the center of the separation inlet, into which the BGE and sample solution were pumped simultaneously. BGE formed sheath flow outside the sample stream, resulting in less band broadening related to hydrodynamics and electrodynamics. Hemoglobin and C-phycocyanin were successfully separated by the proposed method in contrast to the poor separation of free-flow electrophoresis with the traditional injection method without sheath flow. About 3.75 times resolution enhancement could be achieved by sheath-flow sample injection method. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Teduglutide Injection

MedlinePlus

... the medication should read the manufacturer's directions for mixing and injecting the medication before you use it ... Teduglutide must be used within 3 hours after mixing teduglutide powder with the diluent.You can inject ...

Method for operating a spark-ignition, direct-injection internal combustion engine

DOEpatents

Narayanaswamy, Kushal; Koch, Calvin K.; Najt, Paul M.; Szekely, Jr., Gerald A.; Toner, Joel G.

2015-06-02

A spark-ignition, direct-injection internal combustion engine is coupled to an exhaust aftertreatment system including a three-way catalytic converter upstream of an NH3-SCR catalyst. A method for operating the engine includes operating the engine in a fuel cutoff mode and coincidentally executing a second fuel injection control scheme upon detecting an engine load that permits operation in the fuel cutoff mode.

Passive injection control for microfluidic systems

DOEpatents

Paul, Phillip H.; Arnold, Don W.; Neyer, David W.

2004-12-21

Apparatus for eliminating siphoning, "dead" regions, and fluid concentration gradients in microscale analytical devices. In its most basic embodiment, the present invention affords passive injection control for both electric field-driven and pressure-driven systems by providing additional fluid flow channels or auxiliary channels disposed on either side of a sample separation column. The auxiliary channels are sized such that volumetric fluid flow rate through these channels, while sufficient to move the sample away from the sample injection region in a timely fashion, is less than that through the sample separation channel or chromatograph.

Influence of CO2 on the long-term chemomechanical behavior of an oolitic limestone

NASA Astrophysics Data System (ADS)

Grgic, D.

2011-07-01

In order to study the long-term mechanical and petrographical evolutions of a carbonate rock (oolitic limestone) during storage of CO2, CO2 injection tests were performed in triaxial cells at temperature and mechanical stresses (isotropic and deviatoric) corresponding to the depth of the Dogger carbonate reservoirs of the Paris basin (˜800 m). We used a specific "flow-through" triaxial cell which allowed us to measure very low strain rates in both axial and lateral directions, while ensuring the sealing of the samples during the injection of CO2. Under isotropic loading, neither the dynamic percolation (i.e., flow-through tests) of dry supercritical/gaseous CO2, nor the diffusion of CO2, into initially saturated samples was shown to produce significant axial compaction and calcite dissolution. Indeed, even though the interstitial aqueous fluid becomes acidic, the progressive increase in dissolved species induces the H2O-CO2-calcite re-equilibrium. The dynamic injection of CO2-saturated solution induced significant axial compaction due to the dissolution of calcite at the sample/piston interface only under open flow conditions (i.e., the injected acidic solution is continuously renewed). Under closed flow conditions (i.e., acidic solution recirculation or no-flow conditions) which reproduce the physicochemical conditions of CO2 storage at the field scale better, the rapid H2O-CO2-calcite re-equilibrium inhibits calcite dissolution. Under deviatoric loading and closed conditions, the diffusion of CO2 induced a very small increase in the PSC (pressure solution creep) process which was stopped by the H2O-CO2-calcite re-equilibrium inside the sample. Therefore, a significant compaction of limestone samples was obtained only under open conditions and is mainly due to a purely chemical mechanism (calcite dissolution), while the contribution of the chemo-mechanical mechanism (PSC) was found to not be of any great importance. In the context of massive injection of CO2 at the field scale, if the reservoir can be considered as a closed system from a hydrodynamic point of view (i.e., the brine circulates in the aquifer but is not renewed by any groundwater), CO2 will not play a significant role in the chemistry of carbonate reservoirs due to the H2O-CO2-calcite re-equilibrium and will not induce reservoir compaction and affect its long-term storage capacity, whatever the stress state (isotropic or deviatoric).

Pneumatic Microvalve-Based Hydrodynamic Sample Injection for High-Throughput, Quantitative Zone Electrophoresis in Capillaries

PubMed Central

2015-01-01

A hybrid microchip/capillary electrophoresis (CE) system was developed to allow unbiased and lossless sample loading and high-throughput repeated injections. This new hybrid CE system consists of a poly(dimethylsiloxane) (PDMS) microchip sample injector featuring a pneumatic microvalve that separates a sample introduction channel from a short sample loading channel, and a fused-silica capillary separation column that connects seamlessly to the sample loading channel. The sample introduction channel is pressurized such that when the pneumatic microvalve opens briefly, a variable-volume sample plug is introduced into the loading channel. A high voltage for CE separation is continuously applied across the loading channel and the fused-silica capillary separation column. Analytes are rapidly separated in the fused-silica capillary, and following separation, high-sensitivity MS detection is accomplished via a sheathless CE/ESI-MS interface. The performance evaluation of the complete CE/ESI-MS platform demonstrated that reproducible sample injection with well controlled sample plug volumes could be achieved by using the PDMS microchip injector. The absence of band broadening from microchip to capillary indicated a minimum dead volume at the junction. The capabilities of the new CE/ESI-MS platform in performing high-throughput and quantitative sample analyses were demonstrated by the repeated sample injection without interrupting an ongoing separation and a linear dependence of the total analyte ion abundance on the sample plug volume using a mixture of peptide standards. The separation efficiency of the new platform was also evaluated systematically at different sample injection times, flow rates, and CE separation voltages. PMID:24865952

Pneumatic Microvalve-Based Hydrodynamic Sample Injection for High-Throughput, Quantitative Zone Electrophoresis in Capillaries

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

Kelly, Ryan T.; Wang, Chenchen; Rausch, Sarah J.

2014-07-01

A hybrid microchip/capillary CE system was developed to allow unbiased and lossless sample loading and high throughput repeated injections. This new hybrid CE system consists of a polydimethylsiloxane (PDMS) microchip sample injector featuring a pneumatic microvalve that separates a sample introduction channel from a short sample loading channel and a fused silica capillary separation column that connects seamlessly to the sample loading channel. The sample introduction channel is pressurized such that when the pneumatic microvalve opens briefly, a variable-volume sample plug is introduced into the loading channel. A high voltage for CE separation is continuously applied across the loading channelmore » and the fused silica capillary separation column. Analytes are rapidly separated in the fused silica capillary with high resolution. High sensitivity MS detection after CE separation is accomplished via a sheathless CE/ESI-MS interface. The performance evaluation of the complete CE/ESI-MS platform demonstrated that reproducible sample injection with well controlled sample plug volumes could be achieved by using the PDMS microchip injector. The absence of band broadening from microchip to capillary indicated a minimum dead volume at the junction. The capabilities of the new CE/ESI-MS platform in performing high throughput and quantitative sample analyses were demonstrated by the repeated sample injection without interrupting an ongoing separation and a good linear dependence of the total analyte ion abundance on the sample plug volume using a mixture of peptide standards. The separation efficiency of the new platform was also evaluated systematically at different sample injection times, flow rates and CE separation voltages.« less

Direct quantification of lipopeptide biosurfactants in biological samples via HPLC and UPLC-MS requires sample modification with an organic solvent.

PubMed

Biniarz, Piotr; Łukaszewicz, Marcin

2017-06-01

The rapid and accurate quantification of biosurfactants in biological samples is challenging. In contrast to the orcinol method for rhamnolipids, no simple biochemical method is available for the rapid quantification of lipopeptides. Various liquid chromatography (LC) methods are promising tools for relatively fast and exact quantification of lipopeptides. Here, we report strategies for the quantification of the lipopeptides pseudofactin and surfactin in bacterial cultures using different high- (HPLC) and ultra-performance liquid chromatography (UPLC) systems. We tested three strategies for sample pretreatment prior to LC analysis. In direct analysis (DA), bacterial cultures were injected directly and analyzed via LC. As a modification, we diluted the samples with methanol and detected an increase in lipopeptide recovery in the presence of methanol. Therefore, we suggest this simple modification as a tool for increasing the accuracy of LC methods. We also tested freeze-drying followed by solvent extraction (FDSE) as an alternative for the analysis of "heavy" samples. In FDSE, the bacterial cultures were freeze-dried, and the resulting powder was extracted with different solvents. Then, the organic extracts were analyzed via LC. Here, we determined the influence of the extracting solvent on lipopeptide recovery. HPLC methods allowed us to quantify pseudofactin and surfactin with run times of 15 and 20 min per sample, respectively, whereas UPLC quantification was as fast as 4 and 5.5 min per sample, respectively. Our methods provide highly accurate measurements and high recovery levels for lipopeptides. At the same time, UPLC-MS provides the possibility to identify lipopeptides and their structural isoforms.

Plasma Rotation During Neutral Beam Injection In MST

NASA Astrophysics Data System (ADS)

Hudson, Ben; Ding, W.; Fiksel, G.; Prager, S.; Yates, T.

2006-10-01

The effect of fast ions from neutral beam injection (20 keV, 30 A, 1.5 ms) on plasma rotation and magnetic tearing modes is studied. We observe that during co-injected NBI (with the injection in the same direction as the plasma and mode rotation) the rotation of the core-resonant n = 5 magnetic mode decreases and in many instances lock to the vessel wall. There is an associated drop in the poloidal component of n = 5 magnetic mode amplitude. The drop in the mode velocity suggests a counter-directed torque, perhaps due to modification of the radial electric field. The rotation slows during the injection phase, then restores itself on the timescale of the fast ion slowing down time (5 ms @ Te = 100 eV). The fluctuation-induced j x b Maxwell stress is measured using MST's FIR diagnostic and presented for comparison. Equilibrium reconstruction suggests a small increase in on-axis J||, consistent with the presence of a localized fast ion population moving in the direction of the plasma current. Mode rotation during NBI counter-injection is also presented.

Fibrosarcomas at presumed sites of injection in dogs: characteristics and comparison with non-vaccination site fibrosarcomas and feline post-vaccinal fibrosarcomas.

PubMed

Vascellari, M; Melchiotti, E; Bozza, M A; Mutinelli, F

2003-08-01

Fifteen fibrosarcomas, surgically excised from presumed sites of injection in dogs, and 10 canine fibrosarcomas excised from sites not used for injection were histologically and immunohistochemically compared with 20 feline post-vaccinal fibrosarcomas. Canine fibrosarcomas from presumed injection sites were of grade I (3), of grade II (4) and grade III (8). Two fibrosarcomas from non-injection sites were of grade I, four of grade II and four of grade III. Feline samples were classified as grade I (2), grade II (4) and grade III (14). All fibrosarcomas from presumed injection sites of both species showed lymphocytic inflammatory infiltration located at the tumour periphery, while two canine fibrosarcomas from non-injection sites showed perivascular inflammatory infiltration within the neoplasm. All samples were immunohistochemically examined for vimentin, smooth muscle actin, muscle specific actin and desmin expression. All tumours were positive for vimentin. Ten canine fibrosarcomas from presumed injection sites and all feline samples contained cells consistent with a myofibroblastic immunophenotype. Aluminium deposits were detected in eight canine fibrosarcomas from presumed injection sites and 11 feline post-vaccinal fibrosarcomas by the aurintricarboxylic acid method. The present study identifies distinct similarities between canine fibrosarcomas from presumed injection sites and feline post-vaccinal fibrosarcomas, suggesting the possibility of the development of post-injection sarcomas not only in cats, but also in dogs.

Preparation, characterization, and application of an enzyme-immobilized magnetic microreactor for flow injection analysis.

PubMed

Nomura, Akira; Shin, Shigemitsu; Mehdi, Othman Oulad; Kauffmann, Jean-Michel

2004-09-15

Enzyme-immobilized magnetic microparticles (EMMP) have been prepared for use as a microreactor in flow injection analysis (FI). The microparticles were directly injected into the FI system. Their retention occurred within the flow line by small permanent magnets located near the detector. The analytical utility of this concept was illustrated by the assay of glucose using glucose oxidase (GOx), immobilized microparticles, and amperometric detection of liberated hydrogen peroxide. The microparticles were derived from silica gel (nominal pore diameter, 15-80 nm) by impregnation with a citric acid/ethanol solution and a ferric nitrate/ethanol solution and then by calcination in a nitrogen atmosphere to produce ferrimagnetic fine particles of spinel-type iron oxide (gamma-Fe(2)O(3)) inside the pore. They were characterized by X-ray diffraction. The calibration curve of the glucose sample (2 microL injected) was linear between 2.5 x 10(-6) and 5 x 10(-4) mol/L (R = 0.9995), and the detection limit was 1.0 x 10(-6) mol/L or 0.36 ng of injected glucose (S/N = 3). The repeatability for a 5 x 10(-4) mol/L glucose solution was RSD = 1.5% (n = 6). Application to the assay of glucose in a fermentation broth is illustrated. The GOx MMP were stable and active for more than eight months when kept at 10 degrees C.

Effect of Injection Pressure of Infiltration Anesthesia to the Jawbone.

PubMed

Yoshida, Kenji; Tanaka, Eri; Kawaai, Hiroyoshi; Yamazaki, Shinya

To obtain effective infiltration anesthesia in the jawbone, high concentrations of local anesthetic are needed. However, to reduce pain experienced by patients during local anesthetic administration, low-pressure injection is recommended for subperiosteal infiltration anesthesia. Currently, there are no studies regarding the effect of injection pressure on infiltration anesthesia, and a standard injection pressure has not been clearly determined. Hence, the effect of injection pressure of subperiosteal infiltration anesthesia on local anesthetic infiltration to the jawbone was considered by directly measuring lidocaine concentration in the jawbone. Japanese white male rabbits were used as test animals. After inducing general anesthesia with oxygen and sevoflurane, cannulation to the femoral artery was performed and arterial pressure was continuously recorded. Subperiosteal infiltration anesthesia was performed by injecting 0.5 mL of 2% lidocaine containing 1/80,000 adrenaline, and injection pressure was monitored by a pressure transducer for 40 seconds. After specified time intervals (10, 20, 30, 40, 50, and 60 minutes), jawbone and blood samples were collected, and the concentration of lidocaine at each time interval was measured. The mean injection pressure was divided into 4 groups (100 ± 50 mm Hg, 200 ± 50 mm Hg, 300 ± 50 mm Hg, and 400 ± 50 mm Hg), and comparison statistical analysis between these 4 groups was performed. No significant change in blood pressure during infiltration anesthesia was observed in any of the 4 groups. Lidocaine concentration in the blood and jawbone were highest 10 minutes after the infiltration anesthesia in all 4 groups and decreased thereafter. Lidocaine concentration in the jawbone increased as injection pressure increased, while serum lidocaine concentration was significantly lower. This suggests that when injection pressure of subperiosteal infiltration anesthesia is low, infiltration of local anesthetic to the jawbone may be reduced, while transfer to oral mucosa and blood may be increased.

Effect of Injection Pressure of Infiltration Anesthesia to the Jawbone

PubMed Central

Yoshida, Kenji; Tanaka, Eri; Kawaai, Hiroyoshi; Yamazaki, Shinya

2016-01-01

To obtain effective infiltration anesthesia in the jawbone, high concentrations of local anesthetic are needed. However, to reduce pain experienced by patients during local anesthetic administration, low-pressure injection is recommended for subperiosteal infiltration anesthesia. Currently, there are no studies regarding the effect of injection pressure on infiltration anesthesia, and a standard injection pressure has not been clearly determined. Hence, the effect of injection pressure of subperiosteal infiltration anesthesia on local anesthetic infiltration to the jawbone was considered by directly measuring lidocaine concentration in the jawbone. Japanese white male rabbits were used as test animals. After inducing general anesthesia with oxygen and sevoflurane, cannulation to the femoral artery was performed and arterial pressure was continuously recorded. Subperiosteal infiltration anesthesia was performed by injecting 0.5 mL of 2% lidocaine containing 1/80,000 adrenaline, and injection pressure was monitored by a pressure transducer for 40 seconds. After specified time intervals (10, 20, 30, 40, 50, and 60 minutes), jawbone and blood samples were collected, and the concentration of lidocaine at each time interval was measured. The mean injection pressure was divided into 4 groups (100 ± 50 mm Hg, 200 ± 50 mm Hg, 300 ± 50 mm Hg, and 400 ± 50 mm Hg), and comparison statistical analysis between these 4 groups was performed. No significant change in blood pressure during infiltration anesthesia was observed in any of the 4 groups. Lidocaine concentration in the blood and jawbone were highest 10 minutes after the infiltration anesthesia in all 4 groups and decreased thereafter. Lidocaine concentration in the jawbone increased as injection pressure increased, while serum lidocaine concentration was significantly lower. This suggests that when injection pressure of subperiosteal infiltration anesthesia is low, infiltration of local anesthetic to the jawbone may be reduced, while transfer to oral mucosa and blood may be increased. PMID:27585416

Rapid assessment of injection practices in Cambodia, 2002

PubMed Central

Vong, Sirenda; Perz, Joseph F; Sok, Srun; Som, Seiharath; Goldstein, Susan; Hutin, Yvan; Tulloch, James

2005-01-01

Background Injection overuse and unsafe injection practices facilitate transmission of bloodborne pathogens such as hepatitis B virus (HBV), hepatitis C virus (HCV), and human immunodeficiency virus (HIV). Anecdotal reports of unsafe and unnecessary therapeutic injections and the high prevalence of HBV (8.0%), HCV (6.5%), and HIV (2.6%) infection in Cambodia have raised concern over injection safety. To estimate the magnitude and patterns of such practices, a rapid assessment of injection practices was conducted. Methods We surveyed a random sample of the general population in Takeo Province and convenience samples of prescribers and injection providers in Takeo Province and Phnom Penh city regarding injection-related knowledge, attitudes, and practices. Injection providers were observed administering injections. Data were collected using standardized methods adapted from the World Health Organization safe injection assessment guidelines. Results Among the general population sample (n = 500), the overall injection rate was 5.9 injections per person-year, with 40% of participants reporting receipt of ≥ 1 injection during the previous 6 months. Therapeutic injections, intravenous infusions, and immunizations accounted for 74%, 16% and 10% of injections, respectively. The majority (>85%) of injections were received in the private sector. All participants who recalled their last injection reported the injection was administered with a newly opened disposable syringe and needle. Prescribers (n = 60) reported that 47% of the total prescriptions they wrote included a therapeutic injection or infusion. Among injection providers (n = 60), 58% recapped the syringe after use and 13% did not dispose of the used needle and syringe appropriately. Over half (53%) of the providers reported a needlestick injury during the previous 12 months. Ninety percent of prescribers and injection providers were aware HBV, HCV, and HIV were transmitted through unsafe injection practices. Knowledge of HIV transmission through "dirty" syringes among the general population was also high (95%). Conclusion Our data suggest that Cambodia has one of the world's highest rates of overall injection usage, despite general awareness of associated infection risks. Although there was little evidence of reuse of needles and syringes, support is needed for interventions to address injection overuse, healthcare worker safety and appropriate waste disposal. PMID:15929800

Analysis of Supercritical-Extracted Chelated Metal Ions From Mixed Organic-Inorganic Samples

NASA Technical Reports Server (NTRS)

Sinha, Mahadeva P. (Inventor)

1996-01-01

Organic and inorganic contaminants of an environmental sample are analyzed by the same GC-MS instrument by adding an oxidizing agent to the sample to oxidize metal or metal compounds to form metal ions. The metal ions are converted to chelate complexes and the chelate complexes are extracted into a supercritical fluid such as CO2. The metal chelate extract after flowing through a restrictor tube is directly injected into the ionization chamber of a mass spectrometer, preferably containing a refractory metal filament such as rhenium to fragment the complex to release metal ions which are detected. This provides a fast, economical method for the analysis of metal contaminants in a sample and can be automated. An organic extract of the sample in conventional or supercritical fluid solvents can be detected in the same mass spectrometer, preferably after separation in a supercritical fluid chromatograph.

Characterization of Pharmaceuticals and Personal Care products in hospital effluent and waste water influent/effluent by direct-injection LC-MS-MS.

PubMed

Oliveira, Tiago S; Murphy, Mark; Mendola, Nicholas; Wong, Virginia; Carlson, Doreen; Waring, Linda

2015-06-15

Two USEPA Regional Laboratories developed direct-injection LC/MS/MS methods to measure Pharmaceuticals and Personal Care Products (PPCPs) in water matrices. Combined, the laboratories were prepared to analyze 185 PPCPs (with 74 overlapping) belonging to more than 20 therapeutical categories with reporting limits at low part-per-trillion. In partnership with Suffolk County in NY, the laboratories conducted PPCP analysis on 72 samples belonging to 4 Water Systems (WS). Samples were collected at different stages of the WS (hospital effluents, WWTP influents/effluents) to assess PPCP relevance in hospital discharges, impact on WWTP performance and potential ecological risk posed by analytes not eliminated during treatment. Major findings include: a) acceptable accuracy between the two laboratories for most overlapping PPCPs with better agreement for higher concentrations; b) the measurement of PPCPs throughout all investigated WS with total PPCP concentrations ranging between 324 and 965 μg L(-1) for hospital effluent, 259 and 573 μg L(-1) for WWTP influent and 19 and 118 μg L(-1) for WWTP effluent; c) the variable contribution of hospital effluents to the PPCP loads into the WWTP influents (contribution ranging between 1% (WS-2) and 59% (WS-3); d) the PPCP load reduction after treatment for all WS reaching more than 95% for WS using activated sludge processes (WS-2 and WS-4), with inflow above 6500 m(3) d(-1), and having a lower percentage of hospital effluent in the WWTP influent; e) the relevance of four therapeutical categories for the PPCP load in WWTP effluents (analgesics, antidiabetics, antiepileptics and psychoanaleptics); and f) the risk quotients calculated using screening-level Predicted Non Effect Concentration indicate that WWTP effluents contain 33 PPCPs with potential medium to high ecological risk. To our knowledge no other monitoring investigation published in the scientific literature uses direct-injection methods to cover as many PPCPs and therapeutical categories in different types of WS. Copyright © 2015 Elsevier B.V. All rights reserved.

Design and development of a direct injection system for cryogenic engines

NASA Astrophysics Data System (ADS)

Mutumba, Angela; Cheeseman, Kevin; Clarke, Henry; Wen, Dongsheng

2018-04-01

The cryogenic engine has received increasing attention due to its promising potential as a zero-emission engine. In this study, a new robust liquid nitrogen injection system was commissioned and set up to perform high-pressure injections into an open vessel. The system is used for quasi-steady flow tests used for the characterisation of the direct injection process for cryogenic engines. An electro-hydraulic valve actuator provides intricate control of the valve lift, with a minimum cycle time of 3 ms and a frequency of up to 20 Hz. With additional sub-cooling, liquid phase injections from 14 to 94 bar were achieved. Results showed an increase in the injected mass with the increase in pressure, and decrease in temperature. The injected mass was also observed to increases linearly with the valve lift. Better control of the injection process, minimises the number of variables, providing more comparable and repeatable sets of data. Implications of the results on the engine performance were also discussed.

Ultra low injection angle fuel holes in a combustor fuel nozzle

DOEpatents

York, William David

2012-10-23

A fuel nozzle for a combustor includes a mixing passage through which fluid is directed toward a combustion area and a plurality of swirler vanes disposed in the mixing passage. Each swirler vane of the plurality of swirler vanes includes at least one fuel hole through which fuel enters the mixing passage in an injection direction substantially parallel to an outer surface of the plurality of swirler vanes thereby decreasing a flameholding tendency of the fuel nozzle. A method of operating a fuel nozzle for a combustor includes flowing a fluid through a mixing passage past a plurality of swirler vanes and injecting a fuel into the mixing passage in an injection direction substantially parallel to an outer surface of the plurality of swirler vanes.

A robust and fast method of sampling and analysis of delta13C of dissolved inorganic carbon in ground waters.

PubMed

Spötl, Christoph

2005-09-01

The stable carbon isotopic composition of dissolved inorganic carbon (delta13C(DIC)) is traditionally determined using either direct precipitation or gas evolution methods in conjunction with offline gas preparation and measurement in a dual-inlet isotope ratio mass spectrometer. A gas evolution method based on continuous-flow technology is described here, which is easy to use and robust. Water samples (100-1500 microl depending on the carbonate alkalinity) are injected into He-filled autosampler vials in the field and analysed on an automated continuous-flow gas preparation system interfaced to an isotope ratio mass spectrometer. Sample analysis time including online preparation is 10 min and overall precision is 0.1 per thousand. This method is thus fast and can easily be automated for handling large sample batches.

Brillouin micro-spectroscopy through aberrations via sensorless adaptive optics

NASA Astrophysics Data System (ADS)

Edrei, Eitan; Scarcelli, Giuliano

2018-04-01

Brillouin spectroscopy is a powerful optical technique for non-contact viscoelastic characterizations which has recently found applications in three-dimensional mapping of biological samples. Brillouin spectroscopy performances are rapidly degraded by optical aberrations and have therefore been limited to homogenous transparent samples. In this work, we developed an adaptive optics (AO) configuration designed for Brillouin scattering spectroscopy to engineer the incident wavefront and correct for aberrations. Our configuration does not require direct wavefront sensing and the injection of a "guide-star"; hence, it can be implemented without the need for sample pre-treatment. We used our AO-Brillouin spectrometer in aberrated phantoms and biological samples and obtained improved precision and resolution of Brillouin spectral analysis; we demonstrated 2.5-fold enhancement in Brillouin signal strength and 1.4-fold improvement in axial resolution because of the correction of optical aberrations.

Tandem mass spectrometry of coprogen and deferoxamine hydroxamic siderophores.

PubMed

Simionato, Ana V C; de Souza, Gezimar D; Rodrigues-Filho, Edson; Glick, James; Vouros, Paul; Carrilho, Emanuel

2006-01-01

Mechanisms of fragmentation of hydroxamic siderophores are proposed comparing deuterated and nondeuterated samples. Standard siderophores (e.g. deferoxamine and coprogen) were directly injected into both ion trap and linear quadrupole mass spectrometers with electrospray ionization (ESI). Four and two fragmentation steps were carried out for deferoxamine and coprogen (analyzed by positive and negative ESI, respectively). Deferoxamine cleavages occurred in both peptide and hydroxamic bonds while the coprogen fragmentation pattern is more elaborate, since it contains Fe(III) in its structure.

Determination of Caffeine in Beverages by Capillary Zone Electrophoresis: An Experiment for the Undergraduate Analytical Laboratory

NASA Astrophysics Data System (ADS)

Conte, Eric D.; Barry, Eugene F.; Rubinstein, Harry

1996-12-01

Certain individuals may be sensitive to specific compounds in comsumer products. It is important to quantify these analytes in food products in order to monitor their intake. Caffeine is one such compound. Determination of caffeine in beverages by spectrophotometric procedures requires an extraction procedure, which can prove time-consuming. Although the corresponding determination by HPLC allows for a direct injection, capillary zone electrophoresis provides several advantages such as extremely low solvent consumption, smaller sample volume requirements, and improved sensitivity.

Toots, tastes and tester shots: user accounts of drug sampling methods for gauging heroin potency.

PubMed

Mars, Sarah G; Ondocsin, Jeff; Ciccarone, Daniel

2018-05-16

Internationally, overdose is the primary cause of death among people injecting drugs. However, since 2001, heroin-related overdose deaths in the United States (US) have risen sixfold, paralleled by a rise in the death rate attributed to synthetic opioids, particularly the fentanyls. This paper considers the adaptations some US heroin injectors are making to protect themselves from these risks. Between 2015 and 2016, a team of ethnographers collected data through semi-structured interviews and observation captured in field notes and video recording of heroin preparation/consumption. Ninety-one current heroin injectors were interviewed (Baltimore, n = 22; Chicago, n = 24; Massachusetts and New Hampshire, n = 36; San Francisco, n = 9). Experience injecting heroin ranged from < 1-47 years. Eight participants, who were exclusively heroin snorters, were also interviewed. Data were analyzed thematically. Across the study sites, multiple methods of sampling "heroin" were identified, sometimes used in combination, ranging from non-injecting routes (snorting, smoking or tasting a small amount prior to injection) to injecting a partial dose and waiting. Partial injection took different forms: a "slow shot" where the user injected a portion of the solution in the syringe, keeping the needle in the injection site, and continuing or withdrawing the syringe or a "tester shot" where the solution was divided into separate injections. Other techniques included getting feedback from others using heroin of the same batch or observing those with higher tolerance injecting heroin from the same batch before judging how much to inject themselves. Although a minority of those interviewed described using these drug sampling techniques, there is clearly receptivity among some users to protecting themselves by using a variety of methods. The use of drug sampling as a means of preventing an overdose from injection drug use reduces the quantity absorbed at any one time allowing users to monitor drug strength and titrate their dose accordingly. Given the highly unpredictable potency of the drugs currently being sold as heroin in the US, universal precautions should be adopted more widely. Further research is needed into facilitators and barriers to the uptake of these drug sampling methods.

A fully automated and fast method using direct sample injection combined with fused-core column on-line SPE-HPLC for determination of ochratoxin A and citrinin in lager beers.

PubMed

Lhotská, Ivona; Šatínský, Dalibor; Havlíková, Lucie; Solich, Petr

2016-05-01

A new fast and sensitive method based on on-line solid-phase extraction on a fused-core precolumn coupled to liquid chromatography with fluorescence detection has been developed for ochratoxin A (OTA) and citrinin (CIT) determination in lager beer samples. Direct injection of 100 μL filtered beer samples into an on-line SPE-HPLC system enabled fast and effective sample extraction including separation in less than 6 min. Preconcentration of OTA and CIT from beer samples was performed on an Ascentis Express RP C18 guard column (5 × 4.6 mm), particle size 2.7 μm, with a mobile phase of methanol/0.5% aqueous acetic acid pH 2.8 (30:70, v/v) at a flow rate of 2.0 mL min(-1). The flow switch from extraction column to analytical column in back-flush mode was set at 2.0 min and the separation was performed on the fused-core column Ascentis Express Phenyl-Hexyl (100 × 4.6 mm), particle size 2.7 μm, with a mobile phase acetonitrile/0.5% aqueous acetic acid pH 2.8 in a gradient elution at a flow rate of 1.0 mL min(-1) and temperature of 50 °C. Fluorescence excitation/emission detection wavelengths were set at 335/497 nm. The accuracy of the method, defined as the mean recoveries of OTA and CIT from light and dark beer samples, was in the range 98.3-102.1%. The method showed high sensitivity owing to on-line preconcentration; LOQ values were found to be 10 and 20 ng L(-1) for OTA and CIT, respectively. The found values of OTA and CIT in all tested light, dark and wheat beer samples were significantly below the maximum tolerable limits (3.0 μg kg(-1) for OTA and 2000 μg kg(-1) for CIT) set by the European Union.

Effects of large volume injection of aliphatic alcohols as sample diluents on the retention of low hydrophobic solutes in reversed-phase liquid chromatography.

PubMed

David, Victor; Galaon, Toma; Aboul-Enein, Hassan Y

2014-01-03

Recent studies showed that injection of large volume of hydrophobic solvents used as sample diluents could be applied in reversed-phase liquid chromatography (RP-LC). This study reports a systematic research focused on the influence of a series of aliphatic alcohols (from methanol to 1-octanol) on the retention process in RP-LC, when large volumes of sample are injected on the column. Several model analytes with low hydrophobic character were studied by RP-LC process, for mobile phases containing methanol or acetonitrile as organic modifiers in different proportions with aqueous component. It was found that starting with 1-butanol, the aliphatic alcohols can be used as sample solvents and they can be injected in high volumes, but they may influence the retention factor and peak shape of the dissolved solutes. The dependence of the retention factor of the studied analytes on the injection volume of these alcohols is linear, with a decrease of its value as the sample volume is increased. The retention process in case of injecting up to 200μL of upper alcohols is dependent also on the content of the organic modifier (methanol or acetonitrile) in mobile phase. Copyright © 2013 Elsevier B.V. All rights reserved.

Multi-residue analysis of organic pollutants in hair and urine for matrices comparison.

PubMed

Hardy, Emilie M; Duca, Radu C; Salquebre, Guillaume; Appenzeller, Brice M R

2015-04-01

Urine being currently the most classically used matrix for the assessment of human exposure to pesticides, a growing interest is yet observed in hair analysis for the detection of organic pollutants. The aim of the present work was to develop and to validate multi-residue analytical methods, as similar as possible, in order to determine pesticides and their metabolites in these two biological matrices despite their different nature. The list of parent compounds and their metabolites investigated here consisted of 56 compounds, including organochlorines, organophosphates, pyrethroids, carbamates, other pesticides and polychlorinated biphenyls (PCBs). Two different approaches were necessary for the analysis of non-polar compounds (mainly parents) on one hand and polar analytes (mainly metabolites) on the other hand. In the final procedure, extraction from hair was carried out with acetonitrile/water after sample decontamination and pulverization. Extract was split into two fractions, which were analyzed directly with solid phase microextraction (SPME) injection for non-polar compounds and after derivatization with liquid injection for polar compounds. In urine, non-polar compounds were analyzed directly using SPME. Polar compounds were analyzed after acidic hydrolysis, liquid-liquid extraction with acetonitrile-cyclohexane-ethyl acetate, derivatization and liquid injection. Analysis was performed with gas chromatography tandem mass spectrometry operating in negative chemical ionization (GC-MS/MS-NCI) for all the compounds (non-polar and polar) in the two matrices. In hair, limits of quantification (LOQ) ranged from 0.02 pg/mg for trifluralin to 5.5 pg/mg for diethylphosphate. In urine, LOQ ranged from 0.4 pg/mL for α-endosulfan to 4 ng/mL for dimethyldithiophosphate. The analysis of samples supplemented with standards and samples collected from an animal previously submitted to chronic exposure to pesticides confirmed that all the compounds were analyzable in both hair and urine. In addition, the levels of sensitivity reached with these methods were quite satisfactory with regard to previously published studies, and also considering the number of compounds investigated. Copyright © 2014. Published by Elsevier Ireland Ltd.

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

Sevik, James; Pamminger, Michael; Wallner, Thomas

Interest in natural gas as an alternative fuel source to petroleum fuels for light-duty vehicle applications has increased due to its domestic availability and stable price compared to gasoline. With its higher hydrogen-to-carbon ratio, natural gas has the potential to reduce engine out carbon dioxide emissions, which has shown to be a strong greenhouse gas contributor. For part-load conditions, the lower flame speeds of natural gas can lead to an increased duration in the inflammation process with traditional port-injection. Direct-injection of natural gas can increase in-cylinder turbulence and has the potential to reduce problems typically associated with port-injection of naturalmore » gas, such as lower flame speeds and poor dilution tolerance. A study was designed and executed to investigate the effects of direct-injection of natural gas at part-load conditions. Steady-state tests were performed on a single-cylinder research engine representative of current gasoline direct-injection engines. Tests were performed with direct-injection in the central and side location. The start of injection was varied under stoichiometric conditions in order to study the effects on the mixture formation process. In addition, exhaust gas recirculation was introduced at select conditions in order to investigate the dilution tolerance. Relevant combustion metrics were then analyzed for each scenario. Experimental results suggest that regardless of the injector location, varying the start of injection has a strong impact on the mixture formation process. Delaying the start of injection from 300 to 120°CA BTDC can reduce the early flame development process by nearly 15°CA. While injecting into the cylinder after the intake valves have closed has shown to produce the fastest combustion process, this does not necessarily lead to the highest efficiency, due to increases in pumping and wall heat losses. When comparing the two injection configurations, the side location shows the best performance in terms of combustion metrics and efficiencies. For both systems, part-load dilution tolerance is affected by the injection timing, due to the induced turbulence from the gaseous injection event. CFD simulation results have shown that there is a fundamental difference in how the two injection locations affect the mixture formation process. Delayed injection timing increases the turbulence level in the cylinder at the time of the spark, but reduces the available time for proper mixing. Side injection delivers a gaseous jet that interacts more effectively with the intake induced flow field, and this improves the engine performance in terms of efficiency.« less

Hyaluronic Acid (HA)-Polyethylene glycol (PEG) as injectable hydrogel for intervertebral disc degeneration patients therapy

NASA Astrophysics Data System (ADS)

Putri Kwarta, Cityta; Widiyanti, Prihartini; Siswanto

2017-05-01

Chronic Low Back Pain (CLBP) is one health problem that is often encountered in a community. Inject-able hydrogels are the newest way to restore the disc thickness and hydration caused by disc degeneration by means of minimally invasive surgery. Thus, polymers can be combined to improve the characteristic properties of inject-able hydrogels, leading to use of Hyaluronic Acid (a natural polymer) and Polyethylene glycol (PEG) with Horse Radish Peroxide (HRP) cross linker enzymes. The swelling test results, which approaches were the ideal disc values, were sampled with variation of enzyme concentrations of 0.25 µmol/min/mL. The enzyme concentrations were 33.95%. The degradation test proved that the sample degradation increased along with the decrease of the HRP enzyme concentration. The results of the cytotoxicity assay with MTT assay method showed that all samples resulted in the 90% of living cells are not toxic. In vitro injection, models demonstrated that higher concentration of the enzymes was less state of gel which would rupture when released from the agarose gel. The functional group characterization shows the cross linking bonding in sample with enzyme adding. The conclusion of this study is PEG-HA-HRP enzyme are safe polymer composites which have a potential to be applied as an injectable hydrogel for intervertebral disc degeneration.

Flow through electrode with automated calibration

DOEpatents

Szecsody, James E [Richland, WA; Williams, Mark D [Richland, WA; Vermeul, Vince R [Richland, WA

2002-08-20

The present invention is an improved automated flow through electrode liquid monitoring system. The automated system has a sample inlet to a sample pump, a sample outlet from the sample pump to at least one flow through electrode with a waste port. At least one computer controls the sample pump and records data from the at least one flow through electrode for a liquid sample. The improvement relies upon (a) at least one source of a calibration sample connected to (b) an injection valve connected to said sample outlet and connected to said source, said injection valve further connected to said at least one flow through electrode, wherein said injection valve is controlled by said computer to select between said liquid sample or said calibration sample. Advantages include improved accuracy because of more frequent calibrations, no additional labor for calibration, no need to remove the flow through electrode(s), and minimal interruption of sampling.

Collective properties of injection-induced earthquake sequences: 1. Model description and directivity bias

NASA Astrophysics Data System (ADS)

Dempsey, David; Suckale, Jenny

2016-05-01

Induced seismicity is of increasing concern for oil and gas, geothermal, and carbon sequestration operations, with several M > 5 events triggered in recent years. Modeling plays an important role in understanding the causes of this seismicity and in constraining seismic hazard. Here we study the collective properties of induced earthquake sequences and the physics underpinning them. In this first paper of a two-part series, we focus on the directivity ratio, which quantifies whether fault rupture is dominated by one (unilateral) or two (bilateral) propagating fronts. In a second paper, we focus on the spatiotemporal and magnitude-frequency distributions of induced seismicity. We develop a model that couples a fracture mechanics description of 1-D fault rupture with fractal stress heterogeneity and the evolving pore pressure distribution around an injection well that triggers earthquakes. The extent of fault rupture is calculated from the equations of motion for two tips of an expanding crack centered at the earthquake hypocenter. Under tectonic loading conditions, our model exhibits a preference for unilateral rupture and a normal distribution of hypocenter locations, two features that are consistent with seismological observations. On the other hand, catalogs of induced events when injection occurs directly onto a fault exhibit a bias toward ruptures that propagate toward the injection well. This bias is due to relatively favorable conditions for rupture that exist within the high-pressure plume. The strength of the directivity bias depends on a number of factors including the style of pressure buildup, the proximity of the fault to failure and event magnitude. For injection off a fault that triggers earthquakes, the modeled directivity bias is small and may be too weak for practical detection. For two hypothetical injection scenarios, we estimate the number of earthquake observations required to detect directivity bias.

Computational modeling of the effect of external electron injection into a direct-current microdischarge

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

Panneer Chelvam, Prem Kumar; Raja, Laxminarayan L.

2015-12-28

Electron emission from the electrode surface plays an important role in determining the structure of a direct-current microdischarge. Here we have developed a computational model of a direct-current microdischarge to study the effect of external electron injection from the cathode surface into the discharge to manipulate its properties. The model provides a self-consistent, multi-species, multi-temperature fluid representation of the plasma. A microdischarge with a metal-insulator-metal configuration is chosen for this study. The effect of external electron injection on the structure and properties of the microdischarge is described. The transient behavior of the microdischarge during the electron injection is examined. Themore » nonlinearities in the dynamics of the plasma result in a large increase of conduction current after active electron injection. For the conditions simulated a switching time of ∼100 ns from a low-current to high-current discharge state is realized.« less

Open Port Probe Sampling Interface for the Direct Coupling of Biocompatible Solid-Phase Microextraction to Atmospheric Pressure Ionization Mass Spectrometry.

PubMed

Gómez-Ríos, Germán Augusto; Liu, Chang; Tascon, Marcos; Reyes-Garcés, Nathaly; Arnold, Don W; Covey, Thomas R; Pawliszyn, Janusz

2017-04-04

In recent years, the direct coupling of solid phase microextraction (SPME) and mass spectrometry (MS) has shown its great potential to improve limits of quantitation, accelerate analysis throughput, and diminish potential matrix effects when compared to direct injection to MS. In this study, we introduce the open port probe (OPP) as a robust interface to couple biocompatible SPME (Bio-SPME) fibers to MS systems for direct electrospray ionization. The presented design consisted of minimal alterations to the front-end of the instrument and provided better sensitivity, simplicity, speed, wider compound coverage, and high-throughput in comparison to the LC-MS based approach. Quantitative determination of clenbuterol, fentanyl, and buprenorphine was successfully achieved in human urine. Despite the use of short extraction/desorption times (5 min/5 s), limits of quantitation below the minimum required performance levels (MRPL) set by the world antidoping agency (WADA) were obtained with good accuracy (≥90%) and linearity (R 2 > 0.99) over the range evaluated for all analytes using sample volumes of 300 μL. In-line technologies such as multiple reaction monitoring with multistage fragmentation (MRM 3 ) and differential mobility spectrometry (DMS) were used to enhance the selectivity of the method without compromising analysis speed. On the basis of calculations, once coupled to high throughput, this method can potentially yield preparation times as low as 15 s per sample based on the 96-well plate format. Our results demonstrated that Bio-SPME-OPP-MS efficiently integrates sampling/sample cleanup and atmospheric pressure ionization, making it an advantageous configuration for several bioanalytical applications, including doping in sports, in vivo tissue sampling, and therapeutic drug monitoring.

[Detection of rifampicin concentration in cerebrospinal fluid by online enrichment and restricted-access media coupled with high-performance liquid chromatography].

PubMed

Yang, Xiaoping; Zhang, Xiaohui; Huang, Yanping; Wang, Rong; Xia, Hua; Li, Wenbin; Guo, YouMin

2015-11-01

To establish a method for detecting rifampicin in human cerebrospinal fluid (CSF) with restricted access media coupled with high-performance liquid chromatography that allows online direct sample injection and enrichment. We used the column of restricted access media as the pre-treatment column and a C18 column as the analytical column. The mobile phase of pre-treatment column was water-methanol (95:5,V/V) and the flow rate was 1 mL/min; the mobile phase of the analytical column was methanol-acetonitrile-10 mmol/L ammonuium acetate (volume ratio of 60:5:35). The detection wavelength was 254 nm and the column temperature was set at 25 degrees celsius;. For an injection volume of 100 µL, the peak area of rifampicin was 5.33 times that for an injection volume of 20 µL, and the limit of detection was effectively improved. The calibration curve showed an excellent linear relationship (r=0.9997) between rifampicin concentrations and peak areas within the concentration range of 0.25 to 8 µg/mL in CSF. The limits of detection and quantification was 0.07 µg/mL and 0.25 µg/mL, respecetively, with intra-day and inter-day assay precisions and relative standard deviation (RSD%) all below 5%. The recoveries of rifampicin at 3 blank spiked levels (low, medium, and high) ranged from 87.69% to 102.11%. In patients taking oral rifampicin at the dose of 10 mg/kg, the average rifampicin concentration was 0.29 in the CSF at 2 h after medication. The method we established is simple and fast for detecting rifampicin in CSF and allows direct online injection and enrichment with good detection precisions and accuracies.

Hydrogeological characterization of shallow-depth zone for CO2 injection and leak test at a CO2 environmental monitoring site in Korea

NASA Astrophysics Data System (ADS)

Lee, S. S.; Kim, T. W.; Kim, H. H.; Ha, S. W.; Jeon, W. T.; Lee, K. K.

2015-12-01

The main goal of the this study is to evaluate the importance of heterogeneities in controlling the field-scale transport of CO2 are originated from the CO2 injected at saturated zone below the water table for monitoring and prediction of CO2 leakage from a reservoir. Hydrogeological and geophysical data are collected to characterize the site, prior to conducting CO2 injection experiment at the CO2 environmental monitoring site at Eumseong, Korea. The geophysical data were acquired from borehole electromagnetic flowmeter tests, while the hydraulic data were obtained from pumping tests, slug tests, and falling head permeability tests. Total of 13 wells to perform hydraulic and geophysical test are established along groundwater flow direction in regular sequence, revealed by the results of borehole electromagnetic flowmeter test. The results of geophysical tests indicated that hydraulic gradient is not identical with the topographic gradient. Groundwater flows toward the uphill direction in the study area. Then, the hydraulic tests were conducted to identify the hydraulic properties of the study site. According to the results of pumping and slug tests at the study site, the hydraulic conductivity values show ranges between 4.75 x 10-5 cm/day and 9.74 x 10-5 cm/day. In addition, a portable multi-level sampling and monitoring packer device which remains inflated condition for a long period developed and used to isolate designated depths to identify vertical distribution of hydrogeological characteristics. Hydrogeological information obtained from this study will be used to decide the injection test interval of CO2-infused water and gaseous CO2. Acknowledgement: Financial support was provided by "R&D Project on Environmental Mangement of Geologic CO2 Storage" from the KEITI (Project Number: 2014001810003).

Injection characteristics study of high-pressure direct injector for Compressed Natural Gas (CNG) using experimental and analytical method

NASA Astrophysics Data System (ADS)

Taha, Z.; Rahim, MF Abdul; Mamat, R.

2017-10-01

The injection characteristics of direct injector affect the mixture formation and combustion processes. In addition, the injector is converted from gasoline operation for CNG application. Thus measurement of CNG direct injector mass flow rate was done by independently tested a single injector on a test bench. The first case investigated the effect of CNG injection pressure and the second case evaluate the effect of pulse-width of injection duration. An analytical model was also developed to predict the mass flow rate of the injector. The injector was operated in a choked condition in both the experiments and simulation studies. In case 1, it was shown that mass flow rate through the injector is affected by injection pressure linearly. Based on the tested injection pressure of 20 bar to 60 bar, the resultant mass flow rate are in the range of 0.4 g/s to 1.2 g/s which are met with theoretical flow rate required by the engine. However, in Case 2, it was demonstrated that the average mass flow rate at short injection durations is lower than recorded in Case 1. At injection pressure of 50 bar, the average mass flow rate for Case 2 and Case 1 are 0.7 g/s and 1.1 g/s respectively. Also, the measured mass flow rate at short injection duration showing a fluctuating data in the range of 0.2 g/s - 1.3 g/s without any noticeable trends. The injector model able to predict the trend of the mass flow rate at different injection pressure but unable to track the fluctuating trend at short injection duration.

The directional dependence of cometary magnetic energy density in the quasi-parallel and quasi-perpendicular regimes

NASA Technical Reports Server (NTRS)

Miller, R. H.; Gombosi, T. I.; Gary, S. P.; Winske, D.

1991-01-01

The direction of propagation of low frequency magnetic fluctuations generated by cometary ion pick-up is examined by means of 1D electromagnetic hybrid simulations. The newborn ions are injected at a constant rate, and the helicity and direction of propagation of magnetic fluctuations are explored for cometary ion injection angles of 0 and 90 deg relative to the solar wind magnetic field. The parameter eta represents the relative contribution of wave energy propagating in the direction away from the comet, parallel to the beam. For small (quasi-parallel) injection angles eta was found to be of order unity, while for larger (quasi-perpendicular) angles eta was found to be of order 0.5.

Development of CNG direct injection (CNGDI) clean fuel system for extra power in small engine

NASA Astrophysics Data System (ADS)

Ali, Yusoff; Shamsudeen, Azhari; Abdullah, Shahrir; Mahmood, Wan Mohd Faizal Wan

2012-06-01

A new design of fuel system for CNG engine with direct injection (CNGDI) was developed for a demonstration project. The development of the fuel system was done on the engine with cylinder head modifications, for fuel injector and spark plug openings included in the new cylinder head. The piston was also redesigned for higher compression ratio. The fuel rails and the regulators are also designed for the direct injection system operating at higher pressure about 2.0 MPa. The control of the injection timing for the direct injectors are also controlled by the Electronic Control Unit specially designed for DI by another group project. The injectors are selected after testing with the various injection pressures and spray angles. For the best performance of the high-pressure system, selection is made from the tests on single cylinder research engine (SCRE). The components in the fuel system have to be of higher quality and complied with codes and standards to secure the safety of engine for high-pressure operation. The results of the CNGDI have shown that better power output is produced and better emissions were achieved compared to the aspirated CNG engine.

Viscoelastic properties of rabbit vocal folds after augmentation.

PubMed

Hertegård, Stellan; Dahlqvist, Ake; Laurent, Claude; Borzacchiello, Assunta; Ambrosio, Luigi

2003-03-01

Vocal fold function is closely related to tissue viscoelasticity. Augmentation substances may alter the viscoelastic properties of vocal fold tissues and hence their vibratory capacity. We sought to investigate the viscoelastic properties of rabbit vocal folds in vitro after injections of various augmentation substances. Polytetrafluoroethylene (Teflon), cross-linked collagen (Zyplast), and cross-linked hyaluronan, hylan b gel (Hylaform) were injected into the lamina propria and the thyroarytenoid muscle of rabbit vocal folds. Dynamic viscosity of the injected vocal fold as a function of frequency was measured with a Bohlin parallel-plate rheometer during small-amplitude oscillation. All injected vocal folds showed a decreasing dynamic viscosity with increasing frequency. Vocal fold samples injected with hylan b gel showed the lowest dynamic viscosity, quite close to noninjected control samples. Vocal folds injected with polytetrafluoroethylene showed the highest dynamic viscosity followed by the collagen samples. The data indicated that hylan b gel in short-term renders the most natural viscoelastic properties to the vocal fold among the substances tested. This is of importance to restore/preserve the vibratory capacity of the vocal folds when glottal insufficiency is treated with injections.

Porous protective solid phase micro-extractor sheath

DOEpatents

Andresen, Brian D.; Randich, Erik

2005-03-29

A porous protective sheath for active extraction media used in solid phase microextraction (SPME). The sheath permits exposure of the media to the environment without the necessity of extending a fragile coated fiber from a protective tube or needle. Subsequently, the sheath can pierce and seal with GC-MS septums, allowing direct injection of samples into inlet ports of analytical equipment. Use of the porous protective sheath, within which the active extraction media is contained, mitigates the problems of: 1) fiber breakage while the fiber is extended during sampling, 2) active media coating loss caused by physical contact of the bare fiber with the sampling environment; and 3) coating slough-off during fiber extension and retraction operations caused by rubbing action between the fiber and protective needle or tube.

Gas chromatographic determination of fumigant residues in stored grains, using isooctane partitioning and dual column packings.

PubMed

Daft, J L

1983-03-01

A gas chromatographic (GC) procedure for determining fumigants in grains was developed. Fumigants were leached from grain samples with the official AOAC method using acetone-water (5 + 1). They were then partitioned from the leachate with isooctane, yielding a dry, stable extract that was analyzed by GC. Fortified sample recoveries ranged from 90 to 100%. Two GC columns were used, 20% OV-101 and 20% OV-225/20% OV-17 (2 + 1). These columns gave dissimilar retention profiles and baseline resolution for the 7 fumigants investigated: chloroform, ethylene dichloride, carbon tetrachloride, trichloroethylene, chloropicrin, ethylene dibromide, and tetrachloroethylene. Further tests showed that grain samples could be screened for fumigant residues by direct injection of the acetone-water leachates obtained using the AOAC method.

Rapid method for measuring rotenone in water at piscicidal concentrations

USGS Publications Warehouse

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

1983-01-01

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

Sensitive flow-injection spectrophotometric analysis of bromopride.

PubMed

Lima, Liliane Spazzapam; Los Weinert, Patrícia; Pezza, Leonardo; Pezza, Helena Redigolo

2014-12-10

A flow injection spectrophotometric procedure employing merging zones is proposed for direct bromopride determination in pharmaceutical formulations and biological fluids. The proposed method is based on the reaction between bromopride and p-dimethylaminocinnamaldehyde (p-DAC) in acid medium, in the presence of sodium dodecyl sulfate (SDS), resulting in formation of a violet product (λmax=565nm). Experimental design methodologies were used to optimize the experimental conditions. The Beer-Lambert law was obeyed in a bromopride concentration range of 3.63×10(-7) to 2.90×10(-5)molL(-1), with a correlation coefficient (r) of 0.9999. The limits of detection and quantification were 1.07×10(-7) and 3.57×10(-7)molL(-1), respectively. The proposed method was successfully applied to the determination of bromopride in pharmaceuticals and human urine, and recoveries of the drug from these media were in the ranges 99.6-101.2% and 98.6-102.1%, respectively. This new flow injection procedure does not require any sample pretreatment steps. Copyright © 2014 Elsevier B.V. All rights reserved.

On the effect of injection timing on the ignition of lean PRF/air/EGR mixtures under direct dual fuel stratification conditions

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

Luong, Minh Bau; Sankaran, Ramanan; Yu, Gwang Hyeon

2017-06-09

The ignition characteristics of lean primary reference fuel (PRF)/air/exhaust gas recirculation (EGR) mixture under reactivity-controlled compression ignition (RCCI) and direct duel fuel stratification (DDFS) conditions are investigated in this paper by 2-D direct numerical simulations (DNSs) with a 116-species reduced chemistry of the PRF oxidation. The 2-D DNSs of the DDFS combustion are performed by varying the injection timing of iso-octane (i-C 8H 18) with a pseudo-iso-octane (PC 8H 18) model together with a novel compression heating model to account for the compression heating and expansion cooling effects of the piston motion in an engine cylinder. The PC 8H 18more » model is newly developed to mimic the timing, duration, and cooling effects of the direct injection of i-C 8H 18 onto a premixed background charge of PRF/air/EGR mixture with composition inhomogeneities. It is found that the RCCI combustion exhibits a very high peak heat release rate (HRR) with a short combustion duration due to the predominance of the spontaneous ignition mode of combustion. However, the DDFS combustion has much lower peak HRR and longer combustion duration regardless of the fuel injection timing compared to those of the RCCI combustion, which is primarily attributed to the sequential injection of i-C 8H 18. It is also found that the ignition delay of the DDFS combustion features a non-monotonic behavior with increasing fuel-injection timing due to the different effect of fuel evaporation on the low-, intermediate-, and high-temperature chemistry of the PRF oxidation. The budget and Damköhler number analyses verify that although a mixed combustion mode of deflagration and spontaneous ignition exists during the early phase of the DDFS combustion, the spontaneous ignition becomes predominant during the main combustion, and hence, the spread-out of heat release rate in the DDFS combustion is mainly governed by the direct injection process of i-C 8H 18. Finally, a misfire is observed for the DDFS combustion when the direct injection of i-C 8H 18 occurs during the intermediate-temperature chemistry (ITC) regime between the first- and second-stage ignition. Finally, this is because the temperature drop induced by the direct injection of i-C 8H 18 impedes the main ITC reactions, and hence, the main combustion fails to occur.« less

GRIN: “GRoup versus INdividual physiotherapy following lower limb intra-muscular Botulinum Toxin-A injections for ambulant children with cerebral palsy: an assessor-masked randomised comparison trial”: study protocol

PubMed Central

2014-01-01

Background Cerebral palsy is the most common cause of physical disability in childhood. Spasticity is a significant contributor to the secondary impairments impacting functional performance and participation. The most common lower limb spasticity management is focal intramuscular injections of Botulinum Toxin-Type A accompanied by individually-delivered (one on one) physiotherapy rehabilitation. With increasing emphasis on improving goal-directed functional activity and participation within a family-centred framework, it is timely to explore whether physiotherapy provided in a group could achieve comparable outcomes, encouraging providers to offer flexible models of physiotherapy delivery. This study aims to compare individual to group-based physiotherapy following intramuscular Botulinum Toxin-A injections to the lower limbs for ambulant children with cerebral palsy aged four to fourteen years. Methods/Design An assessor-masked, block randomised comparison trial will be conducted with random allocation to either group-based or individual physiotherapy. A sample size of 30 (15 in each study arm) will be recruited. Both groups will receive six hours of direct therapy following Botulinum Toxin-A injections in either an individual or group format with additional home programme activities (three exercises to be performed three times a week). Study groups will be compared at baseline (T1), then at 10 weeks (T2, efficacy) and 26 weeks (T3, retention) post Botulinum Toxin-A injections. Primary outcomes will be caregiver/s perception of and satisfaction with their child’s occupational performance goals (Canadian Occupational Performance Measure) and quality of gait (Edinburgh Visual Gait Score) with a range of secondary outcomes across domains of the International Classification of Disability, Functioning and Health. Discussion This paper outlines the study protocol including theoretical basis, study hypotheses and outcome measures for this assessor-masked, randomised comparison trial comparing group versus individual models of physiotherapy following intramuscular injections of Botulinum Toxin-A to the lower limbs for ambulant children with cerebral palsy. Trial registration ACTRN12611000454976 PMID:24502231

Krokodile Injectors in Ukraine: Fueling the HIV Epidemic?

PubMed

Booth, Robert E; Davis, Jonathan M; Brewster, John T; Lisovska, Oksana; Dvoryak, Sergey

2016-02-01

This study was designed to assess the characteristics of krokodile injectors, a recent phenomenon in Ukraine, and HIV-related risk factors among people who inject drugs (PWID). In three Ukraine cities, Odessa, Donetsk and Nikolayev, 550 PWID were recruited between December 2012 and October 2013 using modified targeted sampling methods. The sample averaged 31 years of age and they had been injecting for over 12 years. Overall, 39 % tested positive for HIV, including 45 % of krokodile injectors. In the past 30 days, 25 % reported injecting krokodile. Those who injected krokodile injected more frequently (p < 0.001) and they injected more often with others (p = 0.005). Despite knowing their HIV status to be positive, krokodile users did not reduce their injection frequency, indeed, they injected as much as 85 % (p = 0.016) more frequently than those who did not know their HIV status or thought they were negative. This behavior was not seen in non-krokodile using PWID. Although only a small sample of knowledgeable HIV positive krokodile users was available (N = 12), this suggests that krokodile users may disregard their HIV status more so than nonkrokodile users. In spite of widespread knowledge of its harmful physical consequences, a growing number of PWID are turning to injecting krokodile in Ukraine. Given the recency of krokodile use the country, the associated higher frequency of injecting, a propensity to inject more often with others, and what could be a unique level of disregard of HIV among krokodile users, HIV incidence could increase in future years.

Polymeric microchip for the simultaneous determination of anions and cations by hydrodynamic injection using a dual-channel sequential injection microchip electrophoresis system.

PubMed

Gaudry, Adam J; Nai, Yi Heng; Guijt, Rosanne M; Breadmore, Michael C

2014-04-01

A dual-channel sequential injection microchip capillary electrophoresis system with pressure-driven injection is demonstrated for simultaneous separations of anions and cations from a single sample. The poly(methyl methacrylate) (PMMA) microchips feature integral in-plane contactless conductivity detection electrodes. A novel, hydrodynamic "split-injection" method utilizes background electrolyte (BGE) sheathing to gate the sample flows, while control over the injection volume is achieved by balancing hydrodynamic resistances using external hydrodynamic resistors. Injection is realized by a unique flow-through interface, allowing for automated, continuous sampling for sequential injection analysis by microchip electrophoresis. The developed system was very robust, with individual microchips used for up to 2000 analyses with lifetimes limited by irreversible blockages of the microchannels. The unique dual-channel geometry was demonstrated by the simultaneous separation of three cations and three anions in individual microchannels in under 40 s with limits of detection (LODs) ranging from 1.5 to 24 μM. From a series of 100 sequential injections the %RSDs were determined for every fifth run, resulting in %RSDs for migration times that ranged from 0.3 to 0.7 (n = 20) and 2.3 to 4.5 for peak area (n = 20). This system offers low LODs and a high degree of reproducibility and robustness while the hydrodynamic injection eliminates electrokinetic bias during injection, making it attractive for a wide range of rapid, sensitive, and quantitative online analytical applications.

Flow injection on-line displacement/solid phase extraction system coupled with flame atomic absorption spectrometry for selective trace silver determination in water samples.

PubMed

Christou, Chrysoula K; Anthemidis, Aristidis N

2009-04-15

A novel flow injection (FI) on-line displacement solid phase extraction preconcentration and/or separation method coupled with FAAS in order to minimize interference from other metals was developed for trace silver determination. The proposed method involved the on-line formation and subsequently pre-sorption of lead diethyldithiocarbamate (Pb-DDTC) into a column packed with PTFE-turnings. The preconcentration and/or separation of the Ag(I) took place through a displacement reaction between Ag(I) and Pb(II) of the pre-sorbed Pb-DDTC. Finally, the retained analyte was eluted with isobutyl methyl ketone (IBMK) and delivered directly to nebulizer for measuring. Interference from co-existing ions with lower DDTC complex stability in comparison with Pb-DDTC, was eliminated without need for any masking reagent. With 120 s of preconcentration time at a sample flow rate of 7.6 mL min(-1), an enhancement factor of 110 and a detection limit (3s) of 0.2 microg L(-1) were obtained. The precision (RSD, n=10) was 3.1% at the 10 mug L(-1) level. The developed method was successfully applied to trace silver determination in a variety of environmental water samples and certified reference material.

Sample injection and electrophoretic separation on a simple laminated paper based analytical device.

PubMed

Xu, Chunxiu; Zhong, Minghua; Cai, Longfei; Zheng, Qingyu; Zhang, Xiaojun

2016-02-01

We described a strategy to perform multistep operations on a simple laminated paper-based separation device by using electrokinetic flow to manipulate the fluids. A laminated crossed-channel paper-based separation device was fabricated by cutting a filter paper sheet followed by lamination. Multiple function units including sample loading, sample injection, and electrophoretic separation were integrated on a single paper based analytical device for the first time, by applying potential at different reservoirs for sample, sample waste, buffer, and buffer waste. As a proof-of-concept demonstration, mixed sample solution containing carmine and sunset yellow were loaded in the sampling channel, and then injected into separation channel followed by electrophoretic separation, by adjusting the potentials applied at the four terminals of sampling and separation channel. The effects of buffer pH, buffer concentration, channel width, and separation time on resolution of electrophoretic separation were studied. This strategy may be used to perform multistep operations such as reagent dilution, sample injection, mixing, reaction, and separation on a single microfluidic paper based analytical device, which is very attractive for building micro total analysis systems on microfluidic paper based analytical devices. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of ground-water flow in the Madison aquifer using fluorescent dyes injected in Spring Creek and Rapid Creek near Rapid City, South Dakota, 2003-04

USGS Publications Warehouse

Putnam, Larry D.; Long, Andrew J.

2007-01-01

The Madison aquifer, which contains fractures and solution openings in the Madison Limestone, is used extensively for water supplies for the city of Rapid City and other suburban communities in the Rapid City, S. Dak., area. The 48 square-mile study area includes the west-central and southwest parts of Rapid City and the outcrops of the Madison Limestone extending from south of Spring Creek to north of Rapid Creek. Recharge to the Madison Limestone occurs when streams lose flow as they cross the outcrop. The maximum net loss rate for Spring and Rapid Creek loss zones are 21 and 10 cubic feet per second (ft3/s), respectively. During 2003 and 2004, fluorescent dyes were injected in the Spring and Rapid Creek loss zones to estimate approximate locations of preferential flow paths in the Madison aquifer and to measure the response and transit times at wells and springs. Four injections of about 2 kilograms of fluorescein dye were made in the Spring Creek loss zone during 2003 (sites S1, S2, and S3) and 2004 (site S4). Injection at site S1 was made in streamflow just upstream from the loss zone over a 12-hour period when streamflow was about equal to the maximum loss rate. Injections at sites S2, S3, and S4 were made in specific swallow holes located in the Spring Creek loss zone. Injection at site R1 in 2004 of 3.5 kilograms of Rhodamine WT dye was made in streamflow just upstream from the Rapid Creek loss zone over about a 28-hour period. Selected combinations of 27 wells, 6 springs, and 3 stream sites were monitored with discrete samples following the injections. For injections at sites S1-S3, when Spring Creek streamflow was greater than or equal to 20 ft3/s, fluorescein was detected in samples from five wells that were located as much as about 2 miles from the loss zone. Time to first arrival (injection at site S1) ranged from less than 1 to less than 10 days. The maximum fluorescein concentration (injection at site S1) of 120 micrograms per liter (ug/L) at well CO, which is located adjacent to the loss zone, was similar to the concentration in the stream. Fluorescein arrived at well NON (injection at site S1), which is located about 2 miles northeast of the loss zone, within about 1.6 days, and the maximum concentration was 44 ug/L. For injection at site S4, when streamflow was about 12 ft3/s, fluorescein was detected in samples from six wells and time to first arrival ranged from 0.2 to 16 days. Following injection at site S4 in 2004, the length of time that dye remained in the capture zone of well NON, which is located approximately 2 miles from the loss zone, was almost an order of magnitude greater than in 2003. For injection at site R1, Rhodamine WT was detected at well DRU and spring TI-SP with time to first arrival of about 0.5 and 1.1 days and maximum concentrations of 6.2 and 0.91 ug/L, respectively. Well DRU and spring TI-SP are located near the center of the Rapid Creek loss zone where the creek has a large meander. Measurable concentrations were observed for spring TI-SP as many as 109 days after the dye injection. The direction of a conduit flow path in the Spring Creek area was to the northeast with ground-water velocities that ranged from 770 to 6,500 feet per day. In the Rapid Creek loss zone, a conduit flow path east of the loss zone was not evident from the dye injection.

Laboratory modeling and analysis of aircraft-lightning interactions

NASA Technical Reports Server (NTRS)

Turner, C. D.; Trost, T. F.

1982-01-01

Modeling studies of the interaction of a delta wing aircraft with direct lightning strikes were carried out using an approximate scale model of an F-106B. The model, which is three feet in length, is subjected to direct injection of fast current pulses supplied by wires, which simulate the lightning channel and are attached at various locations on the model. Measurements are made of the resulting transient electromagnetic fields using time derivative sensors. The sensor outputs are sampled and digitized by computer. The noise level is reduced by averaging the sensor output from ten input pulses at each sample time. Computer analysis of the measured fields includes Fourier transformation and the computation of transfer functions for the model. Prony analysis is also used to determine the natural frequencies of the model. Comparisons of model natural frequencies extracted by Prony analysis with those for in flight direct strike data usually show lower damping in the in flight case. This is indicative of either a lightning channel with a higher impedance than the wires on the model, only one attachment point, or short streamers instead of a long channel.

Direct mass spectrometry approaches to characterize polyphenol composition of complex samples.

PubMed

Fulcrand, Hélène; Mané, Carine; Preys, Sébastien; Mazerolles, Gérard; Bouchut, Claire; Mazauric, Jean-Paul; Souquet, Jean-Marc; Meudec, Emmanuelle; Li, Yan; Cole, Richard B; Cheynier, Véronique

2008-12-01

Lower molecular weight polyphenols including proanthocyanidin oligomers can be analyzed after HPLC separation on either reversed-phase or normal phase columns. However, these techniques are time consuming and can have poor resolution as polymer chain length and structural diversity increase. The detection of higher molecular weight compounds, as well as the determination of molecular weight distributions, remain major challenges in polyphenol analysis. Approaches based on direct mass spectrometry (MS) analysis that are proposed to help overcome these problems are reviewed. Thus, direct flow injection electrospray ionization mass spectrometry analysis can be used to establish polyphenol fingerprints of complex extracts such as in wine. This technique enabled discrimination of samples on the basis of their phenolic (i.e. anthocyanin, phenolic acid and flavan-3-ol) compositions, but larger oligomers and polymers were poorly detectable. Detection of higher molecular weight proanthocyanidins was also restricted with matrix-assisted laser desorption ionization (MALDI) MS, suggesting that they are difficult to desorb as gas-phase ions. The mass distribution of polymeric fractions could, however, be determined by analyzing the mass distributions of bovine serum albumin/proanthocyanidin complexes using MALDI-TOF-MS.

Stratospheric CCN sampling program

NASA Technical Reports Server (NTRS)

Rogers, C. F.

1981-01-01

When Mt. St. Helens produced several major eruptions in the late spring of 1980, there was a strong interest in the characterization of the cloud condensation nuclei (CCN) activity of the material that was injected into the troposphere and stratosphere. The scientific value of CCN measurements is two fold: CCN counts may be directly applied to calculations of the interaction of the aerosol (enlargement) at atmospherically-realistic relative humidities or supersaturations; and if the chemical constituency of the aerosol can be assumed, the number-versus-critical supersaturation spectrum may be converted into a dry aerosol size spectrum covering a size region not readily measured by other methods. The sampling method is described along with the instrumentation used in the experiments.

Spatial Epidemiology of HIV among Injection Drug Users in Tijuana, Mexico.

PubMed

Brouwer, Kimberly C; Rusch, Melanie L; Weeks, John R; Lozada, Remedios; Vera, Alicia; Magis-Rodríguez, Carlos; Strathdee, Steffanie A

2012-01-01

The northwest border city of Tijuana is Mexico's fifth largest and is experiencing burgeoning drug use and human immunodeficiency virus (HIV) epidemics. Since local geography influences disease risk, we explored the spatial distribution of HIV among injection drug users (IDUs). From 2006-2007, 1056 IDUs were recruited using respondent-driven sampling, and then followed for eighteen months. Participants underwent semi-annual surveys, mapping, and testing for HIV, tuberculosis, and syphilis. Using Average Nearest Neighbor and Getis-Ord Gi* statistics, locations where participants lived, worked, bought and injected drugs were compared with HIV status and environmental and behavioral factors. Median age was thirty-seven years; 85 percent were male. Females had higher HIV prevalence than males (10.2 percent vs. 3.4 percent; p =0.001). HIV cases at baseline ( n =47) most strongly clustered by drug injection sites ( Z -Score -6.173; p < 0.001), with a 16 km 2 hotspot near the Mexico/U.S. border, encompassing the red-light district. Spatial correlates of HIV included syphilis infection, female gender, younger age, increased hours on the street per day, and higher number of injection partners. Almost all HIV seroconverters injected within a 2.5 block radius of each other immediately prior to seroconversion. Only history of syphilis infection and female gender were strongly associated with HIV in the area where incident cases injected. Directional trends suggested a largely static epidemic until July-December 2008, when HIV spread to the southeast, possibly related to intensified violence and policing that spiked in the latter half of 2008. While clustering allows for targeting interventions, the dynamic nature of epidemics suggests the importance of mobile treatment and harm reduction programs.

Symptomatic lumbosacral transitional vertebra: a review of the current literature and clinical outcomes following steroid injection or surgical intervention.

PubMed

Holm, Emil Kongsted; Bünger, Cody; Foldager, Casper Bindzus

2017-01-01

Bertolotti's syndrome (BS) refers to the possible association between the congenital malformation lumbosacral transitional vertebra (LSTV), and low back pain (LBP). Several treatments have been proposed including steroid injections, resections of the LSTV, laminectomy, and lumbar spinal fusion. The aim of this review was to compare the clinical outcomes in previous trials and case reports for these treatments in patients with LBP and LSTV. A PubMed search was conducted. We included English studies of patients diagnosed with LSTV treated with steroid injection, laminectomy, spinal fusion or resection of the transitional articulation. Of 272 articles reviewed 20 articles met the inclusion criteria. Their level of evidence were graded I-V and the clinical outcomes were evaluated. Only 1 study had high evidence level (II). The remainders were case series (level IV). Only 5 studies used validated clinical outcome measures. A total of 79 patients were reported: 31 received treatment with steroid injections, 33 were treated with surgical resection of the LSTV, 8 received lumbar spinal fusion, and 7 cases were treated with laminectomy. Surgical management seems to improve the patient's symptoms, especially patients diagnosed with "far out syndrome" treated with laminectomy. Clinical outcomes were more heterogenetic for patient's treated with steroid injections. The literature regarding BS is sparse and generally with low evidence. Non-surgical management (e.g., steroid injections) and surgical intervention could not directly be compared due to lack of standardization in clinical outcome. Generally, surgical management seems to improve patient's clinical outcome over time, whereas steroid injection only improves the patient's symptoms temporarily. Further studies with larger sample size and higher evidence are warranted for the clinical guidance in the treatment of BS. © The Authors, published by EDP Sciences, 2017.

Symptomatic lumbosacral transitional vertebra: a review of the current literature and clinical outcomes following steroid injection or surgical intervention

PubMed Central

Holm, Emil Kongsted; Bünger, Cody; Foldager, Casper Bindzus

2017-01-01

Bertolotti’s syndrome (BS) refers to the possible association between the congenital malformation lumbosacral transitional vertebra (LSTV), and low back pain (LBP). Several treatments have been proposed including steroid injections, resections of the LSTV, laminectomy, and lumbar spinal fusion. The aim of this review was to compare the clinical outcomes in previous trials and case reports for these treatments in patients with LBP and LSTV. A PubMed search was conducted. We included English studies of patients diagnosed with LSTV treated with steroid injection, laminectomy, spinal fusion or resection of the transitional articulation. Of 272 articles reviewed 20 articles met the inclusion criteria. Their level of evidence were graded I–V and the clinical outcomes were evaluated. Only 1 study had high evidence level (II). The remainders were case series (level IV). Only 5 studies used validated clinical outcome measures. A total of 79 patients were reported: 31 received treatment with steroid injections, 33 were treated with surgical resection of the LSTV, 8 received lumbar spinal fusion, and 7 cases were treated with laminectomy. Surgical management seems to improve the patient’s symptoms, especially patients diagnosed with “far out syndrome” treated with laminectomy. Clinical outcomes were more heterogenetic for patient’s treated with steroid injections. The literature regarding BS is sparse and generally with low evidence. Non-surgical management (e.g., steroid injections) and surgical intervention could not directly be compared due to lack of standardization in clinical outcome. Generally, surgical management seems to improve patient’s clinical outcome over time, whereas steroid injection only improves the patient’s symptoms temporarily. Further studies with larger sample size and higher evidence are warranted for the clinical guidance in the treatment of BS. PMID:29243586

Spatial Epidemiology of HIV among Injection Drug Users in Tijuana, Mexico

PubMed Central

Brouwer, Kimberly C.; Rusch, Melanie L.; Weeks, John R.; Lozada, Remedios; Vera, Alicia; Magis-Rodríguez, Carlos; Strathdee, Steffanie A.

2012-01-01

The northwest border city of Tijuana is Mexico’s fifth largest and is experiencing burgeoning drug use and human immunodeficiency virus (HIV) epidemics. Since local geography influences disease risk, we explored the spatial distribution of HIV among injection drug users (IDUs). From 2006–2007, 1056 IDUs were recruited using respondent-driven sampling, and then followed for eighteen months. Participants underwent semi-annual surveys, mapping, and testing for HIV, tuberculosis, and syphilis. Using Average Nearest Neighbor and Getis-Ord Gi* statistics, locations where participants lived, worked, bought and injected drugs were compared with HIV status and environmental and behavioral factors. Median age was thirty-seven years; 85 percent were male. Females had higher HIV prevalence than males (10.2 percent vs. 3.4 percent; p=0.001). HIV cases at baseline (n=47) most strongly clustered by drug injection sites (Z-Score −6.173; p < 0.001), with a 16 km2 hotspot near the Mexico/U.S. border, encompassing the red-light district. Spatial correlates of HIV included syphilis infection, female gender, younger age, increased hours on the street per day, and higher number of injection partners. Almost all HIV seroconverters injected within a 2.5 block radius of each other immediately prior to seroconversion. Only history of syphilis infection and female gender were strongly associated with HIV in the area where incident cases injected. Directional trends suggested a largely static epidemic until July–December 2008, when HIV spread to the southeast, possibly related to intensified violence and policing that spiked in the latter half of 2008. While clustering allows for targeting interventions, the dynamic nature of epidemics suggests the importance of mobile treatment and harm reduction programs. PMID:23606753

Applications of polyamide/cellulose fiber/wollastonite composites for microcellular injection molding

Treesearch

Herman Winata; Lih-Sheng Turng; Daniel F. Caulfield; Tom Kuster; Rick Spindler; Rod Jacobson

2003-01-01

In this study, a cellulose-fiber-reinforced Polyamide-6 (PA-6) composite, a hybrid composite (PA-6/cellulose/Wollastonite), and the neat PA-6 resin were injection molded into ASTM test–bar samples with conventional and microcellular injection molding. The impact and tensile strengths of molded samples were measured and the Scanning Electron Microscopy (SEM) images were...

Comprehensive particle characterization of modern gasoline and diesel passenger cars at low ambient temperatures

NASA Astrophysics Data System (ADS)

Mathis, Urs; Mohr, Martin; Forss, Anna-Maria

Particle measurements were performed in the exhaust of five light-duty vehicles (Euro-3) at +23, -7, and -20 °C ambient temperatures. The characterization included measurements of particle number, active surface area, number size distribution, and mass size distribution. We investigated two port-injection spark-ignition (PISI) vehicles, a direct-injection spark-ignition (DISI) vehicle, a compressed ignition (CI) vehicle with diesel particle filter (DPF), and a CI vehicle without DPF. To minimize sampling effects, particles were directly sampled from the tailpipe with a novel porous tube diluter at controlled sampling parameters. The diluted exhaust was split into two branches to measure either all or only non-volatile particles. Effect of ambient temperature was investigated on particle emission for cold and warmed-up engine. For the gasoline vehicles and the CI vehicle with DPF, the main portion of particle emission was found in the first minutes of the driving cycle at cold engine start. The particle emission of the CI vehicle without DPF was hardly affected by cold engine start. For the PISI vehicles, particle number emissions were superproportionally increased in the diameter size range from 0.1 to 0.3 μm during cold start at low ambient temperature. Based on the particle mass size distribution, the DPF removed smaller particles ( dp<0.5μm) more efficiently than larger particles ( dp>0.5μm). No significant effect of ambient temperature was observed when the engine was warmed up. Peak emission of volatile nanoparticles only took place at specific conditions and was poorly repeatable. Nucleation of particles was predominately observed during or after strong acceleration at high speed and during regeneration of the DPF.

Dual-phase gas-permeation flow-injection thermometric analysis for the determination of carbon dioxide.

PubMed

Liu, S J; Tubino, M

1998-11-01

A flow-injection configuration based on a dual-phase gas-permeation system from a liquid donor to a gas acceptor stream with a thermistor flow-through detector is proposed for the direct analysis of the gas in the acceptor. This system was applied for the determination of carbon dioxide (in the form of carbonate) using the following chemical reaction: CO(2)(g)+2NH(3)(g)+H(2)O(g)=(NH(4))(2)CO(3)(s), with a linear response from 1x10(-3) to 50x10(-3) mol l(-1) of CO(3)(2-). Carbon dioxide was produced in the liquid donor and permeated into the gaseous acceptor stream of air/water vapor. The detection limit is 1x10(-3) mol l(-1) of carbonate, and a sampling frequency of 60 h(-1) is achieved with a relative standard deviation of 4.1% for replicate injections. The dual-phase gas-permeation flow-injection manifold, along with the membrane and phase separations, as well as the chemical reaction, provides enhanced selectivity when compared with the system employing a liquid acceptor stream, as serious interferents in this system, for instance, acetate and formate, among others, do not interfere in the proposed system.

Control of spontaneous combustion of coal in goaf at high geotemperatureby injecting liquid carbon dioxide: inertand cooling characteristics of coal

NASA Astrophysics Data System (ADS)

Liu, Zhenling; Wen, Hu; Yu, Zhijin; Wang, Chao; Ma, Li

2018-02-01

The spontaneous combustion of coal in goaf at high geo temperatures is threatening safety production in coalmine. The TG-DSC is employed to study the variation of mass and energy at 4 atmospheres (mixed gases of N2, O2 and CO2) and heating rates (10°C/min) during oxidation of coal samples. The apparent activation energy and pre-exponential factor of coal oxidation decrease rapidly with increasing theCO2 concentration. Furthermore, its reaction rate is slow, its heat released reduces. Based on the conditions of 1301 face in the Longgucoalmine, a three-dimensional geometry model is developed to simulate the distributions stream field and temperature field and the variation characteristics ofCO2 concentration field after injecting liquidCO2. The results indicate that oxygen reached to depths of˜120m in goaf, 100m in the side of inlet air, and 10m in the side of outlet air before injecting liquidCO2. After injecting liquidCO2for 28.8min, the width of oxidation and heat accumulation zone is shortened by 20m, and the distance is 80m in the side of working face and 40˜60m in goafin the direction of dip affected by temperature.

An Efficient Approach for Mars Sample Return Using Emerging Commercial Capabilities

NASA Technical Reports Server (NTRS)

Gonzales, Andrew A.; Stoker, Carol R.

2016-01-01

Mars Sample Return is the highest priority science mission for the next decade as recommended by the 2011 Decadal Survey of Planetary Science. This article presents the results of a feasibility study for a Mars Sample Return mission that efficiently uses emerging commercial capabilities expected to be available in the near future. The motivation of our study was the recognition that emerging commercial capabilities might be used to perform Mars Sample Return with an Earth-direct architecture, and that this may offer a desirable simpler and lower cost approach. The objective of the study was to determine whether these capabilities can be used to optimize the number of mission systems and launches required to return the samples, with the goal of achieving the desired simplicity. All of the major element required for the Mars Sample Return mission are described. Mission system elements were analyzed with either direct techniques or by using parametric mass estimating relationships. The analysis shows the feasibility of a complete and closed Mars Sample Return mission design based on the following scenario: A SpaceX Falcon Heavy launch vehicle places a modified version of a SpaceX Dragon capsule, referred to as "Red Dragon", onto a Trans Mars Injection trajectory. The capsule carries all the hardware needed to return to Earth Orbit samples collected by a prior mission, such as the planned NASA Mars 2020 sample collection rover. The payload includes a fully fueled Mars Ascent Vehicle; a fueled Earth Return Vehicle, support equipment, and a mechanism to transfer samples from the sample cache system onboard the rover to the Earth Return Vehicle. The Red Dragon descends to land on the surface of Mars using Supersonic Retropropulsion. After collected samples are transferred to the Earth Return Vehicle, the single-stage Mars Ascent Vehicle launches the Earth Return Vehicle from the surface of Mars to a Mars phasing orbit. After a brief phasing period, the Earth Return Vehicle performs a Trans Earth Injection burn. Once near Earth, the Earth Return Vehicle performs Earth and lunar swing-bys and is placed into a Lunar Trailing Orbit - an Earth orbit, at lunar distance. A retrieval mission then performs a rendezvous with the Earth Return Vehicle, retrieves the sample container, and breaks the chain of contact with Mars by transferring the sample into a sterile and secure container. With the sample contained, the retrieving spacecraft makes a controlled Earth re-entry preventing any unintended release of Martian materials into the Earth's biosphere. The mission can start in any one of three Earth to Mars launch opportunities, beginning in 2022.

Computational Fluid Dynamics Analysis of the Venturi Dustiness Tester

PubMed Central

Dubey, Prahit; Ghia, Urmila; Turkevich, Leonid A.

2017-01-01

Dustiness quantifies the propensity of a finely divided solid to be aerosolized by a prescribed mechanical stimulus. Dustiness is relevant wherever powders are mixed, transferred or handled, and is important in the control of hazardous exposures and the prevention of dust explosions and product loss. Limited quantities of active pharmaceutical powders available for testing led to the development (at University of North Carolina) of a Venturi-driven dustiness tester. The powder is turbulently injected at high speed (Re ~ 2 × 104) into a glass chamber; the aerosol is then gently sampled (Re ~ 2 × 103) through two filters located at the top of the chamber; the dustiness index is the ratio of sampled to injected mass of powder. Injection is activated by suction at an Extraction Port at the top of the chamber; loss of powder during injection compromises the sampled dustiness. The present work analyzes the flow inside the Venturi Dustiness Tester, using an Unsteady Reynolds-Averaged Navier-Stokes formulation with the k-ω Shear Stress Transport turbulence model. The simulation considers single-phase flow, valid for small particles (Stokes number Stk <1). Results show that ~ 24% of fluid-tracers escape the tester before the Sampling Phase begins. Dispersion of the powder during the Injection Phase results in a uniform aerosol inside the tester, even for inhomogeneous injections, satisfying a necessary condition for the accurate evaluation of dustiness. Simulations are also performed under the conditions of reduced Extraction-Port flow; results confirm the importance of high Extraction-Port flow rate (standard operation) for uniform distribution of fluid tracers. Simulations are also performed under the conditions of delayed powder injection; results show that a uniform aerosol is still achieved provided 0.5 s elapses between powder injection and sampling. PMID:28638167

Modulating the Biologic Activity of Mesenteric Lymph after Traumatic Shock Decreases Systemic Inflammation and End Organ Injury.

PubMed

Langness, Simone; Costantini, Todd W; Morishita, Koji; Eliceiri, Brian P; Coimbra, Raul

2016-01-01

Trauma/hemorrhagic shock (T/HS) causes the release of pro-inflammatory mediators into the mesenteric lymph (ML), triggering a systemic inflammatory response and acute lung injury (ALI). Direct and pharmacologic vagal nerve stimulation prevents gut barrier failure and alters the biologic activity of ML after injury. We hypothesize that treatment with a pharmacologic vagal agonist after T/HS would attenuate the biologic activity of ML and prevent ALI. ML was collected from male Sprague-Dawley rats after T/HS, trauma-sham shock (T/SS) or T/HS with administration of the pharmacologic vagal agonist CPSI-121. ML samples from each experimental group were injected into naïve mice to assess biologic activity. Blood samples were analyzed for changes in STAT3 phosphorylation (pSTAT3). Lung injury was characterized by histology, permeability and immune cell recruitment. T/HS lymph injected in naïve mice caused a systemic inflammatory response characterized by hypotension and increased circulating monocyte pSTAT3 activity. Injection of T/HS lymph also resulted in ALI, confirmed by histology, lung permeability and increased recruitment of pulmonary macrophages and neutrophils to lung parenchyma. CPSI-121 attenuated T/HS lymph-induced systemic inflammatory response and ALI with stable hemodynamics and similar monocyte pSTAT3 levels, lung histology, lung permeability and lung immune cell recruitment compared to animals injected with lymph from T/SS. Treatment with CPSI-121 after T/HS attenuated the biologic activity of the ML and decreased ALI. Given the superior clinical feasibility of utilizing a pharmacologic approach to vagal nerve stimulation, CPSI-121 is a potential treatment strategy to limit end organ dysfunction after injury.

Simultaneous determination of Cr(III) and Cr(VI) in tannery wastewater using low pressure ion chromatography combined with flow injection spectrophotometry

NASA Astrophysics Data System (ADS)

Chen, Shujuan; Zhang, Xinshen; Yu, Lingyun; Wang, Li; Li, Hui

2012-03-01

Trivalent and hexavalent chromium have been successfully separated and determined using low pressure ion chromatography combined with flow injection spectrophotometric analysis (LPIC-FIA). A column packed with crosslinking starch microspheres was used for on-line separation of Cr(III) from Cr(VI) in a flow-injection system because of its absorptive effect on Cr(III). To determine the concentration of Cr(III) and Cr(VI) in samples, we used 3.0 mmol/L nitric acid to elute adsorbed Cr(III) from the column and then used ceric sulfate-sulfuric acid as oxidant to convert all Cr(III) into Cr(VI). Then, Cr(VI) directly came from the samples and Cr(VI) came from Cr(III) successively formed a amaranthine complex with diphenycarbazide and the complex shows a maximum absorption at 530 nm. Analytical parameters including the concentration of eluent and oxidant solution, oxidizing temperature, length of oxidizing reaction coil, reaction coil and injection coil, interfering effects, etc., were optimized. The limit of detection was 1.25 μg/L for Cr(VI) and 3.76 μg/L for Cr(III). The linear relationship between absorption with the concentration of Cr(VI) and Cr(III) was 0.001-1.000 mg/L and 0.030-1.000 mg/L with correlation coefficients of 0.9995 and 0.9994, respectively. The relative standard deviation of Cr(VI) and Cr(III) was 1.21% and 1.66%, respectively (n = 10). Major cations and anions did not show any interference. We validated this method through certified reference materials and through measuring the recovery in tannery wastewater.

Rapid movement of wastewater from on-site disposal systems into surface waters in the lower Florida Keys

USGS Publications Warehouse

Paul, John H.; McLaughlin, Molly R.; Griffin, Dale W.; Lipp, Erin K.; Stokes, Rodger; Rose, Joan B.

2000-01-01

Viral tracer studies have been used previously to study the potential for wastewater contamination of surface marine waters in the Upper and Middle Florida Keys. Two bacteriophages, the marine bacteriophage φHSIC and the Salmonella phage PRD1, were used as tracers in injection well and septic tank studies in Saddlebunch Keys of the Lower Florida Keys and in septic tank studies in Boot Key Harbor, Marathon, of the Middle Keys. In Boot Key Harbor, both phages were detected in a canal adjacent to the seeded septic tank within 3 h 15 min of the end of the seed period. The tracer was then detected at all sampling sites in Boot Key Harbor, including one on the opposite side of U. S. Highway 1 in Florida Bay, and at an Atlantic Ocean beach outside Boot Key Harbor. Rates of migration based on first appearance of the phage ranged from 1.7 to 57.5 m h-1. In Saddlebunch Keys, φHSIC and PRD1 were used to seed a residential septic tank and a commercial injection well. The septic tank tracer was not found in any surface water samples. The injection well tracer was first detected at a site most distant from the seed site, a channel that connected Sugarloaf Sound with the Atlantic Ocean. The rate of tracer migration from the injection well to this channel ranged from 66.8 to 141 m h-1. Both tracer studies showed a rapid movement of wastewater from on-site sewage treatment and disposal systems in a southeasterly direction toward the reef tract and Atlantic Ocean, with preferential movement through tidal channels. These studies indicate that wastewater disposal systems currently in widespread use in the Florida Keys can rapidly contaminate the marine environment.

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

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

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

2005-01-01

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

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

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

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

2010-07-13

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

Field-based stable isotope analysis of carbon dioxide by mid-infrared laser spectroscopy for carbon capture and storage monitoring.

PubMed

van Geldern, Robert; Nowak, Martin E; Zimmer, Martin; Szizybalski, Alexandra; Myrttinen, Anssi; Barth, Johannes A C; Jost, Hans-Jürg

2014-12-16

A newly developed isotope ratio laser spectrometer for CO2 analyses has been tested during a tracer experiment at the Ketzin pilot site (northern Germany) for CO2 storage. For the experiment, 500 tons of CO2 from a natural CO2 reservoir was injected in supercritical state into the reservoir. The carbon stable isotope value (δ(13)C) of injected CO2 was significantly different from background values. In order to observe the breakthrough of the isotope tracer continuously, the new instruments were connected to a stainless steel riser tube that was installed in an observation well. The laser instrument is based on tunable laser direct absorption in the mid-infrared. The instrument recorded a continuous 10 day carbon stable isotope data set with 30 min resolution directly on-site in a field-based laboratory container during a tracer experiment. To test the instruments performance and accuracy the monitoring campaign was accompanied by daily CO2 sampling for laboratory analyses with isotope ratio mass spectrometry (IRMS). The carbon stable isotope ratios measured by conventional IRMS technique and by the new mid-infrared laser spectrometer agree remarkably well within analytical precision. This proves the capability of the new mid-infrared direct absorption technique to measure high precision and accurate real-time stable isotope data directly in the field. The laser spectroscopy data revealed for the first time a prior to this experiment unknown, intensive dynamic with fast changing δ(13)C values. The arrival pattern of the tracer suggest that the observed fluctuations were probably caused by migration along separate and distinct preferential flow paths between injection well and observation well. The short-term variances as observed in this study might have been missed during previous works that applied laboratory-based IRMS analysis. The new technique could contribute to a better tracing of the migration of the underground CO2 plume and help to ensure the long-term integrity of the reservoir.

Enhancing concentration and mass sensitivities for liquid chromatography trace analysis of clopyralid in drinking water.

PubMed

Gu, Binghe; Meldrum, Brian; McCabe, Terry; Phillips, Scott

2012-01-01

A theoretical treatment was developed and validated that relates analyte concentration and mass sensitivities to injection volume, retention factor, particle diameter, column length, column inner diameter and detection wavelength in liquid chromatography, and sample volume and extracted volume in solid-phase extraction (SPE). The principles were applied to improve sensitivity for trace analysis of clopyralid in drinking water. It was demonstrated that a concentration limit of detection of 0.02 ppb (μg/L) for clopyralid could be achieved with the use of simple UV detection and 100 mL of a spiked drinking water sample. This enabled reliable quantitation of clopyralid at the targeted 0.1 ppb level. Using a buffered solution as the elution solvent (potassium acetate buffer, pH 4.5, containing 10% of methanol) in the SPE procedures was found superior to using 100% methanol, as it provided better extraction recovery (70-90%) and precision (5% for a concentration at 0.1 ppb level). In addition, the eluted sample was in a weaker solvent than the mobile phase, permitting the direct injection of the extracted sample, which enabled a faster cycle time of the overall analysis. Excluding the preparation of calibration standards, the analysis of a single sample, including acidification, extraction, elution and LC run, could be completed in 1 h. The method was used successfully for the determination of clopyralid in over 200 clopyralid monoethanolamine-fortified drinking water samples, which were treated with various water treatment resins. Copyright © 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim.

Simplifying and expanding the screening for peptides <2 kDa by direct urine injection, liquid chromatography, and ion mobility mass spectrometry.

PubMed

Thomas, Andreas; Görgens, Christian; Guddat, Sven; Thieme, Detlef; Dellanna, Frank; Schänzer, Wilhelm; Thevis, Mario

2016-01-01

The analysis of low-molecular-mass peptides in doping controls has become a mandatory aspect in sports drug testing and, thus, the number of samples that has to be tested for these analytes has been steadily increasing. Several peptides <2 kDa with performance-enhancing properties are covered by the list of prohibited substances of the World Anti-Doping Agency including Desmopressin, LH-RH, Buserelin, Triptorelin, Leuprolide, GHRP-1, GHRP-2, GHRP-3, GHRP-4, GHRP-5,GHRP-6, Alexamorelin, Ipamorelin, Hexarelin, ARA-290, AOD-9604, TB-500 and Anamorelin. With the presented method employing direct urine injection into a liquid chromatograph followed by ion-mobility time-of-flight mass spectrometry, a facile, specific and sensitive assay for the aforementioned peptidic compounds is provided. The accomplished sensitivity allows for limits of detection between 50 and 500 pg/mL and thus covers the minimum required performance level of 2 ng/mL accordingly. The method is precise (imprecision <20%) and linear in the estimated working range between 0 and 10 ng/mL. The stability of the peptides in urine was tested, and -20°C was found to be the appropriate storage temperature for sports drug testing. Finally, proof-of-concept was shown by analysing elimination study urine samples collected from individuals having administered GHRP-6, GHRP-2, or LHRH. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimizing direct amplification of forensic commercial kits for STR determination.

PubMed

Caputo, M; Bobillo, M C; Sala, A; Corach, D

2017-04-01

Direct DNA amplification in forensic genotyping reduces analytical time when large sample sets are being analyzed. The amplification success depends mainly upon two factors: on one hand, the PCR chemistry and, on the other, the type of solid substrate where the samples are deposited. We developed a workflow strategy aiming to optimize times and cost when starting from blood samples spotted onto diverse absorbent substrates. A set of 770 blood samples spotted onto Blood cards, Whatman ® 3 MM paper, FTA™ Classic cards, and Whatman ® Grade 1 was analyzed by a unified working strategy including a low-cost pre-treatment, a PCR amplification volume scale-down, and the use of the 3500 Genetic Analyzer as the analytical platform. Samples were analyzed using three different commercial multiplex STR direct amplification kits. The efficiency of the strategy was evidenced by a higher percentage of high-quality profiles obtained (over 94%), a reduced number of re-injections (average 3.2%), and a reduced amplification failure rate (lower than 5%). Average peak height ratio among different commercial kits was 0.91, and the intra-locus balance showed values ranging from 0.92 to 0.94. A comparison with previously reported results was performed demonstrating the efficiency of the proposed modifications. The protocol described herein showed high performance, producing optimal quality profiles, and being both time and cost effective. Copyright © 2017 Elsevier Ltd and Faculty of Forensic and Legal Medicine. All rights reserved.

Fluidized bed injection assembly for coal gasification

DOEpatents

Cherish, Peter; Salvador, Louis A.

1981-01-01

A coaxial feed system for fluidized bed coal gasification processes including an inner tube for injecting particulate combustibles into a transport gas, an inner annulus about the inner tube for injecting an oxidizing gas, and an outer annulus about the inner annulus for transporting a fluidizing and cooling gas. The combustibles and oxidizing gas are discharged vertically upward directly into the combustion jet, and the fluidizing and cooling gas is discharged in a downward radial direction into the bed below the combustion jet.

Fuel-Air Injection Effects on Combustion in Cavity-Based Flameholders in a Supersonic Flow

DTIC Science & Technology

2005-03-01

both fuel and air provided additional capability to tune the cavity such that a more stable decentralized flame results. The addition of air...Mark Gruber of AFRL/PRAS and Mr. Mark Hsu of Innovative Scientific Solutions Inc. for both the support and latitude provided to me in this endeavor...addition of direct air injection to cavity combustion. Direct injection of both fuel and air provided additional capability to tune the cavity such that a

Push-through direct injection NMR: an optimized automation method applied to metabolomics

EPA Science Inventory

There is a pressing need to increase the throughput of NMR analysis in fields such as metabolomics and drug discovery. Direct injection (DI) NMR automation is recognized to have the potential to meet this need due to its suitability for integration with the 96-well plate format. ...

The active and passive sampling of benzene, toluene, ethyl benzene and xylenes compounds using the inside needle capillary adsorption trap device.

PubMed

Shojania, S; Oleschuk, R D; McComb, M E; Gesser, H D; Chow, A

1999-08-23

A new and simple method of solventless extraction of volatile organic compounds (VOCs) from air is presented. The sampling device has an adsorbing carbon coating on the interior surface of a hollow needle, and is called the inside needle capillary adsorption trap (INCAT). This paper describes a study of the reproducibility in the preparation and sampling of the INCAT device. In addition, this paper examines the effects of sample volume in active sampling and exposure time in passive sampling on the analyte adsorption. Analysis was achieved by sampling the air from an environmental chamber doped with benzene, toluene, ethyl benzene and xylenes (BTEX) compounds. Initial rates of adsorption were found to vary among the different compounds, but ranged from 0.0099 to 0.016 nmol h(-1) for passive sampling and from 2.2 to 10 nmol h(-1) for active sampling. Analysis was done by thermal desorption of the adsorbed compounds directly into a gas chromatograph injection port. Quantification of the analysis was done by comparison to actively sampled activated carbon solid phase extraction (SPE) measurements.

Confirming therapeutic target of protopine using immobilized β2 -adrenoceptor coupled with site-directed molecular docking and the target-drug interaction by frontal analysis and injection amount-dependent method.

PubMed

Liu, Guangxin; Wang, Pei; Li, Chan; Wang, Jing; Sun, Zhenyu; Zhao, Xinfeng; Zheng, Xiaohui

2017-07-01

Drug-protein interaction analysis is pregnant in designing new leads during drug discovery. We prepared the stationary phase containing immobilized β 2 -adrenoceptor (β 2 -AR) by linkage of the receptor on macroporous silica gel surface through N,N'-carbonyldiimidazole method. The stationary phase was applied in identifying antiasthmatic target of protopine guided by the prediction of site-directed molecular docking. Subsequent application of immobilized β 2 -AR in exploring the binding of protopine to the receptor was realized by frontal analysis and injection amount-dependent method. The association constants of protopine to β 2 -AR by the 2 methods were (1.00 ± 0.06) × 10 5 M -1 and (1.52 ± 0.14) × 10 4 M -1 . The numbers of binding sites were (1.23 ± 0.07) × 10 -7 M and (9.09 ± 0.06) × 10 -7 M, respectively. These results indicated that β 2 -AR is the specific target for therapeutic action of protopine in vivo. The target-drug binding occurred on Ser 169 in crystal structure of the receptor. Compared with frontal analysis, injection amount-dependent method is advantageous to drug saving, improvement of sampling efficiency, and performing speed. It has grave potential in high-throughput drug-receptor interaction analysis. Copyright © 2017 John Wiley & Sons, Ltd.

Toward a simple, repeatable, non-destructive approach to measuring stable-isotope ratios of water within tree stems

NASA Astrophysics Data System (ADS)

Raulerson, S.; Volkmann, T.; Pangle, L. A.

2017-12-01

Traditional methodologies for measuring ratios of stable isotopes within the xylem water of trees involve destructive coring of the stem. A recent approach involves permanently installed probes within the stem, and an on-site assembly of pumps, switching valves, gas lines, and climate-controlled structure for field deployment of a laser spectrometer. The former method limits the possible temporal resolution of sampling, and sample size, while the latter may not be feasible for many research groups. We present results from initial laboratory efforts towards developing a non-destructive, temporally-resolved technique for measuring stable isotope ratios within the xylem flow of trees. Researchers have used direct liquid-vapor equilibration as a method to measure isotope ratios of the water in soil pores. Typically, this is done by placing soil samples in a fixed container, and allowing the liquid water within the soil to come into isotopic equilibrium with the headspace of the container. Water can also be removed via cryogenic distillation or azeotropic distillation, with the resulting liquid tested for isotope ratios. Alternatively, the isotope ratios of the water vapor can be directly measured using a laser-based water vapor isotope analyzer. Well-established fractionation factors and the isotope ratios in the vapor phase are then used to calculate the isotope ratios in the liquid phase. We propose a setup which would install a single, removable chamber onto a tree, where vapor samples could non-destructively and repeatedly be taken. These vapor samples will be injected into a laser-based isotope analyzer by a recirculating gas conveyance system. A major part of what is presented here is in the procedure of taking vapor samples at 100% relative humidity, appropriately diluting them with completely dry N2 calibration gas, and injecting them into the gas conveyance system without inducing fractionation in the process. This methodology will be helpful in making temporally resolved measurements of the stable isotopes in xylem water, using a setup that can be easily repeated by other research groups. The method is anticipated to find broad application in ecohydrological analyses, and in tracer studies aimed at quantifying age distributions of soil water extracted by plant roots.

Coupling Microdialysis Sampling to Microchip Electrophoresis in a Reversibly Sealed Device

PubMed Central

Mecker, Laura C.; Martin, R. Scott

2007-01-01

In this paper, we describe the fabrication and characterization of a reversibly sealed microchip device that is used to couple microdialysis sampling to microchip electrophoresis. The ability to interface microdialysis sampling and microchip electrophoresis in a device that is amenable to reversible sealing is advantageous from a repeated use standpoint. Commercially available tubing coming from the microdialysis probe is directly inserted into the chip and flow from the probe is interfaced to the electrophoresis portion of the device through integrated pneumatic valves. Fluorescence detection was used to characterize the poly(dimethylsiloxane)-based device in terms of injection reproducibility. It was found that the entire system (microdialysis probe and microchip device) has a concentration response lag time of 170 sec. Microdialysis sampling followed by an electrophoretic separation of amino acids derivatized with naphthalene-2,3-dicarboxaldehyde/cyanide was also demonstrated. PMID:18836517

Correlative multiple porosimetries for reservoir sandstones with adoption of a new reference-sample-guided computed-tomographic method.

PubMed

Jin, Jae Hwa; Kim, Junho; Lee, Jeong-Yil; Oh, Young Min

2016-07-22

One of the main interests in petroleum geology and reservoir engineering is to quantify the porosity of reservoir beds as accurately as possible. A variety of direct measurements, including methods of mercury intrusion, helium injection and petrographic image analysis, have been developed; however, their application frequently yields equivocal results because these methods are different in theoretical bases, means of measurement, and causes of measurement errors. Here, we present a set of porosities measured in Berea Sandstone samples by the multiple methods, in particular with adoption of a new method using computed tomography and reference samples. The multiple porosimetric data show a marked correlativeness among different methods, suggesting that these methods are compatible with each other. The new method of reference-sample-guided computed tomography is more effective than the previous methods when the accompanied merits such as experimental conveniences are taken into account.

Correlative multiple porosimetries for reservoir sandstones with adoption of a new reference-sample-guided computed-tomographic method

PubMed Central

Jin, Jae Hwa; Kim, Junho; Lee, Jeong-Yil; Oh, Young Min

2016-01-01

One of the main interests in petroleum geology and reservoir engineering is to quantify the porosity of reservoir beds as accurately as possible. A variety of direct measurements, including methods of mercury intrusion, helium injection and petrographic image analysis, have been developed; however, their application frequently yields equivocal results because these methods are different in theoretical bases, means of measurement, and causes of measurement errors. Here, we present a set of porosities measured in Berea Sandstone samples by the multiple methods, in particular with adoption of a new method using computed tomography and reference samples. The multiple porosimetric data show a marked correlativeness among different methods, suggesting that these methods are compatible with each other. The new method of reference-sample-guided computed tomography is more effective than the previous methods when the accompanied merits such as experimental conveniences are taken into account. PMID:27445105

Determination of As(III) and total inorganic As in water samples using an on-line solid phase extraction and flow injection hydride generation atomic absorption spectrometry.

PubMed

Sigrist, Mirna; Albertengo, Antonela; Beldoménico, Horacio; Tudino, Mabel

2011-04-15

A simple and robust on-line sequential injection system based on solid phase extraction (SPE) coupled to a flow injection hydride generation atomic absorption spectrometer (FI-HGAAS) with a heated quartz tube atomizer (QTA) was developed and optimized for the determination of As(III) in groundwater without any kind of sample pretreatment. The method was based on the selective retention of inorganic As(V) that was carried out by passing the filtered original sample through a cartridge containing a chloride-form strong anion exchanger. Thus the most toxic form, inorganic As(III), was determined fast and directly by AsH(3) generation using 3.5 mol L(-1) HCl as carrier solution and 0.35% (m/v) NaBH(4) in 0.025% NaOH as the reductant. Since the uptake of As(V) should be interfered by several anions of natural occurrence in waters, the effect of Cl(-), SO(4)(2-), NO(3)(-), HPO(4)(2-), HCO(3)(-) on retention was evaluated and discussed. The total soluble inorganic arsenic concentration was determined on aliquots of filtered samples acidified with concentrated HCl and pre-reduced with 5% KI-5% C(6)H(8)O(6) solution. The concentration of As(V) was calculated by difference between the total soluble inorganic arsenic and As(III) concentrations. Detection limits (LODs) of 0.5 μg L(-1) and 0.6 μg L(-1) for As(III) and inorganic total As, respectively, were obtained for a 500 μL sample volume. The obtained limits of detection allowed testing the water quality according to the national and international regulations. The analytical recovery for water samples spiked with As(III) ranged between 98% and 106%. The sampling throughput for As(III) determination was 60 samplesh(-1). The device for groundwater sampling was especially designed for the authors. Metallic components were avoided and the contact between the sample and the atmospheric oxygen was carried to a minimum. On-field arsenic species separation was performed through the employ of a serial connection of membrane filters and anion-exchange cartridges. Advantages derived from this approach were evaluated. HPLC-ICPMS was employed to study the consistency of the analytical results. Copyright © 2011 Elsevier B.V. All rights reserved.

Sonographically guided deep plantar fascia injections: where does the injectate go?

PubMed

Maida, Eugene; Presley, James C; Murthy, Naveen; Pawlina, Wojciech; Smith, Jay

2013-08-01

To determine the distribution of sonographically guided deep plantar fascia injections in an unembalmed cadaveric model. A single experienced operator completed 10 sonographically guided deep plantar fascia injections in 10 unembalmed cadaveric specimens (5 right and 5 left) obtained from 6 donors (2 male and 4 female) aged 49 to 95 years (mean, 77.5 years) with a mean body mass index of 23.2 kg/m(2) (range, 18.4-26.3 kg/m(2)). A 12-3-MHz linear array transducer was used to direct a 22-gauge, 38-mm stainless steel needle deep to the plantar fascia at the anterior aspect of the calcaneus using an in-plane, medial-to-lateral approach. In each case, 1.5 mL of 50% diluted colored latex was injected deep to the plantar fascia. After a minimum of 72 hours, study coinvestigators dissected each specimen to assess injectate placement. All 10 injections accurately placed latex adjacent to the deep side of the plantar fascia at the anterior calcaneus. However, the flexor digitorum brevis (FDB) origin from the plantar fascia variably limited direct latex contact with the plantar fascia, and small amounts of latex interdigitated with the FDB origin in 90% (9 of 10). In all 10 specimens, latex also covered the traversing first branch of the lateral plantar nerve (FBLPN, ie, Baxter nerve) between the FDB and quadratus plantae muscles. No latex was found in the plantar fat pad or plantar fascia in any specimen. Sonographically guided deep plantar fascia injections reliably deliver latex deep to the plantar fascia while avoiding intrafascial injection. However, the extent of direct plantar fascia contact is variable due to the intervening FDB. On the contrary, the traversing FBLPN is reliably covered by the injection. Deep plantar fascia injections may have a role in the management of refractory plantar fasciitis, particularly following failed superficial perifascial or intrafascial injections, in cases of preferential deep plantar fascia involvement, or when entrapment/irritation of the distal FBLPN is suspected.

Optical gain in 1.3-μm electrically driven dilute nitride VCSOAs

PubMed Central

2014-01-01

We report the observation of room-temperature optical gain at 1.3 μm in electrically driven dilute nitride vertical cavity semiconductor optical amplifiers. The gain is calculated with respect to injected power for samples with and without a confinement aperture. At lower injected powers, a gain of almost 10 dB is observed in both samples. At injection powers over 5 nW, the gain is observed to decrease. For nearly all investigated power levels, the sample with confinement aperture gives slightly higher gain. PMID:24417791

Comparison of intraosseous and infiltration injections for venous lidocaine blood concentrations and heart rate changes after injection of 2% lidocaine with 1:100,000 epinephrine.

PubMed

Wood, Mark; Reader, Al; Nusstein, John; Beck, Mike; Padgett, David; Weaver, Joel

2005-06-01

The purpose of this prospective, randomized study was to compare the venous blood levels of lidocaine and heart rate changes after intraosseous and infiltration injections of 1.8 ml of 2% lidocaine with 1:100,000 epinephrine. Using a crossover design, 20 subjects randomly received an intraosseous and infiltration injection at two separate appointments. The heart rate was measured using a pulse oximeter. Venous blood samples were collected before the injections and at 2, 5, 10, 15, 20, 25, 30, 45, and 60 min after the injections. The blinded plasma samples were analyzed for lidocaine concentrations using high-performance liquid chromatography (HPLC). The intraosseous injection resulted in a statistically significant increase in heart rate, when compared to the infiltration injection, during solution deposition and for 2 min after the injection. The plasma levels of lidocaine were not statistically different for maxillary anterior intraosseous and infiltration injections when using 1.8 ml of 2% lidocaine with 1:100,000 epinephrine.

Development of a split-flow system for high precision variable sample introduction in supercritical fluid chromatography.

PubMed

Sakai, Miho; Hayakawa, Yoshihiro; Funada, Yasuhiro; Ando, Takashi; Fukusaki, Eiichiro; Bamba, Takeshi

2017-09-15

In this study, we propose a novel variable sample injection system based on full-loop injection, named the split-flow sample introduction system, for application in supercritical fluid chromatography (SFC). In this system, the mobile phase is split by the differential pressure between two back pressure regulators (BPRs) after full-loop injection suitable for SFC, and this differential pressure determines the introduction rate. Nine compounds with a wide range of characteristics were introduced with high reproducibility and universality, confirming that a robust variable sample injection system was achieved. We also investigated the control factors of our proposed system. Sample introduction was controlled by the ratio between the column-side pressure drops in splitless and split flow, ΔP columnsideinsplitless and ΔP columnsideinsplit , respectively, where ΔP columnsideinsplitless is related to the mobile phase flow rate and composition and the column resistance. When all other conditions are kept constant, increasing the make-up flow induces an additional pressure drop on the column side of the system, which leads to a reduced column-side flow rate, and hence decreased the amount of sample injected, even when the net pressure drop on the column side remains the same. Thus, sample introduction could be highly controlled at low sample introduction rate, regardless of the introduction conditions. This feature is advantageous because, as a control factor, the solvent in the make-up pump is independent of the column-side pressure drop. Copyright © 2017. Published by Elsevier B.V.

Determination of nitrite and nitrate in water samples by an automated hydrodynamic sequential injection method.

PubMed

Somnam, Sarawut; Jakmunee, Jaroon; Grudpan, Kate; Lenghor, Narong; Motomizu, Shoji

2008-12-01

An automated hydrodynamic sequential injection (HSI) system with spectrophotometric detection was developed. Thanks to the hydrodynamic injection principle, simple devices can be used for introducing reproducible microliter volumes of both sample and reagent into the flow channel to form stacked zones in a similar fashion to those in a sequential injection system. The zones were then pushed to the detector and a peak profile was recorded. The determination of nitrite and nitrate in water samples by employing the Griess reaction was chosen as a model. Calibration graphs with linearity in the range of 0.7 - 40 muM were obtained for both nitrite and nitrate. Detection limits were found to be 0.3 muM NO(2)(-) and 0.4 muM NO(3)(-), respectively, with a sample throughput of 20 h(-1) for consecutive determination of both the species. The developed system was successfully applied to the analysis of water samples, employing simple and cost-effective instrumentation and offering higher degrees of automation and low chemical consumption.

Automated Immunomagnetic Separation and Microarray Detection of E. coli O157:H7 from Poultry Carcass Rinse

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

Chandler, Darrell P.; Brown, Jeremy D.; Call, Douglas R.

2001-09-01

We describe the development and application of a novel electromagnetic flow cell and fluidics system for automated immunomagnetic separation of E. coli directly from unprocessed poultry carcass rinse, and the biochemical coupling of automated sample preparation with nucleic acid microarrays without cell growth. Highly porous nickel foam was used as a magnetic flux conductor. Up to 32% recovery efficiency of 'total' E. coli was achieved within the automated system with 6 sec contact times and 15 minute protocol (from sample injection through elution), statistically similar to cell recovery efficiencies in > 1 hour 'batch' captures. The electromagnet flow cell allowedmore » complete recovery of 2.8 mm particles directly from unprocessed poultry carcass rinse whereas the batch system did not. O157:H7 cells were reproducibly isolated directly from unprocessed poultry rinse with 39% recovery efficiency at 103 cells ml-1 inoculum. Direct plating of washed beads showed positive recovery of O 157:H7 directly from carcass rinse at an inoculum of 10 cells ml-1. Recovered beads were used for direct PCR amplification and microarray detection, with a process-level detection limit (automated cell concentration through microarray detection) of < 103 cells ml-1 carcass rinse. The fluidic system and analytical approach described here are generally applicable to most microbial detection problems and applications.« less

Simplifying and expanding analytical capabilities for various classes of doping agents by means of direct urine injection high performance liquid chromatography high resolution/high accuracy mass spectrometry.

PubMed

Görgens, Christian; Guddat, Sven; Thomas, Andreas; Wachsmuth, Philipp; Orlovius, Anne-Katrin; Sigmund, Gerd; Thevis, Mario; Schänzer, Wilhelm

2016-11-30

So far, in sports drug testing compounds of different classes are processed and measured using different screening procedures. The constantly increasing number of samples in doping analysis, as well as the large number of substances with doping related, pharmacological effects require the development of even more powerful assays than those already employed in sports drug testing, indispensably with reduced sample preparation procedures. The analysis of native urine samples after direct injection provides a promising analytical approach, which thereby possesses a broad applicability to many different compounds and their metabolites, without a time-consuming sample preparation. In this study, a novel multi-target approach based on liquid chromatography and high resolution/high accuracy mass spectrometry is presented to screen for more than 200 analytes of various classes of doping agents far below the required detection limits in sports drug testing. Here, classic groups of drugs as diuretics, stimulants, β 2 -agonists, narcotics and anabolic androgenic steroids as well as various newer target compounds like hypoxia-inducible factor (HIF) stabilizers, selective androgen receptor modulators (SARMs), selective estrogen receptor modulators (SERMs), plasma volume expanders and other doping related compounds, listed in the 2016 WADA prohibited list were implemented. As a main achievement, growth hormone releasing peptides could be implemented, which chemically belong to the group of small peptides (<2kDa) and are commonly determined by laborious and time-consuming stand-alone assays. The assay was fully validated for qualitative purposes considering the parameters specificity, robustness (rRT: <2%), intra- (CV: 1.7-18.4 %) and inter-day precision (CV: 2.3-18.3%) at three concentration levels, linearity (R 2 >0.99), limit of detection (0.1-25ng/mL; 3'OH-stanozolol glucuronide: 50pg/mL; dextran/HES: 10μg/mL) and matrix effects. Copyright © 2016 Elsevier B.V. All rights reserved.

High-sensitivity detection of biological amines using fast Hadamard transform CE coupled with photolytic optical gating.

PubMed

Braun, Kevin L; Hapuarachchi, Suminda; Fernandez, Facundo M; Aspinwall, Craig A

2007-08-01

Here, we report the first utilization of Hadamard transform CE (HTCE), a high-sensitivity, multiplexed CE technique, with photolytic optical gating sample injection of caged fluorescent labels for the detection of biologically important amines. Previous implementations of HTCE have relied upon photobleaching optical gating sample injection of fluorescent dyes. Photolysis of caged fluorescent labels reduces the fluorescence background, providing marked enhancements in sensitivity compared to photobleaching. Application of fast Hadamard transform CE (fHTCE) for fluorescein-based dyes yields a ten-fold higher sensitivity for photolytic injections compared to photobleaching injections, due primarily to the reduced fluorescent background provided by caged fluorescent dyes. Detection limits as low as 5 pM (ca. 18 molecules per injection event) were obtained with on-column LIF detection using fHTCE in less than 25 s, with the capacity for continuous, online separations. Detection limits for glutamate and aspartate below 150 pM (1-2 amol/injection event) were obtained using photolytic sample injection, with separation efficiencies exceeding 1 x 10(6) plates/m and total multiplexed separation times as low as 8 s. These results strongly support the feasibility of this approach for high-sensitivity dynamic chemical monitoring applications.

Parametric investigation of secondary injection in post-chamber on combustion performance for hybrid rocket motor

NASA Astrophysics Data System (ADS)

Cai, Guobiao; Cao, Binbin; Zhu, Hao; Tian, Hui; Ma, Xuan

2017-11-01

The objective of this effort is to study the combustion performance of a hybrid rocket motor with the help of 3D steady-state numerical simulation, which applies 90% hydrogen peroxide as the oxidizer and hydroxyl-terminated polybutadiene as the fuel. A method of secondary oxidizer injection in post-chamber is introduced to investigate the flow field characteristics and combustion efficiency. The secondary injection medium is the mixed gas coming from liquid hydrogen peroxide catalytic decomposition. The secondary injectors are uniformly set along the circumferential direction of the post-chamber. The simulation results obtained by above model are verified by experimental data. Three influencing parameters are considered: secondary injection diameter, secondary injection angle and secondary injection numbers. Simulation results reveals that this design could improve the combustion efficiency with respect to the same motor without secondary injection. Besides, the secondary injection almost has no effect on the regression rate and fuel sueface temperature distribution. It is also presented that the oxidizer is injected by 8 secondary injectors with a diameter of 7-8 mm in the direction of 120°in post-chamber is identified as the optimized secondary injection pattern, through which combustion efficiency, specific impulse efficiency as well as utilization of propellants are all improved obviously.

Outcomes of Direct Vision Internal Urethrotomy for Bulbar Urethral Strictures: Technique Modification with High Dose Triamcinolone Injection.

PubMed

Modh, Rishi; Cai, Peter Y; Sheffield, Alyssa; Yeung, Lawrence L

2015-01-01

Objective. To evaluate the recurrence rate of bulbar urethral strictures managed with cold knife direct vision internal urethrotomy and high dose corticosteroid injection. Methods. 28 patients with bulbar urethral strictures underwent direct vision internal urethrotomy with high dose triamcinolone injection into the periurethral tissue and were followed up for recurrence. Results. Our cohort had a mean age of 60 years and average stricture length of 1.85 cm, and 71% underwent multiple previous urethral stricture procedures with an average of 5.7 procedures each. Our technique modification of high dose corticosteroid injection had a recurrence rate of 29% at a mean follow-up of 20 months with a low rate of urinary tract infections. In patients who failed treatment, mean time to stricture recurrence was 7 months. Patients who were successfully treated had significantly better International Prostate Symptom Scores at 6, 9, and 12 months. There was no significant difference in maximum flow velocity on Uroflowmetry at last follow-up but there was significant difference in length of follow-up (p = 0.02). Conclusions. High dose corticosteroid injection at the time of direct vision internal urethrotomy is a safe and effective procedure to delay anatomical and symptomatic recurrence of bulbar urethral strictures, particularly in those who are poor candidates for urethroplasty.

40 CFR 148.2 - Definitions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) WATER PROGRAMS (CONTINUED) HAZARDOUS WASTE INJECTION RESTRICTIONS General § 148.2 Definitions. Injection interval means that part of the injection zone in which the well is screened, or in which the waste is otherwise directly emplaced...

Supercritical-fluid extraction and chromatography-mass spectrometry for analysis of mycotoxins

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

Smith, R.D.; Udseth, H.R.

1982-07-01

The use of direct supercritical-fluid injection-mass spectrometry for the rapid analysis of mycotoxins of the tricothecene group is demonstrated. A solution containing diacetoxyscirpenol or T-2 toxin is injected into a fluid consisting primarily of pentane or carbon dioxide and is rapidly brought to supercritical conditions. Direct injection of the fluid stream into a chemical ionization source allows thermally labile compounds to be analyzed. Under these conditions trichothecene mass spectra showing significant (M + 1)/sup +/ ions and distinctive fragmentation patterns are obtained. Detection limits are in the subnanogram range. Direct analysis from complex substrates using selective supercritical-fluid extraction is proposed.more » 4 figures.« less

Computational study of interfacial charge transfer complexes of 2-anthroic acid adsorbed on a titania nanocluster for direct injection solar cells

NASA Astrophysics Data System (ADS)

Manzhos, Sergei; Kotsis, Konstantinos

2016-09-01

Adsorption and light absorption properties of interfacial charge transfer complexes of 2-anthroic acid and titania, promising for direct-injection solar cells, are studied ab initio. The formation of interfacial charge transfer bands is observed. The intensity of visible absorption is relatively low, highlighting a key challenge facing direct injection cells. We show that the popular strategy of using a lower level of theory for geometry optimization followed by single point calculations of adsorption or optical properties introduces significant errors which have been underappreciated: by up to 3 eV in adsorption energies, by up to 5 times in light absorption intensity.

Microdialysis pharmacokinetic study of scopolamine in plasma, olfactory bulb and vestibule after intranasal administration.

PubMed

Wei, Yan; Ying, Mingzhen; Xu, Shuai; Wang, Feng; Zou, Aifeng; Cao, Shilei; Jiang, Xinguo; Wang, Yajie

2016-01-01

The purpose of this study was to investigate the microdialysis pharmacokinetic of scopolamine in plasma, olfactory bulb and vestibule after intranasal administration. The pharmacokinetic study of subcutaneous and oral administration was also performed in rats. From the in vivo results, scopolamine intranasal administration can avoid hepatic first-pass effect. Tmax plasma samples after intranasal administration were significantly faster than oral administration and subcutaneous injection. The relative bioavailability of intranasal administrations was 51.8-70% when compared with subcutaneous injection. Moreover, one can see that in comparison with scopolamine subcutaneous administration, scopolamine intranasal gel and solutions can increased drug target index (DTI) with olfactory bulb 1.69 and 2.05, vestibule 1.80 and 2.15, respectively. The results indicated that scopolamine can be absorbed directly through the olfactory mucosa into the olfactory bulb, and then transported to various brain tissue after intranasal administration, with the characteristics of brain drug delivery.

Determination of highly protein bound drugs in plasma using high-performance liquid chromatography and column switching, exemplified by the retinoids.

PubMed

Wyss, R; Bucheli, F

1988-12-02

During method development for the determination of either isotretinoin, tretinoin and their 4-oxo-metabolites, or etretinate, acitretin and 13-cis-acitretin in plasma using high-performance liquid chromatography and column switching, recovery problems arose, when undiluted plasma samples were injected directly onto the precolumn. These recovery problems may be due to the strong binding of the retinoids to different plasma proteins. Measures to overcome this strong protein binding, such as variation of the injection solution composition and the purge mobile phase, were systematically investigated. Best recoveries were obtained by diluting of plasma with 9 mM sodium hydroxide-acetonitrile (8:2, v/v) and protein precipitation with ethanol for the isotretinoin and etretinate series, respectively, in combination with the use of a purge mobile phase containing ammonium acetate and 10-20% acetonitrile. Less effective was the use of a longer precolumn or heating of the precolumn.

[Flow injection biamperometric analysis of isoniazid].

PubMed

Zhang, J C; Zhao, C; Song, J F

2001-09-01

To establish a simple, rapid, and accurate electrochemical method for on-line determination of isoniazid. Based on the flow injection biamperometry for irreversible couple system, and using two preanodized platinum electrodes with the applied potential difference of 0 V, the biamperometric method for the determination of isoniazid has been proposed by coupling the catalytic oxidation of isoniazid and the reduction of platinum oxide. Common excipients, inorganic ions, amino acids, vitamins and proteins do not interfere with the determination. Linear relationship between current and the concentration of isoniazid is obtained in the range of 1.0 x 10(-6)-1.0 x 10(-4) mol.L-1 (gamma = 0.998, n = 11). The RSD of 1.8% was obtained for 8 successive determinations of 1.0 x 10(-5) mol.L-1 isoniazid. The proposed method has been shown to be sensitive, selective, rapid (120 samples.h-1), and suitable for the on-line direct determination of isoniazid.

Screening for basic drugs in equine urine using direct-injection differential-gradient LC-LC coupled to hybrid tandem MS/MS.

PubMed

Stanley, Shawn M R; Foo, Hsiao Ching

2006-05-19

A rapid, selective and robust direct-injection LC/hybrid tandem MS method has been developed for simultaneous screening of more than 250 basic drugs in the supernatant of enzyme hydrolysed equine urine. Analytes, trapped using a short HLB extraction column, are refocused and separated on a Sunfire C(18) analytical column using a controlled differential gradient generated by proportional dilution of the first column's eluent with water. Independent data acquisition (IDA) was configured to trigger a sensitive enhanced product ion (EPI) scan when a multiple reaction monitoring (MRM) survey scan signal exceeded the defined criteria. The decision on whether or not to report a sample as a positive result was based upon both the presence of a MRM response within the correct retention time range and a qualitative match between the EPI spectrum obtained and the corresponding reference standard. Ninety seven percent of the drugs targeted by this method met our detection criteria when spiked into urine at 100 ng/ml; 199 were found at 10 ng/ml, 83 at 1 ng/ml and 4 at 0.1 ng/ml.

Monitoring industrial wastewater by online GC-MS with direct aqueous injection.

PubMed

Wortberg, M; Ziemer, W; Kugel, M; Müller, H; Neu, H-J

2006-03-01

An online GC-MS-system for automated monitoring of crude wastewater at a complex chemical production site is presented. The modular system is, in principal, based on commercial equipment, but utilizes a special, two-stage injector, which consists of a splitless vaporization chamber on top of a PTV injector filled with Tenax. This set-up enables direct injection of wastewater. Almost 140 volatile and semi-volatile compounds are calibrated down to 1 mg L(-1), which is sufficient for analysis of the influent of the wastewater-treatment plant. Two instruments analyze alternately, every 20 min, and the instrument cycle time is 40 min. The quantitative results are transferred to a database which is connected to a process-control system. Depending on the nature and concentration of a compound, an alarm can be generated and the wastewater stream can be diverted into an "off spec tank" if necessary. The GC-MS-system operates quasi-continuously with a system availability >98%. Data quality is automatically controlled in each run and by daily analysis of a quality-control sample. The development of a novel stacked PTV-PTV injector design to expand the range of analytes to selected basic compounds is described.

The Influence of Direct Inoculation of Propionibacterium acnes on Modic Changes in the Spine: Evidence from a Rabbit Model.

PubMed

Shan, Zhi; Zhang, Xuyang; Li, Shengyun; Yu, Tianming; Mamuti, Maiwulanjiang; Zhao, Fengdong

2017-03-15

Modic changes (inflammatory-like changes visible on magnetic resonance imaging [MRI] scans of a vertebral end plate) are common and are associated with low back pain, but their origin is unclear. To our knowledge, there have been no previous in vivo animal models of Modic changes. We hypothesized that Modic changes may be related to Propionibacterium acnes. Ten New Zealand White rabbits were injected percutaneously with 1 mL of P. acnes (1.6 × 10 colony forming units/mL) into the subchondral bone superior to the L4-L5 and L5-L6 discs; 10 other control rabbits received sham injections at L4-L5 and 1 mL of normal saline solution (vehicle) at L5-L6. The subchondral bone superior to L3-L4 discs was untreated (blank). Development of Modic changes was investigated with MRI studies before the operation and at 2 weeks and 1, 2, 3, and 6 months postoperatively. Following sacrifice of the rabbits, histological analysis and microcomputed tomography (micro-CT) were performed, and blood samples were analyzed. Cytokine expression in end-plate tissues was quantified using real-time polymerase chain reaction (PCR). The group that received P. acnes showed significantly increased T1-weighted signal intensity at 6 months (mean and standard deviation, 3.43 ± 0.41 [range, 2.42 to 4.44] compared with 2.43 ± 0.66 [range, 1.98 to 2.87] before the injection) and higher T2-weighted signal intensity at 6 months. Positive culture results were obtained from 9 of 20 samples injected with P. acnes. Specimens with positive cultures had a higher prevalence of Modic changes (4 of 9 samples positive for P. acnes compared with 3 of 11 samples negative for P. acnes). Real-time PCR showed significantly increased expression of tumor necrosis factor-α, interleukin-1β, and interferon-γ following injection of P. acnes, but no changes were seen on histological analysis, micro-CT, or blood analysis. P. acnes can survive within the end-plate region and can initiate mild inflammatory-like responses from host cells, leading to signal intensity changes in MRI scans, which potentially resemble Modic changes. Disc degeneration and low back pain are associated with Modic changes. Our results indicate that Modic changes can be associated with P. acnes in the conjunction area of the disc and subchondral bone. These results may be useful for understanding the underlying mechanisms of Modic changes and related pain.

On the nature of directed behavior to drug-associated light cues in rhesus monkeys (Macaca mulatta).

PubMed

Reilly, Mark P; Berndt, Sonja I; Woods, James H

2016-11-01

The present study investigated the role of drug-paired stimuli in controlling the behavior of rhesus monkeys. Systematic observations were made with nine monkeys who had a history of drug self-administration; they had been lever pressing to produce intravenous infusions of various drugs. These observations revealed that the stimulus light co-occurring with drug infusion produced robust and cue-directed behavior such as orienting, touching and biting. Experiment 1 showed that this light-directed behavior would occur in naïve monkeys exposed to a Pavlovian pairing procedure. Four monkeys were given response-independent injections of cocaine. In two monkeys, a red light preceded cocaine injections by 5 s, and a green light co-occurred with the 5-s cocaine injections. In the other two monkeys, the light presentations and cocaine injections occurred independently. Light-directed behavior occurred in all four monkeys within the first couple of trials and at high levels but decreased across sessions. The cocaine-paired stimulus maintained behavior longer and at higher levels than the uncorrelated stimuli. Furthermore, light-directed behavior was not maintained when cocaine was replaced with saline. Light-directed behavior did not occur in the absence of the lights. When these monkeys were subsequently trained to lever press for cocaine, light-directed behavior increased to levels higher than previously observed. Behavior directed towards drug-paired stimuli is robust, reliable and multiply determined; the mechanisms underlying this activity likely include Pavlovian conditioning, stimulus novelty, habituation and operant conditioning.

Modeling of fault activation and seismicity by injection directly into a fault zone associated with hydraulic fracturing of shale-gas reservoirs

EPA Pesticide Factsheets

LBNL, in consultation with the EPA, expanded upon a previous study by injecting directly into a 3D representation of a hypothetical fault zone located in the geologic units between the shale-gas reservoir and the drinking water aquifer.

A novel needleless liquid jet injection methodology for improving direct cardiac gene delivery: An optimization of parameters, AAV mediated therapy and investigation of host responses in ischemic heart failure

NASA Astrophysics Data System (ADS)

Fargnoli, Anthony Samuel

Heart disease remains the leading cause of mortality and morbidity worldwide, with 22 million new patients diagnosed annually. Essentially, all present therapies have significant cost burden to the healthcare system, yet fail to increase survival rates. One key employed strategy is the genetic reprogramming of cells to increase contractility via gene therapy, which has advanced to Phase IIb Clinical Trials for advanced heart failure patients. It has been argued that the most significant barrier preventing FDA approval are resolving problems with safe, efficient myocardial delivery, whereby direct injection in the infarct and remote tissue areas is not clinically feasible. Here, we aim to: (1) Improve direct cardiac gene delivery through the development of a novel liquid jet device approach (2) Compare the new method against traditional IM injection with two different vector constructions and evaluate outcome (3) Evaluate the host response resulting from both modes of direct cardiac injection, then advance a drug/gene combination with controlled release nanoparticle formulations.

Mixing problems in using indicators for measuring regional blood flow

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

Ushioda, E.; Nuwayhid, B.; Tabsh, K.

A basic requirement for using indicators for measuring blood flow is adequate mixing of the indicator with blood prior to sampling the site. This requirement has been met by depositing the indicator in the heart and sampling from an artery. Recently, authors have injected microspheres into veins and sampled from venous sites. The present studies were designed to investigate the mixing problems in sheep and rabbits by means of Cardio-Green and labeled microspheres. The indicators were injected at different points in the circulatory system, and blood was sampled at different levels of the venous and arterial systems. Results show themore » following: (a) When an indicator of small molecular size (Cardio-Green) is allowed to pass through the heart chambers, adequate mixing is achieved, yielding accurate and reproducible results. (b) When any indicator (Cardio-Green or microspheres) is injected into veins, and sampling is done at any point in the venous system, mixing is inadequate, yielding flow results which are inconsistent and erratic. (c) For an indicator or large molecular size (microspheres), injecting into the left side of the heart and sampling from arterial sites yield accurate and reproducible results regardless of whether blood is sampled continuously or intermittently.« less

Where Does the Transplanted Fat is Located in the Gluteal Region? Research Letter.

PubMed

Ramos-Gallardo, Guillermo; Medina-Zamora, Pablo; Cardenas-Camarena, Lázaro; Orozco-Rentería, David; Duran-Vega, Héctor; Mota-Fonseca, Eduardo

2017-12-29

Liposuction is one of the most popular plastic surgery procedures. As in any surgery, there are risks and complications, especially when combined with fat injection. Case reports of fat embolism have been reported. A possible explanation is the puncture and tearing of gluteal vessels during the procedure, especially when a deep injection is planned. To identify the places where fat can be located after injection during a fat graft in the gluteus. An experimental study was done in which colorant was injected in four directions using four different quadrants of the gluteus. We Injected 10 cc six times following clock hands until 60 cc were injected, and the cutaneous flap and the muscles were then elevated. Our main purpose was to describe where the colorant went and if it was in contact with the vessels (superior and inferior gluteal vessels). In total, four gluteus muscles were injected and dissected. Injection in the lower lateral quadrant was mainly into the muscle, and colorant was observed in the hypogastric vessels. The injection in the upper quadrants stayed mainly in the subcutaneous tissue. During surgery, it is important to identify the location of the perforators and to avoid a deep injection, especially from the lower lateral quadrant to the superior medial quadrant (Q4 to Q1), as the probability of puncturing and injecting fat into the main vessels from this direction is higher.

Comparison of carpal tunnel injection techniques: a cadaver study.

PubMed

Ozturk, Kahraman; Esenyel, Cem Zeki; Sonmez, Mesut; Esenyel, Meltem; Kahraman, Sinan; Senel, Berna

2008-01-01

The purpose of the study was to evaluate the accuracy of injections into the carpal tunnel using three different portals in cadavers, and to define safe guidelines. In this study, 150 wrists of 75 cadavers (54 male, 21 female) were included. To compare three injection sites, 50 wrists of 25 cadavers were used for each technique; we used 23 gauge needles, and acrylic dye. The first injection technique: the needle was inserted 1cm proximal to the wrist crease and directed distally by roughly 45 in an ulnar direction through the flexor carpi radialis tendon. The second injection technique: the needle was inserted into the carpal tunnel from a point just ulnar to the palmaris longus tendon and 1cm proximal to the wrist crease. The third injection technique: the needle was inserted just distal to the distal skin crease of the wrist in line with the fourth ray. The first injection technique gave the highest accuracy rate, and this was also the safest injection site. Median nerve injuries caused by injection was seen mostly with the second technique. Although a steroid injection may provide symptomatic relief in patients with carpal tunnel syndrome, the median nerve and other structures in the carpal tunnel are at risk of injury. Because of that, the injection should be given using the correct technique by physicians skilled in carpal tunnel surgery.

Infectivity of DWV Associated to Flower Pollen: Experimental Evidence of a Horizontal Transmission Route

PubMed Central

Luisi, Elena; Forzan, Mario; Giusti, Matteo; Sagona, Simona; Tolari, Francesco; Felicioli, Antonio

2014-01-01

Deformed wing virus (DWV) is a honeybee pathogen whose presence is generally associated with infestation of the colony by the mite Varroa destructor, leading to the onset of infections responsible for the collapse of the bee colony. DWV contaminates bee products such as royal jelly, bee-bread and honey stored within the infected hive. Outside the hive, DWV has been found in pollen loads collected directly from infected as well as uninfected forager bees. It has been shown that the introduction of virus-contaminated pollen into a DWV-free hive results in the production of virus-contaminated food, whose role in the development of infected bees from virus-free eggs has been experimentally demonstrated. The aim of this study was twofold: (i) to ascertain the presence of DWV on pollen collected directly from flowers visited by honeybees and then quantify the viral load and (ii) determine whether the virus associated with pollen is infective. The results of our investigation provide evidence that DWV is present on pollen sampled directly from visited flowers and that, following injection in individuals belonging to the pollinator species Apis mellifera, it is able to establish an active infection, as indicated by the presence of replicating virus in the head of the injected bees. We also provide the first indication that the pollinator species Osmia cornuta is susceptible to DWV infection. PMID:25419704

Apparatus and method for performing microfluidic manipulations for chemical analysis and synthesis

DOEpatents

Ramsey, J. Michael

2000-01-01

A microchip laboratory system and method provide fluid manipulations for a variety of applications, including sample injection for microchip chemical separations. The microchip is fabricated using standard photolithographic procedures and chemical wet etching, with the substrate and cover plate joined using direct bonding. Capillary electrophoresis and electrochromatography are performed in channels formed in the substrate. Analytes are loaded into a four-way intersection of channels by electrokinetically pumping the analyte through the intersection, followed by switching of the potentials to force an analyte plug into the separation channel.

Apparatus and method for performing microfluidic manipulations for chemical analysis and synthesis

DOEpatents

Ramsey, J. Michael

2000-01-01

A microchip laboratory system and method proved fluid manipulations for a variety of applications, including sample injection for microchip chemical separations. The microchip is fabricated using standard photolithographic procedures and chemical wet etching, with the substrate and cover plate joined using direct bonding. Capillary electrophoresis and electrochromatography are performed in channels formed in the substrate. Analytes are loaded into a four-way intersection of channels by electrokinetically pumping the analyte through the intersection, followed by switching of the potentials to force an analyte plug into the separation channel.

Apparatus and method for performing microfluidic manipulations for chemical analysis and synthesis

DOEpatents

Ramsey, J. Michael

2002-01-01

A microchip laboratory system and method provide fluid manipulations for a variety of applications, including sample injection for microchip chemical separations. The microchip is fabricated using standard photolithographic procedures and chemical wet etching, with the substrate and cover plate joined using direct bonding. Capillary electrophoresis and electrochromatography are performed in channels formed in the substrate. Analytes are loaded into a four-way intersection of channels by electrokinetically pumping the analyte through the intersection, followed by switching of the potentials to force an analyte plug into the separation channel.

Apparatus and method for performing microfluidic manipulations for chemical analysis and synthesis

DOEpatents

Ramsey, J. Michael

1999-01-01

A microchip laboratory system and method provide fluid manipulations for a variety of applications, including sample injection for microchip chemical separations. The microchip is fabricated using standard photolithographic procedures and chemical wet etching, with the substrate and cover plate joined using direct bonding. Capillary electrophoresis and electrochromatography are performed in channels formed in the substrate. Analytes are loaded into a four-way intersection of channels by electrokinetically pumping the analyte through the intersection, followed by switching of the potentials to force an analyte plug into the separation channel.

Apparatus and method for performing microfluidic manipulations for chemical analysis and synthesis

DOEpatents

Ramsey, J.M.

1999-01-12

A microchip laboratory system and method provide fluid manipulations for a variety of applications, including sample injection for microchip chemical separations. The microchip is fabricated using standard photolithographic procedures and chemical wet etching, with the substrate and cover plate joined using direct bonding. Capillary electrophoresis and electrochromatography are performed in channels formed in the substrate. Analytes are loaded into a four-way intersection of channels by electrokinetically pumping the analyte through the intersection, followed by switching of the potentials to force an analyte plug into the separation channel. 46 figs.

The effect on toxicology, biochemistry and immunology investigations by the use of targeted post-mortem computed tomography angiography.

PubMed

Rutty, G N; Smith, P; Visser, T; Barber, J; Amorosa, J; Morgan, B

2013-02-10

It is recognised in autopsy practice that investigations such as toxicology can be affected by post-mortem change. Post-mortem computed tomography angiography (PMCT-A) involves the injection of contrast agents. This could cause dilution of a biological fluid sample or cause the circulation of blood after death by mechanical pumping, and thus has the potential to affect laboratory investigations. We undertook a small sample study to consider whether targeted PMCT-A had any significant effect on subsequent samples taken for biochemical, toxicological or immunological investigations. Although the results of our study do illustrate differences between the pre and post PMCT-A results, these differences are considered not to be of diagnostic significance and not due to the direct effect of targeted PMCT-A. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

[Rapid screening and quality evaluation for the harmful substance 5-hydroxymethyl furfural in commercially available traditional Chinese medicine injection using LC-MS/MS method].

PubMed

Zang, Qing-ce; He, Jing-jing; Bai, Jin-fa; Zheng, Ya-jie; Zhang, Rui-ping; Li, Tie-gang; Wang, Zhong-hua; He, Jiu-ming; Abliz, Zeper

2013-11-01

To screen the harmful substance 5-hydroxymethyl furfural content in commercially available traditional Chinese medicine injection which are commonly used, and to preliminarily evaluate the quality of these injections, 5-hydroxymethyl furfural was taken as an index. The contents of 5-hydroxymethyl furfural in 56 samples which consist of 23 kinds of traditional Chinese medicine injections and glucose injection were determined using LC-MS/MS, and 5-hydroxymethyl furfural was detected in 52 of these samples. The minimal content was 0.0038 microg x L(-1) and the maximum content was 1420 microg x mL(-1). The contents of 5-hydroxymethyl furfural were significantly different in traditional Chinese medicine injection which came from different kinds, manufacturers or batches. The results showed the quality difference of commercially available traditional Chinese medicine injection is significant taking 5-hydroxymethyl furfural content as assessment index. More attention should be paid to the safety of 5-hydroxymethyl furfural in traditional Chinese medicine injection, and unified limitation standard should be set to improve medication safety of traditional Chinese medicine injection.

Experimental Investigation on Dilation Mechanisms of Land-Facies Karamay Oil Sand Reservoirs under Water Injection

NASA Astrophysics Data System (ADS)

Lin, Botao; Jin, Yan; Pang, Huiwen; Cerato, Amy B.

2016-04-01

The success of steam-assisted gravity drainage (SAGD) is strongly dependent on the formation of a homogeneous and highly permeable zone in the land-facies Karamay oil sand reservoirs. To accomplish this, hydraulic fracturing is applied through controlled water injection to a pair of horizontal wells to create a dilation zone between the dual wells. The mechanical response of the reservoirs during this injection process, however, has remained unclear for the land-facies oil sand that has a loosely packed structure. This research conducted triaxial, permeability and scanning electron microscopy (SEM) tests on the field-collected oil sand samples. The tests evaluated the influences of the field temperature, confining stress and injection pressure on the dilation mechanisms as shear dilation and tensile parting during injection. To account for petrophysical heterogeneity, five reservoir rocks including regular oil sand, mud-rich oil sand, bitumen-rich oil sand, mudstone and sandstone were investigated. It was found that the permeability evolution in the oil sand samples subjected to shear dilation closely followed the porosity and microcrack evolutions in the shear bands. In contrast, the mudstone and sandstone samples developed distinct shear planes, which formed preferred permeation paths. Tensile parting expanded the pore space and increased the permeability of all the samples in various degrees. Based on this analysis, it is concluded that the range of injection propagation in the pay zone determines the overall quality of hydraulic fracturing, while the injection pressure must be carefully controlled. A region in a reservoir has little dilation upon injection if it remains unsaturated. Moreover, a cooling of the injected water can strengthen the dilation potential of a reservoir. Finally, it is suggested that the numerical modeling of water injection in the Karamay oil sand reservoirs must take into account the volumetric plastic strain in hydrostatic loading.

Injectable Anisotropic Nanocomposite Hydrogels Direct in Situ Growth and Alignment of Myotubes

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

De France, Kevin J.; Yager, Kevin G.; Chan, Katelyn J. W.

Here, while injectable in situ cross-linking hydrogels have attracted increasing attention as minimally invasive tissue scaffolds and controlled delivery systems, their inherently disorganized and isotropic network structure limits their utility in engineering oriented biological tissues. Traditional methods to prepare anisotropic hydrogels are not easily translatable to injectable systems given the need for external equipment to direct anisotropic gel fabrication and/or the required use of temperatures or solvents incompatible with biological systems. Herein, we report a new class of injectable nanocomposite hydrogels based on hydrazone cross-linked poly(oligoethylene glycol methacrylate) and magnetically aligned cellulose nanocrystals (CNCs) capable of encapsulating skeletal muscle myoblastsmore » and promoting their differentiation into highly oriented myotubes in situ. CNC alignment occurs on the same time scale as network gelation and remains fixed after the removal of the magnetic field, enabling concurrent CNC orientation and hydrogel injection. The aligned hydrogels show mechanical and swelling profiles that can be rationally modulated by the degree of CNC alignment and can direct myotube alignment both in two- and three-dimensions following coinjection of the myoblasts with the gel precursor components. As such, these hydrogels represent a critical advancement in anisotropic biomimetic scaffolds that can be generated noninvasively in vivo following simple injection.« less

Injectable Anisotropic Nanocomposite Hydrogels Direct in Situ Growth and Alignment of Myotubes

DOE PAGES

De France, Kevin J.; Yager, Kevin G.; Chan, Katelyn J. W.; ...

2017-09-28

Here, while injectable in situ cross-linking hydrogels have attracted increasing attention as minimally invasive tissue scaffolds and controlled delivery systems, their inherently disorganized and isotropic network structure limits their utility in engineering oriented biological tissues. Traditional methods to prepare anisotropic hydrogels are not easily translatable to injectable systems given the need for external equipment to direct anisotropic gel fabrication and/or the required use of temperatures or solvents incompatible with biological systems. Herein, we report a new class of injectable nanocomposite hydrogels based on hydrazone cross-linked poly(oligoethylene glycol methacrylate) and magnetically aligned cellulose nanocrystals (CNCs) capable of encapsulating skeletal muscle myoblastsmore » and promoting their differentiation into highly oriented myotubes in situ. CNC alignment occurs on the same time scale as network gelation and remains fixed after the removal of the magnetic field, enabling concurrent CNC orientation and hydrogel injection. The aligned hydrogels show mechanical and swelling profiles that can be rationally modulated by the degree of CNC alignment and can direct myotube alignment both in two- and three-dimensions following coinjection of the myoblasts with the gel precursor components. As such, these hydrogels represent a critical advancement in anisotropic biomimetic scaffolds that can be generated noninvasively in vivo following simple injection.« less

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

PubMed

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

2006-02-01

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

Miniaturized hollow fibre assisted liquid-phase microextraction and gas chromatography for determination of trace concentration of sufentanil and alfentanil in biological samples.

PubMed

Fakhari, Ali Reza; Tabani, Hadi; Nojavan, Saeed

2013-07-01

A simple and highly sensitive method that involves miniaturized hollow fibre assisted liquid-phase microextraction with gas chromatography-flame ionization detector was developed for the determination of trace concentration of sufentanil and alfentanil in biological samples. These drugs were extracted from 5 ml of aqueous solution with pH 10.0 into an organic extracting solvent (1-octanol) impregnated in the pores and lumen of a hollow fibre. After extraction for a prescribed time, 2.0 µl of the extraction solvent was injected directly in to the GC injection port. Under the optimized conditions, (1-octanol as extracting solvent, stirring rate of 700 rpm, 15% (w/v) salt addition, pH 10.0 and 25 min sampling time at 50 °C) large enrichment factors of 535 and 420 were achieved for sufentanil and alfentanil, respectively. Dynamic linear ranges were in the range of 0.05 to 500 ng/ml for sufentanil and 0.1 to 500 ng/ml for alfentanil. Limits of detection 0.01 and 0.02 ng/ml were obtained for sufentanil and alfentanil, respectively. The percent relative intra-day and inter-day standard deviations were found to be less than 8.4% (n = 5). Finally, this method was successfully applied for the separation, preconcentration and determination of trace concentration of sufentanil and alfentanil in plasma and urine samples. Copyright © 2012 John Wiley & Sons, Ltd.

Automated dispersive liquid-liquid microextraction coupled to high performance liquid chromatography - cold vapour atomic fluorescence spectroscopy for the determination of mercury species in natural water samples.

PubMed

Liu, Yao-Min; Zhang, Feng-Ping; Jiao, Bao-Yu; Rao, Jin-Yu; Leng, Geng

2017-04-14

An automated, home-constructed, and low cost dispersive liquid-liquid microextraction (DLLME) device that directly coupled to a high performance liquid chromatography (HPLC) - cold vapour atomic fluorescence spectroscopy (CVAFS) system was designed and developed for the determination of trace concentrations of methylmercury (MeHg + ), ethylmercury (EtHg + ) and inorganic mercury (Hg 2+ ) in natural waters. With a simple, miniaturized and efficient automated DLLME system, nanogram amounts of these mercury species were extracted from natural water samples and injected into a hyphenated HPLC-CVAFS for quantification. The complete analytical procedure, including chelation, extraction, phase separation, collection and injection of the extracts, as well as HPLC-CVAFS quantification, was automated. Key parameters, such as the type and volume of the chelation, extraction and dispersive solvent, aspiration speed, sample pH, salt effect and matrix effect, were thoroughly investigated. Under the optimum conditions, linear range was 10-1200ngL -1 for EtHg + and 5-450ngL -1 for MeHg + and Hg 2+ . Limits of detection were 3.0ngL -1 for EtHg + and 1.5ngL -1 for MeHg + and Hg 2+ . Reproducibility and recoveries were assessed by spiking three natural water samples with different Hg concentrations, giving recoveries from 88.4-96.1%, and relative standard deviations <5.1%. Copyright © 2017 Elsevier B.V. All rights reserved.

Photochemical ozone budget during the BIBLE A and B campaigns

NASA Astrophysics Data System (ADS)

Ko, Malcolm; Hu, Wenjie; Rodríguez, José M.; Kondo, Yutaka; Koike, Makoto; Kita, Kazuyuki; Kawakami, Shuji; Blake, Donald; Liu, Shaw; Ogawa, Toshihiro

2003-02-01

Using the measured concentrations of NO, O3, H2O, CO, CH4, and NMHCs along the flight tracks, a photochemical box model is used to calculate the concentrations of the Ox radicals, the HOx radicals, and the nitrogen species at the sampling points. The calculations make use of the measurements from radiometers to scale clear sky photolysis rates to account for cloud cover and ground albedo at the sampling time/point. The concentrations of the nitrogen species in each of the sampled air parcels are computed assuming they are in instantaneous equilibrium with the measured NO and O3. The diurnally varying species concentrations are next calculated using the box model and used to estimate the diurnally averaged production and removal rates of ozone for the sampled air parcels. Clear sky photolysis rates are used in the diurnal calculations. The campaign also provided measured concentration of NOy. The observed NO/NOy ratio is usually larger than the model calculated equilibrium value. There are several possible explanations. It could be a result of recent injection of NO into the air parcel, recent removal of HNO3 from the parcel, recent rapid transport of an air parcel from another location, or a combination of all processes. Our analyses suggest that the local production rate of O3 can be used as another indicator of recent NO injection. However, more direct studies using air trajectory analyses and other collaborative evidences are needed to ascertain the roles played by individual process.

Photochemical ozone budget during the BIBLE A and B campaigns

NASA Astrophysics Data System (ADS)

Ko, Malcolm; Hu, Wenjie; RodríGuez, José M.; Kondo, Yutaka; Koike, Makoto; Kita, Kazuyuki; Kawakami, Shuji; Blake, Donald; Liu, Shaw; Ogawa, Toshihiro

2002-02-01

Using the measured concentrations of NO, O3, H2O, CO, CH4, and NMHCs along the flight tracks, a photochemical box model is used to calculate the concentrations of the Ox radicals, the HOx radicals, and the nitrogen species at the sampling points. The calculations make use of the measurements from radiometers to scale clear sky photolysis rates to account for cloud cover and ground albedo at the sampling time/point. The concentrations of the nitrogen species in each of the sampled air parcels are computed assuming they are in instantaneous equilibrium with the measured NO and O3. The diurnally varying species concentrations are next calculated using the box model and used to estimate the diurnally averaged production and removal rates of ozone for the sampled air parcels. Clear sky photolysis rates are used in the diurnal calculations. The campaign also provided measured concentration of NOy. The observed NO/NOy ratio is usually larger than the model calculated equilibrium value. There are several possible explanations. It could be a result of recent injection of NO into the air parcel, recent removal of HNO3 from the parcel, recent rapid transport of an air parcel from another location, or a combination of all processes. Our analyses suggest that the local production rate of O3 can be used as another indicator of recent NO injection. However, more direct studies using air trajectory analyses and other collaborative evidences are needed to ascertain the roles played by individual process.

Assay for the simultaneous determination of guanidinoacetic acid, creatinine and creatine in plasma and urine by capillary electrophoresis UV-detection.

PubMed

Zinellu, Angelo; Sotgia, Salvatore; Zinellu, Elisabetta; Chessa, Roberto; Deiana, Luca; Carru, Ciriaco

2006-03-01

Guanidinoacetic acid (GAA) measurement has recently become of great interest for the diagnosis of creatine (Cn) metabolism disorders, and research calls for rapid and inexpensive methods for its detection in plasma and urine in order to assess a large number of patients. We propose a new assay for the measurement of GAA by a simple CZE UV-detection without previous sample derivatization. Plasma samples were filtered by Microcon-10 microconcentrators and directly injected into the capillary, while for urine specimens a simple water dilution before injection was needed. A baseline separation was obtained in less than 8 min using a 60.2 cm x 75 microm uncoated silica capillary, 75 mmol/L Tris-phosphate buffer pH 2.25 at 15 degrees C. The performance of the developed method was assessed by measuring plasma creatinine and Cn in 32 normal subjects and comparing the data obtained by the new method with those found with the previous CE assay. Our new method seems to be an inexpensive, fast and specific tool to assess a large number of patients both in clinical and in research laboratories.

Simplex optimization of the variables influencing the determination of pefloxacin by time-resolved chemiluminescence

NASA Astrophysics Data System (ADS)

Murillo Pulgarín, José A.; Alañón Molina, Aurelia; Jiménez García, Elisa

2018-03-01

A new chemiluminescence (CL) detection system combined with flow injection analysis (FIA) for the determination of Pefloxacin is proposed. The determination is based on an energy transfer from Pefloxacin to terbium (III). The metal ion enhances the weak CL signal produced by the KMnO4/H2SO3/Pefloxacin system. A modified simplex method was used to optimize chemical and instrumental variables. The influence of the interaction of the permanganate, Tb (III), sodium sulphite and sulphuric acid concentrations, flow rate and injected sample volume was thoroughly investigated by using a modified simplex optimization procedure. The results revealed a strong direct relationship between flow rate and CL intensity throughout the studied range that was confirmed by a gamma test. The response factor for the CL emission intensity was used to assess performance in order to identify the optimum conditions for maximization of the response. Under such conditions, the CL response was proportional to the Pefloxacin concentration over a wide range. The detection limit as calculated according to Clayton's criterion 13.7 μg L- 1. The analyte was successfully determined in milk samples with an average recovery of 100.6 ± 9.8%.

Iodine speciation in coastal and inland bathing waters and seaweeds extracts using a sequential injection standard addition flow-batch method.

PubMed

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

2015-02-01

The present work describes the development of a sequential injection standard addition method for iodine speciation in bathing waters and seaweeds extracts without prior sample treatment. Iodine speciation was obtained by assessing the iodide and iodate content, the two inorganic forms of iodine in waters. For the determination of iodide, an iodide ion selective electrode (ISE) was used. The indirect determination of iodate was based on the spectrophotometric determination of nitrite (Griess reaction). For the iodate measurement, a mixing chamber was employed (flow batch approach) to explore the inherent efficient mixing, essential for the indirect determination of iodate. The application of the standard addition method enabled detection limits of 0.14 µM for iodide and 0.02 µM for iodate, together with the direct introduction of the target water samples, coastal and inland bathing waters. The results obtained were in agreement with those obtained by ICP-MS and a colorimetric reference procedure. Recovery tests also confirmed the accuracy of the developed method which was effectively applied to bathing waters and seaweed extracts. Copyright © 2014 Elsevier B.V. All rights reserved.

Multiple injection mode with or without repeated sample injections: Strategies to enhance productivity in countercurrent chromatography.

PubMed

Müller, Marco; Wasmer, Katharina; Vetter, Walter

2018-06-29

Countercurrent chromatography (CCC) is an all liquid based separation technique typically used for the isolation and purification of natural compounds. The simplicity of the method makes it easy to scale up CCC separations from analytical to preparative and even industrial scale. However, scale-up of CCC separations requires two different instruments with varying coil dimensions. Here we developed two variants of the CCC multiple injection mode as an alternative to increase the throughput and enhance productivity of a CCC separation when using only one instrument. The concept is based on the parallel injection of samples at different points in the CCC column system and the simultaneous separation using one pump only. The wiring of the CCC setup was modified by the insertion of a 6-port selection valve, multiple T-pieces and sample loops. Furthermore, the introduction of storage sample loops enabled the CCC system to be used with repeated injection cycles. Setup and advantages of both multiple injection modes were shown by the isolation of the furan fatty acid 11-(3,4-dimethyl-5-pentylfuran-2-yl)-undecanoic acid (11D5-EE) from an ethyl ester oil rich in 4,7,10,13,16,19-docosahexaenoic acid (DHA-EE). 11D5-EE was enriched in one step from 1.9% to 99% purity. The solvent consumption per isolated amount of analyte could be reduced by ∼40% compared to increased throughput CCC and by ∼5% in the repeated multiple injection mode which also facilitated the isolation of the major compound (DHA-EE) in the sample. Copyright © 2018 Elsevier B.V. All rights reserved.

Plasma discharge elemental detector for a mass spectrometer

NASA Astrophysics Data System (ADS)

Heppner, R. A.

1983-06-01

A material to be analyzed is injected into a mirowave-induced plasma discharge unit, in which the material is carried with a flow of buffer gas through an intense microwave energy field which produces a plasma discharge in the buffer gas. As the material exits from the plasma discharge, the material is sampled and conveyed along a capillary transfer tube to a mass spectrometer where it is analyzed. The plasma discharge causes dissociation of complex organic molecules into simpler molecules which return to the neutral ground state before they are analyzed in the mass spectrometer. The buffer gas is supplied to one end portion of the discharge tube and is withdrawn from the other end portion by a vacuum pump which maintains a subatmospheric pressure in the discharge tube. The sample material is injected by a capillary injection tube into the buffer gas flow as it enters the plasma discharge zone. The dissociated materials are sampled by an axial sampling tube having an entrance where the buffer gas exits from the plasma discharge zone. The sample material may be supplied by a gas chromatography having a capillary effluent line connected to the capillary injection tube, so that the effluent material is injected into the microwave induced plasma discharge. The microwave field is produced by a cavity resonator through which the discharge tube passes.

Challenges to Safe Injection Practices in Ambulatory Care.

PubMed

Anderson, Laura; Weissburg, Benjamin; Rogers, Kelli; Musuuza, Jackson; Safdar, Nasia; Shirley, Daniel

2017-05-01

Most recent infection outbreaks caused by unsafe injection practices in the United States have occurred in ambulatory settings. We utilized direct observation and a survey to assess injection practices at 31 clinics. Improper vial use was observed at 13 clinics (41.9%). Pharmacy support and healthcare worker education may improve injection practices. Infect Control Hosp Epidemiol 2017;38:614-616.

Heat transfer to a full-coverage film-cooled surface with 30 degree slant-hole injection

NASA Technical Reports Server (NTRS)

Crawford, M. E.; Kays, W. M.; Moffat, R. J.

1976-01-01

Heat transfer behavior was studied in a turbulent boundary layer with full coverage film cooling through an array of discrete holes and with injection 30 deg to the wall surface in the downstream direction. Stanton numbers were measured for a staggered hole pattern with pitch-to-diameter ratios of 5 and 10, an injection mass flux ratio range of 0.1 to 1.3, and a range of Reynolds number Re sub x of 150,000 to 5 million. Air was used as the working fluid, and the mainstream velocity varied from 9.8 to 34.2 m/sec (32 to 112 ft/sec). The data were taken for secondary injection temperature equal to the wall temperature and also equal to the mainstream temperature. The data may be used to obtain Stanton number as a continuous function of the injectant temperature by use of linear superposition theory. The heat transfer coefficient is defined on the basis of a mainstream-to-wall temperature difference. This definition permits direct comparison of performance between film cooling and transpiration cooling. A differential prediction method was developed to predict the film cooling data base. The method utilizes a two-dimensional boundary layer program with routines to model the injection process and turbulence augmentation. The program marches in the streamwise direction, and when a row of holes is encountered, it stops and injects fluid into the boundary layer. The turbulence level is modeled by algebraically augmenting the mixing length, with the augmentation keyed to a penetration distance for the injected fluid.

Surface Analysis of Nerve Agent Degradation Products by ...

EPA Pesticide Factsheets

Report This sampling and analytical procedure was developed and applied by a single laboratory to investigate nerve agent degradation products, which may persist at a contaminated site, via surface wiping followed by analytical characterization. The performance data presented demonstrate the fitness-for-purpose regarding surface analysis in that single laboratory. Surfaces (laminate, glass, galvanized steel, vinyl tile, painted drywall and treated wood) were wiped with cotton gauze wipes, sonicated, extracted with distilled water, and filtered. Samples were analyzed with direct injection electrospray ionization liquid chromatography tandem mass spectrometry (ESI-LC/MS/MS) without derivatization. Detection limit data were generated for all analytes of interest on a laminate surface. Accuracy and precision data were generated from each surface fortified with these analytes.

Injection of benomyl into elm, oak & maple

Treesearch

Garold F. Gregory; Thomas W. Jones; Percy McWain; Percy McWain

1971-01-01

A newly devised apparatus using pressure to inject fluids into trees was used to inject solubilized benomyl into elms, oaks, and maples. In October and November, injections were made into the outer two annual rings of sapwood at points 2 to 3 feet above ground line. One to 3 weeks after injection, the trees were sampled; and positive bioassays were obtained from branch...

Multiplex gas chromatography for use in space craft

NASA Technical Reports Server (NTRS)

Valentin, J. R.

1985-01-01

Gas chromatography is a powerful technique for the analysis of gaseous mixtures. Some limitations in this technique still exist which can be alleviated with multiplex gas chromatography (MGC). In MGC, rapid multiple sample injections are made into the column without having to wait for one determination to be finished before taking a new sample. The resulting data must then be reduced using computational methods such as cross correlation. In order to efficiently perform multiplexgas chromatography, experiments in the laboratory and on board future space craft, skills, equipment, and computer software were developed. Three new techniques for modulating, i.e., changing, sample concentrations were demonstrated by using desorption, decomposition, and catalytic modulators. In all of them, the need for a separate gas stream as the carrier was avoided by placing the modulator at the head of the column to directly modulate a sample stream. Finally, the analysis of an environmental sample by multiplex chromatography was accomplished by employing silver oxide to catalytically modulate methane in ambient air.

Simultaneous quantification of fluoxetine and norfluoxetine in colostrum and mature human milk using a 2-dimensional liquid chromatography-tandem mass spectrometry system.

PubMed

Lopes, Bianca Rebelo; Cassiano, Neila Maria; Carvalho, Daniela Miarelli; Moisés, Elaine Christine Dantas; Cass, Quezia Bezerra

2018-02-20

A two-dimensional liquid chromatography system coupled to triple quadrupole tandem mass spectrometer (2D LC-MS/MS) was employed for the determination of fluoxetine (FLU) and norfluoxetine (N-FLU) in colostrum and mature milk by direct sample injection. With a run time of 12 min representing a gain in throughput analysis, the validated methods furnished selectivity, extraction efficiency, accuracy, and precision in accordance with the criteria preconized by the European Medicines Agency guidelines. With a linear range of 3.00-150 ng/mL for FLU and 4.00-200 ng/mL for N-FLU they were applied to the analysis of colostrum and mature milk samples from nursing mothers. The paper discusses the differences and similarity of sample preparation for this two sample matrices. The herein reported methods are an advance in sample preparation procedures providing waste reduction and a sustainable approach. Copyright © 2017 Elsevier B.V. All rights reserved.

The impact of previous para-areolar incision in the upper outer quadrant of the breast on the localization of the sentinel lymph node in a canine model

PubMed Central

Vasques, Paulo Henrique Diógenes; Pinheiro, Luiz Gonzaga Porto; de Meneses e Silva, João Marcos; de Moura Torres-de-Melo, José Ricardo; Pinheiro, Karine Bessa Porto; Rocha, João Ivo Xavier

2011-01-01

OBJECTIVES: This paper discusses the influence of a para-areolar incision in the upper outer quadrant of the breast on the location of the sentinel lymph node in a canine model. METHODS: The sentinel lymph node was marked with technetium-99, which was injected into the subareolar skin of the cranial breast. After the marker had migrated to the axilla, an arcuate para-areolar incision was performed 2 cm from the nipple in the upper outer quadrant. Patent blue dye was then injected above the upper border of the incision. At the marked site, an axillary incision was made, and the sentinel lymph node was identified by gamma probe and/or by direct visualization of the dye. The agreement between the two injection sites and the two sentinel lymph node identification methods was determined. Our sample group consisted of 40 cranial breasts of 23 adult females of the species Canis familiaris. The data were analyzed by using the McNemar test and by determining the kappa agreement coefficient. RESULT: Our findings showed that in 95% of the breasts, the sentinel lymph node was identified by the injection of technetium-99 m into the subareolar region, and in 82% of the cases, the sentinel lymph node was identified by the injection of patent blue dye above the upper border of the incision. The methods agreed 82% of the time. CONCLUSIONS: Previous para-areolar incisions in the upper outer quadrant did not interfere significantly with the biopsy when the dye was injected above the upper border of the incision. PMID:21915493

Control of high-Z PFC erosion by local gas injection in DIII-D

NASA Astrophysics Data System (ADS)

Rudakov, D. L.; Stangeby, P. C.; Wong, C. P. C.; McLean, A. G.; Wampler, W. R.; Watkins, J. G.; Boedo, J. A.; Briesemeister, A.; Buchenauer, D. A.; Chrobak, C. P.; Elder, J. D.; Fenstermacher, M. E.; Guo, H. Y.; Lasnier, C. J.; Leonard, A. W.; Maingi, R.; Moyer, R. A.

2015-08-01

Reduced erosion of a high-Z PFC divertor surface was observed in DIII-D with local injection of methane and deuterium gases. Molybdenum-coated silicon samples were exposed in the lower divertor of DIII-D using DiMES under plasma conditions previously shown to cause significant net erosion of Mo. Three exposures with 13CH4 and one exposure with D2 gas injection about 12 cm upstream of the samples located within 1-2 cm of the attached strike point were performed. Reduction of Mo erosion was evidenced in-situ by the suppression of MoI line radiation at 386.4 nm once the gas injection started. Post-mortem ion beam analysis demonstrated that the net erosion of molybdenum near the center of the samples exposed with 13CH4 injection was below the measurement resolution of 0.5 nm, corresponding to a rate of ⩽0.04 nm/s. Compared to the previously measured erosion rates, this constitutes a reduction by a factor of >10.

Silver nanoparticles as a key feature of a plasma polymer composite layer in mitigation of charge injection into polyethylene under dc stress

NASA Astrophysics Data System (ADS)

Milliere, L.; Maskasheva, K.; Laurent, C.; Despax, B.; Boudou, L.; Teyssedre, G.

2016-01-01

The aim of this work is to limit charge injection from a semi-conducting electrode into low density polyethylene (LDPE) under dc field by tailoring the polymer surface using a silver nanoparticles-containing layer. The layer is composed of a plane of silver nanoparticles embedded in a semi-insulating organosilicon matrix deposited on the polyethylene surface by a plasma process. Size, density and surface coverage of the nanoparticles are controlled through the plasma process. Space charge distribution in 300 μm thick LDPE samples is measured by the pulsed-electroacoustic technique following a short term (step-wise voltage increase up to 50 kV mm-1, 20 min in duration each, followed by a polarity inversion) and a longer term (up to 12 h under 40 kV mm-1) protocols for voltage application. A comparative study of space charge distribution between a reference polyethylene sample and the tailored samples is presented. It is shown that the barrier effect depends on the size distribution and the surface area covered by the nanoparticles: 15 nm (average size) silver nanoparticles with a high surface density but still not percolating form an efficient barrier layer that suppress charge injection. It is worthy to note that charge injection is detected for samples tailored with (i) percolating nanoparticles embedded in organosilicon layer; (ii) with organosilicon layer only, without nanoparticles and (iii) with smaller size silver particles (<10 nm) embedded in organosilicon layer. The amount of injected charges in the tailored samples increases gradually in the samples ranking given above. The mechanism of charge injection mitigation is discussed on the basis of complementary experiments carried out on the nanocomposite layer such as surface potential measurements. The ability of silver clusters to stabilize electrical charges close to the electrode thereby counterbalancing the applied field appears to be a key factor in explaining the charge injection mitigation effect.

An improved reference measurement procedure for triglycerides and total glycerides in human serum by isotope dilution gas chromatography-mass spectrometry.

PubMed

Chen, Yizhao; Liu, Qinde; Yong, Sharon; Teo, Hui Ling; Lee, Tong Kooi

2014-01-20

Triglycerides are widely tested in clinical laboratories using enzymatic methods for lipid profiling. As enzymatic methods can be affected by interferences from biological samples, this together with the non-specific nature of triglycerides measurement makes it necessary to verify the accuracy of the test results with a reference measurement procedure. Several such measurement procedures had been published. These procedures generally involved lengthy and laborious sample preparation steps. In this paper, an improved reference measurement procedure for triglycerides and total glycerides was reported which simplifies the sample preparation steps and greatly shortens the time taken. The procedure was based on isotope dilution gas chromatography-mass spectrometry (IDGC-MS)with tripalmitin as the calibration standard. Serum samples were first spiked with isotope-labeled tripalmitin. For the measurement of triglycerides, the serum samples were subjected to lipid extraction followed by separation of triglycerides from diglycerides and monoglycerides. Triglycerides were then hydrolyzed to glycerol, derivatized and injected into the GC–MS for quantification. For the measurement of total glycerides, the serum samples were hydrolyzed directly and derivatized before injection into the GC-MS for quantification. All measurement results showed good precision with CV <1%. A certified reference material (CRM) of lipids in frozen human serum was used to verify the accuracy of the measurement. The obtained values for both triglycerides and total glycerides were well within the certified ranges of the CRM, with deviation <0.4% from the certified values. The relative expanded uncertainties were also comparable with the uncertainties associated with the certified values of the CRM. The validated procedure was used in an External Quality Assessment (EQA) Program organized by our laboratory to establish the assigned values for triglycerides and total glycerides.

Direct memory access transfer completion notification

DOEpatents

Chen, Dong; Giampapa, Mark E.; Heidelberger, Philip; Kumar, Sameer; Parker, Jeffrey J.; Steinmacher-Burow, Burkhard D.; Vranas, Pavlos

2010-07-27

Methods, compute nodes, and computer program products are provided for direct memory access (`DMA`) transfer completion notification. Embodiments include determining, by an origin DMA engine on an origin compute node, whether a data descriptor for an application message to be sent to a target compute node is currently in an injection first-in-first-out (`FIFO`) buffer in dependence upon a sequence number previously associated with the data descriptor, the total number of descriptors currently in the injection FIFO buffer, and the current sequence number for the newest data descriptor stored in the injection FIFO buffer; and notifying a processor core on the origin DMA engine that the message has been sent if the data descriptor for the message is not currently in the injection FIFO buffer.

UHPLC-Q-TOF-MS-based metabolomics approach to compare the saponin compositions of Xueshuantong injection and Xuesaitong injection.

PubMed

Yao, Changliang; Yang, Wenzhi; Zhang, Jingxian; Qiu, Shi; Chen, Ming; Shi, Xiaojian; Pan, Huiqin; Wu, Wanying; Guo, Dean

2017-02-01

Various traditional Chinese medicine preparations developed from Notoginseng total saponins, including Xueshuantong injection and Xuesaitong injection, are extensively used in China to treat cardiocerebrovascular diseases. However, the difference of their saponin compositions remains unknown. An ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry based metabolomics approach was developed to probe the saponin discrimination between Xueshuantong and Xuesaitong and the related factors by large sample analysis. A highly efficient chromatographic separation was achieved on an HSS T3 column within 20 min with the holistic metabolites information recorded in the negative MS E mode. A six-step data pretreatment procedure mainly based on Progenesis QI and mass defect filtering was established. Pattern recognition chemometrics was used to discover the potential saponin markers. The saponin composition of Wuzhou Xueshuantong showed distinct discrimination from the other products. Wuzhou Xueshuantong contains more abundant protopanaxatriol-type noto-R 1 , Rg 1 , Re, and protopanaxadiol-type Rb 1 , but less Rd and other low-polarity protopanaxadiol-type ginsenosides. These differences could not directly correlate to the use of different parts of Panax notoginseng, but possibly to the different preparation techniques employed by different manufacturers. These results are beneficial to the establishment of pharmacopoeia standards and the assessment of the efficacy and adverse drug reactions for these homologous products. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Method for the quantification of vanadyl porphyrins in fractions of crude oils by High Performance Liquid Chromatography-Flow Injection-Inductively Coupled Plasma Mass Spectrometry

NASA Astrophysics Data System (ADS)

Wandekoken, Flávia G.; Duyck, Christiane B.; Fonseca, Teresa C. O.; Saint'Pierre, Tatiana D.

2016-05-01

High performance liquid chromatography hyphenated by flow injection to inductively coupled plasma mass spectrometry (HPLC-FI-ICP-MS) was used to investigate V linked to porphyrins present in fractions of crude oil. First, the crude oil sample was submitted to fractionation by preparative liquid chromatography with UV detection, at the porphyrin Soret band wavelength (400 nm). The obtained porphyrin fractions were then separated in a 250 mm single column, in the HPLC, and eluted with different mobile phases (methanol or methanol:toluene (80:20; v:v)). The quantification of V-porphyrins in the fractions eluted from HPLC was carried out by online measuring the 51V isotope in the ICP-MS, against vanadyl octaethylporphine standard solutions (VO-OEP), prepared in the same solvent as the mobile phase, and injected post-column directly into the plasma. A 20 μg L- 1 Ge in methanol was used as internal standard for minimizing non-spectral interference, such as short-term variations due to injection. The mathematical treatment of the signal based on Fast Fourier Transform smoothing algorithm was employed to improve the precision. The concentrations of V as V-porphyrins were between 2.7 and 11 mg kg- 1 in the fractions, which were close to the total concentration of V in the porphyrin fractions of the studied crude oil.

a bare Nanocapillary for DNA Separation and Genotyping analysis in Gel-Free solutions without application of external electric field

PubMed Central

Wang, Xiayan; Wang, Shili; Veerappan, Vijaykumar; Byun, Chang Kyu; Nguyen, Han; Gendhar, Brina; Allen, Randy D.; Liu, Shaorong

2009-01-01

In this work, we demonstrate DNA separation and genotyping analysis in gel-free solutions using a nanocapillary under pressure-driven conditions without application of an external electric field. The nanocapillary is a ~50-cm-long and 500-nm-radius bare fused silica capillary. After a DNA sample is injected, the analytes are eluted out in a chromatographic separation format. The elution order of DNA molecules follows strictly with their sizes, with the longer DNA being eluted out faster than the shorter ones. High resolutions are obtained for both short (a few bases) and long (tens of thousands of base pairs) DNA fragments. Effects of key experimental parameters, such as eluent composition and elution pressure, on separation efficiency and resolution are investigated. We also apply this technique for DNA separations of real-world genotyping samples to demonstrate its feasibility in biological applications. PCR products (without any purification) amplified from Arabidopsis plant genomic DNA crude preparations are directly injected into the nanocapillary, and PCR-amplified DNA fragments are well resolved, allowing for unambiguous identification of samples from heterozygous and homozygous individuals. Since the capillaries used to conduct the separations are uncoated, column lifetime is virtually unlimited. The only material that is consumed in these assays is the eluent, and hence the operation cost is low. PMID:18500828

Application of a novel large-volume injection method using a stomach-shaped inlet liner in capillary gas chromatographic trace analysis of dioxins in human milk and plasma.

PubMed

Saito, Koichi; Ohmura, Atsuko; Takekuma, Mikiko; Sasano, Ryoichi; Matsuki, Yasuhiko; Nakazawa, Hiroyuki

2007-06-01

A newly developed large-volume injection (LVI) technique that employs a unique stomach-shaped inlet liner (SSIL) inside of a programmable temperature vaporizer was used for the determination of trace amounts of dioxins in human milk and plasma. The initial temperature and the initial dwelling time of the inlet and the kind of solvent used were found to be critical in determining the analytical sensitivity of dioxins due to the loss of these relatively volatile compounds during solvent vaporization. Human milk and plasma were purified and fractionated by pre-packed multi-layered silica-gel chromatography and activated carbon silica-gel column chromatography. A 20-microL aliquot of the fraction collected from the chromatography with toluene was directly applied to the LVI system in high-resolution gas chromatography/high-resolution mass spectrometry. Excellent correlation (r > 0.97) between the values obtained by the LVI method using the SSIL device and those by the conventional regular-volume splitless injection method was obtained for PCDDs, PCDFs and non-ortho PCBs in human milk and plasma samples.

Evaluating outcome-correlated recruitment and geographic recruitment bias in a respondent-driven sample of people who inject drugs in Tijuana, Mexico

PubMed Central

Rudolph, Abby E.; Gaines, Tommi L.; Lozada, Remedios; Vera, Alicia; Brouwer, Kimberly C.

2015-01-01

Respondent-driven sampling’s (RDS) widespread use and reliance on untested assumptions suggests a need for new exploratory/diagnostic tests. We assessed geographic recruitment bias and outcome-correlated recruitment among 1048 RDS-recruited people who inject drugs (Tijuana, Mexico). Surveys gathered demographics, drug/sex behaviors, activity locations, and recruiter-recruit pairs. Simulations assessed geographic and network clustering of active syphilis (RPR titers≥1:8). Gender-specific predicted probabilities were estimated using logistic regression with GEE and robust standard errors. Active syphilis prevalence was 7% (crude: men=5.7% and women=16.6%; RDS-adjusted: men=6.7% and women=7.6%). Syphilis clustered in the Zona Norte, a neighborhood known for drug and sex markets. Network simulations revealed geographic recruitment bias and non-random recruitment by syphilis status. Gender-specific prevalence estimates accounting for clustering were highest among those living/working/injecting/buying drugs in the Zona Norte and directly/indirectly connected to syphilis cases (men:15.9%, women:25.6%) and lowest among those with neither exposure (men:3.0%, women:6.1%). Future RDS analyses should assess/account for network and spatial dependencies. PMID:24969586

Monitoring the occurrence of emerging contaminants in treated wastewater and groundwater between 2008 and 2010. The Baix Llobregat (Barcelona, Spain).

PubMed

Cabeza, Y; Candela, L; Ronen, D; Teijon, G

2012-11-15

The occurrence of 166 emerging compounds and four heavy metals (Cd, Ni, Hg and Pb) in treated wastewater and groundwater has been monitored at the Llobregat delta (Barcelona, Spain) over a period of 3 years. Selected compounds were pharmaceuticals, personal care products (PCPs), dioxins, polycyclic aromatic hydrocarbons (PAHs) and priority substances included in the 2008/105/CE Directive. Analysis was performed in tertiary treated wastewater (TWW), after an additional treatment of ultrafiltration reverse osmosis and UV disinfection, and groundwater from a deep confined aquifer. This aquifer is artificially recharged with TWW through injection wells. After the advanced treatment, 38 pharmaceuticals, 9 PCPs, 9 pesticides and 7 PAHs still showed a frequency of detection higher than 25% in the TWW, although at low concentration levels (ng/l). Not all active compounds found in the TWW were present in groundwater, indicating possible degradation within the aquifer media after the injection. A number of chemicals, mainly 10 pesticides and 10 pharmaceuticals were only present in groundwater samples, confirming a different origin than the injected TWW, probably agricultural activities and/or infiltration of poorly treated wastewater. Copyright © 2012 Elsevier B.V. All rights reserved.

Hydrologic monitoring of a waste-injection well near Milton, Florida, June 1975 - June 1977

USGS Publications Warehouse

Pascale, Charles A.; Martin, J.B.

1978-01-01

This report presents the hydraulic and chemical data collected from June 1, 1975, when injection began, to June 30, 1977 through a monitoring program at a deep-well waste-injection system at the American Cyanamid Company's plant near Milton, about 12 miles northwest of Pensacola. The injection system consists of a primary injection well, a standby injection well, and two deep monitor wells all completed open hole in the lower limestone of the Floridan aquifer and one shallow-monitor well completed in the upper limestone of the Floridan aquifer. Two of the monitor wells and the standby injection well are used to observe hydraulic and geochemical effects of waste injection in the injection zone at locations 8,180 feet northeast, 1,560 feet south, and 1,025 feet southwest of the primary injection well. The shallow-monitor well, used to observe any effects in the first permeable zone above the 200-foot-thick confining bed, is 28 feet north of the primary injection well. Since injection began in June 1975, 607 million gallons of treated industrial liquid waste with a pH of 4.6 to 6.3 and containing high concentrations of nitrate, organic nitrogen and carbon have been injected into a saline-water-filled limestone aquifer. Wellhead pressure at the injection well in June 1977 average 137 pounds per square inch and the hydraulic pressure gradient was 0.53 pound per square inch per foot of depth to the top of the injection zone. Water levels rose from 36 to 74 feet at the three wells used to monitor the injection zone during the 25-month period. The water level in the shallow-monitor well declined about 8 feet. No changes were detected in the chemical character of water from the shallow-monitor well and deep-monitor well-north. Increases in concentration of bicarbonate and dissolved organic carbon were detected in water from the deep-test monitor well in February 1976 and at the standby injection well in August 1976. In addition to increases in bicarbonate and dissolved organic carbon, sulfate, total organic nitrogen, and total nitrogen concentrations have also increased substantially in samples from these wells. Nitrogen gas concentrations in water samples collected at the three deep-monitor wells ranged from 19 to 176 milligrams per liter, methane from 4.5 to 11.4 milligrams per liter, and carbon dioxide from 7.7 to 44 milligrams per liter. The most probable number of denitrifying bacteria in water samples collected at the three deep-monitor wells ranged from less than 2 colonies to 17 colonies per 100 milliliters. None of the water samples collected in April 1977 at the three deep-monitor wells showed positive concentrations of acetone, ethanol, methanol, or acrylonitrile.

Analysis of peptides using an integrated microchip HPLC-MS/MS system.

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

Kirby, Brian J.; Chirica, Gabriela S.; Reichmuth, David S.

Hyphendated LC-MS techniques are quickly becoming the standard tool for protemic analyses. For large homogeneous samples, bulk processing methods and capillary injection and separation techniques are suitable. However, for analysis of small or heterogeneous samples, techniques that can manipulate picoliter samples without dilution are required or samples will be lost or corrupted; further, static nanospray-type flowrates are required to maximize SNR. Microchip-level integration of sample injection with separation and mass spectrometry allow small-volume analytes to be processed on chip and immediately injected without dilution for analysis. An on-chip HPLC was fabricated using in situ polymerization of both fixed and mobilemore » polymer monoliths. Integration of the chip with a nanospray MS emitter enables identification of peptides by the use of tandem MS. The chip is capable of analyzing of very small sample volumes (< 200 pl) in short times (< 3 min).« less

High-efficiency headspace sampling of volatile organic compounds in explosives using capillary microextraction of volatiles (CMV) coupled to gas chromatography-mass spectrometry (GC-MS).

PubMed

Fan, Wen; Almirall, José

2014-03-01

A novel geometry configuration based on sorbent-coated glass microfibers packed within a glass capillary is used to sample volatile organic compounds, dynamically, in the headspace of an open system or in a partially open system to achieve quantitative extraction of the available volatiles of explosives with negligible breakthrough. Air is sampled through the newly developed sorbent-packed 2 cm long, 2 mm diameter capillary microextraction of volatiles (CMV) and subsequently introduced into a commercially available thermal desorption probe fitted directly into a GC injection port. A sorbent coating surface area of ∼5 × 10(-2) m(2) or 5,000 times greater than that of a single solid-phase microextraction (SPME) fiber allows for fast (30 s), flow-through sampling of relatively large volumes using sampling flow rates of ∼1.5 L/min. A direct comparison of the new CMV extraction to a static (equilibrium) SPME extraction of the same headspace sample yields a 30 times improvement in sensitivity for the CMV when sampling nitroglycerine (NG), 2,4-dinitrotoluene (2,4-DNT), and diphenylamine (DPA) in a mixture containing a total mass of 500 ng of each analyte, when spiked into a liter-volume container. Calibration curves were established for all compounds studied, and the recovery was determined to be ∼1 % or better after only 1 min of sampling time. Quantitative analysis is also possible using this extraction technique when the sampling temperature, flow rate, and time are kept constant between calibration curves and the sample.

Determination of trace elements in automotive fuels by filter furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Anselmi, Anna; Tittarelli, Paolo; Katskov, Dmitri A.

2002-03-01

The determination of Cd, Cr, Cu, Pb and Ni was performed in gasoline and diesel fuel samples by electrothermal atomic absorption spectrometry using the Transverse Heated Filter Atomizer (THFA). Thermal conditions were experimentally defined for the investigated elements. The elements were analyzed without addition of chemical modifiers, using organometallic standards for the calibration. Forty-microliter samples were injected into the THFA. Gasoline samples were analyzed directly, while diesel fuel samples were diluted 1:4 with n-heptane. The following characteristic masses were obtained: 0.8 pg Cd, 6.4 pg Cr, 12 pg Cu, 17 pg Pb and 27 pg Ni. The limits of determination for gasoline samples were 0.13 μg/kg Cd, 0.4 μg/kg Cr, 0.9 μg/kg Cu, 1.5 μg/kg Pb and 2.5 μg/kg Ni. The corresponding limit of determination for diesel fuel samples was approximately four times higher for all elements. The element recovery was performed using the addition of organometallic compounds to gasoline and diesel fuel samples and was between 85 and 105% for all elements investigated.

Differentiating organic from conventional peppermints using chromatographic and flow-injection mass spectrometric (FIMS) fingerprints

USDA-ARS?s Scientific Manuscript database

High performance liquid chromatography (HPLC) and flow-injection mass spectrometric (FIMS) fingerprinting techniques were tested for their potential in differentiating organic and conventional peppermint samples. Ten organic and ten conventional peppermint samples were examined using HPLC-UV and FI...

Flame Tube NOx Emissions Using a Lean-Direct-Wall-Injection Combustor Concept

NASA Technical Reports Server (NTRS)

Tacina, Robert R.; Wey, Changlie; Choi, Kyung J.

2001-01-01

A low-NOx emissions combustor concept has been demonstrated in flame tube tests. A lean-direct injection concept was used where the fuel is injected directly into the flame zone and the overall fuel-air mixture is lean. In this concept the air is swirled upstream of a venturi section and the fuel is injected radially inward into the air stream from the throat section using a plain-orifice injector. Configurations have two-, four-, or six-wall fuel injectors and in some cases fuel is also injected from an axially located simplex pressure atomizer. Various orifice sizes of the plain-orifice injector were evaluated for the effect on NOx. Test conditions were inlet temperatures up to 8 1 OK, inlet pressures up to 2760 kPa, and flame temperatures up to 2100 K. A correlation is developed relating the NOx emissions to inlet temperature, inlet pressure, fuel-air ratio and pressure drop. Assuming that 15 percent of the combustion air would be used for liner cooling and using an advanced engine cycle, for the best configuration, the NOx emissions using the correlation is estimated to be <75 percent of the 1996 ICAO standard.

qPCR (quantitative polymerase chain reaction) for the quantification of bacteriophages in stream water samples to investigate hydrological processes: a proof-of-concept study in the Huewelerbach experimental catchment (Luxembourg)

NASA Astrophysics Data System (ADS)

Antonelli, Marta; Narayanan Balasubramanian, Mukundh; Ogorzaly, Leslie; Pfister, Laurent

2016-04-01

Albeit recent technological developments (e.g. field deployable instruments operating at high temporal frequencies), experimental hydrology is a discipline that remains measurement limited. From this perspective, trans-disciplinary approaches may create valuable opportunities to enlarge the amount of tools available for investigating hydrological processes. Bacteriophages have been widely used in hydrology as biological tracer for investigating colloid transport and contamination of ground water systems. However, there are only a few studies focusing on the employability of bacteriophages as surface water tracers (i.e. phage transport, system functioning). Here, we present a proof-of-concept study carried out in the Huewelerbach catchment in Luxembourg in December 2015. The aim of this study was to investigate how viral particles can be used to detect hydrological connectivity between the riparian zone/river bank and the stream during rainfall events. Moreover, this study is one of the first attempts for applying the qPCR (quantitative polymerase chain reaction) technique for the quantification of bacteriophages in stream water samples to investigate hydrological processes. This technique is very sensitive and has a large dynamic range - enhancing ease and speed of phage detection. We used two different male-specific coliphages (GA phage, genogroup II and SP phage, genogroup IV). Two litres of GA phage were injected directly in the stream as a slug injection and two litres of SP phage were poured next to the river bank (alluvial deposition) close to the injection point. We also added NaCl (200 g) to both phage suspensions. We collected stream water samples 100 m and 500 m downstream (i.e. catchment outlet) of the injection point for one week. Phages were concentrated through ultracentrifugation of 100 ml of water sample followed by quantification via qPCR. Conductivity in stream water was monitored for the entire duration of the experiment. Discharge was monitored both immediately upstream of the injection point and at the catchment outlet. Preliminary results show that at the catchment outlet, the GA-phage injected in stream displayed almost complete mass recovery (~93 %), in contrast to the partial recovery (~12%) of the SP phage that was introduced on the river bank. Additionally, the amount of GA phages detected 100 m downstream of the injection point evolved back to its background level after six days. We could not observe a similar evolution for the SP phage. At the outlet, the amount of both phages did not return to background levels after six days. This can be due to a combined action of the occurrence of preferential flowpaths and the behaviour of colloids. During the monitored rain event we observed a dilution effect on both phages and a slight increase of the quantity of SP phage right after the peak of discharge. This finding suggests a release of viral particles from the river bank. Overall, we have demonstrated with this proof-of-concept study the value of phages as eco-hydrological tracer.

Fluorescent blue lights, injecting drug use and related health risk in public conveniences: findings from a qualitative study of micro-injecting environments.

PubMed

Parkin, Stephen; Coomber, Ross

2010-07-01

This paper presents findings relating to injecting drug users' experiences and opinions of public toilets illuminated with fluorescent blue lights and presents an empirical assessment of the intended deterrent effect of such installations. Data analysis identified that blue lights deterred less than half the sample interviewed. Furthermore over half (18/31) of the sample were prepared to inject in conditions specifically designed to deter injecting practice. Of these, 11 respondents were completely undeterred and 7 individuals were only partially deterred by blue light environments. These findings are discussed within the interpretative frameworks of Pierre Bourdieu's theory of habitus and symbolic violence. The authors conclude that fluorescent blue lights contribute towards the development of situated resistance by injecting drug users within a public injecting habitus; a resistance that produces and reproduces drug-related harm and is a behaviour that opposes the symbolic violence of harm reduction intervention. The paper concludes with suggestions for theory-driven practical intervention that may seek to disrupt the harmful elements of the public injecting habitus. 2010 Elsevier Ltd. All rights reserved.

High variability of HIV and HCV seroprevalence and risk behaviours among people who inject drugs: results from a cross-sectional study using respondent-driven sampling in eight German cities (2011-14).

PubMed

Wenz, Benjamin; Nielsen, Stine; Gassowski, Martyna; Santos-Hövener, Claudia; Cai, Wei; Ross, R Stefan; Bock, Claus-Thomas; Ratsch, Boris-Alexander; Kücherer, Claudia; Bannert, Norbert; Bremer, Viviane; Hamouda, Osamah; Marcus, Ulrich; Zimmermann, Ruth

2016-09-05

People who inject drugs (PWID) are at increased risk of acquiring and transmitting HIV and Hepatitis C (HCV) due to sharing injection paraphernalia and unprotected sex. To generate seroprevalence data on HIV and HCV among PWID and related data on risk behaviour, a multicentre sero- and behavioural survey using respondent driven sampling (RDS) was conducted in eight German cities between 2011 and 2014. We also evaluated the feasibility and effectiveness of RDS for recruiting PWID in the study cities. Eligible for participation were people who had injected drugs within the last 12 months, were 16 years or older, and who consumed in one of the study cities. Participants were recruited, using low-threshold drop-in facilities as study sites. Initial seeds were selected to represent various sub-groups of people who inject drugs (PWID). Participants completed a face-to-face interview with a structured questionnaire about socio-demographics, sexual and injecting risk behaviours, as well as the utilisation of health services. Capillary blood samples were collected as dried blood spots and were anonymously tested for serological and molecular markers of HIV and HCV. The results are shown as range of proportions (min. and max. values (%)) in the respective study cities. For evaluation of the sampling method we applied criteria from the STROBE guidelines. Overall, 2,077 PWID were recruited. The range of age medians was 29-41 years, 18.5-35.3 % of participants were female, and 9.2-30.6 % were foreign born. Median time span since first injection were 10-18 years. Injecting during the last 30 days was reported by 76.0-88.4 % of participants. Sharing needle/syringes (last 30 days) ranged between 4.7 and 22.3 %, while sharing unsterile paraphernalia (spoon, filter, water, last 30 days) was reported by 33.0-43.8 %. A majority of participants (72.8-85.8 %) reported incarceration at least once, and 17.8-39.8 % had injected while incarcerated. Between 30.8 and 66.2 % were currently in opioid substitution therapy. Unweighted HIV seroprevalence ranged from 0-9.1 %, HCV from 42.3-75.0 %, and HCV-RNA from 23.1-54.0 %. The implementation of RDS as a recruiting method in cooperation with low-threshold drop in facilities was well accepted by both staff and PWID. We reached our targeted sample size in seven of eight cities. In the recruited sample of mostly current injectors with a long duration of injecting drug use, seroprevalence for HIV and HCV varied greatly between the city samples. HCV was endemic among participants in all city samples. Our results demonstrate the necessity of intensified prevention strategies for blood-borne infections among PWID in Germany.

An efficient approach for Mars Sample Return using emerging commercial capabilities

NASA Astrophysics Data System (ADS)

Gonzales, Andrew A.; Stoker, Carol R.

2016-06-01

Mars Sample Return is the highest priority science mission for the next decade as recommended by the 2011 Decadal Survey of Planetary Science (Squyres, 2011 [1]). This article presents the results of a feasibility study for a Mars Sample Return mission that efficiently uses emerging commercial capabilities expected to be available in the near future. The motivation of our study was the recognition that emerging commercial capabilities might be used to perform Mars Sample Return with an Earth-direct architecture, and that this may offer a desirable simpler and lower cost approach. The objective of the study was to determine whether these capabilities can be used to optimize the number of mission systems and launches required to return the samples, with the goal of achieving the desired simplicity. All of the major element required for the Mars Sample Return mission are described. Mission system elements were analyzed with either direct techniques or by using parametric mass estimating relationships. The analysis shows the feasibility of a complete and closed Mars Sample Return mission design based on the following scenario: A SpaceX Falcon Heavy launch vehicle places a modified version of a SpaceX Dragon capsule, referred to as ;Red Dragon;, onto a Trans Mars Injection trajectory. The capsule carries all the hardware needed to return to Earth Orbit samples collected by a prior mission, such as the planned NASA Mars 2020 sample collection rover. The payload includes a fully fueled Mars Ascent Vehicle; a fueled Earth Return Vehicle, support equipment, and a mechanism to transfer samples from the sample cache system onboard the rover to the Earth Return Vehicle. The Red Dragon descends to land on the surface of Mars using Supersonic Retropropulsion. After collected samples are transferred to the Earth Return Vehicle, the single-stage Mars Ascent Vehicle launches the Earth Return Vehicle from the surface of Mars to a Mars phasing orbit. After a brief phasing period, the Earth Return Vehicle performs a Trans Earth Injection burn. Once near Earth, the Earth Return Vehicle performs Earth and lunar swing-bys and is placed into a Lunar Trailing Orbit-an Earth orbit, at lunar distance. A retrieval mission then performs a rendezvous with the Earth Return Vehicle, retrieves the sample container, and breaks the chain of contact with Mars by transferring the sample into a sterile and secure container. With the sample contained, the retrieving spacecraft makes a controlled Earth re-entry preventing any unintended release of Martian materials into the Earth's biosphere. The mission can start in any one of three Earth to Mars launch opportunities, beginning in 2022.

An Efficient Approach for Mars Sample Return Using Emerging Commercial Capabilities.

PubMed

Gonzales, Andrew A; Stoker, Carol R

2016-06-01

Mars Sample Return is the highest priority science mission for the next decade as recommended by the 2011 Decadal Survey of Planetary Science [1]. This article presents the results of a feasibility study for a Mars Sample Return mission that efficiently uses emerging commercial capabilities expected to be available in the near future. The motivation of our study was the recognition that emerging commercial capabilities might be used to perform Mars Sample Return with an Earth-direct architecture, and that this may offer a desirable simpler and lower cost approach. The objective of the study was to determine whether these capabilities can be used to optimize the number of mission systems and launches required to return the samples, with the goal of achieving the desired simplicity. All of the major element required for the Mars Sample Return mission are described. Mission system elements were analyzed with either direct techniques or by using parametric mass estimating relationships. The analysis shows the feasibility of a complete and closed Mars Sample Return mission design based on the following scenario: A SpaceX Falcon Heavy launch vehicle places a modified version of a SpaceX Dragon capsule, referred to as "Red Dragon", onto a Trans Mars Injection trajectory. The capsule carries all the hardware needed to return to Earth Orbit samples collected by a prior mission, such as the planned NASA Mars 2020 sample collection rover. The payload includes a fully fueled Mars Ascent Vehicle; a fueled Earth Return Vehicle, support equipment, and a mechanism to transfer samples from the sample cache system onboard the rover to the Earth Return Vehicle. The Red Dragon descends to land on the surface of Mars using Supersonic Retropropulsion. After collected samples are transferred to the Earth Return Vehicle, the single-stage Mars Ascent Vehicle launches the Earth Return Vehicle from the surface of Mars to a Mars phasing orbit. After a brief phasing period, the Earth Return Vehicle performs a Trans Earth Injection burn. Once near Earth, the Earth Return Vehicle performs Earth and lunar swing-bys and is placed into a Lunar Trailing Orbit - an Earth orbit, at lunar distance. A retrieval mission then performs a rendezvous with the Earth Return Vehicle, retrieves the sample container, and breaks the chain of contact with Mars by transferring the sample into a sterile and secure container. With the sample contained, the retrieving spacecraft makes a controlled Earth re-entry preventing any unintended release of Martian materials into the Earth's biosphere. The mission can start in any one of three Earth to Mars launch opportunities, beginning in 2022.

An Efficient Approach for Mars Sample Return Using Emerging Commercial Capabilities

PubMed Central

Gonzales, Andrew A.; Stoker, Carol R.

2016-01-01

Mars Sample Return is the highest priority science mission for the next decade as recommended by the 2011 Decadal Survey of Planetary Science [1]. This article presents the results of a feasibility study for a Mars Sample Return mission that efficiently uses emerging commercial capabilities expected to be available in the near future. The motivation of our study was the recognition that emerging commercial capabilities might be used to perform Mars Sample Return with an Earth-direct architecture, and that this may offer a desirable simpler and lower cost approach. The objective of the study was to determine whether these capabilities can be used to optimize the number of mission systems and launches required to return the samples, with the goal of achieving the desired simplicity. All of the major element required for the Mars Sample Return mission are described. Mission system elements were analyzed with either direct techniques or by using parametric mass estimating relationships. The analysis shows the feasibility of a complete and closed Mars Sample Return mission design based on the following scenario: A SpaceX Falcon Heavy launch vehicle places a modified version of a SpaceX Dragon capsule, referred to as “Red Dragon”, onto a Trans Mars Injection trajectory. The capsule carries all the hardware needed to return to Earth Orbit samples collected by a prior mission, such as the planned NASA Mars 2020 sample collection rover. The payload includes a fully fueled Mars Ascent Vehicle; a fueled Earth Return Vehicle, support equipment, and a mechanism to transfer samples from the sample cache system onboard the rover to the Earth Return Vehicle. The Red Dragon descends to land on the surface of Mars using Supersonic Retropropulsion. After collected samples are transferred to the Earth Return Vehicle, the single-stage Mars Ascent Vehicle launches the Earth Return Vehicle from the surface of Mars to a Mars phasing orbit. After a brief phasing period, the Earth Return Vehicle performs a Trans Earth Injection burn. Once near Earth, the Earth Return Vehicle performs Earth and lunar swing-bys and is placed into a Lunar Trailing Orbit - an Earth orbit, at lunar distance. A retrieval mission then performs a rendezvous with the Earth Return Vehicle, retrieves the sample container, and breaks the chain of contact with Mars by transferring the sample into a sterile and secure container. With the sample contained, the retrieving spacecraft makes a controlled Earth re-entry preventing any unintended release of Martian materials into the Earth’s biosphere. The mission can start in any one of three Earth to Mars launch opportunities, beginning in 2022. PMID:27642199

Preferential flow pathways revealed by field based stable isotope analysis of CO2 by mid-infrared laser spectroscopy

NASA Astrophysics Data System (ADS)

van Geldern, Robert; Nowak, Martin; Zimmer, Martin; Szizybalski, Alexandra; Myrttinen, Anssi; Barth, Johannes A. C.; Jost, Hj

2016-04-01

A newly developed and commercially available isotope ratio laser spectrometer for CO2 analyses has been tested during a 10-day field monitoring campaign at the Ketzin pilot site for CO2 storage in northern Germany. The laser instrument is based on tunable laser direct absorption in the mid-infrared. The instrument recorded a continuous 10-day carbon stable isotope data set with 30 minutes resolution directly on-site in a field-based laboratory container during a tracer experiment. To test the instruments performance and accuracy the monitoring campaign was accompanied by daily CO2 sampling for laboratory analyses with isotope ratio mass spectrometry (IRMS). The carbon stable isotope ratios measured by conventional IRMS technique and by the new mid-infrared laser spectrometer agree remarkably well within 2σ analytical precision (<0.3 ‰). This proves the capability of the new mid-infrared direct absorption technique to measure high precision and accurate real-time table isotope data directly in the field. The injected CO2 tracer had a distinct δ13C value that was largely different from the reservoir background value. The laser spectroscopy data revealed a prior to this study unknown, intensive dynamic with fast changing δ13C values. The arrival pattern of the tracer suggest that the observed fluctuations were probably caused by migration along separate and distinct preferential flow paths between injection well and observation well. The new technique might contribute to a better tracing of the migration of the underground CO2 plume and help to ensure the long-term integrity of the reservoir.

On-Line Derivatization Gas Chromatography Ion Trap Mass Spectrometry for Determination of Endocrine Disruptors in Surface Water

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

Tzing, Shin-Hwa; Chang, Jia-Yaw; Ling, Yong-Chien

2004-03-31

A method has been developed for the determination of endocrine disruptors (EDs) (containing hydroxyl groups) in surface water from different sources. The surface water samples from different sites including school and local dormitory sewage effluents, lake water and river water were collected and analyzed. In this method, the pretreated sample is directly analyzed by GC-MS using on-line derivatization, where tetramethylammonium hydroxide (TMA-OH) was used as the derivatizing agent. Use of large-volume direct sample introduction (DSI) and co-injection of the sample and TMAOH avoids external contaminations as observed in conventional derivatization protocols. Additionally, the use of chemical ionization (CI) and CI-MS/MSmore » could enable detection of EDs at lower concentrations and reduce the matrices' interference thereby enhancing detection sensitivity of EDs for quantification. In this work, the use of dichloromethane as CI reagent for EDs is reported for the first time and could detect EDs to concentrations as low as 0.5 pg/mL. The recovery ranged from 74 to 112 % and the relative standard derivations for replicate analyses ranged from 5 to 17 %. We hope that this method will be applicable for routine analysis of EDs with hydroxyl functional groups.« less

Sequential injection spectrophotometric determination of oxybenzone in lipsticks.

PubMed

Salvador, A; Chisvert, A; Camarasa, A; Pascual-Martí, M C; March, J G

2001-08-01

A sequential injection (SI) procedure for the spectrophotometric determination of oxybenzone in lipsticks is reported. The colorimetric reaction between nickel and oxybenzone was used. SI parameters such as sample solution volume, reagent solution volume, propulsion flow rate and reaction coil length were studied. The limit of detection was 3 microg ml(-1). The sensitivity was 0.0108+/-0.0002 ml microg(-1). The relative standard deviations of the results were between 6 and 12%. The real concentrations of samples and the values obtained by HPLC were comparable. Microwave sample pre-treatment allowed the extraction of oxybenzone with ethanol, thus avoiding the use of toxic organic solvents. Ethanol was also used as carrier in the SI system. Seventy-two injections per hour can be performed, which means a sample frequency of 24 h(-1) if three replicates are measured for each sample.

Employment-Based Reinforcement of Adherence to Depot Naltrexone in Unemployed Opioid-Dependent Adults: A Randomized Controlled Trial

PubMed Central

Everly, Jeffrey J.; DeFulio, Anthony; Koffarnus, Mikhail N.; Leoutsakos, Jeannie-Marie S.; Donlin, Wendy D.; Aklin, Will M.; Umbricht, Annie; Fingerhood, Michael; Bigelow, George E.; Silverman, Kenneth

2011-01-01

Aims Naltrexone can be used to treat opioid dependence, but patients refuse to take it. Extended-release depot formulations may improve adherence, but long-term adherence rates to depot naltrexone are not known. This study determined long-term rates of adherence to depot naltrexone and whether employment-based reinforcement can improve adherence. Design Participants who were inducted onto oral naltrexone were randomly assigned to Contingency (n=18) or Prescription (n=17) groups. Participants were offered six depot naltrexone injections and invited to work at the therapeutic workplace weekdays for 26 weeks where they earned stipends for participating in job skills training. Contingency participants were required to accept naltrexone injections to maintain workplace access and to maintain maximum pay. Prescription participants could work independent of whether they accepted injections. Setting The therapeutic workplace, a model employment-based intervention for drug addiction and unemployment. Participants Opioid-dependent unemployed adults. Measurements Depot naltrexone injections accepted and opiate-negative urine samples. Findings Contingency participants accepted significantly more naltrexone injections than Prescription participants (81% versus 42%), and were more likely to accept all injections (66% versus 35%). At monthly assessments (with missing urine samples imputed as positive), the groups provided similar percentages of samples negative for opiates (74% versus 62%) and for cocaine (56% versus 54%). Opiate positive samples were more likely when samples were also positive for cocaine. Conclusions Employment-based reinforcement can maintain adherence to depot naltrexone. Future research should determine whether persistent cocaine use compromises naltrexone's effect on opiate use. Workplaces may be useful for promoting sustained adherence to depot naltrexone. PMID:21320227

Dilution effects on ultrafine particle emissions from Euro 5 and Euro 6 diesel and gasoline vehicles

NASA Astrophysics Data System (ADS)

Louis, Cédric; Liu, Yao; Martinet, Simon; D'Anna, Barbara; Valiente, Alvaro Martinez; Boreave, Antoinette; R'Mili, Badr; Tassel, Patrick; Perret, Pascal; André, Michel

2017-11-01

Dilution and temperature used during sampling of vehicle exhaust can modify particle number concentration and size distribution. Two experiments were performed on a chassis dynamometer to assess exhaust dilution and temperature on particle number and particle size distribution for Euro 5 and Euro 6 vehicles. In the first experiment, the effects of dilution (ratio from 8 to 4 000) and temperature (ranging from 50 °C to 150 °C) on particle quantification were investigated directly from tailpipe for a diesel and a gasoline Euro 5 vehicles. In the second experiment, particle emissions from Euro 6 diesel and gasoline vehicles directly sampled from the tailpipe were compared to the constant volume sampling (CVS) measurements under similar sampling conditions. Low primary dilutions (3-5) induced an increase in particle number concentration by a factor of 2 compared to high primary dilutions (12-20). Low dilution temperatures (50 °C) induced 1.4-3 times higher particle number concentration than high dilution temperatures (150 °C). For the Euro 6 gasoline vehicle with direct injection, constant volume sampling (CVS) particle number concentrations were higher than after the tailpipe by a factor of 6, 80 and 22 for Artemis urban, road and motorway, respectively. For the same vehicle, particle size distribution measured after the tailpipe was centred on 10 nm, and particles were smaller than the ones measured after CVS that was centred between 50 nm and 70 nm. The high particle concentration (≈106 #/cm3) and the growth of diameter, measured in the CVS, highlighted aerosol transformations, such as nucleation, condensation and coagulation occurring in the sampling system and this might have biased the particle measurements.

Development and Validation of a Fast Procedure to Analyze Amoxicillin in River Waters by Direct-Injection LC-MS/MS

ERIC Educational Resources Information Center

Homem, Vera; Alves, Arminda; Santos, Lu´cia

2014-01-01

A laboratory application with a strong component in analytical chemistry was designed for undergraduate students, in order to introduce a current problem in the environmental science field, the water contamination by antibiotics. Therefore, a simple and rapid method based on direct injection and high performance liquid chromatography-tandem mass…

Gaseous Emissions Results from a Three-Cup Flametube Test of a Third-Generation Swirl-Venturi Lean Direct Injection Combustion Concept

NASA Technical Reports Server (NTRS)

Tacina, Kathleen M.; Podboy, Derek P.; Lee, Phil; Dam, Bidhan

2017-01-01

This paper summarizes the development of lean direct injection (LDI) combustor technology at, or in collaboration with, the NASA Glenn Research Center. These configurations differ mainly in fuel-air mixing strategy. The paper reviews the NOx performance and operability characteristics of multiple LDI configurations tested at NASA Glenn.

Vertical-Deformation, Water-Level, Microgravity, Geodetic, Water-Chemistry, and Flow-Rate Data Collected During Injection, Storage, and Recovery Tests at Lancaster, Antelope Valley, California, September 1995 Through September 1998

DTIC Science & Technology

2002-01-01

63 Tiltmeter Network...71 34. Map showing locations of tiltmeters used to monitor the magnitude and direction of ground tilting associated with direct well injection...during cycle 2 at Lancaster, Antelope Valley, California .............................. 72 35. Photograph showing typical tiltmeter installation for

Flex-Fuel Two-Stroke Snowmobile: Development of a Flex-Fuel, Two-Stroke, Direct-Injection Snowmobile for Use in the Clean Snowmobile Challenge and National Parks

DOT National Transportation Integrated Search

2009-09-01

The University of Idaho's entry into the 2009 SAE Clean Snowmobile Challenge (CSC) was a semi-direct-injection (SDI) two-stroke powered REV-XP snowmobile modified to use flex fuel. The flex fuel engine produces stock engine power on any blend of etha...

Plasma metabonomics study on toxicity biomarker in rats treated with Euphorbia fischeriana based on LC-MS.

PubMed

Wang, Yingfeng; Man, Hongxue; Gao, Jian; Liu, Xinfeng; Ren, Xiaolei; Chen, Jianxin; Zhang, Jiayu; Gao, Kuo; Li, Zhongfeng; Zhao, Baosheng

2016-09-01

Lang-du (LD) has been traditionally used to treat human diseases in China. Plasma metabolic profiling was applied in this study based on LC-MS to elucidate the toxicity in rats induced by injected ethanol extract of LD. LD injection was given by intraperitoneal injection at doses of 0.1, 0.05, 0.025 and 0 g kg(-1) body weight per day to rats. The blood biochemical levels of alanine aminotransferase, direct bilirubin, creatinine, serum β2-microglobulin and low-density lipoprotein increased in LD-injected rats, and the levels of total protein and albumin decreased in these groups. The metabolic profiles of the samples were analyzed by multivariate statistics analysis, including principal component analysis, partial least squares discriminant analysis and orthogonal projection to latent structures discriminate analysis (OPLS-DA). The metabolic characters in rats injected with LD were perturbed in a dose-dependent manner. By OPLS-DA, 18 metabolites were served as the potential toxicity biomarkers. Moreover, LD treatment resulted in an increase in the p-cresol, p-cresol sulfate, lysophosphatidylethanolamine (LPE) (18:0), LPE (16:0), lysophosphatidylcholine (16:0) and 12-HETE concentrations, and a decrease in hippuric acid, cholic acid and N-acetyl-l-phenylalanine. These results suggested that chronic exposure to LD could cause a disturbance in lipids metabolism and amino acids metabolism, etc. Therefore, an analysis of the metabolic profiles can contribute to a better understanding of the adverse effects of LD. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Evaluation of bromide mass discharge in a sandy aquifer at Vandenberg AFB, CA

NASA Astrophysics Data System (ADS)

Mackay, D. M.; Rasa, E.; Einarson, M.; Kaiser, P.; Chakraborty, I.; Scow, K. M.

2009-12-01

Side-by-side experiments were conducted by UC Davis research team at a former fuel station at Vandenberg Air Force Base (AFB) to evaluate the rate of transformation of methyl tert-butyl ether (MTBE) to tert-butyl alcohol (TBA) impacted by ethanol and to investigate evidence of TBA degradation under sulfate reducing conditions. On one side we injected groundwater amended with ethanol and MTBE. In the other lane we injected groundwater amended with TBA. On both sides, injected ground water was spiked with bromide tracer to provide estimates of groundwater flow direction variations, flow velocity, dispersion, and mobile mass loss resulting from diffusive sequestration into aquitards. 162 monitoring wells were aligned into seven transects located downgradient of the injection wells. The mass discharge approach was used to evaluate the natural attenuation of the injected constituents. In this talk we will focus on calculations of mass discharge of the bromide tracer at each of the seven monitoring well transects. The amount of bromide mass discharged through each transect was calculated for any sampling time using field measurements of break through curves. Cumulative mass discharges were estimated and, by iteration based on mass balance, the flow properties of the aquifer were estimated. The calibration process resulted in subtle but quantitatively important changes in our assumptions regarding key physical properties of the aquifer (thickness, porosity) which could be only approximately estimated by standard methods (coring, CPT, etc.). On the basis of this calibration, a more robust approach was devised for evaluating the source and fate of TBA in the aquifer.

Do patients with structural abnormalities of the shoulder experience pain after MR arthrography of the shoulder?

PubMed

Steurer-Dober, Isabelle; Rufibach, Kaspar; Hodler, Juerg; Saupe, Nadja; Zanetti, Marco; Fucentese, Sandro F; Pfirrmann, Christian W A

2010-09-01

To assess the pain course after intraarticular injection of a gadolinium-containing contrast material admixed with anesthetic for magnetic resonance (MR) arthrography of the shoulder in relation to internal derangements of the shoulder. Institutional review board approval and informed consent were obtained for this study. The study sample consisted of 655 consecutive patients (249 female, 406 male; median age, 54 years) referred for MR arthrography of the shoulder. Pain level was measured at baseline, directly after intraarticular injection of the gadolinium-containing contrast material admixed with anesthetic, 4 hours after injection, 1 day (18-30 hours) after injection, and 1 week (6-8 days) after injection with a visual analog scale (range, 0-10). MR arthrography was used to assess the following internal derangements: lesions of the rotator cuff tendons and long biceps tendon, adhesive capsulitis (frozen shoulder), fluid in the subacromial bursa, labral tears, and osteoarthritis of the glenohumeral joint. History of shoulder surgery was recorded. Linear regression models were calculated for the dependent variable (difference between follow-up pain and baseline pain), with the independent variable grouping adjusted for age and sex. There was no significant association between pain level over time and internal derangements of the shoulder, nor was there significant association between pain level over time in patients with a history of shoulder surgery and patients without a history of shoulder surgery. Neither internal derangements nor prior surgery have an apparent effect on the pain course after MR arthrography of the shoulder. (c) RSNA, 2010.

Rapid measurement of plasma free fatty acid concentration and isotopic enrichment using LC/MS

PubMed Central

Persson, Xuan-Mai T.; Błachnio-Zabielska, Agnieszka Urszula; Jensen, Michael D.

2010-01-01

Measurements of plasma free fatty acids (FFA) concentration and isotopic enrichment are commonly used to evaluate FFA metabolism. Until now, gas chromatography-combustion-isotope ratio mass spectrometry (GC/C/IRMS) was the best method to measure isotopic enrichment in the methyl derivatives of 13C-labeled fatty acids. Although IRMS is excellent for analyzing enrichment, it requires time-consuming derivatization steps and is not optimal for measuring FFA concentrations. We developed a new, rapid, and reliable method for simultaneous quantification of 13C-labeled fatty acids in plasma using high-performance liquid chromatography-mass spectrometry (HPLC/MS). This method involves a very quick Dole extraction procedure and direct injection of the samples on the HPLC system. After chromatographic separation, the samples are directed to the mass spectrometer for electrospray ionization (ESI) and analysis in the negative mode using single ion monitoring. By employing equipment with two columns connected parallel to a mass spectrometer, we can double the throughput to the mass spectrometer, reducing the analysis time per sample to 5 min. Palmitate flux measured using this approach agreed well with the GC/C/IRMS method. This HPLC/MS method provides accurate and precise measures of FFA concentration and enrichment. PMID:20526002

Transient neurologic deficit after spinal anesthesia: local anesthetic maldistribution with pencil point needles?

PubMed

Beardsley, D; Holman, S; Gantt, R; Robinson, R A; Lindsey, J; Bazaral, M; Stewart, S F; Stevens, R A

1995-08-01

Recent reports of transient neurologic deficits have raised concern about the potential toxicity of single-dose spinal 5% lidocaine in 7.5% dextrose. Two cases of volunteers who experienced minor local sensory deficits after slow (60 s) injections of 2 mL 5% lidocaine via Whitacre needles are described. One case was a result of a double injection because of a "failed" block. It seemed possible that the neurologic deficit in these cases resulted from neurotoxicity associated with maldistribution of local anesthetic. Using an in vitro spinal model, we investigated drug distribution resulting from injections through side-port spinal needles to determine whether the use of these needles could result in high local concentrations of hyperbaric solutions. A spinal canal model was fabricated using human magnetic resonance measurements. The model was placed in a surgical supine position and filled with lactated Ringer's solution to simulate the specific gravity of cerebral spinal fluid at 22 degrees C. A hyperbaric solution of phthalocyanine blue dye and dextrose (SG 1.042), simulating the anesthetic, was injected through three different needles (27-gauge 4 11/16-in. Whitacre, 25-gauge 3 1/2-in. Whitacre, 25-gauge 3 1/2-in. Quincke). Triplicate injections were done at rapid (2 mL/10 s) and slow (2 mL/60 s) rates, with needle side ports oriented in a sacral and cephalad direction. At slow rates of injection, using 27- or 25-gauge sacrally directed Whitacre needles, injections showed evidence of maldistribution with extrapolated peak sacral lidocaine concentrations reaching 2.0%. In contrast, distribution after slow injection through sacrally directed Quincke needles was uniform.(ABSTRACT TRUNCATED AT 250 WORDS)

Liquid Microjunction Surface Sampling Probe Fluid Dynamics: Computational and Experimental Analysis of Coaxial Intercapillary Positioning Effects on Sample Manipulation

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

ElNaggar, Mariam S; Barbier, Charlotte N; Van Berkel, Gary J

A coaxial geometry liquid microjunction surface sampling probe (LMJ-SSP) enables direct extraction of analytes from surfaces for subsequent analysis by techniques like mass spectrometry. Solution dynamics at the probe-to-sample surface interface in the LMJ-SSP has been suspected to influence sampling efficiency and dispersion but has not been rigorously investigated. The effect on flow dynamics and analyte transport to the mass spectrometer caused by coaxial retraction of the inner and outer capillaries from each other and the surface during sampling with a LMJ-SSP was investigated using computational fluid dynamics and experimentation. A transparent LMJ-SSP was constructed to provide the means formore » visual observation of the dynamics of the surface sampling process. Visual observation, computational fluid dynamics (CFD) analysis, and experimental results revealed that inner capillary axial retraction from the flush position relative to the outer capillary transitioned the probe from a continuous sampling and injection mode through an intermediate regime to sample plug formationmode caused by eddy currents at the sampling end of the probe. The potential for analytical implementation of these newly discovered probe operational modes is discussed.« less

Analytical method development for directed enzyme evolution research: a high throughput high-performance liquid chromatography method for analysis of ribose and ribitol and a capillary electrophoresis method for the separation of ribose enantiomers.

PubMed

Sun, Baoguo; Miller, Gregory; Lee, Wan Yee; Ho, Kelvin; Crowe, Michael A; Partridge, Leslie

2013-01-04

Analytical methods were developed for a directed enzyme evolution research programme, which pursued high performance enzymes to produce high quality L-ribose using large scale biocatalytic reaction. A high throughput HPLC method with evaporative light-scattering detection was developed to test ribose and ribitol in the enzymatic reaction, a β-cyclobond 2000 analytical column separated ribose and ribitol in 2.3 min, a C(18) guard column was used as an on-line filter to clean up the enzyme sample matrix and a short gradient was applied to wash the column, the enzymatic reaction solution can be directly injected after quenching. Total run time of each sample was approx. 4 min which provided capability of screening 4×96-well plates/day/instrument. Meanwhile, a capillary electrophoresis method was developed for the separation of ribose enantiomers, while 7-aminonaphthalene-1,3-disulfonic acid was used as derivatisation reagent and 25 mM tetraborate with 5 mM β-cyclodextrin was used as electrolyte. 0.35%of D-ribose in L-ribose can be detected which can be translated into 99.3% ee of L-ribose. Derivatisation reagent and sample matrix did not interfere with the measurement. Copyright © 2012 Elsevier B.V. All rights reserved.

Structure development in melt processing isotactic polypropylene, polypropylene blends/compounds and dynamically vulcanized polyolefin TPEs

NASA Astrophysics Data System (ADS)

Yu, Yishan

The influence of various fillers, nucleating agents and ethylene propylene diene terpolymer (EPDM) additive on crystalline modification (alpha-, beta- and smectic forms) and crystalline orientation of polypropylene in die extrudates, melt spun filaments, thick rods, blow molded bottles and injection molded parts of isotactic polypropylene (PP), its blends/compounds and dynamically vulcanized polypropylene thermoplastic elastomers (TPEs) were experimentally studied under a range of cooling and processing conditions. The phenomena of crystallization, polymorphism and orientation in processing of both thin and thick samples (filaments, rods, bottles and injection molded parts) were simulated through transport laws incorporating polymer crystallization kinetics. Continuous cooling transformation (CCT) curves for the various material systems investigated were developed under quiescent and uniaxial stress conditions. We applied experimental data on polymorphism of thin sections to predict crystalline structure variation in thick parts. The predictions were consistent with experiments. For filaments, the polypropylene crystalline orientation-spinline stress relationship is generally similar for the neat PP, blends/compounds and TPEs. However, the blends and TPEs have much lower birefringence apparently due to a lack of orientation in the rubber phase. It was shown that the polypropylene contribution to the birefringence for the neat PP and its blends is the same at the same spinline stress. For bottles, the inflation pressures used have little effect on orientation of either polypropylene crystals or disc-shaped talc filler. The talc discs are highly oriented parallel to the bottle surface. For the bottles without talc, the orientation of polypropylene crystallographic axes are low. The polypropylene crystallographic b-axes in the talc filled bottles are more highly oriented. For injection molded parts, it was found that a low orientation layer exists between the part surface and an intermediate highly oriented layer in the parts of neat PP and its blends/compounds. The thickness of this layer increases as the injection pressure decreases. This layer was not formed in the TPE parts. This would seem to be associated with the TPEs exhibiting a yield stress in shear flow and not exhibiting fountain flow in mold filling. For all parts studied, the orientation characteristics of polypropylene crystallographic axes in the highly oriented layer are similar from sample to sample. The strong orientation of the c-axis parallel to the machine direction and the b-axis perpendicular to the machine direction are observed in the highly oriented layer. The talc discs in both the highly oriented layer and the intermediate position are highly oriented parallel to the part face due to melt flow. At intermediate position in the talc-filled parts, the polypropylene crystallographic (040) planes prefer to align themselves parallel to the part surface but are not so well oriented when the talc is absent.

Graphite furnace atomic absorption spectrometric determination of vanadium after cloud point extraction in the presence of graphene oxide

NASA Astrophysics Data System (ADS)

López-García, Ignacio; Marín-Hernández, Juan José; Hernández-Córdoba, Manuel

2018-05-01

Vanadium (V) and vanadium (IV) in the presence of a small concentration of graphene oxide (0.05 mg mL-1) are quantitatively transferred to the coacervate obtained with Triton X-114 in a cloud point microextraction process. The surfactant-rich phase is directly injected into the graphite atomizer of an atomic absorption spectrometer. Using a 10-mL aliquot sample and 150 μL of a 15% Triton X-114 solution, the enrichment factor for the analyte is 103, which results in a detection limit of 0.02 μg L-1 vanadium. The separation of V(V) and V(IV) using an ion-exchanger allows speciation of the element at low concentrations. Data for seven reference water samples with certified vanadium contents confirm the reliability of the procedure. Several beer samples are also analyzed, those supplied as canned drinks showing low levels of tetravalent vanadium.

Eos modeling and reservoir simulation study of bakken gas injection improved oil recovery in the elm coulee field, Montana

NASA Astrophysics Data System (ADS)

Pu, Wanli

The Bakken Formation in the Williston Basin is one of the most productive liquid-rich unconventional plays. The Bakken Formation is divided into three members, and the Middle Bakken Member is the primary target for horizontal wellbore landing and hydraulic fracturing because of its better rock properties. Even with this new technology, the primary recovery factor is believed to be only around 10%. This study is to evaluate various gas injection EOR methods to try to improve on that low recovery factor of 10%. In this study, the Elm Coulee Oil Field in the Williston Basin was selected as the area of interest. Static reservoir models featuring the rock property heterogeneity of the Middle Bakken Member were built, and fluid property models were built based on Bakken reservoir fluid sample PVT data. By employing both compositional model simulation and Todd-Longstaff solvent model simulation methods, miscible gas injections were simulated and the simulations speculated that oil recovery increased by 10% to 20% of OOIP in 30 years. The compositional simulations yielded lower oil recovery compared to the solvent model simulations. Compared to the homogeneous model, the reservoir model featuring rock property heterogeneity in the vertical direction resulted in slightly better oil recovery, but with earlier CO2 break-through and larger CO2 production, suggesting that rock property heterogeneity is an important property for modeling because it has a big effect on the simulation results. Long hydraulic fractures shortened CO2 break-through time greatly and increased CO 2 production. Water-alternating-gas injection schemes and injection-alternating-shut-in schemes can provide more options for gas injection EOR projects, especially for gas production management. Compared to CO2 injection, separator gas injection yielded slightly better oil recovery, meaning separator gas could be a good candidate for gas injection EOR; lean gas generated the worst results. Reservoir simulations also indicate that original rock properties are the dominant factor for the ultimate oil recovery for both primary recovery and gas injection EOR. Because reservoir simulations provide critical inputs for project planning and management, more effort needs to be invested into reservoir modeling and simulation, including building enhanced geologic models, fracture characterization and modeling, and history matching with field data. Gas injection EOR projects are integrated projects, and the viability of a project also depends on different economic conditions.

Closed-Loop Control of Chemical Injection Rate for a Direct Nozzle Injection System.

PubMed

Cai, Xiang; Walgenbach, Martin; Doerpmond, Malte; Schulze Lammers, Peter; Sun, Yurui

2016-01-20

To realize site-specific and variable-rate application of agricultural pesticides, accurately metering and controlling the chemical injection rate is necessary. This study presents a prototype of a direct nozzle injection system (DNIS) by which chemical concentration transport lag was greatly reduced. In this system, a rapid-reacting solenoid valve (RRV) was utilized for injecting chemicals, driven by a pulse-width modulation (PWM) signal at 100 Hz, so with varying pulse width the chemical injection rate could be adjusted. Meanwhile, a closed-loop control strategy, proportional-integral-derivative (PID) method, was applied for metering and stabilizing the chemical injection rate. In order to measure chemical flow rates and input them into the controller as a feedback in real-time, a thermodynamic flowmeter that was independent of chemical viscosity was used. Laboratory tests were conducted to assess the performance of DNIS and PID control strategy. Due to the nonlinear input-output characteristics of the RRV, a two-phase PID control process obtained better effects as compared with single PID control strategy. Test results also indicated that the set-point chemical flow rate could be achieved within less than 4 s, and the output stability was improved compared to the case without control strategy.

Design and analysis of a natural-gradient ground-water tracer test in a freshwater tidal wetland, West Branch Canal Creek, Aberdeen Proving Ground, Maryland

USGS Publications Warehouse

Olsen, Lisa D.; Tenbus, Frederick J.

2005-01-01

A natural-gradient ground-water tracer test was designed and conducted in a tidal freshwater wetland at West Branch Canal Creek, Aberdeen Proving Ground, Maryland. The objectives of the test were to characterize solute transport at the site, obtain data to more accurately determine the ground-water velocity in the upper wetland sediments, and to compare a conservative, ionic tracer (bromide) to a volatile tracer (sulfur hexafluoride) to ascertain whether volatilization could be an important process in attenuating volatile organic compounds in the ground water. The tracer test was conducted within the upper peat unit of a layer of wetland sediments that also includes a lower clayey unit; the combined layer overlies an aquifer. The area selected for the test was thought to have an above-average rate of ground-water discharge based on ground-water head distributions and near-surface detections of volatile organic compounds measured in previous studies. Because ground-water velocities in the wetland sediments were expected to be slow compared to the underlying aquifer, the test was designed to be conducted on a small scale. Ninety-seven ?-inch-diameter inverted-screen stainless-steel piezometers were installed in a cylindrical array within approximately 25 cubic feet (2.3 cubic meters) of wetland sediments, in an area with a vertically upward hydraulic gradient. Fluorescein dye was used to qualitatively evaluate the hydrologic integrity of the tracer array before the start of the tracer test, including verifying the absence of hydraulic short-circuiting due to nonnatural vertical conduits potentially created during piezometer installation. Bromide and sulfur hexafluoride tracers (0.139 liter of solution containing 100,000 milligrams per liter of bromide ion and 23.3 milligrams per liter of sulfur hexafluoride) were co-injected and monitored to generate a dataset that could be used to evaluate solute transport in three dimensions. Piezometers were sampled 2 to 15 times each, from July 1998 through September 1999, to assess background conditions and monitor tracer movement. During the test, 644 samples were analyzed for fluorescein, 617 samples were analyzed for bromide with an ion-selective electrode, 213 samples were analyzed for bromide with colorimetric methods, and 603 samples were analyzed for sulfur hexafluoride, including samples collected prior to tracer injection to determine background concentrations. Additional samples were analyzed for volatile organic compounds (96 samples) and methane (37 samples) to determine the distribution of these contaminants and the extent of methanogenic conditions within the tracer array; however, these data were not used for the analysis of the test. During the tracer test, the fluorescein dye, bromide, and sulfur hexafluoride were transported predominantly in the upward direction, although all three tracers also moved outward in all directions from the injection point, and it is likely that some tracer mass moved beyond the lateral edges of the array. An analysis of the tracer-test data was performed through the use of breakthrough curves and isoconcentration contour plots. Results show that movement of the fluorescein dye, a non-conservative tracer, was retarded compared to the other two tracers, likely as a result of sorption onto the wetland sediments. Suspected loss of tracer mass along the lateral edges of the array prevented a straightforward quantitative analysis of tracer transport and ground-water velocity from the bromide and sulfur-hexafluoride data. In addition, the initial density of the bromide/sulfur hexafluoride solution (calculated to be 1.097 grams per milli2 Ground-Water Tracer Test, West Branch Canal Creek, Aberdeen Proving Ground, MD liter) could have caused the solution to sink below the injection point before undergoing dilution and moving back up into the array. For these reasons, the data analysis in this report was performed largely through qualitative method

Implementing and scaling up HCV treatment services for people who inject drugs and other high risk groups in Ukraine: An evaluation of programmatic and treatment outcomes.

PubMed

Mazhnaya, Alyona; Meteliuk, Anna; Barnard, Tetiana; Zelenev, Alexei; Filippovych, Sergii; Altice, Frederick L

2017-09-01

HCV prevalence estimates among people who inject drugs (PWID) in Ukraine is high (60-90%), yet barriers to HCV treatment and care remain substantial including limited access to direct acting antiviral (DAA) medications. A feasibility scale-up project implemented HCV treatment in community-based settings to improve access to DAA treatment for key populations in this context. Using program-level data and verified medical records, we describe the development, implementation processes and outcomes for HCV treatment for PWID and other risks groups. Most participants (76%) received a combination of sofosbuvir, pegylated interferon, and ribavirin for 12 weeks. Treatment enrollment started in June 2015; the first two waves are reported. Data on demographics, HIV characteristics, HCV genotype and RNA levels, including sustained virologic response (SVR) were obtained from verified medical records. We used logistic regression to examine the independent correlates of achieving a SVR. The project was implemented in 19 healthcare institutions from 16 regions of Ukraine, mainly within AIDS specialty centers. Our analytical sample included 1126 participants who were mostly men (73%) and the majority were HIV co-infected (79%). Treatment retention was 97.7%; the proportions of participants who achieved SVR for the overall sample and for those with complete data (N=1029) were 86.2% (95% CI 84.08-88.19%) and 94.3% (95% CI 92.8-95.7%) respectively. The analysis of data restricted to only those with SVR data available showed that PWID who were currently injecting had comparable SVR rates (89.2%, 95% CI 81.5-94.5%) to PWID not injecting (94.4%, 95% CI 92.4-96.1), PWID on methadone (94.4%, 95%CI 92.4-96.1), and 'other' risk groups (95.2%, 95% CI 91.3-97.7). Independent factors associated with achieving a SVR were female sex (AOR: 3.44, 95% CI 1.45-8.14), HCV genotype 3 (AOR: 4.57, 95% CI 1.97-10.59) compared to genotype 1. SVR rates in PWID actively injecting did not differ significantly from any other group. Both patient-level and structural factors influence HCV treatment scale-up in Ukraine, but patient-level outcomes confirm high levels of achieving SVR in PWID, irrespective of injection and treatment status. Copyright © 2017. Published by Elsevier B.V.

Comparison of field-enhanced and pressure-assisted field-enhanced sample injection techniques for the analysis of water-soluble vitamins using CZE.

PubMed

Liu, Qingqing; Liu, Yaling; Guan, Yu; Jia, Li

2009-04-01

A new online concentration method, namely pressure-assisted field-enhanced sample injection (PA-FESI), was developed and compared with FESI for the analysis of water-soluble vitamins by CZE with UV detection. In PA-FESI, negative voltage and positive pressure were simultaneously applied to initialize PA-FESI. PA-FESI uses the hydrodynamic flow generated by the positive pressure to counterbalance the reverse EOF in the capillary column during electrokinetic sample injection, which allowed a longer injection time than usual FESI mode without compromising the separation efficiency. Using the PA-FESI method, the LODs of the vitamins were at ng/mL level based on the S/N of 3 and the RSDs of migration time and peak area for each vitamin (1 microg/mL) were less than 5.1%. The developed method was applied to the analysis of water-soluble vitamins in corns.

Novel sample preparation technique with needle-type micro-extraction device for volatile organic compounds in indoor air samples.

PubMed

Ueta, Ikuo; Mizuguchi, Ayako; Fujimura, Koji; Kawakubo, Susumu; Saito, Yoshihiro

2012-10-09

A novel needle-type sample preparation device was developed for the effective preconcentration of volatile organic compounds (VOCs) in indoor air before gas chromatography-mass spectrometry (GC-MS) analysis. To develop a device for extracting a wide range of VOCs typically found in indoor air, several types of particulate sorbents were tested as the extraction medium in the needle-type extraction device. To determine the content of these VOCs, air samples were collected for 30min with the packed sorbent(s) in the extraction needle, and the extracted VOCs were thermally desorbed in a GC injection port by the direct insertion of the needle. A double-bed sorbent consisting of a needle packed with divinylbenzene and activated carbon particles exhibited excellent extraction and desorption performance and adequate extraction capacity for all the investigated VOCs. The results also clearly demonstrated that the proposed sample preparation method is a more rapid, simpler extraction/desorption technique than traditional sample preparation methods. Copyright © 2012 Elsevier B.V. All rights reserved.

Decreased Odds of Injection Risk Behavior Associated With Direct Versus Indirect Use of Syringe Exchange: Evidence From Two California Cities.

PubMed

Behrends, Czarina N; Li, Chin-Shang; Gibson, David R

2017-07-29

While there is substantial evidence that syringe exchange programs (SEPs) are effective in preventing HIV among people who inject drugs (PWID), nearly all the evidence comes from PWID who obtain syringes from an SEP directly. Much less is known about the benefits of secondary exchange to PWID who get syringes indirectly from friends or acquaintances who visit an SEP for them. We evaluated the effectiveness of direct versus indirect syringe exchange in reducing HIV-related high-risk injecting behavior among PWID in two separate studies conducted in Sacramento and San Jose, California, cities with quite different syringe exchange models. In both studies associations between direct and indirect syringe exchange and self-reported risk behavior were examined with multivariable logistic regression models. Study 1 assessed effects of a "satellite" home-delivery syringe exchange in Sacramento, while Study 2 evaluated a conventional fixed-site exchange in San Jose. Multivariable analyses revealed 95% and 69% reductions, respectively, in high-risk injection associated with direct use of the SEPs in Sacramento and San Jose, and a 46% reduction associated with indirect use of the SEP in Sacramento. Conclusions/Importance: The very large effect of direct SEP use in Sacramento was likely due in part to home delivery of sterile syringes. While more modest effects were associated with indirect use, such use nevertheless is valuable in reducing the risk of HIV transmission of PWID who are unable or unwilling to visit a syringe exchange.

Devascularization of Head and Neck Paragangliomas by Direct Percutaneous Embolization

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

Ozyer, Umut, E-mail: umut_ozyer@yahoo.com; Harman, Ali; Yildirim, Erkan

2010-10-15

Preoperative transarterial embolization of head and neck paragangliomas using particulate agents has proven beneficial for decreasing intraoperative blood loss. However, the procedure is often incomplete owing to extensive vascular structure and arteriovenous shunts. We report our experience with embolization of these lesions by means of direct puncture and intratumoral injection of n-butyl cyanoacrylate (NBCA) or Onyx. Ten patients aged 32-82 years who were referred for preoperative embolization of seven carotid body tumors and three jugular paragangliomas were retrospectively analyzed. Intratumoral injections were primarily performed in four cases with multiple small-caliber arterial feeders and adjunctive to transarterial embolization in six casesmore » with incomplete devascularization. Punctures were performed under ultrasound and injections were performed under roadmap fluoroscopic guidance. Detailed angiographies were performed before and after embolization procedures. Control angiograms showed complete or near-complete devascularization in all tumors. Three tumors with multiple small-caliber arterial feeders were treated with primary NBCA injections. One tumor necessitated transarterial embolization after primary injection of Onyx. Six tumors showed regional vascularization from the vasa vasorum or small-caliber branches of the external carotid artery following the transarterial approach. These regions were embolized with NBCA injections. No technical or clinical complications related to embolization procedures occurred. All except one of the tumors were surgically removed following embolization. In conclusion, preoperative devascularization with percutaneous direct injection of NBCA or Onyx is feasible, safe, and effective in head and neck paragangliomas with multiple small-caliber arterial feeders and in cases of incomplete devascularization following transarterial embolization.« less

Blindness following cosmetic injections of the face.

PubMed

Lazzeri, Davide; Agostini, Tommaso; Figus, Michele; Nardi, Marco; Pantaloni, Marcello; Lazzeri, Stefano

2012-04-01

Complications following facial cosmetic injections have recently heightened awareness of the possibility of iatrogenic blindness. The authors conducted a systematic review of the available literature to provide the best evidence for the prevention and treatment of this serious eye injury. The authors included in the study only the cases in which blindness was a direct consequence of a cosmetic injection procedure of the face. Twenty-nine articles describing 32 patients were identified. In 15 patients, blindness occurred after injections of adipose tissue; in the other 17, it followed injections of various materials, including corticosteroids, paraffin, silicone oil, bovine collagen, polymethylmethacrylate, hyaluronic acid, and calcium hydroxyapatite. Some precautions may minimize the risk of embolization of filler into the ophthalmic artery following facial cosmetic injections. Intravascular placement of the needle or cannula should be demonstrated by aspiration before injection and should be further prevented by application of local vasoconstrictor. Needles, syringes, and cannulas of small size should be preferred to larger ones and be replaced with blunt flexible needles and microcannulas when possible. Low-pressure injections with the release of the least amount of substance possible should be considered safer than bolus injections. The total volume of filler injected during the entire treatment session should be limited, and injections into pretraumatized tissues should be avoided. Actually, no safe, feasible, and reliable treatment exists for iatrogenic retinal embolism. Nonetheless, therapy should theoretically be directed to lowering intraocular pressure to dislodge the embolus into more peripheral vessels of the retinal circulation, increasing retinal perfusion and oxygen delivery to hypoxic tissues. Risk, V.

Use of Adaptive Injection Strategies to Increase the Full Load Limit of RCCI Operation

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

Hanson, Reed; Ickes, Andrew; Wallner, Thomas

2015-01-01

Dual-fuel combustion using port-injection of low reactivity fuel combined with direct injection of a higher reactivity fuel, otherwise known as Reactivity Controlled Compression Ignition (RCCI), has been shown as a method to achieve low-temperature combustion with moderate peak pressure rise rates, low engine-out soot and NOx emissions, and high indicated thermal efficiency. A key requirement for extending to high-load operation is moderating the reactivity of the premixed charge prior to the diesel injection. One way to accomplish this is to use a very low reactivity fuel such as natural gas. In this work, experimental testing was conducted on a 13Lmore » multi-cylinder heavy-duty diesel engine modified to operate using RCCI combustion with port injection of natural gas and direct injection of diesel fuel. Engine testing was conducted at an engine speed of 1200 RPM over a wide variety of loads and injection conditions. The impact on dual-fuel engine performance and emissions with respect to varying the fuel injection parameters is quantified within this study. The injection strategies used in the work were found to affect the combustion process in similar ways to both conventional diesel combustion and RCCI combustion for phasing control and emissions performance. As the load is increased, the port fuel injection quantity was reduced to keep peak cylinder pressure and maximum pressure rise rate under the imposed limits. Overall, the peak load using the new injection strategy was shown to reach 22 bar BMEP with a peak brake thermal efficiency of 47.6%.« less

An on-line potentiometric sequential injection titration process analyser for the determination of acetic acid.

PubMed

van Staden, J F; Mashamba, Mulalo G; Stefan, Raluca I

2002-09-01

An on-line potentiometric sequential injection titration process analyser for the determination of acetic acid is proposed. A solution of 0.1 mol L(-1) sodium chloride is used as carrier. Titration is achieved by aspirating acetic acid samples between two strong base-zone volumes into a holding coil and by channelling the stack of well-defined zones with flow reversal through a reaction coil to a potentiometric sensor where the peak widths were measured. A linear relationship between peak width and logarithm of the acid concentration was obtained in the range 1-9 g/100 mL. Vinegar samples were analysed without any sample pre-treatment. The method has a relative standard deviation of 0.4% with a sample frequency of 28 samples per hour. The results revealed good agreement between the proposed sequential injection and an automated batch titration method.

Rugged large volume injection for sensitive capillary LC-MS environmental monitoring

NASA Astrophysics Data System (ADS)

Roberg-Larsen, Hanne; Abele, Silvija; Demir, Deniz; Dzabijeva, Diana; Amundsen, Sunniva F.; Wilson, Steven R.; Bartkevics, Vadims; Lundanes, Elsa

2017-08-01

A rugged and high throughput capillary column (cLC) LC-MS switching platform using large volume injection and on-line automatic filtration and filter back-flush (AFFL) solid phase extraction (SPE) for analysis of environmental water samples with minimal sample preparation is presented. Although narrow columns and on-line sample preparation are used in the platform, high ruggedness is achieved e.g. injection of 100 non-filtrated water samples would did not result in a pressure rise/clogging of the SPE/capillary columns (inner diameter 300 µm). In addition, satisfactory retention time stability and chromatographic resolution were also features of the system. The potential of the platform for environmental water samples was demonstrated with various pharmaceutical products, which had detection limits (LOD) in the 0.05 - 12.5 ng/L range. Between-day and within-day repeatability of selected analytes were < 20% RSD.

Identification of Staphylococcus aureus infection by aptamers directly radiolabeled with technetium-99m.

PubMed

dos Santos, Sara Roberta; Rodrigues Corrêa, Cristiane; Branco de Barros, André Luís; Serakides, Rogéria; Fernandes, Simone Odília; Cardoso, Valbert Nascimento; de Andrade, Antero Silva Ribeiro

2015-03-01

Aptamers are oligonucleotides that have high affinity and specificity for their molecular targets which are emerging as a new class of molecules for radiopharmaceuticals development. In this study, aptamers selected to Staphylococcus aureus were evaluated for bacterial infection identification. Anti S. aureus aptamers were labeled with (99m)Tc by the direct method. The radiolabel yield and complex stability were assessed by thin-layer chromatography (TLC). Three groups of Swiss mice containing 6 animals each were used. The first group was infected intramuscularly in the right thigh with S. aureus. The second group was infected in the same way with C. albicans and the third group was injected with zymosan to induce aseptic inflammation. After 24 h, radiolabeled aptamers (22.2 MBq) were injected by the tail vein. The mice were euthanized 4 h post injection and tissue sample activities measured in a gamma counter. The (99m)Tc labeled aptamers were stable in saline, plasma and cystein excess. Radiolabeled aptamers showed increased uptake in the kidneys for all groups indicating a main renal excretion, which is consistent with the hydrophilic nature and small size of aptamers. The radiopharmaceutical showed rapid blood clearance indicated by a reduced dose (% ID/g) in the blood. The biodistribution showed that aptamers were able to identify the infection foci caused by S. aureus displaying a target/non-target ratio of 4.0±0.5. This ratio for mice infected with C. albicans was 2.0±0.4 while for mice with aseptic inflammation was 1.2±0.2. Histology confirmed the presence of infection in groups 1 and 2, and inflammation in group 3. The biodistibution study demonstrated a statistically higher uptake in the S. aureus foci relative to inflammation and C. albicans infected areas. These results highlight the potential of aptamers labeled directly with (99m)Tc for bacterial infection diagnosis by scintigraphy. Copyright © 2014 Elsevier Inc. All rights reserved.

Health and Social Problems Associated with Prescription Opioid Misuse Among a Diverse Sample of High Risk Substance-Using MSM

PubMed Central

Buttram, Mance E.; Kurtz, Steven P.; Surratt, Hilary L.; Levi-Minzi, Maria A.

2013-01-01

This study examines associations between prescription opioid misuse and demographics, substance use, sexual behavior, and related health and social problems. Baseline data were collected between 2008 and 2010 from 515 high risk men who have sex with men (MSM), ages 18–55, in the Miami-Ft. Lauderdale metropolitan area who reported heavy substance use and HIV risk in the past 90 days. Prescription opioid misuse was associated with other substance use, drug injection, substance dependence, and history of arrest. Implications, limitations, and directions for future study are discussed. PMID:23971894

[Improvement of the determination method of benzene, toluene, ethylbenzene and xylene(BTEX) in water using activated carbon fiber solid-phase microextraction/gas chromatography-mass spectrometry(GC-MS)].

PubMed

Jia, Jin-ping; Feng, Xue; Fang, Neng-hu; Huang, Jia-liang

2002-01-01

The methods of direct injection, carbon disulfide extraction and activated carbon fiber solid-phase microextraction/GC-MS, usually used in the determination of BTEX in water matrix, are compared and discussed. Experimental data of linearity, precision and limit of detection illustrate that the last one is better than the two other methods. This method was tested by the practical sample experiments and expected to be a simple and sensitive new method for the analysis of BTEX in water.

Si based GeSn light emitter: mid-infrared devices in Si photonics

NASA Astrophysics Data System (ADS)

Yu, S. Q.; Ghetmiri, S. A.; Du, W.; Margetis, J.; Zhou, Y.; Mosleh, A.; Al-Kabi, S.; Nazzal, A.; Sun, G.; Soref, R. A.; Tolle, J.; Li, B.; Naseem, H. A.

2015-02-01

Ge1-xSnx/Ge thin films and Ge/Ge1-xSnx/Ge n-i-p double heterostructure (DHS) have been grown using commercially available reduced pressure chemical vapor deposition (RPCVD) reactor. The Sn compositional material and optical characteristics have been investigated. A direct bandgap GeSn material has been identified with Sn composition of 10%. The GeSn DHS samples were fabricated into LED devices. Room temperature electroluminescence spectra were studied. A maximum emission power of 28mW was obtained with 10% Sn LED under the injection current density of 800 A/cm2.

Development and validation of a liquid chromatography-tandem mass spectrometry method for the determination of pyridostigmine bromide from guinea pig plasma.

PubMed

Needham, Shane R; Ye, Binying; Smith, J Richard; Korte, William D

2003-11-05

An HPLC/MS/MS method was validated for the low level analysis of pyridostigmine bromide (PB) from guinea pig plasma. An advantage of this strong-cation exchange HPLC/MS/MS method was the enhancement of the ESI-MS signal by providing good retention and good peak shape of PB with a mobile phase of 70% acetonitrile. In addition, the use of 70% acetonitrile in the mobile phase allowed the direct injection of the supernant from the protein precipitated extracted sample. The assay was linear from the range of 0.1 to 50 ng/ml using only 25 microl of sample. The precision and accuracy of the assay was better than 9.1 and 113%, respectively.

Flow injection analysis-flame atomic absorption spectrometry system for indirect determination of sulfite after on-line reduction of solid-phase manganese (IV) dioxide reactor.

PubMed

Zare-Dorabei, Rouholah; Boroun, Shokoufeh; Noroozifar, Meissam

2018-02-01

A new and simple flow injection method followed by atomic absorption spectrometry was developed for indirect determination of sulfite. The proposed method is based on the oxidation of sulfite to sulphate ion using solid-phase manganese dioxide (30% W/W suspended on silica gel beads) reactor. MnO 2 will be reduced to Mn(II) by sample injection in to the column under acidic carrier stream of HNO 3 (pH 2) with flow rate of 3.5mLmin -1 at room temperature. Absorption measurement of Mn(II) which is proportional to the concentration of sulfite in the sample was carried out by atomic absorption spectrometry. The calibration curve was linear up to 25mgL -1 with a detection limit (DL) of 0.08mgL -1 for 400µL injection sample volume. The presented method is efficient toward sulfite determination in sugar and water samples with a relative standard deviation (RSD) less than 1.2% and a sampling rate of about 60h -1 . Copyright © 2017 Elsevier B.V. All rights reserved.

Unconventional Hydrocarbon Development Hazards Within the Central United States. Report 1: Overview and Potential Risk to Infrastructure

DTIC Science & Technology

2015-08-01

of the injection purpose, i.e., secondary oil and gas recovery, disposal of waste fluids, geothermal energy, and/or UHP hydraulic fracturing...activities such as reservoir impoundment, mining, wastewater injection, geothermal systems and CO2 capture have been linked directly to induced...activities, e.g., deep fluid injection, geothermal injection, and/or UHP wells, that critically affect deep lithologies and alter the existing mechanical

REDUCTION OF COAL-BASED METAL EMISSIONS BY FURNACE SORBENT INJECTION

EPA Science Inventory

The ability of sorbent injection technology to reduce the potential for trace metal emissions from coal combustion was researched. Pilot scale tests of high-temperature furnace sorbent injection were accompanied by stack sampling for coal-based, metallic air toxics. Tested sorben...

Trace analysis of pesticides in paddy field water by direct injection using liquid chromatography-quadrupole-linear ion trap-mass spectrometry.

PubMed

Pareja, Lucía; Martínez-Bueno, M J; Cesio, Verónica; Heinzen, Horacio; Fernández-Alba, A R

2011-07-29

A multiresidue method was developed for the quantification and confirmation of 70 pesticides in paddy field water. After its filtration, water was injected directly in a liquid chromatograph coupled to a hybrid triple quadrupole-linear ion trap-mass spectrometer (QqLIT). The list of target analytes included organophosphates, phenylureas, sulfonylureas, carbamates, conazoles, imidazolinones and others compounds widely used in different countries where rice is cropped. Detection and quantification limits achieved were in the range from 0.4 to 80 ng L(-1) and from 2 to 150 ng L(-1), respectively. Correlation coefficients for the calibration curves in the range 0.1-50 μg L(-1) were higher than 0.99 except for diazinon (0.1-25 μg L(-1)). Only 9 pesticides presented more than 20% of signal suppression/enhancement, no matrix effect was observed in the studied conditions for the rest of the target pesticides. The method developed was used to investigate the occurrence of pesticides in 59 water samples collected in paddy fields located in Spain and Uruguay. The study shows the presence of bensulfuron methyl, tricyclazole, carbendazim, imidacloprid, tebuconazole and quinclorac in a concentration range from 0.08 to 7.20 μg L(-1). Copyright © 2011 Elsevier B.V. All rights reserved.

Direct sampling of chemical weapons in water by photoionization mass spectrometry.

PubMed

Syage, Jack A; Cai, Sheng-Suan; Li, Jianwei; Evans, Matthew D

2006-05-01

The vulnerability of water supplies to toxic contamination calls for fast and effective means for screening water samples for multiple threats. We describe the use of photoionization (PI) mass spectrometry (MS) for high-speed, high-throughput screening and molecular identification of chemical weapons (CW) threats and other hazardous compounds. The screening technology can detect a wide range of compounds at subacute concentrations with no sample preparation and a sampling cycle time of approximately 45 s. The technology was tested with CW agents VX, GA, GB, GD, GF, HD, HN1, and HN3, in addition to riot agents and precursors. All are sensitively detected and give simple PI mass spectra dominated by the parent ion. The target application of the PI MS method is as a routine, real-time early warning system for CW agents and other hazardous compounds in air and in water. In this work, we also present comprehensive measurements for water analysis and report on the system detection limits, linearity, quantitation accuracy, and false positive (FP) and false negative rates for concentrations at subacute levels. The latter data are presented in the form of receiver operating characteristic curves of the form of detection probability P(D) versus FP probability P(FP). These measurements were made using the CW surrogate compounds, DMMP, DEMP, DEEP, and DIMP. Method detection limits (3sigma) obtained using a capillary injection method yielded 1, 6, 3, and 2 ng/mL, respectively. These results were obtained using 1-microL injections of water samples without any preparation, corresponding to mass detection limits of 1, 6, 3, and 2 pg, respectively. The linear range was about 3-4 decades and the dynamic range about 4-5 decades. The relative standard deviations were generally <10% at CW subacute concentrations levels.

Non-chromatographic speciation analysis of mercury by flow injection on-line preconcentration in combination with chemical vapor generation atomic fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Wu, Hong; Jin, Yan; Han, Weiying; Miao, Qiang; Bi, Shuping

2006-07-01

A novel non-chromatographic approach for direct speciation of mercury, based on the selective retention inorganic mercury and methylmercury on the inner wall of a knotted reactor by using ammonium diethyl dithiophosphate and dithizone as complexing agents respectively, was developed for flow injection on-line sorption preconcentration coupled with chemical vapor generation non-dispersive atomic fluorescence spectrometry. With the sample pH kept at 2.0, the preconcentration of inorganic mercury on the inner walls of the knotted reactor was carried out based on the exclusive retention of Hg-DDP complex in the presence of methylmercury via on-line merging the sample solution with ammonium diethyl dithiophosphate solution, and selective preconcentration methylmercury was achieved with dithizone instead of ammonium diethyl dithiophosphate. A 15% (v/v) HCl was introduced to elute the retained mercury species and merge with KBH 4 solution for atomic fluorescence spectrometry detection. Under the optimal experimental conditions, the sample throughputs of inorganic mercury and methylmercury were 30 and 20 h - 1 with the enhancement factors of 13 and 24. The detection limits were found to be 3.6 ng l - 1 for Hg 2+ and 2.0 ng l - 1 for CH 3Hg +. The precisions (RSD) for the 11 replicate measurements of each 0.2 μg l - 1 of Hg 2+ and CH 3Hg + were 2.2% and 2.8%, respectively. The developed method was validated by the analysis of certified reference materials (simulated natural water, rice flour and pork) and by recovery measurements on spiked samples, and was applied to the determination of inorganic mercury and methylmercury in biological and environmental water samples.

Comparison of direct sampling and brochoalveolar lavage for determining active drug concentrations in the pulmonary epithelial lining fluid of calves injected with enrofloxacin or tilmicosin.

PubMed

Foster, D M; Sylvester, H J; Papich, M G

2017-12-01

Antibiotic distribution to interstitial fluid (ISF) and pulmonary epithelial fluid (PELF) was measured and compared to plasma drug concentrations in eight healthy calves. Enrofloxacin (Baytril ® 100) was administered at a dose of 12.5 mg/kg subcutaneously (SC), and tilmicosin (Micotil ® 300) was administered at a dose of 20 mg/kg SC. PELF, sampled by two different methods-bronchoalveolar lavage (BAL) and direct sampling (DS)-plasma, and ISF were collected from each calf and measured for tilmicosin, enrofloxacin and its metabolite ciprofloxacin by HPLC. Pharmacokinetic analysis was performed on the concentrations in each fluid, for each drug. The enrofloxacin/ciprofloxacin concentration as measured by AUC in DS samples was 137 ± 72% higher than in plasma, but in BAL samples, this value was 535 ± 403% (p < .05). The concentrations of tilmicosin in DS and BAL samples exceeded plasma drug concentrations by 567 ± 189% and 776 ± 1138%, respectively. The enrofloxacin/ciprofloxacin concentrations collected by DS were significantly different than those collected by BAL, but the tilmicosin concentrations were not significantly different between the two methods. Concentrations of enrofloxacin/ciprofloxacin exceeded the MIC values for bovine respiratory disease pathogens but tilmicosin did not reach MIC levels for these pathogens in any fluids. © 2017 John Wiley & Sons Ltd.

Employment-based reinforcement of adherence to depot naltrexone in unemployed opioid-dependent adults: a randomized controlled trial.

PubMed

Everly, Jeffrey J; DeFulio, Anthony; Koffarnus, Mikhail N; Leoutsakos, Jeannie-Marie S; Donlin, Wendy D; Aklin, Will M; Umbricht, Annie; Fingerhood, Michael; Bigelow, George E; Silverman, Kenneth

2011-07-01

Naltrexone can be used to treat opioid dependence, but patients refuse to take it. Extended-release depot formulations may improve adherence, but long-term adherence rates to depot naltrexone are not known. This study determined long-term rates of adherence to depot naltrexone and whether employment-based reinforcement can improve adherence. Participants who were inducted onto oral naltrexone were assigned randomly to contingency (n = 18) or prescription (n = 17) groups. Participants were offered six depot naltrexone injections and invited to work at the therapeutic workplace on week days for 26 weeks, where they earned stipends for participating in job skills training. Contingency participants were required to accept naltrexone injections to maintain workplace access and to maintain maximum pay. Prescription participants could work independently of whether they accepted injections. The therapeutic workplace, a model employment-based intervention for drug addiction and unemployment. Opioid-dependent unemployed adults. Depot naltrexone injections accepted and opiate-negative urine samples. Contingency participants accepted significantly more naltrexone injections than prescription participants (81% versus 42%), and were more likely to accept all injections (66% versus 35%). At monthly assessments (with missing urine samples imputed as positive), the groups provided similar percentages of samples negative for opiates (74% versus 62%) and for cocaine (56% versus 54%). Opiate-positive samples were more likely when samples were also positive for cocaine. Employment-based reinforcement can maintain adherence to depot naltrexone. Future research should determine whether persistent cocaine use compromises naltrexone's effect on opiate use. Workplaces may be useful for promoting sustained adherence to depot naltrexone. © 2011 The Authors, Addiction © 2011 Society for the Study of Addiction.

Stability of levothyroxine injection in glass, polyvinyl chloride, and polyolefin containers.

PubMed

Frenette, Anne Julie; MacLean, Robert D; Williamson, David; Marsolais, Pierre; Donnelly, Ronald F

2011-09-15

The 24-hour stability of a levothyroxine solution admixed and stored in three common infusion containers and infused through polyvinyl chloride (PVC) tubing was evaluated. Levothyroxine sodium 1-μg/mL injection prepared in glass bottles and PVC and polyolefin bags were assayed using high-performance liquid chromatography at 0, 1, 3, 6, 12, and 24 hours; samples drawn directly from the containers, as well as from the distal end of attached PVC tubing, were assayed. The area under the time-versus-concentration curve (AUC) for predicted and delivered doses was calculated; analysis of variance was used for comparison of the percentages of predicted and actual AUC values. The levothyroxine concentration was stable in glass bottles and polyolefin bags through 24 hours (mean ± S.D. percentage of initial concentration remaining, 103.5% ± 2.5% and 100.0% ± 2.9%, respectively). In the PVC infusion bags, the amount of drug decreased to 90% of the initial concentration within 1 hour and then rose and remained within acceptability limits. The levothyroxine concentration of the samples infused through PVC line from glass and polyolefin containers decreased after 1 hour by about 13%; the loss of the drug from the samples infused from PVC bags was higher (18%), presumably due to additive adsorptive effects. In all samples tested, the drug concentration rebounded and remained above 90% to the end of the study. Levothyroxine sodium 1-μg/mL solution was stable for 24 hours in glass bottles and polyolefin bags but when stored in PVC bags, the concentration decreased by 10% after 1 hour.

Injection port derivatization following ion-pair hollow fiber-protected liquid-phase microextraction for determining acidic herbicides by gas chromatography/mass spectrometry.

PubMed

Wu, Jingming; Lee, Hian Kee

2006-10-15

Injection port derivatization following ion-pair hollow fiber-protected liquid-phase microextraction (LPME) for the trace determination of acidic herbicides (2,4-dichlorobenzoic acid, 2,4-dichlorophenoxyacetic acid, 2-(2,4-dichlorophenoxy)propionic acid, 3,5-dichlorobenzoic acid, 2-(2,4,5-trichlorophenoxy)propionic acid) in aqueous samples by gas chromatography/mass spectrometry (GC/MS) was developed. Prior to GC injection port derivatization, acidic herbicides were converted into their ion-pair complexes with tetrabutylammonium chloride in aqueous samples and then extracted by 1-octanol impregnated in the hollow fiber. Upon injection, ion pairs of acidic herbicides were quantitatively derivatized to their butyl esters in the GC injection port. Thus, several parameters related to the derivatization process (i.e., injection temperature, purge-off time) were evaluated, and main parameters affecting the hollow fiber-protected LPME procedure such as extraction organic solvent, ion-pair reagent type, pH of aqueous medium, concentration of ion-pair reagent, sodium chloride concentration added to the aqueous medium, stirring speed, and extraction time profile, optimized. At the selected extraction and derivatization conditions, no matrix effects were observed. This method proved good repeatability (RSDs <12.3%, n = 6) and good linearity (r2 > or = 0.9939) for spiked deionized water samples for five analytes. The limits of detection were in the range of 0.51-13.7 ng x L(-1) (S/N =3) under GC/MS selected ion monitoring mode. The results demonstrated that injection port derivatization following ion-pair hollow fiber-protected LPME was a simple, rapid, and accurate method for the determination of trace acidic herbicides from aqueous samples. In addition, this method proved to be environmentally friendly since it completely avoided open derivatization with potentially hazardous reagents.

Exploring Microbial Processes with Thermal-Hydrological Models of the Eastern Flank of the Juan de Fuca Ridge

NASA Astrophysics Data System (ADS)

Weathers, T. S.; Fisher, A. T.; Winslow, D. M.; Stauffer, P. H.; Gable, C. W.

2017-12-01

The flanks of mid-ocean ridges experience coupled flows of fluid, heat, and solutes that are critical for a wide range of global processes, including the cycling of carbon and nutrients, which supports a vast crustal biosphere. Only a few ridge-flank sites have been studied in detail; hydrogeologic conditions and processes in the volcanic crust are best understood on the eastern flank of the Juan de Fuca Ridge. This area has been extensively explored with decades of drilling, submersible, observatory, and survey expeditions and experiments, including the first hole-to-hole tracer injection experiment in the ocean crust. This study describes the development of reactive transport simulations for this ridge-flank setting using three-dimensional coupled (thermal-hydrological) models of crustal-scale circulation, beginning with the exploration of tracer transport. The prevailing flow direction is roughly south to north as a result of outcrop-to-outcrop flow, with a bulk flow rate in the range of meters/year. However, tracer was detected 500 m south ("upstream") from the injection borehole during the first year following injection. This may be explained by local mixing and/or formation fluid discharge from the southern borehole during and after injection. The constraints and parameters required to fit the observed tracer behavior can be used as a basis for modeling reactive transport processes such as nutrient delivery or microbial community evolution as a function of fluid flow. For example, the sulfate concentration in fluid samples from Baby Bare outcrop ( 8 km south of the tracer transport experiment) was 17.8 mmol/kg, whereas at Mama Bare outcrop ( 8 km to north of the tracer transport experiment) the sulfate concentration was 16.3 mmol/mg. By integrating laboratory-derived sulfate reduction rates from microbial samples originating from Juan de Fuca borehole observatories into reactive transport models, we can explore the range of microbial activity that supports the observed concentration gradients of sulfate and other solutes in the volcanic ocean crust.

Determination of suspected allergens in cosmetic products by headspace-programmed temperature vaporization-fast gas chromatography-quadrupole mass spectrometry.

PubMed

del Nogal Sánchez, Miguel; Pérez-Pavón, José Luis; Moreno Cordero, Bernardo

2010-07-01

In the present work, a strategy for the qualitative and quantitative analysis of 24 volatile compounds listed as suspected allergens in cosmetics by the European Union is reported. The list includes benzyl alcohol, limonene, linalool, methyl 2-octynoate, beta-citronellol, geraniol, citral (two isomers), 7-hydroxycitronellal, anisyl alcohol, cinnamal, cinnamyl alcohol, eugenol, isoeugenol (two isomers), coumarin, alpha-isomethyl ionone, lilial, alpha-amylcinnamal, lyral, alpha-amylcinnamyl alcohol, farnesol (three isomers), alpha-hexyl cinnamal, benzyl cinnamate, benzyl benzoate, and benzyl salicylate. The applicability of a headspace (HS) autosampler in combination with a gas chromatograph (GC) equipped with a programmable temperature vaporizer (PTV) and a quadrupole mass spectrometry (qMS) detector is explored. By using a headspace sampler, sample preparation is reduced to introducing the sample into the vial. This reduces the analysis time and the experimental errors associated with this step of the analytical process. Two different injection techniques were used: solvent-vent injection and hot-split injection. The first offers a way to improve sensitivity at the same time maintaining the simple headspace instrumentation and it is recommended for compounds at trace levels. The use of a liner packed with Tenax-TA allowed the compounds of interest to be retained during the venting process. The signals obtained when hot-split injection was used allowed quantification of all the compounds according to the thresholds of the European Cosmetics Directive. Monodimensional gas chromatography coupled to a conventional quadrupole mass spectrometry detector was used and the 24 analytes were separated appropriately along a run time of about 12 min. Use of the standard addition procedure as a quantification technique overcame the matrix effect. It should be emphasized that the method showed good precision and accuracy. Furthermore, it is rapid, simple, and--in view of the results--highly suitable for the determination of suspected allergens in different cosmetic products.

Design and characterization of poly(dimethylsiloxane)-based valves for interfacing continuous-flow sampling to microchip electrophoresis.

PubMed

Li, Michelle W; Huynh, Bryan H; Hulvey, Matthew K; Lunte, Susan M; Martin, R Scott

2006-02-15

This work describes the fabrication and evaluation of a poly(dimethyl)siloxane (PDMS)-based device that enables the discrete injection of a sample plug from a continuous-flow stream into a microchannel for subsequent analysis by electrophoresis. Devices were fabricated by aligning valving and flow channel layers followed by plasma sealing the combined layers onto a glass plate that contained fittings for the introduction of liquid sample and nitrogen gas. The design incorporates a reduced-volume pneumatic valve that actuates (on the order of hundreds of milliseconds) to allow analyte from a continuously flowing sampling channel to be injected into a separation channel for electrophoresis. The injector design was optimized to include a pushback channel to flush away stagnant sample associated with the injector dead volume. The effect of the valve actuation time, the pushback voltage, and the sampling stream flow rate on the performance of the device was characterized. Using the optimized design and an injection frequency of 0.64 Hz showed that the injection process is reproducible (RSD of 1.77%, n = 15). Concentration change experiments using fluorescein as the analyte showed that the device could achieve a lag time as small as 14 s. Finally, to demonstrate the potential uses of this device, the microchip was coupled to a microdialysis probe to monitor a concentration change and sample a fluorescein dye mixture.

PSR Injection Line Upgrade

NASA Astrophysics Data System (ADS)

Blind, Barbara; Jason, Andrew J.

1997-05-01

We describe the new injection line to be implemented for the Los Alamos Proton Storage Ring in the change from a two-step process to direct H- injection. While obeying all geometrical constraints imposed by the existing structures, the new line has properties not found in the present injection line. In particular, it features decoupled transverse phase spaces downstream of the skew bend and a high degree of tunability of the beam at the injection foil. A comprehensive set of error studies has dictated the component tolerances imposed and has indicated the expected performance of the system.

Understanding the interaction of injected CO2 and reservoir fluids in the Cranfield enhanced oil recovery (EOR) field (MS, USA) by non-radiogenic noble gas isotopes

NASA Astrophysics Data System (ADS)

Gyore, Domokos; Stuart, Finlay; Gilfillan, Stuart

2016-04-01

Identifying the mechanism by which the injected CO2 is stored in underground reservoirs is a key challenge for carbon sequestration. Developing tracing tools that are universally deployable will increase confidence that CO2 remains safely stored. CO2 has been injected into the Cranfield enhanced oil recovery (EOR) field (MS, USA) since 2008 and significant amount of CO2 has remained (stored) in the reservoir. Noble gases (He, Ne, Ar, Kr, Xe) are present as minor natural components in the injected CO2. He, Ne and Ar previously have been shown to be powerful tracers of the CO2 injected in the field (Györe et al., 2015). It also has been implied that interaction with the formation water might have been responsible for the observed CO2 loss. Here we will present work, which examines the role of reservoir fluids as a CO2 sink by examining non-radiogenic noble gas isotopes (20Ne, 36Ar, 84Kr, 132Xe). Gas samples from injection and production wells were taken 18 and 45 months after the start of injection. We will show that the fractionation of noble gases relative to Ar is consistent with the different degrees of CO2 - fluid interaction in the individual samples. The early injection samples indicate that the CO2 injected is in contact with the formation water. The spatial distribution of the data reveal significant heterogeneity in the reservoir with some wells exhibiting a relatively free flow path, where little formation water is contacted. Significantly, in the samples, where CO2 loss has been previously identified show active and ongoing contact. Data from the later stage of the injection shows that the CO2 - oil interaction has became more important than the CO2 - formation water interaction in controlling the noble gas fingerprint. This potentially provides a means to estimate the oil displacement efficiency. This dataset is a demonstration that noble gases can resolve CO2 storage mechanisms and its interaction with the reservoir fluids with high resolution. References: Györe, D., Stuart, F.M., Gilfillan, S.M.V., Waldron, S., 2015. Tracing injected CO2 in the Cranfield enhanced oil recovery field (MS, USA) using He, Ne and Ar isotopes. Int. J. Greenh. Gas Con. 42, 554-561.

Intra-lymph node injection of biodegradable polymer particles.

PubMed

Andorko, James I; Tostanoski, Lisa H; Solano, Eduardo; Mukhamedova, Maryam; Jewell, Christopher M

2014-01-02

Generation of adaptive immune response relies on efficient drainage or trafficking of antigen to lymph nodes for processing and presentation of these foreign molecules to T and B lymphocytes. Lymph nodes have thus become critical targets for new vaccines and immunotherapies. A recent strategy for targeting these tissues is direct lymph node injection of soluble vaccine components, and clinical trials involving this technique have been promising. Several biomaterial strategies have also been investigated to improve lymph node targeting, for example, tuning particle size for optimal drainage of biomaterial vaccine particles. In this paper we present a new method that combines direct lymph node injection with biodegradable polymer particles that can be laden with antigen, adjuvant, or other vaccine components. In this method polymeric microparticles or nanoparticles are synthesized by a modified double emulsion protocol incorporating lipid stabilizers. Particle properties (e.g. size, cargo loading) are confirmed by laser diffraction and fluorescent microscopy, respectively. Mouse lymph nodes are then identified by peripheral injection of a nontoxic tracer dye that allows visualization of the target injection site and subsequent deposition of polymer particles in lymph nodes. This technique allows direct control over the doses and combinations of biomaterials and vaccine components delivered to lymph nodes and could be harnessed in the development of new biomaterial-based vaccines.

Memory modulation across neural systems: intra-amygdala glucose reverses deficits caused by intraseptal morphine on a spatial task but not on an aversive task.

PubMed

McNay, E C; Gold, P E

1998-05-15

Based largely on dissociations of the effects of different lesions on learning and memory, memories for different attributes appear to be organized in independent neural systems. Results obtained with direct injections of drugs into one brain region at a time support a similar conclusion. The present experiments investigated the effects of simultaneous pharmacological manipulation of two neural systems, the amygdala and the septohippocampal system, to examine possible interactions of memory modulation across systems. Morphine injected into the medial septum impaired memory both for avoidance training and during spontaneous alternation. When glucose was concomitantly administered to the amygdala, glucose reversed the morphine-induced deficits in memory during alternation but not for avoidance training. These results suggest that the amygdala is involved in modulation of spatial memory processes and that direct injections of memory-modulating drugs into the amygdala do not always modulate memory for aversive events. These findings are contrary to predictions from the findings of lesion studies and of studies using direct injections of drugs into single brain areas. Thus, the independence of neural systems responsible for processing different classes of memory is less clear than implied by studies using lesions or injections of drugs into single brain areas.

STUDIES ON THE PATHOGENESIS OF FEVER

PubMed Central

King, M. Kenton; Wood, W. Barry

1958-01-01

By means of a method designed to compare the febrile responses produced by intracarotid and intravenous injections, the endogenous pyrogen, which is contained in leucocytic exudates and is present in the serum of rabbits 2 hours after intravenous injections of typhoid vaccine, has been shown to act directly upon the thermoregulatory centers of the brain. In contrast, the exogenous bacterial pyrogen present in serum obtained 5 minutes after vaccine injections was found to act by a different and less direct mechanism. These observations add strong support to the original hypothesis that endogenous pyrogen, presumably derived from polymorphonuclear leucocytes, is an essential factor in the pathogenesis of endotoxin fever. PMID:13491763

Direct link of a mid-infrared QCL to a frequency comb by optical injection.

PubMed

Borri, S; Galli, I; Cappelli, F; Bismuto, A; Bartalini, S; Cancio, P; Giusfredi, G; Mazzotti, D; Faist, J; De Natale, P

2012-03-15

A narrow-linewidth comb-linked nonlinear source is used as master radiation to injection lock a room-temperature mid-infrared quantum cascade laser (QCL). This process leads to a direct lock of the QCL to the optical frequency comb, providing the unique features of narrow linewidth, absolute frequency, higher output power, and wide mode-hop-free tunability. The QCL reproduces the injected radiation within more than 94%, with a reduction of the frequency-noise spectral density by 3 to 4 orders of magnitude up to about 100 kHz, and a linewidth narrowing from a few MHz to 20 kHz.

Characterization of Swirl-Venturi Lean Direct Injection Designs for Aviation Gas-Turbine Combustion

NASA Technical Reports Server (NTRS)

Heath, Christopher M.

2013-01-01

Injector geometry, physical mixing, chemical processes, and engine cycle conditions together govern performance, operability and emission characteristics of aviation gas-turbine combustion systems. The present investigation explores swirl-venturi lean direct injection combustor fundamentals, characterizing the influence of key geometric injector parameters on reacting flow physics and emission production trends. In this computational study, a design space exploration was performed using a parameterized swirl-venturi lean direct injector model. From the parametric geometry, 20 three-element lean direct injection combustor sectors were produced and simulated using steady-state, Reynolds-averaged Navier-Stokes reacting computations. Species concentrations were solved directly using a reduced 18-step reaction mechanism for Jet-A. Turbulence closure was obtained using a nonlinear ?-e model. Results demonstrate sensitivities of the geometric perturbations on axially averaged flow field responses. Output variables include axial velocity, turbulent kinetic energy, static temperature, fuel patternation and minor species mass fractions. Significant trends have been reduced to surrogate model approximations, intended to guide future injector design trade studies and advance aviation gas-turbine combustion research.

Determination of albumin in bronchoalveolar lavage fluid by flow-injection fluorometry using chromazurol S.

PubMed

Sato, Takaji; Saito, Yoshihiro; Chikuma, Masahiko; Saito, Yutaka; Nagai, Sonoko

2008-03-01

A highly sensitive flow injection fluorometry for the determination of albumin was developed and applied to the determination of albumin in human bronchoalveolar lavage fluids (BALF). This method is based on binding of chromazurol S (CAS) to albumin. The calibration curve was linear in the range of 5-200 microg/ml of albumin. A highly linear correlation (r=0.986) was observed between the albumin level in BALF samples (n=25) determined by the proposed method and by a conventional fluorometric method using CAS (CAS manual method). The IgG interference was lower in the CAS flow injection method than in the CAS manual method. The albumin level in BALF collected from healthy volunteers (n=10) was 58.5+/-13.1 microg/ml. The albumin levels in BALF samples obtained from patients with sarcoidosis and idiopathic pulmonary fibrosis were increased. This finding shows that the determination of albumin levels in BALF samples is useful for investigating lung diseases and that CAS flow injection method is promising in the determination of trace albumin in BALF samples, because it is sensitive and precise.

Analytical improvements of hybrid LC-MS/MS techniques for the efficient evaluation of emerging contaminants in river waters: a case study of the Henares River (Madrid, Spain).

PubMed

Pérez-Parada, Andrés; Gómez-Ramos, María del Mar; Martínez Bueno, María Jesús; Uclés, Samanta; Uclés, Ana; Fernández-Alba, Amadeo R

2012-02-01

Instrumental capabilities and software tools of modern hybrid mass spectrometry (MS) instruments such as high-resolution mass spectrometry (HRMS), quadrupole time-of-flight (QTOF), and quadrupole linear ion trap (QLIT) were experimentally investigated for the study of emerging contaminants in Henares River water samples. Automated screening and confirmatory capabilities of QTOF working in full-scan MS and tandem MS (MS/MS) were explored when dealing with real samples. Investigations on the effect of sensitivity and resolution power influence on mass accuracy were studied for the correct assignment of the amoxicillin transformation product 5(R) amoxicillin-diketopiperazine-2',5' as an example of a nontarget compound. On the other hand, a comparison of quantitative and qualitative strategies based on direct injection analysis and off-line solid-phase extraction sample treatment were assayed using two different QLIT instruments for a selected group of emerging contaminants when operating in selected reaction monitoring (SRM) and information-dependent acquisition (IDA) modes. Software-aided screening usually needs a further confirmatory step. Resolving power and MS/MS feature of QTOF showed to confirm/reject most findings in river water, although sensitivity-related limitations are usually found. Superior sensitivity of modern QLIT-MS/MS offered the possibility of direct injection analysis for proper quantitative study of a variety of contaminants, while it simultaneously reduced the matrix effect and increased the reliability of the results. Confirmation of ethylamphetamine, which lacks on a second SRM transition, was accomplished by using the IDA feature. Hybrid MS instruments equipped with high resolution and high sensitivity contributes to enlarge the scope of targeted analytes in river waters. However, in the tested instruments, there is a margin of improvement principally in required sensitivity and data treatment software tools devoted to reliable confirmation and improved automated data processing.

Gas chromatography/isotope ratio mass spectrometry: analysis of methanol, ethanol and acetic acid by direct injection of aqueous alcoholic and acetic acid samples.

PubMed

Ai, Guomin; Sun, Tong; Dong, Xiuzhu

2014-08-15

Methanol, ethanol, and acetic acid are not easily extracted from aqueous samples and are susceptible to isotope fractionation in gas chromatography/isotope ratio mass spectrometry (GC/IRMS) analysis. Developing a direct dilution GC/IRMS method for aqueous samples, by adjusting the sample concentrations in common solvents to be similar to each other and using a fixed GC split ratio, is very convenient and important because any linearity effects caused by amount-dependent isotope fractionation can be avoided. The suitability of acetonitrile and acetone solvents for the GC/IRMS analysis of pure methanol, ethanol and acetic acid, and commercial liquor and vinegar samples was evaluated using n-hexane and water as control solvents. All the solvents including water were separated from the analyte on a HP-INNOWAX column and were diverted away from the combustion interface. The influence of liquor matrix on the ethanol GC/IRMS analyses was evaluated by adding pure ethanol to liquor samples. Acetonitrile and acetone gave similar δ(13) C values for pure ethanol and pure acetic acid to those obtained in water and n-hexane, and also gave similar δ(13) C values of ethanol in liquor and acetic acid in white vinegar to that obtained in water. For methanol analysis, acetonitrile and refined acetone gave similar δ(13) C values to that obtained in water, but n-hexane was not a suitable solvent. In addition, isotopic fractionation caused by solvent and solute interactions was observed. We recommend using acetonitrile for the GC/IRMS analysis of aqueous alcoholic samples, and acetone for the analysis of aqueous acetic acid samples. This direct dilution method can provide high accurate and precise GC/IRMS analysis of the relative changes in δ(13) C values of methanol, ethanol, and acetic acid. Copyright © 2014 John Wiley & Sons, Ltd.

Arterial and venous embolization: Declotting of dialysis shunts by direct injection of streptokinase

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

Zeit, R.M.

1986-06-01

During the past 33 months, thrombolysis of 79 clotted hemodialysis shunts was attempted by injecting small quantities of dilute streptokinase solution directly into the clotted shunt, followed by massage of the clot. Embolization of clot fragments in six of 79 cases (7.6%) was demonstrated angiographically. In four of the six cases embolization involved the brachial artery or its branches. In one case embolization involved an arm vein, and in one case embolization involved both the bracial artery and axillary vein. All patients remained asymptomatic, and repeat angiographic study, usually performed the following day, showed resolution of the emboli in fourmore » of five cases. The incidence of embolization in direct-injection thrombolysis reported in this study appears to be comparable to that reported in studies using the streptokinase infusion technique.« less

2D temperature field measurement in a direct-injection engine using LIF technology

NASA Astrophysics Data System (ADS)

Liu, Yongfeng; Tian, Hongsen; Yang, Jianwei; Sun, Jianmin; Zhu, Aihua

2011-12-01

A new multi-spectral detection strategy for temperature laser- induced- fluorescence (LIF) 2-D imaging measurements is reported for high pressure flames in high-speed diesel engine. Schematic of the experimental set-up is outlined and the experimental data on the diesel engine is summarized. Experiment injection system is a third generation Bosch high-pressure common rail featuring a maximum pressure of 160MPa. The injector is equipped with a six-hole nozzle, where each hole has a diameter of 0.124 mm. and slightly offset to the center of the cylinder axis to allow a better cooling of the narrow bridge between the exhaust valves. The measurement system includes a blower, which supplied the intake flow rate, and a prototype single-valve direct injection diesel engine head modified to lay down the swirled-type injector. 14-bit digital CCD cameras are employed to achieve a greater level of accuracy in comparison to the results of previous measurements. The temperature field spatial distributions in the cylinder for different crank angle degrees are carried out in a single direct-injection diesel engine.

Effect of Fuel Properties on Injection Characteristics of Four Different Diesel Injection Systems.

DTIC Science & Technology

1985-12-01

Effects on Combustion in Direct Injection Diesel Engines," SAE Technical Paper Series, No. 850108, International Congress and Exposi - tion, Detroit, MI...NIEMEYER) I AMXSY-CR 1 DEFENSE STANDARDIZATION OFFICE ABE SYNR R ATTN DR MILER 1 ABERDEEN PROVING GROUND MDATTN: DR S ILLE I 10-06 . 2 1005-5006 5203

Dynamic Pore-Scale Imaging of Reactive Transport in Heterogeneous Carbonates at Reservoir Conditions Across Multiple Dissolution Regimes

NASA Astrophysics Data System (ADS)

Menke, H. P.; Bijeljic, B.; Andrew, M. G.; Blunt, M. J.

2014-12-01

Sequestering carbon in deep geologic formations is one way of reducing anthropogenic CO2 emissions. When supercritical CO2 mixes with brine in a reservoir, the acid generated has the potential to dissolve the surrounding pore structure. However, the magnitude and type of dissolution are condition dependent. Understanding how small changes in the pore structure, chemistry, and flow properties affect dissolution is paramount for successful predictive modelling. Both 'Pink Beam' synchrotron radiation and a Micro-CT lab source are used in dynamic X-ray microtomography to investigate the pore structure changes during supercritical CO2 injection in carbonate rocks of varying heterogeneity at high temperatures and pressures and various flow-rates. Three carbonate rock types were studied, one with a homogeneous pore structure and two heterogeneous carbonates. All samples are practically pure calcium carbonate, but have widely varying rock structures. Flow-rate was varied in three successive experiments by over an order of magnitude whlie keeping all other experimental conditions constant. A 4-mm carbonate core was injected with CO2-saturated brine at 10 MPa and 50oC. Tomographic images were taken at 30-second to 20-minute time-resolutions during a 2 to 4-hour injection period. A pore network was extracted using a topological analysis of the pore space and pore-scale flow modelling was performed directly on the binarized images with connected pathways and used to track the altering velocity distributions. Significant differences in dissolution type and magnitude were found for each rock type and flowrate. At the highest flow-rates, the homogeneous carbonate was seen to have predominately uniform dissolution with minor dissolution rate differences between the pores and pore throats. Alternatively, the heterogeneous carbonates which formed wormholes at high flow rates. At low flow rates the homogeneous rock developed wormholes, while the heterogeneous samples showed evidence of compact dissolution. This study serves as a unique benchmark for pore-scale reactive transport modelling directly on the binarized Micro-CT images. Dynamic pore-scale imaging methods offer advantages in helping explain the dominant processes at the pore scale so that they may be up-scaled for accurate model prediction.

Development of an efficient fractionation method for the preparative separation of sesquiterpenoids from Tussilago farfara by counter-current chromatography.

PubMed

Song, Kwangho; Lee, Kyoung Jin; Kim, Yeong Shik

2017-03-17

A novel application of counter-current chromatography (CCC) to enrich plant extracts using direct and continuous injection (CCC-DCI) was developed to fractionate sesquiterpenoids from the buds of Tussilago farfara L. In this study, an n-hexane-acetonitrile-water (HAcW) solvent system was separately pumped into the CCC column, and an extraction solution (45% acetonitrile) was directly and continuously injected into the CCC column. Since the extraction solution was used as a mobile phase in this method, solvent consumption could be greatly reduced. To enrich the extraction solution (315.9g/5.4L), only 4.2L water, 4.6L acetonitrile, and 1.2L n-hexane were used, including the extraction step. Finally, 6.8g of a sesquiterpenoid-enriched (STE) fraction was obtained from the crude extract (315.9g) of Tussilago farfara (1kg) in a single CCC run with a separation time of 8.5h. The sample injection capacity of CCC-DCI was greater than 300g; this amount of sample could not be handled in conventional CCC or other fractionation methods with the same column volume. Moreover, three major sesquiterpenoids (1: tussilagone, 2: 14-acetoxy-7β-(3'-ethyl cis-crotonoyloxy)-1α-(2'-methylburyryloxy)-notonipetranone, and 3: 7β-(3'-ethyl cis-crotonoyloxy)-1α-(2'-methylburyryloxy)-3, 14-dehydro-Z-notonipetranone) were purified from the STE fraction by CCC, and their chemical structures were elucidated by 1 H NMR and 13 C NMR. A quantification study was conducted, and the contents of compounds 1-3 in the CCC-DCI fraction were higher than those of conventional multi-step fractionations performed in series: solvent partitioning and open column chromatography. Furthermore, the average CCC-DCI recoveries were 96.1% (1), 96.9% (2), and 94.6% (3), whereas the open column chromatography recoveries were 77.7% (1), 66.5% (2), and 58.4% (3). The developed method demonstrates that CCC is a useful technique for enriching target components from natural products. Copyright © 2017 Elsevier B.V. All rights reserved.

Revisiting ocean carbon sequestration by direct injection: a global carbon budget perspective

NASA Astrophysics Data System (ADS)

Reith, Fabian; Keller, David P.; Oschlies, Andreas

2016-11-01

In this study we look beyond the previously studied effects of oceanic CO2 injections on atmospheric and oceanic reservoirs and also account for carbon cycle and climate feedbacks between the atmosphere and the terrestrial biosphere. Considering these additional feedbacks is important since backfluxes from the terrestrial biosphere to the atmosphere in response to reducing atmospheric CO2 can further offset the targeted reduction. To quantify these dynamics we use an Earth system model of intermediate complexity to simulate direct injection of CO2 into the deep ocean as a means of emissions mitigation during a high CO2 emission scenario. In three sets of experiments with different injection depths, we simulate a 100-year injection period of a total of 70 GtC and follow global carbon cycle dynamics over another 900 years. In additional parameter perturbation runs, we varied the default terrestrial photosynthesis CO2 fertilization parameterization by ±50 % in order to test the sensitivity of this uncertain carbon cycle feedback to the targeted atmospheric carbon reduction through direct CO2 injections. Simulated seawater chemistry changes and marine carbon storage effectiveness are similar to previous studies. As expected, by the end of the injection period avoided emissions fall short of the targeted 70 GtC by 16-30 % as a result of carbon cycle feedbacks and backfluxes in both land and ocean reservoirs. The target emissions reduction in the parameter perturbation simulations is about 0.2 and 2 % more at the end of the injection period and about 9 % less to 1 % more at the end of the simulations when compared to the unperturbed injection runs. An unexpected feature is the effect of the model's internal variability of deep-water formation in the Southern Ocean, which, in some model runs, causes additional oceanic carbon uptake after injection termination relative to a control run without injection and therefore with slightly different atmospheric CO2 and climate. These results of a model that has very low internal climate variability illustrate that the attribution of carbon fluxes and accounting for injected CO2 may be very challenging in the real climate system with its much larger internal variability.

Impact of Sodium Bicarbonate-Buffered Lidocaine on Patient Pain During Image-Guided Breast Biopsy.

PubMed

Vasan, Alison; Baker, Jay A; Shelby, Rebecca A; Soo, Mary Scott C

2017-09-01

This randomized, double-blind controlled study evaluated the effectiveness of sodium bicarbonate-buffered lidocaine on reducing pain during imaging-guided breast biopsies. This prospective, HIPAA-compliant study randomly assigned 85 women undergoing ultrasound- or stereotactic-guided core-needle breast biopsies to receive intradermally and intraparenchymally either 1% lidocaine buffered with sodium bicarbonate (9:1 ratio) (bicarbonate study group) or 1% lidocaine alone (control group). Pain was evaluated using a 0-to-10 Likert pain scale during both intradermal and intraparenchymal anesthesia injections and during tissue sampling. Prebiopsy breast pain, anxiety, medical history, demographics, biopsy type, radiologist level of training, breast density, and lesion histology were recorded. Data were analyzed using analysis of variance and analysis of covariance. Unadjusted mean pain scores were 1.47 and 2.07 (study and control groups, respectively; P = .15) during intradermal injections, and 1.84 and 2.98 (study and control groups, respectively; P = .03) during intraparenchymal injections. Tissue sampling mean pain scores were .81 and 1.71 (study and control groups, respectively; P = .07). Moderator analyses found (1) among patients with preprocedural pain, those in the bicarbonate group experienced less intradermal injection pain (0.85 ± 1.23) than patients in the control group (2.50 ± 2.09); (2) among patients with fatty or scattered fibroglandular tissue, those in the bicarbonate group (1.35 ± 1.95) experienced less intraparenchymal injection pain than the control group (3.52 ± 3.13); and (3) during ultrasound-guided biopsies, patients in the bicarbonate group experienced less tissue-sampling pain (0.23 ± 0.63) than the control group (1.79 ± 3.05). Overall, buffering lidocaine with sodium bicarbonate significantly reduced pain during intraparenchymal injections, and additional pain reduction was found in certain patient subgroups during intradermal injections, intraparenchymal injections, and tissue sampling. Copyright © 2017 American College of Radiology. Published by Elsevier Inc. All rights reserved.

Associations between injection risk and community disadvantage among suburban injection drug users in southwestern Connecticut, USA.

PubMed

Heimer, Robert; Barbour, Russell; Palacios, Wilson R; Nichols, Lisa G; Grau, Lauretta E

2014-03-01

Increases in drug abuse, injection, and opioid overdoses in suburban communities led us to study injectors residing in suburban communities in southwestern Connecticut, US. We sought to understand the influence of residence on risk and injection-associated diseases. Injectors were recruited by respondent-driven sampling and interviewed about sociodemographics, somatic and mental health, injection risk, and interactions with healthcare, harm reduction, substance abuse treatment, and criminal justice systems. HIV, hepatitis B and C (HBV and HCV) serological testing was also conducted. Our sample was consistent in geographic distribution and age to the general population and to the patterns of heroin-associated overdose deaths in the suburban towns. High rates of interaction with drug abuse treatment and criminal justice systems contrasted with scant use of harm reduction services. The only factors associated with both dependent variables-residence in less disadvantaged census tracts and more injection risk-were younger age and injecting in one's own residence. This contrasts with the common association among urban injectors of injection-associated risk behaviors and residence in disadvantaged communities. Poor social support and moderate/severe depression were associated with risky injection practices (but not residence in specific classes of census tracts), suggesting that a region-wide dual diagnosis approach to the expansion of harm reduction services could be effective at reducing the negative consequences of injection drug use.