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Sample records for extraction chromatographic resin

  1. Test plan for demonstrating plutonium extraction from 10-L solutions using EIChrom extraction chromatographic resins

    International Nuclear Information System (INIS)

    Barney, G.S.

    1994-01-01

    Corrosive plutonium solutions stored in 10-L containers at the Plutonium Finishing Plant must be treated to convert the plutonium to a safe, solid form for storage and to remove the americium so that radiation exposure can be reduced. Extraction chromatographic resins will be tested for separating plutonium from these solutions in the laboratory. Separation parameters will be developed during the testing for large scale processing of the 10-L solutions and solutions of similar composition. Use of chromatographic resins will allow plutonium separation with minimum of chemical addition to the feed and without the need for plutonium valence adjustment. The separated plutonium will be calcined to plutonium oxide by direct solution calcination

  2. Monitoring for 99Tc in borehole waters using an extraction chromatographic resin

    International Nuclear Information System (INIS)

    Davis, T.M.; Nelson, D.M.; Thompson, E.G.

    1993-01-01

    A technique using an extraction chromatographic resin for the analysis of 99 Tc in borehole waters is presented. The method involves one pass of the sample through two resins, a rinse of the resins, then counting of one of the resins by liquid scintillation counting. The technique is intended to be used as a screening method of 99 Tc. The procedure employs commercially available materials, generates little waste and requires very little operator time

  3. Development of an extractive-scintillating chromatographic resin for the detection of radioactive isotopes

    International Nuclear Information System (INIS)

    Vincze, A.; Halasz, L.; Solymosi, J.; Molnar, A.; Safrany, A.

    2007-01-01

    In this paper, the development of a new-type of resin is presented, which contains selective complexing and scintillating molecules in a chemically bonded form. The resin material is produced via radiation polymerization of a solution of 2-(4-allyloxy-phenyl)-5-phenyl oxazole, 5-(allyloxyphenyl)- 2-[4-(5-phenyl-oxazole-2-il)-phenyl] oxazole, diethylene glycol dimethacrylate (DEGMA), styrene and the allyl derivative of a 18C6 crown ether-dicarbolic acid complexing agent. The product is a macroporous polymer matrix that shows fluorescent properties and ion binding capacity excellent for radioanalytical purposes. (author)

  4. 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.

  5. New extraction chromatographic material for rhenium separation

    International Nuclear Information System (INIS)

    Lucanikova, M.; Czech Technical University, Prague; Kucera, J.; Czech Technical University, Prague; Sebesta, F.

    2008-01-01

    Three types of the extraction chromatographic materials, composed from Aliquat R 336 deposited in the polyacrylonitrile (PAN) beads and prepared by different procedures, were compared for extraction of rhenium. The best properties were exhibited when the solid extractant was prepared by impregnation of the ready-made PAN beads. Solid extractant prepared by direct coagulation of the beads from the suspension of Aliquat R 336 in solution of PAN in nitric acid differs only by lower capacity in dynamic conditions. Material prepared from the PAN solution in dimethylsulfoxide was the worst because Aliquat R 336 was washed out from the beads during coagulation of the polymer and the extraction capacity was low. As it is shown, the first two solid extractants are fully comparable with the commercial TEVA Resin. (author)

  6. Study PWA8 resin for chromatographic uranium concentration

    International Nuclear Information System (INIS)

    Coceancigh, Herman; Ramella, J. L.; Marrero, Julieta; Jiménez Rebagliati, Raúl

    2013-01-01

    For many years nuclear industry have been using resins as filler of chromatographic columns. These methods are specific and give reliable results in different applications, for those reasons are extremely useful as separation process. Currently the nuclear industry is growing and this brings new issues such as the need of reduction of the amount of waste, the optimization of the production process and others that the chromatography could solve with great results. AMBERLITETM PWA8 resin is an anion exchange resin which can be used for the removal of uranium from drinking water. In addition to high exchange capacity, this resin has excellent physical stability and a wide range of pH in which is operational. With the idea of concentrating uranium from wastes solution as main goal we made different experiments to understand the AMBERLITETM PWA8 and obtain the most important characteristics like; pH working range; capacity; activation and elution procedures. These procedures were developed and optimized the capacity was determined using a batch experiment and we obtain that the maximum capacity is 882,5 U ug /resin gr at a pH of 4,2. Following on from these results chromatographic experiments were performed in which both were obtained the percentage of recovery and the concentration factor. The percent recovery (% R) calculated as the percentage ratio between the total mass and the load mass eluted (% R = eluted mass / total mass * 100) was 94% with a concentration factor of 5 times From these results it is intended to concentrate wastes solutions from the fuel cycle processes with two main goals: decreasing volume for storage and for future reusing of the uranium coming from production. (author)

  7. 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.

  8. 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.

  9. Determination of trace levels of uranium and thorium in high purity gadolinium sulfate using the ICP-MS with solid-phase chromatographic extraction resin

    Science.gov (United States)

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

    2017-11-01

    The new Super-Kamiokande-Gadolinium (SK-Gd) project is an upgrade of the Super-Kamiokande (SK) detector. In the SK-Gd project, 0.2% Gd_2(SO_4)_3 is loaded into the 50 kton water tank of the SK. One of the main purposes of the project is to discover supernova relic neutrinos. Neutrino measurements and proton decay searches will also be performed in the SK-Gd. In order to measure solar neutrinos with a low energy threshold of ˜3.5 MeV in the SK-Gd, the main radioactive contaminations, ^{238}U and ^{232}Th, in Gd_2(SO_4)_3{\\cdot}8H_2O, should be minimized before loading. Our maximum levels for U and Th are 5 mBq (U)/kg (Gd_2(SO_4)_3{\\cdot}8H_2O) and 0.05 mBq (Th)/kg (Gd_2(SO_4)_3{\\cdot}8H_2O). In order to measure such low concentrations of U and Th in Gd_2(SO_4)_3{\\cdot}8H_2O, we developed the solid-phase extraction technique. Using this method, about 90% or more U and Th could be efficiently extracted while Gd was reduced by a factor of about 104. This allowed these radioactivity contaminations to be measured precisely as 0.04 mBq/kg (Gd_2(SO_4)_3{\\cdot}8H_2O) for U and 0.01 mBq/kg (Gd_2(SO_4)_3{\\cdot}8H_2O) for Th. We measured three pure Gd_2(SO_4)_3{\\cdot}8H_2O samples using this method and estimated that the purest one contained <0.04 mBq (U)/kg (Gd_2(SO_4)_3{\\cdot}8H_2O) and 0.06 ± 0.01 mBq (Th)/kg (Gd_2(SO_4)_3{\\cdot}8H_2O) by the ICP-MS.

  10. 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.

  11. Column chromatographic separation of Y3+ from Sr2+ by polymeric ionizable crown ether resins

    International Nuclear Information System (INIS)

    Wood, D.J.; Elshani, S.; Wai, C.M.; Bartsch, R.A.; Huntley, M.; Hartenstein, S.

    1993-01-01

    Condensation polymers containing subunits of crown ether carboxylic acid monomers are effective stationary phases for the chromatographic separation of Y 3+ and Sr 2+ . The pH range and metal loading capacities for the resins have been determined under equilibrium conditions. The resin can be regenerated for repeated use without losing its separation capability. Altering the molecular structure of the monomer (sym-dibenzo-16-crown-5-oxyacetic acid) by an alkyl substitution on the macrocyclic cavity decreases the loading capacity of the resin

  12. On-line gross alpha radiation monitoring of natural waters with extractive scintillating resins

    International Nuclear Information System (INIS)

    Hughes, Lara; De Vol, T.A.

    2003-01-01

    Extractive scintillating resins, which are used to simultaneously separate and quantify radioactivity in aqueous solutions, were developed for low-level alpha radiation monitoring of natural waters. Resins were investigated with bis(2-ethylhexyl)methane-diphosphonic acid (H 2 DEH[MDP], Dipex[reg]) extractant, which has a strong affinity for tri-, tetra- and hexavalent actinides in dilute acids. Extractive scintillating resins were manifested (1) as a mixed bed of scintillating resin and extraction chromatographic resin and (2) by diffusing the organic fluor 2-(1-naphtyl)-5-phenyloxazole into macroporous polystyrene chromatographic resin, then coating with H 2 DEH[MDP], or by coating H 2 DEH[MDP] on scintillating polyvinyltoluene beads. The scintillation light was detected with a modified Hidex Triathler to allow for continuous flow measurements. The average detection efficiencies were 51.7±2.6% and 65.8±10.1% for natural uranium and 241 Am, respectively, for the extractant coated scintillator. The resin was stable for solution flow of up to 1000 ml resulting in rapid real-time quantification of natural uranium in groundwater down to 30 μg/ml

  13. Single-column extraction chromatographic separation of U, Pu, Np and Am

    Energy Technology Data Exchange (ETDEWEB)

    Morgenstern, A.; Apostolidis, C.; Carlos-Marquez, R.; Mayer, K.; Molinet, R. [Commission of the European Communities, Karlsruhe (Germany). European Inst. for Transuranium Elements

    2002-07-01

    A rapid, single-column extraction chromatographic method using commercially available UTEVA resin has been developed for the separation of uranium, plutonium, neptunium and americium. The method yields recoveries superior to 90% and allows direct loading of separated fractions on filaments for subsequent analysis by thermal ionization mass spectrometry. The use of reagents compatible with robotized equipment allows automation of the separation process for routine analysis of nuclear materials. The redox reactions between plutonium, neptunium and hydrogen peroxide involved in the separation process were studied by UV/Vis/NIR absorption spectroscopy. (orig.)

  14. Use of coextraction and suppression of extraction in extraction-chromatographic separation of elements

    International Nuclear Information System (INIS)

    Karandashev, V.K.; Kuznetsov, R.A.; Grazhulene, S.S.; Usmanova, M.M.

    1988-01-01

    TBP, solutions of hydrobromic acid, indium and polytetrafluoroethylene powder, carrier for TBP, were used to study the effects of coextraction and extraction suppression on extraction-chromatographic behaviour of microamounts of elements in the presence of macroamounts of other elements. Possibility of using these effects under extraction-chromatographic element separation were considered. A new method for extraction-chromatographic separation of scandium microamounts from the mixture of large amount of elements (Y, Cd, Ce, Eu, Lu, Hf, Ta, W, Np and other) was suggested. 15 refs.; 3 figs

  15. Extraction chromatographic separation of Sr, Pu and Am in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Sidhu, Rajdeep

    2004-04-01

    An accurate determination of radionuclides from various sources in the environment is essential for assessment of the potential hazards and suitable countermeasures both in case of an authorised release, accidents and routine surveillance. Due to the short range of alpha and beta radiation, the accurate determination of pure alpha and beta emitters must always include radiochemical separations to separate the analytes from the matrix and from other interfering stable and radioactive nuclides. Hence, the procedures used for their determination are usually tedious and involve several preconcentration and separation steps. This work deals with the determination of {sup 90}Sr, {sup 241}Am, {sup 238}Pu, {sup 239,240}Pu and {sup 244}Cm, whic some of the most important artificial radionuclides. Due to either absence or low yield of gamma radiation, a secure determination of low concentrations of all these nuclides requires a dedicated chemistry. Selective extraction chromatographic resins (TRU- and Sr-Resin) have been utilised to develop new procedures for the analyses of Pu, Am and Cm isotopes in seawater and both these and {sup 90}Sr in soil, sediment, urine and low-level liquid radioactive effluents. The proposed method for the analyses of Pu and Am in seawater offers a quick and secure mode for the determination of these radionuclides in marine waters. Combined pre-concentration of actinides and strontium (oxalate or phosphate precipitation) followed by dual column separation on TRU- and Sr-Resin significantly reduces the through put time and costs compared to traditional ion exchange and precipitation methods. The greatest gain in productivity and environmental friendliness is achieved in Sr separations using Sr-Resin instead of precipitations involving fuming nitric acid and oxalate, hydroxide, chromate and carbonate precipitations. (author)

  16. Solid phase extraction of Am (III) by resins impregnated with multiply diglycolamide-functionalized ligands

    International Nuclear Information System (INIS)

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

    2016-01-01

    Solvent extraction studies with multiply diglycolamide-functionalized extractants such as tripodal diglycolamide (T-DGA) or diglycolamide-functionalized calix(4)arene (C4DGA) ligands have shown excellent results as compared to those of normal DGA ligands such as TODGA. A very high selectivity for Am(III) has been reported with these ligands with respect to U(VI) and Pu(IV). High selectivities and large extraction efficiencies of these ligands towards trivalent f elements were ascribed to a co-operative complexation mechanism. Furthermore, the extraction efficiency of these ligands increased several folds in ionic liquid medium as compared to paraffinic solvents. It was of interest, therefore, to prepare extraction chromatographic resins by impregnation of solvent systems containing these ligands in an ionic liquid. In the present work, solid phase extraction studies were carried out using these two multiply diglycolamide-functionalized extractants, viz. T-DGA (resin I) and C4DGA (resin-II) containing the ionic liquid C 4 mim. NTf 2 impregnated on Chromosorb-W

  17. 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.

  18. 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)

  19. 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.

  20. 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.

  1. 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.

  2. Preparation of extractive resins for producing terbium-161

    International Nuclear Information System (INIS)

    De la Cruz B, C. C.; Monroy G, F.

    2009-10-01

    This paper presents the development of a methodology for extractive resins preparation to base of HDEHP, which allows to separation of Tb from Gd generating an own technology of preparation of these resins. The study included the extractive resins preparation from 6 different supports: kieselguhr Dg, alumina, red volcanic rock, chiluca, quarry and fluorite; two treatment types of of supports and varied concentrations of HDEHP extractant (di(2-etil hexyl) orthophosphoric acid), in order to determine which resin has improved efficiency of Gd and Tb separation, and radionuclide purity of 161 Tb. Resins were prepared to base of kieselguhr to determine the most appropriate silicon deposition process. Two silicon deposition treatments were realized: treatment I , by contact with silicon deposition solution (dimethyldichlorosilane / heptane 1:30) and treatment II by contact with vapors of dimethyldichlorosilane in vacuum. The extractant retention was carried out to different concentrations of HDEHP / acetone: 1:4, 1:8, 1:15, 1:20, 1:30 and 1:40. According to the results, there is not direct relation of HDEHP concentration used in extractive resins preparation to base of kieselguhr over the efficiency of Gd and Tb separation and of radionuclide purity of 161 Tb. The effect of support in the efficiency of Gd and Tb separation was studied to prepare resins with the supports kieselguhr, alumina, quarry, chiluca, volcanic rock and fluorite, using the silicon deposition treatment II for the supports and a concentration of HDEHP / acetone 1:20, for extractant retention. Only resins based on kieselguhr could separate to Gd from Tb quantitatively, the resin at a concentration of HDEHP / Acetone 1:20 was the best results obtained in Gd and Tb separation, achieving a separation efficiency greater than 90% and a radionuclide purity higher than 99%. (Author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-05-01

    Chromatographic resin containing extractants such as octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide (CMPO) or bis-(2-ethylhexyl)phosphoric acid (HDEHP) or mixture of extractants (CMPO + HDEHP) in an acrylic polymer matrix was prepared and studied for the extraction of Am(III) and Eu(III) over a range of nitric acid concentration. The effect of various parameters such as concentration of nitric acid in aqueous phase and the concentration of CMPO and HDEHP in the resin phase was studied. The distribution coefficient of Am(III) and Eu(III) in the impregnated resin increased with increased in the concentration of nitric acid for CMPO-impregnated resin, whereas a reverse trend was observed in HDEHP impregnated resin. In case of resin containing both the extractants, synergism was observed at low nitric acid concentration and antagonism at high nitric acid concentration. The mechanism of extraction was probed by slope analysis method at 0.01 and 2 M nitric acid concentrations. Citrate-buffered DTPA was used for the selective separation of Am(III), and a separation factor of 3-4 was obtained at pH 3.

  4. 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...

  5. 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 ...

  6. 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

  7. Improved resins and novel materials and methods for solid phase extraction and high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Freeze, Ronald [Iowa State Univ., Ames, IA (United States)

    1997-10-08

    Solid-phase extraction (SPE) has grown to be one of the most widely used methods for isolation and preconcentration of a vast range of compounds from aqueous solutions. By modifying polymeric SPE resins with chelating functional groups, the selective uptake of metals was accomplished. The resin, along with adsorbed metals, was vaporized in the ICP and detection of the metals was then possible using either mass or emission spectroscopy. Drug analyses in biological fluids have received heightened attention as drug testing is on the increase both in sports and in the work environment. By using a direct-injection technique, biological fluids can be injected directly into the liquid chromatographic system with no pretreatment. A new surfactant, a sulfonated form of Brij-30 (Brij-S) is shown to prevent the uptake of serum proteins on commercial HPLC columns by forming a thin coating on the silica C18 surface. Excellent separations of eight or more drugs with a wide range of retention times were obtained. The separations had sharper peaks and lower retention times than similar separations performed with the surfactant sodium dodecylsulfate (SDS). Quantitative recovery of a number of drugs with limits of detection near 1 ppm with a 5 μl injection volume were obtained. Finally, a method for solid-phase extraction in a syringe is introduced. The system greatly reduced the volume of solvent required to elute adsorbed analytes from the SPE bed while providing a semi-automated setup. SPE in a syringe consists of a very small bed of resin-loaded membrane packed into a GC or HPLC syringe. After extraction, elution was performed with just a few μl of solvent. This small elution volume allowed injection of the eluent directly from the syringe into the chromatographic system, eliminating the handling problems associated with such small volumes.

  8. Rapid determination of environmental plutonium in large water samples by means of manganese dioxide Co-precipitation and extraction chromatographic separation

    International Nuclear Information System (INIS)

    Sidhu, R.S.; Hoff, P.

    1999-01-01

    Plutonium activity determinations in environmental water samples are routinely performed in many laboratories. Due to the low plutonium concentrations and the complexity of the plutonium aqueous chemistry, these analysis involve cumbersome preconcentration and separation procedures and long measurement times. We describe a procedure where MnO 2 (s) is used as scavenger to preconcentrate Pu prior to separation by the transuranium specific extraction chromatographic resin TRU-Resin. The ability of MnO 4 - /MnO 2 (s) to destroy organic matter and oxidise plutonium is combined with the specific behaviour of the TRU-resin for transuranium elements. The method facilitates a rapid preconcentration and separation of plutonium. With the use of this procedure, the laboratory work on one sample can be performed in one day with minimum attention. The overall yields from a 200 litre fresh- or seawater sample to a measurable Pu source are between 70-85%. (orig.)

  9. 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

  10. 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...

  11. 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

  12. 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.

  13. 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 ...

  14. 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, ...

  15. Estimation of uranium isotope in urine samples using extraction chromatography resin

    International Nuclear Information System (INIS)

    Thakur, Smita S.; Yadav, J.R.; Rao, D.D.

    2012-01-01

    Internal exposure monitoring for alpha emitting radionuclides is carried out by bioassay samples analysis. For occupational radiation workers handling uranium in reprocessing or fuel fabrication facilities, there exists a possibility of internal exposure and urine assay is the preferred method for monitoring such exposure. Estimation of lower concentration of uranium at mBq level by alpha spectrometry requires preconcentration and its separation from large volume of urine sample. For this purpose, urine samples collected from non radiation workers were spiked with 232 U tracer at mBq level to estimate the chemical yield. Uranium in urine sample was pre-concentrated by calcium phosphate coprecipitation and separated by extraction chromatography resin U/TEVA. In this resin extractant was DAAP (Diamylamylphosphonate) supported on inert Amberlite XAD-7 support material. After co-precipitation, precipitate was centrifuged and dissolved in 10 ml of 1M Al(NO 3 ) 3 prepared in 3M HNO 3 . The sample thus prepared was loaded on extraction chromatography resin, pre-conditioned with 10 ml of 3M HNO 3 . Column was washed with 10 ml of 3M HNO 3 . Column was again rinsed with 5 ml of 9M HCl followed by 20 ml of 0.05 M oxalic acid prepared in 5M HCl to remove interference due to Th and Np if present in the sample. Uranium was eluted from U/TEVA column with 15 ml of 0.01M HCl. The eluted uranium fraction was electrodeposited on stainless steel planchet and counted by alpha spectrometry for 360000 sec. Approximate analysis time involved from sample loading to stripping is 2 hours when compared with the time involved of 3.5 hours by conventional ion exchange method. Seven urine samples from non radiation worker were radio chemically analyzed by this technique and the radiochemical yield was found in the range of 69-91 %. Efficacy of this method against conventional anion exchange technique earlier standardized at this laboratory is also being highlighted. Minimum detectable activity

  16. 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

  17. 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...

  18. 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)

  19. Comparison of solvent extraction and extraction chromatography resin techniques for uranium isotopic characterization in high-level radioactive waste and barrier materials.

    Science.gov (United States)

    Hurtado-Bermúdez, Santiago; Villa-Alfageme, María; Mas, José Luis; Alba, María Dolores

    2018-07-01

    The development of Deep Geological Repositories (DGP) to the storage of high-level radioactive waste (HLRW) is mainly focused in systems of multiple barriers based on the use of clays, and particularly bentonites, as natural and engineered barriers in nuclear waste isolation due to their remarkable properties. Due to the fact that uranium is the major component of HLRW, it is required to go in depth in the analysis of the chemistry of the reaction of this element within bentonites. The determination of uranium under the conditions of HLRW, including the analysis of silicate matrices before and after the uranium-bentonite reaction, was investigated. The performances of a state-of-the-art and widespread radiochemical method based on chromatographic UTEVA resins, and a well-known and traditional method based on solvent extraction with tri-n-butyl phosphate (TBP), for the analysis of uranium and thorium isotopes in solid matrices with high concentrations of uranium were analysed in detail. In the development of this comparison, both radiochemical approaches have an overall excellent performance in order to analyse uranium concentration in HLRW samples. However, due to the high uranium concentration in the samples, the chromatographic resin is not able to avoid completely the uranium contamination in the thorium fraction. Copyright © 2018 Elsevier Ltd. All rights reserved.

  20. 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)

  1. 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.

  2. 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...

  3. 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

  4. 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.

  5. 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.)

  6. 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.

  7. 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

  8. 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.

  9. 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.

  10. 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

  11. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  13. 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.

  14. 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

  15. 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

  16. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  18. 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%.

  19. 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

  20. [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.

  1. 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

  2. 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.

  3. 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

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

    Directory of Open Access Journals (Sweden)

    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.

  5. 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)

  6. 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.

  7. 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.

  8. 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

  9. 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

  10. 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

  11. 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.

  12. 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.

  13. 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)

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 45Ti extraction using hydroxamate resin

    DEFF Research Database (Denmark)

    Gagnon, K.; Severin, Gregory; Barnhart, T. E.

    2012-01-01

    As an attractive radionuclide for positron emission tomography, this study explores the extraction and reactivity of 45Ti produced via the 45Sc(p,n)45Ti reaction on a GE PETtrace. Using a small hydroxamate column, we have demonstrated an overall recovery of >50% of 45Ti in ~1 mL of 1M oxalic acid...

  19. 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

  20. 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)

  1. 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.

  2. 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)

  3. 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.

  4. 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.

  5. The extraction and chromatographic determination of the essentials oils from Ocimum basilicum L. by different techniques

    Energy Technology Data Exchange (ETDEWEB)

    Soran, Maria Loredana; Varodi, Codruta; Lung, Ildiko; Surducan, Emanoil; Surducan, Vasile [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath, 400293 Cluj-Napoca (Romania); Cobzac, Simona Codruta, E-mail: loredana.soran@itim-cj.r [Babes-Bolyai University, Faculty of Chemistry and Chemical Engineering, 11 Arany Janos, 400028 Cluj-Napoca (Romania)

    2009-08-01

    Three different techniques (maceration, sonication and extraction in microwave field) were used for extraction of essential oils from Ocimum basilicum L. The extracts were analyzed by TLC/HPTLC technique and the fingerprint informations were obtained. The GC-FID was used to characterized the extraction efficiency and for identify the terpenic bioactive compounds. The most efficient extraction technique was maceration followed by microwave and ultrasound. The best extraction solvent system was ethyl ether + ethanol (1:1, v/v). The main compounds identified in Ocimum basilicum L. extracts were: {alpha} and {beta}-pinene (mixture), limonene, citronellol, and geraniol.

  6. The extraction and chromatographic determination of the essentials oils from Ocimum basilicum L. by different techniques

    International Nuclear Information System (INIS)

    Soran, Maria Loredana; Varodi, Codruta; Lung, Ildiko; Surducan, Emanoil; Surducan, Vasile; Cobzac, Simona Codruta

    2009-01-01

    Three different techniques (maceration, sonication and extraction in microwave field) were used for extraction of essential oils from Ocimum basilicum L. The extracts were analyzed by TLC/HPTLC technique and the fingerprint informations were obtained. The GC-FID was used to characterized the extraction efficiency and for identify the terpenic bioactive compounds. The most efficient extraction technique was maceration followed by microwave and ultrasound. The best extraction solvent system was ethyl ether + ethanol (1:1, v/v). The main compounds identified in Ocimum basilicum L. extracts were: α and β-pinene (mixture), limonene, citronellol, and geraniol.

  7. 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.

  8. 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)

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

    Directory of Open Access Journals (Sweden)

    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.

  10. 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,...

  11. 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)

  12. Chromatographic profiles of Phyllanthus aqueous extracts samples: a proposition of classification using chemometric models.

    Science.gov (United States)

    Martins, Lucia Regina Rocha; Pereira-Filho, Edenir Rodrigues; Cass, Quezia Bezerra

    2011-04-01

    Taking in consideration the global analysis of complex samples, proposed by the metabolomic approach, the chromatographic fingerprint encompasses an attractive chemical characterization of herbal medicines. Thus, it can be used as a tool in quality control analysis of phytomedicines. The generated multivariate data are better evaluated by chemometric analyses, and they can be modeled by classification methods. "Stone breaker" is a popular Brazilian plant of Phyllanthus genus, used worldwide to treat renal calculus, hepatitis, and many other diseases. In this study, gradient elution at reversed-phase conditions with detection at ultraviolet region were used to obtain chemical profiles (fingerprints) of botanically identified samples of six Phyllanthus species. The obtained chromatograms, at 275 nm, were organized in data matrices, and the time shifts of peaks were adjusted using the Correlation Optimized Warping algorithm. Principal Component Analyses were performed to evaluate similarities among cultivated and uncultivated samples and the discrimination among the species and, after that, the samples were used to compose three classification models using Soft Independent Modeling of Class analogy, K-Nearest Neighbor, and Partial Least Squares for Discriminant Analysis. The ability of classification models were discussed after their successful application for authenticity evaluation of 25 commercial samples of "stone breaker."

  13. 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)

  14. Comparison of column chromatographic and precipitation methods for the purification of a macrocyclic polyether extractant

    Energy Technology Data Exchange (ETDEWEB)

    Dietz, M.L.; Felinto, C.; Rhoads, S.; Clapper, M.; Finch, J.W.; Hay, B.P.

    1999-11-01

    Column chromatography on aminopropyl-derivatized silica and precipitation of a complex with perchloric acid have been evaluated as methods for the purification of di-tert-butylcyclohexano-18-crown-6 (DtBuCH18C6), a compound frequently employed for the selective extraction of strontium from acidic nitrate media. Both methods are shown to provide a simple and effective means of eliminating inactive sample components (i.e., impurities or stereoisomers incapable of extracting strontium) from the crown ether and enriching the material in 4(z),4{prime}(z) cis-syn-cis DtBuCH18C6, a stereoisomer capable of highly efficient strontium extraction.

  15. Comparison of column chromatographic and precipitation methods for the purification of a macrocyclic polyether extractant

    International Nuclear Information System (INIS)

    Dietz, M.L.; Felinto, C.; Rhoads, S.; Clapper, M.; Finch, J.W.; Hay, B.P.

    1999-01-01

    Column chromatography on aminopropyl-derivatized silica and precipitation of a complex with perchloric acid have been evaluated as methods for the purification of di-tert-butylcyclohexano-18-crown-6 (DtBuCH18C6), a compound frequently employed for the selective extraction of strontium from acidic nitrate media. Both methods are shown to provide a simple and effective means of eliminating inactive sample components (i.e., impurities or stereoisomers incapable of extracting strontium) from the crown ether and enriching the material in 4(z),4 prime(z) cis-syn-cis DtBuCH18C6, a stereoisomer capable of highly efficient strontium extraction

  16. Extraction and detection of arsenicals in seaweed via accelerated solvent extraction with ion chromatographic separation and ICP-MS detection

    Energy Technology Data Exchange (ETDEWEB)

    Gallagher, P.A.; Shoemaker, J.A.; Wei Xinyi; Brockhoff-Schwegel, C.A.; Creed, J.T. [Microbiological and Chemical Exposure Assessment Research Div., Cincinnati, OH (United States)

    2001-01-01

    An accelerated solvent extraction (ASE) device was evaluated as a semi-automated means of extracting arsenicals from ribbon kelp. The effect of the experimentally controllable ASE parameters (pressure, temperature, static time, and solvent composition) on the extraction efficiencies of arsenicals from seaweed was investigated. The extraction efficiencies for ribbon kelp (approximately 72.6%) using the ASE were fairly independent (< 7%) of pressure, static time and particle size after 3 ASE extraction cycles. The optimum extraction conditions for the ribbon kelp were obtained by using a 3 mL ASE cell, 30/70 (w/w) MeOH/H{sub 2}O, 500 psi (1 psi = 7 KPa), ambient temperature, 1 min heat step, 1 min static step, 90% vol. flush, and a 120 s purge. Using these conditions, two other seaweed products produced extraction efficiencies of 25.6% and 50.5%. The inorganic species present in the extract represented 62.5% and 27.8% of the extracted arsenic. The speciation results indicated that both seaweed products contained 4 different arsenosugars, DMA (dimethylarsinic acid), and As(V). One seaweed product also contained As(III). Both of these seaweed products contained an arsenosugar whose molecular weight was determined to be 408 and its structure was tentatively identified using ion chromatography-electrospray ionization-mass spectrometry/mass spectrometry (IC-ESI-MS/MS). (orig.)

  17. EXTRACTION-CHROMATOGRAPHIC DETERMINATION OF GLUCOSE AND FRUCTOSE IN THE PRESENCE OF AROMATIC AMINO ACIDS

    Directory of Open Access Journals (Sweden)

    Y. I. Korenman

    2012-01-01

    Full Text Available The extraction of glucose and fructose from aqueous salt solutions containing aromatic amino acids (phenylalanine, tryptophan, tyrosine, hydrophilic solvents (aliphatic alcohols, alkyl acetates, ketones have been studied. The quantitative characteric of the process (the distribution coefficients, the degree of extraction, separation factors are calculeted. The dependence of distribution ratios of monosaccharides from the amino acid content in the solution has been established. A mobile phase for analysis of the concentrate by ascending thin layer chromatography have been developed.

  18. Supercritical fluid extraction (SFE) and gas chromatographic (GC) analysis of products from irradiated foods containing fat

    International Nuclear Information System (INIS)

    Adam, S.T.

    1993-01-01

    Official analytical methods specify the use of organic liquid solvents which may be hazardous to human health. Non-toxic chlorinated fluorocarbons (CFC) which are still recommended for extracting soil samples are known to be detrimental to the stratospheric ozone layer and therefore subject to the ''FCKW-Halon-Verbots-Verordnung''. Therefore, alternative extraction methods using solvents in the supercritical state are currently being developed (Supercritical Fluid Extraction (SFE)). Their low viscosity and the high diffusivity of solutes in the fluids allow selective, efficient and timesaving extractions. Carbon dioxide (CO 2 ) is the fluid of choice in many applications because its critical parameters permit mild operating conditions. CO 2 of high purity is available at low cost, it is neither inflammable nor explosive, physiologically harmless and part of natural cycle processes. Furthermore, it is simply removed from the matrix without any residues left. The combination of SFE and sorptive collection of the extracted substances has been found to lead to high enrichment factors for the analytes. Distillative concentration and solid phase elution steps, required in the classical solvent extraction procedure, are no longer necessary. Loss of analytes occurring in cryogenic or solvent traps is completeley avoided. Plugging of the restrictor as a consequence of the Joule Thomson effect was not observed in the presented method. (orig./vhe)

  19. Chromatographic Evaluation and Characterization of Components of Gentian Root Extract Used as Food Additives.

    Science.gov (United States)

    Amakura, Yoshiaki; Yoshimura, Morio; Morimoto, Sara; Yoshida, Takashi; Tada, Atsuko; Ito, Yusai; Yamazaki, Takeshi; Sugimoto, Naoki; Akiyama, Hiroshi

    2016-01-01

    Gentian root extract is used as a bitter food additive in Japan. We investigated the constituents of this extract to acquire the chemical data needed for standardized specifications. Fourteen known compounds were isolated in addition to a mixture of gentisin and isogentisin: anofinic acid, 2-methoxyanofinic acid, furan-2-carboxylic acid, 5-hydroxymethyl-2-furfural, 2,3-dihydroxybenzoic acid, isovitexin, gentiopicroside, loganic acid, sweroside, vanillic acid, gentisin 7-O-primeveroside, isogentisin 3-O-primeveroside, 6'-O-glucosylgentiopicroside, and swertiajaposide D. Moreover, a new compound, loganic acid 7-(2'-hydroxy-3'-O-β-D-glucopyranosyl)benzoate (1), was also isolated. HPLC was used to analyze gentiopicroside and amarogentin, defined as the main constituents of gentian root extract in the List of Existing Food Additives in Japan.

  20. 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.

  1. 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.

  2. Solid-phase extraction NMR studies of chromatographic fractions of saponins from Quillaja saponaria.

    Science.gov (United States)

    Nyberg, Nils T; Baumann, Herbert; Kenne, Lennart

    2003-01-15

    The saponin mixture QH-B from the tree Quillaja saponaria var. Molina was fractionated by RP-HPLC in several steps. The fractions were analyzed by solid-phase extraction NMR (SPE-NMR), a technique combining the workup by solid-phase extraction with on-line coupling to an NMR flow probe. Together with MALDI-TOF mass spectrometry and comparison with chemical shifts of similar saponins, the structures of both major and minor components in QH-B could be obtained. The procedure described is a simple method to determine the structure of components in a complex mixture. The two major fractions of the mixture were found to contain at least 28 saponins, differing in the carbohydrate substructures. Eight of these have not previously been determined. The 28 saponins formed 14 equilibrium pairs by the migration of an O-acyl group between two adjacent positions on a fucosyl residue.

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

    Directory of Open Access Journals (Sweden)

    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.

  4. Separation of rare earth by column chromatography using organic resins XAD/DEPHA

    International Nuclear Information System (INIS)

    Zini, J.; Ferreira, J.C.; Bergamaschi, V.S.; Santos, I.; Carvalho, F.M.S.

    2013-01-01

    The designation of light and heavy rare earth was used the fractionation used in separation processes. In this study the process of separation of rare earth, in groups, by chromatographic column consisting in fixing of cations these elements in an organic resin Amberlite XAD16 functionalized with the extracting agent DEPHA and another portion functionalized with a mixture of extractors DEPHA/TOP. The preparation of these resins was performed in two forms, one directly as the extracting agent to the resin and the other to be used in ethyl alcohol. Conditioned resins were introduced in chromatographic columns in separation of groups, light and heavy, using a standard solution of cerium nitrate and standard solution of holmium nitrate groups to represent light and heavy respectively. The characterization technique used to identify the rare earth elements was Spectrometry X-Ray Fluorescence (XRF). The results using the technique of chromatography were satisfactory, obtaining 100% separation of the elements. (author)

  5. Separation of rare earth by column chromatography using organic resins XAD/DEPHA

    Energy Technology Data Exchange (ETDEWEB)

    Zini, J.; Ferreira, J.C.; Bergamaschi, V.S.; Santos, I.; Carvalho, F.M.S., E-mail: jcferrei@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (CCCH/IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Celulas a Combustivel e Hidrogenio

    2013-07-01

    The designation of light and heavy rare earth was used the fractionation used in separation processes. In this study the process of separation of rare earth, in groups, by chromatographic column consisting in fixing of cations these elements in an organic resin Amberlite XAD16 functionalized with the extracting agent DEPHA and another portion functionalized with a mixture of extractors DEPHA/TOP. The preparation of these resins was performed in two forms, one directly as the extracting agent to the resin and the other to be used in ethyl alcohol. Conditioned resins were introduced in chromatographic columns in separation of groups, light and heavy, using a standard solution of cerium nitrate and standard solution of holmium nitrate groups to represent light and heavy respectively. The characterization technique used to identify the rare earth elements was Spectrometry X-Ray Fluorescence (XRF). The results using the technique of chromatography were satisfactory, obtaining 100% separation of the elements. (author)

  6. 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).

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

    Directory of Open Access Journals (Sweden)

    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.

  8. Automated solid-phase extraction of herbicides from water for gas chromatographic-mass spectrometric analysis

    Science.gov (United States)

    Meyer, M.T.; Mills, M.S.; Thurman, E.M.

    1993-01-01

    An automated solid-phase extraction (SPE) method was developed for the pre-concentration of chloroacetanilide and triazine herbicides, and two triazine metabolites from 100-ml water samples. Breakthrough experiments for the C18 SPE cartridge show that the two triazine metabolites are not fully retained and that increasing flow-rate decreases their retention. Standard curve r2 values of 0.998-1.000 for each compound were consistently obtained and a quantitation level of 0.05 ??g/l was achieved for each compound tested. More than 10,000 surface and ground water samples have been analyzed by this method.

  9. 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.

  10. Transplutonium elements production program: extraction chromatographic process for plutonium irradiated targets

    International Nuclear Information System (INIS)

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

    1980-01-01

    The treatment of irradiated plutonium targets by extraction chromatography allowed the purification of the isotopes 243 Am and 244 Cm on the scale of few tens of grams. This process proved to be extremely simple and flexible, and yielded results which are reproducible in time. The chief advantage of the TBP process over the HDEHP process in high and medium activity conditions lies in the rapid absorption/desorption kinetics of the elements to be purified and in the separation of americium from curium, which largely offsets its lower selectivity for lanthanide elements. it is certainly possible to improve the performance of this process by: a) optimization of the characteristics of the stationary phase, b) improvement in the filling technique and in hydraulic operation of the columns, c) on-line analysis of americium (the key element in actinide/lanthanide separation) in the eluate. The application of extraction chromatography with HD(DiBM)P to the purification of 243 Am of the end of treatment makes the process more consistent, eliminates the delicate stages implemented in hot cell, and considerably improves final product quality

  11. Disposable pipette extraction for gas chromatographic determination of codeine, morphine, and 6-monoacetylmorphine in vitreous humor.

    Science.gov (United States)

    Kovatsi, Leda; Rentifis, Konstantinos; Giannakis, Dimitrios; Njau, Samuel; Samanidou, Victoria

    2011-07-01

    The availability of a sensitive and rapid analytical method for the determination of opiates, and other substances of forensic interest, in a variety of biological specimens is of utmost importance to forensic laboratories. Solid-phase extraction is very popular in the pre-treatment of forensic samples. Nevertheless, a new approach, disposable pipette extraction (DPX), is gaining increasing interest in sample preparation. DPX has already been applied to the analysis of drugs of abuse in common biological matrices, such as urine and blood, but has not yet been evaluated on alternative biological samples, such as vitreous humor. The objective of this study was to evaluate the applicability of DPX on the analysis of opiates in vitreous humor. The currently developed method is fast, reliable, and easy to perform. The sensitivity, precision, and accuracy are satisfactory. Recoveries obtained are within the range of 72-91%, whereas the sample volume of vitreous humor required is only 100 μL. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Gas chromatographic determination of cholesterol from food samples using extraction/saponification method

    International Nuclear Information System (INIS)

    Ali, Z.M.; Soomro, A.S.A.

    2007-01-01

    A simple and fast one-step extraction/saponification with Na/OH/KOH (Ethanolic, Sodium Hydroxide/Potassium Hydroxide was compared and validated for determination of cholesterol from locally available 10 edible oil and egg samples. The importance of the use of edible oils and eggs in routine diet is unquestionable, but presence of cholesterol is considered as a risk factor for coronary heart disease and hypertension. The lowering of cholesterol level in order to reduce the risk is widely accepted. The cholesterol in the edible oil and eggs was determined by gas chromatography, through elution from the column (2x3 mm i.d) packed with 3% OV-I01, on Chromosorb G/'NAW 80-100 mesh size at 250-300C with programmed heating rate of 3 degree C/min. Nitrogen gas flow rate was 40 ml/min. The cholesterol samples were run under the conditions after selective extraction in diethyl ether. The calibration was linear within 50-500 IJg/ml concentration range. The amount of cholesterol detected were from 12.92-18.05 mg/g in edible oil and 117.54-143.42 mg/g in egg samples with RSD 1.3-2.7%. (author)

  13. 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

  14. 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.

  15. Headspace Solid Phase Micro Extraction Gas Chromatographic Determination of Fenthion in Human Serum

    Directory of Open Access Journals (Sweden)

    Kyriaki Machera

    2008-05-01

    Full Text Available A simple and effective analytical procedure was developed for the determination of fenthion residues in human serum samples. The sample treatment was performed using the headspace solid-phase micro extraction with polyacrylate fiber, which has the advantage to require low amount of serum (1 mL without tedious pre-treatment. The quantification of fenthion was carried out by gas chromatography-mass spectrometry and the recoveries ranged from 79 to 104% at two spiking levels for 6 replicates. Detection and quantification limits were calculated as 1.51 and 4.54 ng/mL of serum respectively. Two fenthion metabolites − fenoxon and fenthion–sulfoxide − were also identified.

  16. Solid-phase extraction and high-performance liquid chromatographic separation of pigments of red wines.

    Science.gov (United States)

    Csiktusnádi Kiss, G A; Forgács, E; Cserháti, T; Candeias, M; Vilas-Boas, L; Bronze, R; Spranger, I

    2000-08-11

    The adsorption and desorption capacities of 11 different solid-phase extraction sorbents were tested for the preconcenration of pigments of various Hungarian red wines. The concentrates were evaluated by multiwavelengh spectrophotometry combined with a spectral mapping technique (SPM) and by reversed-phase high-performance liquid chromatography. The highest (10-fold) concentration of pigments was achieved on octadecylsilica sorbent. It can be used five times without losing adsorption and desorption characteristics. SPM indicated that multiwavelength spectrophotometry can be employed for the differentiation of red wines. Comparison of the chromatograms of pigments with and without preconcentration showed that preconcentration makes possible the separation and detection of pigments present in low concentration in red wines.

  17. Chelating ion exchange with macroreticular hydroxamic acid resins

    International Nuclear Information System (INIS)

    Phillips, R.J.

    1980-01-01

    The synthesis, reactions, and analytical applications of hydroxamic acids, including chelating resins with this functional group, are reviewed. A procedure for attaching N-phenyl hydroxamic acid groups to Amberlite XAD-4 is described. The extraction of 20 metal ions from 2 M hydrochloric acid by this resin is discussed. Conditions for the quantitative extraction and back-extraction of 9 ions are reported. Results are compared with work on solvent extraction with N-phenylbenzohydroxamic acid. Procedures for attaching N-methyl and N-unsubstituted hydroxamic acid groups to Amberlite XAD-4 are described. The N-phenyl, N-methyl, and N-unsubstituted hydroxamic acid resins are compared with respect to metal-ion complexation. The scope of applications for hydroxamic acid resins is investigated by studying the extraction of 19 metal ions as a function of pH. The resins are especially suitable for the extraction of zirconium(IV), titanium(IV), and uranium(IV) from strongly acidic solution. Aluminum(III) is separated from calcium and phosphate by extraction at pH 4. The use of the resins for the purification of reagents, concentration of trace constituents, and chromatographic separation is demonstrated

  18. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  20. 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.

  1. 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)

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

    Directory of Open Access Journals (Sweden)

    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.

  3. 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.

  4. 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%.

  5. 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)

  6. 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

  7. 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.

  8. 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

  9. 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)

  10. 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.

  11. 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

  12. 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

  13. 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

  14. 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.

  15. 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...

  16. 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.

  17. 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.

  18. 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®

  19. 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

  20. 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.

  1. 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.

  2. 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.

  3. 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)

  4. 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)

  5. 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

  6. 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

  7. 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%.

  8. 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.

  9. Evaluation of differences between dual salt-pH gradient elution and mono gradient elution using a thermodynamic model: Simultaneous separation of six monoclonal antibody charge and size variants on preparative-scale ion exchange chromatographic resin.

    Science.gov (United States)

    Lee, Yi Feng; Jöhnck, Matthias; Frech, Christian

    2018-02-21

    The efficiencies of mono gradient elution and dual salt-pH gradient elution for separation of six mAb charge and size variants on a preparative-scale ion exchange chromatographic resin are compared in this study. Results showed that opposite dual salt-pH gradient elution with increasing pH gradient and simultaneously decreasing salt gradient is best suited for the separation of these mAb charge and size variants on Eshmuno ® CPX. Besides giving high binding capacity, this type of opposite dual salt-pH gradient also provides better resolved mAb variant peaks and lower conductivity in the elution pools compared to single pH or salt gradients. To have a mechanistic understanding of the differences in mAb variants retention behaviors of mono pH gradient, parallel dual salt-pH gradient, and opposite dual salt-pH gradient, a linear gradient elution model was used. After determining the model parameters using the linear gradient elution model, 2D plots were used to show the pH and salt dependencies of the reciprocals of distribution coefficient, equilibrium constant, and effective ionic capacity of the mAb variants in these gradient elution systems. Comparison of the 2D plots indicated that the advantage of opposite dual salt-pH gradient system with increasing pH gradient and simultaneously decreasing salt gradient is the noncontinuous increased acceleration of protein migration. Furthermore, the fitted model parameters can be used for the prediction and optimization of mAb variants separation in dual salt-pH gradient and step elution. © 2018 American Institute of Chemical Engineers Biotechnol. Prog., 2018. © 2018 American Institute of Chemical Engineers.

  10. 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.

  11. Extraction estimation and gas chromatographic mass spectrometric analysis of the non polar fraction of the pistia stratiotes

    International Nuclear Information System (INIS)

    Hussain, Z.

    2013-01-01

    The non-polar compounds of the Pistia stratiotes were extracted using n-hexane as solvent. The extraction yields were determined both for the cold and hot extraction procedure as 8.50 +- 0.05% and 12.00 +- 0.05%, respectively. The extract was analyzed and separated into its components using GC equipped with FID and GC mass in separate experiments. The most important compounds identified in n-hexane extract of leaves of P. stratiotes are long chain compound of the nitrogenous nature and oxygenated compounds of mixed functional groups. The antibacterial activity of this fraction was investigated against eight pathogenic bacteria using disc diffusion method. Larger zones of inhibition were observed for Bacillus subtilis, Pseudomonas aeruginosa and Agrobacterium tumefaciens as compared to Klebsiella pneumoniaee and Staphylococcus aureus where the activity was relatively less. No activity was observed against Escherichia coli, Salmonella typhi and Bacillus atrophaeus. (author)

  12. Supercritical fluid extraction and chromatographic analysis (HRGC-FID and HRGC-MS of Lupinus spp. alkaloids

    Directory of Open Access Journals (Sweden)

    Nossack Ana C.

    2000-01-01

    Full Text Available The alkaloid extracts from Lupinus spp., obtained by conventional methods (maceration/sonication - solid phase extraction; maceration/sonication - liquid-liquid extraction and SFE (supercritical fluid extraction using CO2 and modified CO2 (CO2/MeOH, CO2/EtOH, CO2/iPrOH and CO2/H2O were analysed by HRGC-FID (high resolution gas chromatography - flame ionization detector and HRGC-MS (high resolution gas chromatography - mass spectrometry. The HRGC-FID quantitative analyses were performed with an internal standard method for quantification of lupanine, multiflorine and a spartein-like alkaloid. HRGC-MS allowed identification of the chemical constituents (alkaloids and other compounds from these extracts.

  13. Automated chromatographic system with polarimetric detection laser applied in the control of fermentation processes and seaweed extracts characterization

    International Nuclear Information System (INIS)

    Fajer, V.; Naranjo, S.; Mora, W.; Patinno, R.; Coba, E.; Michelena, G.

    2012-01-01

    There are presented applications and innovations of chromatographic and polarimetric systems in which develop methodologies for measuring the input molasses and the resulting product of a fermentation process of alcohol from a rich honey and evaluation of the fermentation process honey servery in obtaining a drink native to the Yucatan region. Composition was assessed optically active substances in seaweed, of interest to the pharmaceutical industry. The findings provide measurements alternative raw materials and products of the sugar industry, beekeeping and pharmaceutical liquid chromatography with automated polarimetric detection reduces measurement times up to 15 min, making it comparable to the times of high chromatography resolution, significantly reducing operating costs. By chromatography system with polarimetric detection (SCDP) is new columns have included standard size designed by the authors, which allow process samples with volumes up to 1 ml and reduce measurement time to 15 min, decreasing to 5 times the volume sample and halving the time of measurement. Was evaluated determining the concentration of substances using the peaks of the chromatograms obtained for the different columns and calculate the uncertainty of measurements. The results relating to the improvement of a data acquisition program (ADQUIPOL v.2.0) and new programs for the preparation of chromatograms (CROMAPOL CROMAPOL V.1.0 and V.1.2) provide important benefits, which allow a considerable saving of time the processing of the results and can be applied in other chromatography systems with the appropriate adjustments. (Author)

  14. 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.)

  15. Chromatographic methods

    International Nuclear Information System (INIS)

    Marhol, M.; Stary, J.

    1975-01-01

    The characteristics are given of chromatographic separation and the methods are listed. Methods and data on materials used in partition, adsorption, precipitation and ion exchange chromatography are listed and conditions are described under which ion partition takes place. Special attention is devoted to ion exchange chromatography where tables are given to show the course of values of the partition coefficients of different ions in dependence on the concentration of agents and the course of equilibrium sorptions on different materials in dependence on the solution pH. A theoretical analysis is given and the properties of the most widely used ion exchangers are listed. Experimental conditions and apparatus used for each type of chromatography are listed. (L.K.)

  16. 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.

  17. New and highly efficient column chromatographic extraction and simple purification of camptothecin from Camptotheca acuminata and Nothapodytes pittosporoides.

    Science.gov (United States)

    Zeng, Xue-Hua; Li, Yue-Hong; Wu, Shan-Shan; Hao, Rui-Lin; Li, Hui; Ni, He; Han, Han-Bing; Li, Hai-Hang

    2013-01-01

    Camptothecin, a widely used natural anti-cancer drug, is difficult to extract and purify effectively from plants. To develop new and highly efficient extraction and purification methods for analysis and production of camptothecin from leaves and fruits of Camptotheca acuminata and Nothapodytes pittosporoides roots. Dried materials were loaded in empty columns with fivefold 60% ethanol for leaves or 70% ethanol for fruits of C. acumnata, and sixfold 70% ethanol for N. pittosporoides roots. The columns were eluted with the same solvents at room temperature. Eluent was collected as extraction solution. Extraction solution from leaves and fruits of C. acuminata was vacuum-evaporated to remove ethanol, precipitated at pH 8.0 to remove alkaline insolubles and fractionated with chloroform at pH 3.0, which yields a crude product with 70% purity. Extraction solution from N. pittosporoides roots was concentrated to 1/10 volume and precipitated at pH 3.0, which yields a crude product with 60% purity. All crude products were purified by crystallisation. All steps were monitored by HPLC. Camptothecin was extracted from the three plant materials at a 98% rate with 15- or 18-fold solvent for content analysis, or at a 97% rate with five- or sixfold solvent for production. All crude products were purified to 98%. The overall recovery rates of camptothecin from plant materials to purified products reached 92% or higher. The new procedures are simple and highly efficient, and have multiple advantages for quantitative analysis and large production of camptothecin from plants. Copyright © 2013 John Wiley & Sons, Ltd.

  18. Chromatographic fingerprinting and free-radical scavenging activity of ethanol extracts of Muntingia calabura L. leaves and stems

    Directory of Open Access Journals (Sweden)

    William Patrick Cruiz Buhian

    2017-02-01

    Conclusions: M. calabura exhibited very high antioxidant activity in its leaves and stems ethanol extracts, both of which are used in traditional medicine. The TLC results demonstrated the presence of diverse secondary metabolites in the leaf and stem ethanol extracts, indicating that the antioxidant activity, including other bioactivities may be attributed to these phytochemical constituents. This paper has reported for the first time the TLC fingerprinting of M. calabura using visible light, UV 254 nm, UV 366 and post-derivatization with vanillin-spray to visualize separate spots on TLC plates.

  19. 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)

  20. Hyphenated chromatographic techniques for the rapid screening and identification of antioxidants in methanolic extracts of pharmaceutically used plants .

    NARCIS (Netherlands)

    Exarchou, V.; Fiamegos, Y.C.; Beek, van T.A.; Nanos, C.G.; Vervoort, J.J.M.

    2006-01-01

    Phytochemical analysis is an important scientific research area, which normally relies on a number of rather laborious and time-consuming techniques for compound identification. Isolation of the ingredients of plant extracts in adequate quantities for spectral and biological analysis was the basis

  1. Validated high-performance liquid chromatographic method for the standardisation of Ptychopetalum olacoides Benth., Olacaceae, commercial extracts

    Directory of Open Access Journals (Sweden)

    Renata Colombo

    2010-10-01

    Full Text Available Ptychopetalum olacoides Benth., Olacaceae, popularly known as marapuama or muirapuama or miriantã, is a species native to the Amazonian region of Brazil. Extracts of the bark of the plant have been used traditionally for its stimulating and aphrodisiac properties and currently commercialised by the herbal industry as constituents in a wide range of phytomedicines. Fractionation by open column chromatography followed by preparative HPLC-UV/PAD of the stem bark and of three commercial extracts of P. olacoides allowed the isolation of three components that were common to all extracts analysed, and these were identified by NMR to be vanillic acid, protocatechuic acid and theobromine. Vanillic acid, which has been proposed as a phytochemical marker for P. olacoides, was employed as an external standard in the development and validation of a rapid qualitative and quantitative HPLC assay for the analyte. The recoveries values of the developed method were 99.02% and the LOD and LOQ values were 0.033 and 0.11 mg.L-1, respectively. The described method may be applied to the standardisation of herbs, extracts or phytomedicines commercialised as marapuama.

  2. Chromatographic finger print analysis of anti-inflammatory active extract fractions of aerial parts of Tribulus terrestris by HPTLC technique

    Science.gov (United States)

    Mohammed, Mona Salih; Alajmi, Mohamed Fahad; Alam, Perwez; Khalid, Hassan Subki; Mahmoud, Abelkhalig Muddathir; Ahmed, Wadah Jamal

    2014-01-01

    Objective To develop HPTLC fingerprint profile of anti-inflammatory active extract fractions of Tribulus terrestris (family Zygophyllaceae). Methods The anti-inflammatory activity was tested for the methanol and its fractions (chloroform, ethyl acetate, n-butanol and aqueous) and chloroform extract of Tribulus terrestris (aerial parts) by injecting different groups of rats (6 each) with carrageenan in hind paw and measuring the edema volume before and 1, 2 and 3 h after carrageenan injection. Control group received saline i.p. The extracts treatment was injected i.p. in doses of 200 mg/kg 1 h before carrageenan administration. Indomethacin (30 mg/kg) was used as standard. HPTLC studies were carried out using CAMAG HPTLC system equipped with Linomat IV applicator, TLC scanner 3, Reprostar 3, CAMAG ADC 2 and WIN CATS-4 software for the active fractions of chloroform fraction of methanol extract. Results The methanol extract showed good antiedematous effect with percentage of inhibition more than 72%, indicating its ability to inhibit the inflammatory mediators. The methanol extract was re-dissolved in 100 mL of distilled water and fractionated with chloroform, ethyl acetate and n-butanol. The four fractions (chloroform, ethyl acetate, n-butanol and aqueous) were subjected to anti-inflammatory activity. Chloroform fraction showed good anti-inflammatory activity at dose of 200 mg/kg. Chloroform fraction was then subjected to normal phase silica gel column chromatography and eluted with petroleum ether-chloroform, chloroform-ethyl acetate mixtures of increasing polarity which produced 15 fractions (F1-F15). Only fractions F1, F2, F4, F5, F7, F9, F11 and F14 were found to be active, hence these were analyzed with HPTLC to develop their finger print profile. These fractions showed different spots with different Rf values. Conclusions The different chloroform fractions F1, F2, F4, F5, F7, F9, F11 and F14 revealed 4, 7, 7, 8, 9, 7, 7 and 6 major spots, respectively. The

  3. Chromatographic finger print analysis of anti-inflammatory active extract fractions of aerial parts of Tribulus terrestris by HPTLC technique.

    Science.gov (United States)

    Mohammed, Mona Salih; Alajmi, Mohamed Fahad; Alam, Perwez; Khalid, Hassan Subki; Mahmoud, Abelkhalig Muddathir; Ahmed, Wadah Jamal

    2014-03-01

    To develop HPTLC fingerprint profile of anti-inflammatory active extract fractions of Tribulus terrestris (family Zygophyllaceae). The anti-inflammatory activity was tested for the methanol and its fractions (chloroform, ethyl acetate, n-butanol and aqueous) and chloroform extract of Tribulus terrestris (aerial parts) by injecting different groups of rats (6 each) with carrageenan in hind paw and measuring the edema volume before and 1, 2 and 3 h after carrageenan injection. Control group received saline i.p. The extracts treatment was injected i.p. in doses of 200 mg/kg 1 h before carrageenan administration. Indomethacin (30 mg/kg) was used as standard. HPTLC studies were carried out using CAMAG HPTLC system equipped with Linomat IV applicator, TLC scanner 3, Reprostar 3, CAMAG ADC 2 and WIN CATS-4 software for the active fractions of chloroform fraction of methanol extract. The methanol extract showed good antiedematous effect with percentage of inhibition more than 72%, indicating its ability to inhibit the inflammatory mediators. The methanol extract was re-dissolved in 100 mL of distilled water and fractionated with chloroform, ethyl acetate and n-butanol. The four fractions (chloroform, ethyl acetate, n-butanol and aqueous) were subjected to anti-inflammatory activity. Chloroform fraction showed good anti-inflammatory activity at dose of 200 mg/kg. Chloroform fraction was then subjected to normal phase silica gel column chromatography and eluted with petroleum ether-chloroform, chloroform-ethyl acetate mixtures of increasing polarity which produced 15 fractions (F1-F15). Only fractions F1, F2, F4, F5, F7, F9, F11 and F14 were found to be active, hence these were analyzed with HPTLC to develop their finger print profile. These fractions showed different spots with different Rf values. The different chloroform fractions F1, F2, F4, F5, F7, F9, F11 and F14 revealed 4, 7, 7, 8, 9, 7, 7 and 6 major spots, respectively. The results obtained in this experiment

  4. 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.

  5. 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...

  6. Hydro-alcoholic Extract of Commiphora mukul Gum Resin May Improve Cognitive Impairments in Diabetic Rats

    Directory of Open Access Journals (Sweden)

    Salehi

    2015-02-01

    Full Text Available Background Diabetes causes cognitive impairment. Medicinal plants due to different mechanisms, such as antioxidant activities may improve diabetes and relieve its symptoms. Commiphora mukul (Burseraceae has a significant antioxidant activity. Objectives This study aimed to examine the effect of hydro- alcoholic extract of C. mukul on passive-avoidance learning and memory in streptozotocin (STZ induced diabetic male rats. Materials and Methods Thirty-two adult male Wistar rats were randomly allocated to four groups: normal, diabetic, normal + extract of C. mukul and diabetic + extract of C. mukul groups with free access to regular rat diet. Diabetes was induced in male rats by single interaperitoneal injection of 60 mg/kg STZ. After the confirmation of diabetes, 300 mg/kg C. mukul extract was orally administered to the extract-treated groups. Control groups received normal saline at the same time. Passive-avoidance memory was tested eight weeks after the STZ treatment, and blood glucose and body weight were measured in all groups at the beginning and end of the experiment. Results In the present study, diabetes decreased learning and memory. Although the administration of C. mukul extract did not affect the step-through latency (STLa and the number of trials of the diabetic groups during the first acquisition trial, a significant decrease was observed in STLr and also a significant increase in time spent in the dark compartment (TDC and number of crossing (NOC in the retention test (after 24 and 48 hours. Although no significant difference was observed in body weight of diabetic + extract of C. mukul (DE and diabetic control (DC groups, the plasma glucose of DE group was significantly lower in comparison to DC group. Conclusions Commiphora mukul extract can improve passive-avoidance learning and memory impairments in the STZ-induced diabetic rats. This improvement may be due to the antioxidant, acetylcholinesterase inhibitory activity, anti

  7. Radioimmunoassay of three oestrogens and three androgens in the same plasma sample after extraction and chromatographic separation

    International Nuclear Information System (INIS)

    Paradisi, R.; Lodi, S.; Bolelli, G.; Venturoli, S.

    1980-01-01

    The plasma levels of oestrone (Oe 1 ), 17β-oestradiol (Oe 2 ), oestriol (Oe 3 ), testosterone (T), 5α-dihydrotestosterone (DHT) and androstenedione (A) were assayed by radioimmunoassay (RIA) in plasma obtained from peripheral venous blood. The hormones are isolated from the plasma extract, first by Sephadex LH-20 column chromatography (Oe 2 /Oe 3 /Oe 1 , T, DHT, A) and after Oe 1 , T, DHT, A by thin layer chromatography (TLC) on silica gel 60 F 254 . The accuracy, reproducibility and sensitivity of the method make it satisfactory for clinical studies. (author)

  8. 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.

  9. Anticholinesterase activity and chemical profile of an active chromatographic fraction of ethanolic extract from Bellis perennis L. (Asteraceae) flowers

    International Nuclear Information System (INIS)

    Marques, Thiago Henrique Costa; Santos, Pauline Sousa dos; Freitas, Rivelilson Mendes de; Carvalho, Rusbene Bruno Fonseca de; Melo, Cassio Herbert Santos de; David, Juceni Pereira; David, Jorge Mauricio; Lima, Luciano Silva

    2013-01-01

    This work describes the isolation of an active flavonoid fraction and identification of isorhamnetin 3-O-β-D-(6’’-acetyl)- alactopyranoside from flowers of B. perennis, and also the evaluation of anticholinesterase (AChE) activity of ethanolic extract from flowers (EEF) and the active fraction. The chemical structure of the flavonoid was defined on the basis of spectroscopic 1 H NMR, IR and UV data. EEF or flavonoid reduces AChE activity in vivo, while flavonoid also reduces AChE activity in vitro, showing a value of 1.49 μM for 50% inhibitory concentration (IC 50 ), suggesting potential use as an insecticide or in the treatment of neurodegenerative diseases such as Alzheimer’s disease. (author)

  10. Multiwalled carbon nanotubes as solid-phase extraction materials for the gas chromatographic determination of organophosphorus pesticides in waters.

    Science.gov (United States)

    Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Angel Rodríguez-Delgado, Miguel

    2008-10-01

    In the present work, a GC method with nitrogen-phosphorus detection (NPD) was developed for the simultaneous determination of eight organophosphorus pesticide (OPP) residues (i.e., ethoprofos, diazinon, chlorpyrifos-methyl, fenitrothion, malathion, chlorpyrifos, fenamiphos, and buprofezin) in water samples. Preconcentration of the water samples was carried out using an SPE procedure with multiwalled carbon nanotubes (MWCNTs) of 10-15 nm od, 2-6 nm id, and 0.1-10 microm length as stationary phase. Extraction parameters, such as the amount of MWCNTs, sample volume, pH, and type and amount of the eluent were optimized. The most favorable conditions were as follows: 40 mg MWCNTs, 800 mL water, pH 6.0, and 20 mL dichloromethane, respectively. The MWCNTs-SPE-GC-NPD method was applied to the determination of these pesticides in real water samples: mineral and ground water as well as run-off water from an agricultural area collected shortly before opening out onto the sea. A recovery study was developed with five consecutive extractions of the three types of water spiked at three concentration levels (n = 15). Mean recovery values were in the range of 75-116% for mineral water (RSD water (RSD waters (RSDs waters, RSDs waters). The proposed method was also applied to the analysis of six water samples (two of each type: mineral, ground, and run-off waters) in which no residues of the selected pesticides were found. Results show that the MWCNTs used in this work have a high adsorbability of the pesticides under study. The main advantage of the use of these MWCNTs is their low cost when compared with those MWCNTs previously used in the literature and with conventional SPE cartridges.

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

    Directory of Open Access Journals (Sweden)

    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.

  12. Pesticide residues in canned foods, fruits, and vegetables: the application of Supercritical Fluid Extraction and chromatographic techniques in the analysis.

    Science.gov (United States)

    El-Saeid, Mohamed H

    2003-12-11

    Multiple pesticide residues have been observed in some samples of canned foods, frozen vegetables, and fruit jam, which put the health of the consumers at risk of adverse effects. It is quite apparent that such a state of affairs calls for the need of more accurate, cost-effective, and rapid analytical techniques capable of detecting the minimum concentrations of the multiple pesticide residues. The aims of this paper were first, to determine the effectiveness of the use of Supercritical Fluid Extraction (SFE) and Supercritical Fluid Chromatography (SFC) techniques in the analysis of the levels of pesticide residues in canned foods, vegetables, and fruits; and second, to contribute to the promotion of consumer safety by excluding pesticide residue contamination from markets. Fifteen different types of imported canned and frozen fruits and vegetables samples obtained from the Houston local food markets were investigated. The major types of pesticides tested were pyrethroids, herbicides, fungicides, and carbamates. By using these techniques, the overall data showed 60.82% of the food samples had no detection of any pesticide residues under this investigation. On the other hand, 39.15% different food samples were contaminated by four different pyrethroid residues +/- RSD% ranging from 0.03 +/- 0.005 to 0.05 +/- 0.03 ppm, of which most of the pyrethroid residues were detected in frozen vegetables and strawberry jam. Herbicide residues in test samples ranged from 0.03 +/- 0.005 to 0.8 +/- 0.01 ppm. Five different fungicides, ranging from 0.05 +/- 0.02 to 0.8 +/- 0.1 ppm, were found in five different frozen vegetable samples. Carbamate residues were not detected in 60% of investigated food samples. It was concluded that SFE and SFC techniques were accurate, reliable, less time consuming, and cost effective in the analysis of imported canned foods, fruits, and vegetables and are recommended for the monitoring of pesticide contaminations.

  13. Pesticide Residues in Canned Foods, Fruits, and Vegetables: The Application of Supercritical Fluid Extraction and Chromatographic Techniques in the Analysis

    Directory of Open Access Journals (Sweden)

    Mohamed H. EL-Saeid

    2003-01-01

    Full Text Available Multiple pesticide residues have been observed in some samples of canned foods, frozen vegetables, and fruit jam, which put the health of the consumers at risk of adverse effects. It is quite apparent that such a state of affairs calls for the need of more accurate, cost-effective, and rapid analytical techniques capable of detecting the minimum concentrations of the multiple pesticide residues. The aims of this paper were first, to determine the effectiveness of the use of Supercritical Fluid Extraction (SFE and Supercritical Fluid Chromatography (SFC techniques in the analysis of the levels of pesticide residues in canned foods, vegetables, and fruits; and second, to contribute to the promotion of consumer safety by excluding pesticide residue contamination from markets. Fifteen different types of imported canned and frozen fruits and vegetables samples obtained from the Houston local food markets were investigated. The major types of pesticides tested were pyrethroids, herbicides, fungicides, and carbamates.By using these techniques, the overall data showed 60.82% of the food samples had no detection of any pesticide residues under this investigation. On the other hand, 39.15% different food samples were contaminated by four different pyrethroid residues ± RSD% ranging from 0.03 ± 0.005 to 0.05 ± 0.03 ppm, of which most of the pyrethroid residues were detected in frozen vegetables and strawberry jam. Herbicide residues in test samples ranged from 0.03 ± 0.005 to 0.8 ± 0.01 ppm. Five different fungicides, ranging from 0.05 ± 0.02 to 0.8 ±0.1 ppm, were found in five different frozen vegetable samples. Carbamate residues were not detected in 60% of investigated food samples. It was concluded that SFE and SFC techniques were accurate, reliable, less time consuming, and cost effective in the analysis of imported canned foods, fruits, and vegetables and are recommended for the monitoring of pesticide contaminations.

  14. 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.

  15. Chromatographic and Spectral Analysis of Two Main Extractable Compounds Present in Aqueous Extracts of Laminated Aluminum Foil Used for Protecting LDPE-Filled Drug Vials

    Science.gov (United States)

    Akapo, Samuel O.; Syed, Sajid; Mamangun, Anicia; Skinner, Wayne

    2009-01-01

    Laminated aluminum foils are increasingly being used to protect drug products packaged in semipermeable containers (e.g., low-density polyethylene (LDPE)) from degradation and/or evaporation. The direct contact of such materials with primary packaging containers may potentially lead to adulteration of the drug product by extractable or leachable compounds present in the closure system. In this paper, we described a simple and reliable HPLC method for analysis of an aqueous extract of laminated aluminum foil overwrap used for packaging LDPE vials filled with aqueous pharmaceutical formulations. By means of combined HPLC-UV, GC/MS, LC/MS/MS, and NMR spectroscopy, the two major compounds detected in the aqueous extracts of the representative commercial overwraps were identified as cyclic oligomers with molecular weights of 452 and 472 and are possibly formed from poly-condensation of the adhesive components, namely, isophthalic acid, adipic acid, and diethylene glycol. Lower molecular weight compounds that might be associated with the “building blocks” of these compounds were not detected in the aqueous extracts. PMID:20140083

  16. 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.

  17. 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.

  18. 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.

  19. A rapid, solid phase extraction (SPE technique for the extraction and gas chromatographic determination lindane pesticide residue in tissue and milk

    Directory of Open Access Journals (Sweden)

    Yuningsih

    2006-03-01

    Full Text Available Organochlorine pesticide contamination in feed can cause residue in animal product (tissue and milk, so its become a problem in food safety. Solid phase extraction (SPE has been carried out for determination organochlorine pesticide residues in food animal production. The technique was rapid, not costly and produce limited amount of hazardous-waste. Samples were homogenized with acetonitrile trough cartridge C18, eluted in fluorocyl column with 2% ether-petroleum or acetonitrile fortissue and milk samples respectively. The recoveries of tissue sample by addition lindane standard solution: 0.50 and 1.00 μg are 85.10 and 103.10% respectively, while that of milk with the addition of 0.50, 1.00 and 1.50 μg are 83.80, 88.69 and 91.24% respectively. Three replicates were carried out for every sample. According of validation criteria of FAO/IAEA the recovery for analysis of pesticide residues was 70-110%. Therefore, the method is applicable.

  20. 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

  1. 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

  2. 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

  3. 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)

  4. 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.

  5. 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...

  6. 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.

  7. 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.

  8. 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.

  9. 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

  10. 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

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. Automation of radiochemical analysis by flow injection techniques. Am-Pu separation using TRU-resinTM sorbent extraction column

    International Nuclear Information System (INIS)

    Egorov, O.; Washington Univ., Seattle, WA; Grate, J.W.; Ruzicka, J.

    1998-01-01

    A rapid automated flow injection analysis (FIA) procedure was developed for efficient separation of Am and Pu from each other and from interfering matrix and radionuclide components using a TRU-resin TM column. Selective Pu elution is enabled via on-column reduction. The separation was developed using on-line radioactivity detection. After the separation had been developed, fraction collection was used to obtain the separated fractions. In this manner, a FIA instrument functions as an automated separation workstation capable of unattended operation. (author)

  16. 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.)

  17. [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.

  18. 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.

  19. 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.

  20. 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.

  1. 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

  2. Validated liquid chromatographic method and analysis of content of tilianin on several extracts obtained from Agastache mexicana and its correlation with vasorelaxant effect.

    Science.gov (United States)

    Hernández-Abreu, Oswaldo; Durán-Gómez, Liliana; Best-Brown, Roberto; Villalobos-Molina, Rafael; Rivera-Leyva, Julio; Estrada-Soto, Samuel

    2011-11-18

    To optimize the obtention of tilianin, an antihypertensive flavonoid isolated from Agastache mexicana (Lamiaceae), a medicinal plant used in Mexico for the treatment of hypertension. Also, a validated HPLC method to quantify tilianin from different extracts, obtained by several extraction methods, was developed. The aerial parts of Agastache mexicana were dried at different temperatures (22, 40, 50, 90, 100 and 180°C) and the dry material was extracted with methanol by maceration to compare the content of the active constituent tilianin in the samples. Furthermore, EtOH:H(2)O (7:3), infusion and decoction extracts were prepared from air-dried samples at room temperature to compare the content and composition of the different extraction methods. Moreover, an ex vivo vasorelaxant test on endothelium-intact aortic rat rings was conducted, in order to correlate the presence of tilianin with the activity of each extract. Higher concentration and amounts of tilianin were determined from chromatograms in the obtained methanolic extracts from plant material dried at 90, 50, 40 and 22°C, followed by 100°C; however, lower concentrations were observed in dried at 180°C and EtOH:H(2)O (7:3). It is worth to notice that methanolic extracts with higher amount of tilianin were the most potent vasorelaxant extracts, even though these extracts were less potent than carbachol, a positive control used. Finally, decoction, infusion and EtOH:H(2)O (7:3) extracts did not show any vasorelaxant effect. Results suggest that extracts with higher concentration of tilianin possess the best vasorelaxant activity, which allowed us to have a HPLC method for future quality control for this medicinal plant. Copyright © 2011 Elsevier Ireland Ltd. All rights reserved.

  3. Determination of strontium-90 from direct separation of yttrium-90 by solid phase extraction using DGA Resin for seawater monitoring.

    Science.gov (United States)

    Tazoe, Hirofumi; Obata, Hajime; Yamagata, Takeyasu; Karube, Zin'ichi; Nagai, Hisao; Yamada, Masatoshi

    2016-05-15

    It is important for public safety to monitor strontium-90 in aquatic environments in the vicinity of nuclear related facilities. Strontium-90 concentrations in seawater exceeding the background level have been observed in accidents of nuclear facilities. However, the analytical procedure for measuring strontium-90 in seawater is highly demanding. Here we show a simple and high throughput analytical technique for the determination of strontium-90 in seawater samples using a direct yttrium-90 separation. The DGA Resin is used to determine the abundance of strontium-90 by detecting yttrium-90 decay (beta-emission) in secular equilibrium. The DGA Resin can selectively collect yttrium-90 and remove naturally occurring radionuclides such as (40)K, (210)Pb, (214)Bi, (238)U, and (232)Th and anthropogenic radionuclides such as (140)Ba, and (140)La. Through a sample separation procedure, a high chemical yield of yttrium-90 was achieved at 95.5±2.3%. The result of IAEA-443 certified seawater analysis (107.7±3.4 mBq kg(-1)) was in good agreement with the certified value (110±5 mBq kg(-1)). By developed method, we can finish analyzing 8 samples per day after achieving secular equilibrium, which is a reasonably fast throughput in actual seawater monitoring. By processing 3 L of seawater sample and applying a counting time of 20 h, minimum detectable activity can be as low as 1.5 mBq kg(-1), which could be applied to monitoring for the contaminated marine environment. Reproducibility was found to be 3.4% according to 10 independent analyses of natural seawater samples from the vicinity of the Fukushima Daiichi Nuclear Power Plant in September 2013. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. The basic characteristics of TRPO-GDX-301 resin extraction chromatography and its application in analysis of uranium ore

    International Nuclear Information System (INIS)

    Jin Wenlong; Yao Mingxia.

    1986-01-01

    The basic characteristic, including capacity of column, loading quality of extraction agent, relationship between flow-rate of solution and height of theorical tower plate, leakage of extraction agent, separation behavior of uranium, of TRPO-extraction chromatography for separation of uranium has been inveistigated. The microamount of uranium on column can be eluted with mixed complex solution at pH 5.8-6.2 and determined by 5-Br-PADAP spectrophotometry. The method is simple and easy to operate. It has reasonable precision and accuracy. It is very suitable for determination of 0.002-0.4% uranium in ore

  5. Total milk fat extraction and quantification of polar and neutral lipids of cow, goat, and ewe milk by using a pressurized liquid system and chromatographic techniques.

    Science.gov (United States)

    Castro-Gómez, M P; Rodriguez-Alcalá, L M; Calvo, M V; Romero, J; Mendiola, J A; Ibañez, E; Fontecha, J

    2014-11-01

    Although milk polar lipids such as phospholipids and sphingolipids located in the milk fat globule membrane constitute 0.1 to 1% of the total milk fat, those lipid fractions are gaining increasing interest because of their potential beneficial effects on human health and technological properties. In this context, the accurate quantification of the milk polar lipids is crucial for comparison of different milk species, products, or dairy treatments. Although the official International Organization for Standardization-International Dairy Federation method for milk lipid extraction gives satisfactory results for neutral lipids, it has important disadvantages in terms of polar lipid losses. Other methods using mixtures of solvents such as chloroform:methanol are highly efficient for extracting polar lipids but are also associated with low sample throughput, long time, and large solvent consumption. As an alternative, we have optimized the milk fat extraction yield by using a pressurized liquid extraction (PLE) method at different temperatures and times in comparison with those traditional lipid extraction procedures using 2:1 chloroform:methanol as a mixture of solvents. Comparison of classical extraction methods with the developed PLE procedure were carried out using raw whole milk from different species (cows, ewes, and goats) and considering fat yield, fatty acid methyl ester composition, triacylglyceride species, cholesterol content, and lipid class compositions, with special attention to polar lipids such as phospholipids and sphingolipids. The developed PLE procedure was validated for milk fat extraction and the results show that this method performs a complete or close to complete extraction of all lipid classes and in less time than the official and Folch methods. In conclusion, the PLE method optimized in this study could be an alternative to carry out milk fat extraction as a routine method. Copyright © 2014 American Dairy Science Association. Published by

  6. 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

  7. 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

  8. Acaricidal activity of ethanolic extracts of Stryphnodendron adstringens and Lafoensia pacari and oil resins from Copaifera sp. and Pterodon emarginatus against Sarcoptes scabiei var. suis

    Directory of Open Access Journals (Sweden)

    Adriana Marques Faria

    Full Text Available ABSTRACT: In vitro bioassay using Sarcoptes scabiei as a test microorganism is a viable method of study for diverse drugs with acaricidal properties. A great amount of assays proves the diverse and efficient biological activity of extracts and compounds from Brazilian savanna plants. This study had as main object, test and compare the acaricidal activity of four Brazilian Cerrado bioproducts: Stryphnodendron adstringens Mart., Copaifera sp., Lafoensia pacari A. St Hil. and Pterodon emarginatus Vogel, 1837. To perform this test S. scabiei mites were collected from crusts removed on ears of highly infected sows. The mites were selected and separated in Petri dishes with three different concentrations (25, 50 and 75% of each bioproduct, to evaluate their potential acaricidal activity. The mortality of the mites was counted in each Petri dish every hour, during five hours. The statistical analyses demonstrated differences between the bioproducts tested. The oleoresin of Copaifera sp. and P. emarginatus presented the best results with 100% of mites mortality after treatment. The ethanolic extracts of S. adstringens and L. pacari demonstrated lower acaricidal activity when compared to the oleoresins, with little or no difference among the control groups tested. This bioassay demonstrated to be efficient, reliable, low cost and easy accomplishment. Oil resins from Copaifera sp. and P. emarginatus have in vitro acaricidal activity against adult females of S. scabiei var. suis.

  9. 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.

  10. Liquid-liquid and solid-phase extractions of phenols from virgin olive oil and their separation by chromatographic and electrophoretic methods.

    Science.gov (United States)

    Bendini, Alessandra; Bonoli, Matteo; Cerretani, Lorenzo; Biguzzi, Barbara; Lercker, Giovanni; Toschi, Tullia Gallina

    2003-01-24

    The high oxidative stability of virgin olive oil is related to its high monounsaturated/polyunsaturated ratio and to the presence of antioxidant compounds, such as tocopherols and phenols. In this paper, the isolation of phenolic compounds from virgin olive oil, by different methods, was tested and discussed. Particularly liquid-liquid and solid-phase extraction methods were compared, assaying, for the latter, three stationary phases (C8, C18 and Diol) and several elution mixtures. Quantification of phenolic and o-diphenolic substances in the extracts was performed by the traditional Folin-Ciocalteau method and the sodium molybdate reaction, respectively. Furthermore, the quantification of phenolic compounds in the extracts and in a standard mixture was carried out both with diode array and mass spectrometric detection and capillary zone electrophoresis.

  11. Sensitive determination of estrogens in environmental waters treated with polymeric ionic liquid-based stir cake sorptive extraction and liquid chromatographic analysis.

    Science.gov (United States)

    Chen, Lei; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

    2016-05-15

    A simple, sensitive and environmentally friendly method using polymeric ionic liquid-based stir cake sorptive extraction followed by high performance liquid chromatography with diode array detection (HPLC/DAD) has been developed for efficient quantification of six selected estrogens in environmental waters. To extract trace estrogens effectively, a poly (1-ally-3-vinylimidazolium chloride-co-ethylene dimethacrylate) monolithic cake was prepared and used as the sorbent of stir cake sorptive extraction (SCSE). The effects of preparation conditions of sorbent and extraction parameters of SCSE for estrogens were investigated and optimized. Under optimal conditions, the developed method showed satisfactory analytical performance for targeted analytes. Low limits of detection (S/N=3) and quantification limits (S/N=10) were achieved within the range of 0.024-0.057 µg/L and 0.08-0.19 µg/L, respectively. Good linearity of method was obtained for analytes with the correlation coefficients (R(2)) above 0.99. At the same time, satisfactory method repeatability and reproducibility was achieved in terms of intra- and inter-day precisions, respectively. Finally, the established SCSE-HPLC/DAD method was successfully applied for the determination of estrogens in different environmental water samples. Recoveries obtained for the determination of estrogens in spiked samples ranged from 71.2% to 108%, with RSDs below 10% in all cases. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. 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.

  13. 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.

  14. Extraction of domoic acid from seawater and urine using a resin based on 2-(trifluoromethyl)acrylic acid.

    Science.gov (United States)

    Piletska, Elena V; Villoslada, Fernando Navarro; Chianella, Iva; Bossi, Alessandra; Karim, Kal; Whitcombe, Michael J; Piletsky, Sergey A; Doucette, Gregory J; Ramsdell, John S

    2008-03-03

    A new solid-phase extraction (SPE) matrix with high affinity for the neurotoxin domoic acid (DA) was designed and tested. A computational modelling study led to the selection of 2-(trifluoromethyl)acrylic acid (TFMAA) as a functional monomer capable of imparting affinity towards domoic acid. Polymeric adsorbents containing TFMAA were synthesised and tested in high ionic strength solutions such as urine and seawater. The TFMAA-based polymers demonstrated excellent performance in solid-phase extraction of domoic acid, retaining the toxin while salts and other interfering compounds such as aspartic and glutamic acids were removed by washing and selective elution. It was shown that the TFMAA-based polymer provided the level of purification of domoic acid from urine and seawater acceptable for its quantification by high performance liquid chromatography-mass spectrometry (HPLC-MS) and enzyme-linked immunosorbent assay (ELISA) without any additional pre-concentration and purification steps.

  15. Validated determination of losartan and valsartan in human plasma by stir bar sorptive extraction based on acrylate monolithic polymer, liquid chromatographic analysis and experimental design methodology.

    Science.gov (United States)

    Babarahimi, Vida; Talebpour, Zahra; Haghighi, Farideh; Adib, Nuoshin; Vahidi, Hamed

    2018-05-10

    In our previous work, a new monolithic coating based on vinylpyrrolidone-ethylene glycol dimethacrylate polymer was introduced for stir bar sorptive extraction. The formulation of the prepared vinylpyrrolidone-ethylene glycol dimethacrylate monolithic polymer was optimized and the satisfactory quality of prepared coated stir bar was demonstrated. In this work, the prepared stir bar was utilized in combination with ultrasound-assisted liquid desorption, followed by high-performance liquid chromatography with ultraviolet detection for the simultaneous determination of losartan (LOS) and valsartan (VAS) in human plasma samples. In a comparison study, the extraction efficiency of the prepared stir bar was accompanied much higher extraction efficiency than the two commercial stir bars (polydimethylsiloxand and polyacrylate) for both target compounds. In order to improve the desorption efficiency of LOS and VAS, the best values for effective parameters on desorption step were selected systematically. Also, the effective parameters on extraction step were optimized using a Box-Behnken design. Under the optimum conditions, the analytical performance of the proposed method displayed excellent linear dynamic ranges for LOS (24-1000 ng mL -1 ) and VAS (91-1000 ng mL -1 ), with correlation coefficients of 0.9998 and 0.9971 and detection limits of 7 and 27 ng mL -1 , respectively. The intra- and inter-day recovery ranged from 98 to 117%, and the relative standard deviations were less than 8%. Finally, the proposed technique was successfully applied to the analysis of LOS and VAS at their therapeutic levels in volunteer patient plasma sample. The obtained results were confirmed using liquid chromatography-mass spectrometry. The proposed technique was more rapid than previously reported stir bar sorptive extraction techniques based on monolithic coatings, and exhibited lower detection limits in comparison with similar methods for the determination of LOS and VLS in

  16. Extraction and Chromatographic Determination of Shikimic Acid in Chinese Conifer Needles with 1-Benzyl-3-methylimidazolium Bromide Ionic Liquid Aqueous Solutions

    Science.gov (United States)

    Chen, Fengli; Hou, Kexin; Li, Shuangyang; Zu, Yuangang; Yang, Lei

    2014-01-01

    An ionic liquids-based ultrasound-assisted extraction (ILUAE) method was successfully developed for extracting shikimic acid from conifer needles. Eleven 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were investigated and 1-benzyl-3-methylimidazolium bromide solution was selected as the solvent. The conditions for ILUAE, including the ionic liquid concentration, ultrasound power, ultrasound time, and liquid-solid ratio, were optimized. The proposed method had good recovery (99.37%–100.11%) and reproducibility (RSD, n = 6; 3.6%). ILUAE was an efficient, rapid, and simple sample preparation technique that showed high reproducibility. Based on the results, a number of plant species, namely, Picea koraiensis, Picea meyeri, Pinus elliottii, and Pinus banksiana, were identified as among the best resources of shikimic acid. PMID:24782942

  17. Molecularly imprinted polymer for selective extraction of malachite green from seawater and seafood coupled with high-performance liquid chromatographic determination

    International Nuclear Information System (INIS)

    Lian Ziru; Wang Jiangtao

    2012-01-01

    Highlights: ► The malachite green molecularly imprinted polymer (MG-MIP) was prepared. ► The characteristics and regeneration property of MIP were studied. ► An off-line method for MG was developed using MIP as solid-phase extraction. ► The MG concentrations from seawater and seafood samples were determined. - Abstract: In this paper, a highly selective sample cleanup procedure combining molecular imprinting technique (MIT) and solid-phase extraction (SPE) was developed for the isolation of malachite green in seawater and seafood samples. The molecularly imprinted polymer (MIP) was prepared using malachite green as the template molecule, methacrylic acid as the functional monomer and ethylene glycol dimethacrylate as the cross-linking monomer. The imprinted polymer and non-imprinted polymer were characterized by scanning electron microscope and static adsorption experiments. The MIP showed a high adsorption capacity and was used as selective sorbent for the SPE of malachite green. An off-line molecularly imprinted solid-phase extraction (MISPE) method followed by high-performance liquid chromatography with diodearray detection for the analysis of malachite green in seawater and seafood samples was also established. Finally, five samples were determined. The results showed that malachite green concentration in one seawater sample was at 1.30 μg L −1 and the RSD (n = 3) was 4.15%.

  18. 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....

  19. 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...

  20. Simple protein precipitation extraction technique followed by validated chromatographic method for linezolid analysis in real human plasma samples to study its pharmacokinetics.

    Science.gov (United States)

    Mohammed, Samah A; Eissa, Maya S; Ahmed, Hytham M

    2017-02-01

    Fast and sensitive HPLC method was developed, optimized and validated for quantification of linezolid (LNZ) in human plasma using guaifenesin as an internal standard (IS). Analyte and IS were extracted from plasma by simple protein precipitation extraction technique using methanol as the precipitating solvent. The pretreated samples were injected in a mobile phase formed of acetonitrile:water:methanol (20:70:10v/v/v) in an isocratic mode at a flow rate of 1.5mL/min with UV detection at 251nm. Separation was done using Aglient ODS C 18 . The method showed linearity in the range of 0.75-50μg/mL with correlation coefficients equals to 0.9991. Precision and accuracy were in conformity with the criteria normally accepted in bio-analytical method validation. The RSDs for intra- and inter-day assays were <3.56 and 4.63%, respectively. The intra- and inter-day accuracies were 94.67-98.28% and 91.25-96.18%, respectively. The mean absolute recoveries ranged from 92.56±1.78 to 95.24±2.84. According to stability results, LNZ was stable in human plasma during the storage and analysis. LNZ a pharmacokinetic behavior was studied by applying the proposed analytical method. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

    International Nuclear Information System (INIS)

    Nakamoto, Akihiro; Nishida, Manami; Saito, Takeshi; Kishiyama, Izumi; Miyazaki, Shota; Murakami, Katsunori; Nagao, Masataka; Namura, Akira

    2010-01-01

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d 5 was used as an internal standard. The linear ranges were 0.01-5.0 μg mL -1 for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 μg mL -1 for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation ≥0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 μg mL -1 of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio ≥ 3) in urine was 5 ng mL -1 for MA and MDMA and 10 ng mL -1 for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  2. Molecularly imprinted polymer for selective extraction of malachite green from seawater and seafood coupled with high-performance liquid chromatographic determination.

    Science.gov (United States)

    Lian, Ziru; Wang, Jiangtao

    2012-12-01

    In this paper, a highly selective sample cleanup procedure combining molecular imprinting technique (MIT) and solid-phase extraction (SPE) was developed for the isolation of malachite green in seawater and seafood samples. The molecularly imprinted polymer (MIP) was prepared using malachite green as the template molecule, methacrylic acid as the functional monomer and ethylene glycol dimethacrylate as the cross-linking monomer. The imprinted polymer and non-imprinted polymer were characterized by scanning electron microscope and static adsorption experiments. The MIP showed a high adsorption capacity and was used as selective sorbent for the SPE of malachite green. An off-line molecularly imprinted solid-phase extraction (MISPE) method followed by high-performance liquid chromatography with diodearray detection for the analysis of malachite green in seawater and seafood samples was also established. Finally, five samples were determined. The results showed that malachite green concentration in one seawater sample was at 1.30 μg L⁻¹ and the RSD (n=3) was 4.15%. Crown Copyright © 2012. Published by Elsevier Ltd. All rights reserved.

  3. The use of dissolvable layered double hydroxide components in an in situ solid-phase extraction for chromatographic determination of tetracyclines in water and milk samples.

    Science.gov (United States)

    Phiroonsoontorn, Nattaphorn; Sansuk, Sira; Santaladchaiyakit, Yanawath; Srijaranai, Supalax

    2017-10-13

    This research presents a simple and green in situ solid phase extraction (is-SPE) combined with high-performance liquid chromatography (HPLC) for the simultaneous analysis of tetracyclines (TCs) including tetracycline, oxytetracycline, and chlortetracycline. In is-SPE, TCs were efficiently extracted through the precipitation formation of dissolvable layered double hydroxides (LDHs) by mixing the LDH components such as magnesium and aluminum ions (both in metal chloride salts) thoroughly in an alkaline sample solution. After the centrifugation, the precipitate was completely dissolved with trifluoroacetic acid to release the enriched TCs, and then analyzed by HPLC. Under optimized conditions, this method gave good enrichment factors (EFs) of 41-93 with low limits of detection (LODs) of 0.7-6μg/L and limits of quantitation (LOQs) of 3-15μg/L. Also, the proposed method was successfully applied for the determination of TCs in water and milk samples with the recoveries ranging from 81.7-108.1% for water and 55.7-88.7% for milk. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Stability of arsenic peptides in plant extracts: off-line versus on-line parallel elemental and molecular mass spectrometric detection for liquid chromatographic separation.

    Science.gov (United States)

    Bluemlein, Katharina; Raab, Andrea; Feldmann, Jörg

    2009-01-01

    The instability of metal and metalloid complexes during analytical processes has always been an issue of an uncertainty regarding their speciation in plant extracts. Two different speciation protocols were compared regarding the analysis of arsenic phytochelatin (As(III)PC) complexes in fresh plant material. As the final step for separation/detection both methods used RP-HPLC simultaneously coupled to ICP-MS and ES-MS. However, one method was the often used off-line approach using two-dimensional separation, i.e. a pre-cleaning step using size-exclusion chromatography with subsequent fraction collection and freeze-drying prior to the analysis using RP-HPLC-ICP-MS and/or ES-MS. This approach revealed that less than 2% of the total arsenic was bound to peptides such as phytochelatins in the root extract of an arsenate exposed Thunbergia alata, whereas the direct on-line method showed that 83% of arsenic was bound to peptides, mainly as As(III)PC(3) and (GS)As(III)PC(2). Key analytical factors were identified which destabilise the As(III)PCs. The low pH of the mobile phase (0.1% formic acid) using RP-HPLC-ICP-MS/ES-MS stabilises the arsenic peptide complexes in the plant extract as well as the free peptide concentration, as shown by the kinetic disintegration study of the model compound As(III)(GS)(3) at pH 2.2 and 3.8. But only short half-lives of only a few hours were determined for the arsenic glutathione complex. Although As(III)PC(3) showed a ten times higher half-life (23 h) in a plant extract, the pre-cleaning step with subsequent fractionation in a mobile phase of pH 5.6 contributes to the destabilisation of the arsenic peptides in the off-line method. Furthermore, it was found that during a freeze-drying process more than 90% of an As(III)PC(3) complex and smaller free peptides such as PC(2) and PC(3) can be lost. Although the two-dimensional off-line method has been used successfully for other metal complexes, it is concluded here that the fractionation and

  5. Combined cation-exchange and extraction chromatographic method of pre-concentration and concomitant separation of Cu(II) with high molecular mass liquid cation exchanger after its online detection.

    Science.gov (United States)

    Mandal, B; Roy, U S; Datta, D; Ghosh, N

    2011-08-19

    A selective method has been developed for the extraction chromatographic trace level separation of Cu(II) with Versatic 10 (liquid cation exchanger) coated on silanised silica gel (SSG-V10). Cu(II) has been extracted from 0.1M acetate buffer at the range of pH 4.0-5.5. The effects of foreign ions, pH, flow-rate, stripping agents on extraction and elution have been investigated. Exchange capacity of the prepared exchanger at different temperatures with respect to Cu(II) has been determined. The extraction equilibrium constant (K(ex)) and different standard thermodynamic parameters have also been calculated by temperature variation method. Positive value of ΔH (7.98 kJ mol⁻¹) and ΔS (0.1916 kJ mol⁻¹) and negative value of ΔG (-49.16 kJ mol⁻¹) indicated that the process was endothermic, entropy gaining and spontaneous. Preconcentration factor was optimized at 74.7 ± 0.2 and the desorption constants K(desorption)¹(1.4 × 10⁻²) and K(desorption)²(9.8 × 10⁻²) were determined. The effect of pH on R(f) values in ion exchange paper chromatography has been investigated. In order to investigate the sorption isotherm, two equilibrium models, the Freundlich and Langmuir isotherms, were analyzed. Cu(II) has been separated from synthetic binary and multi-component mixtures containing various metal ions associated with it in ores and alloy samples. The method effectively permits sequential separation of Cu(II) from synthetic quaternary mixture containing its congeners Bi(III), Sn(II), Hg(II) and Cu(II), Cd(II), Pb(II) of same analytical group. The method was found effective for the selective detection, removal and recovery of Cu(II) from industrial waste and standard alloy samples following its preconcentration on the column. A plausible mechanism for the extraction of Cu(II) has been suggested. Copyright © 2011 Elsevier B.V. All rights reserved.

  6. A novel multiple headspace extraction gas chromatographic method for measuring the diffusion coefficient of methanol in water and in olive oil.

    Science.gov (United States)

    Zhang, Chun-Yun; Chai, Xin-Sheng

    2015-03-13

    A novel method for the determination of the diffusion coefficient (D) of methanol in water and olive oil has been developed. Based on multiple headspace extraction gas chromatography (MHE-GC), the methanol released from the liquid sample of interest in a closed sample vial was determined in a stepwise fashion. A theoretical model was derived to establish the relationship between the diffusion coefficient and the GC signals from MHE-GC measurements. The results showed that the present method has an excellent precision (RSDwater and olive oil, when compared with data reported in the literature. The present method is simple and practical and can be a valuable tool for the determination of the diffusion coefficient of volatile analyte(s) into food simulants from food and beverage packaging material, both in research studies and in actual applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Nakamoto, Akihiro [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nishida, Manami [Hiroshima University Technical Center, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Saito, Takeshi [Department of Emergency and Critical Care Medicine, Tokai University School of Medicine, Shimokasuya 143, Isehara, Kanagawa 259-1143 (Japan); Kishiyama, Izumi; Miyazaki, Shota [GL Sciences Inc., Sayamagahara 237-2, Iruma, Saitama 358-0032 (Japan); Murakami, Katsunori [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nagao, Masataka [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Namura, Akira, E-mail: namera@hiroshima-u.ac.jp [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan)

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d{sub 5} was used as an internal standard. The linear ranges were 0.01-5.0 {mu}g mL{sup -1} for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 {mu}g mL{sup -1} for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation {>=}0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 {mu}g mL{sup -1} of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio {>=} 3) in urine was 5 ng mL{sup -1} for MA and MDMA and 10 ng mL{sup -1} for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  8. Covalent triazine framework-1 as adsorbent for inline solid phase extraction-high performance liquid chromatographic analysis of trace nitroimidazoles in porcine liver and environmental waters.

    Science.gov (United States)

    Zhong, Cheng; Chen, Beibei; He, Man; Hu, Bin

    2017-02-03

    In this study, covalent triazine framework-1 (CTF-1) was adopted as solid phase extraction (SPE) sorbents, and a method of SPE inline coupled with high performance liquid chromatography-ultraviolet (HPLC-UV) detection was developed for trace analysis of three nitroimidazolaes (including metronidazole, ronidazole and dimetridazole) in porcine liver and environmental water samples. CTF-1 has rich π-electron and N containing triazine, thus can form π-π interaction and intermolecular hydrogen bond with three target polar nitroimidazoles, resulting in high extraction efficiency (87%-98%). Besides, CTF-1 has large specific area, which benefits rapid mass transfer and low column pressure, leading to fast adsorption/desorption dynamics. Several parameters affecting inline SPE including pH, sample flow rate, sample volume, desorption reagents, elution flow rate, elution volume, and ionic strength were investigated. Under the optimal experimental conditions, the limits of detection (S/N=3) were found to be in the range of 0.11-0.13μg/L. The enrichment factors (EFs) ranged from 52 to 59 fold (theoretical EF was 60-fold). The relative standard deviations were in the range of 4.3-9.4% (n=7, c=1μg/L), and the linear range was 0.5-500μg/L for three target analytes. The sample throughput is 7/h. The proposed method was successfully applied to the analysis of nitroimidazoles in porcine liver and environmental water samples with good recoveries for the spiked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection.

    Science.gov (United States)

    Nakamoto, Akihiro; Nishida, Manami; Saito, Takeshi; Kishiyama, Izumi; Miyazaki, Shota; Murakami, Katsunori; Nagao, Masataka; Namura, Akira

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation. Copyright 2009 Elsevier B.V. All rights reserved.

  10. 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)

  11. 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.

  12. Derivative spectrum chromatographic method for the determination of trimethoprim in honey samples using an on-line solid-phase extraction technique.

    Science.gov (United States)

    Uchiyama, Kazuhisa; Kondo, Mari; Yokochi, Rika; Takeuchi, Yuri; Yamamoto, Atsushi; Inoue, Yoshinori

    2011-07-01

    A simple, selective and rapid analytical method for determination of trimethoprim (TMP) in honey samples was developed and validated. This method is based on a SPE technique followed by HPLC with photodiode array detection. After dilution and filtration, aliquots of 500 μL honey samples were directly injected to an on-line SPE HPLC system. TMP was extracted on an RP SPE column, and separated on a hydrophilic interaction chromatography column during HPLC analysis. At the first detection step, the noise level of the photodiode array data was reduced with two-dimensional equalizer filtering, and then the smoothed data were subjected to derivative spectrum chromatography. On the second-derivative chromatogram at 254 nm, the limit of detection and the limit of quantification of TMP in a honey sample were 5 and 10 ng/g, respectively. The proposed method showed high accuracy (60-103%) with adequate sensitivity for TMP monitoring in honey samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. 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.

  14. 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...

  15. 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.

  16. Binding of Sr from milk by solid phase extraction with cryptand C222 sorbed on silica gel, cation exchange, chelating or adsorbent resins for simplified 90Sr analysis

    International Nuclear Information System (INIS)

    Tait, David; Wiechen, Arnold; Haase, Gerhard

    1995-01-01

    Several commercially available resins have been found to bind the bicyclic polyether cryptand C222 from aqueous acetonitrile solutions. The presence of C222 on some of these resins strongly improved their affinity for Sr, so that relatively small amounts of such resins sorbed Sr from milk. The resins investigated were silica gel, polyacrylic acid crosslinked with divinylbenzene (DVB), polystyrene crosslinked with divinylbenzene (PS-DVB) and PS-DVB containing sulphonate, aminomethylphosphonate, iminodiacetate and mercapto groups. The resins for which binding of C222 resulted in the largest improvement in Sr sorption from milk were PS-DVB containing mercapto groups (Chelite S) and silica gel (Si 60). Thus, 2 ml wet volume of either Chelite S containing 133 μmol of C222, or silica gel Si-60 containing 143 μmol of C222 sorbed 90 and 48%, respectively, of the Sr from 100-ml milk samples. As the sorption of Sr from milk by these systems is relatively slow, contact times of 24-36 h are required to attain these results. The Chelite S-C222 system separates Sr effectively from Cs and Ca. Under the conditions described here some 6% of the natural 40 K in milk sorbs with Sr to the resin. Ba behaves similarly to Sr. 90 Sr/ 90 Y sorbed on the silica gel Si-60-C222 system can be measured directly and efficiently by liquid scintillation counting. If adequate specificity can be attained this system might provide a very simple method of determining 90 Sr in milk

  17. 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.

  18. 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)

  19. Liquid-liquid extraction/headspace/gas chromatographic/mass spectrometric determination of benzene, toluene, ethylbenzene, (o-, m- and p-)xylene and styrene in olive oil using surfactant-coated carbon nanotubes as extractant.

    Science.gov (United States)

    Carrillo-Carrión, Carolina; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

    2007-11-09

    BTEX-S compounds are widely distributed in the environment and can be present in different foodstuffs, including olive oil. Taking into account the risks of the exposure to these compounds, analytical methods for their determination in different matrices are mandatory. In this paper, the use of surfactant-coated multiwalled carbon nanotubes as additive in liquid-liquid extraction is applied for the determination of single-ring aromatic compounds in olive oil samples. After sample treatment, the aqueous extracts are subsequently analyzed by headspace/gas chromatography/mass spectrometry allowing the determination of BTEX-S within ca. 15 min. Each stage of the proposed LLE/HS/GC/MS configuration involves a selectivity enhancement avoiding the interference of other compounds of the sample matrix. Limits of detection were in the range 0.25 ng mL(-1) (obtained for ethylbenzene) and 0.43 ng mL(-1) (for benzene). The repeatability of the proposed method expressed as RSD varied between 1.9% (styrene) and 3.3% (benzene) (n=11).

  20. 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 ...

  1. Adsorption kinetics, isotherm, and thermodynamics studies of acetyl-11-keto-β-boswellic acids (AKBA) from Boswellia serrata extract using macroporous resin.

    Science.gov (United States)

    Niphadkar, Sonali S; Rathod, Virendra K

    2017-09-14

    An acetyl-11-keto-β-boswellic acid (AKBA) is potent anti-inflammatory agent found in Boswellia serrata oleogum resin. Adsorption characteristics of AKBA from B. serrata were studied using macroporous adsorbent resin to understand separation and adsorption mechanism of targeted molecules. Different macroporous resins were screened for adsorption and desorption of AKBA and Indion 830 was screened as it showed higher adsorption capacity. The kinetic equations were studied and results showed that the adsorption of AKBA on Indion 830 was well fitted to the pseudo first-order kinetic model. The influence of two parameters such as temperature (298, 303, and 308 K) and pH (5-8) on the adsorption process was also studied. The experimental data was further investigated using Langmuir, Freundlich, and Temkin isotherm models. It was observed that Langmuir isotherm model was found to be the best fit for AKBA adsorption by Indion 830 and highest adsorption capacity (50.34 mg/g) was obtained at temperature of 303 K. The values of thermodynamic parameters such as the change of Gibbs free energy (ΔG*), entropy (ΔS*), and enthalpy (ΔH*), indicated that the process of adsorption was spontaneous, favourable, and exothermic.

  2. 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.

  3. 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...

  4. 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

  5. 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.

  6. 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.

  7. 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.

  8. 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

  9. Determination of trace amounts of lead, arsenic, nickel and cobalt in high-purity iron oxide pigment by inductively coupled plasma atomic emission spectrometry after iron matrix removal with extractant-contained resin

    International Nuclear Information System (INIS)

    Xu Yuyu; Zhou Jianfeng; Wang Guoxin; Zhou Jinfan; Tao Guanhong

    2007-01-01

    Inductively coupled plasma atomic emission spectrometry (ICP-AES) was applied to the determination of lead, arsenic, nickel and cobalt in high-purity iron oxide pigment. Samples were dissolved with hydrochloric acid and hydrogen peroxide. The digest was passed through a column, which was packed with a polymer resin containing a neutral organophosphorus extractant, tri-n-butylphosphate. Iron was sorbed selectively on the resin and the analytes of interest passed through the column, allowing the effective separation of them from the iron matrix. Conditions of separation were optimized. The detection limits (3σ) in solution were 10, 40, 7 and 5 μg L -1 , and in pigment were 0.2, 0.8, 0.14 and 0.1 mg kg -1 for lead, arsenic, cobalt and nickel, respectively. The recoveries ranged from 95% to 107% when sample digests were spiked with 5 μg of the analytes of interest, and relative standard deviations (n = 6) were 1.5-17.6% for the determination of the spiked samples. The method was successfully applied to the determination of trace amounts of these elements in high-purity iron oxide pigment samples

  10. 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.)

  11. 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.

  12. 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....

  13. 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.

  14. 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...

  15. 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

  16. 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.

  17. 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.

  18. 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.

  19. 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

  20. 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

  1. 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.

  2. 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

  3. Identification of organic iodocompounds in the PUREX process with the help of methods for chromatographic separation and spectrometric detection as well as characterization of their behavior during extraction. Final report

    International Nuclear Information System (INIS)

    Gaul, G.; Gibau, F.; Knoechel, A.

    1993-01-01

    In the system HNO 3 KI, Dodecan and TBP the radiolytic reactive behaviour of the described compounds during the dissolution of nuclear fuel elements was simulated. External γ-irradiation gave the best informations. As a consequence of radiolyticly induced reactions several volatile and non-volatile iodoorganic compounds like iodoalkanes, iodonitroalkanes and iodonitroalkylphosphates are formed. They were separated by gaschromatography (GC) and high performance liquid chromatography (HPLC). For HPLC a special photolytic/electrochemical detector with comparable sensitivity like the electroncapture detector in the GC-field was developed. With the help of the two described chromatographic techniques the different iodoorganic compounds could be separated singularily or in groups of isomers. The separation of all compounds demands two-dimensional chromatographies including the capillary-SFC, which was not available for this project. Most of the iodoorganic compounds could be identified by comparison of the retention times of well known compounds. In the other cases, the compounds were studied mass-spectrometrically. Unfortunately all available ionisation techniques (EI; CI; FAB) were too hard for the labile C-I-bond. Therefore an identification of these compounds was not possible. In any case, instructive fingerprint spectra are available enabling relationships between the generation of the iodoorganic compounds and the reaction conditions during their formation. (orig.) [de

  4. Vibrational Spectroscopy of Chromatographic Interfaces

    Energy Technology Data Exchange (ETDEWEB)

    Jeanne E. Pemberton

    2011-03-10

    Chromatographic separations play a central role in DOE-supported fundamental research related to energy, biological systems, the environment, and nuclear science. The overall portfolio of research activities in the Separations and Analysis Program within the DOE Office of Basic Energy Sciences includes support for activities designed to develop a molecular-level understanding of the chemical processes that underlie separations for both large-scale and analytical-scale purposes. The research effort funded by this grant award was a continuation of DOE-supported research to develop vibrational spectroscopic methods to characterize the interfacial details of separations processes at a molecular level.

  5. 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....

  6. EXTRACT

    DEFF Research Database (Denmark)

    Pafilis, Evangelos; Buttigieg, Pier Luigi; Ferrell, Barbra

    2016-01-01

    The microbial and molecular ecology research communities have made substantial progress on developing standards for annotating samples with environment metadata. However, sample manual annotation is a highly labor intensive process and requires familiarity with the terminologies used. We have the...... and text-mining-assisted curation revealed that EXTRACT speeds up annotation by 15-25% and helps curators to detect terms that would otherwise have been missed.Database URL: https://extract.hcmr.gr/......., organism, tissue and disease terms. The evaluators in the BioCreative V Interactive Annotation Task found the system to be intuitive, useful, well documented and sufficiently accurate to be helpful in spotting relevant text passages and extracting organism and environment terms. Comparison of fully manual...

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

    Directory of Open Access Journals (Sweden)

    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.

  8. 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.)

  9. Isotope separations using chromatographic methods

    International Nuclear Information System (INIS)

    Leseticky, L.

    1985-01-01

    A survey is given of chromatographic separations of compounds only differing in isotope composition. Isotope effects on physical properties which allow chromatographic separation (vapour tension, adsorption heat, partition coefficient) are very small, with the exception of the simplest molecules. Therefore, separation factors only assume the value of several per cent. From this ensues the necessity of using columns which are specially and very carefully prepared and have a separation efficiency of the order of 10 4 theoretical plates. Briefly discussed is liquid chromatography on ion exchangers which with a varied degree of success was used for separating simple inorganic compounds or ions. Ion exchange chromatography of amino acids labelled with tritium, and chromatography of tritium labelled steroids also provided only a certain degree of separation. A detailed analysis is presented of gas chromatography separation of various deuterium and tritium labelled low-molecular compounds, to which a number of studies has been devoted in the literature. Very promising is the method of complexation gas chromatography based on the reversible formation of a complex of the ligand (the compound being separated) and the compound of the (transition) metal as the steady-state phase. (author)

  10. 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

  11. 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.)

  12. 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

  13. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

    Science.gov (United States)

    Furlong, E.T.; Vaught, D.G.; Merten, L.M.; Foreman, W.T.; Gates, Paul M.

    1996-01-01

    A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

  14. 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.)

  15. 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

  16. A novel analytical method of 1-(3-trifluoromethylphenyl piperazine and 1-(3-chlorophenyl piperazine in fluids of drug addicts using liquid-liquid extraction-gas chromatographic/nitrogen-phosphorous detection

    Directory of Open Access Journals (Sweden)

    Jing Chang

    2017-01-01

    Full Text Available In accordance with the research specifications and guidelines in China, we developed a novel experimental method to detect new piperazine-type drugs, such as 1-(3-trifluoromethylphenyl piperazine and 1-(3-chlorophenyl piperazine. In this study, a new pretreatment method and gas chromatography (GC/nitrogen-phosphorus detector detection technique were used to characterize these two kinds of drugs in urine and blood samples. For the purpose of isolation of these trace drugs from the samples, liquid-liquid extraction/solid-phase extraction was modified and validated for this specific study. The pretreatment method presented in this paper has many advantages, such as high recovery rate, high extraction efficiency, high detection sensitivity, low limit of detection, and simple operation. The GC/NPD instrument is popular in most laboratories because it can meet the routine requirements of forensic science. All these aspects make this combination of sample pretreatment and GC/NPD technique the most suitable choice for drug detection in biological samples.

  17. 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.

  18. 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.

  19. Comparative Chromatographic Analysis and Pharmacodynamic ...

    African Journals Online (AJOL)

    The laboratory analysis of the Garcinia Kolanuts extracts showed receptors inhibition of Beta adrenergic sites, adenosine, melatonin, opiate, purine, calcium channel L-type and 5HT5A. Conclusion: Garcinia kolanut extract exhibits a combined effects of all the known antiglaucoma drugs used in comparison. NQJHM Vol.

  20. Cetylpyridinium chloride functionalized silica-coated magnetite microspheres for the solid-phase extraction and pre-concentration of ochratoxin A from environmental water samples with high-performance liquid chromatographic analysis.

    Science.gov (United States)

    Hu, Meihua; Huang, Pengcheng; Suo, Lili; Wu, Fangying

    2017-06-01

    A new method based on cetylpyridinium chloride coated ferroferric oxide/silica magnetic microspheres as an efficient solid-phase adsorbent was developed for the extraction and enrichment of ochratoxin A. The determination of ochratoxin A was obtained by high-performance liquid chromatography with fluorescence detection. In the presence of cetylpyridinium chloride, the adsorption capacity of ferroferric oxide/silica microspheres was 5.95 mg/g for ochratoxin A. The experimental parameters were optimized, including the amounts of ferroferric oxide/silica microspheres (20 mg) and cetylpyridinium chloride (0.18 mL, 0.5 mg/mL), pH value of media (9), ultrasonic time (5 min), elution solvent and volume [2(1 + 1) mL (washed twice, 1 mL each time) 1% acetic acid acetonitrile]. Under optimal experiment conditions, ochratoxin A had good linearity in the range of 2.5-250.0 ng/L in water samples with correlation coefficient of the calibration curve 0.9995. The limit of detection for ochratoxin A was 0.83 ng/L, and the recoveries were 89.8-96.8% with the relative standard deviation of 1.5-3.5% in environmental water samples. Furthermore, ferroferric oxide/silica microspheres show excellent reusability during extraction procedures for no less than six times. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. 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

  2. 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

  3. 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

  4. Quantification and Purification of Mulberry Anthocyanins with Macroporous Resins

    Directory of Open Access Journals (Sweden)

    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.

  5. Anticholinesterase activity and chemical profile of an active chromatographic fraction of ethanolic extract from Bellis perennis L. (Asteraceae) flowers; Atividade anticolinesterasica e perfil quimico de uma fracao cromatografica ativa do extrato etanolico das flores Bellis perennis L. (Asteraceae)

    Energy Technology Data Exchange (ETDEWEB)

    Marques, Thiago Henrique Costa; Santos, Pauline Sousa dos; Freitas, Rivelilson Mendes de, E-mail: rivelilson@pq.cnpq.br [Universidade Federal do Piaui (UFPI), Teresina, PI (Brazil). Centro de Ciencias da Saude. Departamento de Bioquimica e Farmacologia; Carvalho, Rusbene Bruno Fonseca de; Melo, Cassio Herbert Santos de [Universidade Federal do Piaui (UFPI), Teresina, PI (Brazil). Centro de Ciencias da Natureza. Departamento de Quimica; David, Juceni Pereira [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Faculdade de Farmacia; David, Jorge Mauricio; Lima, Luciano Silva [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Instituto de Quimica

    2013-09-01

    This work describes the isolation of an active flavonoid fraction and identification of isorhamnetin 3-O-{beta}-D-(6''-acetyl)- alactopyranoside from flowers of B. perennis, and also the evaluation of anticholinesterase (AChE) activity of ethanolic extract from flowers (EEF) and the active fraction. The chemical structure of the flavonoid was defined on the basis of spectroscopic {sup 1}H NMR, IR and UV data. EEF or flavonoid reduces AChE activity in vivo, while flavonoid also reduces AChE activity in vitro, showing a value of 1.49 {mu}M for 50% inhibitory concentration (IC{sub 50}), suggesting potential use as an insecticide or in the treatment of neurodegenerative diseases such as Alzheimer's disease. (author)

  6. Comparison of a disposable sorptive sampler with thermal desorption in a gas chromatographic inlet, or in a dedicated thermal desorber, to conventional stir bar sorptive extraction-thermal desorption for the determination of micropollutants in water.

    Science.gov (United States)

    Wooding, Madelien; Rohwer, Egmont R; Naudé, Yvette

    2017-09-01

    The presence of micropollutants in the aquatic environment is a worldwide environmental concern. The diversity of micropollutants and the low concentration levels at which they may occur in the aquatic environment have greatly complicated the analysis and detection of these chemicals. Two sorptive extraction samplers and two thermal desorption methods for the detection of micropollutants in water were compared. A low-cost, disposable, in-house made sorptive extraction sampler was compared to SBSE using a commercial Twister sorptive sampler. Both samplers consisted of polydimethylsiloxane (PDMS) as a sorptive medium to concentrate micropollutants. Direct thermal desorption of the disposable samplers in the inlet of a GC was compared to conventional thermal desorption using a commercial thermal desorber system (TDS). Comprehensive gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-TOFMS) was used for compound separation and identification. Ten micropollutants, representing a range of heterogeneous compounds, were selected to evaluate the performance of the methods. The in-house constructed sampler, with its associated benefits of low-cost and disposability, gave results comparable to commercial SBSE. Direct thermal desorption of the disposable sampler in the inlet of a GC eliminated the need for expensive consumable cryogenics and total analysis time was greatly reduced as a lengthy desorption temperature programme was not required. Limits of detection for the methods ranged from 0.0010 ng L -1 to 0.19 ng L -1 . For most compounds, the mean (n = 3) recoveries ranged from 85% to 129% and the % relative standard deviation (% RSD) ranged from 1% to 58% with the majority of the analytes having a %RSD of less than 30%. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. 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)

  8. Chromatographic and biological aspects of organomercurials

    Energy Technology Data Exchange (ETDEWEB)

    Fishbein, L

    1970-01-01

    A thorough review on the biological and chromatographic aspects of methylmercury, phenylmercurials, and miscellaneous organomercurials is presented. Areas covered include ecology, epidemiology, paper chromatography, thin-layer chromatography, gas chromatography, metabolism and toxicity, and environmental degradation. 183 references.

  9. A Quantitative Gas Chromatographic Ethanol Determination.

    Science.gov (United States)

    Leary, James J.

    1983-01-01

    Describes a gas chromatographic experiment for the quantitative determination of volume percent ethanol in water ethanol solutions. Background information, procedures, and typical results are included. Accuracy and precision of results are both on the order of two percent. (JN)

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

    Directory of Open Access Journals (Sweden)

    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.

  11. 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.

  12. Extraction and high-performance liquid chromatographic analysis of C60, C70, and [6,6]-phenyl C61-butyric acid methyl ester in synthetic and natural waters.

    Science.gov (United States)

    Bouchard, Dermont; Ma, Xin

    2008-09-05

    Studies have shown that C(60) fullerene can form stable colloidal suspensions in water that result in C(60) aqueous concentrations many orders of magnitude above C(60)'s aqueous solubility; however, quantitative methods for the analysis of C(60) and other fullerenes in environmental media are scarce. Using a 80/20v/v toluene-acetonitrile mobile phase and a 4.6 mm x 150 mm Cosmosil 5micron PYE column, C(60), C(70), and PCBM ([6,6]-phenyl C(61)-butyric acid methyl ester) were fully resolved. Selectivity factors (alpha) for C(60) relative to PCBM and C(70) relative to C(60) were 3.18 and 2.19, respectively. The best analytical wavelengths for the fullerenes were determined to be 330, 333, and 333 nm with log molar absorption coefficients (log epsilon) of 4.63, 4.82, and 4.60 for PCBM, C(60), C(70), respectively. Extraction and quantitation of all three fullerenes in aqueous suspensions over a range of pH (4-10) and ionic strengths were very good. Whole-method quantification limits for ground and surface suspensions were 2.87, 2.48, and 6.54 microg/L for PCBM, C(60), and C(70), respectively.

  13. 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)

  14. Determination of biocides as well as some biocide metabolites from facade run-off waters by solid phase extraction and high performance liquid chromatographic separation and tandem mass spectrometry detection.

    Science.gov (United States)

    Bester, K; Lamani, X

    2010-08-06

    Biocides are used to protect buildings, boats, and other materials from microbial infestations. A huge variety of compounds are being used: isothiazolinones, e.g., to prevent bacterial growth in paints, triazines and phenylureas against algal growth on water exposed materials while carbamates are used against fungal investations. However these biocides can be leached from the respective materials. As these are very effective compounds it is important to know the concentrations of these biocides in the leachates as well as their leaching behaviour to assess their risk to the environment. In this study, a method for the determination of biocides from facade material run-off water by means of high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) was developed. Due to the amphiphilic character and the expected varying pH-values in the samples, the extractions as well as the HPLC-method development proved to be demanding. The water samples (leachates) were buffered with a phosphate buffer to pH 7. As some of the biocides are very hydrophilic, different SPE cartridges were tested to identify the SPE material with the highest recovery rates for all compounds. For gaining a good separation, analyte trapping was performed on the HPLC column. Quantification was performed using a mass spectrometer in multi-reaction monitoring with two transitions per compound. The final recovery rates were conducted using a cartridge with a divenylbenzyl polymer sorbent. A combination of methanol and acetonitrile as eluents was used to reach recovery rates in the range of 70-100%. The limit of quantification for the compounds of interest ranged from 0.01 to 0.1 microg/L. Copyright 2010 Elsevier B.V. All rights reserved.

  15. Determination of Human-Health Pharmaceuticals in Filtered Water by Chemically Modified Styrene-Divinylbenzene Resin-Based Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass Spectrometry

    Science.gov (United States)

    Furlong, Edward T.; Werner, Stephen L.; Anderson, Bruce D.; Cahill, Jeffery D.

    2008-01-01

    In 1999, the Methods Research and Development Program of the U.S. Geological Survey National Water Quality Laboratory began the process of developing a method designed to identify and quantify human-health pharmaceuticals in four filtered water-sample types: reagent water, ground water, surface water minimally affected by human contributions, and surface water that contains a substantial fraction of treated wastewater. Compounds derived from human pharmaceutical and personal-care product use, which enter the environment through wastewater discharge, are a newly emerging area of concern; this method was intended to fulfill the need for a highly sensitive and highly selective means to identify and quantify 14 commonly used human pharmaceuticals in filtered-water samples. The concentrations of 12 pharmaceuticals are reported without qualification; the concentrations of two pharmaceuticals are reported as estimates because long-term reagent-spike sample recoveries fall below acceptance criteria for reporting concentrations without qualification. The method uses a chemically modified styrene-divinylbenzene resin-based solid-phase extraction (SPE) cartridge for analyte isolation and concentration. For analyte detection and quantitation, an instrumental method was developed that used a high-performance liquid chromatography/mass spectrometry (HPLC/MS) system to separate the pharmaceuticals of interest from each other and coextracted material. Immediately following separation, the pharmaceuticals are ionized by electrospray ionization operated in the positive mode, and the positive ions produced are detected, identified, and quantified using a quadrupole mass spectrometer. In this method, 1-liter water samples are first filtered, either in the field or in the laboratory, using a 0.7-micrometer (um) nominal pore size glass-fiber filter to remove suspended solids. The filtered samples then are passed through cleaned and conditioned SPE cartridges at a rate of about 15

  16. 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

  17. Radiation curable epoxy resin

    International Nuclear Information System (INIS)

    Najvar, D.J.

    1978-01-01

    A carboxyl containing polymer is either prepared in the presence of a polyepoxide or reacted with a polyepoxide. The polymer has sufficient acid groups to react with only about 1 to 10 percent of the epoxide (oxirane) groups. The remaining epoxide groups are reacted with an unsaturated monocarboxylic acid such as acrylic or methacrylic acid to form a radiation curable resin

  18. 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.

  19. Chromatographic study of Euphorbia cyparissias

    Directory of Open Access Journals (Sweden)

    Cristina, T. Romeo,

    2009-12-01

    Full Text Available The ectoparasitic population control is very difficult and includes numerous chemical substances and therapeutic techniques. Although efficient at first, the repeated use of acaricidal substances leads to the appearance of resistance. The more and more reduced efficacy of the therapeutic arsenal puts serious problems for the practitionersand increases the need of newer substances on the market. Besides this appears the problem of residues in eggs and meat, which is a serious impediment. Because of this the use of plant extracts is an attractive and promising research path. The investigations tied to the parasitic biocontrol have diversified with the study of the numerous control sources (fungi, plant extracts, volatile oils etc..In this context, the plant extracts can become an alternative source for the acaricidal control knowing that they constitute a rich source of efficient bioactive compounds. Unfortunately although at hand until today, not very much data is known about what determines theacaricidal activity of some plant extracts against the argaside ticks.The present work describes an in vitro CG-MS study for identification of Euphorbia cyparissias’ chemical composition.

  20. 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

  1. 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.

  2. 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)

  3. 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

  4. 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

  5. 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.

  6. Embedding in thermosetting resins

    International Nuclear Information System (INIS)

    Buzonniere, A. de

    1985-01-01

    Medium activity waste coming either from nuclear power plants in operation such as evaporator concentrates, spent resins, filter cartridges or the dismantling of installations are embedded in order to obtain a product suitable for long term disposal. Embedding in thermosetting resins (polyester or epoxy) is one among currently used techniques; it is being developed by the CEA (Commissariat a l'Energie Atomique) and Technicatome (subsidiary of CEA and EDF). The process is easy to operate and yields excellent results particularly as far as volume reduction and radioelement containment (cesium particularly) are concerned. The process has already been in operation in four stationary plants for several years. Extension of the process to mobile units has been completed by Technicatome in collaboration with the CEA [fr

  7. Paramagnetic epoxy resin

    Directory of Open Access Journals (Sweden)

    E. C. Vazquez Barreiro

    2017-01-01

    Full Text Available This work illustrates that macrocycles can be used as crosslinking agents for curing epoxy resins, provided that they have appropriate organic functionalities. As macrocycles can complex metal ions in their structure, this curing reaction allows for the introduction of that metal ion into the resin network. As a result, some characteristic physical properties of the metallomacrocycle could be transferred to the new material. The bisphenol A diglycidyl ether (BADGE, n = 0 and hemin (a protoporphyrin IX containing the Fe(III ion, and an additional chloride ligand have been chosen. The new material has been characterized by differential scanning calorimetry (DSC, thermogravimetric analysis (TGA, Fourier Transform Infrared (FT-IR, Nuclear Magnetic Resonance (NMR, Transmission Electron Microscopy (TEM, and magnetic susceptibility measurements. Fe(III remains in the high-spin state during the curing process and, consequently, the final material exhibits the magnetic characteristics of hemin. The loss of the chlorine atom ligand during the cure of the resin allows that Fe(III can act as Lewis acid, catalyzing the crosslinking reactions. At high BADGE n = 0/hemin ratios, the formation of ether and ester bonds occurs simultaneously during the process.

  8. 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)

  9. 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.

  10. 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.

  11. 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

  12. Liquid chromatographic-mass spectrometric method for ...

    African Journals Online (AJOL)

    Tropical Journal of Pharmaceutical Research ... Purpose: To develop and validate a simple, efficient and reliable Liquid chromatographic-mass spectrometric (LC-MS/MS) method for the quantitative determination of two dermatological drugs, ... By Country · List All Titles · Free To Read Titles This Journal is Open Access.

  13. Liquid chromatographic analysis of phenobarbitone, ethosuximide ...

    African Journals Online (AJOL)

    A liquid chromatographic method for the simultaneous assay of four anticonvulsant drugs, phenobarbitone, ethosuximide, phenytoin and carbamazepine on a polystyrene-divinyl benzene column is described. The method was developed by the systematic study of different types of co-polymer materials, type and ...

  14. Validated high performance liquid chromatographic (HPLC) method ...

    African Journals Online (AJOL)

    STORAGESEVER

    2010-02-22

    Feb 22, 2010 ... specific and accurate high performance liquid chromatographic method for determination of ZER in micro-volumes ... tional medicine as a cure for swelling, sores, loss of appetite and ... Receptor Activator for Nuclear Factor κ B Ligand .... The effect of ... be suitable for preclinical pharmacokinetic studies. The.

  15. Chromatographic characterisation, in vitro antioxidant and free ...

    African Journals Online (AJOL)

    Chromatographic fractionation and spectroscopic analysis of the ME4 fraction revealed the presence of four compounds namely garcinia biflavonoids GB1 and GB2, garcinal and garcinoic acid. These findings show that these four compounds are partly responsible for the great antioxidant potential of G. kola seeds.

  16. 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.

  17. 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....

  18. 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

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

    Directory of Open Access Journals (Sweden)

    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.

  20. 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.

  1. 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.

  2. 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)

  3. 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.

  4. 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.)

  5. 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.

  6. 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

  7. 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.

  8. 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.

  9. 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)

  10. [Acrylic resin removable partial dentures

    NARCIS (Netherlands)

    Baat, C. de; 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

  11. Chemoviscosity modeling for thermosetting resins

    Science.gov (United States)

    Tiwari, S. N.; Hou, T. H.; Bai, J. M.

    1985-01-01

    A chemoviscosity model, which describes viscosity rise profiles accurately under various cure cycles, and correlates viscosity data to the changes of physical properties associated with structural transformations of the thermosetting resin system during cure, was established. Work completed on chemoviscosity modeling for thermosetting resins is reported.

  12. Cure shrinkage in casting resins

    Energy Technology Data Exchange (ETDEWEB)

    Spencer, J. Brock [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2015-02-01

    A method is described whereby the shrinkage of a casting resin can be determined. Values for the shrinkage of several resin systems in frequent use by Sandia have been measured. A discussion of possible methods for determining the stresses generated by cure shrinkage and thermal contraction is also included.

  13. 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%.

  14. 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.

  15. GAS CHROMATOGRAPHIC AND SPECTROSCOPIC ANALYSIS OF ...

    African Journals Online (AJOL)

    Peroxyformic acid prepared in-situ was employed for epoxidation of canola oil in the presence of toluene. Gas chromatographic analysis of the product revealed the following species: C16:0; C18:0; C18:1; C18:2; C18:3; monoepoxy C18:0; monoepoxy C18:1; monoepoxy C18:2; diepoxy C18:0; diepoxy C18:1 and triepoxy ...

  16. Amalgam-chromatographic separation of magnesium isotopes

    International Nuclear Information System (INIS)

    Klinskij, G.D.; Levkin, A.V.; Ivanov, S.A.

    1990-01-01

    Separation of magnesium isotopes within Mg(Hg)-MgI 2 system (in dimethylformamide) is conducted under amalgam-chromatographic conditions. Separation maximal degree, that is (1.09), for 24 Mg and 26 Mg and separation coefficient (α = 1.0089±0.006) are determined. Light isotopes are found to concentrate in the amalgam. Technique of thermal conversion of flows within amalgam-dimethylformamide system is suggested on the basis of reversible reaction of Ca-Mg element exchange

  17. Validation for chromatographic and electrophoretic methods

    OpenAIRE

    Ribani, Marcelo; Bottoli, Carla Beatriz Grespan; Collins, Carol H.; Jardim, Isabel Cristina Sales Fontes; Melo, Lúcio Flávio Costa

    2004-01-01

    The validation of an analytical method is fundamental to implementing a quality control system in any analytical laboratory. As the separation techniques, GC, HPLC and CE, are often the principal tools used in such determinations, procedure validation is a necessity. The objective of this review is to describe the main aspects of validation in chromatographic and electrophoretic analysis, showing, in a general way, the similarities and differences between the guidelines established by the dif...

  18. Analyzing chromatographic data using multilevel modeling.

    Science.gov (United States)

    Wiczling, Paweł

    2018-06-01

    It is relatively easy to collect chromatographic measurements for a large number of analytes, especially with gradient chromatographic methods coupled with mass spectrometry detection. Such data often have a hierarchical or clustered structure. For example, analytes with similar hydrophobicity and dissociation constant tend to be more alike in their retention than a randomly chosen set of analytes. Multilevel models recognize the existence of such data structures by assigning a model for each parameter, with its parameters also estimated from data. In this work, a multilevel model is proposed to describe retention time data obtained from a series of wide linear organic modifier gradients of different gradient duration and different mobile phase pH for a large set of acids and bases. The multilevel model consists of (1) the same deterministic equation describing the relationship between retention time and analyte-specific and instrument-specific parameters, (2) covariance relationships relating various physicochemical properties of the analyte to chromatographically specific parameters through quantitative structure-retention relationship based equations, and (3) stochastic components of intra-analyte and interanalyte variability. The model was implemented in Stan, which provides full Bayesian inference for continuous-variable models through Markov chain Monte Carlo methods. Graphical abstract Relationships between log k and MeOH content for acidic, basic, and neutral compounds with different log P. CI credible interval, PSA polar surface area.

  19. nduced hyperlipidemic rats. Methods: Column chromatographic fractionation of butanol fraction of total methanol extract of leaves of Bauhinia variegata (Linn. yields four sub-fractions (sub-fraction A-D. All sub-fractions tested for their anti-hyperlipidemic activity. Sub-fractions administered at a dose of 65 mg/kg (oral to the Triton WR-1339 induced hyperlipidemic rats and total cholesterol, triglycerides, HDL, LDL and VLDL

    Directory of Open Access Journals (Sweden)

    Deepak Kumar

    2012-10-01

    Full Text Available Objective: To investigate the effect and evaluation of Anti-hyperlipidemic activity guided subfraction isolated from total methanolic extract of Bauhinia variegata (Linn. leaves on Triton WR-1339 induced hyperlipidemic rats. Methods: Column chromatographic fractionation of butanol fraction of total methanol extract of leaves of Bauhinia variegata (Linn. yields four subfractions (sub-fraction A-D. All sub-fractions tested for their anti-hyperlipidemic activity. Subfractions administered at a dose of 65 mg/kg (oral to the Triton WR-1339 induced hyperlipidemic rats and total cholesterol, triglycerides, HDL, LDL and VLDL level in the blood were checked. Results: Sub-fraction D showed significant reduction (P<0.05 among four sub-fraction in comparison with standard drug fenofibrate. Conclusions: From the above study it could be concluded that butanol sub-fraction D of Bauhinia variegata (Linn. not only have resulted in significant reduction in cholesterol, triglyceride, LDL, VLDL level but also increases the HDL level at a reduced dose level.

  20. 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.

  1. A simple micro-batch ion-exchange resin extraction method coupled with reverse-phase HPLC (MBRE-HPLC) to quantify lactoferrin in raw and heat-treated bovine milk.

    Science.gov (United States)

    Pochet, Sylvie; Arnould, Céline; Debournoux, Perrine; Flament, Jocelyne; Rolet-Répécaud, Odile; Beuvier, Eric

    2018-09-01

    Lactoferrin is an iron-binding cationic glycoprotein (pI = 8.7) beneficial for mammal health, especially udder and milk preservation. A new simple two-step method of quantification was developed. Lactoferrin in 1 mL of bovine skim milk was first adsorbed onto 100 mg of macroporous sulfonated-resin at pH 6.8 by rotary stirring for 90 min at 20-25 °C. After washing the resin, lactoferrin was desorbed using 1 mL of 2 M NaCl containing phenylalanine as a dilution marker, then fully resolved and quantified by RP-HPLC at 220 nm using a wide-bore C4 silica column. This robust, inexpensive and flexible method improves selectivity (no protein interference) and sensitivity compared to previous HPLC methods. In-laboratory validation demonstrated its linearity (25 to 514 µg Lf mL -1 ), accuracy (110 to 98% recovery), and precision (<4%), which were comparable to immuno-based methods. The results for individual raw cow's milk were strongly correlated with results using an ELISA test. Copyright © 2018 Elsevier Ltd. All rights reserved.

  2. 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.

  3. 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)

  4. [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.

  5. Chromatography resin support

    Science.gov (United States)

    Dobos, James G.

    2002-01-01

    An apparatus and method of using an improved chromatography resin support is disclosed. The chromatography support platform is provided by a stainless steel hollow cylinder adapted for being inserted into a chromatography column. An exterior wall of the stainless steel cylinder defines a groove for carrying therein an "O"-ring. The upper surface of the stainless steel column is covered by a fine stainless steel mesh welded to the edges of the stainless steel cylinder. When placed upon a receiving ledge defined within a chromatography column, the "O"-ring provides a fluid tight seal with the inner edge wall of the chromatography cylinder. The stainless steel mesh supports the chromatography matrix and provides a back flushable support which is economical and simple to construct.

  6. 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.

  7. [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.

  8. 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

  9. 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

  10. 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

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. Chromatographic monitoring procedures in laboratory practice

    Energy Technology Data Exchange (ETDEWEB)

    Kaplina, E G; Belova, O I; Lasunina, N A

    1976-01-01

    The Moscow Coke and Chemical Works consist of three plants in combination, viz., the coking plant, the synthetic ammonia plant using coke-oven-gas hydrogen and the oxygen plant. The plant requirements include daily analyses not only of the coke-oven gas but also of a rich gas and an ethylene fraction. The analyses are carried out in VTI-2 apparatus. The analytical data are used to calculate the calorific values and densities of the gases. The time requirements are very considerable and the laboratory has long been engaged in developing and introducing chromatographic procedures for the major constituents of coke-oven gas, rich gas and ethylene fraction. The procedure developed for the coke-oven and rich gases uses two parallel columns, one packed with molecular sieves and the other with grade KSM silica gel. Hydrogen was determined with argon as the carrier gas, and all other constituents with helium. The procedure was time-consuming and complicated. An attempt was made to separate the gases in an LKhM-7a chromatograph with a programme-controlled 50 to 250/sup 0/C heating cycle, but the procedure still had a number of serious defects and could not be recommended for regular quality control. The final variant involved two parallel columns and a procedure based on that in GOST 14920 (''Dry gas. Proximate analysis''). The chromatograph was a type KhL-69 with a 6-way cock in the gas line so that each of the columns could be brought on stream in succession. The analytical column packings were zeolite (in a 2 m column) and diatomaceous brick with 25% n-hexadecane (in a 6 m column).

  16. 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.

  17. Bending characteristics of resin concretes

    Directory of Open Access Journals (Sweden)

    Ribeiro Maria Cristina Santos

    2003-01-01

    Full Text Available In this research work the influence of composition and curing conditions in bending strength of polyester and epoxy concrete is analyzed. Various mixtures of resin and aggregates were considered in view of an optimal combination. The Taguchi methodology was applied in order to reduce the number of tests, and in order to evaluate the influence of various parameters in concrete properties. This methodology is very useful for the planning of experiments. Test results, analyzed by this methodology, shown that the most significant factors affecting bending strength properties of resin concretes are the type of resin, resin content and charge content. An optimal formulation leading to a maximum bending strength was achieved in terms of material parameters.

  18. Mechanism for transporting used resin

    International Nuclear Information System (INIS)

    Sugimoto, Yoshikazu; Yusa, Hideo; Kamiya, Kunio.

    1975-01-01

    Object: In the operation of a light water reactor type atomic power plant, to permit transport and reuse of used ion exchange resin used for the filtering or cleaning of cooling water or the desalting of radioactive exhaust liquid through an ejector. Structure: Used ion exchange resin within a desalter having high radioactivity is withdrawn through the action of an ejector and led to a solid-liquid separator for separation into used resin and water. The separated resin is directly collected in a storage tank while the separated water is forced through a circulating pump to a gas-liquid separator for separation into gas having radioactivity and water. The separated gas is led to a radioactive gas treatment station while the water deprived of the gas is recirculated by a drive water pump for repeated use. (Kamimura, M.)

  19. 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...

  20. Mechanism for transporting used resin

    Energy Technology Data Exchange (ETDEWEB)

    Sugimoto, Y; Yusa, H; Kamiya, K

    1975-01-16

    In the operation of a light water reactor type atomic power plant the objectives is to permit transport and reuse of used ion exchange resin used for the filtering or cleaning of cooling water or the desalting of radioactive exhaust liquid through an ejector. Used ion exchange resin within a desalter having high radioactivity is withdrawn through the action of an ejector and led to a solid-liquid separator for separation into used resin and water. The separated resin is directly collected in a storage tank while the separated water is forced through a circulating pump to a gas-liquid separator for separation into gas having radioactivity and water. The separated gas is led to a radioactive gas treatment station while the water deprived of the gas is recirculated by a drive water pump for repeated use.

  1. Simple gas chromatographic method for furfural analysis.

    Science.gov (United States)

    Gaspar, Elvira M S M; Lopes, João F

    2009-04-03

    A new, simple, gas chromatographic method was developed for the direct analysis of 5-hydroxymethylfurfural (5-HMF), 2-furfural (2-F) and 5-methylfurfural (5-MF) in liquid and water soluble foods, using direct immersion SPME coupled to GC-FID and/or GC-TOF-MS. The fiber (DVB/CAR/PDMS) conditions were optimized: pH effect, temperature, adsorption and desorption times. The method is simple and accurate (RSDfurfurals will contribute to characterise and quantify their presence in the human diet.

  2. 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

  3. 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.

  4. 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.

  5. 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

  6. 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.

  7. 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)

  8. 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.

  9. 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.)

  10. 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).

  11. 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)

  12. 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

  13. 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

  14. Determination of solute descriptors by chromatographic methods

    International Nuclear Information System (INIS)

    Poole, Colin F.; Atapattu, Sanka N.; Poole, Salwa K.; Bell, Andrea K.

    2009-01-01

    The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298 K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

  15. Determination of solute descriptors by chromatographic methods.

    Science.gov (United States)

    Poole, Colin F; Atapattu, Sanka N; Poole, Salwa K; Bell, Andrea K

    2009-10-12

    The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

  16. Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

    Energy Technology Data Exchange (ETDEWEB)

    Pyo, Dong Jin; Lim, Chang Hyun [Kangwon National University, Chuncheon (Korea, Republic of)

    2005-02-15

    Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures.

  17. Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

    International Nuclear Information System (INIS)

    Pyo, Dong Jin; Lim, Chang Hyun

    2005-01-01

    Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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)

  3. 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.

  4. 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.

  5. 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)

  6. 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.

  7. 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.)

  8. 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)

  9. 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.

  10. 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

  11. 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.

  12. 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

  13. 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

  14. 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.

  15. 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.

  16. 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.

  17. 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

  18. 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.

  19. Chromatographic and electrophoretic approaches in ink analysis.

    Science.gov (United States)

    Zlotnick, J A; Smith, F P

    1999-10-15

    Inks are manufactured from a wide variety of substances that exhibit very different chemical behaviors. Inks designed for use in different writing instruments or printing methods have quite dissimilar components. Since the 1950s chromatographic and electrophoretic methods have played important roles in the analysis of inks, where compositional information may have bearing on the investigation of counterfeiting, fraud, forgery, and other crimes. Techniques such as paper chromatography and electrophoresis, thin-layer chromatography, high-performance liquid chromatography, gas chromatography, gel electrophoresis, and the relatively new technique of capillary electrophoresis have all been explored as possible avenues for the separation of components of inks. This paper reviews the components of different types of inks and applications of the above separation methods are reviewed.

  20. 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 ...

  1. 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.

  2. 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...

  3. Pyrolysis-gas chromatographic method for kerogen typing

    Energy Technology Data Exchange (ETDEWEB)

    Larter, S.R.; Douglas, A.G.

    1980-01-01

    The classification of kerogens according to their type and rank is important for the definition of any kerogen assemblage. Whereas optical methods of rank determination are well known, vitrinite reflectance and spore coloration being the most widely accepted chemical methods for typing kerogens are less developed. In this work we show that pyrograms, produced by pyrolyzing microgram quantities of solvent-extracted kerogens, enable not only their characterization in terms of a chromatographic fingerprint but also the production of a numerical type index determined as the ratio of m(+p)-xylene/n-octene (oct-1-ene) in the pyrogram. This index appears to be a close function of kerogen type. Type 3 kerogens (Tissot et al., 1974), including vitrinite, provide a high type index and have pyrolysates dominated by aromatic and phenolic compounds whereas type 1 kerogens provide an aliphatic-rich pyrolysate and consequently a low type index. The type index described here correlates well with microscopic and elemental analysis data and the pyrogram fingerprint provides an additional level of characterization not attainable with other current typing techniques.

  4. Liquid chromatographic determination of sennosides in Cassia angustifolia leaves.

    Science.gov (United States)

    Srivastava, Alpuna; Pandey, Richa; Verma, Ram K; Gupta, Madan M

    2006-01-01

    A simple liquid chromatographic method was developed for the determination of sennosides B and A in leaves of Cassia angustifolia. These compounds were extracted from leaves with a mixture of methanol-water (70 + 30, v/v) after defatting with hexane. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 270 nm using a photodiode array detector. The method involves the use of an RP-18 Lichrocart reversed-phase column (5 microm, 125 x 4.0 mm id) and a binary gradient mobile-phase profile. The various other aspects of analysis, namely, peak purity, similarity, recovery, repeatability, and robustness, were validated. Average recoveries of 98.5 and 98.6%, with a coefficient of variation of 0.8 and 0.3%, were obtained by spiking sample solution with 3 different concentration solutions of standards (60, 100, and 200 microg/mL). Detection limits were 10 microg/mL for sennoside B and 35 microg/mL for sennoside A, present in the sample solution. The quantitation limits were 28 and 100 microg/mL. The analytical method was applied to a large number of senna leaf samples. The new method provides a reliable tool for rapid screening of C. angustifolia samples in large numbers, which is needed in breeding/genetic engineering and genetic mapping experiments.

  5. Brazilian organic sugarcane spirits: Physicochemical and chromatographic profile

    Directory of Open Access Journals (Sweden)

    Felipe Cimino Duarte

    Full Text Available ABSTRACT There has been a growing demand for products from organic agriculture for the food market. Brazil leads the production of sugarcane spirits and produces about 1.6 billion liters/year. New technologies have been sought throughout the supply chain to improve production, and organic raw material has been used in the production of sugar cane for the production of beverages. This study aimed to define the physicochemical and chromatographic profiles of eleven organic sugarcane spirits samples from various Brazilian states. The secondary components and contaminants were identified and quantified through physicochemical analyses, HPLC and gas chromatography (GC. A significant percentage of the organic sugarcane spirits samples contained concentrations of components that were above the limits required by the Ministry of Agriculture, Livestock and Provisioning (MAPA, specifically the esters (18.20%, copper and dry extract (9.10%. This contamination is caused by bad conditions employed during the production process, which are not in compliance with the good manufacturing practices determined and legislated by Brazilian law.

  6. 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.

  7. 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)

  8. Method for loading resin beds

    International Nuclear Information System (INIS)

    Notz, K.J.; Rainey, R.H.; Greene, C.W.; Shockley, W.E.

    1978-01-01

    An improved method of preparing nuclear reactor fuel by carbonizing a uranium loaded cation exchange resin provided by contacting a H+ loaded resin with a uranyl nitrate solution deficient in nitrate, comprises providing the nitrate deficient solution by a method comprising the steps of reacting in a reaction zone maintained between about 145 to 200 0 C, a first aqueous component comprising a uranyl nitrate solution having a boiling point of at least 145 0 C with a second aqueous component to provide a gaseous phase containing HNO 3 and a reaction product comprising an aqueous uranyl nitrate solution deficient in nitrate

  9. 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.)

  10. 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.).

  11. 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 ...

  12. 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

  13. 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. 

  14. 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.

  15. 21 CFR 177.1680 - Polyurethane resins.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Polyurethane resins. 177.1680 Section 177.1680 Food... of Single and Repeated Use Food Contact Surfaces § 177.1680 Polyurethane resins. The polyurethane...) For the purpose of this section, polyurethane resins are those produced when one or more of the...

  16. Method of removing contaminants from plastic resins

    Science.gov (United States)

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

    2008-11-18

    A method for removing contaminants from synthetic resin material containers using a first organic solvent system and a second carbon dioxide system. The organic solvent is utilized for removing the contaminants from the synthetic resin material and the carbon dioxide is used to separate any residual organic solvent from the synthetic resin material.

  17. Method for removing contaminants from plastic resin

    Science.gov (United States)

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

    2008-12-30

    A method for removing contaminants from synthetic resin material containers using a first organic solvent system and a second carbon dioxide system. The organic solvent is utilized for removing the contaminants from the synthetic resin material and the carbon dioxide is used to separate any residual organic solvent from the synthetic resin material.

  18. 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.

  19. Resins production: batch plant automation

    International Nuclear Information System (INIS)

    Banti, M.; Mauri, G.

    1996-01-01

    Companies that look for automation in their plants without external resources, have at their disposal flexible, custom and easy to use DCS, open towards PLC. In this article it is explained why Hoechts has followed this way of new plants for resins production automation

  20. Occupational exposure to epoxy resins

    NARCIS (Netherlands)

    Terwoert, J.; Kersting, K.

    2014-01-01

    Products based on epoxy resins as a binder have become popular in various settings, among which the construction industry and in windmill blade production, as a result of their excellent technical properties. However, due to the same properties epoxy products are a notorious cause of allergic skin

  1. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Ying [Iowa State Univ., Ames, IA (United States)

    2004-01-01

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  2. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    International Nuclear Information System (INIS)

    Ying Liu

    2004-01-01

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  3. 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.

  4. ANÁLISIS POR CG/EM Y ACTIVIDAD ANTIMICROBIANA DE ALGUNAS FRACCIONES DEL EXTRACTO EN ACETATO DE ETILO DE Pseudopterogorgia acerosa I ANALYSIS BY GC/MS AND ANTIMICROBIAL ACTIVITY OF SOME ChROMATOGRAPhIC FRACTIONS OF ThE Pseudopterogorgia acerosa EThYL ACETATE EXTRACT

    Directory of Open Access Journals (Sweden)

    Gabriel Ordaz

    2014-02-01

    Full Text Available Psudopterogorgia acerosa, showed antimicrobial activity against Salmonella enteritidis, Bacillus subtlis, Staphylococcus aureus and Citrobacter freundii bacteria and the fungus Candida albicans, indicating the presence of bioactive constituents in these fractions. Moreover, the GC/MS analysis of some subfractions obtained through continuous chromatographic separation., allowed the identification of the constituents: pristane, bis(3,5,5-trimethylhexyl ether, 4-octadecanolide, tricloroeicosylsilane, (2-endo,7-exo-7-ethyl-2,4-dimethyl-6,8-dioxabycicle[3,2,1]oct-3-ene,1-methoxy-12-octoherbertene, butylphtalylbutylglycolate, N-methyl-N-(4-(4-methoxy-1-hexahydropyridil-2-butynylacetamide, diisobutylphtalate, 3-(4-(diphenylmethylphenyl-1-phenyl-4,4-dimethyl-1-pentanone, by comparison with WILEY databases and the study of the patterns of fragmentation of their mass spectra

  5. A liquid chromatographic method for determination of theophylline in serum and capillary blood--a comparison.

    Science.gov (United States)

    Gartzke, J; Jäger, H; Vins, I

    1991-01-01

    A simple, fast and reliable liquid chromatographic method for the determination of theophylline in serum and capillary blood after a solid phase extraction is described for therapeutic drug monitoring. The employment of capillary blood permits the determination of an individual drug profile and other pharmacokinetic studies in neonates and infants. There were no differences in venous- and capillary-blood levels but these values compared poorly with those in serum. An adjustment of the results by correction of the different volumes of serum and blood by haematocrit was unsuccessful. Differences in the binding of theophylline to erythrocytes could be an explanation for the differences in serum at blood levels of theophylline.

  6. 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.

  7. 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.

  8. Commercial Ion Exchange Resin Vitrification Studies

    International Nuclear Information System (INIS)

    Cicero-Herman, C.A

    2002-01-01

    In the nuclear industry, ion exchange resins are used for purification of aqueous streams. The major contaminants of the resins are usually the radioactive materials that are removed from the aqueous streams. The use of the ion exchange resins creates a waste stream that can be very high in both organic and radioactive constituents. Therefore, disposal of the spent resin often becomes an economic problem because of the large volumes of resin produced and the relatively few technologies that are capable of economically stabilizing this waste. Vitrification of this waste stream presents a reasonable disposal alternative because of its inherent destruction capabilities, the volume reductions obtainable, and the durable product that it produces

  9. 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)

  10. 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.

  11. 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)

  12. Method for chromatographically recovering scandium and yttrium

    International Nuclear Information System (INIS)

    Snyder, T.S.; Stoltz, R.A.

    1991-01-01

    This paper describes a method for chromatographically recovering scandium and yttrium from the residue of a sand chlorinator. It comprises: providing a residue from a sand chlorinator, the residue containing scandium, yttrium, sodium, calcium and at least one radioactive metal of the group consisting of radium, thorium and uranium; digesting the residue with an acid to produce an aqueous liquid containing scandium, yttrium, sodium, calcium and at least one radioactive metal of the group consisting of radium, thorium and uranium; feeding the metal containing liquid through a cation exchanger; eluding the cation exchanger with an acid eluant to to produce: a first eluate containing at least half of the total weight of the calcium and sodium in the feed liquid; a second eluate containing at least half of the total weight of the one or more radioactive metals in the feed liquid; a third eluate containing at least half of the yttrium in the feed liquid, and a fourth eluate containing at least half of the weight of the scandium in the feed liquid

  13. Chromatographic Techniques for Rare Earth Elements Analysis

    Science.gov (United States)

    Chen, Beibei; He, Man; Zhang, Huashan; Jiang, Zucheng; Hu, Bin

    2017-04-01

    The present capability of rare earth element (REE) analysis has been achieved by the development of two instrumental techniques. The efficiency of spectroscopic methods was extraordinarily improved for the detection and determination of REE traces in various materials. On the other hand, the determination of REEs very often depends on the preconcentration and separation of REEs, and chromatographic techniques are very powerful tools for the separation of REEs. By coupling with sensitive detectors, many ambitious analytical tasks can be fulfilled. Liquid chromatography is the most widely used technique. Different combinations of stationary phases and mobile phases could be used in ion exchange chromatography, ion chromatography, ion-pair reverse-phase chromatography and some other techniques. The application of gas chromatography is limited because only volatile compounds of REEs can be separated. Thin-layer and paper chromatography are techniques that cannot be directly coupled with suitable detectors, which limit their applications. For special demands, separations can be performed by capillary electrophoresis, which has very high separation efficiency.

  14. Chromatographic Separation of Vitamin E Enantiomers

    Directory of Open Access Journals (Sweden)

    Ju-Yen Fu

    2017-02-01

    Full Text Available Vitamin E is recognized as an essential vitamin since its discovery in 1922. Most vegetable oils contain a mixture of tocopherols and tocotrienols in the vitamin E composition. Structurally, tocopherols and tocotrienols share a similar chromanol ring and a side chain at the C-2 position. Owing to the three chiral centers in tocopherols, they can appear as eight different stereoisomers. Plant sources of tocopherol are naturally occurring in the form of RRR while synthetic tocopherols are usually in the form of all-racemic mixture. Similarly, with only one chiral center, natural tocotrienols occur as the R-isoform. In this review, we aim to discuss a few chromatographic methods that had been used to separate the stereoisomers of tocopherols and tocotrienols. These methods include high performance liquid chromatography, gas chromatography and combination of both. The review will focus on method development including selection of chiral columns, detection method and choice of elution solvent in the context of separation efficiency, resolution and chiral purity. The applications for separation of enantiomers in vitamin E will also be discussed especially in terms of the distinctive biological potency among the stereoisoforms.

  15. 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

  16. Spray drying of bead resins: feasibility tests

    International Nuclear Information System (INIS)

    Gay, R.L.; Grantham, L.F.; Jones, L.J.

    1984-01-01

    Rockwell International has developed a volume reduction system for low-level reactor wastes based on drying the wastes in a heated-air spray dryer. The drying of slurries of sodium sulfate, boric acid, and powdered ion exchange resins was demonstrated in previous tests. The drying of bead ion exchange resins can be especially difficult due to the relatively large size of bead resins (about 500 to 800 microns) and their natural affinity for water. This water becomes part of the pore structure of the resins and normally comprises 50 t 60 wt % of the resin weight. A 76-cm-diameter spray dryer was used for feasibility tests of spray drying of cation and anion bead resins. These resins were fed to the dryer in the as-received form (similar to dewatered resins) and as slurries. A dry, free-flowing product was produced in all the tests. The volume of the spray-dried product was one-half to one-third the volume of the as-received material. An economic analysis was made of the potential cost savings that can be achieved using the Rockwel spray dryer system. In-plant costs, transportation costs, and burial costs of spray-dried resins were compared to similar costs for disposal of dewatered resins. A typical utility producing 170 m 3 (6,000 ft 3 ) per year of dewatered resins can save $600,000 to $700,000 per year using this volume reduction system

  17. 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.

  18. Chromatographic separation of low-temperature tar. Part II

    Energy Technology Data Exchange (ETDEWEB)

    Terres, E; Gebert, F; Huelsemann, H; Petereit, H; Toepsch, H; Ruppert, W

    1955-01-01

    Chromatographic methods and apparatus are discussed. The Folin-Denis reagent (Na tungstate molybdate in H/sub 3/PO/sub 4/) is used for developing paper chromatograms of phenol mixtures. Other reagents are given.

  19. 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)

  20. Isolation of Triterpenoid Glycoside from Bark of Terminalia arjuna using Chromatographic Technique and Investigation of Pharmacological Behavior upon Muscle Tissues

    Directory of Open Access Journals (Sweden)

    Tanushree Patnaik

    2007-01-01

    Full Text Available This study reports the isolation and characterization of a new triterpenoid glycoside extracted from the bark of Terminalia arjuna. The isolation of the organic compounds was done using simple chromatographic technique. Compound characterization using various spectroscopic technique identify the final isolated compound as Olean-3β,22β-diol-12-en-28β-D-glucopyranoside-oic acid. The method of isolation is simple, cost effective and efficient. The preliminary bioactivity of the compound was also evaluated.

  1. 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.)

  2. 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.

  3. [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.

  4. 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.

  5. Ion Chromatographic Analyses of Sea Waters, Brines and Related Samples

    OpenAIRE

    Nataša Gros

    2013-01-01

    This review focuses on the ion chromatographic methods for the analyses of natural waters with high ionic strength. At the beginning a natural diversity in ionic composition of waters is highlighted and terminology clarified. In continuation a brief overview of other review articles of potential interest is given. A review of ion chromatographic methods is organized in four sections. The first section comprises articles focused on the determination of ionic composition of water samples as com...

  6. Analysis and chromatographic purification of eicosanoids multiply labeled by tritium

    International Nuclear Information System (INIS)

    Shevchenko, V.P.; Nagaev, I.Yu.; Myasoedov, N.F.

    1989-01-01

    We show the possibility of analysis and chromatographic purification of eicosanoids triply labeled by tritium. The described methods allow us to isolate chromatographically pure products obtained by selective hydrogenatin, chemical, and enzyme methods, with radiochemical purity at least 95-97%. The following methods are used to analyze the reaction mixtures and to isolate the tritium-labeled eicosanoids: gas-liquid chromatography, high-efficiency liquid chromatography, and thin-layer chromatography on supports impregnated with silver nitrate

  7. 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

  8. 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.

  9. Liquid chromatographic determination of seven antioxidants in dry food.

    Science.gov (United States)

    Page, B D; Charbonneau, C F

    1989-01-01

    The liquid chromatographic determinative step of the official method for propyl gallate, trihydroxybutyrophenone, tert-butylhydroquinone, nordihydroguaiaretic acid, butylated hydroxyanisole (BHA), 3,5-di-tert-butyl-4-hydroxymethylphenol, and butylated hydroxytoluene (BHT) in fats and oils has been applied to their determination in a number of dry foods. A representative sample (10 g) is homogenized first with hexane (25 mL), then with 5 mL added water, and finally with 75 mL added acetonitrile. The hexane and acetonitrile are decanted, filtered, and separated; the hexane and rehydrated food are reextracted with 2 additional portions of acetonitrile, and the combined acetonitrile extracts are concentrated and diluted to 10 mL. An aliquot is analyzed as described in the official method, using a 150 x 4.6 mm 5 microns C-18 column. The need for rehydration to maximize the recovery of BHA and other antioxidants from marketplace dry food samples such as potato flakes, dry coffee whiteners, and dessert topping mixes was demonstrated. Rehydration was not required for cheese snacks, breakfast cereals, cake mixes, and some other foods. The need for rehydration should be determined by analyzing other foods with and without the addition of water. Potato and corn chips, popcorn and cheese snacks, breakfast cereals, dry beverage mixes, rice, potato flakes, french fried potatoes, and cake mixes were spiked with the above antioxidants at 10-50 ppm. Overall recoveries ranged from 64.3 to 105.6% and repeatabilities ranged from 0.7 to 10.8%. A total of 109 samples of the above foods were analyzed, and 64% contained detectable (greater than 1-2 ppm) antioxidants, mainly BHA and BHT.

  10. 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

  11. 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.

  12. 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.

  13. 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.

  14. Chromatographic 188W →188Re generator

    International Nuclear Information System (INIS)

    Khujaev, S.

    2005-01-01

    Full text: The main purpose of the generator - reception of daughter radioisotope Rhenium-188 from it by periodic elution for a long period of time (more than half-year). It is generally known that Rhenium-188, in the form of its complex connections, is applied in nuclear medicine in treatment and removal of painful syndromes. The generator possesses convenient nuclear-physical characteristics of a daughter radioisotope Rhenium-188. It is a source of (Irradiation with energy 2.12 MeV (98 %) with small contribution soft γ-radiation with energy 0.155 MeV (15 %). The Period of half-life destruction of radioisotope is 17 hours. The 188 W parent radioisotope for the generator is formed by irradiation of 186 W neutrons based on the following reaction: 186 W (n,γ) 187 W (n,γ) 188 W (69 days) → 188 Re (17 hours) + β The following were used as targets for irradiation: 1) Metal Tungsten (powder) of natural structure; 2) Metal Tungsten (plate) of natural structure; 3) Metal Tungsten (wire) of natural structure, d = 12 mm; 4) Metal Tungsten (powder) with enrichment on isotope 186 W - 99.79 %. The irradiated material was exposed to chemical processing with reception of radioactive solution of tungsten-188, from which sorption Tungsten was carried out onto sorbent as poly-wolframate-ions. It is established that Tungsten sorption depends on many factors as there are various chemical forms of Tungsten (VI) in water solutions, ratio of which depends on pH of the solution, concentration of Tungsten in the solution and presence of foreign ions. Tungsten sorption was carried out in static and in dynamic regimes. At dynamic regime the sorbent was placed directly in the generating column. The generator consisted of chromatographic columns with sorbent and radioisotope 188 W, eluting system and radiation protection. Rhenium-188 was taken from the generator as perrhenate sodium by elution of 0.9 % solution of chloride sodium in 10 ml. Technical characteristics of the generator

  15. 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, ...

  16. Solidifying power station resins and sludges

    International Nuclear Information System (INIS)

    Willis, A.S.D.; Haigh, C.P.

    1984-01-01

    Radioactive ion exchange resins and sludges arise at nuclear power stations from various operations associated with effluent treatment and liquid waste management. As the result of an intensive development programme, the Central Electricity Generating Board (CEGB) has designed a process to convert power station resins and sludges into a shielded, packaged solid monolithic form suitable for final disposal. Research and development, the generic CEGB sludge/resin conditioning plant and the CEGB Active Waste Project are described. (U.K.)

  17. Volumetric polymerization shrinkage of contemporary composite resins

    OpenAIRE

    Nagem Filho, Halim; Nagem, Haline Drumond; Francisconi, Paulo Afonso Silveira; Franco, Eduardo Batista; Mondelli, Rafael Francisco Lia; Coutinho, Kennedy Queiroz

    2007-01-01

    The polymerization shrinkage of composite resins may affect negatively the clinical outcome of the restoration. Extensive research has been carried out to develop new formulations of composite resins in order to provide good handling characteristics and some dimensional stability during polymerization. The purpose of this study was to analyze, in vitro, the magnitude of the volumetric polymerization shrinkage of 7 contemporary composite resins (Definite, Suprafill, SureFil, Filtek Z250, Fill ...

  18. 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.

  19. 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.

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

    International Nuclear Information System (INIS)

    Takatsu, Akiko; Nishi, Sueo

    1988-01-01

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

  1. Headspace solid-phase microextraction procedures for gas chromatographic analysis of biological fluids and materials.

    Science.gov (United States)

    Mills, G A; Walker, V

    2000-12-01

    Solid-phase microextraction (SPME) is a new solventless sample preparation technique that is finding wide usage. This review provides updated information on headspace SPME with gas chromatographic separation for the extraction and measurement of volatile and semivolatile analytes in biological fluids and materials. Firstly the background to the technique is given in terms of apparatus, fibres used, extraction conditions and derivatisation procedures. Then the different matrices, urine, blood, faeces, breast milk, hair, breath and saliva are considered separately. For each, methods appropriate for the analysis of drugs and metabolites, solvents and chemicals, anaesthetics, pesticides, organometallics and endogenous compounds are reviewed and the main experimental conditions outlined with specific examples. Then finally, the future potential of SPME for the analysis of biological samples in terms of the development of new devices and fibre chemistries and its coupling with high-performance liquid chromatography is discussed.

  2. 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

  3. 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)

  4. The absorption of plutonium by anion resins

    Energy Technology Data Exchange (ETDEWEB)

    Durham, R. W.; Mills, R.

    1961-10-15

    Equilibrium experiments have shown Pu{sup +4} to be absorbed from nitric acid onto an anion resin as a complex anion Pu(NO{sub 3}){sub 6}{sup -2}. The amount of absorption is dependent on the plutonium and nitric acid concentrations in the equilibrium solution with a maximum at 7N to 8N HNO{sub 3}. A low cross-linked resin has a higher capacity and reaches equilibrium more rapidly than the normally supplied resin. Saturation capacity of one per cent cross-linked Nalcite SBR (Dowex 1), 50 -- 100 mesh, is 385 mg Pu/gram dry resin. (author)

  5. 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.

  6. 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

  7. 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

  8. 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.

  9. 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.

  10. 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

  11. 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.

  12. Direct chromatographic analysis of metabolites of lipophilic tracers in whole blood by ISRP chromatography

    International Nuclear Information System (INIS)

    Rosenspire, K.C.; Hirth, W.; Jurisson, S.; Nowotnik, D.P.; Eckelman, W.C.; Nunn, A.D.

    1991-01-01

    HPLC using columns packed with 5 μ Internal Surface Reverse Phase (ISRP) resin have shown utility in the analysis of lipophilic drugs and their metabolites by direct injection of serum or plasma samples. We have developed a method for rapid on-line separation of small hydrophobic components from cellular whole blood components. This is achieved through the use of 75 μ GFF (glycine-phenylalanine-phenylalanine) glass bead ISRP chromatographic material packed into a small HPLC column, and used in conjunction with an HPLC system containing a switching valve and a second analytical column. When heparinized whole blood is applied to a 75 μ GFF ISRP column, and the column eluted with an isotonic eluent, lipophilic compounds free in plasma are retained by the column, while plasma proteins, blood cells, and compounds bound to these blood components pass through the ISRP column. Following the elution of these components, the lipophilic compounds retained on the ISRP column are eluted by increasing the percentage of organic solvent in the eluent, and are further resolved (if required) by the analytical column. We have applied this analytical method to the study of metabolism of the 99m Tc-BATO (Boronic acid Adducts of Technetium diOxime) cerebral and myocardial perfusion tracers. (author)

  13. 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...

  14. Artificial saliva effect on toxic substances release from acrylic resins

    Directory of Open Access Journals (Sweden)

    Kostić Milena

    2015-01-01

    Full Text Available Background/Aim. Acrylic-based resins are intensively used in dentistry practice as restorative or denture-base materials. The purpose of this study was to analyze the surface structure of denture base resins and the amount of released potentially toxic substances (PTS immediately upon polymerization and incubation in different types of artificial saliva. Methods. Storage of acrylic samples in two models of artificial saliva were performed in a water bath at the temperature of 37 ± 1°C. Analysis of the surface structure of samples was carried out using scanning electronic microscopy analysis immediately after polymerization and after the 30-day incubation. The amounts of PTS per day, week and month extracts were measured using high-pressure liquid chromatography. Results. Surface design and amount of PTS in acrylic materials were different and depended on the types and duration of polymerization. The surfaces of tested acrylates became flatter after immersing in solutions of artificial saliva. The degree of acrylic materials release was not dependent on the applied model of artificial saliva. Conclusion. In order to improve biological features of acrylic resin materials, it was recommended that dentures lined with soft or hard coldpolymerized acrylates should be kept at least 1 to 7 days in water before being given to a patient. So, as to reach high degree of biocompatibility preparation of prosthetic restorations from heat-polymerized acrylate was unnecessary. [Projekat Ministarstva nauke Republike Srbije, br. 41017

  15. Elution of monomer from different bulk fill dental composite resins.

    Science.gov (United States)

    Cebe, Mehmet Ata; Cebe, Fatma; Cengiz, Mehmet Fatih; Cetin, Ali Rıza; Arpag, Osman Fatih; Ozturk, Bora

    2015-07-01

    The purpose of this study was to evaluate the elution of Bis-GMA, TEGDMA, HEMA, and Bis-EMA monomers from six bulk fill composite resins over four different time periods, using HPLC. Six different composite resin materials were used in the present study: Tetric Evo Ceram Bulk Fill (Ivoclar Vivadent, Amherst, NY), X-tra Fill (VOCO, Cuxhaven, Germany), Sonic Fill (Kerr, Orange, CA, USA), Filtek Bulk Fill (3M ESPE Dental Product, St. Paul, MN), SDR (Dentsply, Konstanz, Germany), EQUIA (GC America INC, Alsip, IL). The samples (4mm thickness, 5mm diameter) were prepared and polymerized for 20s with a light emitted diode unit. After fabrication, each sample was immediately immersed in 75wt% ethanol/water solution used as extraction fluid and stored in the amber colored bottles at room temperature. Ethanol/water samples were taken (0.5mL) at predefined time intervals:10m (T1), 1h (T2), 24h (T3) and 30 days (T4). These samples were analyzed by HPLC. The obtained data were analyzed with one-way ANOVA and Tukey HSD at significance level of pcomposites (pcomposite resins in all time periods and the amount of eluted monomers was increased with time. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  16. 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

    Different solvents were used in paper chromatographic methods to obtain the best system in routine radiochemical control for 131 I-MIBG produced at IPEN-CNEN/SP. The dates were compared with those obtained with eletrophoresis method in buffer acetate, pH=4.5, 350V, during 40 minutes. The stability of the labeled compound store under 4 0 C was studied during 15 days. Miniaturized chromatographic procedures were established using Whatman 3MM (8x1cm) and n-butanol-:acetic acid: water (S:2:1) as a solvent. the Rf values were: 0.3 (I - ) and 1.0 (MIBG). The radiochemical purity was 99.3 and 99.2% (first day) obtained with eletrophoresis and miniaturized chromatographic procedures, respectively and, 84.7% after 15 days of its preparation. It is a rapid, practical and reproductive method. (author) [pt

  17. 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.

  18. 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)

  19. Treatment of liquids of exchange resins washing from RA6

    International Nuclear Information System (INIS)

    Becker, F.L.; Menghini, J.; Rodriguez, D.S.

    2012-01-01

    In this work nanometric magnetite nanoparticles have been synthesized by hydrochemical co-precipitation method to achieve the adsorption and extraction of the contaminant species present in the water coming from the regeneration of exchange resins in Research Reactor RA6. It has been possible to obtain a mean nanoparticle size of 16 nm, necessary to increase the specific surface area of the material and thus, its adsorbent capability. The synthesis parameters and adsorption conditions made it possible to achieve a treatment efficiency superior to 80% for Cs-137 (author)

  20. 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.

  1. 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

  2. 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.

  3. 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

  4. On-line gas chromatographic analysis of airborne particles

    Science.gov (United States)

    Hering, Susanne V [Berkeley, CA; Goldstein, Allen H [Orinda, CA

    2012-01-03

    A method and apparatus for the in-situ, chemical analysis of an aerosol. The method may include the steps of: collecting an aerosol; thermally desorbing the aerosol into a carrier gas to provide desorbed aerosol material; transporting the desorbed aerosol material onto the head of a gas chromatography column; analyzing the aerosol material using a gas chromatograph, and quantizing the aerosol material as it evolves from the gas chromatography column. The apparatus includes a collection and thermal desorption cell, a gas chromatograph including a gas chromatography column, heated transport lines coupling the cell and the column; and a quantization detector for aerosol material evolving from the gas chromatography column.

  5. Properties of the Carboxylate ion exchange resins; Karboxylatjonbytarmassans egenskaper

    Energy Technology Data Exchange (ETDEWEB)

    Allard, Bert; Dario, Maarten [Oerebro Univ. (Sweden); Boren, Hans [Linkoepings Univ. (Sweden); Torstenfelt, Boerje [Swedpower, Stockholm (Sweden); Puigdomenech, Ignasi; Johansson, Claes [Swedish Nuclear Fuel and Waste Management Co., Stockholm (Sweden)

    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)

  6. 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.

  7. 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

  8. 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

  9. 21 CFR 177.1655 - Polysulfone resins.

    Science.gov (United States)

    2010-04-01

    ... disodium salt of 4,4′-isopropylidenediphenol is made to react with 4,4′-dichlorodiphenyl sulfone in such a... Limitations Dimethyl sulfoxide Not to exceed 50 parts per million as residual solvent in finished basic resin... residual solvent in finished basic resin in paragraph (a)(1) of this section. N-methyl-2-pyrrolidone Not to...

  10. 21 CFR 177.1580 - Polycarbonate resins.

    Science.gov (United States)

    2010-04-01

    ...′-iso-propylidenediphenol with molten diphenyl carbonate in the presence of the disodium salt of 4,4... chloride Monochlorobenzene Not to exceed 500 p.p.m. as residual solvent in finished resin. Pentaerythritol...-88-3) Not to exceed 800 parts per million as residual solvent in finished resin. Triethylamine (c...

  11. 21 CFR 177.1595 - Polyetherimide resin.

    Science.gov (United States)

    2010-04-01

    ... polyetherimide resin identified in this section may be safely used as an article or component of an article... substances required in the production of basic resins or finished food-contact articles. The optional... and Applied Nutrition (HFS-200), Food and Drug Administration, 5100 Paint Branch Pkwy., College Park...

  12. 21 CFR 177.2440 - Polyethersulfone resins.

    Science.gov (United States)

    2010-04-01

    ... Components of Articles Intended for Repeated Use § 177.2440 Polyethersulfone resins. Polyethersulfone resins identified in paragraph (a) of this section may be safely used as articles or components of articles intended... Petition Control (HFS-215), Center for Food Safety and Applied Nutrition, 1110 Vermont Ave. NW., suite 1200...

  13. 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.

  14. Extraction and Purification of Flavonoids from Radix Puerariae

    African Journals Online (AJOL)

    and preparations are now on sale. ... significant for optimization of extraction, resin selection and ... and flavonoids as indexes, optimize the proper density. ..... system. Sep Purif Technol. 2008; 62: 590-595. 12. Chen JH, Liau BC, Jong TT.

  15. Embedding of reactor wastes in plastic resins

    International Nuclear Information System (INIS)

    1979-01-01

    STEAG Kernenergie GmbH is so far the only firm commercially to condition radioactive bead ion exchange resins by embedding in polystyrene resins. The objective of the work reported here was to study and develop methods for immobilization of other reactor wastes in plastic resins. Comparison studies on high quality cement however showed favourable results for cement with respect to process safety and economy. For this reason STEAG interrupted its work in the field of resin embedding after about one year. The work carried out during this period is surveyed in this report, which includes a comprehensive literature study on reactor wastes and their solidification in plastic resins as well as on regulations with regard to radioactive waste disposal in the member states of the European Communities

  16. Chemoviscosity modeling for thermosetting resins, 2

    Science.gov (United States)

    Hou, T. H.

    1985-01-01

    A new analytical model for simulating chemoviscosity of thermosetting resin was formulated. The model is developed by modifying the Williams-Landel-Ferry (WLF) theory in polymer rheology for thermoplastic materials. By assuming a linear relationship between the glass transition temperature and the degree of cure of the resin system under cure, the WLF theory can be modified to account for the factor of reaction time. Temperature dependent functions of the modified WLF theory constants were determined from the isothermal cure data of Lee, Loos, and Springer for the Hercules 3501-6 resin system. Theoretical predictions of the model for the resin under dynamic heating cure cycles were shown to compare favorably with the experimental data reported by Carpenter. A chemoviscosity model which is capable of not only describing viscosity profiles accurately under various cure cycles, but also correlating viscosity data to the changes of physical properties associated with the structural transformations of the thermosetting resin systems during cure was established.

  17. Electrodialytic decontamination of spent ion exchange resins

    International Nuclear Information System (INIS)

    Nott, B.R.

    1982-01-01

    Development of a novel electrodialytic decontamination process for the selective removal of radioactive Cs from spent ion exchange resins containing large amounts of Li is described. The process involves passage of a dc electric current through a bed of the spent ion exchange resin in a specially designed electrodialytic cell. The radiocesium so removed from a volume of the spent resin is concentrated onto a much smaller volume of a Cs selective sorbent to achieve a significant radioactive waste volume reduction. Technical feasibility of the electrodialytic resin decontamination process has been demonstrated on a bench scale with a batch of simulated spent ion exchange resin and using potassium cobalt ferrocyanide as the Cs selective sorbent. A volume reduction factor between 10 and 17 has been estimated. The process appears to be economically attractive. Improvements in process economics can be expected from optimization of the process. Other possible applications of the EDRD process have been identified

  18. Chromatographic Methods for the Analysis of Polyphenols in Wines

    Directory of Open Access Journals (Sweden)

    Medić-Šarić, M.

    2009-03-01

    Full Text Available Wine is an excellent source of various classes of polyphenols, including phenolic acids, flavonoids, and trihydroxystilbene resveratrol (Fig.1. Polyphenols play a major role in wine quality since they contribute to the sensory characteristics of wine, particularly color and astringency. A recent interest in these substances has been stimulated by abundant evidence of their beneficial effects on human health, such as anticarcinogenic, antiinflamatory and antimicrobial activities. Therefore, numerous studies have been performed in the attempt to analyze polyphenols in wine. This paper reviews the current advances in the determination of polyphenols in wine by the major chromatographic techniques such as thin-layer chromatography (TLC and high-performance liquid chromatography (HPLC.The great complexity of the polyphenolic content of wine and the difficulty in obtaining some of the standards usually require sample preparation before analysis. Two methods for sample preparation, liquid-liquid extraction and solid-phase extraction, are most commonly applied. Hydrolysis is applied frequently, but not exclusively, to remove the sugar moieties from glycosides.TLC on silica gel plates is useful for the rapid and low-cost separation and identification of the polyphenols present in wine (Fig. 2. Densitometric quantitative analysis of polyphenols in wine extracts is usually performed by scanning the TLC plates with UV light at wavelengths of 350–365 nm or 250–260 nm (Fig. 3. For the evaluation of the most efficient mobile phase and an optimal choice of the combination of two or more mobile phases, two methods may be applied: information theory and numerical taxonomy. HPLC currently represents the most popular technique for the analysis of polyphenols in wine. For this purpose, a reversed-phase HPLC method that uses gradient elution with binary elution system is usually employed. Routine detection is based on measurement of UV-Vis absorption with a diode

  19. Solidification of ion exchange resin wastes

    International Nuclear Information System (INIS)

    1982-08-01

    Solidification media investigated included portland type I, portland type III and high alumina cements, a proprietary gypsum-based polymer modified cement, and a vinyl ester-styrene thermosetting plastic. Samples formulated with hydraulic cement were analyzed to investigate the effects of resin type, resin loading, waste-to-cement ratio, and water-to-cement ratio. The solidification of cation resin wastes with portland cement was characterized by excessive swelling and cracking of waste forms, both after curing and during immersion testing. Mixed bed resin waste formulations were limited by their cation component. Additives to improve the mechanical properties of portland cement-ion exchange resin waste forms were evaluated. High alumina cement formulations dislayed a resistance to deterioration of mechanical integrity during immersion testing, thus providing a significant advantage over portland cements for the solidification of resin wastes. Properties of cement-ion exchange resin waste forms were examined. An experiment was conducted to study the leachability of 137 Cs, 85 Sr, and 60 Co from resins modified in portland type III and high alumina cements. The cumulative 137 Cs fraction release was at least an order of magnitude greater than that of either 85 Sr or 60 Co. Release rates of 137 Cs in high alumina cement were greater than those in portland III cement by a factor of two.Compressive strength and leach testing were conducted for resin wastes solidified with polymer-modified gypsum based cement. 137 Cs, 85 Sr, and 60 Co fraction releases were about one, two and three orders of magnitude higher, respectively, than in equivalent portland type III cement formulations. As much as 28.6 wt % dry ion exchange resin was successfully solidified using vinyl ester-styrene compared with a maximum of 25 wt % in both portland and gypsum-based cement

  20. Chemometrics and chromatographic fingerprints to classify plant food supplements according to the content of regulated plants.

    Science.gov (United States)

    Deconinck, E; Sokeng Djiogo, C A; Courselle, P

    2017-09-05

    Plant food supplements are gaining popularity, resulting in a broader spectrum of available products and an increased consumption. Next to the problem of adulteration of these products with synthetic drugs the presence of regulated or toxic plants is an important issue, especially when the products are purchased from irregular sources. This paper focusses on this problem by using specific chromatographic fingerprints for five targeted plants and chemometric classification techniques in order to extract the important information from the fingerprints and determine the presence of the targeted plants in plant food supplements in an objective way. Two approaches were followed: (1) a multiclass model, (2) 2-class model for each of the targeted plants separately. For both approaches good classification models were obtained, especially when using SIMCA and PLS-DA. For each model, misclassification rates for the external test set of maximum one sample could be obtained. The models were applied to five real samples resulting in the identification of the correct plants, confirmed by mass spectrometry. Therefore chromatographic fingerprinting combined with chemometric modelling can be considered interesting to make a more objective decision on whether a regulated plant is present in a plant food supplement or not, especially when no mass spectrometry equipment is available. The results suggest also that the use of a battery of 2-class models to screen for several plants is the approach to be preferred. Copyright © 2017 Elsevier B.V. All rights reserved.