Characterization of the major odor-active compounds in Thai durian ( Durio zibethinus L. 'Monthong') by aroma extract dilution analysis and headspace gas chromatography-olfactometry.

Science.gov (United States)

Li, Jia-Xiao; Schieberle, Peter; Steinhaus, Martin

2012-11-14

An aroma extract dilution analysis applied on the volatile fraction isolated from Thai durian by solvent extraction and solvent-assisted flavor evaporation resulted in 44 odor-active compounds in the flavor dilution (FD) factor range of 1-16384, 41 of which could be identified and 24 that had not been reported in durian before. High FD factors were found for ethyl (2S)-2-methylbutanoate (fruity; FD 16384), ethyl cinnamate (honey; FD 4096), and 1-(ethylsulfanyl)ethanethiol (roasted onion; FD 1024), followed by 1-(ethyldisulfanyl)-1-(ethylsulfanyl)ethane (sulfury, onion), 2(5)-ethyl-4-hydroxy-5(2)-methylfuran-3(2H)-one (caramel), 3-hydroxy-4,5-dimethylfuran-2(5H)-one (soup seasoning), ethyl 2-methylpropanoate (fruity), ethyl butanoate (fruity), 3-methylbut-2-ene-1-thiol (skunky), ethane-1,1-dithiol (sulfury, durian), 1-(methylsulfanyl)ethanethiol (roasted onion), 1-(ethylsulfanyl)propane-1-thiol (roasted onion), and 4-hydroxy-2,5-dimethylfuran-3(2H)-one (caramel). Among the highly volatile compounds screened by static headspace gas chromatography-olfactometry, hydrogen sulfide (rotten egg), acetaldehyde (fresh, fruity), methanethiol (rotten, cabbage), ethanethiol (rotten, onion), and propane-1-thiol (rotten, durian) were found as additional potent odor-active compounds. Fourteen of the 41 characterized durian odorants showed an alkane-1,1-dithiol, 1-(alkylsulfanyl)alkane-1-thiol, or 1,1-bis(alkylsulfanyl)alkane structure derived from acetaldehyde, propanal, hydrogen sulfide, and alkane-1-thiols. Among these, 1-(propylsulfanyl)ethanethiol, 1-{[1-(methylsulfanyl)ethyl]sulfanyl}ethanethiol, and 1-{[1-(ethylsulfanyl)ethyl]sulfanyl}ethanethiol were reported for the first time in a natural product.

Direct quantification of creatinine in human urine by using isotope dilution extractive electrospray ionization tandem mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Li Xue [Institute of Environmental Pollution and Health, School of Environmental and Chemical Engineering, Shanghai University, Shanghai 200444 (China); Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation, Applied Chemistry Department, East China Institute of Technology, Nanchang 330013 (China); Fang Xiaowei [Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation, Applied Chemistry Department, East China Institute of Technology, Nanchang 330013 (China); Yu Zhiqiang; Sheng Guoying [Guangdong Key Laboratory of Environmental Protection and Resource Utilization, State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Wu Minghong [Shanghai Applied Radiation Institute, School of Environmental and Chemical Engineering, Shanghai University, Shanghai 200444 (China); Fu Jiamo [Institute of Environmental Pollution and Health, School of Environmental and Chemical Engineering, Shanghai University, Shanghai 200444 (China); Guangdong Key Laboratory of Environmental Protection and Resource Utilization, State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Chen Huanwen, E-mail: chw8868@gmail.com [Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation, Applied Chemistry Department, East China Institute of Technology, Nanchang 330013 (China)

2012-10-20

Highlights: Black-Right-Pointing-Pointer High throughput analysis of urinary creatinine is achieved by using ID-EESI-MS/MS. Black-Right-Pointing-Pointer Urine sample is directly analyzed and no sample pre-treatment is required. Black-Right-Pointing-Pointer Accurate quantification is accomplished with isotope dilution technique. - Abstract: Urinary creatinine (CRE) is an important biomarker of renal function. Fast and accurate quantification of CRE in human urine is required by clinical research. By using isotope dilution extractive electrospray ionization tandem mass spectrometry (EESI-MS/MS) a high throughput method for direct and accurate quantification of urinary CRE was developed in this study. Under optimized conditions, the method detection limit was lower than 50 {mu}g L{sup -1}. Over the concentration range investigated (0.05-10 mg L{sup -1}), the calibration curve was obtained with satisfactory linearity (R{sup 2} = 0.9861), and the relative standard deviation (RSD) values for CRE and isotope-labeled CRE (CRE-d3) were 7.1-11.8% (n = 6) and 4.1-11.3% (n = 6), respectively. The isotope dilution EESI-MS/MS method was validated by analyzing six human urine samples, and the results were comparable with the conventional spectrophotometric method (based on the Jaffe reaction). Recoveries for individual urine samples were 85-111% and less than 0.3 min was taken for each measurement, indicating that the present isotope dilution EESI-MS/MS method is a promising strategy for the fast and accurate quantification of urinary CRE in clinical laboratories.

Characterization of the aroma-active compounds in pink guava (Psidium guajava, L.) by application of the aroma extract dilution analysis.

Science.gov (United States)

Steinhaus, Martin; Sinuco, Diana; Polster, Johannes; Osorio, Coralia; Schieberle, Peter

2008-06-11

The volatiles present in fresh, pink-fleshed Colombian guavas ( Psidium guajava, L.), variety regional rojo, were carefully isolated by solvent extraction followed by solvent-assisted flavor evaporation, and the aroma-active areas in the gas chromatogram were screened by application of the aroma extract dilution analysis. The results of the identification experiments in combination with the FD factors revealed 4-methoxy-2,5-dimethyl-3(2 H)-furanone, 4-hydroxy-2,5-dimethyl-3(2 H)-furanone, 3-sulfanylhexyl acetate, and 3-sulfanyl-1-hexanol followed by 3-hydroxy-4,5-dimethyl-2(5 H)-furanone, ( Z)-3-hexenal, trans-4,5-epoxy-( E)-2-decenal, cinnamyl alcohol, ethyl butanoate, hexanal, methional, and cinnamyl acetate as important aroma contributors. Enantioselective gas chromatography revealed an enantiomeric distribution close to the racemate in 3-sulfanylhexyl acetate as well as in 3-sulfanyl-1-hexanol. In addition, two fruity smelling diastereomeric methyl 2-hydroxy-3-methylpentanoates were identified as the ( R,S)- and the ( S,S)-isomers, whereas the ( S,R)- and ( R,R)-isomers were absent. Seven odorants were identified for the first time in guavas, among them 3-sulfanylhexyl acetate, 3-sulfanyl-1-hexanol, 3-hydroxy-4,5-dimethyl-2(5 H)-furanone, trans-4,5-epoxy-( E)-2-decenal, and methional were the most odor-active.

Analysis of trace metals (Cu, Cd, Pb, and Fe) in seawater using single batch nitrilotriacetate resin extraction and isotope dilution inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Lee, Jong-Mi [Department of Earth, Atmospheric, and Planetary Sciences, Massachusetts Institute of Technology, Cambridge, MA 02139 (United States); Boyle, Edward A., E-mail: eaboyle@mit.edu [Department of Earth, Atmospheric, and Planetary Sciences, Massachusetts Institute of Technology, Cambridge, MA 02139 (United States); Echegoyen-Sanz, Yolanda; Fitzsimmons, Jessica N. [Department of Earth, Atmospheric, and Planetary Sciences, Massachusetts Institute of Technology, Cambridge, MA 02139 (United States); Zhang Ruifeng [State Key Laboratory of Estuarine and Coastal Research, East China Normal University, Shanghai 200062 (China); Kayser, Richard A. [Department of Earth, Atmospheric, and Planetary Sciences, Massachusetts Institute of Technology, Cambridge, MA 02139 (United States)

2011-02-07

A simple and accurate low-blank method has been developed for the analysis of total dissolved copper, cadmium, lead, and iron in a small volume (1.3-1.5 mL per element) of seawater. Pre-concentration and salt-separation of a stable isotope spiked sample are achieved by single batch extraction onto nitrilotriacetate (NTA)-type Superflow chelating resin beads (100-2400 beads depending on the element). Metals are released into 0.1-0.5 M HNO{sub 3}, and trace metal isotope ratios are determined by ICPMS. The benefit of this method compared to our previous Mg(OH){sub 2} coprecipitation method is that the final matrix is very dilute so cone-clogging and matrix sensitivity suppression are minimal, while still retaining the high accuracy of the isotope dilution technique. Recovery efficiencies are sensitive to sample pH, number of resin beads added, and the length of time allowed for sample-resin binding and elution; these factors are optimized for each element to yield the highest recovery. The method has a low procedural blank and high sensitivity sufficient for the analysis of pM-nM open-ocean trace metal concentrations. Application of this method to samples from the Bermuda Atlantic Time-Series Study station provides oceanographically consistent Cu, Cd, Pb, and Fe profiles that are in good agreement with other reliable data for this site. In addition, the method can potentially be modified for the simultaneous analysis of multiple elements, which will be beneficial for the analysis of large number of samples.

Analysis of trace metals (Cu, Cd, Pb, and Fe) in seawater using single batch nitrilotriacetate resin extraction and isotope dilution inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Lee, Jong-Mi; Boyle, Edward A.; Echegoyen-Sanz, Yolanda; Fitzsimmons, Jessica N.; Zhang Ruifeng; Kayser, Richard A.

2011-01-01

A simple and accurate low-blank method has been developed for the analysis of total dissolved copper, cadmium, lead, and iron in a small volume (1.3-1.5 mL per element) of seawater. Pre-concentration and salt-separation of a stable isotope spiked sample are achieved by single batch extraction onto nitrilotriacetate (NTA)-type Superflow chelating resin beads (100-2400 beads depending on the element). Metals are released into 0.1-0.5 M HNO 3 , and trace metal isotope ratios are determined by ICPMS. The benefit of this method compared to our previous Mg(OH) 2 coprecipitation method is that the final matrix is very dilute so cone-clogging and matrix sensitivity suppression are minimal, while still retaining the high accuracy of the isotope dilution technique. Recovery efficiencies are sensitive to sample pH, number of resin beads added, and the length of time allowed for sample-resin binding and elution; these factors are optimized for each element to yield the highest recovery. The method has a low procedural blank and high sensitivity sufficient for the analysis of pM-nM open-ocean trace metal concentrations. Application of this method to samples from the Bermuda Atlantic Time-Series Study station provides oceanographically consistent Cu, Cd, Pb, and Fe profiles that are in good agreement with other reliable data for this site. In addition, the method can potentially be modified for the simultaneous analysis of multiple elements, which will be beneficial for the analysis of large number of samples.

Characterization of Key Aroma Compounds in Raw and Thermally Processed Prawns and Thermally Processed Lobsters by Application of Aroma Extract Dilution Analysis.

Science.gov (United States)

Mall, Veronika; Schieberle, Peter

2016-08-24

Application of aroma extract dilution analysis (AEDA) to an aroma distillate of blanched prawn meat (Litopenaeus vannamei) (BPM) revealed 40 odorants in the flavor dilution (FD) factor range from 4 to 1024. The highest FD factors were assigned to 2-acetyl-1-pyrroline, 3-(methylthio)propanal, (Z)-1,5-octadien-3-one, trans-4,5-epoxy-(E)-2-decenal, (E)-3-heptenoic acid, and 2-aminoacetophenone. To understand the influence of different processing conditions on odorant formation, fried prawn meat was investigated by means of AEDA in the same way, revealing 31 odorants with FD factors between 4 and 2048. Also, the highest FD factors were determined for 2-acetyl-1-pyrroline, 3-(methylthio)propanal, and (Z)-1,5-octadien-3-one, followed by 4-hydroxy-2,5-dimethyl-3(2H)-furanone, (E)-3-heptenoic acid, and 2-aminoacetophenone. As a source of the typical marine, sea breeze-like odor attribute of the seafood, 2,4,6-tribromoanisole was identified in raw prawn meat as one of the contributors. Additionally, the aroma of blanched prawn meat was compared to that of blanched Norway and American lobster meat, respectively (Nephrops norvegicus and Homarus americanus). Identification experiments revealed the same set of odorants, however, with differing FD factors. In particular, 3-hydroxy-4,5-dimethyl-2(5H)-furanone was found as the key aroma compound in blanched Norway lobster, whereas American lobster contained 3-methylindole with a high FD factor.

Towards integrated biorefinery from dried distillers grains: Selective extraction of pentoses using dilute acid hydrolysis

International Nuclear Information System (INIS)

Fonseca, Dania A.; Lupitskyy, Robert; Timmons, David; Gupta, Mayank; Satyavolu, Jagannadh

2014-01-01

The abundant availability and high level of hemicellulose content make dried distillers grains (DDG) an attractive feedstock for production of pentoses (C5) and conversion of C5 to bioproducts. One target of this work was to produce a C5 extract (hydrolyzate) with high yield and purity with a low concentration of C5 degradation products. A high selectivity towards pentoses was achieved using dilute acid hydrolysis of DDG in a percolation reactor with liquid recirculation. Pretreatment of starting material using screening and ultrasonication resulted in fractional increase of the pentose yield by 42%. A 94% yield of pentoses on the DDG (280.9 g kg −1 ) was obtained. Selective extraction of individual pentoses has been achieved by using a 2-stage hydrolysis process, resulting in arabinose-rich (arabinose 81.5%) and xylose-rich (xylose 85.2%) streams. A broader impact of this work is towards an Integrated Bio-Refinery based on DDG – for production of biofuels, biochemical intermediates, and other bioproducts. - Highlights: • A process for selective extraction of pentoses from DDG was presented as a part of integrated biorefinery approach. • The selectivity for pentoses was high using dilute acid hydrolysis in a percolation reactor with liquid recirculation. • Pretreatment of DDG using screening and ultrasonication resulted in fractional increase of the pentose yield by 42 %. • A 94% yield in pentoses (280.9 g kg −1 of DDG) was obtained. • A 2-stage hydrolysis process, developed to extract individual pentoses, resulted in arabinose and xylose rich streams

Dynamic structural analysis of the TPSG4 & TPSG6 beam diluters

CERN Document Server

Massidda, L; Kadi, Y; Balhan, B

2005-01-01

In this report we present the technical specification for the numerical model and the study of the dynamic structural behaviour of the beam diluter elements (TPSG4 & 6) protecting the extraction septum magnets (MSE & MST) in the event of an asynchronous firing of the extraction kickers (MKE). The deposited energy densities, estimated by the high-energy particle transport code FLUKA, were converted to internal heat generation rates according to the time dependence of the extracted beam. The transient response to this thermal load was obtained by solving the power deposition and structural deformation problem by the spectral-element code ELSE.

Chiral-glass transition in a diluted dipolar-interaction Heisenberg system

International Nuclear Information System (INIS)

Zhang Kaicheng; Liu Guibin; Zhu Yan

2011-01-01

Recently, numerical simulations reveal that a spin-glass transition can occur in the three-dimensional diluted dipolar system. By defining the chirality of triple spins in a diluted dipolar Heisenberg spin glass, we study the chiral ordering in the system using parallel tempering algorithm and heat bath method. The finite-size scaling analysis reveals that the system undergoes a chiral-glass transition at finite temperature. - Highlights: → We define the chirality in a diluted dipolar Heisenberg system. → The system undergoes a chiral-glass transition at finite temperature. → We extract the critical exponents of the chiral-glass transition.

Hot vacuum extraction-isotopic dilution mass spectrometry for determination of hydrogen isotopes in zircaloys

International Nuclear Information System (INIS)

Shi, Y.; Leeson, P.K.; Wilkin, D.; Britton, A.; Macleod, R.

2016-01-01

A hot vacuum extraction-isotope dilution mass spectrometry (HVE-IDMS) was studied for determination of hydrogen isotopes in zirconium metal and alloys as nuclear reactor materials. A theoretical assessment of the completeness of the extraction of hydrogen isotopes under the chosen condition was carried out based on the hydrogen and deuterium solubility data for zirconium. The optimal isotopic spiking condition for conventional IDMS was further explored for the special case IDMS where the isotope abundance of the samples is varied and non-natural. Applying the optimal conditions, the accurate IDMS determination was realized. The agreement between the measured values and the certified or prepared values of standard reference materials and homemade standard materials validate the method developed. (author)

Double spike isotope dilution GC-ICP-MS for evaluation of mercury species transformation in real fish samples using ultrasound-assisted extraction.

Science.gov (United States)

Esteban-Fernández, Diego; Mirat, Manuela; de la Hinojosa, M Ignacia Martín; Alonso, J Ignacio García

2012-08-29

Sample preparation continues being a key factor to obtain fast and reliable quantification of Hg species. Assisted procedures enhance the efficiency and reduce the extraction time; however, collateral species transformations have been observed. Moreover, differential interconversions have been observed even between similar matrixes, which introduce an important uncertainty for real sample analysis. Trying to minimize Hg species transformations, we have tested a soft ultrasound-assisted extraction procedure. Species quantification and transformations have been evaluated using double spike isotope dilution analysis (IDA) together with gas chromatography inductively coupled plasma mass spectrometry (GC-ICP-MS) for a CRM material (Tort-2) and shark and swordfish muscle samples. Optimum extraction solution and sonication time led to quantitative extraction and accurate determination of MeHg and IHg in a short time, although different behaviors regarding species preservation were observed depending on the sample. Negligible species transformations were observed in the analysis of the CRM, while a small but significant demethylation factor was observed in the case of real samples. In comparison with other extraction procedures, species transformations became smaller, and fewer differences between fish species were found. Similar results were obtained for fresh and lyophilized samples of both fish samples, which permit one to analyze the fresh sample directly and save time in the sample preparation step. The high grade of species preservation and the affordability of the extraction procedure allow one to obtain accurate determinations even for routine laboratories using quantification techniques, which do not estimate species transformations.

Analysis of ochratoxin A in grapes, musts and wines by LC–MS/MS: First comparison of stable isotope dilution assay and diastereomeric dilution assay methods

Energy Technology Data Exchange (ETDEWEB)

Roland, Aurélie, E-mail: aurelie@nyseos.fr [Nyseos, 2 place Pierre Viala, Montpellier Cedex 1 34060 (France); Bros, Pauline, E-mail: pauline.bros@gmail.com [Institut Français de la Vigne et du Vin, UMT Qualinnov, 2 place Pierre Viala, Montpellier Cedex 1 34060 (France); Bouisseau, Anaïs, E-mail: anais.bouisseau@gmail.com [Nyseos, 2 place Pierre Viala, Montpellier Cedex 1 34060 (France); Institut des Biomolécules Max Mousseron, UMR-CNRS-5247, Universités Montpellier I and II, Place Eugène Bataillon, 34095 Montpellier (France); Cavelier, Florine, E-mail: florine@univ-montp2.fr [Institut des Biomolécules Max Mousseron, UMR-CNRS-5247, Universités Montpellier I and II, Place Eugène Bataillon, 34095 Montpellier (France); Schneider, Rémi, E-mail: remi.schneider@vignevin.com [Institut Français de la Vigne et du Vin, UMT Qualinnov, 2 place Pierre Viala, Montpellier Cedex 1 34060 (France)

2014-03-01

Highlights: • OTA extraction on immunoaffinity columns is not adapted for DIDA quantification. • The use of a labeled internal standard is compulsory to obtain reliable results. • SIDA and DIDA quantification approaches have been compared for the first time. Abstract: Ochratoxin A (OTA) exhibits potent nephrotoxic, carcinogenic and teratogenic effects and its maximum level in wines has been set to 2 μg L⁻¹ by regulation. Consequently, the analytical procedures for OTA determination in wines have to be both very sensitive and reliable. In this paper, we compared two quantification methods: the stable isotope dilution assay (SIDA) and the diastereomeric dilution assay (DIDA). For this purpose, non-natural analogues of OTA were synthesized: the labeled OTA (OTA-d₄) as a diastereomeric mixture for the SIDA and one non-natural OTA’s diastereomer (OTA-dia) for the DIDA. To quantify OTA in red grapes, musts or wines, the sample preparation was optimized using immunoaffinity column extraction and the analysis was performed by LC–MS/MS in Multiple Reaction Monitoring mode. A validation procedure in agreement with the International Organization of Vine and Wine recommendations was conducted. It appeared that SIDA quantification exhibited excellent sensitivity (LOD < 1 ng L⁻¹), accuracy (recovery = 98%), repeatability (RSD < 3%) and intermediate reproducibility (RSD < 4%) compared to quantification by DIDA. Indeed, DIDA method did not provide satisfactory results demonstrating that immunoaffinity extraction is exclusively selective for the natural OTA and not for its diastereomer, which therefore cannot be considered as a good internal standard for this particular method.

Analysis of ochratoxin A in grapes, musts and wines by LC–MS/MS: First comparison of stable isotope dilution assay and diastereomeric dilution assay methods

International Nuclear Information System (INIS)

Roland, Aurélie; Bros, Pauline; Bouisseau, Anaïs; Cavelier, Florine; Schneider, Rémi

2014-01-01

Highlights: • OTA extraction on immunoaffinity columns is not adapted for DIDA quantification. • The use of a labeled internal standard is compulsory to obtain reliable results. • SIDA and DIDA quantification approaches have been compared for the first time. - Abstract: Ochratoxin A (OTA) exhibits potent nephrotoxic, carcinogenic and teratogenic effects and its maximum level in wines has been set to 2 μg L −1 by regulation. Consequently, the analytical procedures for OTA determination in wines have to be both very sensitive and reliable. In this paper, we compared two quantification methods: the stable isotope dilution assay (SIDA) and the diastereomeric dilution assay (DIDA). For this purpose, non-natural analogues of OTA were synthesized: the labeled OTA (OTA-d 4 ) as a diastereomeric mixture for the SIDA and one non-natural OTA’s diastereomer (OTA-dia) for the DIDA. To quantify OTA in red grapes, musts or wines, the sample preparation was optimized using immunoaffinity column extraction and the analysis was performed by LC–MS/MS in Multiple Reaction Monitoring mode. A validation procedure in agreement with the International Organization of Vine and Wine recommendations was conducted. It appeared that SIDA quantification exhibited excellent sensitivity (LOD −1 ), accuracy (recovery = 98%), repeatability (RSD < 3%) and intermediate reproducibility (RSD < 4%) compared to quantification by DIDA. Indeed, DIDA method did not provide satisfactory results demonstrating that immunoaffinity extraction is exclusively selective for the natural OTA and not for its diastereomer, which therefore cannot be considered as a good internal standard for this particular method

Chemical characterization of the aroma of Grenache rosé wines: aroma extract dilution analysis, quantitative determination, and sensory reconstitution studies.

Science.gov (United States)

Ferreira, Vicente; Ortín, Natalia; Escudero, Ana; López, Ricardo; Cacho, Juan

2002-07-03

The aroma of a Grenache rosé wine from Calatayud (Zaragoza, Spain) has been elucidated following a strategy consisting of an aroma extract dilution analysis (AEDA), followed by the quantitative analysis of the main odorants and the determination of odor activities values (OAVs) and, finally, by a series of reconstitution and omission tests with synthetic aroma models. Thirty-eight aroma compounds were found in the AEDA study, 35 of which were identified. Twenty-one compounds were at concentrations higher than their corresponding odor thresholds. An aroma model prepared by mixing the 24 compounds with OAV > 0.5 in a synthetic wine showed a high qualitative similarity with the aroma of the rosé wine. The addition of compounds with OAV 10 was very different from that of the wine. Omission tests revealed that the most important odorant of this Grenache rosé wine was 3-mercapto-1-hexanol, with a deep impact on the wine fruity and citric notes. The synergic action of Furaneol and homofuraneol also had an important impact on wine aroma, particularly in its fruity and caramel notes. The omission of beta-damascenone, which had the second highest OAV, caused only a slight decrease on the intensity of the aroma model. Still weaker was the sensory effect caused by the omission of 10 other compounds, such as fatty acids and their ethyl esters, isoamyl acetate, and higher alcohols.

Estimating the extractability of potentially toxic metals in urban soils: A comparison of several extracting solutions

International Nuclear Information System (INIS)

Madrid, F.; Reinoso, R.; Florido, M.C.; Diaz Barrientos, E.; Ajmone-Marsan, F.; Davidson, C.M.; Madrid, L.

2007-01-01

Metals released by the extraction with aqua regia, EDTA, dilute HCl and sequential extraction (SE) by the BCR protocol were studied in urban soils of Sevilla, Torino, and Glasgow. By multivariate analysis, the amounts of Cu, Pb and Zn liberated by any method were statistically associated with one another, whereas other metals were not. The mean amounts of all metals extracted by HCl and by SE were well correlated, but SE was clearly underestimated by HCl. Individual data for Cu, Pb and Zn by both methods were correlated only if each city was considered separately. Other metals gave poorer relationships. Similar conclusions were reached comparing EDTA and HCl, with much lower values for EDTA. Dilute HCl extraction cannot thus be recommended for general use as alternative to BCR SE in urban soils. - Dilute HCl extraction is tested as an alternative to the BCR sequential extraction in urban soils

Isotope Dilution - Thermal Ionisation Mass Spectrometric Analysis for Tin in a Fly Ash Material

International Nuclear Information System (INIS)

Hernandez, C.; Fernandez, M.; Quejido, A. L.

2006-01-01

Isotope dilution-thermal ionisation mass spectrometry (ID-TIMS) analysis has been applied to the determination of tin in a fly ash sample supplied by the EC Joint Research Centre (Ispra, Italy). The proposed procedure includes the silica gel/phosphoric acid technique for tin thermal ionisation activation and a strict heating protocol for isotope ratio measurements. Instrumental mass discrimination factor has been previously determined measuring a natural tin standard solution. Spike solutions has been prepared from 112Sn-enriched metal and quantified by reverse isotope dilution analysis. Two sample aliquots were spiked and tin was extracted with 4,5 M HCI during 25 min ultrasound esposure time. Due to the complex matrix of this fly ash material, a two-steps purification stage using ion-exchange chromatography was required prior TIMS analysis. Obtained results for the two sample-spike blends (10,10 + - 0,55 y 10,50 + - 0,64 imolg-1) are comprarable, both value and uncertainty. Also a good reproducibility is observed between measurements. The proposed ID-TIMS procedure, as a primary method and due to the lack of fly ash reference material certified for tin content, can be used to validate more routine methodologies applied to tin determination in this kind of materials. (Author) 75 refs

Dilution and Mixing in transient velocity fields: a first-order analysis

Science.gov (United States)

Di Dato, Mariaines; de Barros, Felipe, P. J.; Fiori, Aldo; Bellin, Alberto

2017-04-01

An appealing remediation technique is in situ oxidation, which effectiveness is hampered by difficulties in obtaining good mixing of the injected oxidant with the contaminant, particularly when the contaminant plume is contained and therefore its deformation is physically constrained. Under such conditions (i.e. containment), mixing may be augmented by inducing temporal fluctuations of the velocity field. The temporal variability of the flow field may increase the deformation of the plume such that diffusive mass flux becomes more effective. A transient periodic velocity field can be obtained by an engineered sequence of injections and extractions from wells, which may serve also as a hydraulic barrier to confine the plume. Assessing the effectiveness of periodic flows to maximize solute mixing is a difficult task given the need to use a 3D setup and the large number of possible flow configurations that should be analyzed in order to identify the optimal one. This is the typical situation in which analytical solutions, though approximated, may assist modelers in screening possible alternative flow configurations such that solute dilution is maximized. To quantify dilution (i.e. a precondition that enables reactive mixing) we utilize the concept of the dilution index [1]. In this presentation, the periodic flow takes place in an aquifer with spatially variable hydraulic conductivity field which is modeled as a Stationary Spatial Random Function. We developed a novel first-order analytical solution of the dilution index under the hypothesis that the flow can be approximated as a sequence of steady state configurations with the mean velocity changing with time in intensity and direction. This is equivalent to assume that the characteristic time of the transient behavior is small compared to the period characterizing the change in time of the mean velocity. A few closed paths have been analyzed quantifying their effectiveness in enhancing dilution and thereby mixing

Analysis of cesium extracting solvent using GCMS and HPLC

International Nuclear Information System (INIS)

White, T.L.; Herman, C.C.; Crump, S.L.; Marinik, A.R.; Lambert, D.P.; Eibling, R.E.

2007-01-01

A high-level waste (HLW) remediation process scheduled to begin in 2007 at the Savannah River Site is the Modular Caustic Side Solvent Extraction (CSSX) Unit (MCU). The MCU will use a hydrocarbon solvent (diluent) containing a cesium extractant, a calix[4]arene compound, to extract radioactive cesium from caustic HLW. The resulting decontaminated HLW waste or raffinate will be processed into grout at the Saltstone Production Facility (SPF). The cesium containing CSSX stream will undergo washing with dilute nitric acid followed by stripping of the cesium nitrate into a very dilute nitric acid or the strip effluent stream and the CSSX solvent will be recycled. The Defense Waste Processing Facility (DWPF) will receive the strip effluent stream and immobilize the cesium into borosilicate glass. Excess CSSX solvent carryover from the MCU creates a potential flammability problem during DWPF processing. Bench-scale DWPF process testing was performed with simulated waste to determine the fate of the CSSX solvent components. A simple high performance liquid chromatography (HPLC) method was developed to identify the modifier (which is used to increase Cs extraction and extractant solubility) and extractant within the DWPF process. The diluent and trioctylamine (which is used to suppress impurity effect and ion-pair disassociation) were determined using gas chromatography mass spectroscopy (GCMS). To close the organic balance, two types of sample preparation methods were needed. One involved extracting aqueous samples with methylene chloride or hexane, and the second was capturing the off gas of the DWPF process using carbon tubes and rinsing the tubes with carbon disulfide for analysis. This paper addresses the development of the analytical methods and the bench-scale simulated waste study results. (author)

Calculations for BDAS Setpoint with Non-conservative Boron Dilution Analysis

International Nuclear Information System (INIS)

Lee, Hwan Soo; Shin, Ho Cheol; Kim, Yong Bae

2014-01-01

BDAS (Boron Dilution Alarm System) utilizes the ex-core detector instrumentation signals to detect a possible inadvertent boron dilution event during operation mode 3, 4, 5, 6. For boron dilution analysis, discrepancies in the active coolant volume and the assumed linearity of the ex-core instrumentation response were identified for CE type PWR and they were reported by NASL-04-02 These discrepancies have potential to impact to determine BDAS setpoint in a non-conservative manner Therefore, in this study, the calculation of BDAS setpoint with those discrepancies condition about OPR1000 was performed and analyzed for checking the safety of BDAS. The new BDAS setpoint is calculated with conservative condition which recommended from Westinghouse Electric Company. The setpoint of BDAS using non-linear ICRR curve decrease to about 5% compared to the setpoint of that using linear ICRR curve. And this effect of the non-linearity is to slightly delay the boron dilution alarm during the inadvertence boron dilution at mode 3, 4, and 5

Dilute alkali and hydrogen peroxide treatment of microwave liquefied rape straw residue for the extraction of cellulose nanocrystals

Science.gov (United States)

Xingyan Huang; Cornelis F. De Hoop; Feng Li; Jiulong Xie; Chung-Yun Hse; Jinqiu Qi; Yongze Jiang; Yuzhu Chen

2017-01-01

Microwave-assisted liquefaction of rape straw in methanol was conducted to collect the liquefied residues for the extraction of cellulose nanocrystals (CNCs).The liquefied residue with content of 23.44% from 180∘C/7.5 min was used to fibrillate CNCs with dilute alkali (2% NaOH) and hydrogen peroxide (5% H2O2...

A double isotope dilution method for assaying of polycyclic aromatic hydrocarbons in cigarette smoke condensate

International Nuclear Information System (INIS)

Bechtold, W.E.; Chen, B.T.

1988-01-01

This report describes a double isotope dilution method for analysis of the polycyclic aromatic hydrocarbons (PAH) phenanthrene, fluor-anthene, pyrene, and benzo[a]pyrene in cigarette smoke particulates. The first isotope dilution used deuterated analogues of the first three PAH as internal standards. The second isotope dilution, for benzo[a]pyrene, used the tritiated analogue as an internal standard. The PAH were isolated from extracts of cigarette smoke particulates using a two-step procedure based on selective extraction from aqueous dimethyl sulfoxide (DMSO) followed by chromatography on silica gel extraction columns. After isolation, aliquots of the samples were analyzed for phenanthrene, pyrene, and fluoranthene by gas chromatography with mass spectrometric detection (GC/MS). Separate aliquots of the samples were analyzed for benzo[a]pyrene by high pressure liquid chromatography with fluorescence detection followed by liquid scintillation spectrometry. PAH levels from cigarette smoke condensates collected from different exposure modes were compared; no exposure-related differences were found. (author)

Doping control analysis of 46 polar drugs in horse plasma and urine using a 'dilute-and-shoot' ultra high performance liquid chromatography-high resolution mass spectrometry approach.

Science.gov (United States)

Kwok, Wai Him; Choi, Timmy L S; Kwok, Karen Y; Chan, George H M; Wong, Jenny K Y; Wan, Terence S M

2016-06-17

The high sensitivity of ultra high performance liquid chromatography coupled with high resolution mass spectrometry (UHPLC-HRMS) allows the identification of many prohibited substances without pre-concentration, leading to the development of simple and fast 'dilute-and-shoot' methods for doping control for human and equine sports. While the detection of polar drugs in plasma and urine is difficult using liquid-liquid or solid-phase extraction as these substances are poorly extracted, the 'dilute-and-shoot' approach is plausible. This paper describes a 'dilute-and-shoot' UHPLC-HRMS screening method to detect 46 polar drugs in equine urine and plasma, including some angiotensin-converting enzyme (ACE) inhibitors, sympathomimetics, anti-epileptics, hemostatics, the new doping agent 5-aminoimidazole-4-carboxamide-1-β-d-ribofuranoside (AICAR), as well as two threshold substances, namely dimethyl sulfoxide and theobromine. For plasma, the sample (200μL) was protein precipitated using trichloroacetic acid, and the resulting supernatant was diluted using Buffer A with an overall dilution factor of 3. For urine, the sample (20μL) was simply diluted 50-fold with Buffer A. The diluted plasma or urine sample was then analysed using a UHPLC-HRMS system in full-scan ESI mode. The assay was validated for qualitative identification purpose. This straightforward and reliable approach carried out in combination with other screening procedures has increased the efficiency of doping control analysis in the laboratory. Moreover, since the UHPLC-HRMS data were acquired in full-scan mode, the method could theoretically accommodate an unlimited number of existing and new doping agents, and would allow a retrospectively search for drugs that have not been targeted at the time of analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparison of GC-ICP-MS and HPLC-ICP-MS for species-specific isotope dilution analysis of tributyltin in sediment after accelerated solvent extraction

International Nuclear Information System (INIS)

Wahlen, Raimund; Wolff-Briche, Celine

2003-01-01

This study describes a direct comparison of GC and HPLC hyphenated to ICP-MS determination of tributyltin (TBT) in sediment by species-specific isotope dilution analysis (SS-IDMS). The certified reference sediment PACS-2 (NRC, Canada) and a candidate reference sediment (P-18/HIPA-1) were extracted using an accelerated solvent extraction (ASE) procedure. For comparison of GC and LC methods an older bottle of PACS-2 was used, whilst a fresh bottle was taken for demonstration of the accuracy of the methods. The data obtained show good agreement between both methods for both the PACS-2 sediment (LC-ICP-IDMS 828±87 ng g -1 TBT as Sn, GC-ICP-IDMS 848±39 ng g -1 TBT as Sn) and the P-18/ HIPA-1 sediment (LC-ICP-IDMS 78.0±9.7 ng g -1 TBT as Sn, GC-ICP-IDMS 79.2±3.8 ng g -1 TBT as Sn). The analysis by GC-ICP-IDMS offers a greater signal-to-noise ratio and hence a superior detection limit of 0.03 pg TBT as Sn, in the sediment extracts compared to HPLC-ICP-IDMS (3 pg TBT as Sn). A comparison of the uncertainties associated with both methods indicates superior precision of the GC approach. This is related to the better reproducibility of the peak integration, which affects the isotope ratio measurements used for IDMS. The accuracy of the ASE method combined with HPLC-ICP-IDMS was demonstrated during the international interlaboratory comparison P-18 organised by the Comite Consultatif pour la Quantite de Matiere (CCQM). The results obtained by GC-ICP-IDMS for a newly opened bottle of PACS-2 were 1087±77 ng g -1 Sn for DBT and 876±51 ng g -1 Sn for TBT (expanded uncertainties with a coverage factor of 2), which are in good agreement with the certified values of 1090±150 ng g -1 Sn and 980±130 ng g -1 Sn, respectively. (orig.)

Isotope dilution analysis of environmental samples

International Nuclear Information System (INIS)

Tolgyessy, J.; Lesny, J.; Korenova, Z.; Klas, J.; Klehr, E.H.

1986-01-01

Isotope dilution analysis has been used for the determination of several trace elements - especially metals - in a variety of environmental samples, including aerosols, water, soils, biological materials and geological materials. Variations of the basic concept include classical IDA, substoichiometric IDA, and more recently, sub-superequivalence IDA. Each variation has its advantages and limitations. A periodic chart has been used to identify those elements which have been measured in environmental samples using one or more of these methods. (author)

Antimicrobial Activity of Ephedra pachyclada Methanol Extract on Some Enteric Gram Negative Bacteria Which Causes Nosocomial Infections by Agar Dilution Method

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Amin Sadeghi Dosari

2016-10-01

Full Text Available Background Past history indicates that plants were served as an important source of medicine. Otherwise, in developing countries people use medicinal plants against infectious disease because they cannot afford expensive drugs. Due to increasing rate of drug-resistant diseases, there is an urgent need to detect novel antimicrobial compounds from medicinal plants. Objectives The aim of the present study was to determine Antimicrobial activity of Ephedra pachyclada methanol extract on some enteric Gram-negative bacteria which causes nosocomial infections by agar dilution method. Methods In this cross-sectional study, in order to examine the antimicrobial effects of Ephedra pachyclada extract on intestinal Gram-negative bacteria, we exposed them to 0/128, 0/25, 0/5, 1, 2, 4 and 8 mg/mL of the extract. Ephedra pachyclada was collected from Jiroft Heights and methanolic extract was prepared with maceration method, during which, 50 gr powder of Ephedra pachyclada was dissolved in 300 mL of 80% methanol. Results In this study, the antibacterial effects of Ephedra pachyclada extract on Gram-negative bacteria such as Pseudomonas aeruginosa, Escherichia coli (PTCC-O157, Escherichia coli (ATCC-25922, Klebsiella pnemoniae, Serratia marcescens was investigated, defining the minimum inhibitory concentration (MIC by agar dilution method. It has been demonstrated that methanolic extract of Ephedra pachyclada affect intestinal Gram-negative bacteria. Conclusions The result showed that, Ephedra pachyclada extract has effective antimicrobial ingredients which are cheap and readily available. It can be used for medicinal purposes in the production of antimicrobial drug.

Evaluation of xylitol production using corncob hemicellulosic hydrolysate by combining tetrabutylammonium hydroxide extraction with dilute acid hydrolysis.

Science.gov (United States)

Jia, Honghua; Shao, Tingting; Zhong, Chao; Li, Hengxiang; Jiang, Min; Zhou, Hua; Wei, Ping

2016-10-20

In this paper, we produced hemicellulosic hydrolysate from corncob by tetrabutylammonium hydroxide (TBAH) extraction and dilute acid hydrolysis combined, further evaluating the feasibility of the resultant corncob hemicellulosic hydrolysate used in xylitol production by Candida tropicalis. Optimized conditions for corncob hemicellulose extraction by TBAH was obtained via response surface methodology: time of 90min, temperature of 60°C, liquid/solid ratio of 12 (v/w), and TBAH concentration of 55%, resulting in a hemicellulose extraction of 80.07% under these conditions. The FT-IR spectrum of the extracted corncob hemicellulose is consistent with that of birchwood hemicellulose and exhibits specific absorbance of hemicelluloses at 1380, 1168, 1050, and 900cm(-1). In addition, we found that C. tropicalis can ferment the resulting corncob hemicellulosic hydrolysate with pH adjustment and activated charcoal treatment leading to a high xylitol yield and productivity of 0.77g/g and 2.45g/(Lh), respectively. Copyright © 2016 Elsevier Ltd. All rights reserved.

Characterization of the key aroma compounds in beef and pork vegetable gravies á la chef by application of the aroma extract dilution analysis.

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Christlbauer, Monika; Schieberle, Peter

2009-10-14

By application of the aroma extract dilution analysis (AEDA) on an aroma distillate isolated from a freshly prepared, stewed beef/vegetable gravy, 52 odor-active compounds were detected in the flavor dilution (FD) factor range of 4-4096. On the basis of high FD factors in combination with the results of the identification experiments, 3-(methylthio)propanal (cooked potato), 3-mercapto-2-methylpentan-1-ol (gravy-like), (E,E)-2,4-decadienal (deep-fried, fatty), 3-hydroxy-4,5-dimethyl-2(5H)-furanone (lovage-like), vanillin (vanilla-like), (E,E)-2,4-nonadienal (deep-fried), and (E)-2-undecenal (metallic) are suggested as key contributors to the aroma of the gravy. To get an insight into the role of the vegetables as sources of gravy odorants, a beef gravy was prepared without vegetables. The AEDA results revealed that, in particular, onions and leek are important sources of gravy aroma compounds, adding particularly the very potent, gravy-like smelling 3-mercapto-2-methylpentan-1-ol to the overall aroma profile. Further compounds that were clearly derived from the vegetables and, thus, are important modifiers of the overall aroma were 4-vinyl-2-methoxyphenol, (E)-beta-damascenone, beta-ionone, 2-isopropyl-3-methoxypyrazine, and 2-(sec-butyl)-3-methoxypyrazine. Interestingly, none of the key odorants detected in the gravy can be assumed to be formed from a reaction between beef and vegetable constituents. A comparison of the odorants in the beef/vegetable gravy with a gravy prepared according to the same procedure, but substituting beef by pork meat, indicated that most of the aroma compounds were identical-although different in FD factors-but the tallowy smelling 12-methyltridecanal was detected as key odorant only in the beef/vegetable gravy.

Influence of extragent dilution upon light rare earths separation

International Nuclear Information System (INIS)

Korpusova, R.D.; Smirnova, N.N.

1978-01-01

The effect of diluting the extragent on separation of REE in the presence of 6 g-equiv. of LiNO 3 has been studied. For experiments use was made of TBP diluted with kerosene or butylbenzene (40,50,70 vol.%). The separation coefficients have been determined under conditions of saturation. The content of trace amounts of the components has been determined by the weight method; the content of macroimpurities - by the radiometric method. It has been established that the coefficient of Ce-La, Pr-La separation is not affected by the dilution of the extragent. The only exception is the Pr 142 -La pair; in the presence of trace amounts of better extracted element and two-fold dilution the separation coefficient increases almost by 150%. For the Pr-Ce pair the effect of dilution is better noticeable in that case when more extracted element is present in trace amounts. However, a comparison of the effect of dilution on separation coefficients of all REE pairs under study has shown that this effect is the strongest for the samarium-neodymium pair. The data obtained allow an assumption to be made that kerosene, as a diluent, affects the steric factor and coordination. Therefore, upon dilution the coefficient of the samarium-neodymium pair separation is affected most of all

Reverse isotope dilution method for determining benzene and metabolites in tissues

International Nuclear Information System (INIS)

Bechtold, W.E.; Sabourin, P.J.; Henderson, R.F.

1988-01-01

A method utilizing reverse isotope dilution for the analysis of benzene and its organic soluble metabolites in tissues of rats and mice is presented. Tissues from rats and mice that had been exposed to radiolabeled benzene were extracted with ethyl acetate containing known, excess quantities of unlabeled benzene and metabolites. Butylated hydroxytoluene was added as an antioxidant. The ethyl acetate extracts were analyzed with semipreparative reversed-phase HPLC. Isolated peaks were collected and analyzed for radioactivity (by liquid scintillation spectrometry) and for mass (by UV absorption). The total amount of each compound present was calculated from the mass dilution of the radiolabeled isotope. This method has the advantages of high sensitivity, because of the high specific activity of benzene, and relative stability of the analyses, because of the addition of large amounts of unlabeled carrier analogue

Sub-stoichiometric isotope dilution analysis method for the determination of iodine in common salts using iodine-131 tracer

International Nuclear Information System (INIS)

Singh, Vivek; Garg, A.N.

1994-01-01

A sub-stoichiometric isotope dilution analysis (SIDA) method was developed for the determination of iodine in different brands of common salts. An aqueous salt solution containing 131 I tracer and NaI as carrier is oxidized by tartaric acid and KIO 3 and the liberated iodine is extracted with CCl 4 . To the extract an aqueous solution of AgNO 3 is added in substoichiometric amount to obtain a colloidal solution of AgI. On adding sodium thiosulfate solution, the NaI so formed passes into aqueous solution, which is then counted. Several different brands of salt were analysed. The method is especially suitable for the determination of microgram amounts of iodide in the presence of excess of chloride. (Author)

Odorant Screening and Quantitation of Thiols in Carmenere Red Wine by Gas Chromatography-Olfactometry and Stable Isotope Dilution Assays.

Science.gov (United States)

Pavez, Carolina; Agosin, Eduardo; Steinhaus, Martin

2016-05-04

The sensory impact of thiols in Vitis vinifera 'Carmenere' red wines was evaluated. For this purpose, aroma extract dilution analysis was applied to the thiols isolated from a Carmenere red wine by affinity chromatography with a mercurated agarose gel. Results revealed the presence of four odorants, identified as 2-furanylmethanethiol, 3-sulfanylhexyl acetate, 3-sulfanyl-1-hexanol, and 2-methyl-3-sulfanyl-1-butanol, with the latter being described here for the first time in Carmenere red wines. Quantitation of the four thiols in the Carmenere wine screened by aroma extract dilution analysis and in three additional Carmenere wines by stable isotope dilution assays resulted in concentrations above the respective orthonasal odor detection threshold values. Triangle tests applied to wine model solutions with and without the addition of the four thiols showed significant differences, thus suggesting that the compounds do have the potential to influence the overall aroma of red wine.

Characterization and comparison of key aroma compounds in raw and dry porcini mushroom (Boletus edulis) by aroma extract dilution analysis, quantitation and aroma recombination experiments.

Science.gov (United States)

Zhang, Huiying; Pu, Dandan; Sun, Baoguo; Ren, Fazheng; Zhang, Yuyu; Chen, Haitao

2018-08-30

A study was carried out to determine and compare the key aroma compounds in raw and dry porcini mushroom (Boletus edulis). The volatile fractions were prepared by solvent-assisted flavor evaporation (SAFE), and aroma extract dilution analysis (AEDA) combined with gas chromatography-mass spectrometry (GC-MS) was employed to identify the odorants. Selected aroma compounds were quantitated and odor activity values (OAVs) were calculated revealing OAVs ≥ 1 for 12 compounds in raw porcini, among which 1-octen-3-one showed the highest OAV. In addition to compounds with eight carbon atoms, 3-methylbutanal, (E,E)-2,4-decadienal and (E,E)-2,4-nonadienal were also responsible for the unique aroma profile. In dry mushroom OAVs ≥ 1 were obtained for 20 odorants. Among them, 3-(methylthio)propanal, 1-octen-3-one and pyrazines were determined as predominant odorants. Overall, drying increased complexity of volatile compounds, thus significantly changing the aroma profile of porcini, providing more desirable roasted and seasoning-like flavor and less grass-like and earthy notes. Copyright © 2018 Elsevier Ltd. All rights reserved.

Determination of Cd, Pb, Zn and Cu in Sediment Compartments by Sequential Extraction and Isotope Dilution Inductively Coupled Plasma Mass Spectrometry (ID-ICP-MS

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Gardolinski Paulo C. F. C.

2002-01-01

Full Text Available Trace concentrations of Cd, Cu, Pb and Zn in four different sediment fractions extracted in sequence were determined by isotope dilution inductively coupled mass spectrometry (IDICPMS. The metals from each fraction were extracted following the sequential extraction procedure recommended by the Bureau Commun de Référence (BCR of the Commission of the European Communities. As an alternative to external calibration, the elements were quantified by spiking the extracted solutions with 112Cd, 63Cu, 208Pb and 66Zn and application of isotope dilution. The proposed approach was applied to a sample collected from a lake and two standard reference materials, NIST2704 river sediment from the National Institute of Standards & Technology and the BCR-277 estuarine sediment. Detection limits, for each extracted solution, varied from 0.31 to 0.53 mug L¹ for Cd, 0.92 to 2.9 mug L¹ for Cu, 0.22 to 1.1 mug L¹ for Pb and 1.3 to 7.6 mug L¹ for Zn. The sum of the metals concentration in the different fractions was compatible with 95% confidence level found amounts obtained with complete digestion of the samples and with the certified values of the standard reference materials.

Quantitation of Rotundone in Grapefruit (Citrus paradisi) Peel and Juice by Stable Isotope Dilution Assay.

Science.gov (United States)

Nakanishi, Akira; Fukushima, Yusuke; Miyazawa, Norio; Yoshikawa, Keisuke; Maeda, Tomoko; Kurobayashi, Yoshiko

2017-06-21

Aroma extract dilution analyses of the aromas of peels and juices of white and pink grapefruits revealed that rotundone, responsible for peppery, spicy, and woody odors, was detected for the first time at high flavor dilution factors of 256-1024. In both juices, rotundone was detected at the highest flavor dilution factor of 1024. Rotundone in grapefruits was quantitated by a stable isotope dilution assay with a newly synthesized deuterium-labeled internal standard, rotundone-d 2,3 : its levels were 2180 and 1920 ng/kg in white and pink grapefruit peels and 29.6 and 49.8 ng/kg in white and pink grapefruit juices, respectively. On the basis of these results, sensory analysis was performed to assess the effects of rotundone on a white grapefruit juice aroma reconstitute. This sensory analysis revealed that rotundone does not impart a woody odor or affect any of the existing attributes, but increases various attributes, thus confirming that rotundone is indispensable for the aroma of grapefruit juice.

A comparative study on the skin penetration of pure tryptanthrin and tryptanthrin in Isatis tinctoria extract by dermal microdialysis coupled with isotope dilution ESI-LC-MS.

Science.gov (United States)

Oberthür, Christine; Heinemann, Christian; Elsner, Peter; Benfeldt, Eva; Hamburger, Matthias

2003-05-01

The indolo[2,1- b]quinazoline alkaloid tryptanthrin has recently been identified as a pharmacologically active compound in Isatis tinctoria, with potent dual inhibitory activity on prostaglandin and leukotriene synthesis. To investigate the skin penetration of tryptanthrin from solutions of pure compound and Isatis extracts, we developed and validated a cutaneous microdialysis model using ex vivo pig foreleg. Microdialysis was performed by placing linear probes in the dermis of the skin in situ, and tryptanthrin concentrations in the dialysates were determined by isotope dilution electrospray ionization LC-MS in the selected ion mode. Measurable concentrations of tryptanthrin were detected 30 min after application. A dose-dependent increase in tryptanthrin concentrations in the dialysate was observed for the Isatis extracts, but not for pure tryptanthrin. Microscopic analysis showed that the pure compound crystallized from the solution but remained in an amorphous state in the extracts.

Bias due to Preanalytical Dilution of Rodent Serum for Biochemical Analysis on the Siemens Dimension Xpand Plus

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Jennifer L. Johns

2018-02-01

Full Text Available Clinical pathology testing of rodents is often challenging due to insufficient sample volume. One solution in clinical veterinary and exploratory research environments is dilution of samples prior to analysis. However, published information on the impact of preanalytical sample dilution on rodent biochemical data is incomplete. The objective of this study was to evaluate the effects of preanalytical sample dilution on biochemical analysis of mouse and rat serum samples utilizing the Siemens Dimension Xpand Plus. Rats were obtained from end of study research projects. Mice were obtained from sentinel testing programs. For both, whole blood was collected via terminal cardiocentesis into empty tubes and serum was harvested. Biochemical parameters were measured on fresh and thawed frozen samples run straight and at dilution factors 2–10. Dilutions were performed manually, utilizing either ultrapure water or enzyme diluent per manufacturer recommendations. All diluted samples were generated directly from the undiluted sample. Preanalytical dilution caused clinically unacceptable bias in most analytes at dilution factors four and above. Dilution-induced bias in total calcium, creatinine, total bilirubin, and uric acid was considered unacceptable with any degree of dilution, based on the more conservative of two definitions of acceptability. Dilution often caused electrolyte values to fall below assay range precluding evaluation of bias. Dilution-induced bias occurred in most biochemical parameters to varying degrees and may render dilution unacceptable in the exploratory research and clinical veterinary environments. Additionally, differences between results obtained at different dilution factors may confound statistical comparisons in research settings. Comparison of data obtained at a single dilution factor is highly recommended.

Brewing Bokashi: Strengthening Student Skills in Dilution Theory through Fermentation Analysis

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Robert E. Zdor

2016-05-01

Full Text Available One of the basic microbiological techniques that students should master is that of using dilution theory to calculate the levels of bacteria in a fluid. This tip reports on using a rice water-milk fermentation mixture termed Bokashi as an easily implemented exercise in the basic microbiological lab to give students multiple opportunities to use dilution theory. Due to the shifts in bacterial community composition over time, a variety of microbes can be cultured using selective and nonselective media. Microscopic observation and the use of GEN III microplates to determine the collective phenotypic pattern of the mixture both give additional opportunities for students to hone their skills in bacterial analysis. Due to the decrease in the pH of the mixture over time, the notion of acid tolerance in bacteria can be explored and assessed using the microplate. By performing multiple rounds of serial dilutions and spread plating, students can practice their skill at using dilution theory several times over the course of the exercise.

SCREENING OF PLANT EXTRACTS FOR ANTIMICROBIAL ACTIVITY AGAINST BACTERIA

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Alexander Vatľák

2014-02-01

Full Text Available The aim of this study was antimicrobial action of the methanolic extracts of Equisetum arvense L. and Urtica dioica L. against gramnegative and grampositive bacteria. The antimicrobial activities of the extracts against gramnegative bacteria: Escherichia coli CCM 3988, Listeria ivanovii CCM 5884, Listeria innocua CCM 4030, Pseudomonas aeruginosa CCM 1960, Serratia rubidaea CCM 4684 and grampositive bacteria: Brochothrix thermosphacta CCM 4769, Enterococcus raffinosus CCM 4216, Lactobacillus rhamnosus CCM 1828, Paenobacillus larvae CCM 4483 and Staphylococcus epidermis CCM 4418 were determined by the disc diffusion method and the microbroth dilution method according to CLSI. Probit analysis was used in this experiment. Of the 2 plant extracts tested, all extracts showed antimicrobial activity against one or more species of microorganisms. The most antimicrobial activity showed methanolic plant extract of E. arvense against S. epidermis with disc diffusion method and with microbroth dilution method against S. rubidaea and plant extract Urtica dioica with disc diffusion method against P. aeruginosa and with microbroth dilution method against S. rubidaea and E. coli.

Isotope dilution analysis for the determination of zinc in blood samples of diabetic patients

International Nuclear Information System (INIS)

Garg, A.N.; Kumar, A.; Maheshwari, G.; Sharma, S.

2005-01-01

Isotope dilution analysis (IDA) based on solvent extraction has been developed for the determination of zinc in the blood of diabetic patients and healthy adults as controls. The method using 65 Zn as a tracer is based on the formation of a red colored complex with dithizone in chloroform which is measured by counting of the 1115 keV γ-rays by gamma-ray spectrometry. Various extraction parameters such as pH, nature of solvent and amount of reagent were optimized. Zinc concentration in diabetic patients (n = 10) was found in a much wider range (1.5-157 μg/ml) compared to those in healthy adults (3.1-95.9 μg/ml for n = 5). t-Test of data shows 80-90% confidence limits. A comparison of mean values, 28.5 ± 48.5 μg/ml for diabetics and 33.1 ± 34.5 μg/ml for controls shows 13.9% lower zinc concentration in diabetics. No correlation was found with eating (vegetarian/nonvegetarian)/drinking or smoking habits, but in general, females showed somewhat lower concentration compared to those in males though population size in each case was very small. (author)

Dilution Confusion: Conventions for Defining a Dilution

Science.gov (United States)

Fishel, Laurence A.

2010-01-01

Two conventions for preparing dilutions are used in clinical laboratories. The first convention defines an "a:b" dilution as "a" volumes of solution A plus "b" volumes of solution B. The second convention defines an "a:b" dilution as "a" volumes of solution A diluted into a final volume of "b". Use of the incorrect dilution convention could affect…

Gas chromatography/ion trap mass spectrometry applied for the analysis of triazine herbicides in environmental waters by an isotope dilution technique

International Nuclear Information System (INIS)

Cai Zongwei; Wang Dongli; Ma, W.T.

2004-01-01

A gas chromatography/ion trap mass spectrometry method was developed for the analysis of simazine, atrazine, cyanazine, as well as the degradation products of atrazine, such as deethylatrazine and deisopropylatrazine in environmental water samples. Isotope dilution technique was applied for the quantitative analysis of atrazine in water at low ng/l levels. One liter of water sample spiked with stable isotope internal standard atrazine-d 5 was extracted with a C 18 solid-phase extraction cartridge. The analysis was performed on an ion trap mass spectrometer operated in MS/MS method. The extraction recoveries were in the range of 83-94% for the triazine herbicides in water at the concentrations of 24, 200, and 1000 ng/l, while poor recoveries were obtained for the degradation products of atrazine. The relative standard deviation (R.S.D.) were within the range of 3.2-16.1%. The detection limits of the method were between 0.75 and 12 ng/l when 1 l of water was analyzed. The method was successfully applied to analyze environmental water samples collected from a reservoir and a river in Hong Kong for atrazine detected at concentrations between 3.4 and 26 ng/l

Evaluation of accelerated solvent extraction for butyltin speciation in PACS-2 CRM using double-spike isotope dilution-GC/ICPMS.

Science.gov (United States)

Encinar, Jorge Ruiz; Rodriguez-González, Pablo; Fernandez, Julio Rodriguez; Alonso, J Ignacio Garcia; Díez, Sergi; Bayona, Josep M; Sanz-Medelt, Alfredo

2002-10-15

Pressurized liquid extraction using the accelerated solvent extractor (Dionex ASE 200) has been evaluated for the determination of mono-, di- and tributyltin (MBT, DBT, and TBT, respectively) in PACS-2 certified reference material. A double-enriched spike containing 119Sn-enriched MBT and TBT and 118Sn-enriched DBT allowed for the simultaneous determination of the three butyltin species and the factors governing species interconversion. The stability of the spike was evaluated by reverse isotope dilution experiments covering more than one year with satisfactory results. Quantitative recoveries using ASE for TBT and DBT were obtained at temperatures above 110 degrees C. The effect of the extraction time and number of static cycles was evaluated. Results suggest that extraction efficiency was quantitative with extraction times as low as 10 min for all butyltin species at 110 degrees C. Decomposition reactions were only detected at the higher temperatures assayed (140 and 175 degrees C) and that was only for the degradation of DBT to MBT (approximately 4%). The results found for MBT were approximately 25% higher than the certified value for the PACS-2 sediment reference material in agreement with previous results obtained by ultrasonic and microwave assisted extraction.

Radioimmunoassay and liquid-chromatographic analysis for free cortisol in urine compared with isotope dilution-mass spectrometry

International Nuclear Information System (INIS)

Lantto, O.

1982-01-01

Three different routine methods for analysis for urinary cortisol with those by a highly specific reference method based on isotope dilution-mass spectrometry (I) were compared. A ''high-performance'' liquid-chromatographic method (II) gave the most comparable results (regression coefficient 0.86, intercept 9 nmol/L). For some urines much lower values were obtained by I than by II. Two radioimmunoassay (III) methods, one involving direct assay and one involving extraction, gave less-accurate results (regression coefficients of 1.87 and 1.52 and intercepts of 86 and 12 nmol/L, respectively), although values obtained by III and by I correlated well (r = 0.95-0.99), indicating a relation between the free cortisol and the compounds interfering in III. The apparent accuracy for the extraction method was improved by using as calibration standards urine samples previously assayed by I (regression coefficient 0.90, intercept 6 nmol/L). All four methods investigated showed a statistically significant sex-related difference in 24-h urinary cortisol excretion; evidently such a finding should be a prerequisite in any such method proposed for routine use

Mortality reduction by post-dilution online-haemodiafiltration : A cause-specific analysis

NARCIS (Netherlands)

Nubé, Menso J.; Peters, Sanne A E; Blankestijn, Peter J.; Canaud, Bernard; Davenport, Andrew; Grooteman, Muriel P C; Asci, Gulay; Locatelli, Francesco; Maduell, Francisco; Morena, Marion; Ok, Ercan; Torres, Ferran; Bots, Michiel L.; Moreso, Francesc; Pons, Mercedes; Ramos, Rosa; Mora-Macià, Josep; Carreras, Jordi; Soler, Jordi; Campistol, Josep M.; Martinez-Castelao, Alberto; Insensé, B.; Perez, C.; Feliz, T.; Barbetta, M.; Soto, C.; Mora, J.; Juan, A.; Ibrik, O.; Foraster, A.; Nin, J.; Fernández, A.; Arruche, M.; Sánchez, C.; Vidiella, J.; Barbosa, F.; Chiné, M.; Hurtado, S.; Llibre, J.; Ruiz, A.; Serra, M.; Salvó, M.; Poyuelo, T.; Maduell, F.; Carrera, M.; Fontseré, N.; Arias, M.; Merín, A.; Ribera, L.; Galceran, J. M.; Mòdol, J.; Moliner, E.; Ramirez, A.; Aguilera, J.; Alvarez, M.; De La Torre, B.; Molera, M.; Casellas, J.; Martín, G.; Andres, E.; Coll, E.; Valles, M.; Martínez, C.; Castellote, E.; Casals, J. M.; Gabàs, J.; Romero, M.; Martinez-Castelao, A.; Fulladosa, X.; Ramirez-Arellano, M.; Fulquet, M.; Pelegrí, A.; El Manouari, M.; Ramos, N.; Bartolomé, J.; Sans, R.; Fernández, E.; Sarró, F.; Compte, T.; Marco, F.; Mauri, R.; Bronsoms, J.; Arnaiz, J. A.; Beleta, H.; Pejenaute, A.; Ríos, J.; Lara, J.; Ter Wee, P. M.; Van Den Dorpel, M. A.; Dorval, M.; Lévesque, R.; Koopman, M. G.; Konings, C. J A M; Haanstra, W. P.; Kooistra, M.; Van Jaarsveld, B.; Noordzij, T.; Feith, G. W.; Peltenburg, H. G.; Van Buren, M.; Offerman, J. J G; Hoogeveen, E. K.; De Heer, F.; Van De Ven, P. J.; Kremer Hovinga, T. K.; Bax, W. A.; Groeneveld, J. O.; Lavrijssen, A. T J; Schrander-Van Der Meer, A. M.; Reichert, L. J M; Huussen, J.; Rensma, P. L.; Schrama, Y.; Van Hamersvelt, H. W.; Boer, W. H.; Van Kuijk, W. H.; Vervloet, M. G.; Wauters, I. M P M J; Sekse, I.; Toz, Huseyin; Ok, Ebru Sevinc; Kircelli, Fatih; Yilmaz, Mumtaz; Hur, Ender; Demirci, Meltem Sezis; Demirci, Cenk; Duman, Soner; Basci, Ali; Adam, Siddig Momin; Isik, Ismet Onder; Zengin, Murat; Suleymanlar, Gultekin; Yilmaz, Mehmet Emin; Ergin, Mehmet Ozkahya Pinar; Sagdic, Alfert; Kayali, Erkan; Boydak, Can; Colak, Taskin; Caliskan, Sihli; Kaplan, Hakan; Ulas, Hasibe; Kirbiyik, Sait; Berktas, Hakan; Dilbaz, Necati; Cristol, Jean Paul; Leray-Moragues, Hélène; Chenine, Leïla; Picot, Marie Christine; Jaussent, Audrey; Belloc, Claire; Lagarrigue, Mélodie; Chalabi, Lotfi; Debure, Alain; Ouziala, Messaoud; Lefevre, Jean Jacques; Thibaudin, Damien; Mohey, Hesham; Broyet, Christian; Afiani, Aida; Serveaux, Marie Odile; Patrier, Laure; Maurice, François; Rivory, Jean Pierre; Nicoud, Philippe; Durand, Claude; Normand, Michel; Seigneuric, Bruno; Magnant, Eric; Azzouz, Lynda; Islam, Mohamed Shariful; Vido, Sandor; Nzeyimana, Hilaire; Simonin, Danièle; Azymah, Yamina; Farah, Ibrahim; Coindre, Jean Philippe; Puyoo, Olivier; Chabannier, Marie Hélène; Ibos, Richard; Rouleau, Fabienne; Vela, Carlos; Joule, Josiane; Combarnous, François; Turc-Baron, Cécile; Ducret, Francis; Pointet, Philippe; Rey, Isabelle; Potier, Jacky; Bendini, Jean Christophe; Perrin, Franck; Kunz, Kristian; Lefrancois, Gaëlle; Colin, Angélique; Parahy, Sophie; Dancea, Irima; Coupel, Stéphanie; Testa, Angelo; Brunet, Philippe; Lebrun, Gaétan; Jaubert, Dominique; Delcroix, Catherine; Lavainne, Frédéric; Lefebvre, Anne; Guillodo, Marie Paule; Le Grignou, Dominique; Djema, Assia; Maaz, Mehadji; Chiron, Sylvie; Hoffmann, Maxime; Depraetre, Pascale; Haddj-Elmrabet, Atman; Joyeux, Véronique; Fleury, Dominique; Vrigneaud, Laurence; Lemaitre, Vincent; Aguilera, Didier; Guerraoui, Abdallah; Cremault, Alain; Laradi, Achour; Babinet, Francois

Background. From an individual participant data (IPD) meta-analysis from four randomized controlled trials comparing haemodialysis (HD) with post-dilution online-haemodiafiltration (ol-HDF), previously it appeared that HDF decreases all-cause mortality by 14% (95% confidence interval 25; 1) and

Use of image analysis for monitoring the dilution of Physalis peruviana pulp

Directory of Open Access Journals (Sweden)

Silvana Licodiedoff

2013-06-01

Full Text Available The aim of this work was to develop linear models using the image analysis coupled with density measurements to monitor the dilution of the Physalis juice in the concentrations ranging from 0 to 100% in mass of juice pulp. A sample corresponding to 20% in the mass of juice pulp was for validating purposes and a prediction of 19.9±0.3%. The models with three parameters showed the best predictions, providing this technique with a promising future for the monitoring the dilution of fruit juices.

Antimicrobial activity and phytochemical analysis of crude extracts and essential oils from medicinal plants.

Science.gov (United States)

Silva, N C C; Barbosa, L; Seito, L N; Fernandes, A

2012-01-01

We aimed to establish a phytochemical analysis of the crude extracts and performed GC-MS of the essential oils (EOs) of Eugenia uniflora L. (Myrtaceae) and Asteraceae species Baccharis dracunculifolia DC, Matricaria chamomilla L. and Vernonia polyanthes Less, as well as determining their antimicrobial activity. Establishment of the minimal inhibitory concentrations of the crude extracts and EOs against 16 Staphylococcus aureus and 16 Escherichia coli strains from human specimens was carried out using the dilution method in Mueller-Hinton agar. Some phenolic compounds with antimicrobial properties were established, and all EOs had a higher antimicrobial activity than the extracts. Matricaria chamomilla extract and E. uniflora EO were efficient against S. aureus strains, while E. uniflora and V. polyanthes extracts and V. polyanthes EO showed the best antimicrobial activity against E. coli strains. Staphylococcus aureus strains were more susceptible to the tested plant products than E. coli, but all natural products promoted antimicrobial growth inhibition.

Redox substoichiometry in isotope dilution analysis Pt. 4

International Nuclear Information System (INIS)

Kambara, T.; Yoshioka, H.; Ugai, Y.

1980-01-01

The oxidation reaction of antimony(III) with potassium dichromate has been investigated radiometrically. The quantitative oxidation of antimony(III) was found to be not disturbed even in large amounts of tin(IV). On the basis of these results the redox substoichiometric isotope dilution analysis using potassium dichromate as the oxidizing agent was proposed for the determination of antimony in metallic tin. An antimony content of 1.22+-0.05 μg in metallic tin (10 mg) was determined without separation of the matrix element. (author)

Effects of diluting medium and holding time on sperm motility analysis by CASA in ram.

Science.gov (United States)

Mostafapor, Somayeh; Farrokhi Ardebili, Farhad

2014-01-01

The aim of this study was to evaluate the effects of dilution rate and holding time on various motility parameters using computer-assisted sperm analysis (CASA). The semen samples were collected from three Ghezel rams. Samples were diluted in seminal plasma (SP), phosphate-buffered saline (PBS) containing 1% bovine serum albumin (BSA) and Bioexcell. The motility parameters that computed and recorded by CASA include curvilinear velocity (VCL), straight line velocity (VSL), average path velocity (VAP), straightness (STR), linearity (LIN), amplitude of lateral head displacement (ALH), and beat cross frequency (BCF). In all diluters, there was a decrease in the average of all three parameters of sperms movement velocity as the time passed, but density of this decrease was more intensive in SP. The average of ALH between diluters indicated a significant difference, as it was more in Bioexcell in comparison with the similar amount in SP and PBS. The average of LIN in the diluted sperms in Bioexcell was less than two other diluters in all three times. The motility parameters of the diluted sperms in Bioexcell and PBS indicated an important and considerable difference with the diluted sperms in SP. According to the gained results, the Bioexcell has greater ability in preserving motility of sperm in comparison with the other diluters but as SP is considered as physiological environment for sperm. It seems that the evaluation of the motility parameters in Bioexcell and PBS cannot be an accurate and comparable evaluation with SP.

Effects of diluting medium and holding time on sperm motility analysis by CASA in ram

Directory of Open Access Journals (Sweden)

Somayeh Mostafapor

2014-06-01

Full Text Available The aim of this study was to evaluate the effects of dilution rate and holding time on various motility parameters using computer-assisted sperm analysis (CASA. The semen samples were collected from three Ghezel rams. Samples were diluted in seminal plasma (SP, phosphate-buffered saline (PBS containing 1% bovine serum albumin (BSA and Bioexcell. The motility parameters that computed and recorded by CASA include curvilinear velocity (VCL, straight line velocity (VSL, average path velocity (VAP, straightness (STR, linearity (LIN, amplitude of lateral head displacement (ALH, and beat cross frequency (BCF. In all diluters, there was a decrease in the average of all three parameters of sperms movement velocity as the time passed, but density of this decrease was more intensive in SP. The average of ALH between diluters indicated a significant difference, as it was more in Bioexcell in comparison with the similar amount in SP and PBS. The average of LIN in the diluted sperms in Bioexcell was less than two other diluters in all three times. The motility parameters of the diluted sperms in Bioexcell and PBS indicated an important and considerable difference with the diluted sperms in SP. According to the gained results, the Bioexcell has greater ability in preserving motility of sperm in comparison with the other diluters but as SP is considered as physiological environment for sperm. It seems that the evaluation of the motility parameters in Bioexcell and PBS cannot be an accurate and comparable evaluation with SP.

Just add water: Accuracy of analysis of diluted human milk samples using mid-infrared spectroscopy.

Science.gov (United States)

Smith, R W; Adamkin, D H; Farris, A; Radmacher, P G

2017-01-01

To determine the maximum dilution of human milk (HM) that yields reliable results for protein, fat and lactose when analyzed by mid-infrared spectroscopy. De-identified samples of frozen HM were obtained. Milk was thawed and warmed (40°C) prior to analysis. Undiluted (native) HM was analyzed by mid-infrared spectroscopy for macronutrient composition: total protein (P), fat (F), carbohydrate (C); Energy (E) was calculated from the macronutrient results. Subsequent analyses were done with 1 : 2, 1 : 3, 1 : 5 and 1 : 10 dilutions of each sample with distilled water. Additional samples were sent to a certified lab for external validation. Quantitatively, F and P showed statistically significant but clinically non-critical differences in 1 : 2 and 1 : 3 dilutions. Differences at higher dilutions were statistically significant and deviated from native values enough to render those dilutions unreliable. External validation studies also showed statistically significant but clinically unimportant differences at 1 : 2 and 1 : 3 dilutions. The Calais Human Milk Analyzer can be used with HM samples diluted 1 : 2 and 1 : 3 and return results within 5% of values from undiluted HM. At a 1 : 5 or 1 : 10 dilution, however, results vary as much as 10%, especially with P and F. At the 1 : 2 and 1 : 3 dilutions these differences appear to be insignificant in the context of nutritional management. However, the accuracy and reliability of the 1 : 5 and 1 : 10 dilutions are questionable.

LC-HR-MS/MS standard urine screening approach: Pros and cons of automated on-line extraction by turbulent flow chromatography versus dilute-and-shoot and comparison with established urine precipitation.

Science.gov (United States)

Helfer, Andreas G; Michely, Julian A; Weber, Armin A; Meyer, Markus R; Maurer, Hans H

2017-02-01

Comprehensive urine screening for drugs and metabolites by LC-HR-MS/MS using Orbitrap technology has been described with precipitation as simple workup. In order to fasten, automate, and/or simplify the workup, on-line extraction by turbulent flow chromatography and a dilute-and-shoot approach were developed and compared. After chromatographic separation within 10min, the Q-Exactive mass spectrometer was run in full scan mode with positive/negative switching and subsequent data dependent acquisition mode. The workup approaches were validated concerning selectivity, recovery, matrix effects, process efficiency, and limits of identification and detection for typical drug representatives and metabolites. The total workup time for on-line extraction was 6min, for the dilution approach 3min. For comparison, the established urine precipitation and evaporation lasted 10min. The validation results were acceptable. The limits for on-line extraction were comparable with those described for precipitation, but lower than for dilution. Thanks to the high sensitivity of the LC-HR-MS/MS system, all three workup approaches were sufficient for comprehensive urine screening and allowed fast, reliable, and reproducible detection of cardiovascular drugs, drugs of abuse, and other CNS acting drugs after common doses. Copyright © 2016 Elsevier B.V. All rights reserved.

The application of three-phase liquid-liquid extraction to the analysis of bismuth and tellurium in sulphide concentrates

International Nuclear Information System (INIS)

Nicholas, D.J.

1976-01-01

An extraction system consisting of one aqueous and two organic phases is described. Diantipyrylmethane (DAM) is used as the extractant for bismuth and tellurium, which are extracted into the smaller of the two organic phases from nitric acid and perchloric acid respectively. The extraction efficiency is in the range of 90 to 95 per cent, compensation for incomplete extraction being made by the technique of standard addition. Copper, lead, and zinc are not extracted in either procedure. When the solutions contain high concentrations of iron, thioglycolic acid is used as a masking agent for iron in the extraction of bismuth. Atomic-absorption spectrophotometry is used for the analysis of the third phase after it has been diluted with methanol. The precision for bismuth and tellurium is in the range of 3 to 4 per cent. The accuracy, as ascertained from comparative analyses of sulphide concentrates, is good

Quantitative gas chromatography-olfactometry carried out at different dilutions of an extract. Key differences in the odor profiles of four high-quality Spanish aged red wines.

Science.gov (United States)

Ferreira, V; Aznar, M; López, R; Cacho, J

2001-10-01

Four Spanish aged red wines made in different wine-making areas have been extracted, and the extracts and their 1:5, 1:50, and 1:500 dilutions have been analyzed by a gas chromatography-olfactometry (GC-O) approach in which three judges evaluated odor intensity on a four-point scale. Sixty-nine different odor regions were detected in the GC-O profiles of wines, 63 of which could be identified. GC-O data have been processed to calculate averaged flavor dilution factors (FD). Different ANOVA strategies have been further applied on FD and on intensity data to check for significant differences among wines and to assess the effects of dilution and the judge. Data show that FD and the average intensity of the odorants are strongly correlated (r(2) = 0.892). However, the measurement of intensity represents a quantitative advantage in terms of detecting differences. For some odorants, dilution exerts a critical role in the detection of differences. Significant differences among wines have been found in 30 of the 69 odorants detected in the experiment. Most of these differences are introduced by grape compounds such as methyl benzoate and terpenols, by compounds released by the wood, such as furfural, (Z)-whiskey lactone, Furaneol, 4-propylguaiacol, eugenol, 4-ethylphenol, 2,6-dimethoxyphenol, isoeugenol, and ethyl vanillate, by compounds formed by lactic acid bacteria, such as 2,3-butanedione and acetoine, or by compounds formed during the oxidative storage of wines, such as methional, sotolon, o-aminoacetophenone, and phenylacetic acid. The most important differences from a quantitative point of view are due to 2-methyl-3-mercaptofuran, 4-propylguaiacol, 2,6-dimethoxyphenol, and isoeugenol.

Paradigms in isotope dilution mass spectrometry for elemental speciation analysis

International Nuclear Information System (INIS)

Meija, Juris; Mester, Zoltan

2008-01-01

Isotope dilution mass spectrometry currently stands out as the method providing results with unchallenged precision and accuracy in elemental speciation. However, recent history of isotope dilution mass spectrometry has shown that the extent to which this primary ratio measurement method can deliver accurate results is still subject of active research. In this review, we will summarize the fundamental prerequisites behind isotope dilution mass spectrometry and discuss their practical limits of validity and effects on the accuracy of the obtained results. This review is not to be viewed as a critique of isotope dilution; rather its purpose is to highlight the lesser studied aspects that will ensure and elevate current supremacy of the results obtained from this method

Effect of wine dilution on the reliability of tannin analysis by protein precipitation

DEFF Research Database (Denmark)

Jensen, Jacob Skibsted; Werge, Hans Henrik Malmborg; Egebo, Max

2008-01-01

A reported analytical method for tannin quantification relies on selective precipitation of tannins with bovine serum albumin. The reliability of tannin analysis by protein precipitation on wines having variable tannin levels was evaluated by measuring the tannin concentration of various dilutions...... of five commercial red wines. Tannin concentrations of both very diluted and concentrated samples were systematically underestimated, which could be explained by a precipitation threshold and insufficient protein for precipitation, respectively. Based on these findings, we have defined a valid range...... of the tannin response in the protein precipitation-tannin assay, which suffers minimally from these problems....

New Data on Joint Extraction of Nitric Acid, Uranium(VI) and Tetravalent Elements by Diluted TBP and New Approach to Modeling of their Distribution

International Nuclear Information System (INIS)

Zilberman, B.Ya.; Fedorov, Yu.S.; Puzikov, E.A.; Blazheva, I.V.

2008-01-01

HNO 3 and U(IV) extraction by diluted TBP (tributyl phosphate) appeared significantly higher than believed earlier, requiring correction of mathematical model for extraction of all the species. The proposed model of HNO 3 extraction includes its dissolving in the extracted water, as well as its abduction to UO 2 (NO 3 ) 2 (TBP) 2 . Extraction of U(VI) and tetravalent elements is considered as reaction of their hydrated or partially hydrolyzed forms, the latter could be extracted themselves or as neutral forms with water liberation. The equation of element chemical reaction for modeling is determined by the slope of the linear part of the S-shaped curve representing D/S 2 function as a plot of HNO 3 concentration, where D is a distribution coefficient of the micro-component and S is a TBP concentration free of HNO 3 . The description of tetravalent element extraction in U(VI) presence needs the assumption of cation-cation interaction of element hydrolyzed forms with U(VI) in aqueous phase. Zr distribution is affected by micellar effects. (authors)

Laminar Flame Velocity and Temperature Exponent of Diluted DME-Air Mixture

Science.gov (United States)

Naseer Mohammed, Abdul; Anwar, Muzammil; Juhany, Khalid A.; Mohammad, Akram

2017-03-01

In this paper, the laminar flame velocity and temperature exponent diluted dimethyl ether (DME) air mixtures are reported. Laminar premixed mixture of DME-air with volumetric dilutions of carbon dioxides (CO2) and nitrogen (N2) are considered. Experiments were conducted using a preheated mesoscale high aspect-ratio diverging channel with inlet dimensions of 25 mm × 2 mm. In this method, flame velocities are extracted from planar flames that were stabilized near adiabatic conditions inside the channel. The flame velocities are then plotted against the ratio of mixture temperature and the initial reference temperature. A non-linear power law regression is observed suitable. This regression analysis gives the laminar flame velocity at the initial reference temperature and temperature exponent. Decrease in the laminar flame velocity and increase in temperature exponent is observed for CO2 and N2 diluted mixtures. The addition of CO2 has profound influence when compared to N2 addition on both flame velocity and temperature exponent. Numerical prediction of the similar mixture using a detailed reaction mechanism is obtained. The computational mechanism predicts higher magnitudes for laminar flame velocity and smaller magnitudes of temperature exponent compared to experimental data.

The separation and determination of fatty acids by isotopic dilution and radiogas-liquid chromatography

International Nuclear Information System (INIS)

Beardsley, D.A.

1981-01-01

A number of static phases have been evaluated for the GLC separation of fatty acids. Of those investigated, only AT 1200 was capable of resolving the isomeric forms of the acids. A radiogas-liquid chromatographic method incorporating isotopic dilution analysis has been developed for the determination of n-butyric acid. The proposed method has been applied to the determination of the acid in hydrolysed butter fat and milk chocolate extracts. (author)

The interlaboratory experiment IDA-72 on mass spectrometric isotope dilution analysis. Vol. 1

International Nuclear Information System (INIS)

Beyrich, W.; Drosselmeyer, E.

1975-07-01

Within the framework of the Safeguards Project of the Federal Republic of Germany at the Nuclear Research Center Karlsruhe an analytical intercomparison program was carried out in cooperation with 22 laboratories of 13 countries or international organizations. The main objective was the acquisition of basic data on the errors involved in the mass spectrometric isotope dilution analysis if it is applied to the determination of uranium and plutonium in diluted active feed solutions of reprocessing plants in routine operation. The results were evaluated by statistical methods mainly in regard to the calculation of the estimates of the variances for the different error components contributing to the total error of this analytical technique. Furthermore, the performance of two new methods for sample conditioning suggested by the International Atomic Energy Agency, Vienna, and the European Institute for Transuranium Elements (EURATOM), Karlsruhe, was successfully tested. The results of some investigations on the stability of diluted high active feed solutions and on comparison analysis by X-ray fluorescence spectrometry are also included. Data on the analytical efforts (manhours) invested in this study are reported as well as general experiences made in the organization and performance of an experiment on such an extended international level. (orig.) [de

Dehydration of ethanol with salt extractive distillation-a comparative analysis between processes with salt recovery

Energy Technology Data Exchange (ETDEWEB)

Ligero, E.L.; Ravagnani, T.M.K. [Departamento de Engenharia de Sistemas Qumicos, Faculdade de Engenharia Qumica, Universidade Estadual de Campinas, Campinas, Sao Paulo (Brazil)

2003-07-01

Anhydrous ethanol can be obtained from a dilute aqueous solution of ethanol via extractive distillation with potassium acetate. Two process flowsheets with salt recovery were proposed. In the first, dilute ethanol is directly fed to a salt extractive distillation column and, after that, the salt is recovered in a multiple effect evaporator followed by a spray dryer. In the second, the concentrated ethanol from conventional distillation is fed to a salt extractive distillation column. In this case, salt is recovered in a single spray dryer. In both processes the recovered salt is recycled to be used in the extractive distillation column. Every component of each process was rigorously modeled and its behavior was simulated for a wide range of operating conditions. A global simulation was then carried out. The results show that the second process is more interesting in terms of energy consumption than the first. Furthermore, it would be easier to implement changes on existing benzene extractive anhydrous ethanol plants to convert them to more ecologically attractive concentrated ethanol feed processes. (author)

Application of 1- (3,4-dimenthylphenyl)-dodecanedione-1,2-dioxime (MFDDO) to substoichiometris extraction and determination of nickel(II) by the isotope dilution method

Energy Technology Data Exchange (ETDEWEB)

Gorski, Z.; Goraczko, W. [Technical University Poznan, Poznan (Poland). Radio and Photo Chemistry Department

1997-10-01

The conditions for use of 1-3,4-dimenthylphenyl-dodecanedione-1,2-dioxime (MFDDO) in toluene solution for substoichiometric extraction of Ni(II) from aqueous phases are described. This procedure allows the determination of 0.006-0.06 g/ml of nickel(II) in human urine and blood`s serum samples by the isotope dilution method using {sup 63}Ni(II) 9 refs., 5 figs.

A user-friendly robotic sample preparation program for fully automated biological sample pipetting and dilution to benefit the regulated bioanalysis.

Science.gov (United States)

Jiang, Hao; Ouyang, Zheng; Zeng, Jianing; Yuan, Long; Zheng, Naiyu; Jemal, Mohammed; Arnold, Mark E

2012-06-01

Biological sample dilution is a rate-limiting step in bioanalytical sample preparation when the concentrations of samples are beyond standard curve ranges, especially when multiple dilution factors are needed in an analytical run. We have developed and validated a Microsoft Excel-based robotic sample preparation program (RSPP) that automatically transforms Watson worklist sample information (identification, sequence and dilution factor) to comma-separated value (CSV) files. The Freedom EVO liquid handler software imports and transforms the CSV files to executable worklists (.gwl files), allowing the robot to perform sample dilutions at variable dilution factors. The dynamic dilution range is 1- to 1000-fold and divided into three dilution steps: 1- to 10-, 11- to 100-, and 101- to 1000-fold. The whole process, including pipetting samples, diluting samples, and adding internal standard(s), is accomplished within 1 h for two racks of samples (96 samples/rack). This platform also supports online sample extraction (liquid-liquid extraction, solid-phase extraction, protein precipitation, etc.) using 96 multichannel arms. This fully automated and validated sample dilution and preparation process has been applied to several drug development programs. The results demonstrate that application of the RSPP for fully automated sample processing is efficient and rugged. The RSPP not only saved more than 50% of the time in sample pipetting and dilution but also reduced human errors. The generated bioanalytical data are accurate and precise; therefore, this application can be used in regulated bioanalysis.

Accurate quantification of polycyclic aromatic hydrocarbons in dust samples using microwave-assisted solvent extraction combined with isotope-dilution mass spectrometry

International Nuclear Information System (INIS)

Itoh, Nobuyasu; Fushimi, Akihiro; Yarita, Takashi; Aoyagi, Yoshie; Numata, Masahiko

2011-01-01

Highlights: → We applied MAE-IDMS for accurate quantification of PAHs in dust samples. → Both partitioning and isotopic equilibria can be achieved using this technique. → MAE-IDMS can provide accurate concentrations even if extraction efficiencies were low. → Characteristics of samples strongly affected for low extraction efficiencies of PAHs. - Abstract: For accurate quantification of polycyclic aromatic hydrocarbons (PAHs) in dust samples, we investigated the use of microwave-assisted solvent extraction (MAE) combined with isotope-dilution mass spectrometry (IDMS) using deuterium-labelled PAHs (D-PAHs). Although MAE with a methanol/toluene mixture (1:3 by volume) at 160 deg. C for 40 min was best for extracting PAHs from tunnel dust among examined, the recovery yields of D-PAHs decreased with increasing molecular weight (<40% for MW ≥ 264; that of deuterium-labelled indeno[123-cd]pyrene (D-IcdP) was only 7.1%). Although the residues were extracted a second time, the observed concentrations did not change dramatically (<5%), and the recovery yields of heavier D-PAHs (i.e., MW ≥ 264) were approximately half of those of the first extract, including D-IcdP (3.4%). These results suggest that both partitioning and isotopic equilibria of PAHs and D-PAHs between sample and solvent were achieved for extractable heavier PAHs under the condition. Thus, the observed concentrations of PAHs obtained by MAE-IDMS were reasonable, even though recovery yields of D-PAHs were <50%. From the results of carbon analyses and extractable contents, lower recovery yields of D-PAHs from the tunnel dust were due to a large content of char with low extractable contents.

Moderate Dilution of Copper Slag by Natural Gas

Science.gov (United States)

Zhang, Bao-jing; Zhang, Ting-an; Niu, Li-ping; Liu, Nan-song; Dou, Zhi-he; Li, Zhi-qiang

2018-01-01

To enable use of copper slag and extract the maximum value from the contained copper, an innovative method of reducing moderately diluted slag to smelt copper-containing antibacterial stainless steel is proposed. This work focused on moderate dilution of copper slag using natural gas. The thermodynamics of copper slag dilution and ternary phase diagrams of the slag system were calculated. The effects of blowing time, temperature, matte settling time, and calcium oxide addition were investigated. The optimum reaction conditions were identified to be blowing time of 20 min, reaction temperature of 1250°C, settling time of 60 min, CaO addition of 4% of mass of slag, natural gas flow rate of 80 mL/min, and outlet pressure of 0.1 MPa. Under these conditions, the Fe3O4 and copper contents of the residue were 7.36% and 0.50%, respectively.

Chelating agents as stationary phase in extraction chromatography, ch. 11

International Nuclear Information System (INIS)

Sebesta, F.

1975-01-01

Chelating agents have been used largely in extraction chromatography for separations related to activation analysis, for concentration of metals from dilute solutions, and for preparation of radiochemically pure or carrier-free radionuclides. This review deals with the theory of extraction by chelating agents, the experimental technique, and the chelating agents and systems used (β-diketones, oximes, hydroxamic acid, dithizone and diethyldithiocarbamic acid)

Identification of antifungal activity substances on seedborn disease from garlic and taxus extracts

Energy Technology Data Exchange (ETDEWEB)

Chung, I.M.; Paik, S.B. [Konkuk University, Seoul (Korea, Republic of)

1999-02-01

Antifungal substances were isolated and identified from garlic and taxus extracts to develop safe and broad fungicide. The inhibitory effect of seedborn disease of sesame, pepper, radish, chinese cabbage by formulation of antifungal substances was investigated. The antifungal substance isolated through column chromatography from garlic and taxus extracts was confirmed by GC-MS as allicin (C{sub 6}H{sub 10}OS{sub 2}) and taxol(C{sub 47}H{sub 51}NO{sub 14}) and the quantified content from each extracts by HPLC analysis was 0.62%, 0.29%, respectively. The formulation composed of garlic and taxus extracts controlled effectively the seedborn fungi tested in this study at 10X dilution, but at 100X dilution the inhibitory effect decreased. Phytotoxicity of these formulations did not recognized. 22 refs., 6 figs., 5 tabs.

Multiresidue analysis of persistent organic pollutants in contaminated soil using GC-LRMS, GC-HRMS and isotope dilution analysis

International Nuclear Information System (INIS)

Badea, Silviu-Laurentiu; Lundstedt, Staffan; Liljelind, Per; Tysklind, Mats

2009-01-01

In this study we evaluated a multiresidue analytical protocol for selected Persistent Organic Pollutants (POPs) in soil, that later can be used in adsorption and leaching studies. The method used was based on Soxhlet extraction and open column chromatographic fractionation and clean-up, as well as liquid-liquid extraction and acetylation for phenolic compounds. Target analytes, i.e. polychlorinated phenols (PCPhs), hexachlorobenzene (HCB), polychlorinated dibenzodioxins and furans (PCDDs/Fs), polychlorinated biphenyl (PCBs) PAHs, were detected and quantified using Gas Chromatography-Low Resolution Mass Spectrometry (GC-LRMS) and Gas Chromatography-High Resolution Mass Spectrometry (GC-HRMS) and isotope dilution methodology. Generally, the results show a good recovery and a low standard deviation for those isomers that have also a 13 C labeled compound present in the sample: 4-mono, 2,4 di, 2,4,5 tri, 2,3,4,5 and penta chlorinated phenols. Our results clearly demonstrate that it is possible to analyse a wide range of compounds in complex soil matrixes. (authors(

Recovery of Cu(II from diluted aqueous solutions by non-dispersive solvent extraction

Directory of Open Access Journals (Sweden)

Alguacil, E. J.

2002-08-01

Full Text Available The removal of copper from diluted aqueous solutions with ACORGA M5640 extractant using non-dispersive solvent extraction technology was studied. It was possible to remove Cu(II below the international standars from solutions having initially as low concentration as 0,01 g/l under various experimental conditions, i.e aqueous pH 4.0, 10 % v/v ACORGA M5640 in Exxol D100, an organic flow of 100 ml/min, and an aqueous flow 50ml/min. Since the removal occurs by chelating ion exchange between copper from solution and protons from the extractant, the former was stripped by using a 180 g/l sulphuric acid solution which flowed (50 ml/min through the tube side organic was passed (400 ml/min through the shell side of the fibers of the module

Se estudia la eliminación del cobre presente en disoluciones acuosas diluidas empleando el agente de extracción ACORGA M5640 y la tecnología de extracción con disolventes no dispersiva. Bajo las condiciones experimentales estudiadas, pH de la fase acuosa 4,0 ±0,1, 10 % v/v ACORGA M5640 en Exxsol D100, flujo de la fase orgánica 100 ml/min, flujo de la fase acuosa 50 ml/min, es posible eliminar el Cu(II, por debajo de los límites marcados internacionalmente, en disoluciones con un contenido tan bajo como 0,01 g/1 del metal. Debido a que la extracción transcurre mediante un intercambio catiónico (y formación de un compuesto tipo quelato entre el cobre presente en el medio acuoso y los protones del agente de extracción, el metal se puede reextraer mediante la utilización de una disolución de 180 g/1 de ácido sulfúrico que fluye (50 ml/min a través de la parte interior de las fibras del módulo, mientras que la fase orgánica fluye (400 ml/min por la parte exterior de las mismas fibras.

Soluble/insoluble (dilute-HCl-extractable fractionation of Cd, Pb and Cu in Antarctic snow and its relationship with metal fractionations in the aerosol

Directory of Open Access Journals (Sweden)

Annibaldi A.

2013-04-01

Full Text Available A chemical fractionation methodology for determination of the (water soluble and the insoluble (dilute-HCl-extractable fractions of Cd, Pb and Cu in Antarctic snow was set-up and verified for the additivity of the two fractions detected. Molten samples were filtrated and the water-insoluble fraction was extracted by dilute ultrapure HCl (pH ~1.5. Metal determinations were carried out in the two fractions by square wave anodic stripping voltammetry. The total metal concentrations in samples collected in the 2000–2001 austral summer in a clean area (Faraglione Camp in the neighbourhood of the Mario Zucchelli Italian Station were of the order of Cd 10-20 pg g−1, Pb 20–40 pg g−1, Cu 60–120 pg g−1 with an approximate equidistribution between soluble and insoluble fractions. These fractionations compare well (and show a quite consistent temporal trend with those observed in the aerosol samples collected in the same area/period and confirm the close relationship between metal distributions in snow/ice and in the aerosol. At the station metal concentrations increase due to anthropic contribution and the distribution changes with Cd predominantly present in the soluble fraction (~80%, while Pb and Cu are more concentrated in the insoluble fraction, 70–80% and ~70%, respectively.

Modifications to the SPS LSS6 Septa for LHC and the SPS Septa Diluters

CERN Document Server

Borburgh, Y; Goddard, B; Kadi, Y

2006-01-01

The Large Hadron Collider required the modification of the existing extraction channel in the long straight section (LSS) 6 of the CERN Super Proton Synchrotron (SPS), including the suppression of the electrostatic wire septa. The newly set up fast extraction will be used to transfer protons at 450 GeV/c as well as ions via the 2.9 km long transfer line TI 2 to Ring 1 of the LHC. The girder of the existing SPS DC septa was modified to accommodate a new septum protection element. Changes were also applied to the septum diluter in the fast extraction channel in LSS4, leading to the other LHC ring and the CNGS facility. The requirements and the layout of the new LSS6 extraction channel will be described including a discussion of the design and performance of the installed septum diluters.

Determination of nanogram amounts of iodide by electrochemical isotope dilution analysis

International Nuclear Information System (INIS)

Gabrielsson, A.-B.; Beronius, P.

1976-01-01

A known quantity of iodide in ethanol as solvent was labelled with 131 I-and subsequently diluted with a predetermined amount of inactive iodide. Specific activities before and after the isotope dilution were established by anodically depositing small fractions of the halide in each sample on rotating silver micro electrodes and determining the activities of the electrodeposits. The lowest concentration of iodide used in any analysis was 1.10 -5 M. Further deposition studies revealed that iodide can be deposited with 1 100% current efficiency on the rotating silver micro electrode for concentration down to 2.4.10 -6 M. Electrodeposition studies for still lower concentrations have not yet been undertaken. These results suggest that amounts of iodide ion down to about 10 ng, and possibly still smaller quantitites, might be determined with the method developed. Amounts from 42 ng to 1 μg can be determined with an error of 2.5%. (T.G.)

Analysis of boron dilution in a four-loop PWR

International Nuclear Information System (INIS)

Sun, J.G.; Sha, W.T.

1995-03-01

Thermal mixing and boron dilution in a pressurized water reactor were analyzed with COMMIX codes. The reactor system was the four-loop Zion reactor. Two boron dilution scenarios were analyzed. In the first scenario, the plant is in cold shutdown and the reactor coolant system has just been filled after maintenance on the steam generators. To flush the air out of the steam generator tubes, a reactor coolant pump (RCP) is started, with the water in the pump suction line devoid of boron and at the same temperature as the coolant in the system. In the second scenario, the plant is at hot standby and the reactor coolant system has been heated to operating temperature after a long outage. It is assumed that an RCP is started, with the pump suction line filled with cold unborated water, forcing a slug of diluted coolant down the downcomer and subsequently through the reactor core. The subsequent transient thermal mixing and boron dilution that would occur in the reactor system is simulated for these two scenarios. The reactivity insertion rate and the total reactivity are evaluated and a sensitivity study is performed to assess the accuracy of the numerical modeling of the geometry of the reactor coolant system

Diglycolic acid modified zirconium phosphate and studies on the extraction of Am(III) and Eu(III) from dilute nitric acid medium

Energy Technology Data Exchange (ETDEWEB)

Selvan, B. Robert; Suneesh, A.S.; Venkatesan, K.A.; Antony, M.P. [Indira Gandhi Centre for Atomic Research, Kalpakkam (India). Fuel Chemistry Division; Dasthaiah, K.; Gardas, R.L. [Indian Institute of Technology - Madras, Chennai (India). Dept. of Chemistry

2017-06-01

Diglycolic acid modified zirconium phosphate (ZrP-DGA) was prepared and studied for the extraction of Am(III) and Eu(III) from dilute nitric acid medium. The distribution coefficient (K{sub d}, mL.g{sup -1}) of Am(III) and Eu(III) was measured as a function of time, pH and concentration of Eu(III) ion etc. The K{sub d} of Am(III) and Eu(III) increased with increase of pH, reached a maximum value of distribution coefficient at pH 1.5 - 2, followed by decrease in K{sub d} values. Rapid extraction of Am(III) and Eu(III) in ZrP-DGA was observed followed by the establishment of equilibrium occurred in 100 min. Kinetics of extraction was fitted in to pseudo second order rate equation. The amount of Eu(III) loaded in ZrP-DGA increased with increase in the concentration of Eu(III) ion in aqueous phase and the isotherm was fitted in to Langmuir and Freundlich adsorption models. The extraction of Am(III) in ZrP-DGA was higher as compared to Eu(III) and the interference of Eu(III) on the extraction of Am(III) was studied. The distribution coefficient of some lanthanides in ZrP-DGA was measured and the K{sub d} of lanthanides increased across the lanthanide series. The extracted trivalent metal ions were recovered in three contacts of loaded ZrP-DGA with 0.5 M nitric acid.

Effect of Melanin Free Ink Extracted From Squid (Loligo sp.) on Proximate and Sensory Characteristics of Soft-Bone Milkfish (Chanos chanos) During Storage

Science.gov (United States)

Winarni Agustini, Tri; Hadiyanto; Wijayanti, Ima; Amalia, Ulfah; Benjakul, Soottawat

2018-02-01

Antioxidant could be extracted and isolated from squid inks. Squid ink in the form of melanin free ink (MFI) could be act as an electron donor which can stabilize free radicals in lipid oxidation. This study was carried out to assess the antioxidant activity of squid inks converted into MFI in different dilution and to optimize the extraction conditions for the application of MFI as an antioxidative agent on fish product. Three different types of MFI extracts i.e : pure squid ink, squid ink with 5 times dilution and squid ink with 10 times dilutions by using cooled ionized water (4°C). The ink was then centrifuged at 18.000 x g for 30 minutes at cooled centrifuge (4°C) followed by DPPH analysis. The results showed that the IC50 of MFI extracts were 2.84 ppm; 1.11 ppm and 0.34 ppm, respectively (p squid ink with 10 times dilution in extraction of MFI had the highest value in free radical inhibitory. Although the IC50 of three different dilutions are equally low, and are considered as very strong antioxidative agent, however, it showed that the MFI extracted from squid ink had the ability to prevent free radical

Comparison of the methods for tissue triiodothyronine T(3) extraction and subsequent radioimmunoassay

International Nuclear Information System (INIS)

Takaishi, M.; Miyachi, Y.; Aoki, M.; Shishiba, Y.; Asahi Life Foundation, Tokyo

1978-01-01

Although there have been various reports on tissue T 3 concentration, the examination of the quality of radioimmunoassay has not been available. In the present study, we tried to determine whether the available methods for T 3 extraction are adequate for the various methods of T 3 radioimmunoassays used. T 3 was extracted from liver by ethanol extraction or by acid butanol extraction (Flock's method) and the extract was applied to radioimmunoassay either by Seralute T 3 column, ANS-double antibody or the ANS-charcoal method. The values of T 3 were compared with those obtained by isotope-equilibration method. The dilution curve of ethanol extract was not parallel with that of the standard in ANS-charcoal or ANS-double antibody technique. When the extract was tested by Seralate method, the dilution curve was parallel to the standard, whereas the T 3 value obtained with this method was two-fold higher than that with the isotope equilibration technique. The analysis of the ethanol extract suggested that the lipid extracted by ethanol interfered with the assay. The acid butanol extract when tested either by the ANS-double antibody or Seralate method, showed parallelism to the standard curve and gave T 3 values almost identical with those by the isotope-equilibration method. When tested by ANS-charcoal method, the dilution curve of the acid butanol extract was not parallel to the standard. Thus, to obtain reliable results, tissue extraction by Flock's method and subsequent T 3 radioimmunoassay by either ANS-double antibody or Seralate T 3 method are recommended. (author)

Certification of methylmercury in cod fish tissue certified reference material by species-specific isotope dilution mass spectrometric analysis

Energy Technology Data Exchange (ETDEWEB)

Inagaki, Kazumi; Kuroiwa, Takayoshi; Narukawa, Tomohiro; Yarita, Takashi; Takatsu, Akiko; Okamoto, Kensaku; Chiba, Koichi [National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), Environmental Standard Section, Tsukuba, Ibaraki (Japan)

2008-07-15

A new cod fish tissue certified reference material, NMIJ CRM 7402-a, for methylmercury analysis was certified by the National Metrological Institute of Japan in the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Cod fish was collected from the sea close to Japan. The cod muscle was powdered by freeze-pulverization and was placed into 600 glass bottles (10 g each), which were sterilized with {gamma}-ray irradiation. The certification was carried out using species-specific isotope dilution gas chromatography inductively coupled plasma mass spectrometry (SSID-GC-ICPMS), where {sup 202}Hg-enriched methylmercury (MeHg) was used as the spike compound. In order to avoid any possible analytical biases caused by nonquantitative extraction, degradation and/or formation of MeHg in sample preparations, two different extraction methods (KOH/methanol and HCl/methanol extractions) were performed, and one of these extraction methods utilized two different derivatization methods (ethylation and phenylation). A double ID method was adopted to minimize the uncertainty arising from the analyses. In order to ensure not only the reliability of the analytical results but also traceability to SI units, the standard solution of MeHg used for the reverse-ID was prepared from high-purity MeHg chloride and was carefully assayed as follows: the total mercury was determined by ID-ICPMS following aqua regia digestion, and the ratio of Hg as MeHg to the total Hg content was estimated by GC-ICPMS. The certified value given for MeHg is 0.58 {+-} 0.02 mg kg{sup -1} as Hg. (orig.)

Antioxidant and antimicrobial activity of stingless bee bread and propolis extracts

Science.gov (United States)

Akhir, Rabieatul Adawieah Md; Bakar, Mohd Fadzelly Abu; Sanusi, Shuaibu Babaji

2017-10-01

Bee bread and propolis are by-products of honey bee. The main objective of this research was to investigate the antioxidant and antimicrobial activity of stingless bee bread and propolis extracted using 70% ethanol and n-hexane. The antioxidant activity of the sample extracts were determined by spectrophotometry analysis while for the antimicrobial activity, the sample extracts were analyzed using disc diffusion and broth dilution assays. For DPPH and ABTS assays, the results showed that ethanolic extract of bee bread showed the highest free radical scavenging (%) as compared to other samples. However, FRAP values for both hexanic extracts are higher as compared to the ethanolic extracts. For disc diffusion assay, the results showed that the ethanolic extract of bee bread and propolis as well as hexanic extract of propolis were able to inhibit all tested bacteria. Meanwhile, broth dilution assay showed minimum inhibition zone (MIC) ranging from <6.67 to 33.33 µL/mL. As the conclusion, both bee bread and propolis produced by stingless bee in this study displayed antioxidant and antimicrobial effect but there are different in the degree of antioxidant and antimicrobial activity exhibited between each of the samples.

Effect of diluents on the extraction of actinides and nitric acid by bidentate organophosphorus compounds

International Nuclear Information System (INIS)

Rozen, A.M.

1986-01-01

The effect of dilutents on extraction by bidentate organophosphorus compounds (diphosphine dioxides, carbamoyl phosphonates, and phosphine oxides) was studied. Figures show the effect of dilutents on the extraction of americium by TOPO and by carbamoylmethylene phosphonate, and the effect of dilutents on the extraction of nitric acid and americium by carbamoylphosphine oxide. Also shown is the effect of dilutents on the extraction of americium by diphenyldioctyl methylenediphosphine dioxide, and the effect of dilutents on the extraction of americium by tetraphenylmethylenediphosphine dioxide. It was concluded that when TBP is added the distribution coefficient of Am increases but the effect of TBP may not be represented by the usual power relationship between the distribution coefficient and the TBP concentration, which would be expected if TBP was found to be very strong but for dilution by DCE it was relatively weak. The observed facts can be explained if it is assumed that TBP reacts with the bridging protons in the complex, which are free for dilution by benzene and are partially occupied when dichlorethane is used

Spectroscopic analysis of hot-water- and dilute-acid-extracted hardwood and softwood chips

Science.gov (United States)

Lehto, Joni; Louhelainen, Jarmo; Huttunen, Marko; Alén, Raimo

2017-09-01

Hot-water and dilute sulfuric acid pretreatments were performed prior to chemical pulping for silver/white birch (Betula pendula/B. pubescens) and Scots pine (Pinus sylvestris) chips to determine if varying pretreatment conditions on the original wood material were detectable via attenuated total reflectance (ATR) infrared spectroscopy. Pretreatment conditions varied with respect to temperature (130 °C and 150 °C) and treatment time (from 30 min to 120 min). The effects of the pretreatments on the composition of wood chips were determined by ATR infrared spectroscopy. The spectral data were compared to those determined by common wood chemistry analyses to evaluate the suitability of ATR spectroscopy method for rapid detection of changes in the wood chemical composition caused by different pretreatment conditions. In addition to determining wood species-dependent differences in the wood chemical composition, analytical results indicated that most essential lignin- and carbohydrates-related phenomena taking place during hot-water and acidic pretreatments could be described by applying this simple spectral method requiring only a small sample amount and sample preparation. Such information included, for example, the cleavage of essential lignin bonds (i.e., mainly β-O-4 linkages in guaiacyl and syringyl lignin) and formation of newly condensed lignin structures under different pretreatment conditions. Carbohydrate analyses indicated significant removal of hemicelluloses (especially hardwood xylan) and hemicelluloses-derived acetyl groups during the pretreatments, but they also confirmed the highly resistant nature of cellulose towards mild pretreatments.

Quantitative analysis of 39 polybrominated diphenyl ethers by isotope dilution GC/low-resolution MS.

Science.gov (United States)

Ackerman, Luke K; Wilson, Glenn R; Simonich, Staci L

2005-04-01

A GC/low-resolution MS method for the quantitative isotope dilution analysis of 39 mono- to heptabrominated diphenyl ethers was developed. The effects of two different ionization sources, electron impact (EI) and electron capture negative ionization (ECNI), and the effects of their parameters on production of high-mass fragment ions [M - xH - yBr](-) specific to PBDEs were investigated. Electron energy, emission current, source temperature, ECNI system pressure, and choice of ECNI reagent gases were optimized. Previously unidentified enhancement of PBDE high-mass fragment ion [M - xH - yBr](-) abundance was achieved. Electron energy had the largest impact on PBDE high-mass fragment ion abundance for both the ECNI and EI sources. By monitoring high-mass fragment ions of PBDEs under optimized ECNI source conditions, quantitative isotope dilution analysis of 39 PBDEs was conducted using nine (13)C(12) labeled PBDEs on a low-resolution MS with low picogram to femtogram instrument detection limits.

The analysis of uranium in environmental sample by mass spectrometer combined with isotopic dilution

International Nuclear Information System (INIS)

Fu Zhonghua; Jia Baoting; Han Jun

2003-01-01

Uranium in the environmental sample was analyzed by mass spectrometer combined with isotopic dilution. Before mass spectrometer analysis, samples were dissolved in a concentrated acidic solution containing HNO 3 , HF and HClO 4 and chemically processed to suit the analysis requirement. Analysis results indicated that the uranium content was 0.08 μg/g in river water, 0.1 μg/g in evergreen foliage, and 5-11 μg/g in surface soil respectively. (authors)

Pre-column dilution large volume injection ultra-high performance liquid chromatography-tandem mass spectrometry for the analysis of multi-class pesticides in cabbages.

Science.gov (United States)

Zhong, Qisheng; Shen, Lingling; Liu, Jiaqi; Yu, Dianbao; Li, Siming; Yao, Jinting; Zhan, Song; Huang, Taohong; Hashi, Yuki; Kawano, Shin-ichi; Liu, Zhaofeng; Zhou, Ting

2016-04-15

Pre-column dilution large volume injection (PD-LVI), a novel sample injection technique for reverse phase ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), was developed in this study. The PD-LVI UHPLC-MS/MS system was designed by slightly modifying the commercial UHPLC-MS/MS equipment with a mixer chamber. During the procedure of PD-LVI, sample solution of 200μL was directly carried by the organic mobile phase to the mixer and diluted with the aqueous mobile phase. After the mixture was introduced to the UHPLC column in a mobile phase of acetonitrile-water (15/85, v/v), the target analytes were stacked on the head of the column until following separation. Using QuEChERS extraction, no additional steps such as solvent evaporation or residue redissolution were needed before injection. The features of PD-LVI UHPLC-MS/MS system were systematically investigated, including the injection volume, the mixer volume, the precondition time and the gradient elution. The efficiency of this approach was demonstrated by direct analysis of 24 pesticides in cabbages. Under the optimized conditions, low limits of detection (0.00074-0.8 ng/kg) were obtained. The recoveries were in the range of 63.3-109% with relative standard deviations less than 8.1%. Compared with common UHPLC-MS/MS technique, PD-LVI UHPLC-MS/MS showed significant advantages such as excellent sensitivity and reliability. The mechanism of PD-LVI was demonstrated to be based on the column-head stacking effect with pre-column dilution. Based on the results, PD-LVI as a simple and effective sample injection technique of reverse phase UHPLC-MS/MS for the analysis of trace analytes in complex samples showed a great promising prospect. Copyright © 2016 Elsevier B.V. All rights reserved.

Error analysis of isotope dilution mass spectrometry method with internal standard

International Nuclear Information System (INIS)

Rizhinskii, M.W.; Vitinskii, M.Y.

1989-02-01

The computation algorithms of the normalized isotopic ratios and element concentration by isotope dilution mass spectrometry with internal standard are presented. A procedure based on the Monte-Carlo calculation is proposed for predicting the magnitude of the errors to be expected. The estimation of systematic and random errors is carried out in the case of the certification of uranium and plutonium reference materials as well as for the use of those reference materials in the analysis of irradiated nuclear fuels. 4 refs, 11 figs, 2 tabs

An analysis on boron dilution events during SBLOCA for the KNGR

International Nuclear Information System (INIS)

Kim, Young In; Hwang, Young Dong; Park, Jong Kuen; Chung, Young Jong; Sim, Suk Gu

1999-02-01

An analysis on boron dilution events during small break loss of coolant accident (LOCA) for Korea Next Generation Reactor (KNGR) was performed using Computational Fluid Dynamic (CFD) computer program FLUENT code. The maximum size of the water slug was determined based on the source of un borated water slug and the possible flow paths. Axisymmetric computational fluid dynamic analysis model is applied for conservative scoping analysis of un borated water slug mixing with recirculation water of the reactor system following small break LOCA assuming one Reactor Coolant Pump (RCP) restart. The computation grid was determined through the sensitivity study on the grid size, which calculates the most conservative results, and the preliminary calculation for boron mixing was performed using the grid. (Author). 17 refs., 3 tabs., 26 figs

Antimicrobial activity of grapefruit seed and pulp ethanolic extract.

Science.gov (United States)

Cvetnić, Zdenka; Vladimir-Knezević, Sanda

2004-09-01

Antibacterial and antifungal activity of ethanolic extract of grapefruit (Citrus paradisi Macf., Rutaceae) seed and pulp was examined against 20 bacterial and 10 yeast strains. The level of antimicrobial effects was established using an in vitro agar assay and standard broth dilution susceptibility test. The contents of 3.92% of total polyphenols and 0.11% of flavonoids were determined spectrometrically in crude ethanolic extract. The presence of flavanones naringin and hesperidin in the extract was confirmed by TLC analysis. Ethanolic extract exibited the strongest antimicrobial effect against Salmonella enteritidis (MIC 2.06%, m/V). Other tested bacteria and yeasts were sensitive to extract concentrations ranging from 4.13% to 16.50% (m/V).

Dual solid-phase and stir bar sorptive extraction combined with gas chromatography-mass spectrometry analysis provides a suitable tool for assaying limonene-derived mint aroma compounds in red wine.

Science.gov (United States)

Picard, Magali; Franc, Céline; de Revel, Gilles; Marchand, Stéphanie

2018-02-25

A novel analytical method was developed for quantitative determination of eight limonene-derived monoterpenes responsible for the mint aroma in red wine. As these aromatic compounds are present at trace levels, a new dual extraction approach was proposed, combining solid-phase extraction (SPE) and stir bar sorptive extraction (SBSE), followed by gas chromatography-mass spectrometry analysis. The various parameters affecting the efficiency of extracting the analytes from wine samples in both the SPE and SBSE steps were first investigated, to determine the best compromise for the simultaneous analysis of the compounds studied. Following preliminary optimization of the dilution factor, phase ratio, and methanol content in the SBSE sample, cartridge sorbent mass, type of solvent, elution volume, and wine sample volume in the pre-concentration SPE step were studied. Highest response values were obtained when a 90 mL wine sample was extracted on a 500 mg SPE C18 cartridge and eluted with 1.5 mL methanol. The wine extract was then diluted in 10 mL water to obtain a final methanol content of 15% before the SBSE step. Good linearity, repeatability, reproducibility, accuracy and the required low detection and quantification limits were obtained under the conditions described, making this SPE-SBSE combination a suitable, powerful tool for routine analysis of the selected limonene-derived mint aroma compounds in large series of wine samples. Finally, the validated method was applied to 15 commercial red Bordeaux wines, aged from 3 to 23 years. Most of the compounds studied, present within the ng.L -1 range, were easily quantified for the first time in wine. Copyright © 2017 Elsevier B.V. All rights reserved.

Stable isotope dilution analysis by thermal ionization mass spectrometry. Pt. 2

International Nuclear Information System (INIS)

Broekman, A.; Raaphorst, J.G. van

1984-01-01

The combination of stable isotope dilution analysis (SIDA) and thermal ionization mass spectrometry (TIMS) is in use for lead and uranium determination at milligram per kilogram levels for over 20 years. However, several other elements can also be determined accurately by SIDA/TIMS. In this study the determinations of cadmium and copper are described. Details of the digestion, electrochemical and ion-exchange separations and the loading of the elements on a filament are given. The advantages of the SIDA/TIMS technique are shown and illustrated with results for several certified reference materials. (orig.) [de

Two fixed ratio dilutions for soil salinity monitoring in hypersaline wetlands.

Directory of Open Access Journals (Sweden)

Juan Herrero

Full Text Available Highly soluble salts are undesirable in agriculture because they reduce yields or the quality of most cash crops and can leak to surface or sub-surface waters. In some cases salinity can be associated with unique history, rarity, or special habitats protected by environmental laws. Yet in considering the measurement of soil salinity for long-term monitoring purposes, adequate methods are required. Both saturated paste extracts, intended for agriculture, and direct surface and/or porewater salinity measurement, used in inundated wetlands, are unsuited for hypersaline wetlands that often are only occasionally inundated. For these cases, we propose the use of 1:5 soil/water (weight/weight extracts as the standard for expressing the electrical conductivity (EC of such soils and for further salt determinations. We also propose checking for ion-pairing with a 1:10 or more diluted extract in hypersaline soils. As an illustration, we apply the two-dilutions approach to a set of 359 soil samples from saline wetlands ranging in ECe from 2.3 dS m(-1 to 183.0 dS m(-1. This easy procedure will be useful in survey campaigns and in the monitoring of soil salt content.

Two fixed ratio dilutions for soil salinity monitoring in hypersaline wetlands.

Science.gov (United States)

Herrero, Juan; Weindorf, David C; Castañeda, Carmen

2015-01-01

Highly soluble salts are undesirable in agriculture because they reduce yields or the quality of most cash crops and can leak to surface or sub-surface waters. In some cases salinity can be associated with unique history, rarity, or special habitats protected by environmental laws. Yet in considering the measurement of soil salinity for long-term monitoring purposes, adequate methods are required. Both saturated paste extracts, intended for agriculture, and direct surface and/or porewater salinity measurement, used in inundated wetlands, are unsuited for hypersaline wetlands that often are only occasionally inundated. For these cases, we propose the use of 1:5 soil/water (weight/weight) extracts as the standard for expressing the electrical conductivity (EC) of such soils and for further salt determinations. We also propose checking for ion-pairing with a 1:10 or more diluted extract in hypersaline soils. As an illustration, we apply the two-dilutions approach to a set of 359 soil samples from saline wetlands ranging in ECe from 2.3 dS m(-1) to 183.0 dS m(-1). This easy procedure will be useful in survey campaigns and in the monitoring of soil salt content.

Determination of the genotoxic effects of Convolvulus arvensis extracts on corn (Zea mays L.) seeds.

Science.gov (United States)

Sunar, Serap; Yildirim, Nalan; Aksakal, Ozkan; Agar, Guleray

2013-06-01

In this research, the methanolic extracts of Convolvulus arvensis were tested for genotoxic and inhibitor activity on the total soluble protein content and the genomic template stability against corn Zea mays L. seed. The methanol extracts of leaf, stem and root of C. arvensis were diluted to 50, 75 and 100 μl concentrations and applied to corn seed. The total soluble protein and genomic template stability results were compared with the control. The results showed that especially 100 μl extracts of diluted leaf, stem and root had a strong inhibitory activity on the genomic template stability. The changes occurred in random amplification of polymorphic DNA (RAPD) profiles of C. arvensis extract treatment included variation in band intensity, loss of bands and appearance of new bands compared with control. Also, the results obtained from this study revealed that the increase in the concentrations of C. arvensis extract increased the total soluble protein content in maize. The results suggested that RAPD analysis and total protein analysis could be applied as a suitable biomarker assay for the detection of genotoxic effects of plant allelochemicals.

Do VCs use inside rounds to dilute founders? Some evidence from Silicon Valley

OpenAIRE

Fried, Jesse M.; Broughman, Brian J.

2012-01-01

In the bank-borrower setting, a firm’s existing lender may exploit its positional advantage to extract rents from the firm in subsequent financings. Analogously, a startup’s existing venture capital investors (VCs) may dilute the founder through a follow-on financing from these same VCs (an “inside” round) at an artificially low valuation. Using a hand-collected dataset of Silicon Valley startup firms, we find little evidence that VCs use inside rounds to dilute founders. Instead, our finding...

Automated gravimetric sample pretreatment using an industrial robot for the high-precision determination of plutonium by isotope dilution mass spectrometry

International Nuclear Information System (INIS)

Surugaya, Naoki; Hiyama, Toshiaki; Watahiki, Masaru

2008-01-01

A robotized sample-preparation method for the determination of Pu, which is recovered by extraction reprocessing of spent nuclear fuel, by isotope dilution mass spectrometry (IDMS) is described. The automated system uses a six-axis industrial robot, whose motility is very fast, accurate, and flexible, installed in a glove box. The automation of the weighing and dilution steps enables operator-unattended sample pretreatment for the high-precision analysis of Pu in aqueous solutions. Using the developed system, the Pu concentration in a HNO 3 medium was successfully determined using a set of subsequent mass spectrometric measurements. The relative uncertainty in determining the Pu concentration by IDMS using this system was estimated to be less than 0.1% (k=2), which is equal to that expected of a talented analysis. The operation time required was the same as that for a skilled operator. (author)

Thermal diffusion in dilute nanofluids investigated by photothermal interferometry

International Nuclear Information System (INIS)

Philip, J; Nisha, M R

2010-01-01

We have carried out a theoretical analysis of the dependence of the particle mass fraction on the thermal diffusivity of dilute suspensions of nanoparticles in liquids (dilute nanofluids). The analysis takes in to account adsorption of an ordered layer of solvent molecules around the nanoparticles. It is found that thermal diffusivity decreases with mass fraction for sufficiently small particle sizes. Beyond a critical particle size thermal diffusivity begins to increase with mass fraction for the same system. The results have been verified experimentally by measuring the thermal diffusivity of dilute suspensions of TiO 2 nanoparticles dispersed in polyvinyl alcohol (PVA) medium. The effect is attributed to Kapitza resistance of thermal waves in the medium.

Methylbutylmalonamide as an extractant for U(VI), Pu(IV), and Am(III)

International Nuclear Information System (INIS)

Nair, G.M.; Prabhu, D.R.; Mahajan, G.R.

1994-01-01

The unsymmetrical diamide methylbutylmalonamide has been synthesized and used in the extraction of U(VI), Pu(IV), and Am(III) in benzene medium. The distribution ratio for three cations was found to increase with increasing aqueous nitric acid concentration. U(VI) and Pu(IV) were found to be extracted as disolvates while Am(III) as a trisolvate. The thermodynamic parameters determined by the temperature variation method showed the extraction reactions to be mainly enthalphy-controlled. Am(III) was found to be back-extracted with dilute nitric acid, while Pu(IV) by dilute nitric acid - hydrofluoric acid mixture and U(VI) by dilute sodium carbonate solution. (author) 6 refs.; 3 figs.; 2 tabs

Analysis of structure and defects in thin silicon films deposited from hydrogen diluted silane

International Nuclear Information System (INIS)

Elzakker, G. van; Nadazdy, V.; Tichelaar, F.D.; Metselaar, J.W.; Zeman, M.

2006-01-01

Thin silicon layers have been deposited from silane diluted with hydrogen. The dilution ratio R (R = [H 2 ]/[SiH 4 ]) has been varied between R = 0 and R = 40. The structural properties of Si:H films have been studied using transmission electron microscopy imaging and Raman spectroscopy. The phase evolution from the amorphous phase into the mixed and eventually microcrystalline phase strongly depends on the hydrogen dilution. The initiation of the microcrystalline growth occurs between R = 20 and R = 25. The phase transition becomes more abrupt with increasing hydrogen dilution. Optoelectronic properties of the layers have been determined. Increasing hydrogen dilution results in films with increasing effective defect density and Urbach energy, which is related to inhomogeneous growth. The charge deep-level transient spectroscopy technique (Q-DLTS) was applied for the first time on hydrogen diluted thin silicon films in order to investigate the energy distribution of the defect states in these layers as a function of the dilution ratio R. The Q-DLTS spectra indicate a difference in defect-state distribution when the films evolve from the amorphous phase into the microcrystalline phase

Research on extraction of lithium from dilute solution

International Nuclear Information System (INIS)

Takeuchi, Takeji

1983-01-01

Lithium has been used as the refrigerant for air conditioning, the additive for aluminum refining and catalyzer and for high performance grease and small batteries so far. The demand in these existing uses has grown on the average 8.8 % yearly, accordingly the cumulative consumption is estimated to be 0.8 x 10 9 kg by 2000. It is expected that the lithium resources of 1 x 10 9 kg available by 2000 will be used up before the practical use of fusion reactors. Lithium is indispensable for generating tritium in fusion reactors. The lithium concentration in sea water is as thin as 0.2 g/m 3 , therefore it is necessary to develop the method of effectively extracting lithium from a large quantity of sea water. As one of the methods, it was found that the corrosion product of metallic aluminum was able to be utilized. Namely, when metallic aluminum such as foils is immersed in sea water, the corrosion product adheres on the surface, and this corrosion product extracts lithium by cation exchange process preferentially. In this method, the process of making an extracting agent is not necessary, and it is also unnecessary to control the condition of sea water. (Kako, I.)

Experimental design-based isotope-dilution SPME-GC/MS method development for the analysis of smoke flavouring products.

Science.gov (United States)

Giri, Anupam; Zelinkova, Zuzana; Wenzl, Thomas

2017-12-01

For the implementation of Regulation (EC) No 2065/2003 related to smoke flavourings used or intended for use in or on foods a method based on solid-phase micro extraction (SPME) GC/MS was developed for the characterisation of liquid smoke products. A statistically based experimental design (DoE) was used for method optimisation. The best general conditions to quantitatively analyse the liquid smoke compounds were obtained with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre, 60°C extraction temperature, 30 min extraction time, 250°C desorption temperature, 180 s desorption time, 15 s agitation time, and 250 rpm agitation speed. Under the optimised conditions, 119 wood pyrolysis products including furan/pyran derivatives, phenols, guaiacol, syringol, benzenediol, and their derivatives, cyclic ketones, and several other heterocyclic compounds were identified. The proposed method was repeatable (RSD% <5) and the calibration functions were linear for all compounds under study. Nine isotopically labelled internal standards were used for improving quantification of analytes by compensating matrix effects that might affect headspace equilibrium and extractability of compounds. The optimised isotope dilution SPME-GC/MS based analytical method proved to be fit for purpose, allowing the rapid identification and quantification of volatile compounds in liquid smoke flavourings.

Dynamic determination of kinetic parameters for the interaction between polypeptide hormones and cell-surface receptors in the perfused rat liver by the multiple-indicator dilution method

International Nuclear Information System (INIS)

Sato, H.; Sugiyama, Y.; Sawada, Y.; Iga, T.; Sakamoto, S.; Fuwa, T.; Hanano, M.

1988-01-01

Hepatic elimination of epidermal growth factor (EGF) via receptor-mediated endocytosis was studied by a multiple-indicator dilution method in the isolated perfused rat liver, in which cell polarity and spatial organization are maintained. In this method EGF was given with inulin, an extracellular reference, as a bolus into the portal vein, and dilution curves of both compounds in the hepatic vein effluent were analyzed. Analysis of the dilution curve for EGF, compared with that for somatostatin, which showed no specific binding to isolated liver plasma membranes, resulted as follows: (i) both extraction ratio and distribution volume of 125 I-labeled EGF decreased as the injected amount of unlabeled EGF increased; (ii) the ratio plot of the dilution curve for EGF exhibited an upward straight line initially for a short period of time, whereas the ratio plot of somatostatin gradually decreased. The multiple-indicator dilution method was used for other peptides also. Insulin and glucagon, known to have hepatocyte receptors, behaved similarly to EGF in shape of their ratio plots. The kinetic parameters calculated by this analysis were comparable with reported values obtained by in vitro direct binding measurements at equilibrium using liver homogenates. They conclude that the multiple-indicator dilution method is a good tool for analyzing the dynamics of peptide hormones-cell-surface receptor interaction under a condition in which spatial architecture of the liver is maintained

Quantification of fentanyl in serum by isotope dilution analysis using capillary gas chromatography

Energy Technology Data Exchange (ETDEWEB)

Sera, Shoji; Goromaru, Tsuyoshi [Fukuyama Univ., Hiroshima (Japan); Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki

1998-06-01

The quantitative determination of fentanyl (FT) in serum was examined by isotope dilution analysis using a capillary gas chromatograph equipped with a surface ionization detector. The separation of FT and its deuterated analogue, FT-{sup 2}H{sub 19}, was achieved within 15 min a column temperature of 260degC by using a 25 m column. Measurement of the samples prepared by the addition of a known amount of FT in the range of 0.2 to 40 ng/ml with 20 ng/ml of FT-{sup 2}H{sub 19} to human control serum allowed observation of a linear relationship between the peak area ratio and the added amount ratio. The correlation coefficient obtained by regression analysis was 0.999. The advantage of the present isotope dilution method was demonstrated by comparison with other FT analogues which substituted a propionyl group with an acetyl group or a phenethyl group with a benzyl group as the internal standard. The present method was used to determine the serum level of FT in surgical patients after i.v. administration. No endogenous compounds and concomitant drugs interfered with the detection of FT or FT-{sup 2}H{sub 19}. This method was considered to be useful for the pharmacokinetic study of FT in patients. (author)

Quantification of fentanyl in serum by isotope dilution analysis using capillary gas chromatography

International Nuclear Information System (INIS)

Sera, Shoji; Goromaru, Tsuyoshi; Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki

1998-01-01

The quantitative determination of fentanyl (FT) in serum was examined by isotope dilution analysis using a capillary gas chromatograph equipped with a surface ionization detector. The separation of FT and its deuterated analogue, FT- 2 H 19 , was achieved within 15 min a column temperature of 260degC by using a 25 m column. Measurement of the samples prepared by the addition of a known amount of FT in the range of 0.2 to 40 ng/ml with 20 ng/ml of FT- 2 H 19 to human control serum allowed observation of a linear relationship between the peak area ratio and the added amount ratio. The correlation coefficient obtained by regression analysis was 0.999. The advantage of the present isotope dilution method was demonstrated by comparison with other FT analogues which substituted a propionyl group with an acetyl group or a phenethyl group with a benzyl group as the internal standard. The present method was used to determine the serum level of FT in surgical patients after i.v. administration. No endogenous compounds and concomitant drugs interfered with the detection of FT or FT- 2 H 19 . This method was considered to be useful for the pharmacokinetic study of FT in patients. (author)

Mercury speciation analysis in seafood by species-specific isotope dilution: method validation and occurrence data

Energy Technology Data Exchange (ETDEWEB)

Clemens, Stephanie; Guerin, Thierry [Agence Nationale de Securite Sanitaire de l' Alimentation, Laboratoire de Securite des Aliments de Maisons-Alfort, Unite des Contaminants Inorganiques et Mineraux de l' Environnement, ANSES, Maisons-Alfort (France); Monperrus, Mathilde; Donard, Olivier F.X.; Amouroux, David [IPREM UMR 5254 CNRS - Universite de Pau et des Pays de l' Adour, Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, Institut des Sciences Analytiques et de Physico-chimie pour l' Environnement et les Materiaux, Pau Cedex (France)

2011-11-15

Methylmercury (MeHg) and total mercury (THg) in seafood were determined using species-specific isotope dilution analysis and gas chromatography combined with inductively coupled plasma mass spectrometry. Sample preparation methods (extraction and derivation step) were evaluated on certified reference materials using isotopically enriched Hg species. Solid-liquid extraction, derivation by propylation and automated agitation gave excellent accuracy and precision results. Satisfactory figures of merit for the selected method were obtained in terms of limit of quantification (1.2 {mu}g Hg kg{sup -1} for MeHg and 1.4 {mu}g Hg kg{sup -1} for THg), repeatability (1.3-1.7%), intermediate precision reproducibility (1.5% for MeHg and 2.2% for THg) and trueness (bias error less than 7%). By means of a recent strategy based on accuracy profiles ({beta}-expectation tolerance intervals), the selected method was successfully validated in the range of approximately 0.15-5.1 mg kg{sup -1} for MeHg and 0.27-5.2 mg kg{sup -1} for THg. Probability {beta} was set to 95% and the acceptability limits to {+-}15%. The method was then applied to 62 seafood samples representative of consumption in the French population. The MeHg concentrations were generally low (1.9-588 {mu}g kg{sup -1}), and the percentage of MeHg varied from 28% to 98% in shellfish and from 84% to 97% in fish. For all real samples tested, methylation and demethylation reactions were not significant, except in one oyster sample. The method presented here could be used for monitoring food contamination by MeHg and inorganic Hg in the future to more accurately assess human exposure. (orig.)

Field ionization mass spectrometry (FIMS) applied to tracer studies and isotope dilution analysis

International Nuclear Information System (INIS)

Anbar, M.; Heck, H.d'A.; McReynolds, J.H.; St John, G.A.

1975-01-01

The nonfragmenting nature of field ionization mass spectrometry makes it a preferred technique for the isotopic analysis of multilabeled organic compounds. The possibility of field ionization of nonvolatile thermolabile materials significantly extends the potential uses of this technique beyond those of conventional ionization methods. Multilabeled tracers may be studied in biological systems with a sensitivity comparable to that of radioactive tracers. Isotope dilution analysis may be performed reliably by this technique down to picogram levels. These techniques will be illustrated by a number of current studies using multilabeled metabolites and drugs. The scope and limitations of the methodology are discussed

Determination of the interchangeable heavy-metal fraction in soils by isotope dilution mass spectrometry

International Nuclear Information System (INIS)

Gaebler, H.E.; Bahr, A.; Mieke, B.

1999-01-01

An isotope dilution technique using enriched stable isotopes is applied to determine the interchangeable heavy-metal fraction in soils. Metals in two soil samples are extracted at constant pH, with water, NH 4 NO 3 , and EDTA. A spike of enriched stable isotopes is added to the suspension of sample and eluant at the beginning of the extraction. The heavy-metal fraction which exchanges with the added spike during the extraction is called the interchangeable fraction. The extractable heavy-metal fractions are obtained from the heavy-metal concentrations in the eluates. Isotope ratios and concentrations are determined by HR-ICP-MS. The isotope dilution technique described enables both the extractable and the interchangeable heavy-metal fractions to be determined in the same experiment. The combination of both results gives additional information on elemental availability under different conditions that cannot be obtained by analyzing the extractable heavy-metal fractions alone. It is demonstrated that in some cases different eluants just shift the distribution of the interchangeable fraction of an element between the solid and liquid phases (e.g., Pb and Cd in a topsoil sample) while the amount of the interchangeable fraction itself remains constant. For other elements, as Ni, Zn, and Cr, the use of different eluants (different pH, complexing agents) sometimes enlarges the interchangeable fraction. (orig.)

Determination of the alkylpyrazine composition of coffee using stable isotope dilution-gas chromatography-mass spectrometry (SIDA-GC-MS).

Science.gov (United States)

Pickard, Stephanie; Becker, Irina; Merz, Karl-Heinz; Richling, Elke

2013-07-03

A stable isotope dilution analysis based on gas chromatography-mass spectrometry analysis (SIDA-GC-MS) was developed for the quantitative analysis of 12 alkylpyrazines found in commercially available coffee samples. These compounds contribute to coffee flavor. The accuracy of this method was tested by analyzing model mixtures of alkylpyrazines. Comparisons of alkylpyrazine-concentrations suggested that water as extraction solvent was superior to dichloromethane. The distribution patterns of alkylpyrazines in different roasted coffees were quite similar. The most abundant alkylpyrazine in each coffee sample was 2-methylpyrazine, followed by 2,6-dimethylpyrazine, 2,5-dimethylpyrazine, 2-ethylpyrazine, 2-ethyl-6-methylpyrazine, 2-ethyl-5-methylpyrazine, and 2,3,5-trimethylpyrazine, respectively. Among the alkylpyrazines tested, 2,3-dimethylpyrazine, 2-ethyl-3-methylpyrazine, 2-ethyl-3,6-dimethylpyrazine, and 2-ethyl-3,5-dimethylpyrazine revealed the lowest concentrations in roasted coffee. By the use of isotope dilution analysis, the total concentrations of alkylpyrazines in commercially available ground coffee ranged between 82.1 and 211.6 mg/kg, respectively. Decaffeinated coffee samples were found to contain lower amounts of alkylpyrazines than regular coffee samples by a factor of 0.3-0.7, which might be a result of the decaffeination procedure.

Comparison between isotope dilution and activation analysis as a method for determining the macro content of mercury

International Nuclear Information System (INIS)

Soedyartomo; Sunoko, S.R.

1975-01-01

It is true that the mercury content in the environment should be measured accurately because of its toxicity even at levels of microgram order. The assessment of hazards due to environmental contamination with mercury is based on the results of the metal analysis in a number of different samples. Consequently, the study of the character of analytical methods used, i.e. their accuracy, precision, sensitivity, etc. is essential. A brief description on the microanalysis methods of mercury as given. The discussion of the results obtained from analysing some sludge and water by means of isotope dilution and destructive thermal neutron activation analysis is also presented. It is found that both methods are suitable for routine work. It can be concluded that the isotope dilution method has some advantages. It is more simple, more sensitive, more rapid, and has lower radiation hazard. (author)

Aroma extraction dilution analysis of Sauternes wines. Key role of polyfunctional thiols.

Science.gov (United States)

Bailly, Sabine; Jerkovic, Vesna; Marchand-Brynaert, Jacqueline; Collin, Sonia

2006-09-20

The aim of the present work was to investigate Sauternes wine aromas. In all wine extracts, polyfunctional thiols were revealed to have a huge impact. A very strong bacon-petroleum odor emerged at RI = 845 from a CP-Sil5-CB column. Two thiols proved to participate in this perception: 3-methyl-3-sulfanylbutanal and 2-methylfuran-3-thiol. A strong synergetic effect was evidenced between the two compounds. The former, never mentioned before in wines, and not found in the musts of this study, is most probably synthesized during fermentation. 3-Methylbut-2-ene-1-thiol, 3-sulfanylpropyl acetate, 3-sulfanylhexan-1-ol, and 3-sulfanylheptanal also contribute to the global aromas of Sauternes wines. Among other key odorants, the presence of a varietal aroma (alpha-terpineol), sotolon, fermentation alcohols (3-methylbutan-1-ol and 2-phenylethanol) and esters (ethyl butyrate, ethyl hexanoate, and ethyl isovalerate), carbonyls (trans-non-2-enal and beta-damascenone), and wood flavors (guaiacol, vanillin, eugenol, beta-methyl-gamma-octalactone, and Furaneol) is worth stressing.

Large datasets: Segmentation, feature extraction, and compression

Energy Technology Data Exchange (ETDEWEB)

Downing, D.J.; Fedorov, V.; Lawkins, W.F.; Morris, M.D.; Ostrouchov, G.

1996-07-01

Large data sets with more than several mission multivariate observations (tens of megabytes or gigabytes of stored information) are difficult or impossible to analyze with traditional software. The amount of output which must be scanned quickly dilutes the ability of the investigator to confidently identify all the meaningful patterns and trends which may be present. The purpose of this project is to develop both a theoretical foundation and a collection of tools for automated feature extraction that can be easily customized to specific applications. Cluster analysis techniques are applied as a final step in the feature extraction process, which helps make data surveying simple and effective.

Hybridizing pines with diluted pollen

Science.gov (United States)

Robert Z. Callaham

1967-01-01

Diluted pollens would have many uses by the tree breeder. Dilutions would be particularly advantageous in making many controlled pollinations with a limited amount of pollen. They also would be useful in artificial mass pollinations of orchards or single trees. Diluted pollens might help overcome troublesome genetic barriers to crossing. Feasibility o,f using diluted...

Passive vapor extraction feasibility study

International Nuclear Information System (INIS)

Rohay, V.J.

1994-01-01

Demonstration of a passive vapor extraction remediation system is planned for sites in the 200 West Area used in the past for the disposal of waste liquids containing carbon tetrachloride. The passive vapor extraction units will consist of a 4-in.-diameter pipe, a check valve, a canister filled with granular activated carbon, and a wind turbine. The check valve will prevent inflow of air that otherwise would dilute the soil gas and make its subsequent extraction less efficient. The granular activated carbon is used to adsorb the carbon tetrachloride from the air. The wind turbine enhances extraction rates on windy days. Passive vapor extraction units will be designed and operated to meet all applicable or relevant and appropriate requirements. Based on a cost analysis, passive vapor extraction was found to be a cost-effective method for remediation of soils containing lower concentrations of volatile contaminants. Passive vapor extraction used on wells that average 10-stdft 3 /min air flow rates was found to be more cost effective than active vapor extraction for concentrations below 500 parts per million by volume (ppm) of carbon tetrachloride. For wells that average 5-stdft 3 /min air flow rates, passive vapor extraction is more cost effective below 100 ppm

Third phase formation in organic solutions in the extraction of mono-acids by tertiary trialcoyl-amines diluted in very slightly polar organic solvents

International Nuclear Information System (INIS)

Robaglia, Michele

1973-01-01

The phenomena of third phase formation which can occur during the extraction of an acid with a tertiary amine diluted in a low polarity diluent are studied. In the first part a system including water (TnOA - C 6 H 12 - HCl - H 2 O) is compared with an anhydrous system (TnOA - C 6 H 12 - HCl - N 2 ). There are two kinds of gaps. One during amine salification, another one during the extraction of excess acid. The important part of the water content of the organic phase is demonstrated. The presence of water enhances the gaps. The polar water molecules are dissolved inside the tri-octylamine salt micelles. The heavy phase is formed by aggregates, the light phase represents the solubility of the non soluble species in the medium. In the second part are studied the influence of some parameters (like nature of diluent, acid, amine and temperature) on the gaps formation and on the extraction of excess acid and water. In every cases the part played by water remains the same. Finally some comparisons are made between tertiary systems and binary systems which formed them. The binary systems were studied by the mean of crystallization curves. (author) [fr

Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

International Nuclear Information System (INIS)

Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young

2005-01-01

A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties

Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

2005-03-15

A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

Evaluation of matrix effect in isotope dilution mass spectrometry based on quantitative analysis of chloramphenicol residues in milk powder

International Nuclear Information System (INIS)

Li, Xiu Qin; Yang, Zong; Zhang, Qing He; Li, Hong Mei

2014-01-01

Graphical abstract: -- Highlights: •We develop a strategy to evaluate matrix effect and its impact on the IDMS results. •Matrix effect and IDMS correction factor from different conditions are evaluated. •Ion suppression effect is observed in LLE and HLB pre-treated sample solutions. •Ion enhancement effect is found in MCX pre-treated sample solution. •IDMS correction factor in HLB and MCX solutions in three instruments is close to 1 -- Abstract: In the present study, we developed a comprehensive strategy to evaluate matrix effect (ME) and its impact on the results of isotope dilution mass spectrometry (IDMS) in analysis of chloramphenicol (CAP) residues in milk powder. Stable isotope-labeled internal standards do not always compensate ME, which brings the variation of the ratio (the peak area of analyte/the peak area of isotope). In our investigation, impact factors of this variation were studied in the extraction solution of milk powder using three mass spectrometers coupled with different ion source designs, and deuterium-labeled chloramphenicol (D5-CAP) was used as the internal standard. ME from mobile phases, sample solvents, pre-treatment methods, sample origins and instruments was evaluated, and its impact on the results of IDMS was assessed using the IDMS correction factor (θ). Our data showed that the impact of ME of mobile phase on the correction factor was significantly greater than that of sample solvent. Significant ion suppression and enhancement effects were observed in different pre-treated sample solutions. The IDMS correction factor in liquid–liquid extraction (LLE) and molecular imprinted polymer (MIP) extract with different instruments was greater or less 1.0, and the IDMS correction factor in hydrophilic lipophilic balance (HLB) and mix-mode cation exchange (MCX) extract with different instruments was all close to 1.0. To the instrument coupled with different ion source design, the impact of ME on IDMS quantitative results was

Development of an extraction method for perchlorate in soils.

Science.gov (United States)

Cañas, Jaclyn E; Patel, Rashila; Tian, Kang; Anderson, Todd A

2006-03-01

Perchlorate originates as a contaminant in the environment from its use in solid rocket fuels and munitions. The current US EPA methods for perchlorate determination via ion chromatography using conductivity detection do not include recommendations for the extraction of perchlorate from soil. This study evaluated and identified appropriate conditions for the extraction of perchlorate from clay loam, loamy sand, and sandy soils. Based on the results of this evaluation, soils should be extracted in a dry, ground (mortar and pestle) state with Milli-Q water in a 1 ratio 1 soil ratio water ratio and diluted no more than 5-fold before analysis. When sandy soils were extracted in this manner, the calculated method detection limit was 3.5 microg kg(-1). The findings of this study have aided in the establishment of a standardized extraction method for perchlorate in soil.

Comparison of extraction fluids used with contaminated soils

International Nuclear Information System (INIS)

Erickson, D.C.; White, E.; Loehr, R.C.

1991-01-01

Five separate solutions were evaluated for use as leaching fluids with soils containing petroleum refining waste residues. The extraction fluids were: (a) water, (b) dilute hydrochloric acid, (c) 0.05 molar EDTA, (d) acetate buffer and (e) a dilute sulfuric/nitric acid mixture. The soils were collected from former refinery land treatment sites which had been used to treat petroleum refining wastes. The extractions were performed using a rotary tumbler (30 RPM, 18 hours) and the resulting solutions were analyzed for polynuclear aromatic hydrocarbons (PAHs) and metals. Concentrations of the PAHs in each of the five solutions were near or below the analytical quantitation limits. Metal concentrations were highest in the HCL and EDTA extracts, although only a small fraction of the total available metal present in the soils was extracted by the solutions evaluated

Isotope Dilution - Thermal Ionisation Mass Spectrometric Analysis for Tin in a Fly Ash Material; Analisis de Estano en una Ceniza de Combustion mediante Espectrometria de Masas de Ionizacion Termica con Dilucion Isotopica

Energy Technology Data Exchange (ETDEWEB)

Hernandez, C; Fernandez, M; Quejido, A L

2006-07-01

Isotope dilution-thermal ionisation mass spectrometry (ID-TIMS) analysis has been applied to the determination of tin in a fly ash sample supplied by the EC Joint Research Centre (Ispra, Italy). The proposed procedure includes the silica gel/phosphoric acid technique for tin thermal ionisation activation and a strict heating protocol for isotope ratio measurements. Instrumental mass discrimination factor has been previously determined measuring a natural tin standard solution. Spike solutions has been prepared from 112Sn-enriched metal and quantified by reverse isotope dilution analysis. Two sample aliquots were spiked and tin was extracted with 4,5 M HCI during 25 min ultrasound exposure time. Due to the complex matrix of this fly ash material, a two-step purification stage using ion-exchange chromatography was required prior TIMS analysis. Obtained results for the two sample-spike blends (10,10 + - 0,55 y 10,50 + - 0,64 imolg-1) are comprarable, both value and uncertainty. Also a good reproducibility is observed between measurements. The proposed ID-TIMS procedure, as a primary method and due to the lack of fly ash reference material certified for tin content, can be used to validate more routine methodologies applied to tin determination in this kind of materials. (Author) 75 refs.

Radioisotope dilution technique for determination of vitamin B12 in foods

International Nuclear Information System (INIS)

Casey, P.J.; Speckman, K.R.; Ebert, F.J.; Hobbs, W.E.

1982-01-01

A radioisotope dilution (RID) method for the determination of vitamin B 12 is presented. The method combines a standard extraction procedure (AOAC 43.108, 12th ed.) with a commercially available RID assay kit. The method was evaluated on a wide range of fortified and unfortified food products. Recovery studies on both groups yielded average recoveries of 98.1 and 95.8%, respectively. Reproducibility data generated from replicate analysis on both groups gave a relative standard deviation of 6.9% for the fortified group and 9.2% for the unfortified group. For the samples studied, the mean vitamin B 12 content determined by the RID method was 8.01 μ/100 g vs a mean of 7.54 μg/100 g by the AOAC microbiological method; the correlation coefficient was r = 0.983

Titanium leaching from red mud by diluted sulfuric acid at atmospheric pressure

International Nuclear Information System (INIS)

Agatzini-Leonardou, S.; Oustadakis, P.; Tsakiridis, P.E.; Markopoulos, Ch.

2008-01-01

Laboratory-scale research has focused on the recovery of titanium from red mud, which is obtained from bauxite during the Bayer process for alumina production. The leaching process is based on the extraction of this element with diluted sulfuric acid from red mud under atmospheric conditions and without using any preliminary treatment. Statistical design and analysis of experiments were used, in order to determine the main effects and interactions of the leaching process factors, which were: acid normality, temperature and solid to liquid ratio. The titanium recovery efficiency on the basis of red mud weight reached 64.5%. The characterization of the initial red mud, as well as this of the leached residues was carried out by X-ray diffraction, TG-DTA and scanning electron microscopy

Cadmium determination in natural waters at the limit imposed by European legislation by isotope dilution and TiO2 solid-phase extraction.

Science.gov (United States)

García-Ruiz, Silvia; Petrov, Ivan; Vassileva, Emilia; Quétel, Christophe R

2011-11-01

The cadmium content in surface water is regulated by the last European Water Framework Directive to a maximum between 0.08 and 0.25 μg L(-1) depending on the water type and hardness. Direct measurement of cadmium at this low level is not straightforward in real samples, and we hereby propose a validated method capable of addressing cadmium content below μg L(-1) level in natural water. It is based on solid-phase extraction using TiO(2) nanoparticles as solid sorbent (0.05 g packed in mini-columns) to allow the separation and preconcentration of cadmium from the sample, combined to direct isotope dilution and detection by inductively coupled plasma mass spectrometry (ID-ICP-MS). The extraction setup is miniaturised and semi-automated to reduce risks of sample contamination and improve reproducibility. Procedural blanks for the whole measurement process were 5.3 ± 2.8 ng kg(-1) (1 s) for 50 g of ultrapure water preconcentrated ten times. Experimental conditions influencing the separation (including loading pH, sample flow rates, and acid concentration in the eluent) were evaluated. With isotope dilution the Cd recovery rate does not have to be evaluated carefully. Moreover, the mathematical model associated to IDMS is known, and provides transparency for the uncertainty propagation. Our validation protocol was in agreement with guidelines of the ISO/IEC 17025 standard (chapter 5.4.5). Firstly, we assessed the experimental factors influencing the final result. Secondly, we compared the isotope ratios measured after our separation procedure to the reference values obtained with a different protocol for the digested test material IMEP-111 (mineral feed). Thirdly, we analysed the certified reference material BCR-609 (groundwater). Finally, combined uncertainties associated to our results were estimated according to ISO-GUM guidelines (typically, 3-4% k = 2 for a cadmium content of around 100 ng kg(-1)). We applied the developed method to the groundwater and wastewater

Selective Liquid-Liquid Extraction of Lead Ions Using Newly Synthesized Extractant 2-(Dibutylcarbamoylbenzoic Acid

Directory of Open Access Journals (Sweden)

Hossein Soltani

2015-12-01

Full Text Available A new carboxylic acid extractant, named 2-(dibutylcarbamoylbenzoic acid, is prepared and its potential for selective solvent extraction and recovery of lead ions from industrial samples was investigated. The slope analysis indicated that the lead ions are extracted by formation of 1:2 metal to ligand complexes. The effect of the parameters influencing the extraction efficiency including kind of the organic diluent, extractant concentration, type of the salt used for ionic strength adjustment, contact time and temperature was evaluated and discussed. Under optimized conditions (aqueous phase: 5 ml, initial lead concentration 1 × 10-4 M, pH 4, sodium chloride 0.1 M; organic phase: 5 ml dichloromethane, ligand concentration 0.05 M, a quantitative (75.2 ± 0.8% and highly selective extraction of lead ions in the presence of zinc, nickel, cobalt and cadmium ions (each 1 × 10-4 M was achieved, after 20 min. magnetically stirring of the phases, at      25 °C. The extracted lead ions were stripped from the organic phase by diluted nitric acid (0.1 M solution. The proposed method was successfully applied for separation of lead from industrial samples. The study of the effect of temperature allowed evaluating the thermodynamic parameters of the extraction process of lead ions by the studied extractant into dichloromethane.

IDMS of FeO(OH) extracted from blood digests for studies of iron metabolism in humans

International Nuclear Information System (INIS)

Vieira, N.E.; Yergey

1996-01-01

The following isolation procedures were used for the determination of iron in water and digested whole blood matrices in connection with isotope dilution mass spectrometry (IDMS) of iron in blood for metabolic studies: precipitation as hydroxide, ion exchange chromatography using membrane filters, and evaporation of the untreated matrix followed by extraction of the residue with dilute acid. Although recovery is better with the cation exchange techniques, overall precision of IDMS analysis favours direct precipitation, which is also simpler and quicker. 3 refs., 3 tabs

Extraction of thorium from solution using tribenzylamine

International Nuclear Information System (INIS)

Whitehead, N.E.; Ditchburn, R.G.

1975-01-01

A method is described for isolating thorium from solutions in a state sufficiently pure for alpha spectroscopy. It parallels the method described by Moore and Thern (Radiochemical Radioanalytical Letters 19(2), 117-125, 1974), but uses tribenzylamine instead of Adogen 364. The method involves extracting thorium from a solution in 8M nitric acid, into a 6% w/v solution of tribenzylamine in toluene. The thorium is concentrated in a third, interfacial layer which forms. This layer is isolated, diluted with chloroform, and back extracted with 10M HC1. Overall yields range between 83 and 90% for one extraction. The acidic solution is taken down to near dryness, diluted until the pH is 2 and extracted into 1.2 ml of thenoyltrifluoroacetone in toluene. This solution is evaporated onto a stainless steel disk, flamed, and the disk may be used for alpha spectroscopy of thorium isotopes. (auth.)

EXAFS of dilute systems: fluorescence detection

International Nuclear Information System (INIS)

Hastings, J.B.

1979-01-01

Since the first observations of the variation of the absorption coefficient for x-rays above the energy thresholds in the thirties until the early seventies, measurements and analysis of these variations were merely intended for the understanding of the underlying physics. Recently, with the understanding of the information available about the local atomic structure in the neighborhood of the absorbing species and the availability of high intensity synchrotron radiation sources, EXAFS has become a powerful structural tool. In these discussions, the details of the measurements for very dilute species are presented. It is shown that for the more dilute systems the measurement of the emission rather than the direct absorption is a more favorable technique

Forms of vitamin B12 in radioisotope dilution assays

International Nuclear Information System (INIS)

Begley, J.A.; Hall, C.A.

1981-01-01

Since the presence of analogues of vitamin B 12 (B 12 , cobalamin, Cbl) has been postulated as the basis for the high values obtained by some radioisotope dilution assays (RIDA) of serum Cbl, serum was examined for analogues. None could be demonstrated in the extracts of serum prepared for RIDA as sought by both direct and indirect techniques. The natural forms of serum Cbl were converted to cyanocobalamin (CN Cbl) by this process of extraction which included cyanide (CN). The correctly performed RIDA for Cbl based on R binder gave higher values than a RIDA based on intrinsic factor or than by bioassay. By exclusion, the difference appeared to be due to unidentified factors rather than the presence of analogues. (author)

Determination of microquantities of silver in platinum by isotope dilution

International Nuclear Information System (INIS)

Yedinakova, V.; Sladkovska, Y.

1980-01-01

A method is described for determining microquantities of silver in platinum. It is based on isotope dilution by means of substoichiometric extraction of dithizonates with carbon tetrachloride. The determination of silver according to this technique is not interfered by zinc or gold in quantities exceeding the silver content by one order of magnitude nor by a great excess of platinum. In the presence of copper the addition of complexon is necessary. (author)

Chromatographic analysis of wheatgrass extracts

Directory of Open Access Journals (Sweden)

Masood Shah Khan

2015-01-01

Full Text Available Aim: Wheatgrass (WG is the shoot of Triticum aestivum Linn. belongs to the family Gramineae, and possess high chlorophyll content and essential vitamins, minerals, vital enzymes, amino acids, dietary fibers etc., It has been shown to possess anti-cancer, anti-ulcer, antioxidant, and anti-arthritic activity due to the presence of biologically active compounds, and minerals. Therefore, in the present study, high-performance thin layer chromatography (HPTLC, and high-performance liquid chromatography (HPLC methods for qualitative and quantitative analysis have been proposed, which will help in quality evaluation of wheat grass extract. Materials and Methods: Samples for analysis were prepared in methanol and water simply by sonication. These were applied on pre-coated silica plate and chromatograms were developed using toluene: Ethyl acetate: Formic acid. HPLC analysis was done on Waters HPLC system using water, methanol, and acetonitrile as mobile phase. Merck C18 column has been used. Results: HPTLC finger printing of alcoholic extracts of WG was carried out and found 10–11 spots at different wavelengths 254, 366, and 435 nm. HPLC fingerprinting produced 22 peaks at 256 nm. Quantitative HPTLC analysis was done to determine the gallic acid content, and was found to be 0.077% w/w in aqueous extract. By HPLC, the content of gallic acid and rutin was found to be 0.07%, and 0.04% w/w in aqueous extract of WG. Conclusion: The developed HPLC and HPTLC fingerprinting method can be used for the quality control, and standardization of WG and its extracts used as nutritional supplement.

Aqueous Extracts of Hibiscus sabdariffa Calyces to Control Aichi Virus.

Science.gov (United States)

D'Souza, Doris H; Dice, Lezlee; Davidson, P Michael

2016-06-01

Aqueous Hibiscus sabdariffa extracts possess antimicrobial properties with limited information available on their antiviral effects. Aichi virus (AiV) is an emerging foodborne pathogen that causes gastroenteritis. Vaccines are currently unavailable to prevent their disease transmission. The objective of this study was to determine the antiviral effects of aqueous H. sabdariffa extracts against AiV. AiV at ~5 log PFU/ml was incubated with undiluted (200 mg/ml), 1:1 (100 mg/ml) or 1:5 (40 mg/ml) diluted aqueous hibiscus extract (pH 3.6), phosphate-buffered saline (pH 7.2 as control), or malic acid (pH 3.0, acid control) at 37 °C over 24 h. Treatments were stopped by serially diluting in cell-culture media containing fetal bovine serum and titers were determined using plaque assays on confluent Vero cells. Each treatment was replicated thrice and assayed in duplicate. AiV did not show any significant reduction with 1:1 (100 mg/ml) or 1:5 (40 mg/ml) diluted aqueous hibiscus extracts or malic acid after 0.5, 1, or 2 h at 37 °C. However, AiV titers were reduced to non-detectable levels after 24 h with all the three tested concentrations, while malic acid showed only 0.93 log PFU/ml reduction after 24 h. AiV was reduced by 0.5 and 0.9 log PFU/ml with undiluted extracts (200 mg/ml) after 2 and 6 h, respectively. AiV treated with 1:1 (100 mg/ml) and 1:5 (40 mg/ml) diluted extracts showed a minimal ~0.3 log PFU/ml reduction after 6 h. These extracts show promise to reduce AiV titers mainly through alteration of virus structure, though higher concentrations may have improved effects.

In vitro antibacterial effect of Withania somnifera root extract on Escherichia coli

Science.gov (United States)

Kumari, Mamta; Gupta, R. P.

2015-01-01

Aim: The aim was to investigate antibacterial activity of Withania somnifera (Ashwagandha), an Indian traditional medicinal plant against Escherichia coli O78, a pathogenic strain. Materials and Methods: Two-fold serial dilutions of 20% aqueous W. somnifera root (WSR) extract were inoculated with E. coli O78 @ 1*107 colony forming units grown in nutrient broth. Following inoculation, turbidity optical density was measured by spectrophotometer at 600 nm in all the tubes at 0, 2, 4, 6 and 8 h of incubation at 37°C. Result: The results revealed that the maximum inhibition of bacterial growth was observed at 1:8 dilution of WSR extract. The highest dilution of the extract that showed inhibited growth of the test organism when compared with control was 1:16. Therefore, the minimum inhibitory concentration of aqueous extract of WSR is 1:16. Conclusion: It is concluded that WSR possessed good antibacterial activity, confirming the great potential of bioactive compounds and its rationalizing use in health care. PMID:27046997

Extraction, separation, and detections of 14C-diazepam and 14C-metabolites from brain tissue of mature and old rats

International Nuclear Information System (INIS)

Komiskey, H.L.; Rahman, A.; Weisenburger, W.P.; Hayton, W.L.; Zobrist, R.H.; Silvius, W.

1985-01-01

A rapid method for simultaneous determination of brain concentrations of diazepan and each of its three major metabolites in brain tissue by a reverse isotope dilution procedure is presented. Radiolabeled diazepam and metabolites were extracted from brain tissue of mature and senescent rats with ethyl ether. After the ether was evaporated the benzodiazepines were separated from the residue by passing the water soluble portion through C-18 bonded-phase extraction columns. High pressure liquid chromatography (HPLC) was used to separate the benzodiazepines from each other. Reverse isotope dilution analysis was used to quantify diazepam and its metabolites. The percent recovery of diazepam and its metabolites from the brain of mature or senescent rats did not vary significantly

Fast and accurate calculation of dilute quantum gas using Uehling–Uhlenbeck model equation

Energy Technology Data Exchange (ETDEWEB)

Yano, Ryosuke, E-mail: ryosuke.yano@tokiorisk.co.jp

2017-02-01

The Uehling–Uhlenbeck (U–U) model equation is studied for the fast and accurate calculation of a dilute quantum gas. In particular, the direct simulation Monte Carlo (DSMC) method is used to solve the U–U model equation. DSMC analysis based on the U–U model equation is expected to enable the thermalization to be accurately obtained using a small number of sample particles and the dilute quantum gas dynamics to be calculated in a practical time. Finally, the applicability of DSMC analysis based on the U–U model equation to the fast and accurate calculation of a dilute quantum gas is confirmed by calculating the viscosity coefficient of a Bose gas on the basis of the Green–Kubo expression and the shock layer of a dilute Bose gas around a cylinder.

Cadmium determination in natural waters at the limit imposed by European legislation by isotope dilution and TiO{sub 2} solid-phase extraction

Energy Technology Data Exchange (ETDEWEB)

Garcia-Ruiz, Silvia; Quetel, Christophe R. [Institute for Reference Materials and Measurements, Joint Research Centre - European Commission, Geel (Belgium); Petrov, Ivan [Institute for Reference Materials and Measurements, Joint Research Centre - European Commission, Geel (Belgium); Universite Libre de Bruxelles, Department of Earth and Environmental Sciences, Brussels (Belgium); Vassileva, Emilia [Institute for Reference Materials and Measurements, Joint Research Centre - European Commission, Geel (Belgium); IAEA-Marine Environment Laboratories, Monaco (Monaco)

2011-11-15

The cadmium content in surface water is regulated by the last European Water Framework Directive to a maximum between 0.08 and 0.25 {mu}g L{sup -1} depending on the water type and hardness. Direct measurement of cadmium at this low level is not straightforward in real samples, and we hereby propose a validated method capable of addressing cadmium content below {mu}g L{sup -1} level in natural water. It is based on solid-phase extraction using TiO{sub 2} nanoparticles as solid sorbent (0.05 g packed in mini-columns) to allow the separation and preconcentration of cadmium from the sample, combined to direct isotope dilution and detection by inductively coupled plasma mass spectrometry (ID-ICP-MS). The extraction setup is miniaturised and semi-automated to reduce risks of sample contamination and improve reproducibility. Procedural blanks for the whole measurement process were 5.3 {+-} 2.8 ng kg{sup -1} (1 s) for 50 g of ultrapure water preconcentrated ten times. Experimental conditions influencing the separation (including loading pH, sample flow rates, and acid concentration in the eluent) were evaluated. With isotope dilution the Cd recovery rate does not have to be evaluated carefully. Moreover, the mathematical model associated to IDMS is known, and provides transparency for the uncertainty propagation. Our validation protocol was in agreement with guidelines of the ISO/IEC 17025 standard (chapter 5.4.5). Firstly, we assessed the experimental factors influencing the final result. Secondly, we compared the isotope ratios measured after our separation procedure to the reference values obtained with a different protocol for the digested test material IMEP-111 (mineral feed). Thirdly, we analysed the certified reference material BCR-609 (groundwater). Finally, combined uncertainties associated to our results were estimated according to ISO-GUM guidelines (typically, 3-4% k = 2 for a cadmium content of around 100 ng kg{sup -1}). We applied the developed method to the

ISOTOPE-DILUTION AMMONIA CHEMICAL-IONIZATION MASS FRAGMENTOGRAPHIC ANALYSIS OF URINARY 3-O-METHYLATED CATECHOLAMINE METABOLITES - RAPID SAMPLE CLEANUP BY DERIVATIZATION AND EXTRACTION OF LYOPHILIZED SAMPLES

NARCIS (Netherlands)

KEMA, IP; MEIBORG, G; NAGEL, GT; STOB, GJ; MUSKIET, FAJ

1993-01-01

We developed a method for simultaneous quantification of the urinary 3-O-methylated catecholamine metabolites 3-methoxytyramine, normetanephrine and metanephrine by stable isotope-dilution ammonia chemical ionization mass fragmentography. Prepurification of lyophilized samples was done by

Separation of glycols from dilute aqueous solutions via complexation with boronic acids

Energy Technology Data Exchange (ETDEWEB)

Randel, L.A.; King, C.J.

1991-07-01

This work examines methods of separating low molecular weight glycols from dilute aqueous solution. Extraction into conventional solvents is generally not economical, since, in the literature reviewed, distribution ratios for the two- to four-carbon glycols are all less than one. Distribution ratios can be increased, however, by incorporating into the organic phase an extracting agent that will complex with the solute of interest. The extracting agent investigated in this work is 3-nitrophenylboronic acid (NPBA). NPBA, a boric acid derivative, reversibly complexes with many glycols. The literature on complexation of borate and related compounds with glycols, including mechanistic data, measurement techniques, and applications to separation processes, provides information valuable for designing experiments with NPBA and is reviewed herein. 88 refs., 15 figs., 24 tabs.

Experimental Study On The Optimization Of Extraction Process Of ...

African Journals Online (AJOL)

The objective is to study the extraction process of garlic oil and its antibacterial effects. Materials and Methods: CO2 Supercritical extraction was used to investigate the optimal processing conditions for garlic oil extraction; filter paper test and suspension dilution test were applied to determine the bacteriostatic action of ...

Microbial diversity in fecal samples depends on DNA extraction method

DEFF Research Database (Denmark)

Mirsepasi, Hengameh; Persson, Søren; Struve, Carsten

2014-01-01

was to evaluate two different DNA extraction methods in order to choose the most efficient method for studying intestinal bacterial diversity using Denaturing Gradient Gel Electrophoresis (DGGE). FINDINGS: In this study, a semi-automatic DNA extraction system (easyMag®, BioMérieux, Marcy I'Etoile, France......BACKGROUND: There are challenges, when extracting bacterial DNA from specimens for molecular diagnostics, since fecal samples also contain DNA from human cells and many different substances derived from food, cell residues and medication that can inhibit downstream PCR. The purpose of the study...... by easyMag® from the same fecal samples. Furthermore, DNA extracts obtained using easyMag® seemed to contain inhibitory compounds, since in order to perform a successful PCR-analysis, the sample should be diluted at least 10 times. DGGE performed on PCR from DNA extracted by QIAamp DNA Stool Mini Kit DNA...

A theory of stable-isotope dilution mass spectrometry

International Nuclear Information System (INIS)

Pickup, J.F.; McPherson, C.K.

1977-01-01

In order to perform quantitative analysis using stable isotope dilution with mass spectrometry, an equation is derived which describes the relationship between the relative proportions of natural and labelled material and measured isotope ratios

Larvaecidal effects of aqueous extracts of Azadirachta indica (neem ...

African Journals Online (AJOL)

The effect of crude aqueous extracts of Azadirachta indica (neem) against the larvae of Anopheles mosquito was investigated. Exposure of the larvae to undiluted extracts of seed oil, leaf and bark for 12 hours led to 100, 98, and 48% mortality, respectively. Dilution of these extracts also resulted in mortality of the larvae.

A Simple Method for Automated Solid Phase Extraction of Water Samples for Immunological Analysis of Small Pollutants.

Science.gov (United States)

Heub, Sarah; Tscharner, Noe; Kehl, Florian; Dittrich, Petra S; Follonier, Stéphane; Barbe, Laurent

2016-01-01

A new method for solid phase extraction (SPE) of environmental water samples is proposed. The developed prototype is cost-efficient and user friendly, and enables to perform rapid, automated and simple SPE. The pre-concentrated solution is compatible with analysis by immunoassay, with a low organic solvent content. A method is described for the extraction and pre-concentration of natural hormone 17β-estradiol in 100 ml water samples. Reverse phase SPE is performed with octadecyl-silica sorbent and elution is done with 200 µl of methanol 50% v/v. Eluent is diluted by adding di-water to lower the amount of methanol. After preparing manually the SPE column, the overall procedure is performed automatically within 1 hr. At the end of the process, estradiol concentration is measured by using a commercial enzyme-linked immune-sorbent assay (ELISA). 100-fold pre-concentration is achieved and the methanol content in only 10% v/v. Full recoveries of the molecule are achieved with 1 ng/L spiked de-ionized and synthetic sea water samples.

Quantifying the dilution effect for models in ecological epidemiology.

Science.gov (United States)

Roberts, M G; Heesterbeek, J A P

2018-03-01

The dilution effect , where an increase in biodiversity results in a reduction in the prevalence of an infectious disease, has been the subject of speculation and controversy. Conversely, an amplification effect occurs when increased biodiversity is related to an increase in prevalence. We explore the conditions under which these effects arise, using multi species compartmental models that integrate ecological and epidemiological interactions. We introduce three potential metrics for quantifying dilution and amplification, one based on infection prevalence in a focal host species, one based on the size of the infected subpopulation of that species and one based on the basic reproduction number. We introduce our approach in the simplest epidemiological setting with two species, and show that the existence and strength of a dilution effect is influenced strongly by the choices made to describe the system and the metric used to gauge the effect. We show that our method can be generalized to any number of species and to more complicated ecological and epidemiological dynamics. Our method allows a rigorous analysis of ecological systems where dilution effects have been postulated, and contributes to future progress in understanding the phenomenon of dilution in the context of infectious disease dynamics and infection risk. © 2018 The Author(s).

Microbial enhancement of compost extracts based on cattle rumen content compost - characterisation of a system.

Science.gov (United States)

Shrestha, Karuna; Shrestha, Pramod; Walsh, Kerry B; Harrower, Keith M; Midmore, David J

2011-09-01

Microbially enhanced compost extracts ('compost tea') are being used in commercial agriculture as a source of nutrients and for their perceived benefit to soil microbiology, including plant disease suppression. Rumen content material is a waste of cattle abattoirs, which can be value-added by conversion to compost and 'compost tea'. A system for compost extraction and microbial enhancement was characterised. Molasses amendment increased bacterial count 10-fold, while amendment based on molasses and 'fish and kelp hydrolysate' increased fungal count 10-fold. Compost extract incubated at 1:10 (w/v) dilution showed the highest microbial load, activity and humic/fulvic acid content compared to other dilutions. Aeration increased the extraction efficiency of soluble metabolites, and microbial growth rate, as did extraction of compost without the use of a constraining bag. A protocol of 1:10 dilution and aerated incubation with kelp and molasses amendments is recommended to optimise microbial load and fungal-to-bacterial ratio for this inoculum source. Copyright © 2011 Elsevier Ltd. All rights reserved.

Development of isotope dilution gamma-ray spectrometry for plutonium analysis

Energy Technology Data Exchange (ETDEWEB)

Li, T.K.; Parker, J.L. (Los Alamos National Lab., NM (United States)); Kuno, Y.; Sato, S.; Kurosawa, A.; Akiyama, T. (Power Reactor and Nuclear Fuel Development Corp., Tokai, Ibaraki (Japan))

1991-01-01

We are studying the feasibility of determining the plutonium concentration and isotopic distribution of highly radioactive, spent-fuel dissolver solutions by employing high-resolution gamma-ray spectrometry. The study involves gamma-ray plutonium isotopic analysis for both dissolver and spiked dissolver solution samples, after plutonium is eluted through an ion-exchange column and absorbed in a small resin bead bag. The spike is well characterized, dry plutonium containing {approximately}98% of {sup 239}Pu. By using measured isotopic information, the concentration of elemental plutonium in the dissolver solution can be determined. Both the plutonium concentration and the isotopic composition of the dissolver solution obtained from this study agree well with values obtained by traditional isotope dilution mass spectrometry (IDMS). Because it is rapid, easy to operate and maintain, and costs less, this new technique could be an alternative method to IDMS for input accountability and verification measurements in reprocessing plants. 7 refs., 4 figs., 4 tabs.

Transition edge sensor-energy-dispersive spectrometer (TES-EDS) using a cryogen-free dilution refrigerator for material analysis

International Nuclear Information System (INIS)

Tanaka, Keiichi; Odawara, Akikazu; Nagata, Atsushi; Ikeda, Masanori; Baba, Yukari; Nakayama, Satoshi; Chinone, Kazuo

2006-01-01

A cryogen-free energy-dispersive spectrometer (EDS) using a transition edge sensor (TES) was developed for material analysis. This system can maintain a temperature at 130 mK within 30 μK, and has good energy resolution (19 eV for Mn-Kα) for long-time measurement with a drift in the DC level of less than 0.02 eV/min. This system utilizes a dilution refrigerator (φ 272 mmxheight 572 mm) and has a snout (370 mm long and φ25 mm) similar to that in a conventional EDS system. The dilution refrigerator is pre-cooled by a GM refrigerator. A flexible tube between the dilution refrigerator and GM refrigerator damps the mechanical vibration of the GM refrigerator. Two shields (4 and 80 K) thermally protect the Cu rod (φ8 mm) cooled to be 100 mK. Windows composed of polyimide+Al film allow X-ray detection above the C-Kα line. A TES (6 mmx6 mm) and array SQUID amplifier (1.5 mmx3 mm) are mounted on top of the Cu rod. For Mn-Kα, the pulse height is 5.5 μA and decay time (τ eff ) is 90 μs. The maximum count rate (1/20 τ eff ) is estimated at about 500 cps

Study of the extraction of the traces of Cadmium through the method of subestequiometric isotope dilution

International Nuclear Information System (INIS)

Garate V, Z.

1990-01-01

In this work, it has been used the method of subestequiometric isotope dilution for the determination of traces of cadmium and it has been compared with other conventional's methods for study its performance. The conditions of the experiment had been studied carefully in order to optimize the parameters such as pH, (8,0 - 10,1) it used the buffer NH 3 :NH 4 Cl, the time of agitation (>120 s) and the concentration of the organic reactive (dithizone). Besides, it obtains the respective curve of calibration. In this study, we can watch a line relation in all the range studied (5-40 μg of Cd). This method applied to the analysis of Cadmium in a certified sample of H-8 of the IAEA, it gives us the next value: 195 ± 5,4 ppm (LOD= 1,5 ppm, LOQ= 4,8 ppm), it is enough satisfactory in comparison with the certified middle value of 188,9±19 ppm. It demonstrates the utility of the method in the Cadmium traces analysis if it disposes of the radioisotope of this element and the appropriate detection equipment. (DEM). 34 refs., 15 tabs., 7 figs

Extraction of Am, Pu and U by dicyclohexano-18-crown-6/1-octanol from HNO3 solution and simulated HLLW

International Nuclear Information System (INIS)

Wang Xinghai; Wang Jianchen; Liu Xiuqin; Song Chongli

1999-01-01

The extraction of americium, plutonium and uranium by dicyclohexano-18-crown-6 (DCH18C6)/1-octanol from HNO 3 solution and simulated HLLW are studied. The influences of acidity and dilution factor of simulated HLLW are studied. At low HNO 3 concentration and dilution factor above 2, 0.1 mol/L DCH18C6/1-octanol extracts very little americium, plutonium and uranium. the distribution ratios of Am, Pu and U increase with the increase of HNO 3 concentration in aqueous phase, and decrease with increasing of dilution factor of HLLW. The distribution ratio of extraction of Pu(IV) increases with the increase of extractant concentration

Testing sequential extraction methods for the analysis of multiple stable isotope systems from a bone sample

Science.gov (United States)

Sahlstedt, Elina; Arppe, Laura

2017-04-01

Stable isotope composition of bones, analysed either from the mineral phase (hydroxyapatite) or from the organic phase (mainly collagen) carry important climatological and ecological information and are therefore widely used in paleontological and archaeological research. For the analysis of the stable isotope compositions, both of the phases, hydroxyapatite and collagen, have their more or less well established separation and analytical techniques. Recent development in IRMS and wet chemical extraction methods have facilitated the analysis of very small bone fractions (500 μg or less starting material) for PO43-O isotope composition. However, the uniqueness and (pre-) historical value of each archaeological and paleontological finding lead to preciously little material available for stable isotope analyses, encouraging further development of microanalytical methods for the use of stable isotope analyses. Here we present the first results in developing extraction methods for combining collagen C- and N-isotope analyses to PO43-O-isotope analyses from a single bone sample fraction. We tested sequential extraction starting with dilute acid demineralization and collection of both collagen and PO43-fractions, followed by further purification step by H2O2 (PO43-fraction). First results show that bone sample separates as small as 2 mg may be analysed for their δ15N, δ13C and δ18OPO4 values. The method may be incorporated in detailed investigation of sequentially developing skeletal material such as teeth, potentially allowing for the investigation of interannual variability in climatological/environmental signals or investigation of the early life history of an individual.

Inorganic arsenic in seafood: does the extraction method matter?

Science.gov (United States)

Pétursdóttir, Ásta H; Gunnlaugsdóttir, Helga; Krupp, Eva M; Feldmann, Jörg

2014-05-01

Nine different extraction methods were evaluated for three seafood samples to test whether the concentration of inorganic arsenic (iAs) determined in seafood is dependent on the extraction method. Certified reference materials (CRM) DOLT-4 (Dogfish Liver) and TORT-2 (Lobster Hepatopancreas), and a commercial herring fish meal were evaluated. All experimental work described here was carried out by the same operator using the same instrumentation, thus eliminating possible differences in results caused by laboratory related factors. Low concentrations of iAs were found in CRM DOLT-4 (0.012±0.003mgkg(-1)) and the herring fish meal sample (0.007±0.002mgkg(-1)) for all extraction methods. When comparing the concentration of iAs in CRM TORT-2 found in this study and in the literature dilute acids, HNO3 and HCl, showed the highest extracted iAs wheras dilute NaOH (in 50% ethanol) showed significantly lower extracted iAs. However, most other extraction solvents were not statistically different from one another. Copyright © 2013 Elsevier Ltd. All rights reserved.

Comparison of low-level polycyclic aromatic hydrocarbons in sediment revealed by Soxhlet extraction, microwave-assisted extraction, and pressurized liquid extraction

International Nuclear Information System (INIS)

Itoh, Nobuyasu; Numata, Masahiko; Aoyagi, Yoshie; Yarita, Takashi

2008-01-01

We analyzed polycyclic aromatic hydrocarbons (PAHs) present in lake sediment at low levels ( -1 ) by using Soxhlet extraction (Soxhlet), microwave-assisted extraction (MAE), and pressurized liquid extraction (PLE) in combination with gas chromatography and isotope-dilution mass spectrometry. Although all extraction techniques showed good repeatability for five target PAHs (relative standard deviation MAE > Soxhlet. Differences in the results originated mainly from differences in the extraction efficiencies of the techniques for native PAHs, because all techniques gave comparable recovery yields of corresponding 13 C-labeled PAHs ( 13 C-PAHs) (51-84%). Since non-negligible amounts of both native PAHs and 13 C-PAHs were re-adsorbed on matrix in MAE, not only recovery yields of 13 C-PAHs but also efficiencies of extraction of native PAHs should be examined to evaluate the appropriateness of any analytical procedures

Dynamic Stresses in the LHC TCDS Diluter from 7 TeV Beam Loading

CERN Document Server

Goddard, B; Presland, A; Weterings, W

2006-01-01

In the event of an unsynchronised beam abort, the MSD extraction septum of the LHC beam dumping system is protected from damage by the TCDS diluter. The simultaneous constraints of obtaining sufficient beam dilution while ensuring the survival of the TCDS make the design difficult, with high thermally induced dynamic stresses occurring in the material needed to attenuate the particle showers induced by the primary beam impact. In this paper, full 3D simulations are described where the worst-case beam loading has been used to generate the local temperature rise and to follow the resulting time evolution of the mechanical stresses. The results and the accompanying design changes for the TCDS, to provide an adequate performance margin, are detailed.

In vitro Antibacterial Activity of Alchornea cordifolia Bark Extract ...

African Journals Online (AJOL)

Four extracts of Alchornea cordifolia (Schumach.) Müll. Arg. (Euphorbiaceae) bark, including aqueous, methanol, acetone and hexane extracts, were tested for their antibacterial activities against Salmonella typhi, Salmonella paratyphi A and Salmonella paratyphi B, using both agar diffusion and broth dilution methods.

Evaluation of feeds for melt and dilute process using an analytical hierarchy process

Energy Technology Data Exchange (ETDEWEB)

Krupa, J.F.

2000-03-22

Westinghouse Savannah River Company was requested to evaluate whether nuclear materials other than aluminum-clad spent nuclear fuel should be considered for treatment to prepare them for disposal in the melt and dilute facility as part of the Treatment and Storage Facility currently projected for construction in the L-Reactor process area. The decision analysis process used to develop this analysis considered many variables and uncertainties, including repository requirements that are not yet finalized. The Analytical Hierarchy Process using a ratings methodology was used to rank potential feed candidates for disposition through the Melt and Dilute facility proposed for disposition of Savannah River Site aluminum-clad spent nuclear fuel. Because of the scoping nature of this analysis, the expert team convened for this purpose concentrated on technical feasibility and potential cost impacts associated with using melt and dilute versus the current disposition option. This report documents results of the decision analysis.

Evaluation of feeds for melt and dilute process using an analytical hierarchy process

International Nuclear Information System (INIS)

Krupa, J.F.

2000-01-01

Westinghouse Savannah River Company was requested to evaluate whether nuclear materials other than aluminum-clad spent nuclear fuel should be considered for treatment to prepare them for disposal in the melt and dilute facility as part of the Treatment and Storage Facility currently projected for construction in the L-Reactor process area. The decision analysis process used to develop this analysis considered many variables and uncertainties, including repository requirements that are not yet finalized. The Analytical Hierarchy Process using a ratings methodology was used to rank potential feed candidates for disposition through the Melt and Dilute facility proposed for disposition of Savannah River Site aluminum-clad spent nuclear fuel. Because of the scoping nature of this analysis, the expert team convened for this purpose concentrated on technical feasibility and potential cost impacts associated with using melt and dilute versus the current disposition option. This report documents results of the decision analysis

Mycoestrogen determination in cow milk: Magnetic solid-phase extraction followed by liquid chromatography and tandem mass spectrometry analysis.

Science.gov (United States)

Capriotti, Anna Laura; Cavaliere, Chiara; Foglia, Patrizia; La Barbera, Giorgia; Samperi, Roberto; Ventura, Salvatore; Laganà, Aldo

2016-12-01

Recently, magnetic solid-phase extraction has gained interest because it presents various operational advantages over classical solid-phase extraction. Furthermore, magnetic nanoparticles are easy to prepare, and various materials can be used in their synthesis. In the literature, there are only few studies on the determination of mycoestrogens in milk, although their carryover in milk has occurred. In this work, we wanted to develop the first (to the best of our knowledge) magnetic solid-phase extraction protocol for six mycoestrogens from milk, followed by liquid chromatography and tandem mass spectrometry analysis. Magnetic graphitized carbon black was chosen as the adsorbent, as this carbonaceous material, which is very different from the most diffuse graphene and carbon nanotubes, had already shown selectivity towards estrogenic compounds in milk. The graphitized carbon black was decorated with Fe 3 O 4 , which was confirmed by the characterization analyses. A milk deproteinization step was avoided, using only a suitable dilution in phosphate buffer as sample pretreatment. The overall process efficiency ranged between 52 and 102%, whereas the matrix effect considered as signal suppression was below 33% for all the analytes even at the lowest spiking level. The obtained method limits of quantification were below those of other published methods that employ classical solid-phase extraction protocols. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Differential isospin-fractionation in dilute asymmetric nuclear matter

International Nuclear Information System (INIS)

Li Baoan; Chen Liewen; Ma Hongru; Xu Jun; Yong Gaochan

2007-01-01

The differential isospin-fractionation (IsoF) during the liquid-gas phase transition in dilute asymmetric nuclear matter is studied as a function of nucleon momentum. Within a self-consistent thermal model it is shown that the neutron/proton ratio of the gas phase becomes smaller than that of the liquid phase for energetic nucleons, although the gas phase is overall more neutron-rich. Clear indications of the differential IsoF consistent with the thermal model predictions are demonstrated within a transport model for heavy-ion reactions. Future comparisons with experimental data will allow us to extract critical information about the momentum dependence of the isovector strong interaction

Analysis of several hazardous conditions for large transfer and back-dilution sequences in Tank 241-SY-101

International Nuclear Information System (INIS)

CW Stewart; LA Mahoney; WB Barton

2000-01-01

The first transfer of 89 kgal of waste and back-dilution of 61 kgal of water in Hanford Tank 241-SY-101 was accomplished December 18--20, 1999. Limits were placed on the transfer and back-dilution volumes because of concerns about potential gas release, crust sinking, and degradation of mixer pump performance. Additional transfers and back-dilutions are being planned that will bring the total to 500 kgal, which should dissolve a large fraction of the solids in the tank and dilute it well beyond the point where significant gas retention can occur. This report provides the technical bases for removing the limits on transfer and back-dilution volume by evaluating the potential consequences of several postulated hazardous conditions in view of the results of the first campaign and results of additional analyses of waste behavior

Analysis of several hazardous conditions for large transfer and back-dilution sequences in Tank 241-SY-101

Energy Technology Data Exchange (ETDEWEB)

CW Stewart; LA Mahoney; WB Barton

2000-01-28

The first transfer of 89 kgal of waste and back-dilution of 61 kgal of water in Hanford Tank 241-SY-101 was accomplished December 18--20, 1999. Limits were placed on the transfer and back-dilution volumes because of concerns about potential gas release, crust sinking, and degradation of mixer pump performance. Additional transfers and back-dilutions are being planned that will bring the total to 500 kgal, which should dissolve a large fraction of the solids in the tank and dilute it well beyond the point where significant gas retention can occur. This report provides the technical bases for removing the limits on transfer and back-dilution volume by evaluating the potential consequences of several postulated hazardous conditions in view of the results of the first campaign and results of additional analyses of waste behavior.

Enumeration of haemopoietic progenitors (CFU-C and BFU-E) in liquid microculture using a limiting dilution analysis.

Science.gov (United States)

Marchal, G; Milon, G

1980-01-01

In order to overcome the difficulty of scoring multicentric colonies of haemopoietic progenitor cells, cultures in 10 microliter of liquid medium were grown. Plated at three different cell concentrations, progenitor cells (CFU-C or BFU-E) are not present in all wells. Their presence is easily scored in each well of microculture 7 days after incubation. A limiting dilution analysis allows one to obtain accurate quantification.

Certification of butyltins and phenyltins in marine sediment certified reference material by species-specific isotope-dilution mass spectrometric analysis using synthesized {sup 118}Sn-enriched organotin compounds

Energy Technology Data Exchange (ETDEWEB)

Inagaki, Kazumi; Takatsu, Akiko; Watanabe, Takuro; Aoyagi, Yoshie; Yarita, Takashi; Okamoto, Kensaku; Chiba, Koichi [National Institute of Advanced Industrial Science and Technology (AIST), Environmental Standard Section, National Metrology Institute of Japan (NMIJ), Tsukuba, Ibaraki (Japan)

2007-04-15

A new marine sediment certified reference material, NMIJ CRM 7306-a, for butyltin and phenyltin analysis has been prepared and certified by the National Metrological Institute of Japan at the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Candidate sediment material was collected at a bay near industrial activity in Japan. After air-drying, sieving, and mixing the material was sterilized with {gamma}-ray irradiation. The material was re-mixed and packaged into 250 glass bottles (15 g each) and these were stored in a freezer at -30 C. Certification was performed by use of three different types of species-specific isotope-dilution mass spectrometry (SSID-MS) - SSID-GC-ICP-MS, SSID-GC-MS, and SSID-LC-ICP-MS, with {sup 118}Sn-enriched organotin compounds synthesized from {sup 118}Sn-enriched metal used as a spike. The {sup 118}Sn-enriched mono-butyltin (MBT), dibutyltin (DBT), and tributyltin (TBT) were synthesized as a mixture whereas the {sup 118}Sn-enriched di-phenyltin (DPhT) and triphenyltin (TPhT) were synthesized individually. Four different extraction methods, mechanical shaking, ultrasonic, microwave-assisted, and pressurized liquid extraction, were adopted to avoid possible analytical bias caused by non-quantitative extraction and degradation or inter-conversion of analytes in sample preparations. Tropolone was used as chelating agent in all the extraction methods. Certified values are given for TBT 44{+-}3 {mu}g kg{sup -1} as Sn, DBT 51 {+-} 2 {mu}g kg{sup -1} as Sn, MBT 67 {+-} 3 {mu}g kg{sup -1} as Sn, TPhT 6.9 {+-} 1.2 {mu}g kg{sup -1} as Sn, and DPhT 3.4 {+-} 1.2 {mu}g kg{sup -1} as Sn. These levels are lower than in other sediment CRMs currently available for analysis of organotin compounds. (orig.)

Simultaneous analysis of urinary phthalate metabolites of residents in Korea using isotope dilution gas chromatography-mass spectrometry.

Science.gov (United States)

Kim, Miok; Song, Na Rae; Choi, Jong-Ho; Lee, Jeongae; Pyo, Heesoo

2014-02-01

Phthalates are used in industry products, household items, and medical tools as plasticizers. Human exposure to phthalates has raised concern about its toxicity. In the present study, optimization was conducted for the simultaneous analysis of eight kinds of phthalate metabolites using gas chromatography-mass spectrometry (GC-MS): MEP, MiBP, MnBP, MBzP, MiNP, MEHP, MEOHP, and MEHHP. In order to minimize the matrix effect and to do quantitative analysis, isotope dilution and LLE-GC-MS methods were performed. Urine samples were enzymatically hydrolyzed, extracted with a mixture of n-hexane and ethyl ether (8:2; v:v), and subsequently derivatized with trimethylsilylation. All eight kinds of analytes showed clear resolution and high reproducibility in GC-MS results. The method detection limit ranged from 0.05 ng/mL to 0.2 ng/mL. Calibration curves were found to be linear from 0.2 to 100 ng/mL with -(2)>0.992. The relative standard deviation of the intraday precision using water and urine ranged from 2.1% to 16.3%. The analysis was performed with urine samples that were collected from adults residing in the Republic of Korea. The analyzed concentration results were compared according to gender and region. As a result, DEHP metabolites showed the highest detected concentration (75.92 μg/g creatinine, 100%), and MiNP, a metabolite of DiNP, showed the lowest detected concentration (0.42 μg/g creatinine, 22.5%). On average, female urine (200.76 μg/g creatinine) had a higher detected concentration of ∑8 phthalate metabolites than male urine. Samples from rural regions (211.96 μg/g creatinine) had higher levels than samples from urban regions. © 2013.

Studies on the dilution behaviour of effluent discharged into the CCW channel at KGS

International Nuclear Information System (INIS)

Sivasubramanian, K.; Srinivasan, S.; Ponraju, D.; Meenakshisundaram, V.; Munusamy, N.

2003-01-01

The dilution behaviour of the liquid effluent discharged into condenser cooling water channel of Kaiga Power Plant has been studied using salt addition and dye addition methods. Dilution factors determined experimentally showed that the discharged liquid effluent gets thoroughly mixed with stream of water at the weir and further diluted in the down stream. This paper describes both salt and dye addition methods for determining the dilution factor. The velocity of the stream at various locations were measured and compared with reported values. The selection of representative sampling point for routine analysis of water was identified from this experiment. (author)

Isotope dilution and sampling factors of the quality assurance and TQM of environmental analysis

International Nuclear Information System (INIS)

Macasek, F.

1999-01-01

Sampling and preparatory treatment of environmental objects is discussed from the view of their information content, functional speciation of the pollutant, statistical distribution treatment and uncertainty assessment. During homogenization of large samples, a substantial information may be lost and validity of environmental information becomes vague. Isotope dilution analysis is discussed as the most valuable tool for both validity of analysis and evaluation of samples variance. Data collection for a non-parametric statistical treatment of series of 'non-representative' sub-samples, and physico-chemical speciation of analyte may actually better fulfill criteria of similarity and representativeness. Large samples are often required due to detection limits of analysis, but the representativeness of environmental samples should by understood not only by the mean analyte concentration, but also by its spatial and time variance. Hence, heuristic analytical scenarios and interpretation of results must be designed by cooperation of environmentalists and analytical chemists. (author)

Effect of Side Chain Functional Group on Interactions in Ionic Liquid Systems: Insights from Infinite Dilution Thermodynamic Data.

Science.gov (United States)

Paduszyński, Kamil; Królikowska, Marta

2017-11-02

Measurements of infinite dilution activity coefficients of 48 molecular solutes (including alkanes, alkenes, alkynes, aromatics, ethers, alcohols, water, ketones, pyridine, thiophene, acetonitrile, and 1-nitropropane) in two ionic liquids (ILs), namely, 1-(2-hydroxyethyl)-3-methylimidazolium dicyanamide and 1-(2-chloroethyl)-3-methylimidazolium dicyanamide, are reported in the temperature range from T = 308.15 to 358.15 K. Comparative analysis of an effect of OH/Cl substitution of terminal carbon in side chains of imidazolium cations is presented and discussed in terms of different types of intermolecular forces acting between ILs and solutes. The new data also are confronted to those published previously for a "plain" counterpart of the studied ILs, namely, 1-ethyl-3-methylimidazolium dicyanamide. Infinite dilution capacity and selectivity of the studied ILs are presented to evaluate them as separating agents in extraction of aromatics from alkanes and sulfur compounds from alkanes. Three modeling approaches, namely, linear solvation energy relationship (LSER), regular solution theory, and conductor-like screening model for real solvents (COSMO-RS), are tested for their capabilities of capturing the substitution effects detected experimentally.

Evaluation of automated nucleic acid extraction methods for virus detection in a multicenter comparative trial

DEFF Research Database (Denmark)

Rasmussen, Thomas Bruun; Uttenthal, Åse; Hakhverdyan, M.

2009-01-01

between the results obtained for the different automated extraction platforms. In particular, the limit of detection was identical for 9/12 and 8/12 best performing robots (using dilutions of BVDV infected-serum and cell culture material, respectively), which was similar to a manual extraction method used......Five European veterinary laboratories participated in an exercise to compare the performance of nucleic acid extraction robots. Identical sets of coded samples were prepared using serial dilutions of bovine viral diarrhoea virus (BVDV) from serum and cell culture propagated material. Each...

Calorimetric measurement of the enthalpy of extraction of uranyl nitrate by tri-n-amyl phosphate

International Nuclear Information System (INIS)

Srinivasan, T.G.; Vasudeva Rao, P.R.; Venugopal, V.; Sood, D.D.

2002-01-01

Enthalpy of extraction of uranyl nitrate by tri n-amyl phosphate (TAP) and its solutions in n-dodecane has been directly measured by solution calorimetry for the first time. Measurements have been made at 303±1 K, in both forward as well as the reverse extraction modes. The enthalpies of the accompanying reactions such as the dilution of the uranyl nitrate in the aqueous phase, the hydration of TAP, the mixing of TAP and n-dodecane, the mixing of the metal-solvate (UO 2 (NO 3 ) 2 ·2TAP) and n-dodecane and mixing of the metal-solvate and TAP have also been independently measured and used to derive both the equilibrium state enthalpies and the standard state enthalpies for the extraction. Two distinct standard states have been used for the organic phase, viz., 1) all solutes infinitely diluted in diluent (ΔH*) and 2) all solutes infinitely diluted in the water saturated extractant (ΔH 0 ). The results have been compared with the enthalpies of extraction measured by employing the temperature dependence of the distribution ratio as well as calorimetry reported in the literature for extraction of uranyl nitrate by TAP and TBP. (author)

Structural, morphological and magnetic analysis of Cd–Co–S dilute magnetic semiconductor nanofilms

Energy Technology Data Exchange (ETDEWEB)

Kumar, Suresh [Department of Physics and Materials Science, Jaypee University of Information Technology, Waknaghat, Solan, Himachal Pradesh 173234 (India); Negi, N.S. [Department of Physics, Himachal Pradesh University, Summer Hill, Shimla, Himachal Pradesh 171005 (India); Katyal, S.C. [Department of Physics, Jaypee Institute of Information Technology, Sec-128, Noida, Uttar Pradesh 201301 (India); Sharma, Pankaj, E-mail: pankaj.sharma@juit.ac.in [Department of Physics and Materials Science, Jaypee University of Information Technology, Waknaghat, Solan, Himachal Pradesh 173234 (India); Sharma, Vineet [Department of Physics and Materials Science, Jaypee University of Information Technology, Waknaghat, Solan, Himachal Pradesh 173234 (India)

2014-10-01

Cd{sub 1−x}Co{sub x}S dilute magnetic semiconductor nanofilms (0≤x≤0.08 at%) deposited by chemical bath deposition have been investigated using grazing angle x-ray diffraction, atomic force microscopy and vibrating sample magnetometer. The introduction of Co{sup 2+} ions in CdS structure induces structural disorders and hence, results in degradation of crystallinity. The crystallite size, interplanar spacing and lattice parameter ratio decrease with increasing Co{sup 2+} concentration in CdS. The diamagnetic state of CdS disappears with increase in Co concentration and films with x>0.02 exhibit ferromagnetism. This may be explained in terms of the spin–orbit interactions and Co{sup 2+} ion induced the lattice defects and phase separation. - Highlights: • Cd{sub 1−x}Co{sub x}S dilute magnetic semiconductor nanofilms (0≤x≤0.08 at%) deposited by CBD. • The diamagnetic state of CdS vanishes for x=0.02. • For x>0.02, dilute magnetic semiconductor nanofilms shows a ferromagnetic state.

L-edge sum rule analysis on 3d transition metal sites: from d10 to d0 and towards application to extremely dilute metallo-enzymes.

Science.gov (United States)

Wang, Hongxin; Friedrich, Stephan; Li, Lei; Mao, Ziliang; Ge, Pinghua; Balasubramanian, Mahalingam; Patil, Daulat S

2018-03-28

According to L-edge sum rules, the number of 3d vacancies at a transition metal site is directly proportional to the integrated intensity of the L-edge X-ray absorption spectrum (XAS) for the corresponding metal complex. In this study, the numbers of 3d holes are characterized quantitatively or semi-quantitatively for a series of manganese (Mn) and nickel (Ni) complexes, including the electron configurations 3d 10 → 3d 0 . In addition, extremely dilute (edge jump region; and (2) by adding an inert tracer to the sample that provides a prominent spectral feature to replace the weak edge jump for intensity normalization. In this publication, we present for the first time: (1) L-edge sum rule analysis for a series of Mn and Ni complexes that include electron configurations from an open shell 3d 0 to a closed shell 3d 10 ; (2) a systematic analysis on the uncertainties, especially on that from the edge jump, which was missing in all previous reports; (3) a clearly-resolved edge jump between pre-L 3 and post-L 2 regions from an extremely dilute sample; (4) an evaluation of an alternative normalization standard for L-edge sum rule analysis. XAS from two copper (Cu) proteins measured using a conventional semiconductor X-ray detector are also repeated as bridges between Ni complexes and dilute Ni enzymes. The differences between measuring 1% Cu enzymes and measuring edge sum rule analysis to virtually any 3d metal complex and any dilute biological samples that contain 3d metals.

Acetic acid extraction from aqueous solutions using fatty acids

NARCIS (Netherlands)

IJmker, H.M.; Gramblicka, M.; Kersten, Sascha R.A.; van der Ham, Aloysius G.J.; Schuur, Boelo

2014-01-01

A major challenge for production of acetic acid via bio-based routes is cost-effective concentration and purification of the acetic acid from the aqueous solutions, for which liquid–liquid extraction is a possible method. A main challenge in extraction of acetic acid from dilute aqueous solutions is

Measurement of Activity Coefficients at Infinite Dilution for Alcohols in [BMIM][CH3SO4] using HS-SPME/GC-FID

Directory of Open Access Journals (Sweden)

A. M. Elias

Full Text Available ABSTRACT The activity coefficient at infinite dilution (&IN1 and distribution ratios at infinite dilution (&IN2 were determined for alkanols (methanol, ethanol, 1-propanol, 1-butanol, 2-butanol, and 2-methyl-2-propanol in the ionic liquid (IL 1-butyl-3-methylimidazolium methyl sulfate ([BMIM][CH3SO4] by HS-SPME (Headspace - Solid Phase Micro Extraction at four temperatures (298.15, 313.15, 333.15, and 353.15K using headspace - solid phase microextraction (SPME-HS. The results showed significant agreement with literature data. In addition, partial molar excess enthalpies at infinite dilution (&IN3, excess Gibbs energies (&IN4, and excess entropies (&IN5 were calculated from the (&IN6 values.

Effects of extraction and derivatization techniques on recovery of organotin species in environmental matrices (W3)

International Nuclear Information System (INIS)

Wahlen, R.; Catterick, T.

2002-01-01

Full text: Organotin (OT) contamination is still persistent in most coastal environments and estuaries and can be monitored accurately by analysis of sediments and sedentary aquatic animal populations. In addition to human exposure via contaminated seafood, there is increasing concern about OT compounds in man-made consumer products. Organotin analysis involves the extraction from the matrix, derivatization (for GC analysis), separation of the different species and detection. Commonly used extraction techniques are mechanical shaking, ultrasonic agitation and microwave leaching (open or closed vessel). Accelerated solvent extraction (ASE) has also been reported. In this study, closed-vessel microwave extraction and ASE methods are compared for OT analysis in environmental tissues using separation by gas chromatography (GC) and detection by inductively coupled plasma mass-spectrometry (ICP-MS). The efficiency of an ethylation procedure with sodiumtetraethylborate (NABEt 4 ) using different matrices and derivatization durations is monitored by comparing data obtained by external calibration with results by species-specific isotope dilution analysis (SS-IDMS) of dibutyltin (TBT) and dibutyltin (DBT) enriched with 117 Sn. Uncertainty estimates for both quantification techniques will be provided. (author)

Physical modelling of a rapid boron dilution transient

Energy Technology Data Exchange (ETDEWEB)

Anderson, N.G.; Hemstroem, B.; Karlsson, R. [Vattenfall Utveckling AB, Aelvkarleby (Sweden); Jacobson, S. [Vattenfall AB, Ringhals, Vaeroebacka (Sweden)

1995-09-01

The analysis of boron dilution accidents in pressurised water reactors has traditionally assumed that mixing is instantaneous and complete everywhere, eliminating in this way the possibility of concentration inhomogeneities. Situations can nevertheless arise where a volume of coolant with a low boron concentration may eventually enter the core and generate a severe reactivity transient. The work presented in this paper deals with a category of Rapid Boron Dilution Events characterised by a rapid start of a Reactor Coolant Pump (RCP) with a plug of relatively unborated water present in the RCS pipe. Model tests have been made at Vattenfall Utveckling AB in a simplified 1:5 scale model of a Westinghouse PWR. Conductivity measurements are used to determine dimensionless boron concentration. The main purpose of this experimental work is to define an experimental benchmark against which a mathematical model can be tested. The final goal is to be able to numerically predict Boron Dilution Transients. This work has been performed as a part of a Co-operative Agreement with Electricite` de France (EDF).

Determination of 241Am in sediments by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS).

Science.gov (United States)

Agarande, M; Benzoubir, S; Bouisset, P; Calmet, D

2001-08-01

Trace levels (pg kg(-1)) of 241Am in sediments were determined by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS) using a microconcentric nebulizer. 241Am was isolated from major elements like Ca and Fe by different selective precipitations. In further steps. Am was first separated from other transuranic elements and purified by anion exchange and extraction chromatography prior to the mass spectrometric measurements. The ID HR ICP-MS results are compared with isotope dilution alpha spectrometry.

Percolation of polyatomic species on site diluted lattices

International Nuclear Information System (INIS)

Cornette, V.; Ramirez-Pastor, A.J.; Nieto, F.

2006-01-01

In this Letter, the percolation of (a) linear segments of size k and (b) k-mers (particles occupying k adjacent sites) of different structures and forms deposited on a diluted square lattice have been studied. The diluted lattice is built by randomly selecting a fraction of sites which are considered forbidden for deposition. The analysis of the obtained results is made in the framework of the finite size scaling theory. The characteristic parameters of the percolation problem are dependent not only on the form and structure of the k-mers but also on the properties of the lattice where they are deposited. A phase diagram separating a percolating from a non-percolating region is determined and discussed

Qualitative analysis of hexane flour extract of spelt

Directory of Open Access Journals (Sweden)

Vujić Đura N.

2013-01-01

Full Text Available Gas chromatography with mass spectrometry (GC-MS was used for performing a qualitative analysis of the hexane flour extract of three samples of spelt. All the three samples were first treated with hexane and the obtained extracts were used for the analysis of the fatty acid lipid components. The transesterification reaction was performed using TMSH (trimethylsulfonium hydroxide, 0.2M in methanol, and the fatty acids were esterified from acylglycerol to methyl-esters. In all analyzed extracts, the predominant component was methyl linoleate, followed by methyl oleate and methyl palmitate. The subsequent tests, performed by cluster analysis, were used to compare the hexane flour extracts of different types of spelt. [Projekat Ministarstva nauke Republike Srbije, br. III46005 i br. TR 31066

Dilute solution, flow behavior, thixotropy and viscoelastic characterization of cress seed (Lepidium sativum) gum fractions

DEFF Research Database (Denmark)

Razmkhah, Somayeh; Razavi, Seyed Mohammad Ali; Mohammadifar, Mohammad Amin

2017-01-01

In this study, rheological properties of cress seed gum (CSG) and its fractions (F1, F2, F3; fractionated using stepwise extraction with water) were investigated. Cress seed gum and its fractions revealed random coil conformation in dilute regimes; chain flexibility and intrinsic viscosity...... indicated that CSG and the fractions exhibited significantly different rheological properties....

Further development of IDGS: Isotope dilution gamma-ray spectrometry

International Nuclear Information System (INIS)

Li, T.K.; Parker, J.L.; Kuno, Y.; Sato, S.; Kamata, M.; Akiyama, T.

1991-01-01

The isotope dilution gamma-ray spectrometry (IDGS) technique for determining the plutonium concentration and isotopic composition of highly radioactive spent-fuel dissolver solutions has been further developed. Both the sample preparation and the analysis have been improved. The plutonium isotopic analysis is based on high-resolution, low-energy gamma-ray spectrometry. The plutonium concentration in the dissolver solutions then is calculated from the measured isotopic differences among the spike, the dissolver solution, and the spiked dissolver solution. Plutonium concentrations and isotopic compositions of dissolver solutions analyzed from this study agree well with those obtained by traditional isotope dilution mass spectrometry (IDMS) and are consistent with the first IDGS experimental result. With the current detector efficiency, sample size, and a 100-min count time, the estimated precision is ∼0.5% for 239 Pu and 240 Pu isotopic analyses and ∼1% for the plutonium concentration analysis. 5 refs., 2 figs., 7 tabs

Phytochemical screening, antibacterial and anti-oxidant activities of Asparagus laricinus leaf and stem extracts

Directory of Open Access Journals (Sweden)

Polo-Ma-Abiele Hildah Ntsoelinyane

2014-03-01

Full Text Available The aim of this study was to investigate antioxidant activities, antibacterial activities and a phytochemical constituent of Asparagus laricinus stem and leaf extracts. Determination of antibacterial activity of extracts was assessed by agar dilution method and antioxidant properties by 2,2-diphenyl-1-picryl-hydrazyl (DPPH assay. The minimum inhibitory concentration (MIC of the leaf was at a concentration of 0.125 mg/mL against S. saprophyticus and E. cloacae, and at a concentration of 1 mg/mL against S. aureus and B. subtilis. There was no MIC of the stem extract at any concentration. The leaf extract showed effective free radical scavenging activity (72.1%, while stem extract had low activity. Qualitative phytochemical analysis of these plant extracts revealed the presence of tannins, saponins, flavonoids and phlobatannins. The leaf extract further confirmed the presence of glycosides, steroids, ternoids and carbohydrates. Our results indicate that, A. laricinus leaf extracts have potential antimicrobial and antioxidant activities.

The IDA-80 measurement evaluation programme on mass spectrometric isotope dilution analysis of uranium and plutonium. Vol. 1

International Nuclear Information System (INIS)

Beyrich, W.; Golly, W.; Spannagel, G.; Kernforschungszentrum Karlsruhe G.m.b.H.; Bievre, P. de; Wolters, W.

1984-12-01

The main objective was the acquisition of basic data on the uncertainties involved in the mass spectrometric isotope dilution analysis as applied to the determination of uranium and plutonium in active feed solutions of reprocessing plants. The element concentrations and isotopic compositions of all test materials used were determined by CBNM and NBS with high accuracy. The more than 60000 analytical data reported by the participating laboratories were evaluated by statistical methods applied mainly to the calculation of estimates of the variances for the different uncertainty components contributing to the total uncertainty of this analytical technique. Attention was given to such topics as sample ageing, influence of fission products, spike calibration, ion fractionation, Pu-241 decay correction, minor isotope measurement and errors in data transfer. Furthermore, the performance of the 'dried sample' technique and the 'in-situ' spiking method of undiluted samples of reprocessing fuel solution with U-235/Pu-242 metal alloy spikes, were tested successfully. Considerable improvement of isotope dilution analysis in this safeguards relevant application during the last decade is shown as compared to the results obtained in the IDA-72 interlaboratory experiment, organized by KfK in 1972 on the same subject. (orig./HP) [de

VALORIZATION ABOVEGROUND OF THE EXTRACT OF COMPOST OVINE FOR FERTIGATION OF THE VEGETABLES PLANTS IN TUNISIA

Directory of Open Access Journals (Sweden)

Y. M’Sadak

2013-12-01

Full Text Available The main objective of this study was to highlight the fertilizing capacity of the extract of ovine compost (prepared to the simple infusion in gardening nursery, while specifying the appropriate ratios of extraction and dilution ,for soilless plant fertigation intended for two strategic summer crops in Tunisia: seasonal tomato and seasonal pepper. It is clear that such extraction ratio of 1: 5 is effective for plants fertigation of two considered species. In addition, it has been shown that 200 times dilution of the concentrated extract is beneficial for the growth of tomato plants. However, this organic liquid fertilizer with different dilutions applied and in the experimental conditions adopted, wasn’t moderately efficient in stimulating the growth of pepper plants. The importance of this type of compost produced from sheep biomass, widely available in Tunisia, encourage the diversification of its exploitation, which is the object of this preliminary work, deserving more future investigations.

The interlaboratory experiment IDA-72 on mass spectrometric isotope dilution analysis. Vol. 2

International Nuclear Information System (INIS)

Beyrich, W.; Drosselmeyer, E.

1975-07-01

Volume II of the report on the IDA-72 experiment contains papers written by different authors on a number of special topics connected with the preparation, performance and evaluation of the interlaboratory test. In detail the sampling procedures for active samples of the reprocessing plant and the preparation of inactive reference and spike solution from standard material are described as well as new methods of sample conditioning by evaporation. An extra chapter is devoted to the chemical sample treatment as a preparation for mass spectrometric analysis of the U and Pu content of the solutions. Special topics are also methods for mass discrimination corrections, α-spectrometer measurements as a supplement for the determination of Pu-238 and the comparison of concentration determinations by mass spectrometric isotope dilution analysis with those performed by X-ray fluorescence spectrometry. The last part of this volume contains papers connected with the computerized statistical evaluation of the high number of data. (orig.) [de

An assessment of the dilution required to mitigate Hanford tank 241-SY-101

International Nuclear Information System (INIS)

Hudson, J.D.; Bredt, P.R.; Felmy, A.R.; Stewart, C.W.; Tingey, J.M.; Trent, D.S.; Barney, G.S.; Herting, D.L.; Larrick, A.P.; Reynolds, D.A.

1995-02-01

A group of experts from PNL and WHC convened November 2 and 3, 1994, to screen the current state of knowledge about dilution and reach a consensus on the minimum dilution ratio that will achieve passive mitigation of Tank 241-SY-101 wastes and the dilution ratio that would satisfy the given cross-site transfer criteria with reasonable assurance. The panel evaluated the effects of dilution on the parameters important in gas generation, retention, and release and reached the following conclusions, which are deduced from the existing body of data, experience, and analyses: (1) Dissolution of solids is the single most important aspect of mitigation by dilution. We are confident that diluting until nitrates, nitrites, and aluminum salts are dissolved will mitigate Hanford flammable gas tanks; (2) Sufficient solids dissolution can be achieved in Tank 241-SY-101 at a dilution ratio of 1:1, which will result in a average specific gravity of approximately 1.35. It is likely that a 0.5:1 dilution will also mitigate 241-SY-101, but the current uncertainty is too high to recommend this dilution ratio; (3) The recommended dilution requires a diluent with at least 2 molar free hydroxide, because aluminum probably precipitates at lower hydroxide concentrations. The transfer criteria for Tank 241-SY-101 waste were also evaluated. These criteria have been specified as solids content ≤30% (volume), viscosity ≤30% cP and density <1.5 g/mL. (1) Solids content is the limiting criterion if it is defined as volume fraction of settled solids. A 1:1 dilution will satisfy this criterion at nominal premixing conditions in Tank 241-SY-101; however, analysis of Window E core samples suggests that up to 1.5:1 might be required. If the solids content is interpreted simply as solids volume fraction no further dilution is necessary, because Tank 241-SY-101 waste (excluding the crust) is already below 30%; (2) Bulk density is the next limiting criterion and is met at 0.4:1 dilution

Method and apparatus maintaining multi-component sample gas constituents in vapor phase during sample extraction and cooling

Science.gov (United States)

Farthing, William Earl; Felix, Larry Gordon; Snyder, Todd Robert

2009-12-15

An apparatus and method for diluting and cooling that is extracted from high temperature and/or high pressure industrial processes. Through a feedback process, a specialized, CFD-modeled dilution cooler is employed along with real-time estimations of the point at which condensation will occur within the dilution cooler to define a level of dilution and diluted gas temperature that results in a gas that can be conveyed to standard gas analyzers that contains no condensed hydrocarbon compounds or condensed moisture.

Mixotrophic growth and biochemical analysis of Chlorella vulgaris cultivated with diluted monosodium glutamate wastewater.

Science.gov (United States)

Ji, Yan; Hu, Wenrong; Li, Xiuqing; Ma, Guixia; Song, Mingming; Pei, Haiyan

2014-01-01

Monosodium glutamate wastewater (MSGW) is a potential medium for microbial cultivation because of containing abundant organic nutrient. This paper seeks to evaluate the feasibility of growing Chlorella vulgaris with MSGW and assess the influence of MSGW concentration on the biomass productivity and biochemical compositions. The MSGW diluted in different concentrations was prepared for microalga cultivation. C. vulgaris growth was greatly promoted with MSGW compared with the inorganic BG11 medium. C. vulgaris obtained the maximum biomass concentration (1.02 g/L) and biomass productivity (61.47 mg/Ld) with 100-time diluted MSGW. The harvested biomass was rich in protein (36.01-50.64%) and low in lipid (13.47-25.4%) and carbohydrate (8.94-20.1%). The protein nutritional quality and unsaturated fatty acids content of algal increased significantly with diluted MSGW. These results indicated that the MSGW is a feasible alternative for mass cultivation of C. vulgaris. Copyright © 2013 Elsevier Ltd. All rights reserved.

Dilution Refrigeration of Multi-Ton Cold Masses

CERN Document Server

Wikus, P; CERN. Geneva

2007-01-01

Dilution refrigeration is the only means to provide continuous cooling at temperatures below 250 mK. Future experiments featuring multi-ton cold masses require a new generation of dilution refrigeration systems, capable of providing a heat sink below 10 mK at cooling powers which exceed the performance of present systems considerably. This thesis presents some advances towards dilution refrigeration of multi-ton masses in this temperature range. A new method using numerical simulation to predict the cooling power of a dilution refrigerator of a given design has been developed in the framework of this thesis project. This method does not only allow to take into account the differences between an actual and an ideal continuous heat exchanger, but also to quantify the impact of an additional heat load on an intermediate section of the dilute stream. In addition, transient behavior can be simulated. The numerical model has been experimentally verified with a dilution refrigeration system which has been designed, ...

Validation of multi-element isotope dilution ICPMS for the analysis of basalts

Energy Technology Data Exchange (ETDEWEB)

Willbold, M.; Jochum, K.P.; Raczek, I.; Amini, M.A.; Stoll, B.; Hofmann, A.W. [Max-Planck-Institut fuer Chemie, Mainz (Germany)

2003-09-01

In this study we have validated a newly developed multi-element isotope dilution (ID) ICPMS method for the simultaneous analysis of up to 12 trace elements in geological samples. By evaluating the analytical uncertainty of individual components using certified reference materials we have quantified the overall analytical uncertainty of the multi-element ID ICPMS method at 1-2%. Individual components include sampling/weighing, purity of reagents, purity of spike solutions, calibration of spikes, determination of isotopic ratios, instrumental sources of error, correction of mass discrimination effect, values of constants, and operator bias. We have used the ID-determined trace elements for internal standardization to improve indirectly the analysis of 14 other (mainly mono-isotopic trace elements) by external calibration. The overall analytical uncertainty for those data is about 2-3%. In addition, we have analyzed USGS and MPI-DING geological reference materials (BHVO-1, BHVO-2, KL2-G, ML3B-G) to quantify the overall bias of the measurement procedure. Trace element analysis of geological reference materials yielded results that agree mostly within about 2-3% relative to the reference values. Since these results match the conclusions obtained by the investigation of the overall analytical uncertainty, we take this as a measure for the validity of multi-element ID ICPMS. (orig.)

Comparative determination of sucrose content in sugar beet by polarimetric and isotope dilution methods

Energy Technology Data Exchange (ETDEWEB)

Malec, K; Szuchnik, A [Institute of Nuclear Research, Warsaw (Poland); Rydel, S; Walerianaczyk, E [Instytut Przemyslu Cukrowniczego, Warsaw (Poland)

1976-01-01

The comparative determination of sucrose content in sugar beets has been investigated by following methods: polarimetric, direct isotope dilution and double carrier-isotope dilution analysis. Basing upon the obtained results it has been ascertained, that in the case of worse quality beets the polarimetric determinations differ greatly from isotopic data.

The effect of boron dilution transient on the VVER-1000 reactor core using MCNP and COBRA-EN codes

Energy Technology Data Exchange (ETDEWEB)

Jafari, Naser; Talebi, Saeed [Amirkabir Univ. of Technology, Tehran Polytechnic (Iran, Islamic Republic of). Dept. of Energy Engineering and Physics

2017-07-15

In this paper, the effect of boron dilution transient, as a consequence of the malfunction of the boron control system, was investigated in a VVER-1000 reactor, and then an appropriate setpoint was determined for the actuation of the emergency protection system to the reactor shutdown. In order to simulate the boron dilution, first, the whole reactor core was simulated by MCNPX code to compute the radial and axial power distribution. Then, the COBRA-EN code was employed using calculated power distribution for analyzing the thermal-hydraulic of hot fuel assembly and for extracting the safety parameters. For the safe operation of the reactor, certain parameters must be in defined specified ranges. Comparison between our results and FSARs data shows that the present modeling provides a good prediction of boron dilution transient with the maximum relative difference about 4%.

Uranium extraction in phosphoric acid

International Nuclear Information System (INIS)

Araujo Figueiredo, C. de

1984-01-01

Uranium is recovered from the phosphoric liquor produced from the concentrate obtained from phosphorus-uraniferous mineral from Itataia mines (CE, Brazil). The proposed process consists of two extraction cycles. In the first one, uranium is reduced to its tetravalent state and then extracted by dioctylpyrophosphoric acid, diluted in Kerosene. Re-extraction is carried out with concentrated phosphoric acid containing an oxidising agent to convert uranium to its hexavalent state. This extract (from the first cycle) is submitted to the second cycle where uranium is extracted with DEPA-TOPO (di-2-hexylphosphoric acid/tri-n-octyl phosphine oxide) in Kerosene. The extract is then washed and uranium is backextracted and precipitated as commercial concentrate. The organic phase is recovered. Results from discontinuous tests were satisfactory, enabling to establish operational conditions for the performance of a continuous test in a micro-pilot plant. (Author) [pt

Criticality of the D=2 bond-dilute anisotropic Heisenberg ferromagnet

International Nuclear Information System (INIS)

Mariz, A.M.; Tsallis, C.; Caride, A.O.

1984-01-01

The critical frontier and critical exponents associated with the quenched bond-dilute quantum anisotropic spin 1/2 Heisenberg ferromagnet in square lattice are described. To perform the calculations, an approximate real-space renormalization-group framework recently developed by some of us for the pure model (and analysed with some detail) is extended. Whenever comparison with available exact results is possible, the agreement is either perfect or quite satisfactory. Some effort has been dedicated to extract the main asymptotic behaviours of the critical frontier. Also several interesting quantum effects appearing in the composition laws of (Heisenberg) bond arrays are exhibited. (Author) [pt

Smart Extraction and Analysis System for Clinical Research.

Science.gov (United States)

Afzal, Muhammad; Hussain, Maqbool; Khan, Wajahat Ali; Ali, Taqdir; Jamshed, Arif; Lee, Sungyoung

2017-05-01

With the increasing use of electronic health records (EHRs), there is a growing need to expand the utilization of EHR data to support clinical research. The key challenge in achieving this goal is the unavailability of smart systems and methods to overcome the issue of data preparation, structuring, and sharing for smooth clinical research. We developed a robust analysis system called the smart extraction and analysis system (SEAS) that consists of two subsystems: (1) the information extraction system (IES), for extracting information from clinical documents, and (2) the survival analysis system (SAS), for a descriptive and predictive analysis to compile the survival statistics and predict the future chance of survivability. The IES subsystem is based on a novel permutation-based pattern recognition method that extracts information from unstructured clinical documents. Similarly, the SAS subsystem is based on a classification and regression tree (CART)-based prediction model for survival analysis. SEAS is evaluated and validated on a real-world case study of head and neck cancer. The overall information extraction accuracy of the system for semistructured text is recorded at 99%, while that for unstructured text is 97%. Furthermore, the automated, unstructured information extraction has reduced the average time spent on manual data entry by 75%, without compromising the accuracy of the system. Moreover, around 88% of patients are found in a terminal or dead state for the highest clinical stage of disease (level IV). Similarly, there is an ∼36% probability of a patient being alive if at least one of the lifestyle risk factors was positive. We presented our work on the development of SEAS to replace costly and time-consuming manual methods with smart automatic extraction of information and survival prediction methods. SEAS has reduced the time and energy of human resources spent unnecessarily on manual tasks.

The isolation and the separation of Sm, Gd, Dy by extraction

International Nuclear Information System (INIS)

Biyantoro, D.; Lahagu, F.; Basuki, K.T.; Handini, T.; Rosyidin

1996-01-01

The isolation of yttrium and separation of Sm, Gd, y with extraction has been investigated. The steps of the process include of this research were the production the concentrate of lanthanide, the dilution, the isolation of yttrium, and the separation of the Sm, Gd, Dy. The first step was the digestion of xenotime sand, the extraction, the dilution, the filtration, the precipitation, the baking production a lanthanide oxide. The step was the separation of yttrium, the stripping, and the calcination production of yttrium oxide. And the third process was the separation of Sm, Gd, Dy by extraction process using method liquid-liquid extraction with extractant of D 2 EHPA and a solvent of dodecane. From the result have been found concentration of yttrium oxide = 88,71 %. The optimum condition of the separation of Gd/Dy have been found : the concentration of HNO 3 = 0,5 M, time of extraction = 15 minutes, and the concentration of extractant = 30 % D 2 EHPA in dodecane. The results of this condition were the distribution coefficient of Gd = 2,226, the distribution coefficient of Dy = 3,762, and the separation factor of Gd/Dy = 0,592. (author)

A simplified extraction schema to for the analytical characterization of apple orchard soils

Science.gov (United States)

Sager, Manfred

2014-05-01

In agriculture, soil analysis is mainly done to monitor available nutrients as well contaminants, in order to find the optimum fertilization resp. remediation strategy. Traditionally, available nutrients in soils have been obtained from a series of different extractions, some just for one single parameter. In order to simplify the entire procedures, multi-element techniques, like ICP-OES and ICP-MS, have been applied to a sequence of extracts obtained with 0,16M acetic acid and 0,1M oxalate buffer pH 3, which are more suitable for the plasma than traditional salt extractant solutions. Dilute acetic acid should characterize exchangeables plus carbonates, and oxalate buffer the pedogenic oxides. Aqua regia extractions in glass have been replaced by pressure digestion with KClO3 in dilute nitric acid, which yields results equivalent to aqua regia, and additionally permits the determination of total sulfur, as well as acid-leachable boron and silicon. Total digestion was done in PTFE beakers by fuming with HNO3/HClO4, subsequently with HF, and final uptake in 1+1 HCl. The results of total digestion could be verified by XRF analysis of the solid, Ti recovery was the most critical item. The method was applied to 34 soils from apple orchards of different soil types and climatic zones. P and K obtained from standard acetate-lactate extract as well as B obtained from the Baron extract correlated with the results from the acetic acid extract better than 0,9. Just Mg from the CaCl2 extract (Schachtschabel) was independent from all other Mg fractions. The results for Ca, Cu, Mg, Mn, Sr, Pb and Zn obtained from KClO3 digest and from totals, were strongly correlated. The Rare Earth elements formed a strongly intercorrelated group as well after total digestion as in the oxalate leach. Factor analysis was utilized to prove if the obtained fractions part into groups in a geochemically feasible way. The fraction mobilized by dilute acetic acid contained Ca-Mg-carbonates as well as

Method and apparatus for maintaining multi-component sample gas constituents in vapor phase during sample extraction and cooling

Science.gov (United States)

Farthing, William Earl [Pinson, AL; Felix, Larry Gordon [Pelham, AL; Snyder, Todd Robert [Birmingham, AL

2008-02-12

An apparatus and method for diluting and cooling that is extracted from high temperature and/or high pressure industrial processes. Through a feedback process, a specialized, CFD-modeled dilution cooler is employed along with real-time estimations of the point at which condensation will occur within the dilution cooler to define a level of dilution and diluted gas temperature that results in a gas that can be conveyed to standard gas analyzers that contains no condensed hydrocarbon compounds or condensed moisture.

A comparison of accelerated solvent extraction, Soxhlet extraction, and ultrasonic-assisted extraction for analysis of terpenoids and sterols in tobacco.

Science.gov (United States)

Shen, Jinchao; Shao, Xueguang

2005-11-01

The performance of accelerated solvent extraction in the analysis of terpenoids and sterols in tobacco samples was investigated and compared with those of Soxhlet extraction and ultrasonically assisted extraction with respect to yield, extraction time, reproducibility and solvent consumption. The results indicate that although the highest yield was achieved by Soxhlet extraction, ASE appears to be a promising alternative to classical methods since it is faster and uses less solvent, especially when applied to the investigation of large batch tobacco samples. However, Soxhlet extraction is still the preferred method for analyzing sterols since it gives a higher extraction efficiency than other methods.

Simple and accurate measurement of carbamazepine in surface water by use of porous membrane-protected micro-solid-phase extraction coupled with isotope dilution mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Teo, Hui Ling [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543 (Singapore); Wong, Lingkai [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Liu, Qinde, E-mail: liu_qinde@hsa.gov.sg [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Teo, Tang Lin; Lee, Tong Kooi [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Lee, Hian Kee, E-mail: chmleehk@nus.edu.sg [Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543 (Singapore)

2016-03-17

To achieve fast and accurate analysis of carbamazepine in surface water, we developed a novel porous membrane-protected micro-solid-phase extraction (μ-SPE) method, followed by liquid chromatography-isotope dilution tandem mass spectrometry (LC-IDMS/MS) analysis. The μ-SPE device (∼0.8 × 1 cm) was fabricated by heat-sealing edges of a polypropylene membrane sheet to devise a bag enclosing the sorbent. The analytes (both carbamazepine and isotope-labelled carbamazepine) were first extracted by μ-SPE device in the sample (10 mL) via agitation, then desorbed in an organic solvent (1 mL) via ultrasonication. Several parameters such as organic solvent for pre-conditioning of μ-SPE device, amount of sorbent, adsorption time, and desorption solvent and time were investigated to optimize the μ-SPE efficiency. The optimized method has limits of detection and quantitation estimated to be 0.5 ng L{sup −1} and 1.6 ng L{sup −1}, respectively. Surface water samples spiked with different amounts of carbamazepine (close to 20, 500, and 1600 ng L{sup −1}, respectively) were analysed for the validation of method precision and accuracy. Good precision was obtained as demonstrated by relative standard deviations of 0.7% for the samples with concentrations of 500 and 1600 ng kg{sup −1}, and 5.8% for the sample with concentration of 20 ng kg{sup −1}. Good accuracy was also demonstrated by the relative recoveries in the range of 96.7%–103.5% for all samples with uncertainties of 1.1%–5.4%. Owing to the same chemical properties of carbamazepine and isotope-labelled carbamazepine, the isotope ratio in the μ-SPE procedure was accurately controlled. The use of μ-SPE coupled with IDMS analysis significantly facilitated the fast and accurate measurement of carbamazepine in surface water. - Highlights: • μ-SPE coupled with IDMS for the measurement of carbamazepine. • The method is the first report of coupling μ-SPE with IDMS. • μ-SPE is fast, time

Mass spectrometic isotope dilution analysis of Am and Cm in spent fuels

International Nuclear Information System (INIS)

Wantschik, M.; Koch, L.; Commission of the European Communities, Karlsruhe; Ganser, B.

1983-01-01

Spent nuclear fuels contain Am and Cm in the 10 ppb to 100 ppm range. Because of this low abundance and the necessity of handling small samples of the highly toxic fuel material only a mass-spectrometric isotope dilution analysis can give sufficiently accurate results. Since suitable spikes and/or standards have been lacking, this method has not been applied. Using known masses (+- 0.1%) of Am-241 and Cm-244 metal, Am-243 and Cm-248 spikes were calibrated to an accuracy of better than 0.2%. The standards were reanalysed by chemical titration and several radiometric techniques. The chemical conditioning is based on ionexchange chromatography with alpha-hydroxyisobutyric acid. A sample size of 10 -7 g is sufficient. For the mass-spectrometric measurement 10 -9 g of the elements are required. The accuracy for the determination of the main isotope is 0.5%. (orig./BRB)

Analysis of 99Tc in the radioactive liquid waste after extraction into suitable solvent

International Nuclear Information System (INIS)

Sonar, N.L.; Vaishali De; Pardeshi, V.; Raghvendra, Y.; Valsala, T.P.; Sonavane, M.S.; Kulkarni, Y.; Raj Kanwar

2012-01-01

99 Tc is one of the long lived fission product with high fission yield. >From radioactive waste management point of view it is very much essential to evaluate the concentration of technetium in the radioactive liquid waste in order to finalise the treatment process to extract/isolate it from the stream which is discharged to the environment. For the estimation of 99 Tc in the radioactive liquid waste stream, extraction of the stable complex of technetium-tetraphenyl arsonium chloride (TPAC) into chloroform followed by beta counting was studied. Various parameters like pH, time of equilibration, concentration of TPAC in chloroform, use of other solvent for extraction as well as interference of various other radionuclides present in the waste were also studied. The radioactive liquid waste being handled in plant contains high concentrations of salts in the form of sodium nitrate. Hence effect of salt concentration on the percentage extraction was also evaluated. The extraction behavior does not dependent on change in the pH of the solution. Almost 99.5% extraction was observed in the pH range of 1-13.0. High concentration of salt is affecting the extraction. However, this can be taken care by diluting the radioactive waste. It takes almost 90 min time for maximum extraction. Presence of radionuclides like 137 Cs, 90 Sr are not interfering the extraction of 99 Tc. However, 106 Ru is getting slightly extracted along with 99 Tc. The error due to 106 Ru can be eliminated by taking gamma spectrum and deducting the activity from the total beta activity to get 99 Tc activity. Nitrobenzene can be used for extraction of Tc-TPAC complex in place of chloroform. (author)

Isotope dilution analysis for urinary fentanyl and its main metabolite, norfentanyl, in patients by isotopic fractionation using capillary gas chromatography

Energy Technology Data Exchange (ETDEWEB)

Sera, Shoji; Goromaru, Tsuyoshi [Fukuyama Univ., Hiroshima (Japan). Faculty of Pharmacy and Pharmaceutical Sciences; Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki

1998-07-01

Isotope dilution analysis was applied to determine urinary excretion of fentanyl (FT) and its main metabolite, norfentanyl (Nor-FT), by isotopic fractionation using a capillary gas chromatograph equipped with a surface ionization detector (SID). Urinary FT was determined quantitatively in the range of 0.4-40 ng/ml using deuterium labeled FT (FT-{sup 2}H{sub 19}), as an internal standard. We also performed isotope dilution analysis of Nor-FT in urine. N-Alkylation was necessary to sensitively detect Nor-FT with SID. Methyl derivative was selected from 3 kinds of N-alkyl derivatives to increase sensitivity and peak resolution, and to prevent interference with urinary compound. Nor-FT concentration was quantitatively determined in the range of 10-400 ng/ml using deuterium labeled Nor-FT (Nor-FT-{sup 2}H{sub 10}). No endogenous compounds or concomitant drugs interfered with the detection of FT and Nor-FT in the urine of patients. The present method will be useful for pharmacokinetic studies and the evaluation of drug interactions in FT metabolism. (author)

Isotope dilution analysis for urinary fentanyl and its main metabolite, norfentanyl, in patients by isotopic fractionation using capillary gas chromatography

International Nuclear Information System (INIS)

Sera, Shoji; Goromaru, Tsuyoshi; Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki

1998-01-01

Isotope dilution analysis was applied to determine urinary excretion of fentanyl (FT) and its main metabolite, norfentanyl (Nor-FT), by isotopic fractionation using a capillary gas chromatograph equipped with a surface ionization detector (SID). Urinary FT was determined quantitatively in the range of 0.4-40 ng/ml using deuterium labeled FT (FT- 2 H 19 ), as an internal standard. We also performed isotope dilution analysis of Nor-FT in urine. N-Alkylation was necessary to sensitively detect Nor-FT with SID. Methyl derivative was selected from 3 kinds of N-alkyl derivatives to increase sensitivity and peak resolution, and to prevent interference with urinary compound. Nor-FT concentration was quantitatively determined in the range of 10-400 ng/ml using deuterium labeled Nor-FT (Nor-FT- 2 H 10 ). No endogenous compounds or concomitant drugs interfered with the detection of FT and Nor-FT in the urine of patients. The present method will be useful for pharmacokinetic studies and the evaluation of drug interactions in FT metabolism. (author)

Multi-element determination in environmental samples by mass spectrometric isotope dilution analysis using thermal ionization. Pt. 2

International Nuclear Information System (INIS)

Hilpert, K.; Waidmann, E.

1988-01-01

An analytical procedure for the multi-element analysis of the elements Fe, Ni, Cu, Zn, Ga, Rb, Sr, Cd, Ba, Tl, and Pb in pine needles by mass spectrometric isotope dilution analysis using thermal ionization has been reported in Part I of this paper. This procedure is now transferred to the non-vegetable material 'Oyster Tissue' (Standard Reference Material 1566, National Bureau of Standards, USA). By a modification of the analytical procedure, it was possible to determine Cr in this material in addition to the aforementioned elements. No concentrations are certified for the elements Ga, Ba and Tl analyzed in this work. The concentrations of the remaining elements obtained by the multi-element analysis agree well with those certified. (orig.)

Anthelminthic efficacy of aqueous extracts of Garcina kola seed and ...

African Journals Online (AJOL)

At the 100mg/ml concentration of each extract, the reduction in egg hatch was comparable to those obtained with various dilutions of levamisole and albendazole both of which showed 100% reduction in egg hatch. The extracts therefore showed promise for use as possible anthelminthic for the regular treatment and control ...

Extraction of iron(III) with diphenyl-2-pyridylmethane dissolved in benzene from aqueous chloride solutions

International Nuclear Information System (INIS)

Suhail Ahmed; Shamas-Ud-Zuha; Abdul Ghafoor; Ejaz, M.

1978-01-01

The mechanism of extraction has been investigated by partition, slope analysis and loading-ratio data. The results obtained give a picture of the mechanism of extraction of FeCl 4 - ions in relation to the hydration and solvation of the compound extracted. The possible formula of the extracted species is (DPPM)sub(3)Hsub(3)Osup(+)(Hsub(2)O)sub(n)-FeClsub(4)sup(-). In dilute aqueous hydrochloric acid systems the influence of the concentration of a number of salts with cations of different electrical potentials (Ze/r), on iron(III) extraction, has been studied. Splitting of the organic phases occurs at high acid and/or high salt concentrations. The phenomenon is explained on the basis of the variability of the hydration number. Investigations have been made to understand the parameters controlling the extraction of the metal and it is shown that the extraction offers a simple, fast and selective separation method of iron from solutions. (author)

Nutritional assessment by isotope dilution analysis of body composition

International Nuclear Information System (INIS)

Szeluga, D.J.; Stuart, R.K.; Utermohlen, V.; Santos, G.W.

1984-01-01

The three components of body mass, body cell mass (BCM), extracellular fluid (ECF), and fat + extracellular solids (ECS: bone, tendon, etc) can be quantified using established isotope dilution techniques. With these techniques, total body water (TBW) and ECF are measured using 3H 2 O and 82 Bromine, respectively, as tracers. BCM is calculated from intracellular fluid (ICF) where ICF . TBW - ECF. Fat + ECS is estimated as: body weight - (BCM + ECF). TBW and ECF can be determined by either of two calculation methods, one requiring several timed plasma samples (extrapolation method) and one requiring a single plasma sample and a 4-h urine collection (urine-corrected method). The comparability of the two calculation methods was evaluated in 20 studies in 12 bone marrow transplant recipients. We found that for determination of TBW and ECF there was a very strong linear relationship (r2 greater than 0.98) between the calculation methods. Further comparisons (by t test, 2-sided) indicated that for the determination of ECF, the methods were not significantly (p greater than 0.90) different; however, TBW determined by the urine-corrected method was slightly (0.1 to 6%), but significantly (p less than 0.01) greater than that determined by the extrapolation method. Therefore, relative to the extrapolation method, the urine-corrected method ''over-estimates'' BCM and ''under-estimates'' fat + ECS since determination of these compartment sizes depends on measurement of TBW. We currently use serial isotope dilution studies to monitor the body composition changes of patients receiving therapeutic nutritional support

Theoretical modeling of diluted antiferromagnetic systems

International Nuclear Information System (INIS)

Pozo, J; Elgueta, R; Acevedo, R

2000-01-01

Some magnetic properties of a Diluted Antiferromagnetic System (DAFS) are studied. The model of the two sub-networks for antiferromagnetism is used and a Heisenberg Hamiltonian type is proposed, where the square operators are expressed in terms of boson operators with the approach of spin waves. The behavior of the diluted system's fundamental state depends basically on the competition effect between the anisotropy field and the Weiss molecular field. The approach used allows the diluted system to be worked for strong anisotropies as well as when these are very weak

Antioxidant activity of aqueous extract of noni in dilutent for ram semen cryopreservation

Directory of Open Access Journals (Sweden)

Ana Lauren Costa Nascimento

2016-03-01

Full Text Available Noni (Morinda citrifolia L. is a fruit consumed worldwide because of its nutritional and therapeutic properties resulting from the large amount of phenolic compounds, which has aroused interest of the scientific community. In order to identify new natural sources of antioxidants, the objective of this study was to evaluate the performance of noni in diluent for ram semen cryopreservation. A completely randomized design consisting of four treatments and three repetitions per treatment was used. The treatments differed in terms of the concentration of the aqueous extract of noni added to the diluent: control, no addition of the extract, and three concentrations (24, 72, and 120 µg/mL. The physical and chemical variables of the mature fruit were evaluated: total acidity (8.78, pH (4.12, and soluble solids (8.18%. The vitamin C content was 309.42 mg per 100 g fresh matter. The aqueous extract of noni was also evaluated regarding the quantity of total phenolic compounds, antioxidant activity, and lipid peroxidation inhibition capacity. The aqueous extract contained a moderate amount of phenolic compounds (47.96 ± 1.95 mg gallic acid equivalent/100 g extract. The concentrations of the aqueous extract of 72 and 120 µg/mL in diluent used for semen cryopreservation inhibited lipid peroxidation by 21.75% and 51.32%, respectively. There was no positive effect of the lowest concentration (24 µg/mL. The antioxidant activity index of noni was 33.33, corresponding to very strong antioxidant activity. The aqueous extract of noni exhibits very strong antioxidant activity and its addition to the diluent for semen cryopreservation at a concentration of 72 µg/mL is able to inhibit lipid peroxidation.

Water Stress Scatters Nitrogen Dilution Curves in Wheat

Directory of Open Access Journals (Sweden)

Marianne Hoogmoed

2018-04-01

Full Text Available Nitrogen dilution curves relate a crop’s critical nitrogen concentration (%Nc to biomass (W according to the allometric model %Nc = a W-b. This model has a strong theoretical foundation, and parameters a and b show little variation for well-watered crops. Here we explore the robustness of this model for water stressed crops. We established experiments to examine the combined effects of water stress, phenology, partitioning of biomass, and water-soluble carbohydrates (WSC, as driven by environment and variety, on the %Nc of wheat crops. We compared models where %Nc was plotted against biomass, growth stage and thermal time. The models were similarly scattered. Residuals of the %Nc - biomass model at anthesis were positively related to biomass, stem:biomass ratio, Δ13C and water supply, and negatively related to ear:biomass ratio and concentration of WSC. These are physiologically meaningful associations explaining the scatter of biomass-based dilution curves. Residuals of the thermal time model showed less consistent associations with these variables. The biomass dilution model developed for well-watered crops overestimates nitrogen deficiency of water-stressed crops, and a biomass-based model is conceptually more justified than developmental models. This has implications for diagnostic and modeling. As theory is lagging, a greater degree of empiricism might be useful to capture environmental, chiefly water, and genotype-dependent traits in the determination of critical nitrogen for diagnostic purposes. Sensitivity analysis would help to decide if scaling nitrogen dilution curves for crop water status, and genotype-dependent parameters are needed.

Comparison of dilution factors for German wastewater treatment plant effluents in receiving streams to the fixed dilution factor from chemical risk assessment.

Science.gov (United States)

Link, Moritz; von der Ohe, Peter C; Voß, Katharina; Schäfer, Ralf B

2017-11-15

Incomplete removal during wastewater treatment leads to frequent detection of compounds such as pharmaceuticals and personal care products in municipal effluents. A fixed standard dilution factor of 10 for effluents entering receiving water bodies is used during the exposure assessment of several chemical risk assessments. However, the dilution potential of German receiving waters under low flow conditions is largely unknown and information is sparse for other European countries. We calculated dilution factors for two datasets differing in spatial extent and wastewater treatment plant (WWTP) size: a national dataset comprising 1225 large WWTPs in Central and Northern Germany and a federal dataset for 678 WWTPs of a single state in Southwest Germany. We found that the fixed factor approach overestimates the dilution potential of 60% and 40% of receiving waters in the national and the federal dataset, with median dilution factors of 5 and 14.5, respectively. Under mean flow conditions, 8% of calculated dilution factors were below 10, with a median dilution factor of 106. We also calculated regional dilution factors that accounted for effluent inputs from upstream WWTPs. For the national and the federal dataset, 70% and 60% of calculated regional dilution factors fell below 10 under mean low flow conditions, respectively. Decrease of regional dilution potential in small receiving streams was mainly driven by the next WWTP upstream with a 2.5 fold drop of median regional dilution factors. Our results show that using the standard dilution factor of 10 would result in the underestimation of environmental concentrations for authorised chemicals by a factor of 3-5 for about 10% of WWTPs, especially during low flow conditions. Consequently, measured environmental concentrations might exceed predicted environmental concentrations and ecological risks posed by effluents could be much higher, suggesting that a revision of current risk assessment practices may be required

Dilute acid/metal salt hydrolysis of lignocellulosics

Science.gov (United States)

Nguyen, Quang A.; Tucker, Melvin P.

2002-01-01

A modified dilute acid method of hydrolyzing the cellulose and hemicellulose in lignocellulosic material under conditions to obtain higher overall fermentable sugar yields than is obtainable using dilute acid alone, comprising: impregnating a lignocellulosic feedstock with a mixture of an amount of aqueous solution of a dilute acid catalyst and a metal salt catalyst sufficient to provide higher overall fermentable sugar yields than is obtainable when hydrolyzing with dilute acid alone; loading the impregnated lignocellulosic feedstock into a reactor and heating for a sufficient period of time to hydrolyze substantially all of the hemicellulose and greater than 45% of the cellulose to water soluble sugars; and recovering the water soluble sugars.

Process for recovery and purification of lithium from dilute sources

International Nuclear Information System (INIS)

Kunugita, Eiichi; Kim, Jong-Hwa; Komasawa, Isao

1990-01-01

A process was studied for recovery and purification of lithium from hot spring water and leachate of coal fly ash in which lithium is present at very low concentration in a mixture of high concentration of less desirable species such as alkali metals, alkaline earth metals and others. Lithium is, as a first step, adsorbed selectively by an ion-sieve type adsorbent, λ-MnO 2 , which can effect separation by adsorbing lithium alone in its intraparticle spaces while adsorbing most metals on its surface. Stagewise elutions are performed, employing two elutrients: NH 4 NO 3 and then HNO 3 solution. The concentration ratio of lithium and sodium is 1/70∼1/120 in the original feed stream, and this is upgraded to 300/1 in the pregnant elutrient. Some impurities in the pregnant elutrient is removed by a solvent extraction technique, employing a mixed extractant of a β-diketone (LIX51) and tri-n-octyl-phosphine oxide in kerosene. A lithium solution with an undetectable amount of impurities is obtained by single extraction followed by single scrubbing with dilute hydrochloric acid of carefully controlled concentration. (author)

Efficacy of aqueous and ethanolic extracts of leaves of Chromolaena ...

African Journals Online (AJOL)

Otarigho Benson

The molluscicidal activities of aqueous and ethanolic extracts of leaves of Chromolaena odorata were investigated on adult, one week old juveniles and 3 to 4 days old egg-masses of Biomphalaria pfeifferi. Ten adults each were exposed to a serial dilution of 40, 80, 160, 240, 320, 400, and 480 ppm distilled water extracts ...

Analysis of Intracellular Metabolites from Microorganisms: Quenching and Extraction Protocols.

Science.gov (United States)

Pinu, Farhana R; Villas-Boas, Silas G; Aggio, Raphael

2017-10-23

Sample preparation is one of the most important steps in metabolome analysis. The challenges of determining microbial metabolome have been well discussed within the research community and many improvements have already been achieved in last decade. The analysis of intracellular metabolites is particularly challenging. Environmental perturbations may considerably affect microbial metabolism, which results in intracellular metabolites being rapidly degraded or metabolized by enzymatic reactions. Therefore, quenching or the complete stop of cell metabolism is a pre-requisite for accurate intracellular metabolite analysis. After quenching, metabolites need to be extracted from the intracellular compartment. The choice of the most suitable metabolite extraction method/s is another crucial step. The literature indicates that specific classes of metabolites are better extracted by different extraction protocols. In this review, we discuss the technical aspects and advancements of quenching and extraction of intracellular metabolite analysis from microbial cells.

Determination of total cyanide in soil by isotope dilution GC/MS following pentafluorobenzyl derivatization

Energy Technology Data Exchange (ETDEWEB)

Campanella, Beatrice, E-mail: beatrice.campanella@pi.iccom.cnr.it [Università di Pisa, Dipartimento di Chimica e Chimica Industriale, via Moruzzi 13, 56124 Pisa (Italy); Consiglio Nazionale delle Ricerche (CNR), Istituto di Chimica dei Composti Organometallici, UOS di Pisa, via Moruzzi 1, 56124 Pisa (Italy); Biancalana, Lorenzo [Università di Pisa, Dipartimento di Chimica e Chimica Industriale, via Moruzzi 13, 56124 Pisa (Italy); D' Ulivo, Lucia [National Research Council of Canada, 1200 Montreal Road, Ottawa, ON K1A 0R6 (Canada); Onor, Massimo; Bramanti, Emilia [Consiglio Nazionale delle Ricerche (CNR), Istituto di Chimica dei Composti Organometallici, UOS di Pisa, via Moruzzi 1, 56124 Pisa (Italy); Mester, Zoltan; Pagliano, Enea [National Research Council of Canada, 1200 Montreal Road, Ottawa, ON K1A 0R6 (Canada)

2017-04-08

The high toxicity of cyanide, along with its widespread industrial use, has fuelled interest in the development of analytical methods for its determination in complex matrices. In this study, we propose a novel approach for the measurement of total cyanide in soil samples based on single-step derivatization with pentafluorobenzyl bromide (F{sub 5}Bn−Br) followed by quantitation with gas chromatography mass spectrometry in negative chemical ionization mode. The reaction between CN{sup −} and F{sub 5}Bn−Br resulted in the identification of several derivatives such as F{sub 5}Bn−CN, (F{sub 5}Bn)(F{sub 5}Ph)CH−CN, and (F{sub 5}Bn){sub 2}(F{sub 5}Ph)C−CN. The relative proportion between such compounds was dependent on experimental conditions. When a 100 μL aliquot of an alkaline-aqueous extract was reacted with 700 μL of 1.3% F{sub 5}Bn−Br in acetone, the tri-alkylated derivative was the most abundant. In such conditions a detection limit of 0.5 ng/g of CN{sup −} was attained. Soil samples were initially spiked with an alkaline solution of K{sup 13}C{sup 15}N internal standard and suspended in 7.5% aqueous NaOH. Determination of total cyanide was achieved by digestion of the alkaline extract with H{sub 3}PO{sub 4} to produce HCN which was then trapped in 0.1% NaOH in a sealed double vial system, followed by reaction with F{sub 5}Bn−Br. Isotope dilution calibration was chosen for quantitation, and the validity of the novel method was demonstrated by analysis of soil Certified Reference Materials (CRMs) and by spike recovery tests. - Highlights: • A cost-effective, fast and simple method for determination of total cyanide in soil is presented. • A new micro-distillation strategy was developed overcoming the problems of a conventional distillation. • Negative chemical ionization-mass spectrometer has been exploited to obtain a high sensitivity and specificity. • High accuracy was attained for the analysis of certified reference materials with

Dilution thermodynamics of the biologically relevant cation mixtures

International Nuclear Information System (INIS)

Kaczyński, Marek; Borowik, Tomasz; Przybyło, Magda; Langner, Marek

2014-01-01

Graphical abstract: - Highlights: • Dilution energetics of Ca 2+ can be altered by the aqueous phase ionic composition. • Dissipated heat upon Ca 2+ dilution is drastically reduced in the K + presence. • Reduction of the enthalpy change upon Ca 2+ dilution is K + concentration dependent. • The cooperativity of Ca 2+ hydration might be of great biological relevance providing a thermodynamic argument for the specific ionic composition of the intracellular environment. - Abstract: The ionic composition of intracellular space is rigorously controlled by a variety of processes consuming large quantities of energy. Since the energetic efficiency is an important evolutional criterion, therefore the ion fluxes within the cell should be optimized with respect to the accompanying energy consumption. In the paper we present the experimental evidence that the dilution enthalpies of the biologically relevant ions; i.e. calcium and magnesium depend on the presence of monovalent cations; i.e. sodium and potassium. The heat flow generated during the dilution of ionic mixtures was measured with the isothermal titration calorimetry. When calcium was diluted together with potassium the dilution enthalpy was drastically reduced as the function of the potassium concentration present in the solution. No such effect was observed when the potassium ions were substituted with sodium ones. When the dilution of magnesium was investigated the dependence of the dilution enthalpy on the accompanying monovalent cation was much weaker. In order to interpret experimental evidences the ionic cluster formation is postulated. The specific organization of such cluster should depend on ions charges, sizes and organization of the hydration layers

Determination of Glyphosate, its Degradation Product Aminomethylphosphonic Acid, and Glufosinate, in Water by Isotope Dilution and Online Solid-Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry

Science.gov (United States)

Meyer, Michael T.; Loftin, Keith A.; Lee, Edward A.; Hinshaw, Gary H.; Dietze, Julie E.; Scribner, Elisabeth A.

2009-01-01

The U.S. Geological Survey method (0-2141-09) presented is approved for the determination of glyphosate, its degradation product aminomethylphosphonic acid (AMPA), and glufosinate in water. It was was validated to demonstrate the method detection levels (MDL), compare isotope dilution to standard addition, and evaluate method and compound stability. The original method USGS analytical method 0-2136-01 was developed using liquid chromatography/mass spectrometry and quantitation by standard addition. Lower method detection levels and increased specificity were achieved in the modified method, 0-2141-09, by using liquid chromatography/tandem mass spectrometry (LC/MS/MS). The use of isotope dilution for glyphosate and AMPA and pseudo isotope dilution of glufosinate in place of standard addition was evaluated. Stable-isotope labeled AMPA and glyphosate were used as the isotope dilution standards. In addition, the stability of glyphosate and AMPA was studied in raw filtered and derivatized water samples. The stable-isotope labeled glyphosate and AMPA standards were added to each water sample and the samples then derivatized with 9-fluorenylmethylchloroformate. After derivatization, samples were concentrated using automated online solid-phase extraction (SPE) followed by elution in-line with the LC mobile phase; the compounds separated and then were analyzed by LC/MS/MS using electrospray ionization in negative-ion mode with multiple-reaction monitoring. The deprotonated derivatized parent molecule and two daughter-ion transition pairs were identified and optimized for glyphosate, AMPA, glufosinate, and the glyphosate and AMPA stable-isotope labeled internal standards. Quantitative comparison between standard addition and isotope dilution was conducted using 473 samples analyzed between April 2004 and June 2006. The mean percent difference and relative standard deviation between the two quantitation methods was 7.6 plus or minus 6.30 (n = 179), AMPA 9.6 plus or minus 8

Neutron activation analysis for the optimal sampling and extraction of extractable organohalogens in human hari

International Nuclear Information System (INIS)

Zhang, H.; Chai, Z.F.; Sun, H.B.; Xu, H.F.

2005-01-01

Many persistent organohalogen compounds such as DDTs and polychlorinated biphenyls have caused seriously environmental pollution problem that now involves all life. It is know that neutron activation analysis (NAA) is a very convenient method for halogen analysis and is also the only method currently available for simultaneously determining organic chlorine, bromine and iodine in one extract. Human hair is a convenient material to evaluate the burden of such compounds in human body and dan be easily collected from people over wide ranges of age, sex, residential areas, eating habits and working environments. To effectively extract organohalogen compounds from human hair, in present work the optimal Soxhelt-extraction time of extractable organohalogen (EOX) and extractable persistent organohalogen (EPOX) from hair of different lengths were studied by NAA. The results indicated that the optimal Soxhelt-extraction time of EOX and EPOX from human hair was 8-11 h, and the highest EOX and EPOX contents were observed in hair powder extract. The concentrations of both EOX and EPOX in different hair sections were in the order of hair powder ≥ 2 mm > 5 mm, which stated that hair samples milled into hair powder or cut into very short sections were not only for homogeneous. hair sample but for the best hair extraction efficiency.

Kredsløbsmonitorering med lithium dilution cardiac output-systemet

DEFF Research Database (Denmark)

Christiansen, Christian; Hostrup, Anette; Tønnesen, Else

2008-01-01

The lithium dilution cardiac output (LiDCO) system measures cardiac output beat-to-beat with high precision. The system is based on an arterial pulse power analysis which is calibrated every eight hours with a small non-pharmacological dose of lithium. The system is minimally invasive; it requires...

Determination of As concentration in earthworm coelomic fluid extracts by total-reflection X-ray fluorescence spectrometry

Science.gov (United States)

Allegretta, Ignazio; Porfido, Carlo; Panzarino, Onofrio; Fontanella, Maria Chiara; Beone, Gian Maria; Spagnuolo, Matteo; Terzano, Roberto

2017-04-01

Earthworms are often used as sentinel organisms to study As bioavailability in polluted soils. Arsenic in earthworms is mainly sequestrated in the coelomic fluids whose As content can therefore be used to asses As bioavalability. In this work, a method for determining As concentration in coelomic fluid extracts using total-reflection X-ray fluorescence spectrometry (TXRF) is presented. For this purpose coelomic fluid extracts from earthworms living in three polluted soils and one non-polluted (control) soil have been collected and analysed. A very simple sample preparation was implemented, consisting of a dilution of the extracts with polyvinyl alcohol (PVA) using a 1:8 ratio and dropwise deposition of the sample on the reflector. A detection limit of 0.2 μg/l and quantification limit of 0.6 μg/l was obtained in the diluted samples, corresponding to 2 μg/l and 6 μg/l in the coelomic fluid extracts, respectively. This allowed to quantify As concentration in coelomic fluids extracted from earthworms living in soils polluted with As at concentrations higher than 20 mg/kg (considered as a pollution threshold for agricultural soils). The TXRF method has been validated by comparison with As concentrations in standards and by analysing the same samples by ICP-MS, after acid digestion of the sample. The low limit of detection, the proven reliability of the method and the little sample preparation make TXRF a suitable, cost-efficient and "green" technique for the analysis of As in earthworm coelomic fluid extracts for bioavailability studies.

Solvent extraction of no-carrier-added 103Pd from irradiated rhodium target with α-furyldioxime

International Nuclear Information System (INIS)

Mahdi Sadeghi; Behrouz Shirazi; Nami Shadanpour

2006-01-01

Solvent extraction of no-carrier-added 103 Pd was investigated from irradiated rhodium target with a-furyldioxime in chloroform from diluted hydrochloric acid. Extraction yield was 85.3% for a single extraction from 0.37M HCl and 103 Pd purity was better than 99%. (author)

Analysis of Intracellular Metabolites from Microorganisms: Quenching and Extraction Protocols

Directory of Open Access Journals (Sweden)

Farhana R. Pinu

2017-10-01

Full Text Available Sample preparation is one of the most important steps in metabolome analysis. The challenges of determining microbial metabolome have been well discussed within the research community and many improvements have already been achieved in last decade. The analysis of intracellular metabolites is particularly challenging. Environmental perturbations may considerably affect microbial metabolism, which results in intracellular metabolites being rapidly degraded or metabolized by enzymatic reactions. Therefore, quenching or the complete stop of cell metabolism is a pre-requisite for accurate intracellular metabolite analysis. After quenching, metabolites need to be extracted from the intracellular compartment. The choice of the most suitable metabolite extraction method/s is another crucial step. The literature indicates that specific classes of metabolites are better extracted by different extraction protocols. In this review, we discuss the technical aspects and advancements of quenching and extraction of intracellular metabolite analysis from microbial cells.

Evaluation of feeds for melt and dilute process using an Analytical Hierarchy Process

International Nuclear Information System (INIS)

Krupa, J.F.

2000-01-01

WSRC was requested to evaluate whether nuclear materials other than aluminum-clad spent nuclear fuel should be considered for treatment to prepare them for disposal in the melt and dilute facility as part of the Treatment and Storage Facility (TSF) currently projected for construction in the L-Reactor process area. The Analytical Hierarchy Process using a ratings methodology was used to rank potential feed candidates for disposition through the Melt and Dilute facility proposed for disposition of Savannah River Site aluminum-clad spent nuclear fuel. Because of the scoping nature of this analysis, the expert team convened for this purpose concentrated on technical feasibility and potential cost impacts associated with using melt and dilute versus the current disposition option

Determination of zinc stable isotopes in biological materials using isotope dilution inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Patterson, K.Y.; Veillon, Claude

1992-01-01

A method is described for using isotope dilution to determine both the amount of natural zinc and enriched isotopes of zinc in biological samples. Isotope dilution inductively coupled plasma mass spectrometry offers a way to quantify not only the natural zinc found in a sample but also the enriched isotope tracers of zinc. Accurate values for the enriched isotopes and natural zinc are obtained by adjusting the mass count rate data for measurable instrumental biases. Analytical interferences from the matrix are avoided by extracting the zinc from the sample matrix using diethylammonium diethyldithiocarbamate. The extraction technique separates the zinc from elements which form interfering molecular ions at the same nominal masses as the zinc isotopes. Accuracy of the method is verified using standard reference materials. The detection limit is 0.06 μg Zn per sample. Precision of the abundance ratios range from 0.3-0.8%. R.S.D. for natural zinc concentrations is about 200-600 μg g -1 . The accuracy and precision of the measurements make it possible to follow enriched isotopic tracers of zinc in biological samples in metabolic tracer studies. (author). 19 refs.; 1 fig., 4 tabs

Automatic extraction of forward stroke volume using dynamic PET/CT

DEFF Research Database (Denmark)

Harms, Hans; Tolbod, Lars Poulsen; Hansson, Nils Henrik

Background: Dynamic PET can be used to extract forward stroke volume (FSV) by the indicator dilution principle. The technique employed can be automated and is in theory independent on the tracer used and may therefore be added to any dynamic cardiac PET protocol. The aim of this study...... was to validate automated methods for extracting FSV directly from dynamic PET studies for two different tracers and to examine potential scanner hardware bias. Methods: 21 subjects underwent a dynamic 27 min 11C-acetate PET scan on a Siemens Biograph TruePoint 64 PET/CT scanner (scanner I). In addition, 8...... subjects underwent a dynamic 6 min 15O-water PET scan followed by a 27 min 11C-acetate PET scan on a GE Discovery ST PET/CT scanner (scanner II). The LV-aortic time-activity curve (TAC) was extracted automatically from dynamic PET data using cluster analysis. The first-pass peak was isolated by automatic...

The Aperture and Layout of the LHC Extraction Septa and TCDS Diluter with an Enlarged MSDC Vacuum Chamber

CERN Document Server

Goddard, B

2003-01-01

The LHC beam dumping system must safely abort the LHC beams over the whole energy range, under all realistically possible fault conditions. These include normal operation, failure of machine elements and also abnormal performance of subsystems of the beam dumping system itself. To avoid unnecessary irradiation and even equipment damage, the MSD extraction septa must provide sufficient aperture both for the circulating and extracted beams. In order to satisfy this requirement, a modified (enlarged) vacuum chamber design will be used for the limiting MSDC septa. The analysis of the available apertures is presented, with emphasis on the dependence on the local orbit and beam emittance.

Non‐diluted seawater enhances nasal ciliary beat frequency and wound repair speed compared to diluted seawater and normal saline

Science.gov (United States)

Bonnomet, Arnaud; Luczka, Emilie; Coraux, Christelle

2016-01-01

Background The regulation of mucociliary clearance is a key part of the defense mechanisms developed by the airway epithelium. If a high aggregate quality of evidence shows the clinical effectiveness of nasal irrigation, there is a lack of studies showing the intrinsic role of the different irrigation solutions allowing such results. This study investigated the impact of solutions with different pH and ionic compositions, eg, normal saline, non‐diluted seawater and diluted seawater, on nasal mucosa functional parameters. Methods For this randomized, controlled, blinded, in vitro study, we used airway epithelial cells obtained from 13 nasal polyps explants to measure ciliary beat frequency (CBF) and epithelial wound repair speed (WRS) in response to 3 isotonic nasal irrigation solutions: (1) normal saline 0.9%; (2) non‐diluted seawater (Physiomer®); and (3) 30% diluted seawater (Stérimar). The results were compared to control (cell culture medium). Results Non‐diluted seawater enhanced the CBF and the WRS when compared to diluted seawater and to normal saline. When compared to the control, it significantly enhanced CBF and slightly, though nonsignificantly, improved the WRS. Interestingly, normal saline markedly reduced the number of epithelial cells and ciliated cells when compared to the control condition. Conclusion Our results suggest that the physicochemical features of the nasal wash solution is important because it determines the optimal conditions to enhance CBF and epithelial WRS thus preserving the respiratory mucosa in pathological conditions. Non‐diluted seawater obtains the best results on CBF and WRS vs normal saline showing a deleterious effect on epithelial cell function. PMID:27101776

Simultaneous Analysis of Bioactive Markers from Orthosiphon ...

African Journals Online (AJOL)

Erah

the analysis of the crude extracts of Orthosiphon stamineus. Methods: A simple and facile analytical method was developed using RP- HPLC with UV detection for the identification .... The stock solutions were used for further dilutions. Samples were kept in freezer at -20 oC prior ..... the developed method is best suited for.

An application of nitrogen microwave-induced plasma mass spectrometry to isotope dilution analysis of selenium in marine organisms

Energy Technology Data Exchange (ETDEWEB)

Shirasaki, Toshihiro [Hitachi Instruments Engineering Co. Ltd., Hitachinaka, Ibaraki (Japan); Yoshinaga, Jun; Morita, Masatoshi; Okumoto, Toyoharu; Oishi, Konosuke

1996-01-01

Nitrogen microwave-induced plasma mass spectrometry was studied for its applicability to the isotope dilution analysis of selenium in biological samples. Spectroscopic interference by calcium, which is present in high concentrations in biological samples, was investigated. No detectable background spectrum was observed for the major selenium isotopes of {sup 78}Se and {sup 80}Se. No detectable interferences by sodium, potassium, calcium and phosphorus on the isotope ratio {sup 80}Se/{sup 78}Se were observed up to concentration of 200 mg/ml. The method was applied to the analysis of selenium in biological reference materials of marine organisms. The results showed good agreement between the certified and found values. (author).

Ultrasound-assisted extraction of rare-earth elements from carbonatite rocks.

Science.gov (United States)

Diehl, Lisarb O; Gatiboni, Thais L; Mello, Paola A; Muller, Edson I; Duarte, Fabio A; Flores, Erico M M

2018-01-01

In view of the increasing demand for rare-earth elements (REE) in many areas of high technology, alternative methods for the extraction of these elements have been developed. In this work, a process based on the use of ultrasound for the extraction of REE from carbonatite (an igneous rock) is proposed to avoid the use of concentrated reagents, high temperature and excessive extraction time. In this pioneer work for REE extraction from carbonatite rocks in a preliminary investigation, ultrasonic baths, cup horn systems or ultrasound probes operating at different frequencies and power were evaluated. In addition, the power released to the extraction medium and the ultrasound amplitude were also investigated and the temperature and carbonatite mass/volume of extraction solution ratio were optimized to 70°C and 20mg/mL, respectively. Better extraction efficiencies (82%) were obtained employing an ultrasound probe operating at 20kHz for 15min, ultrasound amplitude of 40% (692Wdm -3 ) and using a diluted extraction solution (3% v/v HNO 3 +2% v/v HCl). It is important to mention that high extraction efficiency was obtained even using a diluted acid mixture and relatively low temperature in comparison to conventional extraction methods for REE. A comparison of results with those obtained by mechanical stirring (500rpm) using the same conditions (time, temperature and extraction solution) was carried out, showing that the use of ultrasound increased the extraction efficiency up to 35%. Therefore, the proposed ultrasound-assisted procedure can be considered as a suitable alternative for high efficiency extraction of REE from carbonatite rocks. Copyright © 2017 Elsevier B.V. All rights reserved.

SBR treatment of olive mill wastewaters: dilution or pre-treatment?

Science.gov (United States)

Farabegoli, G; Chiavola, A; Rolle, E

2012-01-01

The olive-oil extraction industry is an economically important activity for many countries of the Mediterranean Sea area, with Spain, Greece and Italy being the major producers. This activity, however, may represent a serious environmental problem due to the discharge of highly polluted effluents, usually referred to as 'olive mill wastewaters' (OMWs). They are characterized by high values of chemical oxygen demand (COD) (80-300 g/L), lipids, total polyphenols (TPP), tannins and other substances difficult to degrade. An adequate treatment before discharging is therefore required to reduce the pollutant load. The aim of the present paper was to evaluate performances of a biological process in a sequencing batch reactor (SBR) fed with pre-treated OMWs. Pre-treatment consisted of a combined acid cracking (AC) and granular activated carbon (GAC) adsorption process. The efficiency of the system was compared with that of an identical SBR fed with the raw wastewater only diluted. Combined AC and GAC adsorption was chosen to be used prior to the following biological process due to its capability of providing high removal efficiencies of COD and TPP and also appreciable improvement of biodegradability. Comparing results obtained with different influents showed that best performances of the SBR were obtained by feeding it with raw diluted OMWs (dOMWs) and at the lowest dilution ratio (1:25): in this case, the removal efficiencies were 90 and 76%, as average, for COD and TPP, respectively. Feeding the SBR with either the pre-treated or the raw dOMWs at 1:50 gave very similar values of COD reduction (74%); however, an improvement of the TPP removal was observed in the former case.

Guideline on Isotope Dilution Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Gaffney, Amy [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

2017-05-19

Isotope dilution mass spectrometry is used to determine the concentration of an element of interest in a bulk sample. It is a destructive analysis technique that is applicable to a wide range of analytes and bulk sample types. With this method, a known amount of a rare isotope, or ‘spike’, of the element of interest is added to a known amount of sample. The element of interest is chemically purified from the bulk sample, the isotope ratio of the spiked sample is measured by mass spectrometry, and the concentration of the element of interest is calculated from this result. This method is widely used, although a mass spectrometer required for this analysis may be fairly expensive.

Gluconeogenesis from labeled carbon: estimating isotope dilution

International Nuclear Information System (INIS)

Kelleher, J.K.

1986-01-01

To estimate the rate of gluconeogenesis from steady-state incorporation of labeled 3-carbon precursors into glucose, isotope dilution must be considered so that the rate of labeling of glucose can be quantitatively converted to the rate of gluconeogenesis. An expression for the value of this isotope dilution can be derived using mathematical techniques and a model of the tricarboxylic acid (TCA) cycle. The present investigation employs a more complex model than that used in previous studies. This model includes the following pathways that may affect the correction for isotope dilution: 1) flux of 3-carbon precursor to the oxaloacetate pool via acetyl-CoA and the TCA cycle; 2) flux of 4- or 5-carbon compounds into the TCA cycle; 3) reversible flux between oxaloacetate (OAA) and pyruvate and between OAA and fumarate; 4) incomplete equilibrium between OAA pools; and 5) isotope dilution of 3-carbon tracers between the experimentally measured pool and the precursor for the TCA-cycle OAA pool. Experimental tests are outlined which investigators can use to determine whether these pathways are significant in a specific steady-state system. The study indicated that flux through these five pathways can significantly affect the correction for isotope dilution. To correct for the effects of these pathways an alternative method for calculating isotope dilution is proposed using citrate to relate the specific activities of acetyl-CoA and OAA

Antibacterial properties of Kurdistan Gundelia tournefortii ethanolic extract against Staphylococcus aureus and Escherichia coli

Directory of Open Access Journals (Sweden)

B. Ayoubi

2016-08-01

Full Text Available Due to the ever-increasing of antibiotic-resistance microorganisms and the tendency towards the application of natural preservatives, in the present study the ethanolic extract of stalk portion of  Kurdistan Gundelia tournefertti L. was extracted in rotary evaporator. The antibacterial effect (MIC and MBC of the extract was investigated against Staphylococcus aureus and Escherichia coli. using agar dilution assay on Muller-Hinton agar. The experiment was conducted with 3 replicates and probity analysis of the data was analyzed using SAS 9.2 software.Result showed that both MIC and MBC for S. aureus was62.5 µg/ml. Moreover, the MBC and MIC values for E. coli were estimated at 31.25 µg/ml and 15.62 µg/ml, respectively.Since ethanolic extract of G. tournefertti was highly effectiveon indicator bacteria,it can be used in combination with the other preservatives to protect foods from foodborne organisms.

Storm Sewage Dilution in Smaller Streams

DEFF Research Database (Denmark)

Larsen, Torben; Vestergaard, Kristian

1987-01-01

A numerical model has been used to show how dilution in smaller streams can be effected by unsteady hydraulic conditions caused by a storm sewage overflow.......A numerical model has been used to show how dilution in smaller streams can be effected by unsteady hydraulic conditions caused by a storm sewage overflow....

The methodology of semantic analysis for extracting physical effects

Science.gov (United States)

Fomenkova, M. A.; Kamaev, V. A.; Korobkin, D. M.; Fomenkov, S. A.

2017-01-01

The paper represents new methodology of semantic analysis for physical effects extracting. This methodology is based on the Tuzov ontology that formally describes the Russian language. In this paper, semantic patterns were described to extract structural physical information in the form of physical effects. A new algorithm of text analysis was described.

Inhibition Effect of Deanol on Mild Steel Corrosion in Dilute ...

African Journals Online (AJOL)

The influence of deanol on the corrosion behaviour of mild steel in dilute sulphuric acid with sodium chloride addition was studied by means of mass-loss, potentiodynamic polarization, electrode potential monitoring, scanning electron microscopy and statistical analysis. Results show that deanol performed excellently with ...

Direct anthelmintic effects of a purified chicory extract against free-living stages of Cooperia oncophora: preliminary results

DEFF Research Database (Denmark)

Pena-Espinoza, Miguel Angel; Williams, A.; Enemark, Heidi L.

2013-01-01

with methanol as the extraction medium. The resulting extract was dried and fractionated using solid-phase extraction (SPE) cartridges to enhance isolation of secondary metabolites such as sesquiterpene lactones. The obtained elutate was dried, dissolved in 100 % DMSO and serially diluted to obtain...

Cryogen-free dilution refrigerators

International Nuclear Information System (INIS)

Uhlig, K

2012-01-01

We review briefly our first cryogen-free dilution refrigerator (CF-DR) which was precooled by a GM cryocooler. We then show how today's dry DRs with pulse tube precooling have developed. A few examples of commercial DRs are explained and noteworthy features pointed out. Thereby we describe the general advantages of cryogen-free DRs, but also show where improvements are still desirable. At present, our dry DR has a base temperature of 10 mK and a cooling capacity of 700 μW at a mixing chamber temperature of 100 mK. In our cryostat, in most recent work, an additional refrigeration loop was added to the dilution circuit. This 4 He circuit has a lowest temperature of about 1 K and a refrigeration capacity of up to 100 mW at temperatures slightly above 1 K; the dilution circuit and the 4 He circuit can be run separately or together. The purpose of this additional loop is to increase the cooling capacity for experiments where the cooling power of the still of the DR is not sufficient to cool cold amplifiers and cables, e.g. in studies on superconducting quantum circuits or astrophysical applications.

Cryogen-free dilution refrigerators

Science.gov (United States)

Uhlig, K.

2012-12-01

We review briefly our first cryogen-free dilution refrigerator (CF-DR) which was precooled by a GM cryocooler. We then show how today's dry DRs with pulse tube precooling have developed. A few examples of commercial DRs are explained and noteworthy features pointed out. Thereby we describe the general advantages of cryogen-free DRs, but also show where improvements are still desirable. At present, our dry DR has a base temperature of 10 mK and a cooling capacity of 700 μW at a mixing chamber temperature of 100 mK. In our cryostat, in most recent work, an additional refrigeration loop was added to the dilution circuit. This 4He circuit has a lowest temperature of about 1 K and a refrigeration capacity of up to 100 mW at temperatures slightly above 1 K; the dilution circuit and the 4He circuit can be run separately or together. The purpose of this additional loop is to increase the cooling capacity for experiments where the cooling power of the still of the DR is not sufficient to cool cold amplifiers and cables, e.g. in studies on superconducting quantum circuits or astrophysical applications.

Dilute chemical decontamination program review

International Nuclear Information System (INIS)

Anstine, L.D.; Blomgren, J.C.; Pettit, P.J.

1980-01-01

The objective of the Dilute Chemical Decontamination Program is to develop and evaluate a process which utilizes reagents in dilute concentrations for the decontamination of BWR primary systems and for the maintenance of dose rates on the out-of-core surfaces at acceptable levels. A discussion is presented of the process concept, solvent development, advantages and disadvantages of reagent systems, and VNC loop tests. Based on the work completed to date it is concluded that (1) rapid decontamination of BWRs using dilute reagents is feasible; (2) reasonable reagent conditions for rapid chemical decontamination are: 0.01M oxalic acid + 0.005M citric acid, pH3.0, 90/degree/C, 0.5 to 1.0 ppm dissolved oxygen; (3) control of dissolved oxygen concentration is important, since high levels suppress the rate of decontamination and low levels allow precipitation of ferrous oxalate. 4 refs

Quantifying dilution caused by execution efficiency

Directory of Open Access Journals (Sweden)

Taís Renata Câmara

Full Text Available Abstract In open pit mining, dilution is not always a factor systematically analyzed and calculated. Often it is only an adjusted number, for example, calculated or even empirically determined for a certain operational condition perpetuating along time in the form of a constant applied to calculating reserves or mine planning in attendance of audit requirements. Dilution and loss are factors that should be always considered for tonnage and grade estimates. These factors are always associated and can be determined considering several particularities of the deposit and the operation itself. In this study, a methodology was determined to identify blocks adjacent to the blocks previously planned to be mined. Thus, it is possible to estimate the dilution caused by poor operating efficiency, taking into account the inability of the equipment to perfectly remove each block, respecting its limits. Mining dilution is defined as the incorporation of waste material to ore due to the operational incapacity to efficiently separate the materials during the mining process, considering the physical processes, and the operating and geometric configurations of the mining with the equipment available.

Defects in dilute nitrides

International Nuclear Information System (INIS)

Chen, W.M.; Buyanova, I.A.; Tu, C.W.; Yonezu, H.

2005-01-01

We provide a brief review our recent results from optically detected magnetic resonance studies of grown-in non-radiative defects in dilute nitrides, i.e. Ga(In)NAs and Ga(Al,In)NP. Defect complexes involving intrinsic defects such as As Ga antisites and Ga i self interstitials were positively identified.Effects of growth conditions, chemical compositions and post-growth treatments on formation of the defects are closely examined. These grown-in defects are shown to play an important role in non-radiative carrier recombination and thus in degrading optical quality of the alloys, harmful to performance of potential optoelectronic and photonic devices based on these dilute nitrides. (author)

Non-diluted seawater enhances nasal ciliary beat frequency and wound repair speed compared to diluted seawater and normal saline.

Science.gov (United States)

Bonnomet, Arnaud; Luczka, Emilie; Coraux, Christelle; de Gabory, Ludovic

2016-10-01

The regulation of mucociliary clearance is a key part of the defense mechanisms developed by the airway epithelium. If a high aggregate quality of evidence shows the clinical effectiveness of nasal irrigation, there is a lack of studies showing the intrinsic role of the different irrigation solutions allowing such results. This study investigated the impact of solutions with different pH and ionic compositions, eg, normal saline, non-diluted seawater and diluted seawater, on nasal mucosa functional parameters. For this randomized, controlled, blinded, in vitro study, we used airway epithelial cells obtained from 13 nasal polyps explants to measure ciliary beat frequency (CBF) and epithelial wound repair speed (WRS) in response to 3 isotonic nasal irrigation solutions: (1) normal saline 0.9%; (2) non-diluted seawater (Physiomer®); and (3) 30% diluted seawater (Stérimar). The results were compared to control (cell culture medium). Non-diluted seawater enhanced the CBF and the WRS when compared to diluted seawater and to normal saline. When compared to the control, it significantly enhanced CBF and slightly, though nonsignificantly, improved the WRS. Interestingly, normal saline markedly reduced the number of epithelial cells and ciliated cells when compared to the control condition. Our results suggest that the physicochemical features of the nasal wash solution is important because it determines the optimal conditions to enhance CBF and epithelial WRS thus preserving the respiratory mucosa in pathological conditions. Non-diluted seawater obtains the best results on CBF and WRS vs normal saline showing a deleterious effect on epithelial cell function. © 2016 The Authors International Forum of Allergy & Rhinology, published by ARSAAOA, LLC.

Dynamic dilution exponent in monodisperse entangled polymer solutions

DEFF Research Database (Denmark)

Shahid, T.; Huang, Qian; Oosterlinck, F.

2017-01-01

of concentration but also depends on the molar mass of the chains. While the proposed approach successfully explains the viscoelastic properties of a large number of semi-dilute solutions of polymers in their own oligomers, important discrepancies are found for semi-dilute entangled polymers in small-molecule......We study and model the linear viscoelastic properties of several entangled semi-dilute and concentrated solutions of linear chains of different molar masses and at different concentrations dissolved in their oligomers. We discuss the dilution effect of the oligomers on the entangled long chains....... In particular, we investigate the influence of both concentration and molar mass on the value of the effective dynamic dilution exponent determined from the level of the storage plateau at low and intermediate frequencies. We show that the experimental results can be quantitatively explained by considering...

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

Science.gov (United States)

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

2015-03-21

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

Solvent extraction of silver(I) from dilute cyanide solutions with 2,4-dihydroxyacetophenone thiosemicarbazone

International Nuclear Information System (INIS)

Reddy, A.V.; Reddy, Y.K.; Reddy, G.S.

1986-01-01

The solvent extraction of silver(I) was carried out in 0.5M nitric acid in the presence of cyanide by 2,4-dihydroxyacetophenone thiosemicarbazone (DATS). Ethyl acetate was used as a solvent and quantitative recovery was possible with 12.5-fold excess of the reagent in a single extraction. In this medium silver(I) forms a 2:2 complex (metal:ligand) with DATS. The effect of diverse ions on the extraction of silver(I) was investigated. (author)

Neutron activation determination of gold and palladium using extraction by organic sulfides

International Nuclear Information System (INIS)

Gil'berg, Eh.N.; Torgov, V.G.; Verevkin, G.V.; AN SSSR, Novosibirsk. Inst. Neorganicheskoj Khimii)

1978-01-01

Compared are methods of gold determination in standard rock samples of the USA National Geological Service: a) extraction by solutions of dioctylsulfide and oil sulfides from irradiated samples; b) preliminary extraction by the above solfides with the following extract radiation; c) the method of isotope dilution with substoichiometry extraction. A possibility is studied to determine palladium in the sulfide extract with gold using the NaI(Tl) thin crystal scintillators. It is established that joint palladium and gold extraction permits to determine them in many natural products simultaneously

Cost effectiveness of dilute chemical decontamination

International Nuclear Information System (INIS)

LeSurf, J.E.; Weyman, G.D.

The basic principles of dilute chemical decontamination are described, as well as the method of application. Methods of computing savings in radiation dose and costs are presented, with results from actual experience and illustrative examples. It is concluded that dilute chemical decontamination is beneficial in many cases. It reduces radiation exposure of workers, saves money, and simplifies maintenance work

Validity of the tritiated thymidine method for estimating bacterial growth rates: measurement of isotope dilution during DNA synthesis

International Nuclear Information System (INIS)

Pollard, P.C.; Moriarty, D.J.W.

1984-01-01

The rate of tritiated thymidine incorporation into DNA was used to estimate bacterial growth rates in aquatic environments. To be accurate, the calculation of growth rates has to include a factor for the dilution of isotope before incorporation. The validity of an isotope dilution analysis to determine this factor was verified in experiments reported here with cultures of a marine bacterium growing in a chemostat. Growth rates calculated from data on chemostat dilution rates and cell density agreed well with rates calculated by tritiated thymidine incorporation into DNA and isotope dilution analysis. With sufficiently high concentrations of exogenous thymidine, de novo synthesis of deoxythymidine monophosphate was inhibited, thereby preventing the endogenous dilution of isoope. The thymidine technique was also shown to be useful for measuring growth rates of mixed suspensions of bacteria growing anaerobically. Thymidine was incorporated into the DNA of a range of marine pseudomonads that were investigated. Three species did not take up thymidine. The common marine cyanobacterium Synechococcus species did not incorporate thymidine into DNA

Lead speciation in 0.1N HCl-extracted residue of analog of Pb-contaminated soil

International Nuclear Information System (INIS)

Wei Yuling; Yang, Y.-W.; Lee, J.-F.

2005-01-01

The heavy metal in-taken by plants from contaminated soils is usually assessed by extraction with 0.1N HCl. This study characterized the chemical form of lead in the solid residue of 0.1N HCl-extracted Pb-contaminated kaolin. The results indicate that most lead in the 0.1N HCl-extracted residue of the Pb(NO 3 ) 2 -contaminated kaolin dried at 105 deg C is mainly in form of PbCl 2 . For other lead-containing kaolin sample heated at 900 deg C, the XAS analysis also shows that majority of the lead compound was converted into PbCl 2 precipitate that remained in the solid residue during the 0.1N HCl extraction. Because PbCl 2 is only slightly soluble in dilute acids or water, it is suggested that using 0.1N HCl liquid as an extracting reagent to represent the heavy metal uptake by plants might actually underestimate the uptake

Food Fish Identification from DNA Extraction through Sequence Analysis

Science.gov (United States)

Hallen-Adams, Heather E.

2015-01-01

This experiment exposed 3rd and 4th y undergraduates and graduate students taking a course in advanced food analysis to DNA extraction, polymerase chain reaction (PCR), and DNA sequence analysis. Students provided their own fish sample, purchased from local grocery stores, and the class as a whole extracted DNA, which was then subjected to PCR,…

Contribution to the study of the physico-chemical mechanisms of metallic cation extraction by alkylphosphoric acids. Extraction of zirconium (IV) by di-2-ethylhexyl phosphoric acid (DEHPA)

International Nuclear Information System (INIS)

Carbonnier, J.-L.

1979-02-01

Extraction of zirconium, especially at high concentration (0.1M), by dodecane diluted DEHPA (HA) from hydrochloric or nitric aqueous phases of 0.1 to 10 M acidity was studied. The composition, structure and polymerisation of the complexes extracted were determined by chemical analysis, viscosimetry, infrared spectrometry and light scattering. A Zr(OH) 2 A 2 .2HNO 3 , type structure is proposed for these complexes instead of the generally accepted form: Zr(OH) 2 (NO 3 ) 2 .2HA. Similarly in hydrochloric solution: Zr(OH) 2 A 2 .2HCl. Polymerisation in the organic phase results from the juxtaposition of two factors; firstly zirconium saturation (formation of bridges by DEHPA between zirconium atoms) and secondly the nature the equeous phase. In slightly acid hydrochloric solution (pH = 1.3) the aqueous plymers of zirconium are extracted in the organic phase as polynuclear complexes; in nitric solution no polynuclear complexes are observed but the nitric acid molecules extracted set up hydrogen bonds which explain the increased viscosity and gelification of the organic phases [fr

Optimisation of beryllium-7 gamma analysis following BCR sequential extraction

International Nuclear Information System (INIS)

Taylor, A.; Blake, W.H.; Keith-Roach, M.J.

2012-01-01

Graphical abstract: Showing decrease in analytical uncertainty using the optimal (combined preconcentrated sample extract) method. nv (no value) where extract activities were 7 Be geochemical behaviour is required to support tracer studies. ► Sequential extraction with natural 7 Be returns high analytical uncertainties. ► Preconcentrating extracts from a large sample mass improved analytical uncertainty. ► This optimised method can be readily employed in studies using low activity samples. - Abstract: The application of cosmogenic 7 Be as a sediment tracer at the catchment-scale requires an understanding of its geochemical associations in soil to underpin the assumption of irreversible adsorption. Sequential extractions offer a readily accessible means of determining the associations of 7 Be with operationally defined soil phases. However, the subdivision of the low activity concentrations of fallout 7 Be in soils into geochemical fractions can introduce high gamma counting uncertainties. Extending analysis time significantly is not always an option for batches of samples, owing to the on-going decay of 7 Be (t 1/2 = 53.3 days). Here, three different methods of preparing and quantifying 7 Be extracted using the optimised BCR three-step scheme have been evaluated and compared with a focus on reducing analytical uncertainties. The optimal method involved carrying out the BCR extraction in triplicate, sub-sampling each set of triplicates for stable Be analysis before combining each set and coprecipitating the 7 Be with metal oxyhydroxides to produce a thin source for gamma analysis. This method was applied to BCR extractions of natural 7 Be in four agricultural soils. The approach gave good counting statistics from a 24 h analysis period (∼10% (2σ) where extract activity >40% of total activity) and generated statistically useful sequential extraction profiles. Total recoveries of 7 Be fell between 84 and 112%. The stable Be data demonstrated that the

Data Extraction Based on Page Structure Analysis

Directory of Open Access Journals (Sweden)

Ren Yichao

2017-01-01

Full Text Available The information we need has some confusing problems such as dispersion and different organizational structure. In addition, because of the existence of unstructured data like natural language and images, extracting local content pages is extremely difficult. In the light of of the problems above, this article will apply a method combined with page structure analysis algorithm and page data extraction algorithm to accomplish the gathering of network data. In this way, the problem that traditional complex extraction model behave poorly when dealing with large-scale data is perfectly solved and the page data extraction efficiency is also boosted to a new level. In the meantime, the article will also make a comparison about pages and content of different types between the methods of DOM structure based on the page and HTML regularities of distribution. After all of those, we may find a more efficient extract method.

Antibacterial activity of honey and medicinal plant extracts against ...

African Journals Online (AJOL)

Using a broth dilution method, the antibacterial activity extracts of six South African honeys and medicinal plants against six enteric microorganisms viz- Enterobacter cloacae, Escheriachia coli, Klebsiella pneumoniae, Citrobacter freundii isolated from geophagia samples and Aeromonas hydrophila and plesiomonas ...

Evaluation of online carbon isotope dilution mass spectrometry for the purity assessment of synthetic peptide standards

Energy Technology Data Exchange (ETDEWEB)

Díaz, Sergio Cueto; Ruiz Encinar, Jorge, E-mail: ruizjorge@uniovi.es; García Alonso, J. Ignacio, E-mail: jiga@uniovi.es

2014-09-24

Highlights: • Purity assessment of peptide standards applicable to any water soluble peptide. • Online {sup 13}C isotope dilution mass spectrometry. • Mass flow chromatogram from measured 44/45 isotope ratios. • Validation by the analysis of NIST 8327. - Abstract: We present a novel method for the purity assessment of peptide standards which is applicable to any water soluble peptide. The method is based on the online {sup 13}C isotope dilution approach in which the peptide is separated from its related impurities by liquid chromatography (LC) and the eluent is mixed post-column with a continuous flow of {sup 13}C-enriched sodium bicarbonate. An online oxidation step using sodium persulfate in acidic media at 99 °C provides quantitative oxidation to {sup 12}CO{sub 2} and {sup 13}CO{sub 2} respectively which is extracted to a gaseous phase with the help of a gas permeable membrane. The measurement of the isotope ratio 44/45 in the mass spectrometer allows the construction of the mass flow chromatogram. As the only species that is finally measured in the mass spectrometer is CO{sub 2}, the peptide content in the standard can be quantified, on the base of its carbon content, using a generic primary standard such as potassium hydrogen phthalate. The approach was validated by the analysis of a reference material (NIST 8327), and applied to the quantification of two commercial synthetic peptide standards. In that case, the results obtained were compared with those obtained using alternative methods, such as amino acid analysis and ICP-MS. The results obtained proved the value of the method for the fast, accurate and precise mass purity assignment of synthetic peptide standards.

Polymorphisms within the canine MLPH gene are associated with dilute coat color in dogs

Directory of Open Access Journals (Sweden)

Günzel-Apel Anne-Rose

2005-06-01

Full Text Available Abstract Background Pinschers and other dogs with coat color dilution show a characteristic pigmentation phenotype. The fur colors are a lighter shade, e.g. silvery grey (blue instead of black and a sandy color (Isabella fawn instead of red or brown. In some dogs the coat color dilution is sometimes accompanied by hair loss and recurrent skin inflammation, the so called color dilution alopecia (CDA or black hair follicular dysplasia (BHFD. In humans and mice a comparable pigmentation phenotype without any documented hair loss is caused by mutations within the melanophilin gene (MLPH. Results We sequenced the canine MLPH gene and performed a mutation analysis of the MLPH exons in 6 Doberman Pinschers and 5 German Pinschers. A total of 48 sequence variations was identified within and between the breeds. Three families of dogs showed co-segregation for at least one polymorphism in an MLPH exon and the dilute phenotype. No single polymorphism was identified in the coding sequences or at splice sites that is likely to be causative for the dilute phenotype of all dogs examined. In 18 German Pinschers a mutation in exon 7 (R199H was consistently associated with the dilute phenotype. However, as this mutation was present in homozygous state in four dogs of other breeds with wildtype pigmentation, it seems unlikely that this mutation is truly causative for coat color dilution. In Doberman Pinschers as well as in Large Munsterlanders with BHFD, a set of single nucleotide polymorphisms (SNPs around exon 2 was identified that show a highly significant association to the dilute phenotype. Conclusion This study provides evidence that coat color dilution is caused by one or more mutations within or near the MLPH gene in several dog breeds. The data on polymorphisms that are strongly associated with the dilute phenotype will allow the genetic testing of Pinschers to facilitate the breeding of dogs with defined coat colors and to select against Large

Identification of ultrasound-contrast-agent dilution systems for ejection fraction measurements

NARCIS (Netherlands)

Mischi, M.; Jansen, A.H.M.; Kalker, A.A.C.M.; Korsten, H.H.M.

2005-01-01

Left ventricular ejection fraction is an important cardiac-efficiency measure. Standard estimations are based on geometric analysis and modeling; they require time and experienced cardiologists. Alternative methods make use of indicator dilutions, but they are invasive due to the need for

Differentiation of the aromas of Merlot and Cabernet Sauvignon wines using sensory and instrumental analysis.

Science.gov (United States)

Kotseridis, Y; Razungles, A; Bertrand, A; Baumes, R

2000-11-01

The aromas of six Merlot and three Cabernet Sauvignon wines of the 1996 vintage from the Bordeaux region were evaluated by sensory analysis. A panel of selected enology students was trained to assess 20 attributes previously generated for these wines by enologists of Bordeaux. Using statistical methods, this 20-attribute list was reduced to a 12-attribute list. The aroma profiles of the wines of Merlot and Cabernet Sauvignon were very close. Differentiation of the wines of these two varieties was significant only for the caramel descriptor, which was rated higher in the Merlot wines. Gas chromatography/olfactometry (GC/O) and GC/MS analyses were used to detect and identify the potent odorants with the caramel odor in the two most differentiated samples for this attribute, a Merlot wine and a Cabernet Sauvignon wine. Two odorant zones with this odor resulted in identification of 4-hydroxy-2,5-dimethylfuran-3(2H)-one (HDMF) and 4-hydroxy-2(or 5)-ethyl-5(or 2)-methylfuran-3(2H)-one (HEMF). Aroma extract dilution analysis (AEDA) method showed a higher dilution factor (FD) for HDMF in the Merlot wine extract than in the Cabernet Sauvignon extract. The HDMF levels determined in the wines studied using a stable isotope dilution assay (SIDA) method were consistent with the results found by sensory analysis and GC/O; i.e., higher HDMF levels were present in the Merlot wines than in the Cabernet Sauvignon wines.

Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction.

Science.gov (United States)

Ghahramanloo, Kourosh Hasanzadeh; Kamalidehghan, Behnam; Akbari Javar, Hamid; Teguh Widodo, Riyanto; Majidzadeh, Keivan; Noordin, Mohamed Ibrahim

2017-01-01

The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE) and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%-61.85%) and oleic acid (1.64%-18.97%). Thymoquinone (0.72%-21.03%) was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly ( P essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique.

Accurate determination and certification of bromine in plastic by isotope dilution inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Ohata, Masaki; Miura, Tsutomu

2014-01-01

Highlights: • Accurate analytical method of Br in plastic was studied by isotope dilution ICPMS. • A microwave acid digestion using quartz vessel was suitable for Br analysis. • Sample dilution by NH 3 solution could remove memory effect for ICPMS measurement. • The analytical result of the ID-ICPMS showed consistency with that of INAA. • The ID-ICPMS developed could apply to certification of Br in candidate plastic CRM. - Abstract: The accurate analytical method of bromine (Br) in plastic was developed by an isotope dilution inductively coupled plasma mass spectrometry (ID-ICPMS). The figures of merit of microwave acid digestion procedures using polytetrafluoroethylene (PTFE) or quartz vessels were studied and the latter one was suitable for Br analysis since its material was free from Br contamination. The sample dilution procedures using Milli-Q water or ammonium (NH 3 ) solution were also studied to remove memory effect for ICPMS measurement. Although severe memory effect was observed on Milli-Q water dilution, NH 3 solution could remove it successfully. The accuracy of the ID-ICPMS was validated by a certified reference material (CRM) as well as the comparison with the analytical result obtained by an instrumental neutron activation analysis (INAA) as different analytical method. From these results, the ID-ICPMS developed in the present study could be evaluated as accurate analytical method of Br in plastic materials and it could apply to certification of Br in candidate plastic CRM with respect to such regulations related to RoHS (restriction of the use of hazardous substances in electrical and electronics equipment) directive

Quality- and dilution losses in the recycling of ferrous materials from end-of-life passenger cars: input-output analysis under explicit consideration of scrap quality.

Science.gov (United States)

Nakamura, Shinichiro; Kondo, Yasushi; Matsubae, Kazuyo; Nakajima, Kenichi; Tasaki, Tomohiro; Nagasaka, Tetsuya

2012-09-04

Metals can in theory be infinitely recycled in a closed-loop without any degradation in quality. In reality, however, open-loop recycling is more typical for metal scrap recovered from end-of-life (EoL) products because mixing of different metal species results in scrap quality that no longer matches the originals. Further losses occur when meeting the quality requirement of the target product requires dilution of the secondary material by adding high purity materials. Standard LCA usually does not address these losses. This paper presents a novel approach to quantifying quality- and dilution losses, by means of hybrid input-output analysis. We focus on the losses associated with the recycling of ferrous materials from end-of-life vehicle (ELV) due to the mixing of copper, a typical contaminant in steel recycling. Given the quality of scrap in terms of copper density, the model determines the ratio by which scrap needs to be diluted in an electric arc furnace (EAF), and the amount of demand for EAF steel including those quantities needed for dilution. Application to a high-resolution Japanese IO table supplemented with data on ferrous materials including different grades of scrap indicates that a nationwide avoidance of these losses could result in a significant reduction of CO(2) emissions.

The analysis study of plutonium in the environmental sample by mass spectrum combined with isotopic dilution

International Nuclear Information System (INIS)

Han Jun; Fu Zhonghua; Mao Xingen; Meng Fanben

2004-01-01

The technology of the rhenium filament carbonization was used to increase the ionization efficiency in this paper. The plutonium in the environmental sample was analyzed by Mass Spectrum combined with isotope dilution. Analysis of the 239 Pu blank in the process: The analysis of 239 Pu from the chemical process was carried out in order to establish the influence of the 239 Pu introduced from the process. The analysis results were shown in Table 1 sample 1 was not gone through the process, sample 2 and sample 3 were gone through the process. It was clear that there was no influence of the 239 Pu from the process within the deviation. Results and Discussions: The environmental samples which were dealed with the chemical method were prepared the sample of mass spectrum, The atomic ratio of the 239 Pu and 242 Pu in the environmental samples was measured by Mass Spectrum. The atomic ratio in the tracer 242 Pu was 0.01476±0.00007.The results for nuclide content in environment were given in Table 2. The content of 239 Pu in the tracer was high, so the existing of 239 Pu in the environmental samples can be determined by the changing of the atomic ratio of 242 Pu to 239 Pu. It was clear that there was 239 Pu in the environmental samples except the cypress leaves-2 and the pine leaves-3 within the deviation, and the content of 239 Pu were given in Table 2. Conclusion: a. Plutonium was separated and purified from the impurity by the anion-exchange and the electrodeposition, it was possible to provide the eligible mass spectrum sample. b. The measurement of plutonium in the environmental samples was not influenced by the flow of the background in the experiment. c. As the technology of the rhenium carbonization was used to increase the ionization efficiency, the content of plutonium which was about 10 -13 g in the environmental sample could be quantitatively analyzed by Mass Spectrum combined with isotope dilution. (authors)

Study of Enzymatic Hydrolysis of Dilute Acid Pretreated Coconut Husk

Directory of Open Access Journals (Sweden)

Rudy Agustriyanto

2012-12-01

Full Text Available Coconut husk is classified as complex lignocellulosic material that contains cellulose, hemicellulose, lignin, and some other extractive compounds. Cellulose from coconut husk can be used as fermentation substrate after enzymatic hydrolysis. In contrary, lignin content from the coconut husk will act as an inhibitor in this hydrolysis process. Therefore, a pretreatment process is needed to enhance the hydrolysis of cellulose. The objective of this research is to investigate the production of the glucose through dilute acid pretreatment and to obtain its optimum operating conditions. In this study, the pretreatment was done using dilute sulfuric acid in an autoclave reactor. The pretreatment condition were varied at 80°C, 100°C, 120°C and 0.9%, 1.2%, 1.5% for temperature and acid concentration respectively. The acid pretreated coconut husk was then hydrolyzed using commercial cellulase (celluclast and β-glucosidase (Novozyme 188. The hydrolysis time was 72 hours and the operating conditions were varied at several temperature and pH. From the experimental results it can be concluded that the delignification temperature variation has greater influence than the acid concentration. The optimum operating condition was obtained at pH 4 and 50°C which was pretreated at 100°C using 1.5% acid concentration. Copyright © 2012 by BCREC UNDIP. All rights reserved. (Selected Paper from International Conference on Chemical and Material Engineering (ICCME 2012Received: 28th September 2012, Revised: 2nd October 2012, Accepted: 4th October 2012[How to Cite: R. Agustriyanto, A. Fatmawati, Y. Liasari. (2012. Study of Enzymatic Hydrolysis of Dilute Acid Pretreated Coconut Husk. Bulletin of Chemical Reaction Engineering & Catalysis, 7(2: 137-141. doi:10.9767/bcrec.7.2.4046.137-141] [How to Link / DOI: http://dx.doi.org/10.9767/bcrec.7.2.4046.137-141 ] | View in 

PRELIMINARY ANTIMICROBIAL AND PHYTOCHEMICAL STUDY OF THE AQUEOUS, ALCHOLIC AND CHLOROFORM EXTRACTS OF THE LEAVES OF NAPOLEONAEA VOGELLI HOOK. AND PLANCH. (LECYTHIDIACEAE

Directory of Open Access Journals (Sweden)

Iriagbonse Asowata

2013-02-01

Full Text Available The antimicrobial activity and phytochemical analysis of Napoleonaea vogelli P. Beauv. {Lecythidiaceae} was done using aqueous, ethanol, methanol and chloroform leaf extracts to determine its antimicrobial and phytochemical constituents. The antimicrobial activities of the extracts were tested against bacteria and fungi isolates using the agar well diffusion method. Commercial antibiotics were used as positive reference standards to determine the sensitivity of the isolates. The leaf extracts of the plant were subjected to phytochemical analysis using standard experimental procedures. The extracts showed significant inhibitory activity against the test microbial isolates: Escherichia coli, Bacillus subtilis, Staphylococcus aureus, Klebsiella pneumoniae, Proteus mirabilis, Pseudomonas aeruginosa, Penicillum notatum, Aspergillus niger, Fusarium oxysporum, Saccharomyces cerevisiae and Candida albicans. The MIC values obtained using the Agar-dilution test ranged from 0.5-10mg/ml. The results demonstrated that the extracts of the leaves (N. vogelli possess broad spectrum antimicrobial activity. These results suggest that it will be useful in the treatment of microbial infections.

Analysis, by RELAP5 code, of boron dilution phenomena in a mid-loop operation transient, performed in PKL III F2.1 RUN 1 test

International Nuclear Information System (INIS)

Mascari, F.; Vella, G.; Del Nevo, A.; D'Auria, F.

2007-01-01

The present paper deals with the post test analysis and accuracy quantification of the test PKL III F2.1 RUN 1 by RELAP5/Mod3.3 code performed in the framework of the international OECD/SETH PKL III Project. The PKL III is a full-height integral test facility (ITF) that models the entire primary system and most of the secondary system (except for turbine and condenser) of pressurized water reactor of KWU design of the 1300-MW (electric) class on a scale of 1:145. Detailed design was based to the largest possible extent on the specific data of Philippsburg nuclear power plant, unit 2. As for the test facilities of this size, the scaling concept aims to simulate overall thermal hydraulic behavior of the full-scale power plant [1]. The main purpose of the project is to investigate PWR safety issues related to boron dilution and in particular this experiment investigates (a) the boron dilution issue during mid-loop operation and shutdown conditions, and (b) assessing primary circuit accident management operations to prevent boron dilution as a consequence of loss of heat removal [2]. In this work the authors deal with a systematic procedure (developed at the university of Pisa) for code assessment and uncertainty qualification and its application to RELAP5 system code. It is used to evaluate the capability of RELAP5 to reproduce the thermal hydraulics of an inadvertent boron dilution event in a PWR. The quantitative analysis has been performed adopting the Fast Fourier Transform Based Method (FFTBM), which has the capability to quantify the errors in code predictions as compared to the measured experimental signal. (author)

Validation of an ultrasound dilution technology for cardiac output measurement and shunt detection in infants and children.

Science.gov (United States)

Lindberg, Lars; Johansson, Sune; Perez-de-Sa, Valeria

2014-02-01

To validate cardiac output measurements by ultrasound dilution technology (COstatus monitor) against those obtained by a transit-time ultrasound technology with a perivascular flow probe and to investigate ultrasound dilution ability to estimate pulmonary to systemic blood flow ratio in children. Prospective observational clinical trial. Pediatric cardiac operating theater in a university hospital. In 21 children (6.1 ± 2.6 kg, mean ± SD) undergoing heart surgery, cardiac output was simultaneously recorded by ultrasound dilution (extracorporeal arteriovenous loop connected to existing arterial and central venous catheters) and a transit-time ultrasound probe applied to the ascending aorta, and when possible, the main pulmonary artery. The pulmonary to systemic blood flow ratio estimated from ultrasound dilution curve analysis was compared with that estimated from transit-time ultrasound technology. Bland-Altman analysis of the whole cohort (90 pairs, before and after surgery) showed a bias between transit-time ultrasound (1.01 ± 0.47 L/min) and ultrasound dilution technology (1.03 ± 0.51 L/min) of -0.02 L/min, limits of agreement -0.3 to 0.3 L/min, and percentage error of 31%. In children with no residual shunts, the bias was -0.04 L/min, limits of agreement -0.28 to 0.2 L/min, and percentage error 19%. The pooled co efficient of variation was for the whole cohort 3.5% (transit-time ultrasound) and 6.3% (ultrasound dilution), and in children without shunt, it was 2.9% (transit-time ultrasound) and 4% (ultrasound dilution), respectively. Ultrasound dilution identified the presence of shunts (pulmonary to systemic blood flow ≠ 1) with a sensitivity of 100% and a specificity of 92%. Mean pulmonary to systemic blood flow ratio by transit-time ultrasound was 2.6 ± 1.0 and by ultrasound dilution 2.2 ± 0.7 (not significant). The COstatus monitor is a reliable technique to measure cardiac output in children with high sensitivity and specificity for detecting the

Analysis of medicinal plant extracts by neutron activation method

International Nuclear Information System (INIS)

Vaz, Sandra Muntz

1995-01-01

This dissertation has presented the results from analysis of medicinal plant extracts using neutron activation method. Instrumental neutron activation analysis was applied to the determination of the elements Al, Br, Ca, Ce, Cl, Cr, Cs, Fe, K, La, Mg, Mn, Na, Rb, Sb, Sc and Zn in medicinal extracts obtained from Achyrolcline satureoides DC, Casearia sylvestris, Centella asiatica, Citrus aurantium L., Solano lycocarpum, Solidago microglossa, Stryphnondedron barbatiman and Zingiber officinale R. plants. The elements Hg and Se were determined using radiochemical separation by means of retention of Se in HMD inorganic exchanger and solvent extraction of Hg by bismuth diethyl-dithiocarbamate solution. Precision and accuracy of the results have been evaluated by analysing reference materials. The therapeutic action of some elements found in plant extracts analyzed was briefly discussed

Extractive spectrophotometric determination of uranium with malachite green

International Nuclear Information System (INIS)

Dubey, S.C.; Nadkarni, M.N.

1977-01-01

A sensitive spectrophotometric method based on the extraction of a uranium-benzoate-Malachite Green complex by chlorobenzene is described. The absorption maximum is at 635 nm and the molar absorptivity is 8.3 x 10 4 1. mole -1 cm -1 . A preliminary separation of uranium by extraction with methyl isobutyl ketone from acid-deficient aluminium nitrate solution is used to avoid interferences. An aliquot of the extract in then diluted with chlorobenzene and shaken with benzoate buffer containing Malachite Green (MG). The method has been applied for the determination of uranium in a synthetic leach solution. The complex extracted is probably [U0 2 (C 6 H 5 C00 3 - ][MG + ]. (author)

Results from Commissioning of the Energy Extraction Facilities of the LHC Machine

CERN Document Server

Coelingh, G J; Mess, K H

2008-01-01

The risk of damage to the superconducting magnets, bus bars and current leads of the LHC machine in case of a resistive transition (quench) is being minimized by adequate protection. The protection is based on early quench detection, bypassing the quenching magnets by cold diodes, energy density dilution in the quenching magnets using heaters and, eventually, energy extraction. For two hundred and twenty-six LHC circuits (600 A and 13 kA) extraction of the stored magnetic energy to external dump resistors was required. All these systems are now installed in the machine and the final hardware commissioning has been undertaken. After a short description of the topology and definitive features, layouts and parameters of these systems the paper will focus on the results from their successful commissioning and an analysis of the system performance.

Extraction of Trivalent Actinides and Lanthanides from Californium Campaign Rework Solution Using TODGA-based Solvent Extraction System

Energy Technology Data Exchange (ETDEWEB)

Benker, Dennis [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Delmau, Laetitia Helene [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Dryman, Joshua Cory [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2017-07-01

This report presents the studies carried out to demonstrate the possibility of quantitatively extracting trivalent actinides and lanthanides from highly acidic solutions using a neutral ligand-based solvent extraction system. These studies stemmed from the perceived advantage of such systems over cationexchange- based solvent extraction systems that require an extensive feed adjustment to make a low-acid feed. The targeted feed solutions are highly acidic aqueous phases obtained after the dissolution of curium targets during a californium (Cf) campaign. Results obtained with actual Cf campaign solutions, but highly diluted to be manageable in a glove box, are presented, followed by results of tests run in the hot cells with Cf campaign rework solutions. It was demonstrated that a solvent extraction system based on the tetraoctyl diglycolamide molecule is capable of quantitatively extracting trivalent actinides from highly acidic solutions. This system was validated using actual feeds from a Cf campaign.

Sponge-associated actinobacterial diversity: validation of the methods of actinobacterial DNA extraction and optimization of 16S rRNA gene amplification.

Science.gov (United States)

Yang, Qi; Franco, Christopher M M; Zhang, Wei

2015-10-01

Experiments were designed to validate the two common DNA extraction protocols (CTAB-based method and DNeasy Blood & Tissue Kit) used to effectively recover actinobacterial DNA from sponge samples in order to study the sponge-associated actinobacterial diversity. This was done by artificially spiking sponge samples with actinobacteria (spores, mycelia and a combination of the two). Our results demonstrated that both DNA extraction methods were effective in obtaining DNA from the sponge samples as well as the sponge samples spiked with different amounts of actinobacteria. However, it was noted that in the presence of the sponge, the bacterial 16S rRNA gene could not be amplified unless the combined DNA template was diluted. To test the hypothesis that the extracted sponge DNA contained inhibitors, dilutions of the DNA extracts were tested for six sponge species representing five orders. The results suggested that the inhibitors were co-extracted with the sponge DNA, and a high dilution of this DNA was required for the successful PCR amplification for most of the samples. The optimized PCR conditions, including primer selection, PCR reaction system and program optimization, further improved the PCR performance. However, no single PCR condition was found to be suitable for the diverse sponge samples using various primer sets. These results highlight for the first time that the DNA extraction methods used are effective in obtaining actinobacterial DNA and that the presence of inhibitors in the sponge DNA requires high dilution coupled with fine tuning of the PCR conditions to achieve success in the study of sponge-associated actinobacterial diversity.

Cloud point extraction for trace inorganic arsenic speciation analysis in water samples by hydride generation atomic fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Li, Shan, E-mail: ls_tuzi@163.com; Wang, Mei, E-mail: wmei02@163.com; Zhong, Yizhou, E-mail: yizhz@21cn.com; Zhang, Zehua, E-mail: kazuki.0101@aliyun.com; Yang, Bingyi, E-mail: e_yby@163.com

2015-09-01

A new cloud point extraction technique was established and used for the determination of trace inorganic arsenic species in water samples combined with hydride generation atomic fluorescence spectrometry (HGAFS). As(III) and As(V) were complexed with ammonium pyrrolidinedithiocarbamate and molybdate, respectively. The complexes were quantitatively extracted with the non-ionic surfactant (Triton X-114) by centrifugation. After addition of antifoam, the surfactant-rich phase containing As(III) was diluted with 5% HCl for HGAFS determination. For As(V) determination, 50% HCl was added to the surfactant-rich phase, and the mixture was placed in an ultrasonic bath at 70 °C for 30 min. As(V) was reduced to As(III) with thiourea–ascorbic acid solution, followed by HGAFS. Under the optimum conditions, limits of detection of 0.009 and 0.012 μg/L were obtained for As(III) and As(V), respectively. Concentration factors of 9.3 and 7.9, respectively, were obtained for a 50 mL sample. The precisions were 2.1% for As(III) and 2.3% for As(V). The proposed method was successfully used for the determination of trace As(III) and As(V) in water samples, with satisfactory recoveries. - Highlights: • Cloud point extraction was firstly established to determine trace inorganic arsenic(As) species combining with HGAFS. • Separate As(III) and As(V) determinations improve the accuracy. • Ultrasonic release of complexed As(V) enables complete As(V) reduction to As(III). • Direct HGAFS analysis can be performed.

Use of diluted urine for cultivation of Chlorella vulgaris.

Science.gov (United States)

Jaatinen, Sanna; Lakaniemi, Aino-Maija; Rintala, Jukka

2016-01-01

Our aim was to study the biomass growth of microalga Chlorella vulgaris using diluted human urine as a sole nutrient source. Batch cultivations (21 days) were conducted in five different urine dilutions (1:25-1:300), in 1:100-diluted urine as such and with added trace elements, and as a reference, in artificial growth medium. The highest biomass density was obtained in 1:100-diluted urine with and without additional trace elements (0.73 and 0.60 g L(-1), respectively). Similar biomass growth trends and densities were obtained with 1:25- and 1:300-diluted urine (0.52 vs. 0.48 gVSS L(-1)) indicating that urine at dilution 1:25 can be used to cultivate microalgal based biomass. Interestingly, even 1:300-diluted urine contained sufficiently nutrients and trace elements to support biomass growth. Biomass production was similar despite pH-variation from < 5 to 9 in different incubations indicating robustness of the biomass growth. Ammonium formation did not inhibit overall biomass growth. At the beginning of cultivation, the majority of the biomass consisted of living algal cells, while towards the end, their share decreased and the estimated share of bacteria and cell debris increased.

Improving the Efficiency of 3-D Hydrogeological Mixers: Dilution Enhancement Via Coupled Engineering-Induced Transient Flows and Spatial Heterogeneity

Science.gov (United States)

Di Dato, Mariaines; de Barros, Felipe P. J.; Fiori, Aldo; Bellin, Alberto

2018-03-01

Natural attenuation and in situ oxidation are commonly considered as low-cost alternatives to ex situ remediation. The efficiency of such remediation techniques is hindered by difficulties in obtaining good dilution and mixing of the contaminant, in particular if the plume deformation is physically constrained by an array of wells, which serves as a containment system. In that case, dilution may be enhanced by inducing an engineered sequence of injections and extractions from such pumping system, which also works as a hydraulic barrier. This way, the aquifer acts as a natural mixer, in a manner similar to the industrialized engineered mixers. Improving the efficiency of hydrogeological mixers is a challenging task, owing to the need to use a 3-D setup while relieving the computational burden. Analytical solutions, though approximated, are a suitable and efficient tool to seek the optimum solution among all possible flow configurations. Here we develop a novel physically based model to demonstrate how the combined spatiotemporal fluctuations of the water fluxes control solute trajectories and residence time distributions and therefore, the effectiveness of contaminant plume dilution and mixing. Our results show how external forcing configurations are capable of inducing distinct time-varying groundwater flow patterns which will yield different solute dilution rates.

A COMPARATIVE STUDY OF EXTRACT OF SUCCULENT LEAVES OF LIVING PLANT WITH METHANOLIC AND AQUEOUS EXTRACT OF BERLERIA LUPULINA LINDL. AGAINST PATHOGENIC MICROBES BY DISC DIFFUSION AND SPECTROPHOTOMETRY

Directory of Open Access Journals (Sweden)

Shibabrata Pattanayak

2014-12-01

Full Text Available Berleria lupulina Lindl. was evaluated for its reported antimicrobial activity in a novel way. The extract of succulent leaves collected from living plant was studied along with conventional methanolic and watery extracts made from the dry leaves of the plant. The extracts were tested on three pathogenic bacteria and the antimicrobial activity was tested both by conventional single disc diffusion method and a novel Spectrophotometric method. In disc diffusion study, it was found that the methanolic extract (100 mg/ml. and 200 mg/ ml. diluted in 70% of methanol and extract of succulent leaves can induce 12 mm, 13 mm and 14 mm diameter zone of inhibition comparable with 24 mm of Ceftriaxone against Escherichia coli. The zone of inhibition against Staphylococcus aureus were 13 mm, 14 mm, 15 mm and 25 mm and against Salmonella enteritides were 12 mm, 14 mm, 15 mm and 28 mm correspondingly. The watery extract made from the dry plant and the methanolic extract diluted in water failed to induce any inhibition in growth of the organisms. In spectrophotometric study, the methanolic extract showed antimicrobial efficacy in the concentration of 10 mg/ml. or above against Salmonella enteritides and Staphylococcus aureus. But against Escherichia coli, effective control was found in 20 mg/ml concentration. The fresh extract of the plant showed antimicrobial efficacy in the concentration of 16.5%. The anti microbial efficacy above that concentration cannot be detected in the available spectrophotometrical method for presence of color material in that fresh extract.

Extraction of rare earth elements with organophosphorus extractants as carriers in supported liquid membranes

International Nuclear Information System (INIS)

Kopunec, R.; Benitez, J.C.

1991-01-01

The membrane extraction of Y, Ce, Eu, Tm and their binary mixtures Ce-Y, Ce-Eu, Ce-Tm with supported liquid membranes containing TBP and HDEHP as carriers in decane-dodecane hydrocarbon solvent, has been studied. Upon extraction with TBP aqueous nitrate solutions of rare earth elements (REE) were used as feed phase. In some cases they also contained EDTA or DCTA. In most cases, the receiving phase was an aqueous solution of EDTA. Extraction with HDEHP was performed from nitrate and chloride solutions and the receiving phase was the corresponding dilute acid. Pertraction of an element through a membrane was studied as a function of time and of initial composition of phases. The results are presented in the following forms: flux of metal through membrane, coefficients of permeability, separation factors and effective diffusion coefficients. (author) 24 refs.; 8 figs.; 3 tabs

Task-specific ionic liquids for An and Ln extraction: unusual speciation and extraction mechanisms

Energy Technology Data Exchange (ETDEWEB)

Billard, Isabelle; Jobin, Emilie; Ouadi, Ali; Gaillard, Clotilde [IPHC-DRS, Chimie nucleaire, 23 rue du Loess, BP28, 67037 Strasbourg cedex 2 (France)

2008-07-01

Extraction mechanisms of uranium by TBP (tributylphosphate) diluted in an ionic liquid BumimTf{sub 2}N (1-butyl-3-methyl-imidazolium bis(tri-fluoro-methyl-sulfonyl)imide) and by Task-Specific Ionic Liquids (TSILs) bearing a phosphoryl group were investigated. Great differences between these mechanisms and the one in the industrial solvent, dodecane, have been put in evidence. While in dodecane, the neutral species, UO{sub 2}(NO{sub 3}){sub 2}(TBP){sub 2}, is the major extracted complex, in BumimTf{sub 2}N and TSILs, at least two species are extracted with more or less similar proportions. Moreover, no uranyl species with two nitrates could be observed in these ionic liquids. Finally, the mechanisms vary from TBP in BumimTf{sub 2}N to TSILs. These results led to a so-to-say new kind of actinide chemistry. (authors)

Evaluation of pharmacological effect of Teucrium stocksianum extract on angiogenesis using chorioallantoic membrane assay

Directory of Open Access Journals (Sweden)

Nazia Tabassum

2016-09-01

Full Text Available The present study was aimed to evaluate the effect of Teucrium stocksianum on angiogenesis by using chorioallantoic membrane (CAM assay. Fertilized eggs were incubated on the 5th day and dose of different dilutions 0.03%, 0.05%, 0.1%, and 0.5% of the plant extract was applied on 6th day. Evaluation of primary, secondary and tertiary blood vessels diameter and CAM area on 7th day by SPIP software. T. stocksianum showed antiangiogenic effect by reducing the diameter of CAM of blood vessels by applying the dilutions while significant results were obtained at dilution of 0.5%.

Trace analysis of U, Th and other heavy metals in high purity aluminium with isotope dilution mass spectrometry

International Nuclear Information System (INIS)

Beer, B.; Heumann, K.G.

1992-01-01

A method for the determination of very low concentrations of U, Th, Fe, Zn, Tl, Cd, Cu and Ag in high purity aluminium with isotope dilution mass spectrometry (IDMS) is developed using a compact and cost-efficient thermal ionization quadrupole mass spectrometer. The detection limits obtained are (in ng/g):U=0.018, Th=0.06, Fe=82, Zn=86, Tl=0.2, Cd=4, Cu=1, Ag=2.6. By this method it is possible to determine the α-emitters U and Th in aluminium down to the sub-ng/g level with good precision of 0.4-10% and 0.5-5%, respectively. The results should also be accurate because IDMS is a reliable analytical method. The dissolution of aluminium is carried out by aqua regia followed by the trace/matrix separation and the isolation of the trace elements by anion exchange chromatography (U, Th, Zn, Tl, Cd), electrodeposition (Cu, Ag) and extraction (Fe). Different aluminium samples are analysed by IDMS and the results are compared with those of other methods. (orig.)

Effects of hydrogen addition and nitrogen dilution on the laminar flame characteristics of premixed methane-air flames

Energy Technology Data Exchange (ETDEWEB)

Tahtouh, T.; Halter, F.; Mounaim-Rousselle, C. [Institut PRISME, Universite d' Orleans, 8 rue Leonard de Vinci-45072, Orleans Cedex 2 (France); Samson, E. [PSA Peugeot Citroen (France)

2009-10-15

The effect of hydrogen addition and nitrogen dilution on laminar flame characteristics was investigated. The spherical expanding flame technique, in a constant volume bomb, was employed to extract laminar flame characteristics. The mole fraction of hydrogen in the methane-hydrogen mixture was varied from 0 to 1 and the mole fraction of nitrogen in the total mixture (methane-hydrogen-air-diluent) from 0 to 0.35. Measurements were performed at an initial pressure of 0.1 MPa and an initial temperature of 300 K. The mixtures investigated were under stoichiometric conditions. Based on experimental measurements, a new correlation for calculating the laminar burning velocity of methane-hydrogen-air-nitrogen mixtures is proposed. The laminar burning velocity was found to increase linearly with hydrogen mass fraction for all dilution ratios while the burned gas Markstein length decreases with the increase in hydrogen amount in the mixture except for high hydrogen mole fractions (>0.6). Nitrogen dilution has a nonlinear reducing effect on the laminar burning velocity and an increasing effect on the burned gas Markstein length. The experimental results and the proposed correlation obtained are in good agreement with literature values. (author)

Helium dilution refrigerator

International Nuclear Information System (INIS)

1973-01-01

A new system of continuous heat exchange for a helium dilution refrigerator is proposed. The 3 He effluent tube is concurrent with the affluent mixed helium tube in a vertical downward direction. Heat exchange efficiency is enhanced by placing in series a number of elements with an enlarged surface area

Relative volatility of dilute solutions of Rb-Cs system

International Nuclear Information System (INIS)

Gromov, P.B.; Izotov, V.P.; Nisel'son, L.A.

1984-01-01

Relative volatility of diluted solutions Rb-Cs in the temperature range 650-820 K and pressures 13-200 gPa has been studied. The system Rb-Cs in the range of diluted solutions obeys the Henry law. It is shown, that liquid-vapour equilibrium in diluted solutions of cesium in rubidium is characterized by negative deviation from perfection

Automatic extraction of forward stroke volume using dynamic PET/CT

DEFF Research Database (Denmark)

Harms, Hans; Tolbod, Lars Poulsen; Hansson, Nils Henrik Stubkjær

2015-01-01

Background The aim of this study was to develop and validate an automated method for extracting forward stroke volume (FSV) using indicator dilution theory directly from dynamic positron emission tomography (PET) studies for two different tracers and scanners. Methods 35 subjects underwent...... a dynamic 11 C-acetate PET scan on a Siemens Biograph TruePoint-64 PET/CT (scanner I). In addition, 10 subjects underwent both dynamic 15 O-water PET and 11 C-acetate PET scans on a GE Discovery-ST PET/CT (scanner II). The left ventricular (LV)-aortic time-activity curve (TAC) was extracted automatically...... from PET data using cluster analysis. The first-pass peak was isolated by automatic extrapolation of the downslope of the TAC. FSV was calculated as the injected dose divided by the product of heart rate and the area under the curve of the first-pass peak. Gold standard FSV was measured using phase...

Neutron activation analysis of medicinal plant extracts

International Nuclear Information System (INIS)

Vaz, S.M.; Saiki, M.; Vasconcellos, M.B.A.; Sertie, J.A.A.

1995-01-01

Instrumental neutron activation analysis was applied to the determination of the elements Br, Ca, Cl, Cs, Fe, K, La, Mg, Mn, Na, Rb and Zn in medicinal extracts obtained from Centella asiatica, Citrus aurantium L., Achyrolcline satureoides DC, Casearia sylvestris, Solano lycocarpum, Zingiber officinale Roscoe, Solidago microglossa and Stryphnondedron barbatiman plants. The elements Hg and Se were determined using radiochemical separation by means of retention of Se in HMD inorganic exchanger and solvent extraction of Hg by bismuth diethyldithiocarbamate solution. Precision and accuracy of the results were evaluated by analyzing biological reference materials. The therapeutic action of some elements found in plant extracts analyzed is briefly discussed. (author). 15 refs., 5 tabs

Evaluation and validation of a single-dilution potency assay based upon serology of vaccines containing diphtheria toxoid: statistical analysis

NARCIS (Netherlands)

Marsman FR; Akkermans AM; Hendriksen CFM; de Jong WH

1993-01-01

This document presents the results of a validation study to the use of a single dilution assay in potency testing of the diphtheria component of DPT-polio vaccines. Based on historical data of multi-dilution assays on 27 consecutive batches a simulation study was performed to test the actual

Use of micro-emulsions in liquid-liquid extraction

International Nuclear Information System (INIS)

Komornicki, Jacques

1982-01-01

As liquid-liquid extraction of metallic cations is an important method of separation and concentration of metals present in diluted aqueous solutions, and as the extraction rate is limited by one or several steps of matter transfer at the liquid-liquid interface, the extraction kinetics can be improved by creating a wide surface interface and by allowing an increased reactivity between species. In this research thesis, the author aims at determining to which extent systems of interface with a wide surface obtained by using for example amphiphile molecules to create micro-emulsions, can be used as reaction media for physical-chemical processes of liquid-liquid extraction. He also aims at identifying their applicability limitations and problems which might arise with their application. The author notably focuses of the liquid-liquid extraction of metallic cations exhibiting particularly slow extraction kinetics

Accurate determination and certification of bromine in plastic by isotope dilution inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Ohata, Masaki, E-mail: m-oohata@aist.go.jp; Miura, Tsutomu

2014-07-21

Highlights: • Accurate analytical method of Br in plastic was studied by isotope dilution ICPMS. • A microwave acid digestion using quartz vessel was suitable for Br analysis. • Sample dilution by NH{sub 3} solution could remove memory effect for ICPMS measurement. • The analytical result of the ID-ICPMS showed consistency with that of INAA. • The ID-ICPMS developed could apply to certification of Br in candidate plastic CRM. - Abstract: The accurate analytical method of bromine (Br) in plastic was developed by an isotope dilution inductively coupled plasma mass spectrometry (ID-ICPMS). The figures of merit of microwave acid digestion procedures using polytetrafluoroethylene (PTFE) or quartz vessels were studied and the latter one was suitable for Br analysis since its material was free from Br contamination. The sample dilution procedures using Milli-Q water or ammonium (NH{sub 3}) solution were also studied to remove memory effect for ICPMS measurement. Although severe memory effect was observed on Milli-Q water dilution, NH{sub 3} solution could remove it successfully. The accuracy of the ID-ICPMS was validated by a certified reference material (CRM) as well as the comparison with the analytical result obtained by an instrumental neutron activation analysis (INAA) as different analytical method. From these results, the ID-ICPMS developed in the present study could be evaluated as accurate analytical method of Br in plastic materials and it could apply to certification of Br in candidate plastic CRM with respect to such regulations related to RoHS (restriction of the use of hazardous substances in electrical and electronics equipment) directive.

Anti-leech activity of Scutellaria baicalensis and Morinda citrifolia extracts against Piscicola geometra

Science.gov (United States)

Rizky, P. N.; Cheng, T. C.; Nursyam, H.

2018-04-01

Piscicola geometra leeches are naturally infecting cobia juvenile. The leeches attach to cobia by sucking and biting its surface and provide the gate of second infection. Water extracts of Scutellaria baicalensis root and Morinda citrifolia leaves were used to be tested through In Vitro method to look for the anti-leeches activity against Piscicola geometra. In this study, a total number of 800 leeches from infected cobia were prepared. The anti-leech activity from water extract of S. baicalensis root and M. citrifolia leaves were compared in different dilutions of plant extracts for 96 hours. Significant anti-leech activity was observed with M. citrifolia leaves with 80% mortality of leeches. S. baicalensis root showed higher anti-leech activity with 100% mortality of leeches. The average time was needed for S.baicalensis root to paralyzing and kill the leeches were 8h, 40h, 48h, 72h, and 96h in various dilutions of S. baicalensis root. This study indicated that S. baicalensis water extract had a potent for new anti-leeches agent.

Analytical and preparative separation of organic acids from water by extraction with trioctylamine

International Nuclear Information System (INIS)

Eberle, S.H.; Hoyer, O.; Knobel, K.P.; Hodenberg, S. von

1977-12-01

The extraction of pure organic acids and of humic and ligninsulfonic acid from water by a solution of trioctylamine in chloroform was investigated (technical grade amine = ALAMINE). Quantitative separation is achieved by double extraction with 5% ALAMINE at pH 3,5 - 4. The acids may be back-extracted with dilute sodium hydroxide solution. Procedures are described for the analytical extraction of water samples of 200 to 2.000 ml and for the flow-through processing of large water volumes. (orig.) [de

Synergistic Extraction of Lactic Acid with Tri-n-Octylamine and Try-n-Butylphosphate

Energy Technology Data Exchange (ETDEWEB)

Matsumoto, Michiaki.; Yuba, Seiji.; Kondo, Kazuo. (Doshisha University, Department of Chemical Engineering and Materials Science (Japan))

1998-12-01

Synergistic extraction system of lactic acid is examined to develop to in situ extractive fermentation process. The addition of try-n-butyl phosphate(TBP) to the extraction system of lactic acid(HA) with tri-n-actylamine(TOA) diluted by hexane causes a large synergism. Extraction reaction with the mixed extractant is interpreted quite well based on the formation of mixed complex, HA[center dot]TOA[center dot]2TBP. Though the addition of hexane solution containing TBP and TOA to the culture of Lactobacillus rhamnosus results in low lactate production, some lactate is produced. (author)

Synergistic Extraction of Lactic Acid with Tri-n-Octylamine and Try-n-Butylphosphate

Energy Technology Data Exchange (ETDEWEB)

Matsumoto, Michiaki.; Yuba, Seiji.; Kondo, Kazuo. [Doshisha University, Department of Chemical Engineering and Materials Science (Japan)

1998-12-01

Synergistic extraction system of lactic acid is examined to develop to in situ extractive fermentation process. The addition of try-n-butyl phosphate(TBP) to the extraction system of lactic acid(HA) with tri-n-actylamine(TOA) diluted by hexane causes a large synergism. Extraction reaction with the mixed extractant is interpreted quite well based on the formation of mixed complex, HA{center_dot}TOA{center_dot}2TBP. Though the addition of hexane solution containing TBP and TOA to the culture of Lactobacillus rhamnosus results in low lactate production, some lactate is produced. (author)

Activity coefficients at infinite dilution for hydrocarbons in furfuryl alcohol at T=(278.15 and 298.15) K, determined by g.l.c

International Nuclear Information System (INIS)

Kozlowska, Marta K.; Letcher, Trevor M.; Domanska, Urszula

2004-01-01

The potential of the polar solvent, furfuryl alcohol, as a solvent in the separation of aromatics from aliphatics and other hydrocarbons, has been investigated by measuring activity coefficients at infinite dilution. The activity coefficients at infinite dilution for some alkanes, cycloalkanes, alkenes, alkynes and benzene in furfuryl alcohol have been determined by g.l.c. at T=(278.15 and 298.15) K. The method used is we believe, a more controlled and reliable method than the alternative pre-saturation method. The results have been used to calculate the selectivity factor and hence predict the potential for furfuryl alcohol as a solvent in separating aromatic compounds from aliphatic compounds and other hydrocarbons using extractive distillation. The results have been compared to the recently published work on a related polar solvent - furfural. The excess enthalpies of mixing at infinite dilution have also been calculated

Optimisation of beryllium-7 gamma analysis following BCR sequential extraction

Energy Technology Data Exchange (ETDEWEB)

Taylor, A. [Plymouth University, School of Geography, Earth and Environmental Sciences, 8 Kirkby Place, Plymouth PL4 8AA (United Kingdom); Blake, W.H., E-mail: wblake@plymouth.ac.uk [Plymouth University, School of Geography, Earth and Environmental Sciences, 8 Kirkby Place, Plymouth PL4 8AA (United Kingdom); Keith-Roach, M.J. [Plymouth University, School of Geography, Earth and Environmental Sciences, 8 Kirkby Place, Plymouth PL4 8AA (United Kingdom); Kemakta Konsult, Stockholm (Sweden)

2012-03-30

Graphical abstract: Showing decrease in analytical uncertainty using the optimal (combined preconcentrated sample extract) method. nv (no value) where extract activities were extraction with natural {sup 7}Be returns high analytical uncertainties. Black-Right-Pointing-Pointer Preconcentrating extracts from a large sample mass improved analytical uncertainty. Black-Right-Pointing-Pointer This optimised method can be readily employed in studies using low activity samples. - Abstract: The application of cosmogenic {sup 7}Be as a sediment tracer at the catchment-scale requires an understanding of its geochemical associations in soil to underpin the assumption of irreversible adsorption. Sequential extractions offer a readily accessible means of determining the associations of {sup 7}Be with operationally defined soil phases. However, the subdivision of the low activity concentrations of fallout {sup 7}Be in soils into geochemical fractions can introduce high gamma counting uncertainties. Extending analysis time significantly is not always an option for batches of samples, owing to the on-going decay of {sup 7}Be (t{sub 1/2} = 53.3 days). Here, three different methods of preparing and quantifying {sup 7}Be extracted using the optimised BCR three-step scheme have been evaluated and compared with a focus on reducing analytical uncertainties. The optimal method involved carrying out the BCR extraction in triplicate, sub-sampling each set of triplicates for stable Be analysis before combining each set and coprecipitating the {sup 7}Be with metal oxyhydroxides to produce a thin source for gamma analysis. This method was applied to BCR extractions of natural {sup 7}Be in four agricultural soils. The approach gave good counting statistics from a 24 h analysis period ({approx}10% (2

Antimicrobial and cytotoxic potentials of Buddleja polystachya extracts

Directory of Open Access Journals (Sweden)

Ghada Ahmed Fawzy

2013-06-01

Full Text Available Most of the species of Buddleja have found applications in folk medicine. This study aimed to evaluate the in vitro antimicrobial and cytotoxic potentials of B. polystachya extracts. Four extracts were prepared A-D (dichloromethane, ethyl acetate, n-butanol, and aqueous extracts, respectively. The antimicrobial activity was evaluated using the broth micro-dilution assay for minimum inhibitory concentrations (MIC. The crystal violet staining method (CVS was used for the evaluation of the cytotoxic activity on HepG-2, MCF-7 and HCT-116 human cell lines. Results showed that the highest antimicrobial activity was given by the ethyl acetate extract followed by the dichloromethane extract, while the n-butanol revealed moderate activity against gram positive bacteria only with no activity against the rest of tested microorganisms. The aqueous extract was totally ineffective against all tested microorganisms at 20 mg/ml. Among the four extracts tested, dichloromethane and ethyl acetate extracts showed the highest cytotoxic activity on all three human cell lines.

Characteristics of Lignin Fractions from Dilute Acid Pretreated Switchgrass and Their Effect on Cellobiohydrolase from Trichoderma longibrachiatum

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Lan Yao

2018-02-01

Full Text Available To investigate the interactions between acid pretreated switchgrass lignin and cellobiohydrolase (CBH, three different lignin fractions were isolated from dilute acid pretreated switchgrass by (i ethanol extraction, followed by (ii dioxane/H2O extraction, and (iii cellulase treatment, respectively. Structural properties of each lignin fraction were elucidated by GPC, 13C-NMR, and 2D-HSQC NMR analyses. The adsorptions of CBH to the isolated lignin fractions were also studied by Langmuir adsorption isotherms. Ethanol-extractable lignin fraction, mainly composed of syringyl (S and guaiacyl (G units, had the lowest molecular weight, while dioxane/H2O-extracted lignin fraction had the lowest S/G ratio with higher content of p-coumaric acid (pCA unit. The residual lignin fraction after enzymatic treatment had the highest S/G ratio without hydroxyphenyl (H unit. Strong associations were found between lignin properties such as lignin composition and S/G ratio and its non-productive enzyme adsorption factors including the maximum adsorption capacity and binding strength.

Human DNA Extraction by Two Extraction Methods for Forensic Typification from Human Feces on FTA Paper

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Shirleny Monserrat Sandoval-Arias

2014-11-01

Full Text Available The identification of suspects in criminal investigations has been facilitated since DNA test are executed on different samples. The application of this technology for forensic typification from human fecal samples still presents complications therefore this research evaluated two DNA extraction protocols with modifications to determine that of major efficiency. Organic extractions and extractions using the commercial kit “IQTM DNA Casework Sample Kit for Maxwell ® 16” on FTA portions of 4cm2 and 1cm2 impregnated with feces from the same individual were done to accomplish the objective. In all the assays the results were useful, however; the best forensic typification (by the electropherogram characteristics was obtained by using the commercial kit in an area of 1 cm2 of FTA paper impregnated in a 1:4 dilution.

Study of oxygen diluted silane plasmas applied for the deposition of silicium oxyde

International Nuclear Information System (INIS)

Magni, D.

2001-09-01

plasmas was studied as a function of the radiofrequency power, at high and low dilution. Analysis of the infrared spectra gives the size, the number density, the structure and the composition of particles. At high dilution conditions ([O 2 ]/[HMDSO] = 30), the particles are amorphous and composed of silicon dioxide. The particles radius is estimated at around 200 nm and the number density at 4 10 12 m-3. At low dilution conditions in oxygen, ([O 2 ]/[HMDSO] = 1), the particles are amorphous and composed of silicon oxide. The particle radius is around 300 nm and the number density in the region of 5 10 12 m-3. At low dilution, the estimations of the HMDSO depletion as a function of the RF power have shown that the increase of the volume fraction is due to the increase of the depletion. The carbon and hydrogen concentrations, based on a qualitative analysis of the infrared absorption spectra, decrease as a function of the RF power. These results were confirmed by high resolution transmission electron microscopy (Hr- Tem) and by electron energy loss spectroscopy (Eels). Particle formation in oxygen-diluted HMDSO plasmas was studied as a function of time by means of in situ infrared absorption spectroscopy, Mie-scattering and optical emission spectroscopy. Analysis of the infrared spectra has shown a first agglomeration of particles of about 40 nm diameter, responsible for a strong increase in the carbon and hydrogen concentrations during the first 30 seconds of the plasma. The infrared spectra also showed that from 60 s to 150 s, the particle radius increases from 200 nm to 300 nm, and then the particles agglomerate to form micrometer sized fractal structures which can leave the plasma through the sheath by gravity . The composition of the particles produced in oxygen-diluted HMDSO plasmas was compared to the composition of thin films produced in the same conditions. It is shown that oxygen etches the carbon present in the particles and the carbon present in the film. Oxygen

Use of real-time PCR to evaluate two DNA extraction methods from food

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Maria Regina Branquinho

2012-03-01

Full Text Available The DNA extraction is a critical step in Genetically Modified Organisms analysis based on real-time PCR. In this study, the CTAB and DNeasy methods provided good quality and quantity of DNA from the texturized soy protein, infant formula, and soy milk samples. Concerning the Certified Reference Material consisting of 5% Roundup Ready® soybean, neither method yielded DNA of good quality. However, the dilution test applied in the CTAB extracts showed no interference of inhibitory substances. The PCR efficiencies of lectin target amplification were not statistically different, and the coefficients of correlation (R² demonstrated high degree of correlation between the copy numbers and the threshold cycle (Ct values. ANOVA showed suitable adjustment of the regression and absence of significant linear deviations. The efficiencies of the p35S amplification were not statistically different, and all R² values using DNeasy extracts were above 0.98 with no significant linear deviations. Two out of three R² values using CTAB extracts were lower than 0.98, corresponding to lower degree of correlation, and the lack-of-fit test showed significant linear deviation in one run. The comparative analysis of the Ct values for the p35S and lectin targets demonstrated no statistical significant differences between the analytical curves of each target.

Studies on the analysis of 25-hydroxyvitamin D3 by isotope-dilution liquid chromatography–tandem mass spectrometry using enzyme-assisted derivatisation

International Nuclear Information System (INIS)

Abdel-Khalik, Jonas; Crick, Peter J.; Carter, Graham D.; Makin, Hugh L.; Wang, Yuqin; Griffiths, William J.

2014-01-01

Highlights: • New method for the analysis of 25-hydroxyvitamin D 3 exploiting Girard P derivatisation. • Method also applicable to vitamin D 3 , 1α,25- and 24,25-dihydroxyvitamin D 3 . • By modification of the method 3-epi-25-hydroxyvitamin D 3 can also be analysed. - Abstract: The total serum concentration of 25-hydroxyvitamins D (25-hydroxyvitamin D 3 and 25-hydroxyvitamin D 2 ) is currently used as an indicator of vitamins D status. Vitamins D insufficiency is claimed to be associated with multiple diseases, thus accurate and precise reference methods for the quantification of 25-hydroxyvitamins D are needed. Here we present a novel enzyme-assisted derivatisation method for the analysis of vitamins D metabolites in adult serum utilising 25-[26,26,26,27,27,27- 2 H 6 ]hydroxyvitamin D 3 as the internal standard. Extraction of 25-hydroxyvitamins D from serum is performed with acetonitrile, which is shown to be more efficient than ethanol. Cholesterol oxidase is used to oxidize the 3β-hydroxy group in the vitamins D metabolites followed by derivatisation of the newly formed 3-oxo group with Girard P reagent. 17β-Hydroxysteroid dehydrogenase type 10 is shown to oxidize selectively the 3α-hydroxy group in the 3α-hydroxy epimer of 25-hydroxyvitamin D 3 . Quantification is achieved by isotope-dilution liquid chromatography–tandem mass spectrometry. Recovery experiments for 25-hydroxyvitamin D 3 performed on adult human serum give recovery of 102–106%. Furthermore in addition to 25-hydroxyvitamin D 3 , 24,25-dihydroxyvitamin D 3 and other uncharacterised dihydroxy metabolites, were detected in adult human serum

Extractive spectrophotometric determination of uranium with malachite green

Energy Technology Data Exchange (ETDEWEB)

Dubey, S C; Nadkarni, M N [Bhabha Atomic Research Centre, Bombay (India). Fuel Reprocessing Div.

1977-04-01

A sensitive spectrophotometric method based on the extraction of a uranium-benzoate-Malachite Green complex by chlorobenzene is described. The absorption maximum is at 635 nm and the molar absorptivity is 8.3 x 10/sup 4/1. mole /sup -1/ cm/sup -1/. A preliminary separation of uranium by extraction with methyl isobutyl ketone from acid-deficient aluminium nitrate solution is used to avoid interferences. An aliquot of the extract in then diluted with chlorobenzene and shaken with benzoate buffer containing Malachite Green (MG). The method has been applied for the determination of uranium in a synthetic leach solution. The complex extracted is probably (U0/sub 2/(C/sub 6/H/sub 5/C00/sub 3//sup -/)(MG/sup +/).

Determination of photooxygenation products of rotenone with isotope dilution method

International Nuclear Information System (INIS)

Chubachi, Mitsuo; Hamada, Masayuki

1975-01-01

When rotenone dissolved in certain solvent was photochemically oxidized, rotenolones, dehydrorotenone and rotenonone were obtained as main products. In order to determine the quantitative yields of these compounds in photooxygenation products, four compounds mentioned above were labeled with carbon-14 and the isotope dilution method by these labeled compounds was applied to the product analysis. (auth.)

On the nitrogen isotope dilution analysis by means of the automated NA-5A type 15N-analyzer

International Nuclear Information System (INIS)

Faust, H.; Mueller, G.; Stoerl, H.J.

1976-01-01

The analytical conditions are investigated under which quantitative nitrogen determination through isotope dilution analysis is possible using the NA-5A type 15 N-analyzer. Calculation of the nitrogen quantity, estimation of the maximum error and the evaluation technique are considered in detail. Test analyses performed on ammonia, urea, and amino acid nitrogen model solutions labelled in different ways yielded good correspondence with preset values. This technique was applied to determine the nitrogen content of biomedical materials. A working scheme for direct quantitative determination of ammonia-N, urea-N, and total-N in urine is presented. (author)

A Study Of The Dilution Of Radio-Active Waste In The Rhone (1961); Etude de la dilution dans le rhone des effluents radioactifs du Centre de Marcoule (1961)

Energy Technology Data Exchange (ETDEWEB)

Rodier, J; Scheidhauer, J; Marichal, M; Court, R [Commissariat a l' Energie Atomique, Centre de Production de Plutonium, Marcoule (France). Centre d' Etudes Nucleaires

1961-07-01

The discharge into the Rhone of liquid radio-active waste from the Marcoule Centre necessitates a large number of measurements, in particular chemical and radio-chemical analysis of the waste, itself and of the waters of the Rhone both above arid below the point of discharge. The results thus obtained during 1960 made it possible to evaluate the total amount of active waste discharged and its dilution in the receiving medium. A statistical study of the results of the analysis of the Rhone waters shows that a satisfactory dilution of the waste occurs rapidly; the experimental results obtained with an experimental discharge of rhodamine are thus confirmed. (authors) [French] Le rejet au Rhone des effluents radioactifs liquides produits sur le Centre de Marcoule donne lieu a un grand nombre de mesures et en particulier d'analyses chimiques et radio-chimiques des effluents eux-memes ainsi que des eaux du Rhone avant et apres rejet. Au cours de l'annee 1960, l'ensemble des resultats ainsi obtenus a permis de dresser un bilan des activites rejetees et de leur dispersion dans le milieu recepteur. Une etude statistique des resultats d'analyses des eaux du Rhone montre qu'une dilution satisfaisante des effluents s'effectue rapidement confirmant ainsi les resultats obtenus lors d'un rejet experimental de rhodamine. (auteurs)

An overview the boron dilution issue in PWRs

International Nuclear Information System (INIS)

Hyvaerinen, J.

1994-01-01

The presentation is an overview of boron (boric acid) dilution in pressurized water reactors (PWRs). Boric acid has been widely used in PWRs as a dissolved poison, as one of the main reactivity controlling means, for a long time, from nearly but not quite from the beginning of the design, construction and operation of PWRs in the present-day sense. The specific safety issue, namely the risk of uncontrolled reactivity insertion due to inadvertent boron dilution, is discussed first, followed by a brief look on the history of boron usage in PWRs. A discussion of boron dilution phenomenology is presented next in general terms. Some particular concerns that boron dilution phenomena arouse in the minds of a regulator will also be presented before concluding with a brief look on the future of dissolved poisons. (11 refs.)

[Analysis of triterpenoids in Ganoderma lucidum by microwave-assisted continuous extraction].

Science.gov (United States)

Lu, Yan-fang; An, Jing; Jiang, Ye

2015-04-01

For further improving the extraction efficiency of microwave extraction, a microwave-assisted contijuous extraction (MACE) device has been designed and utilized. By contrasting with the traditional methods, the characteristics and extraction efficiency of MACE has also been studied. The method was validated by the analysis of the triterpenoids in Ganoderma lucidum. The extraction conditions of MACE were: using 95% ethanol as solvent, microwave power 200 W and radiation time 14.5 min (5 cycles). The extraction results were subsequently compared with traditional heat reflux extraction ( HRE) , soxhlet extraction (SE), ultrasonic extraction ( UE) as well as the conventional microwave extraction (ME). For triterpenoids, the two methods based on the microwaves (ME and MACE) were in general capable of finishing the extraction in 10, 14.5 min, respectively, while other methods should consume 60 min and even more than 100 min. Additionally, ME can produce comparable extraction results as the classical HRE and higher extraction yield than both SE and UE, however, notably lower extraction yield than MASE. More importantly, the purity of the crud extract by MACE is far better than the other methods. MACE can effectively combine the advantages of microwave extraction and soxhlet extraction, thus enabling a more complete extraction of the analytes of TCMs in comparison with ME. And therefore makes the analytic result more accurate. It provides a novel, high efficient, rapid and reliable pretreatment technique for the analysis of TCMs, and it could potentially be extended to ingredient preparation or extracting techniques of TCMs.

Anti-bacterial activities and phytochemical screening of extracts of ...

African Journals Online (AJOL)

Anti-bacterial activity tests were carried out using disc diffusion assay and tube dilution technique, and phytochemical screening was carried out through Thin Layer Chromatography. The crude extracts showed antibacterial effects on M. vaccae, P. aeruginosa and B. subtilis. M. vaccae was most sensitive, particularly to the ...

Specific heat in diluted magnetic semiconductor quantum ring

Science.gov (United States)

Babanlı, A. M.; Ibragimov, B. G.

2017-11-01

In the present paper, we have calculated the specific heat and magnetization of a quantum ring of a diluted magnetic semiconductor (DMS) material in the presence of magnetic field. We take into account the effect of Rashba spin-orbital interaction, the exchange interaction and the Zeeman term on the specific heat. We have calculated the energy spectrum of the electrons in diluted magnetic semiconductor quantum ring. Moreover we have calculated the specific heat dependency on the magnetic field and Mn concentration at finite temperature of a diluted magnetic semiconductor quantum ring.

The dilution effect on the extinction of wall diffusion flame

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Ghiti Nadjib

2014-12-01

Full Text Available The dynamic process of the interaction between a turbulent jet diffusion methane flame and a lateral wall was experimentally studied. The evolution of the flame temperature field with the Nitrogen dilution of the methane jet flame was examined. The interaction between the diffusion flame and the lateral wall was investigated for different distance between the wall and the central axes of the jet flame. The dilution is found to play the central role in the flame extinction process. The flame response as the lateral wall approaches from infinity and the increasing of the dilution rate make the flame extinction more rapid than the flame without dilution, when the nitrogen dilution rate increase the flame temperature decrease.

Validation of the IDS Octeia ELISA for the determination of insulin-like growth factor 1 in equine serum and tendon tissue extracts

DEFF Research Database (Denmark)

Lygren, Tone; Schjerling, Peter; Jacobsen, Stine

2013-01-01

BACKGROUND: Insulin-like growth factor (IGF-1) is an important mediator of tissue repair in horses. OBJECTIVES: The aim of the study was to evaluate whether IGF-1 could be measured reliably in equine serum and tendon tissue extracts, using an IGF-1 ELISA kit developed for human serum and plasma...... diluted equine serum samples and tendon tissue extracts. The recovery of IGF-1 was evaluated in serum and tendon tissue extracts spiked with known amounts of IGF-1. RESULTS: The range of IGF-1 released using the manufacturer's pretreatment was between 23% and 56% of the amount released using the gly...... with serum, and 72 ± 15% when diluted with PBS. The recovery after dilution was 108 ± 17% in tendon tissue extracts. Recovery from serum spiked with a fixed amount of IGF-1 was 101 ± 5% and 99 ± 7% from tendon tissue samples. CONCLUSIONS: The IDS Octeia IGF-1 ELISA kit can be used for measuring IGF-1...

Chemical composition and antibacterial activity of Cordia verbenacea extracts obtained by different methods.

Science.gov (United States)

Michielin, Eliane M Z; Salvador, Ana A; Riehl, Carlos A S; Smânia, Artur; Smânia, Elza F A; Ferreira, Sandra R S

2009-12-01

The present study describes the chemical composition and the antibacterial activity of extracts from Cordia verbenacea DC (Borraginaceae), a traditional medicinal plant that grows widely along the southeastern coast of Brazil. The extracts were obtained using different extraction techniques: high-pressure operations and low-pressure methods. The high-pressure technique was applied to obtain C. verbenacea extracts using pure CO(2) and CO(2) with co-solvent at pressures up to 30MPa and temperatures of 30, 40 and 50 degrees C. Organic solvents such as n-hexane, ethyl acetate, ethanol, acetone and dichloromethane were used to obtain extracts by low-pressure processes. The antibacterial activity of the extracts was also subjected to screening against four strains of bacteria using the agar dilution method. The extraction yields were up to 5.0% w/w and up to 8.6% w/w for supercritical fluid extraction with pure CO(2) and with ethyl acetate as co-solvent, respectively, while the low-pressure extraction indicates yields up to 24.0% w/w in the soxhlet extraction using water and aqueous mixture with 50% ethanol as solvents. The inhibitory activity of the extracts in gram-positive bacteria was significantly higher than in gram-negative. The quantification and the identification of the extracts recovered were accomplished using GC/MS analysis. The most important components identified in the extract were artemetin, beta-sitosterol, alpha-humulene and beta-caryophyllene, among others.

Total cholesterol in serum determined by isotope dilution/mass spectrometry, with liquid-chromatographic separation

International Nuclear Information System (INIS)

Takatsu, Akiko; Nishi, Sueo

1988-01-01

We describe an accurate, precise method for determination of total serum cholesterol by isotope dilution/mass spectrometry (IDMS) with liquid chromatographic separation. After adding [3,4- 13 C] cholesterol to serum and hydrolyzing the cholesterol esters, we extract the total cholesterol. High-performance liquid chromatography (HPLC) is used to separate the extracted cholesterol for measurement by electron-impact mass spectrometry with use of a direct-insertion device. To evaluate the specificity and the accuracy of this method, we also studied the conventional IDMS method, which involves converting cholesterol to the trimethylsilyl ether and assay by gas chromatography-mass spectrometry with use of a capillary column. The coefficient of variation for the HPLC method was a little larger than for the conventional method, but mean values by each method agreed within 1% for all sera tested. (author)

Analysis preliminary phytochemical raw extract of leaves Nephrolepis pectinata

Directory of Open Access Journals (Sweden)

Natally Marreiros Gomes

2017-06-01

Full Text Available The Nephrolepis pectinata popularly known as paulista fern, ladder-heaven, cat tail, belongs to the family Davalliaceae. For the beauty of the arrangements of their leaves ferns are quite commercialized in Brazil, however, have not been described in the literature studies on their pharmacological potential. Thus, the objective of this research was to analyze the phytochemical properties of the crude extract of the leaves of Nephrolepis pectinata. To perform the phytochemical analysis were initially made the collection of the vegetable, preparation of voucher specimen, washing, drying and grinding. Then, extraction by percolation method and end the phytochemical analysis. Preliminary results phytochemicals the crude extract of the leaves of Nephrolepis pectinata tested positive for reducing sugars, phenols/tannins (catechins tannins and catechins.

A report on the aquatic dilution experiment carried out at discharge canal, KGS site

International Nuclear Information System (INIS)

Reji, T.K.; Nayak, P.D.; Sudhakar, J.; Ajith, T.L.; Vishnu, M.S.; Ravi, P.M.; James, J.P.; Joshi, R.M.; Naik, S.B.; Kudtharkar, A.M.; Gaonkar, S.M.; Verma, P.C.; Datta, D.; Dahiya, Sudhir; Brijkumar; Datta, Maduparna; Sajeevan, G.

2009-08-01

Under Nuclear Power Corporation of India Limited (NPCIL), three units of (each of capacity 220MWe) Nuclear Power Stations are operational and one unit of similar capacity is under advanced stage of construction at Kaiga site. The radioactive liquid effluents generated in the plant are diluted with Condenser Coolant Water Stream (CCW) which is then discharged into Kadra reservoir through an artificially made discharge canal. The basic objective of the present study is to estimate the Dilution Factors at various locations of discharge canal and to understand the process of dilution and dispersion of radioactive effluent in the discharge canal. The strategy of the experiment involved the collection of samples from discharge canal lengthwise, breadth wise and depth wise immediately after the routine release of one of the batches of effluent stream into the CCW stream. No additional activity was released for the purpose of this experiment. The study compared the experimentally obtained Dilution Factor with that calculated based on the flow rates of CCW pumps and active liquid effluent discharge pumps. In the present conditions of experiment, Dilution Factor, based on flow rates of CCW pumps and Liquid Effluent Discharge pump, works out to be 8.11 E -05 while experimentally observed Mean Dilution Factor in the discharge canal works out to be (7.75±2.15) E-05. Hence this experiment clearly demonstrate the validity of the method of calculating dilution factor based on the flow rates of CCW line and that of Effluent discharge pump. The data analysis indicates that mass flow seems to be the major process of dispersion in the discharge canal. The tritium activity was found to be moving faster in the midstream as compared to that near the shore. The conclusions are drawn purely based on experimental results. This experimental data can be used for validation of aquatic dispersion models. (author)

Isolation and structural characterization of sugarcane bagasse lignin after dilute phosphoric acid plus steam explosion pretreatment and its effect on cellulose hydrolysis

Science.gov (United States)

Jijiao Zeng; Zhaohui Tong; Letian Wang; J.Y. Zhu; Lonnie Ingram

2014-01-01

The structure of lignin after dilute phosphoric acid plus steam explosion pretreatment process of sugarcane bagasse in a pilot scale and the effect of the lignin extracted by ethanol on subsequent cellulose hydrolysis were investigated. The lignin structural changes caused by pretreatment were identified using advanced nondestructive techniques such as gel permeation...

Isotope dilution mass spectrometry: some present limitations and possibilities to overcome these

International Nuclear Information System (INIS)

De Bievre, P.

1981-01-01

Thermionic mass spectrometry still has great potential for more precise and accurate measurements but it is going to place tremendous requirements on (1) the chemical purity of the samples we measure, (2) the temperature of both ionization and the filaments and (3) the number of molecular species being handled in ion sources which could increase to several dozen for one type of isotopic analysis. The lack of control by mass spectrometrists over the chemical preparation of the samples for isotopic analysis is an inherent limitation to further improvement of isotope dilution mass spectrometry. A limiting factor in isotope dilution is the ability to measure the ratio. At present, uranium isotopic reference materials are 0.1% and recently one was prepared at 0.05%. As these serve to calibrate isotope ratio measurements one cannot do better than these valves. There is no way in which isotope dilution can be improved until these reference values improve. For plutonium there are not even absolute isotope ratio standards. An agreement has been established between CBNM, Geel and the National Bureau of Standards, Washington, to prepare isotope ratio reference materials jointly so that they will be common to both communities. It is recommended that common batches of reference be established and stored at several places to guarantee accessibility at all times

Hydraulic evaluation of the groundwater conditions at Finnsjoen. The effects on dilution in a domestic well

International Nuclear Information System (INIS)

Axelsson, C.L.; Bystroem, J.; Eriksson, Aa.; Holmen, J.; Haitjema, H.M.

1991-09-01

The Swedish Nuclear Fuel and Waste Management Company (SKB) is presently performing a safety analysis study, SKB 91, for a final repository for spent nuclear fuel. The study is carried out for a generic repository located to the Finnsjoen area, which is one of SKBs oldest study-areas. An important part of the safety analysis is the dose calculations. Radionuclides can be transported to the biosphere via the sea, a lake, and via extraction of groundwater from drilled or dug wells. Thus, an important scenario to study is the dilution of radionuclides in a domestic well drilled in the future close to the repository. The present study is discussing; * Localization, drilling and construction of wells. * Specific capacities and chloride content of the rock mass and wells found in the Finnsjoe are. * Risk areas for future drilled wells. * Dilution in future wells drilled in fracture zones or in the hard rock in the vicinity of the repository. The evaluations show that a well pumping 6 m 3 /day, located in a fracture zone or in the rock mass, has no influence on the local groundwater flow system except for the very vicinity of the well. Consequently, a well may be drilled in the hard rock without any risk of pumping groundwater that has passed the repository. Wells may also be located anywhere in fracture zones, except for in the very discharge area, without any risk of getting groundwater affected by the repository. Modelling indicate that a well drilled in the discharge area for contaminated groundwater, may collect all groundwater from the repository. However, this is based on assumptions of homogeneous continuous fracture zones with a high hydraulic conductivity compared to the rock mass, which will give rise to a concentrated discharge area. (44 refs., 31 figs., 6 tabs.) (au)

Effects of dissolved species on radiolysis of diluted seawater

International Nuclear Information System (INIS)

Hata, Kuniki; Hanawa, Satoshi; Kasahara, Shigeki; Motooka, Takafumi; Tsukada, Takashi; Muroya, Yusa; Yamashita, Shinichi; Katsumura, Yosuke

2014-01-01

Fukushima Daiichi Nuclear Power Plants (NPPs) experienced seawater injection into the cores and fuel pools as an emergent measure after the accident. After the accident, retained water has been continuously desalinized, and subsequently the concentration of chloride ion (Cl"-) has been kept at a lower level these days. These ions in seawater are known to affect water radiolysis, which causes the production of radiolytic products, such as hydrogen peroxide (H_2O_2), molecular hydrogen (H_2) and molecular oxygen (O_2). However, the effects of dissolved ions relating seawater on the production of the stable radiolytic products are not well understood in the diluted seawater. To understand of the production behavior in diluted seawater under radiation, radiolysis calculations were carried out. Production of H_2 is effectively suppressed by diluting by up to vol10%. The concentrations of oxidants (H_2O_2 and O_2) are also suppressed by dilution of dissolved species. The effect of oxidants on corrosion of materials is thought to be low when the seawater was diluted by less than 1 vol% by water. It is also shown that deaeration is one of the effective measure to suppress the concentrations of oxidants at a lower level for any dilution conditions. (author)

Yfiler® Plus population samples and dilution series

DEFF Research Database (Denmark)

Andersen, Mikkel Meyer; Mogensen, Helle Smidt; Eriksen, Poul Svante

2017-01-01

DNA complicated the analysis by causing drop-ins of characteristic female DNA artefacts. Even though the customised analytical threshold in combination with the custom-made artefact filters gave more alleles, crime scene samples still needed special attention from the forensic geneticist....... dynamics and performance. We determined dye-dependent analytical thresholds by receiver operating characteristics (ROC) and made a customised artefact filter that includes theoretical known artefacts by use of previously analysed population samples. Dilution series of known male DNA and a selection...

Near-wall molecular ordering of dilute ionic liquids

NARCIS (Netherlands)

Jitvisate, Monchai; Seddon, James Richard Thorley

2017-01-01

The interfacial behavior of ionic liquids promises tunable lubrication as well as playing an integral role in ion diffusion for electron transfer. Diluting the ionic liquids optimizes bulk parameters, such as electric conductivity, and one would expect dilution to disrupt the near-wall molecular

On the Wigner law in dilute random matrices

Science.gov (United States)

Khorunzhy, A.; Rodgers, G. J.

1998-12-01

We consider ensembles of N × N symmetric matrices whose entries are weakly dependent random variables. We show that random dilution can change the limiting eigenvalue distribution of such matrices. We prove that under general and natural conditions the normalised eigenvalue counting function coincides with the semicircle (Wigner) distribution in the limit N → ∞. This can be explained by the observation that dilution (or more generally, random modulation) eliminates the weak dependence (or correlations) between random matrix entries. It also supports our earlier conjecture that the Wigner distribution is stable to random dilution and modulation.

Asymptotic Distribution of Eigenvalues of Weakly Dilute Wishart Matrices

Energy Technology Data Exchange (ETDEWEB)

Khorunzhy, A. [Institute for Low Temperature Physics (Ukraine)], E-mail: khorunjy@ilt.kharkov.ua; Rodgers, G. J. [Brunel University, Uxbridge, Department of Mathematics and Statistics (United Kingdom)], E-mail: g.j.rodgers@brunel.ac.uk

2000-03-15

We study the eigenvalue distribution of large random matrices that are randomly diluted. We consider two random matrix ensembles that in the pure (nondilute) case have a limiting eigenvalue distribution with a singular component at the origin. These include the Wishart random matrix ensemble and Gaussian random matrices with correlated entries. Our results show that the singularity in the eigenvalue distribution is rather unstable under dilution and that even weak dilution destroys it.

Modeling syngas-fired gas turbine engines with two dilutants

Science.gov (United States)

Hawk, Mitchell E.

2011-12-01

Prior gas turbine engine modeling work at the University of Wyoming studied cycle performance and turbine design with air and CO2-diluted GTE cycles fired with methane and syngas fuels. Two of the cycles examined were unconventional and innovative. The work presented herein reexamines prior results and expands the modeling by including the impacts of turbine cooling and CO2 sequestration on GTE cycle performance. The simple, conventional regeneration and two alternative regeneration cycle configurations were examined. In contrast to air dilution, CO2 -diluted cycle efficiencies increased by approximately 1.0 percentage point for the three regeneration configurations examined, while the efficiency of the CO2-diluted simple cycle decreased by approximately 5.0 percentage points. For CO2-diluted cycles with a closed-exhaust recycling path, an optimum CO2-recycle pressure was determined for each configuration that was significantly lower than atmospheric pressure. Un-cooled alternative regeneration configurations with CO2 recycling achieved efficiencies near 50%, which was approximately 3.0 percentage points higher than the conventional regeneration cycle and simple cycle configurations that utilized CO2 recycling. Accounting for cooling of the first two turbine stages resulted in a 2--3 percentage point reduction in un-cooled efficiency, with air dilution corresponding to the upper extreme. Additionally, when the work required to sequester CO2 was accounted for, cooled cycle efficiency decreased by 4--6 percentage points, and was more negatively impacted when syngas fuels were used. Finally, turbine design models showed that turbine blades are shorter with CO2 dilution, resulting in fewer design restrictions.

Extraction of indium from extremely diluted solutions; Gewinnung von Indium aus extrem verduennten Loesungen

Energy Technology Data Exchange (ETDEWEB)

Vostal, Radek; Singliar, Ute; Froehlich, Peter [TU Bergakademie Freiberg (Germany). Inst. fuer Technische Chemie

2017-02-15

The demand for indium is rising with the growth of the electronics industry, where it is mainly used. Therefore, a multistage extraction process was developed to separate indium from a model solution whose composition was adequate to sphalerite ore. The initially very low concentration of indium in the solution was significantly increased by several successive extraction and reextraction steps. The process described is characterized by a low requirement for chemicals and a high purity of the obtained indium oxide.

Screening antimicrobial activity of various extracts of Urtica dioica.

Science.gov (United States)

Modarresi-Chahardehi, Amir; Ibrahim, Darah; Fariza-Sulaiman, Shaida; Mousavi, Leila

2012-12-01

Urtica dioica or stinging nettle is traditionally used as an herbal medicine in Western Asia. The current study represents the investigation of antimicrobial activity of U. dioica from nine crude extracts that were prepared using different organic solvents, obtained from two extraction methods: the Soxhlet extractor (Method I), which included the use of four solvents with ethyl acetate and hexane, or the sequential partitions (Method II) with a five solvent system (butanol). The antibacterial and antifungal activities of crude extracts were tested against 28 bacteria, three yeast strains and seven fungal isolates by the disc diffusion and broth dilution methods. Amoxicillin was used as positive control for bacteria strains, vancomycin for Streptococcus sp., miconazole nitrate (30 microg/mL) as positive control for fungi and yeast, and pure methanol (v/v) as negative control. The disc diffusion assay was used to determine the sensitivity of the samples, whilst the broth dilution method was used for the determination of the minimal inhibition concentration (MIC). The ethyl acetate and hexane extract from extraction method I (EA I and HE I) exhibited highest inhibition against some pathogenic bacteria such as Bacillus cereus, MRSA and Vibrio parahaemolyticus. A selection of extracts that showed some activity was further tested for the MIC and minimal bactericidal concentrations (MBC). MIC values of Bacillus subtilis and Methicillin-resistant Staphylococcus aureus (MRSA) using butanol extract of extraction method II (BE II) were 8.33 and 16.33mg/mL, respectively; while the MIC value using ethyl acetate extract of extraction method II (EAE II) for Vibrio parahaemolyticus was 0.13mg/mL. Our study showed that 47.06% of extracts inhibited Gram-negative (8 out of 17), and 63.63% of extracts also inhibited Gram-positive bacteria (7 out of 11); besides, statistically the frequency of antimicrobial activity was 13.45% (35 out of 342) which in this among 21.71% belongs to

Screening antimicrobial activity of various extracts of Urtica dioica

Directory of Open Access Journals (Sweden)

Amir Modarresi-Chahardehi

2012-12-01

Full Text Available Urtica dioica or stinging nettle is traditionally used as an herbal medicine in Western Asia. The current study represents the investigation of antimicrobial activity of U. dioica from nine crude extracts that were prepared using different organic solvents, obtained from two extraction methods: the Soxhlet extractor (Method I, which included the use of four solvents with ethyl acetate and hexane, or the sequential partitions (Method II with a five solvent system (butanol. The antibacterial and antifungal activities of crude extracts were tested against 28 bacteria, three yeast strains and seven fungal isolates by the disc diffusion and broth dilution methods. Amoxicillin was used as positive control for bacteria strains, vancomycin for Streptococcus sp., miconazole nitrate (30µg/mL as positive control for fungi and yeast, and pure methanol (v/v as negative control. The disc diffusion assay was used to determine the sensitivity of the samples, whilst the broth dilution method was used for the determination of the minimal inhibition concentration (MIC. The ethyl acetate and hexane extract from extraction method I (EA I and HE I exhibited highest inhibition against some pathogenic bacteria such as Bacillus cereus, MRSA and Vibrio parahaemolyticus. A selection of extracts that showed some activity was further tested for the MIC and minimal bactericidal concentrations (MBC. MIC values of Bacillus subtilis and Methicillin-resistant Staphylococcus aureus (MRSA using butanol extract of extraction method II (BE II were 8.33 and 16.33mg/mL, respectively; while the MIC value using ethyl acetate extract of extraction method II (EAE II for Vibrio parahaemolyticus was 0.13mg/mL. Our study showed that 47.06% of extracts inhibited Gram-negative (8 out of 17, and 63.63% of extracts also inhibited Gram-positive bacteria (7 out of 11; besides, statistically the frequency of antimicrobial activity was 13.45% (35 out of 342 which in this among 21.71% belongs to

An isotope-dilution standard GC/MS/MS method for steroid hormones in water

Science.gov (United States)

Foreman, William T.; Gray, James L.; ReVello, Rhiannon C.; Lindley, Chris E.; Losche, Scott A.

2013-01-01

An isotope-dilution quantification method was developed for 20 natural and synthetic steroid hormones and additional compounds in filtered and unfiltered water. Deuterium- or carbon-13-labeled isotope-dilution standards (IDSs) are added to the water sample, which is passed through an octadecylsilyl solid-phase extraction (SPE) disk. Following extract cleanup using Florisil SPE, method compounds are converted to trimethylsilyl derivatives and analyzed by gas chromatography with tandem mass spectrometry. Validation matrices included reagent water, wastewater-affected surface water, and primary (no biological treatment) and secondary wastewater effluent. Overall method recovery for all analytes in these matrices averaged 100%; with overall relative standard deviation of 28%. Mean recoveries of the 20 individual analytes for spiked reagent-water samples prepared along with field samples analyzed in 2009–2010 ranged from 84–104%, with relative standard deviations of 6–36%. Detection levels estimated using ASTM International’s D6091–07 procedure range from 0.4 to 4 ng/L for 17 analytes. Higher censoring levels of 100 ng/L for bisphenol A and 200 ng/L for cholesterol and 3-beta-coprostanol are used to prevent bias and false positives associated with the presence of these analytes in blanks. Absolute method recoveries of the IDSs provide sample-specific performance information and guide data reporting. Careful selection of labeled compounds for use as IDSs is important because both inexact IDS-analyte matches and deuterium label loss affect an IDS’s ability to emulate analyte performance. Six IDS compounds initially tested and applied in this method exhibited deuterium loss and are not used in the final method.

Optimization of the sample dilution for minimization of the matrix effects and achieving maximal sensitivity in XRFA

International Nuclear Information System (INIS)

Dimov, L.; Benova, M.

1989-01-01

The method of neutral medium dilution can lead to practically full leveling of the matrix but the high degree of dilution at which this effect is achieved will inevitably result in loss of sensitivity. In the XRFA of heavy elements in a light matrix the dependence of the fluorescence intensity upon concentration is characterized by gradually decreasing steepness reacting saturation (as in analysis of Pb in a Pb-concentrate). The dilution by neutral medium can shift the concentration range to a zone of greater steepness but this results in an increase of sensitivity towards the concentration in the initial (undiluted) material only to a certain degree of dilution. This work presents an optimization of the degree of dilution by neutral medium which achieves a sufficient leveling of the matrix when using different materials and also maximal sensitivity towards higher concentrations. Furthermore an original solution is found to the problem of selecting a neutral medium enabling to achieve good homogenization with various materials and particularly - with marble flour. (author)

Dilution refrigeration with multiple mixing chambers

International Nuclear Information System (INIS)

Coops, G.M.

1981-01-01

A dilution refrigerator is an instrument to reach temperatures in the mK region in a continuous way. The temperature range can be extended and the cooling power can be enlarged by adding an extra mixing chamber. In this way we obtain a double mixing chamber system. In this thesis the theory of the multiple mixing chamber is presented and tested on its validity by comparison with the measurements. Measurements on a dilution refrigerator with a circulation rate up to 2.5 mmol/s are also reported. (Auth.)

Bioconversion of dilute-acid pretreated sorghum bagasse to ethanol by Neurospora crassa

Energy Technology Data Exchange (ETDEWEB)

Dogaris, Ioannis; Gkounta, Olga; Mamma, Diomi; Kekos, Dimitris [National Technical Univ. of Athens, Zografou (Greece). Biotechnology Lab.

2012-07-15

Bioethanol production from sweet sorghum bagasse (SB), the lignocellulosic solid residue obtained after extraction of sugars from sorghum stalks, can further improve the energy yield of the crop. The aim of the present work was to evaluate a cost-efficient bioconversion of SB to ethanol at high solids loadings (16 % at pretreatment and 8 % at fermentation), low cellulase activities (1-7 FPU/g SB) and co-fermentation of hexoses and pentoses. The fungus Neurospora crassa DSM 1129 was used, which exhibits both depolymerase and co-fermentative ability, as well as mixed cultures with Saccharomyces cerevisiae 2541. A dilute-acid pretreatment (sulfuric acid 2 g/100 g SB; 210 C; 10 min) was implemented, with high hemicellulose decomposition and low inhibitor formation. The bioconversion efficiency of N. crassa was superior to S. cerevisiae, while their mixed cultures had negative effect on ethanol production. Supplementing the in situ produced N. crassa cellulolytic system (1.0 FPU/g SB) with commercial cellulase and {beta}-glucosidase mixture at low activity (6.0 FPU/g SB) increased ethanol production to 27.6 g/l or 84.7 % of theoretical yield (based on SB cellulose and hemicellulose sugar content). The combined dilute-acid pretreatment and bioconversion led to maximum cellulose and hemicellulose hydrolysis 73.3 % and 89.6 %, respectively. (orig.)

Sugar yields from dilute oxalic acid pretreatment of maple wood compared to those with other dilute acids and hot water.

Science.gov (United States)

Zhang, Taiying; Kumar, Rajeev; Wyman, Charles E

2013-01-30

Dilute oxalic acid pretreatment was applied to maple wood to improve compatibility with downstream operations, and its performance in pretreatment and subsequent enzymatic hydrolysis was compared to results for hydrothermal and dilute hydrochloric and sulfuric acid pretreatments. The highest total xylose yield of ∼84% of the theoretical maximum was for both 0.5% oxalic and sulfuric acid pretreatment at 160 °C, compared to ∼81% yield for hydrothermal pretreatment at 200 °C and for 0.5% hydrochloric acid pretreatment at 140 °C. The xylooligomer fraction from dilute oxalic acid pretreatment was only 6.3% of the total xylose in solution, similar to results with dilute hydrochloric and sulfuric acids but much lower than the ∼70% value for hydrothermal pretreatment. Combining any of the four pretreatments with enzymatic hydrolysis with 60 FPU cellulase/g of glucan plus xylan in the pretreated maple wood resulted in virtually the same total glucose plus xylose yields of ∼85% of the maximum possible. Copyright © 2012 Elsevier Ltd. All rights reserved.

Analysis of halogenated and priority pesticides at different concentration levels. Automated SPE extraction followed by isotope dilution-GC/MS

Energy Technology Data Exchange (ETDEWEB)

Planas, C.; Saulo, J.; Rivera, J.; Caixach, J. [Institut Investigacions Quimiques i Ambientals (IIQAB-CSIC), Barcelona (Spain)

2004-09-15

In this work, automatic SPE extraction of 16 pesticides and metabolites with the automated Power-Prep trademark system is evaluated at different concentration levels using polymeric (ENV+) and C{sub 18} sorbent phases. The method was optimised by comparing recoveries obtained using different eluting solvents. The optimised procedure was then applied to spiked water samples at concentration levels of 0.1{mu}g/L (quality standard for individual pesticides in drinking water) and 0.02{mu}g/L (close to the detection limit of most pesticides).

Comparison of DNA extraction protocols to detect Mycobacterium bovis in bovine tissue by PCR

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Cássia Yumi Ikuta

2016-11-01

Full Text Available The current scenario of international beef trading has increased the pressure for better and faster diagnosis of bovine tuberculosis. Although traditional culture remains the gold standard method to confirm Mycobacterium bovis infection, it is exceedingly time consuming, and demands viable mycobacteria. Molecular methods overcome the flaws of the bacteriological methods with faster detection and identification. However, mycobacterial features like a complex cell wall and pathogen–host interaction make the molecular detection a challenge. Three protocols for DNA extraction (A, B and C from bovine tissues were tested to verify the most suitable technique for routine diagnostic assessment of their specificity and sensitivity. Thirty culture-positive and thirty culture-negative granulomatous lesions were included in the trial. From each sample, three tissue suspensions at different dilutions (10-1, 10-2 and 10-3 were prepared and submitted to DNA extraction. PCR procedures targeting IS6110 were performed, employing two volumes of DNA: 5 µL of all three dilutions, and 2.5 µL of the 10-1 dilution. Protocol A was able to detect members of the M. tuberculosis complex in most samples. The sensitivity of the test decreased with increase in tissue-suspension dilution. Although Protocol A presented the highest sensitivity followed by C and B, it showed the lowest specificity, which can be due to a failure in primary isolation caused by the lack of viable organisms or incubation time. Regardless classical bacteriological methods are still recommended by OIE, after evaluating the sensitivity of DNA extraction protocols and PCR procedures, we conclude that the best strategy for M. bovis detection is to follow Protocol A on concentrated tissue suspensions.

Simultaneous determination of platinum group elements and rhenium in rock samples using isotope dilution inductively coupled plasma mass spectrometry after cation exchange separation followed by solvent extraction

International Nuclear Information System (INIS)

Shinotsuka, Kazunori; Suzuki, Katsuhiko

2007-01-01

A simple and precise determination method for platinum group elements (PGEs) and Re in rock samples was developed using isotope dilution coupled with inductively coupled plasma mass spectrometry (ID-ICP-MS). Cation exchange separation was employed for simplicity, because it is applicable to group separation and simultaneous isotopic measurement in contrast with the widely used anion exchange separation which entails separate elution. However, its application to ID-ICP-MS has been limited due to spectral interferences from impurities retained in the PGE fraction even after ion chromatography. To overcome this limitation, solvent extraction using N-benzoyl-N-phenylhydroxylamine (BPHA) in chloroform was successfully applied for further purification. After the examination of optimum experimental parameters in cation exchange separation and solvent extraction using synthetic PGE solution, the established procedure was applied to the determination of PGEs and Re in some geochemical reference materials. The obtained results agreed well with the literature data determined using the different digestion methods (NiS fire assay and the use of a high-pressure asher) within the analytical uncertainties of each other. Significant difference in reproducibility between Ru, Ir, Pt and Os group, and Pd and Re group was observed in the results for BHVO-2 and JA-2. By considering the error factors affecting analytical reproducibility, we concluded that the difference is ascribed to the sample heterogeneity of minor minerals enriched in Ru, Ir, Pt and Os

Antimicrobial potential of ethanol extracts of plants against gramnegative bacilli isolated from cervicovaginal mucosa of sheep bred in the region of Petrolina-PE

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Valdenice Félix da Silva

2014-02-01

Full Text Available Reproductive tract infections are the main causes of losses from the low reproductive efficiency of sheep. Gram negative bacilli belonging to the normal flora of the genital region can trigger diseases. The pathogenicity of these agents is expressed when females are with weakened immune system, either by food or stress management. Flaws in and concern about antibiotic residues in animal production have prompted research regarding alternatives for the treatment of diseases. The herbal medicine hás been considered in this context is the subject of numerous studies. This study aimed to evaluate the antibacterial potential of ethanol extracts of plants belonging to the flora of the Northeast against gram negative bacilli isolated from cervical-vaginal mucosa of sheep. Six plants were selected from Caatinga biome: Encholirium spectabile, Bromelia laciniosa, Neoglaziovia variegata, Amburana cearensis Hymenaea martiana and Selaginella convoluta. The plant material was processed to obtain the crude extract. This was tested by microdilution plate and determining the minimum bactericidal concentration, the second document of Clinical and Laboratory Standards Institute (CLSI and the extracts diluted in water and alcohol. We used 43 gram negative isolates, as follows: 14 E. coli, 10 Enterobacter spp., 10 Acinetobacter spp. 9 and Klebsiella spp. In the aqueous dilution Klebsiella spp. showed response only to species B. laciniosa, S. convoluta and H. martiana. All tested extracts showed antibacterial activity against Acinetobacter spp and no activity against E. coli and Enterobacter spp. Among the extracts diluted in water H. martiana showed the highest antibacterial activity. In all dilution alcoholic extracts showed inhibitory activity against all bacterial genera, but no statistical difference between them.

Rationale for using Peltophorum africanum (Fabaceae extracts in veterinary medicine

Directory of Open Access Journals (Sweden)

S.E. Bizimenyera

2005-06-01

Full Text Available Peltophorum africanum (Fabaceae is a deciduous tree widespread in southern Africa. The plant has many ethnomedical and ethnoveterinary uses. Root and bark decoctions are used to treat diarrhoea, dysentery, sore throat, wounds, back and joint pains, HIV-AIDS, venereal diseases and infertility. Pastoralists and rural farmers use the root and bark extracts to treat diarrhoea, dysentery, infertility, and to promote well-being and resistance to diseases in cattle. To evaluate these ethnobotanical leads, dried leaves, stem bark and root bark were extracted with ethanol, acetone, dichloromethane and hexane. Polyphenols in the extract were determined by the Folin-Ciocalteu method with gallic acid as standard. Qualitative antioxidant activity was screened by spraying thin layer chromatograms (TLC of the extracts with 0.2 % 1, 1-diphenyl-2-picryl hydrazyl (DPPH, and quantified with Trolox equivalent antioxidant capacity (TEAC assay. Minimum inhibitory concentration (MIC and total antibacterial activity (TAA were determined by serial microplate dilution for Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa and Enterococcus faecalis, with gentamicin as standard and tetrazolium violet as growth indicator. Acetone and ethanol extracted the largest quantity of material. Polyphenols concentration was 49.2% in acetone extract of the root and 3.8 % in dichloromethane extract of the leaf. Antioxidant activity of at least 5 antioxidant compounds as measured by TEAC ranged from 1.34 (ethanol extract of the root to 0.01 (hexane extract of the leaf. The total antibacterial activity (volume to which active compounds present in 1 g plant material can be diluted and still inhibit bacterial growth was 1263 mℓ/g for ethanol extract of the root against S. aureus, and 800 mℓ/g for acetone extract of the root against P. aeruginosa. There was substantial activity against both Gram-positive and Gram-negative bacteria, with MIC values of 0.08 mg/mℓ for S

Effect of the Copaifera langsdorffii Desf. Leaf Extract on the Ethylene Glycol-Induced Nephrolithiasis in Rats

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Rejane Barbosa de Oliveira

2013-01-01

Full Text Available The potential of the Copaifera langsdorffii leaves extract to prevent stone formation was analyzed by means of an ethylene glycol (EG animal model of nephrolithiasis and an in vitro crystallization assay. Different doses of the C. langsdorffii leaves extract were administered to rats treated with EG. Urine biochemical parameters were quantified. CaOx deposits count and analysis of osteopontin expression were conducted on kidneys fixed in formalin. The in vitro assay was performed by turbidimetry. Phytochemical analyses of the extract were accomplished by HPLC-UV-DAD, and several compounds were isolated. C. langsdorffii leaf extract was able to avoid stone formation. The number of deposits was 50.30±31.29 at the higher extract dose, compared to the value of 179.5±45.96 achieved with the EG control. Significantly lower oxalate levels and OPN expression and increased citrate levels were observed after extract administration. In the in vitro assay, the extract diluted the formed crystals. Phytochemical analyses showed that the extract is rich in phenolic compounds that are capable of preventing stone formation. Thus, on the basis of our results, we suggest that the C. langsdorffii leaf extract has potential application in the prevention of kidney stone formation.

Dilution Ratios for HB Line Phase I Eductor System

International Nuclear Information System (INIS)

Steimke, J.L.

2002-01-01

HB Line Phase I product transfer includes an eductor which transfers liquid from Product Hold Tank (PHT) RT-33 or RT-34 to Tank 11.1. The eductor also dilutes the liquid from the PHT with eductant. Dilution must be reliably controlled because of criticality concerns with H Canyon Tanks. The eductor system, which contains a 1 inch Model 264 Schutte and Koerting eductor, was previously modeled [1] in 1998 and dilution ratios were calculated for different flow restrictors, eductant pressures and densities for the eductant and the contents of the PHT. The previous calculation was performed using spreadsheet software no longer supported at SRS. For the previous work dilution ratio was defined as the volume of eductant consumed divided by volume of PHT contents transferred. Since 1998 HB Line Engineering has changed the definition of dilution ratio to the total volume of liquid, eductant consumed plus the volume of PHT liquid transferred, divided by the volume of PHT liquid transferred. The 1998 base case calculation was for a restrictor diameter of 0.334 inches, an eductant supply pressure of 15 psig, full PHT, an eductant specific gravity of 1.385 and a PHT density of 1.015. The base case dilution ratio calculated in 1998 using the current definition was 3.52. After accounting for uncertainty the minimum dilution ratio decreased to 3.23. In 2001 HB Line Engineering requested that the calculation be repeated for a manganous nitrate solution eductant and also a process water eductant. The other conditions were the same as for the 1998 calculation. The objective of this report is to document the calculations and the results

In vitro antimicrobial activity of Pistacia lentiscus L. edible oil and phenolic extract.

Science.gov (United States)

Mezni, F; Aouadhi, C; Khouja, M L; Khaldi, A; Maaroufi, A

2015-01-01

Pistacia lentiscus L. is known in some Tunisian forest area by its fixed oil used in traditional medicine as an antiseptic product. This investigation is the first to study the antimicrobial activity of P.lentiscus edible oil and its phenolic extract. Oil was extracted from fruits harvested from six provenances located in Tunisia. The antimicrobial activity was tested using disc diffusion assay and the broth dilution method. Kbouch and Sidi Zid oils were most efficient (p oil and extract.

Comparison of dye dilution method to radionuclide techniques for cardiac output determination in dogs

International Nuclear Information System (INIS)

Eng, S.S.; Robayo, J.R.; Porter, W.; Smith, R.E.

1980-01-01

A study was undertaken to identify the most accurate /sup 99m/Tc-labeled radiopharmaceutical and to determine the accuracy of a noninvasive radionuclide technique or cardiac output determinations. Phase I employed sodium pertechnetate, stannous pyrophosphate with sodium pertechnetate, /sup 99m/Tc red blood cells, and /sup 99m/Tc human serum albumin as radionuclide tracers. Cardiac output was determined by the dye dilution method and then by the invasive radionuclide technique. A pairied t test and regression analysis indicated that /sup 99m/Tc human serum albumin was the most accurate radiopharmaceutical for cardiac output determinations, and the results compared favorably to those obtained by the dye dilution method. In Phase II, /sup 99m/Tc human serum albumin was used as the radionuclide tracer for cardiac output determinations with the noninvasive technique. The results compared favorably to those obtained by the dye dilution method

Solid-phase extraction procedures in systematic toxicological analysis

NARCIS (Netherlands)

Franke, J.P.; de Zeeuw, R.A

1998-01-01

In systematic toxicological analysis (STA) the substance(s) present is (are) not known at the start of the analysis. in such an undirected search the extraction procedure cannot be directed to a given substance but must be a general procedure where a compromise must be reached in that the substances

Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction

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Ghahramanloo KH

2017-07-01

Full Text Available Kourosh Hasanzadeh Ghahramanloo,1 Behnam Kamalidehghan,2 Hamid Akbari Javar,3 Riyanto Teguh Widodo,1 Keivan Majidzadeh,4 Mohamed Ibrahim Noordin1 1Department of Pharmacy, Faculty of Medicine, University of Malaya, Kuala Lumpur, Malaysia; 2Medical Genetics Department, National Institute of Genetic Engineering and Biotechnology (NIGEB, 3Department of Pharmaceutics, Faculty of Pharmacy, Tehran University of Medical Sciences (TUMS, 4Breast Cancer Research Center (BCRC Academic Center for Education, Culture and Research, Tehran, Iran Abstract: The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%–61.85% and oleic acid (1.64%–18.97%. Thymoquinone (0.72%–21.03% was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly (P<0.05 higher than that achieved by the solvent extraction technique. The present study showed that SFE can be used as a more efficient technique for extraction of N. Sativa L. essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique. Keywords: Nigella sativa L., essential oil extraction, supercritical fluid extraction, solvent extraction, fatty acid composition, thymoquinone, linoleic acid

Behaviour of humic-bentonite aggregates in diluted suspensions ...

African Journals Online (AJOL)

Formation and disaggregation of micron-size aggregates in a diluted suspension made up of HSs and bentonite (B) were studied by tracing distribution of aggregate sizes and their counts in freshly prepared and aged suspensions, and at high (10 000) and low (1.0) [HS]/[B] ratios. Diluted HSB suspensions are unstable ...

Development of polymer-extractant composite beads for separation of radionuclides

International Nuclear Information System (INIS)

Kumar, Manmohan; Singh, Krishankant; Bajaj, P.N.

2009-01-01

A novel micro porous polymer-extractant composite bead system, containing liquid extractant encapsulated in the core of a polymeric shell, with required porosity and hydrophilicity, to allow exchange of radionuclides without, any significant leaching out of the encapsulated extractant, has been developed for solid-liquid extraction of radionuclides from acidic waste solutions. The reuse of the beads is possible as there is practically no change in its radionuclide extraction efficiency, after repeated extraction second time. The high porosity and hydrophilicity of the synthesized TBP-encapsulated polymeric beads is evident from the presence of ∼ 78% water in the swollen condition. Evaluation of the synthesized beads for extraction of uranium and plutonium from aqueous acidic waste solutions, indicated possibility of their use under the conditions of PUREX process. The aliquate 336-encapsulated polymeric beads showed selective extraction of plutonium from aqueous nitrate solutions in the presence of uranium, and back extraction of the loaded plutonium, using dilute nitric acid or ascorbic acid. (author)

Insights into the Key Aroma Compounds in Mango (Mangifera indica L. 'Haden') Fruits by Stable Isotope Dilution Quantitation and Aroma Simulation Experiments.

Science.gov (United States)

Munafo, John P; Didzbalis, John; Schnell, Raymond J; Steinhaus, Martin

2016-06-01

Thirty-four aroma-active compounds, previously identified with high flavor dilution factors by application of an aroma extract dilution analysis, were quantified in tree-ripened fruits of mango (Mangifera indica L. 'Haden'). From the results, the odor activity value (OAV) was calculated for each compound as the ratio of its concentration in the mangoes to its odor threshold in water. OAVs > 1 were obtained for 24 compounds, among which ethyl 2-methylbutanoate (fruity; OAV 2100), (3E,5Z)-undeca-1,3,5-triene (pineapple-like; OAV 1900), ethyl 3-methylbutanoate (fruity; OAV 1600), and ethyl butanoate (fruity; OAV 980) were the most potent, followed by (2E,6Z)-nona-2,6-dienal (cucumber-like), ethyl 2-methylpropanoate (fruity), (E)-β-damascenone (cooked apple-like), ethyl hexanoate (fruity), 4-hydroxy-2,5-dimethyl-3(2H)-furanone (caramel-like), 3-methylbut-2-ene-1-thiol (sulfurous), γ-decalactone (peach-like), β-myrcene (terpeny), (3Z)-hex-3-enal (green), 4-methyl-4-sulfanylpentan-2-one (tropical fruit-like), and ethyl octanoate (fruity). Aroma simulation and omission experiments revealed that these 15 compounds, when combined in a model mixture in their natural concentrations, were able to mimic the aroma of the fruits.

Diluted magnetic semiconductor nanowires exhibiting magnetoresistance

Science.gov (United States)

Yang, Peidong [El Cerrito, CA; Choi, Heonjin [Seoul, KR; Lee, Sangkwon [Daejeon, KR; He, Rongrui [Albany, CA; Zhang, Yanfeng [El Cerrito, CA; Kuykendal, Tevye [Berkeley, CA; Pauzauskie, Peter [Berkeley, CA

2011-08-23

A method for is disclosed for fabricating diluted magnetic semiconductor (DMS) nanowires by providing a catalyst-coated substrate and subjecting at least a portion of the substrate to a semiconductor, and dopant via chloride-based vapor transport to synthesize the nanowires. Using this novel chloride-based chemical vapor transport process, single crystalline diluted magnetic semiconductor nanowires Ga.sub.1-xMn.sub.xN (x=0.07) were synthesized. The nanowires, which have diameters of .about.10 nm to 100 nm and lengths of up to tens of micrometers, show ferromagnetism with Curie temperature above room temperature, and magnetoresistance up to 250 Kelvin.

Gas Leak Detection by Dilution of Atmospheric Oxygen

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Armin Lambrecht

2017-12-01

Full Text Available Gas leak detection is an important issue in infrastructure monitoring and industrial production. In this context, infrared (IR absorption spectroscopy is a major measurement method. It can be applied in an extractive or remote detection scheme. Tunable laser spectroscopy (TLS instruments are able to detect CH4 leaks with column densities below 10 ppm·m from a distance of 30 m in less than a second. However, leak detection of non-IR absorbing gases such as N2 is not possible in this manner. Due to the fact that any leaking gas displaces or dilutes the surrounding background gas, an indirect detection is still possible. It is shown by sensitive TLS measurements of the ambient background concentration of O2 that N2 leaks can be localized with extractive and standoff methods for distances below 1 m. Minimum leak rates of 0.1 mbar·L/s were determined. Flow simulations confirm that the leakage gas typically effuses in a narrow jet. The sensitivity is mainly determined by ambient flow conditions. Compared to TLS detection of CH4 at 1651 nm, the indirect method using O2 at 761 nm is experimentally found to be less sensitive by a factor of 100. However, the well-established TLS of O2 may become a universal tool for rapid leakage screening of vessels that contain unknown or inexpensive gases, such as N2.

Quantitation of 5-Methyltetrahydrofolic Acid in Dried Blood Spots and Dried Plasma Spots by Stable Isotope Dilution Assays.

Directory of Open Access Journals (Sweden)

Markus Kopp

Full Text Available Because of minimal data available on folate analysis in dried matrix spots (DMSs, we combined the advantages of stable isotope dilution assays followed by LC-MS/MS analysis with DMS sampling to develop a reliable method for the quantitation of plasma 5-methyltetrahydrofolic acid in dried blood spots (DBSs and dried plasma spots (DPSs as well as for the quantitation of whole blood 5-methyltetrahydrofolic acid in DBSs. We focused on two diagnostically conclusive parameters exhibited by the plasma and whole blood 5-methyltetrahydrofolic acid levels that reflect both temporary and long-term folate status. The method is performed using the [2H4]-labeled isotopologue of the vitamin as the internal standard, and three steps are required for the extraction procedure. Elution of the punched out matrix spots was performed using stabilization buffer including Triton X-100 in a standardized ultrasonication treatment followed by enzymatic digestion (whole blood only and solid-phase extraction with SAX cartridges. This method is sensitive enough to quantify 27 nmol/L whole blood 5-methyltetrahydrofolic acid in DBSs and 6.3 and 4.4 nmol/L plasma 5-methyltetrahydrofolic acid in DBSs and DPSs, respectively. The unprecedented accurate quantification of plasma 5-methyltetrahydrofolic acid in DBSs was achieved by thermal treatment prior to ultrasonication, inhibiting plasma conjugase activity. Mass screenings are more feasible and easier to facilitate for this method in terms of sample collection and storage compared with conventional clinical sampling for the assessment of folate status.

Mobile Melt-Dilute Treatment for Russian Spent Nuclear Fuel

International Nuclear Information System (INIS)

Peacock, H.

2002-01-01

Treatment of spent Russian fuel using a Melt-Dilute (MD) process is proposed to consolidate fuel assemblies into a form that is proliferation resistant and provides critically safety under storage and disposal configurations. Russian fuel elements contain a variety of fuel meat and cladding materials. The Melt-Dilute treatment process was initially developed for aluminum-based fuels so additional development is needed for several cladding and fuel meat combinations in the Russian fuel inventory (e.g. zirconium-clad, uranium-zirconium alloy fuel). A Mobile Melt-Dilute facility (MMD) is being proposed for treatment of spent fuels at reactor site storage locations in Russia; thereby, avoiding the costs of building separate treatment facilities at each site and avoiding shipment of enriched fuel assemblies over the road. The MMD facility concept is based on laboratory tests conducted at the Savannah River Technology Center (SRTC), and modular pilot-scale facilities constructed at the Savannah River Site for treatment of US spent fuel. SRTC laboratory tests have shown the feasibility of operating a Melt-Dilute treatment process with either a closed system or a filtered off-gas system. The proposed Mobile Melt-Dilute process is presented in this paper

A sediment extraction and cleanup method for wide-scope multitarget screening by liquid chromatography-high-resolution mass spectrometry.

Science.gov (United States)

Massei, Riccardo; Byers, Harry; Beckers, Liza-Marie; Prothmann, Jens; Brack, Werner; Schulze, Tobias; Krauss, Martin

2018-01-01

Previous studies on organic sediment contaminants focused mainly on a limited number of highly hydrophobic micropollutants accessible to gas chromatography using nonpolar, aprotic extraction solvents. The development of liquid chromatography-high-resolution mass spectrometry (LC-HRMS) permits the spectrum of analysis to be expanded to a wider range of more polar and ionic compounds present in sediments and allows target, suspect, and nontarget screening to be conducted with high sensitivity and selectivity. In this study, we propose a comprehensive multitarget extraction and sample preparation method for characterization of sediment pollution covering a broad range of physicochemical properties that is suitable for LC-HRMS screening analysis. We optimized pressurized liquid extraction, cleanup, and sample dilution for a target list of 310 compounds. Finally, the method was tested on sediment samples from a small river and its tributaries. The results show that the combination of 100 °C for ethyl acetate-acetone (50:50, neutral extract) followed by 80 °C for acetone-formic acid (100:1, acidic extract) and methanol-10 mM sodium tetraborate in water (90:10, basic extract) offered the best extraction recoveries for 287 of 310 compounds. At a spiking level of 1 μg mL -1 , we obtained satisfactory cleanup recoveries for the neutral extract-(93 ± 23)%-and for the combined acidic/basic extracts-(42 ± 16)%-after solvent exchange. Among the 69 compounds detected in environmental samples, we successfully quantified several pharmaceuticals and polar pesticides.

Plutonium determination by isotope dilution

International Nuclear Information System (INIS)

Lucas, M.

1980-01-01

The principle is to add to a known amount of the analysed solution a known amount of a spike solution consisting of plutonium 242. The isotopic composition of the resulting mixture is then determined by surface ionization mass spectrometry, and the plutonium concentration in the solution is deduced, from this measurement. For irradiated fuels neutronic studies or for fissile materials balance measurements, requiring the knowledge of the ratio U/Pu or of concentration both uranium and plutonium, it is better to use the double spike isotope dilution method, with a spike solution of known 233 U- 242 Pu ratio. Using this method, the ratio of uranium to plutonium concentration in the irradiated fuel solution can be determined without any accurate measurement of the mixed amounts of sample and spike solutions. For fissile material balance measurements, the uranium concentration is determined by using single isotope dilution, and the plutonium concentration is deduced from the ratio Pu/U and U concentration. The main advantages of isotope dilution are its selectivity, accuracy and very high sensitivity. The recent improvements made to surface ionization mass spectrometers have considerably increased the precision of the measurements; a relative precision of about 0.2% to 0.3% is obtained currently, but it could be reduced to 0.1%, in the future, with a careful control of the experimental procedures. The detection limite is around 0.1 ppb [fr

Magnetic ordering in dilute YTb and YEr alloys

International Nuclear Information System (INIS)

Rainford, B.D.; Kilcoyne, S.H.; Mohammed, K.A.; Lanchester, P.C.; Stanley, H.B.; Caudron, R.

1988-01-01

Dilute YEr alloys (Er concentration between 3% and 10%) show the existence of sinusoidally modulated antiferromagnetism down to the lowest impurity concentrations studied. Extrapolation of the Neel temperatures for both YEr and YTb suggests a critical concentration is ≅ 0.8% Tb, Er. Ordering in such dilute alloys may result from exchange enhancement in the yttrium host

Magnetic ordering in dilute YTb and YEr alloys

Energy Technology Data Exchange (ETDEWEB)

Rainford, B.D.; Kilcoyne, S.H.; Mohammed, K.A.; Lanchester, P.C.; Stanley, H.B.; Caudron, R.

1988-12-01

Dilute YEr alloys (Er concentration between 3% and 10%) show the existence of sinusoidally modulated antiferromagnetism down to the lowest impurity concentrations studied. Extrapolation of the Neel temperatures for both YEr and YTb suggests a critical concentration is /approx equal/ 0.8% Tb, Er. Ordering in such dilute alloys may result from exchange enhancement in the yttrium host.

Extraction, characterisation, and enzymatic degradation of lemon peel pectins.

NARCIS (Netherlands)

Ros, J.M.; Schols, H.A.; Voragen, A.G.J.

1996-01-01

The albedo of Spanish lemons (16.0% w/w of lemon fresh weight) was extracted to obtain a chelating agent soluble pectin fraction, a diluted sodium hydroxide soluble pectin fraction and a residue (4.2, 1.8, and 5.0% w/w of fresh albedo, respectively). These fractions represented 61.3, 12.4, and 10.4%

Monte Carlo study of the pure and dilute Baxter-Wu model

International Nuclear Information System (INIS)

Schreiber, Nir; Adler, Joan

2005-01-01

We studied the pure and dilute Baxter-Wu (BW) models using the Wang-Landau (WL) sampling method to calculate the density-of-states (DOS). We first used the exact result for the DOS of the Ising model to test our code. Then we calculated the DOS of the dilute Ising model to obtain a phase diagram, in good agreement with previous studies. We calculated the energy distribution, together with its first, second and fourth moments, to give the specific heat and the energy fourth order cumulant, better known as the Binder parameter, for the pure BW model. For small samples, the energy distribution displayed a doubly peaked shape, and finite size scaling analysis showed the expected reciprocal scaling of the positions of the peaks with L. The energy distribution yielded the expected BW α = 2/3 critical exponent for the specific heat. The Binder parameter minimum appeared to scale with lattice size L with an exponent θ B equal to the specific heat exponent. Its location (temperature) showed a large correction-to-scaling term θ 1 = 0.248 ± 0.025. For the dilute BW model we found a clear crossover to a single peak in the energy distribution even for small sizes and the expected α = 0 was recovered

Electromembrane extraction of peptides - fundamental studies on the supported liquid membrane

DEFF Research Database (Denmark)

Seip, Knut Fredrik; Stigsson, Jeanette; Gjelstad, Astrid

2011-01-01

L) was after extraction analyzed directly, or with some dilution, on CE or HPLC. This article has identified mono- or di-substituted phosphate groups as the prominent group of carrier molecules needed to obtain acceptable recoveries. For the organic solvents, primary alcohols and ketones have shown promise...... in the concentration 10 µg/mL was used. Extraction time was 5 min with an electric potential of 10 V and 900 rpm agitation of the sample vial. The samples were extracted through a hollow fiber-based SLM with different compositions of organic solvents and carriers. A small volume of acidified acceptor solution (25 µ...

Phytochemical analysis and standardization of Strychnos nux-vomica extract through HPTLC techniques

Directory of Open Access Journals (Sweden)

Dinesh Kumar Patel

2012-05-01

Full Text Available Objective: The objective is to develop a noval qualitative and quantitative method by which we can determine different phytoconstituents of Strychnos nux-vomica L. Methods: To profile the phyconstituents of Strychnos nux-vomica, in the present study hydroalcoholic extract of Strychnos nux-vomica was subjected to preliminary phytochemical analysis, antimicrobial activities against certain pathogenic microorganisms, solubility test, loss on drying and pH value. Extract was also subjected to the quantitative analysis including total phenol, flavonoid and heavy metal analysis. Quantitative analysis was performed through HPTLC methods using strychnine and brucine as a standard marker. Results: Phytochemical analysis revealed the presence of alkaloid, carbohydrate, tannin, steroid, triterpenoid and glycoside in the extract. Total flavonoid and phenol content of Strychnos nux-vomica L extract was found to be 0.40 % and 0.43%. Result showed that the level of heavy metal (lead, arsenic, mercury and cadmium complie the standard level. Total bacterial count, yeast and moulds contents were found to be under the limit whereas E. coli and salmonella was found to be absent in the extract. Content of strychnine and brucine were found to be 4.75% and 3.91%. Conclusions: These studies provide valluable information for correct identification and selection of the drug from various adulterations. In future this study will be helpful for the quantitative analysis as well as standardization of the Strychnos nux-vomica L.

A structured understanding of cellobiohydrolase I binding to poplar lignin fractions after dilute acid pretreatment.

Science.gov (United States)

Yao, Lan; Yoo, Chang Geun; Meng, Xianzhi; Li, Mi; Pu, Yunqiao; Ragauskas, Arthur J; Yang, Haitao

2018-01-01

Cellulase adsorption to lignin is considered a cost barrier for bioethanol production; however, its detailed association mechanism is still not fully understood. In this study, two natural poplar variants with high and low sugar release performance were selected as the low and high recalcitrant raw materials (named L and H , respectively). Three different lignin fractions were extracted using ethanol, followed by p -dioxane and then cellulase treatment from the dilute acid pretreated poplar solids (fraction 1, 2, and 3, respectively). Each lignin fraction had different physicochemical properties. Ethanol-extracted lignin had the lowest weight average molecular weight, while the molecular weights for the other two lignin fractions were similar. 31 P NMR analysis revealed that lignin fraction with higher molecular weight contained more aliphatic hydroxyl groups and less phenolic hydroxyl groups. Semi-quantitative analysis by 2D HSQC NMR indicated that the lignin fractions isolated from the natural variants had different contents of syringyl (S), guaiacyl (G) and interunit linkages. Lignin extracted by ethanol contained the largest amount of S units, the smallest amounts of G and p -hydroxybenzoate (PB) subunits, while the contents of these lignin subunits in the other two lignin fractions were similar. The lignin fraction obtained after cellulase treatment was primarily comprised of β- O -4 linkages with small amounts of β-5 and β-β linkages. The binding strength of these three lignin fractions obtained by Langmuir equations were in the order of L 1  >  L 3  >  L 2 for the low recalcitrance poplar and H 1  >  H 2  >  H 3 for the high recalcitrance poplar. Overall, adsorption ability of lignin was correlated with the sugar release of poplar. Structural features of lignin were associated with its binding to CBH. For natural poplar variants, lignin fractions with lower molecular weight and polydispersity index (PDI) exhibited more CBH adsorption

Separation of uranium(VI) by liquid-solid extraction with tri-n-octylphosphine oxide diluted with naphthalene

International Nuclear Information System (INIS)

Shigetomi, Y.; Kojima, T.; Kamba, H.; Yamamoto, Y.

1980-01-01

Liquid-liquid distribution with tri-n-octylphosphine oxide (TOPO) and molten naphthalene has been investigated for the extraction of 20 metals from nitric acid and hydrochloric acid solutions. Uranium is quantitatively extracted from 1 M nitric acid or hydrochloric acid by using 100 mg of TOPO and 200 mg of naphthalene and shaking for 5 min at 80 0 C, and separated from transition metals, alkaline earth metals and rare earth metals (except scandium). Addition of naphthalene increases the extraction efficiency. (Auth.)

Analysis of nitrosamines in water by automated SPE and isotope dilution GC/HRMS Occurrence in the different steps of a drinking water treatment plant, and in chlorinated samples from a reservoir and a sewage treatment plant effluent.

Science.gov (United States)

Planas, Carles; Palacios, Oscar; Ventura, Francesc; Rivera, Josep; Caixach, Josep

2008-08-15

A method based on automated solid-phase extraction (SPE) and isotope dilution gas chromatography/high resolution mass spectrometry (GC/HRMS) has been developed for the analysis of nine nitrosamines in water samples. The combination of automated SPE and GC/HRMS for the analysis of nitrosamines has not been reported previously. The method shows as advantages the selectivity and sensitivity of GC/HRMS analysis and the high efficiency of automated SPE with coconut charcoal EPA 521 cartridges. Low method detection limits (MDLs) were achieved, along with a greater facility of the procedure and less dependence on the operator with regard to the methods based on manual SPE. Quality requirements for isotope dilution-based methods were accomplished for most analysed nitrosamines, regarding to trueness (80-120%), method precision (water samples (16 samples from a drinking water treatment plant {DWTP}, 2 chlorinated samples from a sewage treatment plant {STP} effluent, and 1 chlorinated sample from a reservoir) were analysed. Concentrations of nitrosamines in the STP effluent were 309.4 and 730.2 ng/L, being higher when higher doses of chlorine were applied. N-Nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA) were the main compounds identified in the STP effluent, and NDEA was detected above 200 ng/L, regulatory level for NDMA in effluents stated in Ontario (Canada). Lower concentrations of nitrosamines were found in the reservoir (20.3 ng/L) and in the DWTP samples (n.d. -28.6 ng/L). NDMA and NDEA were respectively found in the reservoir and in treated and highly chlorinated DWTP samples at concentrations above 10 ng/L (guide value established in different countries). The highest concentrations of nitrosamines were found after chlorination and ozonation processes (ozonated, treated and highly chlorinated water) in DWTP samples.

Pomegranate extract exhibits in vitro activity against Clostridium difficile.

Science.gov (United States)

Finegold, Sydney M; Summanen, Paula H; Corbett, Karen; Downes, Julia; Henning, Susanne M; Li, Zhaoping

2014-10-01

To determine the possible utility of pomegranate extract in the management or prevention of Clostridium difficile infections or colonization. The activity of pomegranate was tested against 29 clinical C. difficile isolates using the Clinical and Laboratory Standards Institute-approved agar dilution technique. Total phenolics content of the pomegranate extract was determined by Folin-Ciocalteau colorimetric method and final concentrations of 6.25 to 400 μg/mL gallic acid equivalent were achieved in the agar. All strains had MICs at 12.5 to 25 mg/mL gallic acid equivalent range. Our results suggest antimicrobial in vitro activity for pomegranate extract against toxigenic C. difficile. Pomegranate extract may be a useful contributor to the management and prevention of C. difficile disease or colonization. Copyright © 2014 Elsevier Inc. All rights reserved.

Serum/plasma methylmercury determination by isotope dilution gas chromatography-inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Baxter, Douglas C., E-mail: douglas.baxter@alsglobal.com [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Faarinen, Mikko [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Osterlund, Helene; Rodushkin, Ilia [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Division of Geosciences, Lulea University of Technology, 977 87 Lulea (Sweden); Christensen, Morten [ALS Scandinavia AB, Maskinvaegen 2, 183 53 Taeby (Sweden)

2011-09-09

Highlights: {center_dot} We determine methylmercury in serum and plasma using isotope dilution calibration. {center_dot} Separation by gas chromatography and detection by inductively coupled plasma mass spectrometry. {center_dot} Data for 50 specimens provides first reference range for methylmercury in serum. {center_dot} Serum samples shown to be stable for 11 months in refrigerator. - Abstract: A method for the determination of methylmercury in plasma and serum samples was developed. The method uses isotope dilution with {sup 198}Hg-labeled methylmercury, extraction into dichloromethane, back-extraction into water, aqueous-phase ethylation, purge and trap collection, thermal desorption, separation by gas chromatography, and mercury isotope specific detection by inductively coupled plasma mass spectrometry. By spiking 2 mL sample with 1.2 ng tracer, measurements in a concentration interval of (0.007-2.9) {mu}g L{sup -1} could be performed with uncertainty amplification factors <2. A limit of quantification of 0.03 {mu}g L{sup -1} was estimated at 10 times the standard deviation of concentrations measured in preparation blanks. Within- and between-run relative standard deviations were <10% at added concentration levels of 0.14 {mu}g L{sup -1}, 0.35 {mu}g L{sup -1} and 2.8 {mu}g L{sup -1}, with recoveries in the range 82-110%. Application of the method to 50 plasma/serum samples yielded a median (mean; range) concentration of methylmercury of 0.081 (0.091; <0.03-0.19) {mu}g L{sup -1}. This is the first time methylmercury has been directly measured in this kind of specimen, and is therefore the first estimate of a reference range.

Neurotoxic, cytotoxic, apoptotic and antiproliferative effects of some marine algae extracts on the NA2B cell line.

Science.gov (United States)

Kurt, O; Özdal-Kurt, F; Akçora, C M; Özkut, M; Tuğlu, M I

2018-02-01

Oxidative stress contributes to cancer pathologies and to apoptosis. Marine algae exhibit cytotoxic, antiproliferative and apoptotic effects; their metabolites have been used to treat many types of cancer. We investigated in culture extracts of Petalonia fascia, Jania longifurca and Halimeda tuna to determine their effects on mouse neuroblastoma cell line, NA2B. NA2B cells were treated with algae extracts, and the survival and proliferation of NA2B cells were assessed using the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay. The effects of algae extracts on oxidative stress in NA2B cells also were investigated using nitric oxide synthase (NOS) immunocytochemistry and apoptosis was assessed using terminal deoxynucleotidyl transferase dUTP nick end labeling. We observed significant neurite inhibition with moderate damage by the neurotoxicity-screening test (NST) at IC 50 dilutions of the extracts. MTT demonstrated that J. longifurca extracts were more toxic than P. fascia and H. tuna extracts. We found an increase of endothelial and inducible NOS immunostaining for oxidative stress and TUNEL analysis revealed increased apoptosis after application of extract. Our findings suggest that the algae we tested may have potential use for treatment of cancer.

The measurement of the chemically mobile fraction of lead in soil using isotopic dilution analysis

International Nuclear Information System (INIS)

Kirchhoff, J.; Brand, J.; Schuettelkopf, H.

1992-12-01

The chemically available fraction of lead in eight soils measured by isotopic dilution analysis using 212 Pb ranged from 7 to 16% of the total content of lead in soil. The soluble fractions achieved values up to 63% of the total content in 1 M NH 4 NO 3 , 1 M MgCl 2 and 0.05 M DTPA solutions. Increasing the contact time between water and soil, the water-soil ratio from 1:1 to 5:1 and increasing the temperature of the soil-water suspension raised the chemically available fraction in soil. Comparing various soil parameters and the mobile fraction of lead, only pH shows a significant correlation. The amphoteric character of lead causes a minimum of mobility about pH 6; pH-values below are responsible for the higher mobility of lead as Pb 2+ , at pH-values above 6 soluble hydroxy and humic acid complexes are formed. (orig.) [de

Solvent extraction of aromatics from middle distillates: equilibria prediction method by group contribution

Energy Technology Data Exchange (ETDEWEB)

Rahman, M.; Mikitenko, P.; Asselineau, L.

1984-01-01

A method of calculating liquid-liquid aromatics extraction of a middle distillate is described. The group contribution models of the ASOG and UNIFAC type are investigated. Four vapor liquid equilibrium (VLE), two solid-liquid equilibrium (SLE), three binary and six ternary liquid-liquid equilibrium (LLE) have been measured. The parameters of the models are based mainly on the data of the systems having 10-20 carbon number. VLE, SLE, and infinite dilution activity coefficient data (17-245/sup 0/C) have been used for calculating interaction parameters between hydrocarbon groups and LLE data (20-80/sup 0/C) for interaction parameters of dimethylformamide-hydrocarbon groups. Middle distillate representation is based on mass spectrometric and gas chromatographic analysis and on limited data of middle distillate-DMF liquid-liquid equilibrium. It is shown that the performance of ASOG and UNIFAC models are sufficiently valid in representation of data base and in extraction calculations. Considering the predictive character and the rapidity of its application this method can be useful in the preliminary study of extraction processes. 34 references, 2 figures, 10 tables.

Antibacterial activities of aqueous extracts of terminalia catappa, momordica charantia and acalypha wilkesiana on escherichia coli isolated from pediatrics

International Nuclear Information System (INIS)

Odeyemi, A.O.; Olawande, F.T.

2015-01-01

Antibacterial activity of aqueous extract of Terminalia catappa, Momordica charantia and Acalypha wilkesiana was investigated against Escherichia coli isolated from pediatrics with the minimum inhibitory concentration (MIC) of 0.5mg/mL by agar dilution technique. The antibacterial potency of the extracts as evaluated by broth dilution technique, showed diameter of inhibition zone of 22.80 mm, 14.20 mm and 21.00 mm at a concentration of 0.5 mg/mL for T. catappa, M. charantia and A. wilkesiana, respectively. The antibacterial effect of T. catappa was found to be more pronounced with its plausible use for the treatment of infections caused by E. coli. (author)

Raman Analysis of Dilute Aqueous Samples by Localized Evaporation of Submicroliter Droplets on the Tips of Superhydrophobic Copper Wires.

Science.gov (United States)

Cheung, Melody; Lee, Wendy W Y; McCracken, John N; Larmour, Iain A; Brennan, Steven; Bell, Steven E J

2016-04-19

Raman analysis of dilute aqueous solutions is normally prevented by their low signal levels. A very general method to increase the concentration to detectable levels is to evaporate droplets of the sample to dryness, creating solid deposits which are then Raman probed. Here, superhydrophobic (SHP) wires with hydrophilic tips have been used as supports for drying droplets, which have the advantage that the residue is automatically deposited at the tip. The SHP wires were readily prepared in minutes using electroless galvanic deposition of Ag onto copper wires followed by modification with a polyfluorothiol (3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro-1-decanethiol, HDFT). Cutting the coated wires with a scalpel revealed hydrophilic tips which could support droplets whose maximum size was determined by the wire diameter. Typically, 230 μm wires were used to support 0.6 μL droplets. Evaporation of dilute melamine droplets gave solid deposits which could be observed by scanning electron microscopy (SEM) and Raman spectroscopy. The limit of detection for melamine using a two stage evaporation procedure was 1 × 10(-6) mol dm(-3). The physical appearance of dried droplets of sucrose and glucose showed that the samples retained significant amounts of water, even under high vacuum. Nonetheless, the Raman detection limits of sucrose and glucose were 5 × 10(-4) and 2.5 × 10(-3) mol dm(-3), respectively, which is similar to the sensitivity reported for surface-enhanced Raman spectroscopy (SERS) detection of glucose. It was also possible to quantify the two sugars in mixtures at concentrations which were similar to those found in human blood through multivariate analysis.

Ammonium chloride salting out extraction/cleanup for trace-level quantitative analysis in food and biological matrices by flow injection tandem mass spectrometry.

Science.gov (United States)

Nanita, Sergio C; Padivitage, Nilusha L T

2013-03-20

A sample extraction and purification procedure that uses ammonium-salt-induced acetonitrile/water phase separation was developed and demonstrated to be compatible with the recently reported method for pesticide residue analysis based on fast extraction and dilution flow injection mass spectrometry (FED-FI-MS). The ammonium salts evaluated were chloride, acetate, formate, carbonate, and sulfate. A mixture of NaCl and MgSO4, salts used in the well-known QuEChERS method, was also tested for comparison. With thermal decomposition/evaporation temperature of salts resulted in negligible ion source residual under typical electrospray conditions, leading to consistent method performance and less instrument cleaning. Although all ammonium salts tested induced acetonitrile/water phase separation, NH4Cl yielded the best performance, thus it was the preferred salting out agent. The NH4Cl salting out method was successfully coupled with FI/MS/MS and tested for fourteen pesticide active ingredients: chlorantraniliprole, cyantraniliprole, chlorimuron ethyl, oxamyl, methomyl, sulfometuron methyl, chlorsulfuron, triflusulfuron methyl, azimsulfuron, flupyrsulfuron methyl, aminocyclopyrachlor, aminocyclopyrachlor methyl, diuron and hexazinone. A validation study was conducted with nine complex matrices: sorghum, rice, grapefruit, canola, milk, eggs, beef, urine and blood plasma. The method is applicable to all analytes, except aminocyclopyrachlor. The method was deemed appropriate for quantitative analysis in 114 out of 126 analyte/matrix cases tested (applicability rate=0.90). The NH4Cl salting out extraction/cleanup allowed expansion of FI/MS/MS for analysis in food of plant and animal origin, and body fluids with increased ruggedness and sensitivity, while maintaining high-throughput (run time=30s/sample). Limits of quantitation (LOQs) of 0.01mgkg(-1) (ppm), the 'well-accepted standard' in pesticide residue analysis, were achieved in >80% of cases tested; while limits of detection

MOLECULARLY IMPRINTED SOLID PHASE EXTRACTION FOR TRACE ANALYSIS OF DIAZINON IN DRINKING WATER

Directory of Open Access Journals (Sweden)

M. Rahiminejad ، S. J. Shahtaheri ، M. R. Ganjali ، A. Rahimi Forushani ، F. Golbabaei

2009-04-01

Full Text Available Amongst organophosphate pesticides, the one most widely used and common environmental contaminant is diazinon; thus methods for its trace analysis in environmental samples must be developed. Use of diazinon imprinted polymers such as sorbents in solid phase extraction, is a prominent and novel application area of molecular imprinted polymers. For diazinon extraction, high performance liquid chromatography analysis was demonstrated in this study. During optimization of the molecular imprinted solid phase extraction procedure for efficient solid phase extraction of diazinon, Plackett-Burman design was conducted. Eight experimental factors with critical influence on molecular imprinted solid phase extraction performance were selected, and 12 different experimental runs based on Plackett-Burman design were carried out. The applicability of diazinon imprinted polymers as the sorbent in solid phase extraction, presented obtained good recoveries of diazinon from LC-grade water. An increase in pH caused an increase in the recovery on molecular imprinted solid phase extraction. From these results, the optimal molecular imprinted solid phase extraction procedure was as follows: solid phase extraction packing with 100 mg diazinon imprinted polymers; conditioning with 5 mL of methanol and 6 mL of LC-grade water; sample loading containing diazinon (pH=10; washing with 1 mL of LC-grade water, 1 mL LC- grade water containing 30% acetonitrile and 0.5 mL of acetonitrile, respectively; eluting with 1 mL of methanol containing 2% acetic acid. The percentage recoveries obtained by the optimized molecular imprinted solid phase extraction were more than 90% with drinking water spiked at different trace levels of diazinon. Generally speaking, the molecular imprinted solid phase extraction procedure and subsequent high performance liquid chromatography analysis can be a relatively fast and proper approach for qualitative and quantitative analysis of diazinon in

Effects of soil dilution and amendments (mussel shell, cow bone, and biochar) on Pb availability and phytotoxicity in military shooting range soil.

Science.gov (United States)

Ahmad, Mahtab; Soo Lee, Sang; Yang, Jae E; Ro, Hee-Myong; Han Lee, Young; Sik Ok, Yong

2012-05-01

Bioavailability and bioaccessibility determine the level of metal toxicity in the soils. Inorganic soil amendments may decrease metal bioavailability and enhance soil quality. This study used mussel shell, cow bone, and biochar to reduce lead (Pb) toxicity in the highly contaminated military shooting range soil in Korea. Water-soluble and 1-M ammonium nitrate extractions, and a modified physiologically based extraction test (PBET) were performed to determine Pb bioavailability and bioaccessibility in the soil, respectively. Active C in the soil was also measured to evaluate the effects of the amendments on biological soil quality. The Pb contaminated soil was diluted in serial with uncontaminated soil for the bioassays. Seed germination and root elongation tests using lettuce (Lactuca sativa) showed increases in germination percentage and root length in soil treated with the amendments. Biochar was most effective and increased seed germination by 360% and root length by 189% compared to the unamended soil. Up to 20% soil dilution resulted in more than 50% seed germination. Bioavailability and bioaccessibility of Pb in the soils were decreased by 92.5% and 48.5% with mussel shell, by 84.8% and 34.5% with cow bone, and by 75.8% and 12.5% with biochar, respectively, compared to the unamended soil. We found that the Pb availability in the military shooting range soil can be reduced effectively by the tested amendments or soil dilution alternately, thereby decreasing the risk of ecotoxicity. Furthermore, the increasing active C from the amendments revitalized the soil contaminated with Pb. Copyright © 2012 Elsevier Inc. All rights reserved.

Sulphur containing novel extractants for extraction-separation of palladium (II)

International Nuclear Information System (INIS)

Shukla, J.P.; Sawant, S.R.; Anil Kumar; Singh, R.K.

1995-01-01

Extraction performance of palladium (II) by sulphur containing extragents has unequivocally established their strong extraction ability toward this thiophilic soft metal. Hence a comprehensive investigative study was initiated by us to examine selective reversible extraction-separation of trace and macro amounts of palladium (II) from both aqueous nitric acid as well as hydrochloric acid media into 1,2-dichloroethane by 1,10-dithia-18 crown-6 (1,10-DT18C6), S 6 -pentano-36 (S 6 -P-36) and bis (2-ethylhexyl) sulphoxide (BESO) dissolved in toluene. From the study of aqueous phase acidity, reagent concentration, period of equilibration, diluent, strippant and diverse ions, conditions are established from its quantitative and reversible extraction. Recovery of Pd(II) from loaded thiacrown and sulphoxide phase is easily accomplished by using sodium thiocyanate, ammonium thiocyanate, thiourea, sodium thiosulphate and mixture of (2M Na 2 CO 3 + 0.5 NH 4 OH) (only for BESO) as the strippants. The lack of interference from even appreciable amounts of contaminants like 137 Cs, 106 Ru, 233 U and 239 Pu may be considered as one of the outstanding advantages of the method. Application of these extractants has been successfully tested for the recovery of palladium from high active waste matrix. The extracted complex from both the thiacrowns has been characterized by elemental analyses and UV-Visible spectra, confirmed to be PdA 2 .T (A = NO - 3 , Cl - ) from dilute (pH ∼ 2) acid solutions while composition of organic species with palladium for the sulphoxide, has also been confirmed to be disolvate of the type Pd(NO 3 ) 2 .2BESO. (author). 52 refs., 6 tabs., 6 figs

Effects of extracellular magnesium extract on the proliferation and differentiation of human osteoblasts and osteoclasts in coculture.

Science.gov (United States)

Wu, Lili; Feyerabend, Frank; Schilling, Arndt F; Willumeit-Römer, Regine; Luthringer, Bérengère J C

2015-11-01

Coculture of osteoblasts and osteoclasts is a subject of interest in the understanding of how magnesium (Mg)-based implants influence the bone metabolism and remodeling upon degradation. Human telomerase reverse transcriptase (hTERT) transduced mesenchymal stem cells (SCP-1) were first differentiated into osteoblasts with osteogenic supplements and then further cocultured with peripheral blood mononucleated cells (PBMC) without the addition of osteoclastogenesis promoting factors. Concomitantly, the cultures were exposed to variable Mg extract dilutions (0, 30×, 10×, 5×, 3×, 2× and 1×). Phenotype characterization documented that while 2× dilution of Mg extract was extremely toxic to osteoclast monoculture, monocytes in coculture with osteoblasts exhibited a greater tolerance to higher Mg extract concentration. The dense growth of osteoblasts in cultures with 1× dilution of Mg extract suggested that high concentration of Mg extract promoted osteoblast proliferation/differentiation behavior. The results of intracellular alkaline phosphatase (ALP) and tartrate-resistant acid phosphatase (TRAP) activities as well as protein and gene expressions of receptor activator of nuclear factor kappa-B ligand (RANKL), macrophage colony-stimulating factor (M-CSF), and osteoclast-associated receptor (OSCAR) revealed significantly enhanced formation of osteoblasts whereas decreased osteoclastogenesis in the cultures with high concentrations of Mg extract (2× and 1× dilutions). In conclusion, while an increased osteoinductivity has been demonstrated, the impact of potentially decreased osteoclastogenesis around the Mg-based implants should be also taken into account. Cocultures containing both bone-forming osteoblasts and bone-resorbing osteoclasts should be preferentially performed for in vitro cytocompatibility assessment of Mg-based implants as they more closely mimic the in vivo environment. An attractive human osteoblasts and osteoclasts cocultivation regime was

Evaluation of anti-bacterial properties of ethanol extract of Ficus ...

African Journals Online (AJOL)

Yomi

2012-02-23

Feb 23, 2012 ... pneumoniae were incubated in agar plates after serial dilutions of the extract were added in wells made in the agar and incubated for 24 h at 37°C. Thereafter, zones of inhibition (in mm) around the wells were measured. The same organisms were tested for sensitivity against standard antibiotics using disk.

Evaluation of sample extraction methods for proteomics analysis of green algae Chlorella vulgaris.

Science.gov (United States)

Gao, Yan; Lim, Teck Kwang; Lin, Qingsong; Li, Sam Fong Yau

2016-05-01

Many protein extraction methods have been developed for plant proteome analysis but information is limited on the optimal protein extraction method from algae species. This study evaluated four protein extraction methods, i.e. direct lysis buffer method, TCA-acetone method, phenol method, and phenol/TCA-acetone method, using green algae Chlorella vulgaris for proteome analysis. The data presented showed that phenol/TCA-acetone method was superior to the other three tested methods with regards to shotgun proteomics. Proteins identified using shotgun proteomics were validated using sequential window acquisition of all theoretical fragment-ion spectra (SWATH) technique. Additionally, SWATH provides protein quantitation information from different methods and protein abundance using different protein extraction methods was evaluated. These results highlight the importance of green algae protein extraction method for subsequent MS analysis and identification. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Bioconversion of dilute-acid pretreated sorghum bagasse to ethanol by Neurospora crassa.

Science.gov (United States)

Dogaris, Ioannis; Gkounta, Olga; Mamma, Diomi; Kekos, Dimitris

2012-07-01

Bioethanol production from sweet sorghum bagasse (SB), the lignocellulosic solid residue obtained after extraction of sugars from sorghum stalks, can further improve the energy yield of the crop. The aim of the present work was to evaluate a cost-efficient bioconversion of SB to ethanol at high solids loadings (16 % at pretreatment and 8 % at fermentation), low cellulase activities (1-7 FPU/g SB) and co-fermentation of hexoses and pentoses. The fungus Neurospora crassa DSM 1129 was used, which exhibits both depolymerase and co-fermentative ability, as well as mixed cultures with Saccharomyces cerevisiae 2541. A dilute-acid pretreatment (sulfuric acid 2 g/100 g SB; 210 °C; 10 min) was implemented, with high hemicellulose decomposition and low inhibitor formation. The bioconversion efficiency of N. crassa was superior to S. cerevisiae, while their mixed cultures had negative effect on ethanol production. Supplementing the in situ produced N. crassa cellulolytic system (1.0 FPU/g SB) with commercial cellulase and β-glucosidase mixture at low activity (6.0 FPU/g SB) increased ethanol production to 27.6 g/l or 84.7 % of theoretical yield (based on SB cellulose and hemicellulose sugar content). The combined dilute-acid pretreatment and bioconversion led to maximum cellulose and hemicellulose hydrolysis 73.3 % and 89.6 %, respectively.

Alternate extractants to tributyl phosphate for reactor fuel reprocessing

International Nuclear Information System (INIS)

Crouse, D.J.; Arnold, W.D.; Hurst, F.J.

1983-01-01

Both tri(n-hexyl) phosphate (THP) and tri(2-ethylhexyl) phosphate (TEHP) have some important potential process advantages over TBP for reactor fuel reprocessing. These include negligible aqueous phase solubility and less tendency toward third phase and crud formation. The alkyl chain branching of TEHP makes it much more stable to chemical degradation than TBP and probably also accounts for its much weaker ruthenium extraction. The higher uranium and plutonium extraction power of THP and TEHP allows higher solvent loadings in extraction but makes them somewhat more difficult to strip. The phase separation properties of 1.09 M solutions of THP and TEHP are inferior to those of 1.09 M TBP (30 vol %) but are favorable at lower concentrations. Use of more dilute THP and TEHP solutions is recommended for this reason and to obtain a better balance of extraction power in the extraction versus stripping steps

Studies on the analysis of 25-hydroxyvitamin D{sub 3} by isotope-dilution liquid chromatography–tandem mass spectrometry using enzyme-assisted derivatisation

Energy Technology Data Exchange (ETDEWEB)

Abdel-Khalik, Jonas, E-mail: J.A.F.A.ABDEL-KHALIK.744116@swansea.ac.uk [Institute of Mass Spectrometry, College of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom); Crick, Peter J. [Institute of Mass Spectrometry, College of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom); Carter, Graham D. [DEQAS, Imperial College Healthcare NHS Trust, Clinical Biochemistry Department, Charing Cross Hospital, Fulham Palace Rd, London W6 8RF (United Kingdom); Makin, Hugh L. [Barts and the Royal London School of Medicine and Dentistry, Queen Mary University of London, London E1 2AD (United Kingdom); Wang, Yuqin [Institute of Mass Spectrometry, College of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom); Griffiths, William J., E-mail: w.j.griffiths@swansea.ac.uk [Institute of Mass Spectrometry, College of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom)

2014-04-11

Highlights: • New method for the analysis of 25-hydroxyvitamin D{sub 3} exploiting Girard P derivatisation. • Method also applicable to vitamin D{sub 3}, 1α,25- and 24,25-dihydroxyvitamin D{sub 3}. • By modification of the method 3-epi-25-hydroxyvitamin D{sub 3} can also be analysed. - Abstract: The total serum concentration of 25-hydroxyvitamins D (25-hydroxyvitamin D{sub 3} and 25-hydroxyvitamin D{sub 2}) is currently used as an indicator of vitamins D status. Vitamins D insufficiency is claimed to be associated with multiple diseases, thus accurate and precise reference methods for the quantification of 25-hydroxyvitamins D are needed. Here we present a novel enzyme-assisted derivatisation method for the analysis of vitamins D metabolites in adult serum utilising 25-[26,26,26,27,27,27-{sup 2}H{sub 6}]hydroxyvitamin D{sub 3} as the internal standard. Extraction of 25-hydroxyvitamins D from serum is performed with acetonitrile, which is shown to be more efficient than ethanol. Cholesterol oxidase is used to oxidize the 3β-hydroxy group in the vitamins D metabolites followed by derivatisation of the newly formed 3-oxo group with Girard P reagent. 17β-Hydroxysteroid dehydrogenase type 10 is shown to oxidize selectively the 3α-hydroxy group in the 3α-hydroxy epimer of 25-hydroxyvitamin D{sub 3}. Quantification is achieved by isotope-dilution liquid chromatography–tandem mass spectrometry. Recovery experiments for 25-hydroxyvitamin D{sub 3} performed on adult human serum give recovery of 102–106%. Furthermore in addition to 25-hydroxyvitamin D{sub 3}, 24,25-dihydroxyvitamin D{sub 3} and other uncharacterised dihydroxy metabolites, were detected in adult human serum.

Isotope dilution-GC-MS/MS analysis of 16 polycyclic aromatic hydrocarbons in selected medicinal herbs used as health food additives.

Science.gov (United States)

Yu, L; Cao, Y; Zhang, J; Cui, Z; Sun, H

2012-01-01

Medicinal herbs have a very important role in health protection and disease control, and have been used in health foods. Polycyclic aromatic hydrocarbons (PAHs) have carcinogenic, biological and mutagenic effects. In this paper, the content of 16 PAHs as representative contaminants in nine Chinese medicinal herbs, as additives for health foods, was investigated in order to ensure food safety from this source. A highly sensitive isotope dilution-gas chromatography-tandem mass spectrometry (ID-GC-MS/MS) method combined with gel permeation chromatography (GPC) and solid-phase extraction (SPE) was developed. Calibration curves showed good linearity for all PAHs (R² > 0.999), and the limit of quantification (LOQ) ranged from 0.42 to 2.7 µg kg⁻¹. Average recoveries for these compounds were in the range of 52.5-117%, 52.6-119% and 81.4-108% at the concentrations of 10, 50 and 250 µg kg⁻¹ with RSD of 1.8-15%, 0.9-15% and 1.0-15%, respectively. The proposed method was used for the analysis of nine Chinese medicinal herbs. Total levels of PAHs varied from 98.2 µg kg⁻¹ (cassia seed) to 2245 µg kg⁻¹ (eucommia bark). The highest level was found for phenanthrene (Phe) in liquorice root (631.3 µg kg⁻¹), indigowoad leaf (551.0 µg kg⁻¹), rose flower (435.2 µg kg⁻¹) and eucommia bark (432.3 µg kg⁻¹). The proposed method could provide a useful basis for safety monitoring of herbs and risk management for PAHs in the health food industry.

Endothelial extraction of tracer water varies with extravascular water in dog lungs

International Nuclear Information System (INIS)

Chinard, F.P.; Cua, W.O.

1987-01-01

In multiple indicator-dilution experiments, transvascular passage of a permeating indicator is conventionally derived from the up-slope separation of the curve of the permeating indicator from that of a vascular reference and is expressed as the extraction (Ec). Extraction may be limited by the barrier (barrier-limited distribution). It may be limited by the volume of distribution accessible to it; in the time domain of an indicator-dilution experiment, the passage to and distribution in the extravascular volume are rapid relative to the velocity of blood in the exchange vessels. We examine here the relations of the extraction of tracer water as tritium oxide (THO) [Ec(THO)] and of the extraction of tracer sodium as 22Na [Ec(22Na)] to extravascular lung water, delta V wev, by adding isotonic fluid to the gas phase of the lungs. The net convective transvascular passage of water is negligible relative to the transendothelial molecular exchange. In 10 experiments in vivo and in 10 experiments in isolated perfused lungs, Ec(THO) increases as delta V wev increases. Ec(22Na) and the permeability-surface area product (PS) for 22Na do not change as delta V wev increases. We conclude that the extraction of THO is determined mainly by the volume accessible to it (flow- or volume-limited distribution) and that the extraction of 22Na is determined mainly by the resistance of the endothelium (barrier-limited distribution). A diffusion limitation in the added alveolar fluid rather than a barrier limitation at the endothelium may moderate Ec

Simultaneous speciation of mercury and butyltin compounds in natural waters and snow by propylation and species-specific isotope dilution mass spectrometry analysis

Energy Technology Data Exchange (ETDEWEB)

Monperrus, M.; Tessier, E.; Veschambre, S.; Amouroux, D.; Donard, O. [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique Bio-inorganique et Environnement, CNRS UMR 5034, Helioparc, Pau (France)

2005-02-01

A robust method has been developed for simultaneous determination of mercury and butyltin compounds in aqueous samples. This method is capable of providing accurate results for analyte concentrations in the picogram per liter to nanogram per liter range. The simultaneous determination of the mercury and tin compounds is achieved by species-specific isotope dilution, derivatization, and gas chromatography-inductively coupled plasma mass spectrometer (GC-ICP-MS). In derivatization by ethylation and propylation, reaction conditions such as pH and the effect of chloride were carefully studied. Ethylation was found to be more sensitive to matrix effects, especially for mercury compounds. Propylation was thus the preferred derivatization method for simultaneous determination of organomercury and organotin compounds in environmental samples. The analytical method is highly accurate and precise, with RSD values of 1 and 3% for analyte concentrations in the picogram per liter to nanogram per liter range. By use of cleaning procedures and SIDMS blank measurements, detection limits in the range 10-60 pg L{sup -1} were achieved; these are suitable for determination of background levels of these contaminants in environmental samples. This was demonstrated by using the method for analysis of real snow and seawater samples. This work illustrates the great advantage of species-specific isotope dilution for the validation of an analytical speciation method - the possibility of overcoming species transformations and non-quantitative recovery. Analysis time is saved by use of the simultaneous method, because of the use of a single sample-preparation procedure and one analysis. (orig.)

Determination of six sulfonamide antibiotics, two metabolites and trimethoprim in wastewater by isotope dilution liquid chromatography/tandem mass spectrometry.

Science.gov (United States)

Le-Minh, Nhat; Stuetz, Richard M; Khan, Stuart J

2012-01-30

A highly sensitive method for the analysis of six sulfonamide antibiotics (sulfadiazine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine and sulfamethoxazole), two sulfonamide metabolites (N(4)-acetyl sulfamethazine and N(4)-acetyl sulfamethoxazole) and the commonly co-applied antibiotic trimethoprim was developed for the analysis of complex wastewater samples. The method involves solid phase extraction of filtered wastewater samples followed by liquid chromatography-tandem mass spectral detection. Method detection limits were shown to be matrix-dependent but ranged between 0.2 and 0.4 ng/mL for ultrapure water, 0.4 and 0.7 ng/mL for tap water, 1.4 and 5.9 ng/mL for a laboratory-scale membrane bioreactor (MBR) mixed liquor, 0.7 and 1.7 ng/mL for biologically treated effluent and 0.5 and 1.5 ng/g dry weight for MBR activated sludge. An investigation of analytical matrix effects was undertaken, demonstrating the significant and largely unpredictable nature of signal suppression observed for variably complex matrices compared to an ultrapure water matrix. The results demonstrate the importance of accounting for such matrix effects for accurate quantitation, as done in the presented method by isotope dilution. Comprehensive validation of calibration linearity, reproducibility, extraction recovery, limits of detection and quantification are also presented. Finally, wastewater samples from a variety of treatment stages in a full-scale wastewater treatment plant were analysed to illustrate the effectiveness of the method. Copyright © 2011 Elsevier B.V. All rights reserved.

Applicability of isotopic dilution methods for determination of the zinc supplying capacity of some Indian soils

International Nuclear Information System (INIS)

Iyengar, B.R.V.; Deb, D.L.

1975-01-01

The applicability of the isotopic dilution methods to determine the zinc supplying capacity of some Indian soils belonging to three soil groups was studied using 65 Zn. In these soils 'L' values determined by the pot culture method and the 'E' values by equilibration in soil suspensions by the carrier free and carrier methods and using chemical extractants DTPA-CaCl 2 -NaOAc and EDTA-NH 4 OAc were compared. The 'L' values were significantly correlated with zinc uptake by maize and also with zinc extracted by a number of chemical extractants. The laboratory determinations 'E' values by isotopic exchange equilibria in soil suspension both with and without carrier zinc led to over estimates and gave grossly exggerated values of 'labile zinc' especially in alkaline and high zinc 'fixing' soils. The 'E' values determined in both DTPA-CaCl 2 -NaOAc and EDTA-NH 4 OAc correlated significantly with zinc uptake by maize. These values agreed well with 'L' values and 'available' zinc determined by chemical soil tests. (author)

Larvicidal effects of aqueous extracts of Balanites aegyptiaca (desert ...

African Journals Online (AJOL)

The effect of aqueous extracts of the fruit pulp, seed kernel, roots, bark, and leaves of Balanites aegyptiaca Del. (Zygophyllacea) against the larvae of the Culex pipens mosquito was investigated. Early fourth instars larvae of C. pipiens mosquitoes were exposed, for up to three days, to a dilution of 0, 0.1, 0.25, 0.5, 1.0, and ...

Measurement of isotope abundance variations in nature by gravimetric spiking isotope dilution analysis (GS-IDA).

Science.gov (United States)

Chew, Gina; Walczyk, Thomas

2013-04-02

Subtle variations in the isotopic composition of elements carry unique information about physical and chemical processes in nature and are now exploited widely in diverse areas of research. Reliable measurement of natural isotope abundance variations is among the biggest challenges in inorganic mass spectrometry as they are highly sensitive to methodological bias. For decades, double spiking of the sample with a mix of two stable isotopes has been considered the reference technique for measuring such variations both by multicollector-inductively coupled plasma mass spectrometry (MC-ICPMS) and multicollector-thermal ionization mass spectrometry (MC-TIMS). However, this technique can only be applied to elements having at least four stable isotopes. Here we present a novel approach that requires measurement of three isotope signals only and which is more robust than the conventional double spiking technique. This became possible by gravimetric mixing of the sample with an isotopic spike in different proportions and by applying principles of isotope dilution for data analysis (GS-IDA). The potential and principle use of the technique is demonstrated for Mg in human urine using MC-TIMS for isotopic analysis. Mg is an element inaccessible to double spiking methods as it consists of three stable isotopes only and shows great potential for metabolically induced isotope effects waiting to be explored.

Antimicrobial activity and some phytochemical analysis of two extracts Vinca minor L.

Directory of Open Access Journals (Sweden)

Grujić Sandra M.

2014-01-01

Full Text Available This study investigated the antimicrobial activity as well as some phytochemical analysis of ethanol and diethyl ether extracts from plant species Vinca minor L. In vitro antimicrobial activity of extracts was studied on 20 strains of microorganisms (16 bacteria and four yeasts. Testing was performed by microdilution method and minimum inhibitory concentration (MIC and minimum microbicidal concentration (MMC were determined. The strongest antimicrobial activity was detected on G+ bacteria of the genus Bacillus. Tested G- bacteria and yeasts were not sensitive to the action of the extracts or the sensitivity was insignificant. Phytochemical analysis involved determining the amount of total phenolics, flavonoids and tannins, as well as the determination of antioxidant activity monitoring capability to neutralize free radicals (DPPH and the reductive potential. Phytochemical examination indicates that the total phenolic compounds were more in the ethanolic extract and the content of flavonoids and tannins marginally higher in the diethyl ether extract. The antioxidant activity (DPPH of the ethanolic extract of V. minor was significantly stronger as compared to the diethyl ether extract, and the reduction potential was approximately the same.

Multi-element isotope dilution analyses using ICP-MS

International Nuclear Information System (INIS)

Volpe, A.M.

1996-01-01

Presently, 37 elements ranging from light (Li,B) through transition metals, noble, rare earth and heavy elements, to actinides and transuranics (Pu, Am, Cm) are measured by isotope dilution at Lawrence Livermore National Laboratory. Projects range from geological and hydrological to biological. The research goal is to measure accurately many elements present in diverse matrices at trace (ppb) levels using isotope dilution methods. Major advantages of isotope dilution methods are accuracy, elimination of ion intensity calibration, and quantitation for samples that require chemical separation. Accuracy depends on tracer isotope calibration, tracer-sample isotopic equilibration, and appropriate background, isobaric and mass bias corrections. Propagation of isotope ratio error due to improper tracer isotope addition is a major concern with multi-element analyses when abundances vary widely. 11 refs., 3 figs

Calorimetric approach of lanthanides (3) complexation and extraction by malonamides

International Nuclear Information System (INIS)

Flandin, J.L.

2001-01-01

In the field of long lived radionuclides separation, diamides are interesting extractants because of their ability to co-extract trivalent lanthanides and actinides, which is a preliminary and essential step in high level radioactive waste reprocessing. The research carried out contributes to a better understanding of the mechanisms and the aim is the determination of thermodynamics properties (Δ r G, Δ r H et Δ r S) related to the complexation and the extraction of lanthanides(III) by malonamides. The first part of the document deals with the complexation of lanthanides(III) by an hydrosoluble diamide. The experimental results obtained by UV-visible spectrometry, TRLIF, NMR and microcalorimetric titration proved that lanthanides(III)-TEMA interactions in aqueous medium are very weak and that the complexation reaction is endothermic. The TEMA ligand still stays in the second coordination sphere of coordination of the lanthanide ion. The second part of this study focuses on the extraction of neodymium(III) nitrate by a lipophilic diamide which is an exothermic reaction. The influence of the composition of aqueous and organic phases on the thermodynamics properties Δ r G et Δ r H has been studied by microcalorimetric titration. The most influent parameter is the total concentration in extractant. As a consequence, thermodynamic values are very dependent on the organic phase organisation before and alter extraction. At the same time, this study showed the interest of the calorimetric approach for the analysis of basic reactions like diamide dilution and their organisation as oligomeric aggregates. (author)

Evaluation of Antimicrobial Activity of Root Extracts of Abitulon indicum

Directory of Open Access Journals (Sweden)

Krishna Rao MORTHA

2015-06-01

Full Text Available Antimicrobial activity of Abitulon indicum roots was studied against seven pathogenic bacteria and three fungal strains by agar well diffusion method. Antimicrobial activity was recorded for hexane, chloroform, methanol, ethanol and aqueous extracts. Alcohol (ethanol and methanol extracts exhibited the highest degree of antimicrobial activity compared to aqueous, chloroform and hexane extracts. Pseudomonas aeruginosa was turned out to be the most susceptible bacterium to the crude root chemical constituents, using the standard Tetracycline and Clotrimazole. Minimum inhibition concentration values of hexane, chloroform, methanol, ethanol and aqueous extracts were determined by the agar dilution method and ranged between 62.5 and 1,000 µg. The study suggested that the root extracts possess bioactive compounds with antimicrobial activity against the tested bacteria and fungi, revealing a significant scope to develop a novel broad spectrum of antimicrobial drug formulation from Abitulon indicum.

Trace uranium analysis in geological sample by isotope dilution-alpha spectrometry and comparison with other techniques

International Nuclear Information System (INIS)

Shihomatsu, H.M.; Iyer, S.S.

1988-12-01

Establishment of uranium determination in geological samples by alpha spectrometric isotope dilution technique using 233 U tracer is described in the present work. The various steps involved in the method namely, preparation of the sample, electrodeposition, alpha spectrometry, isotope dilution, calculation of the concentration and error statistics are discussed in detail. The experimental parameters for the electrodeposition of uranium, like current density, pH concentration of the electrolyte solution, deposition time, electrode distance were all optimised based on the efficiency of the deposition. The total accuracy and precision of the IDAS using 233 U tracer in the determination of uranium in mineral and granite samples were of the order of 1 to 2% for the concentration range of 50-1500 ppm of U. Our results are compared with those obtained by others workers using similar and different techniques. (author) [pt

A comparison of DNA extraction protocols from blood spotted on FTA cards for the detection of tick-borne pathogens by Reverse Line Blot hybridization.

Science.gov (United States)

Hailemariam, Zerihun; Ahmed, Jabbar Sabir; Clausen, Peter-Henning; Nijhof, Ard Menzo

2017-01-01

An essential step in the molecular detection of tick-borne pathogens (TBPs) in blood is the extraction of DNA. When cooled storage of blood under field conditions prior to DNA extraction in a dedicated laboratory is not possible, the storage of blood on filter paper forms a promising alternative. We evaluated six DNA extraction methods from blood spotted on FTA Classic ® cards (FTA cards), to determine the optimal protocol for the subsequent molecular detection of TBPs by PCR and the Reverse Line Blot hybridization assay (RLB). Ten-fold serial dilutions of bovine blood infected with Babesia bovis, Theileria mutans, Anaplasma marginale or Ehrlichia ruminantium were made by dilution with uninfected blood and spotted on FTA cards. Subsequently, DNA was extracted from FTA cards using six different DNA extraction protocols. DNA was also isolated from whole blood dilutions using a commercial kit. PCR/RLB results showed that washing of 3mm discs punched from FTA cards with FTA purification reagent followed by DNA extraction using Chelex ® resin was the most sensitive procedure. The detection limit could be improved when more discs were used as starting material for the DNA extraction, whereby the use of sixteen 3mm discs proved to be most practical. The presented best practice method for the extraction of DNA from blood spotted on FTA cards will facilitate epidemiological studies on TBPs. It may be particularly useful for field studies where a cold chain is absent. Copyright © 2016 Elsevier GmbH. All rights reserved.

Extraction and analysis of intact glucosinolates--a validated pressurized liquid extraction/liquid chromatography-mass spectrometry protocol for Isatis tinctoria, and qualitative analysis of other cruciferous plants.

Science.gov (United States)

Mohn, Tobias; Cutting, Brian; Ernst, Beat; Hamburger, Matthias

2007-09-28

Glucosinolates have attracted significant interest due to the chemopreventive properties of some of their transformation products. Numerous protocols for the extraction and analysis of glucosinolates have been published, but limited effort has been devoted to optimize and validate crucial extraction parameters and sample preparation steps. We carried out a systematic optimization and validation of a quantitative assay for the direct analysis of intact glucosinolates in Isatis tinctoria leaves (woad, Brassicaceae). Various parameters such as solvent composition, particle size, temperature, and number of required extraction steps were optimized using pressurized liquid extraction (PLE). We observed thermal degradation of glucosinolates at temperatures above 50 degrees C, and loss of >60% within 10min at 100 degrees C, but no enzymatic degradation in the leaf samples at ambient temperature. Excellent peak shape and resolution was obtained by reversed-phase chromatography on a Phenomenex Aqua column using 10mM ammonium formate as ion-pair reagent. Detection was carried out by electrospray ionisation mass spectrometry in the negative ion mode. Analysis of cruciferous vegetables and spices such as broccoli (Brassica oleracea L. var. italica), garden cress (Lepidium sativum L.) and black mustard (Sinapis nigra L.) demonstrated the general applicability of the method.

Attentional sets influence perceptual load effects, but not dilution effects.

Science.gov (United States)

Benoni, Hanna; Zivony, Alon; Tsal, Yehoshua

2014-01-01

Perceptual load theory [Lavie, N. (1995). Perceptual load as a necessary condition for selective attention. Journal of Experimental Psychology: Human Perception and Performance, 21, 451-468.; Lavie, N., & Tsal, Y. (1994) Perceptual load as a major determinant of the locus of selection in visual attention. Perception & Psychophysics, 56, 183-197.] proposes that interference from distractors can only be avoided in situations of high perceptual load. This theory has been supported by blocked design manipulations separating low load (when the target appears alone) and high load (when the target is embedded among neutral letters). Tsal and Benoni [(2010a). Diluting the burden of load: Perceptual load effects are simply dilution effects. Journal of Experimental Psychology: Human Perception and Performance, 36, 1645-1656.; Benoni, H., & Tsal, Y. (2010). Where have we gone wrong? Perceptual load does not affect selective attention. Vision Research, 50, 1292-1298.] have recently shown that these manipulations confound perceptual load with "dilution" (the mere presence of additional heterogeneous items in high-load situations). Theeuwes, Kramer, and Belopolsky [(2004). Attentional set interacts with perceptual load in visual search. Psychonomic Bulletin & Review, 11, 697-702.] independently questioned load theory by suggesting that attentional sets might also affect distractor interference. When high load and low load were intermixed, and participants could not prepare for the presentation that followed, both the low-load and high-load trials showed distractor interference. This result may also challenge the dilution account, which proposes a stimulus-driven mechanism. In the current study, we presented subjects with both fixed and mixed blocks, including a mix of dilution trials with low-load trials and with high-load trials. We thus separated the effect of dilution from load and tested the influence of attentional sets on each component. The results revealed that whereas

Subcritical water extraction of amino acids from Mars analog soils.

Science.gov (United States)

Noell, Aaron C; Fisher, Anita M; Fors-Francis, Kisa; Sherrit, Stewart

2018-01-18

For decades, the Martian regolith has stymied robotic mission efforts to catalog the organic molecules present. Perchlorate salts, found widely throughout Mars, are the main culprit as they breakdown and react with organics liberated from the regolith during pyrolysis, the primary extraction technique attempted to date on Mars. This work further develops subcritical water extraction (SCWE) as a technique for extraction of amino acids on future missions. The effect of SCWE temperature (185, 200, and 215°C) and duration of extraction (10-120 min) on the total amount and distribution of amino acids recovered was explored for three Mars analog soils (JSC Mars-1A simulant, an Atacama desert soil, and an Antarctic Dry Valleys soil) and bovine serum albumin (as a control solution of known amino acid content). Total amounts of amino acids extracted increased with both time and temperature; however, the distribution shifted notably due to the destruction of the amino acids with charged or polar side chains at the higher temperatures. The pure bovine serum albumin solution and JSC Mars 1A also showed lower yields than the Atacama and Antarctic extractions suggesting that SCWE may be less effective at hydrolyzing large or aggregated proteins. Changing solvent from water to a dilute (10 mM) HCl solution allowed total extraction efficiencies comparable to the higher temperature/time combinations while using the lowest temperature/time (185°C/20 min). The dilute HCl extractions also did not lead to the shift in amino acid distribution observed at the higher temperatures. Additionally, adding sodium perchlorate salt to the extraction did not interfere with recoveries. Native magnetite in the JSC Mars-1A may have been responsible for destruction of glycine, as evidenced by its uncharacteristic decrease as the temperature/time of extraction increased. This work shows that SCWE can extract high yields of native amino acids out of Mars analog soils with minimal disruption of the

Quantifying the Presence and Activity of Aerobic, Vinyl Chloride-Degrading Microorganisms in Dilute Groundwater Plumes by Using Real-Time PCR

Science.gov (United States)

2013-07-01

nested PCR experiment with etnC primers. The initial PCRs were carried out with environmental DNA and the primers NVC105 and NVC106 (72). Then, 2 μl...natural attenuation, dilute VC plumes Acknowledgements We would like to thank Bill Richard (EST Associates, Inc.), Tim McDougall (OASIS Environmental...these steps, the DNA extraction protocol was carried out as recommended by MoBio. Additional experimentation led us to further refine the Sterivex

Phytochemical screening and analysis of antioxidant properties of aqueous extract of wheatgrass.

Science.gov (United States)

Durairaj, Varalakshmi; Hoda, Muddasarul; Shakya, Garima; Babu, Sankar Pajaniradje Preedia; Rajagopalan, Rukkumani

2014-09-01

To screen the phytochemical constituents and study antioxidant properties of the aqueous extract of the wheatgrass. The current study was focused on broad parameters namely, phytochemical analysis, gas chromatography-mass spectrometry analysis and antioxidant properties in order to characterize the aqueous extract of wheatgrass as a potential free radical quencher. The phytochemical screening of the aqueous extract of wheatgrass showed the presence of various secondary metabolites but the absence of sterols and quinone in general. Wheatgrass was proved to be an effective radical scavenger in all antioxidant assays. The gas chromatography-mass spectrometry analysis confirmed the presence of diverse category of bioactive compounds such as squalene, caryophyllene and amyrins in varying percentage. From the results obtained, we conclude that wheatgrass aqueous extract contains various effective compounds. It is a potential source of natural antioxidants. Further analysis of this herb will help in finding new effective compounds which can be of potent use in pharmacological field. Copyright © 2014 Hainan Medical College. Published by Elsevier B.V. All rights reserved.

Extractables analysis of single-use flexible plastic biocontainers.

Science.gov (United States)

Marghitoiu, Liliana; Liu, Jian; Lee, Hans; Perez, Lourdes; Fujimori, Kiyoshi; Ronk, Michael; Hammond, Matthew R; Nunn, Heather; Lower, Asher; Rogers, Gary; Nashed-Samuel, Yasser

2015-01-01

Studies of the extractable profiles of bioprocessing components have become an integral part of drug development efforts to minimize possible compromise in process performance, decrease in drug product quality, and potential safety risk to patients due to the possibility of small molecules leaching out from the components. In this study, an effective extraction solvent system was developed to evaluate the organic extractable profiles of single-use bioprocess equipment, which has been gaining increasing popularity in the biopharmaceutical industry because of the many advantages over the traditional stainless steel-based bioreactors and other fluid mixing and storage vessels. The chosen extraction conditions were intended to represent aggressive conditions relative to the application of single-use bags in biopharmaceutical manufacture, in which aqueous based systems are largely utilized. Those extraction conditions, along with a non-targeted analytical strategy, allowed for the generation and identification of an array of extractable compounds; a total of 53 organic compounds were identified from four types of commercially available single-use bags, the majority of which are degradation products of polymer additives. The success of this overall extractables analysis strategy was reflected partially by the effectiveness in the extraction and identification of a compound that was later found to be highly detrimental to mammalian cell growth. The usage of single-use bioreactors has been increasing in biopharmaceutical industry because of the appealing advantages that it promises regarding to the cleaning, sterilization, operational flexibility, and so on, during manufacturing of biologics. However, compared to its conventional counterparts based mainly on stainless steel, single-use bioreactors are more susceptible to potential problems associated with compound leaching into the bioprocessing fluid. As a result, extractable profiling of the single-use system has become

Interaction Studies of Dilute Aqueous Oxalic Acid

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Kiran Kandpal

2007-01-01

Full Text Available Molecular conductance λm, relative viscosity and density of oxalicacid at different concentration in dilute aqueous solution were measured at 293 K.The conductance data were used to calculate the value association constant.Viscosity and density data were used to calculate the A and B coefficient ofJone-Dole equation and apparent molar volume respectively. The viscosityresults were utilized for the applicability of Modified Jone-Dole equation andStaurdinger equations. Mono oxalate anion acts, as structure maker and thesolute-solvent interaction were present in the dilute aqueous oxalic acid.

The Melt-Dilute Treatment Technology Offgas Development Status Report

International Nuclear Information System (INIS)

Adams, T. M.

1999-01-01

The melt-dilute treatment technology is being developed to facilitate the ultimate disposition of highly enriched Al-Base DOE spent nuclear fuels in a geologic repository such as that proposed for Yucca Mountain. The melt-dilute process is a method of preparing DOE spent nuclear fuel for long term storage

Evaluation of two different HEDP content kits: Stability study against dilution both in vivo and in vitro

International Nuclear Information System (INIS)

Inoue, O.; Ikeda, I.; Kurata, K.

1982-01-01

Two different HEDP content kits (Kit A, HEDP: 1 mg, SnCl 2 x 2H 2 O: 0.5 mg; and Kit B, HEDP: 10 mg, SnCl 2 x 2H 2 O: 0.5 mg) were evaluated for their stability against dillution. Sup(99m)Tc-HEDP solutions prepared from these two kits were diluted from 10 to 6000 fold with 0.9% NaCl solution just before evaluation both in vivo and in vitro. In the case of Kit A, significant soft tissue uptake in vivo and released free pertechnetate in vitro were observed by diluting the sup(99m)Tc-HEDP solution. On the other hand, sup(99m)Tc-HEDP prepared from Kit B was found to be sufficiently stable against dilution. The stability after preparation of each diluted sup(99m)-HEDP was also greatly affected by its HEDP concentration. Preliminary analysis of absorption spectra for each 99 Tc-HEDP indicated the possibility of two different sup(99m)Tc-HEDP complex formation by varied HEDP concentration. These results indicated that a cold reagent like Kit A might cause a higher soft tissue uptake due to its dilution in vivo during a clinical study for bone scanning. (orig.) [de

Single-dilution enzyme-linked immunosorbent assay for quantification of antigen-specific salmonid antibody

Science.gov (United States)

Alcorn, S.W.; Pascho, R.J.

2000-01-01

An enzyme-linked immunosorbent assay (ELISA) was developed on the basis of testing a single dilution of serum to quantify the level of antibody to the p57 protein of Renibaclerium salmoninarum in sockeye salmon (Oncorhynchus nerka). The levels of antibody were interpolated from a standard curve constructed by relating the optical densities (OD) produced by several dilutions of a high-titer rainbow trout (O. mykiss) antiserum to the p57 protein. The ELISA OD values produced by as many as 36 test sera on each microplate were compared with the standard curve to calculate the antigen-specific antibody activity. Repeated measurements of 36 samples on 3 microplates on each of 6 assay dates indicated that the mean intraassay coefficient of variation (CV) was 6.68% (range, 0-23%) and the mean interassay CV was 8.29% (range, 4-16%). The antibody levels determined for the serum sample from 24 sockeye salmon vaccinated with a recombinant p57 protein generally were correlated with the levels determined by endpoint titration (r2 = 0.936) and with results from another ELISA that was based on extrapolation of antibody levels from a standard curve (r2 = 0.956). The single-dilution antibody ELISA described here increases the number of samples that can be tested on each microplate compared with immunoassays based on analysis of several dilutions of each test serum. It includes controls for interassay standardization and can be used to test fish weighing <3 g.

A new method for the determination of NO2 traces using isotope dilution and mass spectrometry analysis

International Nuclear Information System (INIS)

Stevens, C.; Barat, F.; Nguyen Nghi, H.

1975-01-01

A new method for the determination of NO 2 traces, in the order of 1ppb (10 -9 ), in atmosphere and stratosphere is described. The method consists in an isotope dilution technique using 15 NO 2 , followed by the reduction of NO 2 to N 2 and a mass spectrometry analysis. A known amount of 15 NO 2 is added to the air samples. Then, NO 2 is separated from H 2 O, HNO 3 , CO 2 and N 2 O and transferred to a SiO 2 reactor by trapping at -196 deg C. In the reactor NO 2 is reduced to N 2 by reaction with electrolytic Cu heated at 580 deg C. The mass 29/mass 30 ratio corresponding to 15 N 14 N and 15 N 15 N is determined by mass spectrometry. The sensitivity of the method depends on the contamination introduced during the analysis of the sample (reagents, separation and measuring devices). The contamination is reproducible and in the order of 4.5+-0.5 10 -2 mm 3 N 2 [fr

Rapid and precise measurement of serum branched-chain and aromatic amino acids by isotope dilution liquid chromatography tandem mass spectrometry.

Directory of Open Access Journals (Sweden)

Ruiyue Yang

Full Text Available BACKGROUND: Serum branched-chain and aromatic amino acids (BCAAs and AAAs have emerged as predictors for the future development of diabetes and may aid in diabetes risk assessment. However, the current methods for the analysis of such amino acids in biological samples are time consuming. METHODS: An isotope dilution liquid chromatography tandem mass spectrometry (ID-LC/MS/MS method for serum BCAAs and AAAs was developed. The serum was mixed with isotope-labeled BCAA and AAA internal standards and the amino acids were extracted with acetonitrile, followed by analysis using LC/MS/MS. The LC separation was performed on a reversed-phase C18 column, and the MS/MS detection was performed via the positive electronic spray ionization in multiple reaction monitoring mode. RESULTS: Specific analysis of the amino acids was achieved within 2 min. Intra-run and total CVs for the amino acids were less than 2% and 4%, respectively, and the analytical recoveries ranged from 99.6 to 103.6%. CONCLUSION: A rapid and precise method for the measurement of serum BCAAs and AAAs was developed and may serve as a quick tool for screening serum BCAAs and AAAs in studies assessing diabetes risk.

Prediction of two-dimensional diluted magnetic semiconductors: Doped monolayer MoS2 systems

KAUST Repository

Cheng, Yingchun

2013-03-05

Using first-principles calculations, we propose a two-dimensional diluted magnetic semiconductor: monolayer MoS2 doped by transition metals. Doping of transition metal atoms from the IIIB to VIB groups results in nonmagnetic states, since the number of valence electrons is smaller or equal to that of Mo. Doping of atoms from the VIIB to IIB groups becomes energetically less and less favorable. Magnetism is observed for Mn, Fe, Co, Zn, Cd, and Hg doping, while for the other dopants from these groups it is suppressed by Jahn-Teller distortions. Analysis of the binding energies and magnetic properties indicates that (Mo,X)S2 (X=Mn, Fe, Co, and Zn) are promising systems to explore two-dimensional diluted magnetic semiconductors.

Evolution of Analysis of Polyhenols from Grapes, Wines, and Extracts

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Pierre-Louis Teissedre

2013-01-01

Full Text Available Grape and wine phenolics are structurally diverse, from simple molecules to oligomers and polymers usually designated as tannins. They have an important impact on the organoleptic properties of wines, that’s why their analysis and quantification are of primordial importance. The extraction of phenolics from grapes and from wines is the first step involved in the analysis. Then, several analytical methods have been developed for the determination of total content of phenolic, while chromatographic and spectrophotometric analyses are continuously improved in order to achieve adequate separation of phenolic molecules, their subsequent identification and quantification. This review provides a summary of evolution of analysis of polyphenols from grapes, wines and extracts.

Extraction and characterization of anthocyanin colorants from plant sources

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S. Dyankova

2016-03-01

Full Text Available Abstract. Natural pigments (and especially those of anthocyanins are a valuable source of bioactive compounds and may be used in the production of new functional food ingredients. Furthermore, their applications in the treatment and prevention of chronic disorders are becoming more and more widespread. In the last few years consumers have focused their attention on the natural biologically active compounds as functional food ingredients, and therefore, it may be assumed that natural colorants are an alternative source of synthetic additives. The aim of the study was to determine the quantitative content of monomeric anthocyanin pigments in extracts obtained from eight plants. The total content of monomeric anthocyanin pigments was measured by a pH-differential method. The TLC analysis of the pigment extracts from the different plants showed intensive rose, red and violet stripes corresponding to the anthocyanin content. The extracts from chicory and lavender petals were unstable and their color decreased in intensity in 1 month. The analysis of the experimental data shows that the yield of pigment substances depends on a few factors: the type of plant, the preliminary treatment of the plant and the solvent that is used. The largest quantity of extracted substances in the studied plants were isolated from chokeberry (2 195.9 cyd eq mg/l, followed by blackberry (1 466.2 and one variety of the grapes (1 199.3 . In the case of chokeberry, the pigment content included a large number of anthocyanins and the combination of these components was the reason for the deep red/violet color of the extract. Fresh or frozen materials are the most suitable for extraction of anthocyanin pigments. On the whole, fruit pulp yielded a larger quantity of pigments than juice. Anthocyanins are water-soluble compounds and for that reason their isolation requires water and other polar solvents. Better stabilization of color is obtained by a slight acidification of the

Initial magnetic susceptibility of the diluted magnetopolymer elastic composites

International Nuclear Information System (INIS)

Borin, D.Yu.; Odenbach, S.

2017-01-01

In this work diluted magnetopolymer elastic composites based on magnetic microparticles are experimentally studied. Considered samples have varied concentration of the magnetic powder and different structural anisotropy. Experimental data on magnetic properties are accomplished by microstructural observations performed using X-Ray tomography. Influence of the particles amount and structuring effects on the initial magnetic susceptibility of the composites as well as the applicability of the Maxwell-Garnett approximation, which is widely used in considerations of magnetopolymer elastic composites, are evaluated. It is demonstrated that the approximation works well for diluted samples containing randomly distributed magnetic particles and for the diluted samples with chain-like structures oriented perpendicular to an externally applied field, while it fails to predict the susceptibility of the samples with structures oriented parallel to the field. Moreover, it is shown, that variation of the chains morphology does not significantly change the composite initial magnetic susceptibility. - Highlights: • The Maxwell-Garnet prediction works well for the diluted isotropic composites. • The Maxwell-Garnet prediction can be used for composites with structures oriented perpendicular to an applied field. • Chains oriented parallel to an applied field significantly increase the composite initial magnetic susceptibility. • The number and thickness of chains is not of the highest importance for the diluted composites. • The crucial reason of the observed effect is expected to be the demagnetisation factor of the chains.

Antifungal activity evaluation of Aloe arborescens dry extract against trichosporon genus yeasts

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João Ricardo Bueno de Morais Borba

2014-10-01

Full Text Available The objective of this study was to investigate the antifungal activity of Aloe arborescens dry extract against Trichosporon genus yeast species. Extraction was carried out by means of a longitudinal incision in fresh leaves, which were collected on a vat, and the total volume was frozen and subsequently lyophilized. Then, 40 mg of the dry extract was dissolved in DMSO by gentle inversion in order to obtain a solution whose concentration was 4000 µg mL-1. This solution became limpid and slightly yellowish because the pigment of the latex was attenuated. It was performed serial dilutions from 2,000 to 15.625 µg mL-1 with RPMI-1640 broth. There was already no pigment in the first dilution of 2000 μg mL-1. It was analyzed fifteen strains of Trichosporon spp., and Candida albicans ATCC 10231 was used as control strain. We carried out the reading of microplates in the ELISA reader device at a wavelength of 530 nm, after incubation for 24 and 48 hours, and it was determinated the Minimum Inhibitory Concentration (MIC. The MIC50 value obtained for all Trichosporon species and for C. albicans was 500 µg mL-1. As a result, we concluded that Aloe arborescens dry extract has antifungal activity against Trichosporon yeasts.

Dilution physics modeling: Dissolution/precipitation chemistry

International Nuclear Information System (INIS)

Onishi, Y.; Reid, H.C.; Trent, D.S.

1995-09-01

This report documents progress made to date on integrating dilution/precipitation chemistry and new physical models into the TEMPEST thermal-hydraulics computer code. Implementation of dissolution/precipitation chemistry models is necessary for predicting nonhomogeneous, time-dependent, physical/chemical behavior of tank wastes with and without a variety of possible engineered remediation and mitigation activities. Such behavior includes chemical reactions, gas retention, solids resuspension, solids dissolution and generation, solids settling/rising, and convective motion of physical and chemical species. Thus this model development is important from the standpoint of predicting the consequences of various engineered activities, such as mitigation by dilution, retrieval, or pretreatment, that can affect safe operations. The integration of a dissolution/precipitation chemistry module allows the various phase species concentrations to enter into the physical calculations that affect the TEMPEST hydrodynamic flow calculations. The yield strength model of non-Newtonian sludge correlates yield to a power function of solids concentration. Likewise, shear stress is concentration-dependent, and the dissolution/precipitation chemistry calculations develop the species concentration evolution that produces fluid flow resistance changes. Dilution of waste with pure water, molar concentrations of sodium hydroxide, and other chemical streams can be analyzed for the reactive species changes and hydrodynamic flow characteristics

Activity coefficients at infinite dilution and physicochemical properties for organic solutes and water in the ionic liquid 4-(2-methoxyethyl)-4-methylmorpholinium trifluorotris(perfluoroethyl)phosphate

International Nuclear Information System (INIS)

Wlazło, Michał; Marciniak, Andrzej

2012-01-01

Highlights: ► The γ 13 ∞ and K L for 62 solutes in the IL [COC 2 mMOR][FAP] were determined by IGC. ► Partial molar excess thermodynamic functions at infinite dilution were calculated. ► The selectivities and capacities for selected separation problems were calculated. ► LFER system constants as a function of T for [COC 2 mMOR][FAP] were calculated. - Abstract: This paper presents new data on activity coefficients at infinite dilution, γ ∞ for 62 different solutes: alkanes, alkenes, alkynes, cycloalkanes, aromatic hydrocarbons, alcohols, thiophene, ethers, ketones, and water in the ionic liquid 4-(2-methoxyethyl)-4-methylmorpholinium trifluorotris(perfluoroethyl)phosphate, [COC 2 mMOR][FAP]. The data were determined by inverse gas chromatography at six temperatures from T = 318.15 K to T = 368.15 K. These values were compared with ionic liquid based on the same cation and bis(trifluoromethylsulfonyl)-amide anion, [COC 2 mMOR][NTf 2 ]. Additionally the partial molar excess Gibbs free energies ΔG 1 E,∞ , enthalpies ΔH 1 E,∞ , and entropies ΔS 1 E,∞ at infinite dilution were calculated from the experimental γ ∞ values obtained over the temperatures range. The selectivities and capacities at infinite dilution for hexane/benzene, cyclohexane/benzene, and heptane/thiophene extraction problems were calculated from the γ ∞ to verify the possibility of investigated ionic liquid as an entrainer in liquid–liquid extraction and desulphurization of fuels. Obtained values were compared with literature data of other ionic liquids based on trifluorotris(perfluoroethyl)phosphate and bis(trifluoromethylsulfonyl)-amide anions and industrial solvents: NMP and sulfolane. Also the Abraham solvation parameter model was used for evaluation of the solvation characteristic of the ionic liquid. Linear free energy relationship (LFER) system constants as a function of temperature were calculated.

Analysis of the servo-spill control for slow beam extraction

International Nuclear Information System (INIS)

Sato, Hikaru; Toyama, Takeshi; Marutsuka, Katsumi; Shirakata, Masashi.

1994-01-01

This report describes an analysis of servo-spill control system for the slow beam extraction from the KEK PS. Transfer function of extraction process is derived from measurement of the closed-loop characteristic using measured frequency response of each equipment. Result indicates the restriction of the present servo-spill control and give a guide line for the improvement. (author)

Solvent extraction of rare earth nitrates by Versatic Acid 911

Energy Technology Data Exchange (ETDEWEB)

Kazuoka, K; Tanabe, T; Kondo, Y [Kyoto Univ. (Japan)

1975-07-01

The extraction equilibria of cerous, terbium and yttrium nitrates into Versatic Acid 911 were studied. The organic phase was diluted with benzene, and the ionic strength of the aqueous solutions was maintained at unity by adding NaNO/sub 3/. Radioactive isotopes of these elements were used as the tracer. The compositions of the extracted species were CeR/sub 3/.4RH.H/sub 2/O, TbR/sub 3/.4RH.H/sub 2/O and YR/sub 3/.4RH.H/sub 2/o, and the apparent equilibrium constants of extraction were 9.14x10/sup -15/, 3.90x10/sup -14/ and 1.70x10/sup -14/, respectively.

Enhancement of surface magnetism due to bulk bond dilution

International Nuclear Information System (INIS)

Tsallis, C.; Sarmento, E.F.; Albuquerque, E.L. de

1985-01-01

Within a renormalization group scheme, the phase diagram of a semi-infinite simple cubic Ising ferromagnet is discussed, with arbitrary surface and bulk coupling constants, and including possible dilution of the bulk bonds. It is obtained that dilution makes easier the appearance of surface magnetism in the absence of bulk magnetism. (Author) [pt

Gas-liquid chromatography measurements of activity coefficients at infinite dilution of various organic solutes and water in tri-iso-butylmethylphosphonium tosylate ionic liquid

International Nuclear Information System (INIS)

Domanska, Urszula; Paduszynski, Kamil

2010-01-01

Activity coefficients at infinite dilution (γ 13 ∞ ) of 33 different solutes (including alkanes, cycloalkanes, alkenes, alkynes, benzene, alkylbenzenes, water, alcohols, MTBE, thiophene and THF) in the ionic liquid tri-iso-butylmethylphosphonium tosylate have been determined by using the GLC method and have been reported over the temperature range (298.15 to 368.15) K. The partial molar excess enthalpies of mixing at infinite dilution have been determined based on temperature dependence of γ 13 ∞ . Selectivity and capacity at infinite dilution has been also calculated for exemplary separation processes in systems n-hexane/benzene and n-hexane/thiophene, to evaluate if the studied ionic liquid is capable to be a good entrainer for these processes, e.g. in the liquid-liquid extraction. The obtained results are promising however the ionic liquid studied shows a lower selectivity than some of imidazolium-based ionic liquids. To our best knowledge, the results indicate that tri-iso-butylmethylphosphonium tosylate is the best for the separation problem of aliphatic hydrocarbons from aromatic hydrocarbons among all of the studied quaternary phosphonium-based ionic liquids.

Phase diagrams of site diluted ferromagnetic thin film

International Nuclear Information System (INIS)

Hamedoun, M.; Bouslykhane, K.; Bakrim, H.; Hourmatallah, A.; Benzakour, N.; Masrour, R.

2006-01-01

The phase transition properties of Ising, classical XY and Heisenberg of diluted ferromagnetic thin film are studied by the method of exact high-temperature series expansions extrapolated with the Pade approximants method. The reduced critical temperature τ c of the diluted ferromagnetic thin films is studied as a function of film thickness L and the exchange interactions in the bulk J b , in the surface J s and between surface and nearest-neighbour layer J - bar . It is found that τ c increases with the exchange interactions of surface and L. The magnetic phase diagram (τ c versus dilution x) is obtained. A critical value of the surface exchange interaction above which the surface magnetism appears is obtained. The dependence of the critical parameter of surface reduced coupling R 2 c as a function of the dilution x and the ratio of the exchange interaction between the surface and nearest-neighbour layer to the bulk one R 1 for the three studied models has been investigated. The percolation threshold is defined as the concentration x p at which τ c =0. The obtained values are x p ∼0.2 in the bulk and x p ∼0.4 at the surface

Supercritical Fluid Extraction of Quinones from Compost for Microbial Community Analysis

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Ni Luh Gede Ratna Juliasih

2015-01-01

Full Text Available Supercritical fluid extraction (SFE was used to extract quinones from compost to monitor the microbial community dynamics during composting. The 0.3 g of dried compost was extracted using 3 mL min−1 of carbon dioxide (90% and methanol (10% at 45°C and 25 MPa for a 30 min extraction time. The extracted quinones were analysed using ultra performance liquid chromatography (UPLC with 0.3 mL min−1 of methanol mobile phase for a 50 min chromatographic run time. A comparable detected amount of quinones was obtained using the developed method and an organic solvent extraction method, being 36.06 μmol kg−1 and 34.54 μmol kg−1, respectively. Significantly low value of dissimilarity index (D between the two methods (0.05 indicated that the quinone profile obtained by both methods was considered identical. The developed method was then applied to determine the maturity of the compost by monitoring the change of quinone during composting. The UQ-9 and MK-7 were predominant quinones in the initial stage of composting. The diversity of quinone became more complex during the cooling and maturation stages. This study showed that SFE had successfully extracted quinones from a complex matrix with simplification and rapidity of the analysis that is beneficial for routine analysis.

Different approaches to analyze the dipolar interaction effects on diluted and concentrated granular superparamagnetic systems

Energy Technology Data Exchange (ETDEWEB)

Moscoso-Londoño, O., E-mail: omoscoso@ifi.unicamp.br [Instituto de Física ‘Gleb Wataghin’, Universidade Estadual de Campinas (UNICAMP), CEP13083-859 Campinas, São Paulo (Brazil); Tancredi, P. [Laboratorio de Sólidos Amorfos, INTECIN, Facultad de Ingeniería, Universidad de Buenos Aires (UBA), CONICET, C1063ACV Buenos Aires (Argentina); Muraca, D. [Instituto de Física ‘Gleb Wataghin’, Universidade Estadual de Campinas (UNICAMP), CEP13083-859 Campinas, São Paulo (Brazil); Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC (UFABC), Av. Dos Estados, 5001, Santo André, SP (Brazil); Mendoza Zélis, P.; Coral, D.; Fernández van Raap, M.B. [Instituto de Física, Universidad Nacional de La Plata (UNLP), CONICET, CC.67, 1900 La Plata, Buenos Aires (Argentina); Wolff, U.; Neu, V.; Damm, C. [IFW Dresden, Leibniz Institute for Solid State and Materials Research, Dresden, Helmholtzstrasse 20, 01069 Dresden (Germany); Oliveira, C.L.P. de [Instituto de Física, Universidade de São Paulo, São Paulo 05314970 (Brazil); Pirota, K.R. [Instituto de Física ‘Gleb Wataghin’, Universidade Estadual de Campinas (UNICAMP), CEP13083-859 Campinas, São Paulo (Brazil); and others

2017-04-15

Controlled magnetic granular materials with different concentrations of magnetite nanoparticles immersed in a non-conducting polymer matrix were synthesized and, their macroscopic magnetic observables analyzed in order to advance towards a better understanding of the magnetic dipolar interactions and its effects on the obtained magnetic parameters. First, by means of X-ray diffraction, transmission electron microscopy, small angle X-ray scattering and X-ray absorption fine structure an accurate study of the structural properties was carried out. Then, the magnetic properties were analyzed by means of different models, including those that consider the magnetic interactions through long-range dipolar forces as: the Interacting Superparamagnetic Model (ISP) and the Vogel-Fulcher law (V-F). In systems with larger nanoparticle concentrations, magnetic results clearly indicate that the role played by the dipolar interactions affects the magnetic properties, giving rise to obtaining magnetic and structural parameters without physical meaning. Magnetic parameters as the effective anisotropic constant, magnetic moment relaxation time and mean blocking temperature, extracted from the application of the ISP model and V-F Law, were used to simulate the zero-field-cooling (ZFC) and field-cooling curves (FC). A comparative analysis of the simulated, fitted and experimental ZFC/FC curves suggests that the current models depict indeed our dilute granular systems. Notwithstanding, for concentrated samples, the ISP model infers that clustered nanoparticles are being interpreted as single entities of larger magnetic moment and volume, effect that is apparently related to a collective and complex magnetic moment dynamics within the cluster. - Highlights: • Nanoparticle architecture into matrices determines the composite magnetic response. • Magnetically diluted or compacted systems are useful to study magnetism at nanoscale. • Particle aggregation into the matrices was examined

Supercritical extraction of oleaginous: parametric sensitivity analysis

Directory of Open Access Journals (Sweden)

Santos M.M.

2000-01-01

Full Text Available The economy has become universal and competitive, thus the industries of vegetable oil extraction must advance in the sense of minimising production costs and, at the same time, generating products that obey more rigorous patterns of quality, including solutions that do not damage the environment. The conventional oilseed processing uses hexane as solvent. However, this solvent is toxic and highly flammable. Thus the search of substitutes for hexane in oleaginous extraction process has increased in the last years. The supercritical carbon dioxide is a potential substitute for hexane, but it is necessary more detailed studies to understand the phenomena taking place in such process. Thus, in this work a diffusive model for semi-continuous (batch for the solids and continuous for the solvent isothermal and isobaric extraction process using supercritical carbon dioxide is presented and submitted to a parametric sensitivity analysis by means of a factorial design in two levels. The model parameters were disturbed and their main effects analysed, so that it is possible to propose strategies for high performance operation.

A Study on the Stability of Diluted Bee Venom Solution

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Mi-Suk Kang

2003-06-01

Full Text Available Objective : The purpose of this study was to investigate the stability of bee venom according to the keeping method and period. Method : The author observed microbial contamination of bee venom in nutrient agar, broth, YPD agar and YPD media and antibacterial activity for S. aureus, E. coli manufactured 12, 6 and 3 months ago as the two type of room temperature and 4℃ cold storage. Result : 1. 1:3,000 and 1:4,000 diluted bee venom solution did not show microbial contamination both room temperature and cold storage within twelve months. 2. There was antibacterial activity of diluted bee venom for S. aureus in cold storage within twelve months and there was no antibacterial activity of diluted bee venom for S. aureus in twelve months, room temperature storage. 3. We could not observe the zone of inhibition around paper disc of all for E.coli. in 1:3,000, 1:30,000 and 1:3,000,000 diluted bee venom solution, respectively. According to results, we expect that diluted bee venom solution is stable both cold and room temperature storage within twelve months.

Impact of dilution on the microstructure and properties of Ni-based 625 alloy coatings

Directory of Open Access Journals (Sweden)

Tiago Jose Antoszczyszyn

2014-06-01

Full Text Available Nickel-based alloy IN 625 is used to protect components of aircrafts, power generation and oil refinery due to an association of toughness and high corrosion resistance. These properties are associated with the chemical composition and microstructure of coatings which depend on the processing parameters and the composition of the component being protected. This paper assessed impact of dilution on the microstructure and properties of the Ni alloy IN 625 deposited by Plasma Transferred Arc (PTA on two substrates: carbon steel API 5L and stainless steel AISI 316L. Differences due to the interaction with the substrate were maximized analyzing single layer coatings, processed with three deposition current: 120, 150 and 180 A. Correlation with a cast Nickel-based alloy sample contributed to assess the impact of dilution on coatings. Dilution was determined by the area ratio and Vickers hardness measured on the transverse section of coatings. Scanning electron and Laser confocal microscopy and X-ray diffraction analysis were carried out to characterize the microstructure. Results indicated the increasing dilution with the deposition current was deeply influenced by the substrate. Dilution ranging from 5 to 29% was measured on coatings processed on the API 5L steel and from 22 to 51% on the low thermal conductivity AISI 316L steel substrate. Differences on the microstructure and properties of coatings can be associated with the interaction with each substrate. Higher fraction of carbides account for the higher coating hardness when processing on API 5L whereas the low thermal conductivity of AISI 316L and the higher Fe content in solid solution contributed to the lower hardness of coatings.

Calorimetric approach of lanthanides (3) complexation and extraction by malonamides; Approche calorimetrique de la complexation et de l'extraction des lanthanides (3) par les malonamides

Energy Technology Data Exchange (ETDEWEB)

Flandin, J.L

2001-07-01

In the field of long lived radionuclides separation, diamides are interesting extractants because of their ability to co-extract trivalent lanthanides and actinides, which is a preliminary and essential step in high level radioactive waste reprocessing. The research carried out contributes to a better understanding of the mechanisms and the aim is the determination of thermodynamics properties ({delta}{sub r}G, {delta}{sub r}H et {delta}{sub r}S) related to the complexation and the extraction of lanthanides(III) by malonamides. The first part of the document deals with the complexation of lanthanides(III) by an hydrosoluble diamide. The experimental results obtained by UV-visible spectrometry, TRLIF, NMR and microcalorimetric titration proved that lanthanides(III)-TEMA interactions in aqueous medium are very weak and that the complexation reaction is endothermic. The TEMA ligand still stays in the second coordination sphere of coordination of the lanthanide ion. The second part of this study focuses on the extraction of neodymium(III) nitrate by a lipophilic diamide which is an exothermic reaction. The influence of the composition of aqueous and organic phases on the thermodynamics properties {delta}{sub r}G et {delta}{sub r}H has been studied by microcalorimetric titration. The most influent parameter is the total concentration in extractant. As a consequence, thermodynamic values are very dependent on the organic phase organisation before and alter extraction. At the same time, this study showed the interest of the calorimetric approach for the analysis of basic reactions like diamide dilution and their organisation as oligomeric aggregates. (author)

Alkaline Extraction of DNA from Pathogenic Fungi for PCR-RFLP Analysis

OpenAIRE

Matsumoto, Masaru; Mishima, Shinobu; Matsuyama, Nobuaki; 松元, 賢; 松山, 宣明

1997-01-01

For the preparation of DNA samples from fungal mycelia alkaline extraction method was applied and assessed its usefulness for PCR-RFLP analysis. Using alkaline treatment protocols, 18S ribosomal DNAs (rDNA) derived from fungal genomic DNA of Pyricularia oryzae, P. zingiberi, Rhizoctonia solani and R. oryzae were PCR-amplified and digested with Hha I, Msp I and Hae ill. RFLP analysis with HhaI showed the divergent polymorphism between genus Pyricularia and Rhizoctonia. The alkaline DNA extract...

Development of rapid and simple method for DNA extraction from cannabis resin based on the evaluation of relative PCR amplification ability.

Science.gov (United States)

Yamamuro, Tadashi; Iwata, Yuko T; Segawa, Hiroki; Kuwayama, Kenji; Tsujikawa, Kenji; Kanamori, Tatsuyuki; Inoue, Hiroyuki

2018-04-04

In recent years, analysis of cannabis DNA has been increasingly used in forensic drug tests. However, in the case of cannabis resin, a processed marijuana product, complicated procedures are required for the extraction of clean DNA, as the presence of various impurities inhibits PCR amplification. Therefore, in this study, we attempted to identify the factors that would allow quick and simple DNA extraction from cannabis resin with a commercially available kit. We also constructed a simple assay system for comparing relative amplification efficiencies by end-point PCR and used it to evaluate the purity of the obtained DNA solutions. For extraction with a kit that contains a silica column, reducing the starting amount of resin, using the residue remaining after methanol extraction, dilution of the final solution, extraction with an equal amount of powdered activated carbon or an excess amount of polyvinylpolypyrrolidone, and the addition of an appropriate amount of polyvinylpyrrolidone to the solution after extraction were effective measures that improved amplification efficiency. Furthermore, the use of the most rapid alkaline extraction kit combined with the addition of powdered activated carbon allowed obtaining DNA solutions with sufficient amplification efficiency in about 10min. These findings should be useful for routine DNA analysis of cannabis resin during forensic examination. Copyright © 2018 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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

2018-04-01

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

Molecularly imprinted solid-phase extraction in the analysis of agrochemicals.

Science.gov (United States)

Yi, Ling-Xiao; Fang, Rou; Chen, Guan-Hua

2013-08-01

The molecular imprinting technique is a highly predeterminative recognition technology. Molecularly imprinted polymers (MIPs) can be applied to the cleanup and preconcentration of analytes as the selective adsorbent of solid-phase extraction (SPE). In recent years, a new type of SPE has formed, molecularly imprinted polymer solid-phase extraction (MISPE), and has been widely applied to the extraction of agrochemicals. In this review, the mechanism of the molecular imprinting technique and the methodology of MIP preparations are explained. The extraction modes of MISPE, including offline and online, are discussed, and the applications of MISPE in the analysis of agrochemicals such as herbicides, fungicides and insecticides are summarized. It is concluded that MISPE is a powerful tool to selectively isolate agrochemicals from real samples with higher extraction and cleanup efficiency than commercial SPE and that it has great potential for broad applications.