Uranium extraction from sulfuric acid solution using anion exchange resin

International Nuclear Information System (INIS)

Sheta, M. E.; Abdel Aal, M. M.; Kandil, A. T.

2012-12-01

Uranium is currently recovered from sulfuric acid leach liquor using anion exchange resin as Amberlite IRA 402 (CT). This technology is based on fact that, uranium exists as anionic complexes. This takes place by controlling the pH of the solution, agitation time, temperature and resin to solution ratio (R/S). In this work, batch stirrer tank used for uranium extraction from sulfate medium and after extraction, elution process was done using 1M NaCl solution. After extraction and elution process, the resin was separated from the system and uranium was determined in the solution. (Author)

The kinetics of fossil resin extraction from a flotation concentrate

Energy Technology Data Exchange (ETDEWEB)

Li, L.; Yu, Q.; Miller, J.D. [Univ. of Utah, Salt Lake City, UT (United States)

1995-11-01

The kinetics of fossil resin extraction from a flotation concentrate by heptane were investigated as a function of process variables using monosize particles. Experimental results provide for a better understanding of the refining process and the basis for subsequent design and construction of a continuous resin refining circuit. Based on the effect of process variables (particle size, stirring speed, and temperature) the resin extraction rate appears to be controlled by surface solvation phenomena. The initial extraction rate was found to be inversely proportional to the initial particle size and a kinetic model is being developed to describe the experimental results.

Investigation of special resins for the extraction-chromatogaphic separation of Np and Pu from the process stream of a reprocessing plant for HTR fuel elements

Energy Technology Data Exchange (ETDEWEB)

Ritter, G

1977-03-15

The effectiveness of several special resins for extraction chromatographic separation of plutonium and neptunium from the process streams of a reprocessing plant was investigated. These special resins consisted of polystyrol and were loaded with Tri-n-octylamine (TOA) during the polymerization process. A commercial structural body of polytrifluormonochlorethylene (Voltalef), subsequently wetted with TOA, served as reference material. Despite its good separation characteristics, this separation body has considerable disadvantages. The individual particles of separation body are only approximately spherical, the homogeneity of the separation bed is consequently only moderate. This size (85% less than 0.062 mm) and the shape of the separation body particles cause high pressure loss in the solution which streams through. Filling the column with the Voltalef separation body is very complicated and often not reproducible. A relatively high elution rate of the stationary phase and low radiation resistance are other disadvantages of this separation body. Because of the unfavorable characteristics of the Voltalef separation body, the above mentioned polystyrol resins have been developed by the Bayer firm. The individual separation body particles of these resins have ideal spherical shape. The diameter of the spheres is 0.4 to 0.6 mm, causing only slight pressure losses in a chromatographic column. A homogeneous and compact column fill is much simpler to achieve with these resins than with Voltalef. Radiation resistance and elution rate of the polystyrol resins correspond to the expectations which must be met during hot operation. The separation characteristics of the investigated polystyrol resins are not optimum, however. The relatively large separation body particles considerably delay the establishment of equilibrium, for two reasons. The rate-determining step during loading is diffusion through an aqueous film, which surrounds the separation body particles.

Long term stability of cannabis resin and cannabis extracts

DEFF Research Database (Denmark)

Lindholst, Christian

2010-01-01

  The aim of the present study was to investigate the stability of cannabinoids in cannabis resin slabs and cannabis extracts upon long-term storage. The levels of tetrahydrocannabinol (THC), cannabinol (CBN), cannabidiol (CBD) and cannabigerol (CBG) on both neutral and acidic form were measured...... stored in extracted form at room temperature the degradation rate of acidic THC increased significantly relative to resin material with concentration halve-lives of 35 and 91 days in daylight and darkness, respectively. Once cannabis material is extracted into organic solvents, care should be taken...

Use of laminar chromatographic methods for determination of separation conditions in column extraction chromatography

International Nuclear Information System (INIS)

Ghersini, G.; Cerrai, E.

1978-01-01

Possibilities of using laminar chromatographic methods (paper and thin-layer chromatography) to determine optimal separation conditions in column extraction chromatography are analysed. Most of the given laminar methods are presented as Rf-spectra, i.e. as dependences of Rf found experimentally on eluating solution component concentration. Interrelation between Rf and distribution coefficients of corresponding liquid extraction systems and retention volumes of chromatographic columns is considered. Literature data on extraction paper and thin-layer chromatography of elements with various immovable phases are presented

[Corrected Title: Solid-Phase Extraction of Polar Compounds from Water] Automated Electrostatics Environmental Chamber

Science.gov (United States)

Sauer, Richard; Rutz, Jeffrey; Schultz, John

2005-01-01

A solid-phase extraction (SPE) process has been developed for removing alcohols, carboxylic acids, aldehydes, ketones, amines, and other polar organic compounds from water. This process can be either a subprocess of a water-reclamation process or a means of extracting organic compounds from water samples for gas-chromatographic analysis. This SPE process is an attractive alternative to an Environmental Protection Administration liquid-liquid extraction process that generates some pollution and does not work in a microgravitational environment. In this SPE process, one forces a water sample through a resin bed by use of positive pressure on the upstream side and/or suction on the downstream side, thereby causing organic compounds from the water to be adsorbed onto the resin. If gas-chromatographic analysis is to be done, the resin is dried by use of a suitable gas, then the adsorbed compounds are extracted from the resin by use of a solvent. Unlike the liquid-liquid process, the SPE process works in both microgravity and Earth gravity. In comparison with the liquid-liquid process, the SPE process is more efficient, extracts a wider range of organic compounds, generates less pollution, and costs less.

Industrial scale chromatographic separation of valuable compounds from biomass hydrolysates and side streams

Energy Technology Data Exchange (ETDEWEB)

Saari, P.

2011-06-15

Carbohydrates are composed of a number of various monosaccharides, glucose being the most abundant. Some of the monosaccharides are valuable compounds used in the food and pharmaceutical industries. They can be separated from biomass hydrolysates e.g. by chromatographic methods. In this thesis, chromatographic separation of valuable compounds using ion exchange resins was studied on an industrial scale. Of special interest were rare monosaccharides in biomass hydrolysates. A novel chromatographic separation process was developed for fucose, starting from pre-processed spent sulfite liquor. The core of the process consists of three chromatographic separations with different types of ion exchange resins. Chromatographic separation of galactose was tested with three biomass hydrolysates; lactose, gum arabic and hemicellulose hydrolysates. It was demonstrated that also galactose can be separated from complex carbohydrate mixtures. A recovery process for arabinose from citrus pectin liquid residual and for mannose from wood pulp hydrolysate were also developed and experimentally verified. In addition to monosaccharides, chromatographic separation of glycinebetaine from vinasse was examined with a hydrogen form weak acid cation exchange resin. The separation involves untypical peak formation depending, for example, on the pH and the cation composition. The retention mechanism was found to be hydrogen bonding between glycinebetaine and the resin. In the experimental part, all four resin types - strong acid cation, strong base anion, weak acid cation and weak base anion exchange resins - were used. In addition, adsorption equilibria data of seven monosaccharides and sucrose were measured with the resins in sodium and sulfate forms because such data have been lacking. It was found out that the isotherms of all sugars were linear under industrial conditions. A systematic method for conceptual process design and sequencing of chromatographic separation steps were developed

Extraction of high quality DNA from seized Moroccan cannabis resin (Hashish.

Directory of Open Access Journals (Sweden)

Moulay Abdelaziz El Alaoui

Full Text Available The extraction and purification of nucleic acids is the first step in most molecular biology analysis techniques. The objective of this work is to obtain highly purified nucleic acids derived from Cannabis sativa resin seizure in order to conduct a DNA typing method for the individualization of cannabis resin samples. To obtain highly purified nucleic acids from cannabis resin (Hashish free from contaminants that cause inhibition of PCR reaction, we have tested two protocols: the CTAB protocol of Wagner and a CTAB protocol described by Somma (2004 adapted for difficult matrix. We obtained high quality genomic DNA from 8 cannabis resin seizures using the adapted protocol. DNA extracted by the Wagner CTAB protocol failed to give polymerase chain reaction (PCR amplification of tetrahydrocannabinolic acid (THCA synthase coding gene. However, the extracted DNA by the second protocol permits amplification of THCA synthase coding gene using different sets of primers as assessed by PCR. We describe here for the first time the possibility of DNA extraction from (Hashish resin derived from Cannabis sativa. This allows the use of DNA molecular tests under special forensic circumstances.

Extraction chromatographic method for the separation of actinides and lanthanides using EDHBA grafted AXAD-16 polymer

Energy Technology Data Exchange (ETDEWEB)

Akhila Maheswari, M.; Subramanian, M.S. [Department of Chemistry, Indian Institute of Technology, Chennai (India)

2005-02-15

A new extraction chromatographic method has been developed by grafting chloromethylated polymer support with 4-ethoxy-N,N-dihexylbutanamide (EDHBA), for the selective extraction of U(VI), Th(IV), La(III) and Nd(III) from highly acidic matrices. The developed grafted polymer has been characterized using {sup 13}C-CPMAS NMR spectroscopy, FT-NIR spectroscopy and also by CHN elemental analysis. The water regaining capacity of the grafted polymer is studied by TGA measurements and the active participation of the amide moiety towards metal ion complexation has been confirmed by Far IR spectroscopy. For the quantitative extraction of metal ions to the resin phase, various physico-chemical parameters are optimized by both static and dynamic methods. The developed amide grafted polymeric matrix shows good distribution ratio values even at high acidities, with the maximum metal sorption capacity values being 0.36, 0.69, 0.32 and 0.42mmolg{sup -1} for U(VI), Th(IV), La(III) and Nd(III), respectively, at 6M HNO{sub 3} medium. The kinetics of metal ion phase equilibration is found to be moderately fast, with t{sub 1/2} values of <6min, for all the analytes of interest. The limits of analyte quantification (LOQ) using the developed method are in the range of 15-30{mu}gL{sup -1}. Moreover, the sequential separation of the sorbed actinides and lanthanides could be achieved by first eluting with 100mL of distilled water (for actinides) followed by elution with 20mL of 0.1M EDTA (for lanthanides). The selectivity behavior and the practical applicability of the developed resin are tested using synthetic low level nuclear reprocessing mixtures and also with monazite sand. The analytical data are within 3.8% relative standard deviation, reflecting the reproducibility and reliability of the developed method.

Ionic-liquid-impregnated resin for the microwave-assisted solid-liquid extraction of triazine herbicides in honey.

Science.gov (United States)

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

2015-09-01

Microwave-assisted ionic-liquid-impregnated resin solid-liquid extraction was developed for the extraction of triazine herbicides, including cyanazine, metribuzin, desmetryn, secbumeton, terbumeton, terbuthylazine, dimethametryn, and dipropetryn in honey samples. The ionic-liquid-impregnated resin was prepared by immobilizing 1-hexyl-3-methylimidazolium hexafluorophosphate in the microspores of resin. The resin was used as the extraction adsorbent. The extraction and enrichment of analytes were performed in a single step. The extraction time can be shortened greatly with the help of microwave. The effects of experimental parameters including type of resin, type of ionic liquid, mass ratio of resin to ionic liquid, extraction time, amount of the impregnated resin, extraction temperature, salt concentration, and desorption conditions on the extraction efficiency, were investigated. A Box-Behnken design was applied to the selection of the experimental parameters. The recoveries were in the range of 80.1 to 103.4% and the relative standard deviations were lower than 6.8%. The present method was applied to the analysis of honey samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chiral separation of amino-alcohols using extractant impregnated resins

NARCIS (Netherlands)

Babic, K.; Driessen, G.H.M.; van der Ham, Aloysius G.J.; de Haan, A.B.

2007-01-01

The performance of extractant impregnated resin (EIR) technology for chiral separation of amino-alcohols has been investigated. Phenylglycinol was selected as an archetype model enantiomer and azophenolic crown ether was used as a versatile enantioselective extractant. 1-Phenyloctane was selected as

Bead Injection Extraction Chromatography using High-capacity Lab-on-Valve as a Front End to Inductively Coupled Plasma Mass Spectrometry for Rapid Urine Radiobioassay

DEFF Research Database (Denmark)

Qiao, Jixin; Hou, Xiaolin; Roos, Per

2013-01-01

A novel bead injection (BI) extraction chromatographic microflow system exploiting high-capacity lab-on-valve (LOV) platform coupled with inductively coupled plasma mass spectrometric detection is developed for rapid and automated determination of plutonium in human urine. A microconduit (1 m......L) incorporated within the LOV processing unit is loaded on-line with a metered amount of disposable extraction chromatographic resin (up to 330 mg of TEVA) through programmable beads transport. Selective capture and purification of plutonium onto the resin beads is then performed by pressure driven flow after...

Acute and sub-acute oral toxicity of Dracaena cinnabari resin methanol extract in rats.

Science.gov (United States)

Al-Afifi, Nashwan Abdullah; Alabsi, Aied Mohammed; Bakri, Marina Mohd; Ramanathan, Anand

2018-02-05

Dracaena cinnabari (DC) is a perennial tree that located on the Southern coast of Yemen native to the Socotra Island. This tree produces a deep red resin known as the Dragon's blood, the Twobrother's Blood or Damm Alakhwain. The current study performed to evaluate the safety of the DC resin methanol extract after a single or 28 consecutive daily oral administrations. In assessing the safety of DC resin methanol extract, acute and sub-acute oral toxicity tests performed following OECD guidelines 423 and 407, respectively, with slight modifications. In acute oral toxicity test, DC resin methanol extract administered to female Sprague Dawley rats by oral gavage at a single dose of 300 and 2000 mg/kg body weight. Rats observed for toxic signs for 14 days. In sub-acute oral toxicity test, DC resin methanol extract administered to the rats by oral gavage at 500, 1000, and 1500 mg/kg body weight daily up to 28 days to male and female Spradgue Dawley rats. The control and high dose in satellite groups were also maintained and handled as the previous groups to determine the late onset toxicity of DC resin methanol extract. At the end of each test, hematological and biochemical analysis of the collected blood were performed as well as gross and microscopic pathology. In acute oral toxicity, no treatment-related death or toxic signs were observed. It revealed that the DC resin methanol extract could be well tolerated up to the dose 2000 mg/kg body weight and could be classified as Category 5. The sub-acute test observations indicated that there are no treatment-related changes up to the high dose level compared to the control. Food consumption, body weight, organ weight, hematological parameters, biochemical parameters and histopathological examination (liver, kidney, heart, spleen and lung) revealed no abnormalities. Water intake was significantly higher in the DC resin methanol extract treated groups compared to the control. This study demonstrates tolerability of DC

Chronic swelling from entrapment of acrylic resin in a surgical extraction site

OpenAIRE

Weiting Ho; Pin-Chuang Lai; John D Walters

2010-01-01

When acrylic resin is inadvertently embedded in oral tissue, it can result in a pronounced chronic inflammatory response. This report describes a case in which temporary crown and bridge resin was forced into a surgical extraction site after the two adjacent teeth were prepared for a bridge immediately following extraction of a maxillary premolar. The patient experienced swelling at the extraction site over a ten month period despite treatment with antibiotics and anti-inflammatory drugs. Aft...

Homogenization-assisted cavitation hybrid rotation extraction and macroporous resin enrichment of dihydroquercetin from Larix gmelinii.

Science.gov (United States)

Xia, Yu; Wang, Yinhang; Li, Wei; Ma, Chunhui; Liu, Shouxin

2017-12-01

Cavitation hybrid rotation, which was and is still looked upon as an unavoidable nuisance in the flow systems, for extraction processing intensification of active chemical compounds from natural products. In this study, a homogenization-assisted cavitation hybrid rotation extraction method was applied to extract dihydroquercetin (DHQ) from larch (Larix gmelinii) wood root. The extraction parameters were optimized in single factor experiments with the DHQ extraction yields as the response values. The optimum conditions were as follows: number of extractions, three; ethanol volume fraction for the extraction, 60%; liquid-solid ratio for homogenization, 10mL/g; homogenization time, 8min; liquid-solid ratio for cavitation extraction, 9mL/g, and cavitation extraction time, 35min. Under these conditions, the DHQ content in extract was 4.50±0.02mg/g, and the extraction efficiency was higher than those of traditional techniques. Cavitation can be effectively used to improve the extraction rate by increasing the mass transfer rates and possible rupture of cell wall due to formation of microcavities leading to higher product yields with reduced processing time and solvent consumption. After the extraction process, macroporous resin column chromatography was used to concentrate and purify the DHQ. Three resins were selected from fifteen macroporous resins for further investigation of their performance. Among these resins, AB-8 resin exhibited relatively better adsorption capacities and desorption ratios for DHQ. The ethanol volume fraction of the solutions for sample loading and desorption, and flow rates for loading and desorption were optimized for the macroporous resin column chromatography. Copyright © 2017 Elsevier B.V. All rights reserved.

The development of 126Sn separation procedure by means of TBP resin

International Nuclear Information System (INIS)

Andris, Boris; Bena, Jozef

2016-01-01

Separation possibilities of 126 Sn with a new extraction-chromatographic material TBP Resin were studied. Suitable conditions for tin separation were determined in hydrochloric acid medium. 126 Sn was concentrated on TBP resin from 6 mol L -1 HCl and was eluted with 0.1 mol L -1 HCl. A purification step to remove 137 Cs with AMP-PAN column was necessary to obtain sufficiently purified samples which were directly measured with gamma spectrometry for 126 Sn activity. Separation of 126 Sn from a raw sludge sample was done according to proposed procedure, 126 Sn was detected and its activity was determined. (author)

The transverse strength of acrylic resin after Coleus amboinicus, Lour extract solution immersion

OpenAIRE

Rianti, Devi

2006-01-01

A laboratoric experimental study was conducted on the transverse strength of acrylic resin after Coleus amboinicus, Lour extract solution immersion. The aim of this study is to know the difference of acrylic resin transverse strengths caused by immersion time variations in a concentrate solution. The study was carried out on unpolished acrylic resin plates with 65 × 10 × 2,5 mm dimension; solution with 15% Coleus amboinicus, Lour extract, and 30, 60, 90 days immersion times to measure the tra...

Applications of extraction chromatography in the development of radionuclide generator systems for nuclear medicine

International Nuclear Information System (INIS)

Dietz, M.L.; Horwitz, E.P.

2000-01-01

Numerous methods have been described for the separation and purification of radionuclides for application in diagnostic and therapeutic nuclear medicine, among them ion exchange, solvent extraction, and various forms of chromatography. Although extraction chromatography has previously been shown to provide a means of performing a number of separations of potential use in radionuclide generator systems, the application of the technique to generator development has thus far been limited. Recent work directed at improved methods for the determination of radionuclides in biological and environmental samples has led to the development of a series of novel extraction chromatographic resins exhibiting enhanced metal ion retention from strongly acidic media and excellent selectivity, among them materials suitable for the isolation of 212 Bi, 90 Y, and 213 Bi. These resins, along with extraction chromatographic materials employing functionalized supports to improve their physical stability or metal ion retention properties, are shown to offer promise in the development of improved radionuclide generators

Extraction of Tc(VII) and Re(VII) on TRU resin

Energy Technology Data Exchange (ETDEWEB)

Guerin, Nicolas; Riopel, Remi; Kramer-Tremblay, Sheila [Canadian Nuclear Laboratories (CNL), Chalk River, ON (Canada). Radiobiology and Health Branch; De Silva, Nimal; Cornett, Jack [Ottawa Univ., ON (Canada). Dept. of Earth and Environmental Sciences; Dai, Xiongxin [China Institute for Radiation Protection, Beijing (China)

2017-06-01

TRU resin can be used to rapidly and selectively extract Tc(VII) and Re(VII). The retention capacity curves of Tc(VII) and Re(VII) for HNO{sub 3}, HCl, H{sub 2}SO{sub 4} and H{sub 3}PO{sub 4} solutions were studied and prepared. Tc(VII) and Re(VII) were simultaneously extracted in 2 M H{sub 2}SO{sub 4} and 1.5 M H{sub 3}PO{sub 4} and were effectively separated from Mo(VI) and Ru(III). Tc(VII) and Re(VII) remained strongly bonded to the resin even after washing using a large volume of 2 M H{sub 2}SO{sub 4} at a relatively high flow rate. Also, they were both completely eluted from the resin using 15 mL of near boiling water, an eluent directly compatible for ICP-MS instrument measurements.

Purification of bioactive phenolics from Phanerochaete chysosporium biomass extract on selected macroporous resins

Science.gov (United States)

Idris, Z. M.; Dzahir, M. I. H. M.; Jamal, P.; Barkat, A. A.; Xian, R. L. W.

2017-06-01

In this study, two different types of macroporous resins known as XAD-7HP and HP-20 were evaluated for the adsorption and desorption properties against bioactive phenolics extracted from Phanerochaete chrysosporium. From the previous static sorption studies, it was found that the adsorption capacity for both resins had has no significant difference. Then, the kinetic adsorption data were analyzed with both pseudo-first-order and pseudo-second-order equations and the later performed better. The adsorption isotherm data were fitted well by both Langmuir and Freundlich models. Meanwhile in desorption study, HP-20 and XAD-7HP gave 90.52% and 88.28% recoveries, respectively. Considering the desorption results of the macroporous resins, HP-20 and XAD-7HP were packed in chromatography column to further purify the phenolics. For dynamic adsorption, breakthrough capacity of HP-20 (0.522) was found to be higher than XAD-7HP (0.131). Different ethanol concentrations (30% to 50% (v/v)) were investigated at fixed flowrate (1 ml/min) on phenolics recovery from both types of resins. The highest recovery of bioactive phenolics was 94.3% using XAD-7HP resins at 50% (v/v) of ethanol. Only 77.1% of bioactive phenolics were recovered using HP-20 resin at the same experimental conditions. The purified extract subsequently was analyzed using HPLC. The results showed that three phenolics (gallic acid 3,4-dihydroxybenzoic acid and 4-hydroxybenzoic acid) were identified with higher concentrations as compared to non-purified extract. Finally, the purified extract was tested for scavenging activity against DPPH, and it showed that the activity increased significantly to 90.80% from 59.94% in non-purified extract.

Correlation of supercritical-fluid extraction recoveries with supercritical-fluid chromatographic retention data: A fundamental study

NARCIS (Netherlands)

Lou, X.W.; Janssen, J.G.M.; Cramers, C.A.M.G.

1995-01-01

The possibility of using supercritical-fluid chromatographic retention data for examining the effects of operational parameters, such as pressure and flow rate, on the extraction characteristics in supercritical-fluid extraction (SFE) was investigated. A model was derived for calculating the

The transverse strength of acrylic resin after Coleus amboinicus, Lour extract solution immersion

Directory of Open Access Journals (Sweden)

Devi Rianti

2006-12-01

Full Text Available A laboratoric experimental study was conducted on the transverse strength of acrylic resin after Coleus amboinicus, Lour extract solution immersion. The aim of this study is to know the difference of acrylic resin transverse strengths caused by immersion time variations in a concentrate solution. The study was carried out on unpolished acrylic resin plates with 65 × 10 × 2,5 mm dimension; solution with 15% Coleus amboinicus, Lour extract, and 30, 60, 90 days immersion times to measure the transverse strength and sterilized aquadest was used as control. Acrylic resin plates transverse strength was measured using Autograph AG-10 TE. The data was analyzed using One-Way Anova and LSD with 5% degree of significance. The result showed that longer immersion time will decrease the transverse strength of the acrylic resin plates. After 90 days immersion time, the transverse strength decrease is still above the recommended standard transverse strength.

The Use of TOC Reconciliation as a Means of Establishing the Degree to Which Chromatographic Screening of Plastic Material Extracts for Organic Extractables Is Complete.

Science.gov (United States)

Jenke, Dennis; Couch, Thomas R; Robinson, Sarah J; Volz, Trent J; Colton, Raymond H

2014-01-01

Extracts of plastic packaging, manufacturing, and delivery systems (or their materials of construction) are analyzed by chromatographic methods to establish the system's extractables profile. The testing strategy consists of multiple orthogonal chromatographic methods, for example, gas and liquid chromatography with multiple detection strategies. Although this orthogonal testing strategy is comprehensive, it is not necessarily complete and members of the extractables profile can elude detection and/or accurate identification/quantification. Because the chromatographic methods rarely indicate that some extractables have been missed, another means of assessing the completeness of the profiling activity must be established. If the extracts are aqueous and contain no organic additives (e.g., pH buffers), then they can be analyzed for their total organic carbon content (TOC). Additionally, the TOC of an extract can be calculated based on the extractables revealed by the screening analyses. The measured and calculated TOC can be reconciled to establish the completeness and accuracy of the extractables profile. If the reconciliation is poor, then the profile is either incomplete or inaccurate and additional testing is needed to establish the complete and accurate profile. Ten test materials and components of systems were extracted and their extracts characterized for organic extractables using typical screening procedures. Measured and calculated TOC was reconciled to establish the completeness of the revealed extractables profile. When the TOC reconciliation was incomplete, the profiling was augmented with additional analytical testing to reveal the missing members of the organic extractables profile. This process is illustrated via two case studies involving aqueous extracts of sterile filters. Plastic materials and systems used to manufacture, contain, store, and deliver pharmaceutical products are extracted and the extracts analyzed to establish the materials' (or

Resin purification from Dragons Blood by using sub critical solvent extraction method

Science.gov (United States)

Saifuddin; Nahar

2018-04-01

Jernang resin (dragon blood) is the world's most expensive sap. The resin obtained from jernang that grows only on the islands of Sumatra and Borneo. Jernang resin is in demand by the State of China, Hong Kong, and Singapore since they contain compounds that have the potential dracohordin as a medicinal ingredient in the biological and pharmacological activity such as antimicrobial, antiviral, antitumor and cytotoxic activity. The resin extracting process has conventionally been done by drizzly with maceration method as one way of processing jernang, which is done by people in Bireuen, Aceh. However, there are still significant obstacles, namely the quality of the yield that obtained lower than the jernang resin. The technological innovation carried out by forceful extraction process maceration by using methanol produced a yield that is higher than the extraction process maceration method carried out in Bireuen. Nevertheless, the use of methanol as a solvent would raise the production costs due to the price, which is relatively more expensive and non-environmentally friendly. To overcome the problem, this research proposed a process, which is known as subcritical solvent method. This process is cheap, and also abundant and environmentally friendly. The results show that the quality of jernang resins is better than the one that obtained by the processing group in Bireuen. The quality of the obtained jernang by maceration method is a class-A quality based on the quality specification requirements of jernang (SNI 1671: 2010) that has resin (b/b) 73%, water (w/w) of 6.8%, ash (w/b) 7%, impurity (w/w) 32%, the melting point of 88°C and red colours. While the two-stage treatment obtained a class between class-A and super quality, with the resin (b/b) 0.86%, water (w/w) of 6.5%, ash (w/w) of 2.8%, levels of impurities (w/w) of 9%, the melting point of 88 °C and dark-red colours.

Ion chromatography for the analysis of salt splitting capacities of cation and anion resin in premixed resin sample

International Nuclear Information System (INIS)

Ghosh, Satinath; Kumar, Rakesh; Tripathy, M.K.; Dhole, K.; Sharma, R.S.; Varde, P.V.

2017-01-01

Mixed bed ion exchange resin is commonly used in various plants including nuclear reactors for the purpose of fine polishing. The analysis of ion exchange capacities of cation and anion resin in resin mixture is therefore an agenda in the context of purchasing of premixed resin from the manufacturer. An ion chromatographic method for assaying ion exchange capacities of pure as well as mixed resin has been optimized. The proposed method in contrast to the conventional ASTM method has been found to be quite encouraging to consider it as an alternate method for the analysis of premixed resin. (author)

Chromatographic studies of thorium(IV) and its extraction from monazite sand

International Nuclear Information System (INIS)

Bandyopadhyay, Arup; Roy, Uday Sankar

1998-01-01

A simple, rapid and selective method has been developed for reversed phase extraction chromatographic studies of Th IV with high molecular mass monocarboxylic acid (C 15 -C 16 ), SRS-100 as a stationary phase on a column of silica gel. Quantitative extraction of Th IV has been achieved in the pH range 4.8-5.5. The extracted Th IV has been stripped with 1:1 (v/v) mixture of 0.2 M HNO 3 and 0.2 M NaNO 3 and estimated spectrophotometrically. The effect of variables as pH, stripping agents, flow rate on extraction and elution have been studied. Th IV has been separated from various commonly associated elements in binary and synthetic multicomponent mixtures. The method has been applied successfully for the extraction of thorium from monazite sand. (author)

Chemometric strategy for automatic chromatographic peak detection and background drift correction in chromatographic data.

Science.gov (United States)

Yu, Yong-Jie; Xia, Qiao-Ling; Wang, Sheng; Wang, Bing; Xie, Fu-Wei; Zhang, Xiao-Bing; Ma, Yun-Ming; Wu, Hai-Long

2014-09-12

Peak detection and background drift correction (BDC) are the key stages in using chemometric methods to analyze chromatographic fingerprints of complex samples. This study developed a novel chemometric strategy for simultaneous automatic chromatographic peak detection and BDC. A robust statistical method was used for intelligent estimation of instrumental noise level coupled with first-order derivative of chromatographic signal to automatically extract chromatographic peaks in the data. A local curve-fitting strategy was then employed for BDC. Simulated and real liquid chromatographic data were designed with various kinds of background drift and degree of overlapped chromatographic peaks to verify the performance of the proposed strategy. The underlying chromatographic peaks can be automatically detected and reasonably integrated by this strategy. Meanwhile, chromatograms with BDC can be precisely obtained. The proposed method was used to analyze a complex gas chromatography dataset that monitored quality changes in plant extracts during storage procedure. Copyright © 2014 Elsevier B.V. All rights reserved.

Extraction behaviour of Am(III) and Eu(III) from nitric acid medium in TEHDGA-HDEHP impregnated resins

Energy Technology Data Exchange (ETDEWEB)

Saipriya, G.; Kumar, T. [Bhabha Atomic Research Centre Facilities, Kalpakkam (India). Kalpakkam Reprocessing Plant; Kumaresan, R.; Nayak, P.K.; Venkatesan, K.A.; Antony, M.P. [Indira Gandhi Center for Atomic Research, Kalpakkam (India). Fuel Chemistry Div.

2016-07-01

The extraction behaviour of Am(III) and Eu(III) from nitric acid medium was studied in the solvent impregnated resins containing extractants such as tetra-bis(2-ethylhexyl)diglycolamide (TEHDGA) or bis-(2-ethylhexyl)phosphoric acid (HDEHP) or mixture of TEHDGA+HDEHP. The rate of extraction of Am(III) and Eu(III) from 1 M nitric acid and the effect of various parameters, such as the concentration of nitric acid in aqueous phase and concentration of TEHDGA and HDEHP in resin phase, on the distribution coefficient of Am(III) and Eu(III) was studied. The distribution coefficient of Am(III) and Eu(III) in HDEHP-impregnated resin decreased and that in TEHDGA-impregnated resin increased, with increase in the concentration of nitric acid. However, in (TEHDGA+HDEHP) - impregnated resin, synergic extraction was observed at lower nitric acid concentration and antagonism at higher nitric acid concentration. The mechanism of Am(III) and Eu(III) extraction in the combined resin was investigated by slope analysis method. The extraction of various metal ions present in the fast reactor simulated high-level liquid waste was studied. The separation factor of Am(III) over Eu(III) was studied using citrate-buffered diethylenetriaminepentaacetic acid (DTPA) solution.

Evaluation of extractants and chelating resins in polishing actinide-contaminated waste streams

International Nuclear Information System (INIS)

Schreiber, S.B.; Dunn, S.L.; Yarbro, S.L.

1991-06-01

At the Los Alamos National Laboratory Plutonium Facility, anion exchange is used for recovering plutonium from nitric acid solutions. Although this approach recovers >99%, the trace amounts of plutonium and other actinides remaining in the effluent require additional processing. We are doing research to develop a secondary unit operation that can directly polish the effluent so that actinide levels are reduced to below the maximum allowed for facility discharge. We selected solvent extraction, the only unit operation that can meet the stringent process requirements imposed; several carbonyl and phosphoryl extractants were evaluated and their performance characterized. We also investigated various engineering approaches for solvent extraction; the most promising was a chelating resin loaded with extractant. Our research now focuses on the synthesis of malonamides, and our goal is to bond these extractants to a resin matrix. 7 refs., 12 figs., 1 tab

[Mechanism of gold solid extraction from aurocyanide solution using D3520 resin impregnated with TRPO].

Science.gov (United States)

Yang, Xiang-Jun; Wang, Shi-Xiong; Zou, An-Qin; Chen, Jing; Guo, Hong

2014-02-01

Trialkyphosphine oxides (TRPO) was successfully used for the impregnation of D3520 resin to prepare an extractant-impregnated resin (EIR). Solid extraction of Au(I) from alkaline cyanide solution was studied using this extractant-impregnated resin (EIR), with addition of cetyltrimethylammonium bromide (CTMAB), directly into the aurous aqueous phase in advance. The mechanism of solid extraction was further investigated by means of FTIR, XPS and SEM. The column separation studies have shown that cationic surfactant CTMAB played a key role in the solid phase extraction, and the resin containing TRPO were effective for the extraction of gold when the molar ratio of CTMAB: Au( I ) reached 1:1. FTIR spectroscopy of gold loaded EIR showed that the frequency of C[triple bond]N stretching vibration was at 2144 cm(-1), and the frequency of P=O stretching vibration shifted to lower frequency from 1153 to 1150 cm(-1). The XPS spectrum of N(1s), Au(4f7/2) and Au(4f5/2) sugges- ted that the coordination environment of gold did not change before and after extraction, and gold was still as the form of Au (CN)2(-) anion exiting in the loaded resin; O(1s) spectrum showed that the chemically combined water significantly increased after solid extraction from 30.74% to 42.34%; Comparing to the P(2p) spectrum before and after extraction, the binding energy increased from 132. 15 to 132. 45 eV, indicating there maybe existing hydrogen-bond interaction between P=O and water molecule, such as P=O...H-O-H. The above results obtained established that in the solid extraction process, the hydrophobic ion association [CTMA+ x Au(CN)] diffused from the bulk solution into the pores of the EIR, and then be solvated by TRPO adsorbed in the pores through hydrogen bonding bridged by the water molecules.

Evaluation of the separation and purification of 227Th from its decay progeny by anion exchange and extraction chromatography

International Nuclear Information System (INIS)

Ivanov, P.I.; Collins, S.M.; Es, E.M. van; García-Miranda, M.; Jerome, S.M.; Russell, B.C.

2017-01-01

Thorium-227 is currently undergoing evaluation as a potential radionuclide for targeted cancer therapy, and as such a high chemical purity of the material is required. To establish a reliable procedure for radiochemical isolation of 227 Th from the parent 227 Ac and decay progeny, which includes the radiotherapeutic 223 Ra, the performance of three different separation schemes based on ion-exchange and extraction chromatography have been evaluated. The results suggest that both ion exchange and extraction chromatographic techniques can be successfully used for the separation of 227 Th from its decay progeny, however extraction chromatographic resins demonstrate favourable performance in terms of Th recovery and purification from radionuclide impurities. - Highlights: • Development of a radiochemical separation of 227 Th from residual 227Ac as well as from decay progeny. • Evaluation of ion-exchange and extraction chromatography techniques. • TEVA resin demonstrates favourable performance in terms of Th recovery and purification. • Developed method is applicable to both nuclear medicine and environmental analysis.

Application of extraction-chromatographic concentration to atomic absorption determination of lead and cadmium in drinking and sea water

International Nuclear Information System (INIS)

Bol'shova, T.A.; Agapkina, G.I.; Ershova, N.I.; Narankho, K.E.

1988-01-01

To increase the detection limits for lead and cadmium atomic-absorption determination in natural waters methods of extraction-chromatographic concentration of these metals using tri-n-octylamine (TOA) on polytetrafluoroethylene (PTFE) is developed. Chromatograpy was carried out from 1.5-2.0 M HBr solutions. For cadmium and lead elution acetic acid was used. It is shown that extraction-chromatographic concentration permits to decrease limits of metal atomic-absorption detection by 10 3 with the 500 ml volume sample analysis

A simple high-performance liquid chromatographic method for the estimation of boswellic acids from the market formulations containing Boswellia serrata extract.

Science.gov (United States)

Shah, Shailesh A; Rathod, Ishwarsinh S; Suhagia, Bhanubhai N; Pandya, Saurabh S; Parmar, Vijay K

2008-09-01

A simple, rapid, and reproducible reverse-phase high-performance liquid chromatographic method is developed for the estimation of boswellic acids, the active constituents in Boswellia serrata oleo-gum resin. The chromatographic separation is performed using a mobile phase consisting of acetonitrile-water (90:10, % v/v) adjusted to pH 4 with glacial acetic acid on a Kromasil 100 C18 analytical column with flow rate of 2.0 mL/min and detection at 260 nm. The elution times are 4.30 and 7.11 min for 11-keto beta-boswellic acid (11-KBA) and 3-acetyl 11-keto beta-boswellic acid (A-11-KBA), respectively. The calibration curve is linear in the 11.66-58.30 microg/mL and 6.50-32.50 microg/mL range for 11-KBA and A-11-KBA, respectively. The limits of detection are 2.33 microg/mL and 1.30 microg/mL for 11-KBA and A-11-KBA, respectively. The mean recoveries are 98.24% to 104.17% and 94.12% to 105.92% for 11-KBA and A-11-KBA, respectively. The inter- and intra-day variation coefficients are less than 5%. The present method is successfully applied for the estimation of boswellic acids from the market formulations containing Boswellia serrata extract.

Extraction of Co ions from ion-exchange resin by supercritical carbon dioxide

International Nuclear Information System (INIS)

Ju, Min Su; Koh, Moon Sung; Yang, Sung Woo; Park, Kwang Heon; Kim, Hak Won; Kim, Hong Doo

2005-01-01

There are a number of liquid treatment processes for eliminating radioactive ionic contaminants in nuclear facilities. One of the most common treatment methods for aqueous streams is the use of ion exchange, which is a well-developed technique that has been employed for many years in the nuclear industry. More specifically speaking, systems that ion exchange method is applied to in nuclear power plants are liquid radioactive waste treatment system, chemical and volume control system, steam generator blowdown treatment system, and service water supply system. During the operation of nuclear power plants, radioactive contaminants such as Co-60, Mn-54, Fe-59 and Cs-137 are contained in liquid radioactive wastes. And the wastes containing small amount of uranium are generated in nuclear fuel cycle facilities. To treat the liquid radioactive waste, we usually install ion exchangers rather than evaporators due to their simplicity and effectiveness, and this trend is increasing. However, the ion exchange process produces large volume of spent organic resin, and has some problems of radiation damage and thermal instability. And the reuse of the resin is limited due to the degradation of ion-exchanging ability. For this reason, were should consider a better method to expand the lifetime of the resin or to reduce the volume of radioactive resin wastes by extracting radioactive contaminants located in the resin. Supercritical fluid CO 2 has many good points as a process solvent that include low viscosity, negligible surface tension, and variable selectivity. And supercritical fluids have physical properties of both liquid and gas such as good penetration with a high dissolution capability. Supercritical fluids have been widely used in extraction, purification, and recovery processes. A number of workers applied supercritical CO 2 solvent for cleaning of precision devices and waste treatments. Since supercritical CO 2 has its mild critical point at 31 and 73.8bar as .deg. C

Chromatographic profiles of extractives from leaves of Eugenia uniflora

Directory of Open Access Journals (Sweden)

Isabelle C.F. Bezerra

Full Text Available ABSTRACT Eugenia uniflora L., Myrtaceae, popularly known as “pitanga”, is used in traditional medicine due the properties attributed to its chemical content, these being mainly hydrolysable tannins and flavonoids. This study provides a qualitative and quantitative evaluation of chemical profile from leaves of E. uniflora. The HPLC analysis was carried out on a C18 column (4.6 mm × 250 mm, 5 µm by gradient elution with methanol and water (acidified with trifluoracetic acid; and silica gel Plates 60-F 254 with 10–12 µm and 5–6 µm particles, respectively for TLC and High HPTLC analysis. The chromatographic data obtained from HPLC, TLC and HPTLC presented bands and peaks related to flavonoids (myricitrin and derivatives and tannins (gallic and ellagic acids, which were observed from different samples. The chromatographic similarities enabled the building of a typical fingerprint for the herbal material. The similarity analysis of the sample data by Pearson correlation showed R values >0.9 among peaks (HPLC and bands (HPTLC. In addition, the analytical methodology developed by HPLC enabled the satisfactory quantification of marker substances [ellagic acid = 0.22% and 0.20% (m/m; gallic acid = 0.20% and 0.43%; myricitrin = 0.42 and 1.74% (m/m in herbal drug and crude extract, respectively]. The procedure was also validated in accordance with the assays required by Brazilian legislation. Thus, the HPTLC and HPLC methods developed in this study provide helpful and simple tools for the quality evaluation both qualitatively and quantitatively of raw materials and extractives from leaves of E. uniflora.

Adsorption of saponin compound in Carica papaya leaves extract using weakly basic ion exchanger resin

Science.gov (United States)

Abidin, Noraziani Zainal; Janam, Anathasia; Zubairi, Saiful Irwan

2016-11-01

Adsorption of saponin compound in papaya leaves juice extract using Amberlite® IRA-67 resin was not reported in previous studies. In this research, Amberlite® IRA-67 was used to determine the amount of saponin that can be adsorbed using different weights of dry resin (0.1 g and 0.5 g). Peleg model was used to determine the maximum yield of saponin (43.67 mg) and the exhaustive time (5.7 days) prior to a preliminary resin-saponin adsorption study. After adsorption process, there was no significant difference (p>0.05) in total saponin content (mg) for sample treated with 0.1 g (3.79 ± 0.55 mg) and sample treated with 0.5 g (3.43 ± 0.51 mg) dry weight resin. Long-term kinetic adsorption of resin-saponin method (>24 hours) should be conducted to obtain optimum freed saponin extract. Besides that, sample treated with 0.1 g dry weight resin had high free radical scavenging value of 50.33 ± 2.74% compared to sample treated with 0.5 g dry weight resin that had low free radical scavenging value of 24.54 ± 1.66% dry weights. Total saponin content (mg), total phenolic content (mg GAE) and free radical scavenging activity (%) was investigated to determine the interaction of those compounds with Amberlite® IRA-67. The RP-HPLC analysis using ursolic acid as standard at 203 nm showed no peak even though ursolic acid was one of the saponin components that was ubiquitous in plant kingdom. The absence of peak was due to weak solubility of ursolic acid in water and since it was only soluble in solvent with moderate polarity. The Pearson's correlation coefficient for total saponin content (mg) versus total phenolic content (mg GAE) and radical scavenging activity (%) were +0.959 and +0.807. Positive values showed that whenever there was an increase in saponin content (mg), the phenolic content (mg GAE) and radical scavenging activity (%) would also increase. However, as the resin-saponin adsorption was carried out, there was a significant decrease of radical scavenging activity

Chronic swelling from entrapment of acrylic resin in a surgical extraction site

Directory of Open Access Journals (Sweden)

Weiting Ho

2010-01-01

Full Text Available When acrylic resin is inadvertently embedded in oral tissue, it can result in a pronounced chronic inflammatory response. This report describes a case in which temporary crown and bridge resin was forced into a surgical extraction site after the two adjacent teeth were prepared for a bridge immediately following extraction of a maxillary premolar. The patient experienced swelling at the extraction site over a ten month period despite treatment with antibiotics and anti-inflammatory drugs. After detection and removal of the foreign body, the symptoms resolved. The episode contributed to periodontal bone loss around an adjacent tooth. While morbidity of this nature is rare, this case reinforces the need to investigate persistent signs of inflammation and account for dental materials that are lost during the course of treatment.

Simultaneous separation and detection of actinides in acidic solutions using an extractive scintillating resin.

Science.gov (United States)

Roane, J E; DeVol, T A

2002-11-01

An extractive scintillating resin was evaluated for the simultaneous separation and detection of actinides in acidic solutions. The transuranic extractive scintillating (TRU-ES) resin is composed of an inert macroporous polystyrene core impregnated with organic fluors (diphenyloxazole and 1,4-bis-(4-methyl-5-phenyl-2-oxazolyl)benzene) and an extractant (octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide in tributyl phosphate). The TRU-ES resin was packed into FEP Teflon tubing to produce a flow cell (0.2-mL free column volume), which is placed into a scintillation detection system to obtain pulse height spectra and time series data during loading and elution of actinides onto/from the resin. The alpha-particle absolute detection efficiencies ranged from 77% to 96.5%, depending on the alpha energy and quench. In addition to the on-line analyses, off-line analyses of the effluent can be conducted using conventional detection methods. The TRU-ES resin was applied to the quantification of a mixed radionuclide solution and two actual waste samples. The on-line characterization of the mixed radionuclide solution was within 10% of the reported activities whereas the agreement with the waste samples was not as good due to sorption onto the sample container walls and the oxidation state of plutonium. Agreement between the on-line and off-line analyses was within 35% of one another for both waste samples.

Sulfur geochemistry of hydrothermal waters in Yellowstone National Park, Wyoming, USA. III. An anion-exchange resin technique for sampling and preservation of sulfoxyanions in natural waters

Directory of Open Access Journals (Sweden)

Ball James W

2003-06-01

Full Text Available A sampling protocol for the retention, extraction, and analysis of sulfoxyanions in hydrothermal waters has been developed in the laboratory and tested at Yellowstone National Park and Green Lake, NY. Initial laboratory testing of the anion-exchange resin Bio-Rad™ AG1-X8 indicated that the resin was well suited for the sampling, preservation, and extraction of sulfate and thiosulfate. Synthetic solutions containing sulfate and thiosulfate were passed through AG1-X8 resin columns and eluted with 1 and 3 M KCl, respectively. Recovery ranged from 89 to 100%. Comparison of results for water samples collected from five pools in Yellowstone National Park between on-site IC analysis (U.S. Geological Survey mobile lab and IC analysis of resin-stored sample at SUNY-Stony Brook indicates 96 to 100% agreement for three pools (Cinder, Cistern, and an unnamed pool near Cistern and 76 and 63% agreement for two pools (Sulfur Dust and Frying Pan. Attempts to extract polythionates from the AG1-X8 resin were made using HCl solutions, but were unsuccessful. Bio-Rad™ AG2-X8, an anion-exchange resin with weaker binding sites than the AG1-X8 resin, is better suited for polythionate extraction. Sulfate and thiosulfate extraction with this resin has been accomplished with KCl solutions of 0.1 and 0.5 M, respectively. Trithionate and tetrathionate can be extracted with 4 M KCl. Higher polythionates can be extracted with 9 M hydrochloric acid. Polythionate concentrations can then be determined directly using ion chromatographic methods, and laboratory results indicate recovery of up to 90% for synthetic polythionate solutions using AG2-X8 resin columns.

Separation of scutellarin from crude extracts of Erigeron breviscapus (vant.) Hand. Mazz. by macroporous resins.

Science.gov (United States)

Gao, Min; Huang, Wei; Liu, Chun-Zhao

2007-10-15

Scutellarin, a flavone glycoside, popularly used in the treatment of heart disease, has been efficiently separated using macroporous resins from crude extracts of Chinese medicinal plant Erigeron breviscapus (vant.) Hand. Mazz. HPD-800 resin offered the best adsorption and desorption capacity for scutellarin among the eight macroporous resins tested, and its adsorption data at 25 degrees C fit best to the Langmuir isotherm. The dynamic adsorption and desorption experiments have been carried out on a HPD-800 resin packed column to optimize the separation process of scutellarin from the crude extracts of E. breviscapus. After one run treatment with HPD-800 resin, the scutellarin content in the product was increased 15.69-fold from 2.61% to 40.96% with a recovery yield of 95.01%. The preparative separation process via adsorption-desorption method developed in this study provides a new approach for scale-up separation and purification of scutellarin for its wide pharmaceutical use.

Ten years of experience in extraction chromatographic processes for the recovery, separation and purification of actinides elements

International Nuclear Information System (INIS)

Madic, C.; Bourges, J.; Koehly, G.

1984-06-01

Ten years ago the extraction chromatographic technique was developed for preparative purposes and is now applied for all chemicals separations needed for the production of actinides isotopes. That technique appears to be simple and flexible. It can be used for the production of microgram to kilogram amounts of actinide isotopes. This paper focuses on the experience gained and describes some peculiar production of actinide isotopes solved by using extraction chromatographic technique. After a review of extracting molecules and equipment, treatment of irradiated targets (preparation of Pu 238 and removal of neptunium, production of Am 243 and Cm 244), recovery of actinides from alpha aqueous wastes (preparation of Am 241) and recovery of decay products from aged actinide stocks (recovery of Am 241 from Pu stocks, of U 234 from Pu 238 stocks) are described

Preparation of chromatographic and solid-solvent extraction 99mTc generators using gel-type targets

International Nuclear Information System (INIS)

Le Van So

2000-01-01

We have studied two types of targets zirconium-molybdate (ZrMo) and titanium-molybdate (TiMo) prepared by precipitating reaction between ammonium-molybdate and zirconium-chloride or titanium-chloride solutions, respectively. Other types of targets were also prepared by co-precipitating ZrMo or TiMo with hydrous manganese-dioxide, hydrous silica, and hydrous titanium-dioxide or by impregnated ZrMo or TiMo with Iodate anions. The results on extraction of Tc-99m from neutron irradiated TiMo solid phase using solvents such as MEK, aceton, ethylic ether, chloroform, etc showed that separation yield (SY) of Tc-99m in case of aceton extraction was from 70% to 80% and in other cases non higher than 40%. The Tc-99m elution curves and column kinetic in case of aceton extraction (after evaporation of aceton and recovery of Tc-99m in 0,9% NaCl solution) was superior than in case chromatographic generator using saline eluant. As result obtained, two types of generators were successfully prepared and put into use: Chromatographic generator using titanium-molybdate target as packing material and saline as eluant. Solid-solvent extraction 99m Tc generator using titanium-molybdate target (as solid phase) and aceton as extracting solvent. (author)

Long term stability of cannabis resin and cannabis extracts

DEFF Research Database (Denmark)

Lindholst, Christian

2010-01-01

at room temperature, 4 °C and - 20 °C for up to 4 years. Acidic THC degrades exponentially via decarboxylation with concentration halve-lives of approximately 330 and 462 days in daylight and darkness, respectively. The degradation of neutral THC seems to occur somewhat slower. When cannabinoids were...... stored in extracted form at room temperature the degradation rate of acidic THC increased significantly relative to resin material with concentration halve-lives of 35 and 91 days in daylight and darkness, respectively. Once cannabis material is extracted into organic solvents, care should be taken...

Sulfur geochemistry of hydrothermal waters in Yellowstone National Park, Wyoming, USA. III. An anion-exchange resin technique for sampling and preservation of sulfoxyanions in natural waters

Science.gov (United States)

Druschel, G.K.; Schoonen, M.A.A.; Nordstorm, D.K.; Ball, J.W.; Xu, Y.; Cohn, C.A.

2003-01-01

A sampling protocol for the retention, extraction, and analysis of sulfoxyanions in hydrothermal waters has been developed in the laboratory and tested at Yellowstone National Park and Green Lake, NY. Initial laboratory testing of the anion-exchange resin Bio-Rad??? AG1-X8 indicated that the resin was well suited for the sampling, preservation, and extraction of sulfate and thiosulfate. Synthetic solutions containing sulfate and thiosulfate were passed through AG1-X8 resin columns and eluted with 1 and 3 M KCl, respectively. Recovery ranged from 89 to 100%. Comparison of results for water samples collected from five pools in Yellowstone National Park between on-site IC analysis (U.S. Geological Survey mobile lab) and IC analysis of resin-stored sample at SUNY-Stony Brook indicates 96 to 100% agreement for three pools (Cinder, Cistern, and an unnamed pool near Cistern) and 76 and 63% agreement for two pools (Sulfur Dust and Frying Pan). Attempts to extract polythionates from the AG1-X8 resin were made using HCl solutions, but were unsuccessful. Bio-Rad??? AG2-X8, an anion-exchange resin with weaker binding sites than the AG1-X8 resin, is better suited for polythionate extraction. Sulfate and thiosulfate extraction with this resin has been accomplished with KCl solutions of 0.1 and 0.5 M, respectively. Trithionate and tetrathionate can be extracted with 4 M KCl. Higher polythionates can be extracted with 9 M hydrochloric acid. Polythionate concentrations can then be determined directly using ion chromatographic methods, and laboratory results indicate recovery of up to 90% for synthetic polythionate solutions using AG2-X8 resin columns. ?? The Royal Society of Chemistry and the Division of Geochemistry of the American Chemical Society 2003.

Extraction chromatographic method of uranium(VI) with high molecular mass amine (ALIQUAT - 336)

International Nuclear Information System (INIS)

Roy, Uday Sankar; Dutta, Keshab Kumar

1999-01-01

A selective method has been developed for reversed phase extraction chromatographic studies of uranium(VI) with Aliquat - 336 (liquid anion exchanger) coated on silica gel as stationary phase. Quantitative extraction of uranium has been achieved in HCl - medium from 1.25(M)-4(M). The effect of different acids with various concentrations stripping agents, flow rate on extraction and elution have been investigated. The exchange capacity of the prepared exchanger has been determined. Uranium(VI) has been separated quantitatively from Th, Ce, Zr, Pb, Ga, Hg, Fe, La, Pr, Nd, Sm and Cr from a binary mixture by controlling the extraction and elution conditions. The separation of U(VI) from ternary and quarternary mixtures of various metal ions has also been achieved. (author)

Accurate determination of 129I concentrations and 129I/137Cs ratios in spent nuclear resins by Accelerator Mass Spectrometry

International Nuclear Information System (INIS)

Nottoli, Emmanuelle; Bienvenu, Philippe; Labet, Alexandre; Bourlès, Didier; Arnold, Maurice; Bertaux, Maité

2014-01-01

Determining long-lived radionuclide concentrations in radioactive waste has fundamental implications for the long-term management of storage sites. This paper focuses on the measurement of low 129 I contents in ion exchange resins used for primary fluid purification in Pressurised Water Reactors (PWR). Iodine-129 concentrations were successfully determined using Accelerator Mass Spectrometry (AMS) following a chemical procedure which included (1) acid digestion of resin samples in HNO 3 /HClO 4 , (2) radioactive decontamination by selective iodine extraction using a new chromatographic resin (CL Resin), and (3) AgI precipitation. Measured 129 I concentrations ranged from 4 to 12 ng/g, i.e. from 0.03 to 0.08 Bq/g. The calculation of 129 I/ 137 Cs activity ratios used for routine waste management produced values in agreement with the few available data for PWR resin samples. - Highlights: • In the context of radioactive waste management, this study aimed at measuring 129 I in spent resins using accelerator mass spectrometry. • The treatment procedure included microwave acid digestion of samples, iodine extraction by CL resins and AgI precipitation. • Developed first on synthetic matrices, the chemical treatment procedure was then successfully applied to real resin samples. • 129 I concentrations ranged from 4 to 12 ng/g of dry resin. • Results are in agreement with previous measurements and support reference values currently used for nuclear resin management

HTGR fuel development: loading of uranium on carboxylic acid cation-exchange resins using solvent extraction of nitrate

International Nuclear Information System (INIS)

Haas, P.A.

1975-09-01

The reference fuel kernel for recycle of 233 U to HTGR's (High-Temperature Gas-Cooled Reactors) is prepared by loading carboxylic acid cation-exchange resins with uranium and carbonizing at controlled conditions. The purified 233 UO 2 (NO 3 ) 2 solution from a fuel reprocessing plant contains excess HNO 3 (NO 3 - /U ratio of approximately 2.2). The reference flowsheet for a 233 U recycle fuel facility at Oak Ridge uses solvent extraction of nitrate by a 0.3 M secondary amine in a hydrocarbon diluent to prepare acid-deficient uranyl nitrate. This nitrate extraction, along with resin loading and amine regeneration steps, was demonstrated in 14 runs. No significant operating difficulties were encountered. The process is controlled via in-line pH measurements for the acid-deficient uranyl nitrate solutions. Information was developed on pH values for uranyl nitrate solution vs NO 3 - /U mole ratios, resin loading kinetics, resin drying requirements, and other resin loading process parameters. Calculations made to estimate the capacities of equipment that is geometrically safe with respect to control of nuclear criticality indicate 100 kg/day or more of uranium for single nitrate extraction lines with one continuous resin loading contactor or four batch loading contactors. (auth)

Uses of extraction and ion exchange chromatography in the thorium and rare earths separation from industrial residue generated in thorium purification unity at IPEN. Application of rare earths as catalysts for generation of hydrogen

International Nuclear Information System (INIS)

Zini, Josiane

2010-01-01

In the 70's a pilot plant for studies of different concentrates processing obtained from the chemical processing of monazite was operated at IPEN / CNEN-SP, with a view to obtaining thorium of nuclear purity. This unity was operated on an industrial scale since 1985, generating around 25 metric tons of residue and was closed in 2002. This waste containing thorium and rare earths was named Retoter (Rejeito de Torio e Terras Raras, in portuguese) and stored in the IPEN Safeguards shed. This paper studies the treatment of the waste, aimed at environmental, radiological and technology. Were studied two cases for the chromatographic separation of thorium from rare earths. One of them was the chromatographic extraction, where the extracting agent tributyl phosphate was supported on polymeric resins Amberlite XAD16. The other method is studied for comparison purposes, since the material used in chromatographic extraction is unprecedented with regard to the separation of thorium, was the ion-exchange chromatography using DOWEX 1-X8 strong cationic resin. Was studied also the chromatographic process of extraction with the extracting agent DEHPA supported on Amberlite XAD16 for the fractionation in groups of rare earths elements. Thorium was separated with high purity for strategic purposes and rare earths recovered free from thorium, were tested as a catalyst for ethanol reforming to hydrogen obtaining which is used in fuel cells for power generation. (author)

Extraction and Separation of Uranium (VI) and Thorium (IV) Using Tri-n-dodecylamine Impregnated Resins

International Nuclear Information System (INIS)

Metwally, E.; Saleh, A.Sh.; El-Naggar, H.A.

2005-01-01

Extraction of U(VI) and Th(IV) from chloride and nitrate solutions with tri-n- dodecylamine impregnated on Amberlite XAD4, was investigated. The distribution of U(VI) and Th(IV) was studied at different concentrations of acid, salting-out agent, extractant, aqueous metal ion and other parameters. Absorption spectral studies have been investigated for uranium species in both aqueous HCl solution and the resin phase. From these studies, it is suggested that the tetrachloro complex of U(VI) is formed in the extraction of uranium (VI) from hydrochloric acid solutions by TDA impregnated resin. Stripping of the extracted U(VI) and Th(IV) was assayed with HCl and HNO 3 . Finally, the separation of uranium from thorium and fission products in HCl media was achieved

Study of Adsorption Property of Ga(III) onto Strongly Basic Resin for Ga Extraction from Bayer Liquor

Science.gov (United States)

Zhao, Zhuo; Yang, Yongxiang; Lu, Hao; Hua, Zhongsheng; Ma, Xiaoling

Ion-exchange is the main technology used in industry for gallium recovery from Bayer liquor, the largest gallium production resource. However, the co-extraction of vanadium and the degradation of resins are the major issues. Further investigations related to fundamental theory are needed. This paper reports the study of the adsorption properties of a strongly basic resin having a combination of one =NOH group and another active group -NH2 for Ga(III) extraction. The influence of operational conditions such as contact time, initial Ga(III) concentration and temperature on Ga(III) adsorption were extensively investigated. The results revealed that the resin has high adsorption capacity and Ga(III) selectivity. The optimal adsorption condition was obtained at temperatures of 40-50°C and contact time of 40-60 min. The Ga(III) adsorption data on the resin fit well with the pseudo second-order kinetics. Langmuir and Freundlich models were used to describe Ga(III) adsorption isotherms on the resin.

Novel materials and methods for solid-phase extraction and liquid chromatography

Energy Technology Data Exchange (ETDEWEB)

Ambrose, Diana [Iowa State Univ., Ames, IA (United States)

1997-06-24

This report contains a general introduction which discusses solid-phase extraction and solid-phase micro-extraction as sample preparation techniques for high-performance liquid chromatography, which is also evaluated in the study. This report also contains the Conclusions section. Four sections have been removed and processed separately: silicalite as a sorbent for solid-phase extraction; a new, high-capacity carboxylic acid functionalized resin for solid-phase extraction; semi-micro solid-phase extraction of organic compounds from aqueous and biological samples; and the high-performance liquid chromatographic determination of drugs and metabolites in human serum and urine using direct injection and a unique molecular sieve.

Development, modelling, optimisation and scale-up of chromatographic purification of a therapeutic protein

DEFF Research Database (Denmark)

Mollerup, Jørgen; Hansen, Thomas Budde; Kidal, Steffen

2007-01-01

Development of a chromatographic purification step proceeds through a number of stages. High-throughput screening techniques are used to identify suitable resins. This technique is also suitable for the design of a capture step and some intermediate chromatographic steps, but development and true...... by industry. The theory of residence time based scale-up is developed and applied. (c) 2007 Elsevier B.V. All rights reserved....

QSAR models for prediction of chromatographic behavior of homologous Fab variants.

Science.gov (United States)

Robinson, Julie R; Karkov, Hanne S; Woo, James A; Krogh, Berit O; Cramer, Steven M

2017-06-01

While quantitative structure activity relationship (QSAR) models have been employed successfully for the prediction of small model protein chromatographic behavior, there have been few reports to date on the use of this methodology for larger, more complex proteins. Recently our group generated focused libraries of antibody Fab fragment variants with different combinations of surface hydrophobicities and electrostatic potentials, and demonstrated that the unique selectivities of multimodal resins can be exploited to separate these Fab variants. In this work, results from linear salt gradient experiments with these Fabs were employed to develop QSAR models for six chromatographic systems, including multimodal (Capto MMC, Nuvia cPrime, and two novel ligand prototypes), hydrophobic interaction chromatography (HIC; Capto Phenyl), and cation exchange (CEX; CM Sepharose FF) resins. The models utilized newly developed "local descriptors" to quantify changes around point mutations in the Fab libraries as well as novel cluster descriptors recently introduced by our group. Subsequent rounds of feature selection and linearized machine learning algorithms were used to generate robust, well-validated models with high training set correlations (R 2  > 0.70) that were well suited for predicting elution salt concentrations in the various systems. The developed models then were used to predict the retention of a deamidated Fab and isotype variants, with varying success. The results represent the first successful utilization of QSAR for the prediction of chromatographic behavior of complex proteins such as Fab fragments in multimodal chromatographic systems. The framework presented here can be employed to facilitate process development for the purification of biological products from product-related impurities by in silico screening of resin alternatives. Biotechnol. Bioeng. 2017;114: 1231-1240. © 2016 Wiley Periodicals, Inc. © 2016 Wiley Periodicals, Inc.

Response Surface Optimized Extraction of 1-Deoxynojirimycin from Mulberry Leaves (Morus alba L. and Preparative Separation with Resins

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Teng Wang

2014-05-01

Full Text Available In the present study, the extraction technology and preparative separation of 1-deoxynojirimycin from mulberry leaves were systematically investigated. Four extraction parameters (ethanol concentration, extraction temperature, extraction time and ratio of solvent to sample were explored by response surface methodology (RSM. The results indicated that the maximal yield of 1-deoxynojirimycin was achieved with an ethanol concentration of 55%, extraction temperature of 80 °C, extraction time of 1.2 h and ratio of solvent to sample of 12:1. The extraction yield under these optimum conditions was found to be 256 mg/100 g dry mulberry leaves. A column packed with a selected resin was used to perform dynamic adsorption and desorption tests to optimize the separation process. The results show that the preparative separation of 1-deoxynojirimycin from mulberry leaves can be easily and effectively done by adopting 732 resin. In conclusion, 732 resin is the most appropriate for the separation of 1-deoxynojirimycin from other components in mulberry leaves extracts, and its adsorption behavior can be described with Langmuir isotherms and a two-step adsorption kinetics model. The recovery and purity of 1-deoxynojirimycin in the final product were 90.51% and 15.3%, respectively.

Radiotoxicological analyses of 239+240Pu and 241Am in biological samples by anion-exchange and extraction chromatography: a preliminary study for internal contamination evaluations

International Nuclear Information System (INIS)

Ridone, S.; Arginelli, D.; Bortoluzzi, S.; Canuto, G.; Montalto, M.; Nocente, M.; Vegro, M.

2006-01-01

Many biological samples (urines and faeces) have been analysed by means of chromatographic extraction columns, utilising two different resins (AG 1-X2 resin chloride and T.R.U.), in order to detect the possible internal contamination of 239 + 240 Pu and 241 Am, for some workers of a reprocessing nuclear plant in the decommissioning phase. The results obtained show on one hand the great suitability of the first resin for the determination of plutonium, and on the other the great selectivity of the second one for the determination of americium

Radiotoxicological analyses of {sup 239+240}Pu and {sup 241}Am in biological samples by anion-exchange and extraction chromatography: a preliminary study for internal contamination evaluations

Energy Technology Data Exchange (ETDEWEB)

Ridone, S.; Arginelli, D.; Bortoluzzi, S.; Canuto, G.; Montalto, M.; Nocente, M.; Vegro, M. [Italian National Agency for New Technologies, Energy and the Environment (ENEA), Research Centre of Saluggia, Radiation Protection Institute, Saluggia, VC (Italy)

2006-07-01

Many biological samples (urines and faeces) have been analysed by means of chromatographic extraction columns, utilising two different resins (AG 1-X2 resin chloride and T.R.U.), in order to detect the possible internal contamination of {sup 239{sup +}}{sup 240}Pu and {sup 241}Am, for some workers of a reprocessing nuclear plant in the decommissioning phase. The results obtained show on one hand the great suitability of the first resin for the determination of plutonium, and on the other the great selectivity of the second one for the determination of americium.

Chromatographic separation of fructose from date syrup.

Science.gov (United States)

Al Eid, Salah M

2006-01-01

The objective of this study is to provide a process for separating fructose from a mixture of sugars containing essentially fructose and glucose, obtained from date palm fruits. The extraction procedure of date syrup from fresh dates gave a yield of 86.5% solids after vacuum drying. A process for separating fructose from an aqueous solution of date syrup involved adding the date syrup solutions (20, 30 and 40% by weight) to a chromatographic column filled with Dowex polystyrene strong cation exchange gel matrix resin Ca2 + and divinylbenzene, a functional group, sulfonic acid, particle size 320 microm, with a flow rate of 0.025 and 0.05 bed volume/min, under 30 and 70 degrees C column temperature. After the date sugar solution batch, a calculated quantity of water was added to the column. Glucose was retained by the resin more weakly than fructose and proceeded faster into the water batch flowing ahead. Three fractions were collected: a glucose-rich fraction, a return fraction, and a fructose-rich fraction. The return fraction is based on when the peaks of fructose and glucose were reached, which could be determined by means of an analyzer (polarimeter) based on the property of glucose and fructose solutions to turn the polarization level of polarized light. A high yield of fructose is obtained at 70 degrees C column temperature with a flow rate of 0.025 bed volume/min and date syrup solution containing 40% sugar concentration. The low recovery by weight obtained using date syrup solutions having a sugar concentration of 20 and 30%, encourages the use of a concentration of 40%. However, with the 40% date syrup supply the average concentrations of glucose and fructose in the return fractions were more than 40%, which can be used for diluting the thick date syrup solution extracted from dates.

CHEMICAL COMPOSITIONS OF PINE RESIN, ROSIN AND TURPENTINE OIL FROM WEST JAVA

OpenAIRE

Wiyono Bambang; Tachibana Sanro; Djaban Tinambunan

2006-01-01

This study was conducted to identify chemical composition of merkus pine resin, rosin and turpentine oil. Initially, pine resin was separated into neutral and acidic fractions with an aqueous 4% sodium hydroxide solution. After methylation, the fraction containing turpentine oil and rosin were analyzed by gas chromatography (GC), and gas chromatograph mass spectrometry (GC-MS), respectively. The neutral fraction of pine resin and turpentine oil mainly consisted of a-pinene, D-3-carene and b-p...

Modified resins for solid-phase extraction

Science.gov (United States)

Fritz, James S.; Sun, Jeffrey J.

1991-12-10

A process of treating aqueous solutions to remove organic solute contaminants by contacting an aqueous solution containing polar organic solute contaminants with a functionalized polystyrene-divinyl benzene adsorbent resin, with the functionalization of said resin being accomplished by organic hydrophilic groups such as hydroxymethyl, acetyl and cyanomethyl.

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.

Studying the Efficiency of XAD-7HP Anionic Resin in the Extraction of Humic Acid from Surface Water

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Hassan Hashemi

2017-09-01

Results: The average extraction efficiency for XAD-7HP was 77% and HA concentration determined in all seasons ranges from 0.15 to 0.29 mg/L in raw water. Conclusions: From the findings of this study, it can be concluded that the use of XAD-7HP is a proper and effective method for the extraction of HS and its extraction efficiency is more influenced by pH and turbidity than other parameters. It can also be deduced from this study that XAD-7HP resin was most efficient at a pH of 2 and an increase in turbidity resulted in a corresponding decrease in the efficiency of resin.

Effects of chromatographic fractions of Euphorbia hirta on the rat ...

African Journals Online (AJOL)

The effects of the chromatographic fractions of Euphorbia hirta Linn on the serum biochemical parameters in rats were investigated. The ethanolic extract of this plant was subjected to chromatographic separation using the vacuum liquid chromatographic technique, a modified form of classical column chromatography.

Solid phase extraction of copper(II) by fixed bed procedure on cation exchange complexing resins.

Science.gov (United States)

Pesavento, Maria; Sturini, Michela; D'Agostino, Girolamo; Biesuz, Raffaela

2010-02-19

The efficiency of the metal ion recovery by solid phase extraction (SPE) in complexing resins columns is predicted by a simple model based on two parameters reflecting the sorption equilibria and kinetics of the metal ion on the considered resin. The parameter related to the adsorption equilibria was evaluated by the Gibbs-Donnan model, and that related to the kinetics by assuming that the ion exchange is the adsorption rate determining step. The predicted parameters make it possible to evaluate the breakthrough volume of the considered metal ion, Cu(II), from different kinds of complexing resins, and at different conditions, such as acidity and ionic composition. Copyright 2009. Published by Elsevier B.V.

The PILO process: zeolites and titanates in the treatment of spent ion exchange resins

International Nuclear Information System (INIS)

Hultgren, Aa.; Thegerstroem, C.; Forberg, S.; Westermark, T.; Faelt, L.

1981-01-01

Spent ion exchange resins from power reactor operation contain more than 95% of the total radioactivity of wet reactor wastes. Cementation and bituminization are the two methods applied in Sweden up to now for the immobilization of spent resins. Over the last years, however, research and development work has resulted in a proposed process (PILO), where > 99.9 % of cesium and strontium and around 90 % of other radioactive nuclides are eluted from the spent resins and sorbed in zeolites and titanates in a chromatographic process. The inorganic sorbents are dried after loading and sintered to yield long-term stable products, while the treated resins may be incinerated to give ash residues of fairly short-lived activity. The development work has included production, characterization and testing of different zeolites and titanates, bench-scale optimization of the chromatographic process using actual spent resins, heat treatment of the loaded inorganic sorbents, and resin incineration. Over-all system design studies including transport requirements, integrated process flowsheets, and cost estimates are now in progress. The aim is to have a sufficient basis during spring 1982 to decide on the merits of a PILO plant at the planned repository for low and medium level waste (SFR), to be commissioned in 1988. (Auth.)

Determination of levels of organochlorine pesticides in plastic resin pellets on selected beaches in the Greater Accra region of Ghana

International Nuclear Information System (INIS)

Amoatey, A. E.

2012-07-01

The levels of organochlorine pesticides (OCPs) in beached plastic resin pellets were determined with the objective of assessing the status of OCP pollution in the marine ecosystem in selected beaches in Ghana. Samples of plastic resin pellets were collected at seven beaches in Accra (namely Art centre, Sakumono, Osu castle, Labadi, Korle-Gonno, Independence Square and Tema Mighty beaches) and analyzed for organochlorine pesticides, total chlorine and extractable chlorine. The plastic pellets were subjected to Soxhlet extraction and the extracts analyzed using Gas chromatograph coupled with electron capture detector. The detected compounds were alpha-HCH, beta-HCH, gamma-HCH, delta-HCH, hexachlorobenzene, o, p' -DDE, p, p'-DDE, o,p'-DDD, o, p'-DDT, heptachlor, trans-heptachlor epoxy, trans-chlordane, trans-nanochlor, aldrin, dieldrin, endrin, alpha-endosulphan, beta-endosulphan, endosulphan sulphate and methoxychlor. Analysis of the virgin pellets recorded no organochlorine pesticides present. However, plastics pellets collected from all seven beaches were found to contain OCPs with the highest recorded on the Art Centre beach with a total concentration of 106.26 ng/g. Plastic pellets collected on the Labadi beach recorded the lowest OCPs with a concentration of 20.2 ng/g. Total chlorine and extractable organochlorine (EOCI) were also determined in the plastic resin pellets by using the Instrumental Neutron Activation Analysis (INAA). The concentrations of total chlorine analyzed by INAA were between 2.82 and 50.25 mg/kg whereas the EOCR concentrations ranged from 1.67 to 30.90 mg/kg. EOCR accounted for 48.05% of the total chlorine in plastic pellets, suggesting that chlorine in the beached pellet relatively existed as organic and are extractable. The relative proportion of known or identified organochlorines (such as HCHs, DDT s, chlordane compounds, endosulphans, HCB and methoxychlor) to the total extractable organochlorine(EOCI) was averagely 7.4% which suggested

Solid-phase extraction sorbent consisting of alkyltrimethylammonium surfactants immobilized onto strong cation-exchange polystyrene resin.

Science.gov (United States)

Reid, Kendra R; Kennedy, Lonnie J; Crick, Eric W; Conte, Eric D

2002-10-25

Presented is a solid-phase extraction sorbent material composed of cationic alkyltrimethylammonium surfactants attached to a strong cation-exchange resin via ion-exchange. The original hydrophilic cation-exchange resin is made hydrophobic by covering the surface with alkyl chains from the hydrophobic portion of the surfactant. The sorbent material now has a better ability to extract hydrophobic molecules from aqueous samples. The entire stationary phase (alkyltrimethylammonium surfactant) is removed along with the analyte during the elution step. The elution step requires a mild elution solvent consisting of 0.25 M Mg2+ in a 50% 2-propanol solution. The main advantage of using a removable stationary phase is that traditionally utilized toxic elution solvents such as methylene chloride, which are necessary to efficiently release strongly hydrophobic species from SPE stationary phases, may now be avoided. Also, the final extract is directly compatible with reversed-phase liquid chromatography. The performance of this procedure is presented using pyrene as a test molecule.

Aminoalkylated Merrifield Resins Reticulated by Tris-(2-chloroethyl Phosphate for Cadmium, Copper, and Iron (II Extraction

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Mokhtar Dardouri

2015-01-01

Full Text Available We aimed to synthesize novel substituted polymers bearing functional groups to chelate heavy metals during depollution applications. Three polyamine functionalized Merrifield resins were prepared via ethylenediamine (EDA, diethylenetriamine (DETA, and triethylenetetramine (TETA modifications named, respectively, MR-EDA, MR-DETA, and MR-TETA. The aminoalkylated polymers were subsequently reticulated by tris-(2-chloroethyl phosphate (TCEP to obtain new polymeric resins called, respectively, MR-EDA-TCEP, MR-DETA-TCEP, and MR-TETA-TCEP. The obtained resins were characterized via attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR, elemental analysis (EA, and thermogravimetric (TGA, thermodynamic (DTA, and differential thermogravimetric (DTG analysis. The synthesized resins were then assayed to evaluate their efficiency to extract metallic ions such as Cd2+, Cu2+, and Fe2+ from aqueous solutions.

Antimicrobial Activity and Chromatographic Analysis of Extracts from Tropaeolum pentaphyllum Lam. Tubers

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Ritiel Corrêa da Cruz

2016-04-01

Full Text Available Background: Tropaeolum pentaphyllum Lam. tubers (Tropaeolaceae are known and used as a condiment and for the treatment of skin infections in Southern Brazil. However, its activity and composition has not yet been investigated. Thus, different extracts and the essential oil from the tubers were tested against a range of microorganisms. The most active extracts were submitted to chromatographic analysis. Methods: Hydroalcoholic extract (70%, fractions of it, and the essential oil from the tubers were tested against several bacteria, yeasts and molds, furnishing the corresponding inhibitory, bactericidal and fungicidal minimal concentration values. The most active extracts were submitted to GC-MS investigation. Results: The strongest effects against different strains of microorganisms, such as Gram-positive and negative bacteria, Candida spp. and dermatophytes were observed for the essential oil and the chloroform fraction, with minimal inhibitory concentrations (MICs well below 200 µg/mL. GC-MS analysis revealed that the major essential oil constituent is benzyl isothiocyanate (BITC, while the chloroform fraction is constituted of BITC, amides, sulfur, fatty acids and its esters, all compounds that may be related to the demonstrated activity. Conclusions: Overall, the results support the popular use of the plant for the treatment of skin infections, and revealed the main active compounds.

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

Science.gov (United States)

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

2014-02-14

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

Solventless LARC-160 Polyimide Matrix Resin. [applied for use in aerospace engineering

Science.gov (United States)

Stclair, T. L.; Jewell, R. A.

1978-01-01

The addition polyimide, LARC-160, which was originally synthesized from low cost liquid monomers as a laminating resin in ethanol, was prepared as a solventless, high viscosity, neat liquid resin. The resin was processed by hot-melt coating techniques into graphite prepreg with excellent tack and drape. Comparable data on graphite reinforced laminates made from solvent-coated and various hot-melt coated prepreg were generated. LARC-160, because of its liquid nature, can be easily autoclave processed to produce low void laminates. Liquid chromatographic fingerprints indicate good reaction control on resin scale ups. Minor changes in monomer ratios were also made to improve the thermal aging performance of graphite laminates.

Monoclonal antibody fragment removal mediated by mixed mode resins.

Science.gov (United States)

O'Connor, Ellen; Aspelund, Matthew; Bartnik, Frank; Berge, Mark; Coughlin, Kelly; Kambarami, Mutsa; Spencer, David; Yan, Huiming; Wang, William

2017-05-26

Efforts to increase monoclonal antibody expression in cell culture can result in the presence of fragmented species requiring removal in downstream processing. Capto adhere, HEA Hypercel, and PPA Hypercel anion exchange/hydrophobic interaction mixed mode resins were evaluated for their fragment removal capabilities and found to separate large hinge IgG1 antibody fragment (LHF) from monomer. Removal of greater than 75% of LHF population occurred at pH 8 and low conductivity. The mechanism of fragment removal was investigated in two series of experiments. The first experimental series consisted of comparison to chromatographic behavior on corresponding single mode resins. Both single mode anion exchange and hydrophobic interaction resins failed to separate LHF. The second experimental series studied the impact of phase modifiers, ethylene glycol, urea, and arginine on the mixed mode mediated removal. The addition of ethylene glycol decreased LHF removal by half. Further decreases in LHF separation were seen upon incubation with urea and arginine. Therefore, it was discovered that the purification is the result of a mixed mode phenomena dominated by hydrophobic interaction and hydrogen bonding effects. The site of interaction between the LHF and mixed mode resin was determined by chemical labeling of lysine residues with sulfo-NHS acetate. The labeling identified the antibody hinge and light chain regions as mediating the fragment separation. Sequence analysis showed that under separation conditions, a hydrophobic proline patch and hydrogen bonding serine and threonine residues mediate the hinge interaction with the Capto adhere ligand. Additionally, a case study is presented detailing the optimization of fragment removal using Capto adhere resin to achieve purity and yield targets in a manufacturing facility. This study demonstrated that mixed mode resins can be readily integrated into commercial antibody platform processes when additional chromatographic abilities

Chelating resin immobilizing carboxymethylated polyethyleneimine for selective solid-phase extraction of trace elements: Effect of the molecular weight of polyethyleneimine and its carboxymethylation rate.

Science.gov (United States)

Kagaya, Shigehiro; Kajiwara, Takehiro; Gemmei-Ide, Makoto; Kamichatani, Waka; Inoue, Yoshinori

2016-01-15

The effect of the molecular weight of polyethyleneimine (PEI), defined as a compound having two or more ethyleneamine units, and of its carboxymethylation rate (CM/N), represented by the ratio of ion-exchange capacity to the amount of N on the resin, on the selective solid-phase extraction ability of the chelating resin immobilizing carboxymethylated (CM) PEI was investigated. The chelating resins (24 types) were prepared by immobilization of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenehexamine, PEI300 (MW=ca. 300), and PEI600 (MW=ca. 600) on methacrylate resins, followed by carboxymethylation with various amounts of sodium monochloroacetate. When resins with approximately the same CM/N ratio (0.242-0.271) were used, the recovery of Cd, Co, Cu, Fe, Ni, Pb, Ti, Zn, and alkaline earth elements increased with increasing the molecular weight of PEIs under acidic and weakly acidic conditions; however, the extraction behavior of Mo and V was only slightly affected. This was probably due to the increase in N content of the resin, resulting in an increase in carboxylic acid groups; the difference in the molecular weight of PEIs immobilized on the resin exerts an insignificant influence on the selective extraction ability. The CM/N ratio considerably affected the extraction behavior for various elements. Under acidic and neutral conditions, the recovery of Cd, Co, Cu, Fe, Ni, Pb, Ti, and Zn increased with increasing CM/N values. However, under these conditions, the recovery of alkaline earth elements was considerably low when a resin with low CM/N ratio was used. This is presumably attributed to the different stability constants of the complexes of these elements with aminocarboxylic acids and amines, and to the electrostatic repulsion between the elements and the protonated amino groups in the CM-PEI. The recovery of Mo and V decreased or varied with increasing CM/N values, suggesting that the extraction of these elements occurred mainly

Fundulus heteroclitus gonadotropins.5: Small scale chromatographic fractionation of pituitary extracts into components with different steroidogenic activities using homologous bioassays

Directory of Open Access Journals (Sweden)

Petrino Teresa R

2004-03-01

Full Text Available Abstract Fractionation and characterization of gonadotropins (GtH from Fundulus heteroclitus pituitary extracts were carried out using a biocompatible liquid chromatographic procedure (Pharmacia FPLC system. Chromatographic fractions were monitored for gonadotropic activities (induction of oocyte maturation and steroid production using homologous follicle bioassays in vitro. Size-exclusion chromatography eluted gonadotropic activity in one major protein peak (Mr ~ 30,000. Anion-exchange and hydrophobic-interaction chromatography (HIC yielded two distinct peaks of 17beta-estradiol (E2- and 17alpha-hydroxy,20beta-dihydroprogesterone (DHP-promoting activity with associated oocyte maturation. Two-dimensional chromatography (chromatofocusing followed by HIC resolved pituitary extracts into two active fractions; both induced E2 synthesis, but one was relatively poor in eliciting DHP and testosterone production. Thus, using homologous bioassays, at least two quantitatively different gonadotropic (steroidogenic activities: an E2-promoting gonadotropin (GtH I-like and a DHP-promoting gonadotropin (GtH II-like, which has a lower isoelectric point but greater hydrophobicity than the former, can be distinguished from F. heteroclitus pituitaries by a variety of chromatographic procedures. This study complements previous biochemical and molecular data in F. heteroclitus and substantiates the duality of GtH function in a multiple-spawning teleost.

Development of Chromatographic Fingerprints of Eurycoma longifolia (Tongkat Ali Roots Using Online Solid Phase Extraction-Liquid Chromatography (SPE-LC

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Nor Nasriah Zaini

2016-04-01

Full Text Available E. longifolia is attracting interest due to its pharmacological properties and pro-vitality effects. In this study, an online SPE-LC approach using polystyrene divinyl benzene (PSDVB and C18 columns was developed in obtaining chromatographic fingerprints of E. longifolia. E. longifolia root samples were extracted using pressurized liquid extraction (PLE technique prior to online SPE-LC. The effects of mobile phase compositions and column switching time on the chromatographic fingerprint were optimized. Validation of the developed method was studied based on eurycomanone. Linearity was in the range of 5 to 50 µg∙mL−1 (r2 = 0.997 with 3.2% relative standard deviation of peak area. The developed method was used to analyze 14 E. longifolia root samples and 10 products (capsules. Selected chemometric techniques: cluster analysis (CA, discriminant analysis (DA, and principal component analysis (PCA were applied to the fingerprint datasets of 37 selected peaks to evaluate the ability of the chromatographic fingerprint in classifying quality of E. longifolia. Three groups were obtained using CA. DA yielded 100% correlation coefficient with 19 discriminant compounds. Using PCA, E. longifolia root samples were clearly discriminated from the products. This study showed that the developed online SPE-LC method was able to provide comprehensive evaluation of E. longifolia samples for quality control purposes.

A chromatographic determination of water in non-aqueous phases of solvent extraction systems

International Nuclear Information System (INIS)

Lyle, S.J.; Smith, D.B.

1975-01-01

The disadvantages of the Karl Fischer method for the determination of water in the non-aqueous phases of solvent extraction systems are pointed out, and a gas chromatographic method is described which is claimed to be potentially capable of overcoming these disadvantages. The method, as described, was developed to satisfy conditions relevant to measurement of the transfer rate of water from an aqueous phase into tri-n-butylphosphate in toluene, but it can be used for water determination in other solvent extraction systems. The apparatus used is described in detail. The concentration of water in water-saturated TBP was found to be 3.56 mol/litre, compared with a value of 3.55 obtained by Karl Fischer titration and previous literature values of 3.59 and 3.57. Measurements of water content in benzene solutions of long chain alkylamines were also sucessfully carried out. (U.K.)

Releasing Pattern of Applied Phosphorus and Distribution Change of Phosphorus Fractions in the Acid Upland Soils with Successive Resin Extraction

Directory of Open Access Journals (Sweden)

Arief Hartono

2008-05-01

Full Text Available The releasing pattern of applied P in the acid upland soils and the soil properties influencing the pattern were studied. Surface horizons of six acid upland soils from Sumatra, Java and Kalimantan were used in this study. The releasing pattern of applied P (300 mg P kg-1 of these soils were studied by successive resin extraction. P fractionation was conducted to evaluate which fractions released P to the soil solution after successive resin extraction. The cumulative of resin-Pinorganic (Pi release of soils was fitted to the first order kinetic. Regression analyses using factor scores obtained from the previous principal components analyses was applied to determine soil properties influencing P releasing pattern. The results suggested that the maximum P release was significantly (P < 0.05 increased by acidity plus 1.4 nm mineral-related factor (PC2 i.e. exchangeable Al and 1.4 nm minerals (smectite and vermiculite and decreased by oxide related factor (PC1 i.e. aluminum (Al plus 1/2 iron (Fe (by ammonium oxalate, crystalline Al and Fe oxides, cation exchange capacity, and clay content. P fractionation analysis after successive resin extraction showed that both labile and less labile in the form of NaHCO3-Pi and NaOH-Pi fractions, respectively, can be transformed into resin-Pi when in the most labile resin-Pi is depleted. Most of P released in high oxides soils were from NaOH-Pi fraction while in low oxides soils were from NaHCO3-Pi. P release from the former fraction resulted in the maximum P release lower than that of the latter one. When NaHCO3-Pi was high, NaOH-Pi was relatively more stable than NaHCO3-Pi despite resin-Pi removal. NaHCO3-Pi and NaOH-Pi are very important P fractions in replenishing resin-Pi in these acid upland soils.

Gas chromatographic determination of organic acids from fruit juices by combined resin mediated methylation and extraction in supercritical carbon dioxide.

Science.gov (United States)

Barden, T J; Croft, M Y; Murby, E J; Wells, R J

1997-10-17

A procedure in which anionic analytes, trapped on ion exchange resin, are simultaneously methylated and released using methyl iodide in either supercritical carbon dioxide or acetonitrile has been extended to polyfunctional organic acids. The combined SFE methylation of fruit juice acids trapped onto ion exchange resin proceeds in good yield producing the methyl esters of fumaric, succinic, malic, tartaric, isocitric and citric acids which are readily separated by GC. Using this procedure low concentrations of one acid can be detected and quantitated in the presence of very high concentrations of another. This new method detects tartaric acid at levels of 10 ppm in juices containing 10,000 ppm citric acid. Quantitation was performed either by using GC-FID with triethyl citrate or diethyl tartrate as internal standards or with the element specific calibration capability of the GC-AED. A simple new technique for the determination of citric/isocitric acid ratio is now available. Also, in contrast to HPLC methods, the identity of an analyte is readily confirmed by GC-MS.

Mixture-mixture design for the fingerprint optimization of chromatographic mobile phases and extraction solutions for Camellia sinensis.

Science.gov (United States)

Borges, Cleber N; Bruns, Roy E; Almeida, Aline A; Scarminio, Ieda S

2007-07-09

A composite simplex centroid-simplex centroid mixture design is proposed for simultaneously optimizing two mixture systems. The complementary model is formed by multiplying special cubic models for the two systems. The design was applied to the simultaneous optimization of both mobile phase chromatographic mixtures and extraction mixtures for the Camellia sinensis Chinese tea plant. The extraction mixtures investigated contained varying proportions of ethyl acetate, ethanol and dichloromethane while the mobile phase was made up of varying proportions of methanol, acetonitrile and a methanol-acetonitrile-water (MAW) 15%:15%:70% mixture. The experiments were block randomized corresponding to a split-plot error structure to minimize laboratory work and reduce environmental impact. Coefficients of an initial saturated model were obtained using Scheffe-type equations. A cumulative probability graph was used to determine an approximate reduced model. The split-plot error structure was then introduced into the reduced model by applying generalized least square equations with variance components calculated using the restricted maximum likelihood approach. A model was developed to calculate the number of peaks observed with the chromatographic detector at 210 nm. A 20-term model contained essentially all the statistical information of the initial model and had a root mean square calibration error of 1.38. The model was used to predict the number of peaks eluted in chromatograms obtained from extraction solutions that correspond to axial points of the simplex centroid design. The significant model coefficients are interpreted in terms of interacting linear, quadratic and cubic effects of the mobile phase and extraction solution components.

The difference of acrylic resin residual monomer levels with various polymerization method

Directory of Open Access Journals (Sweden)

Sherman Salim

2011-12-01

Full Text Available Background: After polymerization process, heat cured acrylic resin denture base actually still contains residual monomers that can become potential irritants later in oral cavity. Polymerization process is essential to obtain acrylic resin which can meet the requirements of the biocompatible and good physical properties. To meet the requirements, there are several methods of polymerization process used. Purpose: The purpose of this study was to determine the differences of the residual monomer levels of acrylic resin processed by various polymerization methods. Methods: Acrylic resin powder and liquid were mixed based on the rules of factory, and sample was made with size of 30 mm × 50 mm × 3 mm and then polymerized by using microwave at 70° C for 24 hours based on the methods of Japan Industrial Standard (JIS. Each group of samples was cut with weight of ± 0.2 g, dissolved in 5 ml of methyl ethyl ketone in test tubes, and then stored at ± 5° C for four days. Residual monomer level was conducted by using gas chromatograph mass spectrometer. Data obtained were then analyzed by using One-Way ANOVA test with p < 0.05. Results: After the level of polymerizing residual monomer with JIS method was compared to that at 70° C for 24 hours using microwave, it is known that there were significant differences (p < 0.05. Conclusion: The highest level of residual monomer of acrylic resin was that polymerized at 70° C for 24 hours.Latar belakang: Basis gigi tiruan yang berbahan dasar resin akrilik jenis heat cured setelah proses polimerisasi selesai masih mengandung monomer sisa yang berpotensi sebagai bahan iritan dalam rongga mulut. Proses polimerisasi sangat penting untuk mendapatkan resin akrilik yang memenuhi persyaratan biokompatibilitas dan fisik yang baik. Untuk persyaratan tersebut digunakan berbagai macam proses polimerisasi. Tujuan: Penelitian ini bertujuan untuk menentukan kadar monomer sisa resin akrilik yang diproses dengan metode

Preliminary extraction of tannins by 1-butyl-3-methylimidazole bromide and its subsequent removal from Galla chinensis extract using macroporous resins.

Science.gov (United States)

Lu, Chunxia; Luo, Xiaoling; Lu, Liliang; Li, Hongmin; Chen, Xia; Ji, Yong

2013-03-01

In recent years, ionic liquids have become increasingly attractive as 'green solvents' used in the extraction of bioactive compounds from natural plant. However, the separation of ionic liquid from the target compounds was difficult, due to their low vapour pressure and high stabilities. In our study, ionic liquid-based ultrasonic and microwave-assisted extraction was used to obtain the crude tannins, then the macroporous resin adsorption technology was further employed to purify the tannins and remove the ionic liquid from crude extract. The results showed that XDA-6 had higher separation efficiency than other tested resins, and the equilibrium experimental data were well fitted to Langmuir isotherms. Dynamic adsorption and desorption were performed on XDA-6 packed in glass columns to optimise the separation process. The optimum conditions as follows: the ratio of column height to diameter bed was 1:8, flow rate 1 BV/h (bed volume per hour), 85% ethanol was used as eluant while the elution volume was 2 BV. Under the optimised conditions, the adsorption and desoption rate of tannins in XDA-6 were 94.81 and 91.63%, respectively. The content of tannins was increased from 70.24% in Galla chinensis extract to 85.12% with a recovery of 99.06%. The result of ultra-performance liquid chromatography (UPLC)-MS/MS analysis showed that [bmim]Br could be removed from extract. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chromatographic separation process with pellicular ion exchange resins that can be used for ion or isotope separation and resins used in this process

International Nuclear Information System (INIS)

Carles, M.; Neige, R.; Niemann, C.; Michel, A.; Bert, M.; Bodrero, S.; Guyot, A.

1989-01-01

For separation of uranium, boron or nitrogen isotopes, an isotopic exchange is carried out betwen an isotope fixed on an ion exchange resin and another isotope of the same element in the liquid phase contacting the resin. Pellicular resins are used comprising composite particulates with an inert polymeric core and a surface layer with ion exchange groups [fr

Microwave assisted extraction, antioxidant potential and chromatographic studies of some Rasayana drugs.

Science.gov (United States)

Mishra, Ashish; Mishra, Shilpi; Bhargav, Shilpi; Bhargava, Cs; Thakur, Mayank

2015-07-01

To study and compare the conventional extraction procedure with microwave assisted extraction (MAE) for some Ayurvedic Rasayana drugs and to evaluate their antioxidant potential and carry out the characterization of extracts by thin layer chromatography. Three Ayurvedic rasayana plants Allium sativum Linn., Bombax ceiba Linn. and Inula racemosa Hook. were evaluated for an improved MAE methodology by determining the effects of grinding degree, extraction solvent, effect of dielectric constant and duration of time on the extractive value. Antioxidant potential of all three drugs was evaluated with 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging activity and reducing power was determined by using Gallic acid as standard. Further thin layer chromatographic (TLC) analysis was performed on pre-activated Silica Gel G plates and Rf value were compared with those reported for the important biomarkers. The total extractive value for Allium sativum Linn. was 36.95% (w/w) and 49.95% (w/w) for ethanol extraction respectively. In case of Bombax ceiba Linn. the yield of aqueous extract by MAE was 50% (w/w) compared to 42% (w/w) in ethanol (50% v/v). Percent yield of Inula racemosa Hook. in aqueous extract was found to be 27.55% (w/w) which was better than ethanol extract (50%) where the yield was 25.95% (w/w). Upon antioxidant activity evaluation. sativum extract showed an absorbance of 0.980±0.92 at concentration of 500 μg with maximum reducing capacity. This was followed by. ceiba Linn. 0.825±0.98 and. racemosa Hook. with 0.799±2.01 at a concentration of 500 μg. TLC based standardization of. sativum Linn. extract shows single spot with Rf value of 0.38, B. ceiba Linn. extract shows Rf values were 0.23, 0.58, 0.77, 0.92 and I. racemosa Hook. extract spot had a Rf value of 0.72. A significant improvement in extractive values was observed as a factor of time and other advantages by using MAE technology. All three drugs have high antioxidant potential and a TLC

Application of specific extraction chromatographic methods to the Rb-Sr, Sm-Nd isotope study of geological samples: The Hombreiro-Santa Eulalia Granite (Lugo, NW Spain)

OpenAIRE

Santos Zalduegui, J. F.; Pin, C.; Aranguren, A.; Gil Ibarguchi, José Ignacio

1996-01-01

The analytical application to geological samples of three new chromatographic resins, TRU-Spec ®, Sr-Spec ® and LN-Spec ®) has been investigated. Seven samples of the Hombreiro massif (Lugo, NW Spain) have been studied, that yield a Rb-Sr age of 298 ±5 Ma (SrQ = 0.7086, MSWD = 7.64) for the magma crystallization. Sm-Nd data results for the same massif give eNd values dose to -2 at 300 Ma. This suggests that the origin of the magma might be related to the partial melting of immature sediments,...

Determination of hexachlorocyclohexane pesticide residues in wool fat by a combined high-performance liquid chromatographic-gas-liquid chromatographic method

International Nuclear Information System (INIS)

Ali, S.L.

1978-01-01

Beta- and gamma-hexachlorocyclohexane residues were determined in twelve wool fat samples by using a combined high-performance liquid chromatographic (HPLC)-gas-liquid chromatographic (GLC) method. After extraction and chromatographic clean-up on a silca-gel column, the sample was further purified by HPLC on a reversed-phase C-18 column with methanol as the mobile phase. The final determination was effected by GLC with a 1-mCi nickel-63 electron-capture detector. The analytical method was checked by addition of carbon-14-labelled lindane and measurement of the radioactivity in a liquid scintillation counter. (Auth.)

Improved method for the extraction and chromatographic analysis on a fused-core column of ellagitannins found in oak-aged wine.

Science.gov (United States)

Navarro, María; Kontoudakis, Nikolaos; Canals, Joan Miquel; García-Romero, Esteban; Gómez-Alonso, Sergio; Zamora, Fernando; Hermosín-Gutiérrez, Isidro

2017-07-01

A new method for the analysis of ellagitannins observed in oak-aged wine is proposed, exhibiting interesting advantages with regard to previously reported analytical methods. The necessary extraction of ellagitannins from wine was simplified to a single step of solid phase extraction (SPE) using size exclusion chromatography with Sephadex LH-20 without the need for any previous SPE of phenolic compounds using reversed-phase materials. The quantitative recovery of wine ellagitannins requires a combined elution with methanol and ethyl acetate, especially for increasing the recovery of the less polar acutissimins. The chromatographic method was performed using a fused-core C18 column, thereby avoiding the coelution of main ellagitannins, such as vescalagin and roburin E. However, the very polar ellagitannins, namely, the roburins A, B and C, still partially coeluted, and their quantification was assisted by the MS detector. This methodology also enabled the analysis of free gallic and ellagic acids in the same chromatographic run. Copyright © 2017 Elsevier Ltd. All rights reserved.

Characterization of Group V Dubnium Homologs on DGA Extraction Chromatography Resin from Nitric and Hydrofluoric Acid Matrices

Energy Technology Data Exchange (ETDEWEB)

Despotopulos, J D; Sudowe, R

2012-02-21

somewhere between Nb and Pa. Much more recent studies have examined the properties of Db from HNO{sub 3}/HF matrices, and suggest Db forms complexes similar to those of Pa. Very little experimental work into the behavior of element 114 has been performed. Thermochromatography experiments of three atoms of element 114 indicate that the element 114 is at least as volatile as Hg, At, and element 112. Lead was shown to deposit on gold at temperatures about 1000 C higher than the atoms of element 114. Results indicate a substantially increased stability of element 114. No liquid phase studies of element 114 or its homologs (Pb, Sn, Ge) or pseudo-homologs (Hg, Cd) have been performed. Theoretical predictions indicate that element 114 is should have a much more stable +2 oxidation state and neutral state than Pb, which would result in element 114 being less reactive and less metallic than Pb. The relativistic effects on the 7p{sub 1/2} electrons are predicted to cause a diagonal relationship to be introduced into the periodic table. Therefore, 114{sup 2+} is expected to behave as if it were somewhere between Hg{sup 2+}, Cd{sup 2+}, and Pb{sup 2+}. In this work two commercially available extraction chromatography resins are evaluated, one for the separation of Db homologs and pseudo?homologs from each other as well as from potential interfering elements such as Group IV Rf homologs and actinides, and the other for separation of element 114 homologs. One resin, Eichrom's DGA resin, contains a N,N,N',N'-tetra-n-octyldiglycolamide extractant, which separates analytes based on both size and charge characteristics of the solvated metal species, coated on an inert support. The DGA resin was examined for Db chemical systems, and shows a high degree of selectivity for tri-, tetra-, and hexavalent metal ions in multiple acid matrices with fast kinetics. The other resin, Eichrom's Pb resin, contains a di-t-butylcyclohexano 18-crown-6 extractant with isodecanol solvent

Determination of low level of plutonium and uranium isotopes in safeguard swipe sample

Energy Technology Data Exchange (ETDEWEB)

Lee, Myung Ho; Park, Jong Ho; Oh, Seong Yong; Lee, Chang Heon; Ahn, Hong Ju; Song, Kyu Seok [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

2011-10-15

For the determination of radionuclides, the separation techniques based on the principles of anion exchange, liquid-liquid extraction or column extraction chromatography are frequently used in nuclear analytical applications. Recently, a novel extraction chromatographic resin has been developed by Horwitz and co-workers, which are capable of selective extraction of the actinides. General separation of plutonium and uranium with extraction chromatographic techniques are focused on the environmental or radioactive waste samples. Also, the chemical yields for Pu and U isotopes with extraction chromatographic method sometimes are variable. For effective extraction of Pu isotopes in the very level of plutonium sample with UTEVA resin, the valence adjustment of Pu isotopes in the sample solution requires due to unstability in the oxidation state of Pu isotopes during separation step. Therefore, it is necessary to develop a simple and robust radiochemical separation method for nano- or pico gram amounts of uranium and plutonium in safeguard swipe samples. Chemical yields of plutonium and uranium with extraction chromatographic method of Pu and U upgrades in this study were compared with several separation methods for Pu and U generally used in the radiochemistry field. Also, the redox reactions of hydrogen peroxide with plutonium in the nitric acid media were investigated by UV-Vis-NIR absorption spectroscopy. Based on general extraction chromatography method with UTEVA resin, the separation method of nano- and picogram amounts of uranium and plutonium in safeguard swipe samples was developed in this study

Optimization‐based framework for resin selection strategies in biopharmaceutical purification process development

Science.gov (United States)

Liu, Songsong; Gerontas, Spyridon; Gruber, David; Turner, Richard; Titchener‐Hooker, Nigel J.

2017-01-01

This work addresses rapid resin selection for integrated chromatographic separations when conducted as part of a high‐throughput screening exercise during the early stages of purification process development. An optimization‐based decision support framework is proposed to process the data generated from microscale experiments to identify the best resins to maximize key performance metrics for a biopharmaceutical manufacturing process, such as yield and purity. A multiobjective mixed integer nonlinear programming model is developed and solved using the ε‐constraint method. Dinkelbach's algorithm is used to solve the resulting mixed integer linear fractional programming model. The proposed framework is successfully applied to an industrial case study of a process to purify recombinant Fc Fusion protein from low molecular weight and high molecular weight product related impurities, involving two chromatographic steps with eight and three candidate resins for each step, respectively. The computational results show the advantage of the proposed framework in terms of computational efficiency and flexibility. © 2017 The Authors Biotechnology Progress published by Wiley Periodicals, Inc. on behalf of American Institute of Chemical Engineers Biotechnol. Prog., 33:1116–1126, 2017 PMID:28393478

Chromatographic evaluation and antimicrobial activity of Neem (Azadirachta indica A. Juss., Meliaceae leaves hydroalcoholic extracts

Directory of Open Access Journals (Sweden)

Priscila D. Alves

Full Text Available Neem (Azadirachta indica is an Indian tree well known for its several pharmacological activities, including antimicrobial activity. More than 300 composites have already been isolated and azadirachtin (AZA is its main active component. In the present work, Neem leaves hydroalcoholic extracts were prepared by percolation in 96% ethanol different concentrations (50%, 60%, 70%, 80% and 90% (v/v. The presence of AZA was tested by TLC by eluting the extracts and a standard solution of AZA through a chromatographic plate developed with anisaldehyde/sulfuric acid solution followed by heating. By HPLC, extracts elution took place on a C18 column, water:acetonitrile (60:40 as mobile phase, 1.0 mL/min flow rate and detection at λ217 nm. The extracts did not display AZA spots or peaks, however, they were tested against Gram-positive and Gram-negative bacteria, yeasts and a mold fungus. The extracts were tested in different increasing concentrations, in order to detect a dose-dependent relationship of the activity. Despite the absence of AZA, the 70% and 80% (v/v ethanol extracts showed activity against Staphylococcus aureus. However, this activity was not dose-dependent according to Tukey's test (q0,05;3;7.

Chromatography of metal ions with a triazine chelating resin

International Nuclear Information System (INIS)

Wang, W.N.

1979-05-01

The synthesis, characterization, and some analytical applications of a new triazine resin are described. Separation of group IB, IIB, VIB, and VIIB metal ions from group VIII metal ions is achieved by this PDT-4 resin. Calcium(II) and magnesium(II) are taken up at pH = 6, 0.1 M acetate and are eluted at pH = 6, 0.1 M sodium nitrate. Copper(II) is retained at pH = 6, 0.1 M acetate and pH = 1 hydrochloric acid and is eluted subsequently by 5 M perchloric acid. Molybdenum(VI) is sorbed selectively from 0.1 N sulfuric acid or hydrochloric acid and is eluted in a tight band by 0.1 N sodium hydroxide. Numerous rapid column chromatographic separations are reported using this new resin, including analysis of NBS standard samples

Preparation of extraction resin for radio lanthanides separation; Preparacion de resina de extraccion para separacion de radiolantanidos

Energy Technology Data Exchange (ETDEWEB)

Cruz B, C.C. de la; Monroy G, F. [ININ, 52750 La Marquesa, Estado de Mexico (Mexico)]. e-mail: delacruzbc@hotmail.com

2008-07-01

The present work presents the methodology that was developed for the preparation of one extractant resin with the aim of HDEHP, to separate radio lanthanides with serial atomic numbers. In this case it is exemplified with the separation of the following elements: Gadolinium-161 and the Terbium-161; this last radioisotope it is a beta emitting ({beta}{sup -}) that has a great potential to be used in therapy, also in nuclear medicine and in oncology, this is due to the high penetration power of their {beta}{sup -} particles that can kill to the cancerous cells and to inhibit the growth of the same ones. To be able to separate them it is necessary to appeal to extremely selective separation techniques, since the chemical properties of these elements are very similar. The chromatography is one of the more used analytical tools, this is due to its great sensibility and the selectivity in the compounds separation, in particular the use of the extractive chromatography has shown the feasibility of carrying out this type of separations for this type of elements. The resin with base of HDEHP was absorbed in an inert support under diverse preparation conditions. The extractant properties of the resin, in relation to the elements Gd and Tb (distribution coefficients), its were determined by means of the dynamic method, using as eluent solutions of nitric acid. The Gd-159 was prepared by irradiation of Gd-168 with thermal neutrons and the Tb-161 it is the result of the radioactive decay of the Gd-161 that is produced in turn with the irradiation with neutrons of Gd-160. The coefficients of distribution of Gd and Tb, using the prepared resin under diverse conditions are presented. (Author)

Synthesis and characterization of an N-(2-hydroxyethyl)-ethylenediaminetriacetic acid resin

International Nuclear Information System (INIS)

Lai, Y.F.

1977-10-01

A chelating ion-exchange resin with N-(2-hydroxyethyl)ethylene-diaminetriacetic acid (HEDTA) used as the ligand chemically bonded to XAD-4 by an ester linkage, HEDTA-4, was synthesized. It is stable under normal experimental conditions with the liquid chromatograph. The structure of the resin was confirmed by an infrared spectrum, and by potentiometric titrations. The capacity of the resin was also obtained by potentiometric titration and by a nitrogen analysis. The resin was used to pack a column of 5 mm internal diameter and 5 cm long. The effect of pH on the retention of different metal ions on the resin was studied. It was found that the resin was most selective for chromium(III), copper(II), lead(II), mercury(II), uranium(VI), zirconium(IV) and zinc(II) at a pH of less than 3. Furthermore, the resin proves to be functioning with a chelating mechanism rather than ion-exchange, and it can concentrate trace metal ions in the presence of a large excess of calcium and magnesium. This makes the resin potentially useful for purifying and analyzing drinking water

Extractability of water-soluble soil organic matter as monitored by spectroscopic and chromatographic analyses.

Science.gov (United States)

Nkhili, Ezzhora; Guyot, Ghislain; Vassal, Nathalie; Richard, Claire

2012-07-01

Cold and hot water processes have been intensively used to recover soil organic matter, but the effect of extraction conditions on the composition of the extracts were not well investigated. Our objective was to optimize the extraction conditions (time and temperature) to increase the extracted carbon efficiency while minimizing the possible alteration of water extractable organic matter of soil (WEOM). WEOM were extracted at 20°C, 60°C, or 80°C for 24 h, 10-60 min, and 20 min, respectively. The different processes were compared in terms of pH of suspensions, yield of organic carbon, spectroscopic properties (ultraviolet-visible absorption and fluorescence), and by chromatographic analyses. For extraction at 60°C, the time 30 min was optimal in terms of yield of organic carbon extracted and concentration of absorbing and fluorescent species. The comparison of WEOM 20°C, 24 h; 60°C, 30 min; and 80°C, 20 min highlighted significant differences. The content of total organic carbon, the value of specific ultraviolet absorbance (SUVA(254)), the absorbance ratio at 254 and 365 nm (E (2)/E (3)), and the humification index varied in the order: WEOM (20°C, 24 h) < WEOM (80°C, 20 min) < WEOM (60°C, 30 min). The three WEOM contained common fluorophores associated with simple aromatic structures and/or fulvic-like and common peaks of distinct polarity as detected by ultra performance liquid chromatography. For the soil chosen, extraction at 60°C for 30 min is the best procedure for enrichment in organic chemicals and minimal alteration of the organic matter.

Rapid and simultaneous determination of neptunium and plutonium isotopes in environmental samples by extraction chromatography using sequential injection analysis and ICP-MS

DEFF Research Database (Denmark)

Qiao, Jixin; Hou, Xiaolin; Roos, Per

2010-01-01

plutonium and neptunium in three reference materials were in agreement with the recommended or literature values at the 0.05 significance level. The developed method is suitable for the analysis of up to 10 g of soil and 20 g of seaweed samples. The extraction chromatographic separation within the SI system......This paper reports an automated analytical method for rapid and simultaneous determination of plutonium isotopes (239Pu and 240Pu) and neptunium (237Np) in environmental samples. An extraction chromatographic column packed with TrisKem TEVA® resin was incorporated in a sequential injection (SI...... for a single sample takes less than 1.5 h. As compared to batchwise procedures, the developed method significantly improves the analysis efficiency, reduces the labor intensity and expedites the simultaneous determination of plutonium and neptunium as demanded in emergency actions....

HPLC Characterization of Phenol-Formaldehyde Resole Resin Used in Fabrication of Shuttle Booster Nozzles

Science.gov (United States)

Young, Philip R.

1999-01-01

A reverse phase High Performance Liquid Chromatographic method was developed to rapidly fingerprint a phenol-formaldehyde resole resin similar to Durite(R) SC-1008. This resin is used in the fabrication of carbon-carbon composite materials from which Space Shuttle Solid Rocket Booster nozzles are manufactured. A knowledge of resin chemistry is essential to successful composite processing and performance. The results indicate that a high quality separation of over 35 peaks in 25 minutes were obtained using a 15 cm Phenomenex LUNA C8 bonded reverse phase column, a three-way water-acetonitrile-methanol nonlinear gradient, and LTV detection at 280 nm.

Novel chromatographic separation and carbon solid-phase extraction of acetanilide herbicide degradation products.

Science.gov (United States)

Shoemaker, Jody A

2002-01-01

One acetamide and 5 acetanilide herbicides are currently registered for use in the United States. Over the past several years, ethanesulfonic acid (ESA) and oxanilic acid (OA) degradation products of these acetanilide/acetamide herbicides have been found in U.S. ground waters and surface waters. Alachlor ESA and other acetanilide degradation products are listed on the U.S. Environmental Protection Agency's (EPA) 1998 Drinking Water Contaminant Candidate List. Consequently, EPA is interested in obtaining national occurrence data for these contaminants in drinking water. EPA currently does not have a method for determining these acetanilide degradation products in drinking water; therefore, a research method is being developed using liquid chromatography/negative ion electrospray/mass spectrometry with solid-phase extraction (SPE). A novel chromatographic separation of the acetochlor/alachlor ESA and OA structural isomers was developed which uses an ammonium acetate-methanol gradient combined with heating the analytical column to 70 degrees C. Twelve acetanilide degradates were extracted by SPE from 100 mL water samples using carbon cartridges with mean recoveries >90% and relative standard deviations < or =16%.

Autonomous gas chromatograph system for Thermal Enhanced Vapor Extraction System (TEVES) proof of concept demonstration

International Nuclear Information System (INIS)

Peter, F.J.; Laguna, G.R.

1996-09-01

An autonomous gas chromatograph system was designed and built to support the Thermal Enhanced Vapor Extraction System (TEVES) demonstration. TEVES is a remediation demonstration that seeks to enhance an existing technology (vacuum extraction) by adding a new technology (soil heating). A pilot scale unit was set up at one of the organic waste disposal pits at the Sandia National Laboratories Chemical Waste Landfill (CWL) in Tech Area 3. The responsibility for engineering a major part of the process instrumentation for TEVES belonged to the Manufacturing Control Subsystems Department. The primary mission of the one-of-a-kind hardware/software system is to perform on-site gas sampling and analysis to quantify a variety of volatile organic compounds (VOCs) from various sources during TEVES operations. The secondary mission is to monitor a variety of TEVES process physical parameters such as extraction manifold temperature, pressure, humidity, and flow rate, and various subsurface pressures. The system began operation in September 1994 and was still in use on follow-on projects when this report was published

Synergism in the sorption of europium on chromatographic supports impregnated with dicarbollide acid and bidentate phosphororganic extractant

International Nuclear Information System (INIS)

Svoboda, K.; Kyrs, M.; Vanura, P.

1997-01-01

Extraction chromatographic supports (XAD-7) impregnated with binary mixtures of cobalt dicarbollide and one of the two phosphororganic extractants (dibutyl-N,N-diethylcarbamoylmethyl phosphonate, DBDECMP, or octyl(phenyl)-N,N-diisobutylcarbamoylmethyl phosphine oxide, (CMPO) were prepared using methanolic solutions of the extractants and subsequent evaporation of methanol at room temperature. The molar ratios (x) in isomolar series of the two extractants were 0.025, 0.5, 0.75, and 1. The sorbents were used for investigating Eu capture from 0.1 and 1M HNO 3 solutions under static conditions (24 hours shaking, 2 cm 3 aqueous phase with 0.2 g sorbent, Eu initial concentrations 3 * 10 -9 , 0.0001, 0.001, 0.01 and 0.1M). The sorbents containing mixtures of extractants corresponding to the interpolated value x=0.45 (phosphororg./dicarb.) exhibited the highest values of the distribution ratios of Eu. A synergic effect of three orders of magnitude for low concentrations of Eu was observed. A tentative determination is given of the nature and the equilibrium constants of the chemical reactions assumed. (author)

Separation and purification of both tea seed polysaccharide and saponin from camellia cake extract using macroporous resin.

Science.gov (United States)

Yang, Pengjie; Zhou, Mingda; Zhou, Chengyun; Wang, Qian; Zhang, Fangfang; Chen, Jian

2015-02-01

A novel method to separate and purify tea seed polysaccharide and tea seed saponin from camellia cake extract by macroporous resin was developed. Among four kinds of resins (AB-8, NKA-9, XDA-6, and D4020) tested, AB-8 macroporous resin possessed optimal separating capacity for the two substances and thus was selected for the separation, in which deionized water was used to elute tea seed polysaccharide, 0.25% NaOH solution to remove the undesired pigments, and 90% ethanol to elute tea seed saponin. Further dynamic adsorption/desorption experiments on AB-8 resin-based column chromatography were conducted to obtain the optimal parameters. Under optimal dynamic adsorption and desorption conditions, 18.7 and 11.8% yield of tea seed polysaccharide and tea seed saponin were obtained with purities of 89.2 and 96.0%, respectively. The developed method provides a potential approach for the large-scale production of tea seed polysaccharide and tea seed saponin from camellia cake. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid-phase extraction with slurry injection of the resin into ETAAS for trace determination of thallium in natural water

International Nuclear Information System (INIS)

Isoshi, Nukatsuka; Hiroyuki, Seitoh; Kunio, Ohzeki

2004-01-01

Thallium in natural water samples was determined by electrothermal atomic absorption spectrometry after 1000-fold enrichment by mini solid-phase extraction from a 100-mL sample solution. A TI-pyrrolidine-1-carbodithioate complex formed in a sample solution of pH 1.6 was extracted on fine particles of a cellulose nitrate resin dispersed in the sample solution. The cellulose nitrate resin was then collected on a membrane filter (25 mm ) by filtration under suction using a glass funnel with an effective filtration area of 0.64 cm 2 . As a result, a circular thin layer of the resin phase with a diameter of 9 mm was obtained. Then the resin phase was carved out by an acrylate resin puncher with a 10-mm hole to put it into a sample cup containing 100 μL of 10 mM HNO 3 containing 0.5 mM NaCl. The resin phase was suspended in the solution by ultrasonication. 1000-fold enrichment was thus attained within 15 min, and the suspension was delivered to electrothermal atomic absorption spectrometry. The linear calibration graph was obtained in the range of 0-4 ng of TI in 100 mL of a sample solution. The detection limit obtained by 3 σ method was 0.19 ng. The proposed method was applied to the determination of TI in natural water samples. The results showed the concentration of TI in seawater was 12.1 ± 1.8 pg mL -1 for the calibration graph method and 12.6 ± 1.4 pg mL -1 for the standard addition method. A snowmelt sample contained 20.7 ± 1.0 pg mL -1 of TI. (author)

Separation and purification of rebaudioside A from extract of Stevia Rebaudiana leaves by macroporous adsorption resins

Directory of Open Access Journals (Sweden)

Anvari Masoumeh

2016-03-01

Full Text Available The separation and purification of rebaudioside A from Stevia rebaudiana crude extracts (Steviosides by macroporous resin were optimized by Taguchi orthogonal array (OA experimental design methodology. This approach was applied to evaluate the influence of five factors (adsorption temperature, desorption time, elution solution ratio, adsorption volume and type of resin on the rebaudioside A yield. The percentage contribution of each factor was also determined. The results showed that elution solution ratio and adsorption volume made the greatest (59.6% and the lowest (1.3% contribution, respectively. The results showed that the Taguchi method is able to model the purification of rebaudioside A process well (R2 > 0.998 and can therefore be applied in future studies conducted in various fields. Adsorption temperature 35°C, desorption time 60min, elution solution ratio 3, adsorption volume 200ml and HPD-400 as resin were the best conditions determined by the Taguchi method.

Separation and concentration of uranium by extraction chromatography : U(VI) - H3PO4 system

International Nuclear Information System (INIS)

Nobre, J.S.M.

1981-01-01

The feasibility of using the extraction chromatographic technique as a way to recover uranium from phosphatic rocks evaluated. The behaviour of uranium from raw phsophoric acid solutions in chromatographic systems using the mixture di(2-ethylhexyl) orthophosphoric acid (D2EHPA) - tributyl phosphate (TBP) as the stationary phase was studied. Materials as alumina, activated carbon and the macroporous resins XAD-4 and XAD-7 were used as supports for organic stationary phase. The best results were obtained with poliacrilic polymer XAD-7, due to its excellent chromatographic properties and efficient organic phase retention. Uranium was quantitatively retained by D2EHPA-TBP-XAD-7 columns from synthetic phosphoric acid solutions with typical composition of phosphatic acid liquors. The elution of uranium from this system was also studied, and the best results were obtained with phosphoric acid solutions. This chromatographic column presented a high stability, not changing their properties even after more than twenty cycles, including the conditioning, sorption, wasking and elution steps. Uranium determinations were perfpormed by indirect titration with potassium dichromate and by molecular absorption spectrophotometry with hydrogen peroxide- carbonate. A new and more sensitive method for uranium determination in phosphoric medium, which might be applied to acid liquors of phosphatic ores, was developed. An extraction-photometric method was used, with Arsenazo III (1,8-dihydroxynaphtalene-3,6-disulphonic acid-2,7-bis(azo-2)-phenylarsonic acid) as the reagent for uranium. (Author) [pt

Determination of oil reservoir radiotracer (S14CN−) in a single step using a plastic scintillator extractive resin

International Nuclear Information System (INIS)

Bagán, H.; Tarancón, A.; Stavsetra, L.; Rauret, G.; García, J.F.

2012-01-01

Highlights: ► A new procedure for S 14 CN − radiotracer determination using PS resin was established. ► The minimum detectable activity for a 100 mL sample is 0.08 Bq L −1 . ► The minimum quantifiable activity for a 100 mL sample is 0.31 Bq L −1 . ► PS resin is capable to quantify S 14 CN − radiotracer samples with errors lower than 5%. ► PS resin is also capable to quantify complex matrices obtained from oil reservoirs. - Abstract: The analysis of radiotracers is important in the study of oil reservoir dynamics. One of the most widely used radiotracer is S 14 CN − . Prior to activity measurements by Liquid Scintillation (LS), routine determinations require the pretreatment steps of purification and concentration of the samples using anion exchange columns. The final elution media produces samples with high salt concentration that may lead to problems with phase separation during the LS measurement. Plastic Scintillation (PS) is an alternative technique that provides a solid surface that can be used as a platform for the immobilisation of selective extractants to obtain a PS resin. The proposed procedure unifies chemical separation and sample measurement preparation in a single step, serving to reduce the number of reagents needed and manpower required for the analysis while also avoiding mixed waste production by LS. The objective of this study is to develop a PS resin for the determination of 14 C-labelled thiocyanate radiotracer in water samples. For this purpose, the immobilisation procedure was optimised, including optimisation of the proportion of PS microspheres:extractant and the use of a control blank to monitor the PS resin immobilisation process. The breakthrough volume was studied and the detection and quantification limits for 100 mL of sample were determined to be 0.08 Bq L −1 and 0.31 Bq L −1 , respectively. The established procedure was applied to active samples from oil reservoirs and errors lower than 5% in the sample

Two solid-phase recycling method for basic ionic liquid [C4mim]Ac by macroporous resin and ion exchange resin from Schisandra chinensis fruits extract.

Science.gov (United States)

Ma, Chun-hui; Zu, Yuan-gang; Yang, Lei; Li, Jian

2015-01-22

In this study, two solid-phase recycling method for basic ionic liquid (IL) 1-butyl-3-methylimidazolium acetate ([C4mim]Ac) were studied through a digestion extraction system of extracting biphenyl cyclooctene lignans from Schisandra chinensis. The RP-HPLC detection method for [C4mim]Ac was established in order to investigate the recovery efficiency of IL. The recycling method of [C4mim]Ac is divided into two steps, the first step was the separation of lignans from the IL solution containing HPD 5000 macroporous resin, the recovery efficiency and purity of [C4mim]Ac achieved were 97.8% and 67.7%, respectively. This method cannot only separate the lignans from [C4mim]Ac solution, also improve the purity of lignans, the absorption rate of lignans in [C4mim]Ac solution was found to be higher (69.2%) than that in ethanol solution (57.7%). The second step was the purification of [C4mim]Ac by the SK1B strong acid ion exchange resin, an [C4mim]Ac recovery efficiency of 55.9% and the purity higher than 90% were achieved. Additionally, [C4mim]Ac as solvent extraction of lignans from S. chinensis was optimized, the hydrolysis temperature was 90°C and the hydrolysis time was 2h. Copyright © 2014 Elsevier B.V. All rights reserved.

Behavior of copper (II )and uranium ( VI) in precipitation chromatography in the system anion exchange resin - hexacyanoferrate (II )

International Nuclear Information System (INIS)

Seneda, Jose Antonio

1997-01-01

In this work it is shown the efficiency of precipitation chromatography for separation and concentration of metallic elements by using a strong anionic-exchange resin saturated with hexacyanoferrate (II). Metallic cations, like Cu (II) and U (VI), are retained from highly diluted solutions and enriched into the resin, in the form of the correspondent insoluble hexacyanoferrate (II), precipitated inside the resin, which permitted the visual observation of a chromatographic zone on the top of the column. It will be discussed the conditions of sorption and elution of the cations uptake by the resin. This system permits the enrichment of the above mentioned cations onto the resin and offers the possibility of interesting separations as well. (author)

Multi-podant diglycolamides and room temperature ionic liquid impregnated resins: an excellent combination for extraction chromatography of actinides

NARCIS (Netherlands)

Gujar, R.B.; Ansari, S.A.; Verboom, Willem; Mohapatra, P.K.

2016-01-01

Extraction chromatography resins, prepared by impregnating two multi-podant diglycolamide ligands, viz. diglycolamide-functionalized calix[4]arene (C4DGA) and tripodal diglycolamide (T-DGA) dissolved in the room temperature ionic liquid 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide

Multi-podant diglycolamides and room temperature ionic liquid impregnated resins: An excellent combination for extraction chromatography of actinides.

Science.gov (United States)

Gujar, R B; Ansari, S A; Verboom, W; Mohapatra, P K

2016-05-27

Extraction chromatography resins, prepared by impregnating two multi-podant diglycolamide ligands, viz. diglycolamide-functionalized calix[4]arene (C4DGA) and tripodal diglycolamide (T-DGA) dissolved in the room temperature ionic liquid 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide (RTIL: C4mimTf2N) on Chromosorb-W (an inert solid support), gave excellent results for the removal of trivalent actinides from acidic waste solutions. Distribution coefficient measurements on several metal ions showed selective sorption of Am(III) over hexavalent uranyl ions and other fission product elements such as strontium and cesium. The sorbed metal ions could be efficiently desorbed with a complexing solution containing guanidine carbonate and EDTA buffer. The sorption of Am(III) on both resins followed pseudo-second order rate kinetics with rate constants of 1.37×10(-6) and 6.88×10(-7)g/cpmmin for T-DGA and C4DGA resins, respectively. The metal sorption on both resins indicated the Langmuir monolayer chemisorption phenomenon with Eu(III) sorption capacities of 4.83±0.21 and 0.52±0.05mg per g of T-DGA and C4DGA resins, respectively. The results of column studies show that these resins are of interest for a possible application for the recovery of hazardous trivalent actinides from dilute aqueous solutions. Copyright © 2016 Elsevier B.V. All rights reserved.

Molecularly Imprinted Polymers as Extracting Media for the Chromatographic Determination of Antibiotics in Milk

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Dimitrios Bitas

2018-02-01

Full Text Available Milk-producing animals are typically kept stationary in overcrowded large-scale farms and in most cases under unsanitary conditions, which promotes the development of infections. In order to maintain sufficient health status among the herd or promote growth and increase production, farmers administer preventative antibiotic doses to the animals through their feed. However, many antibiotics used in cattle farms are intended for the treatment of bacterial infections in humans. This results in the development of antibiotic-resistant bacteria which pose a great risk for public health. Additionally, antibiotic residues are found in milk and dairy products, with potential toxic effects for the consumers. Hence the need of antibiotic residues monitoring in milk arises. Analytical methods were developed for the determination of antibiotics in milk, with key priority given to the analyte extraction and preconcentration step. Extraction can benefit from the production of molecularly imprinted polymers (MIPs that can be applied as sorbents for the extraction of specific antibiotics. This review focuses on the principals of molecular imprinting technology and synthesis methods of MIPs, as well as the application of MIPs and MIPs composites for the chromatographic determination of various antibiotic categories in milk found in the recent literature.

Antioxidant and Antiangiogenic Properties, and Gas Chromatographic-Time of Flight Analysis of Sonchus arvensis Leaves Extracts

International Nuclear Information System (INIS)

Itam, A.; Shah, A. M.; Majid, A.; Ismail, Z.

2015-01-01

Sonchus arvensis L. (Asteraceae) is one of the medicinal herbs used in traditional medicines, in which the leaf extract was used as a diuretic, lithotriptic and antiurolithiasis agent. The leaves of S. arvensis reported contain several compounds, including a variety of flavonoids, terpenoids and sterol, even this plant also contain silica and potassium. Flavonoids are secondary metabolite compound which have ability as antioxidant. In this study, the aims are to determine of antioxidants and antiangiogenic properties, and phytoconstituents quantitative of aqueous and methanol extracts of S. arvensis leaves. The antioxidant properties were studied using 1,1-Diphenyl-2-picrylhydrazyl (DPPH) free radical, xanthine oxidase and beta-carotene-linoleate models system. Furthermore, the antiangiogenic property was evaluated using ex vivo rat aorta ring assay. Quantitative determination of extracts phytoconstituents were carried out by using Gas Chromatographic-Time of Flight (GC-TOF) mass spectrophotometric methods. The results showed that the aqueous and methanol extracts have ability as antioxidant which is antioxidant activities of aqueous extracts on DPPH radical and inhibition of xanthine oxidase activity are higher than that of methanol extracts. Meanwhile antioxidant activity using beta-carotene-linoleate model system of S. arvensis aqueous extract is lower than that of methanol extracts. Nevertheless, the differences of these antioxidant activities are not significant. Antiangiogenic property of aqueous extract is also higher than that of methanol extract which is measured at 100 meu g mL/sup -1/ of extracts. This indicates that there is correlation between antioxidant activity and antiangigenic property, exhibiting that this plant possesses the potential to prevent or cure the diseases that related to angiogenesis such as cancer. (author)

Production of lipase from Geotrichum sp and adsorption studies on affinity resin

Directory of Open Access Journals (Sweden)

E. S. KAMIMURA

1999-06-01

Full Text Available There is a growing interest in microbial lipase production due to its great potential for industrial applications such as food additives, industrial reagents and stain removers, as well as for medical applications. Specially for medical applications a high degree of purity is required, which is accomplished with high resolution chromatographic techniques. Affinity chromatography is considered a very high resolution chromatographic technique. In this work the adsorption isotherms and kinetics of the adsorption of lipase from Geotrichum sp on biospecific resin were determined. The resin was prepared using EAH sepharose 4B gel (Pharmacia, made to react with oleic acid as the specific ligand.The lipase was produced in a five-liter fermenter, with both complex and synthetic media. Fermentation conditions were a temperature of 30°C, an aeration of 1VVM and an agitation of 400 rpm. Maximum lipase activity was around 28 U/ml after 10 hours of fermentation for the complex medium. The kinetic model and parameters were determined by dynamic fitting to experimental results using the fourth-order Runge-Kutta method.

Separation and concentration of uranium by extraction chromatography : U(VI) - H/sub 3/PO/sub 4/ system

Energy Technology Data Exchange (ETDEWEB)

Nobre, J S.M.

1981-01-01

The feasibility of using the extraction chromatographic technique as a way to recover uranium from phosphatic rocks is evaluated. The behaviour of uranium from raw phsophoric acid solutions in chromatographic systems using the mixture di(2-ethylhexyl) orthophosphoric acid (D2EHPA) - tributyl phosphate (TBP) as the stationary phase was studied. Materials as alumina, activated carbon and the macroporous resins XAD-4 and XAD-7 were used as supports for organic stationary phase. The best results were obtained with poliacrilic polymer XAD-7, due to its excellent chromatographic properties and efficient organic phase retention. Uranium was quantitatively retained by D2EHPA-TBP-XAD-7 columns from synthetic phosphoric acid solutions with typical composition of phosphatic acid liquors. The elution of uranium from this system was also studied, and the best results were obtained with phosphoric acid solutions. This chromatographic column presented a high stability, not changing their properties even after more than twenty cycles, including the conditioning, sorption, washing and elution steps. Uranium determinations were perfpormed by indirect titration with potassium dichromate and by molecular absorption spectrophotometry with hydrogen peroxide- carbonate. A new and more sensitive method for uranium determination in phosphoric medium, which might be applied to acid liquors of phosphatic ores, was developed. An extraction-photometric method was used, with Arsenazo III (1,8-dihydroxynaphtalene-3,6-disulphonic acid-2,7-bis(azo-2)-phenylarsonic acid) as the reagent for uranium.

CHEMICAL COMPOSITIONS OF PINE RESIN, ROSIN AND TURPENTINE OIL FROM WEST JAVA

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Bambang Wiyono

2006-03-01

Full Text Available This study was conducted to identify chemical composition of merkus pine resin, rosin and turpentine oil. Initially, pine resin was separated into neutral and acidic fractions with an aqueous 4% sodium hydroxide solution. After methylation, the fraction containing turpentine oil and rosin were analyzed by gas chromatography (GC, and gas chromatograph mass spectrometry (GC-MS, respectively. The neutral fraction of pine resin and turpentine oil mainly consisted of a-pinene, D-3-carene and b-pinene. Based on mass spectral comparison, the major constituents of the acidic fraction and rosin were identified as sandaracopimaric acid, isopimaric acid, palustric acid, dehydroabietic acid, abietic acid, neoabietic acid, and merkusic acid. The major component of the acidic fractions was palustric acid, while that of rosin was abietic acid. Using TC (tough column 1 and TC 5 columns, levopimaric acid could not be separated from rosin or acidic fraction of pine resin of Indonesian Pinus merkusii.

Separation and determination of high-carbon alcohols using method of column chromatographic and gas-chromatographic analysis

International Nuclear Information System (INIS)

Kang Zhongrong; Li Biping; Zeng Yongchang

1988-01-01

This paper describes the separation and determination of high-carbon alcohols from amine extractant by using the method of column chromatography of aluminium oxide and gas-chromatographic analysis. The total conent of high-carbon alcohols is determined by the method of column chromatography, while the components of the high-carbon alcohols and their relative contents are determined by the method of gas-chromatography. A simple reliable and practical method is provided for the analysis of high-carbon alcohol from the amine extractant in this paper

High Performance Liquid Chromatographic Method for Determination of Dipyridamole in Human Plasma

Directory of Open Access Journals (Sweden)

DAVOOD BEIGI BAND ARAB ADI

1999-08-01

Full Text Available A simple, rapid and specific high-performance liquid chromatographic procedure is reported for"nquantitative determination of dipyridamole in human -plasma. The assay uses a reversed-phase"nhigh-performance liquid chromatographic (HPLC and UV detection at 280nm and has a limit"nof detection of approximately 5ng/mL. The mobile phase consists of MeOH-H20 (60:40"nadjusted to pH 3.3. Dipyridamole was extracted from plasma by back-extraction procedure, with"npropranolol as the internal standard. The reproducibility of the method is satisfactory

Effect of Green Tea Extract as Antioxidant on Shear Bond Strength of Resin Composite to in-Office and Home-Bleached Enamel

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Sharafeddin F

2016-09-01

Full Text Available Statement of Problem: Shear bond strength (SBS of home and office bleached enamel will be compromised by immediate application of composite restoration. Antioxidant agent may overcome this problem. Objectives: This in vitro study assessed the effect of green tea extract on shear bond strength of resin composite to in-office and home-bleached enamel. Materials and Methods: In this experimental study, 40 extracted intact human incisors were embedded in cylindrical acrylic resin blocks (2.5 ×1.5 cm, with the coronal portion above the cemento enamel junction out of the block. Then, after bleaching labial enamel surfaces of 20 teeth with 15% carbamide peroxide 6 hours a day for 5 days, they were randomly divided into two groups: A1 and A2 (n = 10, depending upon whether or not they are treated with antioxidant. Labial enamel surfaces of the remaining 20 teeth were bleached with 38% hydrogen peroxide before being randomly divided into groups B1 and B2 (n = 10, again depending on whether or not the antioxidant was used in their treatment . The experimental groups (A2,B2 were treated with 5% solution of green tea extract before resin composite restoration was done by a cylindrical Teflon mould (5×2 mm. Shear bond strength of the specimens was tested under a universal testing machine (Zwick/Roell Z020. The SBS data were analyzed by using One-way ANOVA and Tukey HSD tests (p < 0.05. Results: There were no statistically significant differences between shear bond strength of the control group (A1 and treated group (A2 but there were statistically significant differences between the groups B1 and B2 (p < 0.05. Conclusions: Application of antioxidant did not increase the shear bond strength of home-bleached enamel to resin composite but its application increased the shear bond strength of in-office bleached enamel to resin composite.

Refining of fossil resin flotation concentrate from western coal. Final report

Energy Technology Data Exchange (ETDEWEB)

Jensen, G.F.; Miller, J.D.

1995-02-16

During the past several years, significant research efforts have been made to develop process technology for the selective flotation of fossil resin from western coals. As a result of these efforts, several new flotation technologies have been developed. Operation of a proof-of-concept continuous flotation circuit showed the selective flotation process to be sufficiently profitable to justify the development of a fossil resin industry. However, little attention has been given to the refining of the fossil resin flotation concentrate although solvent refining is a critical step for the fossil resin to become a marketable product. In view of this situation, DOE funded this two-year project to evaluate the following aspects of the fossil resin refining technology: 1) Characterization of the fossil resin flotation concentrate and its refined products; 2) Kinetics of fossil resin extraction; 3) Effects of operating variables on solvent extraction; 4) Extraction solvents; 5) Proof-of-concept continuous refining tests; and 6) Technical and economic analysis. The results from this research effort have led to the following conclusions: Hexane- or heptane-refined fossil resin has a light-yellow color, a melting point of 140 - 142{degrees}C, a density of 1.034 gram/cm, and good solubility in nonpolar solvents. Among the four solvents evaluated (hexane, heptane, toluene and ethyl acetate), hexane is the most appropriate solvent based on overall technical and economic considerations. Batch extraction tests and kinetic studies suggest that the main interaction between the resin and the solvent is expected to be the forces associated with solvation phenomena. Temperature has the most significant effect on extraction rate. With hexane as the solvent, a recovery of 90% cam be achieved at 50{degrees}C and 10% solids concentration with moderate agitation for 1 hour.

Qualitative Analysis of Polyphenols in Macroporous Resin Pretreated Pomegranate Husk Extract by HPLC-QTOF-MS.

Science.gov (United States)

Abdulla, Rahima; Mansur, Sanawar; Lai, Haizhong; Ubul, Ablikim; Sun, Guangying; Huang, Guozheng; Aisa, Haji Akber

2017-09-01

Pomegranate (Punica granatum L.) husk is a traditional herbal medicine abundant in phenolic compounds and plays some roles in the treatment of oxidative stress, bacterial and viral infection, diabetes mellitus, and acute and chronic inflammation. Identification and determination of polyphenols in macroporous resin pretreated pomegranate husk extract by high performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (HPLC-QTOF-MS). The total polyphenols of pomegranate husk were prepared by ethanol extraction followed by pretreatment with HPD-300 macroporous resin. The polyphenolic compounds were qualitatively analysed by HPLC-QTOF-MS in negative electrospray ionisation (ESI) mode at different collision energy (CE) values. A total of 50 polyphenols were detected in the extract of pomegranate husk, including 35 hydrolysable tannins and 15 flavonoids with distinct retention time, fragmentation behaviours and characteristics, and the accurate mass-to-charge ratios at low, moderate and high CE values. Of these, we identified nine compounds for the first time in the pomegranate husk, including hexahydroxydiphenoyl-valoneoyl-glucoside (HHDP-valoneyl-glucoside), galloyl-O-punicalin, rutin, hyperoside, quercimeritrin, kaempferol-7-O-rhahmano-glucoside, luteolin-3'-O-arabinoside, luteolin-3'-O-glucoside, and luteolin-4'-O-glucoside. To validate the specificity and accuracy of mass spectrometry in the detection of polyphenols, as compared to the fragmentation pathways of granatin B in detail, including the HHDP-valoneyl- glucoside was first identified from pomegranate husk. The study provides evidence for the quality control and development of novel drugs based on polyphenols from the pomegranate husk. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Comparative study of resin sealant and resin modified glass ionomer as pit and fissure sealant

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Shirin Malek

2017-02-01

Full Text Available The purpose of the present study was to compare the marginal integrity of resin modified glass ionomer cement with that of resin sealant, in vitro. Forty artificial pit and fissure cavities were prepared in occlusal surface of extracted premolar teeth by using ¼ round carbide bur. Cavities were condensed with artificial organic debris followed by cleaning with prophylaxis pumice brush and paste and then separated into two treatment groups. In Group A, 15 fissure cavities were sealed by resin sealant and in Group B, 15 fissure cavities were sealed by resin modified glass ionomer sealant. These specimens were subjected to thermo-cycling followed by dye penetration test. The remaining 5 cavities from each group were analyzed for debris score by the SEM. The results of the microleakage test showed that the efficacy of preventing microleakage of samples sealed by resin modified glass ionomer sealant was higher than the samples sealed by resin sealant. However, no significant differences were found. It can be concluded that use of resin modified glass ionomer sealant is a good alternative for sealing pits and fissures.

21 CFR 177.2415 - Poly(aryletherketone) resins.

Science.gov (United States)

2010-04-01

... 12,000, as determined by gel permeation chromatography in comparison with polystyrene standards, and... calorimetry. (b) Optional adjuvant substances. The basic resins identified in paragraph (a) may contain... percent by weight as a residual solvent in the finished basic resin. (c) Extractive limitations. The...

Significance of wood extractives for wood bonding.

Science.gov (United States)

Roffael, Edmone

2016-02-01

Wood contains primary extractives, which are present in all woods, and secondary extractives, which are confined in certain wood species. Extractives in wood play a major role in wood-bonding processes, as they can contribute to or determine the bonding relevant properties of wood such as acidity and wettability. Therefore, extractives play an immanent role in bonding of wood chips and wood fibres with common synthetic adhesives such as urea-formaldehyde-resins (UF-resins) and phenol-formaldehyde-resins (PF-resins). Extractives of high acidity accelerate the curing of acid curing UF-resins and decelerate bonding with alkaline hardening PF-resins. Water-soluble extractives like free sugars are detrimental for bonding of wood with cement. Polyphenolic extractives (tannins) can be used as a binder in the wood-based industry. Additionally, extractives in wood can react with formaldehyde and reduce the formaldehyde emission of wood-based panels. Moreover, some wood extractives are volatile organic compounds (VOC) and insofar also relevant to the emission of VOC from wood and wood-based panels.

Comparison of TEVAR resin beads, PAN fibers, and ePTFE membranes as a solid support for Aliquat-336 in immobilized liquid extraction chromatography for separation of actinides

International Nuclear Information System (INIS)

Joe Dauner; Steve Workman

2012-01-01

The following paper covers a comparison of two new systems to traditional TEVA R resin systems for the analytical separation of actinides by immobilized liquid-liquid extraction using Aliquat-336. The new systems are using expanded polytetrafluroethane (ePTFE) membrane or polyacrylonitrile (PAN) fibers as the solid support. The systems are compared in two ways. First in how much Aliquat-336 they contain with the Vs, ratio of volume of Aliquat-336 to volume of polymeric support, being 0.158, 0.483, and 0.590 for the TEVA R resin, PAN fibers, and the ePTFE systems, respectively. The second comparison is in their performance capacity of extraction of uranyl chloride anion complex. The fiber and resins systems show similar capacities, and the membrane system being an order of magnitude less than the other systems. A cost comparison demonstrates the savings advantages of using a fiber based support compared with resin and membrane support systems. (author)

Comparative study using different resins to determine thorium isotopes

Energy Technology Data Exchange (ETDEWEB)

Rosa, Mychelle M.L.; Silva, Paulo S.C.; Maihara, Vera A., E-mail: my_linhares@yahoo.com.br, E-mail: pscsilva@ipen.br, E-mail: vmaihara@ipen.br [Instituto de Pesquisas Energéticas e Nucleares (IPEN/CNEN-SP), São Paulo, SP (Brazil); Taddei, Maria Helena T., E-mail: mhtaddei@cnen.gov.br [Comissão Nacional de Energia Nuclear (LAPOC/CNEN), Poços de Caldas, MG (Brazil). Laboratório de Pocos de Caldas; Cheberle, Luan T.V., E-mail: luancheberle@gmail.com [Ambientis Radioproteção, Barueri, SP (Brazil)

2017-07-01

Thorium is a naturally occurring radioactive element that is widely distributed in the crust of the Earth. This element is very common in mineral formations in regions with high levels of natural radioactivity, therefore, its determination in environmental samples is important. Thorium isotopes ({sup 228}Th, {sup 230}Th, and {sup 232}Th) were determined in a reference material, the IAEA Soil 327 sample, to validate the two methods employed using different resins. The initial preparation with acid dissolution is the same to both, in the first is used anion exchange resin (DOWEX 1 x 2) and electrodeposition in silver planchets. And in the second method is used a specific chromatographic resin (TEVA) and cerium fluoride microprecipitation. At the end both analysis are quantified by alpha spectrometry. The two methods the results obtained were satisfactory for the reference material used, with relative error of less than 4% for {sup 228}Th, {sup 230}Th, and {sup 232}Th. The main differences found between them were spectrums resolutions, time and cost of analysis. (author)

Determination of 3-chloro-1,2-propanediol in polyamideamine epichlorohydrin resin solution by reaction-based headspace gas chromatography.

Science.gov (United States)

Yan, Ning; Wan, Xiao-Fang; Chai, Xin-Sheng; Chen, Run-Quan

2018-04-01

We report on a headspace gas chromatographic method for determining the content of 3-chloro-1,2-propanediol in polyamideamine epichlorohydrin resin solution. It was based on quantitatively converting 3-chloro-1,2-propanediol to formaldehyde by periodate oxidation in a closed headspace sample vial at a room temperature for 10 min, and then to methanol by borohydride reduction at 90°C for 40 min followed by the headspace gas chromatographic measurement. The results showed that the present method has an excellent measurement precision (relative standard deviation < 2.60%) and accuracy (recoveries from 96.4-102%) in 3-chloro-1,2-propanediol analysis. The limit of quantitation was 0.031 mg/mL. It is simple and suitable for determining the 3-chloro-1,2-propanediol content in polyamideamine epichlorohydrin resin solution. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Mechanical characterisation of agarose-based chromatography resins for biopharmaceutical manufacture.

Science.gov (United States)

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

2017-12-29

Mechanical characterisation of agarose-based resins is an important factor in ensuring robust chromatographic performance in the manufacture of biopharmaceuticals. Pressure-flow profiles are most commonly used to characterise these properties. There are a number of drawbacks with this method, including the potential need for several re-packs to achieve the desired packing quality, the impact of wall effects on experimental set up and the quantities of chromatography media and buffers required. To address these issues, we have developed a dynamic mechanical analysis (DMA) technique that characterises the mechanical properties of resins based on the viscoelasticity of a 1ml sample of slurry. This technique was conducted on seven resins with varying degrees of mechanical robustness and the results were compared to pressure-flow test results on the same resins. Results show a strong correlation between the two techniques. The most mechanically robust resin (Capto Q) had a critical velocity 3.3 times higher than the weakest (Sepharose CL-4B), whilst the DMA technique showed Capto Q to have a slurry deformation rate 8.3 times lower than Sepharose CL-4B. To ascertain whether polymer structure is indicative of mechanical strength, scanning electron microscopy images were also used to study the structural properties of each resin. Results indicate that DMA can be used as a small volume, complementary technique for the mechanical characterisation of chromatography media. Copyright © 2017 The Author(s). Published by Elsevier B.V. All rights reserved.

Roughness comparison of heat cured type of acrylic resin in disinfectant solution immersion (Immersion in a solution of alkaline peroxide and 75% Celery extract (Apium graveolens L

Directory of Open Access Journals (Sweden)

Dewi Puspitasari

2016-08-01

Full Text Available Acrylic resin denture base has the properties absorbing that affecting physical and mechanical properties. One of the physical properties of acrylic resin is surface roughness. The aim of the study was to find out the roughness effect on heat cured acrylic that was immersed in alkaline peroxide and 75% celery (Apium graveoens L extract as a disinfectant solution. The study was a true experimental and posttest with control group designed with a rectangular shape size 65 x 10 x 3.3 mm based on the ISO standard 1567, six samples were used for alkaline peroxide, celery extract 75% and aquadest group for 5 and 15 days. A Surface Roughness Tester was used for the surface roughness changes observation. The statistical test used One-way ANOVA and post hoc Bonferroni. The results of this study showed the value of roughness on 5 days for alkaline peroxide (1.51 µm is greater than celery extract (0.36µm and aquadest (0.30 µm. The soaking for 15 days in alkaline peroxide (1.52 µm is greater than 75% celery extracts (0.38 µm and aquadest (0.34 µm. Alkaline peroxide caused higher roughness value of heat cured acrylic resin than 75% celery extract.

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.

Quantification and Purification of Mulberry Anthocyanins with Macroporous Resins

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Xueming Liu

2004-01-01

Full Text Available Total anthocyanins in different cultivars of mulberry were measured and a process for the industrial preparation of mulberry anthocyanins as a natural food colorant was studied. In 31 cultivars of mulberry, the total anthocyanins, calculated as cyanidin 3-glucoside, ranged from 147.68 to 2725.46 mg/L juice. Extracting and purifying with macroporous resins was found to be an efficient potential method for the industrial production of mulberry anthocyanins as a food colorant. Of six resins tested, X-5 demonstrated the best adsorbent capability for mulberry anthocyanins (91 mg/mL resin. The adsorption capacity of resins increased with the surface area and the pore radius. Residual mulberry fruit juice after extraction of pigment retained most of its nutrients, except for anthocyanins, and may provide a substrate for further processing.

A novel application of resin in pulp in the metallurgical industry

International Nuclear Information System (INIS)

Fleming, C.A.; Cromberge, G.

1985-01-01

The results are presented of several small-scale pilot-plant investigations that demonstrate the feasibility of a resin-in-pulp process for the combined extraction of gold and uranium. Both metals are leached into an aqueous solution as anionic complexes, and, under appropriate conditions, both metal anions can be stabilized in the same solution and extracted from that solution by anion-exchange resins. Three different lead materials containing gold and uranium were tested, and several configurations for leaching and the resin-in-pulp process were examined so that the efficiency of extraction of the process could be demonsrated. The results of the various pilot-plant investigations are discussed with particular emphasis on the deportment of gold and uranium during the leaching extraction, and elution steps

Determination of oil reservoir radiotracer (S{sup 14}CN{sup -}) in a single step using a plastic scintillator extractive resin

Energy Technology Data Exchange (ETDEWEB)

Bagan, H.; Tarancon, A. [Departament de Quimica Analitica, Universitat de Barcelona, Diagonal 645, E-08028 Barcelona (Spain); Stavsetra, L. [Department for Reservoir and Exploration Technology, Institute for Energy Technology (IFE), Instituttveien 18, N-2027 Kjeller (Norway); Rauret, G. [Departament de Quimica Analitica, Universitat de Barcelona, Diagonal 645, E-08028 Barcelona (Spain); Garcia, J.F., E-mail: jfgarcia@ub.edu [Departament de Quimica Analitica, Universitat de Barcelona, Diagonal 645, E-08028 Barcelona (Spain)

2012-07-29

Highlights: Black-Right-Pointing-Pointer A new procedure for S{sup 14}CN{sup -} radiotracer determination using PS resin was established. Black-Right-Pointing-Pointer The minimum detectable activity for a 100 mL sample is 0.08 Bq L{sup -1}. Black-Right-Pointing-Pointer The minimum quantifiable activity for a 100 mL sample is 0.31 Bq L{sup -1}. Black-Right-Pointing-Pointer PS resin is capable to quantify S{sup 14}CN{sup -} radiotracer samples with errors lower than 5%. Black-Right-Pointing-Pointer PS resin is also capable to quantify complex matrices obtained from oil reservoirs. - Abstract: The analysis of radiotracers is important in the study of oil reservoir dynamics. One of the most widely used radiotracer is S{sup 14}CN{sup -}. Prior to activity measurements by Liquid Scintillation (LS), routine determinations require the pretreatment steps of purification and concentration of the samples using anion exchange columns. The final elution media produces samples with high salt concentration that may lead to problems with phase separation during the LS measurement. Plastic Scintillation (PS) is an alternative technique that provides a solid surface that can be used as a platform for the immobilisation of selective extractants to obtain a PS resin. The proposed procedure unifies chemical separation and sample measurement preparation in a single step, serving to reduce the number of reagents needed and manpower required for the analysis while also avoiding mixed waste production by LS. The objective of this study is to develop a PS resin for the determination of {sup 14}C-labelled thiocyanate radiotracer in water samples. For this purpose, the immobilisation procedure was optimised, including optimisation of the proportion of PS microspheres:extractant and the use of a control blank to monitor the PS resin immobilisation process. The breakthrough volume was studied and the detection and quantification limits for 100 mL of sample were determined to be 0.08 Bq L{sup -1

The separation of tungsten and molybdenum by the formation of sulphide complexes and extraction into a weak-base resin

International Nuclear Information System (INIS)

Fleming, C.A.

1985-01-01

The separation of molybdenum from tungten can be achieved if a solution containing molybdate and tungstate ions is reacted with sulphide ions, and the molybdenum sulphide is extracted with an anion-exchangeresin. The separation between molybdenum and tungsten is influenced byfactors such as the pH value of the solution, the concentrations of sulphide and resin in the solution, and the period of contact between theresin and the metal ions in solution. A fundamental study of the interaction between sulphide ions and molybdate or tungstate ions confirmed a mechanism proposed recently in the literature: MeOsup(2-)sub(4)+nHSsup(-)+nHsup(+) is equivalent to MeO 4 sub(-n)Ssub(n)sup(2-)+nH 2 O, where Me = molybdenum or tungsten and n = 1, 2, 3, or 4. In these reaction sequences, each successive step in the reaction (sulphur being substituted for oxygen) is slower than the preceding one, and the molybdate reactions with sulphide are several orders of magnitude faster than the analogous tungsten reactions. As a result, the extent of the complexing of tungsten with sulphide is minimal compared with that of molybdenum in the time span of the extraction experiments. However, the current investigation shows that this is not the cause of the selectivity of anion-exchange resins for molybdenum in this system, and that the separation factor between molybdenum and tungsten is much the same for the precursor tungstate anion as it is for the various tungsten sulphide anions. The selectivity of the resin for molybdenum apparently originates from a thermodynamic preference of the amine functional group on the resin for molybdenum sulphide anions over tungstate or tungsten sulphide anions. It is shown that, under optimum conditions, a separation factor of about 30 between molybdenum and tungsten can be achieved in this system

Sensitive high performance liquid chromatographic method for the ...

African Journals Online (AJOL)

A new simple, sensitive, cost-effective and reproducible high performance liquid chromatographic (HPLC) method for the determination of proguanil (PG) and its metabolites, cycloguanil (CG) and 4-chlorophenylbiguanide (4-CPB) in urine and plasma is described. The extraction procedure is a simple three-step process ...

Purification of gamma-amino butyric acid (GABA) from fermentation of defatted rice bran extract by using ion exchange resin

Science.gov (United States)

Tuan Nha, Vi; Phung, Le Thi Kim; Dat, Lai Quoc

2017-09-01

Rice bran is one of the significant byproducts of rice processing with 10 %w/w of constitution of whole rice grain. It is rich in nutrient compounds, including glutamic acid. Thus, it could be utilized for the fermentation with Lactobateria for synthesis of GABA, a valuable bioactive for antihypertensive effects. However, the concentration and purity of GABA in fermentation broth of defatted rice bran extract is low for production of GABA drug. This research focused on the purification of GABA from the fermentation broth of defatted rice bran extract by using cation exchange resin. The results indicate that, the adsorption isotherm of GABA by Purelite C100 showed the good agreement with Freundlich model, with high adsorption capacity. The effects of pH and concentration of NaCl in eluent on the elution were also investigated. The obtained results show that, at the operating conditions of elution as follows: pH 6.5, 0.8 M of NaCl in eluent, 0.43 of bed volume; concentration of GABA in accumulative eluent, the purity and recovery yield of GABA were 743.8 ppm, 44.0% and 84.2%, respectively. Results imply that, it is feasible to apply cation exchange resin for purification of GABA from fermentation broth of defatted rice bran extract.

Effect of Resin Extract from Commiphora swynnertonii

African Journals Online (AJOL)

Dr Olaleye

of Commiphora swynnertonii resin on biochemical parameters in rats was investigated. Sixty rats were ... significantly elevated protein and albumin levels but had no significant effect on bilirubin and all the liver enzymes in the rats. These findings are ... hypoglycemic and hypolipidemic effects against high fat diet- induced ...

Simultaneous column chromatographic extraction and purification of abscisic acid in peanut plants for direct HPLC analysis.

Science.gov (United States)

Zhang, Ya-Wen; Fan, Wei-Wei; Li, Hui; Ni, He; Han, Han-Bing; Li, Hai-Hang

2015-10-01

Abscisic acid (ABA), a universal signaling molecule, plays important roles in regulating plant growth, development and stress responses. The low contents and complex components in plants make it difficult to be accurately analyzed. A novel one-step sample preparation method for ABA in plants was developed. Fresh peanut (Arachis hypogaea) plant materials were fixed by oven-drying, microwave drying, boiling or Carnoy's fixative, and loaded onto a mini-preparing column. After washed the impurities, ABA was eluted with a small amount of solvent. ABA in plant materials was completely extracted and purified in 2mL solution and directly analyzed by HPLC, with a 99.3% recovery rate. Multiple samples can be simultaneously prepared. Analyses using this method indicated that the endogenous ABA in oven-dried peanut leaves increased 20.2-fold from 1.01 to 20.37μgg(-1) dry weight within 12h and then decreased in 30% polyethylene glycol 6000 treated plants, and increased 3.34-fold from 0.85 to 2.84μgg(-1) dry weight in 5 days and then decreased in soil drought treated plants. The method combined the column chromatographic extraction and solid-phase separation technologies in one step and can completely extracted plant endogenous ABA in a purified and highly concentrated form for direct HPLC analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

Coffee contains cholinomimetic compound distinct from caffeine. I: Purification and chromatographic analysis.

Science.gov (United States)

Tse, S Y

1991-07-01

Both regular and decaffeinated coffees were found to have cholinomimetic actions when tested in urethane-anesthetized rats. These actions were distinct from those of caffeine and reversible by atropine. The bioactive fraction was purified from alcoholic extracts of instant decaffeinated coffee by liquid column chromatography and preparative TLC. The purified compound showed similar pharmacological actions as the starting material. Chromatographic behavior was further characterized by analytical TLC and HPLC. Chromatographic analyses of extracts of green coffee beans and roasted ground coffees showed that the cardioactive compound was only present in roasted coffees. Similar analyses of other commonly consumed beverages, including teas and cocoa, showed that this compound was not present in beverages besides coffee.

Gas chromatographic analysis of simmondsins and simmondsin ferulates in jojoba meal.

Science.gov (United States)

Van Boven, M; Holser, R; Cokelaere, M; Flo, G; Decuypere, E

2000-09-01

A capillary gas chromatographic method was developed for the simultaneous determination of simmondsins and simmondsin ferulates in jojoba meal, in detoxified jojoba meal, in jojoba meal extracts, and in animal food mixtures.

Copaifera multijuga ethanolic extracts, oil-resin, and its derivatives display larvicidal activity against Anopheles darlingi and Aedes aegypti (Diptera: Culicidae

Directory of Open Access Journals (Sweden)

Frances Tatiane Tavares Trindade

2013-06-01

Full Text Available Copaifera spp. is a common tree species found in the tropical region of Latin America, popularly known as copaiba or pau-d'alho. Oil-resin from different Copaifera species and its components present several biological activities such as antimicrobial, anti-inflammatory, antioxidant and insecticidal, including larvicidal activity against mosquitoes. Thus, bark and leaf ethanolic extracts, oil-resin, essential oil and alepterolic acid from Copaifera multijuga Hayne, Fabaceae, were tested as larvicides against the main malaria vector in the north of Brazil, Anopheles darlingi and also Aedes aegypti, the dengue vector. A. darlingi larval mortality was significantly higher than A. aegypti for most tested compounds. Bark and leaf extracts resulted in lower Lethal Concentrations (LC50 values for A. darlingi, 3 and 13 ppm, respectively, while the essential oil provided the lowest LC50 value for A. aegypti, 18 ppm. Despite of that, the lowest LC values were from the alepterolic acid for both species, i.e. 0.9 and 0.7 ppm for A. darlingi and A. aegypti, respectively.

Copaifera multijuga ethanolic extracts, oil-resin, and its derivatives display larvicidal activity against Anopheles darlingi and Aedes aegypti (Diptera: Culicidae

Directory of Open Access Journals (Sweden)

Frances Tatiane Tavares Trindade

2013-05-01

Full Text Available Copaifera spp. is a common tree species found in the tropical region of Latin America, popularly known as copaiba or pau-d'alho. Oil-resin from different Copaifera species and its components present several biological activities such as antimicrobial, anti-inflammatory, antioxidant and insecticidal, including larvicidal activity against mosquitoes. Thus, bark and leaf ethanolic extracts, oil-resin, essential oil and alepterolic acid from Copaifera multijuga Hayne, Fabaceae, were tested as larvicides against the main malaria vector in the north of Brazil, Anopheles darlingi and also Aedes aegypti, the dengue vector. A. darlingi larval mortality was significantly higher than A. aegypti for most tested compounds. Bark and leaf extracts resulted in lower Lethal Concentrations (LC50 values for A. darlingi, 3 and 13 ppm, respectively, while the essential oil provided the lowest LC50 value for A. aegypti, 18 ppm. Despite of that, the lowest LC values were from the alepterolic acid for both species, i.e. 0.9 and 0.7 ppm for A. darlingi and A. aegypti, respectively.

K Basin sludge/resin bead separation test report

International Nuclear Information System (INIS)

Squier, D.M.

1998-01-01

The K Basin sludge is an accumulation of fuel element corrosion products, organic and inorganic ion exchange materials, canister gasket materials, iron and aluminum corrosion products, sand, dirt and minor amounts of other organic material. The sludge will be collected and treated for storage and eventual disposal. This process will remove the large solid materials by a 1/4 inch screen. The screened material will be subjected to nitric acid in a chemical treatment process. The organic ion exchange resin beads produce undesirable chemical reactions with the nitric acid. The resin beads must be removed from the bulk material and treated by another process. An effective bead separation method must extract 95% of the resin bead mass without entraining more than 5% of the other sludge component mass. The test plan I-INF-2729, ''Organic Ion Exchange Resin Separation Methods Evaluation,'' proposed the evaluation of air lift, hydro cyclone, agitated slurry and elutriation resin bead separation methods. This follows the testing strategy outlined in section 4.1 of BNF-2574, ''Testing Strategy to Support the Development of K Basins Sludge Treatment Process''. Engineering study BNF-3128, ''Separation of Organic Ion Exchange Resins from Sludge,'' Rev. 0, focused the evaluation tests on a method that removed the fine sludge particles by a sieve and then extracted the beads by means of a elutriation column. Ninety-nine percent of the resin beads are larger than 125 microns and 98.5 percent are 300 microns and larger. Particles smaller than 125 microns make up the largest portion of sludge in the K Basins. Eliminating a large part of the sludge's non-bead component will reduce the quantity that is lifted with the resin beads in the elutriation column. Resin bead particle size distribution measurements are given in Appendix A The Engineering Testing Laboratory conducted measurements of a elutriation column's ability to extract resin beads from a sieved, non-radioactive sludge

Adsorption and desorption properties of macroporous resins for anthocyanins from the calyx extract of roselle (Hibiscus sabdariffa L.).

Science.gov (United States)

Chang, Xiu-Lian; Wang, Dong; Chen, Bi-Yun; Feng, Yong-Mei; Wen, Shao-Hong; Zhan, Peng-Yuan

2012-03-07

Adsorption of roselle anthocynins, a natural pigment, onto various macroporous resins was optimized to develop a simple and efficient process for industrial separation and purification of roselle anthocyanins. Nine different macroporous resins (AB-8, X-5, HPD-100, SP-207, XAD-4, LS-305A, DM-21, LS-610B, and LS-305) were evaluated for the adsorption properties of the anthocyanins extracted from the calyx extract of Hibiscus sabdariffa L. The influences of phase contact time, solution pH, initial anthocyanin concentration, and ethanol concentration with different citric acid amounts were studied by the static adsorption/desorption method. The adsorption isotherm data were fitted well to the Langmuir isotherm, and according to this model, LS-610B and LS-305 exhibited the highest monolayer sorption capacities of 31.95 and 38.16 mg/g, respectively. The kinetic data were modeled using pseudo-first-order, pseudo-second-order, and intraparticle diffusion equations. The experimental data were well described by the pseudo-second-order kinetic model. Continuous column adsorption-regeneration cycles indicated negligible capacity loss of LS-305 during operation. The overall yield of pigment product was 49.6 mg/g dried calyces. The content of roselle anthocynins in the pigment product was 4.85%.

Hypoglycaemic and hypolipidaemic effects of crude extracts and chromatographic fractions of Morinda morindoides root bark in diabetic rats

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Johnny Olufemi Olukunle

2012-01-01

Full Text Available Hypoglycaemic and hypolipidaemic effects of different extracts and fractions of root bark from the plant Morinda morindoides (Baker Milne-Redh of the family Rubiaceae were evaluated in alloxan-induced diabetic rats. The aqueous and methanolic extracts were administered to 48 rats orally at a dose of 400 mg·kg-1 for 21 days. Fractions (hydromethanol, hexane, chloroform and ethyl acetate from bio-activity guided fractionation and chromatographic sub fractions (CsF A-F from accelerated gradient chromatography were also evaluated in 45 rats for the hypoglycaemic activity at doses of 400 mg·kg-1, 200 mg·kg-1 and 100 mg·kg-1 of solvent fractions and (CsF A-F, respectively. Glibenclamide was used as positive control. Polyoxyethylene sorbitan monooleate and distilled water administered to rats were used as negative controls. The dose of 400 mg·kg-1 of aqueous and methanolic extracts and 100 mg·kg-1 of chloroform CsF B of Morinda morindoides caused (62.8%, 56% and 74%, respectively reductions in blood glucose level (BGL. The aqueous extract caused significant (P -1, low density lipoprotein (66.38 ± 2.5 mg·dl-1 and significant (P -1 when compared to the control. These results confirm the folkloric claim of the hypoglycaemic and hypolipidaemic activities of Morinda morindoides root bark.

A review of the development of resins for use in hydrometallurgy

International Nuclear Information System (INIS)

Green, B.R.

1985-01-01

Commercial resins, including cation exchangers, anion exchangers, and complexing resins, that may be suitable for use in the extraction of metals are reviewed. Areas where further research is required are considered, and potential applications that are of particular interest to the Council for Mineral Technology (Mintek), involving the recovery of uranium, gold, and the base metals, are described. Commercial resins and experimental resins developed at Mintek are evaluated, and the results are reviewed

Extraction of resins from WD-22 tank in Jose Cabrera Nuclear Power Plant

International Nuclear Information System (INIS)

Benavides, E.

1997-01-01

The Spent Resin Tank (WD-22) is located in the Auxiliary Building of Jose Cabrera Nuclear Plant (PWR 150 Mwe). This tank has a nominal capacity of 4 m 3 and is almost full of spent resins that has been stored from the late sixties to early eighties. As the lines are completely plugged with resins and due to the difficulties in the pipe lay-out, it has not been possible to transfer the resins to the cementation plant since that date. The plant decided, by an open bid quotation, to select the most suitable process to transfer the resins to the cementation plant avoiding the high doses existing in the tank cubicle and in a reasonable time schedule. The solution given in this paper contemplates that sometimes there is an imaginative answer to a problem that seems to be difficult to solve. (authors)

Solvent impregnated resin for isolation of U(VI) from industrial wastes

International Nuclear Information System (INIS)

Karve, M.; Rajgor, R.V.

2008-01-01

A solid-phase extraction method based upon impregnation of Cyanex 302 (bis(2,4,4- trimethylpentyl)mono-thio-phosphinic acid) on Amberlite XAD-2 resin is proposed for isolation of U(VI) from uranmicrolite ore tailing samples and industrial effluent samples. U(VI) was sorbed from nitric acid media on the solvent-impregnated resin (SIR) and was recovered completely with 1.0 M HCl. Based upon sorption behavior of U(VI) with Cyanex 302, it was quantitatively sorbed on the SIR in a dynamic method, while the other metal ions were not sorbed by the modified resin. The preparation of impregnated resin is simple, based upon physical interaction of the extractant and solid support, has good sorption capacity for U(VI), and is also reliable for detection of traces of U(VI). (authors)

Chromatographic separation of alkaline phosphatase from dental enamel

DEFF Research Database (Denmark)

Moe, D; Kirkeby, S; Salling, E

1989-01-01

Alkaline phosphatase (AP) was prepared from partly mineralized bovine enamel by extraction in phosphate buffer, centrifugation and various chromatographic techniques. Chromatofocusing showed that the enamel enzyme possessed five isoelectric points at the acid pH level ranging from pH 5.7 to pH 4.......4. Three enzyme peaks were eluted using low pressure chromatography with a Bio-gel column. With a HPLC gel filtration column the separation of the enamel extract resulted in only one peak with AP activity. The fractions of this peak were used to produce an antibody against bovine AP....

Development and evaluation of a gas chromatographic method for the determination of triazine herbicides in natural water samples

Science.gov (United States)

Steinheimer, T.R.; Brooks, M.G.

1984-01-01

A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0.1 ??g/L in a 1-litre sample. Three different natural water samples were used for error analysis via evaluation of recovery efficiencies and estimation of overall method precision. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0. 1 mu g/L in a 1-litre sample. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.

Cytotoxicity Evaluation of Two Bis-Acryl Composite Resins Using Human Gingival Fibroblasts.

Science.gov (United States)

Gonçalves, Fabiano Palmeira; Alves, Gutemberg; Guimarães, Vladi Oliveira; Gallito, Marco Antônio; Oliveira, Felipe; Scelza, Míriam Zaccaro

2016-01-01

Bis-acryl resins are used for temporary dental restorations and have shown advantages over other materials. The aim of this work was to evaluate the in vitro cytotoxicity of two bis-acryl composite resins (Protemp 4 and Luxatemp Star), obtained at 1, 7 and 40 days after mixing the resin components, using a standardized assay employing human primary cells closely related to oral tissues. Human gingival fibroblast cell cultures were exposed for 24 h to either bis-acryl composite resins, polystyrene beads (negative control) and latex (positive control) extracts obtained after incubation by the different periods, at 37 °C under 5% CO2. Cell viability was evaluated using a multiparametric procedure involving sequential assessment (using the same cells) of mitochondrial activity (XTT assay), membrane integrity (neutral red test) and total cell density (crystal violet dye exclusion test). The cells exposed to the resin extracts showed cell viability indexes exceeding 75% after 24 h. Even when cells were exposed to extracts prepared with longer conditioning times, the bis-acryl composite resins showed no significant cytotoxic effects (p>0.05), compared to the control group or in relation to the first 24 h of contact with the products. There were no differences among the results obtained for the bis-acryl composite resins evaluated 24 h, 7 days and 40 days after mixing. It may be concluded that the bis-acryl resins Protemp 4 and Luxatemp Star were cytocompatible with human gingival fibroblasts, suggesting that both materials are suitable for use in contact with human tissues.

Chromatographic decontamination of medium-activity waste concentrates

International Nuclear Information System (INIS)

Faubel, W.; Menzler, P.M.; Sameh, A.A.

1988-01-01

The chromatographic decontamination of a MAW concentrate was carried out in a laboratory plant in 1-l-batches in the following way: In order to purify the nitric MAW concentrate from its solid and organic contamination products, it is passed through a filter and an absorber (SM7) for organic species. Subsequently the purified solution runs on-line through all following columns. First the main activity carrier cesium ( 137 Cs, 134 Cs) is transferred to ammonium molybdate phosphate (AMP-1) by means of a newly developed fluidized bed process. In the further course, 125 Sb is separated on metal oxides (Sb 2 O 5 , MnO 2 ) and the three-valued actinides/lanthanides on an extraction-chromatographic CMPO column. Finally the remaining 106 Ru and 60 Co activities are separated on dimethylglyoximes (DMG) coated on active carbon. (orig./RB) [de

Phosphorus extracted by ion exchange resins and mehlich-1 from oxisols (latosols treated with different phosphorus rates and sources for varied soil-source contact periods

Directory of Open Access Journals (Sweden)

Irio Fernando de Freitas

2013-06-01

Full Text Available Despite the large number of studies addressing the quantification of phosphorus (P availability by different extraction methods, many questions remain unanswered. The aim of this paper was to compare the effectiveness of the extractors Mehlich-1, Anionic Resin (AR and Mixed Resin (MR, to determine the availability of P under different experimental conditions. The laboratory study was arranged in randomized blocks in a [(3 x 3 x 2 + 3] x 4 factorial design, with four replications, testing the response of three soils with different texture: a very clayey Red Latosol (LV, a sandy clay loam Red Yellow Latosol (LVA, and a sandy loam Yellow Latosol (LA, to three sources (triple superphosphate, reactive phosphate rock from Gafsa-Tunisia; and natural phosphate from Araxá-Minas Gerais at two P rates (75 and 150 mg dm-3, plus three control treatments (each soil without P application after four contact periods (15, 30, 60, and 120 days of the P sources with soil. The soil acidity of LV and LVA was adjusted by raising base saturation to 60 % with the application of CaCO3 and MgCO3 at a 4:1 molar ratio (LA required no correction. These samples were maintained at field moisture capacity for 30 days. After the contact periods, the samples were collected to quantify the available P concentrations by the three extractants. In general, all three indicated that the available P-content in soils was reduced after longer contact periods with the P sources. Of the three sources, this reduction was most pronounced for triple superphosphate, intermediate for reactive phosphate, while Araxá phosphate was least sensitive to the effect of time. It was observed that AR extracted lower P levels from all three soils when the sources were phosphate rocks, while MR extracted values close to Mehlich-1 in LV (clay and LVA (medium texture for reactive phosphate. For Araxá phosphate, much higher P values were determined by Mehlich-1 than by the resins, because of the acidity of

Treatment method for stabilization of radioactive exchange resin

International Nuclear Information System (INIS)

Hideo, Oni; Takashi, Miyake; Hitoshi, Miyamoto; Toshio, Funakoshi; Yuzo, Inagaki.

1988-01-01

This is a method for eluting radioactive nuclides from a radioactive ion exchange resin in which it has been absorbed. First, the Cs in this resin is extracted using a neutral salt solution which contains Na + . The Cs that has been transferred to the neutral salt solution is absorbed and expelled by inorganic ion exchangers. Then the Co, Fe, Mn and Sr in said resin are eluted using an acidic solution; the Co, Fe, Mn and Sr that have been transferred to the acidic solution are separated from that solution by means of a diffusion dialysis vat. This process is a unique characteristic of this ion exchange resin treatment method. 1 fig

Determination of Pb-210 and actinides by extraction chromatography and anion exchange chromatography

International Nuclear Information System (INIS)

Kalmykov, St.N.; Sapozhnikov, Yu.A.

1997-01-01

This work is devoted to the determination of Pb-210 and actinides (Pu-238, Pu-239, Am-241, U-235, U-238, Th-232) by means of highly selective chromatographic resins and anion exchangers. The special interest was paid to the analysis of large quantities of samples with high concentration of competitive ions like ocean sediments, bone ash and others.The commercially available TRU-Spec chromatographic resins was used for separation of actinides from the matrix. Then U, Th, Am, and Pu were separated from other using anion exchange chromatography with AG-1X4 anionite in Cl - form, electro-deposed and α-counted.Pb-21- and Bi-210 were determined by liquid scintillation counting. The developed procedure is rather express, effective and could be adopted for the determination of radionuclides like Ba-133, Ra, Np-239

Separation of aliphatic carboxylic acids and benzenecarboxylic acids by ion-exclusion chromatography with various cation-exchange resin columns and sulfuric acid as eluent.

Science.gov (United States)

Ohta, Kazutoku; Ohashi, Masayoshi; Jin, Ji-Ye; Takeuchi, Toyohide; Fujimoto, Chuzo; Choi, Seong-Ho; Ryoo, Jae-Jeong; Lee, Kwang-Pill

2003-05-16

The application of various hydrophilic cation-exchange resins for high-performance liquid chromatography (sulfonated silica gel: TSKgel SP-2SW, carboxylated silica gel: TSKgel CM-2SW, sulfonated polymethacrylate resin: TSKgel SP-5PW, carboxylated polymethacrylate resins: TSKgel CM-5PW and TSKgel OA-Pak A) as stationary phases in ion-exclusion chromatography for C1-C7 aliphatic carboxylic acids (formic, acetic, propionic, butyric, isovaleric, valeric, isocaproic, caproic, 2-methylhexanoic and heptanoic acids) and benzenecarboxylic acids (pyromellitic, trimellitic, hemimellitic, o-phthalic, m-phthalic, p-phthalic, benzoic, salicylic acids and phenol) was carried out using diluted sulfuric acid as the eluent. Silica-based cation-exchange resins (TSKgel SP-2SW and TSKgel CM-2SW) were very suitable for the ion-exclusion chromatographic separation of these benzenecarboxylic acids. Excellent simultaneous separation of these benzenecarboxylic acids was achieved on a TSKgel SP-2SW column (150 x 6 mm I.D.) in 17 min using a 2.5 mM sulfuric acid at pH 2.4 as the eluent. Polymethacrylate-based cation-exchange resins (TSKgel SP-5PW, TSKgel CM-5PW and TSKgel OA-Pak A) acted as advanced stationary phases for the ion-exclusion chromatographic separation of these C1-C7 aliphatic carboxylic acids. Excellent simultaneous separation of these C1-C7 acids was achieved on a TSKgel CM-5PW column (150 x 6 mm I.D.) in 32 min using a 0.05 mM sulfuric acid at pH 4.0 as the eluent.

Selective extraction of U(VI) over Th(IV) from acidic streams using di-bis(2-ethylhexyl) malonamide anchored chloromethylated polymeric matrix

Energy Technology Data Exchange (ETDEWEB)

Prabhakaran, D.; Subramanian, M.S. [Department of Chemistry, Indian Institute of Technology, Chennai 600036 (India)

2005-01-15

A new chelating polymeric sorbent has been developed using Merrifield chloromethylated resin anchored with di-bis (2-ethylhexyl) malonamide (DB2EHM). The modified resin was characterized by {sup 13}C CPMAS NMR spectroscopy, FT-NIR-FIR spectroscopy, CHN elemental analysis and also by thermo gravimetric analysis. The fabricated sorbent showed superior binding affinity for U(VI) over Th(IV) and other diverse ions, even under high acidities. Various physio-chemical parameters, like solution acidity, phase exchange kinetics, metal sorption capacity, electrolyte tolerance studies, etc., influencing the resin's metal extractive behavior were studied by both static and dynamic method. Batch extraction studies performed over a wide range of solution acidity (0.01-10M) revealed that selective extraction of U(VI) could be achieved even up to 4M acidity with distribution ratios (D) in the order of circa 10{sup 3}. The phase exchange kinetics studies performed for U(VI) and Th(IV) revealed that time duration of <15min was sufficient for >99.5% extraction. But similar studies when preformed for trivalent lanthanides gave very low D values (<50), with the extraction time extending up to 60min. The metal sorption studies performed for U(VI) and Th(IV) at 5M HNO{sub 3} was found to be 62.5 and 38.2mgg{sup -1},respectively. Extraction efficiency in the presence of inferring electrolyte species and inorganic cations were also examined. Metal ion desorption was effective using 10-15mL of 1M (NH{sub 4}){sub 2}CO{sub 3} or 0.5M {alpha}-hydroxy isobutyric acid (HIBA). Extraction studies performed on a chromatographic column at 5M acidity were found to give enrichment factor values of 310 and 250 for U(VI) and Th(IV), respectively. The practical utility of the fabricated chelating sorbent and its efficiency to extract actinides from acidic waste streams was tested using a synthetic nuclear spent fuel solution. The R.S.D. values obtained on triplicate measurements (n = 3) were within

Evaluation of selectivity in homologous multimodal chromatographic systems using in silico designed antibody fragment libraries.

Science.gov (United States)

Karkov, Hanne Sophie; Woo, James; Krogh, Berit Olsen; Ahmadian, Haleh; Cramer, Steven M

2015-12-24

This study describes the in silico design, surface property analyses, production and chromatographic evaluations of a diverse set of antibody Fab fragment variants. Based on previous findings, we hypothesized that the complementarity-determining regions (CDRs) constitute important binding sites for multimodal chromatographic ligands. Given that antibodies are highly diversified molecules and in particular the CDRs, we set out to examine the generality of this result. For this purpose, four different Fab fragments with different CDRs and/or framework regions of the variable domains were identified and related variants were designed in silico. The four Fab variant libraries were subsequently generated by site-directed mutagenesis and produced by recombinant expression and affinity purification to enable examination of their chromatographic retention behavior. The effects of geometric re-arrangement of the functional moieties on the multimodal resin ligands were also investigated with respect to Fab variant retention profiles by comparing two commercially available multimodal cation-exchange ligands, Capto MMC and Nuvia cPrime, and two novel multimodal ligand prototypes. Interestingly, the chromatographic data demonstrated distinct selectivity trends between the four Fab variant libraries. For three of the Fab libraries, the CDR regions appeared as major binding sites for all multimodal ligands. In contrast, the fourth Fab library displayed a distinctly different chromatographic behavior, where Nuvia cPrime and related multimodal ligand prototypes provided markedly improved selectivity over Capto MMC. Clearly, the results illustrate that the discriminating power of multimodal ligands differs between different Fab fragments. The results are promising indications that multimodal chromatography using the appropriate multimodal ligands can be employed in downstream bioprocessing for challenging selective separation of product related variants. Copyright © 2015 Elsevier B

Extraction of anthocyanins from black bean canning wastewater with macroporous resins.

Science.gov (United States)

Wang, Xiaoxi; Hansen, Conly; Allen, Karin

2014-02-01

This study investigated purification of anthocyanins from black bean canning wastewater by column chromatography with 5 types of macroporous resins (Diaion Hp20, Sepabeads Sp70, Sepabeads Sp207, Sepabeads Sp700, and Sepabeads Sp710). By-product of canned black beans was partially purified by filtration, in anticipation of higher performance during column chromatography. Equilibrium adsorption isotherms were measured and analyzed using Langmuir and Freundlich isotherm models. Both Langmuir (all R² ≥ 0.98) and Freundlich (all R² ≥ 0.97) models can describe the adsorption process of anthocyanins from black bean canning wastewater using the tested resins. The adsorption and desorption behaviors of anthocyanins were studied using a dynamic method on the 5 types of resins, and Sp700 presented the highest adsorption capacity (39 ± 4 mg/g; P canning wastewater. © 2014 Institute of Food Technologists®

Dual liquid and gas chromatograph system

Science.gov (United States)

Gay, D.D.

A chromatographic system is described that utilizes one detection system for gas chromatographic and micro-liquid chromatographic determinations. The detection system is a direct-current, atmospheric-pressure, helium plasma emission spectrometer. The detector utilizes a nontransparent plasma source unit which contains the plasma region and two side-arms which receive effluents from the micro-liquid chromatograph and the gas chromatograph. The dual nature of this chromatographic system offers: (1) extreme flexibility in the samples to be examined; (2) extreme low sensitivity; (3) element selectivity; (4) long-term stability; (5) direct correlation of data from the liquid and gas samples; (6) simpler operation than with individual liquid and gas chromatographs, each with different detection systems; and (7) cheaper than a commercial liquid chromatograph and a gas chromatograph.

Gas chromatographic-mass spectrometric determination of hydrophilic compounds in environmental water by solid-phase extraction with activated carbon fiber felt.

Science.gov (United States)

Kawata, K; Ibaraki, T; Tanabe, A; Yagoh, H; Shinoda, A; Suzuki, H; Yasuhara, A

2001-03-09

Simple gas chromatographic-mass spectrometric determination of hydrophilic organic compounds in environmental water was developed. A cartridge containing activated carbon fiber felt was made by way of trial and was evaluated for solid-phase extraction of the compounds in water. The hydrophilic compounds investigated were acrylamide, N,N-dimethylacetamide, N,N-dimethylformamide, 1,4-dioxane, furfural, furfuryl alcohol, N-nitrosodiethylamine and N-nitrosodimethylamine. Overall recoveries were good (80-100%) from groundwater and river water. The relative standard deviations ranged from 4.5 to 16% for the target compounds. The minimum detectable concentrations were 0.02 to 0.03 microg/l. This method was successfully applied to several river water samples.

Gas chromatographic determination of calcium propionate added as preservative to bread.

Science.gov (United States)

Lamkin, W M; Unruh, N C; Pomeranz, Y

1987-01-01

A simple and rapid gas chromatographic procedure was developed for determining low concentrations of propionate added as a preservative to bread. A bread sample to be analyzed was ground in a meat grinder with a 3 mm hole plate and finely divided by rubbing through a No. 8 sieve. The propionate was then extracted into 0.050M formic acid in a blender at low speed for 5 min, and an aliquot of a filtrate was analyzed directly by gas chromatography. Chromatographic separation was accomplished on a Carbopack C column coated with 0.3% (w/w) Carbowax 20M and 0.1% (w/w) phosphoric acid. Less than 0.2 ppm propionic acid could be detected in the aqueous extract. Over the range of 0.03-0.23% calcium propionate, average relative error was -1.20% with an average coefficient of variation of 2.02%.

using Supercritical Fluid Extraction

African Journals Online (AJOL)

Methods: Supercritical CO2 extraction technology was adopted in this experiment to study the process of extraction of volatile oil from Polygonatum odoratum while gas chromatograph-mass spectrometer ..... Saponin rich fractions from.

Characterization of dextran-grafted hydrophobic charge-induction resins: Structural properties, protein adsorption and transport.

Science.gov (United States)

Liu, Tao; Angelo, James M; Lin, Dong-Qiang; Lenhoff, Abraham M; Yao, Shan-Jing

2017-09-29

The structural and functional properties of a series of dextran-grafted and non-grafted hydrophobic charge-induction chromatographic (HCIC) agarose resins were characterized by macroscopic and microscopic techniques. The effects of dextran grafting and mobile phase conditions on the pore dimensions of the resins were investigated with inverse size exclusion chromatography (ISEC). A significantly lower pore radius (17.6nm) was found for dextran-grafted than non-grafted resins (29.5nm), but increased salt concentration would narrow the gap between the respective pore radii. Two proteins, human immunoglobulin G (hIgG) and bovine serum albumin (BSA), were used to examine the effect of protein characteristics. The results of adsorption isotherms showed that the dextran-grafted resin with high ligand density had substantially higher adsorption capacity and enhanced the salt-tolerance property for hIgG, but displayed a significantly smaller benefit for BSA adsorption. Confocal laser scanning microscopy (CLSM) showed that hIgG presented more diffuse and slower moving adsorption front compared to BSA during uptake into the resins because of the selective binding of multiple species from polyclonal IgG; polymer-grafting with high ligand density could enhance the rate of hIgG transport in the dextran-grafted resins without salt addition, but not for the case with high salt and BSA. The results indicate that microscopic analysis using ISEC and CLSM is useful to improve the mechanistic understanding of resin structure and of critical functional parameters involving protein adsorption and transport, which would guide the rational design of new resins and processes. Copyright © 2017. Published by Elsevier B.V.

Oxidative degradation of ion-exchange resins in acid medium. Vol. 3

International Nuclear Information System (INIS)

Eskander, S.B.; Ghattas, N.K.

1996-01-01

Volume reduction of spent ion-exchange resins used in nuclear facilities receive increasing importance due to the increase in storage cost, unstable physical and chemical properties and their relatively high specific activity (in some cases up to 1 Ci per liter). The present study is part of research program on the treatment and immobilization of radioactive spent ion-exchange resins simulate; hydrogen peroxide was used for the oxidative degradation of spent ion-exchange resins simulate in sulphuric acid medium. Five liters ring digester developed in Karlsruhe nuclear research center-(KFK)- in germany was the chosen option to perform the oxidation process. The work reported focused on the kinetics and mechanism of the oxidation process. Heating the organic resins in sulphuric acid results in its carbonization and partial oxidation of only 1.7% of the carbon added. Results show that the oxidation reaction is a relatively slow process of first order with K value in the order of 10 -4 min -1 , and the main oxidation product was carbon dioxide. The production of carbon oxide in the off gas stream increased sharply by the addition of hydrogen peroxide to the hot sulphuric acid-resin mixture. The results obtained show that more than 97% of the carbon added was oxidized to carbon dioxide and carbon monoxide. The rate constant value (K) of this reaction was calculated to be (1.69±0.13) x 10 -2 min -1 . The results of gas chromatographic analysis indicate that no significant amounts of hazardous organic materials were detected in the off-gas streams. 6 figs., 4 tabs

Isolation And Purification Of Flavonoids From The Leaves Of Locally Produced Carica Papaya

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Yahaya Mobmi Musa

2015-08-01

Full Text Available ABSTRACT The leaves of Carica papaya 150g was defatted with N-Hexane and extracted with Methanol. The N-Hexane exract showed the presence of Flavonoid Saponin Tannin Glycoside Anthraquinone Resin and Steroid while Methanolic extract showed the presence of Flavonoid Saponin and Resins. 6g of the Methanolic extract was chromatographed using Column chromatography over Silica gel of column 200g60-200 mesh and eluted with the solvent mixture of CH2Cl2CH3OH H2O in the ratio of 70301. The yield of the isolated Flavonoid was 0.23.

Meta-analysis of dragon’s blood resin extract as radio-protective agent

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Subaika Mahmood

2017-09-01

Full Text Available In health sciences, much efforts had been made in past years to explore the radio-protective agents from natural resources due to rapid exposure of radiations to environment such as space traveling, radiotherapy and largely growing telecommunication industry. It becomes crucial to find natural sources for radio-protection. In correspondence, dragon’s blood (DB is a traditional Chinese medicinal plant that possesses great medicinal values due to the presence of several phenolic compounds. For a long time, DB has been used in treatment of blood stasis, inflammation, oxidative stress, immune suppression and tumors, but recently it has been extensively used as radio-protective agent. There is no comprehensive review on radio- protective characterization of DB resin extract in literature. In our review, an attempt has been made to highlight unique and inherent radio-protection in liver, brain, kidney, lung, spleen and cerebrum. This review will help people in exploring the radioactive protectants from natural resources.

Direct measurement of elastic modulus of Nb 3Sn using extracted filaments from superconducting composite wire and resin impregnation method

Science.gov (United States)

Hojo, M.; Matsuoka, T.; Hashimoto, M.; Tanaka, M.; Sugano, M.; Ochiai, S.; Miyashita, K.

2006-10-01

Young's modulus of Nb3Sn filaments in Nb3Sn/Cu superconducting composite wire was investigated in detail. Nb3Sn filaments were first extracted from composite wire. Nitric acid and hydrofluoric acid were used to remove copper stabilizer, Nb3Sn/Nb barrier and bronze. Then, Nb3Sn filaments were impregnated with epoxy resin to form simple filament bundle composite rods. A large difference in Young's moduli of filaments and epoxy resin enhance the accuracy of the measurement of Nb3Sn filament modulus. The ratio of Nb3Sn to Nb in filaments and the number of filaments in the fiber bundle composite rods were used in the final calculation of the Young's modulus of Nb3Sn. The obtained modulus of 127 GPa was the lower bound of the already reported values.

Direct measurement of elastic modulus of Nb3Sn using extracted filaments from superconducting composite wire and resin impregnation method

International Nuclear Information System (INIS)

Hojo, M.; Matsuoka, T.; Hashimoto, M.; Tanaka, M.; Sugano, M.; Ochiai, S.; Miyashita, K.

2006-01-01

Young's modulus of Nb 3 Sn filaments in Nb 3 Sn/Cu superconducting composite wire was investigated in detail. Nb 3 Sn filaments were first extracted from composite wire. Nitric acid and hydrofluoric acid were used to remove copper stabilizer, Nb 3 Sn/Nb barrier and bronze. Then, Nb 3 Sn filaments were impregnated with epoxy resin to form simple filament bundle composite rods. A large difference in Young's moduli of filaments and epoxy resin enhance the accuracy of the measurement of Nb 3 Sn filament modulus. The ratio of Nb 3 Sn to Nb in filaments and the number of filaments in the fiber bundle composite rods were used in the final calculation of the Young's modulus of Nb 3 Sn. The obtained modulus of 127 GPa was the lower bound of the already reported values

Ion-exclusion chromatography with conductimetric detection of aliphatic carboxylic acids on a weakly acidic cation-exchange resin by elution with benzoic acid-beta-cyclodextrin.

Science.gov (United States)

Tanaka, Kazuhiko; Mori, Masanobu; Xu, Qun; Helaleh, Murad I H; Ikedo, Mikaru; Taoda, Hiroshi; Hu, Wenzhi; Hasebe, Kiyoshi; Fritz, James S; Haddad, Paul R

2003-05-16

In this study, an aqueous solution consisting of benzoic acid with low background conductivity and beta-cyclodextrin (beta-CD) of hydrophilic nature and the inclusion effect to benzoic acid were used as eluent for the ion-exclusion chromatographic separation of aliphatic carboxylic acids with different pKa values and hydrophobicity on a polymethacrylate-based weakly acidic cation-exchange resin in the H+ form. With increasing concentration of beta-cyclodextrin in the eluent, the retention times of the carboxylic acids decreased due to the increased hydrophilicity of the polymethacrylate-based cation-exchange resin surface from the adsorption of OH groups of beta-cyclodextrin. Moreover, the eluent background conductivity decreased with increasing concentration of beta-cyclodextrin in 1 mM benzoic acid, which could result in higher sensitivity for conductimetric detection. The ion-exclusion chromatographic separation of carboxylic acids with high resolution and sensitivity was accomplished successfully by elution with a 1 mM benzoic acid-10 mM cyclodextrin solution without chemical suppression.

Recovery of lactic acid from the pretreated fermentation broth based on a novel hyper-cross-linked meso-micropore resin: Modeling.

Science.gov (United States)

Song, Mingkai; Jiao, Pengfei; Qin, Taotao; Jiang, Kangkang; Zhou, Jingwei; Zhuang, Wei; Chen, Yong; Liu, Dong; Zhu, Chenjie; Chen, Xiaochun; Ying, Hanjie; Wu, Jinglan

2017-10-01

An innovative benign process for recovery lactic acid from its fermentation broth is proposed using a novel hyper-cross-linked meso-micropore resin and water as eluent. This work focuses on modeling the competitive adsorption behaviors of glucose, lactic acid and acetic acid ternary mixture and explosion of the adsorption mechanism. The characterization results showed the resin had a large BET surface area and specific pore structure with hydrophobic properties. By analysis of the physicochemical properties of the solutes and the resin, the mechanism of the separation is proposed as hydrophobic effect and size-exclusion. Subsequently three chromatographic models were applied to predict the competitive breakthrough curves of the ternary mixture under different operating conditions. The pore diffusion was the major limiting factor for the adsorption process, which was consistent with the BET results. The novel HD-06 resin can be a good potential adsorbent for the future SMB continuous separation process. Copyright © 2017 Elsevier Ltd. All rights reserved.

A comparison study on the use of Dowex 1 and TEVA-resin in determination of 99Tc in environmental and nuclear coolant samples in a SIA system with ICP-MS detection.

Science.gov (United States)

Kołacińska, Kamila; Samczyński, Zbigniew; Dudek, Jakub; Bojanowska-Czajka, Anna; Trojanowicz, Marek

2018-07-01

This work refers to a comparative study of sorbents widely used in determinations of 99 Tc such as TEVA resin and Dowex 1. Despite having a similar functional group of quaternary amines, both materials represent different chromatographic methods-extraction (TEVA resin) and anion exchange (Dowex 1)-which provides a diverse range of their properties significant in determination of 99 Tc in flow conditions. The comparative tests, carried out in a SIA-LOV (Sequential Injection Analysis-Lab-on-Valve) system combined with mass spectrometric (ICP-MS) detection, considered several factors that are crucial from the standpoint of resin´s utility such as sorption capacity, durability, or selectivity, critical in 99 Tc separation from interferences. The developed and optimized analytical procedure based on the application of the TEVA resin provided determinations of 99 Tc at minimum detectable limit (MDL) 6.00 mBq L -1 in 50 min and has been successfully employed in analyses of samples from nuclear industrial and research units (reactor coolant and sewage) as well as from the river surrounding the nuclear reactor. The method proved to be sufficient for routine analysis of water samples in accordance with EPA standards. The reliability of the method was confirmed in the analysis of the BH standard provided by the NPL for inter-laboratory proficiency tests. The 99 Tc recovery for all real samples was evaluated as 80-100%. Copyright © 2018 Elsevier B.V. All rights reserved.

High-performance liquid chromatographic method for the determination and pharmacokinetic study of oxypeucedanin hydrate and byak-angelicin after oral administration of Angelica dahurica extracts in mongrel dog plasma.

Science.gov (United States)

Xie, Ying; Chen, Yi; Lin, Mei; Wen, Jun; Fan, Guorong; Wu, Yutian

2007-05-09

A high-performance liquid chromatographic method was developed and validated for the determination and pharmacokinetic study of oxypeucedanin hydrate and byak-angelicin after oral administration of Angelica dahurica extracts in mongrel dog plasma. The coumarin components and the internal standard isopsoralen were extracted from plasma samples with the mixture of tert-butyl methyl ether and n-hexane (4:1, v/v). Chromatographic separation was performed on a C(18) column (200 mm x 4.6mm, 5 microm) with the mobile phase acetonitrile-methanol-water-acetic acid (20:15:65:2, v/v/v/v) at a flow-rate of 1.0 ml/min. Only the peak of oxypeucedanin hydrate and byak-angelicin could be detected in dog plasma after oral administration of ethanol extracts of A. dahurica mainly containing xanthotoxol, osthenol, imperatorin, oxypeucedanin hydrate and byak-angelicin. The calibration curves of oxypeucedanin hydrate and byak-angelicin were linear over a range of 22.08-8830.00 and 6.08-2430.00 ng/ml in dog plasma, respectively. The quantification limit of oxypeucedanin hydrate and byak-angelicin in dog plasma was 22.08 and 6.08 ng/ml, respectively. The intra- and inter-day precision was less than 7.6% and 8.5% and the accuracy was from 91.9% to 106.1%. The lowest absolute recoveries of oxypeucedanin hydrate and byak-angelicin were 85.7% and 87.0%, respectively. The method was successfully applied to the pharmacokinetic studies of oxypeucedanin hydrate and byak-angelicin in dog plasma after oral administration of ethanol extracts from A. dahurica.

Chromatographic studies of the lanthanide element separation for the americium/curium large scale separation using ion exchange resins

International Nuclear Information System (INIS)

Ginisty, Claude.

1981-06-01

The Am/Cm large scale separations, operated by chromatography with the use of ion exchange resins, are described by numerous publications. The bibliographic studies allow to retain the followed points: use of sulfonate cationic resins, development by elution with the α-hydroxyisobutyric acid, column loadings between 1 and 30% of the capacity, possibility to use no radioactive lanthanides prior to actinides for trial purposes. The optimisation of such a process is the major part of this thesis. This point is realised by introducing a new definition for the resolution, for non symmetrical elution peaks, and a measure of this dissymmetry by introducing a shape factor F. For the separation itself and for the pressure drop in the column, the influence of the following parameters are studied: composition of the elution solution (concentration and pH), column temperature (20 to 90 0 C), resin size (9 to 27 μm), rate flow of mobile phase (70 ml.cm -2 .mn -1 ), column length and diameter. Symmetrical elution peaks may be obtained, even with a 27% loading. Elution conditions may be modified during the separation process in order to have the best recovery for the two components (1,3 [fr

Evaluation of extractables in processed and unprocessed polymer materials used for pharmaceutical applications.

Science.gov (United States)

Stults, Cheryl L M; Ansell, Jennifer M; Shaw, Arthur J; Nagao, Lee M

2015-02-01

Polymeric materials are often used in pharmaceutical packaging, delivery systems, and manufacturing components. There is continued concern that chemical entities from polymeric components may leach into various dosage forms, particularly those that are comprised of liquids such as parenterals, injectables, ophthalmics, and inhalation products. In some cases, polymeric components are subjected to routine extractables testing as a control measure. To reduce the risk of discovering leachables during stability studies late in the development process, or components that may fail extractables release criteria, it is proposed that extractables testing on polymer resins may be useful as a screening tool. Two studies have been performed to evaluate whether the extractables profile generated from a polymer resin is representative of the extractables profile of components made from that same resin. The ELSIE Consortium pilot program examined polyvinyl chloride and polyethylene, and another study evaluated polypropylene and a copolymer of polycarbonate and acrylonitrile butadiene styrene. The test materials were comprised of polymer resin and processed resin or molded components. Volatile, semi-volatile, and nonvolatile chemical profiles were evaluated after headspace sampling and extraction with solvents of varying polarity and pH. The findings from these studies indicate that there may or may not be differences between extractables profiles obtained from resins and processed forms of the resin depending on the type of material, the compounds of interest, and extraction conditions used. Extractables testing of polymer resins is useful for material screening and in certain situations may replace routine component testing.

Supramolecular solvent-based extraction of benzimidazolic fungicides from natural waters prior to their liquid chromatographic/fluorimetric determination.

Science.gov (United States)

Moral, Antonia; Sicilia, María Dolores; Rubio, Soledad

2009-05-01

A supramolecular solvent made up of vesicles of decanoic acid in the nano- and microscale regimes dispersed in a continuous aqueous phase is proposed for the extraction/preconcentration of benzimidazolic fungicides (BFs) from river and underground water samples prior to their determination by liquid chromatography (LC)/fluorimetry. The solvent is produced from the coacervation of decanoic acid aqueous vesicles by the action of tetrabutylammonium (Bu(4)N(+)). Carbendazim (CB), thiabendazole (TB) and fuberidazole (FB) are extracted on the basis of hydrophobic and pi-cation interactions and the formation of hydrogen bonds. The extraction provides high preconcentration factors (160 for CB and 190 for TB and FB), requires a short time (the procedure takes less than 20 min and several samples can be simultaneously processed) and a low sample volume (20 mL), and avoids the use of toxic organic solvents. Because of the absence of matrix interferences and the low viscosity of the extracts, these can be directly injected into the chromatographic system without the need of cleaning-up or diluting them. Recoveries are not influenced by the presence of salt concentrations up to 1 M. The proposed method provides detection limits for the determination of CB, TB and FB in natural waters of 32, 4 and 0.1 ng L(-1), respectively, and a precision, expressed as relative standard deviation (n=11) of 5.5% for CB (100 ng L(-1)), 4.0% for TB (80 ng L(-1)) and 2.5% for FB (30 ng L(-1)). Recoveries obtained by applying this approach to the analysis of river and underground water samples fortified at the ng L(-1) level are in the intervals 75-83, 95-102 and 97-101% for CB, TB and FB, respectively.

Preliminary evaluation of new polymer matrix for solid-phase extraction of nonylphenol from water samples.

Science.gov (United States)

Guerreiro, António; Soares, Ana; Piletska, Elena; Mattiasson, Bo; Piletsky, Sergey

2008-03-31

Molecularly imprinted (MIP) and blank polymers with affinity for nonylphenol were designed using computational modelling. Chromatographic tests demonstrated higher affinity of imprinted polymers towards the template nonylphenol as compared with blank polymers. The performance of both polymers in solid-phase extraction was however very similar. Both blank and imprinted polymers appeared to be suitable for the removal and pre-concentration of nonylphenol from contaminated water samples with 99% efficiency of the recovery. The commercial resins PH(EC) (Biotage) and C18 (Varian) tested in the same conditions used for comparative purposes had recovery rate <84%. The polymer capacity for nonylphenol was 231 mg g(-1) for blank and 228 mg g(-1) for MIP. The synthesised materials can have significance for sample pre-concentration and environmental analysis of this class of compounds.

Recovery of value-added fossil resin from El-Maghara coal

Energy Technology Data Exchange (ETDEWEB)

Ibrahim, S.S.; Mostafa, S.I. [Central Metallurgical R and D Inst., Cairo (Egypt)

2003-06-01

El-Maghara coal was confirmed to contain a substantial amount of fossil resin intimately associated with its macerals. Macroscopic identification as well as physical diagnosis of solvent refined resinite material proved its particular significance and sufficient value to justify a fossil resin industry in Egypt. This resin has thermosetting properties superior to most synthetics resins available from petrochemicals. It could compete in the market as a chemical commodity in high-speed printing and high-performance adhesive applications. It could have also special values as a feedstock for high-density jet fuel after proper hydrogenation. The froth flotation technique was applied to recover this valuable material from El-Maghara ground coal. The solvent extraction method using commercial solvents was used to refine the resinite fraction collected as flotation concentrate. The variables affecting the flotation technique were studied. Characterization of refined resin was applied. (orig.)

Treatment of a Vertical Root Fracture Using Dual-Curing Resin Cement: A Case Report

Directory of Open Access Journals (Sweden)

Nima Moradi Majd

2012-01-01

Full Text Available Introduction. Vertical root fracture (VRF is one of the most frustrating complications of root canal treatment. The prognosis of the root with VRF is poor therefore tooth extraction and root amputation are usually the only treatment options. However, bonding of the fracture line with adhesive resin cement during the intentional replantation procedure was recently suggested as an alternative to tooth extraction. Methods. A vertically fractured left maxillary incisor was carefully extracted, fracture line was treated with adhesive resin cement, a retrograde cavity was produced and filled with calcium-enriched mixture (CEM cement, and tooth was replanted. Results. After 12 months the tooth was asymptomatic. The size of periapical radiolucency was noticeably reduced and there was no clinical sign of ankylosis. Conclusion. Using adhesive resin cement to bond the fracture lines extraorally in roots with VRF and intentional replantation of the reconstructed teeth could be considered as an alternative to tooth extraction, especially for anterior teeth.

Bioprotective properties of Dragon's blood resin: In vitro evaluation of antioxidant activity and antimicrobial activity

Directory of Open Access Journals (Sweden)

Gupta Rajinder K

2011-02-01

Full Text Available Abstract Background Food preservation is basically done to preserve the natural characteristics and appearance of the food and to increase the shelf life of food. Food preservatives in use are natural, chemical and artificial. Keeping in mind the adverse effects of synthetic food preservatives, there is a need to identify natural food preservatives. The aims of this study were to evaluate in vitro antioxidant and antimicrobial activities of Dragon's blood resin obtained from Dracaena cinnabari Balf f., with a view to develop safer food preservatives. Methods In this study, three solvents of varying polarity were used to extract and separate the medium and high polarity compounds from the non-polar compounds of the Dragon's blood resin. The extracts were evaluated for their antimicrobial activity against the food borne pathogens. The antioxidant activities of the extracts were assessed using DPPH and ABTS radical scavenging, FRAP, metal chelating and reducing power assays. Total phenolics, flavonoids and flavonols of extracts were also estimated using the standard methods. Results Phytochemical analysis of extracts revealed high phenolic content in CH2Cl2 extract of resin. Free radical scavenging of CH2Cl2 extract was found to be highest which is in good correlation with its total phenolic content. All test microorganisms were also inhibited by CH2Cl2 extract. Conclusions Our result provide evidence that CH2Cl2 extract is a potential source of natural antioxidant compounds and exhibited good inhibitory activity against various food borne pathogens. Thus, CH2Cl2 extract of Dragon's blood resin could be considered as possible source of food preservative.

Studies on Brucella interferon: Chromatographic behaviour and purification

International Nuclear Information System (INIS)

Bousquet-Ucla, C.; Wietzerbin, J.; Falcoff, E.

1980-01-01

Interferon was induced by infecting mice with Brucella suis. Serum containing interferon activity was analyzed by chromatography on Concanavalin A-Sepharose and Phenyl-Sepharose CL-4B columns. Antiviral activity was completely retained by the lectin column indicating that all the interferon molecules are glycosylated. The chromatographic behaviour of Brucella interferon on Phenyl-Sepharose CL-4B show that, like other interferons, Brucella interferon displays hydrophobic properties. However, the hydrophobicity of the interferon molecule was masked in the crude preparation and was only detectable when purified Brucella interferon was used for chromatography. The antigenic properties of Brucella interferon provided the means for developing an affinity chromatographic method resulting in about 60.000 fold purification. As in the case of viral interferon, treatment of L cells with Brucella interferon induced specific enhanced in vitro phosphorylation of a 67.000 molecular weight protein after incubation of cell extracts with doublestranded RNA and [γ- 32 p]ATP. (auth.)

New radiochemical methods for determination of 237Np a 241Pu using extraction chromatography (Presentation)

International Nuclear Information System (INIS)

Strisovska, J.

2013-01-01

Thesis was focused on the development of a new methodology for the separation of anthropogenic transuranium radionuclides 237 Np a 241 Pu from different kinds of matrices. The analytical methods used in this study were based on extraction chromatography and were optimized according to the sample type. The proposed radiochemical procedure is a combination of two algorithms, which represent the separation of radionuclides by using extraction chromatographic sorbents TEVA resin and TRU resin supplied by Eichrom Technologies LLC. 239 Np a 237 Np were selectively captured on sorbent TEVA resin in oxidation state 4+. TRU resin was used for purification of plutonium fraction from interfering americium radionuclide. 242 Pu and 239 Np radionuclides as tracers have been used to monitor the radiochemical yields of separation. Before every radiochemical separation tracer radionuclide 239 Np was obtained by separation from the parent radionuclide 2 43 Am, which is in radioactive equilibrium to 239 Np. The average yield of chemical separation was 69,3% for 239 Np at 277 keV energy line and 65,9% at 228 keV energy line. The NPL AH-B08069 (2008) samples which consist of the mixture of alpha-radionuclides were used for the modification and optimization of separation method used for separation of Np and Pu in model samples. This method provided high radiochemical yields of 239,240 Pu (95,0 ± 3,5)% and 237 Np (87,9 ± 3,0)%.. Reliability of the method was verified by applying our modified separation procedures on reference materials IAEA-375 and IAEA-414 supplied by International Atomic Energy Agency. A good agreement between the results is obtained by this procedure and the certified values were found. Samples of contaminated soils from the area of Nuclear power plant A-1 Jaslovske Bohunice which is stored temporarily before disposal were analyzed using developed separation procedure. Specific activity of investigated radionuclides was determined in these samples. (author)

Use of water as displacing agent in ion exchange chromatographic separation of isotope of boron using weak base ion exchange resin

International Nuclear Information System (INIS)

Sharma, B.K.; Mohanakrishnan, G.; Anand Babu, C.; Krishna Prabhu, R.

2008-01-01

Experiments were undertaken to study the feasibility of using weakly basic anion exchange resin for enrichment of isotopes of boron by ion exchange chromatography and water as eluent. The results of experiments carried out to determine total chloride capacity (TCC), strong base capacity (SBC) of the resin at different concentrations of boric acid and enrichment profiles are reported in this paper. (author)

Antimicrobial and Antioxidant Activities of Resins and Essential Oil From Pine (Pinus merkusii, Pinuso ocarpa, Pinus insularis and Agathis (Agathis loranthifolia

Directory of Open Access Journals (Sweden)

Mardho Tillah

2017-04-01

Full Text Available The most common human pathogen that colonizes in a third of healthy people around the world are Staphylococcus aureus, and one of the materials allegedly able to overcome the pathogen is resin. Resin has been used in folk medicine for thousands of years to treat diseases. The antimicrobial activity of natural resins can be associated with a variety of organic compounds contained in them such as diterpenoids and triterpenoids. This research aimed to explore the antibacterial and antioxidant activities of Pinus merkusii, P. oocarpa, P. insularis, Agathis loranthifolia resins and essential oil. Resin was separated by distillation process to get essential oil and the residue was extracted using n-hexane, ethyl acetate (EtOAc, and methanol (MeOH. Antioxidant activity was performed by DPPH (1,1diphenyl-2-picryl hydrazyl radical scavenging method. The antibacterial activity of resins and essential oil of the samples determined using the disc diffusion method against Staphylococcus aureus and Escherichia coli. The results showed that the yield of resin extract was ranging from 8.44 % to 95.56%. All extracts and essential oil could not inhibit E coli growth but inhibit the S. aureus growth. This experiment concluded that resin n-hexane extract from P.oocarpa was the most potent as antibacterial activity against S. aureus. All of the samples used had less potential antioxidant activity compared to positive control ascorbic acid. Result of this study show that pine resin from Indonesia has potential as an antibacterial agent. 

Stereospecific high-performance liquid chromatographic assay of sotalol in plasma.

Science.gov (United States)

Carr, R A; Foster, R T; Bhanji, N H

1991-09-01

A convenient high-performance liquid chromatographic (HPLC) assay was developed for determination of sotalol (STL) enantiomers in plasma. Following addition of the internal standard (IS; racemic atenolol), enantiomers of STL and IS were extracted using ethyl acetate. After evaporation of the organic layer, samples were derivatized with a solution of S-(+)-1-(1-naphthyl)ethyl isocyanate (NEIC). The resulting diastereomers were chromatographed with normal-phase HPLC with chloroform:hexane:methanol [65:33:2 (v/v)] as the mobile phase at a flow rate of 2 ml/min. The fluorescence detection wavelength was set at 220 nm for excitation with no emission filter. The suitability of the assay for pharmacokinetic studies was determined by measuring STL enantiomers in the plasma of a healthy subject after administration of a single 160-mg oral, racemic dose of STL.

Polyphenolic resin synthesis: optimizing plantain peel biomass as heavy metal adsorbent

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Andrés Felipe Cordero

2015-08-01

Full Text Available AbstractPolyphenolic resol resins were obtained from an ethanolic extraction of green plantain peels (Musa paradisiaca grown in Colombia. A synthesis was then performed by polycondensation in an alkaline pH solution in order to perform research on phenolic resin production with high mechanical performance. The polymers were characterized by DSC and TGA analyses and the resins showed a melting point of 94 °C and the typical properties of resol resins. Moreover, the synthesis was controlled using the infrared technique (FTIR where different organic functional groups present in the polymers obtained are observed. The obtained resins were used as heavy metal adsorbents in which the content of those toxic agents is measured by Atomic Absorption Analysis (AA indicating that these resins have a high retention affinity to Pb+2, Ni+2 and Cr+3 (79.01%, 98.48%, 94.14%, respectively as determined by Freundlich isotherms.

The gas-chromatographic and gas-chromatographic-mass-spectrometric identification of halogen-containing organic compounds

Science.gov (United States)

Gidaspov, B. V.; Zenkevich, I. G.; Rodin, A. A.

1989-09-01

The problem of identifying halogen-containing organic compounds in their gas-chromatographic and gas-chromatographic-mass-spectrometric (GC-MS) determination in different materials has been examined. Particular attention has been paid not to the complete characterisation of methods for carrying out this analysis but to the most important problem of increasing the selectivity at the stages of sampling, separation, and interpretation of the gas-chromatographic and GC-MS information. The bibliography contains 292 references.

Gas chromatographic determination of impurities of inorganic compounds

International Nuclear Information System (INIS)

Drugov, Yu.S.

1985-01-01

Methods of concentration, separation, detection in gas chromatographic determination of impurities of inorganic compounds including low-boiling gases, reactive gases, organometallic compounds, free metals, anions, etc. are reviewed. Methods of reaction gas chromatography for determining reactive gases, water, anions, metal chelates are considered in detail as well as methods of reaction-sorption concentration and reaction gas extraction. The application of gas chromatograpny ior anaiysis of water and atmosphere contamination, for determination of impurities in highly pure solid substances and gases is described

Determination of trace level thorium and uranium in high purity gadolinium sulfate using ICP-MS with solid-phase chromatographic extraction resins

Science.gov (United States)

Ito, S.; Takaku, Y.; Ikeda, M.; Kishimoto, Y.

2018-01-01

The Super Kamiokand-Gadolinium (SK-Gd) project is the upgrade of the Super-Kamiokande (SK) detector in order to discover Supernova Relic Neutrinos (SRNs) by loading 0.2% of Gd2(SO4)3 into a 50 kton of the SK water tank. In order to continue solar neutrino measurement with low energy threshold at ˜3.5 MeV, main radioactive contamination, U and Th in Gd2(SO4)3, should be purified before loading. We developed solid-phase extraction technique to measure low concentration of U and Th in Gd2(SO4)3 by ICP-MS. The extraction technique and current status will be presented.

Effect of grape seed extract against biodegradation of composite resin-dentin shear bond strength

Science.gov (United States)

Generosa, D. M.; Suprastiwi, E.; Asrianti, D.

2017-08-01

This study aimed to analyze the effect of grape seed extract (GSE) on resin-dentin shear bond strength. A group of 48 dentin samples were divided into 6 groups. The six groups, each with eight specimens, included group 1 (control), group 2 (control + NaOCl 10%), group 3 (2.9% GSE application before etching), group 4 (2.9% GSE application before etching + NaOCl 10%), group 5 (2.9% GSE application after etching), and group 6 (2.9% GSE application after etching + NaOCl 10%). Shear bond strengths were measured using a universal testing machine. Statistical analysis was done with the Kruskal-Wallis test and the Mann-Whitney U test. The highest median value was in group 3, and the lowest value was in group 5. GSE can improve the shear bond strength (p = 0.002 and 0.001), but it has no effect on reducing biodegradation (p = 0.141).

Optimization of chromatographic conditions and comparison of extraction efficiencies of four different methods for determination and quantification of pesticide content in bovine milk by UFLC-MS/MS

Directory of Open Access Journals (Sweden)

Fabiano A. S. Oliveira

2014-01-01

Full Text Available This paper describes the optimization of a multiresidue chromatographic analysis for the identification and quantification of 20 pesticides in bovine milk, including three carbamates, a carbamate oxime, six organophosphates, two strobilurins, a pyrethroid, an oxazolidinedione, an aryloxyphenoxypropionate acid/ester, a neonicotinoid, a dicarboximide, and three triazoles. The influences of different chromatographic columns and gradients were evaluated. Furthermore, four different extraction methods were evaluated; each utilized both different solvents, including ethyl acetate, methanol, and acetonitrile, and different workup steps. The best results were obtained by a modified QuEChERS method that lacked a workup step, and that included freezing the sample for 2 hours at -20 ºC. The results were satisfactory, yielding coefficients of variation of less than 20%, with the exception of the 50 µg L-1 sample of famoxadone, and recoveries between 70 and 120%, with the exception of acephate and bifenthrin; however, both analytes exhibited coefficients of variation of less than 20%.

Gas-liquid chromatographic determination of resmethrin in corn, cornmeal, flour, and wheat.

Science.gov (United States)

Simonaitis, R A; Cail, R S

1975-09-01

A gas-liquid chromatographic (GLC) method was developed for the determination of residues of resmethrin ((5-benzyl-3-furyl)methyl cis-trans-(+/-)-2,2-dimethyl-3-(2-methylpropenyl)-cyclopropanecarboxylate) in corn, cornmeal, flour, and wheat. The commodity, fortified with resmethrin, was extracted by tumbling with pentane and transferred to acetonitrile, the fat was partitioned off, and the sample was chromatographed with 3% ethyl acetate in pentane on Florisil containing 0.5% water. The resmethrin residue was determined by GLC with a flame ionization detector. The results were compared with known standards that had undergone the same cleanup procedures. The method was sensitive to concentrations of resmethrin to 0.2 ppm, recoveries averaged 83%, and reproducibility was good.

Elaboration of extracting, incinerable and/or conducting resins, for the grouped conversion of actinides; Conception de resines extractantes, incinerables et/ou conductrices, pour la conversion groupee d'actinides

Energy Technology Data Exchange (ETDEWEB)

Mokhtari, H. [Paris-11 Univ., 91 - Orsay (France)]|[CEA Valrho, Lab. de Chimie des Actinides (LCA), 30 - Marcoule (France)

2006-07-01

The first results obtained in the framework of the study called PEACE (Process for the Elaboration of Actinide Carbide from ion Exchange resin) concern the fixation of neodymium(III) (simulating trivalent actinides) on two carboxylic resins: the first one is of gel type and the second one of macroporous type. A kinetic study of the exchange NH{sub 4}{sup +}/Nd{sup 3+} has shown that: 1)neodymium is fixed under the form of a complexed or hydrolyzed specie of neodymium of charge 2+ 2)a high charge rate is reached (40% in mass for the dried resin which corresponds to an exchange capacity of 11 meq/g dry of introduced resin) 3)the exchange kinetics is better for the macroporous resin than for the gel resin. A heat treatment of the macroporous resin charged in neodymium has been carried out until the carbonization by the mean of thermal gravimetric analyses carried out under air and argon. A carbon/neodymium ratio of about 5 is obtained after carbonization under argon. Scanning electron microscopy analyses carried out on the macroporous resin charged in neodymium have revealed a conservation of the sphericity and a consequent reduction of the resin balls diameter after heat treatment and an homogeneous distribution of neodymium inside the sphere. (O.M.)

Immobilization of spent resin with epoxy resin

International Nuclear Information System (INIS)

Gultom, O.; Suryanto; Sayogo; Ramdan

1997-01-01

immobilization of spent resin using epoxy resin has been conducted. The spent resin was mixtured with epoxy resin in variation of concentration, i.e., 30, 40, 50, 60, 70 weight percent of spent resin. The mixture were pour into the plastic tube, with a diameter of 40 mm and height of 40 mm. The density, compressive strength and leaching rate were respectively measured by quanta chrome, paul weber apparatus and gamma spectrometer. The results showed that the increasing of waste concentration would be decreased the compressive strength, and increased density by immobilized waste. The leaching rate of 137 Cs from waste product was not detected in experiment (author)

Chromatographic cation exchange separation of decigram quantities of californium and other transplutonium elements

Energy Technology Data Exchange (ETDEWEB)

Benker, D.E.; Chattin, F.R.; Collins, E.D.; Knauer, J.B.; Orr, P.B.; Ross, R.G.; Wiggins, J.T.

1980-01-01

Decigram quantities of highly radioactive transplutonium elements are routinely partitioned at TRU by chromatographic elution from cation resin using AHIB eluent. By using two high-pressure ion exchange columns, a small one for the initial loading of the feed and a large one for the elution, batch runs containing up to 200 mg of /sup 252/Cf can be made in about 5 hours (2 hours to load the feed and 3 hours for the elution). The number of effluent product fractions and the amount of actinides that must be collected in intermediate fractions are minimized by monitoring response from a flow-through alpha-detector. This process has been reliable and relatively easy to operate, and will continue to be used for partitioning transplutonium elements at TRU.

Secretory immunoglobulin purification from whey by chromatographic techniques.

Science.gov (United States)

Matlschweiger, Alexander; Engelmaier, Hannah; Himmler, Gottfried; Hahn, Rainer

2017-08-15

Secretory immunoglobulins (SIg) are a major fraction of the mucosal immune system and represent potential drug candidates. So far, platform technologies for their purification do not exist. SIg from animal whey was used as a model to develop a simple, efficient and potentially generic chromatographic purification process. Several chromatographic stationary phases were tested. A combination of two anion-exchange steps resulted in the highest purity. The key step was the use of a small-porous anion exchanger operated in flow-through mode. Diffusion of SIg into the resin particles was significantly hindered, while the main impurities, IgG and serum albumin, were bound. In this step, initial purity was increased from 66% to 89% with a step yield of 88%. In a second anion-exchange step using giga-porous material, SIg was captured and purified by step or linear gradient elution to obtain fractions with purities >95%. For the step gradient elution step yield of highly pure SIg was 54%. Elution of SIgA and SIgM with a linear gradient resulted in a step yield of 56% and 35%, respectively. Overall yields for both anion exchange steps were 43% for the combination of flow-through and step elution mode. Combination of flow-through and linear gradient elution mode resulted in a yield of 44% for SIgA and 39% for SIgM. The proposed process allows the purification of biologically active SIg from animal whey in preparative scale. For future applications, the process can easily be adopted for purification of recombinant secretory immunoglobulin species. Copyright © 2017 Elsevier B.V. All rights reserved.

Separation and preconcentration of actinides from acidic media by extraction chromatography

International Nuclear Information System (INIS)

Horwitz, E. Philip; Chiarizia, Renato; Dietz, Mark L.; Diamond, Herbert; Nelson, Donald M.

1993-01-01

A systematic examination of the effect of nitric and hydrochloric acid concentrations and of macro levels of selected elements on the sorption of actinide ions by a novel extraction chromatographic resin comprised of a solution of octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide in tri-n-butyl phosphate supported on an inert polymeric substrate is described. Actinide sorption is demonstrated to be most efficient at high (>1 M) nitric acid concentrations, although tetra- and hexavalent actinides are strongly retained even from dilute (e.g., 0.05 M) nitric acid solutions. Macro concentrations of several common anions (e.g., PO 4 3- and SO 4 2- ) or complexing agents (e.g., oxalic acid) are shown not to adversely affect the sorption of trivalent actinides, while reducing the sorption of tetravalents. Such effects, together with oxidation state adjustments, are shown to provide a basis for the sequential elution of individual actinides and for actinide isolation from environmental and biological matrices

Evaluating resin-enamel bonds by microshear and microtensile bond strength tests: effects of composite resin

Directory of Open Access Journals (Sweden)

Andrea Mello de Andrade

2010-12-01

Full Text Available OBJECTIVES: The aims of this study were to evaluate the effect of resin composite (Filtek Z250 and Filtek Flow Z350 and adhesive system [(Solobond Plus, Futurabond NR (VOCO and Adper Single Bond (3M ESPE] on the microtensile (μTBS and microshear bond strength (μSBS tests on enamel, and to correlate the bond strength means between them. MATERIAL AND METHODS: Thirty-six extracted human molars were sectioned to obtain two tooth halves: one for μTBS and the other one for μSBS. Adhesive systems and resin composites were applied to the enamel ground surfaces and light-cured. After storage (37(0C/24 h specimens were stressed (0.5 mm/min. Fracture modes were analyzed under scanning electron microscopy. The data were analyzed using two-way ANOVA and Tukey's test (α=0.05. RESULTS: The correlation between tests was estimated with Pearson's product-moment correlation statistics (α =0.05. For both tests only the main factor resin composite was statistically significant (p<0.05. The correlation test detected a positive (r=0.91 and significant (p=0.01 correlation between the tests. CONCLUSIONS: The results were more influenced by the resin type than by the adhesives. Both microbond tests seem to be positive and linearly correlated and can therefore lead to similar conclusions.

Aligning of single and multiple wavelength chromatographic

DEFF Research Database (Denmark)

Nielsen, Niels-Peter Vest; Carstensen, Jens Michael; Smedsgaard, Jørn

1998-01-01

optimised warping (COW) using two input parameters which can be estimated from the observed peak width. COW is demonstrated on constructed single trace chromatograms and on single and multiple wavelength chromatograms obtained from HPLC diode detection analyses of fungal extractsA copy of the C program......The use of chemometric data processing is becoming an important part of modern chromatography. Most chemometric analyses are performed on reduced data sets using areas of selected peaks detected in the chromatograms, which means a loss of data and introduces the problem of extracting peak data from...... to utilise the entire data matrix or rely on peak detection, thus having the same limitations as the commonly used chemometric procedures. The method presented uses the entire chromatographic data matrices and does not require any preprocessing e.g., peak detection. It relies on piecewise linear correlation...

Branched polymeric media: Perchlorate-selective resins from hyperbranched polyethyleneimine

KAUST Repository

Chen, Dennis P.

2012-10-02

Perchlorate (ClO4 -) is a persistent contaminant found in drinking groundwater sources in the United States. Ion exchange (IX) with selective and disposable resins based on cross-linked styrene divinylbenzene (STY-DVB) beads is currently the most commonly utilized process for removing low concentrations of ClO4 - (10-100 ppb) from contaminated drinking water sources. However, due to the low exchange capacity of perchlorate-selective STY-DVB resins (∼0.5-0.8 eq/L), the overall cost becomes prohibitive when treating groundwater with higher concentration of ClO4 - (e.g., 100-1000 ppb). In this article, we describe a new perchlorate-selective resin with high exchange capacity. This new resin was prepared by alkylation of branched polyethyleneimine (PEI) beads obtained from an inverse suspension polymerization process. Batch and column studies show that our new PEI resin with mixed hexyl/ethyl quaternary ammonium chloride exchange sites can selectively extract trace amounts of ClO4 - from a makeup groundwater (to below detection limit) in the presence of competing ions. In addition, this resin has a strong-base exchange capacity of 1.4 eq/L, which is 1.75-2.33 times larger than those of commercial perchlorate-selective STY-DVB resins. The overall results of our studies suggest that branched PEI beads provide versatile and promising building blocks for the preparation of perchlorate-selective resins with high exchange capacity. © 2012 American Chemical Society.

Resin impregnation process for producing a resin-fiber composite

Science.gov (United States)

Palmer, Raymond J. (Inventor); Moore, William E. (Inventor)

1994-01-01

Process for vacuum impregnation of a dry fiber reinforcement with a curable resin to produce a resin-fiber composite, by drawing a vacuum to permit flow of curable liquid resin into and through a fiber reinforcement to impregnate same and curing the resin-impregnated fiber reinforcement at a sufficient temperature and pressure to effect final curing. Both vacuum and positive pressure, e.g. autoclave pressure, are applied to the dry fiber reinforcement prior to application of heat and prior to any resin flow to compact the dry fiber reinforcement, and produce a resin-fiber composite of reduced weight, thickness and resin content, and improved mechanical properties. Preferably both a vacuum and positive pressure, e.g. autoclave pressure, are also applied during final curing.

Study of Cs recovery by extraction chromatography (2)

International Nuclear Information System (INIS)

Hoshi, Harutaka; Zhang, Anyun; Uchida, Hiromi; Kuraoka, Etsushu

2005-02-01

In order to apply CalixR14 extractant to extraction chromatography for Cs separation, basic characteristics of CalixR14 adsorbent were studied. CalixR14 impregnated resin and CalixR14 + TBP impregnated resin were prepared. CalixR14 extractant showed no adsorption for Cs by liquid-liquid extraction and CalixR14 impregnated resin also showed no adsorption for Cs. Therefore, it is concluded that CalixR14 itself has no affinity for Cs. On the other hand, Cs was adsorbed onto CalixR14-TBP impregnated resin from a concentrated nitric acid solution. The distribution coefficients of Cs were more than 10 cm 3 /g from 2 to 6 M nitric acid. While Rb showed week adsorption, Na, K, Sr and La showed no adsorption and separation factor was over 100. A slight amount of CalixR14 and TBP was leaked from impregnated resin into the aqueous phase. Separation from simulated liquid waste was carried out by using a column packed with CalixR14-TBP adsorbent. Na, K, Sr and La were not adsorbed onto the column, however, Cs and Rb were adsorbed onto the column. Cs and Rb were eluted from the column by water. Cs and Rb were quantitatively recovered. (author)

Direct injection analysis of fatty and resin acids in papermaking process waters by HPLC/MS.

Science.gov (United States)

Valto, Piia; Knuutinen, Juha; Alén, Raimo

2011-04-01

A novel HPLC-atmospheric pressure chemical ionization/MS (HPLC-APCI/MS) method was developed for the rapid analysis of selected fatty and resin acids typically present in papermaking process waters. A mixture of palmitic, stearic, oleic, linolenic, and dehydroabietic acids was separated by a commercial HPLC column (a modified stationary C(18) phase) using gradient elution with methanol/0.15% formic acid (pH 2.5) as a mobile phase. The internal standard (myristic acid) method was used to calculate the correlation coefficients and in the quantitation of the results. In the thorough quality parameters measurement, a mixture of these model acids in aqueous media as well as in six different paper machine process waters was quantitatively determined. The measured quality parameters, such as selectivity, linearity, precision, and accuracy, clearly indicated that, compared with traditional gas chromatographic techniques, the simple method developed provided a faster chromatographic analysis with almost real-time monitoring of these acids. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Study of stationary phase stability from a column with chromatographic material for steady state treatment of an effluent and/or waste containing Th-232

International Nuclear Information System (INIS)

Felinto, Maria Claudia Franca da Cunha; Martinz, Daniel Ortiz

1999-01-01

This work relates the behavior of a new chromatographic material, AMBERCMPO I, that has been studied to remove actinide elements from the High Level Liquid Waste. It gives emphasis to the behavior of chromatographic materials to the extraction of Th 4+ and its performance after some operation cycle. (author)

SEQUENTIAL EXTRACTION OF PHOSPHORUS BY MEHLICH-1 AND ION EXCHANGE RESIN FROM B HORIZONS OF FERRIC AND PERFERRIC LATOSOLS (OXISOLS

Directory of Open Access Journals (Sweden)

Danilo de Lima Camêlo

2015-08-01

Full Text Available In general, Latosols have low levels of available P, however, the influence of the parent material seems to be decisive in defining the pool and predominant form of P in these soils. This study evaluated P availability by extraction with Mehlich-1 (M-1 and Ion Exchange Resin (IER, from samples of B horizons of Ferric and Perferric Latosols developed from different parent materials. To this end, in addition to the physical and chemical characterization of soils, 10 sequential extractions were performed with M-1 and IER from samples of B horizons (depth between 0.8 and 1.0 m. Total contents of Ca, P, Fe, Al, and Ti were determined after digestion with nitric, hydrofluoric and perchloric acids. The effects of sequential P extractions on Fe oxides were also evaluated from the analyses of dithionite-citrate-bicarbonate and ammonium acid oxalate. The high similarity between contents of P accumulated after sequential extractions with M-1 and IER in soils developed on tuffite indicated a predominance of P-Ca. Higher contents of P after a single IER extraction show greater efficiency in P removal from highly weathered soils, as from the Latosols studied here. The P contents also show the high sensitivity of extractant M-1 in highly buffered soils. Furthermore, a single extraction with extractant M-1 or IER is not sufficient to estimate the amount of labile P in these soils.

Modeling Aquatic Toxicity through Chromatographic Systems.

Science.gov (United States)

Fernández-Pumarega, Alejandro; Amézqueta, Susana; Farré, Sandra; Muñoz-Pascual, Laura; Abraham, Michael H; Fuguet, Elisabet; Rosés, Martí

2017-08-01

Environmental risk assessment requires information about the toxicity of the growing number of chemical products coming from different origins that can contaminate water and become toxicants to aquatic species or other living beings via the trophic chain. Direct toxicity measurements using sensitive aquatic species can be carried out but they may become expensive and ethically questionable. Literature refers to the use of chromatographic measurements that correlate to the toxic effect of a compound over a specific aquatic species as an alternative to get toxicity information. In this work, we have studied the similarity in the response of the toxicity to different species and we have selected eight representative aquatic species (including tadpoles, fish, water fleas, protozoan, and bacteria) with known nonspecific toxicity to chemical substances. Next, we have selected four chromatographic systems offering good perspectives for surrogation of the eight selected aquatic systems, and thus prediction of toxicity from the chromatographic measurement. Then toxicity has been correlated to the chromatographic retention factor. Satisfactory correlation results have been obtained to emulate toxicity in five of the selected aquatic species through some of the chromatographic systems. Other aquatic species with similar characteristics to these five representative ones could also be emulated by using the same chromatographic systems. The final aim of this study is to model chemical products toxicity to aquatic species by means of chromatographic systems to reduce in vivo testing.

Spectroscopic and chromatographic analysis of oil from an oil shale flash pyrolysis unit

Energy Technology Data Exchange (ETDEWEB)

Khraisha, V.H.; Irqsousi, N.A. [University of Jordan, Amman (Jordan). Dept. of Chemical Engineering; Shabib, I.M. [Applied Science Univ., Amman (Jordan). Dept. of Chemistry

2003-01-01

In this investigation, spectroscopic (FT-IR, UV-Vis, {sup 1}H NMR) and chromatographic (GC) techniques were used to analyze two Jordanian shale oils, Sultani and El-Lajjun. The oils were extracted at different pyrolysis temperatures (400-500{sup o}C) using a fluidized bed reactor. The spectroscopic and chromatographic analyses show that the variation of pyrolysis temperature has no significant effect on the composition of the produced oil. The {sup 1}H NMR results indicate that the protons of methyl and methelyene represent the bulk of the hydrogen ({approx}90%) in most shale oil samples. GC analysis reveals that the oil samples contain n-alkanes with a predominant proportion of n-C{sub 25}. (Author)

Extraction of U(VI), Th(IV), and La(III) from acidic streams and geological samples using AXAD-16-POPDE polymer

Energy Technology Data Exchange (ETDEWEB)

Prabhakaran, D.; Subramanian, M.S. [Indian Institute of Technology, Department of Chemistry, Chennai 600 036 (India)

2004-10-01

A new chromatographic extraction method has been developed using Amberlite XAD-16 (AXAD-16) resin chemically modified with (3-hydroxyphosphinoyl-2-oxo-propyl)phosphonic acid dibenzyl ester (POPDE). The chemically modified polymer was characterized by {sup 13}C CPMAS and {sup 31}P solid-state NMR, Fourier Transform-NIR-FIR-Raman spectroscopy, CHNPS elemental analysis, and thermogravimetric analysis. Extraction studies performed for U(VI), Th(IV), and La(III) showed good distribution ratio (D) values of approximately 10{sup 3}, even under high acidities (1-4 M). Various physiochemical parameters that influence the quantitative metal ion extraction were optimized by static and dynamic methods. Data obtained from kinetic studies revealed that a time duration of {<=}10 min was sufficient to achieve complete metal ion extraction. Maximum metal sorption capacity values under optimum pH conditions were found to be 1.38, 1.33, and 0.75 mmol g{sup -1} for U(VI), Th(IV), and La(III), respectively. Interference studies performed in the presence of concentrated diverse ions and electrolyte species showed quantitative analyte recovery with lower limits of analyte detection being 10 and 20 ng cm{sup -3} for U(VI) and both Th(IV) and La(III), respectively. Sample breakthrough studies performed on the extraction column showed an enrichment factor value of 330 for U(VI) and 270 for Th(IV) and La(III), respectively. Analyte desorption was effective using 15 cm{sup 3} of 1 M (NH{sub 4}){sub 2}CO{sub 3} with >99.8% analyte recovery. The analytical applicability of the developed resin was tested with synthetic mixtures mimicking nuclear spent fuels, seawater compositions and real water and geological samples. The rsd values of the data obtained were within 5.2%, thereby reflecting the reliability of the developed method. (orig.)

[Sample preparation methods for chromatographic analysis of organic components in atmospheric particulate matter].

Science.gov (United States)

Hao, Liang; Wu, Dapeng; Guan, Yafeng

2014-09-01

The determination of organic composition in atmospheric particulate matter (PM) is of great importance in understanding how PM affects human health, environment, climate, and ecosystem. Organic components are also the scientific basis for emission source tracking, PM regulation and risk management. Therefore, the molecular characterization of the organic fraction of PM has become one of the priority research issues in the field of environmental analysis. Due to the extreme complexity of PM samples, chromatographic methods have been the chief selection. The common procedure for the analysis of organic components in PM includes several steps: sample collection on the fiber filters, sample preparation (transform the sample into a form suitable for chromatographic analysis), analysis by chromatographic methods. Among these steps, the sample preparation methods will largely determine the throughput and the data quality. Solvent extraction methods followed by sample pretreatment (e. g. pre-separation, derivatization, pre-concentration) have long been used for PM sample analysis, and thermal desorption methods have also mainly focused on the non-polar organic component analysis in PM. In this paper, the sample preparation methods prior to chromatographic analysis of organic components in PM are reviewed comprehensively, and the corresponding merits and limitations of each method are also briefly discussed.

Evaluating resin-enamel bonds by microshear and microtensile bond strength tests: effects of composite resin

Science.gov (United States)

de ANDRADE, Andrea Mello; MOURA, Sandra Kiss; REIS, Alessandra; LOGUERCIO, Alessandro Dourado; GARCIA, Eugenio Jose; GRANDE, Rosa Helena Miranda

2010-01-01

Objectives The aims of this study were to evaluate the effect of resin composite (Filtek Z250 and Filtek Flow Z350) and adhesive system [(Solobond Plus, Futurabond NR (VOCO) and Adper Single Bond (3M ESPE)] on the microtensile (µTBS) and microshear bond strength (µSBS) tests on enamel, and to correlate the bond strength means between them. Material and methods Thirty-six extracted human molars were sectioned to obtain two tooth halves: one for µTBS and the other one for µSBS. Adhesive systems and resin composites were applied to the enamel ground surfaces and light-cured. After storage (37ºC/24 h) specimens were stressed (0.5 mm/ min). Fracture modes were analyzed under scanning electron microscopy. The data were analyzed using two-way ANOVA and Tukey's test (α=0.05). Results The correlation between tests was estimated with Pearson's product-moment correlation statistics (α =0.05). For both tests only the main factor resin composite was statistically significant (padhesives. Both microbond tests seem to be positive and linearly correlated and can therefore lead to similar conclusions. PMID:21308290

Enhancement of 6-pentyl-α-pyrone fermentation activity in an extractive liquid-surface immobilization (Ext-LSI) system by mixing anion-exchange resin microparticles.

Science.gov (United States)

Oda, Shinobu; Michihata, Sayumi; Sakamoto, Naoki; Horibe, Hideo; Kono, Akihiko; Ohashi, Shinichi

2012-12-01

The addition of anion-exchange resin microparticles into a polyacrylonitrile (PAN) ballooned microsphere layer drastically enhanced the fermentative activity of Trichoderma atroviride AG2755-5NM398 in an extractive liquid-surface immobilization (Ext-LSI) system. The production of 6-pentyl-α-pyrone (6PP), a fungicidal secondary metabolite, was 1.92-fold higher than the control (PAN alone). Copyright © 2012 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

Evaluation of the antimicrobial activity of crude extracts and ...

African Journals Online (AJOL)

The study provides some justifications for the folkloric use of AP seed powder as an antiseptic paste and warrants further studies to determine the structure of the active compound in chromatographic fraction ST 13 -15F. Key words: Adenanthera pavonina, antimicrobial activity, chromatographic fractions, methanolic extract.

Pre-Harvest Dropped Kinnow ( Citrus reticulata Blanco) Waste Management through the Extraction of Naringin and Pectin from their Peels using Indigenous Resin

Science.gov (United States)

Laxmi Deepak Bhatlu, M.; Katiyar, Prashant; Singh, Satya Vir; Verma, Ashok Kumar

2016-09-01

About 10-20 % kinnow fruits are dropped in preharvest stage which are waste and are problem to farmer as these create nuisance by rotting and insect rearing ground. The peels of these dropped fruits as well as peels from kinnow processing may be good source of naringin and pectin. Naringin is used in pharmaseutics while pectin is used in food industry. For recovery of naringin and pectn, peels of preharvest dropped kinnow fruits were boiled in water. The extract was passed through macroporus polymeric adsorbent resin Indion PA 800, naringin was adsorbed on it. The adsorbed naringin was desorbed with ethanol. This solution was passed through membrane filter and filtrate was evaporated to obtain naringin. The extract remaining after adsorption of naringin was used to recover pectin using acid extraction method. The recovery of naringin and pectin was about 52 and 58 % respectively. The naringin finally obtained had 91-93 % purity.

Condensate-polisher resin-leakage quantification and resin-transport studies

International Nuclear Information System (INIS)

Stauffer, C.C.; Doss, P.L.

1983-04-01

The objectives of this program were to: (1) determine the extent of resin leakage from current generation condensate polisher systems, both deep bed and powdered resin design, during cut-in, steady-state and flow transient operation, (2) analyze moisture separator drains and other secondary system samples for resin fragments and (3) document the level of organics in the secondary system. Resin leakage samples were obtained from nine-power stations that have either recirculating steam generators or once through steam generators. Secondary system samples were obtained from steam generator feedwater, recirculating steam generator blowdown and moisture separator drains. Analysis included ultraviolet light examination, SEM/EDX, resin quantification and infrared analysis. Data obtained from the various plants were compared and factors affecting resin leakage were summarized

Phloroglucinols from anti-microbial deposit-resins of Australian stingless bees (Tetragonula carbonaria).

Science.gov (United States)

Massaro, C Flavia; Smyth, Thomas J; Smyth, W Franklin; Heard, Tim; Leonhardt, Sara D; Katouli, Mohammad; Wallace, Helen M; Brooks, Peter

2015-01-01

Stingless bees accumulate deposits of plant resins that are mixed with beeswax to produce propolis. Previous studies have reported anti-microbial constituents of stingless bee (Tetragonula carbonaria) propolis from East Australia, but several components remained to be characterized. In the search of natural products yet unreported for Australian propolis, four bee deposit-resins of T. carbonaria bees were analysed by gas and liquid chromatography mass spectrometry with accurate mass measurements. Ethanolic extracts of the deposit-resins were tested in vitro against Staphylococcus aureus ATCC 25983 and Pseudomonas aeruginosa ATCC 27853 by the agar diffusion method. Phloroglucinols, flavonoids and isoprenoids were identified in samples. The crude extracts showed strong anti-staphylococcal effects but were less active against the Gram-negative bacterium. The diagnostic data enabled the identification of markers that can be used for profiling other Australian propolis sources and to target the isolation of bioactive phloroglucinols in future studies against antibiotic resistant S. aureus strains. Copyright © 2014 John Wiley & Sons, Ltd.

Extraction process

International Nuclear Information System (INIS)

Rendall, J.S.; Cahalan, M.J.

1979-01-01

A process is described for extracting at least two desired constituents from a mineral, using a liquid reagent which produces the constituents, or compounds thereof, in separable form and independently extracting those constituents, or compounds. The process is especially valuable for the extraction of phosphoric acid and metal values from acidulated phosphate rock, the slurry being contacted with selective extractants for phosphoric acid and metal (e.g. uranium) values. In an example, uranium values are oxidized to uranyl form and extracted using an ion exchange resin. (U.K.)

Compatibility between dental adhesive systems and dual-polymerizing composite resins.

Science.gov (United States)

Michaud, Pierre-Luc; MacKenzie, Alexandra

2016-10-01

Information is lacking about incompatibilities between certain types of adhesive systems and dual-polymerizing composite resins, and universal adhesives have yet to be tested with these resins. The purpose of this in vitro study was to investigate the bonding outcome of dual-polymerizing foundation composite resins by using different categories of adhesive solutions and to determine whether incompatibilities were present. One hundred and eighty caries-free, extracted third molar teeth were allocated to 9 groups (n=20), in which 3 different bonding agents (Single Bond Plus [SB]), Scotchbond Multi-purpose [MP], and Scotchbond Universal [SU]) were used to bond 3 different composite resins (CompCore AF [CC], Core Paste XP [CP], and Filtek Supreme Ultra [FS]). After restorations had been fabricated using an Ultradent device, the specimens were stored in water at 37°C for 24 hours. The specimens were tested under shear force at a rate of 0.5 mm/min. The data were analyzed with Kruskal-Wallis tests and post hoc pairwise comparisons (α=.05). All 3 composite resins produced comparable shear bond strengths when used with MP (P=.076). However, when either SB or SU was used, the light-polymerized composite resin (FS) and 1 dual-polymerized foundation composite resin (CC) bonded significantly better than the other dual-polymerized foundation composite resin (CP) (Pincompatibilities exist between different products. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Purification of degraded TBP solvent using macroreticular anion exchange resin

International Nuclear Information System (INIS)

Kartha, P.K.S.; Kutty, P.V.E.; Janaradanan, C.; Ramanujam, A.; Dhumwad, R.K.

1989-01-01

Tri-n-butyl phosphate (TBP) diluted with a suitable diluent is commonly used for solvent extraction in Purex process for the recovery of uranium and plutonium from irradiated nuclear fuels. This solvent gets degraded due to various factors, the main degradation product being dibutyl phosphoric acid (HDBP). A solvent cleanup step is generally incorporated in the process for removing the degradation products from the used solvent. A liquid-liquid cleanup system using sodium carbonate or sodium hydroxide solution is routinely used. Considering certain advantages, like the possibility of loading the resin almost to saturation capacity and the subsequent disposal of the spent resin by incineration and the feasibility of adopting it to the process, a liquid-solid system has been tried as an alternate method, employing various available macroreticular anion exchange resins in OH - form for the sorption of HDBP from TBP. After standardizing the various conditions for the satisfactory removal of HDBP from TBP using synthetic mixtures, resins were tested with process solvent in batch contacts. The parameters studied were (1) capacity of different resins for HDBP sorption (2) influence of acidity, uranium and HDBP on the sorption behaviour of the latter (3) removal of fission products from the solvent by the resin and (4) regeneration and recycling of the resin. (author). 2 figs., 13 tabs., 17 refs

Storing of Extracts in Polypropylene Microcentrifuge Tubes Yields Contaminant Peak During Ultra-flow Liquid Chromatographic Analysis.

Science.gov (United States)

Kshirsagar, Parthraj R; Hegde, Harsha; Pai, Sandeep R

2016-05-01

This study was designed to understand the effect of storage in polypropylene microcentrifuge tubes and glass vials during ultra-flow liquid chromatographic (UFLC) analysis. One ml of methanol was placed in polypropylene microcentrifuge tubes (PP material, Autoclavable) and glass vials (Borosilicate) separately for 1, 2, 4, 8, 10, 20, 40, and 80 days intervals stored at -4°C. Contaminant peak was detected in methanol stored in polypropylene microcentrifuge tubes using UFLC analysis. The contaminant peak detected was prominent, sharp detectable at 9.176 ± 0.138 min on a Waters 250-4.6 mm, 4 μ, Nova-Pak C18 column with mobile phase consisting of methanol:water (70:30). It was evident from the study that long-term storage of biological samples prepared using methanol in polypropylene microcentrifuge tubes produce contaminant peak. Further, this may mislead in future reporting an unnatural compound by researchers. Long-term storage of biological samples prepared using methanol in polypropylene microcentrifuge tubes produce contaminant peakContamination peak with higher area under the curve (609993) was obtained in ultra-flow liquid chromatographic run for methanol stored in PP microcentrifuge tubesContamination peak was detected at retention time 9.113 min with a lambda max of 220.38 nm and 300 mAU intensity on the given chromatographic conditionsGlass vials serve better option over PP microcentrifuge tubes for storing biological samples. Abbreviations used: UFLC: Ultra Flow Liquid Chromatography; LC: Liquid Chromatography; MS: Mass spectrometry; AUC: Area Under Curve.

Re-evaluation of solid-phase adsorption and desorption techniques for isolation of trace organic pollutants from chlorinated water.

Science.gov (United States)

Onodera, S; Nagatsuka, A; Rokuhara, T; Asakura, T; Hirayama, N; Suzuki, S

1993-07-16

Amberlite XAD resin and activated carbon columns were tested for their abilities to concentrate trace organic pollutants in chlorinated water. Both XAD-2 and XAD-7 resin columns (20 ml) were capable of adsorbing about 30% of total organic halogen (TOX) present in 20 l of drinking water (pH 7) containing about 100 micrograms/l of TOX, whereas the carbon column (10 ml) adsorbed over 90% of TOX. The adsorption capacity of XAD-7 resin was found to be strongly dependent on the solution pH, as compared with those of XAD-2 and carbon adsorbents. Soxhlet and sonication extractions were also evaluated for their abilities to recover the adsorbed organics from the adsorbents, by measurements of TOX, chromatographable compounds and mutagenicity in the eluates. Soxhlet extraction gave higher recoveries than sonication, as measured with the above indices, but these differences were generally small (ca. 20%), with exception of the carbon extracts. The XAD-2 and XAD-7 extracts of drinking water also showed about 3-4 times higher mutagenic activity than the carbon extracts.

Characterization and disposal of ion exchange resins used in nuclear installations

International Nuclear Information System (INIS)

Flores E, R.M.; Ortiz O, H.B.; Olguin G, M.T.; Emeterio H, M.; Garcia M, H.

2006-01-01

To dispose of an appropriate way the used ion exchange resins so much in the pool water purification systems of the TRIGA Mark III reactor like in the JS6500 gamma irradiator, of the National Institute of Nuclear Research, were carried out a series of analytic nuclear techniques and complementary conventional to those recommended by the ASTM, with the object of to control and to manage 14 lots of worn out resins appropriately. For its were identified the radioactive isotopes, the resins type, the grade of chemical pollution and the physicochemical degradation of the same ones. The lots of resins that didn't contain radioactive isotopes its were regenerated in an usual way, as long as those that if they controlled them they selected options for its final disposition. The first selected option was the extraction method of ion radioactive isotopes, concentrating the elution product by evaporation. As second option it was carried out the resins stabilization damaged by micro-encapsulation by forged to ambient temperature, using an organic polymer. Previous to the immobilization the resins were pretreated by vacuum drying, pulverization and thermal drying, however before carrying out this last, it was carried out a thermal gravimetric analysis to determine the drying conditions of the resins avoiding its chemical decomposition. (Author)

Suitability of conophor oil for the production of aklyd resins, and ...

African Journals Online (AJOL)

Oil was extracted from Tetracaripidum conophorum nut (conophor plant) using solvent extraction method, with hexane as solvent. The oil obtained was used to synthesize an alkyd resin, which in turn was utilized in the production of white gloss paints and vanishes. The IR and UV analysis of the oil showed the presence of ...

Determination of radionuclide levels in rainwater using ion exchange resin and γ-spectrometry

International Nuclear Information System (INIS)

Jungck, Matthias H.A.; Andrey, Jean-Louis; Froidevaux, Pascal

2009-01-01

The evaluation of radioactivity accidentally released into the atmosphere involves determining the radioactivity levels of rainwater samples. Rainwater scavenges atmospheric airborne radioactivity in such a way that surface contamination can be deduced from rainfall rate and rainwater radioactivity content. For this purpose, rainwater is usually collected in large surface collectors and then measured by γ-spectrometry after such treatments as evaporation or iron hydroxide precipitation. We found that collectors can be adapted to accept large surface (diameter 47 mm) cartridges containing a strongly acidic resin (Dowex AG 88) which is able to quantitatively extract radioactivity from rainwater, even during heavy rainfall. The resin can then be measured by γ-spectrometry. The detection limit is 0.1 Bq per sample of resin (80 g) for 137 Cs. Natural 7 Be and 210 Pb can also be measured and the activity ratio of both radionuclides is comparable with those obtained through iron hydroxide precipitation and air filter measurements. Occasionally 22 Na has also been measured above the detection limit. A comparison between the evaporation method and the resin method demonstrated that 2/3 of 7 Be can be lost during the evaporation process. The resin method is simple and highly efficient at extracting radioactivity. Because of these great advantages, we anticipate it could replace former rainwater determination methods. Moreover, it does not necessitate the transportation of large rainwater volumes to the laboratory

Anterior Cantilever Resin-Bonded Fixed Dental Prostheses: A Review of the Literature.

Science.gov (United States)

Mourshed, Bilal; Samran, Abdulaziz; Alfagih, Amal; Samran, Ahalm; Abdulrab, Saleem; Kern, Matthias

2018-03-01

This review evaluated the survival rate of single retainer anterior resin-bonded fixed dental prostheses (RBFDPs) to determine whether the choice of material affects their clinical outcome. An electronic search of the English peer-reviewed dental literature in PubMed was conducted to identify all publications reporting on cantilever RBFDPs until May 2016. Study information extraction and methodological quality assessments were accomplished by two reviewers independently. The searched keywords were as follows: "resin-bonded, single retainer, all-ceramic resin-bonded fixed dental prostheses (RBFDPs), all-ceramic RBFDPs, cantilever resin, RBFDPs, cantilever resin-bonded bridge, two units cantilevered, two-unit cantilevered, metal-ceramic cantilever, and metal-ceramic." Furthermore, the ''Related Articles'' feature of PubMed was used to identify further references of interest within the primary search. The bibliographies of the obtained references were used to identify pertinent secondary references. Review articles were also used to identify relevant articles. After the application of exclusion criteria, the definitive list of articles was screened to extract the qualitative data, and the results were analyzed. Overall 2588 articles were dedicated at the first review phase; however, only 311 studies were left after the elimination of duplicates and unrelated studies. Seventeen studies passed the second review phase. Five studies were excluded because they were follow-up studies of the same study cohort. Twelve studies were finally selected. The use of cantilever RBFDPs showed promising results and high survival rates. © 2016 by the American College of Prosthodontists.

Characteristics of resin floc dispersion of anion and cation exchange resin in precoat filter using powdered ion exchange resin

Energy Technology Data Exchange (ETDEWEB)

Adachi, Tetsurou (Nitto Denko Corp., Ibaraki, Osaka (Japan)); Sawa, Toshio; Shindoh, Toshikazu

1989-09-01

The filtration performance of mixed filter aid consisting of powdered anion and cation exchange resins used in the precoat filter is closely related to the characteristics of resin floc dispersion. The factors related to resin floc dispersion of anion and cation exchange resin were investigated by measuring the specific settle volume of resin floc as an evaluating index in addition to the measurement of physical, chemical and electrochemical properties of powdered ion exchange resin. The effect of adsorption of iron oxide and polymer electrolyte and of ion exchange were determined. In addition, considered floc dispersion with adsorbing iron oxide, it was assumed that the amount and filling ratio of resin floc were related to summation and multiplication of surface electric charge respectively. An experimental expression was obtained for simulation of the change of specific settle volume of resin floc by particle size, surface area, ion exchange capacity and degree of ionization of the powdered ion exchange resin. (author).

Characteristics of resin floc dispersion of anion and cation exchange resin in precoat filter using powdered ion exchange resin

International Nuclear Information System (INIS)

Adachi, Tetsurou; Sawa, Toshio; Shindoh, Toshikazu.

1989-01-01

The filtration performance of mixed filter aid consisting of powdered anion and cation exchange resins used in the precoat filter is closely related to the characteristics of resin floc dispersion. The factors related to resin floc dispersion of anion and cation exchange resin were investigated by measuring the specific settle volume of resin floc as an evaluating index in addition to the measurement of physical, chemical and electrochemical properties of powdered ion exchange resin. The effect of adsorption of iron oxide and polymer electrolyte and of ion exchange were determined. In addition, considered floc dispersion with adsorbing iron oxide, it was assumed that the amount and filling ratio of resin floc were related to summation and multiplication of surface electric charge respectively. An experimental expression was obtained for simulation of the change of specific settle volume of resin floc by particle size, surface area, ion exchange capacity and degree of ionization of the powdered ion exchange resin. (author)

Effects of croton urucurana extracts and crude resin on Anagasta kuehniella (Lepidoptera: Pyralidae

Directory of Open Access Journals (Sweden)

Luciana Barboza Silva

2009-06-01

Full Text Available Hundreds of plant species have been studied in order to find out the active ingredient responsible for their insecticidal activity against the pests of economic importance. To verify the insecticidal activity in the husk of stem of Croton urucurana Baillon 1864 (Euphorbiaceae against Anagasta kuehniella Zeller 1879 (Lepidoptera: Pyralidae, the methanolic (EMeOH extract, dichloromethane fraction (FDM, ethyl acetate fraction (FAE and crude resin, incorporated into an artificial diet were evaluated. EMeOH (0.5, 1.0 and 2.0% and crude resin (2.0% interfered with neither the weight nor the survival of fourth instar larvae and other analyzed parameters. FDM (2.0% fraction caused mortality of 65%, and the artificial diet containing 2.0, 1.0 and 0.5% FAE caused 100, 55 and 68% mortality respectively when compared with the control, confirming the least efficiency rates of food conversion for FDM(2.0% and FAE(1.0%. The tryptic analysis performed with the midgut fluid of fourth-instar larvae demonstrated that tryptic and chymiotryptic activities for the larvae fed artificial diet containing EMeOH and crude resin were not different.Atualmente centenas de plantas são investigadas para se conhecer os princípios ativos responsáveis pela atividade inseticida contra as diversas pragas de importância econômica. Com o objetivo de verificar a atividade inseticida das cascas do caule de Croton urucurana Baillon 1864 (Euphorbiaceae em relação a Anagasta kuehniella Zeller 1879 (Lepidoptera: Pyralidae, avaliou-se o extrato metanólico (EMeOH, fração diclorometano (FDM, a fração acetato de etila (FAE e a resina in natura, os quais foram adicionados à dieta artificial. O EMeOH (0,5, 1,0 e 20,% e a resina in natura (2,0%, não interferiram no peso, sobrevivência das larvas de 4ª ínstar, bem como nos demais parâmetros analisados. A fração FDM (2,0% causou mortalidade de 65%, e a dieta artificial contendo 2,0, 1,0, e 0,5% de FAE causou 100, 55 e 68% de

Resinous constituent extracting process

Energy Technology Data Exchange (ETDEWEB)

Sayer, W F

1947-10-07

The method of recovering oily constituents from coal or oil shale comprising the saturation of coal or oil shale in a sealed vessel with an organic solution having a boiling point at atmospheric pressure of not exceeding 220/sup 0/C, elevating the temperature within the vessel to a temperature below the cracking temperature of the constituents and maintaining the pressure within the vessel below 51 pounds, to extract the oily material from the coal or oil shale and subsequently separating the solvent from the oily material.

Principles of qualitative analysis in the chromatographic context.

Science.gov (United States)

Valcárcel, M; Cárdenas, S; Simonet, B M; Carrillo-Carrión, C

2007-07-27

This article presents the state of the art of qualitative analysis in the framework of the chromatographic analysis. After establishing the differences between two main classes of qualitative analysis (analyte identification and sample classification/qualification) the particularities of instrumental qualitative analysis are commented on. Qualitative chromatographic analysis for sample classification/qualification through the so-called chromatographic fingerprint (for complex samples) or the volatiles profile (through the direct coupling headspace-mass spectrometry using the chromatograph as interface) is discussed. Next, more technical exposition of the qualitative chromatographic information is presented supported by a variety of representative examples.

Studies on resin degradation products encountered during purification of plutonium by anion exchange

International Nuclear Information System (INIS)

Ramanujam, A.; Dhami, P.S.; Gopalakrishnan, V.; Dhumwad, R.K.

1991-01-01

Among the methods available for the purification of plutonium in Purex process, anion exchange method offers several advantages. However, on repeated use, the resin gets degraded due to thermal, radiolytic and chemical attacks resulting in chemical as well as physical damage. Frequently, plutonium product eluted from such resin contains significant quantities of white precipitates. A few anion exchange resins were leached with 8 M HNO 3 at 60-80degC and the resin degradation products (RDP) in the leach-extract were found to give similar precipitates with tetravalent metal ions like Pu(IV), Th(IV) etc. Tetra propyl ammonium hydroxide in 8 M HNO 3 (TPAN) also gave a white precipitate with plutonium similar to the one found in the elution streams. The results indicate that delinked quaternary ammonium functional groups might be responsible for the formation of precipitate. The characteristics of precipitates Th-RDP, Th-TPAN and that isolated from elution stream have been investigated. In a separate study a tentative formula for Th-RDP compound is proposed. The influence of RDP on the extraction of plutonium and other components in Purex process was studied and it was found that RDP complexes metal ions thus marginally affecting the kd values. A spectrophotometric method has been standardised to monitor the extent of degradation of anion exchange resins which is based on the ability of RDP to reduce the colour intensity of Th-thoron complex. This technique can be used to study the stability of the anion exchange resins. (author). 8 refs., 8 tabs., 5 figs.,

Synthesis of a chelate resin with amido and phosphoric acid and its character in uranium extraction

International Nuclear Information System (INIS)

Qiu Yueshuang; Zhang Jianguo; Feng Yu; Zhao Chaoya

2013-01-01

A chelate resin (D814) with amido and phosphoric acid functional group was synthetized by means of the reactions of stytene-divinyl benzene chloromethylated sphere with ethylenedianmine and orth-phosphorous acid and formaldehyde. This resin can be used to adsorb uranium from leaching solution with high chloride ion in the rang of pH l.33-9.05, and the adsorption rate of uranium was above 95%. D814 resin had a good ability resistant to high chloride ion. The loading capacity for uranium was not apparently effected when chlorid ion concentration in solution was 60 g/L. The results of the adsorption experiment show that when the ratio of saturation volume to breakthrough volume was l.82, the uranium saturation capacity of D814 was 40.5 mg/g dry resin. NaCl + NaHCO 3 was used for eluting agent, and the eluting rate of uranium was 96.7%. Adsorption uranium mechanism by D814 was also discussed. (authors)

Extraction, Isolation And Characterization Of Bioactive Compounds ...

African Journals Online (AJOL)

Natural products from medicinal plants, either as pure compounds or as standardized extracts, provide unlimited opportunities for new drug leads because of the ... The analysis of bioactive compounds present in the plant extracts involving the applications of common phytochemical screening assays, chromatographic ...

Sorption of Uranium Ions from Their Aqueous Solution by Resins Containing Nanomagnetite Particles

Directory of Open Access Journals (Sweden)

Mahmoud O. Abd El-Magied

2016-01-01

Full Text Available Magnetic amine resins composed of nanomagnetite (Fe3O4 core and glycidyl methacrylate (GMA/N,N′-methylenebisacrylamide (MBA shell were prepared by suspension polymerization of glycidyl methacrylate with N,N′-methylenebisacrylamide in the presence of nanomagnetite particles and immobilized with different amine ligands. These resins showed good magnetic properties and could be easily retrieved from their suspensions using an external magnetic field. Adsorption behaviors of uranium ions on the prepared resins were studied. Maximum sorption capacities of uranium ions on R-1 and R-2 were found to be 92 and 158 mg/g. Uranium was extracted successfully from three granite samples collected from Gabal Gattar pluton, North Eastern Desert, Egypt. The studied resins showed good durability and regeneration using HNO3.

Determination of drugs in biological fluids by direct injection of samples for liquid-chromatographic analysis.

Science.gov (United States)

Mullett, Wayne M

2007-03-10

The analysis of drugs in various biological fluids is an important criterion for the determination of the physiological performance of a drug. After sampling of the biological fluid, the next step in the analytical process is sample preparation. The complexity of biological fluids adds to the challenge of direct determination of the drug by chromatographic analysis, therefore demanding a sample preparation step that is often time-consuming, tedious, and frequently overlooked. However, direct on-line injection methods offer the advantage of reducing sample preparation steps and enabling effective pre-concentration and clean-up of biological fluids. These procedures can be automated and therefore reduce the requirements for handling potentially infectious biomaterial, improve reproducibility, and minimize sample manipulations and potential contamination. The objective of this review is to present an overview of the existing literature with emphasis on advances in automated sample preparation methods for liquid-chromatographic methods. More specifically, this review concentrates on the use of direct injection techniques, such as restricted-access materials, turbulent-flow chromatography and other automated on-line solid-phase extraction (SPE) procedures. It also includes short overviews of emerging automated extraction-phase technologies, such as molecularly imprinted polymers, in-tube solid-phase micro-extraction, and micro-extraction in a packed syringe for a more selective extraction of analytes from complex samples, providing further improvements in the analysis of biological materials. Lastly, the outlook for these methods and potential new applications for these technologies are briefly discussed.

Chromatographic separations of stereoisomers

Energy Technology Data Exchange (ETDEWEB)

Souter, R.W.

1985-01-01

This text covers both diastereomers and enantiomers; describes techniques for GC, HPLC, and other chromatographic methods; and tabulates results of various applications by both techniques and compound class. It provides current knowledge about separation mechanisms and interactions of asymmetric molecules, as well as experimental and commercial materials such as columns, instruments, and derivatization reagents. The contents also include stereoisomer separations by gas chromatography. Stereoisomer separations by high-performance liquid chromatography. Stereoisomer separations by other chromatographic techniques.

Recent advances in metal-organic frameworks and covalent organic frameworks for sample preparation and chromatographic analysis.

Science.gov (United States)

Wang, Xuan; Ye, Nengsheng

2017-12-01

In the field of analytical chemistry, sample preparation and chromatographic separation are two core procedures. The means by which to improve the sensitivity, selectivity and detection limit of a method have become a topic of great interest. Recently, porous organic frameworks, such as metal-organic frameworks (MOFs) and covalent organic frameworks (COFs), have been widely used in this research area because of their special features, and different methods have been developed. This review summarizes the applications of MOFs and COFs in sample preparation and chromatographic stationary phases. The MOF- or COF-based solid-phase extraction (SPE), solid-phase microextraction (SPME), gas chromatography (GC), high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) methods are described. The excellent properties of MOFs and COFs have resulted in intense interest in exploring their performance and mechanisms for sample preparation and chromatographic separation. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Separation and characterization of resins and asphaltenes coming from Castilla crude Evaluation of their molecular interaction

International Nuclear Information System (INIS)

Navarro, Lina; Alvarez, Mario; Grosso, Jorge Luis; Navarro, Uriel

2004-01-01

The study of resins and asphaltenes, the heaviest fractions of oil, has become an area of interest due to the abundance of heavy crude oils in Colombia and Latin America. We studied the chemical composition of the heavy fractions of Castilla crude oil, evaluated some of its molecular parameters and found evidence of the interaction between the resins extracted from the crude with the asphaltenes of the original crude. With this objective, we carried out at the pilot plant level precipitation of the resin-asphaltene (R-A) aggregate by adding and mixing under controlled conditions, a paraffin solvent, from the Apiay refinery, called Apiasol. By extracting Soxhlet with the same solvent, resin 1 of aggregate R-A was separated. Resin ll defined as the soluble fraction that is part of the maltenes, was separated from the deasphalted crude by open column chromatography, using alumina as support, according to the SAR method (Saturated, Aromatics, Resins). The fractions of resins and the asphaltenes obtained, were characterized by: Nuclear Magnetic Resonance (NMR), FT-lR, DRX, elementary analysis (C, H, N, S), metal content (Ni and V), distribution of molecular weight by GPC, and average molecular weight by VPO. The results obtained show evidence that resin l which is part of the aggregate has less average molecular weight than resin ll which is present in the fraction of maltenes. In addition, some changes were found in the elementary analysis of among the resins. On the one hand, and taking into account the existing theories of molecular interactions among these fractions, it was found that the resins l separated from the R-A aggregate, when added to the crude, they stabilize their asphaltenes. This evaluation was carried out by analyzing the flocculation point of the crude and its mixtures with 1,9% and 3,8% of resin l, when they are titrated with a precipitating agent in an NIR cell that works with high pressure and temperature

Identification of amino acids in Securigera securidaca, a popular medicinal herb in Iranian folk medicine

OpenAIRE

S.E. Sadat-Ebrahimi; M. Hassanpoor Mir; G.R. Amin; H. Hajimehdipoor

2014-01-01

Securigera securidaca (L.) Degen & Dorfl grows in different parts of Iran. The seeds of the species are used in Iranian folk medicine as an anti-diabetic agent. Many studies have established hypoglycemic effects of amino acids and in the present investigation, amino acids of Securigera securidaca seeds have been evaluated. The ground seeds were extracted using petroleum ether, hot ethanol and ethanol 50%, respectively. ethanol 50% extract was chromatographed over cation exchanging resin and t...

Ion chromatographic determination of Di-n-butyl phosphate in degraded organic solvent

International Nuclear Information System (INIS)

Velavendan, P.; Pandey, N.K.; Kamachi Mudali, U.; Natarajan, R.

2011-01-01

In the present work a method for the determination of Di-n-butyl phosphate in organic streams using Ion Chromatography technique is developed and described here. The method involves the separation of Di-n-butyl phosphate (DBP) from 30% TBP-NPH (Tri-n-butylphosphate diluted in Normal Paraffin Hydrocarbon) and uranium/nitric acid matrix by an extraction of DBP in alkaline medium and subsequent ion-exchange separation in ion chromatography column followed by suppressed conductivity detection. Direct determination of DBP in lean/loaded organic solvent will lead to in accurate determination of DBP due to organic interference. DBP is quantified to lower limit of 1 ppm with 3% RSD. The results obtained with ion chromatographic technique are compared with those obtained by standard gas chromatographic technique. The developed method is much faster and total analysis can be completed within two hours. (author)

Separation of tungsten from molybdenum by liquid-liquid extraction and extraction chromatography using thiocyanate and a quarternary ammonium salt

International Nuclear Information System (INIS)

Yonezawa, C.; Onishi, H.

1977-01-01

Methods were developed for the separation of tungsten from molybdenum by liquid-liquid extraction and extraction chromatography using thiocyanate and a quaternary ammonium salt, Zephiramine. Tungsten was extracted into chloroform as an ion associate of tungsten(V)-thiocyanate complex and Zephiramine cation was retained on a column of Teflon powder coated with Zephiramine, but molybdenum(III) was neither extracted nor retained. The extraction chromatographic method was succesfully applied to the determination of trace amounts of tungsten in molybdenum by neutron activation analysis. The γ-ray spectrum, observed with the Ge(Li) detector, of tungsten fraction separated from irradiated molybdenum are shown. The peaks of 99 Mo, sup(99m)Tc, and sup(99m)Nb (produced by 92 Mo(n,p)sup(99m)Nb) were seen, but these nuclides did nit interfere with the determination of tungsten using a NaI(Tl) detector. The results of the neutron activation analysis of a sample of ammonium molybdate agreed quite well with that of the spectrophotometric determination after extraction chromatographic separation. (T.G.)

Resin Viscosity Influence on Fiber Compaction in Tapered Resin Injection Pultrusion Manufacturing

Science.gov (United States)

Masuram, N. B.; Roux, J. A.; Jeswani, A. L.

2018-06-01

Viscosity of the liquid resin effects the chemical and mechanical properties of the pultruded composite. In resin injection pultrusion manufacturing the liquid resin is injected into a specially designed tapered injection chamber through the injection slots present on top and bottom of the chamber. The resin is injected at a pressure so as to completely wetout the fiber reinforcements inside the tapered injection chamber. As the resin penetrates through the fibers, the resin also pushes the fibers away from the wall towards the center of chamber causing compaction of the fiber reinforcements. The fibers are squeezed together due to compaction, making resin penetration more difficult; thus higher resin injection pressures are required to efficaciously penetrate through the compacted fibers and achieve complete wetout. The impact of resin viscosity on resin flow, fiber compaction, wetout and on the final product is further discussed. Injection chamber design predominantly effects the resin flow inside the chamber and the minimum injection pressure required to completely wet the fibers. Therefore, a desirable injection chamber design is such that wetout occurs at lower injection pressures and at low internal pressures inside the injection chamber.

Marginal adaptation of composite resins under two adhesive techniques.

Science.gov (United States)

Dačić, Stefan; Veselinović, Aleksandar M; Mitić, Aleksandar; Nikolić, Marija; Cenić, Milica; Dačić-Simonović, Dragica

2016-11-01

In the present research, different adhesive techniques were used to set up fillings with composite resins. After the application of etch and rinse or self etch adhesive technique, marginal adaptation of composite fillings was estimated by the length of margins without gaps, and by the microretention of resin in enamel and dentin. The study material consisted of 40 extracted teeth. Twenty Class V cavities were treated with 35% phosphorous acid and restored after rinsing by Adper Single Bond 2 and Filtek Ultimate-ASB/FU 3M ESPE composite system. The remaining 20 cavities were restored by Adper Easy One-AEO/FU 3M ESPE composite system. Marginal adaptation of composite fillings was examined using a scanning electron microscope (SEM). The etch and rinse adhesive technique showed a significantly higher percentage of margin length without gaps (in enamel: 92.5%, in dentin: 57.3%), compared with the self-etch technique with lower percentage of margin length without gaps, in enamel 70.4% (p resin tugs in interprismatic spaces of enamel, while the dentin microretention was composed of adhesive and hybrid layers with resin tugs in dentin canals. In the second technique, resin tugs were rarely seen and a microgap was dominant along the border of restoration margins. The SEM analysis showed a better marginal adaptation of composite resin to enamel and dentin with better microretention when the etch and rinse adhesive procedure was applied. © 2016 Wiley Periodicals, Inc.

Bibliography of extraction chromatography, ch. 15

International Nuclear Information System (INIS)

Eschrich, H.; Drent, W.

1975-01-01

A bibliography of reviews, books and publications dealing with laminar extraction chromatography is given. A tabular survey of experimental data on column extraction chromatographic investigations, stationary phases and support materials is presented. An author index and corporative author index are included. This bibliography refers to various publications relevant to nuclear interest

Effects of blood contamination on resin-resin bond strength.

Science.gov (United States)

Eiriksson, Sigurdur O; Pereira, Patricia N R; Swift, Edward J; Heymann, Harald O; Sigurdsson, Asgeir

2004-02-01

Incremental placement and curing of resin composites has been recommended. However, this requires longer operating time, and therefore, increased risk of contamination. The purpose of this study was to evaluate the effects of blood contamination on microtensile bond strengths (microTBS) between resin interfaces and to determine the best decontamination method to re-establish the original resin-resin bond strength. The top surfaces of 64, 4-mm composite blocks (Z-250, Renew, APX, Pertac II) were untreated as the control, or were treated as follows: blood applied and dried on the surface (Treatment 1), blood applied, rinsed, dried (Treatment 2), blood applied, rinsed, and an adhesive applied (Single Bond, One-Step, Clearfil SE, Prompt L-Pop) (Treatment 3). Fresh composite was applied and light-cured in 2-mm increments. After 24 h storage in water, the specimens were sectioned into 0.7-mm thick slabs, trimmed to a cross-sectional area of 1 mm(2), and loaded to failure at a crosshead speed of 1 mm/min using an Instron universal testing machine. Data were analyzed using two-way ANOVA and Fisher's PLSD test (pcontamination resulted in resin-resin bond strengths of only 1.0-13.1 MPa. Rinsing raised bond strengths to over 40 MPa for each material. Use of an adhesive further increased bond strengths except for Pertac II. Rinsing blood from contaminated surfaces increases the resin-resin bond strength significantly and the application of an appropriate adhesive increases the bond strength to control levels.

Distribution ratios on Dowex 50W resins of metal leached in the caron nickel recovery process

Energy Technology Data Exchange (ETDEWEB)

Reynolds, B.A.; Metsa, J.C.; Mullins, M.E.

1980-05-01

Pressurized ion exchange on Dowex 50W-X8 and 50W-X12 resins was investigated using elution techniques to determine distribution ratios for copper, nickel, and cobalt complexes contained in ammonium carbonate solution, a mixture which approximates the waste liquor from the Caron nickel recovery process. Results were determined for different feed concentrations, as well as for different concentrations and pH values of the ammonium carbonate eluant. Distribution ratios were compared with those previously obtained from a continuous annular chromatographic system. Separation of copper and nickel was not conclusively observed at any of the conditions examined.

Distribution ratios on Dowex 50W resins of metal leached in the caron nickel recovery process

International Nuclear Information System (INIS)

Reynolds, B.A.; Metsa, J.C.; Mullins, M.E.

1980-05-01

Pressurized ion exchange on Dowex 50W-X8 and 50W-X12 resins was investigated using elution techniques to determine distribution ratios for copper, nickel, and cobalt complexes contained in ammonium carbonate solution, a mixture which approximates the waste liquor from the Caron nickel recovery process. Results were determined for different feed concentrations, as well as for different concentrations and pH values of the ammonium carbonate eluant. Distribution ratios were compared with those previously obtained from a continuous annular chromatographic system. Separation of copper and nickel was not conclusively observed at any of the conditions examined

Foam, Foam-resin composite and method of making a foam-resin composite

Science.gov (United States)

Cranston, John A. (Inventor); MacArthur, Doug E. (Inventor)

1995-01-01

This invention relates to a foam, a foam-resin composite and a method of making foam-resin composites. The foam set forth in this invention comprises a urethane modified polyisocyanurate derived from an aromatic amino polyol and a polyether polyol. In addition to the polyisocyanurate foam, the composite of this invention further contains a resin layer, wherein the resin may be epoxy, bismaleimide, or phenolic resin. Such resins generally require cure or post-cure temperatures of at least 350.degree. F.

Waterborne hyperbranched alkyd-acrylic resin obtained by miniemulsion polymerization

Directory of Open Access Journals (Sweden)

Edwin Murillo

Full Text Available Abstract Four waterborne hyperbranched alkyd-acrylic resins (HBRAA were synthesized by miniemulsion polymerization from a hyperbranched alkyd resin (HBR, methyl methacrylate (MMA, butyl acrylate (BA and acrylic acid (AA, by using benzoyl peroxide (BPO and ammonium persulfate (AP as initiators. The reaction between HBR and acrylic monomers was evidenced by differential scanning calorimetric (DSC, nuclear magnetic resonance (NMR and gel permeation chromatography (GPC. The conversion percentage, glass transition temperature (Tg, content of acrylic polymer (determined by soxhlet extraction and molecular weight increased with the content of acrylic monomers used in the synthesis. The main structure formed during the synthesis was the HBRAA. The analysis by dynamic light scattering (DLS showed that the particle size distribution of HBRAA2, HBRAA3 and HBRAA4 resins were mainly monomodal. The film properties (gloss, flexibility, adhesion and drying time of the HBRAA were good.

A multiresidue method by high performance liquid chromatography-based fractionation and gas chromatographic determination of trace levels of pesticides in air and water.

Science.gov (United States)

Seiber, J N; Glotfelty, D E; Lucas, A D; McChesney, M M; Sagebiel, J C; Wehner, T A

1990-01-01

A multiresidue analytical method is described for pesticides, transformation products, and related toxicants based upon high performance liquid chromatographic (HPLC) fractionation of extracted residue on a Partisil silica gel normal phase column followed by selective-detector gas chromatographic (GC) determination of components in each fraction. The HPLC mobile phase gradient (hexane to methyl t-butyl ether) gave good chromatographic efficiency, resolution, reproducibility and recovery for 61 test compounds, and allowed for collection in four fractions spanning polarities from low polarity organochlorine compounds (fraction 1) to polar N-methylcarbamates and organophosphorus oxons (fraction 4). The multiresidue method was developed for use with air samples collected on XAD-4 and related trapping agents, and water samples extracted with methylene chloride. Detection limits estimated from spiking experiments were generally 0.3-1 ng/m3 for high-volume air samples, and 0.01-0.1 microgram/L for one-liter water samples. Applications were made to determination of pesticides in fogwater and air samples.

Quantitative Analysis of Radionuclide for the Used Resin of the Primary Purification System in HANARO

International Nuclear Information System (INIS)

Lee, Mun; Kim, Myong Seop; Park, Se Il; Kim, Tae Whan; Kim, Dong Hun; Kim, Young Chil

2005-01-01

In HANARO, a 30 MW research reactor, the ion exchange resin has been used for the purification of the primary coolant system. The resin used in the primary coolant purification system is replaced with new one once every 3 months during 30 MW reactor operation. The extracted resin from the primary coolant purification system is temporarily stored in a shielding treatment of the reactor hall for radiation cooling. After the radiation level of resin decreases enough to be handled for the waste disposal, it is put into the waste drum, and delivered to the waste facility in KAERI. Recently, in this procedure, the quantitative analysis of radionuclide which is contained in resin is required to have more quantitative data for the disposal. Therefore, in this work, a preliminary study was performed to find a sampling method for the representation of the characteristics of radionuclide in the spent resin

Extraction of americium (III) by thermosensitive polymer gel copolymerized with acidic phosphorus compound

International Nuclear Information System (INIS)

Takeshita, Kenji; Nakano, Yoshio; Matsumura, Tatsuro

2001-01-01

A new gel-liquid extraction using a thermosensitive gel was proposed. The thermosensitive gel shows the conformational change of polymer network with temperature, which is known as the phase transition phenomena of gel. The extraction rate and equilibrium of Am(III) in an aqueous solution containing nitrate ion were measured batchwise by using a thermosensitive gel, N-isopropylacrylamide (NIPA) copolymerized with 2-methacryloyloxy- ethylacidphosphate (MR). The effects of the conformational change of polymer network on the extraction rate and equilibrium were discussed. The distribution ratio of Am(III) showed a large value at higher than LCST (low critical solution temperature; 34degC) and was decreased by the phase transition of gel from shrinking to swelling with decreasing temperature. The extraction of Am(III) in the aqueous solution and the release of Am(III) extracted in the gel were repeated stably by the temperature swing operation between 40 and 3degC. The extraction mechanism of Am(III) was described simply as Am 3+ + 3R - OH=(R-O) 3 Am + 3H + (R-OH: MR). The equilibrium constant at the shrinking state (40degC) was more than 3 times of that at swelling state (3degC). The gel-phase diffusivity of Eu(III) used as a substitute of Am(III) was evaluated as the order of 10 -12 m 2 /s at either of 3 or 40degC, which was similar to those for practical extraction chromatographic resins. The temperature-response of gel for the extraction of Eu(III) was very excellent without delay even for the rapid temperature change at 10degC/min. These results suggest that the extraction and release of Am(III) in an aqueous solution can be controlled by the conformational change of polymer network of thermosensitive gel. (author)

Selective extraction of trace mercury and cadmium from drinking water sources.

Science.gov (United States)

Zhao, Xuan; Zhao, Gang; Wang, Jianlong; Yun, Guichun

2005-01-01

In this paper, a new alternative method, i.e., selective extraction by weakly basic anion exchange resin, has been developed for the removal of trace cadmium and mercury ions from drinking water sources. The mechanism of heavy metal removal is based on selective extraction as the results of LEWIS-base-acid interactions. Transfer of trace mercury species from liquid to resin phase coincides well with the performance of film diffusion. The results demonstrated that the presence of chlorine has a negligible influence on the removal of mercury. However, humic acids can strongly bind mercury by the formation of complex compounds and therefore become the obstacle in the diffusion progress. At neutral or base pH, the resin material exhibits the favorable uptake of heavy metals. In filter experiments, the studied resin material offers favorable properties in the selective extraction of trace mercury and cadmium.

Antibacterial activities of some constituents from oleo-gum-resin of Commiphora mukul.

Science.gov (United States)

Saeed, M Asif; Sabir, A W

2004-03-01

The essential oil, chloroform extract and seven sesquiterpenoids compounds newly isolated from the oleo-gum-resin of Commiphora mukul showed a wide range of inhibiting activity against both Gram (+) and Gram (-) bacteria.

High-pressure liquid chromatographic analysis of pramoxine hydrochloride in high lipoid aerosol foam dosage form.

Science.gov (United States)

Weinberger, R; Mann, B; Posluszny, J

1980-04-01

A rapid and quantitative method for the determination of pramoxine hydrochloride by high-pressure liquid chromatography is presented. The drug is extracted as the salt from a preparation with a high lipoid composition by partitioning it to the aqueous phase of an ether-methanol-water-acetic acid system. The extract is chromatographed on an octadecylsilane bonded packing with a methanol-water-acetic acid-methanesulfonic acid mobile phase. The time required for each separation is approximately 6 min. Analytical recoveries of 100.4 +/- 1.5% were obtained.

A modified commercial gas chromatograph for the continuous monitoring of the thermal degradation of sunflower oil and off-line solid phase extraction gas-chromatography-mass spectrometry characterization of released volatiles.

Science.gov (United States)

Ontañon, I; Sanz, J; Escudero, A; de Marcos, S; Ferreira, V; Galbán, J

2015-04-03

A homemade flow cell attached to a commercial Gas Chromatograph equipped with a Flame Ionization Detector (FID) has been designed for the continuous monitoring of volatile compounds released during heating edible oils. Analytical parameters such as mass of sample, temperature and flow rates have been optimized and the obtained results have been compared with the corresponding thermographs from standard TG systems. Results show that under optimum conditions, the profiles of volatiles released upon heating are comparable to the profiles of TG curves, suggesting that the FID based system could be an alternative to TGA. Additionally, volatiles have been retained in a Lichrolut EN(®) resin, eluted and analyzed by Gas Chromatography-Mass Spectrometry. In this case, forty five compounds have been identified (acids, alcohols, alkanes, aldehydes, ketones and furans) and compared with the FID signals, working both in air or nitrogen atmosphere. It has been concluded that the oxidative thermal degradation is prevented in the presence of a nitrogen atmosphere. Copyright © 2015 Elsevier B.V. All rights reserved.

In vitro cytotoxicity of self-curing acrylic resins of different colors

Directory of Open Access Journals (Sweden)

Luciana Borges Retamoso

2014-08-01

Full Text Available OBJECTIVE: The aim of this study was to assess the in vitro cytotoxicity of acrylic resins of different colors over time. METHODS: Specimens were divided into 4 groups (n = 6 according to the color of the acrylic resin (Orto Class, Clássico, Campinas, São Paulo, Brazil: Group 1: clear acrylic resin; group 2: pink acrylic resin; group 3: blue acrylic resin and group 4: green acrylic resin. All specimens were fabricated according to the mass manipulation technique and submitted to mechanical polishing protocol. The control was performed with an amalgam specimen (C+, a glass specimen (C- and cell control (CC. Specimens were immersed in Minimum Eagle's Medium (MEM and incubated for 24 h at 37o C. The extracts from the experimental material were filtered and mixed with L929 fibroblast. Cytotoxicity was evaluated at 4 different times, 24, 48, 72 and 168 h. After contact, cells were incubated for 24 h and added to 100 µ of 0.01% neutral red dye. The cells were incubated for 3 h for pigment incorporation and fixed. Cells viability was determined by a spectroscopic (BioTek, Winooski, Vermont, USA with a 492-nm wavelength λ=492 nm. RESULTS: There were no statistical differences between the experimental groups and the CC and C- groups. CONCLUSION: Clear, pink, blue and green self-curing acrylic resins fabricated by means of the mass manipulation technique and mechanically polished are not cytotoxic. Neither the pigment added to the self-curing acrylic resin nor the factor of time influenced the cytotoxicity of the material.

Improvement of skin condition in striae distensae: development, characterization and clinical efficacy of a cosmetic product containing Punica granatum seed oil and Croton lechleri resin extract.

Science.gov (United States)

Bogdan, Cătălina; Iurian, Sonia; Tomuta, Ioan; Moldovan, Mirela

2017-01-01

Striae distensae are a frequent skin condition associated with pregnancy, weight change or lack of skin elasticity. The aim of this research was to obtain a topical product containing herbal active ingredients with documented antioxidant and anti-inflammatory activity ( Punica granatum seed oil and Croton lechleri resin extract) and demonstrate its positive effect on prevention and treatment of striae distensae. First, the cream base formulation was optimized through experimental design. Secondly, the cream containing the two active ingredients was investigated in an interventional nonrandomized clinical trial. The clinical outcome was assessed through biophysical parameters and ultrasonographic evaluation. The state of the skin was evaluated by biophysical measurements and ultrasonography at the beginning of the study and after 3 and 6 weeks. The experimental design was successfully used to set the best ranges for the technological and formulation factors to obtain a cosmetic formulation with optimal characteristics. The study of clinical efficacy on the optimal formulation revealed an increase in the dermis thickness, hydration and elasticity values in both groups after 6 weeks of cream application. The new oil-in-water cream containing P. granatum seed oil and C. lechleri resin extract can be helpful in the prevention or improving of skin changes associated with striae.

A study on the compatibility between one-bottle dentin adhesives and composite resins using micro-shear bond strength.

Science.gov (United States)

Song, Minju; Shin, Yooseok; Park, Jeong-Won; Roh, Byoung-Duck

2015-02-01

This study was performed to determine whether the combined use of one-bottle self-etch adhesives and composite resins from same manufacturers have better bond strengths than combinations of adhesive and resins from different manufacturers. 25 experimental micro-shear bond test groups were made from combinations of five dentin adhesives and five composite resins with extracted human molars stored in saline for 24 hr. Testing was performed using the wire-loop method and a universal testing machine. Bond strength data was statistically analyzed using two way analysis of variance (ANOVA) and Tukey's post hoc test. Two way ANOVA revealed significant differences for the factors of dentin adhesives and composite resins, and significant interaction effect (p composite resin (p composite resin than other manufacturer's composite resin. Not all combinations of adhesive and composite resin by same manufacturers failed to show significantly higher bond strengths than mixed manufacturer combinations.

Gas chromatographic method fr determination of carbon in metallic uranium

International Nuclear Information System (INIS)

Nikol'skij, V.A.; Markov, V.K.; Evseeva, T.I.; Cherstvenkova, E.P.

1983-01-01

Gas chromatographic device to determine carbon in metal uranium is developed. Burnout unite, permitting to load in the burnout tube simultaneously quite a few (up to 20) weight amounts of materials to be burned is a characteristic feature of the device. As a result amendments for control experiment and determination limit are decreased. The time of a single determination is also reduced. Conditions of carbon burn out from metal uranium are studied and temperature and time of complete extraction of carbon in the form of dioxide from weight amount into gaseous phase are established

Standard Format for Chromatographic-polarimetric System small samples assessment

International Nuclear Information System (INIS)

Naranjo, S.; Fajer, V.; Fonfria, C.; Patinno, R.

2012-01-01

The treatment of samples containing optically active substances to be evaluated as part of quality control of raw material entering industrial process, and also during the modifications exerted on it to obtain the desired final composition is still and unsolved problem for many industries. That is the case of sugarcane industry. Sometimes the troubles implied are enlarged because samples to be evaluated are not bigger than one milliliter. Reduction of gel beds in G-10 and G-50 chromatographic columns having an inner diameter of 16 mm, instead of 25, and bed heights adjustable to requirements by means of sliding stoppers to increase analytical power were evaluated with glucose and sucrose standards in concentrations from 1 to 10 g/dL, using aliquots of 1 ml without undesirable dilutions that could affect either detection or chromatographic profile. Assays with seaweed extracts gave good results that are shown. It is established the advantage to know concentration of a separated substance by the height of its peak and the savings in time and reagents resulting . Sample expanded uncertainty in both systems is compared. It is also presented several programs for data acquisition, storing and processing. (Author)

Fracture Resistance of Endodontically Treated Teeth Restored with Biodentine, Resin Modified GIC and Hybrid Composite Resin as a Core Material.

Science.gov (United States)

Subash, Dayalan; Shoba, Krishnamma; Aman, Shibu; Bharkavi, Srinivasan Kumar Indu; Nimmi, Vijayan; Abhilash, Radhakrishnan

2017-09-01

The restoration of a severely damaged tooth usually needs a post and core as a part of treatment procedure to provide a corono - radicular stabilization. Biodentine is a class of dental material which possess high mechanical properties with excellent biocompatibility and bioactive behaviour. The sealing ability coupled with optimum physical properties could make Biodentine an excellent option as a core material. The aim of the study was to determine the fracture resistance of Biodentine as a core material in comparison with resin modified glass ionomer and composite resin. Freshly extracted 30 human permanent maxillary central incisors were selected. After endodontic treatment followed by post space preparation and luting of Glass fibre post (Reforpost, Angelus), the samples were divided in to three groups based on the type of core material. The core build-up used in Group I was Biodentine (Septodont, France), Group II was Resin-Modified Glass Ionomer Cement (GC, Japan) and Group III was Hybrid Composite Resin (TeEconom plus, Ivoclar vivadent). The specimens were subjected to fracture toughness using Universal testing machine (1474, Zwick/Roell, Germany) and results were compared using One-way analysis of variance with Tukey's Post hoc test. The results showed that there was significant difference between groups in terms of fracture load. Also, composite resin exhibited highest mean fracture load (1039.9 N), whereas teeth restored with Biodentine demonstrated the lowest mean fracture load (176.66 N). Resin modified glass ionomer exhibited intermediate fracture load (612.07 N). The primary mode of failure in Group I and Group II was favourable (100%) while unfavourable fracture was seen in Group III (30%). Biodentine, does not satisfy the requirements to be used as an ideal core material. The uses of RMGIC's as a core build-up material should be limited to non-stress bearing areas. Composite resin is still the best core build-up material owing to its high fracture

Selective extraction of U(VI), Th(IV), and La(III) from acidic matrix solutions and environmental samples using chemically modified Amberlite XAD-16 resin

Energy Technology Data Exchange (ETDEWEB)

Prabhakaran, D.; Subramanian, M.S. [Department of Chemistry, Indian Institute of Technology, 600 036, Chennai (India)

2004-06-01

A new grafted polymer has been developed by the chemical modification of Amberlite XAD-16 (AXAD-16) polymeric matrix with [(2-dihydroxyarsinoylphenylamino)methyl]phosphonic acid (AXAD-16-AsP). The modified polymer was characterized by a combination of {sup 13}C CPMAS and {sup 31}P solid-state NMR, Fourier transform-NIR-FIR-Raman spectroscopy, CHNPS elemental analysis, and thermogravimetric analysis (TGA). The distribution studies for the extraction of U(VI), Th(IV), and La(III) from acidic solutions were performed using an AXAD-16-AsP-packed chromatographic column. The influences of various physiochemical parameters on analyte recovery were optimized by both static and dynamic methods. Accordingly, even under high acidities (>4 M), good distribution ratio (D) values (10{sup 2}-10{sup 4}) were achieved for all the analytes. Metal ion desorption was effective using 1 mol L{sup -1} (NH{sub 4}){sub 2}CO{sub 3}. From kinetic studies, a time duration of <15 min was sufficient for complete metal ion saturation of the resin phase. The maximum metal sorption capacities were found to be 0.25, 0.13, and 1.49 mmol g{sup -1} for U(VI); 0.47, 0.39, and 1.40 mmol g{sup -1} for Th(IV); and 1.44, 1.48, and 1.12 mmol g{sup -1} for La(III), in the presence of 2 mol L{sup -1} HNO{sub 3}, 2 mol L{sup -1} HCl, and under pH conditions, respectively. The analyte selectivity of the grafted polymer was tested in terms of interfering species tolerance studies. The system showed an enrichment factor of 365, 300, and 270 for U(VI), Th(IV), and La(III), and the limit of analyte detection was in the range of 18-23 ng mL{sup -1}. The practical applicability of the polymer was tested with synthetic nuclear spent fuel and seawater mixtures, natural water, and geological samples. The RSD of the total analytical procedure was within 4.9%, thus confirming the reliability of the developed method. (orig.)

HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHIC DETERMINATION OF CAFFEIC ACID AND ROSMARINIC ACID FROM THE LEAVES OF Orthosiphon stamineus

Directory of Open Access Journals (Sweden)

M. Amzad Hossain

2010-06-01

Full Text Available This paper presents the studies performed on extraction of Orthosiphon stamineus, Benth by using different solvent for the identification and quantification of the caffeic acid derivatives such as caffeic acid  and rosmarinic acid which confers to the leaves of this plant with remarkable pharmaceutical properties. High performance thin-layer chromatographic (HPTLC allows the identification and the quantification of more than 20 samples in the same chromatographic run. The analysis of the samples requires 15-30 min compared with more than 2 h using a typical HPLC method. Using the techniques of the HPTLC and the UV-VIS spectra we have found that the extraction of this herb plant contain, the caffeic acid and rosmarinic acid ranging between 0.029% up to 0.506% and up to 0.24% to 2.24% respectively.     Keywords: Caffice acid derivatives, quantification, Malaysian Orthosiphon stamineus, HPTLC

Development of a relatively cheap and simple automated separation system for a routine separation procedure based on extraction chromatography

International Nuclear Information System (INIS)

Petro Zoriy; Reinhold Flucht; Mechthild Burow; Peter Ostapczuk; Reinhard Lennartz; Myroslav Zoriy

2010-01-01

A robust analytical method has been developed in our laboratory for the separation of radionuclides by means of extraction chromatography using an automated separation system. The proposed method is both cheap and simple and provides the advantageous, rapid and accurate separation of the element of interest. The automated separation system enables a shorter separation time by maintaining a constant flow rate of solution and by avoiding clogging or bubbling in the chromatographic column. The present separation method was tested with two types of samples (water and urine) using UTEVA-, TRU- and Sr-specific resins for the separation of U, Th, Am, Pu and Sr. The total separation time for one radionuclide ranged from 60 to 100 min with the separation yield ranging from 68 to 98% depending on the elements separated. We used ICP-QMS, multi-low-level counter and alpha spectroscopy to measure the corresponding elements. (author)

Similarity analyses of chromatographic herbal fingerprints: a review.

Science.gov (United States)

Goodarzi, Mohammad; Russell, Paul J; Vander Heyden, Yvan

2013-12-04

Herbal medicines are becoming again more popular in the developed countries because being "natural" and people thus often assume that they are inherently safe. Herbs have also been used worldwide for many centuries in the traditional medicines. The concern of their safety and efficacy has grown since increasing western interest. Herbal materials and their extracts are very complex, often including hundreds of compounds. A thorough understanding of their chemical composition is essential for conducting a safety risk assessment. However, herbal material can show considerable variability. The chemical constituents and their amounts in a herb can be different, due to growing conditions, such as climate and soil, the drying process, the harvest season, etc. Among the analytical methods, chromatographic fingerprinting has been recommended as a potential and reliable methodology for the identification and quality control of herbal medicines. Identification is needed to avoid fraud and adulteration. Currently, analyzing chromatographic herbal fingerprint data sets has become one of the most applied tools in quality assessment of herbal materials. Mostly, the entire chromatographic profiles are used to identify or to evaluate the quality of the herbs investigated. Occasionally only a limited number of compounds are considered. One approach to the safety risk assessment is to determine whether the herbal material is substantially equivalent to that which is either readily consumed in the diet, has a history of application or has earlier been commercialized i.e. to what is considered as reference material. In order to help determining substantial equivalence using fingerprint approaches, a quantitative measurement of similarity is required. In this paper, different (dis)similarity approaches, such as (dis)similarity metrics or exploratory analysis approaches applied on herbal medicinal fingerprints, are discussed and illustrated with several case studies. Copyright © 2013

[Studies on the process of Herba Clinopodii saponins purified with macroporous adsorption resin].

Science.gov (United States)

Zhang, Yi; Yan, Dan; Han, Yumei

2005-10-01

To study the technological parameters of the purification process of saponins with macroporous adsorption resin. The adsorptive characteristics and elutive parameters of the process were studied by taking the elutive and purified ratio of saponins as markers. 11.4 ml of the extraction of Herba Clinopodii (crude drugs 0.2 g/ml) was purified with a column of macroporous adsorption resin (phi15 mm x H90 mm, dry weight 2.5 g) and washed with 3BV of distilled water, then eluted with 3BV of 30% ethanol and 3BV of 70% ethanol. Most of saponins were collected in the 70% ethanol. With macroporous adsorption resin adsorbing and purifying,the elutive ratio of saponins is 86.8% and the purity reaches 153.2%. So this process of applying macroporous adsorption resin to adsorb and purify Saponins is feasible.

Coupling of Spinosad Fermentation and Separation Process via Two-Step Macroporous Resin Adsorption Method.

Science.gov (United States)

Zhao, Fanglong; Zhang, Chuanbo; Yin, Jing; Shen, Yueqi; Lu, Wenyu

2015-08-01

In this paper, a two-step resin adsorption technology was investigated for spinosad production and separation as follows: the first step resin addition into the fermentor at early cultivation period to decrease the timely product concentration in the broth; the second step of resin addition was used after fermentation to adsorb and extract the spinosad. Based on this, a two-step macroporous resin adsorption-membrane separation process for spinosad fermentation, separation, and purification was established. Spinosad concentration in 5-L fermentor increased by 14.45 % after adding 50 g/L macroporous at the beginning of fermentation. The established two-step macroporous resin adsorption-membrane separation process got the 95.43 % purity and 87 % yield for spinosad, which were both higher than that of the conventional crystallization of spinosad from aqueous phase that were 93.23 and 79.15 % separately. The two-step macroporous resin adsorption method has not only carried out the coupling of spinosad fermentation and separation but also increased spinosad productivity. In addition, the two-step macroporous resin adsorption-membrane separation process performs better in spinosad yield and purity.

Production of renewable phenolic resins by thermochemical conversion of biomass: A review

Energy Technology Data Exchange (ETDEWEB)

Effendi, A.; Gerhauser, H.; Bridgwater, A.V. [Bio-Energy Research Group, Aston University, Birmingham B4 7ET (United Kingdom)

2008-10-15

This review covers the production and utilisation of liquids from the thermal processing of biomass and related materials to substitute for synthetic phenol and formaldehyde in phenol formaldehyde resins. These resins are primarily employed in the manufacture of wood panels such as plywood, MDF, particle-board and OSB. The most important thermal conversion methods for this purpose are fast pyrolysis and vacuum pyrolysis, pressure liquefaction and phenolysis. Many feedstocks have been tested for their suitability as sources of phenolics including hard and softwoods, bark and residual lignins. Resins have been prepared utilising either the whole liquid product, or a phenolics enriched fraction obtained after fractional condensation or further processing, such as solvent extraction. None of the phenolics production and fractionation techniques covered in this review are believed to allow substitution of 100% of the phenol content of the resin without impacting its effectiveness compared to commercial formulations based on petroleum derived phenol. This survey shows that considerable progress has been made towards reaching the goal of a price competitive renewable resin, but that further research is required to meet the twin challenges of low renewable resin cost and satisfactory quality requirements. Particular areas of concern are wood panel press times, variability of renewable resin properties, odour, lack of reactive sites compared to phenol and potential for increased emissions of volatile organic compounds. (author)

Chromatographic hydrogen isotope separation

International Nuclear Information System (INIS)

Aldridge, F.T.

1983-01-01

Intermetallic compounds with the CaCu5 type of crystal structure, particularly LaNiCo and CaNi5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation column. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale multi-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors

Chromatographic hydrogen isotope separation

International Nuclear Information System (INIS)

Aldridge, F.T.

1981-01-01

Intermetallic compounds with the CaCu5 type of crystal structure , particularly LaNiCo and CaNi5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation colum. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale mutli-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors

Fabrication and Evaluation of Graphite Fiber-Reinforced Polyimide Composite Tube Forms Using Modified Resin Transfer Molding

Science.gov (United States)

Exum, Daniel B.; Ilias, S.; Avva, V. S.; Sadler, Bob

1997-01-01

The techniques necessary for the fabrication of a complex three-dimensional tubular form using a PMR-type resin have been developed to allow for the construction of several tubes with good physical and mechanical properties. Employing established resin transfer molding practices, the relatively non-hazardous AMB-21 in acetone formulation was used to successfully impregnate four layers of AS4 braided graphite fiber preform previously loaded around an aluminum cylindrical core in an enclosed mold cavity. Using heat and vacuum, the solvent was evaporated to form a prepreg followed by a partial imidization and removal of condensation products. The aluminum core was replaced by a silicone rubber bladder and the cure cycle continued to the final stage of 550 F with a bladder internal pressure of 200 lbs/sq in while simultaneously applying a strong vacuum to the prepreg for removal of any additional imidization products. A combination of several modifications to the standard resin transfer molding methodology enabled the mold to 'breathe', allowing the imidization products a pathway for escape. AMB-21 resin was chosen because of the carcinogenic nature of the primary commercial polyimide PMR-15. The AMB-21 resin was formulated using commercially available monomers or monomer precursors and dissolved in a mixture of methyl alcohol and acetone. The viscosity of the resulting monomer solution was checked by use of a Brookfield rheometer and adjusted by adding acetone to an easily pumpable viscosity of about 600 cP. In addition, several types of chromatographic and thermal analyses were of the braids, and excess handling of the preforms broke some of the microscopic fibers, needlessly decreasing the strength of the finished part. In addition, three dimensional braided preforms with fibers along the length of the tube will be significantly stronger in tension than the braided preforms used in this study.

High-performance liquid chromatographic analysis of anthraquinone compounds in the Laurera benguelensis

Science.gov (United States)

Manojlović, N.; Marković, Z.; Gritsanapan, W.; Boonpragob, K.

2009-09-01

A high-performance liquid chromatographic (HPLC) method has been developed for the characterization of anthraquinone metabolites in extracts of the lichen Laurera benguelensis. With this method four anthraquinone derivatives 1,8-dihydroxy-3-methoxy-6-methylanthraquinone, 1,8-dihydroxy-3-formyl-6-methoxyanthraquinone, 1,8-dihydroxy-3-hydroxymethyl-6-methoxy-anthraquinone and 1,3,8-trihyroxy-6-methylanthraquinone can be analyzed. Components of lichen were detected by characteristic ultraviolet spectra and relative retention times. This is first report of phytochemical analysis of L. benguelensis. Importance of this research is in recognizing some new source (lichen and its extracts) as a natural emplacement of antioxidants because oxidation with free radicals or autooxidation is big problem for preservation of food products.

Waterborne hyperbranched alkyd-acrylic resin obtained by mini emulsion polymerization

Energy Technology Data Exchange (ETDEWEB)

Murillo, Edwin, E-mail: edwinalbertomurillo@gmail.com [Grupo de Investigacion en Materiales Polimericos (GIMAPOL), Universidad Francisco de Paula Santander, San Jose de Cucuta (Colombia); Lopez, Betty [Grupo de Investigacion en Ciencia de los Materiales, Universidad de Antioquia, Calle, Medellin (Colombia)

2016-10-15

Four waterborne hyper branched alkyd-acrylic resins (HBRAA) were synthesized by mini emulsion polymerization from a hyper branched alkyd resin (HBR), methyl methacrylate (MMA), butyl acrylate (BA) and acrylic acid (AA), by using benzoyl peroxide (BPO) and ammonium persulfate (AP) as initiators. The reaction between HBR and acrylic monomers was evidenced by differential scanning calorimetric (DSC), nuclear magnetic resonance (NMR) and gel permeation chromatography (GPC). The conversion percentage, glass transition temperature (T{sub g}), content of acrylic polymer (determined by soxhlet extraction) and molecular weight increased with the content of acrylic monomers used in the synthesis. The main structure formed during the synthesis was the HBRAA. The analysis by dynamic light scattering (DLS) showed that the particle size distribution of HBRAA2, HBRAA3 and HBRAA4 resins were mainly mono modal. The film properties (gloss, flexibility, adhesion and drying time) of the HBRAA were good. (author)

Volatile hexafluoroacetylacetonates for the isolation and gas-chromatographic determination of trace metals. Pt. 1

International Nuclear Information System (INIS)

Hellmuth, K.H.; Mirzai, H.

1985-01-01

The optimization of the extraction of metal cations [Sc(III), Cr(III), Mn(II), Fe(III), Co(II), Cu(II), Zn(II), Y(III), Ag(I), Cd(II), La(IIII), Ce(III), Eu(III), Yb(III), Hg(II), Pb(II), Th(IV), U(IV, VI) and Am(III)] in the form of mixed-ligand complexes with hexafluoroacetylacetone and neutral donators with nitrogen atoms or P=O-groups is described. The thermal and gas-chromatographic characteristics of the extracted volatile compounds are reported. Optimal results were achieved using tri-n-butyl-phosphine oxide as donator. (orig.) [de

Liquid chromatographic determination of saccharin in beverages and desserts: complementary collaborative study.

Science.gov (United States)

Sjöberg, A M

1988-01-01

A complementary collaborative study was conducted on a liquid chromatographic method for determination of saccharin in accordance with the latest international recommendations. One industrial and 6 official food control laboratories analyzed 3 samples of a juice, a soft drink, and a dessert at concentration levels of 26-90 mg/L, 33-73 mg/L, and 56-147 mg/kg, respectively. Blind duplicates and a blank were supplied for each type of material at each concentration level. The beverage was chromatographed directly and the dessert was extracted with ethanol before chromatography. Average recoveries were 95-107%. The reproducibility relative standard deviations were 6.4-7.3% for the juice, 9.2-20.6% for the soft drink, and 13.4-16.2% for the dessert. The outlier percentage was 14.3%. The results were compared with those of an earlier collaborative study by Nordic laboratories and with general collaborative results obtained by AOAC.

Optimization of the gas chromatographic separations

International Nuclear Information System (INIS)

Gasco Sanchez, L.

1973-01-01

A review and a critical study on the optimization of the gas chromatographic separations are made. After dealing with the fundamental gas chromatographic equations, some methods of expressing column performances are discussed: performance indices, performance parameters, resolution and effective plate number per unit time. This is completed with a comparative study on performances of various types of columns. Moreover, optimization methods for operating chromatographic conditions are extensively dealt with: as resolution optimization, separation time, and normalization techniques for the time of analysis in order to achieve the maximum resolution at constant time. Finally, some others non operating parameters such as: selectivity of stationary phases, column preparation and optimization methods by means of computers are studied. (Author) 68 refs

Extraction chromatographic separation of iron from complex liquid samples and the determination of 55Fe

International Nuclear Information System (INIS)

Grahek, Z.; Rozmaric Macefat, M.

2006-01-01

Iron separation is described from liquid samples with a high concentration of ions that enables simple determination of 55 Fe. One of the described methods consists of iron precipitation from a large volume seawater by sodium hydroxide and/or ammonium carbonate and separation from other elements (Ca, Sr, Cu, Mg, etc.) on a TRU column with 4M HCl or 8M HNO 3 . In the other procedure iron is separated directly from a mixture of seawater samples and HCl on a TRU column. In both methods, the iron recovery is almost 100%. After separation, 55 Fe is determined by counting with a liquid scintillation counter. The binding of Fe and Zn on TEVA, U/TEVA and TRU resins from seawater solutions of HCl and HNO 3 depends on the type of the resin, concentration of acid and other ions. Iron and zinc can be separated from seawater on a U/TEVA column with 2M HCl. (author)

A Small-Scale Low-Cost Gas Chromatograph

Science.gov (United States)

Gros, Natasa; Vrtacnik, Margareta

2005-01-01

The design and application of a small-scale portable gas chromatograph for learning of the basic concepts of chromatography is described. The apparatus consists of two basic separable units, which includes a chromatographic unit and an electronic unit.

Solid-Phase Extraction Combined with High Performance Liquid ...

African Journals Online (AJOL)

Methods: Solid-phase extraction method was employed for the extraction of the estrogen from milk and high performance liquid chromatography-diode array detector (HPLC-DAD) was used for the determination of estrogen. Results: Optimal chromatographic conditions were achieved on an Eclipse XDB-C18 column at a ...

Enrichment of total steroidal saponins from the extracts of Trillium tschonoskii Maxim by macroporous resin and the simultaneous determination of eight steroidal saponins in the final product by HPLC.

Science.gov (United States)

Zhou, Yulan; Gao, Xin; Fu, Qiang; Guo, Pengqi; Xu, Xinya; Zhang, Ting; Ge, Yanhui; Zhang, Bilin; Wang, Mingchan; Zeng, Aiguo; Luo, Zhimin; Chang, Chun

2017-03-01

An effective and simple method was established for the separation and enrichment of steroidal saponins from Trillium tschonoskii Maxim. The adsorption and desorption properties of seven macroporous resins were investigated. Among the tested resins, AB-8 resin showed the best adsorption and desorption capacities. The adsorption of steroidal saponins on AB-8 at 25°C was quite consistent with both the Freundlich isotherm model and the pseudo-second-order kinetics model. By optimizing the dynamic adsorption and desorption parameters, the content of steroidal saponins increased from 5.20% in the crude extracts to 51.93% in the final product, with a recovery yield of 86.67%. Furthermore, by scale-up separation, the concentration and recovery of total steroidal saponins were 43.8 and 85.5%, respectively, which suggested that AB-8 resin had great industrial and pharmaceutical potential because of its high efficiency and cost-effectiveness. In addition, a high-performance liquid chromatography method for the simultaneous determination of eight steroidal saponins was established for the first time, which was employed to qualitatively and quantitatively analyze the final product. Based on the methodological validation results, the high-performance liquid chromatography method can be widely applied to the quality control of steroidal saponins from Trillium tschonoskii Maxim due to its excellent accuracy, stability, and repeatability. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Métodos de extração e/ou concentração de compostos encontrados em fluidos biológicos para posterior determinação cromatográfica Methods of extraction and/or concentration of compounds found in biological fluids for subsequent chromatographic determination

Directory of Open Access Journals (Sweden)

Sonia C. N. Queiroz

2001-02-01

Full Text Available When organic compounds present in biological fluids are analysed by chromatographic methods, it is generally necessary to carry out a prior sample preparation due the high complexity of this type of sample, especially when the compounds to be determinated are found in very low concentrations. This article describes some of the principal methods for sample preparation in analyses of substances present in biological fluids. The methods include liquid-liquid extraction, solid phase extraction, supercritical fluid extraction and extraction using solid and liquid membranes. The advantages and disadvantages of these methods are discussed.

Resole resin products derived from fractionated organic and aqueous condensates made by fast-pyrolysis of biomass materials

Science.gov (United States)

Chum, H.L.; Black, S.K.; Diebold, J.P.; Kreibich, R.E.

1993-08-10

A process for preparing phenol-formaldehyde resole resins by fractionating organic and aqueous condensates made by fast-pyrolysis of biomass materials while using a carrier gas to move feed into a reactor to produce phenolic-containing/neutrals in which portions of the phenol normally contained in said resins are replaced by a phenolic/neutral fractions extract obtained by fractionation.

A simple source preparation method for alpha-ray spectrometry of volcanic rock sample

International Nuclear Information System (INIS)

Takahashi, Masaomi; Kurihara, Yuichi; Sato, Jun

2006-01-01

A simple source preparation method was developed for the alpha-ray spectrometry to determine U and Th in volcanic rockes. Isolation of U and Th from volcanic rocks was made by use of UTEVA-Spec. resin, extraction chromatograph material. U and Th were extracted by TTA-benzene solution and organic phase was evaporated drop by drop on a hot stainless steel planchet to dryness. This method was found to be effective for the preparation of sources for alpha-ray spectrometry. (author)

Extraction and Purification of Flavonoids from Radix Puerariae | Li ...

African Journals Online (AJOL)

Purpose: To develop an efficient method for the purification of flavonoids from Radix puerariae. Methods: Optimal extraction technology was obtained using orthogonal test. Through adsorption and desorption tests, 8 resins with different polarity, diameter, and surface area were studied. Finally, a novel macroporous resin, ...

Rapid evaluation and comparison of natural products and antioxidant activity in calendula, feverfew, and German chamomile extracts.

Science.gov (United States)

Agatonovic-Kustrin, Snezana; Babazadeh Ortakand, Davoud; Morton, David W; Yusof, Ahmad P

2015-03-13

The present study describes a simple high performance thin layer chromatographic (HPTLC) method for the simultaneous quantification of apigenin, chamazulene, bisabolol and the use of DPPH free radical as a post-chromatographic derivatization agent to compare the free radical scavenging activities of these components in leaf and flower head extracts from feverfew, German chamomile and marigold from the Asteraceae family. Feverfew (Tanacetum parthenium) leaves have been traditionally used in the treatment of migraine with parthenolide being the main bioactive compound. However, due to similar flowers, feverfew is sometimes mistaken for the German chamomile (Matricaria recutita). Bisabolol and chamazulene are the main components in chamomile essential oil. Marigold (Calendula officinalis) was included in the study for comparison, as it belongs to the same family. Parthenolide was found to be present in all leaf extracts but was not detected in calendula flower extract. Chamazulene and bisabolol were found to be present in higher concentrations in chamomile and Calendula flowers. Apigenin was detected and quantified only in chamomile extracts (highest concentration in flower head extracts). Antioxidant activity in sample extracts was compared by superimposing the chromatograms obtained after post-chromatographic derivatization with DPPH and post-chromatographic derivatization with anisaldehyde. It was found that extracts from chamomile flower heads and leaves have the most prominent antioxidant activity, with bisabolol and chamazulene being the most effective antioxidants. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

Enrichment of antioxidants in black garlic juice using macroporous resins and their protective effects on oxidation-damaged human erythrocytes.

Science.gov (United States)

Zou, Ying; Zhao, Mouming; Yang, Kun; Lin, Lianzhu; Wang, Yong

2017-08-15

The black garlic juice is popular for its nutritive value. Enrichment of antioxidants is needed to make black garlic extract an effective functional ingredient. Five macroporous resins were evaluated for their capacity in adsorbing antioxidants in black garlic juice. XAD-16 resin was chosen for further study due to its high adsorption and desorption ratios. Pseudo-second-order kinetics (q e =625μmol Trolox equiv/g dry resin, k 2 =0.0001463) and Freundlich isotherm models (ΔH=-10.1547kJ/mol) were suitable for describing the whole exothermic and physical adsorption processes of the antioxidants from black garlic juice on XAD-16 resin. The antioxidants and phenolics were mostly enriched in 40% ethanol fraction by XAD-16 resin column chromatography. The black garlic extract and its fractions could protect erythrocytes against AAPH-induced hemolysis in dose-dependent manners. The pretreatment of AAPH-damaged erythrocytes with 40% ethanol fractions (2.5mg/mL) significantly decreased the hemolysis ratios from 53.58% to 3.79%. The 40% ethanol fraction possessing strong intracellular antioxidant activity could be used as a functional food ingredient. Copyright © 2017 Elsevier B.V. All rights reserved.

Chromatographic-mass spectrometric analysis of ethanol extract of ...

African Journals Online (AJOL)

Purpose: This study analyzes the chemical composition of ethanol root extracts of Maesa perlaria var. formosana by .... obtained over a scanning range of 50 to 550 amu at 2 scans/s. .... 142.53 (2,2,6-Trimethyl-bicyclo[4.1.0]hept-1-yl)-methanol.

Effects of the crisis in the resin sector on the demography of rural municipalities in Spain

Energy Technology Data Exchange (ETDEWEB)

Ortuno Perez, S.; Garcia Robredo, F.; Ayuga Tellez, E.; Fullana Belda, C.

2013-05-01

Aim of study: The aim of this work is to test the positive effect of a substantially developed resin sector on rural demographic evolution. This work shows how in the period between 1970 and 2010 the demographic decline in the interior regions of Spain was more pronounced in areas characterized by the importance of resin-producing forest stands compared to other nearby rural municipalities where this natural resource is not present. Area of study: The study area consists of a set of rural municipalities in Central Spain, both resin and non-resin producing, in the provinces of Segovia, Avila, Valladolid, Burgos, Soria, Cuenca and Guadalajara. Material and methods: The relationship between resin production and population in resin and non-resin producing municipalities was modeled by means of linear regression analysis. Main results: Generally speaking, between 1950 and 1970 the production of resin halted demographic decline in the regions where this activity was substantially developed. However, when the resin sector entered into crisis in the 1970s, and the economic repercussions of this activity gradually ceased to be felt, the demographic decline in the regions which had been involved in resin production was much more acute than in other non-resin-producing rural areas. Research highlights: This work shows the relationship between resin extraction activity and population evolution in rural municipalities. Sustainable resin exploitation can contribute to the maintenance and development of rural communities, and should be used as a tool for generating employment in rural areas. (Author) 37 refs.

Uranium extraction from gold-uranium ores

Energy Technology Data Exchange (ETDEWEB)

Laskorin, B.N.; Golynko, Z.Sh.

1981-01-01

The process of uranium extraction from gold-uranium ores in the South Africa is considered. Flowsheets of reprocessing gold-uranium conglomerates, pile processing and uranium extraction from the ores are presented. Continuous counter flow ion-exchange process of uranium extraction using strong-active or weak-active resins is noted to be the most perspective and economical one. The ion-exchange uranium separation with the succeeding extraction is also the perspective one.

Chelating extractants of improved selectivity. Progress report, September 1, 1976--October 31, 1977

International Nuclear Information System (INIS)

Freiser, H.

1977-07-01

New means of characterizing metal chelating reagent selectivity have been developed and incorporated into a theoretical factor analysis of the chelate stability constants of 24 metal ions with 14 ligands of the EDTA family. The factor analysis will be extended to extracting ligand families. A computer-controlled automated metal chelate stability constant apparatus has been assembled and successfully tested. A high performance liquid chromatograph has been set up and preliminary examination of comparison of reversed phase chromatographic separation of metal ions with their solvent extraction behavior begun

Separation of the lanthanides on high-efficiency bonded phases and conventional ion-exchange resins

International Nuclear Information System (INIS)

Elchuk, S.; Cassidy, R.M.

1979-01-01

High-performance liquid chromatographic separations (< 20 min) of the lanthanides are illustrated for both 5- and 10-μm bonded-phase strong-acid ion exchangers. The performance of these bonded phase packings is compared with that obtained with a 13-μm styrene-divinylbenzene resin. The eluted metal ions are detected with a variable-wavelength detector after a post-column complexation reaction. The requirements and characteristics of post-column reaction for sensitive metal ion detection after separation on high-performance columns are discussed and the linearity, reproducibility, and sensitivity of the system used in the work are illustrated. The potential of on-column preconcentration for the ultratrace (pg/mL) determination of metal ions is also discussed and illustrated. 7 figures, 2 tables

Probabilistic peak detection for first-order chromatographic data.

Science.gov (United States)

Lopatka, M; Vivó-Truyols, G; Sjerps, M J

2014-03-19

We present a novel algorithm for probabilistic peak detection in first-order chromatographic data. Unlike conventional methods that deliver a binary answer pertaining to the expected presence or absence of a chromatographic peak, our method calculates the probability of a point being affected by such a peak. The algorithm makes use of chromatographic information (i.e. the expected width of a single peak and the standard deviation of baseline noise). As prior information of the existence of a peak in a chromatographic run, we make use of the statistical overlap theory. We formulate an exhaustive set of mutually exclusive hypotheses concerning presence or absence of different peak configurations. These models are evaluated by fitting a segment of chromatographic data by least-squares. The evaluation of these competing hypotheses can be performed as a Bayesian inferential task. We outline the potential advantages of adopting this approach for peak detection and provide several examples of both improved performance and increased flexibility afforded by our approach. Copyright © 2014 Elsevier B.V. All rights reserved.

Assessment of Tensile Bond Strength of Fiber-Reinforced Composite Resin to Enamel Using Two Types of Resin Cements and Three Surface Treatment Methods

Directory of Open Access Journals (Sweden)

Tahereh Ghaffari

2015-10-01

Full Text Available Background: Resin-bonded bridgework with a metal framework is one of the most conservative ways to replace a tooth with intact abutments. Visibility of metal substructure and debonding are the complications of these bridgeworks. Today, with the introduction of fiber-reinforced composite resins, it is possible to overcome these complications. The aim of this study was to evaluate the bond strength of fiber-reinforced composite resin materials (FRC to enamel. Methods: Seventy-two labial cross-sections were prepared from intact extracted teeth. Seventy-two rectangular samples of cured Vectris were prepared and their thickness was increased by adding Targis. The samples were divided into 3 groups for three different surface treatments: sandblasting, etching with 9% hydrofluoric acid, and roughening with a round tapered diamond bur. Each group was then divided into two subgroups for bonding to etched enamel by Enforce and Variolink II resin cements. Instron universal testing machine was used to apply a tensile force. The fracture force was recorded and the mode of failure was identified under a reflective microscope. Results: There were no significant differences in bond strength between the three surface treatment groups (P=0.53. The mean bond strength of Variolink II cement was greater than that of Enforce (P=0.04. There was no relationship between the failure modes (cohesive and adhesive and the two cement types. There was some association between surface treatment and failure mode. There were adhesive failures in sandblasted and diamond-roughened groups and the cohesive failure was dominant in the etched group. Conclusion: It is recommended that restorations made of fiber-reinforced composite resin be cemented with VariolinkII and surface-treated by hydrofluoric acid.   Keywords: Tensile bond strength; surface treatment methods; fiber-reinforced composite resin

A chromatographic objective function to characterise chromatograms with unknown compounds or without standards available.

Science.gov (United States)

Alvarez-Segura, T; Gómez-Díaz, A; Ortiz-Bolsico, C; Torres-Lapasió, J R; García-Alvarez-Coque, M C

2015-08-28

Getting useful chemical information from samples containing many compounds is still a challenge to analysts in liquid chromatography. The highest complexity corresponds to samples for which there is no prior knowledge about their chemical composition. Computer-based methodologies are currently considered as the most efficient tools to optimise the chromatographic resolution, and further finding the optimal separation conditions. However, most chromatographic objective functions (COFs) described in the literature to measure the resolution are based on mathematical models fitted with the information obtained from standards, and cannot be applied to samples with unknown compounds. In this work, a new COF based on the automatic measurement of the protruding part of the chromatographic peaks (or peak prominences) that indicates the number of perceptible peaks and global resolution, without the need of standards, is developed. The proposed COF was found satisfactory with regard to the peak purity criterion when applied to artificial peaks and simulated chromatograms of mixtures built using the information of standards. The approach was applied to mixtures of drugs containing unknown impurities and degradation products and to extracts of medicinal herbs, eluted with acetonitrile-water mixtures using isocratic and gradient elution. Copyright © 2015 Elsevier B.V. All rights reserved.

Improved Chromatographic Bioavailability Estimations

National Research Council Canada - National Science Library

Dorsey, John

1996-01-01

.... Since the inception of reversed phase liquid chromatography there have been many attempts to correlate chromatographic retention with bioavailability and the most often used bulk measure, the octanol...

Chromatographic-mass spectrometric analysis of ethanol extract of ...

African Journals Online (AJOL)

Methods: The dried root of Maesa perlaria var. formosana was extracted with 95 % ethanol for composition analysis under the following optimum GC-MS conditions: 250 °C inlet temperature, 250 °C MSD detector temperature, and GC oven temperature programmed as follows: initial temperature held at 70 °C for 15 min, ...

Correlations of norbornenyl crosslinked polyimide resin structures with resin thermo-oxidative stability, resin glass transition temperature and composite initial mechanical properties

Science.gov (United States)

Alston, William B.

1988-01-01

PMR (polymerization of monomeric reactants) methodology was used to prepare 70 different polyimide oligomeric resins and 30 different unidirectional graphite fiber/polyimide composites. Monomeric composition as well as chain length between sites of crosslinks were varied to examine their effects on resin thermo-oxidative stability and glass transition temperature (Tg) of the cured/postcured resins. A linear correlation of decreasing 316 C resin weight loss/surface area versus (1) decreasing aliphatic content, or (2) increasing benzylic/aliphatic content stoichiometry ratio over a wide range of resin compositions was observed. An almost linear correlation of Tg versus molecular distance between the crosslinks was also observed. An attempt was made to correlate Tg with initial composite mechanical properties (flexural strength and interlaminar shear strength). However, the scatter in mechanical strength data prevented obtaining a clear correlation. Instead, only a range of composite mechanical properties was obtained at 25, 288, and 316 C. Perhaps more importantly, what did become apparent during the correlation study was (1) the PMR methodology could be used to prepare composites from resins containing a wide variety of monomer modifications, (2) that these composites almost invariably provided satisfactory initial mechanical properties as long as the resins formulated exhibited satisfactory processing flow, and (3) that PMR resins exhibited predictable rates of 316 C weight loss/surface area based on their benzylic/aliphatic stoichiometery ratio.

Comparison of temperature change among different adhesive resin cement during polymerization process

Directory of Open Access Journals (Sweden)

Murat Alkurt

2017-01-01

Full Text Available Purpose: The aim of this study was to assess the intra-pulpal temperature changes in adhesive resin cements during polymerization. Materials and Methods: Dentin surface was prepared with extracted human mandibular third molars. Adhesive resin cements (Panavia F 2.0, Panavia SA, and RelyX U200 were applied to the dentin surface and polymerized under IPS e.max Press restoration. K-type thermocouple wire was positioned in the pulpal chamber to measure temperature change (n = 7. The temperature data were recorded (0.0001 sensible and stored on a computer every 0.1 second for sixteen minutes. Differences between the baseline temperature and temperatures of various time points (2, 4, 6, 8, 10, 12, 14, and 16 minute were determined and mean temperature changes were calculated. At various time intervals, the differences in temperature values among the adhesive resin cements were analyzed by two-way ANOVA and post-hoc Tukey honestly test (α = 0.05. Results: Significant differences were found among the time points and resin cements (P < 0.05. Temperature values of the Pan SA group were significantly higher than Pan F and RelyX (P < 0.05. Conclusion: Result of the study on self-adhesive and self-etch adhesive resin cements exhibited a safety intra-pulpal temperature change.

Polyvinyl chloride resin

International Nuclear Information System (INIS)

Kim, Hong Jae

1976-06-01

This book contains polyvinyl chloride resin industry with present condition such as plastic industry and polyvinyl chloride in the world and Japan, manufacture of polyvinyl chloride resin ; suspension polymerization and solution polymerization, extruding, injection process, hollow molding vinyl record, vacuum forming, polymer powders process, vinyl chloride varnish, vinyl chloride latex, safety and construction on vinyl chloride. Each chapter has descriptions on of process and kinds of polyvinyl chloride resin.

Evaluation and improvement of gamma-ray stability of chelating resins containing oxy-acid groups of phosphorus

International Nuclear Information System (INIS)

Jyo, Akinori; Yamabe, Kazunori; Shuto, Taketomi

1998-01-01

Chelating resins containing oxy-acid groups of phosphorus, such as phosphonic and phosphoric acid groups have been studied from the point of view of solvent extraction processes for the separation of nuclear fuel elements as well as of fission product ones. The present work was planned to evaluate the effect of gamma-ray on properties of the resins and to obtain directional information for design of the resins having high stability to gamma-ray. It was clarified that gamma-ray stability of the resins is not high; tolerance limit is ca. 2.3x10 3 C/kg. The present work also clarified that polymers crosslinked with divinylbenzene have much higher gamma-ray stability than ones crosslinked with dimetacrylate esters of oligo (ethylene glycol)s. (J.P.N.)

Gas chromatographic analysis of extractive solvent in reprocessing plants

International Nuclear Information System (INIS)

Marlet, B.

1984-01-01

Operation of a reprocessing plant using the Purex process is recalled and analytical controls for optimum performance are specified. The aim of this thesis is the development of analytical methods using gas chromatography required to follow the evolution of the extraction solvent during spent fuel reprocessing. The solvent at different concentrations, is analysed along the reprocessing lines in organic or aqueous phases. Solvent degradation interferes with extraction and decomposition products are analysed. The solvent becomes less and less efficient, also it is distilled and quality is checked. Traces of solvent should also be checked in waste water. Analysis are made as simple as possible to facilitate handling of radioactive samples [fr

Similarity analyses of chromatographic herbal fingerprints: A review

International Nuclear Information System (INIS)

Goodarzi, Mohammad; Russell, Paul J.; Vander Heyden, Yvan

2013-01-01

Graphical abstract: -- Highlights: •Similarity analyses of herbal fingerprints are reviewed. •Different (dis)similarity approaches are discussed. •(Dis)similarity-metrics and exploratory-analysis approaches are illustrated. •Correlation and distance-based measures are overviewed. •Similarity analyses illustrated by several case studies. -- Abstract: Herbal medicines are becoming again more popular in the developed countries because being “natural” and people thus often assume that they are inherently safe. Herbs have also been used worldwide for many centuries in the traditional medicines. The concern of their safety and efficacy has grown since increasing western interest. Herbal materials and their extracts are very complex, often including hundreds of compounds. A thorough understanding of their chemical composition is essential for conducting a safety risk assessment. However, herbal material can show considerable variability. The chemical constituents and their amounts in a herb can be different, due to growing conditions, such as climate and soil, the drying process, the harvest season, etc. Among the analytical methods, chromatographic fingerprinting has been recommended as a potential and reliable methodology for the identification and quality control of herbal medicines. Identification is needed to avoid fraud and adulteration. Currently, analyzing chromatographic herbal fingerprint data sets has become one of the most applied tools in quality assessment of herbal materials. Mostly, the entire chromatographic profiles are used to identify or to evaluate the quality of the herbs investigated. Occasionally only a limited number of compounds are considered. One approach to the safety risk assessment is to determine whether the herbal material is substantially equivalent to that which is either readily consumed in the diet, has a history of application or has earlier been commercialized i.e. to what is considered as reference material. In order

Similarity analyses of chromatographic herbal fingerprints: A review

Energy Technology Data Exchange (ETDEWEB)

Goodarzi, Mohammad [Department of Analytical Chemistry and Pharmaceutical Technology, Center for Pharmaceutical Research, Vrije Universiteit Brussel, Laarbeeklaan 103, B-1090 Brussels (Belgium); Russell, Paul J. [Safety and Environmental Assurance Centre, Unilever, Colworth Science Park, Sharnbrook, Bedfordshire MK44 1LQ (United Kingdom); Vander Heyden, Yvan, E-mail: yvanvdh@vub.ac.be [Department of Analytical Chemistry and Pharmaceutical Technology, Center for Pharmaceutical Research, Vrije Universiteit Brussel, Laarbeeklaan 103, B-1090 Brussels (Belgium)

2013-12-04

Graphical abstract: -- Highlights: •Similarity analyses of herbal fingerprints are reviewed. •Different (dis)similarity approaches are discussed. •(Dis)similarity-metrics and exploratory-analysis approaches are illustrated. •Correlation and distance-based measures are overviewed. •Similarity analyses illustrated by several case studies. -- Abstract: Herbal medicines are becoming again more popular in the developed countries because being “natural” and people thus often assume that they are inherently safe. Herbs have also been used worldwide for many centuries in the traditional medicines. The concern of their safety and efficacy has grown since increasing western interest. Herbal materials and their extracts are very complex, often including hundreds of compounds. A thorough understanding of their chemical composition is essential for conducting a safety risk assessment. However, herbal material can show considerable variability. The chemical constituents and their amounts in a herb can be different, due to growing conditions, such as climate and soil, the drying process, the harvest season, etc. Among the analytical methods, chromatographic fingerprinting has been recommended as a potential and reliable methodology for the identification and quality control of herbal medicines. Identification is needed to avoid fraud and adulteration. Currently, analyzing chromatographic herbal fingerprint data sets has become one of the most applied tools in quality assessment of herbal materials. Mostly, the entire chromatographic profiles are used to identify or to evaluate the quality of the herbs investigated. Occasionally only a limited number of compounds are considered. One approach to the safety risk assessment is to determine whether the herbal material is substantially equivalent to that which is either readily consumed in the diet, has a history of application or has earlier been commercialized i.e. to what is considered as reference material. In order

High-performance liquid chromatographic determination of isoniazid and 1-isonicotinyl-2-lactosylhydrazine in isoniazid tablet formulations.

Science.gov (United States)

Butterfield, A G; Lovering, E G; Sears, R W

1980-02-01

A high-performance liquid chromatographic procedure is presented for the simultaneous determination of isoniazid and 1-isonicotinyl-2-lactosylhydrazine (I) in isoniazid tablet formulations. An aliquot of a diluted aqueous tablet extract is introduced onto a microparticulate cyanopropyl bonded-phase column using a valve-loop injector and chromatographed using a mobile phase of acetonitrile--0.01 M, pH 3.5 aqueous acetate buffer (5:95). Compound I can be determined at levels as low as 0.5% of the isoniazid label claim. The relative standard deviations are 0.4 and 0.7% for the simultaneous determination of isoniazid and I, respectively. Seven commercial tablet formulations contained 93.8--97.0% of the labeled isoniazid amounts and 0.3--5.8% of I, expressed as equivalent isoniazid relative to the labeled isoniazid level.

New Resin for the Selective Extraction of {sup 129}I

Energy Technology Data Exchange (ETDEWEB)

Bombard, A.; Happel, S. [TrisKem International, Bruz (France); Zulauf, A. [NUKEM Technologies GmbH, Alzenau (Germany); Streng, R. [Radiochemistry, Department of Chemistry, Philipps-University Marburg, Marburg (Germany)

2013-07-15

{sup 129}I is an ideal tracer of the marine environment. It has been used for some years particularly in the northeast Atlantic, Nordic seas and Arctic to determine its distribution after its discharges from La Hague and Sellafield reprocessing plants. Various methods for {sup 129}I determination exist. A new resin selective for iodine has been developed, characterized and tested on environmental samples. In order to allow {sup 129}I determination and to obtain accurate and precise results, the samples have to pass a number of sample preparation steps; among these steps are chemical separation and purification. The results of the analysis of seawater samples are presented. (author)

Simultaneous extraction and quantitation of several bioactive amines in cheese and chocolate.

Science.gov (United States)

Baker, G B; Wong, J T; Coutts, R T; Pasutto, F M

1987-04-17

A method is described for simultaneous extraction and quantitation of the amines 2-phenylethylamine, tele-methylhistamine, histamine, tryptamine, m- and p-tyramine, 3-methoxytyramine, 5-hydroxytryptamine, cadaverine, putrescine, spermidine and spermine. This method is based on extractive derivatization of the amines with a perfluoroacylating agent, pentafluorobenzoyl chloride, under basic aqueous conditions. Analysis was done on a gas chromatograph equipped with an electron-capture detector and a capillary column system. The procedure is relatively rapid and provides derivatives with good chromatographic properties. Its application to analysis of the above amines in cheese and chocolate products is described.

Storing of Extracts in Polypropylene Microcentrifuge Tubes Yields Contaminant Peak During Ultra-flow Liquid Chromatographic Analysis

OpenAIRE

Kshirsagar, Parthraj R.; Hegde, Harsha; Pai, Sandeep R.

2016-01-01

Background and Aim: This study was designed to understand the effect of storage in polypropylene microcentrifuge tubes and glass vials during ultra-flow liquid chromatographic (UFLC) analysis. Materials and Methods: One ml of methanol was placed in polypropylene microcentrifuge tubes (PP material, Autoclavable) and glass vials (Borosilicate) separately for 1, 2, 4, 8, 10, 20, 40, and 80 days intervals stored at ?4?C. Results: Contaminant peak was detected in methanol stored in polypropylene m...

Liquid chromatographic and ultraviolet spectrophotometric determination of bevantolol and hydrochlorothiazide in feeds.

Science.gov (United States)

Spurlock, C H; Schneider, H G

1984-01-01

Separate assay methods have been developed for the 2 components of an 80 + 20 drug blend of bevantolol and hydrochlorothiazide (HCT) in admixtures with animal feed. Drug/diet admixtures are extracted with methanol for reverse phase ion-pair liquid chromatographic (LC) assay of bevantolol, and with acetonitrile for ultraviolet spectrophotometric assay of HCT. Bevantolol, a cardioselective beta blocker, is separated from soluble feed components with an RP-18 column, using methanol-water-acetic acid (60 + 40 + 1) containing 0. 005M octane-sulfonic acid, sodium salt, as ion-pairing reagent. HCT is determined spectrophotometrically in acetonitrile extracts, using a suitable blank extract as reference. Average recovery of HCT from an admixture of 0.5 mg blend/g diet is 94.5% +/- 4.3 RSD and at 2.0 mg/g, 101.5% +/- 3.5 RSD. Bevantolol recovery from the same admixtures is 101.8% +/- 2.7 RSD and 99.0% +/- 3.5 RSD, respectively, using the method as described.

EPICOR-II resin degradation results from first resin samples of PF-8 and PF-20

International Nuclear Information System (INIS)

McConnell, J.W. Jr.; Sanders, R.D. Sr.

1985-12-01

The 28 March 1979 accident at Three Mile Island Unit 2 released approximately 560,000 gallons of contaminated water to the Auxiliary and Fuel Handling Buildings. The water was decontaminated using a demineralization system called EPICOR-II developed by Epicor, Inc. The Low-Level Waste Data Base Development - EPICOR-II Resin/Liner Investigation Project is studying the chemical and physical conditions of the synthetic ion exchange resins found in several EPICOR-II prefilters. This report summarizes results and analyses of the first sampling of ion exchange resins from EPICOR-II prefilters PE-8 and -20. Results are compared with baseline data from tests performed on unirradiated Epicor, Inc. resins to determine if degradation has occurred due to the high internal radiation dose received by the EPICOR-II resins. Results also are compared with recent findings on resin degradation by Battelle Columbus Laboratories and Brookhaven National Laboratory. Analyses comparing test results of resins from EPICOR-II prefilters PF-8 and -20 with unirradiated resins obtained from Epicor, Inc. show resin degradation has occurred in some of the EPICOR-II resins examined. The mechanism of degradation is compared with work of other researchers and is consistent with their findings. The strong acid cation resins (divinylbenzene, styrene base structure) are losing effective cross-linking along with scission of functional groups and are experiencing first an increase and eventually a decrease in total exchange capacity as the absorbed radiation dose increases. The phenolic cation resins (phenol-formaldehyde base structure) show a loss of effective cross-linking and oxidation of the polymer chain. Analyses of resins removed from EPICOR-II prefilters PF-8 and -20 over the next several years should show a further increase in degradation

Preparation of molecularly imprinted adsorptive resin for trapping of ligustrazine from the traditional Chinese herb Ligusticum chuanxiong Hort

International Nuclear Information System (INIS)

Guo Zhifeng; Guo Tingting; Guo Mufan

2008-01-01

A highly selective molecularly imprinted adsorptive resin for ligustrazine was prepared by melamine-urea-formaldehyde (MUF) gel. In the experiments, two pieces of MUF gel were synthesized firstly; one was added ligustrazine hydrochloride as the template molecule in it to prepare the imprinted adsorptive resin, and the other was not. Scanning electron microscopy (SEM) revealed that both resins were the porous with a network structure whether or not it was added template molecule. The imprinted adsorptive resin had an absorbability of 85.22% measured by a 200 mg L -1 solution of ligustrazine hydrochloride at room temperature. The resin of MUF without template, on the other hand, displayed an adsorption capacity of almost zero. It illuminated the imprinted adsorptive resin formed ligustrazine recognition sites when the template molecule had been eluted. In the present paper, ligustrazine was effectively separated and enriched from herbs by using a solid-phase adsorptive column filled with the imprinted adsorptive resin. Its eluate, obtained from three kinds of solvents, was analyzed by GC-MS, and the results indicated that the imprinted adsorptive resin showed a high selectivity for ligustrazine. This is believed to be beneficial for extracting natural and highly purified ligustrazine

Chromatographic, Spectroscopic and Mass Spectrometric Approaches for Exploring the Habitability of Mars in 2012 and Beyond with the Curiosity Rover

Science.gov (United States)

Mahaffy, Paul

2012-01-01

The Sample Analysis at Mars (SAM) suite of instruments on the Curiosity Rover of Mars Science Laboratory Mission is designed to provide chemical and isotopic analysis of organic and inorganic volatiles for both atmospheric and solid samples. The goals of the science investigation enabled by the gas chromatograph mass spectrometer and tunable laser spectrometer instruments of SAM are to work together with the other MSL investigations is to quantitatively assess habitability through a series of chemical and geological measurements. We describe the multi-column gas chromatograph system employed on SAM and the approach to extraction and analysis of organic compounds that might be preserved in ancient martian rocks.

Radium separation through complexation by aqueous crown ethers and ion exchange or solvent extraction

Energy Technology Data Exchange (ETDEWEB)

Chiarizia, R.; Dietz, M.L.; Horwitz, E.P. [Argonne National Lab., IL (United States). Chemistry Div.; Burnett, W.C. [Florida State Univ., Tallahassee, FL (United States). Dept. of Oceanography

1997-11-01

The effect of three water-soluble, unsubstituted crown ethers (15-crown-5 (15C5), 18-crown-6 (18C6) and 21-crown-7 (21C7)) on the uptake of Ca, Sr, Ba and Ra cations by a sulfonic acid cation exchange resin, and on the extraction of the same cations by xylene solutions of dinonylnaphthalenesulfonic acid (HDNNS) from aqueous hydrochloric acid solutions has been investigated. The crown ethers enhance the sorption of the larger cations by the ion exchange resin, thereby improving the resin selectivity over calcium, a result of a synergistic interaction between the crown ether and the ionic functional groups of the resin. Similarly, the extraction of the larger alkaline earth cations into xylene by HDNNS is strongly synergized by the presence of the crown ethers in the aqueous phase. Promising results for intra-Group IIa cation separations have been obtained using each of the three crown ethers as the aqueous ligands and the sulfonic acid cation exchange resin. Even greater separation factors for the radium-calcium couple have been measured with the crown-ethers and HDNNS solutions in the solvent extraction mode. The application of the uptake and extraction results to the development of radium separation schemes is discussed and a possible flowchart for the determination of {sup 226}Ra/{sup 228}Ra in natural waters is presented.

Fractional, biodegradable and spectral characteristics of extracted and fractionated sludge extracellular polymeric substances.

Science.gov (United States)

Wei, Liang-Liang; Wang, Kun; Zhao, Qing-Liang; Jiang, Jun-Qiu; Kong, Xiang-Juan; Lee, Duu-Jong

2012-09-15

Correlation between fractional, biodegradable and spectral characteristics of sludge extracellular polymeric substances (EPS) by different protocols has not been well established. This work extracted sludge EPS using alkaline extractants (NH₄OH and formaldehyde + NaOH) and physical protocols (ultrasonication, heating at 80 °C or cation exchange resin (CER)) and then fractionated the extracts using XAD-8/XAD-4 resins. The alkaline extractants yielded more sludge EPS than the physical protocols. However, the physical protocols extracted principally the hydrophilic components which were readily biodegradable by microorganisms. The alkaline extractants dissolved additional humic-like substances from sludge solids which were refractory in nature. Different extraction protocols preferably extracted EPS with distinct fractional, biodegradable and spectral characteristics which could be applied in specific usages. Copyright © 2012 Elsevier Ltd. All rights reserved.

Post-irradiation hardness of resin-modified glass ionomer cements and a polyacid-modified composite resin

International Nuclear Information System (INIS)

Yap, A.U.J.

1997-01-01

This study examined the post-irradiation hardness of resin-modified glass ionomer cements and a polyacid-modified composite resin using a digital microhardness tester. Change in hardness of these materials over a period of 6 months was compared to that of conventional glass ionomer cements and a composite resin. With the exception of the composite resin, all materials showed a significant increase in hardness over 24 h after their initial set. Dual-cure resin-modified glass ionomer cements showed decreased hardness with increased storage time in saline at 37 o C. Results suggest that the addition of resins to glass ionomer cements does not improve initial hardness and does not negate the acid-base reaction of conventional cements. Resin addition may, however, lead to increased water sorption and decreased hardness. (author)

Thermal cycling effects on adhesion of resin-bovine enamel junction among different composite resins.

Science.gov (United States)

Chen, Wen-Cheng; Ko, Chia-Ling; Wu, Hui-Yu; Lai, Pei-Ling; Shih, Chi-Jen

2014-10-01

Thermal cycling is used to mimic the changes in oral cavity temperature experienced by composite resins when used clinically. The purpose of this study is to assess the thermal cycling effects of in-house produced composite resin on bonding strength. The dicalcium phosphate anhydrous filler surfaces are modified using nanocrystals and silanization (w/NP/Si). The resin is compared with commercially available composite resins Filtek Z250, Z350, and glass ionomer restorative material GIC Fuji-II LC (control). Different composite resins were filled into the dental enamel of bovine teeth. The bond force and resin-enamel junction graphical structures of the samples were determined after thermal cycling between 5 and 55°C in deionized water for 600 cycles. After thermal cycling, the w/NP/Si 30wt%, 50wt% and Filtek Z250, Z350 groups showed higher shear forces than glass ionomer GIC, and w/NP/Si 50wt% had the highest shear force. Through SEM observations, more of the fillings with w/NP/Si 30wt% and w/NP/Si 50wt% groups flowed into the enamel tubule, forming closed tubules with the composite resins. The push-out force is proportional to the resin flow depth and uniformity. The push-out tubule pore and resin shear pattern is the most uniform and consistent in the w/NP/Si 50wt% group. Accordingly, this developed composite resin maintains great mechanical properties after thermal cycling. Thus, it has the potential to be used in a clinical setting when restoring non-carious cervical lesions. Copyright © 2014 Elsevier Ltd. All rights reserved.

Resin composites

DEFF Research Database (Denmark)

Benetti, Ana Raquel; Peutzfeldt, Anne; Lussi, Adrian

2014-01-01

OBJECTIVE: To investigate how the modulus of elasticity of resin composites influences marginal quality in restorations submitted to thermocyclic and mechanical loading. METHODS: Charisma, Filtek Supreme XTE and Grandio were selected as they were found to possess different moduli of elasticity...... of resin composite (p=0.81) on the quality of dentine margins was observed, before or after loading. Deterioration of all margins was evident after loading (p....008). CONCLUSIONS: The resin composite with the highest modulus of elasticity resulted in the highest number of gap-free enamel margins but with an increased incidence of paramarginal enamel fractures. CLINICAL SIGNIFICANCE: The results from this study suggest that the marginal quality of restorations can...

Literature search on the use of resins for treatment of radioactive wastes

International Nuclear Information System (INIS)

AlMahamid, I.; Smith, B.M.

1997-10-01

Over 100 commercial providers with mixed-waste treatability capabilities exist in the US. The maturity level of these technologies varies from a bench scale to a pilot or a commercial scale. The techniques include deactivation, chemical oxidation, recovery of metals, stabilization, vitrification, incineration, biodegradation, and chemical extraction. This report focuses on the use of resins to remove actinides and heavy metals from aqueous waste streams. Only the literature that described resins with high removing efficiency are presented here. The majority of the literature reviewed are proceedings and national or international reports ordered through the Berkeley Lab Library. Some of the reports that the authors requested have not yet arrived. Only a few papers were found in the open literature (journals or magazines). Although this report does not include all existing references, it provides an accurate assessment of efficient resins to be considered for waste minimization procedures. 70 refs

Lipase and protease extraction from activated sludge

DEFF Research Database (Denmark)

Gessesse, Amare; Dueholm, Thomas; Petersen, Steffen B.

2003-01-01

of gentle and efficient enzyme extraction methods from environmental samples is very important. In this study we present a method for the extraction of lipases and proteases from activated sludge using the non-ionic detergent Triton X-100, EDTA, and cation exchange resin (CER), alone or in combination...

Chromatographic fingerprint analysis of yohimbe bark and related dietary supplements using UHPLC/UV/MS.

Science.gov (United States)

Sun, Jianghao; Chen, Pei

2012-03-05

A practical ultra high-performance liquid chromatography (UHPLC) method was developed for fingerprint analysis of and determination of yohimbine in yohimbe barks and related dietary supplements. Good separation was achieved using a Waters Acquity BEH C(18) column with gradient elution using 0.1% (v/v) aqueous ammonium hydroxide and 0.1% ammonium hydroxide in methanol as the mobile phases. The study is the first reported chromatographic method that separates corynanthine from yohimbine in yohimbe bark extract. The chromatographic fingerprint analysis was applied to the analysis of 18 yohimbe commercial dietary supplement samples. Quantitation of yohimbine, the traditional method for analysis of yohimbe barks, were also performed to evaluate the results of the fingerprint analysis. Wide variability was observed in fingerprints and yohimbine content among yohimbe dietary supplement samples. For most of the dietary supplements, the yohimbine content was not consistent with the label claims. Copyright © 2011. Published by Elsevier B.V.

Curcumin and Boswellia serrata gum resin extract inhibit chikungunya and vesicular stomatitis virus infections in vitro.

Science.gov (United States)

von Rhein, Christine; Weidner, Tatjana; Henß, Lisa; Martin, Judith; Weber, Christopher; Sliva, Katja; Schnierle, Barbara S

2016-01-01

Chikungunya virus (CHIKV) is a mosquito-transmitted alphavirus that causes chikungunya fever and has infected millions of people mainly in developing countries. The associated disease is characterized by rash, high fever, and severe arthritis that can persist for years. CHIKV has adapted to Aedes albopictus, which also inhabits temperate regions including Europe and the United States of America. CHIKV has recently caused large outbreaks in Latin America. No treatment or licensed CHIKV vaccine exists. Traditional medicines are known to have anti-viral effects; therefore, we examined whether curcumin or Boswellia serrata gum resin extract have antiviral activity against CHIKV. Both compounds blocked entry of CHIKV Env-pseudotyped lentiviral vectors and inhibited CHIKV infection in vitro. In addition, vesicular stomatitis virus vector particles and viral infections were also inhibited to the same extent, indicating a broad antiviral activity. Although the bioavailability of these compounds is rather poor, they might be used as a lead structure to develop more effective antiviral drugs or might be used topically to prevent CHIKV spread in the skin after mosquito bites. Copyright © 2015 Elsevier B.V. All rights reserved.

Eichrom's ABEC trademark resins: Alkaline radioactive waste treatment, radiopharmaceutical, and potential hydrometallurgical applications

International Nuclear Information System (INIS)

Bond, A.H.; Gula, M.J.; Chang, F.; Rogers, R.D.

1997-01-01

Eichrom's ABEC trademark resins selectivity extract certain anions from high ionic strength acidic, neutral, or strongly alkaline media, and solute stripping can be accomplished by eluting with water. ABEC resins are stable to pH extreme and radiolysis and operate in high ionic strength and/or alkaline solutions where anion-exchange is often ineffective. Potential applications of the ABEC materials include heavy metal and ReO 4 - separations in hydrometallurgy and purification of perrhenate iodide, and iodate in radiopharmaceutical production. Separation of 99m TcO 4 - from its 99 MoO 4 2- parent and stripping with water or physiological saline solution have been demonstrated for radiopharmaceutical applications. Removal of 99 TcO 4 - and 129 I - from alkaline tank wastes has also been successfully demonstrated. The authors will discuss the scale-up studies, process-scale testing, and market development of this new extraction material

Comparison of Mechanical Properties of Resin Composites with Resin Modified Glass Ionomers

Directory of Open Access Journals (Sweden)

Taha NA

2015-06-01

Full Text Available Statement of Problem: There are controversial reports regarding physical and mechanical properties of resin composites and glass ionomer cements. Some revealed higher strength and hardness for resin composites while others showed a comparable value for glass ionomer cements. Evaluation of mechanical properties of different types of resin composites in comparison with resin modified glass ionomers is not widely studied. Objectives: To measure and compare the flexural strength and Vickers hardness of three resin composites and two resins modified glass ionomer cements before and after ageing. Materials and Methods: Three resin composites, i.e. Filtek Supreme XTE (3M ESPE, Ice (SDI, Gradia (GC, and two resins modified glass ionomers, i.e. Fuji II LC (GC and Riva Light Cure (SDI, were selected. Ten barshaped specimens were prepared for each material and cured using LED curing light. After 24 hours storage in distilled water at 37oC, the specimens were randomly divided into two equal groups (n=5. The first group was tested as a baseline and the second group was restored at 37oC for another 29 days. Flexural strength was performed by four-point bending test using universal testing machine at crosshead speed of 0.5mm/min, and the maximum load at failure was recorded. The specimen’s halves were used for evaluating Vickers hardness, using a Digital Hardness Tester (300 g/15 sec and the Vickers hardness number (VHN was recorded. Data were analyzed using one-way analysis of variance (ANOVA, Tukey’s and student’s t-test. Results: After 24 hours of immersion, the highest hardness number was found for Filtek Supreme and Ice and the highest flexural strength was obtained for Gradia. After 30 days of storage, hardness of Fuji II LC and Gradia showed a significant decrease; flexural strength of Ice and Fuji II LC revealed a significant increase while Gradia and Filtek Supreme showed a significant decrease. Conclusions: Resin modified glass ionomers showed

Preparation and characterization of molecularly-imprinted polymers for extraction of sanshool acid amide compounds followed by their separation from pepper oil resin derived from Chinese prickly ash (Zanthoxylum bungeanum).

Science.gov (United States)

Chen, Xiaolong; Jin, Xinkai; Li, Yao; Chen, Guangjing; Chen, Kewei; Kan, Jianquan

2018-01-01

Molecularly imprinted polymers were prepared using the molecular structure analogs of sanshool as template molecule, 2-vinylpyridine and β-cyclodextrin as double functional monomers, ethylene dimethacrylate as cross linker, and azobisisobutyronitrile as initiator. The structural characteristics of the polymers were determined by Fourier-transform infrared spectroscopy and scanning electron microscopy. Dynamic adsorption and isothermal adsorption were also investigated. The molecularly imprinted polymers were used to prepare a molecularly imprinted solid-phase extraction column in order to separate acid amide components from pepper oil resin derived from Chinese prickly ash (Zanthoxylum bungeanum). After eluting, the percentage of acid amide components was enhanced to 92.40 ± 1.41% compared with 23.34 ± 1.21% in the initial pepper oil resin, indicating good properties of purification of molecularly imprinted polymers and potential industrial application. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of adhesive resin cements on bond strength of ceramic core materials to dentin.

Science.gov (United States)

Gundogdu, M; Aladag, L I

2018-03-01

The aim of the present study was to evaluate the effects of self-etch and self-adhesive resin cements on the shear bond strength of ceramic core materials bonded to dentin. Extracted, caries-free, human central maxillary incisor teeth were selected, and the vestibule surfaces were cut flat to obtain dentin surfaces. Ceramic core materials (IPS e.max Press and Prettau Zirconia) were luted to the dentin surfaces using three self-etch adhesive systems (Duo-Link, Panavia F 2.0, and RelyX Ultimate Clicker) and two self-adhesive resin systems (RelyX U200 Automix and Maxcem Elite). A shear bond strength test was performed using a universal testing machine. Failure modes were observed under a stereomicroscope, and bonding interfaces between the adhesive resin cements and the teeth were evaluated with a scanning electron microscope. Data were analyzed with Student's t-test and one-way analysis of variance followed by Tukey's test (α = 0.05). The type of adhesive resin cement significantly affected the shear bond strengths of ceramic core materials bonded to dentin (P materials when the specimens were luted with self-adhesive resin cements (P materials.

Sorption Efficiency of a New Sorbent towards Cadmium(II: Methylphosphonic Acid Grafted Polystyrene Resin

Directory of Open Access Journals (Sweden)

Nacer Ferrah

2013-01-01

Full Text Available A new chelating polymeric sorbent has been developed using polystyrene resin grafted with phosphonic acid. After characterization by FTIR and elementary analysis, the new resin has been investigated in liquid-solid extraction of cadmium(II. The results indicated that phosphonic resin could adsorb Cd(II ion effectively from aqueous solution. The adsorption was strongly dependent on the pH of the medium and the optimum pH value level for better sorption was between 3.2 and 5.2. The influence of other analytical parameters including contact time, amount of resin, metal ion concentration, and the presence of some electrolytes was investigated. The maximum uptake capacity of Cd(II ions was 37,9 mg·g−1 grafted resin at ambient temperature, at an initial pH value of 5.0. The overall adsorption process was best described by pseudo second-order kinetic. When Freundlich and Langmuir isotherms were tested, the latter had a better fit with the experimental data. Furthermore, more than 92% of Cd(II could be eluted by using 1.0 mol·L−1 HCl in one cycle.

Probabilistic peak detection for first-order chromatographic data

NARCIS (Netherlands)

Lopatka, M.; Vivó-Truyols, G.; Sjerps, M.J.

2014-01-01

We present a novel algorithm for probabilistic peak detection in first-order chromatographic data. Unlike conventional methods that deliver a binary answer pertaining to the expected presence or absence of a chromatographic peak, our method calculates the probability of a point being affected by

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.

The mechanism of uranium adsorption on Resin 508 and isoelectric point of the resin

International Nuclear Information System (INIS)

Han Qingping; Lu Weichang; Su Huijuan; Hu Jinbo; Zhang Liqin; Chen Banglin

1990-01-01

The adsorption process of uranium by Resin 508 at the solid-liquid interface was investigated and the mechanism of uranium adsorption including adsorption dynamics, adsorption thermodynamics and isoelectric point of resin was studied. The results are as follows: The maximum of uranium adsorption is attained at pH5-7; Uranium adsorption isotherm by Resin 508 in experimental conditions agrees with Langmuir's adsorption isotherm, the maximum of uranium adsorbed (Vm) is 716 mg U/g-dried resin; The adsorption of uranium by Resin 508 is an endothermic reaction and ΔH = 16.87 kJ/mol; The exchange-adsorption rate is mainly controlled by liquid film diffusion; The isoelectric points of Resin 508 before and after uranium adsorption are found to be pH7.5 and pH5.7 respectively. It is a specific adsorption for uranium

Effect of light-curing units on microleakage under dental composite resins

Science.gov (United States)

Queiroz, R. S.; Bandéca, M. C.; Calixto, L. R.; Saade, E. G.; Nadalin, M. R.; Andrade, M. F.; Porto-Neto, S. T.

2009-09-01

The aim of this study was to determine the effect of two light-curing units (QTH and LED) on microleakage of Class II composite resin restorations with dentin cavosurface margins. Twenty extracted mandibular first premolars, free of caries and fractures were prepared two vertical “slot” cavities in the occluso-mesial and -destal surfaces (2 mm buccal-lingually, 2 mm proximal-axially and cervical limit in enamel) and divided into 4 equal groups ( n = 8): GI and GII: packable posterior composite light-activated with LED and QTH, respectively; GIII and GIV: micro-hybrid composite resin light-activated with LED and QTH, respectively. The composite resins were applied following the manufacturer’s instructions. After 24 h of water storage specimens were subjected to thermocycling for a total of 500 cycles at 5 and 55°C and the teeth were then sealed with impermeable material. Teeth were immersed in 0.5% Basic fuchsin during 24 h at room temperature, and zero to three levels of penetration score were attributed. The Mann-Whitney and Kruskal-Wallis tests showed significant statistically similar ( P > 0.05) from GI to GII and GIII to GIV, which the GII (2.750) had the highest mean scores and the GIII and GIV (0.875) had lowest mean scores. The use of different light-curing units has no influence on marginal integrity of Class II composite resin restorations and the proprieties of composite resins are important to reduce the microleakage.

Liquid-chromatographic determination of sarafloxacin residues in channel catfish muscle-tissue

Science.gov (United States)

Meinertz, J.R.; Dawson, V.K.; Gingerich, W.H.; Cheng, B.; Tubergen, M.M.

1994-01-01

A liquid chromatographic method is described for the determination of sarafloxacin hydrochloride residues i n channel catfish (ictalurus punctatus) fillets. Sarafloxacin was extracted from fillet tissue with acetonitrile=water (1 + 1). The extract was centrifuged and the supernatant was partitioned with hexane. The aqueous fraction was filtered through a 0.45 Mum filter and evaporated to dryness. The sample was redissolved with 20% acetonitrile-methanol (3 + 2) and 80% trifluoroacetic acid (0.1%), Centrifuged, and filtered to remove proteins. Samples were analyzed by chromatography with gradient elution on a c18 column and with fluorescence detection (excitation at 280 nm and emission above 389 nm). Mean recoveries ranged from 85.4 To 104%, and relative standard deviations ranged from 1.06 To 5.58% In samples spiked at concentrations of 10.0-863.8 Ng/g. The method detection limit for sarafloxacin was 1.4 Ng/g.

Separation and preconcentration of uranium from different matrices by extraction chromatography on U-TEVA resin

International Nuclear Information System (INIS)

Becquart, Elena T.; Bianco, Gladis N.; Chiacchio, Hugo A.; Palestrini, Leonardo J.; Servant, Roberto E.

1999-01-01

The objectives of this work were the determination of uranium in effluents and spring waters, in high and low U 3 O 8 containing minerals and in Zircaloy. The separations were done by extraction chromatography, using U-TEVA Spec (uranium tetravalent actinide specific, ElChroM, Illinois, USA), a commercial resin consisting of Amberlite XAD-7 (Rohm and Haas), an inert support of a non ionic polymeric adsorbent, soaked by diamylamylphosphonate, a selective extractant. Disposable plastic columns, 7.9 mm internal diameter, 10 cm total length, with a bed 4.5 cm high and 2 ml volume were used. Quantification was done by spectrophotometric determination of uranium with the chromogenic reagent 2-(5-bromo-2-pyridylazo)-5-diethyl aminophenol (Br-PADAP). The following working conditions were optimized: uranium sorption and preconcentration, elution, separation of others cations as Zr (IV), Gd (III), Th (IV) and uranium elution, using different solutions of nitric or hydrochloric acids as convenient. Break through was 30 mg of uranium and capacity at total saturation was between 35 and 40 mg U/ml of bed. Programs were developed for previous leaching of minerals and Zircaloy in a microwave oven. Procedures operations were satisfactory with recoveries higher than 95% and a percent relative standard deviation better than 1% for 100 μg of uranium, on five replicates. Quantification limit was 4 ppb (0.1 μg of U in the 25 ml volumetric flask where color was developed with chromogenic reagent), but if uranium is concentrated 5 times in the column and a 5 ml volume is used for elution, a sample containing 0.4 ppb of uranium can be analysed. Absorbance was measured at λ = 578 nm using 5 cm cells. The extraction system is profitable because it allows to work at room temperature, with gravity flow, high specificity and minimum waste generation. The objectives have been satisfactorily accomplished, so an easy, in small columns, uranium sorbing system is available to be used in the

An integrated methodological approach to the computer-assisted gas chromatographic screening of basic drugs in biological fluids using nitrogen selective detection.

Science.gov (United States)

Dugal, R; Massé, R; Sanchez, G; Bertrand, M J

1980-01-01

This paper presents the methodological aspects of a computerized system for the gas-chromatographic screening and primary identification of central nervous system stimulants and narcotic analgesics (including some of their respective metabolites) extracted from urine. The operating conditions of a selective nitrogen detector for optimized analytical functions are discussed, particularly the effect of carrier and fuel gas on the detector's sensitivity to nitrogen-containing molecules and discriminating performance toward biological matrix interferences. Application of simple extraction techniques, combined with rapid derivatization procedures, computer data acquisition, and reduction of chromatographic data are presented. Results show that this system approach allows for the screening of several drugs and their metabolites in a short amount of time. The reliability and stability of the system have been tested by analyzing several thousand samples for doping control at major international sporting events and for monitoring drug intake in addicts participating in a rehabilitation program. Results indicate that these techniques can be used and adapted to many different analytical toxicology situations.

Resin regenerating device in condensate desalting system

International Nuclear Information System (INIS)

Sato, Yoshiaki; Igarashi, Hiroo; Oosumi, Katsumi; Nishimura, Yusaku; Ebara, Katsuya; Shindo, Norikazu.

1984-01-01

Purpose: To improve the accuracy in the separation of anionic and cationic exchange resins. Constitution: Resins transferred from a condensate desalting column are charged in a cationic exchange resin column. The temperature of water for separating and transferring the resins is measured by a temperature detector disposed in a purified water injection line, and water is adjusted to a suitable flow rate for the separation and transfer of the resins by an automatic flow rate control valve, and then is injected. The resins are separated into cationic exchange resins and anionic exchange resins, in which only the anionic exchange resins are transferred, through an anionic exchange transfer line, into an anionic exchange resin column. By controlling the flow rate depending on the temperature of the injected water, the developing rate of the resin layer is made constant to enable separation and transfer of the resins at high accuracy. (Seki, T.)

Characteristics of floc formation of anion and cation exchange resin in precoat filter using powdered ion exchange resin

International Nuclear Information System (INIS)

Adachi, Tetsurou; Sawa, Toshio; Shindoh, Toshikazu.

1989-01-01

The filtration performance of mixed filter aid consisting of powdered anion and cation exchange resins used in the precoat filter is closely related to the characteristics of floc formation. The physical, chemical and electrochemical properties of powdered ion exchange resin were measured and the factors related to floc formation of anion and cation exchange resin were investigated by measuring the specific settle volume of resin floc as an evaluating index. It was found that these factors were mixing ratio, nature of resins and particle size of resins. In addition, it was assumed on the bases of these results that the amount of resin floc was related to sum of the surface electric charges of both resins. The filling ratio of resin floc was related to their product by multiplication and an experimental expression was obtained. The specific settle volume of resin floc could then be simulated by particle size, surface area, ion exchange capacity and degree of ionization of the powdered ion exchange resin. (author)

Characteristics of floc formation of anion and cation exchange resin in precoat filter using powdered ion exchange resin

Energy Technology Data Exchange (ETDEWEB)

Adachi, Tetsurou (Nitto Denko Corp., Ibaraki, Osaka (Japan)); Sawa, Toshio; Shindoh, Toshikazu

1989-09-01

The filtration performance of mixed filter aid consisting of powdered anion and cation exchange resins used in the precoat filter is closely related to the characteristics of floc formation. The physical, chemical and electrochemical properties of powdered ion exchange resin were measured and the factors related to floc formation of anion and cation exchange resin were investigated by measuring the specific settle volume of resin floc as an evaluating index. It was found that these factors were mixing ratio, nature of resins and particle size of resins. In addition, it was assumed on the bases of these results that the amount of resin floc was related to sum of the surface electric charges of both resins. The filling ratio of resin floc was related to their product by multiplication and an experimental expression was obtained. The specific settle volume of resin floc could then be simulated by particle size, surface area, ion exchange capacity and degree of ionization of the powdered ion exchange resin. (author).

Application of Resin in Pulp Technique for Ion Exchange Separation of Uranium from Alkaline Leachate

International Nuclear Information System (INIS)

Sreenivas, T.; Rajan, K.C.; Chakravartty, J.K.

2014-01-01

Conclusions: • Resin-in-pulp technique was applied for purification and enrichment of uranium values from a finely ground uranium ore leach slurry of alkaline nature using strong base anion exchange resin (size 500 - 675μm). • The chemical composition of the solution phase of the alkaline leach slurry (pH 9.5) was consisting of about 40 g/L of total dissolved solutes (TDS) predominantly with Na_2CO_3 and NaHCO_3 and minor levels of Na_2SO_4. The uranium content was only 730 mg/L and d50 of solids was 34μm. • Amongst the various commercially available resins studied PFA 4740 and 4783 having quaternary ammonium ion on polystyrene crosslink with divibyl benzez (DVB) gave best performance. The maximum loading capacity achieved in the RIP studies was about 60-65 g of U_3O_8/L of wet settled resin amounting to 98% of loading. This has necessitated 4 stages of counter-current extraction with overall contact time of 100 minutes at a resin to leach slurry volume ratio of about 1:50. Practically the entire uranium values loaded on the resin were eluted using NaCl. • The RIP process was found quite efficient for uranium bearing alkaline leach slurries.

Capillary gas chromatographic analysis of nerve agents using large volume injections. Final report

Energy Technology Data Exchange (ETDEWEB)

Deinum, T.; Nieuwenhuy, C.

1994-11-01

The procedure developed at TNO-Prins Maurits Laboratory (TNO-PML) for the verification of intact organophosphorus chemical warfare agents in water samples was improved. The last step in this procedure, the laborious and non-reproducible transfer of an ethyl acetate extract onto a Tenax-adsorption tube followed by thermal desorption of the Tenax-tube, was replaced by large volume injection of the extract onto a capillary gas chromatographic system. The parameters controlling the injection of a large volume of an extract (200 ul) were investigated and optimized. As ethyl acetate caused severe problems, potential new solvents were evaluated. With the improved procedure, the nerve agents sarin, tabun, soman, diisopropyl fluorophosphate (DFP) and VX could be determined in freshly prepared water samples at pg/ml (ppt) levels. The fate of the nerve agents under study in water at two pH`s (4.8 and 6) was investigated. For VX, the pH should be adjusted before extraction. Moreover, it is worthwhile to acidify water samples to diminish hydrolysis.

Characterisation of wax works of art by gas chromatographic procedures.

Science.gov (United States)

Regert, M; Langlois, J; Colinart, S

2005-10-14

To identify the various natural and synthetic substances used by sculptors at the end of the 19th century, several contemporary reference samples were investigated by high temperature gas chromatography (HT GC) and HT GC-MS. Using specific chromatographic conditions and minimising sample preparation, we could separate, detect and identify a wide range of biomolecular markers covering a great variety of molecular weights and volatilities, with a minimum amount of sample, in a single run. Beeswax, spermaceti, carnauba, candellila and Japan waxes as well as pine resin derivatives, animal fats, paraffin, ozokerite and stearin, used as additives in wax works of art, were chemically investigated. In the case of low volatile compounds, transbutylation was performed. The structure of long-chain esters of spermaceti was elucidated for the first time by HT GC-MS analysis. Such a method was then carried out on 10 samples collected on a statuette of Junon by Antoine-Louis Barye (Louvre Museum, Paris, France) and on a sculpture by Aimé-Jules Dalou (Musée de la Révolution Française, Vizille, France). The analytical results obtained provide new data on the complex recipes elaborated by sculptors at the end of the 19th century.

Improvement in char formability of phenolic resin for development of Carbon/Carbon composites

International Nuclear Information System (INIS)

Hajhosseini, M.; Payami, A.; Ghaffarian, S. R.; Rezadoust, A. M.

2008-01-01

In the processing of carbon/carbon composites using polymer resin as the matrix precursor, it is inevitable that a porous structure was formed after carbonization. As a result, densification by liquid phase impregnation followed by recarbonization is required to obtain a densified composite. Consequently, the char formability of resin is an important factor in reducing the number of densification cycles and hence the processing cost. In this study, a novel approach is adopted to improve the densification of carbon/carbon composites by using a new phenolic resin modified by pitch. For this purpose, soluble part of pitch was extracted and dispersed in resol type phenolic resin. The polymerization reaction was performed in presence of para-formaldehyde and a resol-pitch compound was obtained. The second compound was prepared by mixing novolac-furfural in 55:45 weight ratio containing 9% by weight hexamethylene tetramine. This compound was added to resol-pitch compound in 10,20,50 and 80 w %. The microstructure of carbonized resin was investigated by X-ray diffraction and char yield, and the linear and volumetric shrinkage were obtained. Results show that in 80:20 ratio of resol-pitch to novolac-furfural , the char yield would be maximized by 71% and volumetric shrinkage would be minimized at 16.4%. At the same time, XRD results indicate that the resin has a strong ability to graphitize carbon/carbon composites matrix as a necessary step for its processing

EDF specifications on nuclear grade resins

International Nuclear Information System (INIS)

Mascarenhas, Darren; Gressier, Frederic; Taunier, Stephane; Le-Calvar, Marc; Ranchoux, Gilles; Marteau, Herve; Labed, Veronique

2012-09-01

Ion exchange resins are widely used across EDF, especially within the nuclear division for the purification of water. Important applications include primary circuit, secondary circuit and effluent treatment, which require high quality nuclear grade resins to retain the dissolved species, some of which may be radioactive. There is a need for more and more efficient purification in order to decrease worker dose during maintenance but also to decrease volumes of radioactive resin waste. Resin performance is subject to several forms of degradation, including physical, chemical, thermal and radioactive, therefore appropriate resin properties have to be selected to reduce such effects. Work has been done with research institutes, manufacturers and on EDF sites to select these properties, create specifications and to continuously improve on these specifications. An interesting example of research regarding resin performance is the resin degradation under irradiation. Resins used in the CVCS circuit of EDF nuclear power plants are subject to irradiation over their lifetime. A study was carried out on the effects of total integrated doses of 0.1, 1 and 10 MGy on typically used EDF mixed bed resins in a 'mini-CVCS' apparatus to simultaneously test actual primary circuit fluid. The tests confirmed that the resins still perform efficiently after a typical CVCS radiation dose. Certain resins also need additional specifications in order to maintain the integrity of the particular circuits they are used in. Recently, EDF has updated its requirements on these high purity nuclear grade resins, produced generic doctrines for all products and materials used on site which include resins of all grades, and as a result have also updated a guide on recommended resin usage for the French fleet of reactors. An overview of the evolutions will be presented. (authors)

PY-GC-MS applied to the identification of synthetic resins in Brazilian painting

International Nuclear Information System (INIS)

Redigolo, Marcelo M.; Amaral, Priscila O.; Leao, Claudio; Crepaldi, Caike; Munita, Casimiro S.; Bustillos, Oscar V.; Russo, Tatiana; Mendonca, Valeria de

2015-01-01

Works of art are appreciated for their material and immaterial value. Restoring objects of art is a delicate procedure, mostly due to the irreversibility of the interventions. Hence, it is recommended to study the chemical composition of the object to avoid errors. The premise for restoring or conserving these objects is their physical preservation, i.e., it is advisable to avoid sampling and, when necessary, samples must be minute. The analytical techniques that fulfill these requirements are limited. Mass spectrometry (MS) is a versatile technique due to its hyphenation possibilities. Recently, it has being employed in the identification of natural and synthetic resins in works of art. Electron ionization (EI) is a powerful method of molecular fragmentation employed in the detection of volatile organic compounds by mass spectrometry. In this work, two micrograms (μg) of sample from a Brazilian contemporary painting were analyzed by pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) technique. A microfurnace-type pyrolyzer was coupled to a gas chromatograph, using a non-polar capillary column. The electron ionization was achieved applying 70 eV electron energy. This technique is suitable for the analysis of material from objects of art, being specific, accurate and requiring minimal sampling. The synthetic resin diallyl phthalate (DAP) was identified by the Py-GC/MS technique. (author)

PY-GC-MS applied to the identification of synthetic resins in Brazilian painting

Energy Technology Data Exchange (ETDEWEB)

Redigolo, Marcelo M.; Amaral, Priscila O.; Leao, Claudio; Crepaldi, Caike; Munita, Casimiro S.; Bustillos, Oscar V., E-mail: marcelo.redigolo@usp.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Russo, Tatiana; Mendonca, Valeria de [Pinacoteca do Estado de Sao Paulo, SP (Brazil)

2015-07-01

Works of art are appreciated for their material and immaterial value. Restoring objects of art is a delicate procedure, mostly due to the irreversibility of the interventions. Hence, it is recommended to study the chemical composition of the object to avoid errors. The premise for restoring or conserving these objects is their physical preservation, i.e., it is advisable to avoid sampling and, when necessary, samples must be minute. The analytical techniques that fulfill these requirements are limited. Mass spectrometry (MS) is a versatile technique due to its hyphenation possibilities. Recently, it has being employed in the identification of natural and synthetic resins in works of art. Electron ionization (EI) is a powerful method of molecular fragmentation employed in the detection of volatile organic compounds by mass spectrometry. In this work, two micrograms (μg) of sample from a Brazilian contemporary painting were analyzed by pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) technique. A microfurnace-type pyrolyzer was coupled to a gas chromatograph, using a non-polar capillary column. The electron ionization was achieved applying 70 eV electron energy. This technique is suitable for the analysis of material from objects of art, being specific, accurate and requiring minimal sampling. The synthetic resin diallyl phthalate (DAP) was identified by the Py-GC/MS technique. (author)

System for removing contaminants from plastic resin

Science.gov (United States)

Bohnert, George W.; Hand, Thomas E.; DeLaurentiis, Gary M.

2010-11-23

A resin recycling system that produces essentially contaminant-free synthetic resin material in an environmentally safe and economical manner. The system includes receiving the resin in container form. A grinder grinds the containers into resin particles. The particles are exposed to a solvent in one or more solvent wash vessels, the solvent contacting the resin particles and substantially removing contaminants on the resin particles. A separator is used to separate the resin particles and the solvent. The resin particles are then placed in solvent removing element where they are exposed to a solvent removing agent which removes any residual solvent remaining on the resin particles after separation.

Water-compatible dummy molecularly imprinted resin prepared in aqueous solution for green miniaturized solid-phase extraction of plant growth regulators.

Science.gov (United States)

Wang, Mingyu; Chang, Xiaochen; Wu, Xingyu; Yan, Hongyuan; Qiao, Fengxia

2016-08-05

A water-compatible dummy molecularly imprinted resin (MIR) was synthesized in water using melamine, urea, and formaldehyde as hydrophilic monomers of co-polycondensation. A triblock copolymer (PEO-PPO-PEO, P123) was used as porogen to dredge the network structure of MIR, and N-(1-naphthyl) ethylenediamine dihydrochloride, which has similar shape and size to the target analytes, was the dummy template of molecular imprinting. The obtained MIR was used as the adsorbent in a green miniaturized solid-phase extraction (MIR⬜mini-SPE) of plant growth regulators, and there was no organic solvent used in the entire MIR⬜mini-SPE procedure. The calibration linearity of MIR⬜mini-SPE⬜HPLC method was obtained in a range 5⬜250ngmL(↙1) for IAA, IPA, IBA, and NAA with correlation coefficient (r) Ⱕ0.9998. Recoveries at three spike levels are in the range of 87.6⬜100.0% for coconut juice with relative standard deviations Ⱔ8.1%. The MIR⬜mini-SPE method possesses the advantages of environmental friendliness, simple operation, and high efficiency, so it is potential to apply the green pretreatment strategy to extraction of trace analytes in aqueous samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Improvement of skin condition in striae distensae: development, characterization and clinical efficacy of a cosmetic product containing Punica granatum seed oil and Croton lechleri resin extract

Directory of Open Access Journals (Sweden)

Bogdan C

2017-02-01

Full Text Available Cătălina Bogdan,1 Sonia Iurian,2 Ioan Tomuta,2 Mirela Moldovan1 1Department of Dermatopharmacy and Cosmetics, 2Department of Pharmaceutical Technology and Biopharmacy, Faculty of Pharmacy, University of Medicine and Pharmacy Iuliu Hatieganu, Cluj-Napoca, Romania Abstract: Striae distensae are a frequent skin condition associated with pregnancy, weight change or lack of skin elasticity. The aim of this research was to obtain a topical product containing herbal active ingredients with documented antioxidant and anti-inflammatory activity (Punica granatum seed oil and Croton lechleri resin extract and demonstrate its positive effect on prevention and treatment of striae distensae. First, the cream base formulation was optimized through experimental design. Secondly, the cream containing the two active ingredients was investigated in an interventional nonrandomized clinical trial. The clinical outcome was assessed through biophysical parameters and ultrasonographic evaluation. The state of the skin was evaluated by biophysical measurements and ultrasonography at the beginning of the study and after 3 and 6 weeks. The experimental design was successfully used to set the best ranges for the technological and formulation factors to obtain a cosmetic formulation with optimal characteristics. The study of clinical efficacy on the optimal formulation revealed an increase in the dermis thickness, hydration and elasticity values in both groups after 6 weeks of cream application. The new oil-in-water cream containing P. granatum seed oil and C. lechleri resin extract can be helpful in the prevention or improving of skin changes associated with striae. Keywords: stretch marks, ultrasonography, texture analysis, design of experiments, oil-in-water emulsion

Accurate determination of 41Ca concentrations in spent resins from the nuclear industry by Accelerator Mass Spectrometry

International Nuclear Information System (INIS)

Nottoli, Emmanuelle; Bourlès, Didier; Bienvenu, Philippe; Labet, Alexandre; Arnold, Maurice; Bertaux, Maité

2013-01-01

The radiological characterisation of nuclear waste is essential for managing storage sites. Determining the concentration of Long‐Lived RadioNuclides (LLRN) is fundamental for their long-term management. This paper focuses on the measurement of low 41 Ca concentrations in ions exchange resins used for primary fluid purification in Pressurised Water Reactors (PWR). 41 Ca concentrations were successfully measured by Accelerator Mass Spectrometry (AMS) after the acid digestion of resin samples, followed by radioactive decontamination and isobaric suppression through successive hydroxide, carbonate, nitrate and final CaF 2 precipitations. Measured 41 Ca concentrations ranged from 0.02 to 0.03 ng/g, i.e. from 0.06 to 0.09 Bq/g. The 41 Ca/ 60 Co activity ratios obtained were remarkably reproducible and in good agreement with the current ratio used for resins management. - Highlights: • In the context of radioactive waste management, this study aimed at measuring 41 Ca in spent resins using Accelerator Mass Spectrometry. • A chemical treatment procedure was developed to quantitatively recover calcium in solution and selectively extract it. • Developed firstly on synthetic matrices, the chemical treatment procedure was then successfully applied to real resin samples. • Accelerator mass spectrometry allowed measuring concentrations of 41 Ca in spent resins as low as 0.02 ng/g of dry resin. • Final results are in agreement with current data used for spent resins management

[Acrylic resin removable partial dentures].

Science.gov (United States)

de Baat, C; Witter, D J; Creugers, N H J

2011-01-01

An acrylic resin removable partial denture is distinguished from other types of removable partial dentures by an all-acrylic resin base which is, in principle, solely supported by the edentulous regions of the tooth arch and in the maxilla also by the hard palate. When compared to the other types of removable partial dentures, the acrylic resin removable partial denture has 3 favourable aspects: the economic aspect, its aesthetic quality and the ease with which it can be extended and adjusted. Disadvantages are an increased risk of caries developing, gingivitis, periodontal disease, denture stomatitis, alveolar bone reduction, tooth migration, triggering of the gag reflex and damage to the acrylic resin base. Present-day indications are ofa temporary or palliative nature or are motivated by economic factors. Special varieties of the acrylic resin removable partial denture are the spoon denture, the flexible denture fabricated of non-rigid acrylic resin, and the two-piece sectional denture. Furthermore, acrylic resin removable partial dentures can be supplied with clasps or reinforced by fibers or metal wires.

Effect of chromatographic separation on ASP system interface tension and the countermeasures

Directory of Open Access Journals (Sweden)

Jiawei REN

2016-06-01

Full Text Available Because of the existing chromatographic separation phenomenon, ASP flooding changes original nature of the system. Therefore, in laboratory ultra-low interfacial tension ASP system is preferred for sand packs flow experiment to research on the effect of chromatographic separation on ASP system interface tension. The two parameters of "breakthrough time" and "output difference" are used to describe the degree of chromatographic separation, and the produced fluid interfacial tensions at the outlet end at 120 min is measured. The research shows that there exists chromatographic separation between three chemicals of ASP system, with first polymer breakthrough and finally surfactant breakthrough; there is most serious chromatographic separation between surfactant and polymer, while minimum chromatographic separation between alkali and polymer; chromatographic separation makes ASP interfacial tension increase from 10^-3 magnitude to 10^-2 magnitude, affecting flooding effect of ASP system. Thus, reducing the loss of surfactant in the formation will be the main measure to reduce the degree of chromatographic separation. Using sophorolipid as sacrificial agent to replace part of the surfactant injected into formation before ASP system can effectively reduce the impact of chromatography separation and more effectively improve the ultimate recovery ratio.

Determination of antioxidant activity of milk - vegetable extracts byliquid chromatography

Directory of Open Access Journals (Sweden)

E. S. Rudnichenko

2012-01-01

Full Text Available Antioxidant activity of milk-plant extract of natural sweetener yakon has been established. To extract yakon solid tubers for the first time as an extractant used ultrafiltrate of cheese whey - a product of the extraction separation of whey. Antioxidant activity of extracts was measured amperometrically yakon on the liquid chromatograph "Colour-Yauza-01-AA."A technique for measuring the content of antioxidant. The equations for calculating antioxidant activityyakon. The total content of natural antioxidants can be recommended extract yakon to create new foods with high antioxidant activity.

Properties of the Carboxylate ion exchange resins

International Nuclear Information System (INIS)

Allard, Bert; Dario, Maarten; Boren, Hans; Torstenfelt, Boerje; Puigdomenech, Ignasi; Johansson, Claes

2002-09-01

Weakly acidic, carboxylic resin has been selected, together with strong base anion resins, for water purification at the Forsmark 1 and 2 reactors. For the strong (but not the weak) ion exchange resin the Nuclear Power Inspectorate has given permission to dispose the spent resins in the SFR 1 (the Final Repository for Radioactive Operational Waste). This report gives a review of the carboxylic resins and comes to the conclusion that the resins are very stable and that there should not exist any risks for increased leaching of radionuclides from SFR 1 if these resins are disposed (compared to the strong resins)

Evaluation of the antimicrobial activity of crude extracts and ...

African Journals Online (AJOL)

aghomotsegin

2015-03-25

Mar 25, 2015 ... (6.25, 12.5 25, 50 and 100 mg/ ml) against S. aureus PHM 002 strain from the skin. ... Key words: Adenanthera pavonina, antimicrobial activity, chromatographic fractions, methanolic extract. ..... Glossary of Indian medicinal.

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

Science.gov (United States)

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

1986-07-01

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

Bond strength of resin-resin interfaces contaminated with saliva and submitted to different surface treatments

Directory of Open Access Journals (Sweden)

Adilson Yoshio Furuse

2007-12-01

Full Text Available The purpose of this study was to investigate the effect of different surface treatments on shear bond strength of saliva-contaminated resin-resin interfaces. Flat resin surfaces were fabricated. In the control group, no contamination or surface treatment was performed. The resin surfaces of the experimental groups were contaminated with saliva and air-dried, and then submitted to: (G1 rinsing with water and drying; (G2 application of an adhesive system; (G3 rinsing and drying, abrasion with finishing disks, etching and application of adhesive system; (G4 rinsing and drying, etching, application of silane and adhesive system. Resin cylinders were placed over the treated surfaces. The specimens were stored in water or ethanol. Shear bond strength tests were performed and the mode of failure was evaluated. Data were submitted to two-way ANOVA and Dunnett T3 test. Contamination of resin-resin interfaces with saliva significantly reduced shear strength, especially after prolonged storage (p<0.05. Similar values to the original bond strength were obtained after abrasion and application of adhesive (G3 or etching and application of silane and adhesive (G4. If contamination occurs, a surface treatment is required to guarantee an adequate interaction between the resin increments.

Acidic resin-catalysed conversion of fructose into furan derivatives in low boiling point solvents.

Science.gov (United States)

Zhu, Hong; Cao, Quan; Li, Chunhu; Mu, Xindong

2011-09-27

Conversion of fructose into furan derivatives 5-hydroxymethylfurfural (HMF) and 5-methoxymethylfurfural (MMF) is performed in tetrahydrofuran (THF) and methanol-organic solvent systems, catalysed by an acidic resin Amberlyst-15. The melted fructose can be converted into HMF on the surface of the solid resin catalyst in the presence of THF as an extracting phase, which is a good solvent for HMF and other by-products. The solid resin catalyst can be reused eleven times without losing its catalytic ability, with an average HMF yield of approximately 50%. Upon the addition of methanol, the generated HMF can further react with methanol to form MMF, and the total yield of HMF and MMF could be promoted to 65%. GC-MS analysis confirms the formation of a small amount of methyl levulinate in methanolorganic solvent system. Copyright © 2011 Elsevier Ltd. All rights reserved.

Solid-Phase Extraction of Trace Amounts of Uranium(VI in Environmental Water Samples Using an Extractant-Impregnated Resin Followed by Detection with UV-Vis Spectrophotometry

Directory of Open Access Journals (Sweden)

Ahmad Hosseini-Bandegharaei

2013-01-01

Full Text Available A stable extractant-impregnated resin (EIR containing Chrome Azurol B was prepared using Amberlite XAD-2010 as a porous polymeric support. The new EIR was employed for trace separation and preconcentration of U(VI ion followed by spectrophotometric determination with the arsenazo III procedure. CAB/XAD-2010 exhibited excellent selectivity for U(VI ion over coexisting ions. Experimental parameters including pH, contact time, shaking speed, and ionic strength were investigated by batch extraction methods. Maximum sorption of U(VI ions occurred at pH 4.3–6.9. The capacity of EIR was found to be 0.632 mmol·g−1. Equilibrium was reached in 25 min and the loading half-time, t1/2, was less than 6 min. The equilibrium adsorption isotherm of U(VI was fitted with the Langmuir adsorption model. In addition, a column packed with CAB/XAD-2010 was used for column-mode separation and preconcentration of U(VI ion. For the optimization of the dynamic procedure, effects of sample volume, sample and eluent flow rate, eluent concentration, and its volume were investigated. The preconcentration factors for U(VI were found out to be 160. But, for convenience, a preconcentration factor of 150 was utilized for the column-mode preconcentration. The dynamic procedure gave a detection limit of 5.0×10-10 mol·L−1 (0.12 μg·L−1 for U(VI ion. The proposed dynamic method showed good performance in analyzing environmental water samples.

Evaluation of pesticide adsorption in gas chromatographic injector and column

Directory of Open Access Journals (Sweden)

Gevany Paulino de Pinho

2012-01-01

Full Text Available Components in complex matrices can cause variations in chromatographic response during analysis of pesticides by gas chromatography. These variations are related to the competition between analytes and matrix components for adsorption sites in the chromatographic system. The capacity of the pesticides chlorpyrifos and deltamethrin to be adsorbed in the injector and chromatographic column was evaluated by constructing three isotherms and changing the column heating rate to 10 and 30 ºC min-1. By using ANCOVA to compare the slope of calibration graphs, results showed that the higher the injector temperature (310 ºC the lower the pesticide adsorption. Also, deltamethrin influenced the adsorption of chlorpyrifos on the column chromatographic.

The Effect of Resin-modified Glass-ionomer Cement Base and Bulk-fill Resin Composite on Cuspal Deformation.

Science.gov (United States)

Nguyen, K V; Wong, R H; Palamara, J; Burrow, M F

2016-01-01

This study investigated cuspal deformation in teeth restored with different types of adhesive materials with and without a base. Mesio-occluso-distal slot cavities of moderately large dimension were prepared on extracted maxillary premolars (n=24). Teeth were assigned to one of four groups and restored with either a sonic-activated bulk-fill resin composite (RC) (SonicFill), or a conventional nanohybrid RC (Herculite Ultra). The base materials used were a flowable nanofilled RC (Premise Flowable) and a high-viscosity resin-modified glass-ionomer cement (RMGIC) (Riva Light-Cure HV). Cuspal deflection was measured with two direct current differential transformers, each contacting a buccal and palatal cusp. Cuspal movements were recorded during and after restoration placement. Data for the buccal and palatal cusp deflections were combined to give the net cuspal deflection. Data varied widely. All teeth experienced net inward cuspal movement. No statistically significant differences in cuspal deflection were found among the four test groups. The use of a flowable RC or an RMGIC in closed-laminate restorations produced the same degree of cuspal movement as restorations filled with only a conventional nanohybrid or bulk-fill RC.

Comparison of Shear Bond Strength of RMGI and Composite Resin for Orthodontic Bracket Bonding

Science.gov (United States)

Yassaei, Soghra; Davari, Abdolrahim; Goldani Moghadam, Mahjobeh; Kamaei, Ahmad

2014-01-01

Objective: The aim of this study was to compare the shear bond strength (SBS) of resin modified glass ionomer (RMGI) and composite resin for bonding metal and ceramic brackets. Materials and Methods: Eighty-eight human premolars extracted for orthodontic purposes were divided into 4 groups (n=22). In groups 1 and 2, 22 metal and ceramic brackets were bonded using composite resin (Transbond XT), respectively. Twenty-two metal and ceramic brackets in groups 3 and 4, respectively were bonded using RMGI (Fuji Ortho LC, Japan). After photo polymerization, the teeth were stored in water and thermocycled (500 cycles between 5° and 55°). The SBS value of each sample was determined using a Universal Testing Machine. The amount of residual adhesive remaining on each tooth was evaluated under a stereomicroscope. Statistical analyses were done using two-way ANOVA. Results: RMGI bonded brackets had significantly lower SBS value compared to composite resin bonded groups. No statistically significant difference was observed between metal and ceramic brackets bonded with either the RMGI or composite resin. The comparison of the adhesive remnant index (ARI) scores between the groups indicated that the bracket failure mode was significantly different among groups (Porthodontic bonding purposes; however the provided SBS is still within the clinically acceptable range. PMID:25628663

Microwave-assisted extraction of coumarin and related compounds from Melilotus officinalis (L.) Pallas as an alternative to Soxhlet and ultrasound-assisted extraction.

Science.gov (United States)

Martino, Emanuela; Ramaiola, Ilaria; Urbano, Mariangela; Bracco, Francesco; Collina, Simona

2006-09-01

Soxhlet extraction, ultrasound-assisted extraction (USAE) and microwaves-assisted extraction (MAE) in closed system have been investigated to determine the content of coumarin, o-coumaric and melilotic acids in flowering tops of Melilotus officinalis. The extracts were analyzed with an appropriate HPLC procedure. The reproducibility of extraction and of chromatographic analysis was proved. Taking into account the extraction yield, the cost and the time, we studied the effects of extraction variables on the yield of the above-mentioned compounds. Better results were obtained with MAE (50% v/v aqueous ethanol, two heating cycles of 5 min, 50 degrees C). On the basis of the ratio extraction yield/extraction time, we therefore propose MAE as the most efficient method.

In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water

Energy Technology Data Exchange (ETDEWEB)

Varanusupakul, Pakorn [Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Phayathai Road, Patumwan, Bangkok 10330 (Thailand)], E-mail: pakorn.v@chula.ac.th; Vora-adisak, Narongchai; Pulpoka, Bancha [Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Phayathai Road, Patumwan, Bangkok 10330 (Thailand)

2007-08-15

An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 deg. C for 60 min with 20% Na{sub 2}SO{sub 4}. The linear calibration curves were observed for the concentrations ranging from 1 to 300 {mu}g L{sup -1} with the correlation coefficients (R{sup 2}) being greater than 0.99. The method detection limits of most analytes were below 1 {mu}g L{sup -1} except DCAA and MCAA that were 2 and 18 {mu}g L{sup -1}, respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water.

In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water

International Nuclear Information System (INIS)

Varanusupakul, Pakorn; Vora-adisak, Narongchai; Pulpoka, Bancha

2007-01-01

An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 deg. C for 60 min with 20% Na 2 SO 4 . The linear calibration curves were observed for the concentrations ranging from 1 to 300 μg L -1 with the correlation coefficients (R 2 ) being greater than 0.99. The method detection limits of most analytes were below 1 μg L -1 except DCAA and MCAA that were 2 and 18 μg L -1 , respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water

Analysis of {sup 210}Pb in water samples with plastic scintillation resins

Energy Technology Data Exchange (ETDEWEB)

Lluch, E.; Barrera, J. [Department of Analytical Chemistry, University of Barcelona, Martí i Franqués, 1-11, E-08028, Barcelona (Spain); Tarancón, A., E-mail: alex.tarancon@ub.edu [Department of Analytical Chemistry, University of Barcelona, Martí i Franqués, 1-11, E-08028, Barcelona (Spain); Bagán, H. [Department of Pure and Applied Biochemistry, Lund University, Getingevägen 60, Hus II, 22100 SE, Lund (Sweden); García, J.F. [Department of Analytical Chemistry, University of Barcelona, Martí i Franqués, 1-11, E-08028, Barcelona (Spain)

2016-10-12

{sup 210}Pb is a radioactive lead isotope present in the environment as member of the {sup 238}U decay chain. Since it is a relatively long-lived radionuclide (T{sub 1/2} = 22.2 years), its analysis is of interest in radiation protection and the geochronology of sediments and artwork. Here, we present a method for analysing {sup 210}Pb using plastic scintillation resins (PSresins) packaged in solid-phase extraction columns (SPE cartridge). The advantages of this method are its selectivity, the low limit of detection, as well as reductions in the amount of time and reagents required for analysis and the quantity of waste generated. The PSresins used in this study were composed of a selective extractant (4′,4″(5″)-Di-tert-butyldicyclohexano-18-crown-6 in 1-octanol) covering the surface of plastic scintillation microspheres. Once the amount of extractant (1:1/4) and medium of separation (2 M HNO{sub 3}) were optimised, PSresins in SPE cartridges were calibrated with a standard solution of {sup 210}Pb. {sup 210}Pb could be fully separated from its daughters, {sup 210}Bi and {sup 210}Po, with a recovery value of 91(3)% and detection efficiency of 44(3)%. Three spiked water samples (one underground and two river water samples) were analysed in triplicates with deviations lower than 10%, demonstrating the validity of the PS resin method for {sup 210}Pb analysis. - Highlights: • A plastic scintillation resin for selective analysis of {sup 210}Pb has been developed. • A commercial SPE cartridge has been use for separation and scintillation counting. • {sup 210}Pb separation from {sup 210}Bi and {sup 210}Po is achieved with a 91(3)% of recovery. • The method is valid for analysis of {sup 210}Pb in river water samples.

Multivariate analysis of chromatographic retention data as a supplementary means for grouping structurally related compounds.

Science.gov (United States)

Fasoula, S; Zisi, Ch; Sampsonidis, I; Virgiliou, Ch; Theodoridis, G; Gika, H; Nikitas, P; Pappa-Louisi, A

2015-03-27

In the present study a series of 45 metabolite standards belonging to four chemically similar metabolite classes (sugars, amino acids, nucleosides and nucleobases, and amines) was subjected to LC analysis on three HILIC columns under 21 different gradient conditions with the aim to explore whether the retention properties of these analytes are determined from the chemical group they belong. Two multivariate techniques, principal component analysis (PCA) and discriminant analysis (DA), were used for statistical evaluation of the chromatographic data and extraction similarities between chemically related compounds. The total variance explained by the first two principal components of PCA was found to be about 98%, whereas both statistical analyses indicated that all analytes are successfully grouped in four clusters of chemical structure based on the retention obtained in four or at least three chromatographic runs, which, however should be performed on two different HILIC columns. Moreover, leave-one-out cross-validation of the above retention data set showed that the chemical group in which an analyte belongs can be 95.6% correctly predicted when the analyte is subjected to LC analysis under the same four or three experimental conditions as the all set of analytes was run beforehand. That, in turn, may assist with disambiguation of analyte identification in complex biological extracts. Copyright © 2015 Elsevier B.V. All rights reserved.

Factorial experimental design for recovering heavy metals from sludge with ion-exchange resin

International Nuclear Information System (INIS)

Lee, I.H.; Kuan, Y.-C.; Chern, J.-M.

2006-01-01

Wastewaters containing heavy metals are usually treated by chemical precipitation method in Taiwan. This method can remove heavy metals form wastewaters efficiently, but the resultant heavy metal sludge is classified as hazardous solid waste and becomes another environmental problem. If we can remove heavy metals from sludge, it becomes non-hazardous waste and the treatment cost can be greatly reduced. This study aims at using ion-exchange resin to remove heavy metals such as copper, zinc, cadmium, and chromium from sludge generated by a PCB manufacturing plant. Factorial experimental design methodology was used to study the heavy metal removal efficiency. The total metal concentrations in the sludge, resin, and solution phases were measured respectively after 30 min reaction with varying leaching agents (citric acid and nitric acid); ion-exchange resins (Amberlite IRC-718 and IR-120), and temperatures (50 and 70 deg. C). The experimental results and statistical analysis show that a stronger leaching acid and a higher temperature both favor lower heavy metal residues in the sludge. Two-factors and even three-factor interaction effects on the heavy metal sorption in the resin phase are not negligible. The ion-exchange resin plays an important role in the sludge extraction or metal recovery. Empirical regression models were also obtained and used to predict the heavy metal profiles with satisfactory results

Cytotoxicity and antiangiogenic effects of Rhus coriaria, Pistacia vera and Pistacia khinjuk oleoresin methanol extracts.

Science.gov (United States)

Mirian, M; Behrooeian, M; Ghanadian, M; Dana, N; Sadeghi-Aliabadi, H

2015-01-01

Angiogenesis, formation of new blood vessels, play an important role in some diseases such as cancer and its metastasis. Using angiogenesis inhibitors, therefore, is one of the ways for cancer treatment and prevention of metastasis. Medicinal plants have been shown to play a major role in the treatment of a variety of cancers. In this direction, cytotoxic and angiogenic effects of oleo gum resin extracts of Rhus coriaria, Pistacia vera and Pistacia khinjuk from Anacardiaceae family were studied. For IC50 values, cytotoxic effects of the plant extracts were evaluated at different concentrations (1, 10, 20, 40, 80,100 μg/ml) against human umbilical vein endothelial normal cell (HUVEC) and Y79 cell lines using 3-(4, 5-dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide (MTT) assay. In vitro tube formation on matrigel base was used to evaluate angiogenic effects in the presence of increasing concentrations (50, 100, 250 μg/ml) of the extracts. Vascular endothelium growth factor was used as angiogenesis stimulator. Gas chromatography results showed that α-pinene and β-pinene were the major essential oils constituents of all plant extracts. According to the MTT assay results, the R. coriaria resin extract was more cytotoxic than those of P. vera and P. khinjuk extracts (IC50, 9.1 ± 1.6 vs 9.8 ± 2.1 and 12.0 ± 1.9, respectively; P<0.05). Cytotoxic effects of all extracts against Y79 cell line was significantly higher than those of HUVEC used as a normal cell line (P<0.05). Tube formation assay also showed that extract of R. coriaria resin inhibited angiogenesis more significantly than other tested extracts (P<0.05). It could be concluded that R. coriaria resin extract possess cytotoxic effect and antiangiogenesis against cancer cells and as an anticancer natural product has a good potential for future studies.

Aqueous CO2 vs. aqueous extraction of soils as a preparative procedure for acute toxicity testing

International Nuclear Information System (INIS)

Yates, G.W.; Burks, S.L.

1994-01-01

This study was to determine if contaminated soils extracted with supercritical CO 2 (SFE) would yield different results from soils extracted with an aqueous media. Soil samples from an abandoned oil refinery were subjected to aqueous and SFE extraction. Uncontaminated control sites were compared with contaminated sites. Each extract was analyzed for 48 hour acute Ceriodaphnia LC50s and Microtox reg-sign EC50s. Comparisons were then made between the aqueous extracts and the SFE extracts. An additional study was made with HPLC chromatographs of the SFE contaminated site extracts to determine if there was a correlation between LC50 results and peak area of different sections of the chromatograph. The 48 hour Ceriodaphnia LC50 of one contaminated site showed a significant increase in toxicity with the supercritical extract compared to the aqueous extract. All contaminated sites gave toxic responses with the supercritical procedure. The Microtox reg-sign assay showed a toxic response with 2 of the 3 contaminated sites for both aqueous and SFE extracts. Results indicate that the Ceriodaphnia assays were more sensitive than Microtox reg-sign to contaminants found in the refinery soil. SFE controls did not show adverse effects with the Ceriodaphnia, but did have a slight effect with Microtox reg-sign. The best correlation (r 2 > 0.90) between the Ceriodaphnia LC50s and the peak areas of the chromatographs was obtained for sections with an estimated log K ow of 1 to 5. SFE extraction provided a fast, efficient and inexpensive method of collecting and testing moderately non-polar to strongly non-polar organic contaminants from contaminated soils

A comparative evaluation of the staining capacity of microhybrid and nanohybrid resin-based composite to indian spices and food colorants: An In vitro study.

Science.gov (United States)

Usha, Carounanidy; Rao, Sathyanarayanan Rama; George, Geena Mary

2018-01-01

Resin composite restorative materials can mimic the natural color and shade of the tooth. However, exogenous colorants from food and drinks can stain them due to adsorption. The influence of Indian food colorants and spices on resin composite restorations has not been evaluated extensively. This study aims to evaluate the staining capacity of microhybrid and nanohybrid resin-based composites, to saffron extract, tandoori powder, and turmeric powder. Forty samples of microhybrid (Kulzer Charisma) and nanohybrid (3M Filtek Z350) resin composites were prepared using an acrylic template of dimension 5 mm × 3 mm. They were randomly divided into four groups and immersed into solutions of saffron extract, tandoori powder, and turmeric powder. Distilled water was used as the control group. Color values (LFNx01, aFNx01, bFNx01) were measured by colorimeter using the CIE LFNx01aFNx01bFNx01 system before and after 72 h of immersion. Color differences ΔEFNx01ab were statistically analyzed. Two-way ANOVA and post-hoc Tukey (honest significant difference) test were done using IBM SPSS Statistics for Windows, Version 19.0. Armonk, NY: IBM Corp. : All the immersion media changed the color of the resin composites to varying degrees. However, turmeric solution showed the maximum mean color variation ΔEFNx01ab of 14.8 ± 2.57 in microhybrid resin composites and 16.8 ± 3.50 in nanohybrid resin composites. Microhybrid and nanohybrid resin composites tend to stain to Indian food colorants, especially to turmeric powder.

Rheological analysis of the phenolic and furfuryl resins used in the carbon materials processing

Directory of Open Access Journals (Sweden)

Edson Cocchieri Botelho

2000-04-01

Full Text Available Carbon materials processing is an advanced technology due to its aerospace and medical applications. In the aerospace area one can mention the carbon/carbon composites used in rockets and aeronautical brakes; in the medical area one can mention the intrabody implant tools such as heart and hydrocephalic valves and pacemaker electrode tips. The highly sophisticated purpose of its application requires a very tight processing control, which defines the microstructure the mechanical, thermal and electrical characteristics of the final material. The objective of this study is to correlate rheological, chromatographic and thermal analysis of phenolic and furfuryl resins, aiming their use as raw materials in carbon/carbon composite and glassy carbon processing. The obtained results are correlated and used directly in the establishment of the adequate parameters for carbon reinforcement impregnation and to prepare glassy carbon samples with controlled porosity.

4-META opaque resin--a new resin strongly adhesive to nickel-chromium alloy.

Science.gov (United States)

Tanaka, T; Nagata, K; Takeyama, M; Atsuta, M; Nakabayashi, N; Masuhara, E

1981-09-01

1) A new adhesive opaque resin containing a reactive monomer, 4-methacryloxy-ethyl trimellitate anhydride (4-META), was prepared, and its application to thermosetting acrylic resin veneer crowns was studied. 2) The 4-META opaque resin was applied to a variety of nickel-chromium dental alloy specimens which had undergone different treatment, and endurance tests were conducted to evaluate the durability of adhesion. 3) Stable adhesion against water penetration was achieved with metal surfaces first etched with HCl and then oxidized with HNO3. A bond strength of 250 kg/cm2 was maintained even after immersion in water at 37 degrees C for 30 wk or at 80 degrees C for ten wk. Furthermore, this value did not decrease even after the specimens were subjected to 500 thermal cycles. 4) The 4-META opaque resin studied can eliminate the necessity for retention devices on metal castings. 5) The smooth 4-META opaque resin should have no adverse effects on gingivae.

Method of solidifying radioactive ion exchange resin

International Nuclear Information System (INIS)

Minami, Yuji; Tomita, Toshihide

1989-01-01

Spent anion exchange resin formed in nuclear power plants, etc. generally catch only a portion of anions in view of the ion exchange resins capacity and most of the anions are sent while possessing activities to radioactive waste processing systems. Then, the anion exchange resins increase the specific gravity by the capture of the anions. Accordingly, anions are caused to be captured on the anion exchange resin wastes such that the specific gravity of the anion exchange resin wastes is greater than that of the thermosetting resins to be mixed. This enables satisfactory mixing with the thermosetting resins and, in addition, enables to form integral solidification products in which anion exchange resins and cation exchange resins are not locallized separately and which are homogenous and free from cracks. (T.M.)

Chromatographic and anti-motility studies on extracts of Loranthus ...

African Journals Online (AJOL)

The anti-motility properties of the leaves of African mistletoe, Loranthus micranthus (Linn), Loranthaceae harvested from Kola acuminate host tree was studied by the charcoal meal test in mice. The intraperitoneal LD50 of the methanol extract was determined in mice by the Locke's method. The phytochemical constituents of ...

Action of ionizing radiation on epoxy resins

Energy Technology Data Exchange (ETDEWEB)

Van de Voorde, M. E.

1970-12-01

The resistance of classical and experimental epoxy resins to irradiation was studied. The resistance to irradiation of epoxy resins of diverse compositions as well as the development of resins having a radioresistance that approaches that of certain ceramics are discussed. Sources of irradiation and the techniques of dosimetry used are described. The structures of certain epoxy resins and of hardeners are given. The preparation of these resins and their physical properties is described. The effects of radiation on epoxy resins, as well as conditions of irradiation, and suggested mechanisms for degradation of the irradiated resins are discussed. The relationship between chemical structure of the resins and their physical properties is evaluated. (115 references) (JCB)

Epoxidation of linseed oil-Alkyd resins

International Nuclear Information System (INIS)

Motawie, A.M.; Ismail, E.A.; Mazroua, A.M.; Abd EI Aziem, M.S.; Ramadan, A.M.

2004-01-01

Three types of different linseed oil-alkyd resin ( Alk (I), Alk (II), and Alk (III) ) were prepared with the calculated amounts of mono glycerides and adipic acid (1:1, 1:2, and 2:1 Eq.Wt) respectively via monoglyceride method. The obtained alkyd resins were epoxidized via reaction with the calculated quantities of peracetic acid, which was prepared by the reaction of acetic anhydride with H 2 O 2 . Epoxidation occurred with the ratio (1: 1, 1 :3, and 1:6 Eq. Wt) of alkyd to peracetic acid. The effect of reaction time on the epoxy group content was measured during the epoxidation process. The prepared alkyd resins were analyzed by IR and H 1 NMR. The metal coated film properties of epoxidized alkyd resins were compared with those of unmodified alkyd resins. It was observed that the coating films of epoxidized alkyd resins have better in drying properties, hardness, adhesion, impact and flexibility than those of un epoxidized alkyd resins. The flammability properties of the paper coated films for the prepared brominated epoxidized alkyd resins were found to be fire retardant

Gas-Chromatographic Determination Of Water In Freon PCA

Science.gov (United States)

Melton, Donald M.

1994-01-01

Gas-chromatographic apparatus measures small concentrations of water in specimens of Freon PCA. Testing by use of apparatus faster and provides greater protection against accidental contamination of specimens by water in testing environment. Automated for unattended operation. Also used to measure water contents of materials, other than Freon PCA. Innovation extended to development of purgeable sampling accessory for gas chromatographs.

Treatment by absorbers of oil contaminated process waters. Ion exchange resins and filtration

International Nuclear Information System (INIS)

La Gamma, Ana M.; Becquart, Elena T.; Chocron, Mauricio; Ambrosioni, P.M.; Schoenbrod, B.

2003-01-01

Pressurized Heavy Water Reactors have a system devoted to the purification and upgrading of the collected heavy water leaks. The purification train is fed with different degradation ratios (D 2 O/H 2 O) activities and impurities. The water is distilled in a packed bed column filled with a mesh type packing. With the purpose of minimizing the column stack corrosion, the water is pretreated in a train consisting on an activated charcoal bed-strong cationic-anionic resin and a final polishing mixed bed resin. Traces of oils are retained by the charcoal bed but some compounds extracted by the aqueous phase are suspected to be responsible for the resins fouling or precursors of potentially aggressive agents inside the distillation column. In the present work, the identification, evaluation of alternatives for the retention like dead end and cross flow micro filtration, adsorption and ion exchange were tested and the results compared to the original products present in the water upgrading purification train. (author)

Oxygen index tests of thermosetting resins

Science.gov (United States)

Gilwee, W. J., Jr.; Parker, J. A.; Kourtides, D. A.

1980-01-01

The flammability characteristics of nine thermosetting resins under evaluation for use in aircraft interiors are described. These resins were evaluated using the Oxygen Index (ASTM 2863) testing procedure. The test specimens consisted of both neat resin and glass reinforced resin. When testing glass-reinforced samples it was observed that Oxygen Index values varied inversely with resin content. Oxygen values were also obtained on specimens exposed to temperatures up to 300 C. All specimens experienced a decline in Oxygen Index when tested at an elevated temperature.

Study on the pyrolysis of phenol-formaldehyde (PF) resin and modified PF resin

Energy Technology Data Exchange (ETDEWEB)

Wang, Jigang, E-mail: wangjigang@seu.edu.cn [Jiangsu Key Laboratory of Advanced Metallic Materials, School of Materials Science and Engineering, Southeast University, Nanjing 211189 (China); Jiang, Haiyun [Jiangsu Key Laboratory of Advanced Metallic Materials, School of Materials Science and Engineering, Southeast University, Nanjing 211189 (China); School of Materials Science and Engineering, Southeast University, Nanjing Institute of Technology, Nanjing 210013 (China); Jiang, Nan [Institute of Theoretical and Computational Chemistry, Nanjing University, Nanjing 210093 (China)

2009-12-10

The pyrolysis of pure phenol-formaldehyde (PF) resin and boron carbide (B{sub 4}C) modified PF resin was investigated by using thermogravimetry (TG) and pyrolysis gas-chromatography-mass-spectrometry (PY-GC/MS). Scanning electron microscope (SEM) and Fourier transform infrared (FT-IR) spectroscopy were also employed to investigate the micro-structural evolution. It was shown from the TG analysis that the char residues of pure PF resin were 62.9 and 60.5% after being pyrolyzed at 700 and 1000 {sup o}C, respectively. The degradation and failure of the resin matrix were mainly resulted from the release of volatiles. The phenol and its methyl derivates took a large proportion in the amount of volatiles. In comparison with the pure PF resin, the char residues of B{sub 4}C modified PF resin were obviously higher, with the values of 71.9 and 68.4% at 700 and 1000 {sup o}C, respectively. Due to the oxidation-reduction reactions between B{sub 4}C additive and oxygen-containing volatiles including CO and H{sub 2}O, partial carbon and oxygen elements in the volatiles remained in the resin matrix in the forms of amorphous carbon and B{sub 2}O{sub 3}, respectively. The results of SEM and FT-IR characterization demonstrated the occurrence of the modification, and the amorphous carbon existed in the form of reticular substance. In addition, the amount of the released phenol and its methyl derivates was also decreased drastically due to the formation of borate.

Improving Gold Recovery from Artificial Preg-Robbing Ore by Pre-treatment using Blinding Agent and Resin-in-Leach

OpenAIRE

Mohammad Zaki Mubarok; Prasetyo Sandha Irianto

2016-01-01

In the present paper, the effectiveness of the use of blinding agents, ionic exchanger resins and the combination of them in improving gold extraction from simulated preg-robbing ore is discussed. The blinding agents used were kerosene, diesel oil and pine oil, while the ion exchange resins used were Lewatit Monoplus MP 800, Lewatit AF 5 and guanidine. Preg-robbing conditions were simulated by blending fine activated carbon with ore sample. The investigation results show that the presence of ...

Contact allergy to epoxy resin

DEFF Research Database (Denmark)

Bangsgaard, Nannie; Thyssen, Jacob Pontoppidan; Menné, Torkil

2012-01-01

Background. Epoxy resin monomers are strong skin sensitizers that are widely used in industrial sectors. In Denmark, the law stipulates that workers must undergo a course on safe handling of epoxy resins prior to occupational exposure, but the effectiveness of this initiative is largely unknown...... in an educational programme. Conclusion. The 1% prevalence of epoxy resin contact allergy is equivalent to reports from other countries. The high occurrence of epoxy resin exposure at work, and the limited use of protective measures, indicate that reinforcement of the law is required....

Improved recovery of trace amounts of gold (III), palladium (II) and platinum (IV) from large amounts of associated base metals using anion-exchange resins

Energy Technology Data Exchange (ETDEWEB)

Matsubara, I. [Lab. of Chemistry, Tokyo Women' s Medical Univ. (Japan); Takeda, Y.; Ishida, K. [Lab. of Chemistry, Nippon Medical School, Kawasaki-shi, Kanagawa-ken (Japan)

2000-02-01

The adsorption and desorption behaviors of gold (III), palladium (II) and platinum (IV) were surveyed in column chromatographic systems consisting of one of the conventional anion-exchange resins of large ion-exchange capacity and dilute thiourea solutions. The noble metals were strongly adsorbed on the anion-exchange resins from dilute hydrochloric acid, while most base metals did not show any marked adsorbability. These facts made it possible to separate the noble metals from a large quantity of base metals such as Ag (I), Al (III), Co (II), Cu (II), Fe (III), Mn (II), Ni (II), Pb (II), and Zn (II). Although it used to be very difficult to desorb the noble metals from the resins used, the difficulty was easily overcome by use of dilute thiourea solutions as an eluant. In the present study, as little as 1.00 {mu}g of the respective noble metals was quantitatively separated and recovered from as much as ca. 10 mg of a number of metals on a small column by elution with a small amount of dilute thiourea solution. The present systems should be applicable to the separation, concentration and recovery of traces of the noble metals from a number of base metals coexisting in a more extended range of amounts and ratios. (orig.)

A Twofold Comparison between Dual Cure Resin Modified Cement and Glass Ionomer Cement for Orthodontic Band Cementation.

Science.gov (United States)

Attar, Hanaa El; Elhiny, Omnia; Salem, Ghada; Abdelrahman, Ahmed; Attia, Mazen

2016-12-15

To test the solubility of dual cure resin modified resin cement in a food simulating solution and the shear bond strength compared to conventional Glass ionomer cement. The materials tested were self-adhesive dual cure resin modified cement and Glass Ionomer (GIC). Twenty Teflon moulds were divided into two groups of tens. The first group was injected and packed with the modified resin cement, the second group was packed with GIC. To test the solubility, each mould was weighed before and after being placed in an analytical reagent for 30 days. The solubility was measured as the difference between the initial and final drying mass. To measure the Shear bond strength, 20 freshly extracted wisdom teeth were equally divided into two groups and embedded in self-cure acrylic resin. Four mm sections of stainless steel bands were cemented to the exposed buccal surfaces of teeth under a constant load of 500 g. Shear bond strength was measured using a computer controlled materials testing machine and the load required to deband the samples was recorded in Newtons. GIC showed significantly higher mean weight loss and an insignificant lower Shear bond strength, compared to dual cure resin Cement. It was found that dual cure resin modified cement was less soluble than glass ionomer cement and of comparable bond strength rendering it more useful clinically for orthodontic band cementation.

Extractive scintillating polymer sensors for trace-level detection of uranium in contaminated ground water

International Nuclear Information System (INIS)

Duval, Christine E.; DeVol, Timothy A.; Husson, Scott M.

2016-01-01

This contribution describes the synthesis of robust extractive scintillating resin and its use in a flow-cell detector for the direct detection of uranium in environmental waters. The base poly[(4-methyl styrene)-co-(4-vinylbenzyl chloride)-co-(divinylbenzene)-co-(2-(1-napthyl)-4-vinyl-5-phenyloxazole)] resin contains covalently bound fluorophores. Uranium-binding functionality was added to the resin by an Arbuzov reaction followed by hydrolysis via strong acid or trimethylsilyl bromide (TMSBr)-mediated methanolysis. The resin was characterized by Fourier-transform infrared spectroscopy and spectrofluorometry. Fluorophore degradation was observed in the resin hydrolyzed by strong acid, while the resin hydrolyzed by TMSBr-mediated methanolysis maintained luminosity and showed hydrogen bonding-induced Stokes' shift of ∼100 nm. The flow cell detection efficiency for uranium of the TMSBr-mediated methanolysis resin was evaluated at pH 4, 5 and 6 in DI water containing 500 Bq L"−"1 uranium-233 and demonstrated flow cell detection efficiencies of 23%, 16% and 7%. Experiments with pH 4, synthetic groundwater with 50 Bq L"−"1 uranium-233 exhibited a flow cell detection efficiency of 17%. The groundwater measurements show that the resins can concentrate the uranyl cation from waters with high concentrations of competitor ions at near-neutral pH. Findings from this research will lay the groundwork for development of materials for real-time environmental sensing of alpha- and beta-emitting radionuclides. - Highlights: • Extractive scintillating resins synthesized with covalently bound fluor and ligand. • Methylphosphonic acid-derivitized resins characterized for optical properties. • Online detection of uranium in ground water demonstrated at near-neutral pH.

Extractive scintillating polymer sensors for trace-level detection of uranium in contaminated ground water

Energy Technology Data Exchange (ETDEWEB)

Duval, Christine E. [Department of Chemical and Biomolecular Engineering, Clemson University, 127 Earle Hall, Clemson, SC 29634 (United States); DeVol, Timothy A. [Department of Environmental Engineering and Earth Sciences, Clemson University, 342 Computer Court, Anderson, SC 29625 (United States); Husson, Scott M., E-mail: shusson@clemson.edu [Department of Chemical and Biomolecular Engineering, Clemson University, 127 Earle Hall, Clemson, SC 29634 (United States)

2016-12-01

This contribution describes the synthesis of robust extractive scintillating resin and its use in a flow-cell detector for the direct detection of uranium in environmental waters. The base poly[(4-methyl styrene)-co-(4-vinylbenzyl chloride)-co-(divinylbenzene)-co-(2-(1-napthyl)-4-vinyl-5-phenyloxazole)] resin contains covalently bound fluorophores. Uranium-binding functionality was added to the resin by an Arbuzov reaction followed by hydrolysis via strong acid or trimethylsilyl bromide (TMSBr)-mediated methanolysis. The resin was characterized by Fourier-transform infrared spectroscopy and spectrofluorometry. Fluorophore degradation was observed in the resin hydrolyzed by strong acid, while the resin hydrolyzed by TMSBr-mediated methanolysis maintained luminosity and showed hydrogen bonding-induced Stokes' shift of ∼100 nm. The flow cell detection efficiency for uranium of the TMSBr-mediated methanolysis resin was evaluated at pH 4, 5 and 6 in DI water containing 500 Bq L{sup −1} uranium-233 and demonstrated flow cell detection efficiencies of 23%, 16% and 7%. Experiments with pH 4, synthetic groundwater with 50 Bq L{sup −1} uranium-233 exhibited a flow cell detection efficiency of 17%. The groundwater measurements show that the resins can concentrate the uranyl cation from waters with high concentrations of competitor ions at near-neutral pH. Findings from this research will lay the groundwork for development of materials for real-time environmental sensing of alpha- and beta-emitting radionuclides. - Highlights: • Extractive scintillating resins synthesized with covalently bound fluor and ligand. • Methylphosphonic acid-derivitized resins characterized for optical properties. • Online detection of uranium in ground water demonstrated at near-neutral pH.

Input to Resin Column Structural Analysis if Autocatalytic Resin Reaction Occurs in HB-Line Phase II

Energy Technology Data Exchange (ETDEWEB)

Hallman, D.F.

2001-07-10

Solutions of plutonium in nitric acid are purified and concentrated using anion resin prior to precipitation. There have been instances of resin column explosions caused by autocatalytic reactions of anion resins in nitric acid within the DOE complex

Thermosetting behavior of pitch-resin from heavy residue

Energy Technology Data Exchange (ETDEWEB)

Qingfang, Z.; Yansheng, G.; Baohua, H.; Yuzhen, Z. [China Univ. of Petroleum, Dongying, Shandong (China). State Key LAboratory of Heavy Oil Processing, Heavy Oil Research Inst.

2006-07-01

Thermosetting resins are widely employed as a basic matrix for c/c composites in carbon materials production. A new type of synthesized thermosetting resin is called pitch resin. Pitch resin is a cheaper resin and possesses a potential opportunity for future use. However, the thermosetting behavior of pitch resin is not very clear. The hardening process and conditions for thermosetting are very important for future use of pitch resin. B-stage pitch resin is a soluble and meltable inter-media condensed polymer, which is not fully reacted and is of a low molecular weight. The insoluble and unmelted pitch resin can only be obtained from synthesized B-stage resin after a hardening stage. This paper presented an experiment that synthesized B-stage pitch resin with a link agent (PXG) under catalyst action from fluid catalytic cracking (FCC) of the slurry's aromatic enriched component (FCCDF). The paper discussed the experiment, including the synthesis of pitch resin and thermosetting of pitch resin. Two kinds of thermosetting procedures were used in the study called one-step thermosetting and two-step thermosetting. It was concluded that the B-stage pitch resin could be hardened after a thermosetting procedure by heat treatment. The thermosetting pitch resin from 2-step thermosetting possesses was found to have better thermal resistant properties than that of the 1-step thermosetting pitch resin. 13 refs., 2 tabs., 6 figs.

Core-shell in liquid chromatography: application for determining sulphonamides in feed and meat using conventional chromatographic systems

Directory of Open Access Journals (Sweden)

Antonio Armentano

2016-12-01

Full Text Available A C18 column packed with core-shell particles was used for the chromatographic separation of sulphonamides in feed and meat by a conventional high performance liquid chromatography system coupled with a diode array detector. Two analytical methods, already used in our laboratory, have been modified without any changes in the extraction and clean-up steps and in the liquid chromatography instrumentation. Chromatographic conditions applied on a traditional 5-μm column have been optimized on a column packed with 2.6 μm core-shell particles. A binary mobile phase [acetate buffer solution at pH 4.50 and a mixture of methanol acetonitrile 50: 50 (v/v] was employed in gradient mode at the flow rate of 1.2 mL with an injection volume of 6 μL. These chromatographic conditions allow the separation of 13 sulphonamides with an entire run of 13 minutes. Preliminary studies have been carried out comparing blanks and spiked samples of feed and meat. A good resolution and the absence of interferences were achieved in chromatograms for both matrices. Since no change was made to the sample preparation, the optimized method does not require a complete revalidation and can be used to make routine analysis faster.

Gas chromatographic determination of yohimbine in commercial yohimbe products.

Science.gov (United States)

Betz, J M; White, K D; der Marderosian, A H

1995-01-01

The bark of Pausinystalia yohimbe [K. Schumann] Pierre (Rubiaceae), long valued as an aphrodisiac in West Africa, recently has been promoted in the United States as a dietary supplement alternative to anabolic steroids for enhancement of athletic performance. As the number of yohimbe products on the retail market increases, concerns about their safety are raised because of the reported toxicity of yohimbine (the major alkaloid of the plant). Although plant materials are usually identified microscopically, we were unable to identify them in many of the products, because as their labels indicated, the products were mixtures of various botanicals or were bark extracts and contained little or no plant material. A method for extraction and capillary gas chromatographic (GC) separation of the alkaloids of P. yohimbe was, therefore, developed and used to analyze a number of commercial yohimbe products. The method involved solvent extraction and partitioning in chloroform-water followed by separation on a methyl silicone capillary GC column (N-P detection). Comparisons of chromatograms of extracts of authentic bark with those of commercial products indicated that, although many products contained measurable quantities of the alkaloid yohimbine, they were largely devoid of the other alkaloids previously reported in this species. Concentrations of yohimbine in the commercial products ranged from < 0.1 to 489 ppm, compared with 7089 ppm in the authentic material. Authentic bark has been reported to contain up to 6% total alkaloids, 10-15% of which are yohimbine. The possible presence of undeclared diluents in the products was indicated by peaks in product chromatograms but not in those of authentic bark.

Chemometric approach for development, optimization, and validation of different chromatographic methods for separation of opium alkaloids.

Science.gov (United States)

Acevska, J; Stefkov, G; Petkovska, R; Kulevanova, S; Dimitrovska, A

2012-05-01

The excessive and continuously growing interest in the simultaneous determination of poppy alkaloids imposes the development and optimization of convenient high-throughput methods for the assessment of the qualitative and quantitative profile of alkaloids in poppy straw. Systematic optimization of two chromatographic methods (gas chromatography (GC)/flame ionization detector (FID)/mass spectrometry (MS) and reversed-phase (RP)-high-performance liquid chromatography (HPLC)/diode array detector (DAD)) for the separation of alkaloids from Papaver somniferum L. (Papaveraceae) was carried out. The effects of various conditions on the predefined chromatographic descriptors were investigated using chemometrics. A full factorial linear design of experiments for determining the relationship between chromatographic conditions and the retention behavior of the analytes was used. Central composite circumscribed design was utilized for the final method optimization. By conducting the optimization of the methods in very rational manner, a great deal of excessive and unproductive laboratory research work was avoided. The developed chromatographic methods were validated and compared in line with the resolving power, sensitivity, accuracy, speed, cost, ecological aspects, and compatibility with the poppy straw extraction procedure. The separation of the opium alkaloids using the GC/FID/MS method was achieved within 10 min, avoiding any derivatization step. This method has a stronger resolving power, shorter analysis time, better cost/effectiveness factor than the RP-HPLC/DAD method and is in line with the "green trend" of the analysis. The RP-HPLC/DAD method on the other hand displayed better sensitivity for all tested alkaloids. The proposed methods provide both fast screening and an accurate content assessment of the six alkaloids in the poppy samples obtained from the selection program of Papaver strains.

Determination of U and Th α-emitters in NORM samples through extraction chromatography by using new and recycled UTEVA resins

International Nuclear Information System (INIS)

Casacuberta, N.; Lehritani, M.; Mantero, J.; Masqué, P.; Garcia-Orellana, J.; Garcia-Tenorio, R.

2012-01-01

This manuscript describes a protocol for the determination of U and Th isotopes via alpha spectrometry in NORM samples containing high concentrations of these radionuclides, up to kBq kg −1 . This technique is based on extraction chromatography with UTEVA (Triskem Int.) resins and it has been tested using both NORM samples from a phosphate industry and reference materials. The results proved that this method is highly optimized in terms of accuracy and precision when dealing with NORM samples. Recycling of UTEVA columns was also checked using NORM samples and successful results were obtained for both U and Th isotopes, thus proving the feasibility of re-using these type of columns. - Highlights: ► U and Th isotopes in NORM samples are determined via alpha spectrometry. ► The results show a highly optimized data in terms of accuracy and precision. ► Recycling of UTEVA columns was also checked and successful results were obtained.

Ponderosa pine resin defenses and growth: metrics matter.

Science.gov (United States)

Hood, Sharon; Sala, Anna

2015-11-01

Bark beetles (Coleoptera: Curculionidae, Scolytinae) cause widespread tree mortality in coniferous forests worldwide. Constitutive and induced host defenses are important factors in an individual tree's ability to survive an attack and in bottom-up regulation of bark beetle population dynamics, yet quantifying defense levels is often difficult. For example, in Pinus spp., resin flow is important for resistance to bark beetles but is extremely variable among individuals and within a season. While resin is produced and stored in resin ducts, the specific resin duct metrics that best correlate with resin flow remain unclear. The ability and timing of some pine species to produce induced resin is also not well understood. We investigated (i) the relationships between ponderosa pine (Pinus ponderosa Lawson & C. Lawson) resin flow and axial resin duct characteristics, tree growth and physiological variables, and (ii) if mechanical wounding induces ponderosa pine resin flow and resin ducts in the absence of bark beetles. Resin flow increased later in the growing season under moderate water stress and was highest in faster growing trees. The best predictors of resin flow were nonstandardized measures of resin ducts, resin duct size and total resin duct area, both of which increased with tree growth. However, while faster growing trees tended to produce more resin, models of resin flow using only tree growth were not statistically significant. Further, the standardized measures of resin ducts, density and duct area relative to xylem area, decreased with tree growth rate, indicating that slower growing trees invested more in resin duct defenses per unit area of radial growth, despite a tendency to produce less resin overall. We also found that mechanical wounding induced ponderosa pine defenses, but this response was slow. Resin flow increased after 28 days, and resin duct production did not increase until the following year. These slow induced responses may allow

General and selective isolation procedure for high-performance liquid chromatographic determination of anabolic steroids in tissues.

Science.gov (United States)

Laganà, A; Marino, A

1991-12-27

A multi-residue method has been developed for the determination of anabolic steroids in animal tissue. The analytes are extracted from tissue with methanol and the extract is subjected to two solid-phase extractions, one using a non-specific adsorbing material, such as graphitized carbon black (Carbopack B), and the other Amberlite CG-400 I in the OH form. This procedure allowed the neutral anabolics (testosterone, trenbolone and progesterone) to be isolated and separated from the acidic type (phenolic group), such as diethylstilbestrol, oestradiol, zeranol/zearalenone and their respective metabolites. The determination was effected using high-performance liquid chromatography with different detectors (ultraviolet, fluorimetric and electrochemical). Several analytical parameters were studied: chromatographic conditions, recoveries, evaporation step, solvent flow-rate, cartridges reusability, interference of plastic cartridges. For all the anabolics investigated the recoveries were greater than 83.6%.

A simple and reliable anion-exchange resin method for sulfate extraction and purification suitable for multiple O- and S-isotope measurements.

Science.gov (United States)

Le Gendre, Erwann; Martin, Erwan; Villemant, Benoit; Cartigny, Pierre; Assayag, Nelly

2017-01-15

The O- and S-isotope compositions of sulfates can be used as key tracers of the fate and sink of sulfate in both terrestrial and extra-terrestrial environments. However, their application remains limited in those geological systems where sulfate occurs in low concentrations. Here we present a simple and reliable method to extract, purify and concentrate sulfate from natural samples. The method allows us to take into account the separation of nitrate, which is known to be an issue in O-isotope analysis. The separation and concentration of sulfate from other anions in any aqueous solution are performed within a few hours via anion-exchange resin. The possible O- (δ 18 O and Δ 17 O) and S- (δ 34 S, Δ 33 S and Δ 36 S) isotope exchanges, fractionations and/or contaminations are for the first time monitored during the whole procedure using initial O- and S-mass-dependent and mass-independent sulfate solutions. After elution in HCl, pure sulfate is fully retrieved and precipitated into BaSO 4 , which is suitable for O- and S-isotopic measurements using established techniques. The analysis of retrieved barite presents no variation within 2σ uncertainties: ±0.5‰ and ±0.1‰ in O- (δ 18 O, Δ 17 O) and ±0.2‰, ±0.02‰ and ±0.09‰ in S- (δ 34 S, Δ 33 S and Δ 36 S) isotope ratios, respectively. This study shows that the resin method for sulfate extraction and purification, in addition to being cheap, simple and quick, is applicable for the measurements of all O- and S-isotopic ratios in sulfates (including the Δ 17 O, Δ 33 S and Δ 36 S values). Therefore, this method can be easily used for a high range of natural samples in which sulfate occurs in low concentration including aerosols, ice cores, sediments, volcanic deposits, (paleo)soils and rainwater, and thus it can be a key to our understanding of the sulfur cycle on Earth. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Biphenyl liquid crystalline epoxy resin as a low-shrinkage resin-based dental restorative nanocomposite.

Science.gov (United States)

Hsu, Sheng-Hao; Chen, Rung-Shu; Chang, Yuan-Ling; Chen, Min-Huey; Cheng, Kuo-Chung; Su, Wei-Fang

2012-11-01

Low-shrinkage resin-based photocurable liquid crystalline epoxy nanocomposite has been investigated with regard to its application as a dental restoration material. The nanocomposite consists of an organic matrix and an inorganic reinforcing filler. The organic matrix is made of liquid crystalline biphenyl epoxy resin (BP), an epoxy resin consisting of cyclohexylmethyl-3,4-epoxycyclohexanecarboxylate (ECH), the photoinitiator 4-octylphenyl phenyliodonium hexafluoroantimonate and the photosensitizer champhorquinone. The inorganic filler is silica nanoparticles (∼70-100 nm). The nanoparticles were modified by an epoxy silane of γ-glycidoxypropyltrimethoxysilane to be compatible with the organic matrix and to chemically bond with the organic matrix after photo curing. By incorporating the BP liquid crystalline (LC) epoxy resin into conventional ECH epoxy resin, the nanocomposite has improved hardness, flexural modulus, water absorption and coefficient of thermal expansion. Although the incorporation of silica filler may dilute the reinforcing effect of crystalline BP, a high silica filler content (∼42 vol.%) was found to increase the physical and chemical properties of the nanocomposite due to the formation of unique microstructures. The microstructure of nanoparticle embedded layers was observed in the nanocomposite using scanning and transmission electron microscopy. This unique microstructure indicates that the crystalline BP and nanoparticles support each other and result in outstanding mechanical properties. The crystalline BP in the LC epoxy resin-based nanocomposite was partially melted during exothermic photopolymerization, and the resin expanded via an order-to-disorder transition. Thus, the post-gelation shrinkage of the LC epoxy resin-based nanocomposite is greatly reduced, ∼50.6% less than in commercialized methacrylate resin-based composites. This LC epoxy nanocomposite demonstrates good physical and chemical properties and good biocompatibility

Overview on resins available in microlithography

International Nuclear Information System (INIS)

Serre, B.; Schue, F.; Montginoul, C.; Giral, L.

1985-01-01

Lithographic equipments using electrons and X radiation are developed. Velocity and resolution requirements fix the nature of the material to irradiate. Circuit making principles are recalled here; resists (organic polymers) are employed for it. The different types of resins and then needed characteristics are reviewed here. In the scope of electron sensitive resins methyl polymethacrylate and derivative and its copolymers (and copolymers of methacrylonitrile) and reticulated copolymers are studied. Polysulfones are also presented (poly(buten-1 sulfone), poly(styrene sulfone), poly(methyl-1 cyclopentene-1 sulfone). The interest in photosensitive resins (such as AZ) as electron sensitive resins is recalled. In the field of negative resins, the polyepoxyds, polystyrene and halogenated derivates from polystyrene (CMS and PCMS), the poly(vinyl-2 naphtalene) and its derivatives (PSTTF) are presented. The X radiation sensitive resins are also reviewed: the methyl polymethacrylate and its halogenated derivates, the acrylic homopolymers and copolymers (example of poly(acrylate of chlorinated alcoyls). The resins developable by plasma are mentioned. At last, for photosensitive resins, the diazide polydiene systems are presented together with systems diazo-2 2H-naphtalenone-1. The systems with salt photolysis are just recalled [fr

Effects of layering technique on the shade of resin overlays and the microhardness of dual cure resin cement

Directory of Open Access Journals (Sweden)

Hoon-Sang Chang

2014-06-01

Full Text Available The purpose of this study was to assess the color of layered resin overlays and to test the early microhardness of dual cure resin cement (DCRC light cured through the layered resin overlays. Resin overlays of 1.5 mm thickness were fabricated with the A3 shade of Z350 (Group 1L, the A3B and A3E shades of Supreme XT (Group 2L, and the A3, E3, and T1 shades of Sinfony (Group 3L using one, two, and three layers, respectively (n = 7. Each layer of the resin overlays was set in equal thickness. The color of the resin overlays was measured with a colorimeter and compared with an A3 shade resin denture tooth. DCRC was light cured through the resin overlays, and the early microhardness of the DCRC was measured. The ΔE value between the denture tooth and the resin overlays and the Vickers hardness number (VHN of the DCRC were analyzed with one-way ANOVA and Tukey’s HSD test. The color differences were 8.9 ± 0.5, 5.3 ± 1.0, and 7.3 ± 0.5 and the VHNs were 19.4 ± 1.1, 21.1 ± 0.9, and 29.3 ± 0.6 for Groups 1L, 2L, and 3L, respectively. Therefore, to match the designated tooth color of resin inlays and to increase the early microhardness of DCRC, layered resin inlays are more appropriate than single-dentin-layer resin inlays. However, the translucent layer should be used cautiously because the color difference of resin inlays with a translucent layer was affected more than those without a translucent layer.

The influences of N-acetyl cysteine (NAC) on the cytotoxicity and mechanical properties of Poly-methylmethacrylate (PMMA)-based dental resin.

Science.gov (United States)

Jiao, Yang; Ma, Sai; Li, Jing; Shan, Lequn; Yang, Yanwei; Li, Meng; Chen, Jihua

2015-01-01

Objectives. This study aimed to investigate the influences of N-acetyl cysteine (NAC) on cytotoxicity and mechanical properties of Poly-methylmethacrylate (PMMA) dental resins. Methods. Experimental PMMA resin was prepared by incorporating various concentrations of NAC (0, 0.15, 0.3, 0.6 and 0.9 wt.%). MTT assay was performed to investigate viability of human dental pulp cells after exposure to extract of PMMA resin with or without NAC. Cell adhesion on resin specimens was examined with scanning electron microscopy. Degree of conversion was studied with Fourier Transform Infrared Spectroscopy (FTIR). Flexural strength, microhardness and surface roughness was evaluated using a universal testing machine, microhardness tester and optical profilometer, respectively. Results. Incorporation of NAC into PMMA resin significantly reduced its cytotoxicity and enhanced cell adhesion on its surface. NAC induced negative influences on the mechanical and physical properties of PMMA resin in a dose-dependent manner. The degree of conversion for all experimental PMMA resins reached as high as 72% after 24 h of polymerization. All the tested properties were maintained when the concentration of incorporated NAC was 0.15 wt.%. Conclusion. The addition of 0.15 wt.% NAC remarkably improved biocompatibility of PMMA resin without exerting significant negative influence on its mechanical and physical properties.

The application of extraction chromatography for analysis of alkali and alkaline earth uranates

International Nuclear Information System (INIS)

Tomazic, B.; Cukovic, M.

1978-01-01

A method for rapid analysis of alkali and alkaline earth uranates is proposed. The method is based on the use of an HDEHP extraction chromatographic column, which makes possible quantitative separations of alkaline earth ions from macroamounts of uranium(VI). Composition of alkaline earth uranates, based on regression analysis, are presented. The results, which show that under the given experimental conditions alkaline earth triuranates precipitate, are in good agreement with previous data from same laboratory. In addition the HDEHP extraction chromatographic column can be suggested as a tool for separation of representative fission products from irradiated uranium for the purpose of determination of the burn-up factor of nuclear reactor materials. (T.G.)

Sampling and characterization of spent exchange resins of Atucha I nuclear power plant

International Nuclear Information System (INIS)

Varani, Jose L.; Cernadas, D.; Iglesias, Alberto M.; Raffo Calderon, Maria del C.

2004-01-01

The present storage facilities for spent resins in Atucha I NPP would be full within the next 5 years, accordingly some tasks are being planned to conditioning these waste and so generate enough storage capacity for the remaining life of the plant. Among this tasks is the characterization of spent resins that has several objectives: to know their chemical and radiochemical composition; the homogeneity of these parameters in the total volume of spent resins; the existence or not of compact zones; the proportion of 'crud'; the breakage degree of the micro-spheres; etc. The first step was to analyse the criterion to follow for sampling resins in the storage deposit of 40 m 3 . In order to take some samples from different points, a special device was required. It had to be introduced closed in the resin bed, opened to take the sample and then closed again to return to the surface. A device used in cereal industry for sampling silos to different depths was modified in its internal capacity for reducing operator dose and increasing the length of rod in order to reaching the bottom of the pit. The device was tested in cold mock up before to taking actual samples. Active resins samples, five in total up to now, were taken from deposit to different depths and kept in lead containers. After analysing the samples, the following average results were extracted: 1.7 x 10 5 Bq/g of Co-60, 9.7 x 10 5 Bq/g of Cs-137 and 774 Bq/g of total alpha, which corresponds to intermediate activity waste. The differences between the values of activity of the different samples are of up to 310 % for Co-60 and of up to 788 % for the Cs-137 what indicates a great inhomogeneity. The direct observation of resin grains, placed in a transparent glass burette, did not demonstrate an important proportion of broken or divided resins. (author)

Resin for processing radioactive waste water

International Nuclear Information System (INIS)

Onozuka, Teruo; Shindo, Manabu; Kiba, Hideaki; Kubota, Hirohisa; Sawada, Shintaro.

1995-01-01

The present invention concerns an anionic exchange resin having a long service life with less radiation degradation. The resin is an anionic exchange resin in which a trimethyl ammonium group is introduced to a copolymer of 4-bromo-butoxymethyl styrene and divinyl benzene. The resin is excellent in economic performance, and can reduce the frequency for the exchange of cross-linked anionic exchangers. (T.M.)

Resin for processing radioactive waste water

Energy Technology Data Exchange (ETDEWEB)

Onozuka, Teruo; Shindo, Manabu [Tohoku Electric Power Co., Inc., Sendai (Japan); Kiba, Hideaki; Kubota, Hirohisa; Sawada, Shintaro

1995-11-07

The present invention concerns an anionic exchange resin having a long service life with less radiation degradation. The resin is an anionic exchange resin in which a trimethyl ammonium group is introduced to a copolymer of 4-bromo-butoxymethyl styrene and divinyl benzene. The resin is excellent in economic performance, and can reduce the frequency for the exchange of cross-linked anionic exchangers. (T.M.).

Pigment Production from Immobilized Monascus sp. Utilizing Polymeric Resin Adsorption

OpenAIRE

Evans, Patrick J.; Wang, Henry Y.

1984-01-01

Pigment production by the fungus Monascus sp. was studied to determine why Monascus sp. provides more pigment in solid culture than in submerged culture. Adding a sterilized nonionic polymeric adsorbent resin directly to the growing submerged culture did not enhance the pigment production, thus indicating that pigment extraction is probably not a factor. Monascus cells immobilized in hydrogel were studied and exhibited decreased pigment production as a result of immobilization. This result is...

Magnetic hydrophilic-lipophilic balance sorbent for efficient extraction of chemical warfare agents from water samples.

Science.gov (United States)

Singh, Varoon; Purohit, Ajay Kumar; Chinthakindi, Sridhar; Goud D, Raghavender; Tak, Vijay; Pardasani, Deepak; Shrivastava, Anchal Roy; Dubey, Devendra Kumar

2016-02-19

Magnetic hydrophilic-lipophilic balance (MHLB) hybrid resin was prepared by precipitation polymerization using N-vinylpyrrolidone (PVP) and divinylbenzene (DVB) as monomers and Fe2O3 nanoparticles as magnetic material. These resins were successfully applied for the extraction of chemical warfare agents (CWAs) and their markers from water samples through magnetic dispersive solid-phase extraction (MDSPE). By varying the ratios of monomers, resin with desired hydrophilic-lipophilic balance was prepared for the extraction of CWAs and related esters of varying polarities. Amongst different composites Fe2O3 nanoparticles coated with 10% PVP+90% DVB exhibited the best recoveries varying between 70.32 and 97.67%. Parameters affecting the extraction efficiencies, such as extraction time, desorption time, nature and volume of desorption solvent, amount of extraction sorbent and the effect of salts on extraction were investigated. Under the optimized conditions, linearity was obtained in the range of 0.5-500 ng mL(-1) with correlation ranging from 0.9911-0.9980. Limits of detection and limits of quantification were 0.5-1.0 and 3.0-5.0 ng mL(-1) respectively with RSDs varying from 4.88-11.32% for markers of CWAs. Finally, the developed MDSPE method was employed for extraction of analytes from water samples of various sources and the OPCW proficiency test samples. Copyright © 2016 Elsevier B.V. All rights reserved.

New Anion-Exchange Resins for Improved Separations of Nuclear Materials

International Nuclear Information System (INIS)

Bartsch, Richard A.; Barr, Mary E.

2001-01-01

Improved separations of nuclear materials will have a significant impact upon a broad range of DOE activities. DOE-EM Focus Areas and Crosscutting Programs have identified improved methods for the extraction and recovery of radioactive metal ions from process, waste, and environmental waters as critical needs for the coming years. We propose to develop multifunctional anion-exchange resins that facilitate anion uptake by carefully controlling the structure of the anion receptor site. Our new ion-exchange resins interface the field of ion-specific chelating ligands with robust, commercial ion-exchange technology to provide materials which exhibit superior selectivity and kinetics of sorption and desorption. The following Focus Areas and Crosscutting Programs have described needs that would be favorably impacted by the new material: Efficient Separations and Processing - radionuclide removal from aqueous phases; Plutonium - Pu, Am or total alpha removal to meet regulatory requirement s before discharge to the environment; Plumes - U and Tc in groundwater, U, Pu, Am, and Tc in soils; Mixed Waste - radionuclide partitioning; High-Level Tank Waste - actinide and Tc removal from supernatants and/or sludges. The basic scientific issues which need to be addressed are actinide complex speciation along with modeling of metal complex/functional site interactions in order to determine optimal binding-site characteristics. Synthesis of multifunctionalized extractants and ion-exchange materials that implement key features of the optimized binding site, and testing of these materials, will provide feedback to the modeling and design activities. Resin materials which actively facilitate the uptake of actinide complexes from solution should display both improved selectivity and kinetic properties. The long-range implications of this research, however, go far beyond the nuclear complex. This new methodology of ''facilitated uptake'' could revolutionize ion-exchange technology

Isolation of nitrosylruthenium nitrato complexes by ion exchange and extraction chromatography

International Nuclear Information System (INIS)

Huang, H.; Liu, L.

TBP Levextrel and cation exchange resins were used to separate RuNO nitrato complexes of different nitric acid concentrations. 7402 quaternary ammonium salt Levextrel was used instead of an anionic exchange resin to separate anionic and neutral complex ions. The results indicated that D 3 and D 4 , which can easily be extracted by TBP, were anionic and neutral complex ions

Bulk-Fill Resin Composites

DEFF Research Database (Denmark)

Benetti, Ana Raquel; Havndrup-Pedersen, Cæcilie; Honoré, Daniel

2015-01-01

the restorative procedure. The aim of this study, therefore, was to compare the depth of cure, polymerization contraction, and gap formation in bulk-fill resin composites with those of a conventional resin composite. To achieve this, the depth of cure was assessed in accordance with the International Organization...... for Standardization 4049 standard, and the polymerization contraction was determined using the bonded-disc method. The gap formation was measured at the dentin margin of Class II cavities. Five bulk-fill resin composites were investigated: two high-viscosity (Tetric EvoCeram Bulk Fill, SonicFill) and three low......-viscosity (x-tra base, Venus Bulk Fill, SDR) materials. Compared with the conventional resin composite, the high-viscosity bulk-fill materials exhibited only a small increase (but significant for Tetric EvoCeram Bulk Fill) in depth of cure and polymerization contraction, whereas the low-viscosity bulk...

[Physical properties of resins for veneer crown. (Part 1) Bending strength of thermosetting methacrylic resins (author's transl)].

Science.gov (United States)

Kashiwada, T

1979-01-01

The physical properties of thermosetting methacrylic resins contain a kind or more than two kinds of cross linking agents were investigated. Knoop hardness and bending strength after drying, water sorption and thermal cycling were listed in table 4 and 5. Hydrophilic resins absorbed water about 3 times as much as hydrophobic resins. The materials contain a small amount of hydrophobic cross linking agents in MMA indicate comparatively excellent properties after drying, water sorption and thermal cycling. Knoop hardness of resins generally reduced by water sorption, especially in the case of the resin contains a large amount of triethylene glycol dimethacrylate.

Curing reaction of bisphenol-A based benzoxazine with cyanate ester resin and the properties of the cured thermosetting resin

Directory of Open Access Journals (Sweden)

H. Kimura

2011-12-01

Full Text Available Curing reaction of bisphenol-A based benzoxazine with cyanate ester resin and the properties of the cured thermosetting resin were investigated. The cure behavior of benzoxazine with cyanate ester resin was monitored by model reaction using nuclear magnetic resonance (NMR. As a result of the model reaction, the ring opening reaction of benzoxazine ring and thermal self-cyclotrimerization of cyanate ester group occurred, and then the phenolic hydoroxyl group generated by the ring opening reaction of benzoxazine ring co-reacted with cyanate ester group. The properties of the cured thermosetting resin were estimated by mechanical properties, electrical resistivity, water resistance and heat resistance. The cured thermosetting resin from benzoxazine and cyanate ester resin showed good heat resistance, high electrical resistivity and high water resistance, compared with the cured thermosetting resin from benzoxazine and epoxy resin.

Removal of radiocesium using cation exchange resin

International Nuclear Information System (INIS)

Morita-Murase, Yuko; Mizumura, Ryosuke; Tachibana, Yoshitaka; Kanazawa, Hideko

2013-01-01

Cation exchange resins (calcium polystyrene sulfonate, Ca-resin and sodium polystyrene sulfonate, Na-resin) have been used as agents to improve hyperkerlemia. For removing 137 Cs from the human body, the adsorption ability of the resin for 137 Cs was examined and evaluated. Resin (0.03 g) and 137 Cs (ca.1 kBq) were introduced into 3 mL of water, the Japanese Pharmacopoeia 1st fluid for a dissolution test (pH 1.2) and 2nd fluid (pH 6.8), respectively, and shaken. After 1-3 hours, the 137 Cs adsorption (%) of Na-resin was 99% in water, 60% in a pH 1.2 fluid and, 66% in a pH 6.8 fluid. By adding potassium, the 137 Cs adsorption (%) of Ca-resin was reduced. However, the 137 Cs adsorption (%) of Na-resin was almost unchanged. These results show that both resins have adsorption ability for 137 Cs in the stomach and the intestines. Therefore, the proposed method will be an effective means in the case of a radiological emergency due to 137 Cs. (author)

The extraction, identification and quantification of hypoglycemic ...

African Journals Online (AJOL)

Jane

2011-08-22

Aug 22, 2011 ... indicated that extraction U3 and U4 obviously decreased the blood sugar. Also, U3 was .... resin chromatography due to its main component, saponins identified by ..... The authors thank Changchun University of Technology.

Novel silica-based ion exchange resin

Energy Technology Data Exchange (ETDEWEB)

NONE

1997-11-01

Eichrom`s highly successful Diphonixo resin resembles a conventional ion exchange resin in its use of sulfonic acid ligands on a styrene- divinylbenzene matrix. Diphonix resin exhibits rapid exchange kinetics that allow economical operation of ion exchange systems. Unlike conventional resins, Diphonix resin contains chelating ligands that are diphosphonic acid groups that recognize and remove the targeted metals and reject the more common elements such as sodium, calcium and magnesium. This latter property makes Diphonix ideal for many industrial scale applications, including those involving waste treatment. For treatment of low-level, transuranic (TRU) and high- level radioactive wastes, Diphonix`s polystyrene backbone hinders its application due to radiolytic stability of the carbon-hydrogen bonds and lack of compatibility with expected vitrification schemes. Polystyrene-based Diphonix is approximately 60% carbon- hydrogen. In response to an identified need within the Department of Energy for a resin with the positive attributes of Diphonix that also exhibits greater radiolytic stability and final waste form compatibility, Eichrom has successfully developed a new, silica-based resin version of Diphonix. Target application for this new resin is for use in environmental restoration and waste management situations involving the processing of low-level, transuranic and high-level radioactive wastes. The resin can also be used for processing liquid mixed waste (waste that contains low level radioactivity and hazardous constituents) including mixed wastes contaminated with organic compounds. Silica-based Diphonix is only 10% carbon-hydrogen, with the bulk of the matrix silica.

Measurement of opalescence of resin composites.

Science.gov (United States)

Lee, Yong-Keun; Lu, Huan; Powers, John M

2005-11-01

Opalescence is an optical property, where there is light scattering of the shorter wavelengths of the visible spectrum, giving the material a bluish appearance under reflected light and an orange/brown appearance under transmitted light. The objective of this study was to determine the opalescence of resin composites with a color measuring spectrophotometer. Colors of A2 and enamel or translucent shades of four resin composites and of an unfilled resin measured in the reflectance and transmittance modes were compared, and the opalescence parameter (OP) was calculated as the difference in blue-yellow coordinate (Deltab*) and red-green parameter (Deltaa*) between the reflected and transmitted colors of 1-mm thick specimens. The masking effect was calculated as the color difference between the color of a black background and the color of specimen over the black background. The range of OP in resin composites was 5.7-23.7, which was higher than that of the unfilled resin. However, there were significant differences among the brands and shades of the resin composites. Opalescence varied by brand and shade of the resin composites, and contributed to the masking of background color along with translucency parameter. Some of the resin composites actually displayed opalescence.

Multiple chromatographic fingerprinting and its application to the quality control of herbal medicines

International Nuclear Information System (INIS)

Fan Xiaohui; Cheng Yiyu; Ye Zhengliang; Lin Ruichao; Qian Zhongzhi

2006-01-01

Recently, chromatographic fingerprinting has become one of the most powerful approaches to quality control of herbal medicines. However, the performance of reported chromatographic fingerprinting constructed by single chromatogram sometimes turns out to be inadequate for complex herbal medicines, such as multi-herb botanical drug products. In this study, multiple chromatographic fingerprinting, which consists of more than one chromatographic fingerprint and represents the whole characteristics of chemical constitutions of the complex medicine, is proposed as a potential strategy in this complicated case. As a typical example, a binary chromatographic fingerprinting of 'Danshen Dropping Pill' (DSDP), the best-sold traditional Chinese medicine in China, was developed. First, two HPLC fingerprints that, respectively, represent chemical characteristics of depsides and saponins of DSDP were developed, which were used to construct binary chromatographic fingerprints of DSDP. Moreover, the authentication and validation of the binary fingerprints were performed. Then, a data-level information fusion method was employed to capture the chemical information encoded in two chromatographic fingerprints. Based on the fusion results, the lot-to-lot consistency and frauds can be determined either using similarity measure or by chemometrics approach. The application of binary chromatographic fingerprinting to consistency assessment and frauds detection of DSDP clearly demonstrated that the proposed method was a powerful approach to quality control of complex herbal medicines

Disposal of bead ion exchange resin wastes

International Nuclear Information System (INIS)

Gay, R.L.; Granthan, L.F.

1985-01-01

Bead ion exchange resin wastes are disposed of by a process which involves spray-drying a bead ion exchange resin waste in order to remove substantially all of the water present in such waste, including the water on the surface of the ion exchange resin beads and the water inside the ion exchange resin beads. The resulting dried ion exchange resin beads can then be solidified in a suitable solid matrix-forming material, such as a polymer, which solidifies to contain the dried ion exchange resin beads in a solid monolith suitable for disposal by burial or other conventional means

T/sub 4/ radioimmunoassay with ion-exchange resin separation

Energy Technology Data Exchange (ETDEWEB)

Michael, J D; Modha, K [Hoechst Pharmaceuticals Research Ltd., Milton Keynes (UK)

1977-05-28

An explanation is provided for the reports of falsely low values of serum-thyroxine (T/sub 4/) measured by radioimmunoassay (RIA), particularly in sera containing raised concentrations of thyroxine-binding globulin (TBG) (Burr, W.A., Evans, S.E., Hogan, T.C., 1977, Lancet, April 2, 757). A re-examination of the assay technique used in commercial RIA kits ('RIA-gnost T/sub 3/' and 'RIA-gnost T/sub 4/', Behring Diagnostics) showed that blocking of binding proteins by 8-anilino-1-naphthalene sulphonic acid (ANS) was incomplete in sera with raised TBG levels. Spectroscopic determination of the blocker concentration during the time the solution was in contact with the ion exchange resin showed that 98% of the ANS was removed from solution by 10 min contact with the resin, yet 60 min was required to absorb the free T/sub 4/. There was therefore ample time for unblocked TBG to recombine with free T/sub 4/ which was then misclassified as antibody-bound T/sub 4/. The assay technique used in the kits was therefore modified. The less polar TBG blocking agent, ethylmercurithiosalicylate (merthiolate), replaced ANS and it was demonstrated that accurate T/sub 3/ and T/sub 4/ measurements in high TBG sera could be made by resin-separation RIA without resorting to prior denaturation or alcohol extraction.

Curing kinetics of alkyd/melamine resin mixtures

Directory of Open Access Journals (Sweden)

Jovičić Mirjana C.

2009-01-01

Full Text Available Alkyd resins are the most popular and useful synthetic resins applied as the binder in protective coatings. Frequently they are not used alone but are modified with other synthetic resins in the manufacture of the coatings. An alkyd/melamine resin mixture is the usual composition for the preparation of coating called 'baking enamel' and it is cured through functional groups of resins at high temperatures. In this paper, curing kinetics of alkyd resins based on castor oil and dehydrated castor oil with melamine resin, has been studied by DSC method with programmed heating and in isothermal mode. The results determined from dynamic DSC curves were mathematically transformed using the Ozawa isoconversional method for obtaining the isothermal data. These results, degree of curing versus time, are in good agreement with those determined by the isothermal DSC experiments. By applying the Ozawa method it is possible to calculate the isothermal kinetic parameters for the alkyd/melamine resin mixtures curing using only calorimetric data obtained by dynamic DSC runs. Depending on the alkyd resin type and ratio in mixtures the values of activation energies of curing process of resin mixtures are from 51.3 to 114 kJ mol-1. The rate constant of curing increases with increasing the content of melamine resin in the mixture and with curing temperature. The reaction order varies from 1.12 to 1.37 for alkyd based on dehydrated castor oil/melamine resin mixtures and from 1.74 to 2.03 for mixtures with alkyd based on castor oil. Based on the results obtained, we propose that dehydrated castor oil alkyd/melamine resin mixtures can be used in practice (curing temperatures from 120 to 160°C.

Miniaturized chromatographic radiochemical procedure for 131I - MIBG

International Nuclear Information System (INIS)

Barboza, M.F. de; Pereira, N.S. de; Colturato, M.T.; Silva, C.P.G. da.

1989-12-01