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Sample records for chromatography techniques applications

  1. Separation techniques: Chromatography

    PubMed Central

    Coskun, Ozlem

    2016-01-01

    Chromatography is an important biophysical technique that enables the separation, identification, and purification of the components of a mixture for qualitative and quantitative analysis. Proteins can be purified based on characteristics such as size and shape, total charge, hydrophobic groups present on the surface, and binding capacity with the stationary phase. Four separation techniques based on molecular characteristics and interaction type use mechanisms of ion exchange, surface adsorption, partition, and size exclusion. Other chromatography techniques are based on the stationary bed, including column, thin layer, and paper chromatography. Column chromatography is one of the most common methods of protein purification. PMID:28058406

  2. Membrane-based sample preparation for ion chromatography-Techniques, instrumental configurations and applications.

    PubMed

    Frenzel, Wolfgang; Markeviciute, Inga

    2017-01-06

    Sample preparation is the bottleneck of many analytical methods, including ion chromatography (IC). Procedures based on the application of membranes are important, yet not well appreciated means for clean-up and analyte preconcentration of liquid samples. Filtration, ultrafiltration, the variety of dialysis techniques, i.e. passive dialysis, Donnan dialysis and electrodialysis, as well as gas-diffusion are being reviewed here with respect to their application in combination with IC. Instrumental aspects including hardware requirements, configuration of membrane separation units and membrane characteristics are presented. Operation in batch and flow-through mode is described with emphasis on the latter to in-line coupling with IC, permitting fully automated operation. Attention is also drawn to dialysis probes and microdialysis both providing options for in-situ measurements with inherent selective sampling of analytes and sample preparation. The respective features of the various techniques are outlined with respect to the possibilities of matrix removal and selectivity enhancement. In this article, we provide examples of application of the diverse membrane separation techniques and discuss the benefits and limitations thereof.

  3. Advancement and application of gas chromatography isotope ratio mass spectrometry techniques for atmospheric trace gas analysis

    NASA Astrophysics Data System (ADS)

    Giebel, Brian M.

    2011-12-01

    The use of gas chromatography isotope ratio mass spectrometry (GC-IRMS) for compound specific stable isotope analysis is an underutilized technique because of the complexity of the instrumentation and high analytical costs. However stable isotopic data, when coupled with concentration measurements, can provide additional information on a compounds production, transformation, loss, and cycling within the biosphere and atmosphere. A GC-IRMS system was developed to accurately and precisely measure delta13C values for numerous oxygenated volatile organic compounds having natural and anthropogenic sources. The OVOCs include methanol, ethanol, acetone, methyl ethyl ketone, 2-pentanone, and 3-pentanone. Guided by the requirements for analysis of trace components in air, the GC-IRMS system was developed with the goals of increasing sensitivity, reducing dead-volume and peak band broadening, optimizing combustion and water removal, and decreasing the split ratio to the IRMS. The technique relied on a two-stage preconcentration system, a low-volume capillary reactor and water trap, and a balanced reference gas delivery system. Measurements were performed on samples collected from two distinct sources (i.e. biogenic and vehicle emissions) and ambient air collected from downtown Miami and Everglades National Park. However, the instrumentation and the method have the capability to analyze a variety of source and ambient samples. The measured isotopic signatures that were obtained from source and ambient samples provide a new isotopic constraint for atmospheric chemists and can serve as a new way to evaluate their models and budgets for many OVOCs. In almost all cases, OVOCs emitted from fuel combustion were enriched in 13C when compared to the natural emissions of plants. This was particularly true for ethanol gas emitted in vehicle exhaust, which was observed to have a uniquely enriched isotopic signature that was attributed to ethanol's corn origin and use as an alternative

  4. Development and Application of a Fast Chromatography Technique for Analysis of Biogenic Volatile Organic Compounds in Plant Emissions

    NASA Astrophysics Data System (ADS)

    Jones, C. E.; Kato, S.; Nakashima, Y.; Yamazakii, S.; Kajii, Y. J.

    2011-12-01

    Biogenic volatile organic compounds (BVOCs) emitted from vegetation constitute the largest fraction (>90 %) of total global non-methane VOC supplied to the atmosphere, yet the chemical complexity of these emissions means that achieving comprehensive measurements of BVOCs, and in particular the less volatile terpenes, is not straightforward. As such, there is still significant uncertainty associated with the contribution of BVOCs to the tropospheric oxidation budget, and to atmospheric secondary organic aerosol (SOA) formation. The rate of BVOC emission from vegetation is regulated by environmental conditions such as light intensity and temperature, and thus can be highly variable, necessitating high time-resolution BVOC measurements. In addition, the numerous monoterpene and sesquiterpene isomers, which are indistinguishable by some analytical techniques, have greatly varying lifetimes with respect to atmospheric oxidants, and as such quantification of each individual isomer is fundamental to achieving a comprehensive characterisation of the impact of BVOCs upon the atmospheric oxidation capacity. However, established measurement techniques for these trace gases typically offer a trade-off between sample frequency and the level of speciation; detailed information regarding chemical composition may be obtained, but with reduced time resolution, or vice versa. We have developed a Fast-GC-FID technique for quantification of a range of monoterpene, sesquiterpene and oxygenated C10 BVOC isomers, which retains the separation capability of conventional gas chromatography, yet offers considerably improved sample frequency. Development of this system is ongoing, but currently a 20 m x 0.18 mm i.d resistively heated metal column is employed to achieve chromatographic separation of thirteen C10-C15 BVOCs, within a total cycle time of ~15 minutes. We present the instrument specifications and analytical capability, together with the first application of this Fast-GC technique

  5. Application of capillary gas chromatography mass spectrometry/computer techniques to synoptic survey of organic material in bed sediment

    USGS Publications Warehouse

    Steinheimer, T.R.; Pereira, W.E.; Johnson, S.M.

    1981-01-01

    A bed sediment sample taken from an area impacted by heavy industrial activity was analyzed for organic compounds of environmental significance. Extraction was effected on a Soxhlet apparatus using a freeze-dried sample. The Soxhlet extract was fractionated by silica gel micro-column adsorption chromatography. Separation and identification of the organic compounds was accomplished by capillary gas chromatography/mass spectrometry techniques. More than 50 compounds were identified; these include saturated hydrocarbons, olefins, aromatic hydrocarbons, alkylated polycyclic aromatic hydrocarbons, and oxygenated compounds such as aldehydes and ketones. The role of bed sediments as a source or sink for organic pollutants is discussed. ?? 1981.

  6. [Application of liquid chromatography in substitution of the radioimmunoassay technique in order to reduce residues generated in health services in research laboratory].

    PubMed

    Ribeiro Neto, Luciane M; Sugawara, Eduardo K; Verreschi, Ieda T N

    2008-10-01

    Designing a Health Care Service Waste Management Plan, according to the RDC 306 rules, is a responsibility of all those who produce such waste. Since radioimmunoassay (RIA) is one of the most employed techniques, we studied the impact of replacing this technique by liquid chromatography (HPLC) with regard to the reduction of the radioactive residues routinely produced by the Unifesp steroid laboratory. The residues produced by the determination of serum cortisol and 17 alpha-hydroxyprogesterone were classified, and those belonging to groups B and C were evaluated. We observed that, when RIA is used, chemical residues (group B) and radioactive waste (group C) are produced, whereas HPLC generates only chemical residues. Adequation of these techniques showed to be advantageous, by significantly reducing the time of analysis and mainly by eliminating and/or reducing the generation of radioactive waste, encouraging its application to other methodologies, as well as its adoption by other research units.

  7. Emulsion-cryogelation technique for fabricating a versatile toolbox of hierarchical polymeric monolith and its application in chromatography.

    PubMed

    Li, Yaping; Qi, Li; Li, Nan; Ma, Huimin

    2016-05-15

    A novel poly (glycidyl methacrylate-co-ethylene dimethacrylate) monolith has been fabricated via the environmental friendly cryogelation-emulsion technique. The polymerization process is assisted by self-assembly of typical tri-block copolymer Pluronic F127 at sub-zero temperature using ice crystal as template, which can avoid consumption of organic porogenic solvents and thermal unstability of emulsion system. The developed monolith possesses hierarchical networks, which is confirmed by nitrogen adsorption measurement, mercury intrusion porosimetry, scanning electron microscopy and permeability testing. Further, the effect of the amounts of Pluronic F127 on the microstructure has been investigated. Moreover, the prepared polymer monolith undergoes acidic hydrolysis of epoxy groups into hydroxyl groups on the surface and its liquid chromatographic performance is explored by separating model analytes. The results indicate that the unique porous polymer monolith with hierarchical networks could be prepared via an organic porogen-free approach and used for analysis of polar and nonpolar molecules, extending the application of cryogelation-emulsion technique and methacrylate-based monolith.

  8. Application of microscopy technique and high-performance liquid chromatography for quality assessment of the flower bud of Tussilago farfara L. (Kuandonghua)

    PubMed Central

    Li, Da; Liang, Li; Zhang, Jing; Kang, Tingguo

    2015-01-01

    Background: Quality control is one of the bottleneck problems limiting the application and development of traditional Chinese medicine (TCM). In recent years, microscopy and high-performance liquid chromatography (HPLC) techniques have been frequently applied in the quality control of TCM. However, studies combining conventional microscopy and HPLC techniques for the quality control of the flower bud of Tussilago farfara L. (Kuandonghua) have not been reported. Objective: This study was undertaken to evaluate the quality of the flower bud of T. farfara L. and to establish the relationships between the quantity of pollen grains and four main bioactive constituents: tussilagone, chlorogenic acid, rutin and isoquercitrin. Materials and Methods: In this study, microscopic examination was used to quantify microscopic characteristics of the flower bud of T. farfara L., and the chemical components were determined by HPLC. The data were analyzed by Statistical Package for the Social Sciences statistics software. Results: The results of the analysis showed that tussilagone, chlorogenic acid, rutin and isoquercitrin were significantly correlated with the quantity of pollen grains in the flower bud of T. farfara L. There is a positive correlation between them. From these results, it can be deduced that the flower bud of T. farfara L. with a greater quantity of pollen grains should be of better quality. Conclusion: The study showed that the established method can be helpful for evaluating the quality of the flower bud of T. farfara L. based on microscopic characteristic constants and chemical quantitation. PMID:26246737

  9. Application of Liquid Chromatography/Ion Trap Mass Spectrometry Technique to Determine Ergot Alkaloids in Grain Products

    PubMed Central

    Szymczyk, Krystyna; Jędrzejczak, Renata; Roszko, Marek

    2015-01-01

    Summary A liquid chromatography/ion trap mass spectrometry-based method to determine six ergot alkaloids and their isomers is presented. The samples were cleaned on neutral alumina-based solid-phase extraction cartridges. The following method parameters were obtained (depending on the analyte and spiking level): method recovery from 63.0 to 104.6%, relative standard deviation below 18%, linear range from 1 to 325 µg/kg, linear correlation coefficient not less than 0.98. The developed analytical procedure was applied to determine the levels of ergot alkaloids in 65 samples of selected rye-based food products (flour – 34 samples, bran – 12 samples, rye – 18 samples, flakes – 1 sample). Measurable levels of alkaloids were found in majority of the analysed samples, particularly in rye flour. Additionally, alkaloids were determined in ergot sclerotia isolated from rye grains. Total content was nearly 0.01% (97.9 mg/kg). However, the alkaloid profile was dominated by ergocristine at 45.6% (44.7 mg/kg), an alkaloid not commonly found in the tested food products. Ergocorninine at 0.2% (0.2 mg/kg) was the least abundant alkaloid. PMID:27904328

  10. Determination of lysergic acid diethylamide (LSD) by application of online 77 K fluorescence spectroscopy and a sweeping technique in micellar electrokinetic chromatography.

    PubMed

    Fang, Ching; Liu, Ju-Tsung; Lin, Cheng-Huang

    2002-10-16

    The principal advantage of the use of Shopl'skii effect (low temperature spectrum) is that spectral sharpening occurs both in absorption and emission. However, thus far using the technique of capillary electrophoresis/low temperature fluorescence spectroscopy (CE/LTFS) either at 77 or 4.2 K remains difficult to obtain an on-line spectrum, if the analyte is present at low concentration. This paper examines the feasibility of combining the techniques of online concentration and CE/LTFS to identify LSD and related compounds in urine at 77 K. To improve sensitivity, sweeping-micellar electrokinetic chromatography (sweeping-MEKC) and cation-selective exhaustive injection-sweep-micellar electrokinetic chromatography (CSEI-sweep-MEKC) were used for on-line concentration which resulted in detection limits of approximately 20 approximately 60 ppt, respectively.

  11. Application of Solid Sorbent Collection Techniques and High Performance Liquid Chromatography with Electrochemical Detection to the Analysis of Explosives in Water Samples.

    DTIC Science & Technology

    1986-11-01

    Methods were developed for the determination of several explosives components (nitro-organic compounds) in environmental waters. The methods are based on Porapak resin adsorption and Amberlite XAD-4 resin adsorption of the explosives are measured by high performance liquid chromatography with electrochemical detection. The technique provides a high degree of selectivity and sensitivity for these compounds in actual samples. Detection limits approach 1 microgram/l for many components.

  12. Development and application of compact denuder sampling techniques with in situ derivatization followed by gas chromatography-mass spectrometry for halogen speciation in volcanic plumes

    NASA Astrophysics Data System (ADS)

    Rüdiger, Julian; Bobrowski, Nicole; Hoffmann, Thorsten

    2015-04-01

    Volcanoes are a large source for several reactive atmospheric trace gases including sulphur and halogen containing species. The detailed knowledge of volcanic plume chemistry can give insights into subsurface processes and can be considered as a useful geochemical tool for monitoring of volcanic activity, especially halogen to sulphur ratios (e.g. Bobrowski and Giuffrida, 2012; Donovan et al., 2014). The reactive bromine species bromine monoxide (BrO) is of particular interest, because BrO as well as SO2 are readily measurable by UV spectrometers at a safe distance. Furthermore it is formed in the plume by a multiphase reaction mechanism under depletion of ozone in the plume. The abundance of BrO changes as a function of the reaction time and therefore distance from the vent as well as the spatial position in the plume. Due to the lack of analytical approaches for the accurate speciation of certain halogens (HBr, Br2, Br, BrCl, HOBr etc.) there are still uncertainties about the magnitude of volcanic halogen emissions and in particular their specificationtheir species and therefore also in the understanding of the bromine chemistry in volcanic plumes (Bobrowski et al., 2007). In this study, the first application of a 1,3,5-trimethoxybenzene (1,3,5-TMB)-coated gas diffusion denuder (Huang and Hoffmann, 2008) on volcanic gases proved to be suitable to collect selectively gaseous bromine species with oxidation states of +1 or 0 (Br2 and BrO(H)), while being ignorant to HBr (OS -1). The reaction of 1,3,5-TMB with bromine gives 1-bromo-2,4,6-trimethoxybenzene (1-bromo-2,4,6-TMB) - other halogens give corresponding products. The diffusion denuder technique allows sampling of gaseous compounds exclusively without collecting particulate matter. Choosing a flow rate of 500 mL-min-1 and a denuder length of 0.5 m a nearly quantitative collection efficiency was achieved. Solvent elution of the derivatized analytes and subsequent analysis with gas chromatography

  13. Thin layer chromatography residue applicator sampler

    DOEpatents

    Nunes, Peter J.; Kelly, Fredrick R.; Haas, Jeffrey S.; Andresen, Brian D.

    2007-07-24

    A thin layer chromatograph residue applicator sampler. The residue applicator sampler provides for rapid analysis of samples containing high explosives, chemical warfare, and other analyses of interest under field conditions. This satisfied the need for a field-deployable, small, hand-held, all-in-one device for efficient sampling, sample dissolution, and sample application to an analytical technique. The residue applicator sampler includes a sampling sponge that is resistant to most chemicals and is fastened via a plastic handle in a hermetically sealed tube containing a known amount of solvent. Upon use, the wetted sponge is removed from the sealed tube and used as a swiping device across an environmental sample. The sponge is then replaced in the hermetically sealed tube where the sample remains contained and dissolved in the solvent. A small pipette tip is removably contained in the hermetically sealed tube. The sponge is removed and placed into the pipette tip where a squeezing-out of the dissolved sample from the sponge into the pipette tip results in a droplet captured in a vial for later instrumental analysis, or applied directly to a thin layer chromatography plate for immediate analysis.

  14. Basic Principles of Planar Chromatography and Its Potential for Hyphenated Techniques

    NASA Astrophysics Data System (ADS)

    Tuzimski, Tomasz

    Sample preparation, detection, identification, and quantitative determination of biomolecules are presented in this chapter. Advantages of planar chromatography and the basic principles (chambers, sample application, and chromatogram development) are also described. Rapid detection of biomolecules plays a strategical role in their investigation. Hyphenated techniques such as planar chromatography coupled to UV diode array detection and to mass spectrometry provide on-line extensive structural information on the metabolites prior to their isolation. In this chapter, the combination of thin-layer chromatography (TLC) with biomolecules specific detection by diode array scanning (DAD), mass spectrometry (MS), nuclear magnetic resonance (NMR), and Fourier transform infrared spectroscopy (TLC-FTIR) is discussed. In the last part of the chapter, the reader will gain useful information about a recent method of planar chromatography - multidimensional planar chromatography (MD-PC) and information on application of different modes of multidimensional planar chromatography and combination of this technique with diode array detection (MD-PC-DAD) and HPLC-DAD for separation, detection, and qualitative and quantitative determination of biomolecules. Planar chromatography as a pilot technique for HPLC is also described.

  15. Ion-Exchange Chromatography: Basic Principles and Application.

    PubMed

    Cummins, Philip M; Rochfort, Keith D; O'Connor, Brendan F

    2017-01-01

    Ion-Exchange Chromatography (IEC) allows for the separation of ionizable molecules on the basis of differences in charge properties. Its large sample-handling capacity, broad applicability (particularly to proteins and enzymes), moderate cost, powerful resolving ability, and ease of scale-up and automation have led to it becoming one of the most versatile and widely used of all liquid chromatography (LC) techniques. In this chapter, we review the basic principles of IEC, as well as the broader criteria for selecting IEC conditions. By way of further illustration, we outline basic laboratory protocols to partially purify a soluble serine peptidase from bovine whole brain tissue, covering crude tissue extract preparation through to partial purification of the target enzyme using anion-exchange chromatography. Protocols for assaying total protein and enzyme activity in both pre- and post-IEC fractions are also described.

  16. Monitoring the synthesis of new pitches from coal tar and its fractions by chromatography and related techniques.

    PubMed

    Bermejo, J; Fernández, A L; Prada, V; Granda, M; Menéndez, R

    1999-07-23

    The aim of this paper is to study the applications of chromatography and related techniques in the transformation of coal-derived products into pitches for specific uses. Anthracene oil, tar and pitch were thermally treated in the presence of air (and sulfur in the case of anthracene oil) in order to cause the polymerization/condensation of their components. The evolution of the components of the parent materials during the treatments was monitored by gas chromatography-mass spectrometry, gas chromatography-atomic emission detection, probe mass spectrometry and size-exclusion chromatography. From the results obtained, possible mechanisms for the transformation of coal-derived products into new pitches were established.

  17. Application of Electromigration Techniques in Environmental Analysis

    NASA Astrophysics Data System (ADS)

    Bald, Edward; Kubalczyk, Paweł; Studzińska, Sylwia; Dziubakiewicz, Ewelina; Buszewski, Bogusław

    Inherently trace-level concentration of pollutants in the environment, together with the complexity of sample matrices, place a strong demand on the detection capabilities of electromigration methods. Significant progress is continually being made, widening the applicability of these techniques, mostly capillary zone electrophoresis, micellar electrokinetic chromatography, and capillary electrochromatography, to the analysis of real-world environmental samples, including the concentration sensitivity and robustness of the developed analytical procedures. This chapter covers the recent major developments in the domain of capillary electrophoresis analysis of environmental samples for pesticides, polycyclic aromatic hydrocarbons, phenols, amines, carboxylic acids, explosives, pharmaceuticals, and ionic liquids. Emphasis is made on pre-capillary and on-capillary chromatography and electrophoresis-based concentration of analytes and detection improvement.

  18. Application of chromatography technology in the separation of active components from nature derived drugs.

    PubMed

    Zhao, H-Y; Jiang, J-G

    2010-11-01

    Chromatography technology has been widely applied in various aspects of the pharmacy research on traditional Chinese medicine (TCM). This paper reviews literatures, published in the past decades, on the separation of active component from TCM using chromatography technology. Ultra-performance liquid chromatography (UPLC), high-speed counter-current chromatography (HSCCC), rapid resolution liquid chromatography (RRLC), supercritical fluid chromatography (SFC), affinity chromatography (AC), and bio-chromatography (BC) are introduced in detail. Compared to high performance of high-performance liquid chromatography (HPLC), analysis time and solvent loss are significantly reduced by UPLC with increase in resolution and sensitivity. Some ingredients from nature derived drugs can be separated more completely by HSCCC, which has remarkable characteristics such as low cost, simple operation and no pollution. Trace components from complex systems can be selectively and efficiently separated and purified by AC, This feature makes it effective in isolation and identification of active components of Chinese herbs. Interference of some impurities could be excluded by BC. Active ingredients that are difficult to be separated by normal method can be acquired by SFC. Currently, application of novel chromatography techniques in TCM is still in the exploratory stage and many problems, such as preparation of stationary phase and detection, need to be solved.

  19. Chromatography.

    ERIC Educational Resources Information Center

    Brantley, L. Reed, Sr.; Demanche, Edna L.; Klemm, E. Barbara; Kyselka, Will; Phillips, Edwin A.; Pottenger, Francis M.; Yamamoto, Karen N.; Young, Donald B.

    This booklet presents some activities on chromatography. Directions for preparing leaf pigment extracts using alcohol are given, and paper chromatography and thin-layer chromatography are described as modifications of the basic principles of chromatography. (KHR)

  20. High Performance Liquid Chromatography/Video Fluorometry. Part II. Applications.

    DTIC Science & Technology

    1981-09-30

    HIGH PERFORMANCE LIQUID CHROMATOGRAPHY /VIDEO FLUOROMETRY. PART...REP«T_N&:-ŗ/ High Performance Liquid Chromatography /Video Fluorometry» Part II. Applications« by | Dennis C./Shelly* Michael P./Vogarty and...Data EnlirtdJ REPORT DOCUMENTATION PAGE t. REPORT NUMBER 2 GOVT ACCESSION NO 4. T1TI.F (and Submit) lP-^fffsyva High Performance Liquid Chromatography

  1. Immunoaffinity chromatography: an introduction to applications and recent developments

    PubMed Central

    Moser, Annette C

    2010-01-01

    Immunoaffinity chromatography (IAC) combines the use of LC with the specific binding of antibodies or related agents. The resulting method can be used in assays for a particular target or for purification and concentration of analytes prior to further examination by another technique. This review discusses the history and principles of IAC and the various formats that can be used with this method. An overview is given of the general properties of antibodies and of antibody-production methods. The supports and immobilization methods used with antibodies in IAC and the selection of application and elution conditions for IAC are also discussed. Several applications of IAC are considered, including its use in purification, immunodepletion, direct sample analysis, chromatographic immunoassays and combined analysis methods. Recent developments include the use of IAC with CE or MS, ultrafast immunoextraction methods and the use of immunoaffinity columns in microanalytical systems. PMID:20640220

  2. Indirect fluorometric detection techniques on thin layer chromatography and effect of ultrasound on gel electrophoresis

    SciTech Connect

    Yinfa, Ma.

    1990-12-10

    Thin-layer chromatography (TLC) is a broadly applicable separation technique. It offers many advantages over high performance liquid chromatography (HPLC), such as easily adapted for two-dimensional separation, for whole-column'' detection and for handling multiple samples, etc. However, due to its draggy development of detection techniques comparing with HPLC, TLC has not received the attention it deserves. Therefore, exploring new detection techniques is very important to the development of TLC. It is the principal of this dissertation to present a new detection method for TLC -- indirect fluorometric detection method. This detection technique is universal sensitive, nondestructive, and simple. This will be described in detail from Sections 1 through Section 5. Section 1 and 3 describe the indirect fluorometric detection of anions and nonelectrolytes in TLC. In Section 2, a detection method for cations based on fluorescence quenching of ethidium bromide is presented. In Section 4, a simple and interesting TLC experiment is designed, three different fluorescence detection principles are used for the determination of caffeine, saccharin and sodium benzoate in beverages. A laser-based indirect fluorometric detection technique in TLC is developed in Section 5. Section 6 is totally different from Sections 1 through 5. An ultrasonic effect on the separation of DNA fragments in agarose gel electrophoresis is investigated. 262 refs.

  3. Recent applications of hydrophilic interaction liquid chromatography in pharmaceutical analysis.

    PubMed

    Zhang, Qian; Yang, Feng-Qing; Ge, Liya; Hu, Yuan-Jia; Xia, Zhi-Ning

    2017-01-01

    Hydrophilic interaction liquid chromatography, an alternative liquid chromatography mode, is of particular interest in separating hydrophilic and polar ionic compounds. Compared with traditional liquid chromatography techniques, hydrophilic interaction liquid chromatography offers specific advantages mainly including: (1) relatively green and water-soluble mobile phase composition, which enhances the solubility of hydrophilic and polar ionic compounds; (2) no need for ion-pairing reagents and high content of organic solvent, which benefits mass spectrometry detection; (3) high orthogonality to reverse-phase liquid chromatography, well adapted to two-dimensional liquid chromatography for complicated samples. Therefore, hydrophilic interaction liquid chromatography has been rapidly developed in many areas over the past decades. This review summarizes the recent progress (from 2012 to July 2016) of hydrophilic interaction liquid chromatography in pharmaceutical analysis, with the focus on detecting chemical drugs in various matrices, charactering active compounds of natural products and assessing biotherapeutics through typical structure unit. Moreover, the retention mechanism and behavior of analytes in hydrophilic interaction liquid chromatography as well as some novel hydrophilic interaction liquid chromatography columns used for pharmaceutical analysis are also described.

  4. Vapor Pressure Determination of VM Using the Denunder-Liquid Chromatography-Mass Spectrometry Technique

    DTIC Science & Technology

    2015-01-01

    LIQUID CHROMATOGRAPHY –MASS SPECTROMETRY TECHNIQUE ECBC-TR-1278 Amanda L. Jenkins ASK, INC. Hebron, MD 21830-1224 Eric J. Bruni LEIDOS, INC...2012 – Sep 2012 4. TITLE AND SUBTITLE Vapor Pressure Determination of VM Using the Denuder–Liquid Chromatography –Mass Spectrometry Technique 5a...a novel, denuder-based liquid chromatography –mass spectrometry (LC–MS) approach designed specifically for low- volatility and thermally unstable

  5. Simultaneous analysis for water- and fat-soluble vitamins by a novel single chromatography technique unifying supercritical fluid chromatography and liquid chromatography.

    PubMed

    Taguchi, Kaori; Fukusaki, Eiichiro; Bamba, Takeshi

    2014-10-03

    Chromatography techniques usually use a single state in the mobile phase, such as liquid, gas, or supercritical fluid. Chromatographers manage one of these techniques for their purpose but are sometimes required to use multiple methods, or even worse, multiple techniques when the target compounds have a wide range of chemical properties. To overcome this challenge, we developed a single method covering a diverse compound range by means of a "unified" chromatography which completely bridges supercritical fluid chromatography and liquid chromatography. In our method, the phase state was continuously changed in the following order; supercritical, subcritical and liquid. Moreover, the gradient of the mobile phase starting at almost 100% CO2 was replaced with 100% methanol at the end completely. As a result, this approach achieved further extension of the polarity range of the mobile phase in a single run, and successfully enabled the simultaneous analysis of fat- and water-soluble vitamins with a wide logP range of -2.11 to 10.12. Furthermore, the 17 vitamins were exceptionally separated in 4min. Our results indicated that the use of dense CO2 and the replacement of CO2 by methanol are practical approaches in unified chromatography covering diverse compounds. Additionally, this is a first report to apply the novel approach to unified chromatography, and can open another door for diverse compound analysis in a single chromatographic technique with single injection, single column and single system.

  6. Application of coupled affinity-sizing chromatography for the detection of proteolyzed HSA-tagged proteins.

    PubMed

    London, Anne Serdakowski; Patel, Kunal; Quinn, Lisa; Lemmerer, Martin

    2015-04-01

    Coupled affinity liquid chromatography and size exclusion chromatography (ALC-SEC) is a technique that has been shown to successfully report product quality of proteins during cell expression and prior to the commencement of downstream processing chromatography steps. This method was applied to monitoring the degradation and subsequent partial remediation of a HSA-tagged protein which showed proteolysis, allowing for rapid cell line development to address this product quality dilemma. This paper outlines the novel application of this method for measuring and addressing protease-induced proteolysis.

  7. Applications of resistive heating in gas chromatography: a review.

    PubMed

    Jacobs, Matthew R; Hilder, Emily F; Shellie, Robert A

    2013-11-25

    Gas chromatography is widely applied to separate, identify, and quantify components of samples in a timely manner. Increasing demand for analytical throughput, instrument portability, environmental sustainability, and more economical analysis necessitates the development of new gas chromatography instrumentation. The applications of resistive column heating technologies have been espoused for nearly thirty years and resistively heated gas chromatography has been commercially available for the last ten years. Despite this lengthy period of existence, resistively heated gas chromatography has not been universally adopted. This low rate of adoption may be partially ascribed to the saturation of the market with older convection oven technology, coupled with other analytical challenges such as sampling, injection, detection and data processing occupying research. This article assesses the advantages and applications of resistive heating in gas chromatography and discusses practical considerations associated with adoption of this technology.

  8. ENVIRONMENTAL APPLICATION OF GAS CHROMATOGRAPHY/ATOMIC EMISSION DETECTION

    EPA Science Inventory

    A gas chromatography/atomic emission detector (GC/AED) system has been evaluated for its applicability to environmental analysis. Detection limits, elemental response factors, and regression analysis data were determined for 58 semivolatile environmental contaminants. Detection l...

  9. [Applications of fast and ultra performance liquid chromatography in the analysis of Chinese herbal medicines].

    PubMed

    Liu, Ying; Zhou, Jianliang; Li, Ping

    2009-09-01

    The analysis of chemical components of Chinese herbal medicines (CHMs) is one of the most critical issues not only for screening and analyzing the bioactive components but also for controlling their quality. However, due to the complexity of the chemical constituents of CHMs, it is difficult to separate them on column within a short time. In the recent, the fast and ultra performance liquid chromatography, including ultra high pressure liquid chromatography, high performance liquid chromatography based on the monolithic columns and high temperature liquid chromatography, are of particular interest because of the high resolution and fast analytical speed provided by these techniques. This overview covers the principle and separation characteristics of these techniques, as well as their applications in Chinese herbal medicines.

  10. Photogrammetric techniques for aerospace applications

    NASA Astrophysics Data System (ADS)

    Liu, Tianshu; Burner, Alpheus W.; Jones, Thomas W.; Barrows, Danny A.

    2012-10-01

    Photogrammetric techniques have been used for measuring the important physical quantities in both ground and flight testing including aeroelastic deformation, attitude, position, shape and dynamics of objects such as wind tunnel models, flight vehicles, rotating blades and large space structures. The distinct advantage of photogrammetric measurement is that it is a non-contact, global measurement technique. Although the general principles of photogrammetry are well known particularly in topographic and aerial survey, photogrammetric techniques require special adaptation for aerospace applications. This review provides a comprehensive and systematic summary of photogrammetric techniques for aerospace applications based on diverse sources. It is useful mainly for aerospace engineers who want to use photogrammetric techniques, but it also gives a general introduction for photogrammetrists and computer vision scientists to new applications.

  11. Halogen speciation in volcanic plumes - Development of compact denuder sampling techniques with in-situ derivatization followed by gas chromatography-mass spectrometry and their application at Mt. Etna, Mt. Nyiragongo and Mt. Nyamulagira in 2015.

    NASA Astrophysics Data System (ADS)

    Rüdiger, Julian; Bobrowski, Nicole; Hoffmann, Thorsten

    2016-04-01

    products. The diffusion denuder technique allows sampling of gaseous compounds exclusively without collecting particulate matter. Solvent elution of the derivatized analytes and subsequent analysis with gas chromatography-mass spectrometry gives a limit of detection below 1 ng of bromine. The method was applied in 2015 on volcanic gas plumes at Mt. Etna (Italy), Mt. Nyiragongo and Mt. Nyamulagira (DR Congo) giving reactive bromine mixing ratios from 0.3 ppb (Nyiragongo) up to 22 ppb (Etna, NEC). Compared with total halogen data derived by alkaline trap sampling (Raschig-tube) and ion-chromatography analysis the reactive bromine mixing ratios allow the investigation of the conversion of HBr into reactive species due to plume chemistry with progressing plume age. The new method will be described in detail and the first results on the reactive halogen to total halogen output will be discussed (for bromine and chlorine) and compared to earlier volcanic plume chemistry model studies. References Bobrowski, N. and G. Giuffrida: Bromine monoxide / sulphur dioxide ratios in relation to volcanological observations at Mt. Etna 2006-2009. Solid Earth, 3, 433-445, 2012 Bobrowski, N., R. von Glasow, A. Aiuppa, S. Inguaggiato, I. Louban, O. W. Ibrahim and U. Platt: Reactive halogen chemistry in volcanic plumes. J. Geophys. Res., 112, 2007 Donovan A., V. Tsanev, C. Oppenheimer and M. Edmonds: Reactive halogens (BrO and OClO) detected in the plume of Soufrière Hills Volcano during an eruption hiatus. Geochem. Geophys. Geosyst., 15, 3346-3363, 2014 Rüdiger, J., N. Bobrowski, T. Hoffmann (2015), Development and application of compact denuder sampling techniques with in situ derivatization followed by gas chromatography-mass spectrometry for halogen speciation in volcanic plumes (EGU2015-2392-2), EGU General Assembly 2015

  12. Less common applications of monoliths III. Gas chromatography

    PubMed Central

    Svec, Frantisek; Kurganov, Alexander A.

    2008-01-01

    Porous polymer monoliths emerged about two decades ago. Despite this short time, they are finding applications in a variety of fields. In addition to the most common and certainly best known use of this new category of porous media as stationary phases in liquid chromatography, monolithic materials also found their applications in other areas. This review article focuses on monoliths in capillaries designed for separations in gas chromatography. PMID:17645884

  13. Applications of Electromigration Techniques: Applications of Electromigration Techniques in Food Analysis

    NASA Astrophysics Data System (ADS)

    Wieczorek, Piotr; Ligor, Magdalena; Buszewski, Bogusław

    Electromigration techniques, including capillary electrophoresis (CE), are widely used for separation and identification of compounds present in food products. These techniques may also be considered as alternate and complementary with respect to commonly used analytical techniques, such as high-performance liquid chromatography (HPLC), or gas chromatography (GC). Applications of CE concern the determination of high-molecular compounds, like polyphenols, including flavonoids, pigments, vitamins, food additives (preservatives, antioxidants, sweeteners, artificial pigments) are presented. Also, the method developed for the determination of proteins and peptides composed of amino acids, which are basic components of food products, are studied. Other substances such as carbohydrates, nucleic acids, biogenic amines, natural toxins, and other contaminations including pesticides and antibiotics are discussed. The possibility of CE application in food control laboratories, where analysis of the composition of food and food products are conducted, is of great importance. CE technique may be used during the control of technological processes in the food industry and for the identification of numerous compounds present in food. Due to the numerous advantages of the CE technique it is successfully used in routine food analysis.

  14. Use of Chromatography Techniques to Separate a Mixture of Substances

    ERIC Educational Resources Information Center

    Donaldson, W.

    1976-01-01

    Explains the separation of the constituents of mixtures on one piece of chromatography paper. The example presented involves a vitamin C tablet, a disprin tablet, and a glucose tablet. Outlined are two methods for separating the constituents. (GS)

  15. Advanced techniques for energy-efficient industrial-scale continuous chromatography

    SciTech Connect

    DeCarli, J.P. II ); Carta, G. . Dept. of Chemical Engineering); Byers, C.H. )

    1989-11-01

    Continuous annular chromatography (CAC) is a developing technology that allows truly continuous chromatographic separations. Previous work has demonstrated the utility of this technology for the separation of various materials by isocratic elution on a bench scale. Novel applications and improved operation of the process were studied in this work, demonstrating that CAC is a versatile apparatus which is capable of separations at high throughput. Three specific separation systems were investigated. Pilot-scale separations at high loadings were performed using an industrial sugar mixture as an example of scale-up for isocratic separations. Bench-scale experiments of a low concentration metal ion mixture were performed to demonstrate stepwise elution, a chromatographic technique which decreases dilution and increases sorbent capacity. Finally, the separation of mixtures of amino acids by ion exchange was investigated to demonstrate the use of displacement development on the CAC. This technique, which perhaps has the most potential, when applied to the CAC allowed simultaneous separation and concentration of multicomponent mixtures on a continuous basis. Mathematical models were developed to describe the CAC performance and optimize the operating conditions. For all the systems investigated, the continuous separation performance of the CAC was found to be very nearly the same as the batchwise performance of conventional chromatography. the technology appears, thus, to be very promising for industrial applications. 43 figs., 9 tabs.

  16. Gas Chromatography.

    ERIC Educational Resources Information Center

    Karasek, Francis W.; And Others

    1984-01-01

    This review covers fundamental developments in gas chromatography during 1982 and 1983. Literature is considered under these headings: columns; liguid phases; solid supports; sorption processes and solvents; open tubular column gas chromatography; instrumentation; high-resolution columns and applications; other techniques; qualitative and…

  17. Recent advances in bioprocessing application of membrane chromatography.

    PubMed

    Orr, Valerie; Zhong, Luyang; Moo-Young, Murray; Chou, C Perry

    2013-01-01

    Compared to traditional chromatography using resins in packed-bed columns, membrane chromatography is a relatively new and immature bioseparation technology based on the integration of membrane filtration and liquid chromatography into a single-stage operation. Over the past decades, advances in membrane chemistry have yielded novel membrane devices with high binding capacities and improved mass transfer properties, significantly increasing the bioprocessing efficiency for purification of biomolecules. Due to the disposable nature, low buffer consumption, and reduced equipment costs, membrane chromatography can significantly reduce downstream bioprocessing costs. In this review, we discuss technological merits and disadvantages associated with membrane chromatography as well as recent bioseparation applications with a particular attention on purification of large biomolecules.

  18. A practical strategy for characterization of the metabolic profile of chiral drugs using combinatory liquid chromatography-mass spectrometric techniques: application to tetrahydropalmatine enantiomers and their metabolites in rat urine.

    PubMed

    Zhang, Yinying; Dong, Xin; Le, Jian; Wen, Jun; Lin, Zebin; Liu, Yinli; Lou, Ziyang; Chai, Yifeng; Hong, Zhanying

    2014-06-01

    The characterization and quantification of the metabolites of chiral drugs still remain a great challenge due to the complexity of the metabolites and most of them are not commercially available. In this study, a practical approach based on the combinatory liquid chromatography-mass spectrometric techniques has been proposed for the evaluation of metabolism profiles and urinary excretion kinetics of chiral drugs and their metabolites. Racemic tetrahydropalmatine (rac-THP), a biologically active ingredient isolated from a traditional Chinese herb Rhizoma Corydalis, was chosen as the model chiral drug. Ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF/MS) was applied to characterize the metabolites of THP enantiomers in rat urine after administration of (+)-THP or (-)-THP. Accurate mass measurement was used to determine the elemental composition of metabolites and thus to confirm the proposed structures of these metabolites. More than 30 potential metabolites were found in rat urine, most of which were identified for the first time, and the metabolic pathways in vivo were involved in demethylation, oxidation, glucuronide conjugation and sulfation, etc. And the tridesmethlyzed metabolite and didesmethlyzed coupled with oxidation metabolite were found only in (+)-THP treated rats. Afterwards, a liquid chromatography tandem mass spectrometry (LC-QqQ/MS) assay was developed and validated for the determination of the urine level of THP enantiomers and their metabolites. Semi-quantification of three phase I metabolites and two phase II metabolites were performed. Enantiomeric (-/+) cumulative urinary excretion ratios of THP and its five metabolites were obtained, which indicated the stereoselective aspects of metabolites of THP enantiomers in vivo. The study demonstrated the enormous potential of this strategy for the qualitative characterization, quantitative assay and the stereoselectivity of chiral drugs and their

  19. An Application of Trimethylsilyl Derivatives with Temperature Programmed Gas Chromatography to the Senior Analytical Laboratory.

    ERIC Educational Resources Information Center

    Kelter, Paul B.; Carr, James D.

    1983-01-01

    Describes an experiment designed to teach temperature programed gas chromatography (TPGC) techniques and importance of derivatizing many classes of substrated to be separated. Includes equipment needed, procedures for making trimethylsilyl derivatives, applications, sample calculations, and typical results. Procedure required one, three-hour…

  20. Application of gas chromatography to analysis of spirit-based alcoholic beverages.

    PubMed

    Wiśniewska, Paulina; Śliwińska, Magdalena; Dymerski, Tomasz; Wardencki, Waldemar; Namieśnik, Jacek

    2015-01-01

    Spirit-based beverages are alcoholic drinks; their production processes are dependent on the type and origin of raw materials. The composition of this complex matrix is difficult to analyze, and scientists commonly choose gas chromatography techniques for this reason. With a wide selection of extraction methods and detectors it is possible to provide qualitative and quantitative analysis for many chemical compounds with various functional groups. This article describes different types of gas chromatography techniques and their most commonly used associated extraction techniques (e.g., LLE, SPME, SPE, SFE, and SBME) and detectors (MS, TOFMS, FID, ECD, NPD, AED, O or EPD). Additionally, brief characteristics of internationally popular spirit-based beverages and application of gas chromatography to the analysis of selected alcoholic drinks are presented.

  1. Data compression techniques and applications

    NASA Astrophysics Data System (ADS)

    Benelli, G.; Cappellini, V.; Lotti, F.

    1980-02-01

    The paper reviews several data compression methods for signal and image digital processing and transmission, including both established and more recent techniques. Attention is also given to methods of prediction-interpolation, differential pulse code modulation, delta modulation and transformations. The processing of two dimensional data is also considered, and the results of the application of these techniques to space telemetry and biomedical digital signal processing and telemetry systems are presented.

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

    PubMed

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

    2014-03-07

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

  3. multiplex gas chromatography: A novel analytical technique for future planetary studies

    NASA Technical Reports Server (NTRS)

    Valentin, J. R.; Carle, G. C.; Phillips, J. B.

    1986-01-01

    Determination of molecular species comprised of the biogenic elements in the atmospheres of planets and moons of the solar system is one the foremost requirements of the exobiologist studying chemical evolution and the origin of life. Multiplex chromatography is a technique where many samples are pseudo-randomly introduced to the chromatograph without regard to elution of preceding components. The resulting data are then reduced using mathematical techniques such as cross correlation or Fourier Transforms. To demonstrate the utility of this technique for future solar system exploration, chemical modulators were developed. Several advantages were realized from this technique in combination with these modulators: improvement in detection limits of several orders of magnitude, improvement in the analysis of complex mixtures by selectively modulating some of the components present in the sample, increase in the number of analyses that can be conducted in a given period of time, and reduction in the amount of expendables needed to run an analysis. In order to apply this technique in a real application, methane in ambient air was monitored continuously over a period of one week. By using ambient air as its own carrier all expendables beyond power were eliminated.

  4. Chromatography

    MedlinePlus

    Chromatography is a way of separating two or more chemical compounds. Chemical compounds are chemicals that are ... of chemical compound. There are different kinds of chromatography. These include gas, high pressure liquid, or ion ...

  5. Applications of hydrophilic interaction chromatography to amino acids, peptides, and proteins.

    PubMed

    Periat, Aurélie; Krull, Ira S; Guillarme, Davy

    2015-02-01

    This review summarizes the recent advances in the analysis of amino acids, peptides, and proteins using hydrophilic interaction chromatography. Various reports demonstrate the successful analysis of amino acids under such conditions. However, a baseline resolution of the 20 natural amino acids has not yet been published and for this reason, there is often a need to use mass spectrometry for detection to further improve selectivity. Hydrophilic interaction chromatography is also recognized as a powerful technique for peptide analysis, and there are a lot of papers showing its applicability for proteomic applications (peptide mapping). It is expected that its use for peptide mapping will continue to grow in the future, particularly because this analytical strategy can be combined with reversed-phase liquid chromatography, in a two-dimensional setup, to reach very high resolving power. Finally, the interest in hydrophilic interaction chromatography for intact proteins analysis is less evident due to possible solubility issues and a lack of suitable hydrophilic interaction chromatography stationary phases. To date, it has been successfully employed only for the characterization of membrane proteins, histones, and the separation of glycosylated isoforms of an intact glycoprotein. From our point of view, the number of hydrophilic interaction chromatography columns compatible with intact proteins (higher upper temperature limit, large pore size, etc.) is still too limited.

  6. Use and application of hydrophobic interaction chromatography for protein purification.

    PubMed

    McCue, Justin T

    2014-01-01

    The objective of this section is to provide the reader with guidelines and background on the use and experimental application of Hydrophobic Interaction chromatography (HIC) for the purification of proteins. The section will give step by step instructions on how to use HIC in the laboratory to purify proteins. General guidelines and relevant background information is also provided.

  7. Application of an online ion chromatography-based instrument ...

    EPA Pesticide Factsheets

    In North America, the dry component of total nitrogen and sulfur deposition remains uncertain due to a lack of measurements of sufficient chemical speciation and temporal extent to develop complete annual mass budgets or of sufficient process level detail to improve current air-surface exchange models. Over the past decade, significant advances have been made in the development of continuous chemical measurement techniques with sufficient sensitivity and temporal resolution to directly quantify air-surface exchange of nitrogen and sulfur compounds. However, their applicability is generally restricted to only one or a few of the compounds within the deposition budget. We characterize for the first time the performance of the Monitor for AeRosols and GAses in ambient air (MARGA), an on-line ion chromatography-based analyzer, as applied for air-surface exchange measurements of HNO3, NH3, NH4+, NO3-, SO2 and SO42-. Analytical accuracy and precision are assessed under field conditions and total uncertainty of fluxes measured by the aerodynamic gradient method are assessed for a representative 3-week period in the fall of 2012. During this period, percentages of hourly chemical gradients larger than the corresponding gradient detection limit were 86%, 55%, 81%, 74%, 77%, and 71% for NH3, NH4+, HNO3, NO3-, SO2, and SO42-, respectively. As expected, percentages were lowest for aerosol species, owing to their relatively low deposition velocities and correspondingly sma

  8. Simultaneous quantification of chrysophanol and physcion in rat plasma by ultra fast liquid chromatography-tandem mass spectrometry and application of the technique to comparative pharmacokinetic studies of Radix et Rhei Rhizoma extract alone and Dahuang Fuzi Decoction.

    PubMed

    Liu, Xiao; Li, Huan; Wu, Li; Xing, Jiangwa; Poh, Yanhong; Cai, Hao; Cai, Bao Chang

    2015-02-01

    Most herbal medicines are prescribed in combination based on the theory of TCM to obtain synergistic effects or diminish the possible adverse reactions. Compatibility refers to the combination of two or more herbs based on the clinical settings and the properties of herbs. Chrysophanol and physcion are the main effective compounds in Radix et Rhizoma Rhei and Dahuang Fuzi Decoction which is the combination of Radix et Rhizoma Rhei, Radix Aconiti Lateralis Praeparata and Radix et Rhizoma Asari. However, chrysophanol and physcion are difficult to detect in vivo because of their low concentration and interference from endogenous compounds. The aim of this study is to develop a rapid, specific and sensitive ultra high performance liquid chromatography-triple quadrupole tandem mass method to simultaneously quantify chrysophanol and physcion in rat plasma, in order to better understand the pharmacokinetics and compatibility mechanism of Dahuang Fuzi Decoction for the first time. Multiple reaction monitoring (MRM) mode was applied for the quantitation at [M-H](-)m/z 253.0→m/z 225.1 for chrysophanol, [M-H](-) for m/z 283.1→m/z 240.0 physcion and [M-H](-)m/z 239.0→m/z 211.0 for IS. The analytes were separated on an Agilent Eclipse plus C18 column (100mm×2.1mm, 1.8μm) column within a total running time of 6.5min using a mixture of 3mM ammonium acetate in water and methanol (95:5, v/v) with a time program flow gradient according to the "plus gradient chromatography" theory. The inclusion of the ammonium acetate in the UFLC mobile phase dramatically improved the detection limit of the tested compounds and decreased the interference by matrix effects, which have been referred to as "LC-electrolyte effects". Finally, we demonstrated the application of a validated method in a comparative pharmacokinetic study of rats receiving an oral dose of Dahuang Fuzi Decoction or Radix et Rhei Rhizoma, the monarch drug in the prescription. Pharmacokinetic parameters showed

  9. Neptunium(III) application in extraction chromatography.

    PubMed

    Guérin, Nicolas; Nadeau, Kenny; Larivière, Dominic

    2011-12-15

    This paper describes a novel strategy for actinide separation by extraction chromatography with Np(III) valence adjustment. Neptunium(IV) was reduced to Np(III) using Cr(II) and then selectively separated from uranium (IV) on a TEVA resin. After elution, Np(III) was retained on a DGA resin in order to remove any detrimental chromium impurities. Neptunium(III) formation was demonstrated by the complete and selective elution of Np from TEVA resin (99 ± 7%) in less than 12 mL of 9M HCl from U(IV) (0.7 ± 0.7%). It was determined by UV-visible and kinetic studies that Cr(II) was the only species responsible for the elution of Np(IV) as Np(III) and that the Cr(II) solution could be prepared from 2 to 30 min before its use without the need of complex degassing systems to prevent the oxidation of Np(III) by oxygen. The methodology proposed here with TEVA/DGA resins provides removal of Cr(III) impurities produced at high decontamination factors (2.8 × 10(3) and 7.3 × 10(4) respectively).

  10. Diamond based adsorbents and their application in chromatography.

    PubMed

    Peristyy, Anton A; Fedyanina, Olga N; Paull, Brett; Nesterenko, Pavel N

    2014-08-29

    The idea of using diamond and diamond containing materials in separation sciences has attracted a strong interest in the past decade. The combination of a unique range of properties, such as chemical inertness, mechanical, thermal and hydrolytic stability, excellent thermal conductivity with minimal thermal expansion and intriguing adsorption properties makes diamond a promising material for use in various modes of chromatography. This review summarises the recent research on the preparation of diamond and diamond based stationary phases, their properties and chromatographic performance. Special attention is devoted to the dominant retention mechanisms evident for particular diamond containing phases, and their subsequent applicability to various modes of chromatography, including chromatography carried out under conditions of high temperature and pressure.

  11. Microgravimetric Techniques for Geotechnical Applications

    DTIC Science & Technology

    1980-09-01

    Teoria ed Applicata, Vol 13, pp 254-263. Jung, K. 1961. Schwerkraftverfahren in der Angewandten Geophysik, Geest’ und Portig, Leipzig. LaFehr, T. R ...8217"· f ~;-,~". 11 ... , " j MISCRLAN~OUS PAP~ R GL-80-13 ML::ROGRAVIMETRIC TECHNIQUES FOR GEC)TECHNICAL APPLICATIONS by Dv1ain K. Butler...for Assistant: Secrel:ary of the Army ( R &-D) Department: of the Army ’’’/ashington, D. C. 20310 Under Project No. 4AI61101A91D RO 10 .1

  12. Pinch technique: Theory and applications

    NASA Astrophysics Data System (ADS)

    Binosi, Daniele; Papavassiliou, Joannis

    2009-08-01

    We review the theoretical foundations and the most important physical applications of the Pinch Technique (PT). This general method allows the construction of off-shell Green’s functions in non-Abelian gauge theories that are independent of the gauge-fixing parameter and satisfy ghost-free Ward identities. We first present the diagrammatic formulation of the technique in QCD, deriving, at one loop, the gauge independent gluon self-energy, quark-gluon vertex, and three-gluon vertex, together with their Abelian Ward identities. The generalization of the PT to theories with spontaneous symmetry breaking is carried out in detail, and the profound connection with the optical theorem and the dispersion relations are explained within the electroweak sector of the Standard Model. The equivalence between the PT and the Feynman gauge of the Background Field Method (BFM) is elaborated, and the crucial differences between the two methods are critically scrutinized. A variety of field theoretic techniques needed for the generalization of the PT to all orders are introduced, with particular emphasis on the Batalin-Vilkovisky quantization method and the general formalism of algebraic renormalization. The main conceptual and technical issues related to the extension of the technique beyond one loop are described, using the two-loop construction as a concrete example. Then the all-order generalization is thoroughly examined, making extensive use of the field theoretic machinery previously introduced; of central importance in this analysis is the demonstration that the PT-BFM correspondence persists to all orders in perturbation theory. The extension of the PT to the non-perturbative domain of the QCD Schwinger-Dyson equations is presented systematically, and the main advantages of the resulting self-consistent truncation scheme are discussed. A plethora of physical applications relying on the PT are finally reviewed, with special emphasis on the definition of gauge

  13. Recent progress and applications of ion-exclusion/ion-exchange chromatography for simultaneous determination of inorganic anions and cations.

    PubMed

    Nakatani, Nobutake; Kozaki, Daisuke; Mori, Masanobu; Tanaka, Kazuhiko

    2012-01-01

    One of the ultimate goals of ion chromatography is to determine both anions and cations found in samples with a single chromatographic run. In the present article, recent progress in ion-exclusion/ion-exchange chromatography for the simultaneous determinations of inorganic anions and cations are reviewed. Firstly, the principle and the control for the simultaneous separation and detection of analyte ions using ion-exclusion/cation-exchange chromatography with a weakly acidic cation-exchange column are outlined. Then, advanced chromatographic techniques in terms of analytical time, selectively and sensitivity are summarized. As a related method, ion-exclusion/anion-exchange chromatography with an anion-exchange column could be used for the simultaneous determination of inorganic nitrogen species, such as ammonium, nitrite and nitrate ions. Their usefulness and applications to water-quality monitoring and related techniques are also described.

  14. High-performance thin layer chromatography: A powerful analytical technique in pharmaceutical drug discovery

    PubMed Central

    Attimarad, Mahesh; Ahmed, K. K. Mueen; Aldhubaib, Bandar E.; Harsha, Sree

    2011-01-01

    Analysis of pharmaceutical and natural compounds and newer drugs is commonly used in all the stages of drug discovery and development process. High-performance thin layer chromatography is one of the sophisticated instrumental techniques based on the full capabilities of thin layer chromatography. The advantages of automation, scanning, full optimization, selective detection principle, minimum sample preparation, hyphenation, and so on enable it to be a powerful analytical tool for chromatographic information of complex mixtures of pharmaceuticals, natural products, clinical samples, food stuffs, and so on. PMID:23781433

  15. Basic Principles of Chromatography

    NASA Astrophysics Data System (ADS)

    Ismail, Baraem; Nielsen, S. Suzanne

    Chromatography has a great impact on all areas of analysis and, therefore, on the progress of science in general. Chromatography differs from other methods of separation in that a wide variety of materials, equipment, and techniques can be used. [Readers are referred to references (1-19) for general and specific information on chromatography.]. This chapter will focus on the principles of chromatography, mainly liquid chromatography (LC). Detailed principles and applications of gas chromatography (GC) will be discussed in Chap. 29. In view of its widespread use and applications, high-performance liquid chromatography (HPLC) will be discussed in a separate chapter (Chap. 28). The general principles of extraction are first described as a basis for understanding chromatography.

  16. Ultrasound Techniques for Space Applications

    NASA Technical Reports Server (NTRS)

    Rooney, James A.

    1985-01-01

    Ultrasound has proven to be a safe non-invasive technique for imaging organs and measuring cardiovascular function. It has unique advantages for application to problems with man in space including evaluation of cardiovascular function both in serial studies and during critical operations. In addition, specialized instrumentation may be capable of detecting the onset of decompression sickness during EVA activities. A spatial location and three-dimensional reconstruction system is being developed to improve the accuracy and reproducibility for serial comparative ultrasound studies of cardiovascular function. The three-dimensional method permits the acquisition of ultrasonic images from many views that can be recombined into a single reconstruction of the heart or vasculature. In addition to conventional imaging and monitoring systems, it is sometimes necessary or desirable to develop instrumentation for special purposes. One example of this type of development is the design of a pulsed-Doppler system to monitor cerebral blood flow during critical operations such as re-entry. A second example is the design of a swept-frequency ultrasound system for the detection of bubbles in the circulatory system and/or soft tissues as an early indication of the onset of decompression sickness during EVA activities. This system exploits the resonant properties of bubbles and can detect both fundamental and second harmonic emissions from the insonified region.

  17. Aerospace management techniques: Commercial and governmental applications

    NASA Technical Reports Server (NTRS)

    Milliken, J. G.; Morrison, E. J.

    1971-01-01

    A guidebook for managers and administrators is presented as a source of useful information on new management methods in business, industry, and government. The major topics discussed include: actual and potential applications of aerospace management techniques to commercial and governmental organizations; aerospace management techniques and their use within the aerospace sector; and the aerospace sector's application of innovative management techniques.

  18. Liquid chromatography and supercritical fluid chromatography as alternative techniques to gas chromatography for the rapid screening of anabolic agents in urine.

    PubMed

    Desfontaine, Vincent; Nováková, Lucie; Ponzetto, Federico; Nicoli, Raul; Saugy, Martial; Veuthey, Jean-Luc; Guillarme, Davy

    2016-06-17

    This work describes the development of two methods involving supported liquid extraction (SLE) sample treatment followed by ultra-high performance liquid chromatography or ultra-high performance supercritical fluid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS and UHPSFC-MS/MS) for the screening of 43 anabolic agents in human urine. After evaluating different stationary phases, a polar-embedded C18 and a diol columns were selected for UHPLC-MS/MS and UHPSFC-MS/MS, respectively. Sample preparation, mobile phases and MS conditions were also finely tuned to achieve highest selectivity, chromatographic resolution and sensitivity. Then, the performance of these two methods was compared to the reference routine procedure for steroid analyses in anti-doping laboratories, which combines liquid-liquid extraction (LLE) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). For this purpose, urine samples spiked with the compounds of interest at five different concentrations were analyzed using the three analytical platforms. The retention and selectivity of the three techniques were very different, ensuring a good complementarity. However, the two new methods displayed numerous advantages. The overall procedure was much faster thanks to high throughput SLE sample treatment using 48-well plates and faster chromatographic analysis. Moreover, the highest sensitivity was attained using UHPLC-MS/MS with 98% of the doping agents detected at the lowest concentration level (0.1ng/mL), against 76% for UHPSFC-MS/MS and only 14% for GC-MS/MS. Finally, the weakest matrix effects were obtained with UHPSFC-MS/MS with 76% of the analytes displaying relative matrix effect between -20 and 20%, while the GC-MS/MS reference method displayed very strong matrix effects (over 100%) for all of the anabolic agents.

  19. Serial displacement chromatofocusing and its applications in multidimensional chromatography and gel electrophoresis: II. Experimental results.

    PubMed

    Shen, Hong; Li, Xiang; Bieberich, Charles; Frey, Douglas D

    2009-02-06

    Part I of this study investigated the theory and basic characteristics of "serial displacement chromatofocusing" (SDC). In Part II of this study, SDC is applied to two prototype applications which have potential uses in proteomics and related areas involving the analysis of complex analyte mixtures. In the first application, SDC was used as a prefractionation method prior to two-dimensional polyacrylamide gel electrophoresis (2D-PAGE) to separate a human prostate cancer cell lysate. It was observed that the resolution achieved in narrow-pI-range 2D-PAGE was improved when using SDC prefractionation, so that SDC may be useful as a low-cost, high-speed, and highly scalable alternative to electrophoretic prefractionation methods for 2D-PAGE. The second application involves the use of SDC as the first dimension, and reversed-phase chromatography as the second dimension, to produce a novel, fully automated, two-dimensional high-performance liquid chromatography technique. The method was shown to have performance advantages over one-dimensional reversed-phase chromatography for peptide separations.

  20. Liquid chromatography/tandem mass spectrometry of unusual phenols from Yucca schidigera bark: comparison with other analytical techniques.

    PubMed

    Montoro, Paola; Piacente, Sonia; Oleszek, Wieslaw; Pizza, Cosimo

    2004-10-01

    Qualitative and quantitative analyses of phenolic compounds are of interest for both medicinal and food plants. In the present work, the phenolic fraction from Yucca schidigera, a plant bearing the GRAS (Generally Recognized as Safe) label approved by the US Food and Drug Administration, was studied. Crude extracts of Y. schidigera bark were investigated by liquid chromatography/UV spectrophotometry with diode-array detection, liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS) and liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS), in order to develop and optimize simple and rapid techniques to determine both stilbenes and yuccaols for the purposes of quality control of collected material. With optimal LC and MS conditions, stilbenes and yuccaols were quantified with all the proposed methods and the results were compared. Sensitivity was evaluated and the results indicated that MS/MS detection in the multiple reaction monitoring mode is easily applicable to this plant and allows the rapid and direct identification and quantification of these peculiar compounds in crude plant extracts.

  1. Separation of mAbs molecular variants by analytical hydrophobic interaction chromatography HPLC: overview and applications.

    PubMed

    Haverick, Mark; Mengisen, Selina; Shameem, Mohammed; Ambrogelly, Alexandre

    2014-01-01

    Hydrophobic interaction chromatography-high performance liquid chromatography (HIC-HPLC) is a powerful analytical method used for the separation of molecular variants of therapeutic proteins. The method has been employed for monitoring various post-translational modifications, including proteolytic fragments and domain misfolding in etanercept (Enbrel®); tryptophan oxidation, aspartic acid isomerization, the formation of cyclic imide, and α amidated carboxy terminus in recombinant therapeutic monoclonal antibodies; and carboxy terminal heterogeneity and serine fucosylation in Fc and Fab fragments. HIC-HPLC is also a powerful analytical technique for the analysis of antibody-drug conjugates. Most current analytical columns, methods, and applications are described, and critical method parameters and suitability for operation in regulated environment are discussed, in this review.

  2. High Performance Thin Layer Chromatography.

    ERIC Educational Resources Information Center

    Costanzo, Samuel J.

    1984-01-01

    Clarifies where in the scheme of modern chromatography high performance thin layer chromatography (TLC) fits and why in some situations it is a viable alternative to gas and high performance liquid chromatography. New TLC plates, sample applications, plate development, and instrumental techniques are considered. (JN)

  3. Drying techniques for the visualisation of agarose-based chromatography media by scanning electron microscopy.

    PubMed

    Nweke, Mauryn C; Turmaine, Mark; McCartney, R Graham; Bracewell, Daniel G

    2017-03-01

    The drying of chromatography resins prior to scanning electron microscopy is critical to image resolution and hence understanding of the bead structure at sub-micron level. Achieving suitable drying conditions is especially important with agarose-based chromatography resins, as over-drying may cause artefact formation, bead damage and alterations to ultrastructural properties; and under-drying does not provide sufficient resolution for visualization under SEM. This paper compares and contrasts the effects of two drying techniques, critical point drying and freeze drying, on the morphology of two agarose based resins (MabSelect™/dw ≈85 µm and Capto™ Adhere/dw ≈75 µm) and provides a complete method for both. The results show that critical point drying provides better drying and subsequently clearer ultrastructural visualization of both resins under SEM. Under this protocol both the polymer fibers (thickness ≈20 nm) and the pore sizes (diameter ≈100 nm) are clearly visible. Freeze drying is shown to cause bead damage to both resins, but to different extents. MabSelect resin encounters extensive bead fragmentation, whilst Capto Adhere resin undergoes partial bead disintegration, corresponding with the greater extent of agarose crosslinking and strength of this resin. While freeze drying appears to be the less favorable option for ultrastructural visualization of chromatography resin, it should be noted that the extent of fracturing caused by the freeze drying process may provide some insight into the mechanical properties of agarose-based chromatography media.

  4. Recent Advance in Liquid Chromatography/Mass Spectrometry Techniques for Environmental Analysis in Japan

    PubMed Central

    Suzuki, Shigeru

    2014-01-01

    The techniques and measurement methods developed in the Environmental Survey and Monitoring of Chemicals by Japan’s Ministry of the Environment, as well as a large amount of knowledge archived in the survey, have led to the advancement of environmental analysis. Recently, technologies such as non-target liquid chromatography/high resolution mass spectrometry and liquid chromatography with micro bore column have further developed the field. Here, the general strategy of a method developed for the liquid chromatography/mass spectrometry (LC/MS) analysis of environmental chemicals with a brief description is presented. Also, a non-target analysis for the identification of environmental pollutants using a provisional fragment database and “MsMsFilter,” an elemental composition elucidation tool, is presented. This analytical method is shown to be highly effective in the identification of a model chemical, the pesticide Bendiocarb. Our improved micro-liquid chromatography injection system showed substantially enhanced sensitivity to perfluoroalkyl substances, with peak areas 32–71 times larger than those observed in conventional LC/MS. PMID:26819891

  5. Thin-Layer and Paper Chromatography.

    ERIC Educational Resources Information Center

    Sherma, Joseph; Fried, Bernard

    1984-01-01

    Reviews literature on chromatography examining: books, reviews, student experiments; chromatographic systems, techniques, apparatus; detecting and identification of separated zones; preparative chromatography and radiochromatography; and applications related to specific materials (such as acids, alcohols, amino acids, antibiotics, enzymes, dyes,…

  6. High-pressure liquid chromatography: A brief introduction and its application in analyzing the degradation of a C-ether (Thio-ether) liquid lubricant

    NASA Technical Reports Server (NTRS)

    1983-01-01

    The general principles of classical liquid chromatography and high pressure liquid chromatography (HPLC) are reviewed, and their advantages and disadvantages are compared. Several chromatographic techniques are reviewed, and the analytical separation of a C-ether liquid lubricant by each technique is illustrated. A practical application of HPLC is then demonstrated by analyzing a degraded C-ether liquid lubricant from full scale, high temperature bearing tests.

  7. Low thermal mass gas chromatography: principles and applications.

    PubMed

    Luong, Jim; Gras, Ronda; Mustacich, Robert; Cortes, Hernan

    2006-01-01

    In gas chromatography (GC), temperature programming is often considered to be the second most important parameter to control, the first being column selectivity. A radically new GC technology to achieve ultrafast temperature programming with an unprecedented cool down time and low power consumption has recently become available. This technology is referred to as low thermal mass GC (LTMGC). Though the technology has its roots in resistive heating, which forms the basis of principle and design concept, the approach taken to achieve ultrafast heating and cool down time by LTMGC represents a significant break-through in GC. Despite some rectifiable shortcomings, LTMGC has proven to be an ideal methodology to deliver near/real time GC data, high precision, and high throughput applications. It is a new approach for modern high-speed GC. This paper documents the fundamental design principles behind LTMGC, performance data, and examples of applications investigated.

  8. Ion beam analysis techniques in interdisciplinary applications

    SciTech Connect

    Respaldiza, Miguel A.; Ager, Francisco J.

    1999-11-16

    The ion beam analysis techniques emerge in the last years as one of the main applications of electrostatic accelerators. A short summary of the most used IBA techniques will be given as well as some examples of applications in interdisciplinary sciences.

  9. Ion Beam Analysis Techniques in Interdisciplinary Applications

    SciTech Connect

    Respaldiza, Miguel A.; Ager, Francisco J.

    1999-12-31

    The ion beam analysis techniques emerge in the last years as one of the main applications of electrostatic accelerators. A short summary of the most used IBA techniques will be given as well as some examples of applications in interdisciplinary sciences.

  10. ELECTRICAL TECHNIQUES FOR ENGINEERING APPLICATIONS.

    USGS Publications Warehouse

    Bisdorf, Robert J.

    1985-01-01

    Surface electrical geophysical methods have been used in such engineering applications as locating and delineating shallow gravel deposits, depth to bedrock, faults, clay zones, and other geological phenomena. Other engineering applications include determining water quality, tracing ground water contaminant plumes and locating dam seepages. Various methods and electrode arrays are employed to solve particular geological problems. The sensitivity of a particular method or electrode array depends upon the physics on which the method is based, the array geometry, the electrical contrast between the target and host materials, and the depth to the target. Each of the available electrical methods has its own particular advantages and applications which the paper discusses.

  11. Application of ultraperformance liquid chromatography/mass spectrometry-based metabonomic techniques to analyze the joint toxic action of long-term low-level exposure to a mixture of organophosphate pesticides on rat urine profile.

    PubMed

    Du, Longfei; Wang, Hong; Xu, Wei; Zeng, Yan; Hou, Yurong; Zhang, Yuqiu; Zhao, Xiujuan; Sun, Changhao

    2013-07-01

    In previously published articles, we evaluated the toxicity of four organophosphate (OP) pesticides (dichlorvos, dimethoate, acephate, and phorate) to rats using metabonomic technology at their corresponding no observed adverse effect level (NOAEL). Results show that a single pesticide elicits no toxic response. This study aimed to determine whether chronic exposure to a mixture of the above four pesticides (at their corresponding NOAEL) can lead to joint toxic action in rats using the same technology. Pesticides were administered daily to rats through drinking water for 24 weeks. The above mixture of the four pesticides showed joint toxic action at the NOAEL of each pesticide. The metabonomic profiles of rats urine were analyzed by ultraperformance liquid chromatography/mass spectrometry. The 16 metabolites statistically significantly changed in all treated groups compared with the control group. Dimethylphosphate and dimethyldithiophosphate exclusively detected in all treated groups can be used as early, sensitive biomarkers for exposure to a mixture of the OP pesticides. Moreover, exposure to the OP pesticides resulted in increased 7-methylguanine, ribothymidine, cholic acid, 4-pyridoxic acid, kynurenine, and indoxyl sulfate levels, as well as decreased hippuric acid, creatinine, uric acid, gentisic acid, C18-dihydrosphingosine, phytosphingosine, suberic acid, and citric acid. The results indicated that a mixture of OP pesticides induced DNA damage and oxidative stress, disturbed the metabolism of lipids, and interfered with the tricarboxylic acid cycle. Ensuring food safety requires not only the toxicology test data of each pesticide for the calculation of the acceptable daily intake but also the joint toxic action.

  12. Applications of CFD and visualization techniques

    NASA Technical Reports Server (NTRS)

    Saunders, James H.; Brown, Susan T.; Crisafulli, Jeffrey J.; Southern, Leslie A.

    1992-01-01

    In this paper, three applications are presented to illustrate current techniques for flow calculation and visualization. The first two applications use a commercial computational fluid dynamics (CFD) code, FLUENT, performed on a Cray Y-MP. The results are animated with the aid of data visualization software, apE. The third application simulates a particulate deposition pattern using techniques inspired by developments in nonlinear dynamical systems. These computations were performed on personal computers.

  13. Evaluation of flash supercritical fluid chromatography and alternate sample loading techniques for pharmaceutical medicinal chemistry purifications.

    PubMed

    Miller, Larry; Mahoney, Max

    2012-08-10

    Flash chromatography is the preferred approach for small molecule purification in pharmaceutical discovery. This paper will discuss the potential for flash supercritical fluid chromatography (SFC) as an alternative technology for these purifications. It was shown that the high sample loadings seen with flash LC could also be achieved using flash SFC. The dry load injection technique greatly increases the amount of sample that can be applied to a flash SFC column while still achieving separation. Flash SFC has much lower solvent usage and higher purification productivities relative to flash LC. Product concentrations post purification were higher for flash SFC vs. flash LC, reducing the time required to isolate dry product. There still exist a number of technical details to be worked out with flash SFC, mainly around the equipment and column/cartridge technology.

  14. Electrochemically-modulated liquid chromatography (EMLC): Column design, retention processes, and applications

    SciTech Connect

    Ting, En -Yi

    1997-10-08

    This work describes the continued development of a new separation technique, electrochemically-modulated liquid chromatography (EMLC), from column design, retention mechanisms to pharmaceutical applications. The introduction section provides a literature review of the technique as well as a brief overview of the research in each of the chapters. This section is followed by four chapters which investigate the issues of EMLC column design, the retention mechanism of monosubstituted aromatic compounds, and the EMLC-based applications to two important classes of pharmaceutical compounds (i.e., corticosteroids and benzodiazepines). These four sections have been removed to process separately for inclusion on the database. The dissertation concludes with a general summary, a prospectus, and a list of references cited in the General Introduction. 32 refs.

  15. Microfluidic liquid chromatography system for proteomic applications and biomarker screening.

    PubMed

    Lazar, Iulia M; Trisiripisal, Phichet; Sarvaiya, Hetal A

    2006-08-01

    A microfluidic liquid chromatography (LC) system for proteomic investigations that integrates all the necessary components for stand-alone operation, i.e., pump, valve, separation column, and electrospray interface, is described in this paper. The overall size of the LC device is small enough to enable the integration of two fully functional separation systems on a 3 in. x 1 in. glass microchip. A multichannel architecture that uses electroosmotic pumping principles provides the necessary functionality for eluent propulsion and sample valving. The flow rates generated within these chips are fully consistent with the requirements of nano-LC platforms that are routinely used in proteomic applications. The microfluidic device was evaluated for the analysis of a protein digest obtained from the MCF7 breast cancer cell line. The cytosolic protein extract was processed according to a shotgun protocol, and after tryptic digestion and prefractionation using strong cation exchange chromatography (SCX), selected sample subfractions were analyzed with conventional and microfluidic LC platforms. Using similar experimental conditions, the performance of the microchip LC was comparable to that obtained with benchtop instrumentation, providing an overlap of 75% in proteins that were identified by more than two unique peptides. The microfluidic LC analysis of a protein-rich SCX fraction enabled the confident identification of 77 proteins by using conventional data filtering parameters, of 39 proteins with p < 0.001, and of 5 proteins that are known to be cancer-specific biomarkers, demonstrating thus the potential applicability of these chips for future high-throughput biomarker screening applications.

  16. Identification of Explosives from Porous Materials: Applications Using Reverse Phase High Performance Liquid Chromatography and Gas Chromatography

    NASA Astrophysics Data System (ADS)

    Miller, C. J.; Elias, G.; Schmitt, N. C.; Rae, C.

    2010-06-01

    High performance liquid chromatography and gas chromatography techniques are well documented and widely used for the detection of trace explosives from organic solvents. These techniques were modified to identify and quantify explosives extracted from various materials taken from people who had recently handled explosives. Documented techniques were modified to specifically detect and quantify trace levels of the military explosives, RDX, TNT, and PETN from denim, colored flannel, vinyl, and canvas extracted in methanol and filtered using no additional sample cleanup of the sample extract prior to analysis. The filtered methanol extracts were injected directly into several different column types and analyzed by high performance liquid chromatography using ultraviolet detection and/or gas chromatography using electron capture detection. This paper describes general screening methods that were used to determine the presence of explosives (RDX, TNT, and PETN) in unknown samples of denim, colored flannel, vinyl and canvas in addition to techniques that have been optimized for quantification of each explosive from the substrate extracts.

  17. Identification of Explosives from Porous Materials: Applications Using Reverse Phase High Performance Liquid Chromatography and Gas Chromatography

    SciTech Connect

    C.J. Miller; G. Elias; N.C. Schmitt; C. Rae

    2010-06-01

    High performance liquid chromatography and gas chromatography techniques are well documented and widely used for the detection of trace explosives from organic solvents. These techniques were modified to specifically identify and quantify explosives extracted from various materials taken from people who had recently handled explosives. Documented techniques were modified to specifically detect and quantify RDX, TNT, and PETN from denim, colored flannel, vinyl, and canvas extracted in methanol using no sample cleanup prior to analysis. The methanol extracts were injected directly into several different column types and analyzed by HPLC-UV and/or GC-ECD. This paper describes general screening methods that were used to determine the presence of explosives in unknown samples and techniques that have been optimized for quantification of each explosive from the substrate extracts.

  18. Metal-organic frameworks in chromatography.

    PubMed

    Yusuf, Kareem; Aqel, Ahmad; ALOthman, Zeid

    2014-06-27

    Metal-organic frameworks (MOFs) emerged approximately two decades ago and are the youngest class of porous materials. Despite their short existence, MOFs are finding applications in a variety of fields because of their outstanding chemical and physical properties. This review article focuses on the applications of MOFs in chromatography, including high-performance liquid chromatography (HPLC), gas chromatography (GC), and other chromatographic techniques. The use of MOFs in chromatography has already had a significant impact; however, the utilisation of MOFs in chromatography is still less common than other applications, and the number of MOF materials explored in chromatography applications is limited.

  19. Urinary 19-norandrosterone purification by immunoaffinity chromatography: application to gas chromatography/combustion/isotope ratio mass spectrometric analysis.

    PubMed

    Desroches, M C; Mathurin, J C; Richard, Y; Delahaut, P; de Ceaurriz, J

    2002-01-01

    The detection of exogenous 19-norandrosterone (19-NA) in urines was investigated by using gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS). 19-NA is, for the first time to our knowledge, isolated from urinary matrix by specific immunoaffinity chromatography (IAC) before analysis. The sample preparation consisted of a preliminary purification of urine by solid-phase extraction after hydrolysis by beta-glucuronidase. Unconjugated 19-NA was thus isolated by IAC and directly analysed by GC/C/IRMS. Optimisation of IAC purification was achieved and the reliability of the technique for anti-doping control is discussed.

  20. Fast centrifugal partition chromatography as a preparative-scale separation technique for citrus flavones

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Fast centrifugal partition chromatography (FCPC) is a preparative-scale separations methodology based on the principles of counter current chromatography. Separations by FCPC are typically achieved with higher recoveries and with lower solvent use compared to conventional column chromatography. HSCP...

  1. Ultrasound elastography: principles, techniques, and clinical applications.

    PubMed

    Dewall, Ryan J

    2013-01-01

    Ultrasound elastography is an emerging set of imaging modalities used to image tissue elasticity and are often referred to as virtual palpation. These techniques have proven effective in detecting and assessing many different pathologies, because tissue mechanical changes often correlate with tissue pathological changes. This article reviews the principles of ultrasound elastography, many of the ultrasound-based techniques, and popular clinical applications. Originally, elastography was a technique that imaged tissue strain by comparing pre- and postcompression ultrasound images. However, new techniques have been developed that use different excitation methods such as external vibration or acoustic radiation force. Some techniques track transient phenomena such as shear waves to quantitatively measure tissue elasticity. Clinical use of elastography is increasing, with applications including lesion detection and classification, fibrosis staging, treatment monitoring, vascular imaging, and musculoskeletal applications.

  2. [THE TECHNIQUE OF HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY FOR SIMULTANEOUS DIAGNOSTIC OF INHERENT HYPERPLASIA OF ADRENAL GLANDS TYPE I AND II].

    PubMed

    Dutov, A A; Nikitin, D A; Lukyanova, Yu L; Shemiakina, N A

    2016-01-01

    The article considers the technique of high-performance liquid chromatography making it possible simultaneously detect cortisol, cortisone and secondary steroids in serum for consequent analysis of common reversed-phase high-performance liquid chromatography with ultraviolet under 240 nm. The liquid-liquid extraction from alkaline medium in diethyl ether The separation using column of 150x4.6 size ODS 3.5 mkm in isocratic mode. The eluent acetonitrile--0.02 M phosphate buffer pH 8.0--isopropanol (40:60:1). The application of proposed technique managed to separate cortisol, cortisone, dexamethasone, corticosterone, 11-desoxicortisol, testosterone, desoxicorticosterone, 17α-gidroxiprogesterone and androstendion in 20 minutes. The simplicity, reproducibility and sufficient selectivity and sensitivity of technique permit implement it in clinical practice for simultaneous diagnostic of inherent hyperplasia of adrenal glands type I and II.

  3. Supercritical Fluid Chromatography--Theoretical Background and Applications on Natural Products.

    PubMed

    Hartmann, Anja; Ganzera, Markus

    2015-11-01

    The use of supercritical fluid chromatography for natural product analysis as well as underlying theoretical mechanisms and instrumental requirements are summarized in this review. A short introduction focusing on the historical development of this interesting separation technique is followed by remarks on the current instrumental design, also describing possible detection modes and useable stationary phases. The overview on relevant applications is grouped based on their basic intention, may it be (semi)preparative or purely analytical. They indicate that supercritical fluid chromatography is still primarily considered for the analysis of nonpolar analytes like carotenoids, fatty acids, or terpenes. The low polarity of supercritical carbon dioxide, which is used with modifiers almost exclusively as a mobile phase today, combined with high efficiency and fast separations might explain the popularity of supercritical fluid chromatography for the analysis of these compounds. Yet, it has been shown that more polar natural products (e.g., xanthones, flavonoids, alkaloids) are separable too, with the same (if not superior) selectivity and reproducibility than established approaches like HPLC or GC.

  4. Applications of Electromigration Techniques: Electromigration Techniques in Detection of Microorganisms

    NASA Astrophysics Data System (ADS)

    Dziubakiewicz, Ewelina; Buszewski, Bogusław

    The detection and identification of microbes is a challenge and an important aspect in many fields of our lives from medicine to bioterrorism defense. However, the analysis of such complex molecules brings a lot of questions mainly about their behavior. Bacteria are biocolloid, whose surface charge originates from the ionization of carboxyl, phosphate, or amino groups and the adsorption of ions from solution. Consequently, the charged cell wall groups determine the spontaneous formation of the electrical double layer. In this chapter application of electromigration techniques for microorganism's identification and separation are described. This approach represents the possibility to apply electromigration techniques in medical diagnosis, detection of food contamination, and sterility testing.

  5. PHARMACEUTICAL AND BIOMEDICAL APPLICATIONS OF AFFINITY CHROMATOGRAPHY: RECENT TRENDS AND DEVELOPMENTS

    PubMed Central

    Hage, David S.; Anguizola, Jeanethe A.; Bi, Cong; Li, Rong; Matsuda, Ryan; Papastavros, Efthimia; Pfaunmiller, Erika; Vargas, John; Zheng, Xiwei

    2012-01-01

    Affinity chromatography is a separation technique that has become increasingly important in work with biological samples and pharmaceutical agents. This method is based on the use of a biologically-related agent as a stationary phase to selectively retain analytes or to study biological interactions. This review discusses the basic principles behind affinity chromatography and examines recent developments that have occurred in the use of this method for biomedical and pharmaceutical analysis. Techniques based on traditional affinity supports are discussed, but an emphasis is placed on methods in which affinity columns are used as part of HPLC systems or in combination with other analytical methods. General formats for affinity chromatography that are considered include step elution schemes, weak affinity chromatography, affinity extraction and affinity depletion. Specific separation techniques that are examined include lectin affinity chromatography, boronate affinity chromatography, immunoaffinity chromatography, and immobilized metal ion affinity chromatography. Approaches for the study of biological interactions by affinity chromatography are also presented, such as the measurement of equilibrium constants, rate constants, or competition and displacement effects. In addition, related developments in the use of immobilized enzyme reactors, molecularly imprinted polymers, dye ligands and aptamers are briefly considered. PMID:22305083

  6. Determination of trace level bromate and perchlorate in drinking water by ion chromatography with an evaporative preconcentration technique.

    PubMed

    Liu, Yongjian; Mou, Shifen; Heberling, Shawn

    2002-05-17

    A simple sample preconcentration technique employing microwave-based evaporation for the determination of trace level bromate and perchlorate in drinking water with ion chromatography is presented. With a hydrophilic anion-exchange column and a sodium hydroxide eluent in linear gradient, bromate and perchlorate can be determined in one injection within 35 min. Prior to ion chromatographic analysis, the drinking water sample was treated with an OnGuard-Ag cartridge to remove the superfluous chloride and concentrated 20-fold using a PTFE beaker in a domestic microwave oven for 15 min. The recoveries of the anions ranged from 94.6% for NO2- to 105.2% for F-. The detection limits for bromate, perchlorate, iodate and chlorate were 0.1, 0.2, 0.1 and 0.2 microg/l, respectively. The developed method is applicable for the quantitation of bromate and perchlorate in drinking water samples.

  7. Artifical intelligence: Concepts, techniques, and applications

    SciTech Connect

    Shira, Y.; Tsujii, F.R.D.

    1985-01-01

    This book examines the fundamental concepts and various techniques involved in real-world applications of artifical intelligence, such as computer representation of problems, searching and inference mechanisms, intelligent languages, and computer representation and utilization of knowledge. It explores applications in theorem-proving, games, robotics, natural language processing, knowledge engineering, and more.

  8. Applying Chromatography.

    ERIC Educational Resources Information Center

    Klein, Jessie W.; Patev, Paul

    1998-01-01

    Presents three experiments to introduce students to different kinds of chromatography: (1) paper chromatography; (2) gel filtration chromatography; and (3) reverse-phase liquid chromatography. Written in the form of a laboratory manual, explanations of each of the techniques, materials needed, procedures, and a glossary are included. (PVD)

  9. Chiral cyclodextrin-modified micellar electrokinetic chromatography and chemometric techniques for green tea samples origin discrimination.

    PubMed

    Pasquini, Benedetta; Orlandini, Serena; Goodarzi, Mohammad; Caprini, Claudia; Gotti, Roberto; Furlanetto, Sandra

    2016-04-01

    Catechins and methylxanthines were determined in 92 green tea (GT) samples originating from Japan and China by using micellar electrokinetic chromatography with the addition of (2-hydroxypropyl)-β-cyclodextrin. GT samples showed high concentrations of (-)-epigallocatechin gallate and caffeine, with (-)-epigallocatechin, (-)-epicatechin gallate and (-)-epicatechin in relevant content and (+)-catechin, (-)-catechin and theobromine in much lower amounts. The amount of all the considered compounds was higher for Chinese GTs, with the exception of (-)-epicatechin gallate. Pattern recognition methods were applied to discriminate GTs according to geographical origin, which is an important factor to determine quality and reputation of a commercial tea product. Data analysis was performed by principal component analysis and hierarchical cluster analysis as exploratory techniques. Linear discriminant analysis and quadratic discriminant analysis were utilized as discrimination techniques, obtaining a very good rate of correct classification and prediction.

  10. Applications of nanomaterials in liquid chromatography: opportunities for separation with high efficiency and selectivity.

    PubMed

    Zhang, Zhengxiang; Wang, Zhiyong; Liao, Yiping; Liu, Huwei

    2006-08-01

    During recent decades, great efforts have been made to improve the chemical stability, selectivity, and separation efficiency of stationary phases in liquid chromatography. Significant progress has been achieved, especially after the introduction of nanomaterials into separation science. This review covers the applications of nanomaterials playing various roles in liquid chromatography. Future possibilities for developing nanomaterial-based stationary phases are also discussed.

  11. Systematic comparison of static and dynamic headspace sampling techniques for gas chromatography.

    PubMed

    Kremser, Andreas; Jochmann, Maik A; Schmidt, Torsten C

    2016-09-01

    Six automated, headspace-based sample preparation techniques were used to extract volatile analytes from water with the goal of establishing a systematic comparison between commonly available instrumental alternatives. To that end, these six techniques were used in conjunction with the same gas chromatography instrument for analysis of a common set of volatile organic carbon (VOC) analytes. The methods were thereby divided into three classes: static sampling (by syringe or loop), static enrichment (SPME and PAL SPME Arrow), and dynamic enrichment (ITEX and trap sampling). For PAL SPME Arrow, different sorption phase materials were also included in the evaluation. To enable an effective comparison, method detection limits (MDLs), relative standard deviations (RSDs), and extraction yields were determined and are discussed for all techniques. While static sampling techniques exhibited sufficient extraction yields (approx. 10-20 %) to be reliably used down to approx. 100 ng L(-1), enrichment techniques displayed extraction yields of up to 80 %, resulting in MDLs down to the picogram per liter range. RSDs for all techniques were below 27 %. The choice on one of the different instrumental modes of operation (aforementioned classes) was thereby the most influential parameter in terms of extraction yields and MDLs. Individual methods inside each class showed smaller deviations, and the least influences were observed when evaluating different sorption phase materials for the individual enrichment techniques. The option of selecting specialized sorption phase materials may, however, be more important when analyzing analytes with different properties such as high polarity or the capability of specific molecular interactions. Graphical Abstract PAL SPME Arrow during the extraction of volatile analytes from the headspace of an aqueous sample.

  12. Post-column labeling techniques in amino acid analysis by liquid chromatography.

    PubMed

    Rigas, Pantelis G

    2013-10-01

    Amino acid analysis (AAA) has always presented an analytical challenge in terms of sample preparation, separation, and detection. Because of the vast number of amino acids, various separation methods have been applied taking into consideration the large differences in their chemical structures, which span from nonpolar to highly polar side chains. Numerous separation methods have been developed in the past 60 years, and impressive achievements have been made in the fields of separation, derivatization, and detection of amino acids (AAs). Among the separation methods, liquid chromatography (LC) prevailed in the AAA field using either pre-column or post-column labeling techniques in order to improve either separation of AAs or selectivity and sensitivity of AAA. Of the two approaches, the post-column technique is a more rugged and reproducible method and provides excellent AAs separation relatively free from interferences. This review considers current separations combined with post-column labeling techniques for AAA, comparison with the pre-column methods, and the strategies used to develop effective post-column methodology. The focus of the article is on LC methods coupled with post-column labeling techniques and studying the reactions to achieve optimum post-column derivatization (PCD) conditions in order to increase sensitivity and selectivity using various types of detectors (UV-Vis, fluorescence, electrochemical etc.) and illustrating the versatility of the PCD methods for practical analysis.

  13. A novel fully automated on-line coupled liquid chromatography-gas chromatography technique used for the determination of organochlorine pesticide residues in tobacco and tobacco products.

    PubMed

    Qi, Dawei; Fei, Ting; Sha, Yunfei; Wang, Leijun; Li, Gang; Wu, Da; Liu, Baizhan

    2014-12-29

    In this study, a novel fully automated on-line coupled liquid chromatography-gas chromatography (LC-GC) technique was reported and applied for the determination of organochlorine pesticide residues (OCPs) in tobacco and tobacco products. Using a switching valve to isolate the capillary pre-column and the analytical column during the solvent evaporation period, the LC solvent can be completely removed and prevented from reaching the GC column and the detector. The established method was used to determinate the OCPs in tobacco samples. By using Florisil SPE column and employing GPC technique, polarity impurities and large molecule impurities were removed. A dynamic range 1-100ng/mL was achieved with detection limits from 1.5 to 3.3μg/kg. The method exhibited good repeatability and recoveries. This technology may provide an alternative way for trace analysis of complex samples.

  14. Multiresidue analysis of neonicotinoids by solid-phase extraction technique using high-performance liquid chromatography.

    PubMed

    Mohan, Chander; Kumar, Yogesh; Madan, Jyotsana; Saxena, Navneet

    2010-06-01

    For routine monitoring of pesticides, a multiresidue analysis through solid-phase extraction technique and using high-performance liquid chromatography (HPLC) in cotton seed cake (CSC) has been developed. Extraction of fortified samples was carried out with aqueous acetone under vacuum. The concentrated extract was loaded onto the solid-phase extraction units, preconditioned with acetonitrile. The extraction units were then washed with hexane and finally eluted with acetonitrile. The pesticide residues were determined using a multiresidue method by reversed-phase HPLC. The average percentage recoveries were found to range between 65.47% and 110% at spiking levels of 10 to 40 mg/kg. The method developed shows a healthy rate of recovery and can successfully be utilized for the extraction and screening of neonicotinoid residues in CSC. The detection limits for imidacloprid, acetamiprid, and thiacloprid using this method were found to be 5, 10, and 20 mg/kg, respectively.

  15. Comparisons of three dry application autoradiographic techniques

    SciTech Connect

    Parson, M.J.; Parker, B.C. )

    1987-06-01

    We compared three common dry application techniques applied for the first time to phytoplankton taking up water-soluble radioisotopically labeled substrates. Following incubation of live phytoplankton communities in oligotrophic, nitrogen-limited Mountain Lake, Virginia, with Carbon-14 labeled methylamine-hydrochloride, an ammomium analog, we concentrated cells on 0.8 um pore size Millipore filters, then preserved filters in liquid nitrogen, and freeze-dried. Differences in the techniques are application of stripping film, preparation of freshly prepared film by dipping loops into liquid emulsion, and dipping cover slips in liquid emulsion. Following dark-incubation and development, autoradiographs were evaluated microscopically for reproducibility, fine resolution of silver grains, background scatter, and eaes of technique.

  16. A novel antibody immobilization and its application in immunoaffinity chromatography.

    PubMed

    Zhang, Shuoyao; Wang, Junqing; Li, Dawei; Huang, Juan; Yang, Hong; Deng, Anping

    2010-07-15

    A novel antibody immobilization and its application in immunoaffinity chromatography (IAC) were presented. Using acrylamide (AM) as monomer, ethylene glycoldimethacrylate (EGDMA) as cross-linker and bulk polymerization as synthetic method, we prepared a polymer in which the Cu(II) was embedded. The Cu(II)-embedded polymer was tested for its binding with protein. It was found that Cu(II)-embedded polymer displayed a strong binding with bovine serum albumin (BSA). At 80% of methanol, no BSA was released from Cu(II)-embedded polymer. The Cu(II)-embedded polymer was then used as a novel solid support for antibody immobilization. IAC column was prepared by immobilizing polyclonal antibody (pAb) against clenbuterol (CL) on Cu(II)-embedded polymer and packing the Cu(II)-embedded polymer-pAb into a common solid phase extraction (SPE) cartridge. Under optimal extraction conditions, the IAC column was characterized in terms of maximum binding capacity for target analyte, extraction efficiency and reusability. It was revealed that, for IAC column packed with 0.1 g of solid support immobilized with antibody, the maximum capacity for CL was 616 ng; the extraction recoveries of the column for CL from three spiked food samples were 84.4-95.2% with relative standard deviation (RSD) of 9.3-15.5%; after more than 30 times repeated usage, there was not significant loss of specific recognition. The results demonstrated the feasibility of the prepared IAC column for CL extraction. The proposed antibody immobilization method exhibiting the properties of simplicity, low cost, strong binding for target analyte, no leaching of antibody, etc., would be a very useful tool applied in the field of IAC.

  17. [Progress of the hydrokinetic chromatography and its application in the characterization of particulate drug delivery systems].

    PubMed

    Liu, Wei; Li, Hai-Yan; Guo, Zhen; Zhang, Ji-Wen; Sun, Li-Xin

    2011-06-01

    In the present paper, the basic principles, the device and the analytical method of the hydrodynamic chromatography (HDC) were summarized, which is most widely used in hydrokinetic chromatography. The application of the hydrodynamic chromatography in the determination of the particle size and size distribution of the particulate drug delivery system was also reviewed. The method can determine the particle size of nano- and micron-scale particulate drug delivery systems rapidly. And this method also has the advantages of economic, convenient and no damage to the samples. In summary, there will be a good prospect for the application of HDC in the determination of particle size distribution features of particulate drug delivery systems.

  18. Application of Pre-Column Labeling Liquid Chromatography for Canine Plasma-Free Amino Acid Analysis

    PubMed Central

    Azuma, Kazuo; Hirao, Yoshiko; Hayakawa, Yoshihiro; Murahata, Yusuke; Osaki, Tomohiro; Tsuka, Takeshi; Imagawa, Tomohiro; Okamoto, Yoshiharu; Ito, Norihiko

    2016-01-01

    Plasma-free amino acid (PFAA) levels are a useful metric for diagnosing cancer and providing a prognosis. However, the use of analysis of PFAA levels has been limited in the veterinary medicine field. We addressed the application of liquid chromatography (LC) using a pre-column labeling technique for analysis of canine PFAA levels. This method significantly shortened the analysis time relative to conventional methods. No diurnal fluctuations were detected at 9:00 AM in most PFAA levels, and food intake increased the levels of some PFAAs, including valine, leucine, tyrosine, phenylalanine, and proline. These results indicate that LC with pre-column labeling is useful for measuring canine PFAA levels, for which time of day and interval after food intake must be taken into consideration. PMID:26771650

  19. Applications of electrochemically-modulated liquid chromatography (EMLC): Separations of aromatic amino acids and polycyclic aromatic hydrocarbons

    SciTech Connect

    Deng, Li

    1998-03-27

    The research in this thesis explores the separation capabilities of a new technique termed electrochemically-modulated liquid chromatography (EMLC). The thesis begins with a general introduction section which provides a literature review of this technique as well as a brief background discussion of the two research projects in each of the next two chapters. The two papers which follow investigate the application of EMLC to the separation of a mixture of aromatic amino acids and of a mixture of polycyclic aromatic hydrocarbons (PAHs). The last section presents general conclusions and summarizes the thesis. References are compiled in the reference section of each chapter. The two papers have been removed for separate processing.

  20. Current medical research with the application of coupled techniques with mass spectrometry

    PubMed Central

    Kałużna-Czaplińska, Joanna

    2011-01-01

    Summary The most effective methods of analysis of organic compounds in biological fluids are coupled chromatographic techniques. Capillary gas chromatography/mass spectrometry (GC-MS) allows the most efficient separation, identification and quantification of volatile metabolites in biological fluids. Liquid chromatography-mass spectrometry (LC-MS) is especially suitable for the analysis of non-volatile and/or thermally unstable compounds. A major drawback of liquid chromatography-mass spectrometry is that no standard spectral libraries such as NIST and Wiley for GC-MS are available to facilitate the identification of unknown compounds. Moreover, the identification of potential new compounds, especially new biomarkers in LC-MS, is much more challenging than in GC-MS. Capillary electrophoresis coupled with mass spectrometry (CE-MS) has been widely used to characterize metabolomes. Capillary electrophoresis is a powerful technique for the separation of charged metabolites, offering high analyte resolution. The advantages of CE-MS are applicability for hydrophilic metabolites, robust separation efficiency and short duration of analysis. This review provides an overview of current chromatographic methods – gas chromatography – mass spectrometry, liquid chromatography – mass spectrometry and capillary electrophoresis-mass spectrometry – and their applications in current medical research. The focus is on the description of metabonomics research, strategies for biomarkers identification, medical diagnoses of diseases and research of drugs. PMID:21525822

  1. Systematic generation of buffer systems for pH gradient ion exchange chromatography and their application.

    PubMed

    Kröner, Frieder; Hubbuch, Jürgen

    2013-04-12

    pH gradient protein separations are widely used techniques in the field of protein analytics, of which isoelectric focusing is the most well known application. The chromatographic variant, based on the formation of pH gradients in ion exchange columns is only rarely applied due to the difficulties to form controllable, linear pH gradients over a broad pH range. This work describes a method for the systematic generation of buffer compositions with linear titration curves, resulting in well controllable pH gradients. To generate buffer compositions with linear titration curves an in silico method was successfully developed. With this tool, buffer compositions for pH gradient ion exchange chromatography with pH ranges spanning up to 7.5 pH units were established and successfully validated. Subsequently, the buffer systems were used to characterize the elution behavior of 22 different model proteins in cation and anion exchange pH gradient chromatography. The results of both chromatographic modes as well as isoelectric focusing were compared to describe differences in between the methods.

  2. Microextraction techniques coupled to liquid chromatography with mass spectrometry for the determination of organic micropollutants in environmental water samples.

    PubMed

    Padrón, Ma Esther Torres; Afonso-Olivares, Cristina; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan

    2014-07-16

    Until recently, sample preparation was carried out using traditional techniques, such as liquid-liquid extraction (LLE), that use large volumes of organic solvents. Solid-phase extraction (SPE) uses much less solvent than LLE, although the volume can still be significant. These preparation methods are expensive, time-consuming and environmentally unfriendly. Recently, a great effort has been made to develop new analytical methodologies able to perform direct analyses using miniaturised equipment, thereby achieving high enrichment factors, minimising solvent consumption and reducing waste. These microextraction techniques improve the performance during sample preparation, particularly in complex water environmental samples, such as wastewaters, surface and ground waters, tap waters, sea and river waters. Liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS) and time-of-flight mass spectrometric (TOF/MS) techniques can be used when analysing a broad range of organic micropollutants. Before separating and detecting these compounds in environmental samples, the target analytes must be extracted and pre-concentrated to make them detectable. In this work, we review the most recent applications of microextraction preparation techniques in different water environmental matrices to determine organic micropollutants: solid-phase microextraction SPME, in-tube solid-phase microextraction (IT-SPME), stir bar sorptive extraction (SBSE) and liquid-phase microextraction (LPME). Several groups of compounds are considered organic micropollutants because these are being released continuously into the environment. Many of these compounds are considered emerging contaminants. These analytes are generally compounds that are not covered by the existing regulations and are now detected more frequently in different environmental compartments. Pharmaceuticals, surfactants, personal care products and other chemicals are considered micropollutants. These compounds must be

  3. Visual detection technique for efficient screening and isolation of Salmonella based on a novel enrichment assay using chromatography membrane.

    PubMed

    Tang, F; Xiong, Y; Zhang, H; Wu, K; Xiang, Y; Shao, J-B; Ai, H-W; Xiang, Y-P; Zheng, X-L; Lv, J-R; Sun, H; Bao, L-S; Zhang, Z; Hu, H-B; Zhang, J-Y; Chen, L; Lu, J; Liu, W-Y; Mei, H; Ma, Y; Xu, C-F; Fang, A-Y; Gu, M; Xu, C-Y; Chen, Y; Chen, Z; Sun, Z-Y

    2016-03-01

    To detect Salmonella more efficiently and isolate strains more easily, a novel and simple detection method that uses an enrichment assay and two chromogenic reactions on a chromatography membrane was developed. Grade 3 chromatography paper is used as functionalized solid phase support (SPS), which contains specially optimized medium. One reaction for screening is based on the sulfate-reducing capacity of Salmonella. Hydrogen sulfide (H2S) generated by Salmonella reacts with ammonium ferric citrate to produce black colored ferrous sulfide. Another reaction is based on Salmonella C8 esterase that is unique for Enterobacteriaceae except Serratia and interacts with 4-methylumbelliferyl caprylate (MUCAP) to produce fluorescent umbelliferone, which is visible under ultraviolet light. A very low detection limit (10(1) CFU ml(-1)) for Salmonella was achieved on the background of 10(5) CFU ml(-1) Escherichia coli. More importantly, testing with more than 1,000 anal samples indicated that our method has a high positive detection rate and is relatively low cost, compared with the traditional culture-based method. It took only 1 day for the preliminary screening and 2 days to efficiently isolate the Salmonella cells, indicating that the new assay is specific, rapid, and simple for Salmonella detection. In contrast to the traditional culture-based method, this method can be easily used to screen and isolate targeted strains with the naked eye. The results of quantitative and comparative experiments showed that the visual detection technique is an efficient alternative method for the screening of Salmonella spp. in many applications of large-sized samples related to public health surveillance.

  4. Microfluidic desalination techniques and their potential applications.

    PubMed

    Roelofs, S H; van den Berg, A; Odijk, M

    2015-09-07

    In this review we discuss recent developments in the emerging research field of miniaturized desalination. Traditionally desalination is performed to convert salt water into potable water and research is focused on improving performance of large-scale desalination plants. Microfluidic desalination offers several new opportunities in comparison to macro-scale desalination, such as providing a platform to increase fundamental knowledge of ion transport on the nano- and microfluidic scale and new microfluidic sample preparation methods. This approach has also lead to the development of new desalination techniques, based on micro/nanofluidic ion-transport phenomena, which are potential candidates for up-scaling to (portable) drinking water devices. This review assesses microfluidic desalination techniques on their applications and is meant to contribute to further implementation of microfluidic desalination techniques in the lab-on-chip community.

  5. Advanced flow MRI: emerging techniques and applications.

    PubMed

    Markl, M; Schnell, S; Wu, C; Bollache, E; Jarvis, K; Barker, A J; Robinson, J D; Rigsby, C K

    2016-08-01

    Magnetic resonance imaging (MRI) techniques provide non-invasive and non-ionising methods for the highly accurate anatomical depiction of the heart and vessels throughout the cardiac cycle. In addition, the intrinsic sensitivity of MRI to motion offers the unique ability to acquire spatially registered blood flow simultaneously with the morphological data, within a single measurement. In clinical routine, flow MRI is typically accomplished using methods that resolve two spatial dimensions in individual planes and encode the time-resolved velocity in one principal direction, typically oriented perpendicular to the two-dimensional (2D) section. This review describes recently developed advanced MRI flow techniques, which allow for more comprehensive evaluation of blood flow characteristics, such as real-time flow imaging, 2D multiple-venc phase contrast MRI, four-dimensional (4D) flow MRI, quantification of complex haemodynamic properties, and highly accelerated flow imaging. Emerging techniques and novel applications are explored. In addition, applications of these new techniques for the improved evaluation of cardiovascular (aorta, pulmonary arteries, congenital heart disease, atrial fibrillation, coronary arteries) as well as cerebrovascular disease (intra-cranial arteries and veins) are presented.

  6. An application of gas chromatography to planetary atmospheres

    NASA Technical Reports Server (NTRS)

    Oyama, V.

    1974-01-01

    A gas chromatography developed for the Viking experiment is described. The instrument is designed to measure gases in planetary atmospheres and head space in a chamber. It is hoped that the chromatograph will also measure any biological activity present in these environments.

  7. Nonuniform sampling techniques for antenna applications

    NASA Technical Reports Server (NTRS)

    Rahmat-Samii, Yahya; Cheung, Rudolf Lap-Tung

    1987-01-01

    A two-dimensional sampling technique, which can employ irregularly spaced samples (amplitude and phase) in order to generate the complete far-field patterns is presented. The technique implements a matrix inversion algorithm, which depends only on the nonuniform sampled data point locations and with no dependence on the actual field values at these points. A powerful simulation algorithm is presented to allow a real-life simulation of many reflector/feed configurations and to determine the usefulness of the nonuniform sampling technique for the copolar and cross-polar patterns. Additionally, an overlapped window concept and a generalized error simulation model are discussed to identify the stability of the technique for recovering the field data among the nonuniform sampled data. Numerical results are tailored for the pattern reconstruction of a 20-m offset reflector antenna operating at L-band. This reflector is planned to be used in a proposed measurement concept of large antenna aboard the Space Shuttle, whereby it would be almost impractical to accurately control the movement of the Shuttle with respect to the RF source in prescribed directions in order to generate uniform sampled points. Also, application of the nonuniform sampling technique to patterns obtained using near-field measured data is demonstrated. Finally, results of an actual far-field measurement are presented for the construction of patterns of a reflector antenna from a set of nonuniformly distributed measured amplitude and phase data.

  8. On-line sample preconcentration and separation technique based on transient trapping in microchip micellar electrokinetic chromatography.

    PubMed

    Sueyoshi, Kenji; Kitagawa, Fumihiko; Otsuka, Koji

    2008-02-15

    This paper describes a novel on-line sample preconcentration and separation technique named transient trapping (tr-trapping), which improves the efficiencies of separation and concentration by using a partially injected short micellar plug in microchip electrophoresis. Although a longer separation length often provides a better resolution of complexed or closely migrating analytes, our proposed theoretical model indicated that a trap-and-release mechanism enables a short micellar zone, which was partially injected into the separation channel, to work as an effective concentration and separation field. Application of the tr-trapping technique to microchip micellar electrokinetic chromatography (MCMEKC) was performed on a newly fabricated 5-way-cross microchip by using sodium dodecyl sulfate and rhodamine dyes as test micelle and analytes, respectively. When the injection times of micelle (t(inj),M) and sample solution (t(inj),S) were 1.0 and 2.0 s, respectively, both the preconcentration and separation of the dyes were completely finished within only 3.0 s. At t(inj),S of 8.0 s, a 393-fold improvement of the detectability was achieved in comparison with conventional MCMEKC. The resolution obtained with tr-trapping-MCMEKC was also better than that with conventional MCMEKC in spite of the 160-fold shorter length of the injected micellar zone at t(inj),M of 1.0 s. These results clearly demonstrated that the tr-trapping technique in MCMEKC provides a rapid, high-resolution and detectability analysis even in the short separation channel on the microchips.

  9. The contribution of gas chromatography to the resynthesis of the post-Byzantine artist's technique.

    PubMed

    Kouloumpi, Eleni; Lawson, Graham; Pavlidis, Vassilios

    2007-02-01

    Gas chromatographic analysis of ethyl chloroformate derivatives of samples taken from the paint layers of post-Byzantine panel paintings permitted the successful characterisation of the different binding media used in them. This paper describes an analytical study of various post-Byzantine binding media such as egg yolk and egg/oil emulsion, using gas chromatography. The characterisation of these icons' binding media is an important task, as it contributes to our understanding of and the reconstruction of the post-Byzantine artists' palette. It also enables us to investigate the validity of our assumptions about the influences of Venetian style on Greek icon painting techniques from the sixteenth to the early nineteenth century, which up to now have been based on information in artists' handbooks. The methodology involves two experimental steps: (1) hydrolysis of the proteins and triglycerides in the binding media to obtain free amino acids and fatty acids, and (2) the formation of ethyl chloroformate derivatives via derivatization with ethyl chloroformate (ECF). This methodology is of considerable interest, since it permits the identifcation of the nature of the proteinaceous binders used in these works through the simultaneous derivatization and determination of amino acids and fatty acids. Advantages of this methodology include the small quantity of sample required and the minimum preparation time involved. The proteinaceous media can be determined based on the ratios of seven stable amino acids, while the type of emulsions and drying oils used can be determined from the fatty acid ratio.

  10. Neuere Chromatographie

    NASA Astrophysics Data System (ADS)

    Hostettmann, K.

    1983-04-01

    Besides high-performance liquid chromatography (HPLC) which is now a well-established and currently used technique, several emerging methods for the isolation and separation of natural products are receiving considerable attention. Centrifugal thin-layer chromatography is a very rapid technique, but limited in resolution. Of special interest are the recently developed support-free liquid-liquid chromatography methods such as droplet counter-current chromatography (DCCC) and rotation locular counter-current chromatography (RLCC). This latter method was applied to the separation of the enantiomers of (±)-norephedrine.

  11. Principles, Techniques, and Applications of Tissue Microfluidics

    NASA Technical Reports Server (NTRS)

    Wade, Lawrence A.; Kartalov, Emil P.; Shibata, Darryl; Taylor, Clive

    2011-01-01

    The principle of tissue microfluidics and its resultant techniques has been applied to cell analysis. Building microfluidics to suit a particular tissue sample would allow the rapid, reliable, inexpensive, highly parallelized, selective extraction of chosen regions of tissue for purposes of further biochemical analysis. Furthermore, the applicability of the techniques ranges beyond the described pathology application. For example, they would also allow the posing and successful answering of new sets of questions in many areas of fundamental research. The proposed integration of microfluidic techniques and tissue slice samples is called "tissue microfluidics" because it molds the microfluidic architectures in accordance with each particular structure of each specific tissue sample. Thus, microfluidics can be built around the tissues, following the tissue structure, or alternatively, the microfluidics can be adapted to the specific geometry of particular tissues. By contrast, the traditional approach is that microfluidic devices are structured in accordance with engineering considerations, while the biological components in applied devices are forced to comply with these engineering presets.

  12. Magnetic force control technique in industrial application

    NASA Astrophysics Data System (ADS)

    Nishijima, S.

    2010-11-01

    Techniques of the magnetic force control have been examined for industrial application. The problems and the technique are different in dispersion medium of gas and that of liquid. In addition, the method is different depending on the magnetic characteristic of the target objects. In case of the liquid, the dispersion medium having different viscosity was examined. The separation speed is decided with the magnitude of the magnetic force because a drag force increases with the viscosity. When the water is the dispersion medium, magnetic seeding is possible and hence the nonmagnetic materials can be separated and even the dissolved material could be separated. The separation technique has been used for purifying the waste water form paper mill or wash water of drum. On the other hand when the water is not dispersion medium, mainly the ferromagnetism particle becomes the target object because the magnetic seeding becomes difficult. The iron fragments have been separated from the slurry of slicing machine of solar battery. It has been clarified high gradient magnetic separation (HGMS) can be applied for the viscous fluid of which viscosity was as high as 10 Pa s. When the dispersion medium is gaseous material, the air is important. The drag force from air depends greatly on Reynolds number. When speed of the air is small, the Reynolds number is small, and the drag force is calculated by the Stokes' law of resistance. The study with gaseous dispersion medium is not carried out much. The magnetic separation will discuss the possibility of the industrial application of this technique.

  13. High energy heavy ions: techniques and applications

    SciTech Connect

    Alonso, J.R.

    1985-04-01

    Pioneering work at the Bevalac has given significant insight into the field of relativistic heavy ions, both in the development of techniques for acceleration and delivery of these beams as well as in many novel areas of applications. This paper will outline our experiences at the Bevalac; ion sources, low velocity acceleration, matching to the synchrotron booster, and beam delivery. Applications discussed will include the observation of new effects in central nuclear collisions, production of beams of exotic short-lived (down to 1 ..mu..sec) isotopes through peripheral nuclear collisions, atomic physics with hydrogen-like uranium ions, effects of heavy ''cosmic rays'' on satellite equipment, and an ongoing cancer radiotherapy program with heavy ions. 39 refs., 6 figs., 1 tab.

  14. Affinity monolith chromatography: A review of principles and recent analytical applications

    PubMed Central

    Pfaunmiller, Erika L.; Paulemond, Marie Laura; Dupper, Courtney M.; Hage, David S.

    2012-01-01

    Affinity monolith chromatography (AMC) is a type of liquid chromatography that uses a monolithic support and a biologically-related binding agent as a stationary phase. AMC is a powerful method for the selective separation, analysis or studies of specific target compounds in a sample. This review discusses the basic principles of AMC and recent developments or applications of this method, with particular emphasis being given to work that has appeared in the last five years. Various materials that have been used to prepare columns for AMC are examined, including organic monoliths, silica monoliths, agarose monoliths and cryogels. These supports have been used in AMC for formats that have ranged from traditional columns to disks, microcolumns and capillaries. Many binding agents have also been employed in AMC, such as antibodies, enzymes, proteins, lectins, immobilized metal-ions and dyes. Some applications that have been reported with these binding agents in AMC are bioaffinity chromatography, immunoaffinity chromatography or immunoextraction, immobilized metal-ion affinity chromatography, dye-ligand affinity chromatography, chiral separations and biointeraction studies. Examples are presented from fields that include analytical chemistry, pharmaceutical analysis, clinical testing and biotechnology. Current trends and possible future directions in AMC are also discussed. PMID:23187827

  15. Electrochemically modulated liquid chromatography: Theoretical investigations and applications from the perspectives of chromatography and interfacial electrochemistry

    SciTech Connect

    Keller, David W.

    2005-01-01

    Electrochemically modulated liquid chromatography (EMLC) employs a conductive material as both a stationary phase for chromatographic separations and as a working electrode for performing electrochemistry experiments. This dual functionality gives EMLC the capacity to manipulate chromatographic separations by changing the potential applied (Eapp) to the stationary phase with respect to an external reference. The ability to monitor retention as a function of Eapp provides a means to chromatographically monitor electrosorption processes at solid-liquid interfaces. In this dissertation, the retention mechanism for EMLC is examined from the perspective of electrical double layer theory and interfacial thermodynamics. From the chromatographic data, it is possible to determine the interfacial excess (Λ) of a solute and changes in interfacial tension (dγ) as a function of both Eapp and the supporting electrolyte concentration. Taken together, these two experimentally manipulated parameters can be examined within the context of the Gibbs adsorption equation to delineate the contribution of a variety of interfacial properties, including the charge of solute on the stationary phase and the potential of zero charge (PZC), to the mechanism behind EMLC-based retention. The chromatographic probing of interfacial phenomena is complemented by electroanalytical experiments that exploit the ability to monitor the electronic current flowing through an EMLC column. Cyclic voltammetry and chronoamperometry of an EMLC column are used to determine the electronic performance characteristics of an EMLC column. An electrochemical flow injection analysis of a column is provided in which the current required to maintain a constant Eapp is monitored and provides a way to examine the influence that acetonitrile and supporting electrolyte composition, flow rate, column backpressure, and ionic strength have on the structure of electrified interfaces.

  16. The Binding of Biotin to Sepharose-Avidin Column: Demonstration of the Affinity Chromatography Technique

    ERIC Educational Resources Information Center

    Landman, A. D.; Landman, N. N.

    1976-01-01

    Describes a biochemistry experiment that illustrates the methodology of affinity chromatography by attaching avidin, a glycoprotein in egg white, to a Sepharose matrix in order to bind biotin-containing proteins. (MLH)

  17. Principles, Techniques, and Applications of Tissue Microfluidics

    NASA Technical Reports Server (NTRS)

    Wade, Lawrence A.; Kartalov, Emil P.; Shibata, Darryl; Taylor, Clive

    2011-01-01

    The principle of tissue microfluidics and its resultant techniques has been applied to cell analysis. Building microfluidics to suit a particular tissue sample would allow the rapid, reliable, inexpensive, highly parallelized, selective extraction of chosen regions of tissue for purposes of further biochemical analysis. Furthermore, the applicability of the techniques ranges beyond the described pathology application. For example, they would also allow the posing and successful answering of new sets of questions in many areas of fundamental research. The proposed integration of microfluidic techniques and tissue slice samples is called tissue microfluidics because it molds the microfluidic architectures in accordance with each particular structure of each specific tissue sample. Thus, microfluidics can be built around the tissues, following the tissue structure, or alternatively, the microfluidics can be adapted to the specific geometry of particular tissues. By contrast, the traditional approach is that microfluidic devices are structured in accordance with engineering considerations, while the biological components in applied devices are forced to comply with these engineering presets. The proposed principles represent a paradigm shift in microfluidic technology in three important ways: Microfluidic devices are to be directly integrated with, onto, or around tissue samples, in contrast to the conventional method of off-chip sample extraction followed by sample insertion in microfluidic devices. Architectural and operational principles of microfluidic devices are to be subordinated to suit specific tissue structure and needs, in contrast to the conventional method of building devices according to fluidic function alone and without regard to tissue structure. Sample acquisition from tissue is to be performed on-chip and is to be integrated with the diagnostic measurement within the same device, in contrast to the conventional method of off-chip sample prep and

  18. [Determination of acetanilide herbicide residues in tea by gas chromatography-mass spectrometry with two different ionization techniques].

    PubMed

    Shen, Weijian; Xu, Jinzhong; Yang, Wenquan; Shen, Chongyu; Zhao, Zengyun; Ding, Tao; Wu, Bin

    2007-09-01

    An analytical method of solid phase extraction-gas chromatography-mass spectrometry with two different ionization techniques was established for simultaneous determination of 12 acetanilide herbicide residues in tea-leaves. Herbicides were extracted from tea-leaf samples with ethyl acetate. The extract was cleaned-up on an active carbon SPE column connected to a Florisil SPE column. Analytical screening was determined by the technique of gas chromatography (GC)-mass spectrometry (MS) in the selected ion monitoring (SIM) mode with either electron impact ionization (EI) or negative chemical ionization (NCI). It is reliable and stable that the recoveries of all herbicides were in the range from 50% to 110% at three spiked levels, 10 microg/kg, 20 microg/kg and 40 microg/kg, and the relative standard deviations (RSDs) were no more than 10.9%. The two different ionization techniques are complementary as more ion fragmentation information can be obtained from the EI mode while more molecular ion information from the NCI mode. By comparison of the two techniques, the selectivity of NCI-SIM was much better than that of EI-SIM method. The sensitivities of the both techniques were high, the limit of quantitative (LOQ) for each herbicide was no more than 2.0 microg/kg, and the limit of detection (LOD) with NCI-SIM technique was much lower than that of EI-SIM when analyzing herbicides with several halogen atoms in the molecule.

  19. Application of Inverse Liquid Chromatography for Surface Characterization of Biomaterials.

    PubMed

    Adamska, Katarzyna; Kadlec, Karol; Voelkel, Adam

    In the present study, a novel approach for surface characterization of ceramic biomaterials is proposed. Two ceramic biomaterials-hydroxyapatite and β-tricalcium phosphate-were examined by means of inverse liquid chromatography. The Abraham LFER model was applied for physicochemical characteristics of the surface. Different compounds, characterized by different polarity and different donor-acceptor properties of functional group, were used as test solutes. The chromatographic experiments were carried out with two compositions of the mobile phase: pure acetonitrile (MeCN) and the mixture of acetonitrile and water in 80:20 ratio (MeCN/H2O). Thus, the influence of mobile phase on sorption properties of hydroxyapatite and tricalcium phosphate surface was also discussed.

  20. Centrifugal precipitation chromatography, a powerful technique for the isolation of active enzymes from tea leaves (Camellia sinensis).

    PubMed

    Baldermann, Susanne; Fleischmann, Peter; Bolten, Mareike; Watanabe, Naoharu; Winterhalter, Peter; Ito, Yoichiro

    2009-05-08

    Centrifugal precipitation chromatography was developed approximately 10 years ago. In contrast to other counter-current chromatographic techniques, the centrifugal precipitation chromatography system is operated with two mutually miscible solutions separated by a cut-off membrane. Centrifugal precipitation chromatography was firstly introduced for the separation of proteins using an ammonium sulfate gradient. In this study we describe a novel approach using solvent-based protein precipitation for the isolation of active plant enzymes from tea leaves (Camellia sinensis) by centrifugal precipitation chromatography. We developed a gradient based on acetone and Tris-buffer, because the biological activity of carotenases in tea leaves cannot be preserved in the presence of ammonium sulfate. Parameters such as the critical solvent concentration, flow rate, buffer concentration, and sample load were determined and/or optimized. Subsequently, the newly developed separation protocol was successfully used for the isolation of active carotenoid cleavage enzymes from tea leaves. The isolated enzymes showed high enzymatic activities and purities and could be directly used for enzymatic assays and structure elucidation.

  1. Flight Acoustics Measurement Techniques and Applications

    NASA Technical Reports Server (NTRS)

    Preisser, J. S.; Marcolini, M. A.

    1998-01-01

    Careful consideration must be given to data acquisition and analysis techniques in the design of experiments for the measurement of noise generated by flight vehicles. Although noise measurement locations and data reduction procedures are specified for aircraft certification by FAA and ICAO directives, for example, there are virtually no established procedures for aircraft noise measurement for other purposes. To optimize the quality and quantity of information obtained in a flight acoustics experiment, microphone layout, data acquisition, and analysis must be tailored to the specific test objective. This paper will review flight acoustics technology at NASA Langley Research Center developed over the past decade. In particular, the paper will focus on flight experiments performed for three diverse objectives: (1) research applications, such as noise prediction code validation, (2) noise impact modeling, and (3) noise abatement flight procedures. To best achieve these diverse objectives, different deployments of microphone systems on the ground are required, and different data analysis techniques are needed. In all cases, accurate positioning of the aircraft synchronized in time with the data recording is necessary. However, there are some restrictions on flight operations unique to each case for the methods to properly work.

  2. Recent Advances in Techniques for Starch Esters and the Applications: A Review

    PubMed Central

    Hong, Jing; Zeng, Xin-An; Brennan, Charles S.; Brennan, Margaret; Han, Zhong

    2016-01-01

    Esterification is one of the most important methods to alter the structure of starch granules and improve its applications. Conventionally, starch esters are prepared by conventional or dual modification techniques, which have the disadvantages of being expensive, have regent overdoses, and are time-consuming. In addition, the degree of substitution (DS) is often considered as the primary factor in view of its contribution to estimate substituted groups of starch esters. In order to improve the detection accuracy and production efficiency, different detection techniques, including titration, nuclear magnetic resonance (NMR), Fourier transform infrared spectroscopy (FT-IR), thermal gravimetric analysis/infrared spectroscopy (TGA/IR) and headspace gas chromatography (HS-GC), have been developed for DS. This paper gives a comprehensive overview on the recent advances in DS analysis and starch esterification techniques. Additionally, the advantages, limitations, some perspectives on future trends of these techniques and the applications of their derivatives in the food industry are also presented. PMID:28231145

  3. Recent Advances in Techniques for Starch Esters and the Applications: A Review.

    PubMed

    Hong, Jing; Zeng, Xin-An; Brennan, Charles S; Brennan, Margaret; Han, Zhong

    2016-07-09

    Esterification is one of the most important methods to alter the structure of starch granules and improve its applications. Conventionally, starch esters are prepared by conventional or dual modification techniques, which have the disadvantages of being expensive, have regent overdoses, and are time-consuming. In addition, the degree of substitution (DS) is often considered as the primary factor in view of its contribution to estimate substituted groups of starch esters. In order to improve the detection accuracy and production efficiency, different detection techniques, including titration, nuclear magnetic resonance (NMR), Fourier transform infrared spectroscopy (FT-IR), thermal gravimetric analysis/infrared spectroscopy (TGA/IR) and headspace gas chromatography (HS-GC), have been developed for DS. This paper gives a comprehensive overview on the recent advances in DS analysis and starch esterification techniques. Additionally, the advantages, limitations, some perspectives on future trends of these techniques and the applications of their derivatives in the food industry are also presented.

  4. A Gas Chromatography Experiment for Proving the Application of Quantum Symmetry Restrictions in Homonuclear Diatomic Molecules.

    ERIC Educational Resources Information Center

    Dosiere, M.

    1985-01-01

    Background information, procedures used, and typical results obtained are provided for an experiment in which gas chromatography is used to prove the application of quantum symmetry restrictions in homonuclear diatomic molecules. Comparisons between experimental results and theoretical computed values show good agreement, within one to two…

  5. Review of recent developments and applications in low-pressure (vacuum outlet) gas chromatography

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The concept of low pressure (LP) vacuum outlet gas chromatography (GC) was introduced more than 50 years ago, but it was not until the 2000s that its theoretical applicability to fast analysis of GC-amenable chemicals was realized. In practice, LPGC is implemented by placing the outlet of a short, ...

  6. Ion-exchange chromatography: basic principles and application to the partial purification of soluble mammalian prolyl oligopeptidase.

    PubMed

    Cummins, Philip M; Dowling, Oonagh; O'Connor, Brendan F

    2011-01-01

    Ion-exchange chromatography (IEC) allows for the separation of ionizable molecules on the basis of differences in charge properties. Its large sample-handling capacity, broad applicability (particularly to proteins and enzymes), moderate cost, powerful resolving ability, and ease of scale-up and automation have led to it becoming one of the most versatile and widely used of all liquid chromatography (LC) techniques. In this chapter, we review the basic principles of IEC, as well as the broader criteria for selecting IEC conditions. By way of further illustration, we outline protocols necessary to partially purify a serine peptidase from bovine whole brain cytosolic fraction, covering crude tissue extract preparation through to partial purification of the target enzyme using anion-exchange chromatography. Protocols for assaying total protein and enzyme activity in both pre- and post-IEC fractions are also described. The target serine peptidase, prolyl oligopeptidase (POP, EC3.4.21.26), is an 80-kDa enzyme with endopeptidase activity towards peptide substrates of ≤30 amino acids. POP is a ubiquitous post-proline cleaving enzyme with particularly high expression levels in the mammalian brain, where it participates in the metabolism of neuroactive peptides and peptide-like hormones (e.g. thyroliberin, gonadotropin-releasing hormone).

  7. Establishment and application of milk fingerprint by gel filtration chromatography.

    PubMed

    Gao, P; Li, J; Li, Z; Hao, J; Zan, L

    2016-12-01

    Raw milk adulteration frequently occurs in undeveloped countries. It not only reduces the nutritional value of milk, but it is also harmful to consumers. In this paper, we focused on investigating an efficient method for the quality control of raw milk protein. A gel filtration chromatography (GFC) fingerprint method combined with chemometrics was developed for fingerprint analysis of raw milk. To optimize the GFC conditions, milk fat was removed by centrifugation, and GFC analysis was performed on a Superdex 75 10/300GL column (Just Scientific, Shanghai, China) with 0.2 M NaH2PO4-Na2HPO4 buffer (pH 7.0) as the mobile phase. The flow rate was 0.5mL/min, and the detection wavelength was set at 280 nm. Ten batches of 120 raw milk samples were analyzed to establish the GFC fingerprint under optimal conditions. Six major peaks common to the chromatogram of each raw milk sample were selected for fingerprint analysis, and the characteristic peaks were used to establish a standard chromatographic fingerprint. Principal component analysis was then applied to classify GFC information of adulterated milk and raw milk, allowing adulterated samples to be effectively screened out from the raw milk in principal component analysis scores plot. The fingerprint method demonstrates promising features in detecting milk protein adulteration.

  8. Optimization of the separation of lysergic acid diethylamide in urine by a sweeping technique using micellar electrokinetic chromatography.

    PubMed

    Fang, Ching; Liu, Ju-Tsung; Lin, Cheng-Huang

    2002-07-25

    The separation and on-line concentrations of lysergic acid diethylamide (LSD), iso-lysergic acid diethylamide (iso-LSD) and lysergic acid N,N-methylpropylamide (LAMPA) in human urine were investigated by capillary electrophoresis-fluorescence spectroscopy using sodium dodecyl sulfate (SDS) as an anionic surfactant. A number of parameters such as buffer pH, SDS concentration, Brij-30 concentration and the content of organic solvent used in separation, were optimized. The techniques of sweeping-micellar electrokinetic chromatography (sweeping-MEKC) and cation-selective exhaustive injection-sweep-micellar electrokinetic chromatography (CSEI-sweep-MEKC) were used for determining on-line concentrations. The advantages and disadvantages of this procedure with respect to sensitivity, precision and simplicity are discussed and compared.

  9. Digitally Enhanced Thin-Layer Chromatography: An Inexpensive, New Technique for Qualitative and Quantitative Analysis

    ERIC Educational Resources Information Center

    Hess, Amber Victoria Irish

    2007-01-01

    A study conducted shows that if digital photography is combined with regular thin-layer chromatography (TLC), it could perform highly improved qualitative analysis as well as make accurate quantitative analysis possible for a much lower cost than commercial equipment. The findings suggest that digitally enhanced TLC (DE-TLC) is low-cost and easy…

  10. Application of Geophysical Techniques in Glaciology

    NASA Astrophysics Data System (ADS)

    Murray, T.

    2006-05-01

    Glaciologists are faced with the problem that most processes that control ice motion or the transport of water and sediment occur either deep within the glacier ice or at the interface between it and the underlying substrate. However, glaciers are an ideal environment for the application of many geophysical techniques and they have led to significant advances in our understanding of glaciers and ice sheets. Surface and airborne radar has a long pedigree in glaciology and has been used extensively to map beds of the major ice sheets and isochrones within the ice. Cold ice, such as that in Antarctica is easy for radar energy to penetrate, but the water in warm ice scatters radar energy. For this reason it has proved more difficult to image the beds of outlet glaciers in Greenland. Recent advances, particularly in ground-penetrating radar, have meant that it has been possible to image sediment structures within the ice and to use the reflectivity at the bed capture some aspects of the basal water system. Radar energy does not normally penetrate into the beds of ice masses - which are often wet sediments. However, reflection seismics allows us to image further into the basal environment. Using the impedance contrast across the basal interface it is possible to determine whether basal sediments are frozen or unfrozen, and whether they are actively deforming or the ice is sliding over the bed. These questions are key in understanding the dynamics of an ice mass. As a glacier moves overs its bed, seismic energy can be released that provides information on the nature of the basal environment. These events record different source types and relative friction between regions of the bed (so-called "sticky" and "slippery" spots). Considerable work is required to fully exploit the potential of this technique which requires integration with GPS measurements, locating events, and modeling of source types. Geophysical techniques are an ideal tool for exploring the inaccessible

  11. Application of ion chromatography to the study of hydrolysis of some halogenated hydrocarbons at ambient temperatures

    NASA Technical Reports Server (NTRS)

    Otterson, D. A.

    1978-01-01

    The application of ion chromatography to the study of very slow rates of hydrolysis of some halogenated hydrocarbons was investigated. The halide concentrations in the aqueous phase of mixtures of a carbonate buffer (pH = 10.3) and either chloroform (CHC13) or fluorotrichloromethane (CFC13) after aging for various lengths of time at room temperature, were determined by ion chromatography. Hydrolysis of CHC13 caused the C1(-) concentration to increase by about 1500 ppb per day. On the other hand neither the F(-) or C1(-) concentration in the CFC13 mixture increased by as much as 1 ppb per day. The magnitude of errors in the determination of halides prevented any firm conclusions regarding hydrolysis in this mixture. However, these results were used to show how ion chromatography could expedite identification of the hydrolyzing substance as well as investigations of hydrolysis mechanisms.

  12. Measuring fuel contamination using high speed gas chromatography and cone penetration techniques

    SciTech Connect

    Farrington, S.P.; Bratton, W.L.; Akard, M.L.

    1995-10-01

    Decision processes during characterization and cleanup of hazardous waste sites are greatly retarded by the turnaround time and expense incurred through the use of conventional sampling and laboratory analyses. Furthermore, conventional soil and groundwater sampling procedures present many opportunities for loss of volatile organic compounds (VOC) by exposing sample media to the atmosphere during transfers between and among sampling devices and containers. While on-site analysis by conventional gas chromatography can reduce analytical turnaround time, time-consuming sample preparation procedures are still often required, and the potential for loss of VOC is not reduced. This report describes the development of a high speed gas chromatography and cone penetration testing system which can detect and measure subsurface fuel contamination in situ during the cone penetration process.

  13. Automated sample preparation techniques for the determination of drug enantiomers in biological fluids using liquid chromatography with chiral stationary phases.

    PubMed

    Ceccato, A; Toussaint, B; Chiap, P; Hubert, P; Crommen, J

    1999-01-01

    The determination of drug enantiomers has become of prime importance in the field of pharmaceutical and biomedical analysis. Liquid chromatography (LC) is one of the most frequently used techniques for achieving the separation and quantitation of the enantiomers of drug compounds. In the bioanalytical field, the integrated systems present an interesting alternative to time-consuming sample preparation techniques such as liquid-liquid extraction. Solid phase extraction (SPE) on disposable cartridges, dialysis or column switching are sample preparation techniques that can be fully automated and applied to enantioselective analysis in biological fluids. The selection of the most appropriate LC mode and chiral stationary phase for enantioseparations in bioanalysis is discussed and some aspects of these automated sample preparation procedures are compared, such as selectivity, detectability, elution of the analytes from the extraction sorbent, sample volume and analyte stability.

  14. Application of different modes of thin-layer chromatography and mass spectrometry for the separation and detection of large and small biomolecules.

    PubMed

    Tuzimski, Tomasz

    2011-12-09

    Biomolecules are widespread throughout the world. A biomolecule is any organic molecule produced by a living organism, including large polymeric molecules such as proteins, polysaccharides and nucleic acids. Many sample preparation techniques are used in biomolecule analysis; the method selected depends on the complexity of the sample, the nature of the matrix and the analytes, and the analytical technique available. This review covers the current state of knowledge on thin-layer chromatography and mass spectrometry for qualitative analysis of biomolecules. In the first part of the paper the reader will gain useful information to avoid some problems about performing various modes of thin-layer chromatography combined with mass spectrometry experiments and in the second part he will find useful information for application of these techniques for separation, detection, and qualitative investigation of structures and quantitative determination of biomolecules such as proteins, peptides, oligonucleotides, amino acids, DNA, RNA, and lipids.

  15. Principles and Applications of Liquid Chromatography-Mass Spectrometry in Clinical Biochemistry

    PubMed Central

    Pitt, James J

    2009-01-01

    Liquid chromatography-mass spectrometry (LC-MS) is now a routine technique with the development of electrospray ionisation (ESI) providing a simple and robust interface. It can be applied to a wide range of biological molecules and the use of tandem MS and stable isotope internal standards allows highly sensitive and accurate assays to be developed although some method optimisation is required to minimise ion suppression effects. Fast scanning speeds allow a high degree of multiplexing and many compounds can be measured in a single analytical run. With the development of more affordable and reliable instruments, LC-MS is starting to play an important role in several areas of clinical biochemistry and compete with conventional liquid chromatography and other techniques such as immunoassay. PMID:19224008

  16. Homochiral metal-organic frameworks and their application in chromatography enantioseparations.

    PubMed

    Peluso, Paola; Mamane, Victor; Cossu, Sergio

    2014-10-10

    The last frontier in the chiral stationary phases (CSPs) field for chromatography enantioseparations is represented by homochiral metal-organic frameworks (MOFs), a class of organic-inorganic hybrid materials built from metal-connecting nodes and organic-bridging ligands. The modular nature of these materials allows to design focused structures by combining properly metal, organic ligands and rigid polytopic spacers. Intriguingly, chiral ligands introduce molecular chirality in the MOF-network as well as homochirality in the secondary structure of materials (such as homohelicity) producing homochiral nets in a manner mimicking biopolymers (proteins, polysaccharides) which are characterized by a definite helical sense associated with the chirality of their building blocks (amino acids or sugars). Nowadays, robust and flexible materials characterized by high porosity and surface area became available by using preparative procedures typical of the so-called reticular synthesis. This review focuses on recent developments in the synthesis and applications of homochiral MOFs as supports for chromatography enantioseparations. Indeed, despite this field is in its infancy, interesting results have been produced and a critical overview of the 12 reported applications for gas chromatography (GC) and high-performance liquid chromatography (HPLC) can orient the reader approaching the field. Mechanistic aspects are shortly discussed and a view regarding future trends in this field is provided.

  17. Two-dimensional countercurrent chromatography×high performance liquid chromatography with heart-cutting and stop-and-go techniques for preparative isolation of coumarin derivatives from Peucedanum praeruptorum Dunn.

    PubMed

    Liu, Jing-Lan; Wang, Xin-Yuan; Zhang, Ling-Ling; Fang, Mei-Juan; Wu, Yun-Long; Wu, Zhen; Qiu, Ying-Kun

    2014-12-29

    Pure compounds isolated from complex natural plants are important for drug discovery. This study describes a novel two-dimensional hyphenation of counter-current chromatography and high-performance liquid chromatography (2D CCC×HPLC) with heart-cutting and stop-and-go techniques for preparative isolation of multiple targets components from Peucedanum praeruptorum Dunn (Umbelliferae) crude extracts in a single step. The CCC and HPLC were hyphenated via a 4-port valve equipped at the post-end of the CCC column, to heart cut the impure fractions to the 2nd dimensional HPLC for further separation. Furthermore, the stop-and-go flow scheme was applied in the 1st dimensional CCC to fit with the time constraints of the 2nd dimensional preparative HPLC. Last but not least, an optimal biphasic solvent system composed of n-heptane/acetone/water (31:50:19, v/v/v) with suitable Kd values and a higher retention of the stationary phase was chosen to separate target compounds, resulting in the improvement of the CCC column efficiency. By taking the advantages of this rationally designed system, sixteen coumarins were isolated from 1.0g of P. praeruptorum crude extract, with HPLC purity from 90.1% to 99.5%, in a single 2D separation run. More interestingly, two minor linear coumarins and one angular coumarin were isolated from P. praeruptorum Dunn for the first time. As far as we known, this is the first report on the combination of heart-cutting technique and stop-and-go protocol in 2D CCC×HPLC system, by which good separations on comprehensive matrix were achieved. We expect that this approach may have broad applications for simultaneous isolation and purification of multiple components from other complex plant-derived natural products.

  18. Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification

    EPA Science Inventory

    Book Chapter 18, titled Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification, will be published in the book titled High Performance Liquid Chromatography in Pesticide Residue Analysis (Part of the C...

  19. Dancers' Application of the Alexander Technique

    ERIC Educational Resources Information Center

    Fortin, Sylvie; Girard, Fernande

    2005-01-01

    This qualitative study describes the experience of professional contemporary dancers studying and applying the Alexander Technique to their dancing. This study was motivated by: 1. years of teaching both dance and somatics, 2. a strong desire to better understand how the Alexander Technique can be applied by dancers, and 3. a gap that the…

  20. Selective comprehensive multidimensional separation for resolution enhancement in high performance liquid chromatography. Part II: applications.

    PubMed

    Groskreutz, Stephen R; Swenson, Michael M; Secor, Laura B; Stoll, Dwight R

    2012-03-09

    In this second paper of a two-part series, we demonstrate the utility of an approach to enhancing the resolution of select portions of conventional 1D-LC separations, which we refer to as selective comprehensive two-dimensional HPLC (sLC × LC), in three quite different example applications. In the first paper of the series we described the principles of this approach, which breaks the long-standing link in online multi-dimensional chromatography between the timescales of sampling the first dimension (¹D) separation and the separation of fractions of ¹D effluent in the second dimension. In the first example, the power of the sLC × LC approach to significantly reduce the analysis time and method development effort is demonstrated by selectively enhancing the resolution of critical pairs of peaks that are unresolved by a one-dimensional separation (1D-LC) alone. Transfer and subsequent ²D separations of multiple fractions of a particular ¹D peak produces a two-dimensional chromatogram that reveals the coordinates of the peaks in the 2D separation space. The added time dimension of sLC × LC chromatograms also facilitates the application of sophisticated chemometric curve resolution algorithms to further resolve peaks that are otherwise chromatographically unresolved. This is demonstrated in this work by the targeted analysis of phenytoin in urban wastewater effluent using UV diode array detection. Quantitation by both standard addition and external calibration methods yielded results that were not statistically different from 2D-LC/MS/MS analysis of the same samples. Next, we demonstrate the utility of sLC × LC for reducing ion suppression due to matrix effects in electrospray ionization mass spectrometry through the analysis of cocaine in urban wastewater effluent. Finally, we explore the flexibility of the approach in its application to two select regions of a single ¹D separation of triclosan and cocaine. The diversity of these applications demonstrates the

  1. ION-pair liquid chromatography technique for the estimation of metformin in its multicomponent dosage forms.

    PubMed

    Vasudevan, M; Ravi, J; Ravisankar, S; Suresh, B

    2001-04-01

    A simple, precise and accurate high performance liquid chromatography (HPLC) method was developed for the simultaneous estimation of metformin with gliclazide and glipizide present in multicomponent dosage forms. The method was carried out on Inertsil C(18) column. A mobile phase composed of acetonitrile-water containing camphor sulphonic acid (adjusted to pH 7 using 0.1 N sodium hydroxide; 75 mM) at a flow rate of 1 ml min(-1) was used for the separation. Detection was carried out at 225 nm. Tolbutamide was used as internal standard. Validation of the developed HPLC method was carried out.

  2. Development of techniques for complex mixture analysis by means of gas chromatography/triple quadrupole mass spectrometry

    SciTech Connect

    Schubert, A.J.

    1988-01-01

    Current technology in several phases of organic mixture analysis have been integrated to demonstrate the analytical power of the combined technique of gas chromatography/triple quadrupole mass spectrometry (GC/TQMS). This research has included capillary gas chromatography, chemical ionization, triple quadrupole mass spectrometry, and the high speed instrument control and data systems which are required to make such a powerful instrument feasible. The feasibility of GC/TQMS was enhanced by an increase in overall system speed and the development of programs to allow trace-level targeted component analyses on time variant samples introduced via the gas chromatograph. The performance of the instrument control system was achieved by dividing instrument control tasks among multiple processors rather than by increasing the power of the processor being used. Methanol chemical ionization was investigated as a tool for the mass spectrometric determination of trace level polar components in petroleum products. Results from this study indicate that methanol enhances both the selectivity and sensitivity of the ionization when compared to the more conventional technique of methane chemical ionization. Studies on the effect of varying the pressure of the methanol reagent demonstrated a simple approach through which the analyst can adjust both the sensitivity and selectivity of the ionization. Detection limits were determined for the determination of several thiophenes in a commercial jet aviation fuel by means of GC/TQMS. The combined use of capillary gas chromatography, methanol chemical ionization, and TQMS with specialized data acquisition programs, enabled the detection of these targeted components down to the low parts per million.

  3. Investigation of liquid and gas chromatography techniques for separation of diastereomers of beta-(alpha-methylbenzyl) amino isobutyric acid.

    PubMed

    Held, Charles B; Robbins, David K

    2003-09-01

    Cryptophycins are macrolides investigated as potential anticancer agents. These large cyclic molecules are generated via a convergent process, utilizing the coupling of several smaller fragments synthesized individually. During early synthetic development of the beta-amino acid fragment C, analytical methods are necessary for the characterization of products resulting from the various routes being studied. One route being evaluated produces (RR) and (RS) diastereomers of beta-(alpha-methylbenzyl) amino isobutyric acid as intermediates. To measure diastereomeric excess (%de), assay conditions using high-performance liquid chromatography (HPLC) and capillary gas chromatographic (GC) techniques are explored. Derivatization methods using trifluoroacetyl- and silyl-derivatives are investigated for use with capillary GC. The results of the GC investigations are found to be only partially successful. Ion-pair HPLC is determined to be the optimal technique, utilizing pentanesulfonic acid as the counter ion to the amine group of beta-(alpha-methylbenzyl) amino isobutyric acid.

  4. Identification of wood between Phoebe zhennan and Machilus pingii using the gas chromatography-mass spectrometry direct injection technique.

    PubMed

    Xu, Bin; Zhu, Tao; Li, Jingya; Liu, Shuai

    2013-01-01

    In this paper, the technique of direct injection gas chromatography-mass spectrometer (GC-MS) was employed to discriminate between two batches of wood (Phoebe zhennan and Machilus pingii) with characteristic smells. Based on the GC-MS fingerprints obtained, similarities between samples were evaluated via correlation coefficient, hierarchical clustering and characteristic constituents analysis. The results showed that distinct differences in total ion chromatograms existed between the two species of wood and their correlation coefficients were low; however, the relationship between the same species of different batches showed the opposite; meanwhile, the analysis of hierarchical clustering and characteristic constituents also demonstrated an interrelationship. All the analytical methods achieved the goal of identification between the two species of wood, which verified that the technique can be used to identify different species of wood with characteristic smells.

  5. Advances in analytical techniques for neutron capture therapy: thin layer chromatography matrix and track etch thin layer chromatography methods for boron-10 analysis

    SciTech Connect

    Schremmer, J.M.; Noonan, D.J.

    1987-09-01

    A new track etch autoradiographic technique for quantitating boron-10 containing compounds used for neutron capture therapy is described. Instead of applying solutions of Cs2B12H11SH and its oxidation products directly to solid-state nuclear track detectors, diethylaminoethyl cellulose thin layer chromatography (TLC) plates are utilized as sample matrices. The plates are juxtaposed with Lexan polycarbonate detectors and irradiated in a beam of thermal neutrons. The detectors are then chemically etched, and the resultant tracks counted with an optoelectronic image analyzer. Sensitivity to boron-10 in solution reaches the 1 pg/microliter level, or 1 ppb. In heparinized blood samples, 100 pg boron-10/microliter are detected. This TLC matrix method has the advantage that sample plates can be reanalyzed under different reactor conditions to optimize detector response to the boron-10 carrier material. Track etch/TLC allows quantitation of the purity of boron neutron capture therapy compounds by utilizing the above method with TLC plates developed in solvent systems that resolve Cs2B12H11SH and its oxidative analogs. Detectors irradiated in juxtaposition to the thin layer chromatograms are chemically etched, and the tracks are counted in the sample lane from the origin of the plate to the solvent front. A graphic depiction of the number of tracks per field yields a quantitative analysis of compound purity.

  6. Quantification of aroma compounds in Parmigiano Reggiano cheese by a dynamic headspace gas chromatography-mass spectrometry technique and calculation of odor activity value.

    PubMed

    Qian, Michael; Reineccius, G A

    2003-03-01

    Potentially important aroma compounds in Parmigiano Reggiano cheese were quantified. Free fatty acids were isolated with ion-exchange chromatography and quantified by gas chromatography. Neutral aroma compounds were quantified with a purge-trap/gas chromatography-mass spectrometry with selective mass ion technique. Odor activity values were calculated based on sensory thresholds reported in literature. The calculated odor activity values suggest that 3-methylbutanal, 2-methylpropanal, 2-methylbutanal, dimethyl trisulfide, diacetyl, methional, phenylacetaldehyde, ethyl butanoate, ethyl hexanoate, ethyl octanoate, acetic, butanoic, hexanoic, and octanoic acids are the most important aroma contributors to Parmigiano Reggiano cheese.

  7. Application of Headspace Solid Phase Microextraction and Gas Chromatography/Mass Spectrometry for Rapid Detection of the Chemical Warfare Agent Sulfur Mustard

    DTIC Science & Technology

    2002-05-16

    Title of Thesis: “Application of Headspace Solid Phase Microextraction and Gas Chromatography/Mass Spectrometry for Rapid...TITLE AND SUBTITLE Application of Headspace Solid Phase Microextraction and Gas Chromatography/Mass Spectrometry for Rapid Detection of the Chemical...phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS). Five commercially available SPME fibers were investigated to determine the

  8. [Cardiac computed tomography: new applications of an evolving technique].

    PubMed

    Martín, María; Corros, Cecilia; Calvo, Juan; Mesa, Alicia; García-Campos, Ana; Rodríguez, María Luisa; Barreiro, Manuel; Rozado, José; Colunga, Santiago; de la Hera, Jesús M; Morís, César; Luyando, Luis H

    2015-01-01

    During the last years we have witnessed an increasing development of imaging techniques applied in Cardiology. Among them, cardiac computed tomography is an emerging and evolving technique. With the current possibility of very low radiation studies, the applications have expanded and go further coronariography In the present article we review the technical developments of cardiac computed tomography and its new applications.

  9. 48 CFR 9904.417-50 - Techniques for application.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... 48 Federal Acquisition Regulations System 7 2010-10-01 2010-10-01 false Techniques for application... ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.417-50 Techniques for application. (a) The cost of money... capitalized, such as the method used for financial accounting and reporting, may be used, provided...

  10. Determination of fluoxetine enantiomers in pharmaceutical formulations by electrokinetic chromatography-counter current technique.

    PubMed

    Asensi-Bernardi, Lucía; Martín-Biosca, Yolanda; Fornet-Herrero, Eder; Sagrado, Salvador; Medina-Hernández, María José

    2013-03-01

    In this work, an electrokinetic chromatography-counter current procedure for the separation of fluoxetine enantiomers using highly sulfated β-cyclodextrin was optimized and applied to the determination of the enantiomers in three pharmaceutical formulations according to the matrix features. Quality criteria were applied to facilitate its transferability to testing laboratories. Fluoxetine was used therapeutically as the racemate, although a stereospecificity associated with its interactions with the neuronal serotonin-uptake carrier was demonstrated. In this context, the development of enantioselective methods for the chiral analysis of pharmaceuticals allowing stereoisomer ratio estimations has increasing interest in pharmaceutical industry. The proposed method allows the quantification of both enantiomers in less than 2 min with high resolution (R(s) = 2.4).

  11. Discrimination of honeys using colorimetric sensor arrays, sensory analysis and gas chromatography techniques.

    PubMed

    Tahir, Haroon Elrasheid; Xiaobo, Zou; Xiaowei, Huang; Jiyong, Shi; Mariod, Abdalbasit Adam

    2016-09-01

    Aroma profiles of six honey varieties of different botanical origins were investigated using colorimetric sensor array, gas chromatography-mass spectrometry (GC-MS) and descriptive sensory analysis. Fifty-eight aroma compounds were identified, including 2 norisoprenoids, 5 hydrocarbons, 4 terpenes, 6 phenols, 7 ketones, 9 acids, 12 aldehydes and 13 alcohols. Twenty abundant or active compounds were chosen as key compounds to characterize honey aroma. Discrimination of the honeys was subsequently implemented using multivariate analysis, including hierarchical clustering analysis (HCA) and principal component analysis (PCA). Honeys of the same botanical origin were grouped together in the PCA score plot and HCA dendrogram. SPME-GC/MS and colorimetric sensor array were able to discriminate the honeys effectively with the advantages of being rapid, simple and low-cost. Moreover, partial least squares regression (PLSR) was applied to indicate the relationship between sensory descriptors and aroma compounds.

  12. Recent trends in application of multivariate curve resolution approaches for improving gas chromatography-mass spectrometry analysis of essential oils.

    PubMed

    Jalali-Heravi, Mehdi; Parastar, Hadi

    2011-08-15

    Essential oils (EOs) are valuable natural products that are popular nowadays in the world due to their effects on the health conditions of human beings and their role in preventing and curing diseases. In addition, EOs have a broad range of applications in foods, perfumes, cosmetics and human nutrition. Among different techniques for analysis of EOs, gas chromatography-mass spectrometry (GC-MS) is the most important one in recent years. However, there are some fundamental problems in GC-MS analysis including baseline drift, spectral background, noise, low S/N (signal to noise) ratio, changes in the peak shapes and co-elution. Multivariate curve resolution (MCR) approaches cope with ongoing challenges and are able to handle these problems. This review focuses on the application of MCR techniques for improving GC-MS analysis of EOs published between January 2000 and December 2010. In the first part, the importance of EOs in human life and their relevance in analytical chemistry is discussed. In the second part, an insight into some basics needed to understand prospects and limitations of the MCR techniques are given. In the third part, the significance of the combination of the MCR approaches with GC-MS analysis of EOs is highlighted. Furthermore, the commonly used algorithms for preprocessing, chemical rank determination, local rank analysis and multivariate resolution in the field of EOs analysis are reviewed.

  13. Fluorescence Lifetime Techniques in Medical Applications

    PubMed Central

    Marcu, Laura

    2012-01-01

    This article presents an overview of time-resolved (lifetime) fluorescence techniques used in biomedical diagnostics. In particular, we review the development of time-resolved fluorescence spectroscopy (TRFS) and fluorescence lifetime imaging (FLIM) instrumentation and associated methodologies which allows for in vivo characterization and diagnosis of biological tissues. Emphasis is placed on the translational research potential of these techniques and on evaluating whether intrinsic fluorescence signals provide useful contrast for the diagnosis of human diseases including cancer (gastrointestinal tract, lung, head and neck, and brain), skin and eye diseases, and atherosclerotic cardiovascular disease. PMID:22273730

  14. Application of GPC/LALLS to cellulose research. [Gel permeation chromatography/low-angle laser light scattering

    SciTech Connect

    Cael, J.J.; Cietek, D.J.; Kolpak, F.J.

    1983-01-01

    The techniques of gel permeation chromatography and low-angle laser light scattering (GPC/LALLS) have been combined for absolute determination of cellulose molecular weights and molecular weight distributions (MWD). The GPC/LALLS technique has been applied to tetrahydrofuran (THF) solutions of cellulose tricarbanilate (CTC) derivatives prepared from celluloses having a wide range of molecular weights. The molecular weight data obtained are consistent with values determined by intrinsic viscosity methods; and as a consequence of the absolute nature of this technique, Mark-Houswink coefficients can be predicted from a single, broad-distribution, linear homopolymer without recourse to tedious and time-consuming fractional precipitation methods. A unique application of the technique has been in correlating GPC/LALLS molecular weight data with the viscosity of nonderivatized celluloses dissolved in 0.5 M cupiethylenediamine hydroxide (CuEn). The procedure yields an absolute viscosity-molecular weight relationship which is comparable with a similar relationship originally derived from cellulose nitrates. The results indicate that the weight-average degree of polymerization (DP/sub w/) for CTC preparations is considerably greater than that obtained from cellulose nitrates, and this discrepancy, in DP/sub w/ has been attributed to errors in the Mark-Houwink coefficients for the cellulose nitrate-acetone system. 25 references, 9 figures, 7 tables.

  15. Moire Ct technique and its application on laser flexible manufacture

    NASA Astrophysics Data System (ADS)

    Li, Tianze; Hou, Luan; Jiang, Chuan; Zhang, Xia

    2010-10-01

    In the paper, the main properties of Moire fringe, such as average effect, amplification effect, corresponding relation are elaborated, and the principle of Moire Ct technique is represented. On the basis of main features of Moire fringe, multidirectional Moire Ct deflection system is designed using high accuracy Ccd, grating, filter, lens, planar mirror and optical splitter. The system has simple light path, and can be easily made into the one that has large caliber.It can analyze multidirectional records of the probe at the same time, and can obtain clear interference patterns.The iterative technique combined with computer chromatography algorithms is used to achieve inversion of multidirectional clear interference patterns so that the required parameters can be acquired. Moire Ct technique is applied to laser flexible manufacture. Produced parts are delaminated on the paper, and are stratified manufactured until they are connected to forming. Cad/Cam system is adopted to construct Spatial three-dimensional geometric model, and the data files are formed. Then by using the Small triangle plane, the inner and outer surfaces of the data files are discretized. Discretized parts model is made chromatography with mathematical methods using Cam software. A series of parallel horizontal intersecting planes are generated. The problems of filtering arrangement tangent points are solved by recombining the shape and structure relationship among the triangular mesh. Several conclusions are presented.

  16. Determination of organophosphorus pesticides by gas chromatography with mass spectrometry using a large-volume injection technique after magnetic extraction.

    PubMed

    Nedaei, Maryam; Salehpour, Ali-Reza; Mozaffari, Shahla; Yousefi, Seyedeh Mahboobeh; Yousefi, Seyed Reza

    2014-09-01

    A fast and efficient method was developed for the extraction and determination of organophosphorus pesticides in water samples. Organophosphorus pesticides were extracted by solid-phase extraction using magnetic multi-walled carbon nanotubes and determined by gas chromatography with ion-trap mass spectrometry. Parameters affecting the extraction were investigated. Under optimum conditions of the method, 10 mg magnetic multi-walled carbon nanotubes were added into 10 mL sample. After 2 min, adsorbent particles settled at the bottom of test tube with a magnet. After removing aqueous supernatant, the analytes were desorbed with acetonitrile. Then, 70 μL of acetonitrile phase was injected into the gas chromatography and mass spectrometry system that had an ion-trap analyzer. To achieve high sensitivity, the large-volume-injection technique was used with a programmed temperature vaporization inlet, and the ion-trap mass spectrometer was operated in single ion storage mode. Under the best conditions, the enrichment factors and extraction recoveries were in the range of 113-124 and 74-103%, respectively. The limits of detection were between 3 and 15 ng/L, and the relative standard deviations were < 10%. This method was successfully used for the determination of organophosphorus pesticides in dam water, lagoon water, and river water samples with good reproducibility and recovery.

  17. Experimental Techniques Applicable to Turbulent Flows.

    DTIC Science & Technology

    1977-01-01

    dent laser , and Stokesplier, e the electron charge, R the load radiation respectively, I ~, is the co— resistance , E the energy of the scattered... measurements of methane , Sca ttering of a Laser Beam ”, A IAA J. 9— using the spontaneous Ramars effect and the 1971., PIBAL Rep. No. 69—46, Nov...developed Laser Raman and of several species of interest in a flame, Laser Doppler techniques may be ideally their individual temperatures as well as

  18. Valid internal standard technique for arson detection based on gas chromatography-mass spectrometry.

    PubMed

    Salgueiro, Pedro A S; Borges, Carlos M F; Bettencourt da Silva, Ricardo J N

    2012-09-28

    The most popular procedures for the detection of residues of accelerants in fire debris are the ones published by the American Society for Testing and Materials (ASTM E1412-07 and E1618-10). The most critical stages of these tests are the conservation of fire debris from the sampling to the laboratory, the extraction of residues of accelerants from the debris to the activated charcoal strips (ACS) and from those to the final solvent, as well as the analysis of sample extract by gas chromatography-mass spectrometry (GC-MS) and the interpretation of the instrumental signal. This work proposes a strategy for checking the quality of the sample conservation, the accelerant residues transference to final solvent and GC-MS analysis, using internal standard additions. It is used internal standards ranging from a highly volatile compound for checking debris conservation to low volatile compound for checking GC-MS repeatability. The developed quality control (QC) parameters are not affected by GC-MS sensitivity variation and, specifically, the GC-MS performance control is not affected by ACS adsorption saturation that may mask test performance deviations. The proposed QC procedure proved to be adequate to check GC-MS repeatability, ACS extraction and sample conservation since: (1) standard additions are affected by negligible uncertainty and (2) observed dispersion of QC parameters are fit for its intended use.

  19. Expanded separation technique for chlorophyll metabolites in Oriental tobacco leaf using non aqueous reversed phase chromatography.

    PubMed

    Ishida, Naoyuki

    2011-08-26

    An improved separation method for chlorophyll metabolites in Oriental tobacco leaf was developed. While Oriental leaf still gives the green color even after the curing process, little attention has been paid to the detailed composition of the remaining green pigments. This study aimed to identify the green pigments using non aqueous reversed phase chromatography (NARPC). To this end, liquid chromatograph (LC) equipped with a photo diode array detector (DAD) and an atmospheric pressure chemical ionization/mass spectrometer (APCI/MSD) was selected, because it is useful for detecting low polar non-volatile compounds giving green color such as pheophytin a. Identification was based on the wavelength spectrum, mass spectrum and retention time, comparing the analytes in Oriental leaf with the commercially available and synthesized components. Consequently, several chlorophyll metabolites such as hydroxypheophytin a, solanesyl pheophorbide a and solanesyl hydroxypheophorbide a were newly identified, in addition to typical green pigments such as chlorophyll a and pheophytin a. Chlorophyll metabolites bound to solanesol were considered the tobacco specific components. NARPC expanded the number of detectable low polar chlorophyll metabolites in Oriental tobacco leaf.

  20. Molecular authentication and quality control using a high performance liquid chromatography technique of Fructus Evodiae.

    PubMed

    Huang, Dan; Li, Shun Xiang; Cai, Guang Xian; Yue, Chun Hua; Wei, Li Jun; Zhang, Ping

    2008-02-01

    In present paper, the properties of molecular authentication combined with the fingerprints of high performance liquid chromatography (HPLC) were validated by analyzing ten batches of Fructus Evodiae samples (the dried nearly ripe fruit of Evodia rutaecarpa (JUSS.) BENTH., Evodia rutaecarpa (JUSS.) BENTH. var. officinalis (DODE) HUANG or Evodia rutaecarpa (JUSS.) BENTH. var. bodinieri (DODE) HUANG). The results of this investigation show that the similarities of internal transcribed spacer (ITS) sequences were almost 100% in Evodia rutaecarpa (JUSS.) BENTH. var. bodinieri (DODE) HUANG, 97% in Evodia rutaecarpa (JUSS.) BENTH., and 96% in Evodia rutaecarpa (JUSS.) BENTH. var. officinalis (DODE) HUANG. The percentage of identity between the two groups of Evodia rutaecarpa (JUSS.) BENTH. var. bodinieri (DODE) HUANG and Evodia rutaecarpa (JUSS.) BENTH. var. officinalis (DODE) HUANG is almost 96%, but the identity among the group of these three species is only 73%. The results show that Fructus Evodiae comes from three species respectively. The fingerprints of HPLC show that Fructus Evodiae revealed 20 major common peaks. And the three species have almost the same chemical constituents. ITS sequence fingerprint combining the fingerprint of HPLC can not only be developed to identify and distinguish the three species in detail, but also can be used for optimizing location where Fructus Evodiae has much higher bioactive constituents and yield.

  1. Determination of Synthetic Cathinones in Urine Using Gas Chromatography-Mass Spectrometry Techniques.

    PubMed

    Hong, Wei-Yin; Ko, Ya-Chun; Lin, Mei-Chih; Wang, Po-Yu; Chen, Yu-Pen; Chiueh, Lih-Ching; Shih, Daniel Yang-Chih; Chou, Hsiu-Kuan; Cheng, Hwei-Fang

    2016-01-01

    In recent years, the abuse of synthetic cathinones has increased considerably. This study proposes a method, based on gas chromatography/mass spectrometry (GC-MS), to analyze and quantify six synthetic cathinones in urine samples: mephedrone (4-MMC), methylone (bk-MDMA), butylone, ethylone, pentylone and methylenedioxypyrovalerone (MDPV). In our procedure, the urine samples undergo solid-phase extraction (SPE) and derivatization prior to injection into the GC-MS device. Separation is performed using a HP-5MS capillary column. The use of selective ion monitoring (SIM mode) makes it is good sensitivity in this method, and the entire analysis process is within 18 min. In addition, the proposed method maintains linearity in the calibration curve from 50 to 2,000 ng/mL (r(2) > 0.995). The limit of detection of this method is 5 ng/mL, with the exception of MDPV (20 ng/mL); the limit of quantification is 20 ng/mL, with the exception of MDPV (50 ng/mL). In testing, the extraction performance of SPE was between 82.34 and 104.46%. Precision and accuracy results were satisfactory <15%. The proposed method was applied to six real urine samples, one of which was found to contain 4-MMC and bk-MDMA. Our results demonstrate the efficacy of the proposed method in the identification of synthetic cathinones in urine, with regard to the limits of detection and quantification. This method is highly repeatable and accurate.

  2. An overview of heat exchanger enhancement techniques for industrial applications

    SciTech Connect

    Somasundaram, S.; Ohadi, M.M.; Richlen, S.

    1992-06-01

    An assessment is make of selected currently available heat exchanger enhancement techniques for single- and two-phase heat transfer mechanisms to determine their practicality and commercialization potential for different industrial applications. The assessment includes a screening review of the major techniques being investigated in the research community, and identification of selected passive techniques and determine their potential limitations with respect to industrial applications. A more detailed study of the research needs and the technology gaps is being conducted to address the issues of concern for each practical application of the chosen techniques. The technical and economic feasibility and the performance benefits of incorporating a particular technique in a heat transfer process is also discussed. The potential design, operational, and manufacturing cost issues that have prevented a technique from being widely commercialized are identified.

  3. Inverse Raman effect: applications and detection techniques

    SciTech Connect

    Hughes, L.J. Jr.

    1980-08-01

    The processes underlying the inverse Raman effect are qualitatively described by comparing it to the more familiar phenomena of conventional and stimulated Raman scattering. An experession is derived for the inverse Raman absorption coefficient, and its relationship to the stimulated Raman gain is obtained. The power requirements of the two fields are examined qualitatively and quantitatively. The assumption that the inverse Raman absorption coefficient is constant over the interaction length is examined. Advantages of the technique are discussed and a brief survey of reported studies is presented.

  4. Recent developments in sample preparation techniques for chromatography analysis of traditional Chinese medicines.

    PubMed

    Deng, Chunhui; Liu, Ning; Gao, Mingxia; Zhang, Xiangmin

    2007-06-15

    Traditional Chinese medicines (TCMs) have a long history dating back thousands of years. Recently, there has been increasing interest worldwide in the use of TCMs for the prevention and treatment of various illnesses. In China, a large number of analytical tools, especially chromatographic techniques have been used to analyze the constituents of TCMs in order to control their quality and discover new bioactive compounds. In this paper, recent developments in sample preparation techniques for the extraction, clean-up, and concentration of analytes from TCMs are compared. These techniques include headspace solid-phase microextraction (HS-SPME), headspace liquid-phase microextraction (HS-LPME), microwave-assisted extraction (MAE), supercritical-fluid extraction (SFE), pressurized-liquid extraction (PLE), and microwave distillation (MD).

  5. Layered classification techniques for remote sensing applications

    NASA Technical Reports Server (NTRS)

    Swain, P. H.; Wu, C. L.; Landgrebe, D. A.; Hauska, H.

    1975-01-01

    The single-stage method of pattern classification utilizes all available features in a single test which assigns the unknown to a category according to a specific decision strategy (such as the maximum likelihood strategy). The layered classifier classifies the unknown through a sequence of tests, each of which may be dependent on the outcome of previous tests. Although the layered classifier was originally investigated as a means of improving classification accuracy and efficiency, it was found that in the context of remote sensing data analysis, other advantages also accrue due to many of the special characteristics of both the data and the applications pursued. The layered classifier method and several of the diverse applications of this approach are discussed.

  6. In vivo investigation of pharmacokinetics of model drug: comparison of near infrared technique with high-performance liquid chromatography

    NASA Astrophysics Data System (ADS)

    Gu, Yueqing; Liu, Fei; Fang, Chunsheng; Qian, Zhiyu; Achilefu, Samuel

    2010-02-01

    Near infrared spectroscopy possess great potential for in vivo quantitative monitoring of drugs in animal subject. The accuracy of the measurements by near infrared technique should be evaluated by an established method. In this study, a near infrared fluorescence dye, cypate and its conjugation cypate-PEG were used as model drug for in vivo dynamic study. The pharmacokinetics of the model drug in mice subjects were investigated by near infrared spectroscopy and high performance liquid chromatography, respectively. The results from the two techniques were compared. The pharmacokinetic parameters calculated based on the acquired data by DAS software showed that there were no statistical differences between the two methods. The dynamic distribution of the model drugs in mouse model imaged by NIR image system indicated that cypate firstly accumulated in liver and was cleared from the enteron system, while cypate - PEG clearance from the urine system. Results indicated that NIR monitoring technique provide a promising quantitative way for in vivo monitoring the dynamics of drugs in animal subjects.

  7. Chemometrics applications in biotechnology processes: predicting column integrity and impurity clearance during reuse of chromatography resin.

    PubMed

    Rathore, Anurag S; Mittal, Shachi; Lute, Scott; Brorson, Kurt

    2012-01-01

    Separation media, in particular chromatography media, is typically one of the major contributors to the cost of goods for production of a biotechnology therapeutic. To be cost-effective, it is industry practice that media be reused over several cycles before being discarded. The traditional approach for estimating the number of cycles a particular media can be reused for involves performing laboratory scale experiments that monitor column performance and carryover. This dataset is then used to predict the number of cycles the media can be used at manufacturing scale (concurrent validation). Although, well accepted and widely practiced, there are challenges associated with extrapolating the laboratory scale data to manufacturing scale due to differences that may exist across scales. Factors that may be different include: level of impurities in the feed material, lot to lot variability in feedstock impurities, design of the column housing unit with respect to cleanability, and homogeneity of the column packing. In view of these challenges, there is a need for approaches that may be able to predict column underperformance at the manufacturing scale over the product lifecycle. In case such an underperformance is predicted, the operators can unpack and repack the chromatography column beforehand and thus avoid batch loss. Chemometrics offers one such solution. In this article, we present an application of chemometrics toward the analysis of a set of chromatography profiles with the intention of predicting the various events of column underperformance including the backpressure buildup and inefficient deoxyribonucleic acid clearance.

  8. Laser induced fluorescence technique for environmental applications

    NASA Astrophysics Data System (ADS)

    Utkin, Andrei B.; Felizardo, Rui; Gameiro, Carla; Matos, Ana R.; Cartaxana, Paulo

    2014-08-01

    We discuss the development of laser induced fluorescence sensors and their application in the evaluation of water pollution and physiological status of higher plants and algae. The sensors were built on the basis of reliable and robust solid-state Nd:YAG lasers. They demonstrated good efficiency in: i) detecting and characterizing oil spills and dissolved organic matter; ii) evaluating the impact of stress on higher plants (cork oak, maritime pine, and genetically modified Arabidopsis); iii) tracking biomass changes in intertidal microphytobenthos; and iv) mapping macroalgal communities in the Tagus Estuary.

  9. Defectoscopic and Clinical Applications of Infrared Technique

    NASA Astrophysics Data System (ADS)

    Kopal, I.; Koštial, P.; Špička, I.; Pleva, L.; Jančíková, Z.

    2017-02-01

    The article deals with possible visualization of inhomogeneities in inorganic materials, such as laminates, as well as organic materials, such as bones. This work also provides a study of the visualization of internal fixation (nail), introduced in a bone by the IR technique. In the theoretical part, we present thermal wave propagation and a theoretical approach to the possibility of visualization of the boundary between two different materials with different thermal conductivity. Further on, the experimental method is tested with success on discovering artificial defects in glass laminates. In the second part of the article, a successful method of the visualization of the internal fixator position in a bone under IR excitation is presented. Methods of processing the data measured with the use of an infrared camera are presented in detail.

  10. Hybrid Grid Techniques for Propulsion Applications

    NASA Technical Reports Server (NTRS)

    Koomullil, Roy P.; Soni, Bharat K.; Thornburg, Hugh J.

    1996-01-01

    During the past decade, computational simulation of fluid flow for propulsion activities has progressed significantly, and many notable successes have been reported in the literature. However, the generation of a high quality mesh for such problems has often been reported as a pacing item. Hence, much effort has been expended to speed this portion of the simulation process. Several approaches have evolved for grid generation. Two of the most common are structured multi-block, and unstructured based procedures. Structured grids tend to be computationally efficient, and have high aspect ratio cells necessary for efficently resolving viscous layers. Structured multi-block grids may or may not exhibit grid line continuity across the block interface. This relaxation of the continuity constraint at the interface is intended to ease the grid generation process, which is still time consuming. Flow solvers supporting non-contiguous interfaces require specialized interpolation procedures which may not ensure conservation at the interface. Unstructured or generalized indexing data structures offer greater flexibility, but require explicit connectivity information and are not easy to generate for three dimensional configurations. In addition, unstructured mesh based schemes tend to be less efficient and it is difficult to resolve viscous layers. Recently hybrid or generalized element solution and grid generation techniques have been developed with the objective of combining the attractive features of both structured and unstructured techniques. In the present work, recently developed procedures for hybrid grid generation and flow simulation are critically evaluated, and compared to existing structured and unstructured procedures in terms of accuracy and computational requirements.

  11. Surface modification: advantages, techniques, and applications

    SciTech Connect

    Natesan, K.

    2000-03-01

    Adequate performance of materials at elevated temperatures is a potential problem in many systems within the chemical, petroleum, process, and power-generating industries. Degradation of materials occurs because of interaction between the structural material and the exposure environment. These interactions are generally undesired chemical reactions that can lead to accelerated wastage and alter the functional requirements and/or structural integrity of the materials. Therefore, material selection for high-temperature applications must be based not only on a material strength properties but also on resistance to the complex environments prevalent in the anticipated exposure environment. As plants become larger, the satisfactory performance and reliability of components play a greater role in plant availability and economics. However, system designers are becoming increasingly concerned with finding the least expensive material that will satisfactorily perform the design function for the desired service life. This present paper addresses the benefits of surface modification and identified several criteria for selection and application of modified surfaces in the power sector. A brief review is presented on potential methods for modification of surfaces, with the emphasis on coatings. In the final section of the paper, several examples address the requirements of different energy systems and surface modification avenues that have been applied to resolve the issues.

  12. Application of hybrid LRR technique to protein crystallization.

    PubMed

    Jin, Mi Sun; Lee, Jie-Oh

    2008-05-31

    LRR family proteins play important roles in a variety of physiological processes. To facilitate their production and crystallization, we have invented a novel method termed "Hybrid LRR Technique". Using this technique, the first crystal structures of three TLR family proteins could be determined. In this review, design principles and application of the technique to protein crystallization will be summarized. For crystallization of TLRs, hagfish VLR receptors were chosen as the fusion partners and the TLR and the VLR fragments were fused at the conserved LxxLxLxxN motif to minimize local structural incompatibility. TLR-VLR hybridization did not disturb structures and functions of the target TLR proteins. The Hybrid LRR Technique is a general technique that can be applied to structural studies of other LRR proteins. It may also have broader application in biochemical and medical application of LRR proteins by modifying them without compromising their structural integrity.

  13. Autoregressive and bispectral analysis techniques: EEG applications.

    PubMed

    Ning, T; Bronzino, J D

    1990-01-01

    Some basic properties of autoregressive (AR) modeling and bispectral analysis are reviewed, and examples of their application in electroencephalography (EEG) research are provided. A second-order AR model was used to score cortical EEGs in order. In tests performed on five adult rats to distinguish between different vigilance states such a quiet-waking (QW), rapid-eye-movement (REM), and slow-wave sleep (SWS), SWS activity was correctly identified over 96% of the time, and a 95% agreement rate was achieved in recognizing the REM sleep stage. In a bispectral analysis of the rat EEG, third-order cumulant (TOC) sequences of 32 epochs belonging to the same vigilance state were estimated and then averaged. Preliminary results have shown that bispectra of hippocampal EEGs during REM Sleep exhibit significant quadratic phase couplings between frequencies in the 6-8-Hz range, associated with the theta rhythm.

  14. Bile salt surfactants in micellar electrokinetic capillary chromatography: Application to hydrophobic molecule separations

    SciTech Connect

    Cole, R.O.; Sepaniak, M.J. . Dept. of Chemistry); Hinze, W.L. . Dept. of Chemistry); Gorse, J.; Oldiges, K. . Dept. of Chemistry)

    1990-01-01

    Bile Salt surfactants are used in the micellar electrokinetic capillary chromatography (MECC) separation of various hydrophobic compounds. The use of methanol in the mobile phase allows the separation of previously intractable compounds including polyaromatic hydrocarbons. The effects of methanol on critical micelle concentration is investigated for sodium dodecyl sulfate (SDS) and the bile salt sodium cholate. It is determined that the unique structure of the bile salt micelle is much more tolerant to the addition of organic solvents than SDS, thereby increasing the scope of applications of MECC to include hydrophobic compounds. 30 refs., 9 figs.

  15. Instrumentation: Ion Chromatography.

    ERIC Educational Resources Information Center

    Fritz, James S.

    1987-01-01

    Discusses the importance of ion chromatography in separating and measuring anions. The principles of ion exchange are presented, along with some applications of ion chromatography in industry. Ion chromatography systems are described, as well as ion pair and ion exclusion chromatography, column packings, detectors, and programming. (TW)

  16. Radiomics: a new application from established techniques

    PubMed Central

    Parekh, Vishwa; Jacobs, Michael A.

    2016-01-01

    The increasing use of biomarkers in cancer have led to the concept of personalized medicine for patients. Personalized medicine provides better diagnosis and treatment options available to clinicians. Radiological imaging techniques provide an opportunity to deliver unique data on different types of tissue. However, obtaining useful information from all radiological data is challenging in the era of “big data”. Recent advances in computational power and the use of genomics have generated a new area of research termed Radiomics. Radiomics is defined as the high throughput extraction of quantitative imaging features or texture (radiomics) from imaging to decode tissue pathology and creating a high dimensional data set for feature extraction. Radiomic features provide information about the gray-scale patterns, inter-pixel relationships. In addition, shape and spectral properties can be extracted within the same regions of interest on radiological images. Moreover, these features can be further used to develop computational models using advanced machine learning algorithms that may serve as a tool for personalized diagnosis and treatment guidance. PMID:28042608

  17. Radiomics: a new application from established techniques.

    PubMed

    Parekh, Vishwa; Jacobs, Michael A

    2016-01-01

    The increasing use of biomarkers in cancer have led to the concept of personalized medicine for patients. Personalized medicine provides better diagnosis and treatment options available to clinicians. Radiological imaging techniques provide an opportunity to deliver unique data on different types of tissue. However, obtaining useful information from all radiological data is challenging in the era of "big data". Recent advances in computational power and the use of genomics have generated a new area of research termed Radiomics. Radiomics is defined as the high throughput extraction of quantitative imaging features or texture (radiomics) from imaging to decode tissue pathology and creating a high dimensional data set for feature extraction. Radiomic features provide information about the gray-scale patterns, inter-pixel relationships. In addition, shape and spectral properties can be extracted within the same regions of interest on radiological images. Moreover, these features can be further used to develop computational models using advanced machine learning algorithms that may serve as a tool for personalized diagnosis and treatment guidance.

  18. Validation of a new liquid chromatography- tandem mass spectrometry ion-trap technique for the simultaneous determination of thirteen anticoagulant rodenticides, drugs, or natural products.

    PubMed

    Fourel, Isabelle; Hugnet, Christophe; Goy-Thollot, Isabelle; Berny, Philippe

    2010-03-01

    The purpose of this study was to develop and validate a liquid chromatography-tandem mass spectrometry method for the identification and quantification of anticoagulant (anti-vitamin K or AVK) compounds, including rodenticides, drugs, and natural products because no published method could be found. The proposed method is based on ion-trap technology with electrospray ionization (ESI) and multiple reaction monitoring (MRM) technique. Each AVK is identified by means of its retention time, precursor ion, and two product ions. Plasma samples are extracted by liquid-liquid partition on Toxi-tube B((R)). The method was validated on dog plasma and gave good results in terms of specificity, linearity, and percent recovery for the 14 AVK tested (warfarin, acenocoumarol, bromadiolone, brodifacoum, chlorophacinone, coumatetralyl, dicoumarol, difenacoum, difethialone, flocoumafen, fluindione, phenindione, and tioclomarol). The limits of detection ranged from 5 to 25 ng/mL. Intraday repeatability was good, but interday repeatability was more variable though still sufficient for our diagnostic purposes. The technique was successfully applied in a series of clinical investigations to demonstrate its applicability in various animal species and gave very high sensitivity and specificity results.

  19. Therapeutic cell encapsulation techniques and applications in diabetes.

    PubMed

    Steele, J A M; Hallé, J-P; Poncelet, D; Neufeld, R J

    2014-04-01

    The encapsulation of therapeutic cells permits the implantation of allogeneic and xenogeneic cells for the regulation of certain physiological processes damaged by the death or senescence of host tissues. The encapsulation of pancreatic cells for the treatment of diabetes is emphasized; however, many of the techniques are applicable to a wide array of mammalian cell applications. The summary of both established and novel encapsulation techniques, clinical trials, and commercial product developments highlights the metered but steady pace of therapeutic cell encapsulation towards implementation.

  20. Classroom Management Through the Application of Behavior Modification Techniques.

    ERIC Educational Resources Information Center

    Ferinden, William E., Jr.

    The primary aim of this book is to bring to the grade school teacher a survey of the most recent techniques and ideas of behavior modification which are applicable to good classroom management. All of the approaches and techniques presented could be of interest to teachers working at all grade levels. Since research has shown that the systematic…

  1. [Application of molecular biological techniques in Taenia identification].

    PubMed

    Li, Yan; Liu, Hang; Yang, Yi-Mei

    2011-10-01

    The traditional identification of Taenia spp. based on morphological features of adult and cysticercus has difficulties in identifying the morphologically similar species. The recent development of molecular techniques provides more scientific ways for distinguishing Taenia species. This paper summarizes the application of molecular biological techniques in the identification of Taenia, such as analysis of DNA sequence, PCR-RFLP and LAMP.

  2. Diffusion weighted imaging: Technique and applications

    PubMed Central

    Baliyan, Vinit; Das, Chandan J; Sharma, Raju; Gupta, Arun Kumar

    2016-01-01

    Diffusion weighted imaging (DWI) is a method of signal contrast generation based on the differences in Brownian motion. DWI is a method to evaluate the molecular function and micro-architecture of the human body. DWI signal contrast can be quantified by apparent diffusion coefficient maps and it acts as a tool for treatment response evaluation and assessment of disease progression. Ability to detect and quantify the anisotropy of diffusion leads to a new paradigm called diffusion tensor imaging (DTI). DTI is a tool for assessment of the organs with highly organised fibre structure. DWI forms an integral part of modern state-of-art magnetic resonance imaging and is indispensable in neuroimaging and oncology. DWI is a field that has been undergoing rapid technical evolution and its applications are increasing every day. This review article provides insights in to the evolution of DWI as a new imaging paradigm and provides a summary of current role of DWI in various disease processes. PMID:27721941

  3. Sterilization techniques for biodegradable scaffolds in tissue engineering applications

    PubMed Central

    Dai, Zheng; Ronholm, Jennifer; Tian, Yiping; Sethi, Benu; Cao, Xudong

    2016-01-01

    Biodegradable scaffolds have been extensively studied due to their wide applications in biomaterials and tissue engineering. However, infections associated with in vivo use of these scaffolds by different microbiological contaminants remain to be a significant challenge. This review focuses on different sterilization techniques including heat, chemical, irradiation, and other novel sterilization techniques for various biodegradable scaffolds. Comparisons of these techniques, including their sterilization mechanisms, post-sterilization effects, and sterilization efficiencies, are discussed. PMID:27247758

  4. Application of mass spectrometry-based proteomics techniques for the detection of protein doping in sports.

    PubMed

    Kay, Richard G; Creaser, Colin S

    2010-04-01

    Mass spectrometry-based proteomic approaches have been used to develop methodologies capable of detecting the abuse of protein therapeutics such as recombinant human erythropoietin and recombinant human growth hormone. Existing detection methods use antibody-based approaches that, although effective, suffer from long assay development times and specificity issues. The application of liquid chromatography with tandem mass spectrometry and selected reaction-monitoring-based analysis has demonstrated the ability to detect and quantify existing protein therapeutics in plasma. Furthermore, the multiplexing capability of selected reaction-monitoring analysis has also aided in the detection of multiple downstream biomarkers in a single analysis, requiring less sample than existing immunological techniques. The flexibility of mass spectrometric instrumentation has shown that the technique is capable of detecting the abuse of novel and existing protein therapeutics, and has a vital role in the fight to keep sports drug-free.

  5. Analysis of trihalomethanes in drinking water using headspace-SPME technique with gas chromatography.

    PubMed

    Cho, Deok-Hee; Kong, Sung-Ho; Oh, Seong-Geun

    2003-01-01

    In many drinking water treatment plants, the chlorination process is one of the main techniques used for the disinfection of water. This disinfecting treatment leads to the formation of trihalomethanes (THMs) such as chloroform, dichlorobromomethane, chlorodibromomethane and bromoform. In this study, headspace-solid-phase microextraction (HS-SPME, 85 microm carboxen/polydimethylsiloxane fiber) technique was applied for the analysis of THMs in drinking water. The effects of experimental parameters such as kinds of SPME fiber, the volume ratio of sample to headspace, the addition of salts, magnetic stirring, extraction temperature, extraction time and desorption time on the analysis were investigated. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The results of THMs from the survey of Seongnam (Korea) drinking water samples showed that the highest total trihalomethane and chloroform were 24.03 and 13.34 microg/l, which were well within the Korean drinking water quality standard of 100 and 80 microg/l, respectively.

  6. The Application of Nuclear Techniques to Solid State Devices.

    DTIC Science & Technology

    1980-12-15

    35) as the same technique showed. We then applied the method to clarify the atomic transport in bimetal layer silicide reactions. In these experiments...UNCLASSIFIED NL ’ LEVEWL L* . 4’ -.-- C7..:i I) FINAL TECHNICAL REPORT submitted to --- v OFFICE OF NAVAL RESEARCH on THE APPLICATION OF NUCLEAR TECHNIQUES TO...December 15, 1980,. , ...- 1’J I. Introduction The program "The Application of Nuclear Techniques to Solid State Devices" began on 1 January 1975. It was

  7. 48 CFR 9904.416-50 - Techniques for application.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... actuarial present value of benefits applicable to employees already retired shall be amortized over a period... incurred, the amount of the loss to be recognized currently shall be the present value of the future... ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.416-50 Techniques for application. (a) Measurement...

  8. 48 CFR 9904.420-50 - Techniques for application.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.420-50 Techniques for application. (a) The IR&D and B&P... or applicable Cost Accounting Standards for allocation of indirect costs. (b) The IR&D and B&P cost pools for a segment consist of the project costs plus allocable home office IR&D and B&P costs. (c)...

  9. 48 CFR 9904.420-50 - Techniques for application.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.420-50 Techniques for application. (a) The IR&D and B&P... or applicable Cost Accounting Standards for allocation of indirect costs. (b) The IR&D and B&P cost pools for a segment consist of the project costs plus allocable home office IR&D and B&P costs. (c)...

  10. 48 CFR 9904.420-50 - Techniques for application.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.420-50 Techniques for application. (a) The IR&D and B&P... or applicable Cost Accounting Standards for allocation of indirect costs. (b) The IR&D and B&P cost pools for a segment consist of the project costs plus allocable home office IR&D and B&P costs. (c)...

  11. Topics in Chemical Instrumentation: An Introduction to Supercritical Fluid Chromatography--Part 2. Applications and Future Trends.

    ERIC Educational Resources Information Center

    Palmieri, Margo D.

    1989-01-01

    Discussed are selected application and future trends in supercritical fluid chromatography (SFC). The greatest application for SFC involves those analytes that are difficult to separate using GC or LC methods. Optimum conditions for SFC are examined. Provided are several example chromatograms. (MVL)

  12. Core-shell particles: preparation, fundamentals and applications in high performance liquid chromatography.

    PubMed

    Hayes, Richard; Ahmed, Adham; Edge, Tony; Zhang, Haifei

    2014-08-29

    The challenges in HPLC are fast and efficient separation for a wide range of samples. Fast separation often results in very high operating pressure, which places a huge burden on HPLC instrumentation. In recent years, core-shell silica microspheres (with a solid core and a porous shell, also known as fused-core or superficially porous microspheres) have been widely investigated and used for highly efficient and fast separation with reasonably low pressure for separation of small molecules, large molecules and complex samples. In this review, we firstly show the types of core-shell particles and how they are generally prepared, focusing on the methods used to produce core-shell silica particles for chromatographic applications. The fundamentals are discussed on why core-shell particles can perform better with low back pressure, in terms of van Deemter equation and kinetic plots. The core-shell particles are compared with totally porous silica particles and also monolithic columns. The use of columns packed with core-shell particles in different types of liquid chromatography is then discussed, followed by illustrating example applications of such columns for separation of various types of samples. The review is completed with conclusion and a brief perspective on future development of core-shell particles in chromatography.

  13. High-performance liquid chromatography as a technique to determine protein adsorption onto hydrophilic/hydrophobic surfaces.

    PubMed

    Huang, Tongtong; Anselme, Karine; Sarrailh, Segolene; Ponche, Arnaud

    2016-01-30

    The purpose of this study is to evaluate the potential of simple high performance liquid chromatography (HPLC) setup for quantification of adsorbed proteins on various type of plane substrates with limited area (<3 cm(2)). Protein quantification was investigated with a liquid chromatography chain equipped with a size exclusion column or a reversed-phase column. By evaluating the validation of the method according to guidelines of the International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH), all the results obtained by HPLC were reliable. By simple adsorption test at the contact of hydrophilic (glass) and hydrophobic (polydimethylsiloxane: PDMS) surfaces, kinetics of adsorption were determined and amounts of adsorbed bovine serum albumin, myoglobin and lysozyme were obtained: as expected for each protein, the amount adsorbed at the plateau on glass (between 0.15 μg/cm(2) and 0.4 μg/cm(2)) is lower than for hydrophobic PDMS surfaces (between 0.45 μg/cm(2) and 0.8 μg/cm(2)). These results were consistent with bicinchoninic acid protein determination. According to ICH guidelines, both Reversed Phase and Size Exclusion HPLC can be validated for quantification of adsorbed protein. However, we consider the size exclusion approach more interesting in this field because additional informations can be obtained for aggregative proteins. Indeed, monomer, dimer and oligomer of bovine serum albumin (BSA) were observed in the chromatogram. On increasing the temperature, we found a decrease of peak intensity of bovine serum albumin as well as the fraction of dimer and oligomer after contact with PDMS and glass surface. As the surface can act as a denaturation parameter, these informations can have a huge impact on the elucidation of the interfacial behavior of protein and in particular for aggregation processes in pharmaceutical applications.

  14. Application of molecular techniques on heterotrophic hydrogen production research.

    PubMed

    Li, R Y; Zhang, T; Fang, H H P

    2011-09-01

    This paper reviews the application of molecular techniques in heterotrophic hydrogen production studies. Commonly used molecular techniques are introduced briefly first, including cloning-sequencing after polymerase chain reaction (PCR), denaturing gradient gel electrophoresis (DGGE), terminal-restriction fragment length polymorphism (T-RFLP), fluorescence in situ hybridization (FISH) and quantitative real-time PCR. Application of the molecular techniques in heterotrophic hydrogen production studies are discussed in details, focusing on identification of new isolates for hydrogen production, characterization of microbial compositions in bioreactors, monitoring microbial diversity variation, visualization of microbial distribution in hydrogen-producing granular sludge, and quantification of various microbial populations. Some significant findings in recent hydrogen production studies with the application of molecular techniques are discussed, followed by a research outlook of the heterotrophic biohydrogen field.

  15. Millimeter-wave/THz FMCW radar techniques for sensing applications

    NASA Astrophysics Data System (ADS)

    Mirando, D. Amal; Higgins, Michael D.; Wang, Fenggui; Petkie, Douglas T.

    2016-10-01

    Millimeter-wave and terahertz continuous-wave radar systems have been used to measure physiological signatures for biometric applications and for a variety of non-destructive evaluation applications, such as the detection of defects in materials. Sensing strategies for the simplest homodyne systems, such as a Michelson Interferometer, can be enhanced by using Frequency Modulated Continuous Wave (FMCW) techniques. This allows multiple objects or surfaces to be range resolved while monitoring the phase of the signal in a particular range bin. We will discuss the latest developments in several studies aimed at demonstrating how FMCW techniques can enhance mmW/THz sensing applications.

  16. A novel Fast Gas Chromatography based technique for higher time resolution measurements of speciated monoterpenes in air

    NASA Astrophysics Data System (ADS)

    Jones, C. E.; Kato, S.; Nakashima, Y.; Kajii, Y.

    2013-12-01

    Biogenic emissions supply the largest fraction of non-methane volatile organic compounds (VOC) from the biosphere to the atmospheric boundary layer, and typically comprise a complex mixture of reactive terpenes. Due to this chemical complexity, achieving comprehensive measurements of biogenic VOC (BVOC) in air within a satisfactory time resolution is analytically challenging. To address this, we have developed a novel, fully automated Fast Gas Chromatography (Fast-GC) based technique to provide higher time resolution monitoring of monoterpenes (and selected other C9-C15 terpenes) during plant emission studies and in ambient air. To our knowledge, this is the first study to apply a Fast-GC based separation technique to achieve quantification of terpenes in air. Three chromatography methods have been developed for atmospheric terpene analysis under different sampling scenarios. Each method facilitates chromatographic separation of selected BVOC within a significantly reduced analysis time compared to conventional GC methods, whilst maintaining the ability to quantify individual monoterpene structural isomers. Using this approach, the C10-C15 BVOC composition of single plant emissions may be characterised within a ~ 14 min analysis time. Moreover, in situ quantification of 12 monoterpenes in unpolluted ambient air may be achieved within an ~ 11 min chromatographic separation time (increasing to ~ 19 min when simultaneous quantification of multiple oxygenated C9-C10 terpenoids is required, and/or when concentrations of anthropogenic VOC are significant). This corresponds to a two- to fivefold increase in measurement frequency compared to conventional GC methods. Here we outline the technical details and analytical capability of this chromatographic approach, and present the first in situ Fast-GC observations of 6 monoterpenes and the oxygenated BVOC linalool in ambient air. During this field deployment within a suburban forest ~ 30 km west of central Tokyo, Japan, the

  17. Exploring the possibilities of cryogenic cooling in liquid chromatography for biological applications: a proof of principle.

    PubMed

    Eghbali, Hamed; Sandra, Koen; Tienpont, Bart; Eeltink, Sebastiaan; Sandra, Pat; Desmet, Gert

    2012-02-21

    The possibilities to use cryogenic cooling to trap components in liquid chromatography was investigated. In a first step, van 't Hoff plots were measured with a reversed-phase column using the temperature control unit of a conventional high performance liquid chromatography (HPLC) system to gain insight in the retention behavior of proteins at low temperatures. It was estimated that retention factors in the range of k = 10(4) could be achieved at T = -20 °C for lysozyme, indicating that temperature is a usable parameter to trap components in LC. In a next step, trapping experiments were carried out on a nano-LC system, equipped with a UV-detector, using a commercial reversed-phase column. An in-house built setup, allowing cooling of a segment of the column down to temperatures below T = -20 °C, was used to trap components. Experiments were conducted under isocratic and gradient conditions with methanol as organic solvent. It is demonstrated that, by thermally trapping and elution of components, an enhanced S/N ratio and decreased peak widths can be obtained. At the same time, a significant increase in pressure drop occurs during the cooling process. Limitations and benefits of the technique are further discussed.

  18. Aspects of matrix effects in applications of liquid chromatography-mass spectrometry to forensic and clinical toxicology--a review.

    PubMed

    Peters, Frank T; Remane, Daniela

    2012-06-01

    In the last decade, liquid chromatography coupled to (tandem) mass spectrometry (LC-MS(-MS)) has become a versatile technique with many routine applications in clinical and forensic toxicology. However, it is well-known that ionization in LC-MS(-MS) is prone to so-called matrix effects, i.e., alteration in response due to the presence of co-eluting compounds that may increase (ion enhancement) or reduce (ion suppression) ionization of the analyte. Since the first reports on such matrix effects, numerous papers have been published on this matter and the subject has been reviewed several times. However, none of the existing reviews has specifically addressed aspects of matrix effects of particular interest and relevance to clinical and forensic toxicology, for example matrix effects in methods for multi-analyte or systematic toxicological analysis or matrix effects in (alternative) matrices almost exclusively analyzed in clinical and forensic toxicology, for example meconium, hair, oral fluid, or decomposed samples in postmortem toxicology. This review article will therefore focus on these issues, critically discussing experiments and results of matrix effects in LC-MS(-MS) applications in clinical and forensic toxicology. Moreover, it provides guidance on performance of studies on matrix effects in LC-MS(-MS) procedures in systematic toxicological analysis and postmortem toxicology.

  19. High-Performance Liquid Chromatography-Mass Spectrometry.

    ERIC Educational Resources Information Center

    Vestal, Marvin L.

    1984-01-01

    Reviews techniques for online coupling of high-performance liquid chromatography with mass spectrometry, emphasizing those suitable for application to nonvolatile samples. Also summarizes the present status, strengths, and weaknesses of various techniques and discusses potential applications of recently developed techniques for combined liquid…

  20. Analysis of biogenic carbonyl compounds in rainwater by stir bar sorptive extraction technique with chemical derivatization and gas chromatography-mass spectrometry.

    PubMed

    Pang, Xiaobing; Lewis, Alastair C; Shaw, Marvin D

    2017-02-01

    Stir bar sorptive extraction is a powerful technique for the extraction and analysis of organic compounds in aqueous matrices. Carbonyl compounds are ubiquitous components in rainwater, however, it is a major challenge to accurately identify and sensitively quantify carbonyls from rainwater due to the complex matrix. A stir bar sorptive extraction technique was developed to efficiently extract carbonyls from aqueous samples following chemical derivatization by O-(2,3,4,5,6-pentafluorobenzyl) hydroxylamine hydrochloride. Several commercial stir bars in two sizes were used to simultaneously measure 29 carbonyls in aqueous samples with detection by gas chromatography with mass spectrometry. A 100 mL aqueous sample was extracted by stir bars and the analytes on stir bars were desorbed into a 2 mL solvent solution in an ultrasonic bath. The preconcentration Coefficient for different carbonyls varied between 30 and 45 times. The limits of detection of stir bar sorptive extraction with gas chromatography mass spectrometry for carbonyls (10-30 ng/L) were improved by ten times compared with other methods such as gas chromatography with electron capture detection and stir bar sorptive extraction with high-performance liquid chromatography and mass spectrometry. The technique was used to determine carbonyls in rainwater samples collected in York, UK, and 20 carbonyl species were quantified including glyoxal, methylglyoxal, isobutenal, 2-hydroxy ethanal.

  1. Levels of phytosterol oxides in enriched and nonenriched spreads: application of a thin-layer chromatography-gas chromatography methodology.

    PubMed

    Conchillo, Ana; Cercaci, Luisito; Ansorena, Diana; Rodriguez-Estrada, Maria Teresa; Lercker, Giovanni; Astiasarán, Iciar

    2005-10-05

    The content of phytosterol oxidation products (POPs) in enriched and nonenriched commercial spreads was evaluated by thin-layer chromatography-gas chromatography (TLC-GC). Oxides of beta-sitosterol, campesterol, and stigmasterol were produced by thermo-oxidation (7-hydroxy, 7-keto, and epoxy derivatives) and chemical synthesis (triol derivatives), which were then separated and identified by TLC-GC. Their identification was further confirmed by GC-mass spectrometry (GC-MS). The total amounts of phytosterols found were 6.07 and 0.33 g/100 g of sample in phytosterol-enriched and nonenriched spread, respectively, whereas the total POPs contents were 45.60 and 13.31 mg/kg of sample in the enriched and nonenriched products. The main POPs found were the 7-keto derivatives of all phytosterols analyzed; 7-ketositosterol was the most abundant one (14.96 and 5.93 mg/kg of sample in phytosterol-enriched and nonenriched spread). No beta-epoxy and triol derivatives were detected in both types of samples. The enriched spread presented a lower phytosterol oxidation rate (0.07%) than the nonenriched one (0.41%).

  2. Achiral and Chiral Separations Using Micellar Electrokinetic Chromatography, Polyelectrolyte Multilayer Coatings, and Mixed Mode Separation Techniques with Molecular Micelles

    PubMed Central

    Luces, Candace A.; Warner, Isiah M.

    2014-01-01

    Mixed mode separation using a combination of micellar electrokinetic chromatography (MEKC) and polyelectrolyte multilayer (PEM) coatings is herein reported for the separation of achiral and chiral analytes. Many analytes are difficult to separate by MEKC and PEM coatings alone. Therefore, the implementation of a mixed mode separation provides several advantages for overcoming the limitations of these well-established methods. In this study, it was observed that achiral separations using MEKC and PEM coatings individually resulted in partial resolution of 8 very similar aryl ketones when the molecular micelle (sodium poly(N-undecanoyl-l-glycinate) (poly-SUG)) concentration was varied from 0.25% – 1.00% (w/v) and the bilayer number varied from 2 – 4. However, when mixed mode separation was introduced, baseline resolution was achieved for all 8 analytes. In the case of chiral separations, temazepam, aminoglutethimide, benzoin, benzoin methyl ether and coumachlor were separated using the three separation techniques. For chiral separations, the chiral molecular micelle, sodium poly(N-undecanoyl-l-leucylvalinate) (poly-l-SULV), was employed at concentrations of 0.25–1.50% (w/v) for both MEKC and PEM coatings. Overall, the results revealed partial separation with MEKC and PEM coatings individually. However, mixed mode separation enabled baseline separation of each chiral mixture. The separation of achiral and chiral compounds from different compound classes demonstrates the versatility of this mixed mode approach. PMID:20155738

  3. Quantification of 4-Methylimidazole in soft drinks, sauces and vinegars of Greek market using two liquid chromatography techniques.

    PubMed

    Tzatzarakis, Manolis N; Vakonaki, Elena; Moti, Sofia; Alegakis, Athanasios; Tsitsimpikou, Christina; Tsakiris, Ioannis; Goumenou, Marina; Nosyrev, Alexander E; Rizos, Apostolos K; Tsatsakis, Aristidis M

    2017-03-19

    The substance 4-methylimidazole (4-MEI) has raised several concerns regarding its toxicity to humans, although no harmonized classification has yet been decided. The regulatory limits for food products set by various authorities in Europe and the USA differ considerably. The purpose of the present study is to compare two liquid chromatography techniques in order to determine the levels of 4-MEI in food products from the Greek market and roughly estimate the possible exposure and relevant health risk for the consumers. A total of thirty-four samples (soft drinks, beers, balsamic vinegars, energy drinks and sauces) were collected and analyzed. The quality parameters for both analytical methodologies (linearity, accuracy, inter day precision, recovery) are presented. No detectable levels of 4-MEI are found in beers and soft drink samples, other than cola type. On the other hand, 4-MEI was detected in all cola type soft drinks (15.8-477.0 ng/ml), energy drinks (57.1%, 6.6-22.5 ng/ml) and vinegar samples (66.7%, 9.7-3034.7 ng/ml), while only one of the sauce samples was found to have a detectable level of 17.5 ng/ml 4-MEI.

  4. Glycopeptide Site Heterogeneity and Structural Diversity Determined by Combined Lectin Affinity Chromatography/IMS/CID/MS Techniques

    NASA Astrophysics Data System (ADS)

    Zhu, Feifei; Trinidad, Jonathan C.; Clemmer, David E.

    2015-07-01

    Glycopeptides from a tryptic digest of chicken ovomucoid were enriched using a simplified lectin affinity chromatography (LAC) platform, and characterized by high-resolution mass spectrometry (MS) as well as ion mobility spectrometry (IMS)-MS. The LAC platform effectively enriched the glycoproteome, from which a total of 117 glycopeptides containing 27 glycan forms were identified for this protein. IMS-MS analysis revealed a high degree of glycopeptide site heterogeneity. Comparison of the IMS distributions of the glycopeptides from different charge states reveals that higher charge states allow more structures to be resolved. Presumably the repulsive interactions between charged sites lead to more open configurations, which are more readily separated compared with the more compact, lower charge state forms of the same groups of species. Combining IMS with collision induced dissociation (CID) made it possible to determine the presence of isomeric glycans and to reconstruct their IMS profiles. This study illustrates a workflow involving hybrid techniques for determining glycopeptide site heterogeneity and evaluating structural diversity of glycans and glycopeptides.

  5. Characterisation and discrimination of various types of lac resin using gas chromatography mass spectrometry techniques with quaternary ammonium reagents.

    PubMed

    Sutherland, K; del Río, J C

    2014-04-18

    A variety of lac resin samples obtained from artists' suppliers, industrial manufacturers, and museum collections were analysed using gas chromatography mass spectrometry (GCMS) and reactive pyrolysis GCMS with quaternary ammonium reagents. These techniques allowed a detailed chemical characterisation of microgram-sized samples, based on the detection and identification of derivatives of the hydroxy aliphatic and cyclic (sesquiterpene) acids that compose the resin. Differences in composition could be related to the nature of the resin, e.g. wax-containing (unrefined), bleached, or aged samples. Furthermore, differences in the relative abundances of aliphatic hydroxyacids appear to be associated with the biological source of the resin. The diagnostic value of newly characterised lac components, including 8-hydroxyacids, is discussed here for the first time. Identification of derivatised components was aided by AMDIS deconvolution software, and discrimination of samples was enhanced by statistical evaluation of data using principal component analysis. The robustness of the analyses, together with the minimal sample size required, make these very powerful approaches for the characterisation of lac resin in museum objects. The value of such analyses for enhancing the understanding of museum collections is illustrated by two case studies of objects in the collection of the Philadelphia Museum of Art: a restorer's varnish on a painting by Luca Signorelli, and a pictorial inlay in an early nineteenth-century High Chest by George Dyer.

  6. Inter-comparison of laser photoacoustic spectroscopy and gas chromatography techniques for measurements of ethene in the atmosphere.

    PubMed

    Kuster, William C; Harren, Frans J M; de Gouw, Joost A

    2005-06-15

    Laser photoacoustic spectroscopy (LPAS) is highly suitable for the detection of ethene in air due to the overlap between its strongest absorption lines and the wavelengths accessible by high-powered CO2 lasers. Here, we test the ability of LPAS to measure ethene in ambient air by comparing the measurements in urban air with those from a gas chromatography flame-ionization detection (GC-FID) instrument. Over the course of several days, we obtained quantitative agreement between the two measurements. Over this period, the LPAS instrument had a positive offset of 330 +/- 140 pptv (parts-per-trillion by volume) relative to the GC-FID instrument, possibly caused by interference from other species. The detection limit of the LPAS instrument is currently estimated around 1 ppbv and is limited by this offset and the statistical noise in the data. We conclude that LPAS has the potential to provide fast-response measurements of ethene in the atmosphere, with significant advantages over existing techniques when measuring from moving platforms and in the vicinity of emission sources.

  7. Current Applications of Liquid Chromatography/Mass Spectrometry in Pharmaceutical Discovery After a Decade of Innovation

    NASA Astrophysics Data System (ADS)

    Ackermann, Bradley L.; Berna, Michael J.; Eckstein, James A.; Ott, Lee W.; Chaudhary, Ajai K.

    2008-07-01

    Current drug discovery involves a highly iterative process pertaining to three core disciplines: biology, chemistry, and drug disposition. For most pharmaceutical companies the path to a drug candidate comprises similar stages: target identification, biological screening, lead generation, lead optimization, and candidate selection. Over the past decade, the overall efficiency of drug discovery has been greatly improved by a single instrumental technique, liquid chromatography/mass spectrometry (LC/MS). Transformed by the commercial introduction of the atmospheric pressure ionization interface in the mid-1990s, LC/MS has expanded into almost every area of drug discovery. In many cases, drug discovery workflow has been changed owing to vastly improved efficiency. This review examines recent trends for these three core disciplines and presents seminal examples where LC/MS has altered the current approach to drug discovery.

  8. Recent trends in electrospinning of polymer nanofibers and their applications in ultra thin layer chromatography.

    PubMed

    Moheman, Abdul; Alam, Mohammad Sarwar; Mohammad, Ali

    2016-03-01

    Fabrication of polymer derived electrospun nanofibers by electrospinning as chromatographic sorbent bed for ultra-thin layer chromatography (UTLC) is a very demanding topic in analytical chemistry. This review presents an overview of recent development in the fabrication of polymer derived electrospun nanofibers and their applications to design UTLC plates as stationary phases for on-plate identification and separation of analytes from their mixture solutions. It has been reported that electrospun fiber based stationary phases in UTLC have enhanced separation efficiency to provide separation of analyte mixture in a shorter development time than those of traditional particle-based TLC stationary phases. In addition, electrospun UTLC is cost effective and can be modified for obtaining different surface selectivities by changing the polymer materials to electrospun devices. Electrospun UTLC plates are not available commercially till date and efforts are being rendered for their commercialization. The morphology and diameter of electrospun nanofibers are highly dependent on several parameters such as type of polymer, polymer molecular weight, solvent, viscosity, conductivity, surface tension, applied voltage, collector distance and flow rate of the polymer solution during electrospinning process. Among the aforementioned parameters, solution viscosity is an important parameter which is mainly influenced by polymer concentration. This review provides evidence for the fabrication of UTLC plates containing electrospun polymer nanofibers. Furthermore, the future prospects related to electrospinning and its application in obtaining of different types of electrospun nanofibers are discussed. The present communication is aimed to review the work which appeared during 2009-2014 on the application of polymer derived electrospun nanofibers in ultra thin layer chromatography.

  9. Multiple inert gas elimination technique by micropore membrane inlet mass spectrometry--a comparison with reference gas chromatography.

    PubMed

    Kretzschmar, Moritz; Schilling, Thomas; Vogt, Andreas; Rothen, Hans Ulrich; Borges, João Batista; Hachenberg, Thomas; Larsson, Anders; Baumgardner, James E; Hedenstierna, Göran

    2013-10-15

    The mismatching of alveolar ventilation and perfusion (VA/Q) is the major determinant of impaired gas exchange. The gold standard for measuring VA/Q distributions is based on measurements of the elimination and retention of infused inert gases. Conventional multiple inert gas elimination technique (MIGET) uses gas chromatography (GC) to measure the inert gas partial pressures, which requires tonometry of blood samples with a gas that can then be injected into the chromatograph. The method is laborious and requires meticulous care. A new technique based on micropore membrane inlet mass spectrometry (MMIMS) facilitates the handling of blood and gas samples and provides nearly real-time analysis. In this study we compared MIGET by GC and MMIMS in 10 piglets: 1) 3 with healthy lungs; 2) 4 with oleic acid injury; and 3) 3 with isolated left lower lobe ventilation. The different protocols ensured a large range of normal and abnormal VA/Q distributions. Eight inert gases (SF6, krypton, ethane, cyclopropane, desflurane, enflurane, diethyl ether, and acetone) were infused; six of these gases were measured with MMIMS, and six were measured with GC. We found close agreement of retention and excretion of the gases and the constructed VA/Q distributions between GC and MMIMS, and predicted PaO2 from both methods compared well with measured PaO2. VA/Q by GC produced more widely dispersed modes than MMIMS, explained in part by differences in the algorithms used to calculate VA/Q distributions. In conclusion, MMIMS enables faster measurement of VA/Q, is less demanding than GC, and produces comparable results.

  10. Preparation and characterization of alkyl methacrylate-based monolithic columns for capillary gas chromatography applications.

    PubMed

    Yusuf, Kareem; Aqel, Ahmad; A L Othman, Zeid; Badjah-Hadj-Ahmed, Ahmed Yacine

    2013-08-02

    Gas chromatography (GC) is considered the least common application of both polymer and silica-based monolithic columns. This study describes the fabrication of alkyl methacrylate monolithic materials for use as stationary phases in capillary gas chromatography. Following the deactivation of the capillary surface with 3-(trimethoxysilyl)propyl methacrylate (TMSM), the monoliths were formed by the co-polymerization of either hexyl methacrylate (HMA) or lauryl methacrylate (LMA) with different percentage of ethylene glycol dimethacrylate (EDMA) in presence of an initiator (azobisisobutyronitrile, AIBN) and a mixture of porogens include 1-propanol, 1,4-butanediol and water. The monoliths were prepared in 500mm length capillaries possessing inner diameters of 250μm. The efficiencies of the monolithic columns for low molecular weight compounds significantly improved as the percentage of crosslinker was increased, because of the greater proportion of pores less than 50nm. The columns containing lower percentages of crosslinker were able to rapidly separate a series of 8 alkane members in 0.7min, but the separation was less efficient for the light alkanes. Columns prepared with the lauryl methacrylate monomer yielded a different morphology for the monolith-interconnected channels. The channels were more branched, which increased the separation time, and unlike the other columns, allowed for temperature programming.

  11. Applications of monolithic solid-phase extraction in chromatography-based clinical chemistry assays.

    PubMed

    Bunch, Dustin R; Wang, Sihe

    2013-04-01

    Complex matrices, for example urine, serum, plasma, and whole blood, which are common in clinical chemistry testing, contain many non-analyte compounds that can interfere with either detection or in-source ionization in chromatography-based assays. To overcome this problem, analytes are extracted by protein precipitation, solid-phase extraction (SPE), and liquid-liquid extraction. With correct chemistry and well controlled material SPE may furnish clean specimens with consistent performance. Traditionally, SPE has been performed with particle-based adsorbents, but monolithic SPE is attracting increasing interest of clinical laboratories. Monoliths, solid pieces of stationary phase, have bimodal structures consisting of macropores, which enable passage of solvent, and mesopores, in which analytes are separated. This structure results in low back-pressure with separation capabilities similar to those of particle-based adsorbents. Monoliths also enable increased sample throughput, reduced solvent use, varied support formats, and/or automation. However, many of these monoliths are not commercially available. In this review, application of monoliths to purification of samples from humans before chromatography-based assays will be critically reviewed.

  12. Videogrammetric Model Deformation Measurement Technique for Wind Tunnel Applications

    NASA Technical Reports Server (NTRS)

    Barrows, Danny A.

    2006-01-01

    Videogrammetric measurement technique developments at NASA Langley were driven largely by the need to quantify model deformation at the National Transonic Facility (NTF). This paper summarizes recent wind tunnel applications and issues at the NTF and other NASA Langley facilities including the Transonic Dynamics Tunnel, 31-Inch Mach 10 Tunnel, 8-Ft high Temperature Tunnel, and the 20-Ft Vertical Spin Tunnel. In addition, several adaptations of wind tunnel techniques to non-wind tunnel applications are summarized. These applications include wing deformation measurements on vehicles in flight, determining aerodynamic loads based on optical elastic deformation measurements, measurements on ultra-lightweight and inflatable space structures, and the use of an object-to-image plane scaling technique to support NASA s Space Exploration program.

  13. Bioanalytical Applications of Fluorescence Line-Narrowing and Non-Line-Narrowing Spectroscopy Interfaced with Capillary Electrophoresis and High-Performance Liquid Chromatography

    SciTech Connect

    Roberts, Kenneth Paul

    2001-01-01

    Capillary electrophoresis (CE) and high-performance liquid chromatography (HPLC) are widely used analytical separation techniques with many applications in chemical, biochemical, and biomedical sciences. Conventional analyte identification in these techniques is based on retention/migration times of standards; requiring a high degree of reproducibility, availability of reliable standards, and absence of coelution. From this, several new information-rich detection methods (also known as hyphenated techniques) are being explored that would be capable of providing unambiguous on-line identification of separating analytes in CE and HPLC. As further discussed, a number of such on-line detection methods have shown considerable success, including Raman, nuclear magnetic resonance (NMR), mass spectrometry (MS), and fluorescence line-narrowing spectroscopy (FLNS). In this thesis, the feasibility and potential of combining the highly sensitive and selective laser-based detection method of FLNS with analytical separation techniques are discussed and presented. A summary of previously demonstrated FLNS detection interfaced with chromatography and electrophoresis is given, and recent results from on-line FLNS detection in CE (CE-FLNS), and the new combination of HPLC-FLNS, are shown.

  14. Application of Material Characterization Techniques to Electrical Forensic Analysis

    SciTech Connect

    Mills, T.D.

    2003-03-11

    The application of forensic science techniques to electrical equipment failure investigation has not been widely documented in the engineering world. This paper is intended to share an example of using material characterization techniques to support an initial cause determination of an electrical component failure event. The resulting conclusion supported the initial cause determination and ruled out the possibility of design deficiencies. Thus, the qualification testing of the equipment was allowed to continue to successful completion.

  15. Sample Processing technique onboard ExoMars (MOMA) to analyze organic compounds by Gas Chromatography-Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Buch, A.; Freissinet, C.; Sternberg, R.; Szopa, C.; Coll, P. J.; Brault, A.; Pinnick, V.; Siljeström, S.; Raulin, F.; Steininger, H.; Goesmann, F.; MOMA Team

    2011-12-01

    With the aim of separating and detecting organic compounds from Martian soil onboard the Mars Organic Molecule Analyzer (MOMA) experiment of the ExoMars 2018 upcoming joint ESA/NASA mission, we have developed three different space compatible sample preparation techniques compatible with space missions, able to extract and analyze by GC-MS a wide range of volatile and refractory compounds, including chirality analysis. Then, a sample processing utilizing three derivatization/extraction reactions has been carried out. The first reaction is based on a silyl reagent N-Methyl-N- (Tert-Butyldimethylsilyl)trifluoroacetamide (MTBSTFA) [1], the second one, N,N-Dimethylformamide Dimethylacetal (DMF-DMA) [2,3] is dedicated to the chirality detection and the third one is a thermochemolysis based on the use of tetramethylammoniumhydroxide (TMAH). The sample processing system is performed in an oven, dedicated to the MOMA experiment containing the solid sample (50-100mg). The internal temperature of the oven ranges from 20 to 900 °C. The extraction step is achieved by using thermodesorption in the range of 100 to 300°C for 5 to 20 min. Then, the chemical derivatization of the extracted compounds is performed directly on the soil sample by using a derivatyization capsule which contains a mixture of MTBSTFA-DMF or DMF-DMA solution when enantiomeric separation is required. By decreasing the polarity of the targeted molecules, this step allows their volatilization at a temperature below 250°C without any thermal degradation. Once derivatized, the volatile target molecules are trapped in a chemical trap and promptly desorbed into the gas chromatograph coupled to a mass spectrometer. Thermochemolysis is directly performed in the oven at 400°C during 5 min with a 25% (w/w) methanol solution of tetramethylammonium hydroxide (TMAH). Then, pyrolysis in the presence of TMAH allows both an efficient cleavage of polar bonds and the subsequent methylation of COOH, OH and NH2 groups, hence

  16. Review and classification of variability analysis techniques with clinical applications.

    PubMed

    Bravi, Andrea; Longtin, André; Seely, Andrew J E

    2011-10-10

    Analysis of patterns of variation of time-series, termed variability analysis, represents a rapidly evolving discipline with increasing applications in different fields of science. In medicine and in particular critical care, efforts have focussed on evaluating the clinical utility of variability. However, the growth and complexity of techniques applicable to this field have made interpretation and understanding of variability more challenging. Our objective is to provide an updated review of variability analysis techniques suitable for clinical applications. We review more than 70 variability techniques, providing for each technique a brief description of the underlying theory and assumptions, together with a summary of clinical applications. We propose a revised classification for the domains of variability techniques, which include statistical, geometric, energetic, informational, and invariant. We discuss the process of calculation, often necessitating a mathematical transform of the time-series. Our aims are to summarize a broad literature, promote a shared vocabulary that would improve the exchange of ideas, and the analyses of the results between different studies. We conclude with challenges for the evolving science of variability analysis.

  17. Review and classification of variability analysis techniques with clinical applications

    PubMed Central

    2011-01-01

    Analysis of patterns of variation of time-series, termed variability analysis, represents a rapidly evolving discipline with increasing applications in different fields of science. In medicine and in particular critical care, efforts have focussed on evaluating the clinical utility of variability. However, the growth and complexity of techniques applicable to this field have made interpretation and understanding of variability more challenging. Our objective is to provide an updated review of variability analysis techniques suitable for clinical applications. We review more than 70 variability techniques, providing for each technique a brief description of the underlying theory and assumptions, together with a summary of clinical applications. We propose a revised classification for the domains of variability techniques, which include statistical, geometric, energetic, informational, and invariant. We discuss the process of calculation, often necessitating a mathematical transform of the time-series. Our aims are to summarize a broad literature, promote a shared vocabulary that would improve the exchange of ideas, and the analyses of the results between different studies. We conclude with challenges for the evolving science of variability analysis. PMID:21985357

  18. Phytochemical and morphological characterization of hop (Humulus lupulus L.) cones over five developmental stages using high performance liquid chromatography coupled to time-of-flight mass spectrometry, ultrahigh performance liquid chromatography photodiode array detection, and light microscopy techniques.

    PubMed

    Kavalier, Adam R; Litt, Amy; Ma, Chunhui; Pitra, Nicholi J; Coles, Mark C; Kennelly, Edward J; Matthews, Paul D

    2011-05-11

    Hop (Humulus lupulus L.) inflorescences, commonly known as "hop cones", are prized for their terpenophenolic contents, used in beer production and, more recently, in biomedical applications. In this study we investigated morphological and phytochemical characteristics of hop cones over five developmental stages, using liquid chromatography coupled to time-of-flight mass spectrometry (LC-TOF-MS), and ultrahigh performance liquid chromatography photodiode array detection (UHPLC-PDA) methods to quantitate 21 polyphenolics and seven terpenophenolics. Additionally, we used light microscopy to correlate phytochemical quantities with changes in the morphology of the cones. Significant increases in terpenophenolics, concomitant with glandular trichome development and associated gross morphological changes, were mapped over development to fluctuations in contents of polyphenolic constituents and their metabolic precursor compounds. The methods reported here can be used for targeted metabolic profiling of flavonoids, phenolic acids, and terpenophenolics in hops, and are applicable to quantitation in other crops.

  19. Renaissance of Aliphatic Polycarbonates: New Techniques and Biomedical Applications

    PubMed Central

    Xu, Jianwen; Feng, Ellva; Song, Jie

    2014-01-01

    Aliphatic polycarbonates were discovered a long time ago, with their conventional applications mostly limited to low molecular weight oligomeric intermediates for copolymerization with other polymers. Recent developments in polymerization techniques have overcome the difficulty in preparing high molecular weight aliphatic polycarbonates. These in turn, along with new functional monomers, have enabled the preparation of a wide range of aliphatic polycarbonates with diverse chemical compositions and structures. This review summarizes the latest polymerization techniques for preparing well-defined functional aliphatic polycarbonates, as well as the new applications of those aliphatic polycarbonates, esecially in the biomedical field. PMID:24994939

  20. Edible holography: the application of holographic techniques to food processing

    NASA Astrophysics Data System (ADS)

    Begleiter, Eric

    1991-07-01

    Reports on current research efforts in the application of holographic techniques to food processing. Through a simple and inexpensive production process, diffractive and holographic effects of color, depth, and motion can be transferred to edible products. Processes are discussed which can provide a competitive advantage to the marketing of a diverse group of sugar and non-sugar-based consumable products, i.e. candies, chocolates, lollipops, snacks, cereals and pharmaceuticals. Techniques, applications, and products are investigated involving the shift from a chemical to a physical basis for the production of food coloring and decorating.

  1. Direct and comprehensive analysis of ginsenosides and diterpene alkaloids in Shenfu injection by combinatory liquid chromatography-mass spectrometric techniques.

    PubMed

    Yang, Hua; Liu, Lei; Gao, Wen; Liu, Ke; Qi, Lian-Wen; Li, Ping

    2014-04-01

    Shenfu injection (SFI) is a widely used Chinese herbal formulation for cardiac diseases prepared from red ginseng and processed aconite root. Clinical observations and pharmacological effects on SFI have been well investigated. Chemical analysis and quality control studies of this formulation, however, are relatively limited, especially regarding toxic aconite alkaloids. In this work, a high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF MS) method was applied to comprehensive analysis of constituents in SFI. Highly sensitive MS allows direct analysis of injections without additional sample pretreatment required. Using diagnostic ions and fragmentation rules, we identified 23 trace diterpene alkaloids, nineteen ginseng saponins, one panaxytriol, and one 5-hydroxymethylfurfural in SFI. A LC-MS method with selected ion monitoring was then used to quantify 24 major alkaloids and ginsenosides. The method was validated in terms of linearity, accuracy and precision. Especially, the limits of quantification were low to 0.4-18ng/mL for diterpene alkaloids. The total concentrations of saponins and alkaloids were about 676-742μg/mL and 3-7μg/mL in five batches of SFI samples, respectively. Finally, cosine ratio and euclidean distance were introduced to evaluate the batch-to-batch reproducibility of SFI samples, and the results demonstrated high quality consistency. Global identification and quantification of complex constituents based on LC-MS promises wide applications in quality control and batch monitoring for herbal products.

  2. Application of thermoluminescence technique to identify radiation processed foods

    NASA Astrophysics Data System (ADS)

    Kiyak, N.

    1995-02-01

    Research studies reported by various authors have shown that a few methods one of which is thermoluminescence technique- may be suitable for identification of some certain irradiated spicies and food containing bones. This study is an application of the thermoluminescence technique for identifying the irradiated samples. The investigation was carried out on different types of foodstuffs such as onions, potatoes and kiwi. Measurements show that the technique can be applied as a reliable method to distinguish the irradiated food products from non-irradiated ones. The results demonstrate also that it is possible to use this method for determining the absorbed dose of irradiated samples from the established dose-effect curve.

  3. Group decision-making techniques for natural resource management applications

    USGS Publications Warehouse

    Coughlan, Beth A.K.; Armour, Carl L.

    1992-01-01

    This report is an introduction to decision analysis and problem-solving techniques for professionals in natural resource management. Although these managers are often called upon to make complex decisions, their training in the natural sciences seldom provides exposure to the decision-making tools developed in management science. Our purpose is to being to fill this gap. We present a general analysis of the pitfalls of group problem solving, and suggestions for improved interactions followed by the specific techniques. Selected techniques are illustrated. The material is easy to understand and apply without previous training or excessive study and is applicable to natural resource management issues.

  4. Bioanalytical applications of isothermal nucleic acid amplification techniques.

    PubMed

    Deng, Huimin; Gao, Zhiqiang

    2015-01-01

    The most popular in vitro nucleic acid amplification techniques like polymerase chain reaction (PCR) including real-time PCR are costly and require thermocycling, rendering them unsuitable for uses at point-of-care. Highly efficient in vitro nucleic acid amplification techniques using simple, portable and low-cost instruments are crucial in disease diagnosis, mutation detection and biodefense. Toward this goal, isothermal amplification techniques that represent a group of attractive in vitro nucleic acid amplification techniques for bioanalysis have been developed. Unlike PCR where polymerases are easily deactivated by thermally labile constituents in a sample, some of the isothermal nucleic acid amplification techniques, such as helicase-dependent amplification and nucleic acid sequence-based amplification, enable the detection of bioanalytes with much simplified protocols and with minimal sample preparations since the entire amplification processes are performed isothermally. This review focuses on the isothermal nucleic acid amplification techniques and their applications in bioanalytical chemistry. Starting off from their amplification mechanisms and significant properties, the adoption of isothermal amplification techniques in bioanalytical chemistry and their future perspectives are discussed. Representative examples illustrating the performance and advantages of each isothermal amplification technique are discussed along with some discussion on the advantages and disadvantages of each technique.

  5. Core-Shell Columns in High-Performance Liquid Chromatography: Food Analysis Applications

    PubMed Central

    Preti, Raffaella

    2016-01-01

    The increased separation efficiency provided by the new technology of column packed with core-shell particles in high-performance liquid chromatography (HPLC) has resulted in their widespread diffusion in several analytical fields: from pharmaceutical, biological, environmental, and toxicological. The present paper presents their most recent applications in food analysis. Their use has proved to be particularly advantageous for the determination of compounds at trace levels or when a large amount of samples must be analyzed fast using reliable and solvent-saving apparatus. The literature hereby described shows how the outstanding performances provided by core-shell particles column on a traditional HPLC instruments are comparable to those obtained with a costly UHPLC instrumentation, making this novel column a promising key tool in food analysis. PMID:27143972

  6. Application of turbulent flow chromatography to the metabonomic analysis of human plasma: comparison with protein precipitation.

    PubMed

    Michopoulos, Filippos; Edge, Antony M; Theodoridis, Georgios; Wilson, Ian D

    2010-06-01

    The use of turbulent flow chromatography (TFC) as a method for the rapid metabonomic LC-MS analysis of plasma as an alternative to solvent-based protein precipitation has been investigated. This comparison has shown that TFC can be effectively used in this application with the benefit that off-line sample handling is significantly reduced. However, analysis of the data obtained via TFC for human plasma reveals substantial differences in the overall metabolite profiles compared with methanol-precipitated HPLC-MS. This seems in part at least to be related to greatly reduced amounts of phospholipids (ca. 10 fold reduction) for the turbulent flow methodology compared with protein-precipitated samples. The significance of these differences with respect to metabolite profiles as a result of the sample preparation method used are discussed.

  7. Comparison of turbulent-flow chromatography with automated solid-phase extraction in 96-well plates and liquid-liquid extraction used as plasma sample preparation techniques for liquid chromatography-tandem mass spectrometry.

    PubMed

    Zimmer, D; Pickard, V; Czembor, W; Müller, C

    1999-08-27

    Turbulent flow chromatography (TFC) combined with the high selectivity and sensitivity of tandem mass spectrometry (MS-MS) is a new technique for the fast direct analysis of drugs from crude plasma. TFC in the 96-well plate format reduces significantly the time required for sample clean-up in the laboratory. For example, for 100 samples the workload for a technician is reduced from about 8 h by a manual liquid-liquid extraction (LLE) assay to about 1 h in the case of TFC. Sample clean-up and analysis are performed on-line on the same column. Similar chromatographic performance and validation results were achieved using HTLC Turbo-C18 columns (Cohesive Technologies) and Oasis HLB extraction columns (Waters). One 96-well plate with 96 plasma samples is analyzed within 5.25 h, corresponding to 3.3 min per sample. Compared to this LLE and analysis of 96 samples takes about 16 h. Two structurally different and highly protein bound compounds, drug A and drug B, were analyzed under identical TFC conditions and the assays were fully validated for the application to toxicokinetics studies (compliant with Good Laboratory Practices-GLP). The limit of quantitation was 1.00 microg/l and the linear working range covered three orders of magnitude for both drugs. In the case of drug A the quality of analysis by TFC was similar to the reference LLE assay and slightly better than automated solid-phase extraction in 96-well plates. The accuracy was -3.1 to 6.7% and the precision was 3.1 to 6.8% in the case of drug A determined for dog plasma by TFC-MS-MS. For drug B the accuracy was -3.7 to 3.5% and the precision was 1.6 to 5.4% for rat plasma, which is even slightly better than what was achieved with the validated protein precipitation assay.

  8. Application of the cell sheet technique in tissue engineering

    PubMed Central

    CHEN, GUANGNAN; QI, YIYING; NIU, LIE; DI, TUOYU; ZHONG, JINWEI; FANG, TINGTING; YAN, WEIQI

    2015-01-01

    The development and application of the tissue engineering technique has shown a significant potential in regenerative medicine. However, the limitations of conventional tissue engineering methods (cell suspensions, scaffolds and/or growth factors) restrict its application in certain fields. The novel cell sheet technique can overcome such disadvantages. Cultured cells can be harvested as intact sheets without the use of proteolytic enzymes, such as trypsin or dispase, which can result in cell damage and loss of differentiated phenotypes. The cell sheet is a complete layer, which contains extracellular matrix, ion channel, growth factor receptors, nexin and other important cell surface proteins. Mesenchymal stem cells (MSCs), which have the potential for multiple differentiation, are promising candidate seed cells for tissue engineering. The MSC sheet technique may have potential in the fields of regenerative medicine and tissue engineering in general. Additionally, induced pluripotent stem cell and embryonic stem cell-derived cell sheets have been proposed for tissue regeneration. Currently, the application of cell sheet for tissue reconstruction includes: Direct recipient sites implantation, superposition of cell sheets to construct three-dimensional structure for implantation, or cell sheet combined with scaffolds. The present review discusses the progress in cell sheet techniques, particularly stem cell sheet techniques, in tissue engineering. PMID:26623011

  9. 48 CFR 9904.408-50 - Techniques for application.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    .... 9904.408-50 Section 9904.408-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.408-50 Techniques for application. (a)...

  10. 48 CFR 9904.402-50 - Techniques for application.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    .... 9904.402-50 Section 9904.402-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.402-50 Techniques for application. (a) The...

  11. 48 CFR 9904.404-50 - Techniques for application.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    .... 9904.404-50 Section 9904.404-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.404-50 Techniques for application. (a) The cost...

  12. 48 CFR 9904.401-50 - Techniques for application.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    .... 9904.401-50 Section 9904.401-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.401-50 Techniques for application. (a) The...

  13. 48 CFR 9904.401-50 - Techniques for application.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    .... 9904.401-50 Section 9904.401-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.401-50 Techniques for application. (a) The...

  14. 48 CFR 9904.402-50 - Techniques for application.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    .... 9904.402-50 Section 9904.402-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.402-50 Techniques for application. (a) The...

  15. 48 CFR 9904.401-50 - Techniques for application.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    .... 9904.401-50 Section 9904.401-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.401-50 Techniques for application. (a) The...

  16. 48 CFR 9904.402-50 - Techniques for application.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    .... 9904.402-50 Section 9904.402-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.402-50 Techniques for application. (a) The...

  17. 48 CFR 9904.404-50 - Techniques for application.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    .... 9904.404-50 Section 9904.404-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.404-50 Techniques for application. (a) The cost...

  18. 48 CFR 9904.402-50 - Techniques for application.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    .... 9904.402-50 Section 9904.402-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.402-50 Techniques for application. (a) The...

  19. 48 CFR 9904.404-50 - Techniques for application.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    .... 9904.404-50 Section 9904.404-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.404-50 Techniques for application. (a) The cost...

  20. 48 CFR 9904.406-50 - Techniques for application.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    .... 9904.406-50 Section 9904.406-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.406-50 Techniques for application. (a) The cost of...

  1. 48 CFR 9904.405-50 - Techniques for application.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    .... 9904.405-50 Section 9904.405-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.405-50 Techniques for application. (a) The detail...

  2. 48 CFR 9904.405-50 - Techniques for application.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    .... 9904.405-50 Section 9904.405-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.405-50 Techniques for application. (a) The detail...

  3. DYNAMIC 3D QSAR TECHNIQUES: APPLICATIONS IN TOXICOLOGY

    EPA Science Inventory

    Two dynamic techniques recently developed to account for conformational flexibility of chemicals in 3D QSARs are presented. In addition to the impact of conformational flexibility of chemicals in 3D QSAR models, the applicability of various molecular descriptors is discussed. The...

  4. Dynamic mechanical analysis: A practical introduction to techniques and applications

    SciTech Connect

    Menard, K.

    1999-01-01

    This book introduces DMA, its history, and its current position as part of thermal analysis on polymers. It discusses major types of instrumentation, including oscillatory rotational, oscillatory axial, and torsional pendulum. It also describes analytical techniques in terms of utility, quality of data, methods of calibration, and suitability for different types of materials and assesses applications for thermoplastics, thermosetting systems, and thermosets.

  5. Techniques for Field Application of Lingual Ultrasound Imaging

    ERIC Educational Resources Information Center

    Gick, Bryan; Bird, Sonya; Wilson, Ian

    2005-01-01

    Techniques are discussed for using ultrasound for lingual imaging in field-related applications. The greatest challenges we have faced distinguishing the field setting from the laboratory setting are the lack of controlled head/transducer movement, and the related issue of tissue compression. Two experiments are reported. First, a pilot study…

  6. Application of Data Collection Techniques by Human Performance Technology Practitioners

    ERIC Educational Resources Information Center

    Duan, Minjing

    2011-01-01

    By content-analyzing 22 published cases from a variety of professional and academic books and journals, this study examines the status quo of human performance technology (HPT) practitioners' application of five major data collection techniques in their everyday work: questionnaire, interview, focus group, observation, and document collection. The…

  7. 48 CFR 9904.403-50 - Techniques for application.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    .... 9904.403-50 Section 9904.403-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD, OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.403-50 Techniques for application. (a)(1)...

  8. IBM Applications and Techniques of Operations Research. A Selected Bibliography.

    ERIC Educational Resources Information Center

    International Business Machines Corp., White Plains, NY. Data Processing Div.

    This bibliography on the tools and applications of operations research, management science, industrial engineering, and systems engineering lists many entries which appeared between 1961 and 1966 in 186 periodicals and trade journals. Twenty-six texts in operations research are also listed along with an indication as to which of 37 techniques or…

  9. APPLICATION OF STABLE ISOTOPE TECHNIQUES TO AIR POLLUTION RESEARCH

    EPA Science Inventory

    Stable isotope techniques provide a robust, yet under-utilized tool for examining pollutant effects on plant growth and ecosystem function. Here, we survey a range of mixing model, physiological and system level applications for documenting pollutant effects. Mixing model examp...

  10. Photographic Enlargement of Printed Music: Technique, Application, and Implications.

    ERIC Educational Resources Information Center

    Flynn, Pauline T.; Rich, A. Jeanette

    1982-01-01

    Addressed a need for enlargement of music when retirement home residents were deprived of a self-fulfillment opportunity from choir activities due to failing eyesight. A photographic process yielded the needed feasible large reproductions. Innovative application of this technique affords wide-ranging potential for positive benefit beyond music…

  11. 48 CFR 9904.404-50 - Techniques for application.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    .... 9904.404-50 Section 9904.404-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD... ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.404-50 Techniques for application. (a) The cost to... assets of the acquired company that during the most recent cost accounting period prior to a...

  12. 48 CFR 9904.411-50 - Techniques for application.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    .... 9904.411-50 Section 9904.411-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD... ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.411-50 Techniques for application. (a) Material cost...) The method of computation used for any inventory costing method selected pursuant to the provisions...

  13. 48 CFR 9904.406-50 - Techniques for application.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ...) When a transitional cost accounting period is required under the provisions of 9904.406-40(a)(3), the.... 9904.406-50 Section 9904.406-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD... ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS 9904.406-50 Techniques for application. (a) The cost of...

  14. Application of optical correlation techniques to particle imaging velocimetry

    NASA Technical Reports Server (NTRS)

    Wernet, Mark P.; Edwards, Robert V.

    1988-01-01

    Pulsed laser sheet velocimetry yields nonintrusive measurements of velocity vectors across an extended 2-dimensional region of the flow field. The application of optical correlation techniques to the analysis of multiple exposure laser light sheet photographs can reduce and/or simplify the data reduction time and hardware. Here, Matched Spatial Filters (MSF) are used in a pattern recognition system. Usually MSFs are used to identify the assembly line parts. In this application, the MSFs are used to identify the iso-velocity vector contours in the flow. The patterns to be recognized are the recorded particle images in a pulsed laser light sheet photograph. Measurement of the direction of the partical image displacements between exposures yields the velocity vector. The particle image exposure sequence is designed such that the velocity vector direction is determined unambiguously. A global analysis technique is used in comparison to the more common particle tracking algorithms and Young's fringe analysis technique.

  15. Toner and paper-based fabrication techniques for microfluidic applications.

    PubMed

    Coltro, Wendell Karlos Tomazelli; de Jesus, Dosil Pereira; da Silva, José Alberto Fracassi; do Lago, Claudimir Lucio; Carrilho, Emanuel

    2010-08-01

    The interest in low-cost microfluidic platforms as well as emerging microfabrication techniques has increased considerably over the last years. Toner- and paper-based techniques have appeared as two of the most promising platforms for the production of disposable devices for on-chip applications. This review focuses on recent advances in the fabrication techniques and in the analytical/bioanalytical applications of toner and paper-based devices. The discussion is divided in two parts dealing with (i) toner and (ii) paper devices. Examples of miniaturized devices fabricated by using direct-printing or toner transfer masking in polyester-toner, glass, PDMS as well as conductive platforms as recordable compact disks and printed circuit board are presented. The construction and the use of paper-based devices for off-site diagnosis and bioassays are also described to cover this emerging platform for low-cost diagnostics.

  16. Applications of monolithic columns in liquid chromatography-based clinical chemistry assays.

    PubMed

    Bunch, Dustin R; Wang, Sihe

    2011-08-01

    Monolithic columns have slowly been applied to HPLC methods for clinical chemistry testing in the last 10 years. The application areas include therapeutic drug monitoring, drugs of abuse, vitamins, porphyrins, and steroids. In comparison with conventional particulate columns, the monolithic columns may offer shorter chromatography time, more robustness, and better resolution for certain analytes. The potential drawback of large mobile phase consumption may be improved with smaller id columns, which are currently on the market. Methods covered in this review are those searchable in PubMed up to December 2010. This review highlights the emergence of monolithic column technology in HPLC methods used for clinical chemistry testing. The goals of this review are threefold: (i) To identify the areas of clinical chemistry that analytical monolithic columns have been used in HPLC methods. (ii) To demonstrate the application of analytical monolithic columns in HPLC methods using different detection systems. (iii) To discuss the advantages and limitations of the monolithic columns compared with particulate columns in the clinical chemistry applications.

  17. A concise review of applications of micellar liquid chromatography to study biologically active compounds.

    PubMed

    Stępnik, Katarzyna E

    2017-01-01

    The features of micellar systems are outstanding compared with conventional RP-LC ones. Therefore, the unique properties of micellar chromatography (MLC) are widely recognized. In this short review the applicability of MLC as an in vitro method for the determination of biological activity is discussed. For this purpose many specific examples of MLC applications supported by the theoretical backgrounds of the cited biological activity areas as well as the factors affecting them are presented. This study collects and organizes the most important references of bioactivity determination which were created both recently and in the past, using the MLC method. Although there are many papers on the MLC there is no literature review focused particularly on its applicability in the study of biological activity of various compounds. This work can be treated as a significant review of so far published papers which particularly emphasizes the importance of MLC as in vitro method for determination of bioactivity of different compounds. Copyright © 2016 John Wiley & Sons, Ltd.

  18. [Determination of 10 sedative-hypnotics in human plasma using pulse splitless injection technique and gas chromatography-mass spectrometry].

    PubMed

    Chang, Qing; Ma, Hongying; Wang, Fangjie; Ou, Honglian; Zou, Ming

    2011-11-01

    A simple, precise and sensitive gas chromatography-mass spectrometry (GC-MS) method coupled with pulse splitless injection technique was developed for the determination of 10 sedative-hypnotics (barbital, amobarbital, phenobarbital, oxazepam, diazepam, nitrazepam, clonazepam, estazolam, alprazolam, triazolam) in human plasma. The drugs spiked in plasma were extracted with ethyl acetate after alkalization with 0.1 mol/L NaOH solution. The organic solvent was evaporated under nitrogen stream, and the residues were redissolved by ethyl acetate. The separation was performed on an HP-5MS column (30 m x 250 microm x 0.25 microm). The analytes were determined and identified using selected ion monitoring (SIM) mode and scan mode, respectively. The internal standard method was used for the determination. The target analytes were well separated from each other on their SIM chromatograms and also on the total ion current (TIC) chromatograms. The blank extract from human plasma gave no peaks that interfered with all the analytes on the chromatogram. The calibration curves for 10 sedative-hypnotics showed excellent linearity. The correlation coefficients of all the drugs were higher than 0.9954. The recoveries of the drugs spiked in human plasma ranged from 92.28% to 111.7%, and the relative standard deviations (RSDs) of intra-day and inter-day determinations were from 4.09% to 14.26%. The detection limits ranged from 2 to 20 microg/L. The method is simple, reliable, rapid and sensitive for the determination and the quantification of 10 sedative-hypnotics in human plasma and seems to be useful in the practice of clinical toxicological cases.

  19. Enantioresolution in electrokinetic chromatography-complete filling technique using sulfated gamma-cyclodextrin. Software-free topological anticipation.

    PubMed

    Escuder-Gilabert, Laura; Martín-Biosca, Yolanda; Medina-Hernández, María José; Sagrado, Salvador

    2016-10-07

    Few papers have tried to predict the resolution ability of chiral selectors in capillary electrophoresis for the separation of the enantiomers of chiral compounds. In a previous work, we have used molecular information available on-line to establish enantioresolution levels of basic compounds using highly sulfated β-CD (HS-β-CD) as chiral selector in electrokinetic chromatography-complete filling technique (EKC-CFT). The present study is a continuation of this previous work, introducing some novelties. In this work, the ability of sulfated γ-cyclodextrin (S-γ-CD) as chiral selector in EKC-CFT is modelled for the first time. Thirty-three structurally unrelated cationic and neutral compounds (drugs and pesticides) are studied. Categorical enantioresolution levels (RsC, 0 or 1) are assigned from experimental enantioresolution values obtained at different S-γ-CD concentrations. Novel topological parameters connected to the chiral carbon (C(*)-parameters) are introduced. Four C(*)-parameters and a topological parameter of the whole molecule (aromatic atom count) are the most important variables according to a discriminant partial least squares-variable selection process. It suggests the preponderance of the topology adjacent to the chiral carbon to anticipate the RsC levels. A software-free anticipation protocol for new molecules is proposed. Over the current set of molecules evaluated, 100% of correct anticipations (resolved and non-resolved compounds) are obtained, while anticipation of some compounds remains undetermined. A criterion is introduced to alert on compounds which should not be anticipated.

  20. Novel mesoporous carbonaceous materials: Synthesis, characterization and applications in liquid chromatography

    NASA Astrophysics Data System (ADS)

    Li, Zuojiang

    The ability to control the porous structure in carbonaceous materials has been significantly improved in the past decade due to the appearance of new synthetic routes and novel templating materials. In this dissertation, novel mesoporous carbonaceous materials with controlled structural and surface properties were prepared and investigated using low temperature nitrogen adsorption, thermal analysis, X-ray diffraction and other analytical techniques. The performance of these novel mesoporous carbons in liquid chromatography was also investigated. Carbons with extremely high mesoporosity were synthesized by using mesophase pitch and polyacrylonitrile as precursors in the silica gel templating method, which led to a dramatic reduction of microporosity and high carbonization yield. The most important achievement of this dissertation is the initiation of a colloidal imprinting technique, in which spherical pores were created in the particles of mesophase pitch by using silica colloids of proper size. This method allows us to prepare carbons with uniform spherical pores in the range of 7--70 nm and narrow pore size distribution, filling the pore size gap between carbons templated with ordered silicas and colloidal silica crystals. The introduction of air stabilization further improved the ability to control the pore development at a given stage in the imprinting process. For the first time, carbon particles with mesoporous shell/nonporous core structure were obtained. In this way, carbons with controlled pore size, surface area, pore volume and particle size were synthesized. Moreover, the colloidal imprinting technique was extended to a more general imprinting concept, in which porous particles were used to obtain carbon particles having ordered or disordered structure on their surface. Graphitization of the imprinted carbons provided carbonaceous materials of tailored mesopores and graphitic structure. Also, this high-temperature treatment removed surface functional

  1. Usability evaluation techniques in mobile commerce applications: A systematic review

    NASA Astrophysics Data System (ADS)

    Hussain, Azham; Mkpojiogu, Emmanuel O. C.

    2016-08-01

    Obviously, there are a number of literatures concerning the usability of mobile commerce (m-commerce) applications and related areas, but they do not adequately provide knowledge about usability techniques used in most of the empirical usability evaluation for m-commerce application. Therefore, this paper is aimed at producing the usability techniques frequently used in the aspect of usability evaluation for m-commerce applications. To achieve the stated objective, systematic literature review was employed. Sixty seven papers were downloaded in usability evaluation for m-commerce and related areas; twenty one most relevant studies were selected for review in order to extract the appropriate information. The results from the review shows that heuristic evaluation, formal test and think aloud methods are the most commonly used methods in m-commerce application in comparison to cognitive walkthrough and the informal test methods. Moreover, most of the studies applied control experiment (33.3% of the total studies); other studies that applied case study for usability evaluation are 14.28%. The results from this paper provide additional knowledge to the usability practitioners and research community for the current state and use of usability techniques in m-commerce application.

  2. Microwave-assisted derivatization: application to steroid profiling by gas chromatography/mass spectrometry.

    PubMed

    Casals, Gregori; Marcos, Josep; Pozo, Oscar J; Alcaraz, José; Martínez de Osaba, María Jesús; Jiménez, Wladimiro

    2014-06-01

    Gas chromatography-mass spectrometry (GC-MS) remains as the gold-standard technique for the study of the steroid metabolome. A main limitation is the need of performing a derivatization step since incubation with strong silylations agents for long periods of time (usually 16 h) is required for the derivatization of hindered hydroxyls present in some steroids of interest. In the present work, a rapid, simple and reproducible microwave-assisted derivatization method was developed. In the method, 36 steroids already treated with methoxyamine (2% in pyridine) were silylated with 50 μl of N-trimethylsilylimidazole by using microwave irradiation, and the formed methyloxime-trimethylsilyl derivatives were analyzed by GC-MS. Microwave power and derivatization time silylation conditions were optimized being the optimum conditions 600 W and 3 min respectively. In order to evaluate the usefulness of this technique, the urine steroid profiles for 20 healthy individuals were analyzed. The results of a comparison of microwave irradiation with the classical heating protocol showed similar derivatization yields, thus suggesting that microwave-assisted silylation is a valid tool for the rapid steroid metabolome study.

  3. Fun with Paper Chromatography.

    ERIC Educational Resources Information Center

    Coleman, Dava; Hounshell, Paul B.

    1982-01-01

    Discusses paper chromatographic techniques and provides examples of typical classroom activities. Includes description of retardation values obtained during chromatography exercises and suggests using them for math lessons. (JN)

  4. Improved esthetic results with fine-tip Dermabond application technique.

    PubMed

    Santibanez-Gallerani, Alberto; Armstrong, Milton B; Thaller, Seth R

    2004-09-01

    Tissue glues and adhesives have achieved increasing popularity as alternatives to small wound closure. When applying these substances, it is often difficult to avoid contact with the surrounding skin and foreign objects such as surgical gloves. A technique for the application of Dermabond is described in this report. Twenty wounds less than 10 cm in length were reapproximated using a fine-tip tuberculin syringe applicator. The wounds were evaluated immediately after the application, and 2, 4, and 6 weeks after surgery. Use of the tuberculin fine-tip technique allowed reapproximation of the wound edges with no clinical evidence of surrounding tissue damage. There were no apparent decreases in wound strength or associated discoloration or fuzziness onto the skin. Esthetic results were considered good to excellent by patients. Dermabond can be accurately applied with a tuberculin syringe, avoiding the surrounding tissue damage and foreign object adhesion reported in the literature.

  5. A High Performance Image Data Compression Technique for Space Applications

    NASA Technical Reports Server (NTRS)

    Yeh, Pen-Shu; Venbrux, Jack

    2003-01-01

    A highly performing image data compression technique is currently being developed for space science applications under the requirement of high-speed and pushbroom scanning. The technique is also applicable to frame based imaging data. The algorithm combines a two-dimensional transform with a bitplane encoding; this results in an embedded bit string with exact desirable compression rate specified by the user. The compression scheme performs well on a suite of test images acquired from spacecraft instruments. It can also be applied to three-dimensional data cube resulting from hyper-spectral imaging instrument. Flight qualifiable hardware implementations are in development. The implementation is being designed to compress data in excess of 20 Msampledsec and support quantization from 2 to 16 bits. This paper presents the algorithm, its applications and status of development.

  6. Quantification of levoglucosan and its isomers by High Performance Liquid Chromatography - Electrospray Ionization tandem Mass Spectrometry and its applications to atmospheric and soil samples

    NASA Astrophysics Data System (ADS)

    Piot, C.; Jaffrezo, J.-L.; Cozic, J.; Pissot, N.; El Haddad, I.; Marchand, N.; Besombes, J.-L.

    2011-07-01

    The determination of atmospheric concentrations of levoglucosan and its two isomers, unambiguous tracers of biomass burning emissions, became even more important with the development of wood as renewable energy for domestic heating. Many researches demonstrated the increase during recent years of atmospheric particulate matter load due to domestic biomass combustion in developed countries. Analysis of biomass burning tracers is traditionally performed with Gas Chromatography-Mass Spectrometry (GC-MS) technique after derivatization and requires an organic solvent extraction. A simpler and faster technique using Liquid Chromatography - Electrospray Ionisation - tandem Mass Spectrometry (LC-ESI-MS/MS) was optimized for the analysis of levoglucosan, mannosan and galactosan isomers after an aqueous extraction. This technique allows a good separation between the three compounds in a very reduced time (runtime ~5 min). LOD and LOQ of this method are 30 μg l-1 and 100 μg l-1 respectively, allowing the use of filters from low-volume sampler (as commonly used in routine campaigns). A comparison of simultaneous levoglucosan measurements by GC-MS and LC-ESI-MS/MS for about 50 samples coming from different types of sampling sites and seasons was realized and shows very good agreement between the two methods. Therefore LC-ESI-MS/MS method can be used as an alternative to GC-MS particularly for measurement campaigns in routine where analysis time is important and detection limit is reduced. This paper shows that this method is also applicable to other environmental sample types like soil.

  7. Quantification of levoglucosan and its isomers by High Performance Liquid Chromatography - Electrospray Ionization tandem Mass Spectrometry and its applications to atmospheric and soil samples

    NASA Astrophysics Data System (ADS)

    Piot, C.; Jaffrezo, J.-L.; Cozic, J.; Pissot, N.; El Haddad, I.; Marchand, N.; Besombes, J.-L.

    2012-01-01

    The determination of atmospheric concentrations of levoglucosan and its two isomers, unambiguous tracers of biomass burning emissions, became even more important with the development of wood as renewable energy for domestic heating. Many researches demonstrated the increase during recent years of atmospheric particulate matter load due to domestic biomass combustion in developed countries. Analysis of biomass burning tracers is traditionally performed with Gas Chromatography-Mass Spectrometry (GC-MS) technique after derivatization and requires an organic solvent extraction. A simpler and faster technique using Liquid Chromatography - Electrospray Ionisation - tandem Mass Spectrometry (LC-ESI-MS/MS) was optimized for the analysis of levoglucosan, mannosan and galactosan isomers after an aqueous extraction. This technique allows a good separation between the three compounds in a very reduced time (runtime ~5 min). LOD and LOQ of this method are 30 μg l-1 and 100 μg l-1 respectively, allowing the use of filters from low-volume sampler (as commonly used in routine campaigns). A comparison of simultaneous levoglucosan measurements by GC-MS and LC-ESI-MS/MS for about 50 samples coming from different types of sampling sites and seasons was realized and shows very good agreement between the two methods. Therefore LC-ESI-MS/MS method can be used as an alternative to GC-MS particularly for measurement campaigns in routine where analysis time is important and detection limit is reduced. This paper shows that this method is also applicable to other environmental sample types like soil.

  8. Applications of ion chromatography with electrospray mass spectrometric detection to the determination of environmental contaminants in water.

    PubMed

    Roehl, R; Slingsby, R; Avdalovic, N; Jackson, P E

    2002-05-17

    Ion chromatography (IC) is widely used for the compliance monitoring of common inorganic anions in drinking water. However, there has recently been considerable interest in the development of IC methods to meet regulatory requirements for analytes other than common inorganic anions, including disinfection byproduct anions, perchlorate, and haloacetic acids. Many of these new methods require the use of large injection volumes, high capacity columns and analyte specific detection schemes, such as inductively coupled plasma mass spectrometry or postcolumn reaction with UV-Vis detection, in order to meet current regulatory objectives. Electrospray ionization mass spectrometry (ESI-MS) is a detection technique that is particularly suitable for the analysis of permanently ionized or polar, ionizable compounds. The combination of IC with MS detection is emerging as an important tool for the analysis of ionic compounds in drinking water, as it provides increased specificity and sensitivity compared to conductivity detection. This paper reports on the application of IC-ESI-MS for the confirmation and quantitation of environmentally significant contaminants, i.e. compounds with adverse health effects which are either regulated or being considered for regulation, such as bromate, perchlorate, haloacetic acids, and selenium species, in various water samples.

  9. Improvements and application of a modified gas chromatography atomic fluorescence spectroscopy method for routine determination of methylmercury in biota samples.

    PubMed

    Gorecki, Jerzy; Díez, Sergi; Macherzynski, Mariusz; Kalisinska, Elżbieta; Golas, Janusz

    2013-10-15

    Improvements to the application of a combined solid-phase microextraction followed by gas chromatography coupled to pyrolysis and atomic fluorescence spectrometry method (SPME-GC-AFS) for methylmercury (MeHg) determination in biota samples are presented. Our new method includes improvements in the methodology of determination and the quantification technique. A shaker instead of a stirrer was used, in order to reduce the possibility of sample contamination and to simplify cleaning procedures. Then, optimal rotation frequency and shaking time were settled at 800 rpm and 10 min, respectively. Moreover, the GC-AFS system was equipped with a valve and an argon heater to eliminate the effect of the decrease in analytical signal caused by the moisture released from SPME fiber. For its determination, MeHg was first extracted from biota samples with a 25% KOH solution (3h) and then it was quantified by two methods, a conventional double standard addition method (AC) and a modified matrix-matched calibration (MQ) which is two times faster than the AC method. Both procedures were successfully tested with certified reference materials, and applied for the first time to the determination of MeHg in muscle samples of goosander (Mergus merganser) and liver samples of white-tailed eagle (Haliaeetus albicilla) with values ranging from 1.19 to 3.84 mg/kg dry weight (dw), and from 0.69 to 6.23 mg kg(-1) dw, respectively.

  10. Application of the DREADD technique in biomedical brain research.

    PubMed

    Dobrzanski, Grzegorz; Kossut, Małgorzata

    2017-04-01

    The DREADD (Designer Receptors Exclusively Activated by Designer Drugs) technique is a new chemogenetic approach allowing for selective and remote control of neural activity with a high degree of spatial resolution. Since its discovery in 2007 the DREADD technique was successfully employed into basic research, and together with the optogenetic method provided so far the best tool to influence the activity of the brain circuits and cell populations. The first aim of this review was to concisely describe the technique with regard to such issues like the history of its development, biochemistry as well as modes of the designer receptors delivery and expression. The other aim was to summarize approaches employed for probing of the brain circuits using the DREADD technique and to characterize the current knowledge of the method's application in medical research focusing on two diseases - Parkinson's disease and drug addiction - in which designer receptors were found notably valuable.

  11. Mutually supportive use of stable isotope and gas chromatography techniques to understand ecohydrological interactions in dryland environments

    NASA Astrophysics Data System (ADS)

    Puttock, A.; Brazier, R. E.; Dungait, J. A. J.; Bol, R.; Dixon, E. R.; Macleod, C. J. A.

    2012-04-01

    Many drylands globally are experiencing extensive vegetation change. In the semi-arid Southwestern United States, this change is characterised by the encroachment of woody vegetation into environments previously dominated by grassland (Van Auken. 2009). The transition from grass to woody vegetation results in a change in ecosystem structure and function (Turnbull et al. 2008). Structural change is typically characterised by an increased heterogeneity of soil and vegetation resources, associated with reduced vegetation coverage and an increased vulnerability to soil erosion and the potential loss of key nutrients to adjacent fluvial systems. This project uses an ecohydrological approach, monitoring natural rainfall-runoff events and resulting water and sediment fluxes over six bounded plots with different vegetation coverage at the Sevilleta National Wildlife Refuge, New Mexico, USA. The experiment takes advantage of a shift in the photosynthetic pathway of dominant vegetation from C3 piñon-juniper (Pinus edulis-Juniperus monosperma) mixed stand through a C4 pure-grass (Bouteloua eriopoda) to C3 shrub (Larrea tridentate). This allows for the utilisation of natural abundance tracing techniques, specifically stable 13C isotope and gas chromatography lipid biomarker analyses. Results collected during the 2010 and 2011 monsoon seasons will be presented, using biogeochemical signatures, to trace and partition fluvial soil organic matter and carbon fluxes during runoff generating rainfall events. Results show that biogeochemical signatures specific to individual plant species can be used to define the provenance of carbon, quantifying whether more Pinus edulis-Juniperus monosperma derived carbon is mobilised from the upland plots, or whether more Larrea tridentata carbon is lost when compared to bouteloa eripoda losses in the lowlands. Results also show that biogeochemical signatures vary with event characteristics, raising the possibility of using these tracing

  12. Green chromatography.

    PubMed

    Płotka, Justyna; Tobiszewski, Marek; Sulej, Anna Maria; Kupska, Magdalena; Górecki, Tadeusz; Namieśnik, Jacek

    2013-09-13

    Analysis of organic compounds in samples characterized by different composition of the matrix is very important in many areas. A vast majority of organic compound determinations are performed using gas or liquid chromatographic methods. It is thus very important that these methods have negligible environmental impact. Chromatographic techniques have the potential to be greener at all steps of the analysis, from sample collection and preparation to separation and final determination. The paper summarizes the approaches used to accomplish the goals of green chromatography. While complete elimination of sample preparation would be an ideal approach, it is not always practical. Solventless extraction techniques offer a very good alternative. Where solvents must be used, the focus should be on the minimization of their consumption. The approaches used to make chromatographic separations greener differ depending on the type of chromatography. In gas chromatography it is advisable to move away from using helium as the carrier gas because it is a non-renewable resource. GC separations using low thermal mass technology can be greener because of energy savings offered by this technology. In liquid chromatography the focus should be on the reduction of solvent consumption and replacement of toxic and environmentally hazardous solvents with more benign alternatives. Multidimensional separation techniques have the potential to make the analysis greener in both GC and LC. The environmental impact of the method is often determined by the location of the instrument with respect to the sample collection point.

  13. Inclusion of a MALDI ion source in the ion chromatography technique: conformational information on polymer and biomolecular ions

    NASA Astrophysics Data System (ADS)

    von Helden, Gert; Wyttenbach, Thomas; Bowers, Michael T.

    1995-08-01

    A matrix-assisted laser desorption ionization (MALDI) source has been coupled to the ion chromatography instrument developed at UCSB. The source produces a strong, consistent signal for several hours on a single sample. In this paper we report the application of this method to a series of poly(ethylene glycol) (PEG) polymers cationized by sodium. Data have been taken for Na+PEG5 to Na+PEG19. The temperature dependence of the ion mobility (collision cross-section) in He gas for Na+PEG9, Na+PEG13 and Na+PEG17 has been measured from 80 to 580 K. A detailed analysis of these three systems has been accomplished in order to extract the conformations of the ion and how they vary with temperature. This analysis included several significant changes from methods used previously. Molecular mechanics methods were used both to obtain the lowest energy 0 K structures and to predict how these structures would change as temperature increases. In order to account for the observed low temperature results, a 12-6-4 potential was incorporated in place of the hard-sphere potential used previously. For all three systems studied in detail, the oxygen atoms on the PEG units solvated the Na+ ion, forming a crown ether type ring of five oxygens surrounding Na+ and several others above and below this ring. The molecular mechanics model was also applied to neutral PEG13. In this instance a quite compact structure is obtained for T <= 200 K but a sudden melting type transition occurs between 200 and 300 K and chaotic motion dominates at and above 300 K. Data are also reported on the temperature dependence of the ion mobility of C60+. This ion is expected to change shape only slightly over the temperature range reported here. Consequently it provided an excellent set of calibration data for evaluating the intramolecular interaction potentials used to describe the collision process.

  14. Application of AI techniques to blast furnace operations

    SciTech Connect

    Iida, Osamu; Ushijima, Yuichi; Sawada, Toshiro

    1995-10-01

    It was during the first stages of application of artificial intelligence (AI) to industrial fields, that the ironmaking division of Mizushima works at Kawasaki Steel recognized its potential. Since that time, the division has sought applications for these techniques to solve various problems. AI techniques applied to control the No. 3 blast furnace operations at the Mizushima works include: Blast furnace control by a diagnostic type of expert system that gives guidance to the actions required for blast furnace operation as well as control of furnace heat by automatically setting blast temperature; Hot stove combustion control by a combination of fuzzy inference and a physical model to insure good thermal efficiency of the stove; and blast furnace burden control using neural networks makes it possible to connect the pattern of gas flow distribution with the condition of the furnace. Experience of AI to control the blast furnace and other ironmaking operations has proved its capability for achieving automation and increased operating efficiency. The benefits are very high. For these reasons, the applications of AI techniques will be extended in the future and new techniques studied to further improve the power of AI.

  15. Review: Current applications and challenges for liquid chromatography coupled to isotope ratio mass spectrometry (LC/IRMS).

    PubMed

    Godin, Jean-Philippe; McCullagh, James S O

    2011-10-30

    High-precision isotope analysis is recognized as an essential research tool in many fields of study. Until recently, continuous flow isotope ratio mass spectrometry (CF-IRMS) was available via an elemental analyzer or a gas chromatography inlet system for compound-specific analysis of light stable isotopes. In 2004, however, an interface that coupled liquid chromatography with IRMS (LC/IRMS) became commercially available for the first time. This brought the capability for new areas of application, in particular enabling compound-specific δ(13)C analysis of non-volatile, aqueous soluble, compounds from complex mixtures. The interface design brought with it several analytical constraints, however, in particular a lack of compatibility with certain types of chromatography as well as limited flow rates and mobile phase compositions. Routine LC/IRMS methods have, however, been established for measuring the δ(13)C isotopic ratios of underivatized individual compounds for application in archeology, nutrition and physiology, geochemistry, hydrology, soil science and food authenticity. Seven years after its introduction, we review the technical advances and constraints, methodological developments and new applications of liquid chromatography coupled to isotope ratio mass spectrometry.

  16. Application of optimization techniques to vehicle design: A review

    NASA Technical Reports Server (NTRS)

    Prasad, B.; Magee, C. L.

    1984-01-01

    The work that has been done in the last decade or so in the application of optimization techniques to vehicle design is discussed. Much of the work reviewed deals with the design of body or suspension (chassis) components for reduced weight. Also reviewed are studies dealing with system optimization problems for improved functional performance, such as ride or handling. In reviewing the work on the use of optimization techniques, one notes the transition from the rare mention of the methods in the 70's to an increased effort in the early 80's. Efficient and convenient optimization and analysis tools still need to be developed so that they can be regularly applied in the early design stage of the vehicle development cycle to be most effective. Based on the reported applications, an attempt is made to assess the potential for automotive application of optimization techniques. The major issue involved remains the creation of quantifiable means of analysis to be used in vehicle design. The conventional process of vehicle design still contains much experience-based input because it has not yet proven possible to quantify all important constraints. This restraint on the part of the analysis will continue to be a major limiting factor in application of optimization to vehicle design.

  17. Extraction chromatography: Progress and opportunities

    SciTech Connect

    Dietz, M.L.; Horwitz, E.P.; Bond, A.H.

    1997-10-01

    Extraction chromatography provides a simple and effective method for the analytical and preparative-scale separation of a variety of metal ions. Recent advances in extractant design, particularly the development of extractants capable of metal ion recognition or of strong complex formation in highly acidic media, have significantly improved the utility of the technique. Advances in support design, most notably the introduction of functionalized supports to enhance metal ion retention, promise to yield further improvements. Column instability remains a significant obstacle, however, to the process-scale application of extraction chromatography. 79 refs.

  18. The application of artificial intelligence techniques to large distributed networks

    NASA Technical Reports Server (NTRS)

    Dubyah, R.; Smith, T. R.; Star, J. L.

    1985-01-01

    Data accessibility and transfer of information, including the land resources information system pilot, are structured as large computer information networks. These pilot efforts include the reduction of the difficulty to find and use data, reducing processing costs, and minimize incompatibility between data sources. Artificial Intelligence (AI) techniques were suggested to achieve these goals. The applicability of certain AI techniques are explored in the context of distributed problem solving systems and the pilot land data system (PLDS). The topics discussed include: PLDS and its data processing requirements, expert systems and PLDS, distributed problem solving systems, AI problem solving paradigms, query processing, and distributed data bases.

  19. [Clinical applications of arterial spin labeling technique in brain diseases].

    PubMed

    Wang, Li; Zheng, Gang; Zhao, Tiezhu; Guo, Chao; Li, Lin; Lu, Guangming

    2013-02-01

    Arterial spin labeling (ASL) technique is a kind of perfusion functional magnetic resonance imaging method that is based on endogenous contrast, and it can measure cerebral blood flow (CBF) noninvasively. The ASL technique has advantages of noninvasiveness, simplicity and relatively lower costs so that it is more suitable for longitudinal studies compared with previous perfusion methods, such as positron emission tomography (PET), single photon emission computed tomography (SPECT), CT and the contrast agent based magnetic resonance perfusion imaging. This paper mainly discusses the current clinical applications of ASL in brain diseases as cerebrovascular diseases, brain tumors, Alzheimer's disease and epilepsy, etc.

  20. Application of Nondestructive Testing Techniques to Materials Testing.

    DTIC Science & Technology

    1986-02-01

    7D-Al?2 605 APPLICATION OF NONDESTRUCTIVE TESTING TECHNIQUES To / MATERIALS TESTING(U) STANFORD UNIV CA EDWARD L GINZTON LAB OF PHYSICS G S KIND FEB...U EDWARD L. GINTZON LAB, W.W. HANSEN LAB OF PHYSIC ! 2306/A2 (%J STANFORD CA 94305’ 11 ,. CONTROLLING OFFICE NAME AND ADDRESS 12. REPORT DATE Feb 1986...we could improve optical systems by employing modern electronic techniques within the optical system. Our purpose has been to make accurate profile

  1. Review of optimization techniques of polygeneration systems for building applications

    NASA Astrophysics Data System (ADS)

    Y, Rong A.; Y, Su; R, Lahdelma

    2016-08-01

    Polygeneration means simultaneous production of two or more energy products in a single integrated process. Polygeneration is an energy-efficient technology and plays an important role in transition into future low-carbon energy systems. It can find wide applications in utilities, different types of industrial sectors and building sectors. This paper mainly focus on polygeneration applications in building sectors. The scales of polygeneration systems in building sectors range from the micro-level for a single home building to the large- level for residential districts. Also the development of polygeneration microgrid is related to building applications. The paper aims at giving a comprehensive review for optimization techniques for designing, synthesizing and operating different types of polygeneration systems for building applications.

  2. Thin-layer and paper chromatography

    SciTech Connect

    Sherma, J.

    1988-06-15

    This is a selective review of the literature of thin-layer chromatography (TLC) and paper chromatography (PC) cited in Chemical Abstracts from December 2, 1985, to December 14, 1987, and Analytical Abstracts from December 1985 to November 1987. Also searched directly were the following important journals publishing papers on TLC and PC: Journal of Chromatography (including its bibliography issues), Journal of High Resolution Chromography and Chromatography Communications (HRC and CC), Journal of Chromotographic Science, Chromatographia, Analytical Chemistry, JAOAC, and Journal of Liquid Chromatography. Approximately 4300 papers were published in the two-year period on the theory, technique, and applications of TLC. Only a few papers continue to report new work in PC. A high number of TLC papers were published in the Russian, Chinese, Japanese, Polish, and Italian languages, many involving quantification by densitometry. Because these papers are in journals and languages not readily accessible to US scientists, they are in most cases not included in the review.

  3. Literature survey of heat transfer enhancement techniques in refrigeration applications

    SciTech Connect

    Jensen, M.K.; Shome, B.

    1994-05-01

    A survey has been performed of the technical and patent literature on enhanced heat transfer of refrigerants in pool boiling, forced convection evaporation, and condensation. Extensive bibliographies of the technical literature and patents are given. Many passive and active techniques were examined for pure refrigerants, refrigerant-oil mixtures, and refrigerant mixtures. The citations were categorized according to enhancement technique, heat transfer mode, and tube or shell side focus. The effects of the enhancement techniques relative to smooth and/or pure refrigerants were illustrated through the discussion of selected papers. Patented enhancement techniques also are discussed. Enhanced heat transfer has demonstrated significant improvements in performance in many refrigerant applications. However, refrigerant mixtures and refrigerant-oil mixtures have not been studied extensively; no research has been performed with enhanced refrigerant mixtures with oil. Most studies have been of the parametric type; there has been inadequate examination of the fundamental processes governing enhanced refrigerant heat transfer, but some modeling is being done and correlations developed. It is clear that an enhancement technique must be optimized for the refrigerant and operating condition. Fundamental processes governing the heat transfer must be examined if models for enhancement techniques are to be developed; these models could provide the method to optimize a surface. Refrigerant mixtures, with and without oil present, must be studied with enhancement devices; there is too little known to be able to estimate the effects of mixtures (particularly NARMs) with enhanced heat transfer. Other conclusions and recommendations are offered.

  4. Application of image processing techniques to fluid flow data analysis

    NASA Technical Reports Server (NTRS)

    Giamati, C. C.

    1981-01-01

    The application of color coding techniques used in processing remote sensing imagery to analyze and display fluid flow data is discussed. A minicomputer based color film recording and color CRT display system is described. High quality, high resolution images of two-dimensional data are produced on the film recorder. Three dimensional data, in large volume, are used to generate color motion pictures in which time is used to represent the third dimension. Several applications and examples are presented. System hardware and software is described.

  5. Advances in dental veneers: materials, applications, and techniques

    PubMed Central

    Pini, Núbia Pavesi; Aguiar, Flávio Henrique Baggio; Lima, Débora Alves Nunes Leite; Lovadino, José Roberto; Terada, Raquel Sano Suga; Pascotto, Renata Corrêa

    2012-01-01

    Laminate veneers are a conservative treatment of unaesthetic anterior teeth. The continued development of dental ceramics offers clinicians many options for creating highly aesthetic and functional porcelain veneers. This evolution of materials, ceramics, and adhesive systems permits improvement of the aesthetic of the smile and the self-esteem of the patient. Clinicians should understand the latest ceramic materials in order to be able to recommend them and their applications and techniques, and to ensure the success of the clinical case. The current literature was reviewed to search for the most important parameters determining the long-term success, correct application, and clinical limitations of porcelain veneers. PMID:23674920

  6. Preparation, characterization and application of a reversed phase liquid chromatography/hydrophilic interaction chromatography mixed-mode C18-DTT stationary phase.

    PubMed

    Wang, Qing; Long, Yao; Yao, Lin; Xu, Li; Shi, Zhi-Guo; Xu, Lanying

    2016-01-01

    A mixed-mode chromatographic stationary phase, C18-DTT (dithiothreitol) silica (SiO2) was prepared through "thiol-ene" click chemistry. The obtained material was characterized by fourier transform infrared spectroscope, nitrogen adsorption analysis and contact angle analysis. Chromatographic performance of the C18-DTT was systemically evaluated by studying the effect of acetonitrile content, pH, buffer concentration of the mobile phase and column temperature. It was demonstrated that the novel stationary phase possessed reversed phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode property. The stop-flow test revealed that C18-DTT exhibited excellent compatibility with 100% aqueous mobile phase. Additionally, the stability and column-to-column reproducibility of the C18-DTT material were satisfactory, with relative standard deviations of retention factor of the tested analytes (verapamil, fenbufen, guanine, tetrandrine and nicotinic acid) in the range of 1.82-3.72% and 0.85-1.93%, respectively. Finally, the application of C18-DTT column was demonstrated in the separation of non-steroidal anti-inflammatory drugs, aromatic carboxylic acids, alkaloids, nucleo-analytes and polycyclic aromatic hydrocarbons. It had great resolving power in the analysis of various compounds in HILIC and RPLC chromatographic conditions and was a promising RPLC/HILIC mixed-mode stationary phase.

  7. Application of thermal analysis techniques in activated carbon production

    USGS Publications Warehouse

    Donnals, G.L.; DeBarr, J.A.; Rostam-Abadi, M.; Lizzio, A.A.; Brady, T.A.

    1996-01-01

    Thermal analysis techniques have been used at the ISGS as an aid in the development and characterization of carbon adsorbents. Promising adsorbents from fly ash, tires, and Illinois coals have been produced for various applications. Process conditions determined in the preparation of gram quantities of carbons were used as guides in the preparation of larger samples. TG techniques developed to characterize the carbon adsorbents included the measurement of the kinetics of SO2 adsorption, the performance of rapid proximate analyses, and the determination of equilibrium methane adsorption capacities. Thermal regeneration of carbons was assessed by TG to predict the life cycle of carbon adsorbents in different applications. TPD was used to determine the nature of surface functional groups and their effect on a carbon's adsorption properties.

  8. Instrument platforms for thin-layer chromatography.

    PubMed

    Bernard-Savary, Pierre; Poole, Colin F

    2015-11-20

    High performance column and thin-layer chromatography are both instrumental techniques but differ in that column chromatography requires a fully integrated instrument platform with high pressure capability while for thin-layer chromatography separate devices are used for each unit operation, usually at or close to atmospheric pressure, and afford higher flexibility supporting on-line or off-line operation. The unit operations of thin-layer chromatography are defined as sample application, development and evaluation with derivatization as an optional step. The diversity of equipment for each operation contributes to the flexibility of analysis by thin-layer chromatography and supports manual, semi-automated or full-automation of the separation process. Instrument platforms are more than a convenience as they affect performance, repeatability, sample detectability, and time management. The current trend in thin-layer chromatography is to make the unit operations independent of the user so that analysts can perform other tasks while each step is performed. In addition, in thin-layer chromatography it is general practice to separate several samples simultaneously, and instrument platforms are required to accommodate this feature. In this article, we review contemporary instrumentation employed in thin-layer chromatography for sample application, development, derivatization, photodocumentation, densitometric evaluation, and hyphenation with spectroscopic detectors with an emphasis on the variety and performance of commercially available systems. Some suggestions for best practices and avoidance of common mistakes are included.

  9. Chromatography in Industry

    NASA Astrophysics Data System (ADS)

    Schoenmakers, Peter

    2009-07-01

    This review focuses on the chromatography research that has been carried out within industry or in close cooperation with industry and that has been reported in the scientific literature between 2006 and mid-2008. Companies in the health care sector, such as pharmaceutical and biotechnology companies, are the largest contributors. Industrial research seems to take place in an open environment in cooperation with academia, peer companies, and institutions. Industry appears ready to embrace new technologies as they emerge, but they focus strongly on making chromatography work robustly, reliably, rapidly, and automatically. “Hyphenated” systems that incorporate on-line sample-preparation techniques and mass-spectrometric detection are the rule rather than the exception. Various multidimensional separation methods are finding numerous applications. Strategies aimed at speeding up the development of new chromatographic methods remain the focus of attention. Also, there is a clear trend toward exploring chromatographic methods for parallel processing along with other strategies for high-throughput analysis.

  10. Application of TRIZ Theory in Patternless Casting Manufacturing Technique

    NASA Astrophysics Data System (ADS)

    Yang, Weidong; Gan, Dequan; Jiang, Ping; Tian, Yumei

    The ultimate goal of Patternless Casting Manufacturing (referred to as PCM) is how to obtain the casts by casting the sand mold directly. In the previous PCM, the resin content of sand mold is much higher than that required by traditional resin sand, so the casts obtained are difficult to be sound and qualified products, which limits the application of this technique greatly. In this paper, the TRIZ algorithm is introduced to the innovation process in PCM systematically.

  11. Analytical techniques of pilot scanning behavior and their application

    NASA Technical Reports Server (NTRS)

    Harris, R. L., Sr.; Glover, B. J.; Spady, A. A., Jr.

    1986-01-01

    The state of the art of oculometric data analysis techniques and their applications in certain research areas such as pilot workload, information transfer provided by various display formats, crew role in automated systems, and pilot training are documented. These analytical techniques produce the following data: real-time viewing of the pilot's scanning behavior, average dwell times, dwell percentages, instrument transition paths, dwell histograms, and entropy rate measures. These types of data are discussed, and overviews of the experimental setup, data analysis techniques, and software are presented. A glossary of terms frequently used in pilot scanning behavior and a bibliography of reports on related research sponsored by NASA Langley Research Center are also presented.

  12. Application of the electrosorption technique to remove Metribuzin pesticide.

    PubMed

    Kitous, O; Cheikh, A; Lounici, H; Grib, H; Pauss, A; Mameri, N

    2009-01-30

    The present work deals with the removal of Metribuzin from aqueous solutions in a batch and continuous mode using electrosorption technique. This technique is based on the combination of two processes: the adsorption of Metribuzin into activated granular carbon (GAC) column and the application of the electrochemical potential. The effects of various experimental parameters (electrochemical potential, volumetric flow rate and initial Metribuzin concentration) on the removal efficiency were investigated. The pesticide sorption capacity at the breakthrough point of the GAC column reached 22 mg(pesticide)g(GAC)(-1). It was increased by more than 100% when the desired electrical potential (-50 mV/SCE) was applied in comparison with the conventional GAC column in similar experimental conditions without electrical potential. Evenmore, the electrosorption technique reduced considerably the drastic decrease encountered when passing from batch mode to continuous column mode.

  13. Applications notice. [application of space techniques to earth resources, environment management, and space processing

    NASA Technical Reports Server (NTRS)

    1978-01-01

    The discipline programs of the Space and Terrestrial (S&T) Applications Program are described and examples of research areas of current interest are given. Application of space techniques to improve conditions on earth are summarized. Discipline programs discussed include: resource observations; environmental observations; communications; materials processing in space; and applications systems/information systems. Format information on submission of unsolicited proposals for research related to the S&T Applications Program are given.

  14. Cylindrical millimeter-wave imaging technique and applications

    NASA Astrophysics Data System (ADS)

    Sheen, David M.; McMakin, Douglas L.; Hall, Thomas E.

    2006-05-01

    The wideband microwave or millimeter-wave cylindrical imaging technique has been developed at Pacific Northwest National Laboratory (PNNL) for several applications including concealed weapon detection and automated body measurement for apparel fitting. This technique forms a fully-focused, diffraction-limited, three-dimensional image of the person or imaging target by scanning an inward-directed vertical array around the person or imaging target. The array is switched electronically to sequence across the array at high-speed, so that a full 360 degree mechanical scan over the cylindrical aperture can occur in 2-10 seconds. Wideband, coherent reflection data from each antenna position are recorded in a computer and subsequently reconstructed using an FFT-based image reconstruction algorithm developed at PNNL. The cylindrical scanning configuration is designed to optimize the illumination of the target and minimize non-returns due to specular reflection of the illumination away from the array. In this paper, simulated modeling data are used to explore imaging issues that affect the cylindrical imaging technique. Physical optics scattering simulations are used to model realistic returns from curved surfaces to determine the extent to which specular reflection affects the signal return and subsequent image reconstruction from these surfaces. This is a particularly important issue for the body measurement application. Also, an artifact in the imaging technique, referred to as "circular convolution aliasing" is discussed including methods to reduce or eliminate it. Numerous simulated and laboratory measured imaging results are presented.

  15. [Application of cell co-culture techniques in medical studies].

    PubMed

    Luo, Yun; Sun, Gui-Bo; Qin, Meng; Yao, Fan; Sun, Xiao-Bo

    2012-11-01

    As the cell co-culture techniques can better imitate an in vivo environment, it is helpful in observing the interactions among cells and between cells and the culture environment, exploring the effect mechanisms of drugs and their possible targets and filling the gaps between the mono-layer cell culture and the whole animal experiments. In recently years, they has attracted much more attention from the medical sector, and thus becoming one of research hotspots in drug research and development and bio-pharmaceutical fields. The cell co-culture techniques, including direct and indirect methods, are mainly used for studying pathological basis, new-type treatment methods and drug activity screening. Existing cell co-culture techniques are used for more pharmacological studies on single drug and less studies on interaction of combined drugs, such as collaborative compatibility and attenuation and synergistic effect among traditional Chinese medicines (TCMs). In line with the action characteristics of multi-component and multi-target, the cell co-culture techniques provide certain reference value for future studies on the effect and mechanism of combined TCMs on organisms as well as new methods for studies on TCMs and their compounds. This essay summarizes cell co-culture methods and their application and look into the future of their application in studies on TCMs and compounds.

  16. Cylindrical Millemeter-Wave Imaging Technique and Applications

    SciTech Connect

    Sheen, David M.; McMakin, Douglas L.; Hall, Thomas E.

    2006-08-01

    The wideband microwave or millimeter-wave cylindrical imaging technique has been developed at Pacific Northwest National Laboratory (PNNL) for several applications including concealed weapon detection and automated body measurements for apparel fitting. This technique forms a fully-focused, diffraction-limited, three-dimensional image of the person or imaging target by scanning an inward-directed vertical array around the person or imaging target. The array is switched electronically to sequence across the array at high-speed, so that a full 360 degree mechanical scan over the cylindrical aperture can occur in 2-10 seconds. Wideband, coherent reflection data from each antenna position are recorded in a computer and subsequently reconstructed using an FFT-based image reconstruction algorithm developed at PNNL. The cylindrical scanning configuration is designed to optimize the illumination of the target and minimize non-returns due to specular reflection of the illumination away from the array. In this paper, simulated modeling data is used to explore imaging issues that affect the cylindrical imaging technique. Physical optics scattering simulations are used to model realistic returns from curved surfaces to determine the extent to which specular reflection affects the signal return and subsequent image reconstruction from these surfaces. This is a particularly important issue for the body measurement application. Also, an artifact in the imaging technique, referred to as "circular convolution aliasing" is discussed including methods to reduce or eliminate it. Numerous simulated and laboratory measured imaging results are presented.

  17. [Comparison of standard methods for determination of pseudocumene in urine using gas chromatography with the headspace technique and a new method using a headspace automatic sampler].

    PubMed

    Kostrzewski, P; Wiaderna-Brycht, A; Czerski, B

    1996-01-01

    The biological indicators that have been proposed for monitoring occupational exposure are: concentration of the solvent or metabolized compounds in alveolar or expired air samples, in venous or arterial capillary blood samples and in urine samples. Recently, many researches have reported significant relationships between the time-weighted average exposure and the urinary concentrations for various solvents. The aim of our study was to compare two methods in which urinary concentrations of pseudocumene were determined by gas chromatography using headspace technique. The standard method was based on determining concentration of organic solvents in 100 mm3 or 1 cm3 samples of urine. The incubation conditions were as follows: equilibration temperature and time: 70 degrees C, 30 min., respectively. 1 cm3 of gas phase was sampled with a gas-tight syringe and injected into a gas chromatograph. The new method using Headspace Sampler was based on determining concentrations of solvents in 10 cm3 samples of urine. The operating conditions were: equilibration time 30 min.; equlibration temperature 80 degrees C; pressurization time 0.1 min.; loop fill time 0.1 min.; loop equilibration 0.1 min.; loop equilibration time 0.05 min.; inject time 1 min.; loop temperature 150 degrees C, transfer line temperature 150 degrees C. HP 7694 Headspace Sampler minimizes sample degradation with a chemically inert pathway extending from the sample loop to the column head. The analytical parameters of both methods (linearity, precision, reproducibility, stability and sensitivity) are fully compatible with the principles of biological monitoring. Application of the headspace autosampler eliminated interference from the biological matrix and made it possible to achieve very low detection limit.

  18. Novel one-step headspace dynamic in-syringe liquid phase derivatization-extraction technique for the determination of aqueous aliphatic amines by liquid chromatography with fluorescence detection.

    PubMed

    Muniraj, Sarangapani; Shih, Hou-Kung; Chen, Ying-Fang; Hsiech, Chunming; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

    2013-06-28

    A novel one-step headspace (HS) dynamic in-syringe (DIS) based liquid-phase derivatization-extraction (LPDE) technique has been developed for the selective determination of two short-chain aliphatic amines (SCAAs) in aqueous samples using high performance liquid chromatography (HPLC) with fluorescence detection (FLD). Methylamine (MA) and dimethylamine (DMA) were selected as model compounds of SCAAs. In this method, a micro-syringe pre-filled with derivatizing reagent solution (9-fluorenylmethyl chloroformate) in the barrel was applied to achieve the simultaneous derivatization and extraction of two methylamines evolved from alkalized aqueous samples through the automated reciprocated movements of syringe plunger. After the derivatization-extraction process, the derivatized phase was directly injected into HPLC-FLD for analysis. Parameters influencing the evolution of methylamines and the HS-DIS-LPDE efficiency, including sample pH and temperature, sampling time, as well as the composition of derivatization reagent, reaction temperature, and frequency of reciprocated plunger movements, were thoroughly examined and optimized. Under optimal conditions, detections were linear in the range of 25-500μgL(-1) for MA and DMA with correlation coefficients all above 0.995. The limits of detection (based on S/N=3) were 5 and 19ngmL(-1) for MA and DMA, respectively. The applicability of the developed method was demonstrated for the determination of MA and DMA in real water samples without any prior cleanup of the sample. The present method provides a simple, selective, automated, low cost and eco-friendly procedure to determine aliphatic amines in aqueous samples.

  19. Separation of single-walled carbon nanotubes by gel-based chromatography using surfactant step-gradient techniques and development of new instrumentation for studying SWCNT reaction processes

    NASA Astrophysics Data System (ADS)

    Breindel, Leonard M.

    Single-walled carbon nanotube (SWCNT) synthesis methods such as CoMoCATTM, HiPcoTM, pulsed laser vaporization (PLV), and catalytic chemical vapor deposition (CCVD) produce several different distributions of (n,m) SWCNT structures, where ( n,m) defines the nanotube diameter and chiral wrapping angle. Post-synthesis processing such as functionalization and/or separations must therefore be employed to yield high purity electronic or single (n,m) samples. Through the use of a surfactant gradient across a gel-based chromatographic column, separations of single (n,m) species can be achieved. Anionic surfactants such as SDS, SDBS, and AOT display different separation effectiveness for single (n,m) species. Results of near-infrared optical absorption for separated SWCNT surfactant suspensions will be discussed, leading to a broader understanding of the important factors necessary for the gel chromatography separation technique. In particular, the effects of SWCNT/surfactant micelle structure are found to be key to achieving fast, simple SWCNT electronic type separations. Additionally, development of new instrumentation for the near-infrared spectrofluorimetric analysis (NIR-SFA) of SWCNTs is useful to the advancement of fundamental SWCNT research and applications. NIR-SFA, for instance, allows for the (n,m) structures of a sample to be identified and monitored during the progress of a chemical reaction or separation experiment. Seeking to achieve the time resolutions necessary for such experiments, the design and optimizations of a system utilizing single-wavelength excitation by diode lasers coupled with a fast NIR detection system are presented.

  20. Secondary metabolites isolation in natural products chemistry: comparison of two semipreparative chromatographic techniques (high pressure liquid chromatography and high performance thin-layer chromatography).

    PubMed

    Do, Thi Kieu Tiên; Hadji-Minaglou, Francis; Antoniotti, Sylvain; Fernandez, Xavier

    2014-01-17

    Chemical investigations on secondary metabolites in natural products chemistry require efficient isolation techniques for characterization purpose as well as for the evaluation of their biological properties. In the case of phytochemical studies, the performance of the techniques is critical (resolution and yield) since the products generally present a narrow range of polarity and physicochemical properties. Several techniques are currently available, but HPLC (preparative and semipreparative) is the most widely used. To compare the performance of semipreparative HPLC and HPTLC for the isolation of secondary metabolites in different types of extracts, we have chosen carvone from spearmint essential oil (Mentha spicata L.), resveratrol from Fallopia multiflora (Thunb.) Haraldson, and rosmarinic acid from rosemary (Rosmarinus officinalis L.) extracts. The comparison was based on the chromatographic separation, the purity and quantity of isolated compounds, the solvent consumption, the duration and the cost of the isolation operations. The results showed that semipreparative HPTLC can in some case offer some advantages over conventional semipreparative HPLC.

  1. Using Aspen to Teach Chromatographic Bioprocessing: A Case Study in Weak Partitioning Chromatography for Biotechnology Applications

    ERIC Educational Resources Information Center

    Evans, Steven T.; Huang, Xinqun; Cramer, Steven M.

    2010-01-01

    The commercial simulator Aspen Chromatography was employed to study and optimize an important new industrial separation process, weak partitioning chromatography. This case study on antibody purification was implemented in a chromatographic separations course. Parametric simulations were performed to investigate the effect of operating parameters…

  2. MEMS-based power generation techniques for implantable biosensing applications.

    PubMed

    Lueke, Jonathan; Moussa, Walied A

    2011-01-01

    Implantable biosensing is attractive for both medical monitoring and diagnostic applications. It is possible to monitor phenomena such as physical loads on joints or implants, vital signs, or osseointegration in vivo and in real time. Microelectromechanical (MEMS)-based generation techniques can allow for the autonomous operation of implantable biosensors by generating electrical power to replace or supplement existing battery-based power systems. By supplementing existing battery-based power systems for implantable biosensors, the operational lifetime of the sensor is increased. In addition, the potential for a greater amount of available power allows additional components to be added to the biosensing module, such as computational and wireless and components, improving functionality and performance of the biosensor. Photovoltaic, thermovoltaic, micro fuel cell, electrostatic, electromagnetic, and piezoelectric based generation schemes are evaluated in this paper for applicability for implantable biosensing. MEMS-based generation techniques that harvest ambient energy, such as vibration, are much better suited for implantable biosensing applications than fuel-based approaches, producing up to milliwatts of electrical power. High power density MEMS-based approaches, such as piezoelectric and electromagnetic schemes, allow for supplemental and replacement power schemes for biosensing applications to improve device capabilities and performance. In addition, this may allow for the biosensor to be further miniaturized, reducing the need for relatively large batteries with respect to device size. This would cause the implanted biosensor to be less invasive, increasing the quality of care received by the patient.

  3. MEMS-Based Power Generation Techniques for Implantable Biosensing Applications

    PubMed Central

    Lueke, Jonathan; Moussa, Walied A.

    2011-01-01

    Implantable biosensing is attractive for both medical monitoring and diagnostic applications. It is possible to monitor phenomena such as physical loads on joints or implants, vital signs, or osseointegration in vivo and in real time. Microelectromechanical (MEMS)-based generation techniques can allow for the autonomous operation of implantable biosensors by generating electrical power to replace or supplement existing battery-based power systems. By supplementing existing battery-based power systems for implantable biosensors, the operational lifetime of the sensor is increased. In addition, the potential for a greater amount of available power allows additional components to be added to the biosensing module, such as computational and wireless and components, improving functionality and performance of the biosensor. Photovoltaic, thermovoltaic, micro fuel cell, electrostatic, electromagnetic, and piezoelectric based generation schemes are evaluated in this paper for applicability for implantable biosensing. MEMS-based generation techniques that harvest ambient energy, such as vibration, are much better suited for implantable biosensing applications than fuel-based approaches, producing up to milliwatts of electrical power. High power density MEMS-based approaches, such as piezoelectric and electromagnetic schemes, allow for supplemental and replacement power schemes for biosensing applications to improve device capabilities and performance. In addition, this may allow for the biosensor to be further miniaturized, reducing the need for relatively large batteries with respect to device size. This would cause the implanted biosensor to be less invasive, increasing the quality of care received by the patient. PMID:22319362

  4. Non-intrusive measurement techniques for hydroelectric applicants

    SciTech Connect

    Birch, R.; Lemon, D.

    1995-12-31

    Non-intrusive acoustic methods for measuring flows, originally developed for oceanographic applications, are being used in and around hydroelectric dams. The acoustic methods can be categorized as either back-scattering or forward-scattering. The first, using the back-scattered signal, measures the Doppler shift of the returning echo to determine the along-beam component of flow. These instruments are generally called Acoustic Doppler Current Profilers (ADCP). Three beam solutions allow computation of the velocity components. Time gating the return provides a velocity profile with bin segments as small as 0.25 in. In areas of strong magnetic deviation, often the case beside large dams, a gyrocompass can be used to provide directional orientation. The velocity data can also be used to quickly compute river or channel discharge. Typical applications and several case studies are presented. The second acoustic technique is based on a forward-scattering phenomenon known as scintillation. This technique has been used on the Fraser River to monitor flows, and properties of the signal have recently been correlated with the biomass of upstream-migrating salmon. Acoustic scintillation flow measurements are well suited to applications with limited space in the along-flow direction. Applications to hydroelectric dams include turbine intake flow measurements, and a system has been developed to measure flow along fish diversion screens.

  5. The 2-D Ion Chromatography Development and Application: Determination of Sulfate in Formation Water at Pre-Salt Region

    NASA Astrophysics Data System (ADS)

    Tonietto, G. B.; Godoy, J. M.; Almeida, A. C.; Mendes, D.; Soluri, D.; Leite, R. S.; Chalom, M. Y.

    2015-12-01

    Formation water is the naturally-occurring water which is contained within the geological formation itself. The quantity and quality of the formation water can both be problematic. Over time, the water volume should decrease as the gas volumes increase. Formation water has been found to contain high levels of Cl, As, Fe, Ba, Mn, PAHs and may even contain naturally occurring radioactive materials. Chlorides in some cases have been found to be in excess of four-five times the level of concentrations found in the ocean. Within the management of well operation, there is sulfate between the analytes of greatest importance due to the potential for hydrogen sulphide formation and consequent corrosion of pipelines. As the concentration of sulfate in these waters can be less than n times that of chloride, a quantitative determination, using the technique of ion chromatography, constitutes an analytical challenge. This work aimed to develop and validate a method for the determination of sulphate ions in hyper-saline waters coming from the oil wells of the pre-salt, using 2D IC. In 2D IC the first column can be understood as a separating column, in which the species with retention times outside a preset range are discarded, while those belonging to this range are retained in a pre-concentrator column to further injecting a second column, the second dimension in which occurs the separation and quantification of the analytes of interest. As the chloride ions have a retention time lower than that of sulfate, a method was developed a for determining sulfate in very low range (mg L-1) by 2D IC, applicable to hypersaline waters, wherein the first dimension is used to the elimination of the matrix, ie, chloride ions, and the second dimension utilized in determining sulfate. For sulphate in a concentration range from 1.00 mg L-1 was obtained an accuracy of 1.0%. The accuracy of the method was tested by the standard addition method different samples of formation water in the pre

  6. Application of split window technique to TIMS data

    NASA Technical Reports Server (NTRS)

    Matsunaga, Tsuneo; Rokugawa, Shuichi; Ishii, Yoshinori

    1992-01-01

    Absorptions by the atmosphere in thermal infrared region are mainly due to water vapor, carbon dioxide, and ozone. As the content of water vapor in the atmosphere greatly changes according to weather conditions, it is important to know its amount between the sensor and the ground for atmospheric corrections of thermal Infrared Multispectral Scanner (TIMS) data (i.e. radiosonde). On the other hand, various atmospheric correction techniques were already developed for sea surface temperature estimations from satellites. Among such techniques, Split Window technique, now widely used for AVHRR (Advanced Very High Resolution Radiometer), uses no radiosonde or any kind of supplementary data but a difference between observed brightness temperatures in two channels for estimating atmospheric effects. Applications of Split Window technique to TIMS data are discussed because availability of atmospheric profile data is not clear when ASTER operates. After these theoretical discussions, the technique is experimentally applied to TIMS data at three ground targets and results are compared with atmospherically corrected data using LOWTRAN 7 with radiosonde data.

  7. Modern acoustic emission technique and its application in aviation industry.

    PubMed

    Geng, Rongsheng

    2006-12-22

    This paper proposes the concept of modern acoustic emission (MAE) technique and describes its application in aviation industry. Modern AE is characterized by the combination of AE parameter and waveform analysis based on the understanding of AE source mechanism, the property of sound wave propagation and the interaction between sound wave and the medium in which the sound wave is propagating. Another feature of MAE is characterized by the application of so-called fully digital AE apparatus with low noise, high speed of data transmission and accurate AE source locating capability. MAE is merely an imagination without the realization of the advanced fully digital AE instrument. The application of MAE in monitoring the conditions of aircraft structures during a fatigue test was taken as an example for showing the important role played by AE. Roles of AE in the evaluation of (environment-related) corrosion damage of aircraft were also presented.

  8. Determination of lysergic acid diethylamide (LSD) in mouse blood by capillary electrophoresis/ fluorescence spectroscopy with sweeping techniques in micellar electrokinetic chromatography.

    PubMed

    Fang, Ching; Liu, Ju-Tsung; Chou, Shiu-Huey; Lin, Cheng-Huang

    2003-03-01

    The separation and on-line concentration of lysergic acid diethylamide (LSD) in mouse blood was achieved by means of capillary electrophoresis/fluorescence spectroscopy using sodium dodecyl sulfate (SDS) as the surfactant. Techniques involving on-line sample concentration, including sweeping micellar electrokinetic chromatography (sweeping-MEKC) and cation-selective exhaustive injection-sweep-micellar electrokinetic chromatography (CSEI-sweep-MEKC) were applied; the optimum on-line concentration and separation conditions were determined. In the analysis of an actual sample, LSD was found in a blood sample from a test mouse (0.1 mg LSD fed to a 20 g mouse; approximately 1/10 to the value of LD(50)). As a result, 120 and 30 ng/mL of LSD was detected at 20 and 60 min, respectively, after ingestion of the doses.

  9. On-line identification of lysergic acid diethylamide (LSD) in tablets using a combination of a sweeping technique and micellar electrokinetic chromatography/77 K fluorescence spectroscopy.

    PubMed

    Fang, Ching; Liu, Ju-Tsung; Lin, Cheng-Huang

    2003-03-01

    This work describes a novel method for the accurate determination of lysergic acid diethylamide (LSD) in tablets. A technique involving sweeping-micellar electrokinetic chromatography (MEKC) was used for the initial on-line concentration and separation, after which a cryogenic molecular fluorescence experiment was performed at 77 K. Using this approach, not only the separation of LSD from the tablet extract was achieved, but on-line spectra were readily distinguishable and could be unambiguously assigned. The results are in agreement with analyses by gas chromatography-mass spectrometry (GC-MS). Thus, this method, which was found to be accurate, sensitive and rapid, has the potential for use as a reliable complementary method to GC-MS in such analyses.

  10. Coupling ultra high-pressure liquid chromatography with mass spectrometry: constraints and possible applications.

    PubMed

    Rodriguez-Aller, Marta; Gurny, Robert; Veuthey, Jean-Luc; Guillarme, Davy

    2013-05-31

    The introduction of columns packed with porous sub-2μm particles and the extension of the upper pressure limit of HPLC instrumentation to 1300bar (ultra-high pressure liquid chromatography, UHPLC) has opened new frontiers in resolution and speed of analysis. However, certain constraints appear when coupling UHPLC technology with mass spectrometry (MS). First, the most significant limitation is related to the narrow peaks that are produced by UHPLC that require a fast duty cycle, which is only available on the latest generations of MS devices. Thus, certain analyzers are more readily compatible with UHPLC (e.g., QqQ or TOF/MS) than others (e.g., ion trap or FT-MS). Second, due to the reduction of the column volume, extra-column band broadening can become significant, leading to a reduction in the kinetic performance of the UHPLC-MS configuration. Third, as the mobile phase linear velocity is higher in UHPLC, the electrospray ionization source must also be able to provide high sensitivity at flow rates of up to 1mL/min. Despite these limitations, the UHPLC-MS/MS platform has successfully been employed over the last decade for various types of applications, including those related to bioanalysis, drug metabolism, multi-residue screening, metabolomics, biopharmaceuticals and polar compounds.

  11. Applications of surface analytical techniques in Earth Sciences

    NASA Astrophysics Data System (ADS)

    Qian, Gujie; Li, Yubiao; Gerson, Andrea R.

    2015-03-01

    to show how each technique is applied and used to obtain specific information and to resolve real problems, which forms the central theme of this review. Although this review focuses on applications of these techniques to study mineralogical and geological samples, we also anticipate that researchers from other research areas such as Material and Environmental Sciences may benefit from this review.

  12. Application of Artificial Intelligence Techniques in Unmanned Aerial Vehicle Flight

    NASA Technical Reports Server (NTRS)

    Bauer, Frank H. (Technical Monitor); Dufrene, Warren R., Jr.

    2003-01-01

    This paper describes the development of an application of Artificial Intelligence for Unmanned Aerial Vehicle (UAV) control. The project was done as part of the requirements for a class in Artificial Intelligence (AI) at Nova southeastern University and as an adjunct to a project at NASA Goddard Space Flight Center's Wallops Flight Facility for a resilient, robust, and intelligent UAV flight control system. A method is outlined which allows a base level application for applying an AI method, Fuzzy Logic, to aspects of Control Logic for UAV flight. One element of UAV flight, automated altitude hold, has been implemented and preliminary results displayed. A low cost approach was taken using freeware, gnu, software, and demo programs. The focus of this research has been to outline some of the AI techniques used for UAV flight control and discuss some of the tools used to apply AI techniques. The intent is to succeed with the implementation of applying AI techniques to actually control different aspects of the flight of an UAV.

  13. The application of seismic techniques to hydrogeological investigations

    NASA Astrophysics Data System (ADS)

    Jarvis, Kevin Donald Gibson

    The objective of this thesis is to demonstrate some new applications of seismic techniques for hydrogeological applications. A compressional-wave, surface-based, reflection seismic technique is used to map aquifer boundaries within a series of Pleistocene near-surface sediments. The interpretation uses both water wells and sequence stratigraphic concepts to identify the boundaries of new and existing aquifers. The use of the cone penetrometer is an integral part of this thesis. The seismic cone is demonstrated to be both cost-effective and reliable for the acquisition of high-quality vertical seismic profile (VSP) data. Other data from the cone, in particular the tip resistance data, are shown to be an integral link for the conversion of shear-wave velocities to values of hydraulic conductivity. Surface-based, shear-wave reflection seismic data are used to image an aquifer contained within Holocene deltaic sediments. A Bayesian inversion of the shear-wave seismic amplitudes (using cone-derived velocities) results in the generation of a two-dimensional profile of shear-wave velocity that is a direct indication of aquifer heterogeneity. Conversion of the velocity to hydraulic conductivity (using a cone-derived relationship) results in the distribution of a key hydrogeologic property within the aquifer. The results from the thesis show significant promise for improving groundwater flow models and providing new techniques for the management and protection of our groundwater resources.

  14. The Applications and Features of Liquid Chromatography-Mass Spectrometry in the Analysis of Traditional Chinese Medicine

    PubMed Central

    2016-01-01

    With increasingly improved separation of complex samples and detection of unknown material capabilities, liquid chromatography coupled with mass spectrometry (LC-MS) has been widely used in traditional Chinese medicine (TCM) research. This article describes the principles of liquid chromatography (LC) and mass spectrometry (MS) and their advantages and disadvantages in qualitative and quantitative analysis of TCM. We retrieved research literatures about the application of LC-MS in TCM published during the past five years at home and abroad. To better guide the analysis of TCM, this review mainly focuses on the applications category of LC-MS, how often different kinds of LC-MS are used, and the qualitative and quantitative ability of various LC-MS in the study of TCM. PMID:27956918

  15. Application of seismic-refraction techniques to hydrologic studies

    USGS Publications Warehouse

    Haeni, F.P.

    1986-01-01

    Seismic-refraction methods have been extensively used in petroleum, mineral, and engineering investigations and to some extent, for hydrologic applications during the past 30 years. Recent advances in equipment, sound sources, and computer-interpretation techniques make seismic-refraction methods a highly effective and economical means of obtaining subsurface data in hydrologic studies. Aquifers that can be defined by one or more high seismic-velocity surfaces, such as alluvial or glacial deposits in consolidated rock valleys, limestone or sandstone underlain by metamorphic or igneous rock, or saturated unconsolidated deposits overlain by unsaturated unconsolidated deposits, are ideally suited for applying seismic-refraction methods. These methods allow the economical collection of subsurface data and provide the basis for more efficient collection of subsurface data by test drilling or aquifer tests and results in improved hydrologic studies. This manual briefly reviews the basics of seismic refraction theory and principles. It emphasizes the use of this technique in hydrologic investigations and describes the planning, equipment, field procedures, and interpretation techniques needed for this type of study. Examples of the use of seismic refraction techniques in a wide variety of hydrologic studies are presented. (USGS)

  16. Application of seismic-refraction techniques to hydrologic studies

    USGS Publications Warehouse

    Haeni, F.P.

    1988-01-01

    During the past 30 years, seismic-refraction methods have been used extensively in petroleum, mineral, and engineering investigations and to some extent for hydrologic applications. Recent advances in equipment, sound sources, and computer interpretation techniques make seismic refraction a highly effective and economical means of obtaining subsurface data in hydrologic studies. Aquifers that can be defined by one or more high-seismic-velocity surface, such as (1) alluvial or glacial deposits in consolidated rock valleys, (2) limestone or sandstone underlain by metamorphic or igneous rock, or (3) saturated unconsolidated deposits overlain by unsaturated unconsolidated deposits, are ideally suited for seismic-refraction methods. These methods allow economical collection of subsurface data, provide the basis for more efficient collection of data by test drilling or aquifer tests, and result in improved hydrologic studies. This manual briefly reviews the basics of seismic-refraction theory and principles. It emphasizes the use of these techniques in hydrologic investigations and describes the planning, equipment, field procedures, and interpretation techniques needed for this type of study. Further-more, examples of the use of seismic-refraction techniques in a wide variety of hydrologic studies are presented.

  17. MR urography in children and adolescents: techniques and clinical applications.

    PubMed

    Dillman, Jonathan R; Trout, Andrew T; Smith, Ethan A

    2016-06-01

    Renal and urinary tract imaging is commonly performed in the pediatric population, particularly in the setting of suspected or known congenital anomalies. In most cases, adequate anatomic assessment can be achieved using ultrasound and fluoroscopic techniques, and evaluation of differential renal function and urinary tract drainage can be accomplished with renal scintigraphy. However, in a subset of children, anatomic or functional questions may remain after this routine evaluation. In this setting, magnetic resonance imaging (MRI) tailored to evaluate the kidneys and urinary tract, known as MR urography (MRU), can be used to depict the kidneys, ureters, and urinary bladder in detail and to determine differential renal function and assess urinary tract drainage. The objectives of this review article are to (1) describe pediatric-specific MRI techniques for assessment of the kidneys and urinary tract and (2) present common clinical applications for pediatric MRU where imaging can "add value" in terms of diagnosis and patient management.

  18. Techniques For Microfabricating Coils For Microelectromechanical Systems Applications

    SciTech Connect

    Woods, R. C.; Powell, A. L.

    2008-01-21

    The advanced technology necessary for building future space exploration vehicles includes microfabricated coils for making possible self-inductances integrated with other passive and active electronic components. Integrated inductances make possible significant improvements in reliability over the traditional arrangement of using external discrete inductances, as well as allowing significant size (volume) reductions (also important in space vehicles). Two possible fabrication techniques (one using proprietary branded 'Foturan' glass, the other using silicon wafer substrates) for microscopic coils are proposed, using electroplating into channels. The techniques have been evaluated for fabricating the planar electrical coils needed for typical microelectromechanical systems applications. There remain problems associated with processing using 'Foturan' glass, but coil fabrication on silicon wafers was successful. Fabrication methods such as these are expected to play an important part in the development of systems and subsystems for forthcoming space exploration missions.

  19. Techniques For Microfabricating Coils For Microelectromechanical Systems Applications

    NASA Astrophysics Data System (ADS)

    Woods, R. C.; Powell, A. L.

    2008-01-01

    The advanced technology necessary for building future space exploration vehicles includes microfabricated coils for making possible self-inductances integrated with other passive and active electronic components. Integrated inductances make possible significant improvements in reliability over the traditional arrangement of using external discrete inductances, as well as allowing significant size (volume) reductions (also important in space vehicles). Two possible fabrication techniques (one using proprietary branded "Foturan" glass, the other using silicon wafer substrates) for microscopic coils are proposed, using electroplating into channels. The techniques have been evaluated for fabricating the planar electrical coils needed for typical microelectromechanical systems applications. There remain problems associated with processing using "Foturan" glass, but coil fabrication on silicon wafers was successful. Fabrication methods such as these are expected to play an important part in the development of systems and subsystems for forthcoming space exploration missions.

  20. Novel atmospheric extinction measurement techniques for aerospace laser system applications

    NASA Astrophysics Data System (ADS)

    Sabatini, Roberto; Richardson, Mark

    2013-01-01

    Novel techniques for laser beam atmospheric extinction measurements, suitable for manned and unmanned aerospace vehicle applications, are presented in this paper. Extinction measurements are essential to support the engineering development and the operational employment of a variety of aerospace electro-optical sensor systems, allowing calculation of the range performance attainable with such systems in current and likely future applications. Such applications include ranging, weaponry, Earth remote sensing and possible planetary exploration missions performed by satellites and unmanned flight vehicles. Unlike traditional LIDAR methods, the proposed techniques are based on measurements of the laser energy (intensity and spatial distribution) incident on target surfaces of known geometric and reflective characteristics, by means of infrared detectors and/or infrared cameras calibrated for radiance. Various laser sources can be employed with wavelengths from the visible to the far infrared portions of the spectrum, allowing for data correlation and extended sensitivity. Errors affecting measurements performed using the proposed methods are discussed in the paper and algorithms are proposed that allow a direct determination of the atmospheric transmittance and spatial characteristics of the laser spot. These algorithms take into account a variety of linear and non-linear propagation effects. Finally, results are presented relative to some experimental activities performed to validate the proposed techniques. Particularly, data are presented relative to both ground and flight trials performed with laser systems operating in the near infrared (NIR) at λ = 1064 nm and λ = 1550 nm. This includes ground tests performed with 10 Hz and 20 kHz PRF NIR laser systems in a large variety of atmospheric conditions, and flight trials performed with a 10 Hz airborne NIR laser system installed on a TORNADO aircraft, flying up to altitudes of 22,000 ft.

  1. Recent Advances in Seismic Wavefront Tracking Techniques and Their Applications

    NASA Astrophysics Data System (ADS)

    Sambridge, M.; Rawlinson, N.; Hauser, J.

    2007-12-01

    In observational seismology, wavefront tracking techniques are becoming increasingly popular as a means of predicting two point traveltimes and their associated paths. Possible applications include reflection migration, earthquake relocation and seismic tomography at a wide variety of scales. Compared with traditional ray based techniques such as shooting and bending, wavefront tracking has the advantage of locating traveltimes between the source and every point in the medium; in many cases, improved efficiency and robustness; and greater potential for tracking multiple arrivals. In this presentation, two wavefront tracking techniques will be considered: the so-called Fast Marching Method (FMM), and a wavefront construction (WFC) scheme. Over the last several years, FMM has become a mature technique in seismology, with a number of improvements to the underlying theory and the release of software tools that allow it to be used in a variety of applications. At its core, FMM is a grid based solver that implicitly tracks a propagating wavefront by seeking finite difference solutions to the eikonal equation along an evolving narrow band. Recent developments include the use of source grid refinement to improve accuracy, the introduction of a multi-stage scheme to allow reflections and refractions to be tracked in layered media, and extension to spherical coordinates. Implementation of these ideas has led to a number of different applications, including teleseismic tomography, wide-angle reflection and refraction tomography, earthquake relocation, and ambient noise imaging using surface waves. The WFC scheme represents the wavefront surface as a set of points in 6-D phase space; these points are advanced in time using local initial value ray tracing in order to form a sequence of wavefront surfaces that fill the model volume. Surface refinement and simplification techniques inspired by recent developments in computer graphics are used to maintain a fixed density of nodes

  2. Enantioselective gas chromatography/mass spectrometry of methylsulfonyl PCBs with application to arctic marine mammals.

    PubMed

    Wiberg, K; Letcher, R; Sandau, C; Duffe, J; Norstrom, R; Haglund, P; Bidleman, T

    1998-09-15

    Four different commercially available cyclodextrin (CD) capillary gas chromatography (GC) columns were tested for the enantioselective separation of nine environmentally persistent atropisomeric 3- and 4-methylsulfonyl PCBs (MeSO2-CBs). The selected columns contained cyclodextrins with various cavity diameters (beta- or gamma-CD), which were methylated and/or tert-butyldimethylsilylated (TBDMS) in the 2,3,6-O-positions. The beta-CD column with TBDMS substituents in all of the 2,3,6-O-positions was by far the most selective column for the MeSO2-CBs tested. Enantiomers of congeners with 3-MeSO2 substitution were more easily separated than those with 4-MeSO2 substitution. The separation also seemed to be enhanced for congeners with the chlorine atoms on the non-MeSO2-containing ring and clustered on one side of the same ring. The 2,3-di-O-methyl-6-O-TBDMS-beta-CD was found to give somewhat better selectivity than the corresponding gamma-CD, in comparison between the two columns, which were identical in all other respects. Enantioselective analysis of arctic ringed seal (Phoca hispida) and polar bear (Ursus maritimus) adipose tissue revealed a strong dominance of certain enantiomers. For example, the enantiomer ratio (ER) of 3-MeSO2-CB149 was 0.32 and < 0.1 in ringed seal blubber and polar bear fat, respectively. These low ER values are indicative of highly enantioselective formation, enantioselective metabolism, enantioselective transport across cell membranes, or a combination of the three in both species. Comparable results for the enantiomeric analysis of MeSO2-CBs in biotic tissue extracts were obtained using two highly selective mass spectrometric techniques, ion trap mass spectrometry/mass spectrometry and electron capture negative ion low-resolution mass spectrometry.

  3. Evaluating Credit Applications: A Validation of Multiattribute Utility Techniques Against a Real World Criterion,

    DTIC Science & Technology

    1980-06-01

    science research institute RESEARCH REPORT EVALUATING CREDIT APPLICATIONS: A Z’ VALIDATION OF MULTIATTRIBUTE UTILITY TECHNIQUES AGAINST A REAL WORLD...8217_, ", ’- .’.- .. .- ... . .. ,-*,. . .. EVALUATING CREDIT APPLICATIONS: A VALIDATION OF MULTIATTRIBUTE UTILITY TECHNIQUES AGAINST A REAL WORLD CRITERION...validation of multiattribute utility elicitation techniques. The techniques tested were the Holistic Orthogonal Parameter Estimation (HOPE) technique

  4. Development and Application of Immunoaffinity Chromatography for Coplanar PCBs in Soil and Sediment

    EPA Science Inventory

    An immunoaffinity chromatography (IAC) column was developed as a simple cleanup procedure for preparing environmental samples for analysis of polychlorinated biphenyls (PCBs). Soil and sediment samples were prepared using pressurized liquid extraction (PLE), followed by the IAC c...

  5. Application of digital image processing techniques to astronomical imagery, 1979

    NASA Technical Reports Server (NTRS)

    Lorre, J. J.

    1979-01-01

    Several areas of applications of image processing to astronomy were identified and discussed. These areas include: (1) deconvolution for atmospheric seeing compensation; a comparison between maximum entropy and conventional Wiener algorithms; (2) polarization in galaxies from photographic plates; (3) time changes in M87 and methods of displaying these changes; (4) comparing emission line images in planetary nebulae; and (5) log intensity, hue saturation intensity, and principal component color enhancements of M82. Examples are presented of these techniques applied to a variety of objects.

  6. Electromagnetic and Thermal Dosimetric Techniques in Humans and its Application

    NASA Astrophysics Data System (ADS)

    Hirata, Akimasa; Fujiwara, Osamu

    There has been increasing public concern about the adverse health effects of human exposure to radio frequency fields. Radio frequency fields are also used for medical application. This paper reviews electromagnetic and thermal computational dosimetric techniques, which has been developed by the authors. The feature of the thermal dosimetric method is that body core temperature can be computed reasonably unlike conventional method. This scheme is particularly useful for intense localized or whole-body electromagnetic wave exposure. Computational examples are shown to verify the effectiveness of the proposal.

  7. Application of adaptive antenna techniques to future commercial satellite communication

    NASA Technical Reports Server (NTRS)

    Ersoy, L.; Lee, E. A.; Matthews, E. W.

    1987-01-01

    The purpose of this contract was to identify the application of adaptive antenna technique in future operational commercial satellite communication systems and to quantify potential benefits. The contract consisted of two major subtasks. Task 1, Assessment of Future Commercial Satellite System Requirements, was generally referred to as the Adaptive section. Task 2 dealt with Pointing Error Compensation Study for a Multiple Scanning/Fixed Spot Beam Reflector Antenna System and was referred to as the reconfigurable system. Each of these tasks was further sub-divided into smaller subtasks. It should also be noted that the reconfigurable system is usually defined as an open-loop system while the adaptive system is a closed-loop system. The differences between the open- and closed-loop systems were defined. Both the adaptive and reconfigurable systems were explained and the potential applications of such systems were presented in the context of commercial communication satellite systems.

  8. Surface Plasmon Resonance: A Versatile Technique for Biosensor Applications

    PubMed Central

    Nguyen, Hoang Hiep; Park, Jeho; Kang, Sebyung; Kim, Moonil

    2015-01-01

    Surface plasmon resonance (SPR) is a label-free detection method which has emerged during the last two decades as a suitable and reliable platform in clinical analysis for biomolecular interactions. The technique makes it possible to measure interactions in real-time with high sensitivity and without the need of labels. This review article discusses a wide range of applications in optical-based sensors using either surface plasmon resonance (SPR) or surface plasmon resonance imaging (SPRI). Here we summarize the principles, provide examples, and illustrate the utility of SPR and SPRI through example applications from the biomedical, proteomics, genomics and bioengineering fields. In addition, SPR signal amplification strategies and surface functionalization are covered in the review. PMID:25951336

  9. An Acoustic Communication Technique of Nanorobot Swarms for Nanomedicine Applications.

    PubMed

    Loscrí, Valeria; Vegni, Anna Maria

    2015-09-01

    In this contribution, we present a communication paradigm among nanodevices, based on acoustic vibrations for medical applications. We consider a swarm of nanorobots able to communicate in a distributed and decentralized fashion, propelled in a biological environment (i.e., the human brain). Each nanorobot is intended to i) recognize a cancer cell, ii) destroy it, and then iii) forward information about the presence of cancer formation to other nanorobots, through acoustic signals. The choice of acoustic waves as communication mean is related to the application context, where it is not advisable either to use indiscriminate chemical substances or electromagnetic waves. The effectiveness of the proposed approach is assessed in terms of achievement of the objective (i.e., to destroy the majority of tumor cells), and the velocity of detection and destruction of cancer cells, through a comparison with other related techniques.

  10. An Analysis of Performance Enhancement Techniques for Overset Grid Applications

    NASA Technical Reports Server (NTRS)

    Djomehri, J. J.; Biswas, R.; Potsdam, M.; Strawn, R. C.; Biegel, Bryan (Technical Monitor)

    2002-01-01

    The overset grid methodology has significantly reduced time-to-solution of high-fidelity computational fluid dynamics (CFD) simulations about complex aerospace configurations. The solution process resolves the geometrical complexity of the problem domain by using separately generated but overlapping structured discretization grids that periodically exchange information through interpolation. However, high performance computations of such large-scale realistic applications must be handled efficiently on state-of-the-art parallel supercomputers. This paper analyzes the effects of various performance enhancement techniques on the parallel efficiency of an overset grid Navier-Stokes CFD application running on an SGI Origin2000 machine. Specifically, the role of asynchronous communication, grid splitting, and grid grouping strategies are presented and discussed. Results indicate that performance depends critically on the level of latency hiding and the quality of load balancing across the processors.

  11. Some essential techniques for developing efficient petascale applications

    NASA Astrophysics Data System (ADS)

    Kalé, L. V.

    2008-07-01

    Multiple petaflops-lass machines will appear during the coming year, and many multipetaflops machines are on the anvil. It will be a substantial challenge to make existing parallel CSE applications run efficiently on them, and even more challenging to design new applications that can effectively leverage the large computational power of these machines. Multicore chips and SMP nodes are becoming popular and pose challenges of their own. Further, a new set of challenges in productivity arise, especially if we wish to have a broader set of applications and people to use these machines. Reviewed here is a set of techniques that have proved useful in multiple parallel applications that have scaled to tens of thousands of processors, on machines such as the Blue Gene/L, Blue Gene/P, Cray XT3, and XT4. New challenges and potential solutions for the performance issues are identified. Issues presented by multicore chips and SMP nodes also rre addressed. Also reviewed are some new and old ideas for increasing productivity in parallel programming substantially.

  12. State-of-the-art in fast liquid chromatography-mass spectrometry for bio-analytical applications.

    PubMed

    Núñez, Oscar; Gallart-Ayala, Héctor; Martins, Claudia P B; Lucci, Paolo; Busquets, Rosa

    2013-05-15

    There is an increasing need of new bio-analytical methodologies with enough sensitivity, robustness and resolution to cope with the analysis of a large number of analytes in complex matrices in short analysis time. For this purpose, all steps included in any bio-analytical method (sampling, extraction, clean-up, chromatographic analysis and detection) must be taken into account to achieve good and reliable results with cost-effective methodologies. The purpose of this review is to describe the state-of-the-art of the most employed technologies in the period 2009-2012 to achieve fast analysis with liquid chromatography coupled to mass spectrometry (LC-MS) methodologies for bio-analytical applications. Current trends in fast liquid chromatography involve the use of several column technologies and this review will focus on the two most frequently applied: sub-2μm particle size packed columns to achieve ultra high pressure liquid chromatography (UHPLC) separations and porous-shell particle packed columns to attain high efficiency separations with reduced column back-pressures. Additionally, recent automated sample extraction and clean-up methodologies to reduce sample manipulation, variability and total analysis time in bio-analytical applications such as on-line solid phase extraction coupled to HPLC or UHPLC methods, or the use of other approaches such as molecularly imprinted polymers, restricted access materials, and turbulent flow chromatography will also be addressed. The use of mass spectrometry and high or even ultra-high resolution mass spectrometry to reduce sample manipulation and to solve ion suppression or ion enhancement and matrix effects will also be presented. The advantages and drawbacks of all these methodologies for fast and sensitive analysis of biological samples are going to be discussed by means of relevant applications.

  13. Applicability of ultra-performance liquid chromatography-tandem mass spectrometry for heroin profiling.

    PubMed

    Lurie, Ira S; Toske, Steven G

    2008-04-25

    The applicability of ultra- performance liquid chromatography tandem-mass spectrometry (UPLC-MS/MS) for heroin profiling is described. The coupling of the high separation power of UPLC with the highly selective and sensitive detection of MS/MS is well suited for heroin profiling. An Acquity UPLC BEH C18 1.7 microm particle column (100 mm x 2.1mm) with binary gradients containing 1% formic acid (pH 2.0) or 10 mM ammonium bicarbonate (pH 10.0)/acetonitrile mixtures was investigated for the profiling. For MS/MS detection, an atmospheric pressure positive electrospray source was employed with multiple reaction monitoring (MRM). MRMs for individual basic impurities were generated for heroin profiling using low and high pH mobile phases, while MRMs for neutral impurities were generated using a high pH mobile phase. Compared to a pH 2.2 mobile phase, the use of a pH 10 mobile phase allowed for significantly greater sample loading, major selectivity differences, and lower MRM sensitivity. UPLC-MS/MS allowed for the highly selective and sensitive detection of many of the targeted solutes in seized heroin exhibits. Basic impurities detected included morphine, codeine, noscapine, papaverine and the previously unreported solutes reticuline, reticuline monoacetate (2 products), reticuline diacetate, narceine, codamine, laudanidine, cryptopine, laudanosine, and norlaudanosine. Neutral impurities found included N,3,6-triacetylnormorphine, N-acetylnorcodeine, N-acetylnornarcotine, 3,6-dimethoxy-4-acetyloxy-5-[2-(N-methylacetamido)]-ethylphenanthrene, and cis-n-acetylanhydronornarceine. The detection of these impurities, at levels as low as 10(-6)% w/w should allow for greatly enhanced heroin profiles.

  14. Plasma cleaning techniques and future applications in environmentally conscious manufacturing

    SciTech Connect

    Ward, P.P.

    1995-07-01

    Plasmas have frequently been used in industry as a last step surface preparation technique in an otherwise predominantly wet-etch process. The limiting factor in the usefulness of plasma cleaning techniques has been the rate at which organic materials are removed. Recent research in the field of plasma chemistry has provided some understanding of plasma processes. By controlling plasma conditions and gas mixtures, ultra-fast plasma cleaning and etching is possible. With enhanced organic removal rates, plasma processes become more desirable as an environmentally sound alternative to traditional solvent or acid dominated process, not only as a cleaning tool, but also as a patterning and machining tool. In this paper, innovations in plasma processes are discussed including enhanced plasma etch rates via plasma environment control and aggressive gas mixtures. Applications that have not been possible with the limited usefulness of past plasma processes are now approaching the realm of possibility. Some of these possible applications will be discussed along with their impact to environmentally conscious manufacturing.

  15. Review: Recent application of chiral liquid chromatography-tandem mass spectrometric methods for enantiomeric pharmaceutical and biomedical determinations.

    PubMed

    Nie, Yanfang; Liu, Xiumei; Yang, Xinmei; Zhao, Zhongxi

    2013-09-01

    The technology of analyzing the pharmacological and toxicological properties of chiral drugs has become more commonly utilized since the knowledge of the biological actions of enantiomers has been gradually acquired during the last few decades. This work reviews the applications of chiral liquid chromatography coupled to tandem mass spectrometry (LC-MS) for the analysis of chiral pharmaceuticals since 2005. The enantioselective determinations in pharmaceutical and biomedical fields with LC-MS are classified based on three mobile phase modes, including normal phase, reversed phase and polar organic solvent, in terms of their compatibility with various ionization sources and specific applications.

  16. Surface dating of bricks, an application of luminescence techniques

    NASA Astrophysics Data System (ADS)

    Galli, Anna; Martini, Marco; Maspero, Francesco; Panzeri, Laura; Sibilia, Emanuela

    2014-05-01

    Luminescence techniques are a powerful tool to date archaeological ceramic materials and geological sediments. Thermoluminescence (TL) is widely used for bricks dating to reconstruct the chronology of urban complexes and the development of human cultures. However, it can sometimes be inconclusive, since TL assesses the firing period of bricks, which can be reused, even several centuries later. This problem can be circumvented using a dating technique based on a resetting event different from the last heating. OSL (Optically Stimulated Luminescence) exploits the last light exposition of the brick surface, which resets the light-sensitive electron traps until the surface is definitely shielded by mortar and superimposed bricks. This advanced application (surface dating) has been successfully attempted on rocks, marble and stone artifacts, but not yet on bricks. A recent conservation campaign at the Certosa di Pavia gave the opportunity to sample some bricks belonging to a XVII century collapsed wall, still tied to their mortars. This was an advantageous condition to test this technique, comparing the dating results with precise historical data. This attempt gave satisfactory results, allowing to identify bricks surely reused and to fully confirm that the edification of the perimetral wall occurred at the end of XVII century.

  17. A Review of Diagnostic Techniques for ISHM Applications

    NASA Technical Reports Server (NTRS)

    Patterson-Hine, Ann; Biswas, Gautam; Aaseng, Gordon; Narasimhan, Sriam; Pattipati, Krishna

    2005-01-01

    System diagnosis is an integral part of any Integrated System Health Management application. Diagnostic applications make use of system information from the design phase, such as safety and mission assurance analysis, failure modes and effects analysis, hazards analysis, functional models, fault propagation models, and testability analysis. In modern process control and equipment monitoring systems, topological and analytic , models of the nominal system, derived from design documents, are also employed for fault isolation and identification. Depending on the complexity of the monitored signals from the physical system, diagnostic applications may involve straightforward trending and feature extraction techniques to retrieve the parameters of importance from the sensor streams. They also may involve very complex analysis routines, such as signal processing, learning or classification methods to derive the parameters of importance to diagnosis. The process that is used to diagnose anomalous conditions from monitored system signals varies widely across the different approaches to system diagnosis. Rule-based expert systems, case-based reasoning systems, model-based reasoning systems, learning systems, and probabilistic reasoning systems are examples of the many diverse approaches ta diagnostic reasoning. Many engineering disciplines have specific approaches to modeling, monitoring and diagnosing anomalous conditions. Therefore, there is no "one-size-fits-all" approach to building diagnostic and health monitoring capabilities for a system. For instance, the conventional approaches to diagnosing failures in rotorcraft applications are very different from those used in communications systems. Further, online and offline automated diagnostic applications are integrated into an operations framework with flight crews, flight controllers and maintenance teams. While the emphasis of this paper is automation of health management functions, striking the correct balance between

  18. Application of optical spectroscopic techniques for disease diagnosis

    NASA Astrophysics Data System (ADS)

    Saha, Anushree

    Optical spectroscopy, a truly non-invasive tool for remote diagnostics, is capable of providing valuable information on the structure and function of molecules. However, most spectroscopic techniques suffer from drawbacks, which limit their application. As a part of my dissertation work, I have developed theoretical and experimental methods to address the above mentioned issues. I have successfully applied these methods for monitoring the physical, chemical and biochemical parameters of biomolecules involved in some specific life threatening diseases like lead poisoning and age-related macular degeneration (AMD). I presented optical studies of melanosomes, which are one of the vital organelles in the human eye, also known to be responsible for a disease called age-related macular degeneration (AMD), a condition of advanced degeneration which causes progressive blindness. I used Raman spectroscopy, to first chemically identify the composition of melanosome, and then monitor the changes in its functional and chemical behavior due to long term exposure to visible light. The above study, apart from explaining the role of melanosomes in AMD, also sets the threshold power for lasers used in surgeries and other clinical applications. In the second part of my dissertation, a battery of spectroscopic techniques was successfully applied to explore the different binding sites of lead ions with the most abundant carrier protein molecule in our circulatory system, human serum albumin. I applied optical spectroscopic tools for ultrasensitive detection of heavy metal ions in solution which can also be used for lead detection at a very early stage of lead poisoning. Apart from this, I used Raman microspectroscopy to study the chemical alteration occurring inside a prostate cancer cell as a result of a treatment with a low concentrated aqueous extract of a prospective drug, Nerium Oleander. The experimental methods used in this study has tremendous potential for clinical

  19. 1,1-dimethylhydrazine as a high purity nitrogen source for MOVPE-water reduction and quantification using nuclear magnetic resonance, gas chromatography-atomic emission detection spectroscopy and cryogenic-mass spectroscopy analytical techniques

    SciTech Connect

    Odedra, R.; Smith, L.M.; Rushworth, S.A.

    2000-01-01

    Hydrazine derivatives are attractive low temperature nitrogen sources for use in MOVPE due to their low thermal stability. However their purification and subsequent analysis has not previously been investigated in depth for this application. A detailed study on 1,1-dimethylhydrazine {l{underscore}brace}(CH{sub 3}){sub 2}N-NH{sub 2}{r{underscore}brace} purified by eight different methods and the subsequent quantitative measurements of water present in the samples obtained is reported here. A correlation between {sup 1}H nuclear magnetic resonance spectroscopy (NMR), gas chromatography-atomic emission detection (GC-AED) and cryogenic mass spectroscopy (Cryogenic-MS) has been performed. All three analysis techniques can be used to measure water in the samples and with the best purification the water content can be lowered well below 100 ppm. The high purity of this material has been demonstrated by growth results and the state-of-the-art performance of laser diodes.

  20. AI techniques for a space application scheduling problem

    NASA Technical Reports Server (NTRS)

    Thalman, N.; Sparn, T.; Jaffres, L.; Gablehouse, D.; Judd, D.; Russell, C.

    1991-01-01

    Scheduling is a very complex optimization problem which can be categorized as an NP-complete problem. NP-complete problems are quite diverse, as are the algorithms used in searching for an optimal solution. In most cases, the best solutions that can be derived for these combinatorial explosive problems are near-optimal solutions. Due to the complexity of the scheduling problem, artificial intelligence (AI) can aid in solving these types of problems. Some of the factors are examined which make space application scheduling problems difficult and presents a fairly new AI-based technique called tabu search as applied to a real scheduling application. the specific problem is concerned with scheduling application. The specific problem is concerned with scheduling solar and stellar observations for the SOLar-STellar Irradiance Comparison Experiment (SOLSTICE) instrument in a constrained environment which produces minimum impact on the other instruments and maximizes target observation times. The SOLSTICE instrument will gly on-board the Upper Atmosphere Research Satellite (UARS) in 1991, and a similar instrument will fly on the earth observing system (Eos).

  1. Application of an online ion-chromatography-based instrument for gradient flux measurements of speciated nitrogen and sulfur

    NASA Astrophysics Data System (ADS)

    Rumsey, Ian C.; Walker, John T.

    2016-06-01

    The dry component of total nitrogen and sulfur atmospheric deposition remains uncertain. The lack of measurements of sufficient chemical speciation and temporal extent make it difficult to develop accurate mass budgets and sufficient process level detail is not available to improve current air-surface exchange models. Over the past decade, significant advances have been made in the development of continuous air sampling measurement techniques, resulting with instruments of sufficient sensitivity and temporal resolution to directly quantify air-surface exchange of nitrogen and sulfur compounds. However, their applicability is generally restricted to only one or a few of the compounds within the deposition budget. Here, the performance of the Monitor for AeRosols and GAses in ambient air (MARGA 2S), a commercially available online ion-chromatography-based analyzer is characterized for the first time as applied for air-surface exchange measurements of HNO3, NH3, NH4+, NO3-, SO2 and SO42-. Analytical accuracy and precision are assessed under field conditions. Chemical concentrations gradient precision are determined at the same sampling site. Flux uncertainty measured by the aerodynamic gradient method is determined for a representative 3-week period in fall 2012 over a grass field. Analytical precision and chemical concentration gradient precision were found to compare favorably in comparison to previous studies. During the 3-week period, percentages of hourly chemical concentration gradients greater than the corresponding chemical concentration gradient detection limit were 86, 42, 82, 73, 74 and 69 % for NH3, NH4+, HNO3, NO3-, SO2 and SO42-, respectively. As expected, percentages were lowest for aerosol species, owing to their relatively low deposition velocities and correspondingly smaller gradients relative to gas phase species. Relative hourly median flux uncertainties were 31, 121, 42, 43, 67 and 56 % for NH3, NH4+, HNO3, NO3-, SO2 and SO42-, respectively. Flux

  2. Evaluation of peripheral blood microsampling techniques in combination with liquid chromatography-high resolution mass spectrometry for the determination of drug pharmacokinetics in clinical studies.

    PubMed

    Rincón, Juan P; Meesters, Roland J W

    2014-06-01

    New bioanalytical assays were developed, validated, and applied in a clinical study for quantitative measurement of acetaminophen concentrations in blood and plasma samples. Furthermore, after validation, the bioanalytical assays were used for determination of pharmacokinetics within a group of six healthy male human volunteers after admission of a single oral dose of 500 mg of acetaminophen. Quantitative analyses were done by means of liquid chromatography-high resolution mass spectrometry and blood samples were collected at various sampling time points using different peripheral blood microsampling techniques. Post-dose peripheral collected blood samples were applied for the preparation of dry blood spots, dried matrix on paper discs, and peripheral plasma. Pharmacokinetic parameters determined were clearance (Cl), area under the curve (AUC), volume of distribution (Vd ), peak concentration (Cmax ), time of occurrence of peak concentration (Tmax ) and half-life time (T½ ). Observed pharmacokinetic values were not statistically (ANOVA) different compared to in literature reported values based on venous blood collection. The present pilot study demonstrated the feasibility of peripheral blood microsampling techniques in combination with quantitative liquid chromatography-high resolution mass spectrometry analysis for the determination of pharmacokinetics in clinical studies.

  3. Quantitative determination of diazepam, nitrazepam and flunitrazepam in tablets using thin-layer chromatography-densitometry technique.

    PubMed

    Bakavoli, Mehdi; Kaykhaii, Massoud

    2003-04-10

    A simple and reliable assay for diazepam, nitrazepam and flunitrazepam in tablets by high-performance liquid chromatography (HPLC) and thin-layer chromatography (TLC)-densitometry is described. A quantity of a ground tablet mass, equal to the average weight of one tablet was sonicated in MeOH, mixed with appropriate internal standard, filtered and either injected directly into the liquid chromatograph, or after evaporation and reconstitution of an aliquot of the extract, was spotted on a silica gel thin-layer plate. A variable UV detector, operated at 254 nm was employed in both procedures. A C18, reversed phase 7 microm column was used for HPLC analysis; the mobile phase was a 1:1 (v/v) mixture of MeOH (40 degrees C) and 0.01 M phosphate buffer (pH 7, 80 degrees C). The TLC plate was developed in an unsaturated chromatographic chamber containing 100 ml chloroform-acetone (9:1); at room temperature, the mobile phase was allowed to travel 15 cm. The percentage of the active ingredient content of each tablet obtained by both procedures, was in the range of the stated amount except for one brand of diazepam tablets which contained approximately 23% less active ingredient than the minimum prescribed amount. The TLC densitometry, although yields slightly higher values than the HPLC method, is preferred due to its simplicity, ease and low cost.

  4. An Ultra-Trace Analysis Technique for SF6 Using Gas Chromatography with Negative Ion Chemical Ionization Mass Spectrometry.

    PubMed

    Jong, Edmund C; Macek, Paul V; Perera, Inoka E; Luxbacher, Kray D; McNair, Harold M

    2015-07-01

    Sulfur hexafluoride (SF6) is widely used as a tracer gas because of its detectability at low concentrations. This attribute of SF6 allows the quantification of both small-scale flows, such as leakage, and large-scale flows, such as atmospheric currents. SF6's high detection sensitivity also facilitates greater usage efficiency and lower operating cost for tracer deployments by reducing quantity requirements. The detectability of SF6 is produced by its high molecular electronegativity. This property provides a high potential for negative ion formation through electron capture thus naturally translating to selective detection using negative ion chemical ionization mass spectrometry (NCI-MS). This paper investigates the potential of using gas chromatography (GC) with NCI-MS for the detection of SF6. The experimental parameters for an ultra-trace SF6 detection method utilizing minimal customizations of the analytical instrument are detailed. A method for the detection of parts per trillion (ppt) level concentrations of SF6 for the purpose of underground ventilation tracer gas analysis was successfully developed in this study. The method utilized a Shimadzu gas chromatography with negative ion chemical ionization mass spectrometry system equipped with an Agilent J&W HP-porous layer open tubular column coated with an alumina oxide (Al2O3) S column. The method detection limit (MDL) analysis as defined by the Environmental Protection Agency of the tracer data showed the method MDL to be 5.2 ppt.

  5. Improving accuracy in the quantitation of overlapping, asymmetric, chromatographie peaks by deconvolution: theory and application to coupled gas chromatography atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Johansson, M.; Berglund, M.; Baxter, D. C.

    1993-09-01

    Systematic errors in the measurement of overlapping asymmetric, Chromatographic peaks are observed using the perpendicular-drop and tangent-skimming algorithms incorporated in commercial integrators. The magnitude of such errors increases with the degree of tailing and differences in peak size, and was found to be as great as 80% for peak-area and 100% for peak-height measurements made on the smaller, second component of simulated, noise-free chromatograms containing peaks at a size ratio of 10 to 1. Initial deconvolution of overlapping peaks, by mathematical correction for asymmetry, leads to significant improvements in the accuracy of both peak-area and height measurements using the simple, perpendicular-drop algorithm. A comparison of analytical data for the separation and determination of three organolead species by coupled gas chromatography atomic absorption spectrometry using peak-height and area measurements also demonstrates the improved accuracy obtained following deconvolution. It is concluded that the deconvolution method described could be beneficial in a variety of Chromatographic applications where overlapping, asymmetric peaks are observed.

  6. Spaceborne synthetic-aperture imaging radars - Applications, techniques, and technology

    NASA Technical Reports Server (NTRS)

    Elachi, C.; Bicknell, T.; Jordan, R. L.; Wu, C.

    1982-01-01

    In June 1978, the Seasat satellite was placed into orbit around the earth with a synthetic-aperture imaging radar (SAR) as one of the payload sensors. The Seasat SAR provided, for the first time, synoptic radar images of the earth's surface with a resolution of 25 m. In November 1981, the second imaging radar was successfully operated from space on the Shuttle. The Shuttle Imaging Radar-A acquired images over a variety of regions around the world with an imaging geometry different from the one used by the Seasat SAR. The spaceborne SAR principle is discussed, taking into account ambiguities, orbital and environmental factors, range curvature and range walk, surface interaction mechanisms, thermal and speckle noise, key tradeoff parameters, and nonconventional SAR systems. Attention is also given to spaceborne SAR sensors, the digital processing of spaceborne SAR data, the optical processing of spaceborne SAR data, postimage formation processing, data interpretation techniques and applications, and the next decade.

  7. An ultra-low-power filtering technique for biomedical applications.

    PubMed

    Zhang, Tan-Tan; Mak, Pui-In; Vai, Mang-I; Mak, Peng-Un; Wan, Feng; Martins, R P

    2011-01-01

    This paper describes an ultra-low-power filtering technique for biomedical applications designated as T-wave sensing in heart-activities detection systems. The topology is based on a source-follower-based Biquad operating in the sub-threshold region. With the intrinsic advantages of simplicity and high linearity of the source-follower, ultra-low-cutoff filtering can be achieved, simultaneously with ultra low power and good linearity. An 8(th)-order 2.4-Hz lowpass filter design example optimized in a 0.35-μm CMOS process was designed achieving over 85-dB dynamic range, 74-dB stopband attenuation and consuming only 0.36 nW at a 3-V supply.

  8. Imaging In focus: Reflected light imaging: Techniques and applications.

    PubMed

    Guggenheim, Emily J; Lynch, Iseult; Rappoport, Joshua Z

    2017-02-01

    Reflectance imaging is a broad term that describes the formation of images by the detection of illumination light that is back-scattered from reflective features within a sample. Reflectance imaging can be performed in a variety of different configurations, such as confocal, oblique angle illumination, structured illumination, interferometry and total internal reflectance, permitting a plethora of biomedical applications. Reflectance imaging has proven indispensable for critical investigations into the safety and understanding of biomedically and environmentally relevant nano-materials, an area of high priority and investment. The non-destructive in vivo imaging ability of reflectance techniques permits alternative diagnostic strategies that may eventually facilitate the eradication of some invasive biopsy procedures. Reflectance can also provide additional structural information and clarity necessary in fluorescent based in vivo studies. Near-coverslip interrogation techniques, such as reflectance interferometry and total internal reflection, have provided a label free means to investigate cell-surface contacts, cell motility and vesicle trafficking in vivo and in vitro. Other key advances include the ability to acquire superresolution reflectance images providing increased spatial resolution.

  9. Surgical Tips in Frozen Abdomen Management: Application of Coliseum Technique.

    PubMed

    Kyriazanos, Ioannis D; Manatakis, Dimitrios K; Stamos, Nikolaos; Stoidis, Christos

    2015-01-01

    Wound dehiscence is a serious postoperative complication, with an incidence of 0.5-3% after primary closure of a laparotomy incision, and represents an acute mechanical failure of wound healing. Relatively recently the concept of "intentional open abdomen" was described and both clinical entities share common pathophysiological and clinical pathways ("postoperative open abdominal wall"). Although early reconstruction is the target, a significant proportion of patients will develop adhesions between abdominal viscera and the anterolateral abdominal wall, a condition widely recognized as "frozen abdomen," where delayed wound closure appears as the only realistic alternative. We report our experience with a patient who presented with frozen abdomen after wound dehiscence due to surgical site infection and application of the "Coliseum technique" for its definitive surgical management. This novel technique represents an innovative alternative to abdominal exploration, for cases of "malignant" frozen abdomen due to peritoneal carcinomatosis. Lifting the edges of the surgical wound upwards and suspending them under traction by threads from a retractor positioned above the abdomen facilitates approach to the peritoneal cavity, optimizes exposure of intra-abdominal organs, and prevents operative injury to the innervation and blood supply of abdominal wall musculature, a crucial step for subsequent hernia repair.

  10. Investigating Coincidence Techniques in Biomedical Applications of Neutron Activation Analysis

    NASA Astrophysics Data System (ADS)

    Chowdhury, P.; Gramer, R.; Tandel, S. K.; Reinhardt, C. J.

    2004-05-01

    While neutron activation analysis has been widely used in biomedical applications for some time, the use of non-radioactive tracer techniques, to monitor, for example, organ blood flow, is more recent. In these studies, pre-clinical animal models are injected with micro-spheres labeled with stable isotopes of elements that have a high neutron absorption cross-section. Subsequently, samples of blood and/or tissue from different locations in the body are subjected to neutron activation analysis to measure the propagation of the labeled micro-spheres through the body. Following irradiation, the counting (with high-resolution Ge detectors) is typically delayed by a few days to dissipate short-lived activity in the samples and improve signal-to-noise for the peaks of interest in the activation spectrum. The aim of the present study was to investigate whether coincidence techniques (for isotopes which decay via two-photon cascades) could improve signal-to-noise and turn-around times. The samples were irradiated at the 1 MW research reactor at the UMass Lowell Radiation Laboratory. The analysis of the multi-parameter coincidence data recorded in event-mode will be presented and compared with the standard method of recording singles spectra.

  11. Nonlinear plasmonic imaging techniques and their biological applications

    NASA Astrophysics Data System (ADS)

    Deka, Gitanjal; Sun, Chi-Kuang; Fujita, Katsumasa; Chu, Shi-Wei

    2017-01-01

    Nonlinear optics, when combined with microscopy, is known to provide advantages including novel contrast, deep tissue observation, and minimal invasiveness. In addition, special nonlinearities, such as switch on/off and saturation, can enhance the spatial resolution below the diffraction limit, revolutionizing the field of optical microscopy. These nonlinear imaging techniques are extremely useful for biological studies on various scales from molecules to cells to tissues. Nevertheless, in most cases, nonlinear optical interaction requires strong illumination, typically at least gigawatts per square centimeter intensity. Such strong illumination can cause significant phototoxicity or even photodamage to fragile biological samples. Therefore, it is highly desirable to find mechanisms that allow the reduction of illumination intensity. Surface plasmon, which is the collective oscillation of electrons in metal under light excitation, is capable of significantly enhancing the local field around the metal nanostructures and thus boosting up the efficiency of nonlinear optical interactions of the surrounding materials or of the metal itself. In this mini-review, we discuss the recent progress of plasmonics in nonlinear optical microscopy with a special focus on biological applications. The advancement of nonlinear imaging modalities (including incoherent/coherent Raman scattering, two/three-photon luminescence, and second/third harmonic generations that have been amalgamated with plasmonics), as well as the novel subdiffraction limit imaging techniques based on nonlinear behaviors of plasmonic scattering, is addressed.

  12. A planar Mie scattering visualization technique for turbo machinery application

    NASA Astrophysics Data System (ADS)

    Gawehn, Thomas; Schodl, Richard

    2007-12-01

    A planar Mie scattering technique is described which allows for the systematical analysis of three-dimensional shock configurations without the need for velocity measurements. For that, small particles are added to the flow upstream of the shock and illuminated by a laser light sheet. The scattered light is captured by a CCD camera so that the position of the shock wave can be determined from the increase of the light intensity across the shock. To analyze the three-dimensional structure of a shock wave, the light sheet is moved perpendicular to the flow direction. The measurement technique is applied to both a supersonic wedge flow at Ma = 2.43 and a more complex shock wave configuration in a transonic cascade flow at Ma = 1.09. The gathered results are conclusive with Schlieren photographs, numerical simulations and surface pressure measurements. As the chosen setup allows the application to test sections with restricted optical access and a synchronization of the image capturing process with an external triggering signal, the three-dimensional shock configurations inside a transonic compressor rotor can also be visualized.

  13. Nonlinear plasmonic imaging techniques and their biological applications

    NASA Astrophysics Data System (ADS)

    Deka, Gitanjal; Sun, Chi-Kuang; Fujita, Katsumasa; Chu, Shi-Wei

    2016-07-01

    Nonlinear optics, when combined with microscopy, is known to provide advantages including novel contrast, deep tissue observation, and minimal invasiveness. In addition, special nonlinearities, such as switch on/off and saturation, can enhance the spatial resolution below the diffraction limit, revolutionizing the field of optical microscopy. These nonlinear imaging techniques are extremely useful for biological studies on various scales from molecules to cells to tissues. Nevertheless, in most cases, nonlinear optical interaction requires strong illumination, typically at least gigawatts per square centimeter intensity. Such strong illumination can cause significant phototoxicity or even photodamage to fragile biological samples. Therefore, it is highly desirable to find mechanisms that allow the reduction of illumination intensity. Surface plasmon, which is the collective oscillation of electrons in metal under light excitation, is capable of significantly enhancing the local field around the metal nanostructures and thus boosting up the efficiency of nonlinear optical interactions of the surrounding materials or of the metal itself. In this mini-review, we discuss the recent progress of plasmonics in nonlinear optical microscopy with a special focus on biological applications. The advancement of nonlinear imaging modalities (including incoherent/coherent Raman scattering, two/three-photon luminescence, and second/third harmonic generations that have been amalgamated with plasmonics), as well as the novel subdiffraction limit imaging techniques based on nonlinear behaviors of plasmonic scattering, is addressed.

  14. Application of computerized tomography techniques to tokamak diagnostics

    NASA Astrophysics Data System (ADS)

    Stalker, K. T.; Kelly, J. G.

    1980-08-01

    A Coded Aperture Imaging System (CAIS) has been developed at Sandia National Laboratories to image the motion of nuclear fuel rods undergoing tests simulating accident conditions within a liquid metal fast breeder reactor. The tests require that the motion of the test fuel be monitored while it is immersed in a liquid sodium coolant precluding the use of normal optical means of imaging. However, using the fission gamma rays emitted by the fuel itself and coded aperture techniques, images with 1.5 mm radial and 5 mm axial resolution have been attained. Using an electro-optical detection system coupled to a high speed motion picture camera a time resolution of one millisecond can be achieved. This paper will discuss the application of coded aperture imaging to the problem, including the design of the one-dimensional Fresnel zone plate apertures used and the special problems arising from the reactor environment and use of high energy gamma ray photons to form the coded image. Also to be discussed will be the reconstruction techniques employed and the effect of various noise sources on system performance. Finally, some experimental results obtained using the system will be presented.

  15. pH-zone-refining counter-current chromatography: origin, mechanism, procedure and applications.

    PubMed

    Ito, Yoichiro

    2013-01-04

    Since 1980, high-speed counter-current chromatography (HSCCC) has been used for separation and purification of natural and synthetic products in a standard elution mode. In 1991, a novel elution mode called pH-zone refining CCC was introduced from an incidental discovery that an organic acid in the sample solution formed the sharp peak of an acid analyte. The cause of this sharp peak formation was found to be bromoacetic acid present in the sample solution which formed a sharp trailing border to trap the acidic analyte. Further studies on the separation of DNP-amino acids with three spacer acids in the stationary phase revealed that increased sample size resulted in the formation of fused rectangular peaks, each preserving high purity and zone pH with sharp boundaries. The mechanism of this phenomenon was found to be the formation of a sharp trailing border of an acid (retainer) in the column which moves at a lower rate than that of the mobile phase. In order to facilitate the application of the method, a new method was devised using a set of retainer and eluter to form a sharp retainer rear border which moves through the column at a desired rate regardless of the composition of the two-phase solvent system. This was achieved by adding the retainer in the stationary phase and the eluter in the mobile phase at a given molar ratio. Using this new method the hydrodynamics of pH-zone-refining CCC was diagrammatically illustrated by three acidic samples. In this review paper, typical pH-zone-refining CCC separations were presented, including affinity separations with a ligand and a separation of a racemic mixture using a chiral selector in the stationary phase. Major characteristics of pH-zone-refining CCC over conventional HSCCC are as follows: the sample loading capacity is increased over 10 times; fractions are highly concentrated near saturation level; yield is improved by increasing the sample size; minute charged compounds are concentrated and detected at the peak

  16. Multiplex gas chromatography

    NASA Technical Reports Server (NTRS)

    Valentin, Jose R.

    1990-01-01

    The principles of the multiplex gas chromatography (GC) technique, which is a possible candidate for chemical analysis of planetary atmospheres, are discussed. Particular attention is given to the chemical modulators developed by present investigators for multiplex GC, namely, the thermal-desorption, thermal-decomposition, and catalytic modulators, as well as to mechanical modulators. The basic technique of multiplex GC using chemical modulators and a mechanical modulator is demonstrated. It is shown that, with the chemical modulators, only one gas stream consisting of the carrier in combination with the components is being analyzed, resulting in a simplified instrument that requires relatively few consumables. The mechanical modulator demonstrated a direct application of multiplex GC for the analysis of gases in atmosphere of Titan at very low pressures.

  17. Advanced proteomic liquid chromatography

    SciTech Connect

    Xie, Fang; Smith, Richard D.; Shen, Yufeng

    2012-10-26

    Liquid chromatography coupled with mass spectrometry is the predominant platform used to analyze proteomics samples consisting of large numbers of proteins and their proteolytic products (e.g., truncated polypeptides) and spanning a wide range of relative concentrations. This review provides an overview of advanced capillary liquid chromatography techniques and methodologies that greatly improve separation resolving power and proteomics analysis coverage, sensitivity, and throughput.

  18. Column Liquid Chromatography.

    ERIC Educational Resources Information Center

    Majors, Ronald E.; And Others

    1984-01-01

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

  19. Infrared band strengths: Laboratory techniques and applications to astronomical observations

    NASA Astrophysics Data System (ADS)

    Gerakines, P. A.

    2002-09-01

    Whenever an abundance measurement is derived by way of infrared spectroscopy, it will typically make use of a laboratory-obtained conversion factor between the size of an IR absorption feature and the (column) density of the molecule under study. This factor is usually called the "absolute absorption intensity" by a chemist or the "band strength" by a typical IR astronomer. Band strengths have been studied in chemistry since the 1950s, and the commonly quoted "accuracy to with a factor of ten" historically required of astronomical calculations has not required much new input into this area. Today, however, astronomical measurements require much higher precision, and it is time for IR astronomers to ask more of laboratory measurements and to understand when and why to use IR band strengths in a more appropriate manner. The history, interpretation, measurement, and common astrophysical applications of infrared band strengths will be discussed. The "secrets" of the laboratory techniques involved in their measurement are described, and a compilation of results from the literature is given along with some new results. Typical astrophysical applications and appropriate uses will also be discussed. Common misconceptions are confronted and two challenges are presented: (i) to the laboratory astrophysics community to produce and advertise accurate values with caveats when necessary, and (ii) to the observational community to use the most appropriate results for the environment under study.

  20. Processing Techniques and Applications of Silk Hydrogels in Bioengineering

    PubMed Central

    Floren, Michael; Migliaresi, Claudio; Motta, Antonella

    2016-01-01

    Hydrogels are an attractive class of tunable material platforms that, combined with their structural and functional likeness to biological environments, have a diversity of applications in bioengineering. Several polymers, natural and synthetic, can be used, the material selection being based on the required functional characteristics of the prepared hydrogels. Silk fibroin (SF) is an attractive natural polymer for its excellent processability, biocompatibility, controlled degradation, mechanical properties and tunable formats and a good candidate for the fabrication of hydrogels. Tremendous effort has been made to control the structural and functional characteristic of silk hydrogels, integrating novel biological features with advanced processing techniques, to develop the next generation of functional SF hydrogels. Here, we review the several processing methods developed to prepare advanced SF hydrogel formats, emphasizing a bottom-up approach beginning with critical structural characteristics of silk proteins and their behavior under specific gelation environments. Additionally, the preparation of SF hydrogel blends and other advanced formats will also be discussed. We conclude with a brief description of the attractive utility of SF hydrogels in relevant bioengineering applications. PMID:27649251

  1. Multi-mode application of graphene quantum dots bonded silica stationary phase for high performance liquid chromatography.

    PubMed

    Wu, Qi; Sun, Yaming; Zhang, Xiaoli; Zhang, Xia; Dong, Shuqing; Qiu, Hongdeng; Wang, Litao; Zhao, Liang

    2017-04-07

    Graphene quantum dots (GQDs), which possess hydrophobic, hydrophilic, π-π stacking and hydrogen bonding properties, have great prospect in HPLC. In this study, a novel GQDs bonded silica stationary phase was prepared and applied in multiple separation modes including normal phase, reversed phase and hydrophilic chromatography mode. Alkaloids, nucleosides and nucleobases were chosen as test compounds to evaluate the separation performance of this column in hydrophilic chromatographic mode. The tested polar compounds achieved baseline separation and the resolutions reached 2.32, 4.62, 7.79, 1.68 for thymidine, uridine, adenosine, cytidine and guanosine. This new column showed satisfactory chromatographic performance for anilines, phenols and polycyclic aromatic hydrocarbons in normal and reversed phase mode. Five anilines were completely separated within 10min under the condition of mobile phase containing only 10% methanol. The effect of water content, buffer concentration and pH on chromatographic separation was further investigated, founding that this new stationary phase showed a complex retention mechanism of partitioning, adsorption and electrostatic interaction in hydrophilic chromatography mode, and the multiple retention interactions such as π-π stacking and π-π electron-donor-acceptor interaction played an important role during the separation process. This GQDs bonded column, which allows us to adjust appropriate chromatography mode according to the properties of analytes, has possibility in actual application after further research.

  2. Application of Ion Chromatography to the Investigation of Real-World Samples

    ERIC Educational Resources Information Center

    Whelan, Rebecca J.; Hannon, Theresa E.; Zare, Richard N.

    2004-01-01

    The use of ion chromatography (IC) as a means to teach important analytical concepts while giving the students a valuable opportunity to identify and investigate a real-world system of interest to them is described. A single IC apparatus can be tailored for different classes of analyses by the selection of different column-eluent combinations.

  3. Fourier transform-infrared spectroscopy and Gas chromatography-mass spectroscopy: reliable techniques for analysis of Parthenium mediated vermicompost.

    PubMed

    Rajiv, P; Rajeshwari, Sivaraj; Venckatesh, Rajendran

    2013-12-01

    Fourier transform infrared spectroscopy (FT-IR) and Gas chromatography-mass spectroscopy have been carried out to investigate the chemical composition of Parthenium mediated vermicompost. Four different concentrations of Parthenium and cow dung mixtures were vermicomposted using the earthworms (Eudrilus eugeniae). FT-IR spectra reveal the absence of Parthenin toxin (sesquiterpene lactone) and phenols in vermicompost which was obtained from high concentration of cow dung mixed treatments. GC-MS analysis shows no phenolic compounds and predominant level of intermediate metabolites such as 4,8,12,16-Tetramethylheptadecan-4-olide (7.61%), 2-Pentadecanone, 6,10,14-trimethyl- (5.29%) and Methyl 16-methyl-heptadecanoate (4.69%) during the vermicomposting process. Spectral results indicated that Parthenin toxin and phenols can be eradicated via vermicomposting if mixed with appropriate quantity of cow dung.

  4. Fourier transform-infrared spectroscopy and Gas chromatography-mass spectroscopy: Reliable techniques for analysis of Parthenium mediated vermicompost

    NASA Astrophysics Data System (ADS)

    Rajiv, P.; Rajeshwari, Sivaraj; Venckatesh, Rajendran

    2013-12-01

    Fourier transform infrared spectroscopy (FT-IR) and Gas chromatography-mass spectroscopy have been carried out to investigate the chemical composition of Parthenium mediated vermicompost. Four different concentrations of Parthenium and cow dung mixtures were vermicomposted using the earthworms (Eudrilus eugeniae). FT-IR spectra reveal the absence of Parthenin toxin (sesquiterpene lactone) and phenols in vermicompost which was obtained from high concentration of cow dung mixed treatments. GC-MS analysis shows no phenolic compounds and predominant level of intermediate metabolites such as 4,8,12,16-Tetramethylheptadecan-4-olide (7.61%), 2-Pentadecanone, 6,10,14-trimethyl- (5.29%) and Methyl 16-methyl-heptadecanoate (4.69%) during the vermicomposting process. Spectral results indicated that Parthenin toxin and phenols can be eradicated via vermicomposting if mixed with appropriate quantity of cow dung.

  5. Analytical Electrochemistry: Methodology and Applications of Dynamic Techniques.

    ERIC Educational Resources Information Center

    Heineman, William R.; Kissinger, Peter T.

    1980-01-01

    Reports developments involving the experimental aspects of finite and current analytical electrochemistry including electrode materials (97 cited references), hydrodynamic techniques (56), spectroelectrochemistry (62), stripping voltammetry (70), voltammetric techniques (27), polarographic techniques (59), and miscellany (12). (CS)

  6. Mass spectrometry detection in comprehensive liquid chromatography: basic concepts, instrumental aspects, applications and trends.

    PubMed

    Donato, Paola; Cacciola, Francesco; Tranchida, Peter Quinto; Dugo, Paola; Mondello, Luigi

    2012-01-01

    The review, as can be deduced from the title, focuses on both theoretical and practical aspects of the use of mass spectrometry as a third, added dimension to a comprehensive LC (LC × LC) system, generating the most powerful analytical tool today for non-volatile analytes. The first part deals with the technical requirements for linkage of an LC × LC system to an MS one, including the choice of the mobile phase (buffer and salts), flow rate (splitting), type of ionization (interface); advantages and disadvantages of off-line and on-line methods are discussed, as well. A discussion of the various aspects of instrumentation is provided, both from a chromatographic and mass spectrometry standpoint, with particular emphasis directed to the choice of column sets, spatial resolution, mass resolving power, mass accuracy, and tandem-MS capabilities. The extent to which mass spectrometry may be of aid in unraveling column-outlet multicompound bands is highlighted, along with its effectiveness as a chromatographic detector of excellent sensitivity, universality yet with potential in terms of selectivity and amenability to quantitative analysis over a wide dynamic range. The following section of the review contains significant applications of comprehensive two-dimensional LC coupled to MS in different areas of research, with details on interfaces, column stationary phases, modulation and MS parameters. It is not the intention of the authors to provide a comprehensive description of the techniques, but merely to discuss only those aspects which are essential for successful applications of the LC-MS combination. The reader will be acquainted with the enormous potential of this hyphenated technique, and the factors and instrumental developments that have concurred to make it emerge to a central role in specialized fields, such as proteomics.

  7. Geochemical Exploration Techniques Applicable in the Search for Copper Deposits

    USGS Publications Warehouse

    Chaffee, Maurice A.

    1975-01-01

    media. Samples of ice and snow have been used for limited geochemical surveys. Both geobotanical and biogeochemical surveys have been successful in locating copper deposits in many parts of the world. Micro-organisms, including bacteria and algae, are other unproved media that should be studied. Animals can be used in geochemical-prospecting programs. Dogs have been used quite successfully to sniff out hidden and exposed sulfide minerals. Tennite mounds are commonly composed of subsurface material, but have not as yet proved to be useful in locating buried mineral deposits. Animal tissue and waste products are essentially unproved but potentially valuable sampling media. Knowledge of the location of areas where trace-element-associated diseases in animals and man are endemic as well as a better understanding of these diseases, may aid in identifying regions that are enriched in or depleted of various elements, including copper. Results of analyses of gases in the atmosphere are proving valuable in mineral-exploration surveys. Studies involving metallic compounds exhaled by plants into the atmosphere, and of particulate matter suspended in the atmosphere are reviewed these methods may become important in the future. Remote-sensing techniques are useful for making indirect measurements of geochemical responses. Two techniques applicable to geochemical exploration are neutron-activation analysis and gamma-ray spectrometry. Aerial photography is especially useful in vegetation surveys. Radar imagery is an unproved but potentially valuable method for use in studies of vegetation in perpetually clouded regions. With the advent of modern computers, many new techniques, such as correlation analysis, regression analysis, discriminant analysis, factor analysis, cluster analysis, trend-surface analysis, and moving-average analysis can be applied to geochemical data sets. Selective use of these techniques can provide new insights into the interpretatio

  8. Gas chromatography for space exploration : application to the in situ analysis of Titan's atmosphere, comets nucleus and martian soil

    NASA Astrophysics Data System (ADS)

    Sternberg, R.; Szopa, C.; Buch, A.; Mettetal, F.; Coscia, D.; Coll, P.; Cabane, M.; Rodier, C.; Vidal-Madjar, C.; Raulin, F.

    Gas chromatography is one of the most powerful technique for the in situ chemical investigation of extraterrestrial environments Its successful use in past planetary missions to Mars 1976-78 and Venus 1978-85 made it the main method selected for the in situ molecular characterization of the Titan s atmosphere comets and the Martian soil Indeed gas chromatography fully meet the severe constraints required in space instrumentation such as small weight and size low power consumption high mechanical strength and resistance to deep space conditions vacuum cosmic rays This paper presents the gas chromatographic subsystems which have been developed at LISA and SA respectively for the Huygens probe of the Cassini-Huygens mission to Titan 1 the Philae probe of the Rosetta mission to a comet 2 and the future landing probe of the MSL 2009 mission to Mars 3 The coupling of these GC subsystems with pyrolysis and chemical derivatization techniques allows the chemical analysis of a wide range of molecules including non-volatiles complex organics such as aminoacides and nucleobases the search of wich is of particular interest for exobiology The analytical capabilities of these subsystems with a particular emphasis of their exobiological aspects and implications are described 1 G Israel C Szopa F Raulin M Cabane P Coll R Sternberg et al Nature vol438 796-799 2005 2 C Szopa R Sternberg F Raulin and H Rosenbauer PSS 863-877 2003 3 Cabane M P Coll C Szopa G Isra e l F Raulin

  9. Liquid chromatography-tandem mass spectrometry application, for the determination of extracellular hepatotoxins in Irish lake and drinking waters.

    PubMed

    Allis, Orla; Dauphard, Justine; Hamilton, Brett; Shuilleabhain, Aine Ni; Lehane, Mary; James, Kevin J; Furey, Ambrose

    2007-05-01

    A novel method for the determination of hepatotoxins; microcystins (MCs), and nodularin (Nod) in lake water and domestic chlorinated tap water has been developed using liquid chromatography hyphenated with electrospray ionization triple quadrupole mass spectrometry (LC-ESI-MS/MS). Optimization of the mass spectrometer parameters and mobile-phase composition was performed to maximize the sensitivity and reproducibility of the method. Detection of the hepatotoxins was carried out using multiple reaction monitoring experiments, thus improving the selectivity of the method. A total ion chromatogram and a precursor ion scan on ion m/z 135 was also applied to all samples to detect unknown microcystins or microcystins for which there are no standards available. A comprehensive validation of the LC-ESI-MS/MS method was completed that took into account matrix effects, specificity, linearity, accuracy, and precision. Good linear calibrations were obtained for MC-LR (1-200 microg/L; R2=0.9994) in spiked lake and tap water samples (1-50 microg/L; R2=0.9974). Acceptable interday repeatability was achieved for MC-LR in lake water with RSD values (n=9) ranging from 9.9 (10 microg/L) to 5.1% (100 microg/L). Excellent limits of detection (LOD) and limits of quantitation (LOQ) were achieved with spiked MCs and Nod samples; LOD=0.27 microg/L and LOQ=0.90 microg/L for MC-LR in the "normal linear range" and LOD=0.08 microg/L and LOQ=0.25 microg/L in the "low linear range" in both lake and chlorinated tap water. Similar results were obtained for a suite of microcystins and nodularin. This sensitive and rapid method does not require any sample preconcentration, including the elimination of solid-phase extraction (SPE) for the effective screening of hepatotoxins in water below the 1 microg/L WHO provisional guideline limit for MC-LR. Furthermore, SPE techniques are time-consuming, nonreproducible at trace levels, and offer poor recoveries with chlorinated water. The application of this LC

  10. Application of capillary gas chromatography to the study of hydrolysis of the nerve agent VX in rat plasma.

    PubMed

    Bonierbale, E; Debordes, L; Coppet, L

    1997-01-24

    We present here a gas chromatography technique allowing the detection and quantification of VX [O-ethyl S-(2-diisopropylaminoethyl)methylphosphonothiolate] as well as its P-S bond hydrolysis product diisopropylaminoethanethiol directly from spiked rat plasma. This technique was applied to study VX hydrolysis in rat plasma. We observed that 53 +/- 4% of 374 microM VX disappeared from spiked plasma after 2 h. VX disappearance was mainly related to enzymatic cleavage of the P-S bond (Km = 2.5 mM and Vmax = 13.3 nmol min-1 ml-1 of rat plasma). The activity was totally inhibited by 1 mM Hg2+ and was also inhibited by metal chelators.

  11. Applications of pattern recognition techniques to online fault detection

    SciTech Connect

    Singer, R.M.; Gross, K.C.; King, R.W.

    1993-11-01

    A common problem to operators of complex industrial systems is the early detection of incipient degradation of sensors and components in order to avoid unplanned outages, to orderly plan for anticipated maintenance activities and to assure continued safe operation. In such systems, there usually are a large number of sensors (upwards of several thousand is not uncommon) serving many functions, ranging from input to control systems, monitoring of safety parameters and component performance limits, system environmental conditions, etc. Although sensors deemed to measure important process conditions are generally alarmed, the alarm set points usually are just high-low limits and the operator`s response to such alarms is based on written procedures and his or her experience and training. In many systems this approach has been successful, but in situations where the cost of a forced outage is high an improved method is needed. In such cases it is desirable, if not necessary, to detect disturbances in either sensors or the process prior to any actual failure that could either shut down the process or challenge any safety system that is present. Recent advances in various artificial intelligence techniques have provided the opportunity to perform such functions of early detection and diagnosis. In this paper, the experience gained through the application of several pattern-recognition techniques to the on-line monitoring and incipient disturbance detection of several coolant pumps and numerous sensors at the Experimental Breeder Reactor-II (EBR-II) which is located at the Idaho National Engineering Laboratory is presented.

  12. The innovative application of surface geophysical techniques for remedial investigations

    SciTech Connect

    Saunders, W.R.; Smith, S.; Gilmore, P.; Cox, S.

    1993-03-01

    When researchers are investigating potential subsurface contamination at hazardous waste landfills, the surface geophysical techniques they may use are often limited. Many geophysical surveys are concerned with areas next to and not directly within the landfill units. The highly variable properties of the materials within the landfill may result in geophysical data that are either difficult or impossible to interpret. Therefore, contamination at these sites may not be detected until substantial lateral migration away from the unit has occurred. In addition, because of the poor resolution of some techniques, the landfill as a whole must be considered as a source, where discrete disposal areas within landfill units may be the actual point sources of contaminants. In theory, if specific sources within the landfill are identified and isolated, then reduced time, effort, and expenditures will be required for remediation activities. In the summer of 1989, the Idaho National Engineering Laboratory (INEL) investigated a small potentially hazardous waste landfill to determine if contaminant hot spots could be identified within the landfill and to determine if significant vertical and lateral migration of contaminants was occurring away from these locations. Based on the present hydrogeologic conditions, researchers anticipated that subsurface flow would be primarily vertical, with the zone of saturation at a depth greater than 150 meters. This necessitated that the survey be performed, for the most part, directly on the capped portion of the landfill. Focused geophysical surveys conducted off the landfill would not have provided useful information concerning conditions directly beneath the landfill. This paper discusses the planning, application, and analysis of four combined sensing methods: two methods of electromagnetic induction [low induction (Em) and time domain (TEM)], ground penetrating radar (GPR), and soil gas.

  13. Autumn Leaf Chromatography.

    ERIC Educational Resources Information Center

    Scharmann, Lawrence C.

    1984-01-01

    Describes an experiment designed to introduce students to chromatographic techniques. Also describes a teacher demonstration in which leaves obtained during the spring and fall are analyzed using chromatography. Procedures for both the experiment and the demonstration are outlined. (JN)

  14. Application of micellar liquid chromatography for the determination of antitumoral and antiretroviral drugs in plasma.

    PubMed

    Peris-Vicente, Juan; Casas-Breva, Inmaculada; Roca-Genovés, Pasqual; Esteve-Romero, Josep

    2014-01-01

    In micellar liquid chromatography, the mobile phase is made of a surfactant and, eventually, an alcohol. This article describes several methods to measure the concentration of antitumoral and antiretroviral drugs in plasma, utilizing micellar liquid chromatography. Samples can be injected after dilution with a micellar solution and filtration, because proteins and other endogenous compounds are solubilized in micellar medium. We will discuss the following optimized parameters: dilution ratio, type of column, detection conditions and mobile phase composition. This article will also cover the validation performed following the International Conference on Harmonization guidelines and the results reported in the literature, indicating that the methods are useful for the routine analysis of plasma samples for clinical purposes.

  15. Applicability of the modified universal calibration of gel permeation chromatography on proteins.

    PubMed

    Dondos, Anastasios

    2006-09-15

    The modified universal calibration of gel permeation chromatography (GPC) has been applied in the case of native proteins. Plotting log([eta]M/Phi) versus elution volume, instead of log[eta]M versus elution volume used till now, we obtain unique curves with different proteins and non-proteonic polymers ([eta]: intrinsic viscosity, M: molecular mass, Phi: Flory's parameter). The values of Flory's parameter Phi are calculated for each protein using an indirect method based on GPC.

  16. Development of Backscatter X-Ray Imaging Techniques for Space Vehicle Applications

    NASA Technical Reports Server (NTRS)

    Bartha, Bence B.; Hope, Dale; Vona, Paul; Born, Martin; Corak, Tony

    2009-01-01

    This slide presentation reviews the development of backscatter x ray (BSX) imaging techniques to perform inspection of spacecraft components. The techniques are currently being enhanced to advance Non-Destructive Testing (NDT) methods for future space vehicle applications. The presentation includes an overview of x ray techniques, a description of current BSX applications used on the space shuttle, the development for Constellation applications, and the use of the system for foam applications.

  17. Simultaneous Quantitative Analysis of Olmesartan Medoxomil and Amlodipine Besylate in Plasma by High-performance Liquid Chromatography Technique

    PubMed Central

    Shah, SK; Asnani, AJ; Kawade, DP; Dangre, SC; Arora, SK; Yende, SR

    2012-01-01

    A rapid, simple and sensitive high-performance liquid chromatography (HPLC) method has been developed for quantification of olmesartan medoxomil (OLM) and amlodipine besylate (AM) in plasma. The assay enables the measurement of OLM and AM for therapeutic drug monitoring with a minimum detectable limit of 2 ng mL. The method involves a simple, one-step extraction procedure and analytical recovery was above 50%. The separation was performed on an analytical 250 × 4.6 mm Eurospher 100-5 C18 column. The wavelength was set at 239 nm. The mobile phase was a mixture of acetonitrile:0.05 M ammonium acetate buffer: 0.1 mL triethylamine at pH 6.8 was selected at a flow rate of 1.0 mL min. The calibration curve for the determination of OLM and AM in plasma was linear over the range 2–2500 and 8–10,000 ng mL AM and OLM. The coefficients of variation for interday and intraday assay were found to be <15%. The method can be applied to a pharmacokinetic and pharmacodynamic study of OLM and AM in a combined dosage form. PMID:22754260

  18. Stability-indicating micellar electrokinetic chromatography technique for simultaneous measurement of delapril and manidipine from a combination drug formulation.

    PubMed

    Todeschini, Vítor; Sangoi, Maximiliano da Silva; Meira, Alianise da Silva; Miron, Diogo; Lange, Alini Dall Cortivo; Volpato, Nadia Maria

    2014-01-01

    A stability-indicating micellar electrokinetic chromatography (MEKC) method was developed and validated for simultaneous analysis of delapril (DEL) and manidipine (MAN) using salicylic acid as an internal standard. The MEKC method was performed using a fused-silica capillary (effective length of 72 cm) with 50 mM of borate buffer and 5 mM of anionic surfactant sodium dodecylsulfate at pH 9.0 as the background electrolyte. The separation was achieved at 25 kV applied voltage and 35 degrees C. The injection was performed at 50 mbar for 5 s, with detection at 208 nm. The method was linear in the range of 15-150 microg/mL (r2 = 0.9966) for DEL and 5-50 microg/mL (r2 = 0.9985) for MAN with adequate results for the precision (< or = 1.87%) and accuracy (98.94% for DEL and 100.65% for MAN). The specificity of the method and its stability-indicating capability was demonstrated through forced degradation studies, which showed that there was no interference from the excipients. The Plackett-Burman experimental design was used for robustness evaluation, giving results within the acceptable range. The method was successfully applied for analysis of the drugs, and the results were compared to an LC method, resulting in nonsignificant differences (P = 0.78 and 0.84 for DEL and MAN, respectively).

  19. Two-dimensional liquid chromatography technique coupled with mass spectrometry analysis to compare the proteomic response to cadmium stress in plants.

    PubMed

    Visioli, Giovanna; Marmiroli, Marta; Marmiroli, Nelson

    2010-01-01

    Plants are useful in studies of metal toxicity, because their physiological responses to different metals are correlated with the metal exposure dose and chemical state. Moreover a network of proteins and biochemical cascades that may lead to a controlled homeostasis of metals has been identified in many plant species. This paper focuses on the global protein variations that occur in a Populus nigra spp. clone (Poli) that has an exceptional tolerance to the presence of cadmium. Protein separation was based on a two-dimensional liquid chromatography technique. A subset of 20 out of 126 peaks were identified as being regulated differently under cadmium stress and were fingerprinted by MALDI-TOF. Proteins that were more abundant in the treated samples were located in the chloroplast and in the mitochondrion, suggesting the importance of these organelles in the response and adaptation to metal stress.

  20. A simple and rapid technique for recovery of (99m)Tc from low specific activity (n,gamma)(99)Mo based on solvent extraction and column chromatography.

    PubMed

    Chattopadhyay, Sankha; Das, Sujata Saha; Barua, Luna

    2010-01-01

    A simple and inexpensive method of separation of (99m)Tc from (99)Mo produced by neutron activation of (98)Mo via the (98)Mo(n,gamma)(99)Mo nuclear reaction is described. The recovery of (99m)Tc was performed by solvent extraction technique followed by column (active alumina) chromatography. The overall radiochemical yield for the complete separation of (99m)Tc was 85-95% (n=10). The separated Na[(99m)Tc]TcO(4) was of high radionuclidic, radiochemical, and chemical purities. The method can be adopted for routine use of (99m)Tc in hospital radio-pharmacies utilizing low-medium specific activity (n,gamma)(99)Mo produced in a research reactor.

  1. Gas chromatography in space

    NASA Technical Reports Server (NTRS)

    Akapo, S. O.; Dimandja, J. M.; Kojiro, D. R.; Valentin, J. R.; Carle, G. C.

    1999-01-01

    Gas chromatography has proven to be a very useful analytical technique for in situ analysis of extraterrestrial environments as demonstrated by its successful operation on spacecraft missions to Mars and Venus. The technique is also one of the six scientific instruments aboard the Huygens probe to explore Titan's atmosphere and surface. A review of gas chromatography in previous space missions and some recent developments in the current environment of fiscal constraints and payload size limitations are presented.

  2. Power cepstrum technique with application to model helicopter acoustic data

    NASA Technical Reports Server (NTRS)

    Martin, R. M.; Burley, C. L.

    1986-01-01

    The application of the power cepstrum to measured helicopter-rotor acoustic data is investigated. A previously applied correction to the reconstructed spectrum is shown to be incorrect. For an exact echoed signal, the amplitude of the cepstrum echo spike at the delay time is linearly related to the echo relative amplitude in the time domain. If the measured spectrum is not entirely from the source signal, the cepstrum will not yield the desired echo characteristics and a cepstral aliasing may occur because of the effective sample rate in the frequency domain. The spectral analysis bandwidth must be less than one-half the echo ripple frequency or cepstral aliasing can occur. The power cepstrum editing technique is a useful tool for removing some of the contamination because of acoustic reflections from measured rotor acoustic spectra. The cepstrum editing yields an improved estimate of the free field spectrum, but the correction process is limited by the lack of accurate knowledge of the echo transfer function. An alternate procedure, which does not require cepstral editing, is proposed which allows the complete correction of a contaminated spectrum through use of both the transfer function and delay time of the echo process.

  3. Application of electrically invisible antennas to the Modulated Scatterer Technique

    SciTech Connect

    Crocker, Dylan A.; Donnell, Kristen M.

    2015-09-16

    The modulated scatterer technique (MST) has shown promise for applications in microwave imaging, electric field mapping, and materials characterization. Traditionally, MST scatterers are dipoles centrally loaded with an element capable of modulation (e.g., a p-i-n diode). By modulating the load element, signals scattered from the MST scatterer are also modulated. However, due to the small size of such scatterers, it can be difficult to reliably detect the modulated signal. Increasing the modulation depth (MD; a parameter related to how well the scatterer modulates the scattered signal) may improve the detectability of the scattered signal. In an effort to improve the MD, the concept of electrically invisible antennas is applied to the design of MST scatterers. Our paper presents simulations and measurements of MST scatterers that have been designed to be electrically invisible during the reverse bias state of the modulated element (a p-i-n diode in this case), while producing detectable scattering during the forward bias state (i.e., operate in an electrically visible state). Furthermore, the results using the new design show significant improvement to the MD of the scattered signal as compared with a traditional MST scatterer (i.e., dipole centrally loaded with a p-i-n diode).

  4. Application of electrically invisible antennas to the Modulated Scatterer Technique

    DOE PAGES

    Crocker, Dylan A.; Donnell, Kristen M.

    2015-09-16

    The modulated scatterer technique (MST) has shown promise for applications in microwave imaging, electric field mapping, and materials characterization. Traditionally, MST scatterers are dipoles centrally loaded with an element capable of modulation (e.g., a p-i-n diode). By modulating the load element, signals scattered from the MST scatterer are also modulated. However, due to the small size of such scatterers, it can be difficult to reliably detect the modulated signal. Increasing the modulation depth (MD; a parameter related to how well the scatterer modulates the scattered signal) may improve the detectability of the scattered signal. In an effort to improve themore » MD, the concept of electrically invisible antennas is applied to the design of MST scatterers. Our paper presents simulations and measurements of MST scatterers that have been designed to be electrically invisible during the reverse bias state of the modulated element (a p-i-n diode in this case), while producing detectable scattering during the forward bias state (i.e., operate in an electrically visible state). Furthermore, the results using the new design show significant improvement to the MD of the scattered signal as compared with a traditional MST scatterer (i.e., dipole centrally loaded with a p-i-n diode).« less

  5. Application of Dynamic Speckle Techniques in Monitoring Biofilms Drying Process

    NASA Astrophysics Data System (ADS)

    Enes, Adilson M.; Júnior, Roberto A. Braga; Dal Fabbro, Inácio M.; da Silva, Washington A.; Pereira, Joelma

    2008-04-01

    Horticultural crops exhibit losses far greater than grains in Brazil which are associated to inappropriate maturation, mechanical bruising, infestation by microorganisms, wilting, etc. Appropriate packing prevents excessive mass loss associated to transpiration as well as to respiration, by controlling gas exchanging with outside environment. Common packing materials are identified as plastic films, waxes and biofilms. Although research developed with edible films and biopolymers has increased during last years to attend the food industry demands, avoiding environmental problems, little efforts have been reported on biofilm physical properties investigations. These properties, as drying time and biofilm interactions with environment are considered of basic importance. This research work aimed to contribute to development of a methodology to evaluate yucca (Maniot vulgaris) based biofilms drying time supported by a biospeckle technique. Biospeckle is a phenomenon generated by a laser beam scattered on a dynamic active surface, producing a time varying pattern which is proportional to the surface activity level. By capturing and processing the biospeckle image it is possible to attribute a numerical quantity to the surface bioactivity. Materials exhibiting high moisture content will also show high activity, which will support the drying time determination. Tests were set by placing biofilm samples on polyetilen plates and further submitted to laser exposition at four hours interval to capture the pattern images, generating the Intensities Dispersion Modulus. Results indicates that proposed methodology is applicable in determining biofilm drying time as well as vapor losses to environment.

  6. Application of a Dense Gas Technique for Sterilizing Soft Biomaterials

    PubMed Central

    Karajanagi, Sandeep S.; Yoganathan, Roshan; Mammucari, Raffaella; Park, Hyoungshin; Cox, Julian; Zeitels, Steven M.; Langer, Robert; Foster, Neil R.

    2017-01-01

    Sterilization of soft biomaterials such as hydrogels is challenging because existing methods such as gamma irradiation, steam sterilization, or ethylene oxide sterilization, while effective at achieving high sterility assurance levels (SAL), may compromise their physicochemical properties and biocompatibility. New methods that effectively sterilize soft biomaterials without compromising their properties are therefore required. In this report, a dense-carbon dioxide (CO2)-based technique was used to sterilize soft polyethylene glycol (PEG)-based hydrogels while retaining their structure and physicochemical properties. Conventional sterilization methods such as gamma irradiation and steam sterilization severely compromised the structure of the hydrogels. PEG hydrogels with high water content and low elastic shear modulus (a measure of stiffness) were deliberately inoculated with bacteria and spores and then subjected to dense CO2. The dense CO2-based methods effectively sterilized the hydrogels achieving a SAL of 10−7 without compromising the viscoelastic properties, pH, water-content, and structure of the gels. Furthermore, dense CO2-treated gels were biocompatible and non-toxic when implanted subcutaneously in ferrets. The application of novel dense CO2-based methods to sterilize soft biomaterials has implications in developing safe sterilization methods for soft biomedical implants such as dermal fillers and viscosupplements. PMID:21337339

  7. Applications of nuclear analytical techniques to environmental studies

    NASA Astrophysics Data System (ADS)

    Freitas, M. C.; Pacheco, A. M. G.; Marques, A. P.; Barros, L. I. C.; Reis, M. A.

    2001-07-01

    A few examples of application of nuclear-analytical techniques to biological monitors—natives and transplants—are given herein. Parmelia sulcata Taylor transplants were set up in a heavily industrialized area of Portugal—the Setúbal peninsula, about 50 km south of Lisbon—where indigenous lichens are rare. The whole area was 10×15 km around an oil-fired power station, and a 2.5×2.5 km grid was used. In north-western Portugal, native thalli of the same epiphytes (Parmelia spp., mostly Parmelia sulcata Taylor) and bark from olive trees (Olea europaea) were sampled across an area of 50×50 km, using a 10×10 km grid. This area is densely populated and features a blend of rural, urban-industrial and coastal environments, together with the country's second-largest metro area (Porto). All biomonitors have been analyzed by INAA and PIXE. Results were put through nonparametric tests and factor analysis for trend significance and emission sources, respectively.

  8. Techniques of DNA methylation analysis with nutritional applications.

    PubMed

    Mansego, Maria L; Milagro, Fermín I; Campión, Javier; Martínez, J Alfredo

    2013-01-01

    Epigenetic mechanisms are likely to play an important role in the regulation of metabolism and body weight through gene-nutrient interactions. This review focuses on methods for analyzing one of the most important epigenetic mechanisms, DNA methylation, from single nucleotide to global measurement depending on the study goal and scope. In addition, this study highlights the major principles and methods for DNA methylation analysis with emphasis on nutritional applications. Recent developments concerning epigenetic technologies are showing promising results of DNA methylation levels at a single-base resolution and provide the ability to differentiate between 5-methylcytosine and other nucleotide modifications such as 5-hydroxymethylcytosine. A large number of methods can be used for the analysis of DNA methylation such as pyrosequencing™, primer extension or real-time PCR methods, and genome-wide DNA methylation profile from microarray or sequencing-based methods. Researchers should conduct a preliminary analysis focused on the type of validation and information provided by each technique in order to select the best method fitting for their nutritional research interests.

  9. Risk-based maintenance--techniques and applications.

    PubMed

    Arunraj, N S; Maiti, J

    2007-04-11

    Plant and equipment, however well designed, will not remain safe or reliable if it is not maintained. The general objective of the maintenance process is to make use of the knowledge of failures and accidents to achieve the possible safety with the lowest possible cost. The concept of risk-based maintenance was developed to inspect the high-risk components usually with greater frequency and thoroughness and to maintain in a greater manner, to achieve tolerable risk criteria. Risk-based maintenance methodology provides a tool for maintenance planning and decision making to reduce the probability of failure of equipment and the consequences of failure. In this paper, the risk analysis and risk-based maintenance methodologies were identified and classified into suitable classes. The factors affecting the quality of risk analysis were identified and analyzed. The applications, input data and output data were studied to understand their functioning and efficiency. The review showed that there is no unique way to perform risk analysis and risk-based maintenance. The use of suitable techniques and methodologies, careful investigation during the risk analysis phase, and its detailed and structured results are necessary to make proper risk-based maintenance decisions.

  10. Thin-layer chromatography with flame ionization detection

    SciTech Connect

    Ranny, M.

    1986-01-01

    This book, TLC-FID (thin-layer chromatography with flame ionization detection), represents a significant advance in the further development of thin-layer chromatography. It permits fast FID quantification of the zones separated on reusable TLC rods coated with sintered glass silicagel and glass-alumina layers. This book discusses in detail the basic characteristics and applications possibilities for this novel, flexible and developing technique.

  11. Application of digital image processing techniques to astronomical imagery 1977

    NASA Technical Reports Server (NTRS)

    Lorre, J. J.; Lynn, D. J.

    1978-01-01

    Nine specific techniques of combination of techniques developed for applying digital image processing technology to existing astronomical imagery are described. Photoproducts are included to illustrate the results of each of these investigations.

  12. Comparison of the sensitivity of different aroma extraction techniques in combination with gas chromatography-mass spectrometry to detect minor aroma compounds in wine.

    PubMed

    Gamero, Amparo; Wesselink, Wilma; de Jong, Catrienus

    2013-01-11

    MicroVinification platforms are used for screening purposes to study aroma development in wine. These high-throughput methodologies require flavor analysis techniques that allow fast detection of a high number of aroma compounds which often appear in very low concentrations (μg/l). In this work, a selection of aroma extraction techniques in combination with gas chromatography-mass spectrometry (GC-MS) were evaluated to detect minor wine aroma compounds in low sample volume. The techniques evaluated were headspace (HS), headspace solid-phase dynamic extraction (HS-SPDE), headspace solid-phase microextraction (HS-SPME), direct immersion solid-phase microextraction (DI-SPME), stir bar sorptive extraction (SBSE) and monolithic material sorptive extraction (MMSE). DI-SPME showed the highest sensitivity as expressed by detection of the highest percentage of total aroma compounds at concentrations around 0.1 μg/l. SBSE and MMSE followed DI-SPME in terms of sensitivity. HS-SPME was less sensitive but considered sensitive enough for detection of most of the volatile compounds present in highly aromatic wines. Matrix effect was shown to strongly affect aroma extraction and therefore the sensitivity of the different extraction methods.

  13. Vortex-assisted liquid-liquid-liquid microextraction (VALLLME) technique: A new microextraction approach for direct liquid chromatography and capillary electrophoresis analysis.

    PubMed

    Makahleh, Ahmad; Yap, Hui Fang; Saad, Bahruddin

    2015-10-01

    A new, rapid and sensitive microextraction technique named vortex-assisted liquid-liquid-liquid microextraction (VALLLME) is proposed. The complete extraction process involves two steps. First, a vortex-assisted liquid-liquid microextraction (VALLME) procedure was used to extract the analytes from a relatively large volume of sample (donor phase) to a small volume of organic solvent (intermediate phase). Next, a micro-vortex-assisted liquid-liquid extraction (µ-VALLE) was used to extract the target analytes from the intermediate phase to a smaller volume of aqueous solution (acceptor phase). The final extract (acceptor phase) can be directly injected into the high performance liquid chromatography or capillary electrophoresis units without any further treatments. The selection of the intermediate phase and the manipulation of pH are key parameters that ensure good extraction efficiency of the technique. The proposed technique has been successfully applied for the determination of carvedilol (used as model analyte) in biological fluid samples. The optimum extraction conditions were: toluene as intermediate phase (150 μL); pH of the donor phase, 9.5; vortex time of the VALLME, 45 s (maximum speed, 2500 rpm); 0.1M HCl (15 μL) as acceptor phase; vortexing time of the µ-VALLME, 75 s (maximum stirring speed, 2500 rpm) and salt concentration in the donor phase, 5% (w/v). Under these conditions, enrichment factors of 51- and 418-fold for VALLME step and VALLLME procedure, respectively, were achieved.

  14. Identification of potential antioxidant compounds in the essential oil of thyme by gas chromatography with mass spectrometry and multivariate calibration techniques.

    PubMed

    Masoum, Saeed; Mehran, Mehdi; Ghaheri, Salehe

    2015-02-01

    Thyme species are used in traditional medicine throughout the world and are known for their antiseptic, antispasmodic, and antitussive properties. Also, antioxidant activity is one of the interesting properties of thyme essential oil. In this research, we aim to identify peaks potentially responsible for the antioxidant activity of thyme oil from chromatographic fingerprints. Therefore, the chemical compositions of hydrodistilled essential oil of thyme species from different regions were analyzed by gas chromatography with mass spectrometry and antioxidant activities of essential oils were measured by a 1,1-diphenyl-2-picrylhydrazyl radical scavenging test. Several linear multivariate calibration techniques with different preprocessing methods were applied to the chromatograms of thyme essential oils to indicate the peaks responsible for the antioxidant activity. These techniques were applied on data both before and after alignment of chromatograms with correlation optimized warping. In this study, orthogonal projection to latent structures model was found to be a good technique to indicate the potential antioxidant active compounds in the thyme oil due to its simplicity and repeatability.

  15. Profiling analysis of volatile compounds from fruits using comprehensive two-dimensional gas chromatography and image processing techniques.

    PubMed

    Schmarr, Hans-Georg; Bernhardt, Jörg

    2010-01-22

    An image processing approach originating from the proteomics field has been transferred successfully to the processing of data obtained with comprehensive two-dimensional gas chromatographic separations data. The approach described here has proven to be a useful analytical tool for unbiased pattern comparison or profiling analyses, as demonstrated with the differentiation of volatile patterns ("aroma") from fruits such as apples, pears, and quince fruit. These volatile patterns were generated by headspace solid phase microextraction coupled to comprehensive two-dimensional gas chromatography (HS-SPME-GC x GC). The data obtained from GC x GC chromatograms were used as contour plots which were then converted to gray-scale images and analyzed utilizing a workflow derived from 2D gel-based proteomics. Run-to-run variations between GC x GC chromatograms, respectively their contour plots, have been compensated by image warping. The GC x GC images were then merged into a fusion image yielding a defined and project-wide spot (peak) consensus pattern. Within detected spot boundaries of this consensus pattern, relative quantities of the volatiles from each GC x GC image have been calculated, resulting in more than 700 gap free volatile profiles over all samples. These profiles have been used for multivariate statistical analysis and allowed clustering of comparable sample origins and prediction of unknown samples. At present state of development, the advantage of using mass spectrometric detection can only be realized by data processing off-line from the identified software packages. However, such information provides a substantial basis for identification of statistically relevant compounds or for a targeted analysis.

  16. Mass defect filter technique and its applications to drug metabolite identification by high-resolution mass spectrometry.

    PubMed

    Zhang, Haiying; Zhang, Donglu; Ray, Kenneth; Zhu, Mingshe

    2009-07-01

    Identification of drug metabolites by liquid chromatography/mass spectrometry (LC/MS) involves metabolite detection in biological matrixes and structural characterization based on product ion spectra. Traditionally, metabolite detection is accomplished primarily on the basis of predicted molecular masses or fragmentation patterns of metabolites using triple-quadrupole and ion trap mass spectrometers. Recently, a novel mass defect filter (MDF) technique has been developed, which enables high-resolution mass spectrometers to be utilized for detecting both predicted and unexpected drug metabolites based on narrow, well-defined mass defect ranges for these metabolites. This is a new approach that is completely different from, but complementary to, traditional molecular mass- or MS/MS fragmentation-based LC/MS approaches. This article reviews the mass defect patterns of various classes of drug metabolites and the basic principles of the MDF approach. Examples are given on the applications of the MDF technique to the detection of stable and chemically reactive metabolites in vitro and in vivo. Advantages, limitations, and future applications are also discussed on MDF and its combinations with other data mining techniques for the detection and identification of drug metabolites.

  17. Application Of Iterative Reconstruction Techniques To Conventional Circular Tomography

    NASA Astrophysics Data System (ADS)

    Ghosh Roy, D. N.; Kruger, R. A.; Yih, B. C.; Del Rio, S. P.; Power, R. L.

    1985-06-01

    Two "point-by-point" iteration procedures, namely, Iterative Least Square Technique (ILST) and Simultaneous Iterative Reconstructive Technique (SIRT) were applied to classical circular tomographic reconstruction. The technique of tomosynthetic DSA was used in forming the tomographic images. Reconstructions of a dog's renal and neck anatomy are presented.

  18. A direct comparison of the performance of ground, beaded and silica-grafted MIPs in HPLC and turbulent flow chromatography applications.

    PubMed

    Fairhurst, Robert E; Chassaing, Christophe; Venn, Richard F; Mayes, Andrew G

    2004-12-15

    Spherical molecularly imprinted polymers (MIPs) specific to the beta-blocker propranolol have been synthesised using two different approaches and compared to traditional ground monolithic MIPs in HPLC and TFC applications. TFC is a LC technique used for rapid extraction of compounds directly from complex matrices. It can be easily coupled to HPLC and MS for automation of an extraction/analysis procedure. Spherical MIP beads were produced using a suspension polymerisation technique and silica/MIP composite beads by grafting MIP to spherical silica particles using a surface-bound initiator species. Synthesis of both beaded and silica-grafted MIPs was more practical than using the traditional grinding method and yields of spherical particles of the required size between 80 and 100% were routinely achieved. Under HPLC conditions, beaded and ground MIP materials showed a degree of chiral separation for all of the nine beta-blockers tested. The beaded MIP, however, showed much better flow properties and peak shape than the ground material. Silica-grafted MIP showed some separation in five of the drugs and a large improvement in peak shape and analysis times compared with both ground and beaded MIPs. The materials prepared were also used in extraction columns for Turbulent Flow Chromatography (TFC). Although no imprinting effect was observed under typical TFC conditions, beaded polymer materials showed promise for use as TFC extraction columns due to the good flow properties and clean extracts obtained.

  19. Application of GFP-Technique for Cytoskeleton Visualization Onboard

    NASA Astrophysics Data System (ADS)

    Kordyum, E. L.; Shevchenko, G. V.; Yemets, A. I.; Nyporko, A. I.; Blume, Ya. B.

    2002-01-01

    gravity perception and transduction. Elucidation of cytoskeleton involvement in the above processes will be a great contribution into the fundamental biology, namely, in signaling mechanisms. One of the useful models for investigation of cell gravisensing are higher plants where the sites of gravity perception and reaction are spatially separated. From this point of view the localization of cytoskeletal elements at the different stages of plant development with the special emphasis on cytoskeleton dynamics during development of gravisensitive regions are of special interests. It should be noted that most of plant cytoskeletal researches are conducted by the means of immunohistochemical reactions with the application of monoclonal antibodies specific to specific cytoskeletal proteins. Different modifications of these methods are beneficial for the ground-based experiments, but for the performance onboard the latter represents quite routine and complicated technique, which requires time and special skills for astronauts. Besides, immunohistochemistry provides only static images of the cytoskeleton arrangement in fixed cells while its localization in living cells is needed for better understanding of cytoskeleton function. In this connection we propose new approach for cytoskeleton visualization onboard in particular, use of green fluorescent protein (GFP) from Aequorea victoria, which has the unique properties as a marker for protein localization in vivo. Recently appeared this method helped to obtain significant data on the cytoskeleton dynamics in living cells, including plant cells. The creation of chimaeric protein-GFP gene constructs, obtaining the transformed plant cells possessed protein-GFP in their cytoskeletal composition will allow receiving a simple and efficient model for screening of cytoskeleton functional status in microgravity. To realize this idea at present state of art it would be possible to produce a respective chimaeric plant tubulin gene

  20. Applications of thin layer chromatography, high performance liquid chromatography and mass spectrometry in the fermentation and isolation of the antibiotic nybomycin.

    PubMed

    Pope, J A; Nelson, R A; Schaffner, C P; Rosen, R T; Pandey, R C

    1990-09-01

    Thin layer chromatography (TLC), high performance liquid chromatography (HPLC) and mass spectrometry (MS) methods have been developed for the analysis of the antibiotic nybomycin, its derivatives deoxynybomycin and nybomycin acetate, during the fermentation and isolation of nybomycin. Using a quantitative HPLC based assay, the time course of nybomycin production (nybomycin titers) in 1000 liter fermentations was determined. Desorption chemical ionization mass spectrometry (DCI/MS) of standard nybomycin samples, fermentation broth samples and purified fractions suggested the co-production of deoxynybomycin which was not reported previously from this organism. TLC and HPLC were used to confirm the presence of deoxynybomycin in the crude extracts of fermentation broths.

  1. Application of Borehole SIP Technique to Sulfide Mineral Exploration

    NASA Astrophysics Data System (ADS)

    Kim, Changryol; Park, Mi Kyung; Park, Samgyu; Sung, Nak Hoon; Shin, Seung Wook

    2016-04-01

    In the study, SIP (Spectral Induced Polarization) well logging probe system was developed to rapidly locate the metal ore bodies with sulfide minerals in the boreholes. The newly developed SIP logging probe employed the non-polarizable electrodes, consisting of zinc chloride (ZnCl2), sodium chloride (NaCl), gypsum (CaSO4·2H2O), and water (H2O), instead of existing copper electrodes, leading to eliminating the EM coupling effect in the IP surveys as much as possible. In addition, the SIP logging system is designed to make measurements down to maximum 500 meters in depth in the boreholes. The SIP well logging was conducted to examine the applicability of the SIP probe system to the boreholes at the ore mine in Jecheon area, Korea. The boreholes used in the SIP logging are known to have penetrated the metal ore bodies with sulfide minerals from the drilling investigations. The ore mine of the study area is the scarn deposits surrounded by the limestone or lime-silicate rocks in Ordovician period. The results of the SIP well logging have shown that the borehole segments with limestone or lime-silicate rocks yielded the insignificant SIP responses while the borehole segments with sulfide minerals (e.g. pyrite) provided the significant phase shifts of the SIP responses. The borehole segments penetrating the metal ore body, so-called cupola, have shown very high response of the phase shift, due to the high contents of the sulfide mineral pyrite. The phase shifts of the SIP response could be used to estimate the grade of the ore bodies since the higher contents of the sulfide minerals, the higher magnitudes of the phase shifts in the SIP responses. It is, therefore, believed that the borehole SIP technique can be applied to investigate the metal ore bodies with sulfide minerals, and that could be used to estimate the ore grades as a supplementary tool in the future.

  2. Gas chromatography: Possible application of advanced instrumentation developed for solar system exploration to space station cabin atmospheres

    NASA Technical Reports Server (NTRS)

    Carle, G. C.

    1985-01-01

    Gas chromatography (GC) technology was developed for flight experiments in solar system exploration. The GC is a powerful analytical technique with simple devices separating individual components from complex mixtures to make very sensitive quantitative and qualitative measurements. It monitors samples containing mixtures of fixed gases and volatile organic molecules. The GC was used on the Viking mission in support of life detection experiments and on the Pioneer Venus Large Probe to determine the composition of the venusian atmosphere. A flight GC is under development to study the progress and extent of STS astronaut denitrogenation prior to extravehicular activity. Advanced flight GC concepts and systems for future solar system exploration are also studied. Studies include miniature ionization detectors and associated control systems capable of detecting from ppb up to 100% concentration levels. Further miniaturization is investigated using photolithography and controlled chemical etching in silicon wafers. Novel concepts such as ion mobility drift spectroscopy and multiplex gas chromatography are also developed for future flight experiments. These powerful analytical concepts and associated hardware are ideal for the monitoring of cabin atmospheres containing potentially dangerous volatile compounds.

  3. Applications of liquid chromatography-mass spectrometry in metabolic studies of explosives.

    PubMed

    Yinon, J; Hwang, D G

    1987-05-08

    Liquid chromatography-mass spectrometry was used for the detection and identification of metabolites of 2,4,6-trinitrotoluene (TNT) in urine and blood. The metabolites were found in the urine of rats and in the blood of rabbits fed with TNT, in the urine of rats exposed to TNT by skin absorption and in the urine of TNT munition workers. The detected metabolites, formed by reduction processes, included 2-amino-4,6-dinitrotoluene, 4-amino-2,6-dinitrotoluene, 2,4-diamino-6-nitrotoluene and 2,6-diamino-4-nitrotoluene, in addition to untransformed TNT.

  4. The novel technique of vapor pressure analysis to monitor the enzymatic degradation of PHB by HPLC chromatography.

    PubMed

    Polyák, Péter; Rácz, Piroska; Rózsa, Péter; Nagy, Gergely N; Vértessy, Beáta G; Pukánszky, Béla

    2017-03-15

    A novel method was introduced for the quantitative determination of substances in aqueous solutions by using the evaporative light scattering (ELS) detector of a high performance liquid chromatograph (HPLC). The principle of the measurement is the different equilibrium vapor pressure of the solvent and the analyte resulting in decreasing evaporation rate, larger droplets and stronger signal with increasing concentration. The new technique based on vapor pressure analysis was validated with traditional UV-Vis detection carried out with a diode array detector (DAD). The new technique was used for monitoring the concentration of solutions obtained during the enzymatic degradation of poly(3-hydroxybutyrate) yielding the 3-hydroxybutyrate monomer as the product. The accuracy of the measurement allowed the determination of degradation kinetics as well. The results obtained with the two techniques showed excellent agreement at small concentrations. Deviations at larger concentrations were explained with the non-linear correlation between analyte concentration and detector signal and the linear regression used for calibration. Mathematical analysis of the method made possible the determination of the evaporation enthalpy of the analyte as well. The new approach is especially suitable for the quantitative analysis of compounds, which do not absorb in the detection range of the DAD detector or if their characteristic absorbance is close to the lower end of its wavelength range.

  5. Application of an automatic thermal desorption-gas chromatography-mass spectrometry system for the analysis of polycyclic aromatic hydrocarbons in airborne particulate matter.

    PubMed

    Gil-Moltó, J; Varea, M; Galindo, N; Crespo, J

    2009-02-27

    The application of the thermal desorption (TD) method coupled with gas chromatography-mass spectrometry (GC-MS) to the analysis of aerosol organics has been the focus of many studies in recent years. This technique overcomes the main drawbacks of the solvent extraction approach such as the use of large amounts of toxic organic solvents and long and laborious extraction processes. In this work, the application of an automatic TD-GC-MS instrument for the determination of particle-bound polycyclic aromatic hydrocarbons (PAHs) is evaluated. This device offers the advantage of allowing the analysis of either gaseous or particulate organics without any modification. Once the thermal desorption conditions for PAH extraction were optimised, the method was verified on NIST standard reference material (SRM) 1649a urban dust, showing good linearity, reproducibility and accuracy for all target PAHs. The method has been applied to PM10 and PM2.5 samples collected on quartz fibre filters with low volume samplers, demonstrating its capability to quantify PAHs when only a small amount of sample is available.

  6. Calcium-modulated conformational affinity chromatography. Application to the purification of calmodulin and S100 proteins.

    PubMed

    Fleminger, G; Neufeld, T; Star-Weinstock, M; Litvak, M; Solomon, B

    1992-04-24

    The purification of proteins by affinity chromatography is based on their highly specific interaction with an immobilized ligand followed by elution under conditions where their affinity towards the ligand is markedly reduced. Thus, a high-degree purification by a single chromatographic step is achieved. However, when several proteins in the crude mixture share affinity to a common immobilized ligand, they may not be resolved by affinity chromatography and subsequent "real" chromatographic purification steps may be required. It is shown that by using properly selected gradient elution conditions, the affinities of the various proteins towards the immobilized ligand may be gradually modulated and their separation may be achieved. This is exemplified by the isolation and separation of a group of Ca(2+)-activated proteins, Calmodulin, S100a and S100b, from bovine brain extract, using a melittin-Eupergit C affinity column which is developed with Ca(2+)-chelator gradients. As expected, separation of the three proteins into individual peaks, eluted in order of increasing affinity to the matrix, was obtained. Sigmoid selectivity curves calculated from the elution volumes under different elution conditions for each of the proteins were obtained, illustrating the chromatographic behaviour of the gradient affinity separation system.

  7. One-pot preparation of a novel monolith for high performance liquid chromatography applications.

    PubMed

    Jiao, Xiaoyan; Shen, Shigang; Shi, Tiesheng

    2015-12-15

    Various novel porous organic-based monoliths with the mode of hydrophobicity were synthesized by in situ free-radical crosslinking copolymerization and optimized for the separations of small molecules and high-performance reversed-phase chromatography (RP-chromatography). These monoliths contained co-polymers based on glycidyl methacrylate (GMA)/ethylene glycol dimethacrylate (EDMA)/tripropylene glycol diacrylate (TPGDA) or EDMA/TPGDA. A mixture of cetanol, methanol and poly (ethylene glycol) (PEG) was used as the porogen, with the ratio of these solvents being varied along with the polymerization temperature to generate a library of monoliths. The conditions were optimized and the resulting poly (GMA-co-TPGDA-co-EDMA) monolith was investigated by infrared spectrometer (IR), field emission scanning electron microscope (FESEM), and mercury intrusion porosimetry (MIP), respectively. The column performance was assessed by the separation of a series of neutral solutes of benzene derivatives. The result demonstrated that the prepared monolith exhibited an RP-chromatographic behavior and relatively homogeneous structure, good permeability and separation performance. Moreover, the relative standard deviations (RSDs) of the retention factor values for benzene derivatives were less than 1.5% (n=7, column-to-column). The approach used in this study was extended to the separation of anilines.

  8. Application of isothermal titration calorimetry and column chromatography for identification of biomolecular targets.

    PubMed

    Zhou, Xingding; Kini, R Manjunatha; Sivaraman, J

    2011-02-01

    This protocol describes a method for identifying unknown target proteins from a mixture of biomolecules for a given drug or a lead compound. This method is based on a combination of chromatography and isothermal titration calorimetry (ITC) where ITC is used as a tracking tool. The first step involves the use of ITC to confirm the binding of ligand to a component in the biomolecular mixture. Subsequently, the biomolecular mixture is fractionated by chromatography, and the binding of the ligand with individual fractions (or subfractions) is verified by ITC. The iteration of chromatographic purification on the fractions combined with ITC results in identifying the target protein. This method is useful when the target protein or ligand is unknown and/or not amenable to labeling, chemical modification or immobilization. This protocol has been successfully used by our team and by others to identify both low-abundance and highly abundant target proteins present in biomolecular mixtures. With this protocol, it takes approximately 3-5 d to identify the target protein from a mixture.

  9. High-performance liquid chromatography with electrospray ionization ion mobility spectrometry: Characterization, data management, and applications.

    PubMed

    Zühlke, Martin; Riebe, Daniel; Beitz, Toralf; Löhmannsröben, Hans-Gerd; Andreotti, Sandro; Reinert, Knut; Zenichowski, Karl; Diener, Marc

    2016-12-01

    The combination of high-performance liquid chromatography and electrospray ionization ion mobility spectrometry facilitates the two-dimensional separation of complex mixtures in the retention and drift time plane. The ion mobility spectrometer presented here was optimized for flow rates customarily used in high-performance liquid chromatography between 100 and 1500 μL/min. The characterization of the system with respect to such parameters as the peak capacity of each time dimension and of the 2D spectrum was carried out based on a separation of a pesticide mixture containing 24 substances. While the total ion current chromatogram is coarsely resolved, exhibiting coelutions for a number of compounds, all substances can be separately detected in the 2D plane due to the orthogonality of the separations in retention and drift dimensions. Another major advantage of the ion mobility detector is the identification of substances based on their characteristic mobilities. Electrospray ionization allows the detection of substances lacking a chromophore. As an example, the separation of a mixture of 18 amino acids is presented. A software built upon the free mass spectrometry package OpenMS was developed for processing the extensive 2D data. The different processing steps are implemented as separate modules which can be arranged in a graphic workflow facilitating automated processing of data.

  10. Application of polymeric macroporous supports for temperature-responsive chromatography of pharmaceuticals.

    PubMed

    Lamprou, Alexandros; Gavriilidou, Agni-Faviola-Mika; Storti, Giuseppe; Soos, Miroslav; Morbidelli, Massimo

    2015-08-14

    A macroporous particulate support prepared previously by reactive gelation under shear and functionalized with poly(N-isopropylacrylamide), PNIPAM, brushes of variable length is applied for temperature-responsive chromatography, whereby temperature modulates hydrophobic interactions. Several different analytes, including small pharmaceuticals, peptides, proteins and monoclonal antibodies are employed. Contrary to the most commonly observed behavior in conventional chromatography, increasing retention is observed at elevated temperatures. Peak broadening is quantified using the peak standard deviation, which depends on both the polymer chain conformation and analyte adsorptivity. The favorable effect of grafted polymer thickness on retention becomes progressively less pronounced for thicker grafted PNIPAM layers. The effect of eluent composition on solute-sorbent interactions was investigated by introducing NaCl, methanol, dioxane and by varying the pH. Salt or organic solvent addition affects apart from the analytes solution properties, the hydrophobicity of the stationary phase itself. Frontal analyses performed at different temperatures to determine dynamic binding capacities, indicate small mass transfer resistances imposed by this novel packing material.

  11. An application of high performance liquid chromatography to analysis of lipids in archaeological samples.

    PubMed

    Passi, S; Rothschild-Boros, M C; Fasella, P; Nazzaro-Porro, M; Whitehouse, D

    1981-07-01

    Five samples from three different types of 1500-year-old Mediterranean amphorae, as well as from a contemporary oil lamp found in the same deposit, were analyzed for the presence of lipid residues. Each sample of finely ground amphorae powder weighed 1-2 g. The abundance of interfering secondary products makes thin-layer chromatography (TLC) an essential step of the procedure. The fractionation of the extract into its various lipid components by means of TLC was followed by quantitative recovery of the triglyceride (TG) and free fatty acid (FFA) fractions from the plates and by the measurement of their components by high performance liquid chromatography (HPLC) after esterification. The minimum detectable level is 1 ng. The amphorae samples revealed a more abundant FFA fraction than a TG fraction, which is the reverse of what we know about the composition of fresh oil. Despite the considerable age of the amphorae and their preservation under non-ideal conditions, the lipid residues have retained certain identifiable characteristics that enable one to make valid suggestions as to the type of commodity originally transported in the amphorae. The results of these experiments yield important information that enables the biochemist to observe an aging process irreproducible in the laboratory and provides the archaeologist with previously unavailable information about trade 15 centuries ago.

  12. Application of a chromatography model with linear gradient elution experimental data to the rapid scale-up in ion-exchange process chromatography of proteins.

    PubMed

    Ishihara, Takashi; Kadoya, Toshihiko; Yamamoto, Shuichi

    2007-08-24

    We applied the model described in our previous paper to the rapid scale-up in the ion exchange chromatography of proteins, in which linear flow velocity, column length and gradient slope were changed. We carried out linear gradient elution experiments, and obtained data for the peak salt concentration and peak width. From these data, the plate height (HETP) was calculated as a function of the mobile phase velocity and iso-resolution curve (the separation time and elution volume relationship for the same resolution) was calculated. The scale-up chromatography conditions were determined by the iso-resolution curve. The scale-up of the linear gradient elution from 5 to 100mL and 2.5L column sizes was performed both by the separation of beta-lactoglobulin A and beta-lactoglobulin B with anion-exchange chromatography and by the purification of a recombinant protein with cation-exchange chromatography. Resolution, recovery and purity were examined in order to verify the proposed method.

  13. Determination of chlorpromazine and its major metabolites by gas chromatography/mass spectrometry: application to biological fluids.

    PubMed

    Gruenke, L D; Craig, J C; Klein, F D; Nguyen, T L; Hitzemann, B A; Holaday, J W; Loh, H H; Braff, L; Fischer, A; Glick, I D

    1985-12-01

    A method for the quantitative determination of chlorpromazine and five of its major metabolites in a single sample of biological fluid in the ng/ml range has been developed utilizing gas chromatography/mass spectrometry with selected ion recording. The assay is highly specific and quantification is accomplished by an inverse stable isotope dilution technique, using deuterium-labeled variants of the compounds as internal standards. In this way the concentrations of chlorpromazine and five of its major metabolites (the sulfoxide, the N-oxide, the monodemethylated, the didemethylated, and the 7-hydroxylated compounds) can be determined in biological fluids. Levels in humans have been measured both in plasma and in red blood cells and are compared to those found in related in vitro studies.

  14. Biomedical application of plasmid DNA in gene therapy: a new challenge for chromatography.

    PubMed

    Sousa, F; Passarinha, L; Queiroz, J A

    2010-01-01

    Gene therapy and DNA vaccination are clinical fields gradually emerging in the last few decades, in particular after the discovery of some gene-related diseases. The increased relevance of biomedical applications of plasmid DNA (pDNA) to induce therapeutic effects has had a great impact on biopharmaceutical research and industry. Although there are several steps involved in the pDNA manufacturing process, the several unit operations must be designed and integrated into a global process. After the plasmid has been designed according to the requirements for clinical administeration to humans, it is biosynthesised mainly by an E. coli host. The overriding priority of the production process is to improve plasmid quantity - the production conditions need to be optimised to guarantee pDNA stability and biological activity. The complexity and diversity of biomolecules present on the pDNA-containing extracts represent the main concern and limitation to achieve pure and biologically active pDNA. There has been a recent intenstification of the improvement of existing purification procedures or the establishment of novel schemes for plasmid purification. This review focuses on the progress and relevance of chromatographic methodologies in the purification of pDNA-based therapeutic products. The review will attempt to assemble their different contributions of the different chromatographic procedures that are being used in the pDNA purification area. The advantages and disadvantages of the different chromatographic techniques, as well as the most significant improvements in response to the challenge of purifying pDNA will be discussed, emphasizing the future directions in this field.

  15. Application of integrated comprehensive/multidimensional gas chromatography with mass spectrometry and olfactometry for aroma analysis in wine and coffee.

    PubMed

    Chin, Sung-Tong; Eyres, Graham T; Marriott, Philip J

    2015-10-15

    Component coelution in chromatographic analysis complicates identification and attribution of individual odour-active volatile molecules in complex multi-component samples. An integrated system incorporating comprehensive two-dimensional gas chromatography (GC × GC) and multidimensional gas chromatography (MDGC), with flame ionisation, olfactometry and mass spectrometry detection was developed to circumvent data correlation across different systems. Identification of potent odorants in Shiraz wine and the headspace of ground coffee are demonstrated as selected applications. Multiple solid-phase microextraction (SPME) sampling with GC-O located odour-active regions; GC × GC established the complexity of odour-active regions; MDGC provided high-resolution separation for each region; simultaneous 'O' and MS detection completed the analysis for target resolved peaks. Seven odour regions in Shiraz were analysed with MDGC-O/MS detection, revealing 11 odour volatiles through matching of mass spectrometry and retention indices from both separating dimensions, including acetic acid; octen-3-ol; ethyl octanoate; methyl-2-oxo-nonanoate; butanoic acid, 2-methylbutanoic acid, and 3-methylbutanoic acid; 3-(methylthio)-1-propanol; hexanoic acid; β-damascenone; and ethyl-3-phenylpropanoate. A capsicum odour in ground coffee was identified as 2-methoxy-3-isobutylpyrazine with a 5-fold increase in S/N of the odorant when acquired using a 6-time cumulative SPME sampling approach.

  16. [The applications for Fourier transform infrared spectrum analysis technique in preventive medicine field].

    PubMed

    Yang, Jiao-lan; Luo, Tian

    2002-08-01

    This paper expatriated the applications for Fourier transform infrared spectrum analysis technique in preventive medicine field from four aspects of environmental pollution, life science, and the latest infrared analysis methods and near infrared analysis technique. In the environmental pollution field, it mainly described the advantages, the limitations and the solutions of the combined applications for gas chromatograph and Fourier transform infrared spectrum. In the life science field, it described the application for Fourier transform infrared spectrum analysis technique on protein secondary structure, membrane protein, phospholipid, nucleic acid, cell, tissue. In addition, it also introduced a few latest infrared analysis methods and the applications for near infrared spectrum analysis technique in food, cosmetic, drug.

  17. [Online enrichment ability of restricted-access column coupled with high performance liquid chromatography by column switching technique for benazepril hydrochloride].

    PubMed

    Zhang, Xiaohui; Wang, Rong; Xie, Hua; Yin, Qiang; Li, Xiaoyun; Jia, Zhengping; Wu, Xiaoyu; Zhang, Juanhong; Li, Wenbin

    2013-05-01

    The online enrichment ability of the restricted-access media (RAM) column coupled with high performance liquid chromatography by column switching technique for benazepril hydrochloride in plasma was studied. The RAM-HPLC system consisted of an RAM column as enrichment column and a C18 column as analytical column coupled via the column switching technique. The effects of the injection volume on the peak area and the systematic pressure were studied. When the injection volume was less than 100 microL, the peak area increased with the increase of the injection volume. However, when the injection volume was more than 80 microL, the pressure of whole system increased obviously. In order to protect the whole system, 80 microL was chosen as the maximum injection volume. The peak areas of ordinary injection and the large volume injection showed a good linear relationship. The enrichment ability of RAM-HPLC system was satisfactory. The system was successfully used for the separation and detection of the trace benazepril hydrochloride in rat plasma after its administration. The sensitivity of HPLC can be improved by RAM pre-enrichment. It is a simple and economic measurement method.

  18. Multiclass pesticide analysis in fruit-based baby food: A comparative study of sample preparation techniques previous to gas chromatography-mass spectrometry.

    PubMed

    Petrarca, Mateus H; Fernandes, José O; Godoy, Helena T; Cunha, Sara C

    2016-12-01

    With the aim to develop a new gas chromatography-mass spectrometry method to analyze 24 pesticide residues in baby foods at the level imposed by established regulation two simple, rapid and environmental-friendly sample preparation techniques based on QuEChERS (quick, easy, cheap, effective, robust and safe) were compared - QuEChERS with dispersive liquid-liquid microextraction (DLLME) and QuEChERS with dispersive solid-phase extraction (d-SPE). Both sample preparation techniques achieved suitable performance criteria, including selectivity, linearity, acceptable recovery (70-120%) and precision (⩽20%). A higher enrichment factor was observed for DLLME and consequently better limits of detection and quantification were obtained. Nevertheless, d-SPE provided a more effective removal of matrix co-extractives from extracts than DLLME, which contributed to lower matrix effects. Twenty-two commercial fruit-based baby food samples were analyzed by the developed method, being procymidone detected in one sample at a level above the legal limit established by EU.

  19. Multivariate optimization approach for chiral resolution of drugs using human serum albumin in affinity electrokinetic chromatography-partial filling technique.

    PubMed

    Martinez-Gomez, Maria A; Villanueva-Camañas, Rosa M; Sagrado, Salvador; Medina-Hernández, Maria J

    2005-11-01

    The enantiomeric resolution of chiral compounds using HSA by means of affinity EKC (AEKC)-partial filling technique is the result of a delicate balance between different experimental variables such as protein concentration, running pH (background electrophoretic buffer, protein and compound solutions) and protein solution plug length. In this paper multivariate optimization approaches for chiral separation of four basic drugs (alprenolol, oxprenolol, promethazine and propranolol) using HSA as chiral selector in AEKC-partial filling technique are studied. The experimental conditions to achieve maximum resolution are optimized using the Box-Behnken experimental design. Partial least squares and pareto charts are used to analyse the main effects on the resolution. The experimental resolutions observed for all compounds studied in optimum conditions agree with the estimated values based on response surface models. The results obtained show that the range of experimental conditions that provided enantioresolution narrows as hydrophobicity of analytes decreases. This fact can be explained by assuming that hydrophobicity controls the interaction of basic compounds with HSA.

  20. Assessment of speciation techniques including the application of photoacoustic spectroscopy

    SciTech Connect

    Bucher, J.; Gehmecker, H.; Edelstein, N.

    1985-08-01

    This document describes laboratory experiments that compare chromatographic and spectroscopic methods for rapidly characterizing ionic species in detail. These techniques were tested on various radioactive ion systems to develop a rapid, accurate approach to site characterization for use with Remedial Action Programs. Promising techniques were evaluated. 9 refs., 16 figs., 2 tabs.

  1. Application of the Overclaiming Technique to Scholastic Assessment

    ERIC Educational Resources Information Center

    Paulhus, Delroy L.; Dubois, Patrick J.

    2014-01-01

    The overclaiming technique is a novel assessment procedure that uses signal detection analysis to generate indices of knowledge accuracy (OC-accuracy) and self-enhancement (OC-bias). The technique has previously shown robustness over varied knowledge domains as well as low reactivity across administration contexts. Here we compared the OC-accuracy…

  2. Potential of human serum albumin as chiral selector of basic drugs in affinity electrokinetic chromatography-partial filling technique.

    PubMed

    Martínez-Gómez, Maria A; Villanueva-Camañas, R M; Sagrado, Salvador; Medina-Hernández, Maria J

    2006-11-01

    The enantiomeric resolution of compounds using HSA by means of affinity EKC (AEKC)-partial filling technique is the result of a delicate balance between different experimental variables such as protein concentration, running pH (background electrophoretic buffer (BGE), protein, and compound solutions), and plug length. In this paper, the possibility of using HSA as chiral selector for enantioseparation of 28 basic drugs using this methodology is studied. The effect of the physicochemical parameters, the structural properties of compounds, and compound-HSA protein binding percentages over their chiral resolution with HSA is outlined. Based on the results obtained, a decision tree is proposed for the "a priori" prediction of the capability of HSA for enantioseparation of basic drugs in AEKC. The results obtained indicated that enantioresolution of basic compounds with HSA depends on the hydrophobicity, polarity, and molar volume of compounds.

  3. Enantioseparation of nuarimol by affinity electrokinetic chromatography-partial filling technique using human serum albumin as chiral selector.

    PubMed

    Martínez-Gómez, Maria Amparo; Escuder-Gilabert, Laura; Villanueva-Camañas, Rosa M; Sagrado, Salvador; Medina-Hernández, Maria J

    2008-10-01

    The present paper deals with the enantiomeric separation of nuarimol enantiomers by affinity EKC-partial filling technique using HSA as chiral selector. Firstly, a study of nuarimol interactions with HSA by CE-frontal analysis was performed. The binding parameters obtained for the first site of interaction were n(1) = 0.84; K(1) = 9.7 +/- 0.3x10(3 )M(-1) and the protein binding percentage of nuarimol at physiological concentration of HSA was 75.2 +/- 0.2%. Due to the moderate affinity of nuarimol towards HSA the possibility of using this protein as chiral selector for the separation of nuarimol using the partial filling technique was evaluated. A multivariate optimization approach of the most critical experimental variables in enantioresolution, running pH, HSA concentration and plug length was carried out. Separation of nuarimol enantiomers was obtained under the following selected conditions: electrophoretic buffer composed of 50 mM Tris at pH 7.3; 160 muM HSA solution applied at 50 mbar for 156 s as chiral selector; nuarimol solutions in the range of 2-8x10(-4) M injected hydrodynamically at 30 mbar for 2 s and the electrophoretic runs performed at 30 degrees C applying 15 kV voltage. Resolution, accuracy, reproducibility speed and cost of the proposed method make it suitable for quality control of the enantiomeric composition of nuarimol in formulations and for further toxicological studies. The results showed a different affinity between nuarimol enantiomers towards HSA.

  4. Traditional Versus Rule-Based Programming Techniques: Application To The Control Of Optional Flight Information

    NASA Astrophysics Data System (ADS)

    Ricks, Wendell R.; Abbott, Kathy H.

    1987-05-01

    To the software design community, the concern over the costs associated with a program's execution time and implementation is great. It is always desirable, and sometimes imperative, that the proper programming technique is chosen which minimizes all costs for a given application or type of application. This paper describes a study that compared the cost-related factors associated with traditional programming techniques to rale-based programming techniques for a specific application. The results of this study favored the traditional approach regarding execution efficiency, but favored the rule-based approach regarding programmer productivity (implementation ease). Although this study examined a specific application, the resuli:s should be widely applicable.

  5. Application of micellar electrokinetic chromatography to the determination of sultamicillin in oral pharmaceutical preparations.

    PubMed

    Pajchel, Genowefa; Tyski, Stefan

    2002-12-06

    A micellar electrokinetic capillary electrophoretic method for determination of sultamicillin in Unasyn oral preparations--tablets and suspension--was evaluated. Phosphate-borate buffer at pH 7.0 containing 1.0% sodium dodecylsulfate was used as a mobile phase. The elaborated method ensures separation of sultamicillin from p-toluenesulfonic acid and the impurities, ampicillin, sulbactam and penicillamine. The method was validated for specificity, reproducibility, precision, accuracy and assay linearity (in a concentration range of sultamicillin of 0.05-1.5 mg/ml). Statistical analysis by Student's t-test showed no significant differences between the results obtained by micellar electrokinetic chromatography and HPLC, t(calculated) 0.519 for suspension assays and 0.284 for tablets assays were smaller then t(tabulated).

  6. Analysis of Iranian rosemary essential oil: application of gas chromatography-mass spectrometry combined with chemometrics.

    PubMed

    Jalali-Heravi, Mehdi; Moazeni, Rudabeh Sadat; Sereshti, Hassan

    2011-05-06

    This paper focuses on characterization of the components of Iranian rosemary essential oil using gas chromatography-mass spectrometry (GC-MS). Multivariate curve resolution (MCR) approach was used to overcome the problem of background, baseline offset and overlapping/embedded peaks in GC-MS. The analysis of GC-MS data revealed that sixty eight components exist in the rosemary essential oil. However, with the help of MCR this number was extended to ninety nine components with concentrations higher than 0.01%, which accounts for 98.23% of the total relative content of the rosemary essential oil. The most important constituents of the Iranian rosemary are 1,8-cineole (23.47%), α-pinene (21.74%), berbonone (7.57%), camphor (7.21%) and eucalyptol (4.49%).

  7. Application of a micromembrane chromatography module to the examination of protein adsorption equilibrium.

    PubMed

    Káňavová, Natália; Kosior, Anna; Antošová, Monika; Faber, René; Polakovič, Milan

    2012-11-01

    A micromembrane chromatography module based on a 96-well plate design and enabling fast and simple separation of small amounts of proteins was used for the determination of binding capacities of lysozyme, bovine serum albumin, ovalbumin, bovine γ-globulin, and human immunoglobulin G on a hydrophobic membrane Sartobind® Phenyl. Dependence of the binding capacity of the proteins on the ammonium sulfate concentration was examined in the salt concentration range of 0.5-2.0 mol L(-1). An exponential increase of the binding capacity was observed for all proteins. Simple Langmuir one-component isotherm was found suitable for the characterization of the effect of protein concentration in all cases. A combined effect of protein and salt concentrations was expressed via the Langmuir exponential isotherm and fitted the adsorption data for three of the investigated proteins well.

  8. DIONEX ICS3000 ION CHROMATOGRAPHY SYSTEM INSTALLATION AND INSTRUMENT ASSESSMENT FOR SRNL APPLICATIONS

    SciTech Connect

    Wiedenman, B.; White, T.

    2009-11-16

    Ion Chromatography (IC) is routinely used at the Savannah River National Laboratory (SRNL) for sample analysis and characterization. Results from IC analysis are valued in corrosion control maintenance and measurement programs, remediation waste process control, soil and ground water measurement, nuclear materials processing, and various other research and development programs. Presented in this report are analytical methods developed on a DIONEX ICS3000 Reagent Free Ion Chromatography (RFIC) system located in AD at SRNL. This IC system contains two independent analysis channels comprising of a mobile phase generator, a pump, stationary phase columns, a suppressor and a conductivity detector. One channel is dedicated to anion analysis using Potassium Hydroxide (KOH) as the mobile phase while a second channel is configured for cation analysis using Methanesulfonic Acid (MSA) as the mobile phase. Both channels share an autosampler and the peak analysis software, Chromeleon{reg_sign} v.6.8. Instrument configuration is modified from the manufacturer for radiological service. Listed within this report are Dionex ICS3000 parameters and results for the analysis of routine anions and cations. Additional method parameters and discussion are presented on the analysis of Acetate (CH{sub 3}COO{sup -}) and Iodate (IO{sub 3}{sup -}). Previous IC analysis instruments at AD have been based upon carbonate/bicarbonate buffer mobile phase chemistry. This report represents a transition to hydroxide as a mobile phase eluent. The hydroxide eluent offers a lower baseline conductivity, which allows for greater sample dilution and/or lower detection limits. Also the hydroxide mobile phase and column set has a significant separation of the phosphate peak from the nitrate and sulfate peaks vs. the carbonate/bicarbonate mobile phase and column set, an advantage for the industrial waste analyzed at SRNL.

  9. Application of matrix solid-phase dispersion and high-performance liquid chromatography for determination of sulfonamides in honey.

    PubMed

    Zou, Qiong-Hui; Wang, Jin; Wang, Xiang-Feng; Liu, Yuan; Han, Jie; Hou, Feier; Xie, Meng-Xia

    2008-01-01

    A novel method for simultaneous determination of 8 sulfonamide residues (sulfathiazole, sulfapyridine, sulfadiazine, sulfamerazine, sulfamonome-thoxine, sulfachloropyridazine, sulfamethoxazole, and sulfadimethoxine) in honey samples by high-performance liquid chromatography (HPLC) has been developed on the basis of precolumn derivatization with 9-fluorenylmethyl-chloroformate (FMOC-Cl). Sulfonamide residues in honey samples were extracted and purified by matrix solid-phase dispersion with C18 as the solid support. The residues were derivatized by FMOC-CI, and the FMOC-sulfonamide derivatives were further purified by solid-phase extraction with silica gel as the solid support prior to HPLC analysis. The average recoveries for most sulfonamide compounds at different spiking levels (from 10 to 250 microg/kg) were > 70% with relative standard deviations < 16%, and their limits of detection were 4.0 microg/kg. The established analytical method has high sensitivity and repeatability and can be applicable for determining the sulfonamide residues in various honey matrixes.

  10. Gas Chromatography

    NASA Astrophysics Data System (ADS)

    Qian, Michael C.

    Gas chromatography (GC) has many applications in the analysis of food products. GC has been used for the determination of fatty acids, triglycerides, cholesterol, gases, water, alcohols, pesticides, flavor compounds, and many more. While GC has been used for other food components such as sugars, oligosaccharides, amino acids, peptides, and vitamins, these substances are more suited to analysis by high performance liquid chromatography. GC is ideally suited to the analysis of volatile substances that are thermally stable. Substances such as pesticides and flavor compounds that meet these criteria can be isolated from a food and directly injected into the GC. For compounds that are thermally unstable, too low in volatility, or yield poor chromatographic separation due to polarity, a derivatization step must be done before GC analysis. The two parts of the experiment described here include the analysis of alcohols that requires no derivatization step, and the analysis of fatty acids which requires derivatization. The experiments specify the use of capillary columns, but the first experiment includes conditions for a packed column.

  11. Pilot Application of a Teaching Technique in Social Medicine

    ERIC Educational Resources Information Center

    Wegman, David H.; and others

    1969-01-01

    Using techniques that combine community health services with a learning situation, Boston area medical students interviewed people within a community to determine whether existing medical facilities meet or fail to meet their health needs. (LP)

  12. Wave Propagation Through Inhomogeneities With Applications to Novel Sensing Techniques

    NASA Technical Reports Server (NTRS)

    Adamovsky, G.; Tokars, R.; Varga, D.; Floyd B.

    2008-01-01

    The paper describes phenomena observed as a result of laser pencil beam interactions with abrupt interfaces including aerodynamic shocks. Based on these phenomena, a novel flow visualization technique based on a laser scanning pencil beam is introduced. The technique reveals properties of light interaction with interfaces including aerodynamic shocks that are not seen using conventional visualization. Various configurations of scanning beam devices including those with no moving parts, as well as results of "proof-of-concept" tests, are included.

  13. Bioassay-guided isolation of proanthocyanidins with antioxidant activity from peanut (Arachis hypogaea) skin by combination of chromatography techniques.

    PubMed

    Oldoni, Tatiane L C; Melo, Priscilla S; Massarioli, Adna P; Moreno, Ivani A M; Bezerra, Rosângela M N; Rosalen, Pedro L; da Silva, Gil V J; Nascimento, Andréa M; Alencar, Severino M

    2016-02-01

    Purification and bioassay-guided fractionation were employed to isolate proanthocyanidins with antioxidant activity from peanut skin (Arachis hypogaea Runner 886). The crude extract was prepared with acetone (60% v/v) and purified using chromatographic methods, including a semipreparative HPLC technique. As a result, two proanthocyanidins were isolated and identified using NMR, epicatechin-(2 β → O → 7, 4 β → 8)-catechin (proanthocyanidin A1) and epicatechin-(β → 2 O → 7, 4 β → 8)-epicatechin (proanthocyanidin A2). Despite the structural similarity, differences were observed in their antioxidant activity. Proanthocyanidin A1 proved to be more active, with EC50 value for DPPH radical scavenging of 18.25 μg/mL and reduction of Fe(3+)-TPTZ complex of 7.59 mmol/g, higher than that of synthetic antioxidant BHT. This compound evaluated by ABTS(+) was similar to that of natural quercetin. Therefore, peanut skin is an important source of bioactive compounds that may be used as a mild antioxidant for food preservation.

  14. Development of a rapid screening technique for organochlorine pesticides using solvent microextraction (SME) and fast gas chromatography (GC).

    PubMed

    de Jager, L S; Andrews, A R

    2000-11-01

    A novel, fast screening method for organochlorine pesticides (OCPs) in water samples has been developed. Total analysis time was less than 9 min, allowing 11 samples to be screened per hour. The relatively new technique of solvent microextraction (SME) was used to extract and preconcentrate the pesticides into a single drop of hexane. The use of a conventional carbon dioxide cryotrap was investigated for introduction of the extract onto a micro-bore (0.1 mm) capillary column for fast GC analysis. A pulsed-discharge electron capture detector was used which yielded selective and sensitive measurement of the pesticide peaks. Fast GC conditions were optimised and tested with the previously developed SME procedure. Calibration curves yielded good linearity and concentrations down to 0.25 ng mL-1 were detectable with RSD values ranging from 12.0 to 28% and LOD for most OCPs at 0.25 ng mL-1. Spiked river water samples were tested and using the developed screen we were able to differentiate between spiked samples and samples containing no OCPs.

  15. Application of filtering techniques in preprocessing magnetic data

    NASA Astrophysics Data System (ADS)

    Liu, Haijun; Yi, Yongping; Yang, Hongxia; Hu, Guochuang; Liu, Guoming

    2010-08-01

    High precision magnetic exploration is a popular geophysical technique for its simplicity and its effectiveness. The explanation in high precision magnetic exploration is always a difficulty because of the existence of noise and disturbance factors, so it is necessary to find an effective preprocessing method to get rid of the affection of interference factors before further processing. The common way to do this work is by filtering. There are many kinds of filtering methods. In this paper we introduced in detail three popular kinds of filtering techniques including regularized filtering technique, sliding averages filtering technique, compensation smoothing filtering technique. Then we designed the work flow of filtering program based on these techniques and realized it with the help of DELPHI. To check it we applied it to preprocess magnetic data of a certain place in China. Comparing the initial contour map with the filtered contour map, we can see clearly the perfect effect our program. The contour map processed by our program is very smooth and the high frequency parts of data are disappeared. After filtering, we separated useful signals and noisy signals, minor anomaly and major anomaly, local anomaly and regional anomaly. It made us easily to focus on the useful information. Our program can be used to preprocess magnetic data. The results showed the effectiveness of our program.

  16. The use of ultra-high pressure liquid chromatography with tandem mass spectrometric detection of analysis of agrochemical residues and mycotoxines in food - challenges and applications

    Technology Transfer Automated Retrieval System (TEKTRAN)

    In the field of food contaminant analysis, the most significant development of recent years has been the integration of ultra-high pressure liquid chromatography (UHPLC), coupled to tandem quadrupole mass spectrometry (MS/MS), into analytical applications. In this review, we describe the emergence o...

  17. Analysis of nitroguanidine in Aqueous Solutions by HPLC (High Performance Liquid Chromatography) with electrochemical Detection and Voltammetry

    DTIC Science & Technology

    1987-04-01

    The nitroguanidine was analyzed by high performance liquid chromatography (HPLC) with electrochemical detection at a hanging miercury drop electrode...previously reported on the application of solid sorbent collection techniques to the analysis of several explosives in water by high performance liquid chromatography (HPLC

  18. Chiral derivatizations applied for the separation of unusual amino acid enantiomers by liquid chromatography and related techniques.

    PubMed

    Ilisz, István; Aranyi, Anita; Péter, Antal

    2013-06-28

    Amino acids are essential for life, and have many functions in metabolism. One particularly important function is to serve as the building blocks of peptides and proteins, giving rise complex three dimensional structures through disulfide bonds or crosslinked amino acids. Peptides are frequently cyclic and contain proteinogenic as well as nonproteinogenic amino acids in many instances. Since most of the proteinogenic α-amino acids contain at least one stereogenic center (with the exception of glycine), the stereoisomers of all these amino acids and the peptides in which they are to be found may possess differences in biological activity in living systems. The impetus for advances in chiral separation has been highest in the past 25 years and this still continues to be an area of high focus. The important analytical task of the separation of isomers is achieved mainly by chromatographic and electrophoretic methods. This paper reviews indirect separation approaches, i.e. derivatization reactions aimed at creating the basis for the chromatographic resolution of biologically and pharmaceutically important enantiomers of unusual amino acids and related compounds, with emphasis on the literature published from 1980s. The main aspects of the chiral derivatization of amino acids are discussed, i.e. derivatization on the amino group, transforming the molecules into covalently bonded diastereomeric derivatives through the use of homochiral derivatizing agents. The diastereomers formed (amides, urethanes, urea and thiourea derivatives, etc.) can be separated on achiral stationary phases. The applications are considered, and in some cases different derivatizing agents for the resolution of complex mixtures of proteinogenic d,l-amino acids, non-proteinogenic amino acids and peptides/amino acids from peptide syntheses or microorganisms are compared.

  19. Application of Active Learning Techniques to an Advanced Course

    NASA Astrophysics Data System (ADS)

    Knop, R. A.

    2004-05-01

    The New Faculty Workshop provided a wealth of techniques as well as an overriding philosophy for the teaching of undergraduate Physics and Astronomy courses. The focus of the workshop was active learning, summarized in ``Learner-Centered Astronomy Teaching" by Slater & Adams: it's not what you do in class that matters, it's what the students do. Much of the specific focus of the New Faculty Workshop is on teaching the large, introductory Physics classes that many of the faculty present are sure to teach, both algebra-based and calculus-based. Many of these techniques apply directly and with little modification to introductory Astronomy courses. However, little direct attention is given to upper-division undergraduate, or even graduate, courses. In this presentation, I will share my experience in attempting to apply some of the techniques discussed at the New Faculty Workshop to an upper-division course in Galactic Astrophysics at Vanderbilt University during the Spring semester of 2004.

  20. Adiabatic Pseudospectral Technique: Applications to Four Atom Molecules

    NASA Astrophysics Data System (ADS)

    Antikainen, Jyrki Tapio

    1995-01-01

    After the introduction, in chapter 2 we review some of the well established techniques used to solve the Schrodinger equation. The following methods are discussed: the Finite Basis Representation, the Discrete Variable Representation, the Basic Light basis set truncation, and the Lanczos tridiagonalization. After reviewing the previous techniques we present the main features of our Adiabatic Pseudospectral (APS) technique. The Adiabatic Pseudospectral technique is a synthesis of several powerful computational methods such as the sequential adiabatic basis set reduction, the iterative Lanczos diagonalization, the collocation techniques, and a careful implementation of the matrix -vector product for the Hamiltonian in the reduced adiabatic representation. In chapter 3 we use our adiabatic pseudospectral method (APS) to calculate energy levels of the H _2O_2 molecule up to 5000 cm ^{-1}. Reasonably high accuracy (a few wavenumbers) is achieved for a fully six dimensional calculation in a few hours of CPU time on an IBM 580 workstation. These results are a great improvement over previous calculations on the same system which required 50-100 times more computational effort for a similar level of accuracy. The method presented here is both general and robust. It will allow for routine studies of six dimensional potential surfaces and the associated spectroscopy, while making calculations on still larger systems feasible. In chapter 4 the adiabatic pseudospectral method is used to study the high energy vibrational levels of the H_2C_2 molecule. We calculate stimulated emission pumping spectra initialized by the excited electronic state vibrational trans-bent state ~ A_sp{u}{1 }3_{nu}_3 . The calculations show that with the APS-method we can easily investigate energy regions in the excess of 15,000 cm^{-1}; these high energy regions have been previously unattainable by computational techniques.

  1. Applications of Indirect Imaging Techniques in X-ray Binaries

    NASA Astrophysics Data System (ADS)

    Harlaftis, E. T.

    A review is given on aspects of indirect imaging techniques in X-ray binaries which are used as diagnostics tools for probing the X-ray dominated accretion disc physics. These techniques utilize observed properties such as the emission line profile variability, the time delays between simultaneous optical/X-ray light curves, the light curves of eclipsing systems and the pulsed emission from the compact object in order to reconstruct the accretion disc's line emissivity (Doppler tomography), the irradiated disc and heated secondary (echo mapping), the outer disc structure (modified eclipse mapping) and the accreting regions onto the compact object, respectively.

  2. Single-cell epigenomics: techniques and emerging applications.

    PubMed

    Schwartzman, Omer; Tanay, Amos

    2015-12-01

    Epigenomics is the study of the physical modifications, associations and conformations of genomic DNA sequences, with the aim of linking these with epigenetic memory, cellular identity and tissue-specific functions. While current techniques in the field are characterizing the average epigenomic features across large cell ensembles, the increasing interest in the epigenetics within complex and heterogeneous tissues is driving the development of single-cell epigenomics. We review emerging single-cell methods for capturing DNA methylation, chromatin accessibility, histone modifications, chromosome conformation and replication dynamics. Together, these techniques are rapidly becoming a powerful tool in studies of cellular plasticity and diversity, as seen in stem cells and cancer.

  3. Extended MHD simulations for application to ITER disruption mitigation techniques

    NASA Astrophysics Data System (ADS)

    Woodruff, Simon; Stuber, James; Schetterer, Sam; ITER Disruption Mitigation Collaboration

    2013-10-01

    Various disruption scenarios are modeled computationally by use of the CORSICA and NIMROD codes, following the work of Kruger and Strauss with the aim of providing starting-points for investigation of tokamak disruption mitigation techniques. It is found that pressure-driven instabilities previously observed in simulations of DIII-D are verified, and that halo currents from vertical displacements are observed in simulations with implementation of resistive walls for ITER. We discuss implications and plans for simulations of disruption mitigation techniques. We outline validation activities for existing facilities. Work performed for USITER under DE-AC05-00OR22725 subcontract # 4000118643.

  4. Practical applications of activation analysis and other nuclear techniques

    SciTech Connect

    Lyon, W S

    1982-01-01

    Neeutron activation analysis (NAA) is a versatile, sensitive multielement, usually nondestructive analytical technique used to determine elemental concentrations in a variety of materials. Samples are irradiated with neutrons in a nuclear reactor, removed, and for the nondestructive technique, the induced radioactivity measured. This measurement of ..gamma.. rays emitted from specific radionuclides makes possible the quantitative determination of elements present. The method is described, advantages and disadvantages listed and a number of examples of its use given. Two other nuclear methods, particle induced x-ray emission and synchrotron produced x-ray fluorescence are also briefly discussed.

  5. Application of bag sampling technique for particle size distribution measurements.

    PubMed

    Mazaheri, M; Johnson, G R; Morawska, L

    2009-11-01

    Bag sampling techniques can be used to temporarily store the aerosol and therefore provide sufficient time to utilize sensitive but slow instrumental techniques for recording detailed particle size distributions. Laboratory based assessment of the method was conducted to examine size dependant deposition loss coefficients for aerosols held in Velostat bags conforming to a horizontal cylindrical geometry. Deposition losses of NaCl particles in the range of 10 nm to 160 nm were analysed in relation to the bag size, storage time, and sampling flow rate. Results of this study suggest that the bag sampling method is most useful for moderately short sampling periods of about 5 minutes.

  6. Atmospheric turbulence simulation techniques with application to flight analysis

    NASA Technical Reports Server (NTRS)

    Wang, S. T.; Frost, W.

    1980-01-01

    Statistical modeling of atmospheric turbulence is discussed. The statistical properties of atmospheric turbulence, in particular the probability distribution, the spectra, and the coherence are reviewed. Different atmospheric turbulence simulation models are investigated, and appropriate statistical analyses are carried out to verify their validity. The models for simulation are incorporated into a computer model of aircraft flight dynamics. Statistical results of computer simulated landings for an aircraft having characteristics of a DC-8 are reported for the different turbulence simulation techniques. The significance of various degrees of sophistication in the turbulence simulation techniques on the landing performance of the aircraft is discussed.

  7. Overview of image security techniques with applications in multimedia systems

    NASA Astrophysics Data System (ADS)

    Wolfgang, Raymond B.; Delp, Edward J., III

    1998-02-01

    The growth of networked multimedia system has created a need for the copyright protection of digital images and video. Copyright protection involves the authentication of image content and/or ownership. This can be used to identify illegal copies of an image. One approach is to mark an image by adding an invisible structure known as a digital watermark to the image. Techniques of incorporating such a watermark into digital images include spatial-domain techniques, transform-domain algorithms and sub-band filtering approaches.

  8. The application of image enhancement techniques to remote manipulator operation

    NASA Technical Reports Server (NTRS)

    Gonzalez, R. C.

    1974-01-01

    Methods of image enhancement which can be used by an operator who is not experienced with the mechanisms of enhancement to obtain satisfactory results were designed and implemented. Investigation of transformations which operate directly on the image domain resulted in a new technique of contrast enhancement. Transformations on the Fourier transform of the original image, including such techniques as homomorphic filtering, were also investigated. The methods of communication between the enhancement system and the computer operator were analyzed, and a language was developed for use in image enhancement. A working enhancement system was then created, and is included.

  9. Phosphoproteomics and molecular cardiology: techniques, applications and challenges.

    PubMed

    Sun, Zeyu; Hamilton, Karyn L; Reardon, Kenneth F

    2012-09-01

    Protein phosphorylation has been widely documented as a key regulatory and signaling mechanism associated with many cardiac diseases. Recent advances in phosphoproteomic technologies such as phosphopeptide enrichment, novel mass spectrometry applications, and bioinformatic tools have resulted in high-throughput identification and quantitation of protein phosphorylation in a global manner. This review summarizes mainstream phosphoproteomic workflows and highlights the most recent applications of phosphoproteomics used in a range of molecular cardiology research.

  10. Hydrogen sulfide measurement by headspace-gas chromatography-mass spectrometry (HS-GC-MS): application to gaseous samples and gas dissolved in muscle.

    PubMed

    Varlet, Vincent; Giuliani, Nicole; Palmiere, Cristian; Maujean, Géraldine; Augsburger, Marc

    2015-01-01

    The aim of our study was to present a new headspace-gas chromatography-mass spectrometry (HS-GC-MS) method applicable to the routine determination of hydrogen sulfide (H(2)S) concentrations in biological and gaseous samples. The primary analytical drawback of the GC/MS methods for H(2)S measurement discussed in the literature was the absence of a specific H(2)S internal standard required to perform quantification. Although a deuterated hydrogen sulfide (D(2)S) standard is currently available, this standard is not often used because this standard is expensive and is only available in the gas phase. As an alternative approach, D(2)S can be generated in situ by reacting deuterated chloride with sodium sulfide; however, this technique can lead to low recovery yield and potential isotopic fractionation. Therefore, N(2)O was chosen for use as an internal standard. This method allows precise measurements of H(2)S concentrations in biological and gaseous samples. Therefore, a full validation using accuracy profile based on the β-expectation tolerance interval is presented. Finally, this method was applied to quantify H(2)S in an actual case of H(2)S fatal intoxication.

  11. Physicochemical properties of silica gel coated with a thin layer of polyaniline (PANI) and its application in non-suppressed ion chromatography.

    PubMed

    Sowa, Ireneusz; Kocjan, Ryszard; Wójciak-Kosior, Magdalena; Swieboda, Ryszard; Zajdel, Dominika; Hajnos, Mieczysław

    2013-10-15

    Physicochemical properties of a new sorbent and its potential application in non-suppressed ion chromatography (IC) have been investigated. The sorbent was obtained in a process of covering silica gel particles with a film of polyaniline (PANI). The properties of silica modified with polyaniline such as particle size, porosity, average quantity of polyaniline covering carrier and density of sorbent were determined. In our study the following methods were used: microscopic analysis, laser diffraction technique, combustion analysis, mercury porosimetry and helium pycnometry. Column with the newly obtained packing was used for the separation of inorganic anions. Optimized chromatographic system was successfully employed for analysis of iodide and bromide in selected pharmaceutical products (Bochnia salt and Iwonicz salt) applied in chronic respiratory disease. Analysis was carried out using 0.1M solution of HCl in mixture of methanol/water (50:50v/v) as a mobile phase; the flow rate was 0.3 mL min(-1), temperature was 24°C and λ=210 nm. Validation parameters such as correlation coefficient, RSD values, recovery, detection and quantification limits were found to be satisfactory.

  12. Vortex-assisted hollow fibre liquid-phase microextraction technique combined with high performance liquid chromatography-diode array detection for the determination of oestrogens in milk samples.

    PubMed

    Wang, Peijin; Xiao, Yu; Liu, Wenjun; Wang, Juan; Yang, Yaling

    2015-04-01

    A rapid, simple, sensitive and environmentally friendly method has been developed for the determination of three oestrogens (17β-estradiol (17β-E2), estrone (E1), and diethylstilbestrol (DES)) in milk samples by using vortex-assisted hollow fibre liquid-phase microextraction (VA-HF-LPME) and high performance liquid chromatography. Method is based on the microextraction of oestrogens from sample solution into 15 μL of nonanoic acid as extracting agent, which is placed inside the hollow fibre followed by vortex-mixing. Vortex provided effective and mild mixing of sample solution and increased the contact between analytes and boundary layers of the hollow fibre, thereby enhancing mass transfer rate and leading to high recovery of target analytes. The extraction equilibrium is achieved within 2 min. Parameters influencing the recovery were investigated and optimized. The proposed technique provided good linearity (>0.9984), repeatability (RSD = 2.56-4.38), low limits of detection (0.06-0.17 ng mL(-1)), and high enrichment factor (330).

  13. Rapid determination of trace dicyandiamide in mussels from Zhejiang coast by ultra-fast liquid chromatography-tandem mass spectrometry with isotope internal standard dilution technique.

    PubMed

    Zhang, Yun; Gong, Wen-Jie; Zhao, Yong-Gang; Zhou, Hua

    2014-12-01

    In this study, a rapid and accurate ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) method coupled with the isotope internal standard dilution technique was established and validated to determine trace dicyandiamide (DCD) in mussels. The sample was extracted by acetonitrile, and chromatographic separations were performed on an Acquity UPLC BEH Amide column by using water-acetonitrile (9:91, v/v) as the mobile phase within 3 min. DCD was determined by using DCD-(15)N4 as an internal standard. The results showed that the recoveries were between 96.2 and 103 % with relative standard deviations (RSDs) in the range of 0.6-6.0 %. The limit of quantification (LOQ) was 0.05 μg/kg. This method can be applied to the routine analysis for the rapid and sensitive determination of trace DCD in mussels. Overall, the data reiterate the importance of investigating the presence of DCD in marine biological samples, which can act as food quality controls for human health.

  14. Rapid confirmation of enzyme multiplied immunoassay technique (EMIT) cocaine positive urine samples by capillary gas-liquid chromatography/nitrogen phosphorus detection (GLC/NPD).

    PubMed

    Verebey, K; DePace, A

    1989-01-01

    A rapid gas-liquid chromatographic (GLC) method was developed for the confirmation of benzoylecgonine (BE) positive urine samples screened by the enzyme multiplied immunoassay technique (EMIT) assay. The procedure is performed by solvent extraction of BE from 0.1 or 0.2 mL of urine, followed by an aqueous wash of the solvent and evaporation. The dried residue was derivatized with 50 microL of pentafluoropropionic anhydride and 25 microL of pentafluoropropropanol at 90 degrees C for 15 min. The derivatizing reagents were evaporated to dryness, and the derivatized BE, and cocaine if present, were reconstituted and injected into the gas chromatograph. The column was a 15-m by 0.2-mm fused silica capillary column, coated with 0.25 micron of DB-1, terminating in a nitrogen phosphorus detector (NPD). Cocaine and the pentafluoro BE derivatives retention times were 3.2 and 2.6 min, respectively. Nalorphine was used as reference or internal standard with a retention time of 4.78 min. The complete procedure can be performed in approximately 1.5 h. The EMIT cutoff between positive and negative urine samples is 300 ng/mL of BE. The lower limit of sensitivity of this method is 25 ng of BE extracted from urine. Validation studies resulted in confirmation of 101 out of 121 EMIT cocaine positive urine samples that could not be confirmed by thin-layer chromatography (TLC). This represents 84% confirmation efficiency.

  15. Extraction of three bioactive diterpenoids from Andrographis paniculata: effect of the extraction techniques on extract composition and quantification of three andrographolides using high-performance liquid chromatography.

    PubMed

    Kumar, Satyanshu; Dhanani, Tushar; Shah, Sonal

    2014-10-01

    Andrographis paniculata (Burm.f.) wall.ex Nees (Acanthaceae) or Kalmegh is an important medicinal plant finding uses in many Ayurvedic formulations. Diterpenoid compounds andrographolides (APs) are the main bioactive phytochemicals present in leaves and herbage of A. paniculata. The efficiency of supercritical fluid extraction (SFE) using carbon dioxide was compared with the solid-liquid extraction techniques such as solvent extraction, ultrasound-assisted solvent extraction and microwave-assisted solvent extraction with methanol, water and methanol-water as solvents. Also a rapid and validated reverse-phase high-performance liquid chromatography-diode array detection method was developed for the simultaneous determination of the three biologically active compounds, AP, neoandrographolide and andrograpanin, in the extracts of A. paniculata. Under the best SFE conditions tested for diterpenoids, which involved extraction at 60°C and 100 bar, the extractive efficiencies were 132 and 22 µg/g for AP and neoandrographolide, respectively. The modifier percentage significantly affected the extraction efficiency.

  16. Application of Frontal Affinity Chromatography to Study the Biomolecular Interactions with Trypsin.

    PubMed

    Hu, YuanYuan; Qian, Junqing; Guo, Hui; Jiang, ShengLan; Zhang, Zheng

    2015-07-01

    Trypsin is a serine protease that has been proposed as a potential therapeutic target for metabolic disorders and malignancy diseases, thus the identification of biomolecular interactions of compounds to trypsin could be of great therapeutic importance. In this study, trypsin was immobilized on a monolithic silica capillary column via sol-gel. The binding properties of four small molecules (daidzin, genistin, matrine and oxymatrine) to trypsin were examined using the trypsin affinity columns by frontal analysis. The results indicate that the matrine (dissociation constant, Kd = 7.904 μM) has stronger interaction with trypsin than the oxymatrine (Kd = 8.204 μM), whereas daidzin and genistin were nearly have no affinity with trypsin. The results demonstrated that the frontal affinity chromatography can be used for the direct determination of protein-protease inhibitor binding interactions and have several significant advantages, including easy fabricating, reproducible, minimal technological requirements and potential to become a reliable alternative for quantitative studies of biomolecular interactions.

  17. Application of finite inverse gas chromatography in hypromellose acetate succinate-water-acetone systems.

    PubMed

    Chiu, Sheng-Wei; Sturm, Derek R; Moser, Justin D; Danner, Ronald P

    2016-09-30

    A modification of a GC was developed to investigate both infinitely dilute and finite concentrations of solvents in polymers. Thermodynamic properties of hypromellose acetate succinate (HPMCAS-L)-acetone-water systems are important for the optimization of spray-drying processes used in pharmaceutical manufacturing of solid dispersion formulations. These properties, at temperatures below the glass transition temperature, were investigated using capillary column inverse gas chromatography (CCIGC). Water was much less soluble in the HPMCAS-L than acetone. Experiments were also conducted at infinitely dilute concentrations of one of the solvents in HPMCAS-L that was already saturated with the other solvent. Overall the partitioning of the water was not significantly affected by the presence of either water or acetone in the polymer. The acetone partition coefficient decreased as either acetone or water was added to the HPMCAS-L. A representation of the HPMCAS-L structure in terms of UNIFAC groups has been developed. With these groups, the UNIFAC-vdw-FV model did a reasonable job of predicting the phase equilibria in the binary and ternary systems. The Flory-Huggins correlation with fitted interaction parameters represented the data well.

  18. Liquid chromatography/tandem mass spectrometry method for quantitation of cremophor el and its applications.

    PubMed

    Vijaya Bhaskar, V; Middha, Anil

    2013-01-01

    A rapid sensitive and selective MRM based method for the determination of Cremophor EL (CrEL) in rat plasma was developed using liquid chromatography/tandem mass spectrometry (LC-MS/MS). CrEL and polypropylene glycol (internal standard) were extracted from rat plasma with acetonitrile and analysed on C18 column (XBridge, 50 × 4.6 mm, 3.5  μ m). The most abundant molecular ions corresponding to PEG oligomers at m/z 828, 872, 916 and 960 with daughter ion at m/z 89 were selected for multiple reaction monitoring (MRM) in electrospray mode of ionisation. Plasma concentrations of CrEL were quantified after administration through oral and intravenous routes in male sprague dawley rats at a dose of 0.26 g/kg. The standard curve was linear (0.9972) over the concentration range of 1.00 to 200  μ g/mL. The lower limit of quantitation for CrEL was 1.00  μ g/mL using 50  μ L plasma. The coefficient of variation and relative error for inter and intra assay at three QC levels were 0.69 to 9.21 and -7.60 to 4.74 respectively. A novel proposal was conveyed to the scientific community, where formulation excipient can be analysed as qualifier in the analysis of NCEs to address the spiky plasma concentration profiles.

  19. Application of knowledge-based network processing to automated gas chromatography data interpretation

    SciTech Connect

    Levis, A.P.; Timpany, R.G.; Klotter, D.A.

    1995-10-01

    A method of translating a two-way table of qualified symptom/cause relationships into a four layer Expert Network for diagnosis of machine or sample preparation failure for Gas Chromatography is presented. This method has proven to successfully capture an expert`s ability to predict causes of failure in a Gas Chromatograph based on a small set of symptoms, derived from a chromatogram, in spite of poorly defined category delineations and definitions. In addition, the resulting network possesses the advantages inherent in most neural networks: the ability to function correctly in the presence of missing or uncertain inputs and the ability to improve performance through data-based training procedures. Acquisition of knowledge from the domain experts produced a group of imprecise cause-to-symptom relationships. These are reproduced as parallel pathways composed of Symptom-Filter-Combination-Cause node chains in the network representation. Each symptom signal is passed through a Filter node to determine if the signal should be interpreted as positive or negative evidence and then modified according to the relationship established by the domain experts. The signals from several processed symptoms are then combined in the Combination node(s) for a given cause. The resulting value is passed to the Cause node and the highest valued Cause node is then selected as the most probable cause of failure.

  20. Determination of tolperisone in human plasma by liquid chromatography/tandem mass spectrometry for clinical application.

    PubMed

    Choi, Chang-Ik; Park, Jung-In; Lee, Hye-In; Lee, Yun-Jeong; Jang, Choon-Gon; Bae, Jung-Woo; Lee, Seok-Yong

    2012-12-12

    We have developed and validated a simple, rapid, and sensitive liquid chromatography analytical method employing tandem mass spectrometry (LC-MS/MS) for the determination of tolperisone, a centrally acting muscle relaxant, in human plasma. After liquid-liquid extraction with methyl t-butyl ether, chromatographic separation of tolperisone was performed using a reversed-phase Luna C(18) column (2.0mm×50mm, 5μm particles) with a mobile phase of 10mM ammonium formate buffer (pH 3.5) - methanol (12:88, v/v) and quantified by tandem mass detection in ESI positive ion mode. The flow rate of the mobile phase was 250μL/min and the retention times of tolperisone and the internal standard (IS, dibucaine) were both 0.6min. The calibration curves were linear over a range of 0.5-300ng/mL (r>0.999). The lower limit of quantification, using 200μL human plasma, was 0.5ng/mL. The mean accuracy and precision for intra- and inter-day validation of tolperisone were within acceptable limits. The LC-MS/MS method reported here showed improved sensitivity for quantification of tolperisone in human plasma compared with previously described analytical methods. Lastly, the validated method was successfully applied to a pharmacokinetic study in humans.

  1. Parameter estimation techniques and application in aircraft flight testing

    NASA Technical Reports Server (NTRS)

    1974-01-01

    Technical papers presented at the symposium by selected representatives from industry, universities, and various Air Force, Navy, and NASA installations are given. The topics covered include the newest developments in identification techniques, the most recent flight-test experience, and the projected potential for the near future.

  2. Techniques for application of tissue adhesive for corneal perforations.

    PubMed

    Erdey, R A; Lindahl, K J; Temnycky, G O; Aquavella, J V

    1991-06-01

    We describe a modified technique of using cyanoacrylate adhesive to seal corneal perforations. Easily performed at the slit lamp, its advantages over previously described methods include a smooth, contoured collagen surface overlying the adhesive, which is easily wet by the tear film. Even greater comfort and protection are provided by the addition of a hydrophilic bandage lens or collagen shield.

  3. PROGRAM EVALUATION AND REVIEW TECHNIQUE--APPLICATIONS IN EDUCATION.

    ERIC Educational Resources Information Center

    COOK, DESMOND L.

    THIS MONOGRAPH IS INTENDED TO DISSEMINATE TO THE EDUCATIONAL COMMUNITY THE BASIC CONCEPTS AND PRINCIPLES OF A RECENTLY DEVELOPED PROJECT MANAGEMENT INFORMATION SYSTEM ENTITLED PROGRAM EVALUATION AND REVIEW TECHNIQUE (PERT). PERT IS A METHODOLOGY FOR PLANNING THE DIVERSE ACTIVITIES IN EITHER LARGE OR SMALL PROJECTS. STEPS OF THE PERT TECHNIQUE…

  4. 48 CFR 9904.420-50 - Techniques for application.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... shall be excluded from the IR&D and B&P cost pools to be allocated to other segments and the base data... final cost objectives and the particular final cost objective's base data shall be excluded from the... 48 Federal Acquisition Regulations System 7 2010-10-01 2010-10-01 false Techniques for...

  5. 48 CFR 9905.502-50 - Techniques for application.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ..., OFFICE OF FEDERAL PROCUREMENT POLICY, OFFICE OF MANAGEMENT AND BUDGET PROCUREMENT PRACTICES AND COST ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS FOR EDUCATIONAL INSTITUTIONS 9905.502-50 Techniques for... submitted by the educational institution will require that the institution set forth its cost...

  6. 48 CFR 9905.506-50 - Techniques for application.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... transitional cost accounting period is required under the provisions of 9905.506-40(a)(3), the institution may.... 9905.506-50 Section 9905.506-50 Federal Acquisition Regulations System COST ACCOUNTING STANDARDS BOARD... ACCOUNTING STANDARDS COST ACCOUNTING STANDARDS FOR EDUCATIONAL INSTITUTIONS 9905.506-50 Techniques...

  7. One-step multiple component isolation from the oil of Crinitaria tatarica (Less) Sojak by preparative capillary gas chromatography with characterization by spectroscopic and spectrometric techniques

    Technology Transfer Automated Retrieval System (TEKTRAN)

    In the present work multiple component isolation from the oil of Crinitaria tatarica (Less.) Sojak. by Preparative Capillary Gas Chromatography (PCGC) with characterization by mass spectrometry (MS) and nuclear magnetic resonance (NMR) spectroscopy have been carried out. Gas chromatography (GC-FID) ...

  8. Improved analysis of vitamin D metabolites in plasma using liquid chromatography tandem mass spectrometry, and its application to cardiovascular research.

    PubMed

    Sandhu, Jatinderpal K; Auluck, Janica; Ng, Leong L; Jones, Donald J L

    2014-06-01

    The accurate and specific measurement of vitamin D is increasingly important for determining the role of vitamin D in the pathogenesis of disease. Liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS) has increasingly become the analytical modality of choice for the analysis of vitamin D. There are many advantages to using LC/MS/MS, such as high specificity and sensitivity to help distinguish the isomers of vitamin D. This rapid method, modified from a Waters Corporation application note, consists of minimal sample manipulation using liquid-liquid extraction and incorporates an internal standard. The supernatant is dried down and injected onto an ultra-high-performance liquid chromatography/electrospray ionization tandem mass spectrometer. The total analysis time is 10 min per injection, enabling high throughput of samples. This method also incorporates two commercial quality control standards to provide a robust system with acceptable coefficient of variation. The analysis of control and heart failure plasma samples showed significant differences in the levels of vitamin D3 between these two groups; however, in the control group, there were individuals who were vitamin D deficient. Overall, the vitamin D3 levels were higher in control samples than in heart failure individuals. As expected, vitamin D2 levels were not observed in many of the samples analysed. This modified method is quick and incorporates an internal standard to allow for any loss in the extraction procedure. The method also includes quality control samples to enable assay standardization. The assay involves inexpensive pre-sample clean-up, aiding high throughput, which is important in many laboratories.

  9. Quantitation of metformin in human plasma and urine by hydrophilic interaction liquid chromatography and application to a pharmacokinetic study.

    PubMed

    Nielsen, Flemming; Christensen, Mette M H; Brøsen, Kim

    2014-04-01

    We describe an analytical method for the quantification of the widely used antihyperglycemic agent, metformin, in human plasma and urine. The separation was performed using isocratic hydrophilic interaction liquid chromatography on a Luna hydrophilic interaction liquid chromatography column (125 × 4.6 mm, 3 μm). The sample preparation was accomplished by solid-phase extraction. Validation of the method was performed in the range 10-2000 ng/mL for plasma and 5-30 mcg/mL for urine. The methods were linear within the investigated range (r(2) > 0.988). Within-day repeatability ranged from 3.1% to 7.5% in plasma and 1.6% to 6.2% in urine. Between-day reproducibility ranged from 2.9% to 5.3% in plasma and 0.6% to 1.8% in urine. The inaccuracy expressed as bias ranged from -3.1% to 1.9% in plasma and from -7.2% to 0.7% in urine. The lower limit of quantification for metformin in plasma was 5 ng/mL and in urine was 40 ng/mL. The method was therefore considered to be precise, accurate, reproducible, and sensitive enough to be appropriate for pharmacokinetic studies of metformin. The applicability of the method for human pharmacokinetic studies was demonstrated by dosing a healthy male volunteer with 500-mg metformin hydrochloride as a single oral dose; plasma and urine concentrations were measured for 24 hours.

  10. Exploring the potentialities of an improved ultrasound-assisted quick, easy, cheap, effective, rugged, and safe-based extraction technique combined with ultrahigh pressure liquid chromatography-fluorescence detection for determination of Zearalenone in cereals.

    PubMed

    Porto-Figueira, Priscilla; Camacho, Irene; Câmara, José S

    2015-08-21

    Zearalenone (ZEA), a secondary metabolite from Fusarium graminearum fungi that invade crops and grow during blooming in moist cool field conditions, is a nonsteroidal oestrogen, biologically very potent, although hardly toxic. Different analytical methods, among which a quick, easy, cheap, effective, rugged, and safe (QuEChERS) strategy, combined with or liquid chromatography, have been proposed for ZEA determination in foods. However, this extraction procedure has the disadvantage of using large amount of organic solvents, partitioning salts and sample volume, which limits the technique application on the fields where the sample amount is critical. Therefore in this work an improved sample preparation step based on the original QuEChERS (O-QuEChERS) approach, the μ-QuEChERS, combined with ultrasound-assisted extraction (USAE) and ultrahigh pressure liquid chromatography (UHPLC) analysis with fluorescence detection (FLR) is proposed for the sensitive and high-throughput quantification of ZEA in cereals. The proposed analytical strategy, μ-QuEChERSUSAE, uses up to 32 times lower amounts of partitioning salts, lower sample amount and lower extraction solvents, in comparison with O-QuEChERS technique. The performance of the analytical approach was assessed by studying the selectivity, specificity, limits of detection and quantification, linear dynamic range, matrix effect and precision. Good linearity (r(2)>0.99) was achieved for ZEA, and limits of detection (LOD=3.4μgkg(-1)) and limits of quantification (LOQ=4.7μgkg(-1)) were found below the tolerance levels set by European Commission. Good recoveries were obtained with different spiked concentrations, ranged from 80.2% to 109.7%, with relative standard deviations (RSD) lower than 5.0%. The comparison of the analytical performance of the proposed μ-QuEChERSUSAE with O-QuEChERS showed the powerful ability of the proposed strategy since it gives comparable results but using lower amounts of sample, partitioning

  11. Techniques of EMG signal analysis: detection, processing, classification and applications

    PubMed Central

    Hussain, M.S.; Mohd-Yasin, F.

    2006-01-01

    Electromyography (EMG) signals can be used for clinical/biomedical applications, Evolvable Hardware Chip (EHW) development, and modern human computer interaction. EMG signals acquired from muscles require advanced methods for detection, decomposition, processing, and classification. The purpose of this paper is to illustrate the various methodologies and algorithms for EMG signal analysis to provide efficient and effective ways of understanding the signal and its nature. We further point up some of the hardware implementations using EMG focusing on applications related to prosthetic hand control, grasp recognition, and human computer interaction. A comparison study is also given to show performance of various EMG signal analysis methods. This paper provides researchers a good understanding of EMG signal and its analysis procedures. This knowledge will help them develop more powerful, flexible, and efficient applications. PMID:16799694

  12. Apt strain measurement technique for impulsive loading applications

    NASA Astrophysics Data System (ADS)

    Ranjan Nanda, Soumya; Kulkarni, Vinayak; Sahoo, Niranjan

    2017-03-01

    The necessity of precise measurement of strain time history for impulsive loading applications has been addressed in the present investigation. Finite element modeling is initially carried out for a hemispherical test model and stress bar assembly to arrive at an appropriate location for strain measurement. In dynamic calibration experiments, strain measurements are performed using two wire and three wire quarter bride arrangements along with half bridge circuit. Usefulness of these arrangements has been verified by analyzing strain signals in time and frequency domains. Comparison of recovered force time histories proved that the half bridge circuit is the most suitable for such applications. Actual shock tube testing of the instrumented hemispherical test model confirmed the applicability of half bridge circuit for short duration strain measurements.

  13. Combinative application of pH-zone-refining and conventional high-speed counter-current chromatography for preparative separation of caged polyprenylated xanthones from gamboge.

    PubMed

    Xu, Min; Fu, Wenwei; Zhang, Baojun; Tan, Hongsheng; Xiu, Yanfeng; Xu, Hongxi

    2016-02-01

    An efficient method for the preparative separation of four structurally similar caged xanthones from the crude extracts of gamboge was established, which involves the combination of pH-zone-refining counter-current chromatography and conventional high-speed counter-current chromatography for the first time. pH-zone-refining counter-current chromatography was performed with the solvent system composed of n-hexane/ethyl acetate/methanol/water (7:3:8:2, v/v/v/v), where 0.1% trifluoroacetic acid was added to the upper organic stationary phase as a retainer and 0.03% triethylamine was added to the aqueous mobile phase as an eluter. From 3.157 g of the crude extract, 1.134 g of gambogic acid, 180.5 mg of gambogenic acid and 572.9 mg of a mixture of two other caged polyprenylated xanthones were obtained. The mixture was further separated by conventional high-speed counter-current chromatography with a solvent system composed of n-hexane/ethyl acetate/methanol/water (5:5:10:5, v/v/v/v) and n-hexane/methyl tert-butyl ether/acetonitrile/water (8:2:6:4,v/v/v/v), yielding 11.6 mg of isogambogenic acid and 10.4 mg of β-morellic acid from 218.0 mg of the mixture, respectively. The purities of all four of the compounds were over 95%, as determined by high-performance liquid chromatography, and the chemical structures of the four compounds were confirmed by electrospray ionization mass spectrometry and NMR spectroscopy. The combinative application of pH-zone-refining counter-current chromatography and conventional high-speed counter-current chromatography shows great advantages in isolating and enriching the caged polyprenylated xanthones.

  14. Dynamic mechanical analysis: A practical introduction to techniques and applications

    SciTech Connect

    Menard, K.

    1999-03-01

    This introduction provides the chemist, chemical engineer, or materials scientists with a starting point to understand the applications of dynamic mechanical analysis, its workings, and its advantages and limitations. This book serves as a systematic study of manufacturing polymeric materials and components as well as for developing new materials. Contents include: introduction to dynamic mechanical analysis; basic rheological concepts: stress, strain, and flow; rheology basic: creep-recovery and stress relaxation; dynamic testing; time-temperature scans part 1: transitions in polymers; time and temperature studies part 2: thermosets; frequency scans; DMA applications to real problems: guidelines; and appendix: sample experiments for the DMA.

  15. Application of Artificial Intelligence Techniques in Uninhabited Aerial Vehicle Flight

    NASA Technical Reports Server (NTRS)

    Dufrene, Warren R., Jr.

    2004-01-01

    This paper describes the development of an application of Artificial Intelligence (AI) for Unmanned Aerial Vehicle (UAV) control. The project was done as part of the requirements for a class in AI at NOVA Southeastearn University and a beginning project at NASA Wallops Flight Facility for a resilient, robust, and intelligent UAV flight control system. A method is outlined which allows a base level application for applying an Artificial Intelligence method, Fuzzy Logic, to aspects of Control Logic for UAV flight. One element of UAV flight, automated altitude hold, has been implemented and preliminary results displayed.

  16. Application of Artificial Intelligence Techniques in Uninhabitated Aerial Vehicle Flight

    NASA Technical Reports Server (NTRS)

    Dufrene, Warren R., Jr.

    2003-01-01

    This paper describes the development of an application of Artificial Intelligence (AI) for Unmanned Aerial Vehicle (UAV) control. The project was done as part of the requirements for a class in AI at NOVA southeastern University and a beginning project at NASA Wallops Flight Facility for a resilient, robust, and intelligent UAV flight control system. A method is outlined which allows a base level application for applying an Artificial Intelligence method, Fuzzy Logic, to aspects of Control Logic for UAV flight. One element of UAV flight, automated altitude hold, has been implemented and preliminary results displayed.

  17. Nightmares in crisis: clinical applications of lucid dreaming techniques.

    PubMed

    Brylowski, A

    1990-06-01

    A patient in crisis was offered treatment with a major focus on alleviating nightmares using lucid dreaming (dreaming while knowing that one is dreaming). Of sixty-eight non-psychotic patients seen consecutively in a psychiatry emergency room, she was one of 16 (23.5%) found to have a concurrent complaint of nightmares (dream anxiety disorder). The benefits of the skills developed with lucid dreaming extended into areas other than nightmares as the patient entered psychotherapy. The techniques appeared to play a role in the reduction of nightmare frequency, intensity, and distress, and to enhance ego growth and personal development. Further research in lucid dreaming as an adjunctive treatment for patients with nightmares and as a useful technique in psychotherapy is suggested.

  18. On the selection of dimension reduction techniques for scientific applications

    SciTech Connect

    Fan, Y J; Kamath, C

    2012-02-17

    Many dimension reduction methods have been proposed to discover the intrinsic, lower dimensional structure of a high-dimensional dataset. However, determining critical features in datasets that consist of a large number of features is still a challenge. In this paper, through a series of carefully designed experiments on real-world datasets, we investigate the performance of different dimension reduction techniques, ranging from feature subset selection to methods that transform the features into a lower dimensional space. We also discuss methods that calculate the intrinsic dimensionality of a dataset in order to understand the reduced dimension. Using several evaluation strategies, we show how these different methods can provide useful insights into the data. These comparisons enable us to provide guidance to a user on the selection of a technique for their dataset.

  19. Image Guidance in Radiation Therapy: Techniques and Applications

    PubMed Central

    Kataria, Tejinder

    2014-01-01

    In modern day radiotherapy, the emphasis on reduction on volume exposed to high radiotherapy doses, improving treatment precision as well as reducing radiation-related normal tissue toxicity has increased, and thus there is greater importance given to accurate position verification and correction before delivering radiotherapy. At present, several techniques that accomplish these goals impeccably have been developed, though all of them have their limitations. There is no single method available that eliminates treatment-related uncertainties without considerably adding to the cost. However, delivering “high precision radiotherapy” without periodic image guidance would do more harm than treating large volumes to compensate for setup errors. In the present review, we discuss the concept of image guidance in radiotherapy, the current techniques available, and their expected benefits and pitfalls. PMID:25587445

  20. MR enterography in children: Principles, technique, and clinical applications.

    PubMed

    Chavhan, Govind B; Babyn, Paul S; Walters, Thomas

    2013-04-01

    MR enterography is a constantly advancing technique for assessment of bowel with newer technology and sequences. It is being increasingly used for the assessment of inflammatory bowel disease and has almost replaced barium follow through examinations in many institutions. Its lack of radiation makes it an attractive alternative for bowel evaluation in children. It has been proved to be highly sensitive in the detection of Crohn disease in adults and children. It is also superior to barium studies in showing extra-enteric findings and detecting complications such as fistulas and abscesses. Even though at present it is almost exclusively used for the evaluation of inflammatory bowel disease, it has the potential to be used in other conditions affecting the bowel. The principles, MR enterography technique pertinent to children, and its utility in the assessment of Crohn disease in children are discussed in this review.

  1. Estimation and filtering techniques for high-accuracy GPS applications

    NASA Technical Reports Server (NTRS)

    Lichten, S. M.

    1989-01-01

    Techniques for determination of very precise orbits for satellites of the Global Positioning System (GPS) are currently being studied and demonstrated. These techniques can be used to make cm-accurate measurements of station locations relative to the geocenter, monitor earth orientation over timescales of hours, and provide tropospheric and clock delay calibrations during observations made with deep space radio antennas at sites where the GPS receivers have been collocated. For high-earth orbiters, meter-level knowledge of position will be available from GPS, while at low altitudes, sub-decimeter accuracy will be possible. Estimation of satellite orbits and other parameters such as ground station positions is carried out with a multi-satellite batch sequential pseudo-epoch state process noise filter. Both square-root information filtering (SRIF) and UD-factorized covariance filtering formulations are implemented in the software.

  2. [Functional magnetic resonance imaging: physiopathology, techniques and applications].

    PubMed

    Delmaire, C; Krainik, A; Lethuc, V; Reyns, N; Duffau, H; Capelle, L; Lehéricy, S

    2007-03-01

    Brain functional MRI (fMRI) provides an indirect mapping of cerebral activity, based on the detection of local changes in blood flow and oxygenation levels that are associated with neuronal activity (BOLD contrast). fMRI allows noninvasive studies of normal and pathological aspects of the brain's functional organization. It is based on the comparison of two or more cognitive states. Echoplanar imaging is the technique of choice, providing the quickest study of the entire brain. Activation maps are calculated from a statistical analysis of the local signal changes. fMRI has become one of the most widely used functional imaging techniques in neuroscience. In clinical practice, fMRI can identify eloquent areas involved in motor and language functions in surgical patients and can evaluate the risk of postoperative neurological deficit.

  3. New Developments in LC-MS and Other Hyphenated Techniques

    SciTech Connect

    Belov, Mikhail E.; Kurulugama, Ruwan T.; Lopez-Ferrer, Daniel; Ibrahim, Yehia M.; Baker, Erin Shammel

    2011-06-21

    Extensive challenges faced by analytical chemists in studying real world complex samples such as biological body fluids, tissue samples, environmental and geological samples have lead to the development of advanced analytical approaches. The vast array of contemporary technologies can be categorized into two major areas: sample separation and mass spectrometry analysis. Current state-of-the-art sample separation methods include gas chromatography, high performance liquid chromatography, ultra high pressure liquid chromatography, solid phase extraction, capillary electrophoresis, and gas phase separation techniques such as ion mobility spectrometry. The recent trend in sample separation is to combine (or hyphenate) multiple techniques that employ different separation mechanisms to maximize separation efficiency. The most widely used combinations include two-dimensional gas chromatography, strong cation exchange or weak cation exchange chromatography followed by reversed-phase liquid chromatography, two-dimensional reversed-phase liquid chromatography, liquid chromatography followed by ion mobility spectrometry and two-dimensional electrophoresis techniques. The introduction of atmospheric pressure ionization techniques such as electrospray ionization and matrix assisted laser desorption ionization and variations of the two have drastically increased the impact of mass spectrometry on bioanalytical applications. Mass spectrometry itself has tremendously improved over the years in terms of sensitivity, detection limits, dynamic range and sequencing capabilities. Currently, mass spectrometers can attain zeptomolole detection limits with five orders of magnitude dynamic range. In this chapter, we summarize recent developments in hyphenated techniques and their applications to complex sample analysis.

  4. Coupling Temperature Control with Electrochemically Modulated Liquid Chromatography: Fundamental Aspects and Applications

    SciTech Connect

    Ponton, Lisa M.

    2004-12-19

    The primary focus of the doctoral research presented herein has been the integration of temperature control into electrochemically modulated liquid chromatography (EMLC). The combination of temperature control and the tunable characteristics of carbonaceous EMLC stationary phases have been invaluable in deciphering the subtleties of the retention mechanism. The effects of temperature and Eapp on the retention of several naphthalene disulfonates were therefore examined by the van' Hoff relationship. The results indicate that while the retention of both compounds is exothermic at levels comparable to that in many reversed-phase separations, the potential dependence of the separation is actually entropically affected in a manner paralleling that of several classical ion exchange systems. Furthermore, the retention of small inorganic anions at constant temperature also showed evidence of an ion exchange type of mechanism. While a more complete mechanistic description will come from examining the thermodynamics of retention for a wider variety of analytes, this research has laid the groundwork for full exploitation of temperature as a tool to develop retention rules for EMLC. Operating EMLC at elevated temperature and flow conditions has decreased analysis time and has enabled the separation of analytes not normally achievable on a carbon stationary phase. The separation of several aromatic sulfonates was achieved in less than 1 min, a reduction of analysis time by more than a factor of 20 as compared to room temperature separations. The use of higher operating temperatures also facilitated the separation of this mixture with an entirely aqueous mobile phase in less than 2 min. This methodology was extended to the difficult separation of polycyclic aromatic hydrocarbons on PGC. This study also brought to light the mechanistic implications of the unique retention behavior of these analytes through variations of the mobile phase composition.

  5. Application of oil gas-chromatography in reservoir compartmentalization in a mature Venezuelan oil field

    SciTech Connect

    Munoz, N.G.; Mompart, L.; Talukdar, S.C.

    1996-08-01

    Gas chromatographic oil {open_quotes}fingerprinting{close_quotes} was successfully applied in a multidisciplinary production geology project by Maraven, S.A. to define the extent of vertical and lateral continuity of Eocene and Miocene sandstone reservoirs in the highly faulted Bloque I field, Maracaibo Basin, Venezuela. Seventy-five non-biodegraded oils (20{degrees}-37.4{degrees} API) were analyzed with gas chromatography. Fifty were produced from the Eocene Misoa C-4, C-5, C-6 or C-7 horizons, fifteen from the Miocene basal La Rosa and ten from multizone completions. Gas chromatographic and terpane and sterane biomarker data show that all of the oils are genetically related. They were expelled from a type II, Upper Cretaceous marine La Luna source rock at about 0.80-0.90% R{sub o} maturity. Alteration in the reservoir by gas stripping with or without subsequent light hydrocarbons mixing was observed in some oils. Detailed chromatographic comparisons among the oils shown by star plots and cluster analysis utilizing several naphthenic and aromatic peak height ratios, resulted in oil pool groupings. This led to finding previously unknown lateral and vertical reservoir communication and also helped in checking and updating the scaling character of faults. In the commingled oils, percentages of each contributing zone in the mixture were also determined giving Maraven engineers a proven, rapid and inexpensive tool for production allocation and reservoir management The oil pool compartmentalization defined by the geochemical fingerprinting is in very good agreement with the sequence stratigraphic interpretation of the reservoirs and helped evaluate the influence of structure in oil migration and trapping.

  6. Innovative instrument design and applications in supercritical fluid chromatography and extraction

    SciTech Connect

    Oudsema, J.W.

    1992-01-01

    A novel sample introduction system was developed for supercritical fluid chromatography. The solventless injector utilizes a gas purge for solvent elimination and is capable of handling large sample volumes. Successful operation depends on the difference in volatility between the solvent and the analyte along with effective refocusing mechanisms at the head of the column. Reduced analysis times are achieved by in-line derivatization to permit the separation of polar analytes and elimination of volatile reagents and by products. The construction of a SFC restrictor from a 2 mm metal disc was described. The design is compact, robust and will readily interface with existing detectors. Preliminary results indicate that variable flow control can be achieved by temperature programming. The Knox equation was useful in illustrating the limitations of the solventless injector during isochloric conditions and proved that small particle (<10[mu]m) columns packed by the supercritical fluid displacement method are identical to those packed by the high pressure slurry packing method developed for HPLC. Supercritical CO[sub 2] and microbore columns are compatible with GC style detectors (FID). The use of formamide as a modifier improves the chromatographic properties for compounds containing nitrogen atoms and is compatible with the FID. SFE/SFC with formic acid modified CO[sub 2], polymer encapsulated stationary phases and the FID represent a considerable advance in the analysis of organotin compounds. The method is capable of extracting and separating a diverse group of industrially important organotin compounds. Triorganotins were determined in marine paint, potatoes, almonds and cation exchange resin. Diorganotin compounds were determined in PVC and cation exchange resin. The solventless injector allowed on line collection from the SFE cell and direct introduction to the analytical column.

  7. Application of phased array techniques to coarse grain components inspection.

    PubMed

    Mahaut, Steve; Godefroit, Jean-Louis; Roy, Olivier; Cattiaux, Gérard

    2004-04-01

    Ultrasonic inspection of cast stainless steel components from primary and auxiliary cooling circuits of French Nuclear Power Plant has to face with major difficulties due to the coarse grained structure of these materials. Attenuation losses and structural noise are encountered, which limits the performances of defect detection ability, mostly in terms of degraded signal-to-noise ratio and poor sensitivity. To overcome such problems, theoretical and experimental studies have been achieved at the French Atomic Energy Commission, with support from the French Institute for Radiological Protection and Nuclear Safety. Experimental studies have been performed over stainless steel specimen of known coarse structure (equiaxial grains and/or elongated grains), containing artificial reflectors (cylindrical holes and electro-eroded surface breaking notches). Those mock-ups have been inspected using contact probes of different array designs (linear or matrix splitting), and using pulse echo or dual-element techniques. Such arrays allow to control the ultrasonic beam so as to investigate different inspection angles and focusing depths. Experiments were carried out using oblique longitudinal waves, using delay laws computed by a specific model, taking account of acoustical and geometrical properties of the probes and the inspected component. In addition, specific reconstruction techniques have been investigated to enhance the signal-to-noise ratio as well as spatial resolution. These techniques are based on beam-forming summation and multi-angle inspections. Experimental results show that such techniques allow to reduce the speckle noise and to optimise the beam resolution. Those increased performances allow to detect and to size small planar defects located at the inner wall of a thick specimen, using corner and tip diffraction echoes.

  8. Application of Nondestructive Testing Techniques to Materials Testing.

    DTIC Science & Technology

    1987-12-01

    phase . The ideas behind it are basic to much of the present work we are carrying out on new programs on phase contrast microscopy , and...of phase contrast microscopy are already familiar. In reflection mi- croscopy, measurement of phase makes it possible to measure profiles, or height...frequency shifting, and a novel "heterodyne phase contrast " technique using a time-variable electro-optic phase plate, somewhat similar to a Zernike

  9. Magnetic resonance elastography (MRE) in cancer: Technique, analysis, and applications

    PubMed Central

    Pepin, Kay M.; Ehman, Richard L.; McGee, Kiaran P.

    2015-01-01

    Tissue mechanical properties are significantly altered with the development of cancer. Magnetic resonance elastography (MRE) is a noninvasive technique capable of quantifying tissue mechanical properties in vivo. This review describes the basic principles of MRE and introduces some of the many promising MRE methods that have been developed for the detection and characterization of cancer, evaluation of response to therapy, and investigation of the underlying mechanical mechanisms associated with malignancy. PMID:26592944

  10. Determination of perfluorinated surfactants in surface water samples by two independent analytical techniques: liquid chromatography/tandem mass spectrometry and 19F NMR.

    PubMed

    Moody, C A; Kwan, W C; Martin, J W; Muir, D C; Mabury, S A

    2001-05-15

    Perfluorinated surfactants are an important class of specialty chemicals that have received recent attention as a result of their persistence in the environment. Two analytical methods for the determination of perfluorinated surfactants in aqueous samples were developed in order to investigate a spill of 22000 L of fire retardant foam containing perfluorinated surfactants into Etobicoke Creek (Toronto, Ontario). With the first method, aliquots of surface water (0.2-200 mL) were preconcentrated using solid-phase extraction. Liquid chromatography/tandem mass spectrometry was employed for identification and quantification of each perfluorinated surfactant. Total perfluorinated surfactant concentrations in surface water samples ranged from 0.011 to 2270 microg/L, and perfluorooctanesulfonate was the predominant surfactant observed. Interestingly, perfluorooctanoate was detected in surface water sampled upstream of the spill. A second method employing 19F NMR was developed for the determination of total perfluorinated surfactant concentrations in aqueous samples (2-100 mL). By 19F NMR, the surface water concentrations ranged from nondetect (method detection limit, 10 microg/L for a 100-mL sample) to 17000 microg/L. These methods permit comprehensive evaluation of aqueous samples for the presence of perfluorinated surfactants and have applicability to other sample matrixes.

  11. A high-throughput 2D-analytical technique to obtain single protein parameters from complex cell lysates for in silico process development of ion exchange chromatography.

    PubMed

    Kröner, Frieder; Elsäßer, Dennis; Hubbuch, Jürgen

    2013-11-29

    The accelerating growth of the market for biopharmaceutical proteins, the market entry of biosimilars and the growing interest in new, more complex molecules constantly pose new challenges for bioseparation process development. In the presented work we demonstrate the application of a multidimensional, analytical separation approach to obtain the relevant physicochemical parameters of single proteins in a complex mixture for in silico chromatographic process development. A complete cell lysate containing a low titre target protein was first fractionated by multiple linear salt gradient anion exchange chromatography (AEC) with varying gradient length. The collected fractions were subsequently analysed by high-throughput capillary gel electrophoresis (HT-CGE) after being desalted and concentrated. From the obtained data of the 2D-separation the retention-volumes and the concentration of the single proteins were determined. The retention-volumes of the single proteins were used to calculate the related steric-mass action model parameters. In a final evaluation experiment the received parameters were successfully applied to predict the retention behaviour of the single proteins in salt gradient AEC.

  12. Differentiation between isomeric oxidative metabolites of a piperidine-containing drug by liquid chromatography-tandem mass spectrometry with stable-isotope tracer technique.

    PubMed

    Kato, Koji; Jingu, Shigeji; Ogawa, Naoyoshi; Higuchi, Shohei

    2002-02-01

    This report describes the application of a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to differentiation of hydroxylations and N-oxidations and of two different aliphatic hydroxylations in the investigation of the metabolism of pibutidine hydrochloride, a novel H2 antagonist, the structure of which includes a piperidine ring. Pibutidine metabolites in urine samples from adult male volunteers after oral administration of pibutidine hydrochloride were separated by reversed-phase LC and ionized using an electrospray ionization (ESI) interface. A hydroxylated form of pibutidine was distinguished from the N-oxide by comparison of their product ion spectra, although their mass-to-charge ratios of protonated molecules were identical. Further, two hydroxylated compounds were present in rat microsomal incubation mixtures with pibutidine. The distinction between their positions of hydroxylation (beta- and gamma-carbon hydroxylation) on the piperidine ring was studied using [piperidine-2H10] pibutidine as incubation substrate. The production of the beta-hydroxylated form was accompanied by the elimination of three 2H, resulting from a mechanism including the formation of iminium/enamine. The participation of the iminium ion intermediate in the beta-hydroxylation was confirmed by the observation that a cyanide adduct of pibutidine was formed instead of the beta-hydroxylated form when another incubation was performed in the presence of cyanide.

  13. Trace analysis of impurities in bulk gases by gas chromatography-pulsed discharge helium ionization detection with "heart-cutting" technique.

    PubMed

    Weijun, Yao

    2007-10-12

    A method has been developed for the detection of low-nL/L-level impurities in bulk gases such as H(2), O(2), Ar, N(2), He, methane, ethylene and propylene, respectively. The solution presented here is based upon gas chromatography-pulsed discharge helium ionization detection (GC-PDHID) coupled with three two-position valves, one two-way solenoid valve and four packed columns. During the operation, the moisture and heavy compounds are first back-flushed via a pre-column. Then the trace impurities (except CO(2) which is diverted to a separate analytical column for separation and detection) together with the matrix enter onto a main column, followed by the heart-cut of the impurities onto a longer analytical column for complete separation. Finally the detection is performed by PDHID. This method has been applied to different bulk gases and the applicability of detecting impurities in H(2), Ar, and N(2) are herewith demonstrated. As an example, the resulting detection limit of 100 nL/L and a dynamic range of 100-1000 nL/L have been obtained using an Ar sample containing methane.

  14. Application of physical and chemical characterization techniques to metallic powders

    SciTech Connect

    Slotwinski, J. A.; Watson, S. S.; Stutzman, P. E.; Ferraris, C. F.; Peltz, M. A.; Garboczi, E. J.

    2014-02-18

    Systematic studies have been carried out on two different powder materials used for additive manufacturing: stainless steel and cobalt-chrome. The characterization of these powders is important in NIST efforts to develop appropriate measurements and standards for additive materials and to document the property of powders used in a NIST-led additive manufacturing material round robin. An extensive array of characterization techniques was applied to these two powders, in both virgin and recycled states. The physical techniques included laser diffraction particle size analysis, X-ray computed tomography for size and shape analysis, and optical and scanning electron microscopy. Techniques sensitive to chemistry, including X-ray diffraction and energy dispersive analytical X-ray analysis using the X-rays generated during scanning electron microscopy, were also employed. Results of these analyses will be used to shed light on the question: how does virgin powder change after being exposed to and recycled from one or more additive manufacturing build cycles? In addition, these findings can give insight into the actual additive manufacturing process.

  15. Application of multivariable search techniques to structural design optimization

    NASA Technical Reports Server (NTRS)

    Jones, R. T.; Hague, D. S.

    1972-01-01

    Multivariable optimization techniques are applied to a particular class of minimum weight structural design problems: the design of an axially loaded, pressurized, stiffened cylinder. Minimum weight designs are obtained by a variety of search algorithms: first- and second-order, elemental perturbation, and randomized techniques. An exterior penalty function approach to constrained minimization is employed. Some comparisons are made with solutions obtained by an interior penalty function procedure. In general, it would appear that an interior penalty function approach may not be as well suited to the class of design problems considered as the exterior penalty function approach. It is also shown that a combination of search algorithms will tend to arrive at an extremal design in a more reliable manner than a single algorithm. The effect of incorporating realistic geometrical constraints on stiffener cross-sections is investigated. A limited comparison is made between minimum weight cylinders designed on the basis of a linear stability analysis and cylinders designed on the basis of empirical buckling data. Finally, a technique for locating more than one extremal is demonstrated.

  16. Application of multivariate statistical techniques in microbial ecology.

    PubMed

    Paliy, O; Shankar, V

    2016-03-01

    Recent advances in high-throughput methods of molecular analyses have led to an explosion of studies generating large-scale ecological data sets. In particular, noticeable effect has been attained in the field of microbial ecology, where new experimental approaches provided in-depth assessments of the composition, functions and dynamic changes of complex microbial communities. Because even a single high-throughput experiment produces large amount of data, powerful statistical techniques of multivariate analysis are well suited to analyse and interpret these data sets. Many different multivariate techniques are available, and often it is not clear which method should be applied to a particular data set. In this review, we describe and compare the most widely used multivariate statistical techniques including exploratory, interpretive and discriminatory procedures. We consider several important limitations and assumptions of these methods, and we present examples of how these approaches have been utilized in recent studies to provide insight into the ecology of the microbial world. Finally, we offer suggestions for the selection of appropriate methods based on the research question and data set structure.

  17. Application of multivariate statistical techniques in microbial ecology

    PubMed Central

    Paliy, O.; Shankar, V.

    2016-01-01

    Recent advances in high-throughput methods of molecular analyses have led to an explosion of studies generating large scale ecological datasets. Especially noticeable effect has been attained in the field of microbial ecology, where new experimental approaches provided in-depth assessments of the composition, functions, and dynamic changes of complex microbial communities. Because even a single high-throughput experiment produces large amounts of data, powerful statistical techniques of multivariate analysis are well suited to analyze and interpret these datasets. Many different multivariate techniques are available, and often it is not clear which method should be applied to a particular dataset. In this review we describe and compare the most widely used multivariate statistical techniques including exploratory, interpretive, and discriminatory procedures. We consider several important limitations and assumptions of these methods, and we present examples of how these approaches have been utilized in recent studies to provide insight into the ecology of the microbial world. Finally, we offer suggestions for the selection of appropriate methods based on the research question and dataset structure. PMID:26786791

  18. A survey of reflectometry techniques with applications to TFTR

    SciTech Connect

    Collazo, I.; Stacey, W.M.; Wilgen, J.; Hanson, G.; Bigelow, T.; Thomas, C.E.; Bretz, N.

    1993-12-01

    This report presents a review of reflectometry with particular attention to eXtraordinary mode (X-mode) reflectometry using the novel technique of dual frequency differential phase. The advantage of using an X-mode wave is that it can probe the edge of the plasma with much higher resolution and using a much smaller frequency range than with the Ordinary mode (O-Mode). The general problem with previous full phase reflectometry techniques is that of keeping track of the phase (on the order of 1000 fringes) as the frequency is swept over the band. The dual frequency phase difference technique has the advantage that since it is keeping track of the phase difference of two frequencies with a constant frequency separation, the fringe counting is on the order of only 3 to 5 fringes. This fringe count, combined with the high resolution of the X-mode wave and the small plasma access requirements of reflectometry, make X-mode reflectometry a very attractive diagnostic for today`s experiments and future fusion devices.

  19. [Research Progress of Application of Microfluidics Techniques in Cryopreservation].

    PubMed

    Zhou, Nanfeng; Yang, Yun; Zhou, Xinli

    2015-06-01

    Microfluidics technology may be an effective method to solve some problems in cryopreservation. This review presents the research progress of microfluidics technology in the field of cell membrane transport properties, cryoprotectant addition and washout and the vitrification for cryopreservation of biological materials. Existing problems of microfluidics technology in the application of cryopreservation are summarized and future research directions are indicated as well.

  20. Psychotherapeutic Techniques Applicable to Remedial Treatment of Reading Disabilities.

    ERIC Educational Resources Information Center

    Rosen, Carl L.

    The disabled reader's measurably low success in processing print creates tension, stress, and increasingly negative perceptions of the reading act and of the reader's own beliefs about his or her personal competencies. The task of the reading specialist might be facilitated by conscious and increasingly skilled application of psychotherapeutic…