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Sample records for silicic acid chromatography

  1. Biological and therapeutic effects of ortho-silicic acid and some ortho-silicic acid-releasing compounds: New perspectives for therapy

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    Jurkić Lela Munjas

    2013-01-01

    Full Text Available Abstract Silicon (Si is the most abundant element present in the Earth's crust besides oxygen. However, the exact biological roles of silicon remain unknown. Moreover, the ortho-silicic acid (H4SiO4, as a major form of bioavailable silicon for both humans and animals, has not been given adequate attention so far. Silicon has already been associated with bone mineralization, collagen synthesis, skin, hair and nails health atherosclerosis, Alzheimer disease, immune system enhancement, and with some other disorders or pharmacological effects. Beside the ortho-silicic acid and its stabilized formulations such as choline chloride-stabilized ortho-silicic acid and sodium or potassium silicates (e.g. M2SiO3; M= Na,K, the most important sources that release ortho-silicic acid as a bioavailable form of silicon are: colloidal silicic acid (hydrated silica gel, silica gel (amorphous silicon dioxide, and zeolites. Although all these compounds are characterized by substantial water insolubility, they release small, but significant, equilibrium concentration of ortho-silicic acid (H4SiO4 in contact with water and physiological fluids. Even though certain pharmacological effects of these compounds might be attributed to specific structural characteristics that result in profound adsorption and absorption properties, they all exhibit similar pharmacological profiles readily comparable to ortho-silicic acid effects. The most unusual ortho-silicic acid-releasing agents are certain types of zeolites, a class of aluminosilicates with well described ion(cation-exchange properties. Numerous biological activities of some types of zeolites documented so far might probably be attributable to the ortho-silicic acid-releasing property. In this review, we therefore discuss biological and potential therapeutic effects of ortho-silicic acid and ortho-silicic acid -releasing silicon compounds as its major natural sources.

  2. Effects of Calcium Lignosulfonate and Silicic Acid on Ammonium Nitrate Degradation

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    Ahmet Ozan Gezerman

    2014-01-01

    Full Text Available Ammonium nitrate salts are the most commonly used nitrogenous fertilizers in industry. However, storage of ammonium nitrate is problematic, since its initial properties can decline because of environmental factors, leading to large economic losses. In this study, in order to prevent the caking and degradation of ammonium nitrate, an alternative composition with additional calcium lignosulfonate and silicic acid was studied. The resulting fertilizer was analyzed by screening analysis, ion chromatography, and electron microscopy methods.

  3. Decomposition of pre calcined aluminium silicate ores of Afghanistan by hydrochloric acid

    International Nuclear Information System (INIS)

    Khomidi, A.K.; Mamatov, E.D.

    2015-01-01

    Present article is devoted to decomposition of pre calcined aluminium silicate ores of Afghanistan by hydrochloric acid. The physicochemical properties of initial aluminium silicate ores were studied by means of X-ray phase, differential thermal and silicate analysis. The chemical composition of aluminium containing ores was determined. The optimal conditions of interaction of initial and pre calcined siallites with hydrochloric acid were defined. The kinetics of acid decomposition of aluminium silicate ores was studied as well.

  4. Silicic acid competes for dimethylarsinic acid (DMA) immobilization by the iron hydroxide plaque mineral goethite.

    Science.gov (United States)

    Kersten, Michael; Daus, Birgit

    2015-03-01

    A surface complexation modeling approach was used to extend the knowledge about processes that affect the availability of dimethylarsinic acid (DMA) in the soil rhizosphere in presence of a strong sorbent, e.g., Fe plaques on rice roots. Published spectroscopic and molecular modeling information suggest for the organoarsenical agent to form bidentate-binuclear inner-sphere surface complexes with Fe hydroxides similar to the inorganic As oxyanions. However, since also the ubiquitous silicic acid oxyanion form the same bidentate binuclear surface complexes, our hypothesis was that it may have an effect on the adsorption of DMA by Fe hydroxides in soil. Our experimental batch equilibrium data show that DMA is strongly adsorbed in the acidic pH range, with a steep adsorption edge in the circumneutral pH region between the DMA acidity constant (pKa=6.3) and the point of zero charge value of the goethite adsorbent (pHpzc=8.6). A 1-pK CD-MUSIC surface complexation model was chosen to fit the experimental adsorption vs. pH data. The same was done for silicic acid batch equilibrium data with our goethite adsorbent. Both model parameters for individual DMA and silicic acid adsorption were then merged into one CD-MUSIC model to predict the binary DMA+Si adsorption behavior. Silicic acid (500 μM) was thus predicted by the model to strongly compete for DMA with up to 60% mobilization of the latter at a pH6. This model result could be verified subsequently by experimental batch equilibrium data with zero adjustable parameters. The thus quantified antagonistic relation between DMA and silicic acid is discussed as one of factors to explain the increase of the DMA proportion in rice grains as observed upon silica fertilization of rice fields. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Leaf application of silicic acid to upland rice and corn

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    Carlos Alexandre Costa Crusciol

    2013-12-01

    Full Text Available This study aimed to evaluate the effect of Si (stabilized silicic acid, Silamol® leaf application on mineral nutrition and yield in upland rice and corn crops. The treatments were the control (without Si and Si foliar split spraying using 2 L ha-1 of the Silamol® commercial product, with 0.8% soluble Si as concentrated stabilized silicic acid. Silicon leaf application increased the concentrations of K, Ca and Si in rice and corn leaves, the number of panicles per m2 of rice and the number of grains per ear of corn; accordingly, the Si leaf application provided a higher grain yield in both crops.

  6. Solid-phase extraction of galloyl- and caffeoylquinic acids from natural sources (Galphimia glauca and Arnicae flos) using pure zirconium silicate and bismuth citrate powders as sorbents inside micro spin columns.

    Science.gov (United States)

    Hussain, Shah; Schönbichler, Stefan A; Güzel, Yüksel; Sonderegger, Harald; Abel, Gudrun; Rainer, Matthias; Huck, Christian W; Bonn, Günther K

    2013-10-01

    Galloyl- and caffeoylquinic acids are among the most important pharmacological active groups of natural compounds. This study describes a pre-step in isolation of some selected representatives of these groups from biological samples. A selective solid-phase extraction (SPE) method for these compounds may help assign classes and isomer designations within complex mixtures. Pure zirconium silicate and bismuth citrate powders (325 mesh) were employed as two new sorbents for optimized SPE of phenolic acids. These sorbents possess electrostatic interaction sites which accounts for additional interactions for carbon acid moieties as compared to hydrophilic and hydrophobic sorbents alone. Based on this principle, a selective SPE method for 1,3,4,5-tetragalloylquinic acid (an anti-HIV and anti-asthamatic agent) as a starting compound was developed and then deployed upon other phenolic acids with success. The recoveries and selectivities of both sorbents were compared to most commonly applied and commercially available sorbents by using high performance liquid chromatography. The nature of interaction between the carrier sorbent and the acidic target molecules was investigated by studying hydrophilic (silica), hydrophobic (C18), mixed-mode (ionic and hydrophobic: Oasis(®) MAX) and predominantly electrostatic (zirconium silicate) materials. The newly developed zirconium silicate and bismuth citrate stationary phases revealed promising results for the selective extraction of galloyl- and caffeoylquinic acids from natural sources. It was observed that zirconium silicate exhibited maximum recovery and selectivity for tetragalloylquinic acid (84%), chlorogenic acid (82%) and dicaffeoylquinic acid (94%) among all the tested sorbents. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Radiochemical investigations to the complex formation of uranium (VI) with silicic acid

    International Nuclear Information System (INIS)

    Hrnecek, E.

    1997-12-01

    The complexation of tracer amounts of UO 2 2+ by silicic acid was investigated by an extraction method using 2,5. 10 -3 M 1-(2-thenoyl)-3,3,3-trifloroacetone (IMA) in benzene as extractant at 25 degree C. The tracer used in the experiments was uranium-232, which has been separated from its daughter nuclides by ion exchange from 10 M HCl on Dowex 1x2. The ionic strength in the aqueous phase for the extractions was kept constant at 0,2 M (Na, H)ClO 4 and the pH was varied between pH 2,5 and pH 4,5. For the determination of the stability constants, a silicic acid concentration of 0,01 M, 0,03 M and 0,067 M in the (Na, H)ClO 4 solution was used. The time- and pH- dependence of the polymerization of these silicic acid solutions was determined by kinetical investigations with an ammoniumheptamolybdate-reagent. The uranium concentration in the aqueous and organic phases was determined by liquid scintillation counting using α/β -discrimination. The stability constants determined were log Q1, = -2,20 for the reaction UO 2 2+ Si(OH) 4 = UO 2 OSi(OH) 3 + + H + and Q 2 = -5,87 for the reaction of the polymeric silicate UO 2 2+ (-SiOH) j (-SiOH) j-2 (SiO) 2 UO 2 +2 H + . The influence of silicate on the speciation calculations for uranium in a model natural water is also discussed. (author)

  8. Creep of Sylramic-iBN Fiber Tows at Elevated Temperature in Air and in Silicic Acid-Saturated Steam

    Science.gov (United States)

    2015-06-01

    CREEP OF SYLRAMIC-iBN FIBER TOWS AT ELEVATED TEMPERATURE IN AIR AND IN SILICIC ACID-SATURATED STEAM ...protection in the United States. AFIT-ENY-15-J-46 CREEP OF SYLRAMIC-iBN FIBER TOWS AT ELEVATED TEMPERATURE IN AIR AND IN SILICIC ACID-SATURATED STEAM ...DISTRIBUTION UNLIMITED. AFIT-ENY-15-J-46 CREEP OF SYLRAMIC-iBN FIBER TOWS AT ELEVATED TEMPERATURE IN AIR AND IN SILICIC ACID-SATURATED STEAM

  9. 40 CFR 721.3100 - Oligomeric silicic acid ester compound with a hy-droxyl-al-kyla-mine.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Oligomeric silicic acid ester compound with a hy-droxyl-al-kyla-mine. 721.3100 Section 721.3100 Protection of Environment ENVIRONMENTAL... Significant New Uses for Specific Chemical Substances § 721.3100 Oligomeric silicic acid ester compound with a...

  10. Alleviating aluminum toxicity in an acid sulfate soil from Peninsular Malaysia by calcium silicate application

    Science.gov (United States)

    Elisa, A. A.; Ninomiya, S.; Shamshuddin, J.; Roslan, I.

    2016-03-01

    In response to human population increase, the utilization of acid sulfate soils for rice cultivation is one option for increasing production. The main problems associated with such soils are their low pH values and their associated high content of exchangeable Al, which could be detrimental to crop growth. The application of soil amendments is one approach for mitigating this problem, and calcium silicate is an alternative soil amendment that could be used. Therefore, the main objective of this study was to ameliorate soil acidity in rice-cropped soil. The secondary objective was to study the effects of calcium silicate amendment on soil acidity, exchangeable Al, exchangeable Ca, and Si content. The soil was treated with 0, 1, 2, and 3 Mg ha-1 of calcium silicate under submerged conditions and the soil treatments were sampled every 30 days throughout an incubation period of 120 days. Application of calcium silicate induced a positive effect on soil pH and exchangeable Al; soil pH increased from 2.9 (initial) to 3.5, while exchangeable Al was reduced from 4.26 (initial) to 0.82 cmolc kg-1. Furthermore, the exchangeable Ca and Si contents increased from 1.68 (initial) to 4.94 cmolc kg-1 and from 21.21 (initial) to 81.71 mg kg-1, respectively. Therefore, it was noted that calcium silicate was effective at alleviating Al toxicity in acid sulfate, rice-cropped soil, yielding values below the critical level of 2 cmolc kg-1. In addition, application of calcium silicate showed an ameliorative effect as it increased soil pH and supplied substantial amounts of Ca and Si.

  11. Influence of acid/ore relation in the uranium-silicate ore treatment

    International Nuclear Information System (INIS)

    Antaki, C.; Cipriani, M.; Bruno, J.B.

    1985-01-01

    The estimation of acid addition effect (Kg of H 2 SO 4 /t of ore) in uranium extraction from an uranium-silicate ore, with a view to the control of silica concentration in leach under 0,6 g/l is presented. The analysis was effected based on bench-scale tests, with different quantities of sulfuric acid addition. (Author) [pt

  12. Effect of Silicic Acid on some Anatomical and Biochemical Characteristics of Pelargonium graveolens under Salinity Stress

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    fateme hasanvand

    2017-08-01

    Full Text Available Introduction: Scented geranium (Pelargonium graveolens is a perennial plant of the family Geranium (Geraniaceae. Although CaCl2 at higher concentrations than NaCl in the soils and ground water in many areas of the word, most studies have been based on experiments that NaCl is the predominant salt. Relatively few studies have focused on the effects of CaCl2 on plant growth and physiology. Silicon (Si is considered as an essential element in several crops enhancing growth and alleviating different biotic and abiotic stresses. In this study, the role of Si in alleviation the deleterious effects of salinity on geranium have been studied. Materials and Methods: This experiment was conducted in spring-summer 2014 in research greenhouse situated on the Faculty of Agriculture, Lorestan University, Khorramabad, Iran. The greenhouse temperature was 16.5–37.5 ◦C and relative humidity of greenhouse was 30–80%. Terminal stem cuttings with five nodes were obtained from mother plants in the same greenhouse and placed in a sand substrate for rooting in April. Uniform rooted cuttings were then transplanted into plastic pots (22 cm diameter and height filled with sand substrates and grown hydroponically. Transplanting was done in May and one plant per pot was cultivated. Cultivated plants were irrigated with Hoagland’s medium electrical conductivity (EC 1.8 dS/m, (pH 5.8 twice a day. Experiment was arranged as factorial based on a completely randomized design with five replications. Factors consisted of daily application of 1.8, 4 and 6 ds/m CaCl2 and weekly application of 0, 0.5 and 1 mM silicic acid in nutrient solution. Plants were harvested in November. In this research some characteristics include the number of leaf, leaf area, photosynthetic pigments (chla, chlb. Total chl, carotenoids, MDA, EL, RWC, proline, number of stomata in surface unit of leaf, density of stomata and stomata index and antioxidant enzyme include CAT and POD measured. Results

  13. The acid aging as alternative process for uranium recovery from silicated ores

    International Nuclear Information System (INIS)

    Cipriani, M.; Della Testa, A.

    1984-01-01

    The influence of different variables on the extraction uranium efficiency and on the silicate solubility by means of acid aging is studied. The variables studied in bench scale were: acid/ore, oxidizing/ore and liquid/solid relationships; reaction time; temperature and recovery time. The results are discussed and compared with the ones of continuous operation of a semi-pilot plant. A flowsheet of the industrial process application is presented. (M.A.C.) [pt

  14. Determination of silica in silicates by differential spectrophotometry as α-molybdosilicic acid

    International Nuclear Information System (INIS)

    Ohlweiler, O.A.; Meditsch, J.O.; Silva, S.

    1980-01-01

    A method for determining silica in silicates by differential spectrophotometry, using β-molybdosilic acid, is described. The sample is attacked by a mixture of boron trioxide and lithium carbonate (10:1). α-molydbosilicic acid is developed in a buffered solution (pH approximatelly 3.9) containing acetic acid and sodium acetate. The analytical procedure involves a series of preliminary steps which were previously elaborated for the gravimetric determination of silica as oxine molybdosilicate and which account for the removal of phosphorus, titanium and zirconium through ion exchange resins. (C.L.B.) [pt

  15. Spherical oligo-silicic acid SOSA disclosed as possible endogenous digitalis-like factor

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    Franz eKerek

    2015-01-01

    Full Text Available Na+/K+-ATPase is a membrane ion-transporter protein, specifically inhibited by digitalis glycosides used in cardiac-therapy. The existence in mammals of some endogenous digitalis-like factors (EDLF as presumed ATPase ligands is generally accepted. But the chemical structure of these factors remained elusive because no weighable amounts of pure EDLF have been isolated. Recent high resolution crystal structure data of Na+/K+-ATPase have located the hydrophobic binding pocket of the steroid glycoside ouabain. Our recently disclosed spherical oligo-silicic acids (SOSA fulfill the main criteria to be identified with the presumed EDL factor. SOSA was found as a very potent inhibitor of the Na+/K+-ATPase, Ca2+-ATPase, H+/K+-ATPase and of K-dp-ATPase, with IC50 values between 0.2-0.5µg/ml. These findings are even more astonishing while so far, neither mono silicic acid nor its poly-condensed derivatives have been remarked biologically active. With the diameter ϕ between 1 - 3nm, SOSA still belong to molecular species definitely smaller than silica nano-particles with ϕ >5nm. In SOSA molecules almost all Si-OH bonds are displayed on the external shell which facilitates the binding to hydrophilic ATPase domains. SOSA is stable for long-term in solution but is sensitive to freeze-drying which could explain the failure of countless attempts to isolate pure EDLF. There is a strong resemblance between SOSA and vanadates, the previously known general inhibitors of P-type ATPases. SOSA may be generated endogenously by spherical oligomerization of the mono-silicic acid ubiquitously present in animal cells and fluids. Based on the finding that the SOSA structure is sensitive to the concentration and nature of the cationic species a presumably archaic mechanism to regulate the activity of the ATPase pumps is proposed.

  16. Ion-pair chromatography of nucleic acid derivatives

    International Nuclear Information System (INIS)

    Perrone, P.A.; Brown, P.R.

    1985-01-01

    Little work has been done on the ion-pair chromatography of nucleic acid constituents, although there is a great potential for the use of this technique in the field. Since the classic work in 1949, nucleotides, as well as nucleosides and bases, have been separated by ion-exchange chromatography. However, ion exchange is a difficult mode and most researchers prefer the use of reversed-phase whenever possible. Although reversed-phase is now the method of choice, ionic compounds like nucleotides and some of the more polar bases are not adequately retained by many systems of this type. In addition, it is difficult to analyze simultaneously members of all three classes of nucleic acid compounds (bases, nucleosides, and nucleotides) using a reversed-phase system, even with gradient elution. Ion pairing can be a useful technique because, theoretically, the separation of nonionic bases and nucleosides along with the ionic nucleotides can be achieved. Additionally, each group of compounds may be separated isocratically. In this chapter, they will discuss ion-pair chromatography as applied to nucleic acid constituents. The current theories, advantages and disadvantages, a limited number of applications, and potential for future work are presented

  17. Rice Hull Ash and Silicic Acid as Adsorbents for Concentration of Bacteriocins†

    OpenAIRE

    Janes, M. E.; Nannapaneni, R.; Proctor, A.; Johnson, M. G.

    1998-01-01

    A model procedure has been developed for the rapid extraction of five bacteriocins (nisin, pediocin RS2, leucocin BC2, lactocin GI3, and enterocin CS1) from concentrated freeze-dried crude culture supernatants by adsorption onto acid or alkaline rice hull ash (RHA) or silicic acid (SA). Bacteriocins were adsorbed onto RHA or SA by a pH-dependent method and desorbed by decreasing the pH to 2.5 or 3.0 and heating at 90°C for 5 min. The maximum adsorption and optimal pH range for different bacte...

  18. Nanostructured silicate polymer concrete

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    Figovskiy Oleg L'vovich

    2014-03-01

    Full Text Available It has been known that acid-resistant concretes on the liquid glass basis have high porosity (up to 18~20 %, low strength and insufficient water resistance. Significant increasing of silicate matrix strength and density was carried out by incorporation of special liquid organic alkali-soluble silicate additives, which block superficial pores and reduce concrete shrinkage deformation. It was demonstrated that introduction of tetrafurfuryloxisilane additive sharply increases strength, durability and shock resistance of silicate polymer concrete in aggressive media. The experiments showed, that the strength and density of silicate polymer concrete increase in case of decreasing liquid glass content. The authors obtained optimal content of silicate polymer concrete, which possesses increased strength, durability, density and crack-resistance. Diffusive permeability of concrete and its chemical resistance has been investigated in various corroding media.

  19. Simultaneous analysis of small organic acids and humic acids using high performance size exclusion chromatography

    NARCIS (Netherlands)

    Qin, X.P.; Liu, F.; Wang, G.C.; Weng, L.P.

    2012-01-01

    An accurate and fast method for simultaneous determination of small organic acids and much larger humic acids was developed using high performance size exclusion chromatography. Two small organic acids, i.e. salicylic acid and 2,3-dihydroxybenzoic acid, and one purified humic acid material were used

  20. Determination of gangliosides as 2,4-dinitrophenylhydrazides by high-performance liquid chromatography.

    OpenAIRE

    Miyazaki, K; Okamura, N; Kishimoto, Y; Lee, Y C

    1986-01-01

    A specific, sensitive and easily performed method for the determination of gangliosides in tissue was developed. After removal of water-soluble compounds, total lipids were extracted from tissue and then treated with 2,4-dinitrophenylhydrazine hydrochloride and dicyclohexylcarbodi-imide in dimethylformamide at 0 degrees C to form ganglioside hydrazides. After removal of excess reagents by column chromatography on silicic acid, the ganglioside 2,4-dinitrophenylhydrazides were eluted from the c...

  1. Occurrence of Conjugated Linolenic Acids in Purified Soybean Oil

    OpenAIRE

    Kinami, Tomohisa; Horii, Naoto; Narayan, Bhaskar; Arato, Shingo; Hosokawa, Masashi; Miyashita, Kazuo; Negishi, Hironori; Ikuina, Junichi; Noda, Ryuji; Shirasawa, Seiichi

    2007-01-01

    A high-performance liquid chromatographic (HPLC) method is described for the determination of conjugated linoleic acids (CLA) and conjugated linolenic acids (CLN). Methyl esters prepared from purified lipid fractions of soybean oil were analyzed using an HPLC system equipped with photodiode-array detector to detect peaks having maximum absorption around 233 and 275 nm. These peaks were concentrated by AgNO3-silicic acid column chromatography and reversed-phase HPLC. The structural analysis, o...

  2. Utilization of Ion-Exclusion Chromatography for Water Quality Monitoring in a Suburban River in Jakarta, Indonesia

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    Daisuke Kozaki

    2014-07-01

    Full Text Available We evaluated the use of ion-exclusion chromatographic systems for analyzing the behavior of inorganic ions (e.g., bicarbonate, sulfate, chloride, nitrate, phosphate, dissolved silicate, sodium, ammonium, potassium, magnesium, and calcium ions in a suburban river located in Jakarta, Indonesia. Carbonate, phosphate, and silicate ion concentrations were determined using ion-exclusion chromatography (IEC on a weakly acidic cation-exchange resin column (WCX in the H+-form with water eluent. Other ions were identified by ion-exclusion/cation-exchange chromatography (IEC/CEC on a WCX column with tartaric acid eluent. The use of IEC systems for water quality monitoring was advantageous for the following reasons: (1 the concentrations of analyte ions, except NO3− and silicate ions, increased from upstream to downstream; and (2 the speciation of inorganic nitrogen ions could be analyzed by single injection into the IEC/CEC. The IEC approach provided beneficial information for the construction of sewage treatment facilities in our study area. Results showed that (1 the analyte concentrations for samples obtained in the downstream area were higher than those in the upstream area owing to contamination by domestic sewage; (2 the concentrations of NO3− and NH4+ correlated with the concentration of dissolved oxygen; and (3 bicarbonate concentrations increased downstream, likely due to respiration of bacteria and dissolution of concrete under low-oxygen conditions.

  3. Identification of Cyclopentenyl Fatty Acids by Gas Liquid Chromatography and Mass Spectrometry

    DEFF Research Database (Denmark)

    Shukla, V. K. S.; Abdel-Moety, E. M.; Larsen, Elfinn

    1979-01-01

    The straight chain fatty acids and the cyclopentenyl fatty acids present in the lipids of Hydnocarpus wightiana seeds were separated as their pyrrolidides by means of gas chromatography. A gas chromatography-mass spectrometry system confirmed the complete separation and permitted the identification...

  4. Analysis of short-chain acids from anaerobic bacteria by high-performance liquid chromatography.

    OpenAIRE

    Guerrant, G O; Lambert, M A; Moss, C W

    1982-01-01

    A standard mixture of 25 short-chain fatty acids was resolved by high-performance liquid chromatography, using an Aminex HPX-87 column. The acids produced in culture media by anaerobic bacteria were analyzed by high-performance liquid chromatography after extraction with ether and reextraction into a small volume of 0.1 N NaOH. The presence of fumaric acid in culture extracts of Peptostreptococcus anaerobius was confirmed by gas chromatography-mass spectrometry analysis of the trapped eluent ...

  5. Microwave-Assisted Conversion of Levulinic Acid to γ-Valerolactone Using Low-Loaded Supported Iron Oxide Nanoparticles on Porous Silicates

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    Alfonso Yepez

    2015-09-01

    Full Text Available The microwave-assisted conversion of levulinic acid (LA has been studied using low-loaded supported Fe-based catalysts on porous silicates. A very simple, productive, and highly reproducible continuous flow method has been used for the homogeneous deposition of metal oxide nanoparticles on the silicate supports. Formic acid was used as a hydrogen donating agent for the hydrogenation of LA to effectively replace high pressure H2 mostly reported for LA conversion. Moderate LA conversion was achieved in the case of non-noble metal-based iron oxide catalysts, with a significant potential for further improvements to compete with noble metal-based catalysts.

  6. High Performance Liquid Chromatography Determination of Urinary Hippuric Acid and Benzoic Acid as Indices for Glue Sniffer Urine

    OpenAIRE

    Abdul Rahim Yacob; Mohamad Raizul Zinalibdin

    2010-01-01

    A simple method for the simultaneous determination of hippuric acid and benzoic acid in urine using reversed-phase high performance liquid chromatography was described. Chromatography was performed on a Nova-Pak C18 (3.9 x 150 mm) column with a mobile phase of mixed solution methanol: water: acetic acid (20:80:0.2) and UV detection at 254 nm. The calibration curve was linear within concentration range at 0.125 to 6.0 mg/ml of hippuric acid and benzoic acid. The recovery, ...

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

    Science.gov (United States)

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

    2015-02-01

    This review summarizes the recent advances in the analysis of amino acids, peptides, and proteins using hydrophilic interaction chromatography. Various reports demonstrate the successful analysis of amino acids under such conditions. However, a baseline resolution of the 20 natural amino acids has not yet been published and for this reason, there is often a need to use mass spectrometry for detection to further improve selectivity. Hydrophilic interaction chromatography is also recognized as a powerful technique for peptide analysis, and there are a lot of papers showing its applicability for proteomic applications (peptide mapping). It is expected that its use for peptide mapping will continue to grow in the future, particularly because this analytical strategy can be combined with reversed-phase liquid chromatography, in a two-dimensional setup, to reach very high resolving power. Finally, the interest in hydrophilic interaction chromatography for intact proteins analysis is less evident due to possible solubility issues and a lack of suitable hydrophilic interaction chromatography stationary phases. To date, it has been successfully employed only for the characterization of membrane proteins, histones, and the separation of glycosylated isoforms of an intact glycoprotein. From our point of view, the number of hydrophilic interaction chromatography columns compatible with intact proteins (higher upper temperature limit, large pore size, etc.) is still too limited. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Pre-staining thin layer chromatography method for amino acid ...

    African Journals Online (AJOL)

    Jane

    2010-12-13

    Dec 13, 2010 ... inexpensive and the results obtained were clean and reproducible. However, it is suitable for the high throughput screening of amino acid-producing strains. Key words: Thin layer chromatography, pre-staining, amino acid detection. INTRODUCTION. Several analytical techniques have been often used for.

  9. 5-O-caffeoylshikimic acid from Solanum somalense leaves: advantage of centrifugal partition chromatography over conventional column chromatography.

    Science.gov (United States)

    Chideh, Saïda; Pilard, Serge; Attoumbré, Jacques; Saguez, Robert; Hassan-Abdallah, Alshaimaa; Cailleu, Dominique; Wadouachi, Anne; Baltora-Rosset, Sylvie

    2014-09-01

    Solanum somalense leaves, used in Djibouti for their medicinal properties, were extracted by MeOH. Because of the high polyphenol and flavonoid contents of the extract, respectively, determined at 80.80 ± 2.13 mg gallic acid equivalent/g dry weight and 24.4 ± 1.01 mg quercetin equivalent/g dry weight, the isolation and purification of the main polyphenols were carried out by silica gel column chromatography and centrifugal partition chromatography. Column chromatography led to 11 enriched fractions requiring further purification, while centrifugal partition chromatography allowed the easy recovery of the main compound of the extract. In a solvent system composed of CHCl3/MeOH/H2O (9.5:10:5), 21.8 mg of this compound at 97% purity was obtained leading to a yield of 2.63%. Its structure was established as 5-O-caffeoylshikimic acid by mass spectrometry and NMR spectroscopy. This work shows that S. somalense leaves contain very high level of 5-O-caffeoylshikimic acid (0.74% dry weight), making it a potential source of production of this secondary metabolite that is not commonly found in nature but could be partly responsible of the medicinal properties of S. somalense leaves. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Measurement of the efficacy of calcium silicate for the protection and repair of dental enamel.

    Science.gov (United States)

    Parker, Alexander S; Patel, Anisha N; Al Botros, Rehab; Snowden, Michael E; McKelvey, Kim; Unwin, Patrick R; Ashcroft, Alexander T; Carvell, Mel; Joiner, Andrew; Peruffo, Massimo

    2014-06-01

    To investigate the formation of hydroxyapatite (HAP) from calcium silicate and the deposition of calcium silicate onto sound and acid eroded enamel surfaces in order to investigate its repair and protective properties. Calcium silicate was mixed with phosphate buffer for seven days and the resulting solids analysed for crystalline phases by Raman spectroscopy. Deposition studies were conducted on bovine enamel surfaces. Acid etched regions were produced on the enamel surfaces using scanning electrochemical cell microscopy (SECCM) with acid filled pipettes and varying contact times. Following treatment with calcium silicate, the deposition was visualised with FE-SEM and etch pit volumes were measured by AFM. A second set of bovine enamel specimens were pre-treated with calcium silicate and fluoride, before acid exposure with the SECCM. The volumes of the resultant acid etched pits were measured using AFM and the intrinsic rate constant for calcium loss was calculated. Raman spectroscopy confirmed that HAP was formed from calcium silicate. Deposition studies demonstrated greater delivery of calcium silicate to acid eroded than sound enamel and that the volume of acid etched enamel pits was significantly reduced following one treatment (penamel was 0.092 ± 0.008 cm/s. This was significantly reduced, 0.056 ± 0.005 cm/s, for the calcium silicate treatments (penamel surfaces. Calcium silicate can provide significant protection of sound enamel from acid challenges. Calcium silicate is a material that has potential for a new approach to the repair of demineralised enamel and the protection of enamel from acid attacks, leading to significant dental hard tissue benefits. © 2014 Elsevier Ltd. All rights reserved.

  11. Method of gradual acid leaching of uranium ores of silicate and aluminosilicate nature

    International Nuclear Information System (INIS)

    Bosina, B.; Krepelka, J.; Urban, P.; Kropacek, J.; Stransky, J.

    1987-01-01

    Leaching uranium ore pulp is divided into two stages. The first stage takes place without any addition of a leaching agent at elevated pressure and temperature. In the second stage, sulfuric acid is added to the pulp (50 to 1000 kg per tonne of ore) or an oxidation agent. Leaching then proceeds according to routine procedures. The procedure is used to advantage for silicate or aluminosilicate ores which contain uranium minerals which are difficult to leach, pyrite and reducing substances. The two stage leaching allows to use the technology of pressure leaching, reduces consumption of sulfuric acid and oxidation agents and still achieves the required reduction oxidation potential. (E.S.)

  12. Regularities in Low-Temperature Phosphatization of Silicates

    Science.gov (United States)

    Savenko, A. V.

    2018-01-01

    The regularities in low-temperature phosphatization of silicates are defined from long-term experiments on the interaction between different silicate minerals and phosphate-bearing solutions in a wide range of medium acidity. It is shown that the parameters of the reaction of phosphatization of hornblende, orthoclase, and labradorite have the same values as for clayey minerals (kaolinite and montmorillonite). This effect may appear, if phosphotization proceeds, not after silicate minerals with a different structure and composition, but after a secondary silicate phase formed upon interaction between silicates and water and stable in a certain pH range. Variation in the parameters of the reaction of phosphatization at pH ≈ 1.8 is due to the stability of the silicate phase different from that at higher pH values.

  13. Intercomparison of the measurements of oxalic acid in aerosols by gas chromatography and ion chromatography

    Science.gov (United States)

    Kawamura, Kimitaka; Barrie, Leonard A.; Toom-Sauntry, Desiree

    2010-12-01

    Oxalate, the anion of oxalic acid, is one of the most abundant measurable organic species in atmospheric aerosols. Traditionally, this bifunctional species has been measured by gas chromatography (GC) after derivatization to butyl ester and by ion chromatography (IC) without derivatization. However, there are few published comparisons of the two techniques. Here, we report the results of an intercomparison study for the measurement of oxalic acid in Arctic aerosols (oxalic acid by GC ranged from 6.5-59.1 ng m -3 (av. 26.0 ng m -3, median 26.2 ng m -3) whereas those by IC ranged from 6.6-52.1 ng m -3 (av. 26.6 ng m -3, median 25.4 ng m -3). They showed a good correlation ( r = 0.84) with a slope of 0.96. Thus, observations of oxalate obtained by GC employing dibutyl esters are almost equal to those by IC. Because the accuracy of oxalic acid by GC method largely depends on the method used, it is important to strictly examine the recovery in each study.

  14. Process for the conversion of sugars to lactic acid and 2-hydroxy-3-butenoic acid or esters thereof comprising a metallo-silicate material and a metal ion

    DEFF Research Database (Denmark)

    2015-01-01

    A process for the preparation of lactic acid and 2-hydroxy- 3-butenoic acid or esters thereof from a sugar in the presence of a metallo-silicate material, a metal ion and a solvent, wherein the metal ion is selected from one or more of the group consisting of potassium ions, sodium ions, lithium...

  15. An on-line monitor for cation exchange elution chromatography using lithium silicate glass beads as solid scintillator

    International Nuclear Information System (INIS)

    Zhu Rongbao; Yang Liucheng; Wei Liansheng; Ji Liqiang; Zhang Zengrui

    1988-03-01

    A new type of on-line monitoring system used to monitor radioactive nuclides with α or soft β radiation in the effluent from a high pressure ion exchange column is described. The beads made of cerium-impregnated lithium silicate glass are used as scientillation material. They are filled into a quartz glass tube to form a flow cell. By reducing the diameter of glass beads to more closly approximate the average range of α or soft β radiation in solution, the absolute counting efficiency for 241 Am, 242 Cm α radiation have reached and 85.8% and 92.8% respectively, for 14 C, 90 Sr- 90 Y β radiation, 62.1% and 88.6% respectively. These values can be comparable to those achieved with on-line liquid scientillation technique. When the total amount of 241 Am added into column is decreased to 7.4 Bq it is still possible to obtain a clear chromatography peak (half peak width = 0.22 mL)

  16. Concentration and fractionation of hydrophobic organic acid constituents from natural waters by liquid chromatography

    Science.gov (United States)

    Thurman, E.M.; Malcolm, R.L.

    1979-01-01

    A scheme is presented which used adsorption chromatography with pH gradient elution and size-exclusion chromatography to concentrate and separate hydrophobic organic acids from water. A review of chromatographic processes involved in the flow scheme is also presented. Organic analytes which appear in each aqueous fraction are quantified by dissolved organic carbon analysis. Hydrophobic organic acids in a water sample are concentrated on a porous acrylic resin. These acids usually constitute approximately 30-50 percent of the dissolved organic carbon in an unpolluted water sample and are eluted with an aqueous eluent (dilute base). The concentrate is then passed through a column of polyacryloylmorpholine gel, which separates the acids into high- and low-molecular-weight fractions. The high- and low-molecular-weight eluates are reconcentrated by adsorption chromatography, then are eluted with a pH gradient into strong acids (predominately carboxylic acids) and weak acids (predominately phenolic compounds). For standard compounds and samples of unpolluted waters, the scheme fractionates humic substances into strong and weak acid fractions that are separated from the low molecular weight acids. A new method utilizing conductivity is also presented to estimate the acidic components in the methanol fraction.

  17. Gas chromatography/mass spectrometry analysis of very long chain fatty acids, docosahexaenoic acid, phytanic acid and plasmalogen for the screening of peroxisomal disorders

    NARCIS (Netherlands)

    Takemoto, Yasuhiko; Suzuki, Yasuyuki; Horibe, Ryoko; Shimozawa, Nobuyuki; Wanders, Ronald J. A.; Kondo, Naomi

    2003-01-01

    Very long chain fatty acids (VLCFAs) and docosahexaenoic acid (DHA), phytanic acid, and plasmalogens are usually measured individually. A novel method for the screening of peroxisomal disorders, using gas chromatography/mass spectrometry (GC/MS), was developed. Saturated and unsaturated fatty acids,

  18. Stability constants for silicate adsorbed to ferrihydrite

    DEFF Research Database (Denmark)

    Hansen, Hans Christian Bruun; Wetche, T.P.; Raulund-Rasmussen, Karsten

    1994-01-01

    Intrinsic surface acidity constants (K(a1)intr, K(a2)intr) and surface complexation constant for adsorption of orthosilicate onto synthetic ferrihydrite (K(Si) for the complex = FeOSi(OH)3) have been determined from acid/base titrations in 0.001-0.1 m NaClO4 electrolytes and silicate adsorption...... experiments in 0.01 m NaNO3 electrolyte (pH 3-6). The surface equilibrium constants were calculated according to the two-layer model by Dzombak & Morel (1990). Near equilibrium between protons/hydroxyls in solution and the ferrihydrite surface was obtained within minutes while equilibration with silicate...

  19. Identification of bound alcohols in soil humic acids by gas chromatography-mass spectrometry

    OpenAIRE

    Berthier , Gersende; Dou , Sen; Peakman , Torren; Lichtfouse , Eric

    2000-01-01

    International audience; Humic acids are complex, partly macromolecular, yellow-brownish substances occurring in soils, waters and sediments. In order to shed some light on their molecular structure, crop humic acids were cleaved by alkaline hydrolysis (KOH). The products were fractionated by thin layer chromatography to give mono-alcohols which were analysed as acetate derivatives by gas chromatography coupled to mass spectrometry. Linear alcohols, sterols, stanols and plant-derived triterpen...

  20. Gas chromatography of alkylphosphonic and dialkylphosphinic acids

    International Nuclear Information System (INIS)

    Gasco, L.; Barrera, R.; Ramirez, A.; Martin Munoz, N.

    1978-01-01

    After carrying out an optimization study on the separation conditions for the TMS-derivatives, of the hexyl-, cyclohexyl-, heptyl-, and octyl-phosphonic acids; dihexyl-, dicyclohexyl-, heptyl-, and octyl-phosphinic acids, and dioctylphosphine oxide, their retention indices (I) at two temperatures and on the 0V-1 and 0V-17 stationary phase were determined. Correlations between I and molecular structure were established. Calibration factors of these compounds in the flame ionization detector were studied, and the results analized taking into account the variables afecting the quantitative results. These results were unbiased but they had a lower precission than usually achieveble in gas chromatography. (author)

  1. Ligand exchange chromatography of free amino acids and proteins on porous microparticulate zirconium oxide

    International Nuclear Information System (INIS)

    Blackwell, J.A.; Carr, P.W.

    1992-01-01

    The Lewis acid sites present on the underlying zirconium oxide particles are responsible for the unusual elution sequence for amino acids on copper loaded, phosphated zirconium oxide supports reported in an earlier study. To more thoroughly examine the effect of these strong Lewis acid sites in this paper. The authors have studied ligand exchange chromatography on copper loaded zirconium oxide particles. It is shown here that carboxylate functional groups on amino acid solutes strongly interact with surface Lewis acid sites. Addition of competing hard Lewis bases to the eluent attenuates these specific interactions. The result is a chromatographic system with high selectivity which is also suitable for ligand exchange chromatography of proteins

  2. Single-column ion chromatography with determination of hydrazoic acid produced in spent nuclear fuel reprocessing

    International Nuclear Information System (INIS)

    Ma Guilan; Tan Shuping

    2006-01-01

    The reaction of hydrazine and its derivative with ammonium metavanadate may produce hydrazoic acid (HN 3 ). A single-column ion chromatography is used for the determination of HN 3 after neutralizing the rest acid in the sample with sodium hydroxide. Chromatography separation of HN 3 is carried out on a 25 cm x 0.46 cm (inside diameter) stainless steel column packed with Vydac IC302 ion Chromatography packing. The eluent is 1 mmol/L o-phthalic acid, and the ion is detected by conductivity detector. The detection limit in the presence chromatography is 5 μg/mL, the linear range is from 5 to 201 μg/mL, the linear correlation coefficient is 0.9994, respectively. The analysis accuracy is 2% for standard sample, and the detection limit is 51 μg/mL for HN 3 in the real sample. (authors)

  3. Ligand exchange chromatography for analysis and preparative separation of tritium-labelled amino acids

    International Nuclear Information System (INIS)

    Zolotarev, Yu.A.; Zaitsev, D.A.; Penkina, V.I.; Dostavalov, I.N.; Myasoedov, N.F.

    1988-01-01

    Racemic tritium-labelled amino acids were separated into optical isomers by chromatography on a chiral polyacrylamide sorbent filled with copper ions. The polyacrylamide sorbent is synthesized by Mannich's reaction through the action of formaldehyde and L-phenylalanine upon polyacrylamide Biogel P-4 in an alkali phosphate buffer. Tritium-labelled amino acids are eluted by a weak alkali solution of ammonium carbonate. Data are presented on the ligand exchange chromatography of amino acids depending on the degree to which the sorbent is filled with copper ions and on the eluent concentration. Amino acids are isolated from the eluent on short columns filled with sulfonated cation exchanger in the H + form. HPLC on modified silica gel sorbents is also used for the analysis of tritium-labelled optically active amino acids. Amino acids are eluted by a weakly acidic water-methanol solution containing ammonium acetate. UV and scintillation flow type detectors are used. (author) 7 refs.; 8 figs

  4. Estimation of brassylic acid by gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mohammed J. Nasrullah, Erica N. Pfarr, Pooja Thapliyal, Nicholas S. Dusek, Kristofer L. Schiele, Christy Gallagher-Lein, and James A. Bahr

    2010-10-29

    The main focus of this work is to estimate Brassylic Acid (BA) using gas chromatography-mass spectrometry (GC-MS). BA is a product obtained from the oxidative cleavage of Erucic Acid (EA). BA has various applications for making nylons and high performance polymers. BA is a 13 carbon compound with two carboxylic acid functional groups at the terminal end. BA has a long hydrocarbon chain that makes the molecule less sensitive to some of the characterization techniques. Although BA can be characterized by NMR, both the starting material (EA) and products BA and nonanoic acid (NA) have peaks at similar {delta}, ppm values. Hence it becomes difficult for the quick estimation of BA during its synthesis.

  5. The utilization of waste by-products for removing silicate from mineral processing wastewater via chemical precipitation.

    Science.gov (United States)

    Kang, Jianhua; Sun, Wei; Hu, Yuehua; Gao, Zhiyong; Liu, Runqing; Zhang, Qingpeng; Liu, Hang; Meng, Xiangsong

    2017-11-15

    This study investigates an environmentally friendly technology that utilizes waste by-products (waste acid and waste alkali liquids) to treat mineral processing wastewater. Chemical precipitation is used to remove silicate from scheelite (CaWO 4 ) cleaning flotation wastewater and the waste by-products are used as a substitute for calcium chloride (CaCl 2 ). A series of laboratory experiments is conducted to explain the removal of silicate and the characterization and formation mechanism of calcium silicate. The results show that silicate removal reaches 90% when the Ca:Si molar ratio exceeds 1.0. The X-ray diffraction (XRD) results confirm the characterization and formation of calcium silicate. The pH is the key factor for silicate removal, and the formation of polysilicic acid with a reduction of pH can effectively improve the silicate removal and reduce the usage of calcium. The economic analysis shows that the treatment costs with waste acid (0.63 $/m 3 ) and waste alkali (1.54 $/m 3 ) are lower than that of calcium chloride (2.38 $/m 3 ). The efficient removal of silicate is confirmed by industrial testing at a plant. The results show that silicate removal reaches 85% in the recycled water from tailings dam. Copyright © 2017 Elsevier Ltd. All rights reserved.

  6. Gas chromatography-vacuum ultraviolet spectroscopy for analysis of fatty acid methyl esters.

    Science.gov (United States)

    Fan, Hui; Smuts, Jonathan; Bai, Ling; Walsh, Phillip; Armstrong, Daniel W; Schug, Kevin A

    2016-03-01

    A new vacuum ultraviolet (VUV) detector for gas chromatography was recently developed and applied to fatty acid methyl ester (FAME) analysis. VUV detection features full spectral acquisition in a wavelength range of 115-240nm, where virtually all chemical species absorb. VUV absorption spectra of 37 FAMEs, including saturated, monounsaturated, and polyunsaturated types were recorded. Unsaturated FAMEs show significantly different gas phase absorption profiles than saturated ones, and these classes can be easily distinguished with the VUV detector. Another advantage includes differentiating cis/trans-isomeric FAMEs (e.g. oleic acid methyl ester and linoleic acid methyl ester isomers) and the ability to use VUV data analysis software for deconvolution of co-eluting signals. As a universal detector, VUV also provides high specificity, sensitivity, and a fast data acquisition rate, making it a powerful tool for fatty acid screening when combined with gas chromatography. The fatty acid profile of several food oil samples (olive, canola, vegetable, corn, sunflower and peanut oils) were analyzed in this study to demonstrate applicability to real world samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

  7. Aluminum Silicate Nanotube Coating of Siloxane-Poly(lactic acid-Vaterite Composite Fibermats for Bone Regeneration

    Directory of Open Access Journals (Sweden)

    Shuji Yamazaki

    2012-01-01

    Full Text Available In our earlier work, a flexible fibermat consisting of a biodegradable composite with soluble silicate species, which has been reported to enhance bone formation, was prepared successfully using poly(L-lactic acid and siloxane-containing calcium carbonate particles by electrospinning. The fibermat showed enhanced bone formation in an in vivo test. In the present work, to improve the hydrophilicity of skeletal fibers in a fibermat, they were coated with nanotubular aluminum silicate crystals, which have a hydrophilic surface that has excellent affinity to body fluids and a high surface area advantageous for pronounced protein adsorption. The nanotubes were coated easily on the fiber surface using an electrophoretic method. In a conventional contact angle test, a drop of water rapidly penetrated into the nanotube-coated fibermat. The culture test using murine osteoblast-like cells (MC3T3-E1 showed that the cell attachment to the nanotube-coated fibermat at an early stage after seeding was enhanced in comparison with that to the noncoated one. This approach may provide a new method of improving the surface of polymer-based biomaterials.

  8. Gas chromatography of alkylphosphonic and dialkyl phosphinic acids

    International Nuclear Information System (INIS)

    Gasco Sanchez, L.; Barrera Pinero, R.; Ramirez Caceres, A.; Martin Munoz, M.

    1978-01-01

    After carrying out an optimization study on the separation conditions for the TMSr- derivatives, of the hexyl-, cyclohexyl-, heptyl-, and octyl-phosphonic acids; dihexyl dicyclohexyl-, heptyl-, and octyl-phosphinic acids, and dioctyl phosphine oxide, their retention indices (I) at two temperatures and on the OV-1 and OV-17 stationary phase were determined. Correlations between I and molecular structure were established. Calibration factors of these compounds in the flame ionization detector were studied, and the results analyzed taking into account the variables affecting the quantitative results, These results were unbiased but they had a lower precision than that usually achievable in gas chromatography. (Author) 24 refs

  9. Determination of 4-Chloroindole-3-Acetic Acid Methyl Ester in Lathyrus Vicia and Pisum by Gas Chromatography - Mass Spectrometry

    DEFF Research Database (Denmark)

    Engvild, Kjeld Christensen; Egsgaard, Helge; Larsen, Elfinn

    1980-01-01

    4-Chloroindole-3-acetic acid methyl ester was identified unequivocally in Lathyrus latifolius L., Vicia faba L. and Pisum sativum L. by thin layer chromatography, gas chromatography and mass spectrometry. The gas chromatographic system was able to separate underivatized chloroindole-3-acetic acid...... methyl ester isomers. The quantitative determination of 4-chloroindole-3-acetic acid methyl ester in immature seeds of these three species was performed by gas chromatography – mass spectrometry using deuterium labelled 4-chloro-indole-3-acetic acid methyl ester as an internal standard. P. sativum...

  10. Effect of antioxidants and silicates on peroxides in povidone.

    Science.gov (United States)

    Narang, Ajit S; Rao, Venkatramana M; Desai, Divyakant S

    2012-01-01

    Reactive peroxides in povidone often lead to degradation of oxidation-labile drugs. To reduce peroxide concentration in povidone, the roles of storage conditions, antioxidants, and silicates were investigated. Povidone alone and its physical mixtures with ascorbic acid, propyl gallate, sodium sulfite, butylated hydroxyanisole (BHA), or butylated hydroxytoluene (BHT) were stored at 25 °C and 40 °C, at 11%, 32%, and 50% relative humidity. In addition, povidone solution in methanol was equilibrated with silicates (silica gel and molecular sieves), followed by solvent evaporation to recover povidone powder. Peroxide concentrations in povidone were measured. The concentration of peroxides in povidone increased under very-low-humidity storage conditions. Among the antioxidants, ascorbic acid, propyl gallate, and sodium sulfite reduced the peroxide concentration in povidone, whereas BHA and BHT did not. Water solubility appeared to determine the effectiveness of antioxidants. Also, some silicates significantly reduced peroxide concentration in povidone without affecting its functionality as a tablet binder. Porosity of silicates was critical to their ability to reduce the peroxide concentration in povidone. A combination of these approaches can reduce the initial peroxide concentration in povidone and minimize peroxide growth under routine storage conditions. Copyright © 2011 Wiley-Liss, Inc.

  11. Immunoaffinity chromatography of abscisic acid combined with electrospray liquid chromatography–mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Hradecká, Veronika; Novák, Ondřej; Havlíček, Libor; Strnad, Miroslav

    2007-01-01

    Roč. 847, č. 2 (2007), s. 162-173 ISSN 1570-0232 R&D Projects: GA MŠk(CZ) LC06034; GA AV ČR IBS5038351 Institutional research plan: CEZ:AV0Z50380511 Source of funding: V - iné verejné zdroje ; V - iné verejné zdroje Keywords : abscisic acid * immunoaffinity chromatography * liquid chromatography-mass spectrometry Subject RIV: ED - Physiology Impact factor: 2.935, year: 2007

  12. Simultaneous determination of acidic 3,4-dihydroxyphenylalanine metabolites and 5-hydroxyindole-3-acetic acid in urine by high-performance liquid chromatography

    NARCIS (Netherlands)

    Stroomer, A. E.; Overmars, H.; Abeling, N. G.; van Gennip, A. H.

    1990-01-01

    We describe a simple and rapid quantitative method for the simultaneous determination of 3,4-dihydroxyphenylalanine acid metabolites and 5-hydroxyindole-3-acetic acid. After solvent extraction from acidified urine, the acids are analyzed by reversed-phase high-performance liquid chromatography. For

  13. Sensitive Thin-Layer Chromatography Detection of Boronic Acids Using Alizarin

    NARCIS (Netherlands)

    Duval, F.L.; Beek, van T.A.; Zuilhof, H.

    2012-01-01

    A new method for the selective and sensitive detection of boronic acids on thin-layer chromatography plates is described. The plate is briefly dipped in an alizarin solution, allowed to dry in ambient air, and observed under 366 nm light. Alizarin emits a bright yellow fluorescence only in the

  14. Selective silicate-directed motility in diatoms

    DEFF Research Database (Denmark)

    Bondoc, Karen Grace V.; Heuschele, Jan; Gillard, Jeroen

    2016-01-01

    the major sink in the global Si cycle. Dissolved silicic acid (dSi) availability frequently limits diatom productivity and influences species composition of communities. We show that benthic diatoms selectively perceive and behaviourally react to gradients of dSi. Cell speed increases under d...

  15. Determination of organophosphorus acids by thermo-spray liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Wils, E.R.J.; Hulst, A.G.

    1988-01-01

    The determination of thirteen organophosphorus acids, hydrolysis products of nerve agents and pesticides, by a combination of ion-pair liquid chromatography on a reversed-phase C18 column and thermospray mass spectrometry was investigated. Ammonium acetate and three tetraalkylammonium salts with

  16. Ion-exclusion/cation-exchange chromatography with dual detection of the conductivity and spectrophotometry for the simultaneous determination of common inorganic anionic species and cations in river and wastewater.

    Science.gov (United States)

    Nakatani, Nobutake; Kozaki, Daisuke; Mori, Masanobu; Hasebe, Kiyoshi; Nakagoshi, Nobukazu; Tanaka, Kazuhiko

    2011-01-01

    Simultaneous determinations of common inorganic anionic species (SO(4)(2-), Cl(-), NO(3)(-), phosphate and silicate) and cations (Na(+), NH(4)(+), K(+), Mg(2+) and Ca(2+)) were conducted using an ion-chromatography system with dual detection of conductivity and spectrophotometry in tandem. The separation of ionic species on a weakly acidic cation-exchange resin was accomplished using a mixture of 100 mM ascorbic acid and 4 mM 18-crown-6 as an acidic eluent (pH 2.6), after which the ions were detected using a conductivity detector. Subsequently, phosphate and silicate were analyzed based on derivatization with molybdate and spectrophotometry at 700 nm. The detection limits at S/N = 3 ranged from 0.11 to 2.9 µM for analyte ionic species. This method was applied to practical river water and wastewater with acceptable criteria for the anion-cation balance and comparisons of the measured and calculated electrical conductivity, demonstrating the usefulness of the present method for water quality monitoring.

  17. Advances in silver ion chromatography for the analysis of fatty acids and triacylglycerols-2001 to 2011.

    Science.gov (United States)

    Momchilova, Svetlana M; Nikolova-Damyanova, Boryana M

    2012-01-01

    An effort is made to critically present the achievements in silver ion chromatography during the last decade. Novelties in columns, mobile-phase compositions and detectors are described. Recent applications of silver ion chromatography in the analysis of fatty acids and triacylglycerols are presented while stressing novel analytical strategies or new objects. The tendencies in the application of the method in complementary ways with reversed-phase chromatography, chiral chromatography and, especially, mass detection are outlined.

  18. Inorganic polymers from laterite using activation with phosphoric acid and alkaline sodium silicate solution: Mechanical and microstructural properties

    Energy Technology Data Exchange (ETDEWEB)

    Lassinantti Gualtieri, Magdalena, E-mail: magdalena.gualtieri@unimore.it [Dipartimento di Ingegneria " Enzo Ferrari" , Università degli studi di Modena e Reggio Emilia, Via Vignolese 905/a, I-41125 Modena (Italy); Romagnoli, Marcello [Dipartimento di Ingegneria " Enzo Ferrari" , Università degli studi di Modena e Reggio Emilia, Via Vignolese 905/a, I-41125 Modena (Italy); Pollastri, Simone; Gualtieri, Alessandro F. [Dipartimento di Scienze Chimiche e Geologiche, Università degli studi di Modena e Reggio Emilia, Via S. Eufemia 19I, I-41121 Modena (Italy)

    2015-01-15

    Geopolymers from laterite, an iron-rich soil available in developing countries, have great potential as building materials. In this work, laterite from Togo (Africa) was used to prepare geopolymers using both phosphoric acid and alkaline sodium silicate solution. Microstructural properties were investigated by scanning electron microscopy, X-ray powder diffraction and mercury porosimetry, whereas thermal properties were evaluated by thermal analyses. The local environment of iron was studied by X-ray Absorption Spectroscopy (XANES region). The mechanical properties were determined. Modulus of Rupture and Young's modulus fell in the ranges 3.3–4.5 MPa and 12–33 GPa, respectively, rendering the materials good candidates for construction purposes. Heating above 900 °C results in weight-gain, presumably due to iron redox reactions. X-ray Absorption Spectroscopy data evidence changes in the chemical and structural environments of iron following thermal treatment of geopolymers. These changes indicate interaction between the geopolymer structure and iron during heating, possibly leading to redox properties. -- Highlights: •Geopolymerization of laterite is promising for fabrication of building materials. •Both phosphoric acid and alkaline sodium silicate solution can be used for activation. •Thermally activated redox properties of the inorganic polymers were observed.

  19. Inorganic polymers from laterite using activation with phosphoric acid and alkaline sodium silicate solution: Mechanical and microstructural properties

    International Nuclear Information System (INIS)

    Enzo Ferrari, Università degli studi di Modena e Reggio Emilia, Via Vignolese 905/a, I-41125 Modena (Italy))" data-affiliation=" (Dipartimento di Ingegneria Enzo Ferrari, Università degli studi di Modena e Reggio Emilia, Via Vignolese 905/a, I-41125 Modena (Italy))" >Lassinantti Gualtieri, Magdalena; Enzo Ferrari, Università degli studi di Modena e Reggio Emilia, Via Vignolese 905/a, I-41125 Modena (Italy))" data-affiliation=" (Dipartimento di Ingegneria Enzo Ferrari, Università degli studi di Modena e Reggio Emilia, Via Vignolese 905/a, I-41125 Modena (Italy))" >Romagnoli, Marcello; Pollastri, Simone; Gualtieri, Alessandro F.

    2015-01-01

    Geopolymers from laterite, an iron-rich soil available in developing countries, have great potential as building materials. In this work, laterite from Togo (Africa) was used to prepare geopolymers using both phosphoric acid and alkaline sodium silicate solution. Microstructural properties were investigated by scanning electron microscopy, X-ray powder diffraction and mercury porosimetry, whereas thermal properties were evaluated by thermal analyses. The local environment of iron was studied by X-ray Absorption Spectroscopy (XANES region). The mechanical properties were determined. Modulus of Rupture and Young's modulus fell in the ranges 3.3–4.5 MPa and 12–33 GPa, respectively, rendering the materials good candidates for construction purposes. Heating above 900 °C results in weight-gain, presumably due to iron redox reactions. X-ray Absorption Spectroscopy data evidence changes in the chemical and structural environments of iron following thermal treatment of geopolymers. These changes indicate interaction between the geopolymer structure and iron during heating, possibly leading to redox properties. -- Highlights: •Geopolymerization of laterite is promising for fabrication of building materials. •Both phosphoric acid and alkaline sodium silicate solution can be used for activation. •Thermally activated redox properties of the inorganic polymers were observed

  20. Feedlot lamb meat fatty acids profile characterization employing gas chromatography

    Directory of Open Access Journals (Sweden)

    M.I. Cruz-Gonzalez

    2014-06-01

    Full Text Available Fat is an important constituent in diet, not only as an energy source, but for its essential fatty acids associated to fats in foods, considering that some polyunsaturated fatty acids like linoleic, linolenic and arachidonic cannot be synthesized by superior animals like humans. Scientific evidence show that the fatty acids ingest can affect the thrombotic tendency, cardiac rhythm, endothelial function systematic inflammation, insulin sensibility and oxidative stress. Samples from 21 ovine crossbreds from Pelibuey, Blackbelly, Dorper and Katahadin (40 kg average weight feed with corn based balanced diets were taken from loin area 18 h after refrigeration. Saturated and polyunsaturated fatty acids levels were analyzed by gas chromatography. Results in this work showed that the healthy fatty acids levels are higher as compared to saturated fatty acids levels, indicating that this meat can influence consumer’s buying choice decision regarded to their health.

  1. The application of silicon and silicates in dentistry: a review.

    Science.gov (United States)

    Lührs, A-K; Geurtsen, Werner

    2009-01-01

    Silicates and silicate-based compounds are frequently used materials in dentistry. One of their major applications is their use as fillers in different dental filling materials such as glass-ionomer cements, compomers, composites, and adhesive systems. In these materials, the fillers react with acids during the setting process or they improve the mechanical properties by increasing physical resistance, thermal expansion coefficient and radiopacity in acrylic filling materials. They also reduce polymerization shrinkage, and increase esthetics as well as handling properties. Furthermore, silicates are used for the tribochemical silication of different surfaces such as ceramics or alloys. The silicate layer formed in this process is the chemical basis for silanes that form a bond between this layer and the organic composite matrix. It also provides a micromechanical bond between the surface of the material and the composite matrix. Silicates are also a component of dental ceramics, which are frequently used in dentistry, for instance for veneers, inlays, and onlays, for denture teeth, and for full-ceramic crowns or as crown veneering materials.

  2. Hydroxylapatite chromatography.

    Science.gov (United States)

    Broadhurst, A V

    2001-05-01

    Hydroxylapatite (also called hydroxyapatite), a form of calcium phosphate, can be used as a matrix for the chromatography of both proteins and nucleic acids. Protocols are provided for both standard low-pressure chromatography of a protein mixture using a hydroxylapatite column prepared in the laboratory, and an HPLC method, applicable to proteins and nucleic acids, that uses a commercially available column. Alternate protocols describe column chromatography using a step gradient or batch binding and step-gradient elution.

  3. Purification of Peptide Components including Melittin from Bee Venom using gel filtration chromatography and propionic acid/urea polyacrylamide gel electrophoresis

    Directory of Open Access Journals (Sweden)

    Young Chon Choi

    2006-06-01

    Full Text Available Objectives : This study was conducted to carry out Purification of Melittin and other peptide components from Bee Venom using gel filtration chromatography and propionic acid/urea polyacrylamide gel electrophoresis Methods : Melittin and other peptide components were separated from bee venom by using gel filtration chromatography on Sephadex G-50 column in 0.05M ammonium acetate buffer. Results : Melittin and other peptide components were separated from bee venom by using gel filtration chromatography on Sephadex G-50 column in 0.05M ammonium acetate buffer. The fractions obtained from gel filtration chromatography was analyzed by using SDS-PAGE and propionic acid/urea polyacrylamide gel electrophoresis. The melittin obtained from the gel filtration contained residual amount of phospholipase A2 and a protein with molecular weight of 6,000. The contaminating proteins were removed by the second gel filtration chromatography. Conclusion : Gel filtration chromatography and propionic acid/urea polyacrylamide gel electrophoresis are useful to separate peptide components including melittin from bee venom.

  4. Zirconium silicate assisted removal of residual proteins after organic solvent deproteinization of human plasma, enhancing the stability of the LC–ESI-MS response for the bioanalysis of small molecules

    Energy Technology Data Exchange (ETDEWEB)

    Hussain, Shah; Pezzei, Cornelia [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); Güzel, Yüksel [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); ADSI-Austrian Drug Screening Institute, Innrain 66a, 6020 Innsbruck (Austria); Rainer, Matthias [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); Huck, Christian W., E-mail: Christian.W.Huck@uibk.ac.at [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); Bonn, Günther K. [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); ADSI-Austrian Drug Screening Institute, Innrain 66a, 6020 Innsbruck (Austria)

    2014-12-10

    Highlights: • A novel sample preparation technique for isolation of small molecules from human plasma. • Effectiveness of zirconium silicate for the removal of residual proteins after protein precipitation. • Abolishing the consumption of salts for the depletion of residual proteins after protein precipitation. • More than 99.6% removal of plasma proteins. - Abstract: An efficient blood plasma clean-up method was developed, where methanol protein precipitation was applied, followed by zirconium silicate assisted exclusion of residual proteins. A strong binding of zirconium (IV) silicate to the proteins enabled the elimination of remaining proteins after solvent deproteinization through a rapid solid-phase extraction (SPE) procedure. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI/TOF MS) was used for monitoring the proteins during clean-up practice applied to human plasma samples. The proteins were quantified by colorimetric detection using the bicinchoninic acid (BCA) assay. The presented analytical strategy resulted in the depletion of >99.6% proteins from human plasma samples. Furthermore, high-performance liquid chromatography hyphenated to diode-array and electrospray ionization mass spectrometric detection (HPLC–DAD/ESI MS) was applied for qualitative and quantitative analysis of the caffeoylquinic acids (CQAs) and their metabolites in human plasma. The procedure demonstrated high recoveries for the standard compounds spiked at different concentrations. Cynarin and chlorogenic acid were recovered in the range of 81–86% and 78–83%, respectively. Caffeic acid was extracted in the excess of 89–92%, while ferulic acid and dihydroxyhydrocinnamic acid showed a recovery of 87–91% and 92–95%, respectively. The method was partially validated in accordance with FDA-Industry Guidelines for Bioanalytical Method Validation (2001). The presented scheme improves the clean-up efficacy of the methanol deproteinization

  5. Zirconium silicate assisted removal of residual proteins after organic solvent deproteinization of human plasma, enhancing the stability of the LC–ESI-MS response for the bioanalysis of small molecules

    International Nuclear Information System (INIS)

    Hussain, Shah; Pezzei, Cornelia; Güzel, Yüksel; Rainer, Matthias; Huck, Christian W.; Bonn, Günther K.

    2014-01-01

    Highlights: • A novel sample preparation technique for isolation of small molecules from human plasma. • Effectiveness of zirconium silicate for the removal of residual proteins after protein precipitation. • Abolishing the consumption of salts for the depletion of residual proteins after protein precipitation. • More than 99.6% removal of plasma proteins. - Abstract: An efficient blood plasma clean-up method was developed, where methanol protein precipitation was applied, followed by zirconium silicate assisted exclusion of residual proteins. A strong binding of zirconium (IV) silicate to the proteins enabled the elimination of remaining proteins after solvent deproteinization through a rapid solid-phase extraction (SPE) procedure. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI/TOF MS) was used for monitoring the proteins during clean-up practice applied to human plasma samples. The proteins were quantified by colorimetric detection using the bicinchoninic acid (BCA) assay. The presented analytical strategy resulted in the depletion of >99.6% proteins from human plasma samples. Furthermore, high-performance liquid chromatography hyphenated to diode-array and electrospray ionization mass spectrometric detection (HPLC–DAD/ESI MS) was applied for qualitative and quantitative analysis of the caffeoylquinic acids (CQAs) and their metabolites in human plasma. The procedure demonstrated high recoveries for the standard compounds spiked at different concentrations. Cynarin and chlorogenic acid were recovered in the range of 81–86% and 78–83%, respectively. Caffeic acid was extracted in the excess of 89–92%, while ferulic acid and dihydroxyhydrocinnamic acid showed a recovery of 87–91% and 92–95%, respectively. The method was partially validated in accordance with FDA-Industry Guidelines for Bioanalytical Method Validation (2001). The presented scheme improves the clean-up efficacy of the methanol deproteinization

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

    Science.gov (United States)

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

    2003-05-16

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

  7. An optimized method for fatty acid analysis, including quantification of trans fatty acids, in human adipose tissue by gas-liquid chromatography

    DEFF Research Database (Denmark)

    Bysted, Anette; Cold, S; Hølmer, Gunhild Kofoed

    1999-01-01

    Considering the need for a quick direct method for measurement of the fatty acid composition including trans isomers ofhuman adipose tissue we have developed a procedure using gas-liquid chromatography (GLC) alone, which is thussuitable for validation of fatty acid status in epidemiological studies...... for 25 min, and finally raised at 25 degrees C/min to 225 degrees C. The trans and cis isomers of18:1 were well separated from each other, as shown by silver-ion thin-layer chromatography. Verification by standardsshowed that the trans 18:1 isomers with a double bond in position 12 or lower were...

  8. Determination of reactivity rates of silicate particle-size fractions

    Directory of Open Access Journals (Sweden)

    Angélica Cristina Fernandes Deus

    2014-04-01

    Full Text Available The efficiency of sources used for soil acidity correction depends on reactivity rate (RR and neutralization power (NP, indicated by effective calcium carbonate (ECC. Few studies establish relative efficiency of reactivity (RER for silicate particle-size fractions, therefore, the RER applied for lime are used. This study aimed to evaluate the reactivity of silicate materials affected by particle size throughout incubation periods in comparison to lime, and to calculate the RER for silicate particle-size fractions. Six correction sources were evaluated: three slags from distinct origins, dolomitic and calcitic lime separated into four particle-size fractions (2, 0.84, 0.30 and <0.30-mm sieves, and wollastonite, as an additional treatment. The treatments were applied to three soils with different texture classes. The dose of neutralizing material (calcium and magnesium oxides was applied at equal quantities, and the only variation was the particle-size material. After a 90-day incubation period, the RER was calculated for each particle-size fraction, as well as the RR and ECC of each source. The neutralization of soil acidity of the same particle-size fraction for different sources showed distinct solubility and a distinct reaction between silicates and lime. The RER for slag were higher than the limits established by Brazilian legislation, indicating that the method used for limes should not be used for the slags studied here.

  9. Analysis of radioactive mixed hazardous waste using derivatization gas chromatography/mass spectrometry, liquid chromatography, and liquid chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Campbell, J.A.; Lerner, B.D.; Bean, R.M.; Grant, K.E.; Lucke, R.B.; Mong, G.M.; Clauss, S.A.

    1994-08-01

    Six samples of core segments from Tank 101-SY were analyzed for chelators, chelator fragments, and several carboxylic acids by derivatization gas chromatography/mass spectrometry. The major components detected were ethylenediaminetetraacetic acid, nitroso-iminodiacetic acid, nitrilotriacetic acid, citric acid, succinic acid, and ethylenediaminetriacetic acid. The chelator of highest concentration was ethylenediaminetetraacetic acid in all six samples analyzed. Liquid chromatography was used to quantitate low molecular weight acids including oxalic, formic, glycolic, and acetic acids, which are present in the waste as acid salts. From 23 to 61% of the total organic carbon in the samples analyzed was accounted for by these acids

  10. Determination of water-soluble forms of oxalic and formic acids in soils by ion chromatography

    Science.gov (United States)

    Karicheva, E.; Guseva, N.; Kambalina, M.

    2016-03-01

    Carboxylic acids (CA) play an important role in the chemical composition origin of soils and migration of elements. The content of these acids and their salts is one of the important characteristics for agrochemical, ecological, ameliorative and hygienic assessment of soils. The aim of the article is to determine water-soluble forms of same carboxylic acids — (oxalic and formic acids) in soils by ion chromatography with gradient elution. For the separation and determination of water-soluble carboxylic acids we used reagent-free gradient elution ion-exchange chromatography ICS-2000 (Dionex, USA), the model solutions of oxalate and formate ions, and leachates from soils of the Kola Peninsula. The optimal gradient program was established for separation and detection of oxalate and formate ions in water solutions by ion chromatography. A stability indicating method was developed for the simultaneous determination of water-soluble organic acids in soils. The method has shown high detection limits such as 0.03 mg/L for oxalate ion and 0.02 mg/L for formate ion. High signal reproducibility was achieved in wide range of intensities which correspond to the following ion concentrations: from 0.04 mg/g to 10 mg/L (formate), from 0.1 mg/g to 25 mg/L (oxalate). The concentration of formate and oxalate ions in soil samples is from 0.04 to 0.9 mg/L and 0.45 to 17 mg/L respectively.

  11. Poly (Lactic Acid)/Layered Silicate Nanocomposite Films: Effect of Irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Dadbin, S.; Naimian, F.; Akhavan, A.; Hasanpoor, S., E-mail: sdadbin@yahoo.com, E-mail: sdadbin@aeoi.org.ir [Atomic Energy Organization of Iran (AEOI), Nuclear Science and Technology Research Institute, P.O. Box 11365-8486, Tehran, North Kargar (Iran, Islamic Republic of)

    2010-07-01

    Poly (Lactic acid) –layered silicate nanocomposite films were prepared by solution casting method. The films were irradiated with Co{sup 60} radiation facility at dose of 30 kGy. The effect of gamma irradiation on mechanical properties of the neat PLA and nanocomposites was evaluated by data obtained from tensile testing measurements. The tensile strength of the irradiated PLA films increased with addition of 1 wt% Triallyl Cyanurate (TAC) indicating crosslink formation. Significant ductile behavior was observed in the PLA nanocomposites containing 4 pph of nanoclay. Incorporation of nanoclay particles in the PLA matrix stimulated crystal growth as it was studied by differential scanning calorimetry (DSC). The morphology of the nanocomposites characterized by transmission electron microscopy (TEM) and X- ray diffraction (XRD) revealed an exfoliated morphology in the PLA nanocomposite films containing 4 pph of nanoclay. Only very small changes were observed in the chemical structure of the irradiated samples as it was investigated by Fourier transform infrared (FTIR) spectroscopy. Enzymatic degradation rate of PLA and its nanocomposite decreased with increasing crystallinity of the samples. The rate of weight loss was also affected by the morphology of the nanocomposites. (author)

  12. Poly (Lactic Acid)/Layered Silicate Nanocomposite Films: Effect of Irradiation

    International Nuclear Information System (INIS)

    Dadbin, S.; Naimian, F.; Akhavan, A.; Hasanpoor, S.

    2010-01-01

    Poly (Lactic acid) –layered silicate nanocomposite films were prepared by solution casting method. The films were irradiated with Co 60 radiation facility at dose of 30 kGy. The effect of gamma irradiation on mechanical properties of the neat PLA and nanocomposites was evaluated by data obtained from tensile testing measurements. The tensile strength of the irradiated PLA films increased with addition of 1 wt% Triallyl Cyanurate (TAC) indicating crosslink formation. Significant ductile behavior was observed in the PLA nanocomposites containing 4 pph of nanoclay. Incorporation of nanoclay particles in the PLA matrix stimulated crystal growth as it was studied by differential scanning calorimetry (DSC). The morphology of the nanocomposites characterized by transmission electron microscopy (TEM) and X- ray diffraction (XRD) revealed an exfoliated morphology in the PLA nanocomposite films containing 4 pph of nanoclay. Only very small changes were observed in the chemical structure of the irradiated samples as it was investigated by Fourier transform infrared (FTIR) spectroscopy. Enzymatic degradation rate of PLA and its nanocomposite decreased with increasing crystallinity of the samples. The rate of weight loss was also affected by the morphology of the nanocomposites. (author)

  13. Method for the routine quantitative gas chromatographic analysis of major free fatty acids in butter and cream.

    Science.gov (United States)

    Woo, A H; Lindsay, R C

    1980-07-01

    A rapid quantiative method was developed for routine analysis of the major, even carbon-numbered free fatty acids in butter and cream. Free fatty acids were isolated directly from intact samples by a modified silicic acid-potassium hydroxide arrestant column and were separated by gas chromatography with a 1.8 m x 2 mm inner diameter glass column packed with 10% neopentyl glycol adipate on 80/100 Chromosorb W. Purified, formic acid-saturated carrier gas was required for minimal peak tailing and extended column life. The accuracy and reproducibility of the mmethod was established through quantitative recovery studies of free fatty acid mixtures, free fatty acids added to butter, and replicate analysis of butter and cream samples.

  14. [Determination a variety of acidic gas in air of workplace by Ion Chromatography].

    Science.gov (United States)

    Li, Shiyong

    2014-10-01

    To establish a method for determination of a variety of acid gas in the workplace air by Ion Chromatography. (hydrofluoric acid, hydrogen chloride or hydrochloric acid, sulfur anhydride or sulfuric acid, phosphoric acid, oxalic acid). The sample in workplace air was collected by the porous glass plate absorption tube containing 5 ml leacheate. (Sulfuric acid fog, phosphoric acid aerosol microporous membrane after collection, eluted with 5 ml of eluent.) To separated by AS14+AG14 chromatography column, by carbonate (2.0+1.0) mmol/L (Na(2)CO(3)-NaHCO(3)) as eluent, flow rate of 1 ml/min, then analyzed by electrical conductivity detector. The retain time was used for qualitative and the peak area was used for quantitation. The each ion of a variety of acid gas in the air of workplace were excellent in carbonate eluent separation. The linear range of working curve of 0∼20 mg/L. The correlation coefficient r>0.999; lower detection limit of 3.6∼115 µg/L; quantitative limit of 0.012∼0.53 mg/L; acquisition of 15L air were measured, the minimum detection concentration is 0.004 0∼0.13 mg/m(3). The recovery rate is 99.7%∼101.1%. In the sample without mutual interference ions. Samples stored at room temperature for 7 days. The same analysis method, the detection of various acidic gases in the air of workplace, simple operation, good separation effect, high sensitivity, high detection efficiency, easy popularization and application.

  15. Isolation of a furan fatty acid from Hevea brasiliensis latex employing the combined use of pH-zone-refining and conventional countercurrent chromatography.

    Science.gov (United States)

    Englert, Michael; Ulms, Kerstin; Wendlinger, Christine; Vetter, Walter

    2016-02-01

    Furan fatty acids are valuable and bioactive minor fatty acids that usually contribute chromatography. A first run using pH-zone-refining countercurrent chromatography provided 48.4 mg of 9-(3-methyl-5-pentylfuran-2-yl)-nonanoic acid from 210 mg latex extract in a purity of 95%. The purity was increased to 99% by means of one second run in conventional countercurrent chromatography mode. The Structure and purity of 9-(3-methyl-5-pentylfuran-2-yl)-nonanoic acid were determined by gas chromatography coupled to mass spectrometry and (1)H and (13)C NMR spectroscopy. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Aluminum Silicate Nanotube Modification of Cotton-Like Siloxane-poly(L-lactic acid-vaterite Composites

    Directory of Open Access Journals (Sweden)

    Daiheon Lee

    2013-01-01

    Full Text Available In our earlier work, a cotton-like biodegradable composite, consisting of poly(L-lactic acid with siloxane-containing vaterite, has been prepared by electrospinning. In the present work, the fibers skeleton of the cotton-like composites was modified successfully with imogolite, which is hydrophilic and biocompatible, via a dip process using ethanol diluted solution to improve the cellular initial attachment. Almost no change in the fiber morphology after the surface modification was observed. The surface-modified composite showed the similar calcium and silicate ions releasabilities, for activating the osteoblasts, as an unmodified one. Cell culture tests showed that the initial adhesion of murine osteoblast-like cells on the surface of the fibers was enhanced by surface modification.

  17. Steam based conversion coating on AA6060 alloy: Effect of sodium silicate chemistry and corrosion performance

    Science.gov (United States)

    Din, Rameez Ud; Bordo, Kirill; Tabrizian, Naja; Jellesen, Morten Stendahl; Ambat, Rajan

    2017-11-01

    Surface treatment of aluminium alloy AA6060 using an industrially applicable pilot steam jet system with and without silicate chemistry has been investigated. Treatment using steam alone and steam with silicate, resulted in an oxide layer formation with thickness ∼425 nm and ∼160 nm, respectively. Moreover, the use of sodium silicate resulted in the formation of distinct microstructure and incorporation of silicate into the oxide film. These oxide films reduced the anodic activity 4 times, while the corrosion protection by silicate containing oxide was the function of its concentration. Further, in acid salt spray and filiform corrosion tests, oxide layer containing silicate exhibited two times higher corrosion resistance.

  18. Comparison of Genetic Parameters Estimation of Fatty Acids from Gas Chromatography and FT-IR in Holsteins

    DEFF Research Database (Denmark)

    Poulsen, Nina Aagaard; Eskildsen, Carl Emil; Skov, T.

    or on fatty acids data measured from gas chromatography in 371 Danish Holstein cows. Results showed similar heritability estimates and strong genomic correlations for most of the fatty acids. However, for some fatty acids, the choice of data affected the genetic parameter estimation, which may be due...

  19. Synthesis and Characterization of Modified Epoxy Resins by Silicic Acid Tetraethyl Ester and Nano-SiO2

    Institute of Scientific and Technical Information of China (English)

    李海燕; 张之圣

    2004-01-01

    A kind of modified epoxy resins was obtained by condensation of epoxy resin with silicic acid tetraethyl ester(TEOS) and nano-SiO2. The reactions were performed with hydrochloric acid as a catalyst at 63 °C.The structure, thermal stability and morphological characteristics of the modified epoxy resins were studied through infrared spectra(FT-IR) analysis, thermogravimetric (TG) analysis and scanning electron microscopy respectively. It has been found from the IR and TG study that modified epoxy resins have greater thermal stability than epoxy resins, and its thermal stability has been improved by the formation of inter-crosslinked network structure. The modified epoxy resins exhibit heterogeneous morphology and heterogeneity increases with more TEOS feeding, which in turn confirms the formation of inter-crosslinked network structure in modified epoxy resins.

  20. Production of a calcium silicate cement material from alginate impression material.

    Science.gov (United States)

    Washizawa, Norimasa; Narusawa, Hideaki; Tamaki, Yukimichi; Miyazaki, Takashi

    2012-01-01

    The purpose of this study was to synthesize biomaterials from daily dental waste. Since alginate impression material contains silica and calcium salts, we aimed to synthesize calcium silicate cement from alginate impression material. Gypsum-based investment material was also investigated as control. X-ray diffraction analyses revealed that although firing the set gypsum-based and modified investment materials at 1,200°C produced calcium silicates, firing the set alginate impression material did not. However, we succeeded when firing the set blend of pre-fired set alginate impression material and gypsum at 1,200°C. SEM observations of the powder revealed that the featured porous structures of diatomite as an alginate impression material component appeared useful for synthesizing calcium silicates. Experimentally fabricated calcium silicate powder was successfully mixed with phosphoric acid solution and set by depositing the brushite. Therefore, we conclude that the production of calcium silicate cement material is possible from waste alginate impression material.

  1. Wear and chemistry of zirconium-silicate, aluminium-silicate and zirconium-aluminium-silicate glasses in alkaline medium

    International Nuclear Information System (INIS)

    Rouse, C.G.; Lemos Guenaga, C.M. de

    1984-01-01

    A study of the chemical durability, in alkaline solutions, of zirconium silicate, aluminium silicate, zirconium/aluminium silicate glasses as a function of glass composition is carried out. The glasses were tested using standard DIN-52322 method, where the glass samples are prepared in small polished pieces and attacked for 3 hours in a 800 ml solution of 1N (NaOH + NA 2 CO 3 ) at 97 0 C. The results show that the presence of ZrO 2 in the glass composition increases its chemical durability to alkaline attack. Glasses of the aluminium/zirconium silicate series were melted with and without TiO 2 . It was shown experimentally that for this series of glasses, the presence of both TiO 2 and ZrO 2 gave better chemical durability results. However, the best overall results were obtained from the simpler zirconium silicate glasses, where it was possible to make glasses with higher values of ZrO 2 . (Author) [pt

  2. Application and comparison of high-speed countercurrent chromatography and high performance liquid chromatography in preparative enantioseparation of α-substitution mandelic acids.

    Science.gov (United States)

    Tong, Shengqiang; Zhang, Hu; Shen, Mangmang; Ito, Yoichiro; Yan, Jizhong

    2015-04-01

    Preparative enantioseparations of α-cyclopentylmandelic acid and α-methylmandelic acid by high-speed countercurrent chromatography (HSCCC) and high performance liquid chromatography (HPLC) were compared using hydroxypropy-β-cyclodextrin (HP-β-CD) and sulfobutyl ether-β-cyclodextrin (SBE-β-CD) as the chiral mobile phase additives. In preparative HPLC the enantioseparation was achieved on the ODS C 18 reverse phase column with the mobile phase composed of a mixture of acetonitrile and 0.10 mol L -1 phosphate buffer at pH 2.68 containing 20 mmol L -1 HP-β-CD for α-cyclopentylmandelic acid and 20 mmol L -1 SBE-β-CD for α-methylmandelic acid. The maximum sample size for α-cyclopentylmandelic acid and α-methylmandelic acid was only about 10 mg and 5 mg, respectively. In preparative HSCCC the enantioseparations of these two racemates were performed with the two-phase solvent system composed of n -hexane-methyl tert. -butyl ether-0.1 molL -1 phosphate buffer solution at pH 2.67 containing 0.1 mol L -1 HP-β-CD for α-cyclopentylmandelic acid (8.5:1.5:10, v/v/v) and 0.1 mol L -1 SBE-β-CD for α-methylmandelic acid (3:7:10, v/v/v). Under the optimum separation conditions, total 250 mg of racemic α-cyclopentylmandelic acid could be completely enantioseparated by HSCCC with HP-β-CD as a chiral mobile phase additive in a single run, yielding 105-110 mg of enantiomers with 95-98% purity and 85-90% recovery. But, no complete enantioseparation of α-methylmandelic acid was achieved by preparative HSCCC with either of the chiral selectors due to their limited enantioselectivity. In this paper preparative enantioseparation by HSCCC and HPLC was compared from various aspects.

  3. Separation of phenolic acids from sugarcane rind by online solid-phase extraction with high-speed counter-current chromatography.

    Science.gov (United States)

    Geng, Ping; Fang, Yingtong; Xie, Ronglong; Hu, Weilun; Xi, Xingjun; Chu, Qiao; Dong, Genlai; Shaheen, Nusrat; Wei, Yun

    2017-02-01

    Sugarcane rind contains some functional phenolic acids. The separation of these compounds from sugarcane rind is able to realize the integrated utilization of the crop and reduce environment pollution. In this paper, a novel protocol based on interfacing online solid-phase extraction with high-speed counter-current chromatography (HSCCC) was established, aiming at improving and simplifying the process of phenolic acids separation from sugarcane rind. The conditions of online solid-phase extraction with HSCCC involving solvent system, flow rate of mobile phase as well as saturated extent of absorption of solid-phase extraction were optimized to improve extraction efficiency and reduce separation time. The separation of phenolic acids was performed with a two-phase solvent system composed of butanol/acetic acid/water at a volume ratio of 4:1:5, and the developed online solid-phase extraction with HSCCC method was validated and successfully applied for sugarcane rind, and three phenolic acids including 6.73 mg of gallic acid, 10.85 mg of p-coumaric acid, and 2.78 mg of ferulic acid with purities of 60.2, 95.4, and 84%, respectively, were obtained from 150 mg sugarcane rind crude extracts. In addition, the three different elution methods of phenolic acids purification including HSCCC, elution-extrusion counter-current chromatography and back-extrusion counter-current chromatography were compared. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Steam based conversion coating on AA6060 alloy: Effect of sodium silicate chemistry and corrosion performance

    DEFF Research Database (Denmark)

    Din, Rameez Ud; Bordo, Kirill; Tabrizian, Naja

    2017-01-01

    . Moreover, the use of sodium silicate resulted in the formation of distinct microstructure and incorporation of silicate into the oxide film. These oxide films reduced the anodic activity 4 times, while the corrosion protection by silicate containing oxide was the function of its concentration. Further......Surface treatment of aluminium alloy AA6060 using an industrially applicable pilot steam jet system with and without silicate chemistry has been investigated. Treatment using steam alone and steam with silicate, resulted in an oxide layer formation with thickness ∼425 nm and ∼160 nm, respectively......, in acid salt spray and filiform corrosion tests, oxide layer containing silicate exhibited two times higher corrosion resistance....

  5. FRACTIONATION OF FATTY ACID OMEGA 3, 6 AND 9 FROM SNAIL (Achatina fulica USING COLOUM CHROMATOGRAPHY

    Directory of Open Access Journals (Sweden)

    Winarto Haryadi

    2010-06-01

    Full Text Available The extraction of fat from snail has been carried out by Soxhlet extractor with petroleum ether solvent. Fatty product from extraction was transesterificated in BF3/methanol solvent for an hour by reflux procedure, then extracted by n-hexane to produce methyl ester fatty acid. Free water fatty acid methyl ester was analyzed by Gas Chromatography-Mass spectrometer (GC-MS. Fatty acid ester was separated from its fractions use column chromatography in n-hexane, n-hexane:dietil eter (2:1 v/v, dietil eter, aseton, ethanol and methanol. This fractions wer also analized by GC-MS. From GC-MS data sheet can be obtained 5 fractions which details are; fraction 1 contains omega 3: 27.54 %, omega 6: 15.40 % and omega 9: 6.77 %. Fraction 2 contains omega 3: 3.08 %, omega 6: 15.62 % and omega 9: 10.72 %. Fraction 3 contains omega 6: 3.57 %, omega 9: 7.02 % and none omega 3 inside it. Omega 3, 6 and 9 can't be identification in fraction 4 and 5.   Keywords: extraction, transesterification, column chromatography, GC-MS

  6. Estimation of Fatty Acids in Corn Oil by Gas Capillary Chromatography

    International Nuclear Information System (INIS)

    Kamal, Mohammad A; Klein Peter

    2007-01-01

    Fatty acids provide energy as well as play important role in some cellular structures like cell membrane and certain hormones. Saturated fatty acids are usually found in animal products and in some vegetable oils as well. These saturated fatty acids may be a factor in weight gain and obesity but eating them in moderate amounts may not be damaging to health of every person. Monounsaturated fatty acids can lower blood levels of low density lipoprotein cholesterol and have potential to increase blood levels of high density lipoprotein cholesterol and by this way plays protective role against heart disease. The omega 3 and 6 fatty acids have vital roles in many biological systems such as nervous, immune, cardiovascular, dermal and vision systems. Therefore, it is essential to optimize the instrumental conditions and column specification for the estimation of various fatty acids in the oil, which was considered in the current study using Gas Capillary Chromatography. (author)

  7. Rubber curing chemistry governing the orientation of layered silicate

    Directory of Open Access Journals (Sweden)

    2007-11-01

    Full Text Available The effect of curing systems on the orientation and the dispersion of the layered silicates in acrylonitrile butadiene rubber nanocomposite is reported. Significant differences in X-ray diffraction pattern between peroxide curing and sulfur curing was observed. Intense X-ray scattering values in the XRD experiments from peroxide cured vulcanizates indicate an orientation of the layers in a preferred direction as evinced by transmission electron micrographs. However, sulfur cured vulcanizates show no preferential orientation of the silicate particles. Nevertheless, a closer inspection of transmission electron microscopy (TEM images of peroxide and sulfur cured samples shows exfoliated silicate layers in the acrylonitrile butadiene rubber (NBR matrix. It was revealed in the prevailing study that the use of an excess amount of stearic acid in the formulation of the sulfur curing package leads to almost exfoliated type X-ray scattering pattern.

  8. High-Throughput Analysis of Sucrose Fatty Acid Esters by Supercritical Fluid Chromatography/Tandem Mass Spectrometry

    Science.gov (United States)

    Hori, Katsuhito; Tsumura, Kazunobu; Fukusaki, Eiichiro; Bamba, Takeshi

    2014-01-01

    Supercritical fluid chromatography (SFC) coupled with triple quadrupole mass spectrometry was applied to the profiling of sucrose fatty acid esters (SEs). The SFC conditions (column and modifier gradient) were optimized for the effective separation of SEs. In the column test, a silica gel reversed-phase column was selected. Then, the method was used for the detailed characterization of commercial SEs and the successful analysis of SEs containing different fatty acids. The present method allowed for fast and high-resolution separation of monoesters to tetra-esters within a shorter time (15 min) as compared to the conventional high-performance liquid chromatography. The applicability of our method for the analysis of SEs was thus demonstrated. PMID:26819875

  9. SEPARATION OF T-MAZ ETHOXYLATED SORBITAN FATTY ACID ESTERS BY SUPERCRITICAL FLUID CHROMATOGRAPHY

    Science.gov (United States)

    The application of supercritical fluid chromatography (SFC) to the analysis of T-MAZ ethoxylated sorbitan fatty acid esters is described. FC separation methods utilize a density programming technique and a 50 um I.D. capillary column. his work demonstrates that capillary column S...

  10. An Efficient Protocol for Preparation of Gallic Acid from Terminalia bellirica (Gaertn.) Roxb by Combination of Macroporous Resin and Preparative High-Performance Liquid Chromatography.

    Science.gov (United States)

    Zou, Denglang; Chen, Tao; Chen, Chen; Li, Hongmei; Liu, Yongling; Li, Yulin

    2016-08-01

    In this article, macroporous resin column chromatography and preparative high-performance liquid chromatography were applied for preparation of gallic acid from Terminalia bellirica (Gaertn.) Roxb. In the first step, six kinds of resins were investigated by adsorption and desorption tests and AB-8 macroporous resin was selected for the enrichment of gallic acid. As a result, 20 g of gallic acid at a purity of 71% could be separated from 100 g of crude extract in which the content of gallic acid was 16.7% and the recovery of gallic acid reached 85.0%. In the second step, preparative high-performance liquid chromatography was selected to purify gallic acid. As a result, 640 mg of gallic acid at a purity of 99.1% was obtained from 1 g of sample in 35 min. The results demonstrated that macroporous resin coupled with preparative high-performance liquid chromatography was suitable for preparation of gallic acid from T. bellirica (Gaertn.) Roxb. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  11. Argillization by descending acid at Steamboat Springs, Nevada

    Science.gov (United States)

    Schoen, Robert; White, Donald E.; Hemley, J.J.

    1974-01-01

    Steamboat Springs, Nevada, an area of present-day hot springs, clearly illustrates the genetic dependence of some kaolin deposits on hot-spring activity. Andesite, granodiorite and arkosic sediments are locally altered at the land surface to siliceous residues consisting of primary quartz and anatase, plus opal from primary silicates. These siliceous residues commonly exhibit the textural and structural features of their unaltered equivalents. Beneath the siliceous residues, kaolin and alunite replace primary silicates and fill open spaces, forming a blanketlike deposit. Beneath the kaolin-alunite zone, montmorillonite, commonly accompanied by pyrite, replaces the primary silicates. On the ground surface, the same alteration mineral zones can be traced outward from the siliceous residue; however, hematite rather than pyrite accompanies montmorillonite.Chemical analysis indicates that sulfuric acid is the active altering agent. The acid forms from hydrogen sulfide that exsolves from deep thermal water, rises above the water table and is oxidized by sulfur-oxidizing bacteria living near the ground surface. This acid dissolves in precipitation or condensed water vapor and percolates downward destroying most of the primary minerals producing a siliceous residue. Coincidence of the water table with the downward transition from siliceous residue to kaolin-alunite signifies decreasing hydrogen metasomatism because of dilution of descending acid by ground water.In hot-spring areas, beds of siliceous sinter deposited at the surface by hypogene thermal water look, superficially, like areas of surficial acid alteration. Features diagnostic of a surficial alteration are the relict rock structures of a siliceous residue and a kaolin-alunite zone immediately beneath.

  12. Effects of surface application of dolomitic limestone and calcium-magnesium silicate on soybean and maize in rotation with green manure in a tropical region

    Directory of Open Access Journals (Sweden)

    Gustavo Spadotti Amaral Castro

    2015-01-01

    Full Text Available Although lime is currently the material most frequently used to ameliorate soil acidity in Brazil, silicate could efficiently replace this source because of its greater solubility and its greater silicon content, which are beneficial for plant development. This study aimed to evaluate the effects of superficial lime and silicate application on soil chemical attributes as well as on soybean and maize nutrition and grain yields when these crops are grown in rotation with green manure. The experimental design was a complete randomized block with sixteen replicates. Plots were treated with one of two materials for acidity correction (dolomitic lime and calcium/magnesium silicate or with no soil correction, as a control. Silicate corrected soil acidity and increased exchangeable base levels in soil at greater depths faster than does liming. The application of both acidity-correcting materials increased N, Ca and Mg leaf concentrations, and all yield components and grain yield in soybean; but in maize, just silicate also increased N and Si when compared with lime, whereas both acidity-correcting increased just two yield components: grains per ear and mass of 100 grains, resulting in highest grain yield. The application of both acidity-correcting materials increased dry matter production of green manures, but for pigeon pea the silicate provided the best result in this dry-winter region.

  13. The importance of the Maillard-metal complexes and their silicates in astrobiology

    Science.gov (United States)

    Liesch, Patrick J.; Kolb, Vera M.

    2007-09-01

    The Maillard reaction occurs when sugars and amino acids are mixed together in the solid state or in the aqueous solution. Since both amino acids and sugar-like compounds are found on meteorites, we hypothesized that they would also undergo the Maillard reaction. Our recent work supports this idea. We have shown previously that the water-insoluble Maillard products have substantial similarities with the insoluble organic materials from the meteorites. The Maillard organic materials are also part of the desert varnish on Earth, which is a dark, shiny, hard rock coating that contains iron and manganese and is glazed in silicate. Rocks that are similar in appearance to the desert varnish have been observed on the Martian surface. They may also contain the organic materials. We have undertaken study of the interactions between the Maillard products, iron and other metals, and silicates, to elucidate the role of the Maillard products in the chemistry of desert varnish and meteorites. Specifically, we have synthesized a series of the Maillard-metal complexes, and have tested their reactivity towards silicates. We have studied the properties of these Maillard-metal-silicate products by the IR spectroscopy. The astrobiological potential of the Maillard-metal complexes is assessed.

  14. Enhanced detection of amino acids in hydrophilic interaction chromatography electrospray tandem mass spectrometry with carboxylic acids as mobile phase additives.

    Science.gov (United States)

    Yin, Dengyang; Hu, Xunxiu; Liu, Dantong; Du, Wencheng; Wang, Haibo; Guo, Mengzhe; Tang, Daoquan

    2017-06-01

    Liquid chromatography coupled with mass spectrometry technique has been widely used in the analysis of biological targets such as amino acids, peptides, and proteins. In this work, eight common single carboxylic acids or diacids, which contain different pKa have been investigated as the additives to the analysis of amino acids. As the results, carboxylic acid additive can improve the signal intensity of acidity amino acids such as Asp and Glu and the chromatographic separation of basic amino acids such as Arg, His, and Lys. In particular, the diacids have better performance than single acids. The proposed mechanism is that the diacid has hydrogen bond interaction with amino acids to reduce their polarity/amphiprotic characteristics. Besides, oxalic acid has been found having better enhancement than phthalic acid by overall consideration. Therefore, we successfully quantified the 15 amino acids in Sepia bulk pharmaceutical chemical by using oxalic acid as the additive.

  15. Oxygen and silicon stable isotopes of diatom silica. Reconstructing changes in surface water hydrography and silicic acid utilization in the late Pleistocene subarctic Pacific

    Energy Technology Data Exchange (ETDEWEB)

    Maier, Edith

    2014-03-05

    Deglacial variations in upper ocean nutrient dynamics and stratification in high latitudes, as well as associated changes in thermohaline overturning circulation, are thought to have played a key role in changing atmospheric CO{sub 2} concentrations. This thesis examines the relationship between past changes in subarctic Pacific upper ocean stratification and nutrient (silicic acid) utilization, using oxygen and silicon stable isotopes of diatom silica, for the first time at millennial-scale resolution and analyzed with a new and efficient instrumentation set-up. The isotopic data, presented in three manuscripts, show a consistent picture of millennial-scale variability in upper ocean stratification and silicic acid utilization during the last ∝50 ka BP, e.g. indicating that the subarctic Pacific was a source region for atmospheric CO{sub 2} during the last deglaciation (late Heinrich Stadial 1 and the Boelling/Alleroed). The presented results demonstrate the high potential of combined diatom oxygen and silicon stable isotope analysis especially for, but not restricted to, marine regions characterized by a low biogenic carbonate content like the subarctic Pacific and the Southern Ocean.

  16. Oxygen and silicon stable isotopes of diatom silica. Reconstructing changes in surface water hydrography and silicic acid utilization in the late Pleistocene subarctic Pacific

    International Nuclear Information System (INIS)

    Maier, Edith

    2014-01-01

    Deglacial variations in upper ocean nutrient dynamics and stratification in high latitudes, as well as associated changes in thermohaline overturning circulation, are thought to have played a key role in changing atmospheric CO 2 concentrations. This thesis examines the relationship between past changes in subarctic Pacific upper ocean stratification and nutrient (silicic acid) utilization, using oxygen and silicon stable isotopes of diatom silica, for the first time at millennial-scale resolution and analyzed with a new and efficient instrumentation set-up. The isotopic data, presented in three manuscripts, show a consistent picture of millennial-scale variability in upper ocean stratification and silicic acid utilization during the last ∝50 ka BP, e.g. indicating that the subarctic Pacific was a source region for atmospheric CO 2 during the last deglaciation (late Heinrich Stadial 1 and the Boelling/Alleroed). The presented results demonstrate the high potential of combined diatom oxygen and silicon stable isotope analysis especially for, but not restricted to, marine regions characterized by a low biogenic carbonate content like the subarctic Pacific and the Southern Ocean.

  17. Composite nanoparticles: A new way to siliceous materials and a model of biosilica synthesis

    International Nuclear Information System (INIS)

    Annenkov, Vadim V.; Pal'shin, Viktor A.; Verkhozina, Olga N.; Larina, Lyudmila I.; Danilovtseva, Elena N.

    2015-01-01

    A new polyampholyte based on poly (acrylic acid) which bears pendant polyamine oligomeric chains (average number of the nitrogen atoms is 11.2) is obtained. This polymer is a model of silaffins – proteins playing important role in formation of siliceous structures in diatom algae and sponges. The polymer catalyses condensation of silicic acid. The obtained solutions contain oligosilicates coordinated with the polymer chains. The action of 50,000 g gravity on this solution results in concentrating-induced condensation of the pre-condensed siliceous oligomers. The obtained solid silica contains 4% admixture of the organic polymer which is close to the silica from diatom frustules. These results confirm the hypothesis about formation of biosilica under the action of desiccation agent, e.g. aquaporins. The formation of solid substances during centrifugation of solutions containing soluble oligomers is a new promising approach to inorganic and composite materials which allows to work in aqueous medium and to reuse the organic polymer. - Highlights: • A polyampholyte with pendant polyamine chains is obtained. • The polymer catalyses condensation of silicic acid giving stable solutions. • Gravity-induced (50,000 g) formation of solid silica was observed in these solutions. • The obtained silica is close to biosilica from diatom frustules. • A new approach to inorganic and composite materials is proposed.

  18. Composite nanoparticles: A new way to siliceous materials and a model of biosilica synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Annenkov, Vadim V., E-mail: annenkov@lin.irk.ru [Limnological Institute, Siberian Branch of the Russian Academy of Sciences, Irkutsk 664033 (Russian Federation); Pal' shin, Viktor A.; Verkhozina, Olga N. [Limnological Institute, Siberian Branch of the Russian Academy of Sciences, Irkutsk 664033 (Russian Federation); Larina, Lyudmila I. [A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, Irkutsk 664033 (Russian Federation); Danilovtseva, Elena N. [Limnological Institute, Siberian Branch of the Russian Academy of Sciences, Irkutsk 664033 (Russian Federation)

    2015-09-01

    A new polyampholyte based on poly (acrylic acid) which bears pendant polyamine oligomeric chains (average number of the nitrogen atoms is 11.2) is obtained. This polymer is a model of silaffins – proteins playing important role in formation of siliceous structures in diatom algae and sponges. The polymer catalyses condensation of silicic acid. The obtained solutions contain oligosilicates coordinated with the polymer chains. The action of 50,000 g gravity on this solution results in concentrating-induced condensation of the pre-condensed siliceous oligomers. The obtained solid silica contains 4% admixture of the organic polymer which is close to the silica from diatom frustules. These results confirm the hypothesis about formation of biosilica under the action of desiccation agent, e.g. aquaporins. The formation of solid substances during centrifugation of solutions containing soluble oligomers is a new promising approach to inorganic and composite materials which allows to work in aqueous medium and to reuse the organic polymer. - Highlights: • A polyampholyte with pendant polyamine chains is obtained. • The polymer catalyses condensation of silicic acid giving stable solutions. • Gravity-induced (50,000 g) formation of solid silica was observed in these solutions. • The obtained silica is close to biosilica from diatom frustules. • A new approach to inorganic and composite materials is proposed.

  19. Analyses and predictions of the thermodynamic properties and phase diagrams of silicate systems

    Energy Technology Data Exchange (ETDEWEB)

    Blander, M. (Argonne National Lab., IL (United States)); Pelton, A.; Eriksson, G. (Ecole Polytechnique, Montreal, PQ (Canada). Dept. of Metallurgy and Materials Engineering)

    1992-01-01

    Molten silicates are ordered solutions which can not be well represented by the usual polynomial representation of deviations from ideal solution behavior (i.e. excess free energies of mixing). An adaptation of quasichemical theory which is capable of describing the properties of ordered solutions represents the measured properties of binary silicates over broad ranges of composition and temperature. For simple silicates such as the MgO-FeO-SiO{sub 2} ternary system, in which silica is the only acid component, a combining rule generally leads to good predictions of ternary solutions from those of the binaries. In basic solutions, these predictions are consistent with those of the conformal ionic solution theory. Our results indicate that our approach could provide a potentially powerful tool for representing and predicting the properties of multicomponent molten silicates.

  20. Analyses and predictions of the thermodynamic properties and phase diagrams of silicate systems

    Energy Technology Data Exchange (ETDEWEB)

    Blander, M. [Argonne National Lab., IL (United States); Pelton, A.; Eriksson, G. [Ecole Polytechnique, Montreal, PQ (Canada). Dept. of Metallurgy and Materials Engineering

    1992-07-01

    Molten silicates are ordered solutions which can not be well represented by the usual polynomial representation of deviations from ideal solution behavior (i.e. excess free energies of mixing). An adaptation of quasichemical theory which is capable of describing the properties of ordered solutions represents the measured properties of binary silicates over broad ranges of composition and temperature. For simple silicates such as the MgO-FeO-SiO{sub 2} ternary system, in which silica is the only acid component, a combining rule generally leads to good predictions of ternary solutions from those of the binaries. In basic solutions, these predictions are consistent with those of the conformal ionic solution theory. Our results indicate that our approach could provide a potentially powerful tool for representing and predicting the properties of multicomponent molten silicates.

  1. Geographic variation in the relationships of temperature, salinity or sigma sub t versus plant nutrient concentrations in the world ocean. [silicic acid, nitrate, and phosphate concentration

    Science.gov (United States)

    Kamykowski, D.; Zentara, S. J.

    1985-01-01

    A NODC data set representing all regions of the world ocean was analyzed for temperature and sigma-t relationships with nitrate, phosphate or silicic acid. Six cubic regressions were for each ten degree square of latitude and longitude containing adequate data. World maps display the locations that allow the prediction of plant nutrient concentrations from temperature or sigma-t. Geographic coverage improves along the sequence: nitrate, phosphate, and silicic acid and is better for sigma-t than for temperature. Contour maps of the approximate temperature of sigma-t at which these nitrients are no longer measurable in a parcel of water are generated, based on a percentile analysis of the temperature or sigma-t at which less than a selected amount of plant nutrient occurs. Results are stored on magnetic tape in tabular form. The global potential to predict plant nutrient concentrations from remotely sensed temperature of sigma-t and to emphasize the latitudinally and longitudinally changing phytoplankton growth environment in present and past oceans is demonstrated.

  2. Combined thin layer chromatography and gas chromatography with mass spectrometric analysis of lipid classes and fatty acids in malnourished polar bears (Ursus maritimus) which swam to Iceland.

    Science.gov (United States)

    Eibler, Dorothee; Krüger, Sabine; Skírnisson, Karl; Vetter, Walter

    2017-03-01

    Between 2008 and 2011, four polar bears (Ursus maritimus) from the Greenland population swam and/or drifted on ice to Iceland where they arrived in very poor body condition. Body fat resources in these animals were only between 0% and 10% of the body weight (usually 25%). Here we studied the lipid composition in different tissues (adipose tissue if available, liver, kidney and muscle). Lipid classes were determined by thin layer chromatography (TLC) and on-column gas chromatography with mass spectrometry (GC/MS). The fatty acid pattern of total lipids and free fatty acids was analyzed by GC/MS in selected ion monitoring (SIM) mode. Additionally, cholesteryl esters and native fatty acid methyl esters, initially detected as zones in thin layer chromatograms, were enriched by solid phase extraction and quantified by GC/MS. The ratio of free fatty acids to native fatty acid methyl esters could be correlated with the remained body lipids in the polar bears and thus may also serve as a marker for other starving animals or even for humans. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Thin-Layer and Paper Chromatography.

    Science.gov (United States)

    Sherma, Joseph; Fried, Bernard

    1984-01-01

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

  4. Optical and Thermal Behaviors of Polyamide-Layered Silicate Nanocomposites Based on 4,4'-Azodibenzoic Acid by Solution Intercalation Technique

    Science.gov (United States)

    Faghihi, Khalil; Shabanian, Meisam

    2011-04-01

    Two new samples of polyamide-montmorillonite reinforced nanocomposites based on 4,4'-azodibenzoic acid were prepared by a convenient solution intercalation technique. Polyamide (PA) 4 as a source of polymer matrix was synthesized by the direct polycondensation reaction of 4,4'-azodibenzoic acid 2 with 4,4'-diamino diphenyl sulfone 3 in the presence of triphenyl phosphate (TPP), CaCl2, pyridine and N-methyl-2-pyrrolidone (NMP). Morphology and structure of the resulting PA-nanocomposite films 4a and 4b with 10 and 20% silicate particles were characterized by FTIR spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The effect of clay dispersion and the interaction between clay and polymeric chains on the properties of nanocomposite films were investigated by using Uv-vis spectroscopy, thermogravimetric analysis (TGA) and water uptake measurements.

  5. Synthesis and characterization of silica gel from siliceous sands of southern Tunisia

    Directory of Open Access Journals (Sweden)

    Ali Sdiri

    2014-09-01

    Full Text Available The present work aimed to achieve valorization of Albian sands for the preparation of sodium silicates that are commonly used as a precursor to prepare silica gel. A siliceous sand sample was mixed with sodium carbonate and heated at a high temperature (1060 °C to prepare sodium silicates. The sodium silicates were dissolved in distilled water to obtain high quality sodium silicate solution. Hydrochloric acid was then slowly added to the hydrated sodium silicates to obtain silica gel. The collected raw siliceous sands, as well as the prepared silica gels, were characterized by different techniques, such as X-ray fluorescence (XRF, X-ray diffraction (XRD, scanning electron microscopy (SEM and thermal analysis (DSC. XRF confirmed that the detrital sand deposits of southern Tunisia contain high amounts of silica, with content ranging from 88.8% to 97.5%. The internal porosity varied between 17% and 22%, and the specific surface area was less than 5 m2/g. After the treatment described above, it was observed that the porosity of the obtained silica gel reached 57% and the specific surface area exceeded 340 m2/g. Nitrogen adsorption isotherms showed that the prepared silica gels are microporous and mesoporous materials with high adsorption capacities. These results suggest that the obtained silica gels are promising materials for numerous environmental applications.

  6. I-Xe dating of silicate and troilite from IAB iron meteorites

    International Nuclear Information System (INIS)

    Niemeyer, S.

    1979-01-01

    Silicate and troilite (FeS) from IAB irons were analyzed by the I-Xe technique. Four IAB silicate samples gave well-defined I-Xe ages [in millions of years relative to Bjurbole: - 3.7 +- 0.3 for Woodbine, -0.7 +- 0.6 for Mundrabilla, + 1.4 +- 0.7 for Copiapo, and +2.6 +- 0.6 for Landes. The ( 129 Xe/ 132 Xe)sub(trapped) ratios are consistent with previous values for chondrites, with the exception of Landes which has an extraordinary trapped ratio of 3.5 +- 0.2. Both analyses of silicate from Pitts gave anomalous I-Xe patterns. Troilite samples were also analyzed: Pitts troilite gave a complex I-Xe pattern, which suggests an age of +17 Myr; Mundrabilla troilite defined a good I-Xe correlation, which after correction for neutron capture on 128 Te gave an age of -10.8 +- 0.7 Myr. Thus, low-melting troilite predates high-melting silicate in Mundrabilla. Abundances of Ga, Ge, and Ni in metal from these meteorites are correlated with I-Xe ages of the silicate; meteorites with older silicates have greater Ni contents. No model easily accounts for this result as well as other properties of IAB irons; nevertheless, these results, taken at face value, favour a nebular formation model. The great age of troilite from Mundrabilla suggests that this troilite formed in a different nebular region from the silicate and metal, and was later mechanically mixed with these other phases. The correlation between the trace elements in the metal and the I-Xe ages of the silicate provides one of the first known instances in which another well-defined meteoritic property correlates with I-Xe ages. In addition, almost all the 129 Xe in Mundrabilla silicate (etched in acid) was correlated with 128 Xe. These two results further support the validity of the I-Xe dating method. (author)

  7. Comparison of different amino acid derivatives and analysis of rat brain microdialysates by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Uutela, Päivi; Ketola, Raimo A; Piepponen, Petteri; Kostiainen, Risto

    2009-02-09

    The efficiencies of three derivatisation reagents that react with either the amine (9-fluorenylmethyl chloroformate (FMOC)) or the carboxylic acid group (butanol) of amino acid or with both types of functional groups (propyl chloroformate) were compared in the analysis of amino acids by liquid chromatography-electrospray-tandem mass spectrometry (LC-ESI-MS/MS). Separation of 20 amino acids derivatised with these three reagents was studied on reversed-phase chromatography. Linearity, repeatability and limits of detection of the LC-ESI-MS/MS method were determined by analysing FMOC-, butanol- and propyl chloroformate-derivatised lysine, beta-aminobutyric acid, threonine and glutamic acid. The limits of detection for the derivatised amino acids (7.5-75fmol) were as much as 2-60 times lower than those of the corresponding underivatised molecules. The best linearity was observed for amino acids derivatised with propyl chloroformate or butanol (r(2)=0.996-0.999, range=100-8500nmolL(-1)). Propyl chloroformate was the best suited of the reagents tested for the analysis of amino acids with LC-MS/MS and was used for the analysis of amino acids in rat brain microdialysis samples.

  8. [Determination of glycyrrhizinic acid in biotransformation system by reversed-phase high performance liquid chromatography].

    Science.gov (United States)

    Li, Hui; Lu, Dingqiang; Liu, Weimin

    2004-05-01

    A method for determining glycyrrhizinic acid in the biotransformation system by reversed-phase high performance liquid chromatography (RP-HPLC) was developed. The HPLC conditions were as follows: Hypersil C18 column (4.6 mm i.d. x 250 mm, 5 microm) with a mixture of methanol-water-acetic acid (70:30:1, v/v) as the mobile phase; flow rate at 1.0 mL/min; and UV detection at 254 nm. The linear range of glycyrrhizinic acid was 0.2-20 microg. The recoveries were 98%-103% with relative standard deviations between 0.16% and 1.58% (n = 3). The method is simple, rapid and accurate for determining glycyrrhizinic acid.

  9. Final report on the safety assessment of potassium silicate, sodium metasilicate, and sodium silicate.

    Science.gov (United States)

    Elmore, Amy R

    2005-01-01

    Potassium Silicate, Sodium Metasilicate, and Sodium Silicate combine metal cations with silica to form inorganic salts used as corrosion inhibitors in cosmetics. Sodium Metasilicate also functions as a chelating agent and Sodium Silicate as a buffering and pH adjuster. Sodium Metasilicate is currently used in 168 formulations at concentrations ranging from 13% to 18%. Sodium Silicate is currently used in 24 formulations at concentrations ranging from 0.3% to 55%. Potassium Silicate and Sodium Silicate have been reported as being used in industrial cleaners and detergents. Sodium Metasilicate is a GRAS (generally regarded as safe) food ingredient. Aqueous solutions of Sodium Silicate species are a part of a chemical continuum of silicates based on an equilibrium of alkali, water, and silica. pH determines the solubility of silica and, together with concentration, determines the degree of polymerization. Sodium Silicate administered orally is readily absorbed from the alimentary canal and excreted in the urine. The toxicity of these silicates has been related to the molar ratio of SiO2/Na2O and the concentration being used. The Sodium Metasilicate acute oral LD50 ranged from 847 mg/kg in male rats to 1349.3 mg/kg in female rats and from 770 mg/kg in female mice to 820 mg/kg in male mice. Gross lesions of variable severity were found in the oral cavity, pharynx, esophagus, stomach, larynx, lungs, and kidneys of dogs receiving 0.25 g/kg or more of a commercial detergent containing Sodium Metasilicate; similar lesions were also seen in pigs administered the same detergent and dose. Male rats orally administered 464 mg/kg of a 20% solution containing either 2.0 or 2.4 to 1.0 ratio of sodium oxide showed no signs of toxicity, whereas doses of 1000 and 2150 mg/kg produced gasping, dypsnea, and acute depression. Dogs fed 2.4 g/kg/day of Sodium Silicate for 4 weeks had gross renal lesions but no impairment of renal function. Dermal irritation of Potassium Silicate, Sodium

  10. Uranium-thorium silicates, with specific reference to the species in the Witwatersrand reefs

    International Nuclear Information System (INIS)

    Smits, G.

    1987-01-01

    (U,Th)-silicates form two complete series of anhydrous and hydrated species with general formulae (U,Th)SiO 4 and (U,Th)SiO 4 .nH 2 O respectively. The end-members of the anhydrous series are anhydrous coffinite and thorite, and those of the hydrated series, coffinite and thorogummite. Although the silicates are relatively rare in nature, coffinite is a common ore mineral in uranium deposits of the sandstone type. In the Witwatersrand reefs, (U,Th)-silicates are extremely rare in most reefs, except for the Elsburg Reefs on the West Rand Goldfield and the Dominion Reef. In these reefs detrital uraninite has been partly or entirely transformed to (U,Th)-silicates of coffinite composition, but thorite and thorogummite of detrital origin are also found in the Dominion Reef. In leaching tests on polished sections of rock samples containing (U,Th)-silicates, a dilute sulphuric acid solution, to which ferric iron had been added, was used as the lixiviant. It appeared that the dissolution of coffinite is less rapid than that of uraninite and uraniferous leucoxene. However, the reaction of silicates of high thorium content is much slower, and was not completed during the tests

  11. Solidification of low-level radioactive liquid waste using a cement-silicate process

    International Nuclear Information System (INIS)

    Grandlund, R.W.; Hayes, J.F.

    1979-01-01

    Extensive use has been made of silicate and Portland cement for the solidification of industrial waste and recently this method has been successfully used to solidify a variety of low level radioactive wastes. The types of wastes processed to date include fuel fabrication sludges, power reactor waste, decontamination solution, and university laboratory waste. The cement-silicate process produces a stable solid with a minimal increase in volume and the chemicals are relatively inexpensive and readily available. The method is adaptable to either batch or continuous processing and the equipment is simple. The solid has leaching characteristics similar to or better than plain Portland cement mixtures and the leaching can be further reduced by the use of ion-exchange additives. The cement-silicate process has been used to solidify waste containing high levels of boric acid, oils, and organic solvents. The experience of handling the various types of liquid waste with a cement-silicate system is described

  12. 21 CFR 573.260 - Calcium silicate.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Calcium silicate. 573.260 Section 573.260 Food and... Listing § 573.260 Calcium silicate. Calcium silicate, including synthetic calcium silicate, may be safely used as an anticaking agent in animal feed, provided that the amount of calcium silicate does not...

  13. CONDUCT AN INVESTIGATION OF CIGUATERA POISON

    Science.gov (United States)

    Research on ciguatera toxin resulted in a satisfactory method for extracting the toxin from fish muscle. Partial purification was also accomplished...by precipitation and silicic acid adsorption. The most precise fractionation of ciguatera toxin is accomplished on a silicic acid column developed...WILL LEAD TO HIGHLY PURIFIED SAMPLES OF CIGUATERA TOXIN. Paper chromatography was examined using fourteen different solvent systems, but none proved

  14. The use of ion chromatography for the determination of impurities in crude phosphoric acid

    International Nuclear Information System (INIS)

    Pires, M.A.F.; Atalla, L.T.; Abrao, A.

    1988-07-01

    The determination of fluoride, nitrate, sulphate and phosphate ions in crude phosphoric acid by means of ion chromatography is described. A previous separation of interferent cations was made by using a cationic resin or EDTA complexation. The last alternative allowed more reproductible results. The technique described is very quick and is being applied for the simultaneous determination of impurities in phosphoric acid and its own phosphospate concentration. The method is quick and has good reprodutibility. (author) [pt

  15. Determination of the Acid Dissociation Constant of a Phenolic Acid by High Performance Liquid Chromatography: An Experiment for the Upper Level Analytical Chemistry Laboratory

    Science.gov (United States)

    Raboh, Ghada

    2018-01-01

    A high performance liquid chromatography (HPLC) experiment for the upper level analytical chemistry laboratory is described. The students consider the effect of mobile-phase composition and pH on the retention times of ionizable compounds in order to determine the acid dissociation constant, K[subscript a], of a phenolic acid. Results are analyzed…

  16. Liquid chromatography-tandem mass spectrometry assay for the quantification of free and total sialic acid in human cerebrospinal fluid.

    NARCIS (Netherlands)

    Ham, M. van der; Koning, T.J. de; Lefeber, D.J.; Fleer, A.; Prinsen, B.H.; Sain-van der Velden, M.G. de

    2010-01-01

    BACKGROUND: Analysis of sialic acid (SA) metabolites in cerebrospinal fluid (CSF) is important for clinical diagnosis. In the present study, a high-performance liquid chromatography-tandem mass spectrometry (HPLC/MS/MS) method for free sialic acid (FSA) and total sialic acid (TSA) in human CSF was

  17. Determination of Free Fatty Acids and Triglycerides by Gas Chromatography Using Selective Esterification Reactions

    Energy Technology Data Exchange (ETDEWEB)

    Kail, Brian W; Link, Dirk D; Morreale, Bryan D

    2012-11-01

    A method for selectively determining both free fatty acids (FFA) and triacylglycerides (TAGs) in biological oils was investigated and optimized using gas chromatography after esterification of the target species to their corresponding fatty acid methyl esters (FAMEs). The method used acid catalyzed esterification in methanolic solutions under conditions of varying severity to achieve complete conversion of more reactive FFAs while preserving the concentration of TAGs. Complete conversion of both free acids and glycerides to corresponding FAMEs was found to require more rigorous reaction conditions involving heating to 120°C for up to 2 h. Method validation was provided using gas chromatography–flame ionization detection, gas chromatography–mass spectrometry, and liquid chromatography–mass spectrometry. The method improves on existing methods because it allows the total esterified lipid to be broken down by FAMEs contributed by FFA compared to FAMEs from both FFA and TAGs. Single and mixed-component solutions of pure fatty acids and triglycerides, as well as a sesame oil sample to simulate a complex biological oil, were used to optimize the methodologies. Key parameters that were investigated included: HCl-to-oil ratio, temperature and reaction time. Pure free fatty acids were found to esterify under reasonably mild conditions (10 min at 50°C with a 2.1:1 HCl to fatty acid ratio) with 97.6 ± 2.3% recovery as FAMEs, while triglycerides were largely unaffected under these reaction conditions. The optimized protocol demonstrated that it is possible to use esterification reactions to selectively determine the free acid content, total lipid content, and hence, glyceride content in biological oils. This protocol also allows gas chromatography analysis of FAMEs as a more ideal analyte than glyceride species in their native state.

  18. Selective Precipitation of Thorium lodate from a Tartaric Acid-Hydrogen Peroxide Medium Application to Rapid Spectrophotometric Determination of Thorium in Silicate Rocks and in Ores

    Science.gov (United States)

    Grimaldi, F.S.

    1957-01-01

    This paper presents a selective iodate separation of thorium from nitric acid medium containing d-tartaric acid and hydrogen peroxide. The catalytic decomposition of hydrogen peroxide is prevented by the use of 8quinolinol. A few micrograms of thorium are separated sufficiently clean from 30 mg. of such oxides as cerium, zirconium, titanium, niobium, tantalum, scandium, or iron with one iodate precipitation to allow an accurate determination of thorium with the thoronmesotartaric acid spectrophotometric method. The method is successful for the determination of 0.001% or more of thorium dioxide in silicate rocks and for 0.01% or more in black sand, monazite, thorite, thorianite, eschynite, euxenite, and zircon.

  19. Topotactic conversion of β-helix-layered silicate into AST-type zeolite through successive interlayer modifications.

    Science.gov (United States)

    Asakura, Yusuke; Takayama, Ryosuke; Shibue, Toshimichi; Kuroda, Kazuyuki

    2014-02-10

    AST-type zeolite with a plate morphology can be synthesized by topotactic conversion of a layered silicate (β-helix-layered silicate; HLS) by using N,N-dimethylpropionamide (DPA) to control the layer stacking of silicate layers and the subsequent interlayer condensation. Treatment of HLS twice with 1) hydrochloric acid/ethanol and 2) dimethylsulfoxide (DMSO) are needed to remove interlayer hydrated Na ions and tetramethylammonium (TMA) ions in intralayer cup-like cavities (intracavity TMA ions), both of which are introduced during the preparation of HLS. The utilization of an amide molecule is effective for the control of the stacking sequence of silicate layers. This method could be applicable to various layered silicates that cannot be topotactically converted into three-dimensional networks by simple interlayer condensation by judicious choice of amide molecules. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Simultaneous determination of furfural and its degradation products, furoic acid and maleic acid, in transformer oil by the reversed-phase vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography.

    Science.gov (United States)

    Wang, Yifan; Li, Haiyan; Yang, Zhen; Zhang, Weijie; Hua, Jia

    2017-12-01

    To explore why the use of furfural as a transformer oil-paper insulation aging characteristic is problematic in real world application, we developed a method for the simultaneous determination of furfural, furoic acid, and maleic acid in transformer oil by reversed-phase vortex-assisted liquid-liquid microextraction combined with high-performance liquid chromatography. The conditions for the proposed method were optimized, and the obtained extract can be directly analyzed by high-performance liquid chromatography. The detection limits (signal-to-noise ratio = 3) of the method ranged from 1.0 to 4.6 μg/L, the enrichment factors for furfural, furoic acid, maleic acid, and fumaric acid were 4.6, 25.1, 15.6, and 17.5, respectively, and the recovery rates for three analytes (fumaric acid was undetected) range from 82.1 to 106.2%. The contents of furfural, furoic acid, and maleic acid resulted from accelerated aging of transformer insulation oil-paper were measured using the present method for the first time, and the aging samples were analyzed by liquid chromatography with mass spectrometry for the identification of furoic acid and maleic acid in the aging transformer oil samples. Using the optimal method, the target products of samples at different aging time were tracked and measured. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Characterization of free and bound fatty acids in human gallstones by capillary gas liquid chromatography

    International Nuclear Information System (INIS)

    Channa, N.A.; Khand, F.D.; Noorani, M.A.; Bhanger, M.I.

    2002-01-01

    Forty-four human gallstone samples either of pure cholesterol or cholesterol and bilirubin were randomly selected and analyzed by capillary gas liquid chromatography for the relative percentage composition of free and total fatty acids. The results showed that bound fatty acids were present in higher amounts than the free fatty acids. Amongst the bound fatty acids the percentage occurrence for palmitic acid was highest followed by stearic, oleic, linoleic and myristic acids. Fatty acids myristic, palmitic and linoleic were present in higher amounts in cholesterol gallstones, whereas stearic acid in cholesterol and bilirubin gallstones. When compared, no significant difference (p < 0.05) in the levels of free and bound fatty acids were seen in gallstones of males and females. The results suggest that bound fatty acids have a role to play in the structure of gallstones. (author)

  2. Silicic Acid and Beer Consumption Reverses the Metal Imbalance and the Prooxidant Status Induced by Aluminum Nitrate in Mouse Brain.

    Science.gov (United States)

    González-Muñoz, María José; Garcimartán, Alba; Meseguer, Isabel; Mateos-Vega, Carmen José; Orellana, José María; Peña-Fernández, Antonio; Benedí, Juana; Sánchez-Muniz, Francisco J

    2017-01-01

    Emerging evidence suggests that by affecting mineral balance, aluminum (Al) may enhance some events associated with neurodegenerative diseases. To examine the effect of Al(NO3)3 exposure on brain Al, cooper (Cu), iron (Fe), magnesium (Mg), manganese (Mn), silicon (Si), and zinc (Zn) levels, and the metal-change implication in brain oxidant and inflammatory status. Four groups of six-week-old male NMRI mice were treated for three months: i) controls, administrated with deionized water; ii) Al, which received Al(NO3)3; iii) Al+silicic acid, which were given Al(NO3)3 plus silicic acid; and iv) Al+beer, which received Al(NO3)3 plus beer. Brain Al and TBARS levels and TNFα and GPx expressions increased, while Cu, Mn, and Zn levels, and catalase and CuZn-SOD expression decreased (at least, p beer specimens while Cu, Mn, and Zn levels and antioxidant expression increased versus the Al group. Brain Al levels correlated negatively with those of Cu, Fe, Mn, and Zn, and catalase, CuZn-SOD, and GPx enzyme expressions but positively with Si and TBARS levels and TNFα expression. Two components of the principal component analysis (PCA) explained 71.2% of total data variance (p beer administration.

  3. On the distribution of silicic acid as a frontal zone tracer in the Indian sector of the Southern Ocean

    Directory of Open Access Journals (Sweden)

    R. Prego

    1999-06-01

    Full Text Available The subantarctic frontal zone surveyed during the April-May 1991 SUZIL cruise in the Crozet-Kerguelen-Amsterdam area shows a strong horizontal (north to south gradient of dissolved silicate, increasing with depth, from 5 to 10 µmolSi kg-1 at 100 m, and 10 to 70 µmolSi kg-1 at 600 m. The northern limit of this frontal zone, which is formed by the confluence of the Subtropical and Subantarctic Fronts, is delimited at the surface by the 2 µmolSi kg-1 silicate isoline. Silicate-salinity diagrams also allow different water regimes to be positioned relative to the frontal zone. This sloping interface is between two water bodies, one to the north with more saline subtropical waters of less concentrated silicate than the southern one, corresponding to subantarctic waters which are less saline and richer in silicate. It is concluded that dissolved silicate can be used as a useful tracer of frontal zone water masses in the Indian sector of the Southern Ocean, providing a sound complement to other hydrographic data.

  4. First identification of dimethoxycinnamic acids in human plasma after coffee intake by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Nagy, Kornél; Redeuil, Karine; Williamson, Gary; Rezzi, Serge; Dionisi, Fabiola; Longet, Karin; Destaillats, Frédéric; Renouf, Mathieu

    2011-01-21

    There is a substantial amount of published literature on the bioavailability of various coffee components including the most abundant metabolites, caffeic and ferulic acids. Surprisingly, to date, the appearance of dimethoxycinnamic acid derivatives in humans has not been reported despite the fact that methylated form of catechol-type polyphenols could help maintain, modify or even improve their biological activities. This study reports an LC-MS method for the detection of dimethoxycinnamic acid in human plasma after treatment with an esterase. Liquid chromatography, including the combination of methanol and acetonitrile as organic eluent, was optimized to resolve all interferences and enable reliable detection and identification of 3,4-dimethoxycinnamic and 3,4-dimethoxy-dihydrocinnamic acids. In addition to the good mass accuracy achieved (better than 5 ppm), tandem mass spectrometric and co-chromatography experiments further confirmed the identity of the compounds. The optimized method was applied to analyze samples obtained immediately, 1 and 10 h after coffee ingestion. The results show that in particular 3,4-dimethoxycinnamic acid appears in high abundance (∼380 nM at 60 min) in plasma upon coffee intake, indicating that it is important to consider these derivatives in future bioavailability and bioefficacy studies. Copyright © 2010 Elsevier B.V. All rights reserved.

  5. Chromatographical analysis of phenolic acids in some species of Polygonum L. genus. Part 1 Qualitative analysis by two-dimensional thin layer chromatography (TLC

    Directory of Open Access Journals (Sweden)

    Helena D. Smolarz

    2014-01-01

    Full Text Available The Two-Dimensional Thin Layer Chromatography method has been used for the separation and identification of phenolic acids from six taxons of Pohygonum L. genus. The following acids were found: caffeic, p-coumaric, ferulic, p-hydroxybenzoic, m-hydroxybenzoic, vanillic, syringic, p-hydroxyphenylacetic, o-hydroxyphenylacetic, synapic, melillotic, salicylic, gentisic, elagic, gallic, chlorogenic, protocatechuic and homoprotocatechuic. Gallic, ferulic, vanillic, p-coumaric and p-hydroxybenzoic acids were isolated from herb Polygonum convolvulus L. using column chromatography.

  6. Formation mechanisms of colloidal silica via sodium silicate

    International Nuclear Information System (INIS)

    Tsai, M.-S.; Huang, P.Y.; Yang, C.-H.

    2006-01-01

    Colloidal silica is formed by titrating active silicic acid into a heated KOH with seed solution. The colloidal silica formation mechanisms are investigated by sampling the heated solution during titration. In the initial stage, the added seeds were dissolved. This might due to the dilution of seed concentration, the addition of potassium hydroxide (KOH) and the heating at 100 deg. C. Homogenous nucleation and surface growth occur simultaneously in the second stage of colloidal silica formation. Homogenous nucleation is more important when the seed concentration is relatively low. On the other hand, surface growth plays an important role when the seed concentration is increased. In the middle seed concentration, the seed particles grow up and some new small particles are born by the homogenous nucleation process to form a bimodal size distribution product. As the titrating volume of active silicic acid exceeds a specific value in the last stage the particle size increases rapidly and the particle number decreases, which may be caused by the aggregation of particles. The intervals between each stage were varied with the seed concentration. Increasing the seed concentration led to the formation of uniform particle size colloidal silica

  7. Determination of neurotransmitters and their metabolites using one- and two-dimensional liquid chromatography with acidic potassium permanganate chemiluminescence detection.

    Science.gov (United States)

    Holland, Brendan J; Conlan, Xavier A; Stevenson, Paul G; Tye, Susannah; Reker, Ashlie; Barnett, Neil W; Adcock, Jacqui L; Francis, Paul S

    2014-09-01

    High-performance liquid chromatography with chemiluminescence detection based on the reaction with acidic potassium permanganate and formaldehyde was explored for the determination of neurotransmitters and their metabolites. The neurotransmitters norepinephrine and dopamine were quantified in the left and right hemispheres of rat hippocampus, nucleus accumbens and prefrontal cortex, and the metabolites vanillylmandelic acid, 3,4-dihydrophenylacetic acid, 5-hydroxyindole-3-acetic acid and homovanillic acid were identified in human urine. Under optimised chemiluminescence reagent conditions, the limits of detection for these analytes ranged from 2.5 × 10(-8) to 2.5 × 10(-7) M. For the determination of neurotransmitter metabolites in urine, a two-dimensional high-performance liquid chromatography (2D-HPLC) separation operated in heart-cutting mode was developed to overcome the peak capacity limitations of the one-dimensional separation. This approach provided the greater separation power of 2D-HPLC with analysis times comparable to conventional one-dimensional separations.

  8. Separation of Transfer Ribonucleic Acids by Reverse Phase Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Kelmers, A. D.; Novelli, G. David; Stulberg, M. P.

    1965-10-01

    Numerous experimental techniques for the separation of transfer ribonucleic acids have been successful in preparing partially purified fractions of several specific t-RNAs. Many of the existing methods have depended upon the differential solubility of specific t-RNAs in complex two-phase systems (1-6) and the separation was achieved by means of counter-current extraction techniques. Column chromatography experiments using cellulose exchangers, (7,8) methylated albumin (9,10) or with solvent phases supported on inert material (11-13) have also shown partial separation of specific t-RNAs. Paper chromatographic procedures have produced partial resolutions of t-RNA.14 Methods involving chemical treatment of specific t-RNAs have been reported (15-19).

  9. Porous Silicates Modified with Zirconium Oxide and Sulfate Ions for Alcohol Dehydration Reactions

    Directory of Open Access Journals (Sweden)

    Heriberto Esteban Benito

    2015-01-01

    Full Text Available Porous silicates were synthesized by a nonhydrothermal method, using sodium silicate as a source of silica and cetyltrimethylammonium bromide as a template agent. Catalysts were characterized using thermogravimetric analysis, N2 physisorption, X-ray diffraction, FTIR spectroscopy, pyridine adsorption, potentiometric titration with n-butylamine, scanning electronic microscopy, and transmission electronic microscopy. The surface area of the materials synthesized was greater than 800 m2/g. The introduction of zirconium atoms within the porous silicates increased their acid strength from −42 to 115 mV, while the addition of sulfate ions raised this value to 470 mV. The catalytic activity for the dehydration of alcohols yields conversions of up to 70% for ethanol and 30% for methanol.

  10. The removal of uranium from acidic media using ion exchange and/or extraction chromatography

    International Nuclear Information System (INIS)

    FitzPatrick, J.R.; Schake, B.S.; Murphy, J.; Holmes, K.; West, M.H.

    1996-06-01

    The separation and purification of uranium from either nitric acid or hydrochloric acid media can be accomplished by using either solvent extraction or ion-exchange. Over the past two years at Los Alamos, emerging programs are focused on recapturing the expertise required to do limited, small-quantity processing of enriched uranium. During this period of time, we have been investigating ion-addition, waste stream polishing is associated with this effort in order to achieve more complete removal of uranium prior to recycle of the acid. Extraction chromatography has been demonstrated to further polish the uranium from both nitric and hydrochloric acid media thus allowing for a more complete recovery of the actinide material and creation of less waste during the processing steps

  11. 21 CFR 172.410 - Calcium silicate.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Calcium silicate. 172.410 Section 172.410 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) FOOD FOR HUMAN... Agents § 172.410 Calcium silicate. Calcium silicate, including synthetic calcium silicate, may be safely...

  12. Peak broadening in paper chromatography and related techniques VI. The efficiency of various kinds of chromatography paper and thin-layer cellulose powder for the separation of amino acids

    NARCIS (Netherlands)

    Ligny, C.L. de; Kok, E.C.M.

    1968-01-01

    The efficiency of several chromatography papers and thin-layer cellulose powders for the separation of amino acids is investigated, using the minimum elution time for a given resolution as the criterion.

  13. Enzymatic exchange of mycolic acid in mycobacterium smegmatis involving free trehalose and trehalose 6-mono-mycolate

    International Nuclear Information System (INIS)

    Sathyamoorthy, N.; Qureshi, N.; Takayama, K.

    1986-01-01

    When a dialyzed, cell-free extract of Mycobacterium smegmatis was incubated with [ 14 C]trehalose and unlabeled trehalose 6-monomycolate (TM), radiolabeled TM was formed. This appears to be an enzymatic mycolic acid exchange reaction. The TM was purified by DEAE cellulose and silicic acid column chromatography, followed by reverse-phase HPLC using a C 18 -bonded silica column with a linear gradient of 0-60% hexane-isopropanol (2:1, v/v) in isopropanol-water (9:1, v/v). The donor lipid, the 14 C-labeled product, and authentic TM all comigrated on HPLC. Three peak fractions were obtained from HPLC and analyzed by laser desorption mass spectrometry (LDMS) and the structural series of mycolic acids were identified. The major TM components gave molecular ions (M+K) + at m/z 1486, 1500, and 1528. This corresponded to the presence of dienyl mycolic acids with M/sub r/ of 1106, 1120, and 1148, respectively. Using organically synthesized TM, the authors confirmed that the donor lipid as well as the labeled product of this reaction are indeed TM. This enzyme has now been partially purified by ammonium sulfate precipitation and QAE-Sephadex A-50 column chromatography. This newly discovered mycolic acid exchange reaction might be an integral part of the last step in the biosynthesis of mycolic acid as well as the mycolic acid utilization pathway in Mycobacteria

  14. Acid monomer analysis in waterborne polymer systems by targeted labeling of carboxylic acid functionality, followed by pyrolysis - gas chromatography.

    Science.gov (United States)

    Brooijmans, T; Okhuijsen, R; Oerlemans, I; Schoenmakers, P J; Peters, R

    2018-05-14

    Pyrolysis - gas chromatography - (PyGC) is a common method to analyse the composition of natural and synthetic resins. The analysis of acid functionality in, for example, waterborne polyacrylates and polyurethanes polymers has proven to be difficult due to solubility issues, inter- and intramolecular interaction effects, lack of detectability in chromatographic analysis, and lack of thermal stability. Conventional analytical techniques, such as PyGC, cannot be used for the direct detection and identification of acidic monomers, due to thermal rearrangements that take place during pyrolysis. To circumvent this, the carboxylic acid groups are protected prior to thermal treatment by reaction with 2-bromoacetophenone. Reaction conditions are investigated and optimised wrt. conversion measurements. The aproach is applied to waterborne polyacryalates and the results are discussed. This approach enables identification and (semi)quantitative analysis of different acid functionalities in waterborne polymers by PyGC. Copyright © 2018 Elsevier B.V. All rights reserved.

  15. Environmental silicate nano-biocomposites

    CERN Document Server

    Pollet, Eric

    2012-01-01

    Environmental Silicate Nano-Biocomposites focuses on nano-biocomposites, which are obtained by the association of silicates such as bioclays with biopolymers. By highlighting recent developments and findings, green and biodegradable nano-composites from both renewable and biodegradable polymers are explored. This includes coverage of potential markets such as packaging, agricultures, leisure and the fast food industry. The knowledge and experience of more than twenty international experts in diverse fields, from chemical and biochemical engineering to applications, is brought together in four different sections covering: Biodegradable polymers and Silicates, Clay/Polyesters Nano-biocomposites, Clay/Agropolymers Nano-biocomposites, and Applications and biodegradation of Nano-biocomposites. By exploring the relationships between the biopolymer structures, the processes, and the final properties Environmental Silicate Nano-Biocomposites explains how to design nano-materials to develop new, valuable, environmenta...

  16. Quantification of Fatty Acid Oxidation Products Using On-line High Performance Liquid Chromatography Tandem Mass Spectrometry

    Science.gov (United States)

    Levison, Bruce S.; Zhang, Renliang; Wang, Zeneng; Fu, Xiaoming; DiDonato, Joseph A.; Hazen, Stanley L.

    2013-01-01

    Oxidized fatty acids formed via lipid peroxidation are implicated in pathological processes such as inflammation and atherosclerosis. A number of methods may be used to detect specific oxidized fatty acids containing a single or multiple combinations of epoxide, hydroxyl, ketone and hydroperoxide moieties on varying carbon chain lengths from C8 up to C30. Some of these methods are nonspecific and their use in biological systems is fraught with difficulty. Measures of specific-oxidized fatty acid derivatives help in identifying oxidation pathways in pathological processes. We used liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC-MS/MS) as efficient, selective and sensitive methods for identifying and analyzing multiple specific fatty acid peroxidation products in human plasma and other biological matrices. We then distilled the essential components of a number of these analyses to provide an efficient protocol by which fatty acid oxidation products and their parent compounds can be determined. In this protocol, addition of synthetic internal standard to the sample, followed by base hydrolysis at elevated temperature, and liquid-liquid phase sample extraction with lighter than water solvents facilitates isolation of the oxidized fatty acid species. These species can be identified and accurately quantified using stable isotope dilution and multiple reaction monitoring. Use of a coupled multiplexed gradient HPLC system on the front end enables high-throughput chromatography and more efficient use of mass spectrometer time. PMID:23499838

  17. [Determination of aspirin and free salicylic acid in lysinipirine injection by high performance liquid chromatography].

    Science.gov (United States)

    Dong, Yu; Zhao, Yuan-zheng; Zhang, Yi-na

    2002-05-01

    The contents of aspirin and free salicylic acid in lysinipirine injection were determined by high performance liquid chromatography (HPLC). A Hypersil BDS C18 column was used with the mobile phase of methanol-water-acetic acid (35:65:3, volume ratio) and the detection wavelength of 280 nm. The average recoveries of aspirin and salicylic acid added were 99.27% (RSD = 0.8%) and 99.61%(RSD = 1.3%), respectively. The calibration curves had good linearity in the range of 0.028 g/L -0.141 mg/L and 0.77 mg/L -3.85 mg/L, and the correlation coefficients were 0.9999 and 0.9998 for aspirin and salicylic acid respectively.

  18. Comprehensive two-dimensional liquid chromatography: Ion chromatography × reversed-phase liquid chromatography for separation of low-molar-mass organic acids

    NARCIS (Netherlands)

    Brudin, S.S.; Shellie, R.A.; Haddad, P.R.; Schoenmakers, P.J.

    2010-01-01

    In the work presented here a novel approach to comprehensive two-dimensional liquid chromatography is evaluated. Ion chromatography is chosen for the first-dimension separation and reversed-phase liquid chromatography is chosen for the second-dimension separation mode. The coupling of these modes is

  19. Quantification of sulphur amino acids by ultra-high performance liquid chromatography in aquatic invertebrates.

    Science.gov (United States)

    Thera, Jennifer C; Kidd, Karen A; Dodge-Lynch, M Elaine; Bertolo, Robert F

    2017-12-15

    We examined the performance of an ultra-high performance liquid chromatography method to quantify protein-bound sulphur amino acids in zooplankton. Both cysteic acid and methionine sulfone were linear from 5 to 250 pmol (r 2  = 0.99), with a method detection limit of 13 pmol and 9 pmol, respectively. Although there was no matrix effect on linearity, adjacent peaks and co-eluting noise from the invertebrate proteins increased the detection limits when compared to common standards. Overall, performance characteristics were reproducible and accurate, and provide a means for quantifying sulphur amino acids in aquatic invertebrates, an understudied group. Copyright © 2017 Elsevier Inc. All rights reserved.

  20. SILICATE COMPOSITION OF THE INTERSTELLAR MEDIUM

    International Nuclear Information System (INIS)

    Fogerty, S.; Forrest, W.; Watson, D. M.; Koch, I.; Sargent, B. A.

    2016-01-01

    The composition of silicate dust in the diffuse interstellar medium and in protoplanetary disks around young stars informs our understanding of the processing and evolution of the dust grains leading up to planet formation. An analysis of the well-known 9.7 μ m feature indicates that small amorphous silicate grains represent a significant fraction of interstellar dust and are also major components of protoplanetary disks. However, this feature is typically modeled assuming amorphous silicate dust of olivine and pyroxene stoichiometries. Here, we analyze interstellar dust with models of silicate dust that include non-stoichiometric amorphous silicate grains. Modeling the optical depth along lines of sight toward the extinguished objects Cyg OB2 No. 12 and ζ Ophiuchi, we find evidence for interstellar amorphous silicate dust with stoichiometry intermediate between olivine and pyroxene, which we simply refer to as “polivene.” Finally, we compare these results to models of silicate emission from the Trapezium and protoplanetary disks in Taurus.

  1. SILICATE COMPOSITION OF THE INTERSTELLAR MEDIUM

    Energy Technology Data Exchange (ETDEWEB)

    Fogerty, S.; Forrest, W.; Watson, D. M.; Koch, I. [Department of Physics and Astronomy, University of Rochester, Rochester, NY 14627 (United States); Sargent, B. A., E-mail: sfogerty@pas.rochester.edu [Center for Imaging Science and Laboratory for Multiwavelength Astrophysics, Rochester Institute of Technology, 54 Lomb Memorial Drive, Rochester, NY 14623 (United States)

    2016-10-20

    The composition of silicate dust in the diffuse interstellar medium and in protoplanetary disks around young stars informs our understanding of the processing and evolution of the dust grains leading up to planet formation. An analysis of the well-known 9.7 μ m feature indicates that small amorphous silicate grains represent a significant fraction of interstellar dust and are also major components of protoplanetary disks. However, this feature is typically modeled assuming amorphous silicate dust of olivine and pyroxene stoichiometries. Here, we analyze interstellar dust with models of silicate dust that include non-stoichiometric amorphous silicate grains. Modeling the optical depth along lines of sight toward the extinguished objects Cyg OB2 No. 12 and ζ Ophiuchi, we find evidence for interstellar amorphous silicate dust with stoichiometry intermediate between olivine and pyroxene, which we simply refer to as “polivene.” Finally, we compare these results to models of silicate emission from the Trapezium and protoplanetary disks in Taurus.

  2. Simultaneous determination of oxalic, citric, nitrilotriacetic and ethylenediamenetetraacetic acids by gas liquid chromatography of their methyl esters

    International Nuclear Information System (INIS)

    Eskell, C.J.; Pick, M.E.

    1980-04-01

    A procedure for simultaneous determination of ethylenediaminetetraacetic acid (EDTA), nitrilotriacetic acid (NTA), citric acid and oxalic acid by gas liquid chromatography is described. The involatile acids are first concerted to their volatile methyl ester derivatives by reaction with boron trifluoride in methanol. Transition metal ions (Fe 3+ , Cr 3+ and Ni 2+ ) which will be present in decontamination liquors from nuclear reactors, and form strong chelates with the acids, have been shown to cause no interference to the esterification reaction. The esters were separated by temperature programming on a 3.5 metre capillary column packed with 3% OV1 on Diatomite CQ and were detected by flame ionisation. (author)

  3. Determination of anions in pure and commercial phosphoric acid by ion chromatography and manual of 792 basic IC

    International Nuclear Information System (INIS)

    Al-Kabani, F.; Abdulbaki, M. K.

    2007-01-01

    A method for determination of anions in pure and concentrated phosphoric and samples (85%) and commercial phosphoric acid ion chromatography was developed, in order to control the specification of phosphoric acid produced in the pilot plant for phosphoric acid purification. The accuracy of the method was studied and the standard deviation was found to be between 0.09 and 0.10. Operation instructions of 792 Basic IC was described. (author)

  4. Simple, rapid, and sensitive liquid chromatography-fluorescence method for the quantification of tranexamic acid in blood

    NARCIS (Netherlands)

    Huertas-Pérez, José Fernando; Heger, Michal; Dekker, Henk; Krabbe, Hans; Lankelma, Jan; Ariese, Freek

    2007-01-01

    Tranexamic acid (TA) is a synthetic antifibrinolytic agent that is being considered as a candidate adjuvant drug for site-specific pharmaco-laser therapy of port wine stains. For drug utility studies, a high-performance liquid chromatography (HPLC)-fluorescence method was developed for the

  5. Silicate complexation of NpO2+ ion in perchlorate media

    International Nuclear Information System (INIS)

    Pathak, P.N.; Choppin, G.R.

    2007-01-01

    Complexation behavior of NpO 2 + with ortho-silicic acid (o-SA) has been studied using solvent extraction at ionic strengths varying from 0.10 to 1.00M (NaClO 4 ) at pcH 3.68±0.08 and 25 deg C with bis-(2-ethylhexyl) phosphoric acid (HDEHP) as the extractant. The stability constant value (log β 1 ) for the 1:1 complex, NpO 2 (OSi(OH) 3 ), was found to decrease with increase in ionic strength of the aqueous phase [6.83±0.01 at I = 0.10M to 6.51±0.02 at I = 1.00M]. These values have been fitted in the SIT model expression and compared with similar values of complexation of the metal ions Am 3+ , Eu 3+ , UO 2 2+ , PuO 2 2+ , Np 4+ , Ni 2+ and Co 2+ . The speciation of NpO 2 + -o-silicate/carbonate system has been calculated as a function of pcH under ground water conditions. (author)

  6. Modifying Silicates for Better Dispersion in Nanocomposites

    Science.gov (United States)

    Campbell, Sandi

    2005-01-01

    An improved chemical modification has been developed to enhance the dispersion of layered silicate particles in the formulation of a polymer/silicate nanocomposite material. The modification involves, among other things, the co-exchange of an alkyl ammonium ion and a monoprotonated diamine with interlayer cations of the silicate. The net overall effects of the improved chemical modification are to improve processability of the nanocomposite and maximize the benefits of dispersing the silicate particles into the polymer. Some background discussion is necessary to give meaning to a description of this development. Polymer/silicate nanocomposites are also denoted polymer/clay composites because the silicate particles in them are typically derived from clay particles. Particles of clay comprise layers of silicate platelets separated by gaps called "galleries." The platelet thickness is 1 nm. The length varies from 30 nm to 1 m, depending on the silicate. In order to fully realize the benefits of polymer/silicate nanocomposites, it is necessary to ensure that the platelets become dispersed in the polymer matrices. Proper dispersion can impart physical and chemical properties that make nanocomposites attractive for a variety of applications. In order to achieve nanometer-level dispersion of a layered silicate into a polymer matrix, it is typically necessary to modify the interlayer silicate surfaces by attaching organic functional groups. This modification can be achieved easily by ion exchange between the interlayer metal cations found naturally in the silicate and protonated organic cations - typically protonated amines. Long-chain alkyl ammonium ions are commonly chosen as the ion-exchange materials because they effectively lower the surface energies of the silicates and ease the incorporation of organic monomers or polymers into the silicate galleries. This completes the background discussion. In the present improved modification of the interlayer silicate surfaces

  7. Evaluation of Aroma in Oriental Tobaccos as Based On Valeric Acid Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Dagnon S

    2014-12-01

    Full Text Available Levels of valeric acids (isovaleric and 3-methylvaleric in leaves and smoke of different tobacco types were quantified by capillary gas chromatography (GC using flame ionization detector (FID. The aroma characteristics of the smoke were scored by sensory evaluation. It was found that leaves of Oriental and burley tobaccos contain higher amounts of both valeric acid derivatives than Virginia tobaccos containing isovaleric acid but no 3-methylvaleric acid. Strong correlation between the aroma and pleasantness scores of smoke and the content of valeric acids in the leaves of Oriental tobaccos was observed, while it was not the case for leaves of Virginia and burley tobaccos. In all tobacco types no correlation between smoking characteristics and the content of valeric acids in the smoke was established. Regression models involving leaf isovaleric acid were developed that can be used to evaluate aroma and pleasantness of smoke in Oriental tobaccos. The data obtained allow the following conclusions to be drawn: a 3-methylvaleric acid may be a chemical marker to distinguish Virginia tobaccos from Oriental and burley tobaccos; b isovaleric acid content in leaves of Oriental tobaccos may be used for objective aroma evaluation that can be exploited for breeding and market purposes.

  8. Origins of saccharide-dependent hydration at aluminate, silicate, and aluminosilicate surfaces.

    Science.gov (United States)

    Smith, Benjamin J; Rawal, Aditya; Funkhouser, Gary P; Roberts, Lawrence R; Gupta, Vijay; Israelachvili, Jacob N; Chmelka, Bradley F

    2011-05-31

    Sugar molecules adsorbed at hydrated inorganic oxide surfaces occur ubiquitously in nature and in technologically important materials and processes, including marine biomineralization, cement hydration, corrosion inhibition, bioadhesion, and bone resorption. Among these examples, surprisingly diverse hydration behaviors are observed for oxides in the presence of saccharides with closely related compositions and structures. Glucose, sucrose, and maltodextrin, for example, exhibit significant differences in their adsorption selectivities and alkaline reaction properties on hydrating aluminate, silicate, and aluminosilicate surfaces that are shown to be due to the molecular architectures of the saccharides. Solid-state (1)H, (13)C, (29)Si, and (27)Al nuclear magnetic resonance (NMR) spectroscopy measurements, including at very high magnetic fields (19 T), distinguish and quantify the different molecular species, their chemical transformations, and their site-specific adsorption on different aluminate and silicate moieties. Two-dimensional NMR results establish nonselective adsorption of glucose degradation products containing carboxylic acids on both hydrated silicates and aluminates. In contrast, sucrose adsorbs intact at hydrated silicate sites and selectively at anhydrous, but not hydrated, aluminate moieties. Quantitative surface force measurements establish that sucrose adsorbs strongly as multilayers on hydrated aluminosilicate surfaces. The molecular structures and physicochemical properties of the saccharides and their degradation species correlate well with their adsorption behaviors. The results explain the dramatically different effects that small amounts of different types of sugars have on the rates at which aluminate, silicate, and aluminosilicate species hydrate, with important implications for diverse materials and applications.

  9. Phosphorus availability in oxidic soils treated with lime and silicate applications

    Directory of Open Access Journals (Sweden)

    Aline da Silva Sandim

    2014-08-01

    Full Text Available Based on the assumption that silicate application can raise soil P availability for crops, the aim of this research was to compare the effect of silicate application on soil P desorption with that of liming, in evaluations based on two extractors and plant growth. The experiment was carried out in randomized blocks with four replications, in a 3 × 3 × 5 factorial design, in which three soil types, three P rates, and four soil acidity correctives were evaluated in 180 experimental plots. Trials were performed in a greenhouse using corn plants in 20-dm³ pots. Three P rates (0, 50 and 150 mg dm-3 were applied in the form of powder triple superphosphate and the soil was incubated for 90 days. After this period, soil samples were collected for routine chemical analysis and P content determination by the extraction methods resin, Mehlich-1 and remaining P. Based on the results, acidity correctives were applied at rates calculated for base saturation increased to 70 %, with subsequent incubation for 60 more days, when P content was determined again. The acidity correctives consisted of: dolomitic lime, steelmaking slag, ladle furnace slag, and wollastonite. Therefore, our results showed that slags raised the soil P content more than lime, suggesting a positive correlation between P and Si in soil. Silicon did not affect the extractor choice since both Mehlich-1 and resin had the same behavior regarding extracted P when silicon was applied to the soil. For all evaluated plant parameters, there was significant interaction between P rates and correctives; highest values were obtained with silicate.

  10. Simultaneous determination of ascorbic acid and caffeine in commercial soft drinks using reversed-phase ultraperformance liquid chromatography.

    Science.gov (United States)

    Turak, Fatma; Güzel, Remziye; Dinç, Erdal

    2017-04-01

    A new reversed-phase ultraperformance liquid chromatography method with a photodiode array detector was developed for the quantification of ascorbic acid (AA) and caffeine (CAF) in 11 different commercial drinks consisting of one energy drink and 10 ice tea drinks. Separation of the analyzed AA and CAF with an internal standard, caffeic acid, was performed on a Waters BEH C 18 column (100 mm × 2.1 mm, 1.7 μm i.d.), using a mobile phase consisting of acetonitrile and 0.2M H 3 PO 4 (11:89, v/v) with a flow rate of 0.25 mL/min and an injection volume of 1.0 μL. Calibration graphs for AA and CAF were computed from the peak area ratio of AA/internal standard and CAF/internal standard detected at 244.0 nm and 273.6 nm, respectively. The developed reversed-phase ultraperformance liquid chromatography method was validated by analyzing standard addition samples. The proposed reversed-phase ultraperformance liquid chromatography method gave us successful results for the quantitative analysis of commercial drinks containing AA and CAF substances. Copyright © 2016. Published by Elsevier B.V.

  11. Simultaneous determination of ascorbic acid and caffeine in commercial soft drinks using reversed-phase ultraperformance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Fatma Turak

    2017-04-01

    Full Text Available A new reversed-phase ultraperformance liquid chromatography method with a photodiode array detector was developed for the quantification of ascorbic acid (AA and caffeine (CAF in 11 different commercial drinks consisting of one energy drink and 10 ice tea drinks. Separation of the analyzed AA and CAF with an internal standard, caffeic acid, was performed on a Waters BEH C18 column (100 mm × 2.1 mm, 1.7 μm i.d., using a mobile phase consisting of acetonitrile and 0.2M H3PO4 (11:89, v/v with a flow rate of 0.25 mL/min and an injection volume of 1.0 μL. Calibration graphs for AA and CAF were computed from the peak area ratio of AA/internal standard and CAF/internal standard detected at 244.0 nm and 273.6 nm, respectively. The developed reversed-phase ultraperformance liquid chromatography method was validated by analyzing standard addition samples. The proposed reversed-phase ultraperformance liquid chromatography method gave us successful results for the quantitative analysis of commercial drinks containing AA and CAF substances.

  12. Decreased water flowing from a forest amended with calcium silicate

    Science.gov (United States)

    Mark B. Green; Amey S. Bailey; Scott W. Bailey; John J. Battles; John L. Campbell; Charles T. Driscoll; Timothy J. Fahey; Lucie C. Lepine; Gene E. Likens; Scott V. Ollinger; Paul G. Schaberg

    2013-01-01

    Acid deposition during the 20th century caused widespread depletion of available soil calcium (Ca) throughout much of the industrialized world. To better understand how forest ecosystems respond to changes in a component of acidification stress, an 11.8-ha watershed was amended with wollastonite, a calcium silicate mineral, to restore available soil Ca to preindustrial...

  13. Simultaneous Analysis of Ursolic Acid and Oleanolic Acid in Guava Leaves Using QuEChERS-Based Extraction Followed by High-Performance Liquid Chromatography

    OpenAIRE

    Xu, Chang; Liao, Yiyi; Fang, Chunyan; Tsunoda, Makoto; Zhang, Yingxia; Song, Yanting; Deng, Shiming

    2017-01-01

    In this paper, a novel method of QuEChERS-based extraction coupled with high-performance liquid chromatography has been developed for the simultaneous determination of ursolic acid (UA) and oleanolic acid (OA) in guava leaves. The QuEChERS-based extraction parameters, including the amount of added salt, vortex-assisted extraction time, and absorbent amount, and the chromatographic conditions were investigated for the analysis of UA and OA in guava leaves. Under the optimized conditions, the m...

  14. Retention prediction and hydrophobicity estimation of weak acidic compounds by reversed-phase liquid chromatography using acetic and perchloric acids as ion suppressors.

    Science.gov (United States)

    Han, Shu-ying; Ming, Xin; Qi, Zheng-chun; Sheng, Dong; Lian, Hong-zhen

    2010-11-01

    Simple acids are usually applied to suppress the ionization of weakly ionizable acidic analytes in reversed-phase liquid chromatography. The purpose of this study is to investigate the retention behavior of various weak acidic compounds (monoprotic, diprotic, triprotic, and tetraprotic acids) using acetic or perchloric acid as ion suppressor in a binary hydroorganic mobile phase. The apparent n-octanol-water partition coefficient (K(ow)") was proposed to calibrate the n-octanol-water partition coefficient (K(ow)) of weak acidic compound. LogK(ow)" was found to have a better linear correlation with logk(w), the logarithm of the retention factor obtained by extrapolating to neat aqueous fraction of the mobile phase, for all weakly ionizable acidic compounds. This straightforward relationship offers a potential medium for direct measurement of K(ow) data of weak acidic analytes and can be used to predict retention behavior of these compounds in the ion suppression reversed-phase liquid chromatographic mode.

  15. Silicate fertilization of tropical soils: silicon availability and recovery index of sugarcane

    Directory of Open Access Journals (Sweden)

    Mônica Sartori de Camargo

    2013-10-01

    Full Text Available Sugarcane is considered a Si-accumulating plant, but in Brazil, where several soil types are used for cultivation, there is little information about silicon (Si fertilization. The objectives of this study were to evaluate the silicon availability, uptake and recovery index of Si from the applied silicate on tropical soils with and without silicate fertilization, in three crops. The experiments in pots (100 L were performed with specific Si rates (0, 185, 370 and 555 kg ha-1 Si, three soils (Quartzipsamment-Q, 6 % clay; Rhodic Hapludox-RH, 22 % clay; and Rhodic Acrudox-RA, 68 % clay, with four replications. The silicon source was Ca-Mg silicate. The same Ca and Mg quantities were applied to all pots, with lime and/or MgCl2, when necessary. Sugarcane was harvested in the plant cane and first- and second-ratoon crops. The silicon rates increased soil Si availability and Si uptake by sugarcane and had a strong residual effect. The contents of soluble Si were reduced by harvesting and increased with silicate application in the following decreasing order: Q>RH>RA. The silicate rates promoted an increase in soluble Si-acetic acid at harvest for all crops and in all soils, except RA. The amounts of Si-CaCl2 were not influenced by silicate in the ratoon crops. The plant Si uptake increased according to the Si rates and was highest in RA at all harvests. The recovery index of applied Si (RI of sugarcane increased over time, and was highest in RA.

  16. Monitoring of monooctanoyl phosphatidylcholine synthesis by enzymatic acidolysis between soybean phosphatidylcholine and caprylic acid by thin-layer chromatography with a flame ionization detector

    DEFF Research Database (Denmark)

    Vikbjerg, Anders Falk; Mu, Huiling; Xu, Xuebing

    2005-01-01

    Thin-layer chromatography with flame ionization detector (TLC-FID) method was used for monitoring the production of structured phospholipids (ML-type: L-long chain fatty acids; M-medium chain fatty acids) by enzyme-catalyzed acidolysis between soybean phosphatidylcholine (PC) and caprylic acid....... It was found that the structured PC fractionated into 2-3 distinct bands on both plate thin layer chromatography (TLC) and Chromarod TLC. These 3 bands represented PC of LL-type, ML-type and MM-type, respectively. The TLC-FID method was applied in the present study to examine the influence of enzyme dosage...

  17. Synthesis and characterization of functional copolymer/organo-silicate nanoarchitectures through interlamellar complex-radical (coterpolymerization

    Directory of Open Access Journals (Sweden)

    2008-09-01

    Full Text Available The functional copolymers, having a combination of rigid/flexible linkages and an ability of complex-formation with interlayered surface of organo-silicate, and their nanocomposites have been synthesized by interlamellar complex-radical (coterpolymerization of intercalated monomer complexes of maleic anhydride (MA and itaconic acid (IA with dimethyl dodecylamine surface modified montmorillonite (organo-MMT (MA…DMDA-MMT and IA…DMDA-MMT n-butyl methacrylate (BMA and/or BMA/styrene monomer mixtures. The results of nanocomposite structure–composition– property relationship studies indicate that interlamellar complex-formation between anhydride/acid units and surface alkyl amine and rigid/flexible linkage balance in polymer chains are important factors providing the effective intercalation/ exfoliation of the polymer chains into the silicate galleries, the formation of nanostructural hybrids with higher thermal stability, dynamic mechanical behaviour and well dispersed morphology.

  18. Fast derivatization of fatty acids in different meat samples for gas chromatography analysis.

    Science.gov (United States)

    Figueiredo, Ingrid Lima; Claus, Thiago; Oliveira Santos Júnior, Oscar; Almeida, Vitor Cinque; Magon, Thiago; Visentainer, Jesuí Vergilio

    2016-07-22

    In order to analyze the composition of fatty acids employing gas chromatography as the separation method, a derivatization of lipids using esterification and transesterification reactions is needed. The methodologies currently available are time consuming and use large amounts of sample and reagents. Thus, this work proposes a new procedure to carry out the derivatization of fatty acids without the need for prior extraction of lipids. The use of small amounts of sample (100mg) allows the analysis to be performed in specific parts of animals, in most cases without having them slaughtered. Another benefit is the use of small amounts of reagents (only 2mL of NaOH/Methanol and H2SO4/Methanol). The use of an experimental design procedure (Design Expert software) allows the optimization of the alkaline and acid reaction times. The procedure was validated for five minutes in both steps. The method was validated for bovine fat, beef, chicken, pork, fish and shrimp meats. The results for the merit figures of accuracy (from 101.07% to 109.18%), precision (RSDintra-day (from 0.65 to 3.93%), RSDinter-day (from 1.57 to 5.22%)), linearity (R(2)=0.9864) and robustness confirmed that the new method is satisfactory within the linear range of 2-30% of lipids in the sample. Besides the benefits of minimizing the amount of samples and reagents, the procedure enables gas chromatography sample preparation in a very short time compared with traditional procedures. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Extraction chromatography of actinides

    International Nuclear Information System (INIS)

    Muller, W.

    1978-01-01

    Extraction chromatography of actinides in the oxidation state from 2 to 6 is reviewed. Data on using neutral (tbp), basic (substituted ammonium salts) and acidic [di-(2-ethylhexyl)-phosphoric acid (D2EHPA)] extracting agents ketones, esters, alcohols and β-diketones in this method are given. Using the example of actinide separation using D2EHPA, discussed are factors influencing the efficiency of their chromatography separation (nature and particle size of the carrier materials, extracting agents amount on the carrier, temperature and elution rate)

  20. Influence of Bath Composition at Acidic pH on Electrodeposition of Nickel-Layered Silicate Nanocomposites for Corrosion Protection

    Directory of Open Access Journals (Sweden)

    Jeerapan Tientong

    2013-01-01

    Full Text Available Nickel-layered silicates were electrochemically deposited from acidic bath solutions. Citrate was used as a ligand to stabilize nickel (II ions in the plating solution. The silicate, montmorillonite, was exfoliated by stirring in aqueous solution over 24 hours. The plating solutions were analyzed for zeta-potential, particle size, viscosity, and conductivity to investigate the effects of the composition at various pHs. The solution particles at pH 2.5 (−22.2 mV and pH 3.0 (−21.9 mV were more stable than at pH 1.6 (−10.1 mV as shown by zeta-potential analysis of the nickel-citrate-montmorillonite plating solution. Ecorr for the films ranged from −0.32 to −0.39 V with varying pH from 1.6 to 3.0. The films were immersed in 3.5% NaCl and the open circuit potential monitored for one month. The coatings deposited at pH 3.0 were stable 13 days longer in the salt solution than the other coatings. X-ray diffraction showed a change in the (111/(200 ratio for the coatings at the various pHs. The scanning electron microscopy and hardness results also support that the electrodeposition of nickel-montmorillonite at pH 3.0 (234 GPa had improved hardness and morphology compared to pH 2.5 (174 GPa and pH 1.6 (147 GPa.

  1. Improved separation of conjugated fatty acid methyl esters by silver ion-high-performance liquid chromatography.

    Science.gov (United States)

    Sehat, N; Rickert, R; Mossoba, M M; Kramer, J K; Yurawecz, M P; Roach, J A; Adlof, R O; Morehouse, K M; Fritsche, J; Eulitz, K D; Steinhart, H; Ku, Y

    1999-04-01

    Operating from one to six silver ion-high-performance liquid chromatography (Ag+-HPLC) columns in series progressively improved the resolution of the methyl esters of conjugated linoleic acid (CLA) isomeric mixtures from natural and commercial products. In natural products, the 8 trans, 10 cis-octadecadienoic (18:2) acid was resolved from the more abundant 7 trans, 9 cis-18:2, and the 10 trans, 12 cis-18:2 was separated from the major 9 cis, 11 trans-18:2 peak. In addition, both 11 trans, 13 cis-18:2 and 11 cis, 13 trans-18:2 isomers were found in natural products and were separated; the presence of the latter, 11 cis, 13 trans-18:2, was established in commercial CLA preparations. Three Ag+-HPLC columns in series appeared to be the best compromise to obtain satisfactory resolution of most CLA isomers found in natural products. A single Ag+-HPLC column in series with one of several normal-phase columns did not improve the resolution of CLA isomers as compared to that of the former alone. The 20:2 conjugated fatty acid isomers 11 cis, 13 trans-20:2 and 12 trans, 14 cis-20:2, which were synthesized by alkali isomerization from 11 cis, 14 cis-20:2, eluted in the same region of the Ag+-HPLC chromatogram just before the corresponding geometric CLA isomers. Therefore, CLA isomers will require isolation based on chain length prior to Ag+-HPLC separation. The positions of conjugated double bonds in 20:2 and 18:2 isomers were established by gas chromatography-electron ionization mass spectrometry as their 4,4-dimethyloxazoline derivatives. The double-bond geometry was determined by gas chromatography-direct deposition-Fourier transform infrared spectroscopy and by the Ag+-HPLC relative elution order.

  2. Lipids and Fatty Acids in Algae: Extraction, Fractionation into Lipid Classes, and Analysis by Gas Chromatography Coupled with Flame Ionization Detector (GC-FID).

    Science.gov (United States)

    Guihéneuf, Freddy; Schmid, Matthias; Stengel, Dagmar B

    2015-01-01

    Despite the number of biochemical studies exploring algal lipids and fatty acid biosynthesis pathways and profiles, analytical methods used by phycologists for this purpose are often diverse and incompletely described. Potential confusion and potential variability of the results between studies can therefore occur due to change of protocols for lipid extraction and fractionation, as well as fatty acid methyl esters (FAME) preparation before gas chromatography (GC) analyses. Here, we describe a step-by-step procedure for the profiling of neutral and polar lipids using techniques such as solid-liquid extraction (SLE), thin-layer chromatography (TLC), and gas chromatography coupled with flame ionization detector (GC-FID). As an example, in this protocol chapter, analyses of neutral and polar lipids from the marine microalga Pavlova lutheri (an EPA/DHA-rich haptophyte) will be outlined to describe the distribution of fatty acid residues within its major lipid classes. This method has been proven to be a reliable technique to assess changes in lipid and fatty acid profiles in several other microalgal species and seaweeds.

  3. Analysis of defense signals in Arabidopsis thaliana leaves by ultra-performance liquid chromatography/tandem mass spectrometry: jasmonates, salicylic acid, abscisic acid.

    Science.gov (United States)

    Stingl, Nadja; Krischke, Markus; Fekete, Agnes; Mueller, Martin J

    2013-01-01

    Defense signaling compounds and phytohormones play an essential role in the regulation of plant responses to various environmental abiotic and biotic stresses. Among the most severe stresses are herbivory, pathogen infection, and drought stress. The major hormones involved in the regulation of these responses are 12-oxo-phytodienoic acid (OPDA), the pro-hormone jasmonic acid (JA) and its biologically active isoleucine conjugate (JA-Ile), salicylic acid (SA), and abscisic acid (ABA). These signaling compounds are present and biologically active at very low concentrations from ng/g to μg/g dry weight. Accurate and sensitive quantification of these signals has made a significant contribution to the understanding of plant stress responses. Ultra-performance liquid chromatography (UPLC) coupled with a tandem quadrupole mass spectrometer (MS/MS) has become an essential technique for the analysis and quantification of these compounds.

  4. 21 CFR 582.2227 - Calcium silicate.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Calcium silicate. 582.2227 Section 582.2227 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) ANIMAL... Calcium silicate. (a) Product. Calcium silicate. (b) Tolerance. 2 percent and 5 percent. (c) Limitations...

  5. Study and make sulfur dioxide treatment equipment for degradation process of fine silicate zircon ore by sulfuric acid

    International Nuclear Information System (INIS)

    Cao Dinh Thanh; Le Xuan Thu; Tran Van Hoa; Pham Kim Thoa

    2003-01-01

    The against absorbent method was researched by research group to solve the above issue. This method was carried out by adsorbent lime-milk agent on the buffer of porous material with diameter D=9 cm and height H=1.2 m. The main parameters were gained: absorbent effect reached 98% with lime-milk concentration of 14% in water, against air flow speed of 0.7 m/s and lime-milk output of 0.45 liter/minute. Base on the above main researched parameter, the SO 2 treatment equipment system by sulfuric acid was worked out with the scale of 0.5 ton/batch/day; absorbent tower diameter D=0.47 m, buffer height H=3.5 m and expenditure of 33.2 kg CaO/ton of zircon silicate. (author)

  6. 21 CFR 182.2227 - Calcium silicate.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Calcium silicate. 182.2227 Section 182.2227 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) FOOD FOR... Calcium silicate. (a) Product. Calcium silicate. (b) Tolerance. 2 percent and 5 percent. (c) Limitations...

  7. Determination of feedstuff amino acids composition by ion-exchange chromatography

    Directory of Open Access Journals (Sweden)

    A. A. Volnin

    2018-01-01

    Full Text Available Determination of animal feeds amino acids composition is the very important part of agricultural sciences and livestock management. This is necessary for normalization and balanced of farm animal’s diets parameters. Advances in husbandry techniques are making in response to the needs for rearing high genetic merit livestock. The nutrition of livestock has a critical role in these developments and is an element which needs to be continually updated as new scientific information becomes available. This article is devoted to the use of ion-exchange chromatography with post-colum derivatization by ninhydrin in the study of the amino acid composition and evaluation of the biological value of livestock feedstuff components. The amino acid composition (except tryptophan of the livestock feed-stuff component is presented for threonine – 3.26 g/100g of protein, leucine – 6.43, isoleucine – 3.24, valine – 4.77, methionine – 2.18, lysine – 2.90, phenylalanine – 3.16, histidine – 2.03, tyrosine – 2.33, sum of asparagine and aspartate – 6.76, serine – 3.97, sum of glutamine and glutamic acid – 12.04, glycine – 6.00, alanine – 6.71, arginine – 6.93, proline – 3.08, sum of cystine and cysteine – 1.38. Biological value of feedstuff component compared with the "ideal" protein (FAO WHO is estimated, limiting amino acids were found. The amino acid score was calculated: for threonine – 81.5%, leucine – 91.9%, isoleucine – 81%, valine – 95.4%, lysine – 52.7%, phenylalanine and tyrosine sum – 91.5%, methionine and cysteine sum – 101.7%. Feedstuff component had a low level of essential amino acids in compare with "ideal" protein (FAO WHO. Feedstuff component can be used for livestock nutrition as a component of essential amino-acid balanced diet.

  8. Elucidation and identification of amino acid containing membrane lipids using liquid chromatography/high-resolution mass spectrometry

    NARCIS (Netherlands)

    Moore, E.K.; Hopmans, E.C.; Rijpstra, W.I.C.; Villanueva, L.; Sinninghe Damsté, J.S.

    2016-01-01

    RATIONALE: Intact polar lipids (IPLs) are the building blocks of cell membranes, and amino acid containing IPLs havebeen observed to be involved in response to changing environmental conditions in various species of bacteri a. High-performance liquid chromatography/mass spectrometry (HPLC/MS) has

  9. Fatty acid profiling of raw human plasma and whole blood using direct thermal desorption combined with gas chromatography-mass spectrometry.

    NARCIS (Netherlands)

    Akoto, L.; Vreuls, J.J.; Irth, H.; Pel, R.; Stellaard, F.

    2008-01-01

    Gas chromatography (GC) has in recent times become an important tool for the fatty acid profiling of human blood and plasma. An at-line procedure used in the fatty acid profiling of whole/intact aquatic micro-organisms without any sample preparation was adapted for this work. A direct thermal

  10. Fatty acid profiling of raw human plasma and whole blood using direct thermal desorption combined with gas chromatography-mass spectrometry

    NARCIS (Netherlands)

    Akoto, Lawrence; Vreuls, Rene J. J.; Irth, Hubertus; Pel, Roel; Stellaard, Frans

    2008-01-01

    Gas chromatography (GC) has in recent times become an important tool for the fatty acid profiling of human blood and plasma. An at-line procedure used in the fatty acid profiling of whole/intact aquatic micro-organisms without any sample preparation was adapted for this work. A direct thermal

  11. delta 13C analyses of vegetable oil fatty acid components, determined by gas chromatography--combustion--isotope ratio mass spectrometry, after saponification or regiospecific hydrolysis.

    Science.gov (United States)

    Woodbury, S E; Evershed, R P; Rossell, J B

    1998-05-01

    The delta 13C values of the major fatty acids of several different commercially important vegetable oils were measured by gas chromatography--combustion--isotope ratio mass spectrometry. The delta 13C values obtained were found to fall into two distinct groups, representing the C3 and C4 plants classes from which the oils were derived. The delta 13C values of the oils were measured by continuous flow elemental isotope ratio mass spectrometry and were found to be similar to their fatty acids, with slight differences between individual fatty acids. Investigations were then made into the influence on the delta 13C values of fatty acids of the position occupied on the glycerol backbone. Pancreatic lipase was employed to selectively hydrolyse fatty acids from the 1- and 3-positions with the progress of the reaction being followed by high-temperature gas chromatography in order to determine the optimum incubation time. The 2-monoacylglycerols were then isolated by thin-layer chromatography and fatty acid methyl esters prepared. The delta 13C values obtained indicate that fatty acids from any position on the glycerol backbone are isotopically identical. Thus, whilst quantification of fatty acid composition at the 2-position and measurement of delta 13C values of oils and their major fatty acids are useful criteria in edible oil purity assessment, measurement of delta 13C values of fatty acids from the 2-position does not assist with oil purity assignments.

  12. NON-AUTOCLAVE SILICATE BRICK

    Directory of Open Access Journals (Sweden)

    V. N. Yaglov

    2015-01-01

    Full Text Available The paper proposes a technology for obtaining bricks on the basis of lime-silica mixtures where chemical interactions are practically completely realized in dispersive state at the stage of preparation of binding contact maturing and raw mixture as a whole. The role of forming operation (moulding is changed in principle because in this case conversion of dispersive system into a rock-like solid occurs and due to this the solid obtains complete water-resistance in contact with water immediately after forming operation. Theoretical basis for the developed technology is capability of silicate dispersive substances (hydrated calcium silicate to transit in non-stable state, to form a rock-like water-resistant solid in the moment of mechanical load application during forming process. Specific feature of the proposed method is an exclusion of additional operations for autoclaving of products from the process of obtaining a silicate brick.Synthetic hydrated calcium silicate in contrast to natural ones are more uniform in composition and structure, they contain less impurities and they are characterized by dispersive composition and due to the mentioned advantages they find wider practical application. Contact-condensation binders permit to manipulate product properties on their basis and ensure maximum correspondence to the requirements of the concrete application. Raw material sources for obtaining synthetic hydrated calcium silicates are practically un-limited because calcium-silicon containing substances are found as in various technogenic wastes so in natural compounds as well. So the problem for obtaining hydrated calcium silicates having contact-condensation ability for structure formation becomes more and more actual one. This transition is considered as dependent principally on arrangement rate of substance particles which determined the level of its instability.

  13. [Determination of naphthenic acids in distillates of crude oil by gas chromatography/chemical ionization-mass spectrometry].

    Science.gov (United States)

    Lü, Zhenbo; Tian, Songbai; Zhai, Yuchun; Sun, Yanwei; Zhuang, Lihong

    2004-05-01

    The petroleum carboxylic acids in 200-420 degrees C distillate of crude oil were separated by the extraction with column chromatography on an anion exchange resin. The effect of the composition and structure of naphthenic acids on separation were studied by the infra-red (IR) spectroscopic techniques. Naphthenic acids and iso-butane reagent gas were introduced into the ion source for chemical ionization, in which the ions represented by [M + C4H9]+ were used to calculate the relative molecular mass for each acid. Based on the mass spectra of pure fatty and naphthenic acids, in combination with the z-series formula CnH(2n + z)O2, the naphthenic acids can be classified into fatty, mono-, bi- ... hexa-cyclic types. The results indicated that the relative molecular mass range of naphthenic acids in this distillates was 170-510, and the carbon number range was C10-C35. The contents of bi-cyclic and tri-cyclic naphthenic acids were higher than others.

  14. Attributes of the soil fertilized with sewage sludge and calcium and magnesium silicate

    Directory of Open Access Journals (Sweden)

    Geraldo R. Zuba Junio

    2015-11-01

    Full Text Available ABSTRACTThis study aimed to evaluate the chemical attributes of an Inceptisol cultivated with castor bean (Ricinus communis L., variety ‘BRS Energia’, fertilized with sewage sludge compost and calcium (Ca and magnesium (Mg silicate. The experiment was conducted at the ICA/UFMG, in a randomized block design, using a 2 x 4 factorial scheme with three replicates, and the treatments consisted of two doses of Ca-Mg silicate (0 and 1 t ha-1 and four doses of sewage sludge compost (0, 23.81, 47.62 and 71.43 t ha-1, on dry basis. Soil organic matter (OM, pH, sum of bases (SB, effective cation exchange capacity (CEC(t, total cation exchange capacity (CEC(T, base saturation (V% and potential acidity (H + Al were evaluated. There were no significant interactions between doses of sewage sludge compost and doses of Ca-Mg silicate on soil attributes, and no effect of silicate fertilization on these attributes. However, fertilization with sewage sludge compost promoted reduction in pH and increase in H + Al, OM and CEC. The dose of 71.43 t ha-1 of sewage sludge compost promoted the best soil chemical conditions.

  15. Simultaneous determination of amoxicillin and clavulanic acid in the human plasma by high performance liquid chromatography: Mass spectrometry (UPLC/MS

    Directory of Open Access Journals (Sweden)

    Ćirić Biljana

    2010-01-01

    Full Text Available Background/Aim. Quantitative analysis of amoxicillin and clavulanic acid in biological matrices requires sensitive and specific methods which allow determination of therapeutic concentration in μg/mL range. Analytical methods for determination of their concentrations in body fluids described in literature include high performance liquid chromatography coupled to UV detector (HPLC-UV and liquid chromatography-mass spectrometry (LC-MS. The aim of this study was to develop sensitive and specific ultra performance liquid chromatography/ mass spectrometry (UPLC/MS method which could be used for the spectral identification and quantification of the low concentrations of amoxicillin and clavulanic acid in the human plasma. Method. A sensitive and specific UPLC/MS method for amoxicillin and clavulanic acid determination was developed in this study. The samples were taken from the adult healthy volunteers receiving per os one tablet of amoxicillin (875 mg in combination with clavulanic acid (125 mg. Results. Plasma samples were pretreated by direct deproteinization with perchloric acid. Quantification limit of 0.01 μg/ml for both amoxicillin and clavulanic acid was achieved. The method was reproducible day by day (RSD < 7 %. Analytical recoveries for amoxicillin ranged from 98.82% to 100.9% (for concentrations of 1, 5 and 20 μg/mL, and recoveries for clavulanic acid were 99,89% to 100.1% (for concentrations of 1, 2 and 5 μg/mL. This assay was successfully applied to a pilot pharmacokinetic study in healthy volunteers after a single-oral administration of amoxicillin/ clavulanic combination. The determined plasma concentrations of both amoxicillin and clavulanic acid were in the range of the expected values upon the literature data for HPLC-UV and LC-MS methods. Conclusion. The described method provided a few advantages comparing with LC/MS-MS method. The method is faster using running time of 5 minute, has lower limit of quantification (LOQ and it

  16. Production of precipitated calcium carbonate from calcium silicates and carbon dioxide

    International Nuclear Information System (INIS)

    Teir, Sebastian; Eloneva, Sanni; Zevenhoven, Ron

    2005-01-01

    The possibilities for reducing carbon dioxide emissions from the pulp and paper industry by calcium carbonation are presented. The current precipitated calcium carbonate (PCC) production uses mined, crushed calcium carbonate as raw materials. If calcium silicates were used instead, carbon dioxide emissions from the calcination of carbonates would be eliminated. In Finland, there could, thus, be a potential for eliminating 200 kt of carbon dioxide emissions per year, considering only the PCC used in the pulp and paper industry. A preliminary investigation of the feasibility to produce PCC from calcium silicates and the potential to replace calcium carbonate as the raw material was made. Calcium carbonate can be manufactured from calcium silicates by various methods, but only a few have been experimentally verified. The possibility and feasibility of these methods as a replacement for the current PCC production process was studied by thermodynamic equilibrium calculations using HSC software and process modelling using Aspen Plus[reg]. The results from the process modelling showed that a process that uses acetic acid for extraction of the calcium ions is a high potential option for sequestering carbon dioxide by mineral carbonation. The main obstacle seems to be the limited availability and relatively high price of wollastonite, which is a mineral with high calcium silicate content. An alternative is to use the more common, but also more complex, basalt rock instead

  17. Liquid chromatography mass spectrometry determination of perfluoroalkyl acids in environmental solid extracts after phospholipid removal and on-line turbulent flow chromatography purification.

    Science.gov (United States)

    Mazzoni, M; Polesello, S; Rusconi, M; Valsecchi, S

    2016-07-01

    An on-line TFC (Turbulent Flow Chromatography) clean up procedures coupled with UHPLC-MS/MS (Ultra High Performance Liquid Chromatography Mass Spectrometry) multi-residue method was developed for the simultaneous determination of 8 perfluroalkyl carboxylic acids (PFCA, from 5 to 12 carbon atoms) and 3 perfluoroalkyl sulfonic acids (PFSA, from 4 to 8 carbon atoms) in environmental solid matrices. Fast sample preparation procedure was based on a sonication-assisted extraction with acetonitrile. Phospholipids in biological samples were fully removed by an off-line SPE purification before injection, using HybridSPE(®) Phospholipid Ultra cartridges. The development of the on-line TFC clean-up procedure regarded the choice of the stationary phase, the optimization of the mobile phase composition, flow rate and injected volume. The validation of the optimized method included the evaluation of matrix effects, accuracy and reproducibility. Signal suppression in the analysis of fortified extracts ranged from 1 to 60%, and this problem was overcome by using isotopic dilution. Since no certified reference materials were available for PFAS in these matrices, accuracy was evaluated by recoveries on spiked clam samples which were 98-133% for PFCAs and 40-60% for PFSAs. MLDs and MLQs ranged from 0.03 to 0.3ngg(-1) wet weight and from 0.1 to 0.9ngg(-1) wet weight respectively. Repeatability (intra-day precision) and reproducibility (inter-day precision) showed RSD from 3 to 13% and from 4 to 27% respectively. Validated on-line TFC/UHPLC-MS/MS method has been applied for the determination of perfluoroalkyl acids in different solid matrices (sediment, fish, bivalves and bird yolk). Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Electrospun nanofibrous scaffolds of poly (L-lactic acid)-dicalcium silicate composite via ultrasonic-aging technique for bone regeneration

    Energy Technology Data Exchange (ETDEWEB)

    Dong, Shengjie [Department of Orthopaedics, The First Affiliated Hospital of Soochow University, 188 Shizi St, Suzhou, Jiangsu 215006 (China); Sun, Junying, E-mail: wodaoshi@sohu.com [Department of Orthopaedics, The First Affiliated Hospital of Soochow University, 188 Shizi St, Suzhou, Jiangsu 215006 (China); Li, Yadong [College of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou, Jiangsu 215123 (China); Li, Jun [Department of Orthopaedics, The First Affiliated Hospital of Soochow University, 188 Shizi St, Suzhou, Jiangsu 215006 (China); Cui, Wenguo [Orthopedic Institute, Soochow University, 708 Renmin Rd, Suzhou, Jiangsu 215007 (China); Li, Bin, E-mail: binli@suda.edu.cn [Department of Orthopaedics, The First Affiliated Hospital of Soochow University, 188 Shizi St, Suzhou, Jiangsu 215006 (China)

    2014-02-01

    Polymeric nanofibrous composite scaffolds incorporating bioglass and bioceramics have been increasingly promising for bone tissue engineering. In the present study, electrospun poly (L-lactic acid) (PLLA) scaffolds containing dicalcium silicate (C{sub 2}S) nanoparticles (approximately 300 nm) were fabricated. Using a novel ultrasonic dispersion and aging method, uniform C{sub 2}S nanoparticles were prepared and they were homogenously distributed in the PLLA nanofibers upon electrospinning. In vitro, the PLLA-C{sub 2}S fibers induced the formation of HAp on the surface when immersed in simulated body fluid (SBF). During culture, the osteoblastic MC3T3-E1 cells adhered well on PLLA-C{sub 2}S scaffolds, as evidenced by the well-defined actin stress fibers and well-spreading morphology. Further, compared to pure PLLA scaffolds without C{sub 2}S, PLLA-C{sub 2}S scaffolds markedly promoted the proliferation of MC3T3-E1 cells as well as their osteogenic differentiation, which was characterized by the enhanced alkaline phosphatase (ALP) activity. Together, findings from this study clearly demonstrated that PLLA-C{sub 2}S composite scaffold may function as an ideal candidate for bone tissue engineering. - Highlights: • Dicalcium silicate (C{sub 2}S) nanoparticles were prepared via a sol–gel process. • C{sub 2}S nanoparticles were stabilized using ultrasonic-aging technique. • PLLA-C{sub 2}S composite nanofibers were fabricated through electrospinning technique. • C{sub 2}S nanoparticles could be homogenously distributed in nanofibers. • The composite scaffolds enhanced proliferation and differentiation of osteoblasts.

  19. Large-scale separation of amino acids by continuous displacement chromatography

    Energy Technology Data Exchange (ETDEWEB)

    DeCarli, J.P. II; Carta, G.; Byers, C.H.

    1989-10-01

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

  20. Calcium isotope fractionation in liquid chromatography with benzo-18-crown-6 resin in aqueous hydrobromic acid medium

    International Nuclear Information System (INIS)

    Sato, Takuya; Oi, Takao

    2015-01-01

    Liquid chromatography operated in a breakthrough mode was employed to study calcium isotope fractionation in the aqueous hydrobromic acid medium. Highly porous silica beads, the inner pores of which were embedded with a benzo-18-crown-6 ether resin, were used as column packing material. Enrichment of heavier isotopes of calcium was observed in the frontal part of respective calcium chromatograms. The values of the isotope fractionation coefficient were on the order of 10 -3 . The observed isotope fractionation coefficient was dependent on the concentration of hydrobromic acid in the calcium feed solution; a higher HBr concentration resulted in a smaller fractionation coefficient value. The present calcium isotope effects were most probably mass-dependent, indicating that they mostly came from isotope effects based on molecular vibration. Molecular orbital calculations supported the present experimental results in a qualitative fashion. Chromatography operated in aqueous HBr media is a better system of Ca isotope separation than that operated in aqueous HCl media. (author)

  1. Dosage simultané des acides sorbique et benzoïque dans les vins par chromatographie en phase gazeuse

    Directory of Open Access Journals (Sweden)

    F. Ureta

    1984-12-01

    Dans ce travail nous décrivons une méthode par chromatographie en phase gazeuse sur colonne capillaire qui permet en une seule opération de déterminer les acides benzoïque et sorbique dans les vins.

  2. Thermodynamics and Kinetics of Silicate Vaporization

    Science.gov (United States)

    Jacobson, Nathan S.; Costa, Gustavo C. C.

    2015-01-01

    Silicates are a common class of materials that are often exposed to high temperatures. The behavior of these materials needs to be understood for applications as high temperature coatings in material science as well as the constituents of lava for geological considerations. The vaporization behavior of these materials is an important aspect of their high temperature behavior and it also provides fundamental thermodynamic data. The application of Knudsen effusion mass spectrometry (KEMS) to silicates is discussed. There are several special considerations for silicates. The first is selection of an appropriate cell material, which is either nearly inert or has well-understood interactions with the silicate. The second consideration is proper measurement of the low vapor pressures. This can be circumvented by using a reducing agent to boost the vapor pressure without changing the solid composition or by working at very high temperatures. The third consideration deals with kinetic barriers to vaporization. The measurement of these barriers, as encompassed in a vaporization coefficient, is discussed. Current measured data of rare earth silicates for high temperature coating applications are discussed. In addition, data on magnesium-iron-silicates (olivine) are presented and discussed.

  3. An integrated scheme for the simultaneous determination of biogenic amines, precursor amino acids, and related metabolites by liquid chromatography with electrochemical detection.

    Science.gov (United States)

    Oka, K; Kojima, K; Togari, A; Nagatsu, T; Kiss, B

    1984-06-08

    A new method using high-performance liquid chromatography with electrochemical detection (HPLC-ED) for the simultaneous determination of monoamines, their precursor amino acids, and related major metabolites in small samples of brain tissue weighing from 0.5 to 50 mg is described. The method is based on the preliminary isolation of monoamines (dopamine, norepinephrine, epinephrine, and serotonin), their precursor amino acids (tyrosine, 3,4-dihydroxyphenylalanine, tryptophan and 5-hydroxytryptophan), and their major metabolites (3-methoxytyramine, normetanephrine, 3,4-dihydroxyphenylacetic acid, homovanillic acid, vanillylmandelic acid, 3-methoxy-4-hydroxyphenylethyleneglycol, and 5-hydroxyindoleacetic acid) by chromatography on small columns of Amberlite CG-50 and Dowex 50W, and by ethyl acetate extraction. All the compounds in the four isolated fractions were measured by HPLC-ED on a reversed-phase column under four different conditions. The sensitivity was from 0.1 to 40 pmol, depending on the substances analysed. This newly established method was applied to the study of the effects of an aromatic L-amino acid decarboxylase inhibitor (NSD-1015) and a monoamine oxidase inhibitor (pargyline) on the levels of monoamines, their precursor amino acids and their major metabolites in brain regions of mice.

  4. Preparation and characterization of new poly(amide–imide reinforced layer silicate nanocomposite containing N,N′-pyrromellitoyl-bis-l-phenyl acetic acid

    Directory of Open Access Journals (Sweden)

    Khalil Faghihi

    2014-12-01

    Full Text Available Two new samples of poly(amide–imide/montmorillonite reinforced nanocomposites containing N,N′-pyrromellitoyl-bis-l-phenyl acetic acid moiety in the main chain were synthesized by a convenient solution intercalation technique. Poly(amide–imide (PAI 3 as a source of polymer matrix was synthesized by the direct polycondensation reaction of N,N′-pyrromelitoyl-bis-l-phenyl acetic acid 1 with 4,4′-diamino diphenyl ether 2 in the presence of triphenyl phosphite (TPP, CaCl2, pyridine and N-methyl-2-pyrrolidone (NMP. Morphology and structure of the resulting PAI-nanocomposite films 4a and 4b with 10% and 20% silicate particles were characterized by FTIR spectroscopy, X-ray diffraction (XRD and scanning electron microscopy (SEM. The effect of clay dispersion and the interaction between clay and polymeric chains on the properties of nanocomposite films were investigated by using UV–vis spectroscopy, thermogravimetric analysis (TGA and water uptake measurements.

  5. Development of an ultrahigh-performance liquid chromatography-electrospray ionization-tandem mass spectrometry method for the simultaneous determination of salicylic acid, jasmonic acid, and abscisic acid in rose leaves.

    Science.gov (United States)

    Bosco, Renato; Daeseleire, Els; Van Pamel, Els; Scariot, Valentina; Leus, Leen

    2014-07-09

    This paper describes a method to detect and quantitate the endogenous plant hormones (±)-2-cis-4-trans-abscisic acid, (-)-jasmonic acid, and salicylic acid by means of ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) in hybrid rose leaf matrices. Deuterium-labeled [(2)H6] (+)-2-cis-4-trans-abscisic acid, [(2)H6] (±)-jasmonic acid, and [(2)H4]-salicylic acid were used as internal standards. Rose samples (10 mg) were extracted with methanol/water/acetic acid (10:89:1) and subsequently purified on an Oasis MCX 1 cm(3) Vac SPE cartridge. Performance characteristics were validated according to Commission Decision 2002/657/EC. Recovery, repeatability, and within-laboratory reproducibility were acceptable for all phytohormones tested at three different concentrations. The decision limit and detection capability for (±)-2-cis-4-trans-abscisic acid, (-)-jasmonic acid, and salicylic acid were 0.0075 and 0.015 μg/g, 0.00015 and 0.00030 μg/g, and 0.0089 and 0.018 μg/g, respectively. Matrix effects (signal suppression or enhancement) appeared to be high for all substances considered, implying the need for quantitation based on matrix-matched calibration curves.

  6. PREPARATIVE ISOLATION AND PURIFICATION OF THREE GLYCINE-CONJUGATED CHOLIC ACIDS FROM PULVIS FELLIS SUIS BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY COUPLED WITH ELSD DETECTION

    OpenAIRE

    He, Jiao; Li, Jing; Sun, Wenji; Zhang, Tianyou; Ito, Yoichiro

    2012-01-01

    Coupled with evaporative light scattering detection, a high-speed counter-current chromatography (HSCCC) method was developed for preparative isolation and purification of three glycine-conjugated cholic acids, glycochenodeoxycholic acid (GCDCA), glycohyodeoxycholic acid (GHDCA) and glycohyocholic acid (GHCA) from Pulvis Fellis Suis (Pig gallbladder bile) for the first time. The separation was performed with a two-phase solvent system consisted of chloroform-methanol-water-acetic acid (65:30:...

  7. Plasma capric acid concentrations in healthy subjects determined by high-performance liquid chromatography.

    Science.gov (United States)

    Shrestha, Rojeet; Hui, Shu-Ping; Imai, Hiromitsu; Hashimoto, Satoru; Uemura, Naoto; Takeda, Seiji; Fuda, Hirotoshi; Suzuki, Akira; Yamaguchi, Satoshi; Hirano, Ken-Ichi; Chiba, Hitoshi

    2015-09-01

    Capric acid (FA10:0, decanoic acid) is a medium-chain fatty acid abundant in tropical oils such as coconut oil, whereas small amounts are present in milk of goat, cow, and human. Orally ingested FA10:0 is transported to the liver and quickly burnt within it. Only few reports are available for FA10:0 concentrations in human plasma. Fasting (n = 5, male/female = 3/2, age 31 ± 9.3 years old) and non-fasting (n = 106, male/female = 44/62, age 21.9 ± 3.2 years old) blood samples were collected from apparently healthy Japanese volunteers. The total FA10:0 in the plasma were measured by high-performance liquid chromatography after derivatization with 2-nitrophenylhydrazine followed by UV detection. Inter and intra-assay coefficient of variation of FA10:0 assay at three different concentrations ranged in 1.7-3.9 and 1.3-5.4%, respectively, with an analytical recovery of 95.2-104.0%. FA10:0 concentration was below detection limit (0.1 µmol/L) in each fasting human plasma. FA10:0 was not detected in 50 (47.2%) of 106 non-fasting blood samples, while 29 (27.4%) plasma samples contained FA10:0 less than or equal to 0.5 µmol/L (0.4 ± 0.1), and 27 (25.5%) contained it at more than 0.5 µmol/L (0.9 ± 0.3). A half of the non-fasting plasma samples contained detectable FA10:0. This simple, precise, and accurate high-performance liquid chromatography method might be useful for monitoring plasma FA10:0 during medium-chain triglycerides therapy. © The Author(s) 2015.

  8. Analysis of polycyclic aromatic hydrocarbons. I. Determination by gas chromatography with glass and fused solica capillary columns

    International Nuclear Information System (INIS)

    Perez Garcia, M.; Gonzalez, D.

    1987-01-01

    A study of the analysis by gas chromatography of aromatic polycyclic hydrocarbons is presented. The separation has been carried out by glass and fused silice capillary column. The limitations and the advantages of the procedure are discussed in terms of separation efficiency, sensitivity and precision. (author). 3 figs., 17 refs

  9. Polymer-Layer Silicate Nanocomposites

    DEFF Research Database (Denmark)

    Potarniche, Catalina-Gabriela

    Nowadays, some of the material challenges arise from a performance point of view as well as from recycling and biodegradability. Concerning these aspects, the development of polymer layered silicate nanocomposites can provide possible solutions. This study investigates how to obtain polymer layered...... with a spectacular improvement up to 300 % in impact strength were obtained. In the second part of this study, layered silicate bio-nanomaterials were obtained starting from natural compounds and taking into consideration their biocompatibility properties. These new materials may be used for drug delivery systems...... and as biomaterials due to their high biocompatible properties, and because they have the advantage of being biodegradable. The intercalation process of natural compounds within silicate platelets was investigated. By uniform dispersing of binary nanohybrids in a collagen matrix, nanocomposites with intercalated...

  10. Chiral separation of amino acids in biological fluids by micellar electrokinetic chromatography with laser-induced fluorescence detection.

    Science.gov (United States)

    Thorsén, G; Bergquist, J

    2000-08-18

    A method is presented for the chiral analysis of amino acids in biological fluids using micellar electrokinetic chromatography (MEKC) and laser-induced fluorescence (LIF). The amino acids are derivatized with the chiral reagent (+/-)-1-(9-anthryl)-2-propyl chloroformate (APOC) and separated using a mixed micellar separation system. No tedious pre-purification of samples is required. The excellent separation efficiency and good detection capabilities of the MEKC-LIF system are exemplified in the analysis of urine and cerebrospinal fluid. This is the first time MEKC has been reported for chiral analysis of amino acids in biological fluids. The amino acids D-alanine, D-glutamine, and D-aspartic acid have been observed in cerebrospinal fluid, and D-alanine and D-glutamic acid in urine. To the best of our knowledge no measurements of either D-alanine in cerebrospinal fluid or D-glutamic acid in urine have been presented in the literature before.

  11. LABORATORY INVESTIGATIONS OF SILICATE MUD CONTAMINATION WITH CALCIUM

    Directory of Open Access Journals (Sweden)

    Nediljka Gaurina-Međimurec

    2004-12-01

    Full Text Available The silicate-based drilling fluid is a low solids KCl/polymer system with the addition of soluble sodium or potassium silicate to enhance inhibition and wellbore stability. Silicate-based drilling fluids exhibit remarkable shale and chalk stabilizing properties, resulting in gauge hole and the formation of firm cuttings when drilling reactive shales and soft chalks. Silicates protect shales by in-situ gellation when exposed to the neutral pore fluid and precipitation, which occurs on contact with divalent ions present at the surface of the shale. Also, silicates prevent the dispersion and washouts when drilling soft chalk by reacting with the Ca2+ ions present on chalk surfaces of cutting and wellbore to form a protective film. The silicate-based drilling fluid can be used during drilling hole section through shale interbeded anhydrite formations because of its superior shale stabilizing characteristics. However, drilling through the anhydrite can decrease the silicate concentration and change rheological and filtration fluid properties. So, the critical concentration of calcium ions should be investigated by lab tests. This paper details the mechanism of shale inhibition using silicate-based drilling fluid, and presents results of lab tests conducted to ascertain the effect of Ca2+ ions on silicate level in the fluid and the fluid properties.

  12. 21 CFR 582.2122 - Aluminum calcium silicate.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Aluminum calcium silicate. 582.2122 Section 582.2122 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED....2122 Aluminum calcium silicate. (a) Product. Aluminum calcium silicate. (b) Tolerance. 2 percent. (c...

  13. 21 CFR 182.2122 - Aluminum calcium silicate.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Aluminum calcium silicate. 182.2122 Section 182.2122 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED....2122 Aluminum calcium silicate. (a) Product. Aluminum calcium silicate. (b) Tolerance. 2 percent. (c...

  14. Spiculogenesis in the siliceous sponge Lubomirskia baicalensis studied with fluorescent staining.

    Science.gov (United States)

    Annenkov, Vadim V; Danilovtseva, Elena N

    2016-04-01

    Siliceous sponges are the most primitive multicellular animals whose skeleton consists of spicules - needle-like constructions from silicon dioxide surrounding organic axial filaments. Mechanisms of spicule formation have been intensively studied due to the high ecological importance of sponges and their interest to materials science. Light and electron microscopy are not appropriate enough to display the process from silicon-enriched cells to mature spicules because of composite structure of the sponge tissues. In this article, spiculogenesis in the siliceous sponge has been studied for the first time with the use of fluorescent microscopy. Fluorescent vital dye NBD-N2 was applied to stain growing siliceous structures in the sponge and primmorph cell system. The main stages of spicule growth in the fresh-water sponge Lubomirskia baicalensis (Pallas, 1773) were visualized: silicon accumulation in sclerocytes; formation of an organic filament protruding from the cell; further elongation of the filament and growth of the spicule in a spindle-like form with enlargement in the center; merger with new sclerocytes and formation of the mature spicule. Fluorescent microscopy combined with SEM allows us to overcome the virtual differentiation between intra- and extracellular mechanisms of spicule growth. The growing spicule can capture silicic acid from the extracellular space and merge with new silicon-enriched cells. Visualization of the growing spicules with the fluorescent dye allows us to monitor sponge viability in ecological or toxicological experiments and to apply genomic, proteomic and biochemical techniques. Copyright © 2016 Elsevier Inc. All rights reserved.

  15. Analysis of Caffeic Acid Extraction From Ocimum gratissimum Linn. by High Performance Liquid Chromatography and its Effects on a Cervical Cancer Cell Line

    Directory of Open Access Journals (Sweden)

    Je-Chiuan Ye

    2010-09-01

    Conclusion: This paper shows that high performance liquid chromatography is a suitable analytical method for determining caffeic acid levels in O. gratissimum, Ju ZenTa, and several vegetable oils. Caffeic acid can suppress the proliferation of HeLa cells.

  16. Determination of Monochloroacetic Acid in Swimming Pool Water by Ion Chromatography-Conductivity Detection

    Directory of Open Access Journals (Sweden)

    Maria Pythias B. Espino

    2013-12-01

    Full Text Available In this study, an analytical method involving ion chromatography with conductivity detection was developed and optimized for the determination of monochloroacetic acid in swimming pool water. The ion chromatographic method has a detection limit of 0.02 mg L-1 and linear range of 0.05 to 1.0 mg L-1 with correlation coeff icient of 0.9992. The method is reproducible with percent RSD of 0.052% (n=10. The recovery of monochloroacetic acid spiked in different water types (bottled, tap and swimming pool water ranged from 28 to 122%. In dilute solutions, chloride and bromide were simultaneously analyzed along with monochloroacetic acid using the optimized method. Chloride and bromide have detection limits of 0.01 to 0.05 mg L-1, respectively. The usefulness of the ion chromatographic method was demonstrated in the analysis of monochloroacetic acid in swimming pool water samples. In such highly-chlorinated samples, an Ag/H cartridge was used prior to the ion chromatographic determination so as to minimize the signal due to chloride ion. Monochloroacetic acid was detected in concentrations between 0.020 and 0.093 mg L-1 in three of the six swimming pool water samples studied. The presence of monochloroacetic acid in the swimming pool water samples suggests the possible occurrence of other disinfection by-products in these waters.

  17. Determination of Monochloroacetic Acid in Swimming Pool Water by Ion Chromatography-Conductivity Detection

    Directory of Open Access Journals (Sweden)

    Maria Pythias B. Espino

    2013-02-01

    Full Text Available In this study, an analytical method involving ion chromatography with conductivity detection was developed and optimized for the determination of monochloroacetic acid in swimming pool water. The ion chromatographic method has a detection limit of 0.02 mg L-1 and linear range of 0.05 to 1.0 mg L-1 with correlation coeff icient of 0.9992. The method is reproducible with percent RSD of 0.052% (n=10. The recovery of monochloroacetic acid spiked in different water types (bottled, tap and swimming pool water ranged from 28 to 122%. In dilute solutions, chloride and bromide were simultaneously analyzed along with monochloroacetic acid using the optimized method. Chloride and bromide have detection limits of 0.01 to 0.05 mg L-1, respectively. The usefulness of the ion chromatographic method was demonstrated in the analysis of monochloroacetic acid in swimming pool water samples. In such highly-chlorinated samples, an Ag/H cartridge was used prior to the ion chromatographic determination so as to minimize the signal due to chloride ion. Monochloroacetic acid was detected in concentrations between 0.020 and 0.093 mg L-1 in three of the six swimming pool water samples studied. The presence of monochloroacetic acid in the swimming pool water samples suggests the possible occurrence of other disinfection by-products in these waters.

  18. Sensitive determination of D-lactic acid and L-lactic acid in urine by high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Henry, H; Marmy Conus, N; Steenhout, P; Béguin, A; Boulat, O

    2012-04-01

    D-lactic acid in urine originates mainly from bacterial production in the intestinal tract. Increased D-lactate excretion as observed in patients affected by short bowel syndrome or necrotizing enterocolitis reflects D-lactic overproduction. Therefore, there is a need for a reliable and sensitive method able to detect D-lactic acid even at subclinical elevation levels. A new and highly sensitive method for the simultaneous determination of L- and D-lactic acid by a two-step procedure has been developed. This method is based on the concentration of lactic acid enantiomers from urine by supported liquid extraction followed by high-performance liquid chromatography-tandem mass spectrometry. The separation was achieved by the use of an Astec Chirobiotic™ R chiral column under isocratic conditions. The calibration curves were linear over the ranges of 2-400 and 0.5-100 µmol/L respectively for L- and D-lactic acid. The limit of detection of D-lactic acid was 0.125 µmol/L and its limit of quantification was 0.5 µmol/L. The overall accuracy and precision were well within 10% of the nominal values. The developed method is suitable for production of reference values in children and could be applied for accurate routine analysis. Copyright © 2011 John Wiley & Sons, Ltd.

  19. Antibacterial Activity of Silicate Bioceramics

    Institute of Scientific and Technical Information of China (English)

    HU Sheng; NING Congqin; ZHOU Yue; CHEN Lei; LIN Kaili; CHANG Jiang

    2011-01-01

    Four kinds of pure silicate ceramic particles, CaSiO3, Ca3SiO5, bredigite and akermanite were prepared and their bactericidal effects were systematically investigated. The phase compositions of these silicate ceramics were characterized by XRD. The ionic concentration meas urement revealed that the Calcium (Ca) ion concentration were relatively higher in Ca3SiO5 and bredigite, and much lower in CaSiO3 and akermanite. Accordingly, the pH values of the four silicate ceramics extracts showed a positive correlation with the particle concentrations. Meanwhile, by decreasing the particle size, higher Ca ion concentrations can be achieved, leading to the increase of aqueous pH value as well. In summary, all of the four silicate ceramics tested in our study showed antibacterial effect in a dose-dependent manner. Generally, the order of their antibacterial activity against E.coli from strong to weak is Ca3SiO5, bredigite, CaSiO3 and akermanite.

  20. Amended Silicated for Mercury Control

    Energy Technology Data Exchange (ETDEWEB)

    James Butz; Thomas Broderick; Craig Turchi

    2006-12-31

    Amended Silicates{trademark}, a powdered, noncarbon mercury-control sorbent, was tested at Duke Energy's Miami Fort Station, Unit 6 during the first quarter of 2006. Unit 6 is a 175-MW boiler with a cold-side electrostatic precipitator (ESP). The plant burns run-of-the-river eastern bituminous coal with typical ash contents ranging from 8-15% and sulfur contents from 1.6-2.6% on an as-received basis. The performance of the Amended Silicates sorbent was compared with that for powdered activated carbon (PAC). The trial began with a period of baseline monitoring during which no sorbent was injected. Sampling during this and subsequent periods indicated mercury capture by the native fly ash was less than 10%. After the baseline period, Amended Silicates sorbent was injected at several different ratios, followed by a 30-day trial at a fixed injection ratio of 5-6 lb/MMACF. After this period, PAC was injected to provide a comparison. Approximately 40% mercury control was achieved for both the Amended Silicates sorbent and PAC at injection ratios of 5-6 lbs/MMACF. Higher injection ratios did not achieve significantly increased removal. Similar removal efficiencies have been reported for PAC injection trials at other plants with cold-side ESPs, most notably for plants using medium to high sulfur coal. Sorbent injection did not detrimentally impact plant operations and testing confirmed that the use of Amended Silicates sorbent does not degrade fly ash quality (unlike PAC). The cost for mercury control using either PAC or Amended Silicates sorbent was estimated to be equivalent if fly ash sales are not a consideration. However, if the plant did sell fly ash, the effective cost for mercury control could more than double if those sales were no longer possible, due to lost by-product sales and additional cost for waste disposal. Accordingly, the use of Amended Silicates sorbent could reduce the overall cost of mercury control by 50% or more versus PAC for locations where

  1. Interstellar silicate analogs for grain-surface reaction experiments: Gas-phase condensation and characterization of the silicate dust grains

    Energy Technology Data Exchange (ETDEWEB)

    Sabri, T.; Jäger, C. [Laboratory Astrophysics Group of the Max Planck Institute for Astronomy at the Friedrich Schiller University Jena Institute of Solid State Physics, Helmholtzweg 3, D-07743 Jena (Germany); Gavilan, L.; Lemaire, J. L.; Vidali, G. [Observatoire de Paris/Université de Cergy-Pontoise, 5 mail Gay Lussac, F-95000 Cergy-Pontoise (France); Mutschke, H. [Laboratory Astrophysics Group of the Astrophysical Institute and University Observatory, Friedrich Schiller University Jena Schillergässchen 3, D-07743 Jena (Germany); Henning, T., E-mail: tolou.sabri@uni-jena.de [Max Planck Institute for Astronomy Königstuhl 17, D-69117 Heidelberg (Germany)

    2014-01-10

    Amorphous, astrophysically relevant silicates were prepared by laser ablation of siliceous targets and subsequent quenching of the evaporated atoms and clusters in a helium/oxygen gas atmosphere. The described gas-phase condensation method can be used to synthesize homogeneous and astrophysically relevant silicates with different compositions ranging from nonstoichiometric magnesium iron silicates to pyroxene- and olivine-type stoichiometry. Analytical tools have been used to characterize the morphology, composition, and spectral properties of the condensates. The nanometer-sized silicate condensates represent a new family of cosmic dust analogs that can generally be used for laboratory studies of cosmic processes related to condensation, processing, and destruction of cosmic dust in different astrophysical environments. The well-characterized silicates comprising amorphous Mg{sub 2}SiO{sub 4} and Fe{sub 2}SiO{sub 4}, as well as the corresponding crystalline silicates forsterite and fayalite, produced by thermal annealing of the amorphous condensates, have been used as real grain surfaces for H{sub 2} formation experiments. A specifically developed ultra-high vacuum apparatus has been used for the investigation of molecule formation experiments. The results of these molecular formation experiments on differently structured Mg{sub 2}SiO{sub 4} and Fe{sub 2}SiO{sub 4} described in this paper will be the topic of the next paper of this series.

  2. Separation of amino acids and antibiotics by narrow-bore and normal-bore high-performance liquid chromatography with pre-column derivatization.

    Science.gov (United States)

    Fiedler, H P; Plaga, A

    1987-01-16

    The selectivity, efficiency and lifetime of normal- and narrow-bore columns for high-performance liquid chromatography were investigated for the separation and quantification of amino acids and the amino acid-like antibiotics phosphinothricin and phosphinothricylalanylalanine in biological samples. These compounds were determined by an automated pre-column derivatization with o-phthalaldehyde-2-mercaptoethanol reagent and UV detection at 338 nm.

  3. Quantitative chromatography in the analysis of labelled compounds 1. Quantitative paper chromotography of amino acids by A spot comparison technique

    International Nuclear Information System (INIS)

    Barakat, M.F.; Farag, A.N.; El-Gharbawy, A.A.

    1974-01-01

    For the determination of the specific activity of labelled compounds separated by paper sheet chromatography, it was found essential to perfect the quantitative aspect of the paper chromatographic technique. Actually, so far paper chromatography has been used as a separation tool mainly and its use in quantification of the separated materials is by far less studied. In the present work, the quantitative analysis of amino acids by paper sheet chromatography has been carried out by methods, depending on the use of the relative spot area values for correcting the experimental data obtained. The results obtained were good and reproducible. The main advantage of the proposed technique is its extreme simplicity. No complicated equipment of procedures are necessary

  4. Effect of moisture and chitosan layered silicate on morphology and properties of chitosan/layered silicates films

    International Nuclear Information System (INIS)

    Silva, J.R.M.B. da; Santos, B.F.F. dos; Leite, I.F.

    2014-01-01

    Thin chitosan films have been for some time an object of practical assessments. However, to obtain biopolymers capable of competing with common polymers a significant improvement in their properties is required. Currently, the technology of obtaining polymer/layered silicates nanocomposites has proven to be a good alternative. This work aims to evaluate the effect of chitosan content (CS) and layered silicates (AN) on the morphology and properties of chitosan/ layered silicate films. CS/AN bionanocomposites were prepared by the intercalation by solution in the proportion 1:1 and 5:1. Then were characterized by infrared spectroscopy (FTIR), diffraction (XRD) and X-ray thermogravimetry (TG). It is expected from the acquisition of films, based on different levels of chitosan and layered silicates, choose the best composition to serve as a matrix for packaging drugs and thus be used for future research. (author)

  5. Use of a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin column and propionic acid as an eluent in ion-exclusion/adsorption chromatography of aliphatic carboxylic acids and ethanol in food samples.

    Science.gov (United States)

    Mori, Masanobu; Hironaga, Takahiro; Kajiwara, Hiroe; Nakatani, Nobutake; Kozaki, Daisuke; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2011-01-01

    We developed an ion-exclusion/adsorption chromatography (IEAC) method employing a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin (PS-WCX) column with propionic acid as the eluent for the simultaneous determination of multivalent aliphatic carboxylic acids and ethanol in food samples. The PS-WCX column well resolved mono-, di-, and trivalent carboxylic acids in the acidic eluent. Propionic acid as the eluent gave a higher signal-to-noise ratio, and enabled sensitive conductimetric detection of analyte acids. We found the optimal separation condition to be the combination of a PS-WCX column and 20-mM propionic acid. Practical applicability of the developed method was confirmed by using a short precolumn with a strongly acidic cation-exchange resin in the H(+)-form connected before the separation column; this was to remove cations from food samples by converting them to hydrogen ions. Consequently, common carboxylic acids and ethanol in beer, wine, and soy sauce were successfully separated by the developed method.

  6. Partial Purification of Antimicrobial Compounds Isolated from Mycelia of Tropical Lentinus cladopus LC4

    OpenAIRE

    SUDIRMAN, LISDAR IDWAN

    2010-01-01

    Lentinus cladopus LC4 produced at least eight antimicrobial compounds (ACs) which are active against plant and human pathogens. Three ACs in its crude mycelial were extracted with methanol and partial purification was carried out with silicic acid column chromatography and by thin layer chromatography (PTLC). The antimicrobial activity was tested by paper disc method and antibiographic method. The chromatography purification eluted with dichloromethane containing 5% methanol gave one active f...

  7. Preparation of polymer monolithic column functionalized by arsonic acid groups for mixed-mode capillary liquid chromatography.

    Science.gov (United States)

    Qin, Zhang-Na; Yu, Qiong-Wei; Wang, Ren-Qi; Feng, Yu-Qi

    2018-04-27

    A mixed-mode polymer monolithic column functionalized by arsonic acid groups was prepared by single-step in situ copolymerization of monomers p-methacryloylaminophenylarsonic acid (p-MAPHA) and pentaerythritol triacrylate (PETA). The prepared poly(p-MAPHA-co-PETA) monolithic column has a homogeneous monolithic structure with good permeability and mechanical stability. Zeta potential measurements reveal that the monolithic stationary phase holds a negative surface charge when the mobile phase resides in the pH range of 3.0-8.0. The retention mechanisms of prepared monolithic column are explored by the separation of selected polycyclic aromatic hydrocarbons (PAHs), nucleosides, and three basic compounds. The results indicate that the column functions in three different separation modes associated with reversed-phase chromatography based on hydrophobic interaction, hydrophilic interaction chromatography, and cation-exchange chromatography. The column efficiency of prepared monolithic column is estimated to be 70,000 and 76,000 theoretical plates/m for thiourea and naphthalene, respectively, at a linear flow velocity of 0.85 mm/s using acetonitrile/H 2 O (85/15, v/v) as the mobile phase. Furthermore, an analysis of the retention factors obtained for the PAHs indicates that the prepared monolithic column exhibits good reproducibility with relative standard deviations of 2.9%, 4.0%, and 4.7% based on run-to-run injections, column-to-column preparation, and batch-to-batch preparation, respectively. Finally, we investigate the separation performance of the proposed monolithic column for select phenols, sulfonamides, nucleobases and nucleosides. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. Simultaneous determination of gallic acid and gentisic acid in organic anion transporter expressing cells by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Wang, Li; Halquist, Matthew S; Sweet, Douglas H

    2013-10-15

    In order to elucidate the role of organic anion transporters (OATs) in the renal elimination of gallic acid and gentisic acid, a new, rapid, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the simultaneous determination of gallic acid and gentisic acid in cell lysate, using Danshensu as the internal standard (IS). After a simple liquid-liquid extraction, the analytes were detected in negative ESI mode using selected reaction monitoring. The precursor-to-product ion transitions (m/z) were 169.0→125.0, 153.1→108.0, and 196.8→135.2 for gallic acid, gentisic acid, and the IS, respectively. Chromatographic separation was achieved on a C18 column using mobile phases consisting of water with 0.1% acetic acid (A) and acetonitrile with 0.05% formic acid. (B) The total run time was 3min and calibration curves were linear over the concentrations of 0.33-2400ng/mL for both compounds (r(2)>0.995). Good precision (between 3.11% and 14.1% RSD) and accuracy (between -12.7% and 11% bias) was observed for quality controls at concentrations of 0.33 (lower limit of quantification), 1, 50, and 2000ng/mL. The mean extraction recovery of gallic acid and gentisic acid was 80.7% and 83.5%, respectively. Results from post-column infusion and post-extraction methods indicated that the analytical method exhibited negligible matrix effects. Finally, this validated assay was successfully applied in a cellular uptake study to determine the intracellular concentrations of gallic acid and gentisic acid in OAT expressing cells. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Carbonate-silicate ratio for soil correction and influence on nutrition, biomass production and quality of palisade grass

    Directory of Open Access Journals (Sweden)

    Renato Ferreira de Souza

    2011-10-01

    Full Text Available Silicates can be used as soil correctives, with the advantage of being a source of silicon, a beneficial element to the grasses. However, high concentrations of silicon in the plant would affect the digestibility of the forage. To evaluate the influence of the substitution of the calcium carbonate by calcium silicate on the nutrition, biomass production and the feed quality of the palisade grass [Urochloa brizantha (C. Hochstetter ex A. Rich. R. Webster], three greenhouse experiments were conducted in completely randomized designs with four replications. Experimental units (pots contained a clayey dystrophic Rhodic Haplustox, a sandy clay loam dystrophic Typic Haplustox and a sandy loam dystrophic Typic Haplustox. Each soil received substitution proportions (0, 25, 50, 75 and 100 % of the carbonate by calcium silicate. The increase in the proportion of calcium silicate elevated the concentrations and accumulations of Si, Ca, Mg, and B, reduced Zn and did not alter P in the shoot of plants. The effects of the treatments on the other nutrients were influenced by the soil type. Inclusion of calcium silicate also increased the relative nutritional value and the digestibility and ingestion of the forage, while the concentration and accumulation of crude protein and the neutral detergent and acid detergent fibers decreased. Biomass production and feed quality of the palisade grass were generally higher with the 50 % calcium silicate treatment.

  10. Adsorption of aqueous silicate on hematite

    International Nuclear Information System (INIS)

    Taylor, P.; Ticknor, K.V.

    1997-08-01

    During radioisotope sorption studies, adsorption of silicate from synthetic groundwaters by synthetic hematite was observed. To further investigate this observation, the adsorption of silicate onto hematite (α-Fe 2 O 3 ) powder from a neutral, aqueous NaC1 solution (0.1 mol/dm 3 ), containing 2.56 x 10 -4 mol/dm 3 of Si added as Na 2 SiO 3 ·9H 2 O, was measured at ∼21 deg C. Equilibrium adsorption of silicate amounted to ∼1.93 μmol/m 2 (one Si(O,OH) 4 moiety per 86 A 2 ). It is important to take this adsorption into account when evaluating the ability of iron oxides to adsorb other species, especially anions, from groundwaters. Silicate adsorption is known to diminish the ability of iron oxides to adsorb other anions. (author)

  11. Water-Dispersible Silica-Polyelectrolyte Nanocomposites Prepared via Acid-Triggered Polycondensation of Silicic Acid and Directed by Polycations

    Directory of Open Access Journals (Sweden)

    Philip Overton

    2016-03-01

    Full Text Available The present work describes the acid-triggered condensation of silicic acid, Si(OH4, as directed by selected polycations in aqueous solution in the pH range of 6.5–8.0 at room temperature, without the use of additional solvents or surfactants. This process results in the formation of silica-polyelectrolyte (S-PE nanocomposites in the form of precipitate or water-dispersible particles. The mean hydrodynamic diameter (dh of size distributions of the prepared water-dispersible S-PE composites is presented as a function of the solution pH at which the composite formation was achieved. Poly(2-(dimethylaminoethyl methacrylate (PDMAEMA and block copolymers of DMAEMA and oligo(ethylene glycol methyl ether methacrylate (OEGMA were used as weak polyelectrolytes in S-PE composite formation. The activity of the strong polyelectrolytes poly(methacryloxyethyl trimethylammonium iodide (PMOTAI and PMOTAI-b-POEGMA in S-PE formation is also examined. The effect of polyelectrolyte strength and the OEGMA block on the formation of the S-PE composites is assessed with respect to the S-PE composites prepared using the PDMAEMA homopolymer. In the presence of the PDMAEMA60 homopolymer (Mw = 9400 g/mol, the size of the dispersible S-PE composites increases with solution pH in the range pH 6.6–8.1, from dh = 30 nm to dh = 800 nm. S-PDMAEMA60 prepared at pH 7.8 contained 66% silica by mass (TGA. The increase in dispersible S-PE particle size is diminished when directed by PDMAEMA300 (Mw = 47,000 g/mol, reaching a maximum of dh = 75 nm. S-PE composites formed using PDMAEMA-b-POEGMA remain in the range dh = 20–30 nm across this same pH regime. Precipitated S-PE composites were obtained as spheres of up to 200 nm in diameter (SEM and up to 65% mass content of silica (TGA. The conditions of pH for the preparation of dispersible and precipitate S-PE nanocomposites, as directed by the five selected polyelectrolytes PDMAEMA60, PDMAEMA300, PMOTAI60, PDMAEMA60-b-POEGMA38 and

  12. Self-assembly of natural light-harvesting bacteriochlorophylls of green sulfur photosynthetic bacteria in silicate capsules as stable models of chlorosomes.

    Science.gov (United States)

    Saga, Yoshitaka; Akai, Sho; Miyatake, Tomohiro; Tamiaki, Hitoshi

    2006-01-01

    Naturally occurring bacteriochlorophyll(BChl)s-c, -d, and -e from green sulfur photosynthetic bacteria were self-assembled in an aqueous solution in the presence of octadecyltriethoxysilane and tetraethoxysilane, followed by polycondensation of the alkoxysilanes by incubation for 50 h at 25 degrees C. The resulting BChl self-assemblies in silicate capsules exhibited visible absorption and circular dichroism spectra similar to the corresponding natural light-harvesting systems (chlorosomes) of green sulfur bacteria. Dynamic light scattering measurements indicated that the silicate capsules had an average hydrodynamic diameter of several hundred nanometers. BChl self-aggregates in silicate capsules were significantly stable to a nonionic surfactant Triton X-100, which was apt to decompose the BChl aggregates to their monomeric form, compared with conventional micelle systems. BChls in silicate capsules were more tolerant to demetalation of the central magnesium under acidic conditions than the natural systems.

  13. Derivatisation/solid-phase microextraction followed by gas chromatography-mass spectrometry for the analysis of phenoxy acid herbicides in aqueous samples

    DEFF Research Database (Denmark)

    Nilsson, Torben; Baglio, Daniela; Galdo-Miguez, Isabel

    1998-01-01

    Different combinations of derivatisation and solid-phase microextraction followed by gas chromatography-mass spectrometry were optimised and evaluated for the analysis of phenoxy acid herbicides in water. The most successful derivatisation approach was aqueous-phase derivatisation with benzyl...

  14. Synthesis, Purification, and Quantification of Fatty Acid Ethyl Esters After trans-Esterification of Large Batches of Tobacco Seed Oil

    Directory of Open Access Journals (Sweden)

    Ashraf-Khorassani Mehdi

    2015-03-01

    Full Text Available L'objectif de la présente étude était de quantifier les esters éthyliques d'acides gras (FAEE produits à partir de deux grands lots d'huile de graines de tabac soumis à une transéstérification éthanolique en présence d'un catalyseur d'acide sulfurique. La purification des produits combinés de la réaction des esters éthyliques visait la suppression, autant que faire se peut, de la couleur et de l'odeur du produit final et fut accomplie via une chromatographie sur colonne conventionnelle avec silice sublimée et une élution en tandem de l'hexane, dans un premier temps et de l'alcool éthylique, dans un deuxième temps, en guise de phase mobile. La chromatographie en phase gazeuse fut utilisée afin de quantifier les esters éthyliques des acides gras spécifiques dans la matière purifiée. Le pourcentage d'esters éthyliques d'acides gras purs récupérés dans le lot n°1 s'éleva à près de 87% tandis que le pourcentage d'esters éthyliques d'acides gras purs récupérés dans le lot n°2 fut supérieur à 89% avec des rendements à la préparation supérieurs à 400 g d'esters éthyliques par essai d'estérification. Les esters éthyliques d'acides gras ne possédaient pas d'arome détectable et ne présentaient qu'une légère coloration jaune à l'issue de ce traitement chromatographique. Pour caractériser la pureté de chaque lot d'esters éthyliques d'acides gras produits, une chromatographie en phase supercritique dont la phase mobile était un fluide composé de dioxyde de carbone modifié au méthanol/acétonitrile et une phase fixe composée d'une silice greffée avec groupement fonctionnel octadécyle furent utilisées. Aucune impureté liée au glycérol ou à des acides gras libres ne fut détectée dans le produit transestérifié purifié. Notre article est le premier rapport décrivant la transestérification optimisée de l'huile de graines de tabac à une échelle relativement grande, ladite transest

  15. Silicates materials of high vacuum technology

    CERN Document Server

    Espe, Werner

    2013-01-01

    Materials of High Vacuum Technology, Volume 2: Silicates covers silicate insulators of special importance to vacuum technology. The book discusses the manufacture, composition, and physical and chemical properties of technical glasses, quartz glass, quartzware, vycor glass, ceramic materials, mica, and asbestos.

  16. Online stable carbon isotope ratio measurement in formic acid, acetic acid, methanol and ethanol in water by high performance liquid chromatography-isotope ratio mass spectrometry

    International Nuclear Information System (INIS)

    Tagami, Keiko; Uchida, Shigeo

    2008-01-01

    A suitable analysis condition was determined for high performance liquid chromatography-isotope ratio mass spectrometry (HPLC-IRMS) while making sequential measurements of stable carbon isotope ratios of δ 13 C in formic acid, acetic acid, methanol and ethanol dissolved in water. For this online column separation method, organic reagents are not applicable due to carbon contamination; thus, water and KH 2 PO 4 at low concentrations were tested as mobile phase in combination with a HyPURITY AQUASTAR TM column. Formic acid, acetic acid, methanol and ethanol were separated when 2 mM KH 2 PO 4 aqueous solution was used. Under the determined analysis condition for HPLC-IRMS, carbon concentrations could be measured quantitatively as well as carbon isotope ratio when carbon concentration was higher than 0.4 mM L for each chemical

  17. Determination of short chain carboxylic acids in vegetable oils and fats using ion exclusion chromatography electrospray ionization mass spectrometry.

    Science.gov (United States)

    Viidanoja, Jyrki

    2015-02-27

    A new method for quantification of short chain C1-C6 carboxylic acids in vegetable oils and fats by employing Liquid Chromatography Mass Spectrometry (LC-MS) has been developed. The method requires minor sample preparation and applies non-conventional Electrospray Ionization (ESI) liquid phase chemistry. Samples are first dissolved in chloroform and then extracted using water that has been spiked with stable isotope labeled internal standards that are used for signal normalization and absolute quantification of selected acids. The analytes are separated using Ion Exclusion Chromatography (IEC) and detected with Electrospray Ionization Mass Spectrometry (ESI-MS) as deprotonated molecules. Prior to ionization the eluent that contains hydrochloric acid is modified post-column to ensure good ionization efficiency of the analytes. The averaged within run precision and between run precision were generally lower than 8%. The accuracy was between 85 and 115% for most of the analytes. The Lower Limit of Quantification (LLOQ) ranged from 0.006 to 7mg/kg. It is shown that this method offers good selectivity in cases where UV detection fails to produce reliable results. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. High CO2 and silicate limitation synergistically increase the toxicity of Pseudo-nitzschia fraudulenta.

    Directory of Open Access Journals (Sweden)

    Avery O Tatters

    Full Text Available Anthropogenic CO(2 is progressively acidifying the ocean, but the responses of harmful algal bloom species that produce toxins that can bioaccumulate remain virtually unknown. The neurotoxin domoic acid is produced by the globally-distributed diatom genus Pseudo-nitzschia. This toxin is responsible for amnesic shellfish poisoning, which can result in illness or death in humans and regularly causes mass mortalities of marine mammals and birds. Domoic acid production by Pseudo-nitzschia cells is known to be regulated by nutrient availability, but potential interactions with increasing seawater CO(2 concentrations are poorly understood. Here we present experiments measuring domoic acid production by acclimatized cultures of Pseudo-nitzschia fraudulenta that demonstrate a strong synergism between projected future CO(2 levels (765 ppm and silicate-limited growth, which greatly increases cellular toxicity relative to growth under modern atmospheric (360 ppm or pre-industrial (200 ppm CO(2 conditions. Cellular Si:C ratios decrease with increasing CO(2, in a trend opposite to that seen for domoic acid production. The coastal California upwelling system where this species was isolated currently exhibits rapidly increasing levels of anthropogenic acidification, as well as widespread episodic silicate limitation of diatom growth. Our results suggest that the current ecosystem and human health impacts of toxic Pseudo-nitzschia blooms could be greatly exacerbated by future ocean acidification and 'carbon fertilization' of the coastal ocean.

  19. PREPARATIVE ISOLATION AND PURIFICATION OF THREE GLYCINE-CONJUGATED CHOLIC ACIDS FROM PULVIS FELLIS SUIS BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY COUPLED WITH ELSD DETECTION.

    Science.gov (United States)

    He, Jiao; Li, Jing; Sun, Wenji; Zhang, Tianyou; Ito, Yoichiro

    2012-01-01

    Coupled with evaporative light scattering detection, a high-speed counter-current chromatography (HSCCC) method was developed for preparative isolation and purification of three glycine-conjugated cholic acids, glycochenodeoxycholic acid (GCDCA), glycohyodeoxycholic acid (GHDCA) and glycohyocholic acid (GHCA) from Pulvis Fellis Suis (Pig gallbladder bile) for the first time. The separation was performed with a two-phase solvent system consisted of chloroform-methanol-water-acetic acid (65:30:10:1.5, v/v/v/v) by eluting the lower phase in the head-to-tail elution mode. The revolution speed of the separation column, flow rate of the mobile phase and separation temperature were 800 rpm, 2 ml/min and 25 °C, respectively. In a single operation, 33 mg of GCDCA, 38 mg of GHDCA and 23 mg of GHCA were obtained from 200 mg of crude extract with the purity of 95.65%, 96.72% and 96.63%, respectively, in one step separation. The HSCCC fractions were analyzed by high-performance liquid chromatography (HPLC) and the structures of the three glycine-conjugated cholic acids were identified by ESI-MS, (1)H NMR and (13)C NMR.

  20. Location of silicic caldera formation in arc settings

    Energy Technology Data Exchange (ETDEWEB)

    Hughes, Gwyneth R; Mahood, Gail A [Department of Geological and Environmental Sciences, Stanford University, 450 Serra, Mall, Building 320, Stanford, CA 94305-2115 (United States)

    2008-10-01

    Silicic calderas are the surface expressions of silicic magma chambers, and thus their study may yield information about what tectonic and crustal features favor the generation of evolved magma. The goal of this study is to determine whether silicic calderas in arc settings are preferentially located behind the volcanic front. After a global analysis of young, arc-related calderas, we find that silicic calderas at continental margins do form over a wide area behind the front, as compared to other types of arc volcanoes.

  1. Analysis of perfluorinated carboxylic acids in soils II: optimization of chromatography and extraction.

    Science.gov (United States)

    Washington, John W; Henderson, W Matthew; Ellington, J Jackson; Jenkins, Thomas M; Evans, John J

    2008-02-15

    With the objective of detecting and quantitating low concentrations of perfluorinated carboxylic acids (PFCAs), including perfluorooctanoic acid (PFOA), in soils, we compared the analytical suitability of liquid chromatography columns containing three different stationary phases, two different liquid chromatography-tandem mass spectrometry (LC/MS/MS) systems, and eight combinations of sample-extract pretreatments, extractions and cleanups on three test soils. For the columns and systems we tested, we achieved the greatest analytical sensitivity for PFCAs using a column with a C(18) stationary phase in a Waters LC/MS/MS. In this system we achieved an instrument detection limit for PFOA of 270 ag/microL, equating to about 14 fg of PFOA on-column. While an elementary acetonitrile/water extraction of soils recovers PFCAs effectively, natural soil organic matter also dissolved in the extracts commonly imparts significant noise that appears as broad, multi-nodal, asymmetric peaks that coelute with several PFCAs. The intensity and elution profile of this noise is highly variable among soils and it challenges detection of low concentrations of PFCAs by decreasing the signal-to-noise contrast. In an effort to decrease this background noise, we investigated several methods of pretreatment, extraction and cleanup, in a variety of combinations, that used alkaline and unbuffered water, acetonitrile, tetrabutylammonium hydrogen sulfate, methyl-tert-butyl ether, dispersed activated carbon and solid-phase extraction. For the combined objectives of complete recovery and minimization of background noise, we have chosen: (1) alkaline pretreatment; (2) extraction with acetonitrile/water; (3) evaporation to dryness; (4) reconstitution with tetrabutylammonium-hydrogen-sulfate ion-pairing solution; (5) ion-pair extraction to methyl-tert-butyl ether; (6) evaporation to dryness; (7) reconstitution with 60/40 acetonitrile/water (v/v); and (8) analysis by LC/MS/MS. Using this method, we

  2. New Silica Magnetite Sorbent: The Influence of Variations of Sodium Silicate Concentrations on Silica Magnetite Character

    Science.gov (United States)

    Azmiyawati, C.; Pratiwi, P. I.; Darmawan, A.

    2018-04-01

    The adsorption capacity of an adsorbent is determined by the adsorbent and the adsorbate properties. The character of the adsorbent will play a major role in its ability to adsorb the corresponding adsorbate. Therefore, in this study we looked at the effects of variations of sodium silicate concentrations on the resulting magnetite silica adsorbent properties. The application of silica coating on the magnetite was carried out through a sol-gel process with sodium silicate and HCl precursors. Based on the characterization data obtained, it was found that the silica coating on magnetite can increase the resistance to acid leaching, increase the particle size, but decrease the magnetic properties of the magnetite. Based on Gas Sorption Analyzer (GSA) and X-ray Difraction (XRD) data it can successively be determined that increase in concentration of sodium silicate will increase the surface area and amorphous structure of the Silica Magnetie.

  3. Synthesis and crystal structures of a novel layered silicate SSA-1 and its microporous derivatives by topotactic transformation.

    Science.gov (United States)

    Takahashi, S; Kurita, Y; Ikeda, T; Miyamoto, M; Uemiya, S; Oumi, Y

    2016-10-18

    The synthesis of a novel layered silicate SSA-1 (SSA: silicate synthesized with a quaternary amine) was achieved in the SiO 2 -H 2 O-TEAOH (TEAOH: tetraethylammonium hydroxide - as an organic structural directing agent) system. The crystal structure of SSA-1 involved two silicate layers composed of bre [10T]-type CBU (Composite Building Unit) and TEAOH in interlayers. The topotactic transformation of SSA-1 by calcination was examined, resulting in a porous material (PML-1: porous material transformed from a layered silicate) with a 108 m 2 g -1 BET surface area and 0.035 cm 3 g -1 pore volume. PML-1 is a siliceous microporous material with silanols in the framework and possesses unique properties, such as hydrophilicity, in spite of all its silica composition. The most reasonable crystal structure of PML-1 was successfully determined on the basis of the crystal structure of SSA-1 by a combination of manual modelling, PXRD pattern simulation, DFT optimization and Rietveld analysis. Additionally, an interlayer expanded siliceous zeolite SSA-1 (IEZ-SSA-1) was also successfully prepared by silylation using trichloro(methyl)silane under acidic conditions. IEZ-SSA-1 showed hydrophilicity or hydrophobicity properties by changing the functional group of the pillar part in the interlayer. Additionally, IEZ-SSA-1 showed a large gas adsorption property (537 m 2 g -1 and 0.21 cm 3 g -1 ).

  4. TiO2 on magnesium silicate monolith: effects of different preparation techniques on the photocatalytic oxidation of chlorinated hydrocarbons

    International Nuclear Information System (INIS)

    Cardona, Ana I.; Candal, Roberto; Sanchez, Benigno; Avila, Pedro; Rebollar, Moises

    2004-01-01

    In this article, the comparative results of the photocatalytic oxidation of trichloroethylene (TCE) alone and a mixture of chlorinated hydrocarbons (trichloroethylene, perchloroethylene and chloroform) in gas phase, obtained with three different monolithic catalysts in a flat reactor frontally illuminated with a Xenon lamp are presented. The three catalysts incorporate titanium dioxide (TiO 2 ) as active phase on a magnesium silicate support, by means of different procedures: (i) incorporation of commercial TiO 2 powder into the silicate matrix ('massic monolith'); (ii) sol-gel coating of the silicate support; (iii) impregnation with a commercial TiO 2 aqueous suspension of the same silicate support. In the first case, the massic monolith was made from a 50:50 w/w mixture of magnesium silicate and 'Titafrance G5' TiO 2 powder. In the second case, a magnesium silicate monolith was coated with several layers of an aqueous TiO 2 sol prepared from hydrolysis and condensation of titanium tetra-isopropoxide (Ti(OC 3 H 7 ) 4 ) in excess of acidified water (acid catalysis). The third catalyst was prepared by impregnating the same silicate support with several layers of 'Titafrance G5' TiO 2 powder water suspension. All the catalysts were thermal treated under comparable conditions in order to fix the TiO 2 active phase to the silicate support. Although the performance of the massic monolith was better than the sol-gel monolith, the latter is of great interest because this technique allows the chemical composition of the active films to be easily modified

  5. Investigation of the presence of β-hydroxy-β-methylbutyric acid and α-hydroxyisocaproic acid in bovine whole milk and fermented dairy products by a validated liquid chromatography-mass spectrometry method.

    Science.gov (United States)

    Ehling, Stefan; Reddy, Todime M

    2014-02-19

    A simple, rugged, quantitative, and confirmatory method based on liquid chromatography-mass spectrometry was developed and comprehensively validated for the analysis of the leucine metabolites β-hydroxy-β-methylbutyric acid (HMB) and α-hydroxyisocaproic acid (HICA) in bovine whole milk and yogurt. Mean accuracy (90-110% for HMB and 85-115% for HICA) and total precision (dairy products with HMB and/or HICA appears to be justified.

  6. Preparation of [13C3]-melamine and [13C3]-cyanuric acid and their application to the analysis of melamine and cyanuric acid in meat and pet food using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Varelis, P; Jeskelis, R

    2008-10-01

    For the determination of melamine and cyanuric acid the labelled internal standards [(13)C(3)]-melamine and [(13)C(3)]-cyanuric acid were synthesized using the common substrate [(13)C(3)]-cyanuric chloride by reaction with ammonia and acidified water, respectively. Standards with excellent isotopic and chemical purities were obtained in acceptable yields. These compounds were used to develop an isotope dilution liquid chromatography/mass spectrometry (LC/MS) method to determine melamine and cyanuric acid in catfish, pork, chicken, and pet food. The method involved extraction into aqueous methanol, liquid-liquid extraction and ion exchange solid phase clean-up, with normal phase high-performance liquid chromatography (HPLC) in the so-called hydrophilic interaction mode. The method had a limit of detection (LOD) of 10 microg kg(-1) for both melamine and cyanuric acid in the four foods with a percentage coefficient of variation (CV) of less than 10%. The recovery of the method at this level was in the range of 87-110% and 96-110% for melamine and cyanuric acid, respectively.

  7. [Determination of fatty acids in natural cream and artificial cream by comprehensive two-dimensional gas chromatography-mass spectrometry].

    Science.gov (United States)

    Zhou, Ruize; Zhou, Ya; Mao, Ting; Jiang, Jie

    2018-01-08

    A method for the determination of 37 fatty acids in natural cream and artificial cream was developed by comprehensive two-dimensional gas chromatography-mass spectrometry (GC×GC-MS). The samples were extracted with toluene and acetyl chloride-methanol (1:9,v/v) solution was added to the extract for fat esterification. Finally, the fatty acids were analyzed by GC×GC-MS. The GC conditions were as follows:a DB-5 column (30 m×0.25 mm×0.25 μm) was set as the 1st dimensional column and a BPX-50 column (2.5 m×0.1 mm×0.25 μm) was the 2nd dimensional column. The primary oven temperature was programmed from 50℃ (held for 2 min) to 180℃ at a rate of 20℃/min, followed by an increase to 250℃ at 2.5℃/min, then raised up to 300℃ (held for 5 min) at 3℃/min. The ion source temperature was 200℃ with auxiliary temperature of 300℃ in scan mode. All fatty acids were separated effectively and determined accurately while the modulation period was 5s and the scan range of MS was m/z 40-385. This procedure was applied to analyze the fatty acids in commercial natural cream and artificial cream from Chinese markets, among which we found the characteristic components in different kinds of samples. Compared with gas chromatography-flame ionization detector (GC-FID), GC×GC-MS method was more sensitive and more components of fatty acids were detected. Conclusively, this work suggests a new technical approach in analyzing fatty acids in natural cream and artificial cream, which is meaningful to ensure the quality identification and safety of natural cream.

  8. Osteoblast cell membrane chromatography coupled with liquid chromatography and time-of-flight mass spectrometry for screening specific active components from traditional Chinese medicines.

    Science.gov (United States)

    Wang, Nani; Zhang, Qiaoyan; Xin, Hailiang; Shou, Dan; Qin, Luping

    2017-11-01

    A method using osteoblast membrane chromatography coupled with liquid chromatography and time-of-flight mass spectrometry was developed to recognize and identify the specific active components from traditional Chinese medicines. Primary rat osteoblasts were used for the preparation of the stationary phase in the cell chromatography method. Retention components from the cell chromatography were collected and analyzed by liquid chromatography with time-of-flight mass spectrometry. This method was applied in screening active components from extracts of four traditional Chinese medicines. In total, 24 potentially active components with different structures were retained by osteoblast cell chromatography. There were five phenolic glucosides and one triterpenoid saponin from Curculigo orchioides Gaertn, two organic acids and ten flavonoids from Epimedium sagittatum Maxim, one phthalide compound and one organic acid from Angelica sinensis Diels, and two flavonoids and two saponins from Anemarrhena asphodeloides Bunge. Among those, four components (icariin, curculigoside, ferulaic acid, and timosaponin BII) were used for in vitro pharmacodynamics validation. They significantly increased the osteoblast proliferation, alkaline phosphatase activity, levels of bone gla protein and collagen type 1, and promoted mineralized nodule formation. The developed method was an effective screening method for finding active components from complex medicines that act on bone diseases. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Evaluation of cyclonic ash, commercial Na-silicates, lime and phosphoric acid for metal immobilisation purposes in contaminated soils in Flanders (Belgium)

    International Nuclear Information System (INIS)

    Geebelen, Wouter; Sappin-Didier, Valerie; Ruttens, Ann; Carleer, Robert; Yperman, Jan; Bongue-Boma, Kwele; Mench, Michel; Lelie, Niels van der; Vangronsveld, Jaco

    2006-01-01

    In order to reduce the health risks associated with historically enriched metal smelting sites in Flanders (Belgium), the capacities of a non-beringite cyclonic ash and commercial Na-silicates to fix metals and create conditions to restore vegetation cover were evaluated and compared to lime and H 3 PO 4 . All tested amendments reduced Ca(NO 3 ) 2 -extractable soil metal concentrations and reduced metal uptake in Agrostis capillaris seedlings. Sodium released by Na-silicates was possibly toxic to bean plants while an isotopic dilution technique revealed that metals were only weakly sorbed by silicates (i.e. reversible sorption). Cyclonic ash appeared more efficient than lime in both reducing oxidative stress in beans and Zn, Cu and Pb uptake in grasses. The metal fixing mechanism for both amendments appeared similar (i.e. irreversible fixation at constant pH), in contrast to H 3 PO 4 where at least part of the immobilised Cd was irreversibly fixed across a range of pH. - Metal immobilising capacities of Na-silicates are weak, while the active mechanism of cyclonic ash is the same as lime

  10. Peak broadening in paper chromatography and related techniques : III. Peak broadening in thin-layer chromatography on cellulose powder

    NARCIS (Netherlands)

    Ligny, C.L. de; Remijnse, A.G.

    1968-01-01

    The mechanism of peak broadening in thin-layer chromatography on cellulose powder was investigated by comparing the peak widths obtained in chromatography with those caused only by diffusion in the cellulose powder, for a set of amino acids of widely differing RF values and six kinds of cellulose

  11. Use of chelating agents as immovable phase in extraction chromatography

    International Nuclear Information System (INIS)

    Sebesta, F.

    1978-01-01

    Extraction chromatography using chelating agents is reviewed. The theory of element extraction by chelating agents and factors influencing this process (pH, extracting agent concentration in organic phase, masking agent concentration in aqueous phase) are briefly considered. The effect of kinetic factors on the extraction chromatography process is discussed. Ways of preparing columns are emphasized. Examples of using chelating reagents in various extraction chromatography systems are given. β-Diketones, oximes, hydroxamic acids, dithizon, diethyl dithiocarbamic acid are chosen as chelating agents

  12. Application of perfluorinated acids as ion-pairing reagents for reversed-phase chromatography and retention-hydrophobicity relationships studies of selected beta-blockers.

    Science.gov (United States)

    Flieger, J

    2010-01-22

    The addition of the homologous series of perfluorinated acids-trifluoroacetic acid (TFAA), pentafluoropropionic acid (PFPA), heptafluorobutyric acid (HFBA) to mobile phases for reversed-phase high-performance liquid chromatography (RP-HPLC) of beta-blockers was tested. Acidic modifiers were responsible for acidification of mobile phase (pH 3) ensuring the protonation of the beta-blockers and further ion pairs creation. The effect of the type and concentration of mobile phase additives on retention parameters, the efficiency of the peaks, their symmetry and separation selectivity of the beta-blockers mixture were all studied. It appeared that at increasing acid concentration, the retention factor, for all compounds investigated, increased to varying degrees. It should be stressed that the presence of acids more significantly affected the retention of the most hydrophobic beta-blockers. Differences in hydrophobicity of drugs can be maximized through variation of the hydrophobicity of additives. Thus, the relative increase in the retention depends on either concentration and hydrophobicity of the anionic mobile phase additive or hydrophobicity of analytes. According to QSRR (quantitative structure retention relationship) methodology, chromatographic lipophilicity parameters: isocratic log k and log k(w) values (extrapolated retention to pure water) were correlated with the molecular (log P(o/w)) and apparent (log P(app)) octanol-water partition coefficients obtained experimentally by countercurrent chromatography (CCC) or predicted by Pallas software. The obtained, satisfactory retention-hydrophobicity correlations indicate that, in the case of the basic drugs examined in RP-HPLC systems modified with perfluorinated acids, the retention is mainly governed by their hydrophobicity. Copyright 2009 Elsevier B.V. All rights reserved.

  13. Determination of long-chain fatty acids in serum by gas chromatography coupled to mass spectrometry

    International Nuclear Information System (INIS)

    Nuevas Paz, Lauro; Camayd Viera, Ivette

    2014-01-01

    The quantification of long-chain fatty acids is fundamental for the diagnosis of several peroxisome disorders, particularly those in which the β-oxidation peroxisome of fatty acids is affected. In this work the implementation of an analytical method for the determination of these markers in serum by gas chromatography coupled to mass spectrometry is described. Besides, samples from patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome were analyzed. The necessary experimental conditions were achieved for the separation and quantification of C22:0, C24:0 and C26:0 fatty acids in serum, which are biochemical markers of various peroxisome diseases. The application of this method allowed confirming the diagnosis of three patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome. The application of the method in daily practice will allow the Cuban medical system to count on a new laboratory parameter for the diagnosis of peroxisome disorders

  14. Simultaneous determination of amino acids and carbohydrates in culture media of Clostridium thermocellum by valve-switching ion chromatography.

    Science.gov (United States)

    Fa, Yun; Yang, Haiyan; Ji, Chengshuai; Cui, He; Zhu, Xinshu; Du, Juan; Gao, Jun

    2013-10-10

    An improved method for the simultaneous determination of 20 amino acids and 7 carbohydrates using one-valve switching after injection, ion chromatography, and integrated pulsed amperometric detection is proposed. The resolution of the amino acids and carbohydrates in the cation trap column was investigated. In addition, parameters including flow liquid type, flow rate, concentration, and valve-switch timing were optimized. The method is time-saving, effective, and accurate for the simultaneous separation of amino acids and carbohydrates, with a mean correlation coefficient of >0.99 and repeatability of 0.5-4.6% for eight replicates. The method was successfully applied in the analysis of amino acids and carbohydrates in aseptic media and in extracellular culture media of three phenotypes of Clostridium thermocellum. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Monolithic columns based on a poly(styrene-divinylbenzene-methacrylic acid) copolymer for capillary liquid chromatography of small organic molecules

    Czech Academy of Sciences Publication Activity Database

    Svobodová, A.; Křížek, T.; Širc, Jakub; Šálek, Petr; Tesařová, E.; Coufal, P.; Štulík, K.

    2011-01-01

    Roč. 1218, č. 11 (2011), s. 1544-1547 ISSN 0021-9673 R&D Projects: GA AV ČR KAN200520804 Institutional research plan: CEZ:AV0Z40500505 Keywords : capillary liquid chromatography * methacrylic acid * polystyrene-based monolithic stationary phase Subject RIV: EI - Biotechnology ; Bionics Impact factor: 4.531, year: 2011

  16. On crystallochemistry of uranil silicates

    International Nuclear Information System (INIS)

    Sidorenko, G.A.; Moroz, I.Kh.; Zhil'tsova, I.G.

    1975-01-01

    A crystallochemical analysis has been made of uranil silicates. It is shown that on crystallochemical grounds it is justified to distinguish among them uranophane-kasolite, soddyite and viksite groups differing in the uranil-anion [SiO 4 ] -4 ratio and, as a consequence, in their crystallochemical structures. Widespread silicates of the uranophane-kasolite group is the formation of polytype modifications where, depending on the interlaminar cation, crystalline structures are formed with various packing of single-type uranil-anion layers. It has been shown experimentally that silicates of the uranophanekasolite group contain no oxonium ion in their crystalline structures. Minerals of the viksite group belong to a group of isostructural (homeotypic) laminated formation apt to form phases of different degrees of hydration. Phases with a smaller interlaminar cation form hydrates with a greater number of water molecules in the formulas unit

  17. Changes in monosaccharides, organic acids and amino acids during Cabernet Sauvignon wine ageing based on a simultaneous analysis using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Zhang, Xin-Ke; Lan, Yi-Bin; Zhu, Bao-Qing; Xiang, Xiao-Feng; Duan, Chang-Qing; Shi, Ying

    2018-01-01

    Monosaccharides, organic acids and amino acids are the important flavour-related components in wines. The aim of this article is to develop and validate a method that could simultaneously analyse these compounds in wine based on silylation derivatisation and gas chromatography-mass spectrometry (GC-MS), and apply this method to the investigation of the changes of these compounds and speculate upon their related influences on Cabernet Sauvignon wine flavour during wine ageing. This work presented a new approach for wine analysis and provided more information concerning red wine ageing. This method could simultaneously quantitatively analyse 2 monosaccharides, 8 organic acids and 13 amino acids in wine. A validation experiment showed good linearity, sensitivity, reproducibility and recovery. Multiple derivatives of five amino acids have been found but their effects on quantitative analysis were negligible, except for methionine. The evolution pattern of each category was different, and we speculated that the corresponding mechanisms involving microorganism activities, physical interactions and chemical reactions had a great correlation with red wine flavours during ageing. Simultaneously quantitative analysis of monosaccharides, organic acids and amino acids in wine was feasible and reliable and this method has extensive application prospects. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  18. Rapid and Precise Measurement of Serum Branched-Chain and Aromatic Amino Acids by Isotope Dilution Liquid Chromatography Tandem Mass Spectrometry

    OpenAIRE

    Yang, Ruiyue; Dong, Jun; Guo, Hanbang; Li, Hongxia; Wang, Shu; Zhao, Haijian; Zhou, Weiyan; Yu, Songlin; Wang, Mo; Chen, Wenxiang

    2013-01-01

    BACKGROUND: Serum branched-chain and aromatic amino acids (BCAAs and AAAs) have emerged as predictors for the future development of diabetes and may aid in diabetes risk assessment. However, the current methods for the analysis of such amino acids in biological samples are time consuming. METHODS: An isotope dilution liquid chromatography tandem mass spectrometry (ID-LC/MS/MS) method for serum BCAAs and AAAs was developed. The serum was mixed with isotope-labeled BCAA and AAA internal standar...

  19. Gas chromatography of alkylphosphonic and dialkyl phosphinic acids; Cromatografia en fase gaseosa de acidos alquifosfonicos y dialquilfosinicos

    Energy Technology Data Exchange (ETDEWEB)

    Gasco Sanchez, L; Barrera Peniero, R; Ramirez Caceres, A; Marin Munoz, M

    1978-07-01

    After carrying out an optimization study on the separation conditions for the TMSr- derivatives, of the hexyl-, cyclohexyl-, heptyl-, and octyl-phosphonic acids; dihexyl dicyclohexyl-, heptyl-, and octyl-phosphinic acids, and dioctyl phosphine oxide, their retention indices (I) at two temperatures and on the OV-1 and OV-17 stationary phase were determined. Correlations between I and molecular structure were established. Calibration factors of these compounds in the flame ionization detector were studied, and the results analyzed taking into account the variables affecting the quantitative results, These results were unbiased but they had a lower precision than that usually achievable in gas chromatography. (Author) 24 refs.

  20. Biosynthetic Studies of the Male Marking Pheromone in Bumblebees by Using Labelled Fatty Acids and Two-Dimensional Gas Chromatography with Mass Detection

    Czech Academy of Sciences Publication Activity Database

    Žáček, Petr; Kindl, Jiří; Frišonsová, K.; Průchová, Markéta; Votavová, A.; Hovorka, Oldřich; Kovalczuk, T.; Valterová, Irena

    2015-01-01

    Roč. 80, č. 5 (2015), s. 839-850 ISSN 2192-6506 Institutional support: RVO:61388963 Keywords : biosynthesis * bumblebees * fatty acids * gas chromatography * pheromones Subject RIV: CC - Organic Chemistry Impact factor: 2.836, year: 2015

  1. Thermogravimetric analysis of phase transitions in cement compositions mixed by sodium silicate solution

    Directory of Open Access Journals (Sweden)

    Fedosov Sergey Viktorovich

    2014-01-01

    Full Text Available This paper presents a study of the capability to modify cement by mechanical activation of sodium silicate water solution. Admixtures or blends of binding agents were employed for modifying concrete properties. The liquid glass is applied to protect from chemically or physically unfavorable environmental impacts, such as acidic medium and high temperature. The sodium silicate is a high-capacity setting accelerator. The increasing of the liquid glass proportion in the mix leads to the degradation of the cement paste plasticity and for this reason it is necessary to reduce the amount of liquid glass in the cement paste. The activation of dilute water solution of sodium silicate into rotary pulsating apparatus directly before tempering of the cement paste is an effective way to decrease mass fraction of liquid glass in the cement paste. The results of the combined influence of liquid glass and mechanical activation on physicochemical processes taking place in cement stone are represented in this research. Thermogravimetric analysis was used in order to study cement blends. Thermogravimetric analysis of modified cement stone assays was performed by thermo analyzer SETARAM TGA 92-24. The results of the analysis of phase transition taking place under high-temperature heating of cement stone modified by the mechanical activation of the water solution of the sodium silicate were introduced. Thermograms of cement stone assays were obtained at different hardening age. The comparison of these thermograms allows us to come to a conclusion on the formation and the retention during long time of a more dense structure of the composite matrix mixed by the mechanical activation of sodium silicate water solution. The relation between the concrete composition and its strength properties was stated. Perhaps, the capability of modified concrete to keep calcium ions in sparingly soluble hydrosilicates leads to the increase in its durability and corrosion resistance.

  2. Algerian mint species:high performance thin layer chromatography quantitative determination of rosmarinic acid and in vitro inhibitory effects on linoleic acid peroxidation

    Institute of Scientific and Technical Information of China (English)

    Brahmi Fatiha; Madani Khodir; Stvigny Caroline; Chibane Mohamed; Duez Pierre

    2014-01-01

    Objective: To determine the quantitative paremeters of rosmarinic acid in Algerian mints,Mentha spicata L. (M. spicata), Mentha pulegium L. and Mentha rotundifolia (L.) Huds by high performance thin layer chromatography (HPTLC)-densitometric method and screen the effects of these plant extracts on linoleic acid peroxidation.Methods:The analyses were performed on HPTLC silica gel 60 F254 plates with chloroform:acetone: formic acid (75:16.5:8.5, v/v) as the mobile phase. Rosmarinic acid was determined in UV at 365 nm and fluorescence at λexc 325 nm with a 550 nm filter, respectively. The effects of plants extracts on linoleic acid peroxidation were measured by an indirect in vitro colorimetric method.Results:Chromatographic resolution permitted reliable quantification in both measurement modes and calibration curves were linear in a range of 150-1000 ng/spot. M. spicata was found to contain significantly higher concentrations of rosmarinic acid. The densitometric quantification allowed the analysis of many samples in a short time with reasonable precision (total precision for Mentha spp extracts, 5.1% and 5.8% for UV and fluorescence detection, respectively). The HPTLC data, allied to assays of linoleic acid peroxidation prevention, suggested the potential of M. spicata (52% Trolox®equivalents) as a natural source for inhibitors of lipid peroxidation.Conclusions:Densitometry can be used for routine determination and quality control of rosmarinic acid in herbal and formulations containing Mentha species.

  3. Algerian mint species: high performance thin layer chromatography quantitative determination of rosmarinic acid and in vitro inhibitory effects on linoleic acid peroxidation

    Directory of Open Access Journals (Sweden)

    Brahmi Fatiha

    2014-12-01

    Full Text Available Objective: To determine the quantitative paremeters of rosmarinic acid in Algerian mints, Mentha spicata L. (M. spicata, Mentha pulegium L. and Mentha rotundifolia (L. Huds by high performance thin layer chromatography (HPTLC-densitometric method and screen the effects of these plant extracts on linoleic acid peroxidation. Methods: The analyses were performed on HPTLC silica gel 60 F254 plates with chloroform: acetone: formic acid (75:16.5:8.5, v/v as the mobile phase. Rosmarinic acid was determined in UV at 365 nm and fluorescence at λexc 325 nm with a 550 nm filter, respectively. The effects of plants extracts on linoleic acid peroxidation were measured by an indirect in vitro colorimetric method. Results: Chromatographic resolution permitted reliable quantification in both measurement modes and calibration curves were linear in a range of 150-1 000 ng/spot. M. spicata was found to contain significantly higher concentrations of rosmarinic acid. The densitometric quantification allowed the analysis of many samples in a short time with reasonable precision (total precision for Mentha spp extracts, 5.1% and 5.8% for UV and fluorescence detection, respectively. The HPTLC data, allied to assays of linoleic acid peroxidation prevention, suggested the potential of M. spicata (52% Trolox® equivalents as a natural source for inhibitors of lipid peroxidation. Conclusions: Densitometry can be used for routine determination and quality control of rosmarinic acid in herbal and formulations containing Mentha species.

  4. Radiochemical separation of {sup 231}Pa from siliceous cake prior to its determination by gamma ray spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dalvi, Aditi A. [Bhabha Atomic Research Centre, Mumbai (India). Analytical Chemistry Div.; Homi Bhabha National Institute, Mumbai (India); Verma, Rakesh

    2017-07-01

    A simple and fast radiochemical method for the separation of protactinium ({sup 231}Pa) from siliceous cake for its determination by gamma ray spectrometry is described. The method involves (a) a novel approach, the fusion of the siliceous cake with sodium peroxide, (b) the dissolution of the fused mass in nitric acid and (c) the co-precipitation of {sup 231}Pa with manganese dioxide formed in-situ by the addition of solid manganous sulfate and potassium permanganate to the solution. The fusion, effected in a single step, is simpler and highly effective in comparison to methods reported hitherto in literature. The radiochemical yield of {sup 231}Pa, determined using 311.9 keV gamma ray of {sup 233}Pa radiotracer is quantitative (∝90%). The decontamination factors calculated using gamma ray spectrometry and energy dispersive X-ray fluorescence measurements show that the separation from the interfering radionuclides is high whereas separation from major and minor elements is good. Separation by ion-exchange method in hydrochloric acid, hydrofluoric acid and oxalic acid media have comparatively much lower yields. The concentration of {sup 231}Pa in the siliceous cake measured using interference-free 283.6 keV gamma ray was found to be (6.4 ± 0.33) μg kg{sup -1}. The measured concentration of {sup 231}Pa was well above the limit of quantitation whereas the coefficient of variation was ∝5%. The improvement in the limit of detection was due to the reduction in spectral background. Systematic evaluation of various uncertainty parameters showed that the major contributors to the combined uncertainty were efficiency of the high purity germanium detector and the counting statistics. The present sample decomposition and separation methods are robust, simple to perform and can be effectively used for the determination and hence source prospecting of protactinium.

  5. Effect of silicate module of water glass on rheological parameters of poly(sodium acrylate)/sodium silicate hydrogels

    Science.gov (United States)

    Mastalska-Popiawska, J.; Izak, P.

    2017-01-01

    The poly(sodium acrylate)/sodium silicate hydrogels were synthesized in the presence of sodium thiosulphate and potassium persulphate as the redox initiators and N,N’-methylene-bisacrylamide as the cross-linking monomer. 20 wt% aqueous solution of sodium acrylate was polymerized together with water glass with different silicate modules (M) from 1.74 to 2.29, in three mass ratio of the monomer solution to the water glass 2:1, 1:1 and 1:2. Such obtained hybrid composites were rheologically tested using the oscillation method. It allowed to designate the crossover point during polymerization, as well as to define the viscoelastic properties of the casted hydrogel samples one week after the reaction. The obtained results of the oscillation measurements showed that cross-linking reaction proceeds very quickly and the lower the silicate module is, the process starts faster. After the completion of the reaction the silicate-polymer hydrogels are strongly elastic materials and the highest elasticity characterizes systems with the mass ratio 1:2, i.e. with the highest water glass content.

  6. 40 CFR 721.9513 - Modified magnesium silicate polymer (generic).

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Modified magnesium silicate polymer... Specific Chemical Substances § 721.9513 Modified magnesium silicate polymer (generic). (a) Chemical... as modified magnesium silicate polymer (PMN P-98-604) is subject to reporting under this section for...

  7. The composition of bile acids in patients with cholelithiasis according to the data of liquid chromatography with mass spectrometric detection

    Directory of Open Access Journals (Sweden)

    V. M. Klymenko

    2017-12-01

    Full Text Available Bile acids play a leading role in the physical and colloidal properties of bile stabilization. Lack of bile acids consequences result in the formation of cholesterol stones in the gall bladder, diarrhea and steatorrhea, fat-soluble vitamins impaired absorption, and kidney stones formation (oxalates. Investigation of altered bile composition, especially the content of bile acids, in patients with gallstone disease by means of modern analytical analysis methods (liquid chromatography with mass spectrometric detection would complement the modern ideas about mechanisms of lithogenesis and aim efforts at prevention of stone formation in the gall bladder, that was the purpose of our work. Materials and methods. Bile samples were tested for bile acid content using liquid chromatography with mass spectrometry. 14 samples of bile from patients with cholelithiasis were included in the main group, and control group consisted of 7 bile samples from practically healthy persons. Results. In patients with cholelithiasis there is an increase in the content of conjugated forms of bile acids – glycolic acid in 2 times (p = 0.002, taurocholic acid in 1.57 times (p = 0.062 compared with practically healthy persons. In patients with cholelithiasis, the ratio of taurocholic to glycolic acidі content (0.95 vs. 1.27, p = 0.0179, as well as glycogenodeoxycholic to glycodeoxycholic acid (1.11 vs. 1.58, p = 0.027 is significantly less than that in practically healthy persons. In addition, one in two patients with cholelithiasis does not reveal the presence of ursodeoxycholic acid in the bile. Conclusions. The lithogenic properties of bile are primarily caused by conjugated forms of cholic acid with glycine and taurine content violation. The ratio of taurocholic to glycolic acid content in patients with cholelithiasis is significantly lower than the similar index in practically healthy persons (0.95 vs. 1.27, p = 0.0179. The ratio of glycine conjugated bile acids

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

    Science.gov (United States)

    Darwin; WipaCharles; Cord-Ruwisch, Ralf

    2018-01-01

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

  9. Characterization of the fermentation process by gas chromatography Lasiodiplodia theobromae and gas chromatography coupled with mass spectrometry

    International Nuclear Information System (INIS)

    Castillo Portela, Grolamys; Eng Sanchez, Felipe; Nogueiras Lima, Clara

    2014-01-01

    Lasiodiplodia theobromae is a fungus, which has been reported by some authors as a high yield producer of the phytohormone jasmonic acid (JA). An indigenous strain of this fungus has been used for producing a fermentation broth with a high JA concentration by the Cuban Research Institute for Sugar Cane Derivatives (ICIDCA), registered as BIOJAS. The broth has been applied to some agricultural crops and demonstrated its economic feasibility as plant growth regulator and biological control of various phytopathogenic microorganisms and pests. Both fermentation broth and biomass from this fungus contain some other metabolites having bioactive properties, for instance, fatty acids. This paper shows the composition and quantification of fatty acids in the biomass using Gas Chromatography (GC) and the identification of substances profile in fermentation broth by Gas Chromatography coupled to Mass Spectrometry (GC-MS). The most fatty acids in the biomass are palmitic, stearic, oleic, linoleic and linolenic acids, being oleic acid the major component. On the other hand, 2,32 % of fatty acid esters; 2,47 % of alkenes; 14,40 % of alcohols; 30,15 % of aldehydes and 21,73 % of paraffins were detected in the composition of fermentation broth

  10. Lattice thermal conductivity of silicate glasses at high pressures

    Science.gov (United States)

    Chang, Y. Y.; Hsieh, W. P.

    2016-12-01

    Knowledge of the thermodynamic and transport properties of magma holds the key to understanding the thermal evolution and chemical differentiation of Earth. The discovery of the remnant of a deep magma ocean above the core mantle boundary (CMB) from seismic observations suggest that the CMB heat flux would strongly depend on the thermal conductivity, including lattice (klat) and radiative (krad) components, of dense silicate melts and major constituent minerals around the region. Recent measurements on the krad of dense silicate glasses and lower-mantle minerals show that krad of dense silicate glasses could be significantly smaller than krad of the surrounding solid mantle phases, and therefore the dense silicate melts would act as a thermal insulator in deep lower mantle. This conclusion, however, remains uncertain due to the lack of direct measurements on the lattice thermal conductivity of silicate melts under relevant pressure-temperature conditions. Besides the CMB, magmas exist in different circumstances beneath the surface of the Earth. Chemical compositions of silicate melts vary with geological and geodynamic settings of the melts and have strong influences on their thermal properties. In order to have a better view of heat transport within the Earth, it is important to study compositional and pressure dependences of thermal properties of silicate melts. Here we report experimental results on lattice thermal conductivities of silicate glasses with basaltic and rhyolitic compositions up to Earth's lower mantle pressures using time-domain thermoreflectance coupled with diamond-anvil cell techniques. This study not only provides new data for the thermal conductivity of silicate melts in the Earth's deep interior, but is crucial for further understanding of the evolution of Earth's complex internal structure.

  11. High Pressure/Temperature Metal Silicate Partitioning of Tungsten

    Science.gov (United States)

    Shofner, G. A.; Danielson, L.; Righter, K.; Campbell, A. J.

    2010-01-01

    The behavior of chemical elements during metal/silicate segregation and their resulting distribution in Earth's mantle and core provide insight into core formation processes. Experimental determination of partition coefficients allows calculations of element distributions that can be compared to accepted values of element abundances in the silicate (mantle) and metallic (core) portions of the Earth. Tungsten (W) is a moderately siderophile element and thus preferentially partitions into metal versus silicate under many planetary conditions. The partitioning behavior has been shown to vary with temperature, silicate composition, oxygen fugacity, and pressure. Most of the previous work on W partitioning has been conducted at 1-bar conditions or at relatively low pressures, i.e. pressure. Predictions based on extrapolation of existing data and parameterizations suggest an increased pressured dependence on metal/ silicate partitioning of W at higher pressures 5. However, the dependence on pressure is not as well constrained as T, fO2, and silicate composition. This poses a problem because proposed equilibration pressures for core formation range from 27 to 50 GPa, falling well outside the experimental range, therefore requiring exptrapolation of a parametereized model. Higher pressure data are needed to improve our understanding of W partitioning at these more extreme conditions.

  12. Separation of transition-metal and 8-hydroxyquinoline-5-sulfonic acid complexes using ion-pair liquid chromatography

    International Nuclear Information System (INIS)

    Basova, E.M.; Demurov, L.M.; Shpigun, O.A.; Van Iyuchun'

    1994-01-01

    The retention of chelates of Fe(3), Cu(2), Co(2), Ni(2), Zn(2), Cd(2), Hg(2), and Pb)(2) with 8-hydroxyquinoline-5-sulfonic acid depending on the concentration of cetyltrimethylammonium bromide, acetonitrile, and pH of the mobile phase was investigated using the ion-pair reversed-phase high-performance liquid chromatography on separon C 18 . Under the optimum conditions, the separation of mixtures of Fe(3), Co(2) and Ni(2) is performed within 8 to 12 min

  13. Glutamic acid and folic acid production in aerobic and anaerobic probiotics

    Directory of Open Access Journals (Sweden)

    Zohre Taghi Abadi

    2018-03-01

    Full Text Available Introduction:From an industrial application or commercial point of view, glutamic acid is one of the most important amino acids and its microbial production has been reported from some bacteria. Regarding the role of probiotics to modulate human health and the ever-increasing demand of prebiotics in the food industry, in the current study, production of glutamic acid and folic acid from three probiotic bacteria (Bifidobacterium, Bifidobacterium bifidum, Sporolactobacillus was evaluated for the first time. Materials and methods: MRS broth and exclusive media was used for probiotic culture. The glutamic acid was identified using thin-layer chromatography and folic acid production was measured by folate kit. Each bacterium in terms of quality and quantity were measured by high pressure liquid chromatography. Results: Production of glutamic acid confirmed is based on the thin layer chromatography analysis and high pressure liquid chromatography results. In addition, it was observed that all three probiotics produce folic acid. The prevalence of folate in Bifidobacterium was measured as 315 mg/ml that was more than two other bacteria. Discussion and conclusion: To the best of our knowledge, this is the first report of microbial production of glutamic acid and folate from the probiotic bacteria. These beneficial bacteria can be used as a good source for mass production of these valuable compounds.

  14. Validation of ascorbic acid tablets of national production by igh-performance liquid chromatography method

    International Nuclear Information System (INIS)

    Rodriguez Hernandez, Yaslenis; Suarez Perez, Yania; Izquierdo Castro, Idalberto

    2009-01-01

    We validate an analytical method by high-performance liquid chromatography to determine ascorbic acid proportion in vitamin C tablets, which was designed as an alternative method to quality control and to follow-up of active principle chemical stability, since official techniques to quality control of ascorbic acid in tablets are not selective with degradation products. Method was modified according to that reported in USP 28, 2005 for analysis of injectable product. We used a RP-18 column of 250 x 4.6 mm 5 μm with a UV detector to 245 nm. Its validation was necessary for both objectives, considering parameters required for methods of I and II categories. This method was enough linear, exact, and precise in the rank of 100-300 μg/mL. Also, it was selective with remaining components of matrix and with the possible degradation products achieved in stressing conditions. Detection and quantification limits were estimated. When method was validated it was applied to ascorbic acid quantification in two batches of expired tablets and we detected a marked influence of container in active degradation principle after 12 months at room temperature. (Author)

  15. Suppressive effects of a polymer sodium silicate solution on ...

    African Journals Online (AJOL)

    Sodium silicate was dissolved in water in either a monomer form or polymer form; the effects of both forms of sodium silicate aqueous solution on rose powdery mildew and root rot diseases of miniature rose were examined. Both forms of sodium silicate aqueous solution were applied to the roots of the miniature rose.

  16. TiO{sub 2} on magnesium silicate monolith: effects of different preparation techniques on the photocatalytic oxidation of chlorinated hydrocarbons

    Energy Technology Data Exchange (ETDEWEB)

    Cardona, Ana I.; Candal, Roberto; Sanchez, Benigno; Avila, Pedro; Rebollar, Moises

    2004-05-01

    In this article, the comparative results of the photocatalytic oxidation of trichloroethylene (TCE) alone and a mixture of chlorinated hydrocarbons (trichloroethylene, perchloroethylene and chloroform) in gas phase, obtained with three different monolithic catalysts in a flat reactor frontally illuminated with a Xenon lamp are presented. The three catalysts incorporate titanium dioxide (TiO{sub 2}) as active phase on a magnesium silicate support, by means of different procedures: (i) incorporation of commercial TiO{sub 2} powder into the silicate matrix ('massic monolith'); (ii) sol-gel coating of the silicate support; (iii) impregnation with a commercial TiO{sub 2} aqueous suspension of the same silicate support. In the first case, the massic monolith was made from a 50:50 w/w mixture of magnesium silicate and 'Titafrance G5' TiO{sub 2} powder. In the second case, a magnesium silicate monolith was coated with several layers of an aqueous TiO{sub 2} sol prepared from hydrolysis and condensation of titanium tetra-isopropoxide (Ti(OC{sub 3}H{sub 7}){sub 4}) in excess of acidified water (acid catalysis). The third catalyst was prepared by impregnating the same silicate support with several layers of 'Titafrance G5' TiO{sub 2} powder water suspension. All the catalysts were thermal treated under comparable conditions in order to fix the TiO{sub 2} active phase to the silicate support. Although the performance of the massic monolith was better than the sol-gel monolith, the latter is of great interest because this technique allows the chemical composition of the active films to be easily modified.

  17. Spectral properties of porphyrins in the systems with layered silicates

    International Nuclear Information System (INIS)

    Ceklovsky, A.

    2009-03-01

    This work is focused on investigation of hybrid materials based on layered silicates, representing host inorganic component, and porphyrin dyes as organic guest. Aqueous colloidal dispersions, as well as thin solid films of layered silicate/porphyrin systems were studied. Modification of photophysical properties, such as absorption and fluorescence of molecules, adsorbed or incorporated in layered silicate hosts, were studied mainly to spread the knowledge about the environments suitable for incorporating aromatic compounds, providing photoactive properties of potential technological interest. TMPyP cations interact with the surfaces of layered silicates via electrostatic interactions. The extent of dye adsorption on colloidal particles of the silicates is influenced by the CEC values and swelling ability of silicates. Interaction of porphyrins with layered silicate hosts leads to significant changes of dye spectral properties. One of the key parameters that has a crucial impact on this interaction is the layer charge of silicate template. Other factors influence the resulting spectral properties of hybrid systems, such as the method of hybrid material preparation, the material's type (colloid, film), and the modification of the silicate host. Molecular orientation studies using linearly-polarized spectroscopies in VIS and IR regions revealed that TMPyP molecules were oriented in almost parallel fashion with respect to the silicate surface plane. Slightly higher values of the orientation angle of TMPyP transition moment were observed for the TMPyP/FHT system. Thus, flattening of the guest TMPyP molecules is the next important factor (mainly in the systems with lower layer charge), influencing its spectral properties upon the interaction with layered silicates. Fluorescence was effectively quenched in the systems based on solid films prepared from the high concentration of the dye (10-3 mol.dm-3). The quenching is most probably related to the structure of the

  18. Determination of trace elements in acid rain by reversed phase extraction chromatography and neutron activation

    International Nuclear Information System (INIS)

    Rao, R.R.; Goski, D.G.; Chatt, A.

    1991-01-01

    A preconcentration neutron activation analysis (PNAA) method has been developed for the simultaneous determination of selected trace elements in acid rain and other water samples. The method consists of preconcentration of the elements by reversed phase extraction chromatography using oxine-loaded Amberlite XAD-2 resin. Nearly 100% recoveries were obtained for Co, Cu, Hg, V and Zn at pH 6.0 and for Cd at pH 7.0. Manganese gave incomplete recoveries at the pH range of 4.0-8.0 studies. Various factors that can influence preconcentration of the elements have been investigated in detail. The precision and accuracy of measurements have been evaluated by analyzing certified reference materials. The detection limits have been found to be of the order of ppb. The PNAA method has been applied to a number of acid rain and other water samples

  19. [Determination of residual solvents in 7-amino-3-chloro cephalosporanic acid by gas chromatography].

    Science.gov (United States)

    Ma, Li; Yao, Tong-wei

    2011-01-01

    To develop a gas chromatography method for determination of residual solvents in 7-amino-3-chloro cephalosporanic acid (7-ACCA). The residual levels of acetone, methanol, dichloromethane, ethyl acetate, isobutanol, pyridine and toluene in 7-ACCA were measured by gas chromatography using Agilent INNOWAX capillary column (30 m × 0.32 mm,0.5 μm). The initial column temperature was 70° maintained for 6 min and then raised (10°C/min) to 160°C for 1 min. Nitrogen gas was used as carrier and FID as detector. The flow of carrier was 1.0 ml/min, the temperature of injection port and detector was 200°C and 250°C, respectively. The limits of detection for acetone, methanol, dichloromethane, ethyl acetate, isobutanol, pyridine, toluene in 7-ACCA were 2.5 μg/ml, 1.5 μg/ml, 15 μg/ml, 2.5 μg/ml, 2.5 μg/ml, 2.5 μg/ml and 11 μg/ml, respectively. Only acetone was detected in the sample, and was less than the limits of Ch.P. The method can effectively detect the residual solvents in 7-ACCA.

  20. The kinetic fragility of natural silicate melts

    International Nuclear Information System (INIS)

    Giordano, Daniele; Dingwell, Donald B

    2003-01-01

    Newtonian viscosities of 19 multicomponent natural and synthetic silicate liquids, with variable contents of SiO 2 (41-79 wt%), Al 2 O 3 (10-19 wt%), TiO 2 (0-3 wt%), FeO tot (0-11 wt%); alkali oxides (5-17 wt%), alkaline-earth oxides (0-35 wt%), and minor oxides, obtained at ambient pressure using the high-temperature concentric cylinder, the low-temperature micropenetration, and the parallel plates techniques, have been analysed. For each silicate liquid, regression of the experimentally determined viscosities using the well known Vogel-Fulcher-Tammann (VFT) equation allowed the viscosity of all these silicates to be accurately described. The results of these fits, which provide the basis for the subsequent analysis here, permit qualitative and quantitative correlations to be made between the VFT adjustable parameters (A VFT , B VFT , and T 0 ). The values of B VFT and T 0 , calibrated via the VFT equation, are highly correlated. Kinetic fragility appears to be correlated with the number of non-bridging oxygens per tetrahedrally coordinated cation (NBO/T). This is taken to infer that melt polymerization controls melt fragility in liquid silicates. Thus NBO/T might form an useful ingredient of a structure-based model of non-Arrhenian viscosity in multicomponent silicate melts

  1. Synthesis of non-siliceous mesoporous oxides.

    Science.gov (United States)

    Gu, Dong; Schüth, Ferdi

    2014-01-07

    Mesoporous non-siliceous oxides have attracted great interest due to their unique properties and potential applications. Since the discovery of mesoporous silicates in 1990s, organic-inorganic assembly processes by using surfactants or block copolymers as soft templates have been considered as a feasible path for creating mesopores in metal oxides. However, the harsh sol-gel conditions and low thermal stabilities have limited the expansion of this method to various metal oxide species. Nanocasting, using ordered mesoporous silica or carbon as a hard template, has provided possibilities for preparing novel mesoporous materials with new structures, compositions and high thermal stabilities. This review concerns the synthesis, composition, and parameter control of mesoporous non-siliceous oxides. Four synthesis routes, i.e. soft-templating (surfactants or block copolymers as templates), hard-templating (mesoporous silicas or carbons as sacrificial templates), colloidal crystal templating (3-D ordered colloidal particles as a template), and super lattice routes, are summarized in this review. Mesoporous metal oxides with different compositions have different properties. Non-siliceous mesoporous oxides are comprehensively described, including a discussion of constituting elements, synthesis, and structures. General aspects concerning pore size control, atomic scale crystallinity, and phase control are also reviewed.

  2. Rapid Determination of Bile Acids in Bile from Various Mammals by Reversed-Phase Ultra-Fast Liquid Chromatography.

    Science.gov (United States)

    Si, Gu Leng Ri; Yao, Peng; Shi, Luwen

    2015-08-01

    A valid and efficient reversed-phase ultra-fast liquid chromatography method was developed for the simultaneous determination of 13 bile acids in the bile of three mammal species, including rat, pig and human gallstone patients. Chromatographic separation was performed with a Shim-pack XR-ODS column, and the mobile phase consisted of acetonitrile and potassium phosphate buffer (pH 2.6) at a flow rate of 0.5 mL min(-1). The linear detection range of most bile acids ranged from 2 to 600 ng µL(-1) with a good correlation coefficient (>0.9995). The precision of each bile acid was bile acids were separated in 15 min with satisfactory resolution, and the total analysis time was 18 min, including equilibration. The method was successfully applied in rapid screening of bile samples from the three mammals. Significant metabolic frameworks of bile acids among various species were observed, whereas considerable quantitative variations in both inter- and intraspecies were also observed, especially for gallstone patients. Our results suggest that detecting the change of bile acid profiles could be applied for the diagnosis of gallstone disease. © Crown copyright 2014.

  3. Formic acid hydrolysis/liquid chromatography isotope dilution mass spectrometry: An accurate method for large DNA quantification.

    Science.gov (United States)

    Shibayama, Sachie; Fujii, Shin-Ichiro; Inagaki, Kazumi; Yamazaki, Taichi; Takatsu, Akiko

    2016-10-14

    Liquid chromatography-isotope dilution mass spectrometry (LC-IDMS) with formic acid hydrolysis was established for the accurate quantification of λDNA. The over-decomposition of nucleobases in formic acid hydrolysis was restricted by optimizing the reaction temperature and the reaction time, and accurately corrected by using deoxynucleotides (dNMPs) and isotope-labeled dNMPs as the calibrator and the internal standard, respectively. The present method could quantify λDNA with an expanded uncertainty of 4.6% using 10fmol of λDNA. The analytical results obtained with the present method were validated by comparing with the results of phosphate-base quantification by inductively coupled plasma-mass spectrometry (ICP-MS). The results showed good agreement with each other. We conclude that the formic acid hydrolysis/LC-IDMS method can quantify λDNA accurately and is promising as the primary method for the certification of DNA as reference material. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Determination of total tin in silicate rocks by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Elsheimer, H.N.; Fries, T.L.

    1990-01-01

    A method is described for the determination of total tin in silicate rocks utilizing a graphite furnace atomic absorption spectrometer with a stabilized-temperature platform furnace and Zeeman-effect background correction. The sample is decomposed by lithium metaborate fusion (3 + 1) in graphite crucibles with the melt being dissolved in 7.5% hydrochloric acid. Tin extractions (4 + 1 or 8 + 1) are executed on portions of the acid solutions using a 4% solution of tricotylphosphine oxide in methyl isobutyl ketone (MIBK). Ascorbic acid is added as a reducing agent prior to extraction. A solution of diammonium hydrogenphosphate and magnesium nitrate is used as a matrix modifier in the graphite furnace determination. The limit of detection is > 10 pg, equivalent to > 1 ??g l-1 of tin in the MIBK solution or 0.2-0.3 ??g g-61 in the rock. The concentration range is linear between 2.5 and 500 ??g l-1 tin in solution. The precision, measured as relative standard deviation, is < 20% at the 2.5 ??g l-1 level and < 7% at the 10-30 ??g l-1 level of tin. Excellent agreement with recommended literature values was found when the method was applied to the international silicate rock standards BCR-1, PCC-1, GSP-1, AGV-1, STM-1, JGb-1 and Mica-Fe. Application was made to the determination of tin in geological core samples with total tin concentrations of the order of 1 ??g g-1 or less.

  5. Serum markers in alkaptonuria: simultaneous analysis of homogentisic acid, tyrosine and nitisinone by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Hughes, Andrew T; Milan, Anna M; Davison, Andrew S; Christensen, Peter; Ross, Gordon; Gallagher, James A; Dutton, John J; Ranganath, Lakshminarayan R

    2015-09-01

    Alkaptonuria is a rare debilitating autosomal recessive disorder of tyrosine metabolism, where deficiency of homogentisate 1,2-dioxygenase results in increased homogentisic acid. Homogentisic acid is deposited as an ochronotic pigment in connective tissues, especially cartilage, leading to a severe early onset form of osteoarthritis, increased renal and prostatic stone formation and hardening of heart vessels. Treatment with the orphan drug, nitisinone, an inhibitor of 4-hydroxyphenylpyruvate dioxygenase has been shown to reduce urinary excretion of homogentisic acid. A reverse phase liquid chromatography tandem mass spectrometry method has been developed to simultaneously analyse serum homogentisic acid, tyrosine and nitisinone. Using matrix-matched calibration standards, two product ion transitions were identified for each compound (homogentisic acid, tyrosine, nitisinone) and their respective isotopically labelled internal standards ((13)C6-homogentisic acid, d2-tyrosine, (13)C6-nitisinone). Intrabatch accuracy was 94-108% for homogentisic acid, 95-109% for tyrosine and 89-106% for nitisinone; interbatch accuracy (n = 20) was 88-108% for homogentisic acid, 91-104% for tyrosine and 88-103% for nitisinone. Precision, both intra- and interbatch were alkaptonuria patients, pre- and post-nitisinone therapy. © The Author(s) 2015.

  6. Determination of aminopolycarboxylic acids at ultra-trace levels by means of online coupling ion exchange chromatography and inductively coupled plasma-mass spectrometry with indirect detection via their Pd2+-complexes

    International Nuclear Information System (INIS)

    Nette, David; Seubert, Andreas

    2015-01-01

    Highlights: • 8 important APCA’s analyzed in one run instead of 3 in the previous method. • Pd 2+ extents the methods applicability to 3 and more dentate amino carboxylic acids. • Separation system optimized for the isocratic determination of important APCA’s. • Thermodynamic stability of APCA–Pd 2+ complexes is higher than for Fe 3+ and In 3+ . • Pd 2+ is kinetically much slower than Fe 3+ and In 3+ and makes the method more rugged. - Abstract: A new indirect IC-ICP-MS method for the determination of aminopolycarboxylic acids in water samples is described. It is based on the addition of an excess of Pd(II) to water samples. The analytes are forced into very strong and negatively charged palladium complexes, separated by ion exchange chromatography and detected by their palladium content, utilizing an on-line coupled ICP-MS. This method is suitable to determine the concentration of 8 aminopolycarboxylic acids (nitrilotriacetic acid (NTA), (2-carboxyethyl) iminodiacetic acid (β-ADA), methylglycinediacetic acid (MGDA), 2-hydroxyethyl) ethylenediamine triacetic acid (HEDTA), diethylene triamine pentaacetic acid (DTPA), ethylendiamine tetraacetic acid (EDTA), 1,3-diaminopropane tetraacetic acid (1,3-PDTA) and 1,2-diaminopropane tetraacetic acid (1,2-PDTA) at the ng kg −1 level. The method is faster and easier than the established gas chromatography (GC)-method ISO 16588:2002 [1] and up to two orders of magnitude more sensitive than the ion pair chromatography based method of DIN 38413-8. Analytic performance is superior to ISO 16588:2002 and the comparability is good

  7. Ion exclusion chromatography for the purification of L-glutamine; Ion haijo chromatography ni yoru L-glutamine no seiseiho no kenkyu

    Energy Technology Data Exchange (ETDEWEB)

    Ito, H.; Nishi, A.; Naruse, M. [Ajinomoto Co. Inc., Kawasaki (Japan)

    1998-09-05

    Ion exclusion chromatography for the purification of L-glutamine is studied. L-glutamine is usually produced by fermentation and used in pharmaceuticals. By using a model solution of L-glutamine and L-glutamic acid, the optimum cation exchange resin is examined. As a result of the experiments, it is found that a cation exchange resin which has smaller crosslinkage and smaller diameter is better. Ammonium sulfate, L-glutamic acid and pyrrolidonecarboxylic acid, which are usually contained in fermentation broth as impurities, are effectively separated by this method. Moreover, the experimental data of the chromatography is expressed fairly well by the differential equations which express the mass transfer in the fixed bed. 8 refs., 5 figs., 2 tabs.

  8. Impacts of Steel-Slag-Based Silicate Fertilizer on Soil Acidity and Silicon Availability and Metals-Immobilization in a Paddy Soil.

    Directory of Open Access Journals (Sweden)

    Dongfeng Ning

    Full Text Available Slag-based silicate fertilizer has been widely used to improve soil silicon- availability and crop productivity. A consecutive early rice-late rice rotation experiment was conducted to test the impacts of steel slag on soil pH, silicon availability, rice growth and metals-immobilization in paddy soil. Our results show that application of slag at a rate above higher or equal to 1 600 mg plant-available SiO2 per kg soil increased soil pH, dry weight of rice straw and grain, plant-available Si concentration and Si concentration in rice shoots compared with the control treatment. No significant accumulation of total cadmium (Cd and lead (Pb was noted in soil; rather, the exchangeable fraction of Cd significantly decreased. The cadmium concentrations in rice grains decreased significantly compared with the control treatment. In conclusion, application of steel slag reduced soil acidity, increased plant-availability of silicon, promoted rice growth and inhibited Cd transport to rice grain in the soil-plant system.

  9. [Gas chromatography in quantitative analysis of hydrocyanic acid and its salts in cadaveric blood].

    Science.gov (United States)

    Iablochkin, V D

    2003-01-01

    A direct gas chromatography method was designed for the quantitative determination of cyanides (prussic acid) in cadaveric blood. Its sensitivity is 0.05 mg/ml. The routine volatile products, including substances, which emerge due to putrefaction of organic matters, do not affect the accuracy and reproducibility of the method; the exception is H-propanol that was used as the internal standard. The method was used in legal chemical expertise related with acute cyanide poisoning (suicide) as well as with poisoning of products of combustion of nonmetals (foam-rubber). The absolute error does not exceed 10% with a mean quadratic deviation of 0.0029-0.0033 mg.

  10. Qualitative and Quantitative Analysis of Volatile Components of Zhengtian Pills Using Gas Chromatography Mass Spectrometry and Ultra-High Performance Liquid Chromatography.

    Science.gov (United States)

    Liu, Cui-Ting; Zhang, Min; Yan, Ping; Liu, Hai-Chan; Liu, Xing-Yun; Zhan, Ruo-Ting

    2016-01-01

    Zhengtian pills (ZTPs) are traditional Chinese medicine (TCM) which have been commonly used to treat headaches. Volatile components of ZTPs extracted by ethyl acetate with an ultrasonic method were analyzed by gas chromatography mass spectrometry (GC-MS). Twenty-two components were identified, accounting for 78.884% of the total components of volatile oil. The three main volatile components including protocatechuic acid, ferulic acid, and ligustilide were simultaneously determined using ultra-high performance liquid chromatography coupled with diode array detection (UHPLC-DAD). Baseline separation was achieved on an XB-C18 column with linear gradient elution of methanol-0.2% acetic acid aqueous solution. The UHPLC-DAD method provided good linearity (R (2) ≥ 0.9992), precision (RSD components, protocatechuic acid, ferulic acid, and ligustilide, in 13 batches of ZTPs, which is suitable for discrimination and quality assessment of ZTPs.

  11. Multiplexed microfluidic approach for nucleic acid enrichment

    Science.gov (United States)

    VanderNoot, Victoria A.; Langevin, Stanley Alan; Bent, Zachary; Renzi, Ronald F.; Ferko, Scott M.; Van De Vreugde, James L.; Lane, Todd; Patel, Kamlesh; Branda, Steven

    2016-04-26

    A system for enhancing a nucleic acid sample may include a one pump, a denaturing chamber; a microfluidic hydroxyapatite chromatography device configured for performing hydroxyapatite chromatography on the nucleic acid sample, a sample collector, and tubing connecting the pump with the denaturing chamber, the hydroxyapatite chromatography device and the sample collector such that the pump may be used to move the nucleic acid sample from the denaturing chamber to the hydroxyapatite chromatography device and then to the sample collector.

  12. Analysis of naphthenic acid mixtures as pentafluorobenzyl derivatives by gas chromatography-electron impact mass spectrometry.

    Science.gov (United States)

    Gutierrez-Villagomez, Juan Manuel; Vázquez-Martínez, Juan; Ramírez-Chávez, Enrique; Molina-Torres, Jorge; Trudeau, Vance L

    2017-01-01

    In this study, we report for the first time the efficiency of pentafluorobenzyl bromide (PFBBr) for naphthenic acid (NA) mixtures derivatization, and the comparison in the optimal conditions to the most common NAs derivatization reagents, BF 3 /MeOH and N-(t-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA). Naphthenic acids are carboxylic acid mixtures of petrochemical origin. These compounds are important for the oil industry because of their corrosive properties, which can damage oil distillation infrastructure. Moreover, NAs are commercially used in a wide range of products such as paint and ink driers, wood and fabric preservatives, fuel additives, emulsifiers, and surfactants. Naphthenic acids have also been found in sediments after major oils spills in the United States and South Korea. Furthermore, the toxicity of the oil sands process-affected water (OSPW), product of the oil sands extraction activities in Canada's oil sands, has largely been attributed to NAs. One of the main challenges for the chromatographic analysis of these mixtures is the resolution of the components. The derivatization optimization was achieved using surface response analysis with molar ratio and time as factors for derivatization signal yield. After gas chromatography-electron impact mass spectrometry (GC/EIMS) analysis of a mixture of NA standards, it was found that the signal produced by PFB-derivatives was 2.3 and 1.4 times higher than the signal produced by methylated and MTBS-derivatives, respectively. The pentafluorobenzyl derivatives have a characteristic fragment ion at 181m/z that is diagnostic for the differentiation of carboxylic and non-carboxylic acid components within mixtures. In the analysis of a Sigma and a Merichem derivatized oil extract NA mixtures, it was found that some peaks lack the characteristic fragment ion; therefore they are not carboxylic acids. Open column chromatography was used to obtain a hexane and a methanol fraction of the Sigma and

  13. Comparison of silicon nanoparticles and silicate treatments in fenugreek.

    Science.gov (United States)

    Nazaralian, Sanam; Majd, Ahmad; Irian, Saeed; Najafi, Farzaneh; Ghahremaninejad, Farrokh; Landberg, Tommy; Greger, Maria

    2017-06-01

    Silicon (Si) fertilization improves crop cultivation and is commonly added in the form of soluble silicates. However, most natural plant-available Si originates from plant formed amorphous SiO 2 particles, phytoliths, similar to SiO 2 -nanoparticles (SiNP). In this work we, therefore, compared the effect by sodium silicate and that of SiNP on Si accumulation, activity of antioxidative stress enzymes catalase, peroxidase, superoxide dismutase, lignification of xylem cell walls and activity of phenylalanine ammonia-lyase (PAL) as well as expression of genes for the putative silicon transporter (PST), defensive (Tfgd 1) and phosphoenolpyruvate carboxykinase (PEPCK) and protein in fenugreek (Trigonella foenum-graecum L.) grown in hydroponics. The results showed that Si was taken up from both silicate and SiNP treatments and increasing sodium silicate addition increased the translocation of Si to the shoot, while this was not shown with increasing SiNP addition. The silicon transporter PST was upregulated at a greater level when sodium silicate was added compared with SiNP addition. There were no differences in effects between sodium silicate and SiNP treatments on the other parameters measured. Both treatments increased the uptake and accumulation of Si, xylem cell wall lignification, cell wall thickness, PAL activity and protein concentration in seedlings, while there was no effect on antioxidative enzyme activity. Tfgd 1 expression was strongly downregulated in leaves at Si addition. The similarity in effects by silicate and SiNP would be due to that SiNP releases silicate, which may be taken up, shown by a decrease in SiNP particle size with time in the medium. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

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

    Science.gov (United States)

    Arning, Erland; Bottiglieri, Teodoro

    2016-01-01

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

  15. Hierarchical CaCO3 chromatography: a stationary phase based on biominerals.

    Science.gov (United States)

    Sato, Kosuke; Oaki, Yuya; Takahashi, Daisuke; Toshima, Kazunobu; Imai, Hiroaki

    2015-03-23

    In biomineralization, acidic macromolecules play important roles for the growth control of crystals through a specific interaction. Inspired by this interaction, we report on an application of the hierarchical structures in CaCO3 biominerals to a stationary phase of chromatography. The separation and purification of acidic small organic molecules are achieved by thin-layer chromatography and flash chromatography using the powder of biominerals as the stationary phase. The unit nanocrystals and their oriented assembly, the hierarchical structure, are suitable for the adsorption site of the target organic molecules and the flow path of the elution solvents, respectively. The separation mode is ascribed to the specific adsorption of the acidic molecules on the crystal face and the coordination of the functional groups to the calcium ions. The results imply that a new family of stationary phase of chromatography can be developed by the fine tuning of hierarchical structures in CaCO3 materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Silicate enamel for alloyed steel

    International Nuclear Information System (INIS)

    Ket'ko, K.K.

    1976-01-01

    The use of silicate enamels in the metallurgical industry is discussed. Presented are the composition and the physico-chemical properties of the silicate enamel developed at the factory 'Krasnyj Oktyabr'. This enamel can be used in the working conditions both in the liquid and the solid state. In so doing the enamel is melted at 1250 to 1300 deg C, granulated and then reduced to a fraction of 0.3 to 0.5 mm. The greatest homogeneity is afforded by a granulated enamel. The trials have shown that the conversion of the test ingots melted under a layer of enamel leads to the smaller number of the ingots rejected for surface defect reasons and the lower metal consumption for slab cleaning. The cost of the silicate enamel is somewhat higher than that of synthetic slags but its application to the melting of stainless steels is still economically beneficial and technologically reasonable. Preliminary calculations only for steel EhI4IEh have revealed that the use of this enamel saves annually over 360000 roubles [ru

  17. Study on analysis of waste edible oil with deterioration and removal of acid value, carbonyl value, and free fatty acid by a food additive (calcium silicate).

    Science.gov (United States)

    Ogata, Fumihiko; Tanaka, Yuko; Tominaga, Hisato; Kangawa, Moe; Inoue, Kenji; Ueda, Ayaka; Iwata, Yuka; Kawasaki, Naohito

    2013-01-01

    This study investigated the regeneration of waste edible oil using a food additive (calcium silicate, CAS). Waste edible oil was prepared by combined heat and aeration treatment. Moreover, the deterioration of edible oil by combined heat and aeration treatment was greater than that by heat treatment alone. The acid value (AV) and carbonyl value (CV) increased with increasing deterioration; conversely, the tocopherol concentration decreased with increasing deterioration. The specific surface area, pore volume, and mean pore diameter of the 3 CAS formulations used (CAS30, CAS60, and CAS90) were evaluated, and scanning electron microscopic images were taken. The specific surface area increased in the order of CAS30 (115.54 m(2)/g) edible oil was possible with CAS treatment. The AV reduced by 15.2%, 10.8%, and 23.1% by CAS30, CAS60, and CAS90 treatment, respectively, and the CV was reduced by 35.6%, 29.8%, and 31.3% by these 3 treatments, respectively. Moreover, the concentrations of tocopherol and free fatty acids did not change with CAS treatment. The characteristics of CAS were not related to the degree of change of AV and CV. However, the adsorption mechanism of polar and non-polar compounds generated in waste edible oil by CAS was related with the presence of silica gel molecules in CAS. The findings indicated that CAS was useful for the regeneration of waste edible oil.

  18. Capillary gas chromatographic analysis of mycolic acid cleavage products, cellular fatty acids, and alcohols of Mycobacterium xenopi.

    OpenAIRE

    Luquin, M; Lopez, F; Ausina, V

    1989-01-01

    The fatty acids, alcohols, and mycolic acids of 26 strains of Mycobacterium xenopi were studied by capillary gas chromatography and thin-layer chromatography. All strains contained alpha-, keto-, and omega-carboxymycolates. The primary mycolic acid cleavage product was hexacosanoic acid. The fatty acid patterns and, especially, the presence of 2-docosanol are characteristic markers of M. xenopi.

  19. Analysis of the fatty acid composition of taraxicuum officinale flowers oil by gas chromatography mass spectrometer

    International Nuclear Information System (INIS)

    Hussain, I.; Ullah, R.

    2013-01-01

    Taraxicum officinale, is a highly valuable medicinal plant. The roots is an important herbal drug, having long been used on the continent as a remedy for liver complaints. Keeping in view the importance and wide applications in the pharmaceutical industries, the present study was therefore aimed to analyze the chemical constituents of the flowers of T. officinale. The T. officinale flowers oil constituents of methyl ester derivatives of fatty acids were analyzed applying gas chromatography coupled to mass spectrometer. The results obtained showed the presence of both containing the saturated as well as unsaturated fatty acids in T. officinale flower oils. A total of 19 different components were identified and quantified. The concentration level of Methyl ester of Lenolenic acid was found very effective in concentration 3.33%, among the identified analytes of interest. In addition, the level of other chemical constituents of methyl ester of palmitic acid 3.11%, myristic acid 1.87, linolenic acids 1.67%, stearic acid 0.97 were found. The concentration level of the rest of identified fatty acids analytes were below 1%. Thus the results obtained from the current initiative is very promising due to the presence of high percentage of valuable analytes concentrations recorded in the fatty acid of T. officinale flower oil. Thus due to the presence of highly important analytes which have increased their importance for consumption in the pharmaceuticals as well as its applications in the new formulations for different skin, cosmetics and health purposes and for use by local practioners. The study will also provide a scientific database line. (author)

  20. Preparation and utilization of amorphous siliceous materials from serpentine (Mg3Si2O5(OH)4) by acid treatment; Jamonseki no kofuka kachika ni kansuru kenkyu

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1997-01-30

    Concerning the conversion of serpentine, not only its magnesium component but also silica component, into industrial materials, conditions suitable for the production of porous materials and amorphous silica by acid treatment were evaluated, and the properties of the products were evaluated. The silica resulting from the acid treatment of serpentine comes out in different forms, each reflecting the structure of the parent rock, that is, an amorphous mass of planar particles from antigorite and a fascicular mass of filaments from chrysotile. A microporic structure resulted when a small quantity of magnesium was allowed to remain in the skeleton structure and acid treatment conditions were properly adjusted. Several siliceous compounds were prepared for the purpose of finding use for silica from this rock, and then it was found that high-efficiency production of high-crystallinity compounds was possible and that they were furnished with properties fit for use as materials. Furthermore, study was made about the kaolinite reaction in which serpentine would be directly converted into useful materials. 105 refs., 55 figs., 6 tabs.

  1. Separation behavior of octadecadienoic acid isomers and identification of cis- and trans-isomers using gas chromatography.

    Science.gov (United States)

    Shibamoto, Shigeaki; Gooley, Andrew; Yamamoto, Kouhei

    2015-01-01

    Using a strongly polar cyanopropyl capillary column we have investigated the gas chromatography (GC) separation behaviors of 24 octadecadienoic acid methyl ester (18:2ME) isomers compared against saturated methyl stearate (18:0ME) and arachidic acid methyl ester (20:0ME), and the dependency on the GC column temperature. The 24 isomers were obtained by performing cis-to trans-isomerization of six regioisomers: five of the 18:2ME isomers were prepared by the partial reduction of methyl α-linolenate and methyl γ-linolenate C18 trienoic acids with different double bond positions, whereas the sixth isomer, 18:2ME (c5, c9), was obtained from a raw constituent fatty acid methyl ester (FAME) sample extracted from Japanese yew seeds. There are no reference standards commercially available for 18:2ME isomers, and in elucidating the elution order of these isomers this study should help the future identification of cis- and trans-type of 18:2ME. We also report the identification method of cis- and trans-type of FAME using equivalent chain lengths and attempt the identification of cis- and trans-type of 18:2ME isomers from partially hydrogenated canola oil.

  2. L-ascorbic acid losses in Kenyan vegetables during cooking as determined by high performance liquid chromatography

    OpenAIRE

    N.M.N. Wekesa; S.C. Chhabra; H.M. Thairu

    2001-01-01

    The loss of L-ascorbic acid (L-AA) in 14 different cooked local vegetables found in Nairobi markets was determined by high performance liquid chromatography. The effect of quantity of water on the loss of L-AA during cooking was studied with cowpea leaves. It was found that more L-AA was lost when larger amount of water was used than when smaller amount was used. The effect of the sharpness of the knife on the loss of L-AA was studied with spinach. It was found that more loss of L-AA occurred...

  3. Determination of gamma-aminobutyric acid in food matrices by isotope dilution hydrophilic interaction chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Zazzeroni, Raniero; Homan, Andrew; Thain, Emma

    2009-08-01

    The estimation of the dietary intake of gamma-aminobutyric acid (GABA) is dependent upon the knowledge of its concentration values in food matrices. To this end, an isotope dilution liquid chromatography-mass spectrometry method has been developed employing the hydrophilic interaction chromatography technique for analyte separation. This approach enabled accurate quantification of GABA in apple, potato, soybeans, and orange juice without the need of a pre- or post-column derivatization reaction. A selective and precise analytical measurement has been obtained with a triple quadrupole mass spectrometer operating in multiple reaction monitoring using the method of standard additions and GABA-d(6) as an internal standard. The concentrations of GABA found in the matrices tested are 7 microg/g of apple, 342 microg/g of potatoes, 211 microg/g of soybeans, and 344 microg/mL of orange juice.

  4. Determination of aristolochic acids by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Wang, Yinan; Chan, Wan

    2014-06-25

    Nephrotoxic and carcinogenic aristolochic acids (AAs) are naturally occurring nitrophenanthrene carboxylic acids in the herbal genus Aristolochia. The misuse of AA-containing herbs in preparing slimming drugs has caused hundred of cases of kidney disease in Belgium women in a slimming regime in the early 1990s. Accumulating evidence also suggested that prolong dietary intake of AA-contaminated food is one of the major causes to the Balkan endemic nephropathy that was first observed in the late 1950s. Therefore, analytical methods of high sensitivity are extremely important for safeguarding human exposure to AA-containing herbal medicines, herbal remedies, and food composites. In this paper, we describe the development of a new high-performance liquid chromatography coupled fluorescence detector (HPLC-FLD) method for the sensitive determination of AAs. The method makes use of a novel cysteine-induced denitration reaction that "turns on" the fluorescence of AAs for fluorometric detections. Our results showed that the combination of cysteine-induced denitration and HPLC-FLD analysis allows for sensitive quantification of AA-I and AA-II at detection limits of 27.1 and 25.4 ng/g, respectively. The method was validated and has been successfully applied in quantifying AAs in Chinese herbal medicines.

  5. OPTIMAL METHOD FOR PREPARATION OF SILICATE ROCK SAMPLES FOR ANALYTICAL PURPOSES

    Directory of Open Access Journals (Sweden)

    Maja Vrkljan

    2004-12-01

    Full Text Available The purpose of this study was to determine an optimal dissolution method for silicate rock samples for further analytical purposes. Analytical FAAS method of determining cobalt, chromium, copper, nickel, lead and zinc content in gabbro sample and geochemical standard AGV-1 has been applied for verification. Dissolution in mixtures of various inorganic acids has been tested, as well as Na2CO3 fusion technique. The results obtained by different methods have been compared and dissolution in the mixture of HNO3 + HF has been recommended as optimal.

  6. Chiral ligand exchange high-speed countercurrent chromatography: mechanism, application and comparison with conventional liquid chromatography in enantioseparation of aromatic α-hydroxyl acids

    Science.gov (United States)

    Tong, Shengqiang; Shen, Mangmang; Cheng, Dongping; Ito, Yoichiro; Yan, Jizhong

    2014-01-01

    This work concentrates on the separation mechanism and application of chiral ligand exchange high-speed countercurrent chromatography (HSCCC) in enantioseparations, and comparison with traditional chiral ligand exchange high performance liquid chromatography (HPLC). The enantioseparation of ten aromatic α-hydroxyl acids were performed by these two chromatographic methods. Results showed that five of the racemates were successfully enantioseparated by HSCCC while only three of the racemates could be enantioseparated by HPLC using a suitable chiral ligand mobile phase additive. For HSCCC, the two-phase solvent system was composed of butanol-water (1:1, v/v), to which N-n-dodecyl-L-proline was added in the organic phase as chiral ligand and cupric acetate was added in the aqueous phase as a transition metal ion. Various operation parameters in HSCCC were optimized by enantioselective liquid-liquid extraction. Based on the results of the present studies the separation mechanism for HSCCC was proposed. For HPLC, the optimized mobile phase composed of aqueous solution containing 6 mmol L−1 L-phenylalanine and 3 mmol L−1 cupric sulfate and methanol was used for enantioseparation. Among three ligands tested on a conventional reverse stationary phase column, only one was found to be effective. In the present studies HSCCC presented unique advantages due to its high versatility of two-phase solvent systems and it could be used as an alternative method for enantioseparations. PMID:25087742

  7. Heterogeneous nucleation of protein crystals on fluorinated layered silicate.

    Directory of Open Access Journals (Sweden)

    Keita Ino

    Full Text Available Here, we describe an improved system for protein crystallization based on heterogeneous nucleation using fluorinated layered silicate. In addition, we also investigated the mechanism of nucleation on the silicate surface. Crystallization of lysozyme using silicates with different chemical compositions indicated that fluorosilicates promoted nucleation whereas the silicates without fluorine did not. The use of synthesized saponites for lysozyme crystallization confirmed that the substitution of hydroxyl groups contained in the lamellae structure for fluorine atoms is responsible for the nucleation-inducing property of the nucleant. Crystallization of twelve proteins with a wide range of pI values revealed that the nucleation promoting effect of the saponites tended to increase with increased substitution rate. Furthermore, the saponite with the highest fluorine content promoted nucleation in all the test proteins regardless of their overall net charge. Adsorption experiments of proteins on the saponites confirmed that the density of adsorbed molecules increased according to the substitution rate, thereby explaining the heterogeneous nucleation on the silicate surface.

  8. Schinus terebinthifolius scale-up countercurrent chromatography (Part I): High performance countercurrent chromatography fractionation of triterpene acids with off-line detection using atmospheric pressure chemical ionization mass spectrometry.

    Science.gov (United States)

    Vieira, Mariana Neves; Costa, Fernanda das Neves; Leitão, Gilda Guimarães; Garrard, Ian; Hewitson, Peter; Ignatova, Svetlana; Winterhalter, Peter; Jerz, Gerold

    2015-04-10

    'Countercurrent chromatography' (CCC) is an ideal technique for the recovery, purification and isolation of bioactive natural products, due to the liquid nature of the stationary phase, process predictability and the possibility of scale-up from analytical to preparative scale. In this work, a method developed for the fractionation of Schinus terebinthifolius Raddi berries dichloromethane extract was thoroughly optimized to achieve maximal throughput with minimal solvent and time consumption per gram of processed crude extract, using analytical, semi-preparative and preparative 'high performance countercurrent chromatography' (HPCCC) instruments. The method using the biphasic solvent system composed of n-heptane-ethyl acetate-methanol-water (6:1:6:1, v/v/v/v) was volumetrically scaled up to increase sample throughput up to 120 times, while maintaining separation efficiency and time. As a fast and specific detection alternative, the fractions collected from the CCC-separations were injected to an 'atmospheric pressure chemical ionization mass-spectrometer' (APCI-MS/MS) and reconstituted molecular weight MS-chromatograms of the APCI-ionizable compounds from S. terebinthifolius were obtained. This procedure led to the direct isolation of tirucallane type triterpenes such as masticadienonic and 3β-masticadienolic acids. Also oleanonic and moronic acids have been identified for the first time in the species. In summary, this approach can be used for other CCC scale-up processes, enabling MS-target-guided isolation procedures. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Simultaneous determination of 18α-glycyrrhetinic acid and 18β-glycyrrhetinic acid in Glycyrrhiza glabra root by reversed phase high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Ambika Chamoli

    2016-01-01

    Full Text Available Background: The aim of the present research work is to develop a high-performance liquid chromatography (HPLC method for simultaneous analysis of 18α-glycyrrhetinic acid (18α-GA and 18β-GA (18β-GA of Glycyrrhiza glabra. Materials and Methods: About 20 μL aliquots of each 18α-GA and 18β-GA were analyzed using reversed-phase C-18 column. The mobile phase was acetonitrile:tetrahydrofuran:water (10:80:10, v/v/v. The run time was 10 min at flow rate of 1 ml/min. Ultraviolet detection was carried out at 254 nm. Results: 18α-GA and 18β-GA were well resolved in reversed phase C-18 column using mobile phase acetonitrile: tetrahydrofuran: water (10:80:10, v/v/v, pH 7.9. The Rtof 18α-GA and 18β-GA was detected at 2.091 and 2.377 min, respectively. Conclusion: The developed chromatography method could be extended for potential quantification or simultaneous determination of these markers in plant as well as in herbal formulation.

  10. Wind-eroded silicate as a source of hydrogen peroxide on Mars

    DEFF Research Database (Denmark)

    Bak, Ebbe Norskov; Merrison, Jonathan P.; Jensen, Svend Knak

    -sists of silicates [4] that due to wind erosion has a very fine grained texture. Based on the composition of the surface material and investigations showing that crushing of silicates can give rise to reactive oxygen species [5], we hypothesized that wind erosion of silicates can explain the reactivity of Martian...... soil. Wind-erosion of silicate could thus be one of several causes of the soil’s reactivity. As our experiments show, the globally distributed wind eroded silicate dust can lead to the production of hydrogen peroxide which might explain the reactivity of the Martian soil. The reactivity of eroded...

  11. Selective on-line detection of boronic acids and derivatives in high-performance liquid chromatography eluates by post-column reaction with alizarin

    NARCIS (Netherlands)

    Duval, F.L.; Wardani, P.A.; Zuilhof, H.; Beek, van T.A.

    2015-01-01

    An on-line high-performance liquid chromatography (HPLC) method for the rapid and selective detection of boronic acids in complex mixtures was developed. After optimization experiments at an HPLC flow rate of 0.40 mL/min, the HPLC-separated analytes were mixed post-column with a solution of 75 µM

  12. Identification and quantification of amino acids from psoriatic and normal epidermis by high performance liquid chromatography

    International Nuclear Information System (INIS)

    Mahesar, S.M.; Khuhawar, M.Y.

    2010-01-01

    In this study, a modified fluorescence technique high performance liquid chromatography (HPLC) was adapted to separate the amino acids from the hydrolyzed keratin samples. These samples obtained from the epidermal layer of the normal and psoriatic human subjects. The keratin extracts are quantified in gram percentage of the dried skin and the amino acids concentrations are measured in mu g/g, mean retention time (tR), slope value and the coefficient of determination (r2) of each eluted amino acid is calculated. The coefficients of variation for amino acid standards ranged from 0.12% to 0.28%, mean, standard deviation of peak area and coefficients of variation of peak area were calculated. From the normal hydrolysated keratin protein fraction, 12 amino acids were determined and identified as aspartic acid, glutamic acid, asparagines, serine, glutamine, glycine, histidine, citrulline, arganine, fi-alanine, tyrosine, and valine. These amino acids were also determined in psoriatic samples while standard deviations (SD), standard error mean (SEM) and coefficient variation (CV%) of normal and psoriatic samples were also calculated. The higher concentration of amino acids in normal samples against psoriatic samples determined as glutamic acid 92.76+- 16. 83/50. 87+-9.88, glutamine 198.05+-18.74/19.74+-3.74 while higher concentrations of amino acids determined in psoriatic samples against normal samples as asparagines 81. 06+-10+-10.62/29. 98+-3.641; arganine 164.42+-35. 11/46. 14+-46, tyrosine 214.38+-29. 61/59. 64+-8. 82, and valine 169.7+-19.35/128.06+-15.14.1 is concluded that the absolute concentration of amino acids in psoriatic skin indicated a number of variations as compared to normal skin samples. (author)

  13. Development and Validation of a Reversed-Phase Liquid Chromatography Method for the Simultaneous Determination of Indole-3-Acetic Acid, Indole-3-Pyruvic Acid, and Abscisic Acid in Barley (Hordeum vulgare L.).

    Science.gov (United States)

    Nakurte, Ilva; Keisa, Anete; Rostoks, Nils

    2012-01-01

    A simple, sensitive, precise, and specific reverse HPLC method was developed and validated for the determination of plant hormones in barley (Hordeum vulgare L.). The method includes extraction in aqueous organic solvent followed by solid-phase extraction, sample evaporation, and reversed-phase HPLC analysis in a general purpose UV-visible (abscisic acid (ABA)) and fluorescence detection (indole-3-acetic acid (IAA) and indole-3-pyruvic acid (IPA)), high-performance liquid chromatography system. The separation was carried out on Zorbax Eclipse XDB C8 column (150  ×  4.6  mm I.D) with a mobile phase composed of methanol and 1% acetic acid (60 : 40 v/v) in isocratic mode at a flow rate of 1 ml min(-1). The detection was monitored at 270 nm (ABA) and at 282 nm (Ex) and 360 nm (Em) (IAA, IPA). The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantification, and robustness. The determined validation parameters are in the commonly acceptable ranges for that kind of analysis.

  14. Determination of homovanillic acid and vanillylmandelic acid in urine of autistic children by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Kałuzna-Czaplińska, Joanna; Socha, Ewa; Rynkowski, Jacek

    2010-09-01

    Studies suggest dopamine nervous systems are involved in the pathogenesis of autistic disorder. Quantification of urinary homovanillic acid (HVA) and vanillylmandelic acid (VMA) can be a very important tool in the study of disorders of dopamine metabolism in autistic children. The urine specimens were collected from 20 autistic children and 36 neurologically normal children. Urinary HVA and VMA were simultaneously analyzed by gas chromatography-mass spectrometry. The method involves extraction of HVA and VMA from urinary samples and derivatization to N,O-bis(trimethylsilyl)trifluoroacetamide derivatives. The detection limits are 0.15 microg/mL and 0.23 microg/mL for VMA and HVA, respectively. The levels of HVA and VMA were higher in the urine of autistic children (28.8+/-15.5 micromol/mmol creatinine and 22.2+/-13.0 micromol/mmol creatinine, respectively) compared with those of the generally healthy children (4.6+/-0.7 micromol/mmol creatinine for HVA and 3.8+/-0.6 micromol/mmol creatinine for VMA). We proposed a simple, rapid method for a routine analysis of human urine to detect HVA and VMA related to an abnormal functional imbalance of the dopamine system, and showed our experience of application of this method to patients with a diagnosis of autism spectrum disorders. These results suggest significant differences in the levels of HVA and VMA between autistic and healthy children.

  15. Zirconia silicate modified with phytic acid (IP6) and its effect on uranyl sorption

    International Nuclear Information System (INIS)

    Escalante G, D. C.

    2016-01-01

    In this work the sorption capacity of uranyl ions on zirconium silicate (ZrSiO_4) extracted from sea sand of Baja California Sur was studied, the effect of phytic acid (IP6) accompanied by a perchlorate salt of sodium (NaClO_4) on the surface of the mineral. In the first stage, ZrSiO_4 was obtained from sea sand by extraction using hydrofluoric acid, the purified and hydrated material was later characterized by instrumental techniques such as X-ray diffraction to determine its purity and crystallinity. The ZrSiO_4-purified, ZrSiO_4/NaClO_4 and ZrSiO_4/IP6 were studied by physicochemical and surface characterization. By scanning electron microscopy was observed that ZrSiO_4 initially is formed by flat structures, however, when it is hydrated with NaClO_4 the formation of particles on the material exists, whereas when the IP6 is added the crystals on the surface are elongated forming structures geometric shapes. This modification on the surface of the ZrSiO_4 was corroborated by atomic force microscopy where significant changes were observed in the topography of the purified and hydrated material. By Fourier transform infrared spectroscopy is identifies the presence of functional groups from hydration with IP6 and NaClO_4 on the surface of SrSiO_4. Characterization of surface properties was performed by determining the surface area of the purified ZrSiO_4, SrSiO_4/NaClO_4 and ZrSiO_4/IP6 systems using the Bet multipoint and fractal dimension technique; the hydration time, zero loading point was evaluated by means of a bulk titration and surface site density (Ds). The fluorescence and phosphorescence techniques allowed determining the optimum hydration point and the uranium species sorbed on the surface of the ZrSiO_4 as in the systems hydrated with IP6 and with NaClO_4. This technique provided relevant information about the speciation and complex formation of IP6 with uranyl ions on the surface of ZrSiO_4. Sorption isotherms and kinetics were prepared by the liquid

  16. [Structural characterization of Astragalus polysaccharides using partial acid hydrolysis-hydrophilic interaction liquid chromatography-mass spectrometry].

    Science.gov (United States)

    Liang, Tu; Fu, Qing; Xin, Huaxia; Li, Fangbing; Jin, Yu; Liang, Xinmiao

    2014-12-01

    Water-soluble polysaccharides from traditional Chinese medicine (TCM) have properties of broad-spectrum treatment and low toxicity, making them as important components in natural medicines and health products. In order to solve the problem of polysaccharides characterization caused by their complex structures, a "bottom-up" approach was developed to complete the characterization of polysaccharides from Astragalus. Firstly, Astragalus pieces were extracted with hot water and then were precipitated by ethanol to obtain Astragalus polysaccharides. Secondly, a partial acid hydrolysis method was carried out and the effects of time, acid concentration and temperature on hydrolysis were investigated. The degree of hydrolysis increased along with the increase of hydrolysis time and acid concentration. The temperature played a great role in the hydrolysis process. No hydrolysis of the polysaccharides occurred at low temperature, while the polysaccharides were almost hydrolyzed to monosaccharide at high temperature. Under the optimum hydrolysis conditions (4 h, 1.5 mol/L trifluoroacetic acid, and 80 °C), Astragalus polysaccharides were hydrolyzed to characteristic oligosaccharide fragments. At last, a hydrophilic liquid chromatography-mass spectrometry method was used for the separation and structural characterization of the polysaccharide hydrolysates. The results showed that the resulting polysaccharides were mainly 1--> 4 linear glucan, and gluco-oligosaccharides with the degrees of polymerization (DP) of 4 - 11 were obtained after partial acid hydrolysis. The significance of this study is that it is the guidance for the characterization of other TCM polysaccharides.

  17. PETROLOGY AND GEOCHEMISTRY OF CALC-SILICATE SCHISTS ...

    African Journals Online (AJOL)

    DR OKONKOWO

    2012-02-29

    silicate reaction bands have higher contents of CaO and Sr and lower concentrations of K2O, Rb, Ni, and Ba relative to the calc-silicate schists; and relatively higher SiO2, TiO2, Al2O3, Fe2O3, MgO, Na2O, K2O and P2O5 and lower ...

  18. Simultaneous quantification of eight organic acid components in Artemisia capillaris Thunb (Yinchen extract using high-performance liquid chromatography coupled with diode array detection and high-resolution mass spectrometry

    Directory of Open Access Journals (Sweden)

    Fangjun Yu

    2018-04-01

    Full Text Available We aim to determine the chemical constituents of Yinchen extract and Yinchen herbs using high-performance liquid chromatography coupled with diode array detection and high-resolution mass spectrometry. The method was developed to analyze of eight organic acid components of Yinchen extract (including neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, 1,3-dicaffeoylquinic acid, 3,4-dicaffeoylquinic acid, 3,5-dicaffeoylquinic acid and 4,5-dicaffeoylquinic acid. The separation was conducted using an Agilent TC-C18 column with acetonitrile – 0.2% formic acid solution as the mobile phases under gradient elution. The analytical method was fully validated in terms of linearity, sensitivity, precision, repeatability as well as recovery, and subsequently the method was performed for the quantitative assessment of Yinchen extracts and Yinchen herbs. In addition, the changes of selected markers were studied when Yinchen herbs decocting in water and isomerization occurred between the chlorogenic acids. The proposed method enables both qualitative and quantitative analyses and could be developed as a new tool for the quality evaluation of Yinchen extract and Yinchen herbs. The changes of selected markers in water decoction process could give us some novel idea when studying the link between substances and drug efficacy. Keywords: Artemisia capillaris Thunb (Yinchen extract, Quality control, Organic acid, Transformation pathways, High-performance liquid chromatography

  19. Screening and quantitative determination of twelve acidic and neutral pharmaceuticals in whole blood by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Simonsen, Kirsten Wiese; Steentoft, Anni; Buck, Maike

    2010-01-01

    . The method was fully validated for salicylic acid, paracetamol, phenobarbital, carisoprodol, meprobamate, topiramate, etodolac, chlorzoxazone, furosemide, ibuprofen, warfarin, and salicylamide. The method also tentatively includes thiopental, theophylline, piroxicam, naproxen, diclophenac, and modafinil......We describe a multi-method for simultaneous identification and quantification of 12 acidic and neutral compounds in whole blood. The method involves a simple liquid-liquid extraction, and the identification and quantification are performed using liquid chromatography-tandem mass spectrometry...

  20. Surface charges and Np(V) sorption on amorphous Al- and Fe- silicates

    International Nuclear Information System (INIS)

    Del Nero, M.; Assada, A.; Barillon, R.; Duplatre, G.; Made, B.

    2005-01-01

    Full text of publication follows: Sorption onto Si-rich alteration layers of crystalline minerals and nuclear glasses, and onto amorphous secondary silicates of rocks and soils, are expected to retard the migration of actinides in the near- and far-field of HLW repositories. We present experimental and modeling studies on the effects of silicate structure and bulk chemistry, and of solution chemistry, on charges and adsorption of neptunyl ions at surfaces of synthetic, amorphous or poorly ordered silica, Al-silicates and Fe-silicates. The Al-silicates display similar pH-dependent surface charges characterized by predominant Si-O - Si sites, and similar surface affinities for neptunyl ions, irrespective to their Si/Al molar ratio (varying from 10 to 4.3). Such experimental features are explained by incorporation of Al atoms in tetrahedral position in the silicate lattice, leading to only trace amounts of high-affinity Al-OH surface groups due to octahedral Al. By contrast, the structure of the Fe-silicates ensures the occurrence of high-affinity Fe-OH surface groups, whose concentration is shown by proton adsorption measurements to increase with decreasing of the silicate Si/Fe molar ratio (from 10 to 2.3). Nevertheless, experimental data of the adsorption of neptunyl and electrolyte ions show unexpectedly weak effect of the Si/Fe ratio, and suggest predominant Si-OH surface groups. A possible explanation is that aqueous silicate anions, released by dissolution, adsorb at OH Fe - surface groups and / or precipitate as silica gel coatings, because experimental solutions were found at near-equilibrium with respect to amorphous silica. Therefore, the environmental sorption of Np(V) onto Si-rich, amorphous or poorly ordered Al-silicates may primarily depend on pH and silicate specific surface areas, given the low overall chemical affinity of such phases for dissolved metals. By contrast, the sorption of Np(V) on natural, amorphous or poorly ordered Fe-silicates may be a

  1. Quantitative analysis of fatty-acid-based biofuels produced by wild-type and genetically engineered cyanobacteria by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Guan, Wenna; Zhao, Hui; Lu, Xuefeng; Wang, Cong; Yang, Menglong; Bai, Fali

    2011-11-11

    Simple and rapid quantitative determination of fatty-acid-based biofuels is greatly important for the study of genetic engineering progress for biofuels production by microalgae. Ideal biofuels produced from biological systems should be chemically similar to petroleum, like fatty-acid-based molecules including free fatty acids, fatty acid methyl esters, fatty acid ethyl esters, fatty alcohols and fatty alkanes. This study founded a gas chromatography-mass spectrometry (GC-MS) method for simultaneous quantification of seven free fatty acids, nine fatty acid methyl esters, five fatty acid ethyl esters, five fatty alcohols and three fatty alkanes produced by wild-type Synechocystis PCC 6803 and its genetically engineered strain. Data obtained from GC-MS analyses were quantified using internal standard peak area comparisons. The linearity, limit of detection (LOD) and precision (RSD) of the method were evaluated. The results demonstrated that fatty-acid-based biofuels can be directly determined by GC-MS without derivation. Therefore, rapid and reliable quantitative analysis of fatty-acid-based biofuels produced by wild-type and genetically engineered cyanobacteria can be achieved using the GC-MS method founded in this work. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. Radioanalysis of siliceous materials

    International Nuclear Information System (INIS)

    Das, H.A.

    2003-01-01

    Both natural and induced radioactivity as well as man-made radiotracers may be applied to assess quality and its maintenance a widely varying range of siliceous materials. One example of industrial application is given for each of these three branches. Natural Radioactivity: The measurement of 222-Rn emanation from building material components serves the determination of the internal diffusion and thus of the effective porosity as well as the usual environmental control. Radiotracers: The specific surface area of silica components can be obtained from measurements of the chemisorptions of fluoride and its kinetics, using acid fluoride solutions and carrier-free 18-F, Tl/2 = 110 min, as the radiotracer. This also enables the determination of fluoride in drinking water at the (sub-) ppm level by spiking isotope dilution and substoichiometric adsorption to small glass beads. Neutron activation analysis (NAA): Concentration profiles down to the micro m-range of trace elements in small electronic components of irregular shape are derived from combination of NAA with controlled sequential etching flux in dilute HF-solutions. The cases of Na, Mn, Co and Se by instrumental NAA and that of W by chemical isolation from the reagent solution are considered. (author)

  3. Chromatographic retention prediction and octanol-water partition coefficient determination of monobasic weak acidic compounds in ion-suppression reversed-phase liquid chromatography using acids as ion-suppressors.

    Science.gov (United States)

    Ming, Xin; Han, Shu-ying; Qi, Zheng-chun; Sheng, Dong; Lian, Hong-zhen

    2009-08-15

    Although simple acids, replacing buffers, have been widely applied to suppress the ionization of weakly ionizable acidic analytes in reversed-phase liquid chromatography (RPLC), none of the previously reported works focused on the systematic studies about the retention behavior of the acidic solutes in this ion-suppression RPLC mode. The subject of this paper was therefore to investigate the retention behavior of monobasic weak acidic compounds using acetic, perchloric and phosphoric acids as the ion-suppressors. The apparent octanol-water partition coefficient (K" ow) was proposed to calibrate the octanol-water partition coefficient (K(ow)) of these weak acidic compounds, which resulted in a better linear correlation with log k(w), the logarithm of the hypothetical retention factor corresponding to neat aqueous fraction of hydroorganic mobile phase. This log K" ow-log k w linear correlation was successfully validated by the results of monocarboxylic acids and monohydrating phenols, and moreover by the results under diverse experimental conditions for the same solutes. This straightforward relationship not only can be used to effectively predict the retention values of weak acidic solutes combined with Snyder-Soczewinski equation, but also can offer a promising medium for directly measuring K(ow) data of these compounds via Collander equation. In addition, the influence of the different ion-suppressors on the retention of weak acidic compounds was also compared in this RPLC mode.

  4. Determination of aminopolycarboxylic acids at ultra-trace levels by means of online coupling ion exchange chromatography and inductively coupled plasma-mass spectrometry with indirect detection via their Pd{sup 2+}-complexes

    Energy Technology Data Exchange (ETDEWEB)

    Nette, David; Seubert, Andreas, E-mail: seubert@staff.uni-marburg.de

    2015-07-16

    Highlights: • 8 important APCA’s analyzed in one run instead of 3 in the previous method. • Pd{sup 2+} extents the methods applicability to 3 and more dentate amino carboxylic acids. • Separation system optimized for the isocratic determination of important APCA’s. • Thermodynamic stability of APCA–Pd{sup 2+} complexes is higher than for Fe{sup 3+} and In{sup 3+}. • Pd{sup 2+} is kinetically much slower than Fe{sup 3+} and In{sup 3+} and makes the method more rugged. - Abstract: A new indirect IC-ICP-MS method for the determination of aminopolycarboxylic acids in water samples is described. It is based on the addition of an excess of Pd(II) to water samples. The analytes are forced into very strong and negatively charged palladium complexes, separated by ion exchange chromatography and detected by their palladium content, utilizing an on-line coupled ICP-MS. This method is suitable to determine the concentration of 8 aminopolycarboxylic acids (nitrilotriacetic acid (NTA), (2-carboxyethyl) iminodiacetic acid (β-ADA), methylglycinediacetic acid (MGDA), 2-hydroxyethyl) ethylenediamine triacetic acid (HEDTA), diethylene triamine pentaacetic acid (DTPA), ethylendiamine tetraacetic acid (EDTA), 1,3-diaminopropane tetraacetic acid (1,3-PDTA) and 1,2-diaminopropane tetraacetic acid (1,2-PDTA) at the ng kg{sup −1} level. The method is faster and easier than the established gas chromatography (GC)-method ISO 16588:2002 [1] and up to two orders of magnitude more sensitive than the ion pair chromatography based method of DIN 38413-8. Analytic performance is superior to ISO 16588:2002 and the comparability is good.

  5. Properties of Tricalcium Silicate Sealers.

    Science.gov (United States)

    Khalil, Issam; Naaman, Alfred; Camilleri, Josette

    2016-10-01

    Sealers based on tricalcium silicate cement aim at an interaction of the sealer with the root canal wall, alkalinity with potential antimicrobial activity, and the ability to set in a wet field. The aim of this study was to characterize and investigate the properties of a new tricalcium silicate-based sealer and verify its compliance to ISO 6876 (2012). A new tricalcium silicate-based sealer (Bio MM; St Joseph University, Beirut, Lebanon), BioRoot RCS (Septodont, St Maure de Fosses, France), and AH Plus (Dentsply, DeTrey, Konstanz, Germany) were investigated. Characterization using scanning electron microscopy, energy-dispersive spectroscopy, and X-ray diffraction analysis was performed. Furthermore, sealer setting time, flow, film thickness, and radiopacity were performed following ISO specifications. pH and ion leaching in solution were assessed by pH analysis and inductively coupled plasma. Bio MM and BioRoot RCS were both composed of tricalcium silicate and tantalum oxide in Bio MM and zirconium oxide in BioRoot RCS. In addition, the Bio MM contained calcium carbonate and a phosphate phase. The inorganic components of AH Plus were calcium tungstate and zirconium oxide. AH Plus complied with the ISO norms for both flow and film thickness. BioRoot RCS and Bio MM exhibited a lower flow and a higher film thickness than that specified for sealer cements in ISO 6876. All test sealers exhibited adequate radiopacity. Bio MM interacted with physiologic solution, thus showing potential for bioactivity. Sealer properties were acceptable and comparable with other sealers available clinically. Copyright © 2016 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

  6. Developing a novel magnesium glycerophosphate/silicate-based organic-inorganic composite cement for bone repair.

    Science.gov (United States)

    Ding, Zhengwen; Li, Hong; Wei, Jie; Li, Ruijiang; Yan, Yonggang

    2018-06-01

    Considering that the phospholipids and glycerophosphoric acid are the basic materials throughout the metabolism of the whole life period and the bone is composed of organic polymer collagen and inorganic mineral apatite, a novel self-setting composite of magnesium glycerophosphate (MG) and di-calcium silicate(C2S)/tri-calcium silicate(C3S) was developed as bio-cement for bone repair, reconstruction and regeneration. The composite was prepared by mixing the MG, C2S and C3S with the certain ratios, and using the deionized water and phosphoric acid solution as mixed liquid. The combination and formation of the composites was characterized by FTIR, XPS and XRD. The physicochemical properties were studied by setting time, compressive strength, pH value, weight loss in the PBS and surface change by SEM-EDX. The biocompatibility was evaluated by cell culture in the leaching solution of the composites. The preliminary results showed that when di- and tri-calcium silicate contact with water, there are lots of Ca(OH) 2 generated making the pH value of solution is higher than 9 which is helpful for the formation of hydroxyapatite(HA) that is the main bone material. The new organic-inorganic self-setting bio-cements showed initial setting time is ranged from 20 min to 85 min and the compressive strength reached 30 MPa on the 7th days, suitable as the bone fillers. The weight loss was 20% in the first week, and 25% in the 4th week. Meanwhile, the new HA precipitated on the composite surface during the incubation in the SBF showed bioactivity. The cell cultured in the leaching liquid of the composite showed high proliferation inferring the new bio-cement has good biocompatibility to the cells. Copyright © 2018 Elsevier B.V. All rights reserved.

  7. Identification of organic acids as potential biomarkers in the urine of autistic children using gas chromatography/mass spectrometry.

    Science.gov (United States)

    Kałużna-Czaplińska, Joanna; Żurawicz, Ewa; Struck, Wiktoria; Markuszewski, Michał

    2014-09-01

    There is a need to identify metabolic phenotypes in autism as they might each require unique approaches to prevention. Biological markers can help define autism subtypes and reveal potential therapeutic targets. The aim of the study was to identify alterations of small molecular weight compounds and to find potential biomarkers. Gas chromatography/mass spectrometry was employed to evaluate major metabolic changes in low molecular weight urine metabolites of 14 children with autism spectrum disorders vs. 10 non-autistic subjects. The results prove the usefulness of an identified set of 21 endogenous compounds (including 14 organic acids), whose levels are changed in diseased children. Gas chromatography/mass spectrometry method combined with multivariate statistical analysis techniques provide an efficient way of depicting metabolic perturbations of diseases, and may potentially be applicable as a novel strategy for the noninvasive diagnosis and treatment of autism. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Determination of undecylenic and sorbic acids in cosmetic preparations by high performance liquid chromatography with electrochemical detection.

    Science.gov (United States)

    Bousquet, Ennio; Spadaro, A; Santagati, N A; Scalia, S; Ronsisvalle, G

    2002-11-07

    A highly sensitive and selective method for the determination of sorbic (SA) and undecylenic acid (UA) in cosmetic formulations by a high performance liquid chromatography method with electrochemical detection (ECD) is described. The pre-column derivatizations of SA and UA and the internal standard (cyclohexanoic acid (cHA)) were carried out using 1-(2,5-dihydroxyphenyl)-2-bromoethanone (2,5-DBE) as an electroactive labeling reagent previously synthesized in our lab. The resulting electroactive esters were separated by isocratic elution of a 5 micrometer Hypersil CN column with acetonitrile-acetate buffer eluent. The compounds were detected by a porous graphite electrode set at an oxidation potential of +0.45 V. The analytical method developed in this study is suitable for quality control assays of complex cosmetic formulations containing sorbic and/or UA.

  9. Use of depleted uranium silicate glass to minimize release of radionuclides from spent nuclear fuel waste packages

    International Nuclear Information System (INIS)

    Forsberg, C.W.

    1996-01-01

    A Depleted Uranium Silicate Container Backfill System (DUSCOBS) is proposed that would use small, isotopically-depleted uranium silicate glass beads as a backfill material inside repository waste packages containing spent nuclear fuel (SNF). The uranium silicate glass beads would fill the void space inside the package including the coolant channels inside SNF assemblies. Based on preliminary analysis, the following benefits have been identified. DUSCOBS improves repository waste package performance by three mechanisms. First, it reduces the radionuclide releases from SNF when water enters the waste package by creating a local uranium silicate saturated groundwater environment that suppresses (a) the dissolution and/or transformation of uranium dioxide fuel pellets and, hence, (b) the release of radionuclides incorporated into the SNF pellets. Second, the potential for long-term nuclear criticality is reduced by isotopic exchange of enriched uranium in SNF with the depleted uranium (DU) in the glass. Third, the backfill reduces radiation interactions between SNF and the local environment (package and local geology) and thus reduces generation of hydrogen, acids, and other chemicals that degrade the waste package system. Finally, DUSCOBS provides a potential method to dispose of significant quantities of excess DU from uranium enrichment plants at potential economic savings. DUSCOBS is a new concept. Consequently, the concept has not been optimized or demonstrated in laboratory experiments

  10. Preparative separation of polyphenols from artichoke by polyamide column chromatography and high-speed counter-current chromatography

    International Nuclear Information System (INIS)

    Shu, Xikai; Wang, Mei; Liu, Daicheng; Wang, Daijie; Lin, Xiaojing; Liu, Jianhua; Wang, Xiao; Huang, Luqi

    2013-01-01

    An efficient method for the rapid separation and purification of polyphenols from artichoke by polyamide column chromatography in combination with high-speed counter-current chromatography (HSCCC) was successfully built. The crude ethanol extracts from dry artichoke were first pre-separated by polyamide column chromatography and divided in two parts as sample 1 and sample 2. Then, the samples were further separated by HSCCC and yielded 7.8 mg of chlorogenic acid (compound I), 24.5 mg of luteolin-7-O-β-D-rutinoside (compound II), 18.4 mg of luteolin-7-O-β-D-glucoside (compound III), and 33.4 mg of cynarin (compound IV) with purity levels of 92.0%, 98.2%, 98.5%, and 98.0%, respectively, as determined by high-performance liquid chromatography (HPLC) method. The chemical structures of these compounds were identified by electrospray ionization-mass spectrometry (ESI-MS) and nuclear magnetic resonance (NMR). (author)

  11. Preparative separation of polyphenols from artichoke by polyamide column chromatography and high-speed counter-current chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Shu, Xikai; Wang, Mei; Liu, Daicheng [College of Life Science, Shandong Normal University, Jinan, Shandong (China); Wang, Daijie; Lin, Xiaojing; Liu, Jianhua; Wang, Xiao; Huang, Luqi, E-mail: wxjn1998@126.com [Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan, Shandong (China)

    2013-09-01

    An efficient method for the rapid separation and purification of polyphenols from artichoke by polyamide column chromatography in combination with high-speed counter-current chromatography (HSCCC) was successfully built. The crude ethanol extracts from dry artichoke were first pre-separated by polyamide column chromatography and divided in two parts as sample 1 and sample 2. Then, the samples were further separated by HSCCC and yielded 7.8 mg of chlorogenic acid (compound I), 24.5 mg of luteolin-7-O-{beta}-D-rutinoside (compound II), 18.4 mg of luteolin-7-O-{beta}-D-glucoside (compound III), and 33.4 mg of cynarin (compound IV) with purity levels of 92.0%, 98.2%, 98.5%, and 98.0%, respectively, as determined by high-performance liquid chromatography (HPLC) method. The chemical structures of these compounds were identified by electrospray ionization-mass spectrometry (ESI-MS) and nuclear magnetic resonance (NMR). (author)

  12. Application of liquid chromatography-mass spectrometry to measure the concentrations and study the synthesis of short chain fatty acids following stable isotope infusions

    NARCIS (Netherlands)

    Meesters, R.J.W.; Eijk, H.M.H. van; Have, G.A.M. ten; Graaf, A.A. de; Venema, K.; Rossum, B.E.J. van; Deutz, N.E.P.

    2007-01-01

    A new method involving zinc sulphate deproteinization was developed to study short chain fatty acids (SCFA) production in the colon and subsequent occurrence of SCFA in blood. SCFA were baseline separated in a 30 min cycle using ion-exclusion chromatography and detected by mass spectrometry.

  13. Silicic magma generation at Askja volcano, Iceland

    Science.gov (United States)

    Sigmarsson, O.

    2009-04-01

    Rate of magma differentiation is an important parameter for hazard assessment at active volcanoes. However, estimates of these rates depend on proper understanding of the underlying magmatic processes and magma generation. Differences in isotope ratios of O, Th and B between silicic and in contemporaneous basaltic magmas have been used to emphasize their origin by partial melting of hydrothermally altered metabasaltic crust in the rift-zones favoured by a strong geothermal gradient. An alternative model for the origin of silicic magmas in the Iceland has been proposed based on U-series results. Young mantle-derived mafic protolith is thought to be metasomatized and partially melted to form the silicic end-member. However, this model underestimates the compositional variations of the hydrothermally-altered basaltic crust. New data on U-Th disequilibria and O-isotopes in basalts and dacites from Askja volcano reveal a strong correlation between (230Th/232Th) and delta 18O. The 1875 AD dacite has the lowest Th- and O isotope ratios (0.94 and -0.24 per mille, respectively) whereas tephra of evolved basaltic composition, erupted 2 months earlier, has significantly higher values (1.03 and 2.8 per mille, respectively). Highest values are observed in the most recent basalts (erupted in 1920 and 1961) inside the Askja caldera complex and out on the associated fissure swarm (Sveinagja basalt). This correlation also holds for older magma such as an early Holocene dacites, which eruption may have been provoked by rapid glacier thinning. Silicic magmas at Askja volcano thus bear geochemical signatures that are best explained by partial melting of extensively hydrothermally altered crust and that the silicic magma source has remained constant during the Holocene at least. Once these silicic magmas are formed they appear to erupt rapidly rather than mixing and mingling with the incoming basalt heat-source that explains lack of icelandites and the bi-modal volcanism at Askja

  14. COMPARISON OF SOL-GEL SILICATE COATINGS ON Ti SUBSTRATE

    Directory of Open Access Journals (Sweden)

    DIANA HORKAVCOVÁ

    2012-12-01

    Full Text Available The objective of the submitted work was to prepare and to characterize two types of silicate coatings prepared by the sol-gel method using the dip-coating technique on a titanium substrate. Efforts have been made to use mechanical properties of bio-inert titanium and bioactive properties of a silicate layer enriched with an admixture of compounds identified below. The first group consisted of silicate coatings containing silver, brushite and monetite. The other group of silicate coatings contained calcium nitrate and triethyl phosphate. Mechanically and chemically treated titanium substrates were dipped into sols and dried and fired. Silicate coatings from the first group were also chemically treated in 10 mol.l-1 solution of sodium hydroxide. All coatings were measured to determine their adhesive and bioactive properties and furthermore the antibacterial properties were tested in the case of first group. Surfaces of the coated substrates were investigated after the firing and after the individual tests with optical and electron microscopy and X-ray microdiffraction. A tape test demonstrated excellent adhesive property of all coatings to the substrate, classified with degree 5. A static in vitro test demonstrated bioactivity of nearly all the coatings. The basic silicate coating from the first group and one type of coating from the second group were identified as inert. Antibacterial properties of silicate coatings containing silver showed to be different when tested against Escherichia coli bacteria. A complete inhibition of the growth of bacteria under our experimental conditions was observed for the coating containing silver and monetite and a partial inhibition of the growth of bacteria for coatings containing silver and silver in combination with brushite.

  15. Conversion of rice hull ash into soluble sodium silicate

    Directory of Open Access Journals (Sweden)

    Edson Luiz Foletto

    2006-09-01

    Full Text Available Sodium silicate is used as raw material for several purposes: silica gel production, preparation of catalysts, inks, load for medicines, concrete hardening accelerator, component of detergents and soaps, refractory constituent and deflocculant in clay slurries. In this work sodium silicate was produced by reacting rice hull ash (RHA and aqueous sodium hydroxide, in open and closed reaction systems. The studied process variables were time, temperature of reaction and composition of the reaction mixture (expressed in terms of molar ratios NaOH/SiO2 and H2O/SiO2. About 90% silica conversion contained in the RHA into sodium silicate was achieved in closed system at 200 °C. The results showed that sodium silicate production from RHA can generate aggregate value to this residue.

  16. DUSCOBS - a depleted-uranium silicate backfill for transport, storage, and disposal of spent nuclear fuel

    International Nuclear Information System (INIS)

    Forsberg, C.W.; Pope, R.B.; Ashline, R.C.; DeHart, M.D.; Childs, K.W.; Tang, J.S.

    1995-01-01

    A Depleted Uranium Silicate COntainer Backfill System (DUSCOBS) is proposed that would use small, isotopically-depleted uranium silicate glass beads as a backfill material inside storage, transport, and repository waste packages containing spent nuclear fuel (SNF). The uranium silicate glass beads would fill all void space inside the package including the coolant channels inside SNF assemblies. Based on preliminary analysis, the following benefits have been identified. DUSCOBS improves repository waste package performance by three mechanisms. First, it reduces the radionuclide releases from SNF when water enters the waste package by creating a local uranium silicate saturated groundwater environment that suppresses (1) the dissolution and/or transformation of uranium dioxide fuel pellets and, hence, (2) the release of radionuclides incorporated into the SNF pellets. Second, the potential for long-term nuclear criticality is reduced by isotopic exchange of enriched uranium in SNF with the depleted uranium (DU) in the glass. Third, the backfill reduces radiation interactions between SNF and the local environment (package and local geology) and thus reduces generation of hydrogen, acids, and other chemicals that degrade the waste package system. In addition, the DUSCOBS improves the integrity of the package by acting as a packing material and ensures criticality control for the package during SNF storage and transport. Finally, DUSCOBS provides a potential method to dispose of significant quantities of excess DU from uranium enrichment plants at potential economic savings. DUSCOBS is a new concept. Consequently, the concept has not been optimized or demonstrated in laboratory experiments

  17. Analysis of trace inorganic anions in weak acid salts by single pump cycling-column-switching ion chromatography.

    Science.gov (United States)

    Huang, Zhongping; Ni, Chengzhu; Zhu, Zhuyi; Pan, Zaifa; Wang, Lili; Zhu, Yan

    2015-05-01

    The application of ion chromatography with the single pump cycling-column-switching technique was described for the analysis of trace inorganic anions in weak acid salts within a single run. Due to the hydrogen ions provided by an anion suppressor electrolyzing water, weak acid anions could be transformed into weak acids, existing as molecules, after passing through the suppressor. Therefore, an anion suppressor and ion-exclusion column were adopted to achieve on-line matrix elimination of weak acid anions with high concentration for the analysis of trace inorganic anions in weak acid salts. A series of standard solutions consisting of target anions of various concentrations from 0.005 to 10 mg/L were analyzed, with correlation coefficients r ≥ 0.9990. The limits of detection were in the range of 0.67 to 1.51 μg/L, based on the signal-to-noise ratio of 3 and a 25 μL injection volume. Relative standard deviations for retention time, peak area, and peak height were all less than 2.01%. A spiking study was performed with satisfactory recoveries between 90.3 and 104.4% for all anions. The chromatographic system was successfully applied to the analysis of trace inorganic anions in five weak acid salts. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Urinary metabonomics study in a rat model in response to protein-energy malnutrition by using gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Wu, Zeming; Li, Min; Zhao, Chunxia; Zhou, Jia; Chang, Yuwei; Li, Xiang; Gao, Peng; Lu, Xin; Li, Yousheng; Xu, Guowang

    2010-11-01

    Systematic studies were performed on the biological perturbations in metabolic phenotype responding to protein-energy malnutrition through global metabolic profiling analysis, in combination with pattern recognition. The malnutrition rat model was established through five weeks of strict diet restriction, and the metabonome data obtained from gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS) were integrated to approximate the comprehensive metabolic signature. Principal component analysis and orthogonal projection to latent structure analysis were used for the classification of metabolic phenotypes and discovery of differentiating metabolites. The perturbations in the urine profiles of malnourished rats were marked by higher levels of creatine, threitol, pyroglutamic acid, gluconic acid and kynurenic acid, as well as decreased levels of succinic acid, cis-aconitic acid, citric acid, isocitric acid, threonic acid, trimethylglycine, N-methylnicotinic acid and uric acid. The alterations in these metabolites were associated with perturbations in energy metabolism, carbohydrate, amino acid, and fatty acid metabolism, purine metabolism, cofactor and vitamin metabolism, in response to protein and energy malnutrition. Our findings show the integration of GC-MS and LC-MS techniques for untargeted metabolic profiling analysis was promising for nutriology.

  19. Influência da escória silicatada na acidez do solo e na produtividade de grãos do arroz de terras altas Influence of calcium silicate slag on soil acidity and upland rice grain yield

    Directory of Open Access Journals (Sweden)

    Morel Pereira Barbosa Filho

    2004-04-01

    Full Text Available Apesar dos elevados teores de SiO2 total geralmente encontrados nos solos brasileiros, o teor na solução do solo pode ser baixo, em conseqüência do processo de dessilicificação que ocorre durante a intemperização dos solos. A aplicação de escórias de processamento industrial, ricas em silicatos de cálcio, tem mostrado efeitos positivos quanto à ação corretiva da acidez do solo e ao fornecimento de Si às plantas acumuladoras desse elemento, com aumentos significativos de produtividade. Conduziu-se este trabalho com o seguinte objetivo: avaliar em dois anos de cultivo sucessivos a ação corretiva, a produtividade de grãos e a absorção de Si pelo arroz de terras altas. Foram aplicadas ao solo de cerrado classificado como latossolo vermelho distroférrico de cerrado seis doses (0, 2, 4, 6, 8 e 10 t ha-1 de uma escória silicatada com 20% de SiO2 total, proveniente do processo de fabricação de superfosfatos em forno elétrico. Utilizou-se o delineamento de blocos completos casualizados com cinco repetições. Foram detectados aumentos significativos de produtividade de grãos, teor e acumulação de Si na palha e da porcentagem de grãos cheios por panícula, nos dois anos de cultivo do arroz. Houve ação corretiva no solo das doses de escória, reduzindo a acidez e aumentando a disponibilidade de P, Si, Ca trocável e a porcentagem de saturação por bases. O nível crítico de Si na palha por ocasião da colheita, para obtenção de produtividade satisfatória de grãos, foi estabelecido em 2,25 g kg-1 de matéria seca.Despite the high SiO2 total content often found in Brazilian soils, the soluble silicon content in soil solution can be low due to weathering that occur in soils. The application of calcium silicate slags, under these conditions, has demonstrated positive effects in relation to correction of soil acidity, the supply of Si to plants that accumulate this element and significant yield increase. The objectives of

  20. Structure and properties of polymer-silicate nanocomposites based on polytetrafluoroethylene

    Energy Technology Data Exchange (ETDEWEB)

    Sleptsova, Sardana A.; Okhlopkova, Aitalina A. [North-Eastern Federal University, Yakutsk (Russian Federation)

    2011-07-01

    The results of physicomechanical, tribological , and structural investigation of polytetrafluoroethylene based polymers and natural layered silicates are reported. It is shown that the tribological behaviour of the composites can be significantly improved by introducing a small amount of activated silicates. The results of structural examination of the composite friction surfaces by scanning-probe microscopy and IR spectroscopy are discussed. Key words: polytetrafluoroethylene, layered silicates, wear resistance, friction coefficient, structure, IR-spectrum.

  1. Isotopic variants of light and heavy L-pyroglutamic acid succinimidyl esters as the derivatization reagents for DL-amino acid chiral metabolomics identification by liquid chromatography and electrospray ionization mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mochizuki, Toshiki; Todoroki, Kenichiro; Inoue, Koichi; Min, Jun Zhe; Toyo’oka, Toshimasa, E-mail: toyooka@u-shizuoka-ken.ac.jp

    2014-02-06

    Graphical abstract: -- Highlights: •Isotopic variants of chiral labeling reagents were newly synthesized. •Analysis of DL-amino acids was performed by UPLC–ESI–MS/MS. •Highly efficient enantioseparation and detection of DL-amino acids were performed. •Differential analysis of DL-amino acid was successfully performed in real samples. -- Abstract: L-Pyroglutamic acid succinimidyl ester (L-PGA-OSu) and its isotopic variant (L-PGA[d{sub 5}]-OSu) were newly synthesized and evaluated as the chiral labeling reagents for the enantioseparation of amino acids, in terms of separation efficiency by reversed-phase chromatography and detection sensitivity by ESI-MS/MS. The enantiomers of amino acids were easily labeled with the reagents at 60 °C within 10 min in an alkaline medium containing triethylamine. Although all the diastereomers derived from 18 proteolytic amino acids could not be satisfactorily separated, the pairs of 9 amino acids were completely separated by reversed-phase chromatography using the small particle (1.7 μm) ODS column (Rs = 1.95–8.05). The characteristic daughter ions, i.e., m/z 84.04 and m/z 89.04, were detected from all the derivatives by the collision induced dissociation of the protonated molecular ions. A highly sensitive detection at a low-fmol level (0.5–3.2 fmol) was also obtained from the selected reaction monitoring (SRM) chromatograms. An isotope labeling strategy using light and heavy L-PGA-OSu for the differential analysis of the DL-amino acids in different sample groups is also presented in this paper. The differential analysis of biological sample (i.e., human serum) and food product (i.e., yogurt) were tried to demonstrate the efficiency of the proposed method. The ratios of the DL-amino acids in human serum samples, spiked with the different concentrations of D-amino acids, were determined by the procedures using L-PGA-OSu and L-PGA[d{sub 5}]-OSu. The D/L ratios in the two sample groups at different concentrations of

  2. Isotopic variants of light and heavy L-pyroglutamic acid succinimidyl esters as the derivatization reagents for DL-amino acid chiral metabolomics identification by liquid chromatography and electrospray ionization mass spectrometry

    International Nuclear Information System (INIS)

    Mochizuki, Toshiki; Todoroki, Kenichiro; Inoue, Koichi; Min, Jun Zhe; Toyo’oka, Toshimasa

    2014-01-01

    Graphical abstract: -- Highlights: •Isotopic variants of chiral labeling reagents were newly synthesized. •Analysis of DL-amino acids was performed by UPLC–ESI–MS/MS. •Highly efficient enantioseparation and detection of DL-amino acids were performed. •Differential analysis of DL-amino acid was successfully performed in real samples. -- Abstract: L-Pyroglutamic acid succinimidyl ester (L-PGA-OSu) and its isotopic variant (L-PGA[d 5 ]-OSu) were newly synthesized and evaluated as the chiral labeling reagents for the enantioseparation of amino acids, in terms of separation efficiency by reversed-phase chromatography and detection sensitivity by ESI-MS/MS. The enantiomers of amino acids were easily labeled with the reagents at 60 °C within 10 min in an alkaline medium containing triethylamine. Although all the diastereomers derived from 18 proteolytic amino acids could not be satisfactorily separated, the pairs of 9 amino acids were completely separated by reversed-phase chromatography using the small particle (1.7 μm) ODS column (Rs = 1.95–8.05). The characteristic daughter ions, i.e., m/z 84.04 and m/z 89.04, were detected from all the derivatives by the collision induced dissociation of the protonated molecular ions. A highly sensitive detection at a low-fmol level (0.5–3.2 fmol) was also obtained from the selected reaction monitoring (SRM) chromatograms. An isotope labeling strategy using light and heavy L-PGA-OSu for the differential analysis of the DL-amino acids in different sample groups is also presented in this paper. The differential analysis of biological sample (i.e., human serum) and food product (i.e., yogurt) were tried to demonstrate the efficiency of the proposed method. The ratios of the DL-amino acids in human serum samples, spiked with the different concentrations of D-amino acids, were determined by the procedures using L-PGA-OSu and L-PGA[d 5 ]-OSu. The D/L ratios in the two sample groups at different concentrations of amino

  3. Silicon K-edge XANES spectra of silicate minerals

    Science.gov (United States)

    Li, Dien; Bancroft, G. M.; Fleet, M. E.; Feng, X. H.

    1995-03-01

    Silicon K-edge x-ray absorption near-edge structure (XANES) spectra of a selection of silicate and aluminosilicate minerals have been measured using synchrotron radiation (SR). The spectra are qualitatively interpreted based on MO calculation of the tetrahedral SiO{4/4-}cluster. The Si K-edge generally shifts to higher energy with increased polymerization of silicates by about 1.3 eV, but with considerable overlap for silicates of different polymerization types. The substitution of Al for Si shifts the Si K-edge to lower energy. The chemical shift of Si K-edge is also sensitive to cations in more distant atom shells; for example, the Si K-edge shifts to lower energy with the substitution of Al for Mg in octahedral sites. The shifts of the Si K-edge show weak correlation with average Si-O bond distance (dSi-O), Si-O bond valence (sSi-O) and distortion of SiO4 tetrahedra, due to the crystal structure complexity of silicate minerals and multiple factors effecting the x-ray absorption processes.

  4. Preparation of β-belite using liquid alkali silicates

    International Nuclear Information System (INIS)

    Koutník, P.

    2017-01-01

    The aim of this study is the preparation of β-belite by a solid-state reaction using powdered limestone, amorphous silica and liquid alkali silicates. The raw materials were blended, the mixtures were agglomerated and then burnt. The resulting samples were characterized by X-ray diffraction analysis and scanning electron microscopy. Free lime content in the β-belite samples was also determined. The effects of CaO/SiO2 ratio (1.6–2.1), burning temperature (800–1400 °C), utilization of different raw materials (silica fume, synthetic silica, potassium silicate, sodium silicate, potassium hydroxide) and burning time (0.5–16 h) on free lime content and mineralogical composition were investigated. The purest ?-belite samples were prepared from a mixture of powdered limestone, silica fume and liquid potassium silicate with a ratio CaO/SiO2 = 2 by burning at temperatures between 1100 and 1300 °C for more than 2 h. Decreasing of the CaO/SiO2 ratio led to rankinite formation and lower a burning temperature led to the formation of wollastonite. [es

  5. Thin-layer chromatography can resolve phosphotyrosine, phosphoserine, and phosphothreonine in a protein hydrolyzate

    International Nuclear Information System (INIS)

    Neufeld, E.; Goren, H.J.; Boland, D.

    1989-01-01

    A solution of propionic acid, 1 M ammonium hydroxide, and isopropyl alcohol (45/17.5/17.5, v/v) was the ascending solvent in the separation of phosphotyrosine, phosphothreonine, and phosphoserine by thin-layer chromatography. The immobile phase was cellulose. The relative migrations were 0.44, 0.38, and 0.2, respectively. A previously described thin-layer system consisting of isobutyric acid and 0.5 M ammonium hydroxide (50/30, v/v) gave very similar relative migrations. To determine the usefulness of thin-layer chromatography in phosphoamino acid analysis, the propionic acid/ammonium hydroxide/isopropyl alcohol solution was used to characterize phosphorylated residues in a plasma membrane protein which is a substrate for the insulin receptor kinase, in insulin receptor phosphorylated histone H2B, and in an in vivo phosphorylated 90000-Da protein from IM9 cells. 32 P-labeled proteins were separated by dodecyl sulfate-gel electrophoresis, digested with trypsin, and then hydrolyzed with 6 N HCl, 2 h, 110 degrees C. Following thin-layer chromatography of the hydrolyzates and autoradiography, phosphotyrosine was detected in insulin receptor substrates, and phosphoserine and phosphothreonine were found in the in vivo-phosphorylated protein. This study supports previous reports about the practicality of thin-layer chromatography in phosphoamino acid analysis and it demonstrates that a propionic acid, ammonium hydroxide, isoprophyl alcohol solution may be a useful ascending solvent mixture for this purpose

  6. Lead-silicate glass optical microbubble resonator

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Pengfei, E-mail: pengfei.wang@dit.ie [Photonics Research Centre, Dublin Institute of Technology, Kevin Street, Dublin 8 (Ireland); Optoelectronics Research Centre, University of Southampton, Southampton SO17 1BJ (United Kingdom); Ward, Jonathan; Yang, Yong; Chormaic, Síle Nic [Light-Matter Interactions Unit, OIST Graduate University, 1919-1 Tancha, Onna-son, Okinawa 904-0495 (Japan); Feng, Xian; Brambilla, Gilberto [Optoelectronics Research Centre, University of Southampton, Southampton SO17 1BJ (United Kingdom); Farrell, Gerald [Photonics Research Centre, Dublin Institute of Technology, Kevin Street, Dublin 8 (Ireland)

    2015-02-09

    Microbubble whispering gallery resonators have the potential to become key components in a variety of active and passive photonic circuit devices by offering a range of significant functionalities. Here, we report on the fabrication, optical characterization, and theoretical analysis of lead-silicate glass and optical microbubble resonators. Evanescent field coupling to the microbubbles was achieved using a 1 μm diameter, silica microfiber at a wavelength of circa 775 nm. High Q-factor modes were efficiently excited in both single-stem and two-stem, lead-silicate glass, and microbubble resonators, with bubble diameters of 38 μm (single-stem) and 48 μm (two-stem). Whispering gallery mode resonances with Q-factors as high as 2.3 × 10{sup 5} (single-stem) and 7 × 10{sup 6} (two-stem) were observed. By exploiting the high-nonlinearity of the lead-silicate glass, this work will act as a catalyst for studying a range of nonlinear optical effects in microbubbles, such as Raman scattering and four-wave mixing, at low optical powers.

  7. Glassin, a histidine-rich protein from the siliceous skeletal system of the marine sponge Euplectella, directs silica polycondensation.

    Science.gov (United States)

    Shimizu, Katsuhiko; Amano, Taro; Bari, Md Rezaul; Weaver, James C; Arima, Jiro; Mori, Nobuhiro

    2015-09-15

    The hexactinellids are a diverse group of predominantly deep sea sponges that synthesize elaborate fibrous skeletal systems of amorphous hydrated silica. As a representative example, members of the genus Euplectella have proved to be useful model systems for investigating structure-function relationships in these hierarchically ordered siliceous network-like composites. Despite recent advances in understanding the mechanistic origins of damage tolerance in these complex skeletal systems, the details of their synthesis have remained largely unexplored. Here, we describe a previously unidentified protein, named "glassin," the main constituent in the water-soluble fraction of the demineralized skeletal elements of Euplectella. When combined with silicic acid solutions, glassin rapidly accelerates silica polycondensation over a pH range of 6-8. Glassin is characterized by high histidine content, and cDNA sequence analysis reveals that glassin shares no significant similarity with any other known proteins. The deduced amino acid sequence reveals that glassin consists of two similar histidine-rich domains and a connecting domain. Each of the histidine-rich domains is composed of three segments: an amino-terminal histidine and aspartic acid-rich sequence, a proline-rich sequence in the middle, and a histidine and threonine-rich sequence at the carboxyl terminus. Histidine always forms HX or HHX repeats, in which most of X positions are occupied by glycine, aspartic acid, or threonine. Recombinant glassin reproduces the silica precipitation activity observed in the native proteins. The highly modular composition of glassin, composed of imidazole, acidic, and hydroxyl residues, favors silica polycondensation and provides insights into the molecular mechanisms of skeletal formation in hexactinellid sponges.

  8. Deinking of different furnishes of recycled MOW, ONP, and OMG pulps in silicate-free conditions using organic complex of PHASS

    Directory of Open Access Journals (Sweden)

    Iman Akbarpour

    2013-02-01

    Full Text Available Sodium silicate causes problems in papermaking such as deposit formation, decreased retention, and lower sheet strength. Due to these problems, chemical deinking of different recycled papers furnishes including 100% ONP, 80% ONP, and 20% OMG, and a combination of 70% ONP/ 20% OMG/ 10% MOW was accomplished using an organic complexing agent which included poly-hydroxyl acrylic acid and sodium salt (PHAAS in silicate-free conditions. PHAAS was utilized at four levels of 0.3, 0.5, 0.7, and 1% (based on oven-dry weight of recycled paper rather than sodium silicate. The optical and physical properties of deinked pulp were compared to control pulp (conventional deinking containing 2% sodium silicate. The results showed that the paper brightness was improved and the yellowness, dirt count, and dirt area were decreased significantly by increasing PHAAS charge up to 0.9%. Also, in different recycled paper furnishes above mentioned, using different charges of PHAAS had different effects on paper opacity. Using different charges of PHAAS (especially 0.7 to 0.9% decreased paper caliper, increased paper air resistance, increased freeness, and gave similar or slightly better paper tear indices. Differences of tear indices were not significant at confidence level of 99%. Based on the present research, the use of 0.7 to 0.9% PHAAS in place of sodium silicate is advisable because of the better quality of final papers compared to conventional deinking process.

  9. On the Relation of Silicates and SiO Maser in Evolved Stars

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Jiaming; Jiang, Biwei, E-mail: bjiang@bnu.edu.cn [Department of Astronomy, Beijing Normal University, Beijing 100875 (China)

    2017-04-01

    The SiO molecule is one of the candidates for the seed of silicate dust in the circumstellar envelope of evolved stars, but this opinion is challenged. In this work we investigate the relation of the SiO maser emission power and the silicate dust emission power. With both our own observation by using the PMO/Delingha 13.7 m telescope and archive data, a sample is assembled of 21 SiO v  = 1, J  = 2 − 1 sources and 28 SiO v  = 1, J  = 1 − 0 sources that exhibit silicate emission features in the ISO /SWS spectrum as well. The analysis of their SiO maser and silicate emission power indicates a clear correlation, which is not against the hypothesis that the SiO molecules are the seed nuclei of silicate dust. On the other hand, no correlation is found between SiO maser and silicate crystallinity, which may imply that silicate crystallinity does not correlate with mass-loss rate.

  10. Reversed-phase liquid chromatography coupled on-line with capillary gas chromatography use of an anion-exchange membrane to remove an ion-pair reagent from the eluent.

    NARCIS (Netherlands)

    Brinkman, U.A.T.; Goosens, E.C.; de Jong, D.; de Jong, G.J.; Beerthuizen, I.M.

    1995-01-01

    In order to enable the coupling of reversed-phase liquid chromatography (RPLC) with capillary gas chromatography (GC), the performance of an anion-exchange micromembrane device has been studied to remove the ion-pair reagent methanesulphonic acid from an acetonitrile/water LC eluent. The regenerant

  11. Thin-layer chromatography - liquid chromatography, an ideal supplement demonstrated by the separation of lanthanoids

    International Nuclear Information System (INIS)

    Specker, H.; Hufnagel, A.

    1984-01-01

    All lanthanoids have been separated by thin-layer chromatography (TLC) with short retention times by using a mixture of ether/tetrahydrofurane (THF)/bis-(2-ethylhexyl)-phosphate (HDEHP)/nitric acid. The eluent was empirically tested by synergistic effects. The results have been transferred to high-performance liquid chromatography /HPLC). It was possible to use the same eluent in TLC and HPLC both for the analytical separation of all lanthanoids and for the separation of fission products. The experimental experience gained in HPLC could be applied to the pre-concentration of isotopes in TLC. Both methods excellently supplemented each other in the separation of lanthanoids. (orig.) [de

  12. Quantitative determination of chlorogenic acid in γ-ray-irradiated potato tubers by high performance liquid chromatography

    International Nuclear Information System (INIS)

    Nishizawa, Makoto; Chonan, Takao; Yamagishi, Takashi; Ando, Yoshiaki

    1984-01-01

    Chlorogenic acid (CGA) and caffeic acid (CA) in lyophilized potato tubers were quantitatively determined by high performance liquid chromatography (HPLC), and the changes in CGA contents of γ-ray-irradiated potato tubers (100 Gy) during storage at 25 0 C were studied. The CGA contents of the irradiated potato tubers slightly increased immediately after irradiation, but decreased gradually after 29th day and reached the same level as that in the beginning of storage on the 73rd day after irradiation. However, the CGA contents of the unirradiated potato tubers increased steadily with increasing days of storage period, and reached twice that in the beginning of storage on the 73rd day after irradiation. The CGA contents in potato tubers determined by Diazo and Folin-Denis methods were shown to be two - eight times higher than those by HPLC method, and there appeared to be no significant relation between the CGA contents determined by HPLC method and by colorimetrical methods. (author)

  13. Comparison of two derivatization methods for the analysis of fatty acids and trans fatty acids in bakery products using gas chromatography.

    Science.gov (United States)

    Salimon, Jumat; Omar, Talal A; Salih, Nadia

    2014-01-01

    Two different procedures for the methylation of fatty acids (FAs) and trans fatty acids (TFAs) in food fats were compared using gas chromatography (GC-FID). The base-catalyzed followed by an acid-catalyzed method (KOCH3/HCl) and the base-catalyzed followed by (trimethylsilyl)diazomethane (TMS-DM) method were used to prepare FA methyl esters (FAMEs) from lipids extracted from food products. In general, both methods were suitable for the determination of cis/trans FAs. The correlation coefficients (r) between the methods were relatively small (ranging from 0.86 to 0.99) and had a high level of agreement for the most abundant FAs. The significant differences (P = 0.05) can be observed for unsaturated FAs (UFAs), specifically for TFAs. The results from the KOCH3/HCl method showed the lowest recovery values (%R) and higher variation (from 84% to 112%), especially for UFAs. The TMS-DM method had higher R values, less variation (from 90% to 106%), and more balance between variation and %RSD values in intraday and interday measurements (less than 4% and 6%, resp.) than the KOCH3/HCl method, except for C12:0, C14:0, and C18:0. Nevertheless, the KOCH3/HCl method required shorter time and was less expensive than the TMS-DM method which is more convenient for an accurate and thorough analysis of rich cis/trans UFA samples.

  14. Comparison of Two Derivatization Methods for the Analysis of Fatty Acids and Trans Fatty Acids in Bakery Products Using Gas Chromatography

    Science.gov (United States)

    Salimon, Jumat; Omar, Talal A.; Salih, Nadia

    2014-01-01

    Two different procedures for the methylation of fatty acids (FAs) and trans fatty acids (TFAs) in food fats were compared using gas chromatography (GC-FID). The base-catalyzed followed by an acid-catalyzed method (KOCH3/HCl) and the base-catalyzed followed by (trimethylsilyl)diazomethane (TMS–DM) method were used to prepare FA methyl esters (FAMEs) from lipids extracted from food products. In general, both methods were suitable for the determination of cis/trans FAs. The correlation coefficients (r) between the methods were relatively small (ranging from 0.86 to 0.99) and had a high level of agreement for the most abundant FAs. The significant differences (P = 0.05) can be observed for unsaturated FAs (UFAs), specifically for TFAs. The results from the KOCH3/HCl method showed the lowest recovery values (%R) and higher variation (from 84% to 112%), especially for UFAs. The TMS-DM method had higher R values, less variation (from 90% to 106%), and more balance between variation and %RSD values in intraday and interday measurements (less than 4% and 6%, resp.) than the KOCH3/HCl method, except for C12:0, C14:0, and C18:0. Nevertheless, the KOCH3/HCl method required shorter time and was less expensive than the TMS-DM method which is more convenient for an accurate and thorough analysis of rich cis/trans UFA samples. PMID:24719581

  15. Comparison of Two Derivatization Methods for the Analysis of Fatty Acids and Trans Fatty Acids in Bakery Products Using Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Jumat Salimon

    2014-01-01

    Full Text Available Two different procedures for the methylation of fatty acids (FAs and trans fatty acids (TFAs in food fats were compared using gas chromatography (GC-FID. The base-catalyzed followed by an acid-catalyzed method (KOCH3/HCl and the base-catalyzed followed by (trimethylsilyldiazomethane (TMS–DM method were used to prepare FA methyl esters (FAMEs from lipids extracted from food products. In general, both methods were suitable for the determination of cis/trans FAs. The correlation coefficients (r between the methods were relatively small (ranging from 0.86 to 0.99 and had a high level of agreement for the most abundant FAs. The significant differences (P=0.05 can be observed for unsaturated FAs (UFAs, specifically for TFAs. The results from the KOCH3/HCl method showed the lowest recovery values (%R and higher variation (from 84% to 112%, especially for UFAs. The TMS-DM method had higher R values, less variation (from 90% to 106%, and more balance between variation and %RSD values in intraday and interday measurements (less than 4% and 6%, resp. than the KOCH3/HCl method, except for C12:0, C14:0, and C18:0. Nevertheless, the KOCH3/HCl method required shorter time and was less expensive than the TMS-DM method which is more convenient for an accurate and thorough analysis of rich cis/trans UFA samples.

  16. Amino acid δ13C analysis of hair proteins and bone collagen using liquid chromatography/isotope ratio mass spectrometry

    DEFF Research Database (Denmark)

    Raghavan, Maanasa; McCullagh, James S. O.; Lynnerup, Niels

    2010-01-01

    We report a novel method for the chromatographic separation and measurement of stable carbon isotope ratios (delta(13)C) of individual amino acids in hair proteins and bone collagen using the LC-IsoLink system, which interfaces liquid chromatography (LC) with isotope ratio mass spectrometry (IRMS......). This paper provides baseline separation of 15 and 13 of the 18 amino acids in bone collagen and hair proteins, respectively. We also describe an approach to analysing small hair samples for compound-specific analysis of segmental hair sections. The LC/IRMS method is applied in a historical context...... by the delta(13)C analysis of hair proteins and bone collagen recovered from six individuals from Uummannaq in Greenland. The analysis of hair and bone amino acids from the same individual, compared for the first time in this study, is of importance in palaeodietary reconstruction. If hair proteins can be used...

  17. EFFECT OF SILICATE ON GRAM STAINING AND VIABILITY OF PNEUMOCOCCI AND OTHER BACTERIA

    Science.gov (United States)

    MacLeod, Colin M.; Roe, Amy S.

    1956-01-01

    Application of silicate solutions to living or heat-killed pneumococci and to certain "viridans" streptococci causes their conversion from a Gram-positive to a Gram-negative state. The original staining properties can be restored by suspending the silicate-treated bacteria in alkaline solutions of various salts but not by simple washing in water. Living pneumococci and the strains of streptococci whose staining properties are similarly affected are killed when suspended in silicate solutions. In other Gram-positive species silicate causes conversion to Gram negativity but restoration to positivity occurs upon washing in water. In a third group of Gram-positive organisms silicate has no effect on the Gram reaction. The viability of organisms in these two groups is unaffected by silicate under the conditions employed. No effect on staining or viability of Gram-negative bacteria has been observed. The effects of silicate on staining and viability are inhibited by nutrient broth or whole serum but not by purified serum albumin. Lecithin, choline, and other substituted ammonium compounds also inhibit the effects of silicate on pneumococci. PMID:13306854

  18. Simultaneous Determination of Chelating Agents by Ion-Suppression and Ion-Pair Chromatography in Wastewater

    International Nuclear Information System (INIS)

    Dodi, Alain; Bouscarel, Maelle

    2008-01-01

    This article describes two methods for analysing chelating agents found in nuclear waste. First, ion-suppression chromatography using an anion exchange stationary phase and mobile phase consisting of a nitric acid solution and pure water gradient. UV detection was performed at 330 nm after the reaction with a post-column reagent composed of iron nitrate in perchloric acid. Secondly, ion-pair chromatography with a mobile phase consisting of a mixture of nitric acid, tetra-butyl-ammonium hydrogeno-sulphate, tetra-butyl-ammonium hydroxide and iron chloride. A reversed-phase material was used as a stationary phase and detection was performed by direct measurement of the UV absorption at 260 nm. The quantification limits were lower for ion-pair chromatography than for ion-suppression chromatography. Both methods were easy to implement and allow a multi-element separation in less than 30 min with low detection limits. (authors)

  19. Simultaneous Determination of Chelating Agents by Ion-Suppression and Ion-Pair Chromatography in Wastewater

    Energy Technology Data Exchange (ETDEWEB)

    Dodi, Alain; Bouscarel, Maelle [Commissariat a l' energie atomique - C.E.A, Centre d' Etude de Cadarache, Laboratoire d' Analyses Radiochimiques et Chimiques, St Paul lez Durance (France)

    2008-07-01

    This article describes two methods for analysing chelating agents found in nuclear waste. First, ion-suppression chromatography using an anion exchange stationary phase and mobile phase consisting of a nitric acid solution and pure water gradient. UV detection was performed at 330 nm after the reaction with a post-column reagent composed of iron nitrate in perchloric acid. Secondly, ion-pair chromatography with a mobile phase consisting of a mixture of nitric acid, tetra-butyl-ammonium hydrogeno-sulphate, tetra-butyl-ammonium hydroxide and iron chloride. A reversed-phase material was used as a stationary phase and detection was performed by direct measurement of the UV absorption at 260 nm. The quantification limits were lower for ion-pair chromatography than for ion-suppression chromatography. Both methods were easy to implement and allow a multi-element separation in less than 30 min with low detection limits. (authors)

  20. Carbonation of metal silicates for long-term CO2 sequestration

    Science.gov (United States)

    Blencoe, James G; Palmer, Donald A; Anovitz, Lawrence M; Beard, James S

    2014-03-18

    In a preferred embodiment, the invention relates to a process of sequestering carbon dioxide. The process comprises the steps of: (a) reacting a metal silicate with a caustic alkali-metal hydroxide to produce a hydroxide of the metal formerly contained in the silicate; (b) reacting carbon dioxide with at least one of a caustic alkali-metal hydroxide and an alkali-metal silicate to produce at least one of an alkali-metal carbonate and an alkali-metal bicarbonate; and (c) reacting the metal hydroxide product of step (a) with at least one of the alkali-metal carbonate and the alkali-metal bicarbonate produced in step (b) to produce a carbonate of the metal formerly contained in the metal silicate of step (a).

  1. Viscosity of Heterogeneous Silicate Melts: A Non-Newtonian Model

    Science.gov (United States)

    Liu, Zhuangzhuang; Blanpain, Bart; Guo, Muxing

    2017-12-01

    The recently published viscosity data of heterogeneous silicate melts with well-documented structure and experimental conditions are critically re-analyzed and tabulated. By using these data, a non-Newtonian viscosity model incorporating solid fraction, solid shape, and shear rate is proposed on the basis of the power-law equation. This model allows calculating the viscosity of the heterogeneous silicate melts with solid fraction up to 34 vol pct. The error between the calculated and measured data is evaluated to be 32 pct, which is acceptable considering the large error in viscosity measurement of the completely liquid silicate melt.

  2. Release of Si from Silicon, a Ferrosilicon (FeSi) Alloy and a Synthetic Silicate Mineral in Simulated Biological Media

    Science.gov (United States)

    Herting, Gunilla; Jiang, Tao; Sjöstedt, Carin; Odnevall Wallinder, Inger

    2014-01-01

    Unique quantitative bioaccessibility data has been generated, and the influence of surface/material and test media characteristics on the elemental release process were assessed for silicon containing materials in specific synthetic body fluids at certain time periods at a fixed loading. The metal release test protocol, elaborated by the KTH team, has previously been used for classification, ranking, and screening of different alloys and metals. Time resolved elemental release of Si, Fe and Al from particles, sized less than 50 µm, of two grades of metallurgical silicon (high purity silicon, SiHG, low purity silicon, SiLG), an alloy (ferrosilicon, FeSi) and a mineral (aluminium silicate, AlSi) has been investigated in synthetic body fluids of varying pH, composition and complexation capacity, simple models of for example dermal contact and digestion scenarios. Individual methods for analysis of released Si (as silicic acid, Si(OH)4) in synthetic body fluids using GF-AAS were developed for each fluid including optimisation of solution pH and graphite furnace parameters. The release of Si from the two metallurgical silicon grades was strongly dependent on both pH and media composition with the highest release in pH neutral media. No similar effect was observed for the FeSi alloy or the aluminium silicate mineral. Surface adsorption of phosphate and lactic acid were believed to hinder the release of Si whereas the presence of citric acid enhanced the release as a result of surface complexation. An increased presence of Al and Fe in the material (low purity metalloid, alloy or mineral) resulted in a reduced release of Si in pH neutral media. The release of Si was enhanced for all materials with Al at their outermost surface in acetic media. PMID:25225879

  3. Release of Si from silicon, a ferrosilicon (FeSi alloy and a synthetic silicate mineral in simulated biological media.

    Directory of Open Access Journals (Sweden)

    Gunilla Herting

    Full Text Available Unique quantitative bioaccessibility data has been generated, and the influence of surface/material and test media characteristics on the elemental release process were assessed for silicon containing materials in specific synthetic body fluids at certain time periods at a fixed loading. The metal release test protocol, elaborated by the KTH team, has previously been used for classification, ranking, and screening of different alloys and metals. Time resolved elemental release of Si, Fe and Al from particles, sized less than 50 µm, of two grades of metallurgical silicon (high purity silicon, SiHG, low purity silicon, SiLG, an alloy (ferrosilicon, FeSi and a mineral (aluminium silicate, AlSi has been investigated in synthetic body fluids of varying pH, composition and complexation capacity, simple models of for example dermal contact and digestion scenarios. Individual methods for analysis of released Si (as silicic acid, Si(OH4 in synthetic body fluids using GF-AAS were developed for each fluid including optimisation of solution pH and graphite furnace parameters. The release of Si from the two metallurgical silicon grades was strongly dependent on both pH and media composition with the highest release in pH neutral media. No similar effect was observed for the FeSi alloy or the aluminium silicate mineral. Surface adsorption of phosphate and lactic acid were believed to hinder the release of Si whereas the presence of citric acid enhanced the release as a result of surface complexation. An increased presence of Al and Fe in the material (low purity metalloid, alloy or mineral resulted in a reduced release of Si in pH neutral media. The release of Si was enhanced for all materials with Al at their outermost surface in acetic media.

  4. Adsorption of endotoxins on Ca2+ -iminodiacetic acid by metal ion affinity chromatography.

    Science.gov (United States)

    Lopes, André Moreni; Romeu, Jorge Sánchez; Meireles, Rolando Páez; Perera, Gabriel Marquez; Morales, Rolando Perdomo; Pessoa, Adalberto; Cárdenas, Lourdes Zumalacárregui

    2012-11-01

    Endotoxins (also known as lipopolysaccharides (LPS)) are undesirable by-products of recombinant proteins, purified from Escherichia coli. LPS can be considered stable under a wide range of temperature and pH, making their removal one of the most difficult tasks in downstream processes during protein purification. The inherent toxicity of LPS makes their removal an important step for the application of these proteins in several biological assays and for a safe parenteral administration. Immobilized metal affinity chromatography (IMAC) enables the affinity interactions between the metal ions (immobilized on the support through the chelating compound) and the target molecules, thus enabling high-efficiency separation of the target molecules from other components present in a mixture. Affinity chromatography is applied with Ca2+ -iminodiacetic acid (IDA) to remove most of the LPS contaminants from the end product (more than 90%). In this study, the adsorption of LPS on an IDA-Ca2+ was investigated. The adsorption Freundlich isotherm of LPS-IDA-Ca2+ provides a theoretical basis for LPS removal. It was found that LPS is bound mainly by interactions between the phosphate group in LPS and Ca2+ ligands on the beads. The factors such as pH (4.0 or 5.5) and ionic strength (1.0 mol/L) are essential to obtain effective removal of LPS for contaminant levels between endotoxin' concentration values less than 100 EU/mL and 100 000 EU/mL. This new protocol represents a substantial advantage in time, effort, and production costs.

  5. Application of thin-layer chromatography of fat and oil, fatty acid and mineral oil for science education. Yushi, shibosan, koyu no hakuso chromatography to sono kyozaiteki katsuyo

    Energy Technology Data Exchange (ETDEWEB)

    Kawabuchi, K [Ehime Univ., Ehime (Japan); Takechi, Y; Morimoto, M [Ehime (Japan)

    1990-08-20

    In this article, with regard to application of thin-layer chromatography of fat and oil, fatty acid and mineral oil for science education, a study was made mainly on quality finding of n-hexane extracts provided in the law of prevention of water pollution, and separation of hydrolysis products of fat and oil. As a result, the existance of fat and oil, fatty acid and mineral oil in the enviromental water and the hydrolysis process of fat and oil could experimentally be confirmed. This is considered to be useful for studying teaching material on fat and oil. This report deals with the reagents and device, and specifies standard solution, thin-layer plate, spread solvent, spread tank and thermostat, and states, for its operation, the method using enzyme for hydrolysis of fat and oil and the method using potassium hydroxide. It also contemplates on R {sub f} values of fat and oil, fatty acid and mineral oil, etc., as well as spread of fat and oil, oils contained in n-hexane extracts and hydrolysis products of fat and oil. 6 refs., 4 figs., 1 tab.

  6. UTILIZATION OF RICE HUSK AS RAW MATERIAL IN SYNTHESIS OF MESOPOROUS SILICATES MCM-41

    Directory of Open Access Journals (Sweden)

    Suyanta Suyanta

    2011-12-01

    Full Text Available The research about synthesis and characterization of MCM-41 from rice husk has been done. Silica (SiO2 was extracted from rice husk by refluxing with 3M hydrochloric solution at 80 °C for 3 h. The acid-leached rice husk was filtered, washed, dried and calcined at 650 °C for 6 h lead the rough powder of rice husk silica with light brown in color. Characterization was carried out by X-ray diffraction (XRD and FTIR spectroscopy method. Rice husk silica was dissolved into the sodium hydroxide solution leading to the solution of sodium silicate, and used as silica source for the synthesis of MCM-41. MCM-41 was synthesized by hydrothermal process to the mixture prepared from 29 g of distilled water, 8.67 g of cetyltrimethyl ammonium bromide (CTMAB, 9.31 g of sodium silicate solution, and amount mL of 1 M H2SO4. Hydrothermal process was carried out at 100 °C in a teflon-lined stainless steel autoclave heated in the oven for 36 h. The solid phase was filtered, then washed with deionised water, and dried in the oven at 100 °C for 2 h. The surfactant CTMAB was removed by calcination at 550 °C for 10 h with heating rate 2 °C/min. The as-synthesized and calcined crystals were characterized by using FTIR spectroscopy, X-ray diffraction and N2 physisorption methods. In order to investigate the effect of silica source, the same procedure was carried out by using pure sodium silicate as silica source. It was concluded that silica extracted from rice husk can be used as raw materials in the synthesis of MCM-41, there is no significant difference in crystallinity and pore properties when was compared to material produced from commercial sodium silicate.

  7. Sodium Silicate Behavior in Porous Media Applied for In-Depth Profile Modifications

    Directory of Open Access Journals (Sweden)

    Hossein A. Akhlaghi Amiri

    2014-03-01

    Full Text Available This paper addresses alkaline sodium silicate (Na-silicate behavior in porous media. One of the advantages of the Na-silicate system is its water-like injectivity during the placement stage. Mixing Na-silicate with saline water results in metal silicate precipitation as well as immediate gelation. This work demonstrated that low salinity water (LSW, sea water diluted 25 times could be used as a pre-flush in flooding operations. A water override phenomenon was observed during gel formation which is caused by gravity segregation. Dynamic adsorption tests in the sand-packed tubes showed inconsiderable adsorbed silicon density (about 8.5 × 10−10 kg/cm3 for a solution with 33 mg/L silicon content, which is less than the estimated mono-layer adsorption density of 1.4 × 10−8 kg/cm3. Na-silicate enhanced water sweep efficiency after application in a dual-permeability sand-pack system, without leak off into the oil-bearing low permeability (LP zone. Field-scale numerical sensitivity studies in a layered reservoir demonstrated that higher permeability and viscosity contrasts and lower vertical/horizontal permeability ratio result in lower Na-silicate leakoff into the matrix. The length of the mixing zone between reservoir water and the injected Na-silicate solution, which is formed by low salinity pre-flush, acts as a buffer zone.

  8. Separation of zirconium and hafnium from acompanying elements by paper chromatography in the systems of alcohol-acid

    International Nuclear Information System (INIS)

    Lebedeva, G.G.; Viktorova, M.E.

    1980-01-01

    Solvents have been chosen and investigated which provide expressed separation of zirconium and hafnium at the analysis of mineral raw materials by paper chromatography. The systems with HNO 3 and HCl containing methyl, ethyl, propyl and butyl alcohols have been studied as mobile phases for separation of zirconium and hafnium. It has been shown that alcohol contents and solvent acidity affect the Rsub(f) value of these elements. The C 2 H 5 OH-5MHCl and C 2 H 5 OH-5MHNO 3 systems are most optimal for pre-concentration of zirconium and hafnium

  9. Could Mineral Surfaces have Oriented Amino Acid Polymerization Towards Useful Products?

    Science.gov (United States)

    Lambert, J. F.; Sakhno, Y.; Battistella, A.; Ribetto, B.; Mezzetti, A.; Georgelin, T.; Jaber, M.; Michot, L.

    2017-07-01

    We investigated selective amino acid polymerization on the surface of silicic minerals. Specific amino acid couples were deposited on silica or clays, thermally activated, and the oligomers formed were analyzed. Very different behaviors were observed.

  10. Identification of phenolic acids and flavonoids in monofloral honey from Bangladesh by high performance liquid chromatography: determination of antioxidant capacity.

    Science.gov (United States)

    Moniruzzaman, Mohammed; Yung An, Chua; Rao, Pasupuleti Visweswara; Hawlader, Mohammad Nurul Islam; Azlan, Siti Amirah Binti Mohd; Sulaiman, Siti Amrah; Gan, Siew Hua

    2014-01-01

    The aim of the present study was to characterize the phenolic acids, flavonoids, and antioxidant properties of monofloral honey collected from five different districts in Bangladesh. A new high performance liquid chromatography (HPLC) equipped with a UV detector method was developed for the identification of the phenolic acids and flavonoids. A total of five different phenolic acids were identified, with the most abundant being caffeic acid, benzoic acid, gallic acid, followed by chlorogenic acid and trans-cinnamic acid. The flavonoids, kaempferol, and catechin were most abundant, followed by myricetin and naringenin. The mean moisture content, total sugar content, and color characteristics of the honey samples were 18.36 ± 0.95%, 67.40 ± 5.63 g/100 g, and 129.27 ± 34.66 mm Pfund, respectively. The mean total phenolic acids, total flavonoid content, and proline content were 199.20 ± 135.23, 46.73 ± 34.16, and 556.40 ± 376.86 mg/kg, respectively, while the mean FRAP values and DPPH radical scavenging activity were 327.30 ± 231.87 μM Fe (II)/100 g and 36.95 ± 20.53%, respectively. Among the different types of honey, kalijira exhibited the highest phenolics and antioxidant properties. Overall, our study confirms that all the investigated honey samples are good sources of phenolic acids and flavonoids with good antioxidant properties.

  11. SILICATE EVOLUTION IN BROWN DWARF DISKS

    International Nuclear Information System (INIS)

    Riaz, B.

    2009-01-01

    We present a compositional analysis of the 10 μm silicate spectra for brown dwarf disks in the Taurus and Upper Scorpius (UppSco) star-forming regions, using archival Spitzer/Infrared Spectrograph observations. A variety in the silicate features is observed, ranging from a narrow profile with a peak at 9.8 μm, to nearly flat, low-contrast features. For most objects, we find nearly equal fractions for the large-grain and crystalline mass fractions, indicating both processes to be active in these disks. The median crystalline mass fraction for the Taurus brown dwarfs is found to be 20%, a factor of ∼2 higher than the median reported for the higher mass stars in Taurus. The large-grain mass fractions are found to increase with an increasing strength in the X-ray emission, while the opposite trend is observed for the crystalline mass fractions. A small 5% of the Taurus brown dwarfs are still found to be dominated by pristine interstellar medium-like dust, with an amorphous submicron grain mass fraction of ∼87%. For 15% of the objects, we find a negligible large-grain mass fraction, but a >60% small amorphous silicate fraction. These may be the cases where substantial grain growth and dust sedimentation have occurred in the disks, resulting in a high fraction of amorphous submicron grains in the disk surface. Among the UppSco brown dwarfs, only usd161939 has a signal-to-noise ratio high enough to properly model its silicate spectrum. We find a 74% small amorphous grain and a ∼26% crystalline mass fraction for this object.

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

    Science.gov (United States)

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

    2003-03-01

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

  13. I-Xe dating of silicate and troilite from IAB iron meteorites

    International Nuclear Information System (INIS)

    Niemeyer, S.

    1978-01-01

    The IAB iron meteorites may be related to the chondrites; siderophile elements in the metal matrix have chondritic abundances, and the abundant silicate inclusions are chondritic both in mineralogy and in chemical composition. Silicate and troilite (FeS) and IAB irons were analyzed by the I-Xe technique. Four IAB silicate samples gave well-defined I-Xe ages [in millions of years relative to Bjurboele; the monitor error (+-2.5 m.y.) is not included]: -3.7 +- 0.3 for Woodbine, -0.7 +- 0.6 for Mundrabilla, +1.4 +- 0.7 for Copiapo, and +2.6 +- 0.6 for Landes. The ( 129 Xe/ 132 Xe)/sub trapped/ ratios are consistent with previous values for chondrites, with the exception of Landes which has an extraordinary trapped ratio of 3.5 +- 0.2. Both analyses of silicate from Pitts gave anomalous I-Xe patterns: intermediate-temperature points defined good correlations but higher-temperature (greater than or equal to 1400 0 C) points lay above (extra 129 Xe) these lines. The two correlations have different slopes, so it cannot be assigned a definite I-Xe age to Pitts silicate. Troilite samples from Mundrabilla and Pitts were also analyzed: Pitts troilite gave a complex I-Xe pattern, which suggests an age of +17 m.y.; Mundrabilla troilite defined a good I-Xe correlation, which after correction for neutron capture on 128 Te an age of -10.8 +- 0.7 m.y. Thus, surprisingly, low-melting troilite substantially predates high-melting silicate in Mundrabilla. Abundances of Ga, Ge, and Ni in metal from these meteorites are correlated with I-Xe ages of the silicate (referred to henceforth as the metal-silicate correlation). After exploring possible relationships between the I-Xe ages and other properties of the IAB group, it was concluded that the metal-silicate correlation, the old Mundrabilla troilite, and other results favor a nebular formation model (e.g. Wasson, 1970a)

  14. Preparative separation of chlorogenic acid by centrifugal partition chromatography from highbush blueberry leaves (Vaccinium corymbosum L.).

    Science.gov (United States)

    Kim, Sang-Min; Shang, Ya Fang; Um, Byung-Hun

    2010-01-01

    Blueberries (genus Vaccinium) have gained worldwide focus because of the high anthocyanin content of their fruits. In contrast, the leaves of blueberry have not attracted any attention, even though they contain large quantities of chlorogenic acid, a strong antioxidant compound. The aim of this investigation was the quantification and preparative isolation of chlorogenic acid (5-caffeoylquinic acid, 5-CQA) from blueberry leaves using a new separation scheme, centrifugal partition chromatography (CPC). A water fraction containing a high concentration of 5-CQA (14.5% of dry weight extract) was obtained by defatting a crude methanol extract from blueberry leaves. CPC was applied to isolate 5-CQA from this water fraction using a two-phase solvent system of ethyl acetate-ethanol-water at a volume ratio 4:1:5 (v/v/v). The flow-rate of mobile phase was 2 mL/min with the ascending mode while rotating at 1200 rpm. The eluate was monitored at 330 nm. The structure of chlorogenic acid in the CPC fraction was confirmed with HPLC, UV, ESI/MS and NMR spectra. The HPLC chromatogram showed that the fractions collected by CPC contained chlorogenic acid with 96% purity based on peak area percentage. The total amount of chlorogenic acid isolated from 0.5 g of a water fraction was 52.9 mg, corresponding to 10.6% of the water fraction. The isolated compound was identified successively as 5-CQA with MS (parent ion at m/z 355.1 [M + H](+)) and (1)H NMR spectra [caffeoyl moiety in the down field (δ 6.0-8.0 ppm) and quinic acid moiety in the up field (δ 2.0-5.5 ppm)]. 5-CQA was successfully isolated from blueberry leaves by the CPC method in a one-step procedure, indicating a further potential use for blueberry leaves. Copyright © 2010 John Wiley & Sons, Ltd.

  15. Determination of vitamin E acid succinate in biodegradable microspheres by reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Martínez Sancho, C; Herrero Vanrell, R; Negro, S

    2004-01-01

    A simple, rapid, and reproducible reversed-phase high-performance liquid chromatographic (HPLC) method is applied to the routine assay of vitamin E acid succinate in biodegradable microspheres. Vitamin E acid-succinate-containing poly-(D,L-lactic-co-glycolic acid) microspheres are prepared by the solvent evaporation method. The starting drug-polymer ratio is 1:10 (w/w) and the total amount of drug and polymer processed is always 440 mg. The content of vitamin E acid succinate in the microspheres is evaluated by HPLC. Chromatography is carried out isocratically at 25 degrees C +/- 0.5 degrees C on an Extrasil ODS-2 column with a mobile phase composed of methanol-water (97:3, v/v) (pH 5.6) at a flow rate of 2 mL/min and UV detection at 284 nm. Parameters such as linearity, limits of quantitation (LOQ) and detection (LOD), precision, accuracy, recovery, specificity, and ruggedness are studied as reported in the International Conference on Harmonization guidelines. The stability of vitamin E acid succinate is also studied with satisfactory results after 48 h at 25 degrees C. The method is selective and linear for drug concentrations in the range 15-210 micro g/mL. The LOQ and LOD are 15 and 3 micro g/mL, respectively. The results for accuracy studies are good. Values for coefficient of variation for intra- and interassay are 2.08% and 2.32%, respectively. The mean percentage of vitamin E acid succinate in the recovery studies is 99.52% +/- 0.81%. The mean loading efficiency for microspheres is 96.53% +/- 1.31%.

  16. Retention of nucleic acids in ion-pair reversed-phase high-performance liquid chromatography depends not only on base composition but also on base sequence.

    Science.gov (United States)

    Qiao, Jun-Qin; Liang, Chao; Wei, Lan-Chun; Cao, Zhao-Ming; Lian, Hong-Zhen

    2016-12-01

    The study on nucleic acid retention in ion-pair reversed-phase high-performance liquid chromatography mainly focuses on size-dependence, however, other factors influencing retention behaviors have not been comprehensively clarified up to date. In this present work, the retention behaviors of oligonucleotides and double-stranded DNAs were investigated on silica-based C 18 stationary phase by ion-pair reversed-phase high-performance liquid chromatography. It is found that the retention of oligonucleotides was influenced by base composition and base sequence as well as size, and oligonucleotides prone to self-dimerization have weaker retention than those not prone to self-dimerization but with the same base composition. However, homo-oligonucleotides are suitable for the size-dependent separation as a special case of oligonucleotides. For double-stranded DNAs, the retention is also influenced by base composition and base sequence, as well as size. This may be attributed to the interaction of exposed bases in major or minor grooves with the hydrophobic alky chains of stationary phase. In addition, no specific influence of guanine and cytosine content was confirmed on retention of double-stranded DNAs. Notably, the space effect resulted from the stereostructure of nucleic acids also influences the retention behavior in ion-pair reversed-phase high-performance liquid chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. A radiochemical assay for detection of leukotriene B4 production from isolated cells

    International Nuclear Information System (INIS)

    Aharony, D.; Dobson, P.; Krell, R.D.

    1984-01-01

    A radiochemical procedure for quantitating the effect of inhibitors of leukotriene B4 (LTB4) biosynthesis is described. Rat peritoneal cells were labeled with 3 H-arachidonic acid and stimulated with the calcium ionophore A23187. 3 H-LTB4 was isolated by processing on C18-Sep Pak cartridges followed by reverse-phase high pressure liquid chromatography (HPLC). The identity of this product, as well as other arachidonic acid metabolites, was verified by using silicic acid column chromatography followed by straight-phase HPLC and thin layer chromatography. Using this assay, LTB4 release by ionophore A23187 has been shown to be both time- and concentration-dependent. Indomethacin enhanced, while NDGA and ETYA inhibited, the A23187-induced production of LTB4. This procedure is both simple and direct and is capable of assessing the ability of novel compounds to alter LTB4 production

  18. Selective enrichment of sialic acid-containing glycopeptides using titanium dioxide chromatography with analysis by HILIC and mass spectrometry

    DEFF Research Database (Denmark)

    Palmisano, Giuseppe; Lendal, Sara Eun; Engholm-Keller, Kasper

    2010-01-01

    -containing glycopeptides is achieved by using a low-pH buffer that contains a substituted acid such as glycolic acid to improve the binding efficiency and selectivity of SA-containing glycopeptides to the TiO(2) resin. By combining TiO(2) enrichment of sialylated glycopeptides with HILIC separation of deglycosylated...... of glycosylation sites and the characterization of glycan structures. In this paper, we describe a protocol for the selective enrichment of SA-containing glycopeptides using a combination of titanium dioxide (TiO(2)) and hydrophilic interaction liquid chromatography (HILIC). The selectivity of TiO(2) toward SA...... peptides, a more comprehensive analysis of formerly sialylated glycopeptides by MS can be achieved. Here we illustrate the efficiency of the method by the identification of 1,632 unique formerly sialylated glycopeptides from 817 sialylated glycoproteins. The TiO(2)/HILIC protocol requires 2 d...

  19. Fatty acid and drug binding to a low-affinity component of human serum albumin, purified by affinity chromatography

    DEFF Research Database (Denmark)

    Vorum, H; Pedersen, A O; Honoré, B

    1992-01-01

    Binding equilibria for decanoate to a defatted, commercially available human serum albumin preparation were investigated by dialysis exchange rate determinations. The binding isotherm could not be fitted by the general binding equation. It was necessary to assume that the preparation was a mixture...... of two albumin components about 40% of the albumin having high affinity and about 60% having low affinity. By affinity chromatography we succeeded in purifying the low-affinity component from the mixture. The high-affinity component, however, could not be isolated. We further analyzed the fatty acid...... and drug binding abilities of the low-affinity component. The fatty acids decanoate, laurate, myristate and palmitate were bound with higher affinity to the mixture than to the low-affinity component. Diazepam was bound with nearly the same affinity to the low-affinity component as to the albumin mixture...

  20. Potassium Silicate Foliar Fertilizer Grade from Geothermal Sludge and Pyrophyllite

    Directory of Open Access Journals (Sweden)

    Muljani Srie

    2016-01-01

    Full Text Available Potassium silicate fertilizer grade were successfully produced by direct fusion of silica (SiO2 and potasium (KOH and K2CO3 in furnaces at temperatures up to melting point of mixture. The geothermal sludge (98% SiO2 and the pyrophyllite (95% SiO2 were used as silica sources. The purposes of the study was to synthesise potassium silicate fertilizer grade having solids concentrations in the range of 31-37% K2O, and silica in the range of 48-54% SiO2. The weight ratio of silicon dioxide/potasium solid being 1:1 to 5:1. Silica from geothermal sludge is amorphous, whereas pyrophylite is crystalline phase. The results showed that the amount of raw materials needed to get the appropriate molar ratio of potassium silicate fertilizer grade are different, as well as the fusion temperature of the furnace. Potassium silicate prepared from potassium hydroxide and geothermal sludge produced a low molar ratio (2.5: 1 to 3: 1. The potassium required quite small (4:1 in weight ratio, and on a fusion temperature of about 900 °C. Meanwhile, the potassium silicate prepared from pyrophyllite produced a high molar ratio (1.4 - 9.4 and on a fusion temperature of about 1350 °C, so that potassium needed large enough to meet the required molar ratio for the fertilizer grade. The product potassium silicate solid is amorphous with a little trace of crystalline.

  1. The role of boric acid in the synthesis of Eni Carbon Silicates.

    Science.gov (United States)

    Zanardi, Stefano; Bellussi, Giuseppe; Parker, Wallace O'Neil; Montanari, Erica; Bellettato, Michela; Cruciani, Giuseppe; Carati, Angela; Guidetti, Stefania; Rizzo, Caterina; Millini, Roberto

    2014-07-21

    The influence of H3BO3 on the crystallization of hybrid organic-inorganic aluminosilicates denoted as Eni Carbon Silicates (ECS's) was investigated. Syntheses were carried out at 100 °C under different experimental conditions, using bridged silsesquioxanes of general formula (EtO)3Si-R-Si(OEt)3 (R = -C6H4- (BTEB), -C10H6- (BTEN) and -C6H4-C6H4- (BTEBP)), in the presence of equimolar concentrations of NaAlO2 and H3BO3. The study, involving the synthesis of three different but structurally related phases (ECS-14 from BTEB, ECS-13 here described for the first time from BTEN, and ECS-5 from BTEBP), confirmed a catalytic role for H3BO3 which in general increased the crystallization rate and improved the product quality in terms of amount of crystallized phase (crystallinity), size of the crystallites and phase purity, while it was weakly incorporated in trace amounts in the framework of ECS's.

  2. Fractionation of equine antivenom using caprylic acid precipitation in combination with cationic ion-exchange chromatography.

    Science.gov (United States)

    Raweerith, Rutai; Ratanabanangkoon, Kavi

    2003-11-01

    A combined process of caprylic acid (CA) precipitation and ion-exchange chromatography on SP-Sepharose was studied as a means to fractionate pepsin-digested horse antivenom F(ab')(2) antibody. In the CA precipitation, the optimal concentration for fractionation of F(ab')(2) from pepsin-digested horse plasma was 2%, in which 89.61% of F(ab')(2) antibody activity was recovered in the supernatant with 1.5-fold purification. A significant amount of pepsin was not precipitated and remained active under these conditions. An analytical cation exchanger Protein-Pak SP 8HR HPLC column was tested to establish optimal conditions for the effective separation of IgG, albumin, pepsin and CA from the F(ab')(2) product. From these results, the supernatant from CA precipitation of pepsin-digested plasma was subjected to a SP-Sepharose column chromatography using a linear salt gradient. With stepwise elution, a peak containing F(ab')(2) antibody could be obtained by elution with 0.25 M NaCl. The total recovery of antibody was 65.56% with 2.91-fold purification, which was higher than that achieved by ammonium sulfate precipitation. This process simultaneously and effectively removed residual pepsin, high molecular weight aggregates and CA in the final F(ab')(2) product, and should be suitable for large-scale fractionation of therapeutic equine antivenoms.

  3. Surface properties of calcium and magnesium oxide nanopowders grafted with unsaturated carboxylic acids studied with inverse gas chromatography.

    Science.gov (United States)

    Maciejewska, Magdalena; Krzywania-Kaliszewska, Alicja; Zaborski, Marian

    2012-09-28

    Inverse gas chromatography (IGC) was applied at infinite dilution to evaluate the surface properties of calcium and magnesium oxide nanoparticles and the effect of surface grafted unsaturated carboxylic acid on the nanopowder donor-acceptor characteristics. The dispersive components (γ(s)(D)) of the free energy of the nanopowders were determined by Gray's method, whereas their tendency to undergo specific interactions was estimated based on the electron donor-acceptor approach presented by Papirer. The calcium and magnesium oxide nanoparticles exhibited high surface energies (79 mJ/m² and 74 mJ/m², respectively). Modification of nanopowders with unsaturated carboxylic acids decreased their specific adsorption energy. The lowest value of γ(s)(D) was determined for nanopowders grafted with undecylenic acid, approximately 55 mJ/m². The specific interactions were characterised by the molar free energy (ΔG(A)(SP)) and molar enthalpy (ΔH(A)(SP)) of adsorption as well as the donor and acceptor interaction parameters (K(A), K(D)). Copyright © 2012 Elsevier B.V. All rights reserved.

  4. Isotope derivative assay of human serum bile acids

    International Nuclear Information System (INIS)

    Pageaux, J.F.; Duperray, B.; Dubois, M.; Pacheco, H.

    1981-01-01

    A new method for the selective determination of the main serum bile acids has been developed. Serum samples with added 14 C-labeled bile acid were submitted to deproteinization, alkaline hydrolysis, methylation, and were then chromatographed on alumina before acetylation with 2 microliters of [ 3 H]acetic anhydride. Excess reagent was eliminated by evaporation; elimination of residual tritiated contaminants and separation of the doubly labeled bile acid derivatives were obtained by thin-layer chromatography, column chromatography on Lipidex 5000, and crystallization. The sensitivity of the method is about 10 pmol of each bile acid. Analyses of seven sera with normal or elevated concentration of bile acids by the proposed method and gas-liquid chromatography showed a close correlation

  5. Controlled structure and properties of silicate nanoparticle networks for incorporation of biosystem components

    International Nuclear Information System (INIS)

    Sakai-Kato, Kumiko; Kawanishi, Toru; Hasegawa, Toshiaki; Takaoka, Akio; Kato, Masaru; Toyo'oka, Toshimasa; Utsunomiya-Tate, Naoko

    2011-01-01

    Inorganic nanoparticles are of technological interest in many fields. We created silicate nanoparticle hydrogels that effectively incorporated biomolecules that are unstable and involved in complicated reactions. The size of the silicate nanoparticles strongly affected both the physical characteristics of the resulting hydrogel and the activity of biomolecules incorporated within the hydrogel. We used high-resolution transmission electron microscopy (TEM) to analyze in detail the hydrogel network patterns formed by the silicate nanoparticles. We obtained clear nanostructured images of biomolecule-nanoparticle composite hydrogels. The TEM images also showed that larger silicate nanoparticles (22 nm) formed more loosely associated silicate networks than did smaller silicate nanoparticles (7 nm). The loosely associated networks formed from larger silicate nanoparticles might facilitate substrate diffusion through the network, thus promoting the observed increased activity of the entrapped biomolecules. This doubled the activity of the incorporated biosystems compared with that of biosystems prepared by our own previously reported method. We propose a reaction scheme to explain the formation of the silicate nanoparticle networks. The successful incorporation of biomolecules into the nanoparticle hydrogels, along with the high level of activity exhibited by the biomolecules required for complicated reaction within the gels, demonstrates the nanocomposites' potential for use in medical applications.

  6. Identification of an Extremely 180-Rich Presolar Silicate Grain in Acfer 094

    Science.gov (United States)

    Nguyen, A. N.; Messenger, S.

    2009-01-01

    Presolar silicate grains have been abundantly identified since their first discovery less than a decade ago [1,2,3]. The O isotopic compositions of both silicate and oxide stardust indicate the vast majority (>90%) condensed around Orich asymptotic giant branch (AGB) stars. Though both presolar phases have average sizes of 300 nm, grains larger than 1 m are extremely uncommon for presolar silicates. Thus, while numerous isotopic systems have been measured in presolar oxide grains [4], very few isotopic analyses for presolar silicates exist outside of O and Si [2,5]. And still, these measurements suffer from isotopic dilution with surrounding matrix material [6]. We conduct a search for presolar silicates in the primitive carbonaceous chondrite Acfer 094 and in some cases obtain high spatial resolution, high precision isotopic ratios.

  7. Nanostructure of Calcium Silicate Hydrates in Cements

    KAUST Repository

    Skinner, L. B.; Chae, S. R.; Benmore, C. J.; Wenk, H. R.; Monteiro, P. J. M.

    2010-01-01

    Calcium silicate hydrate (CSH) is the major volume phase in the matrix of Portland cement concrete. Total x-ray scattering measurements with synchrotron x rays on synthetic CSH(I) shows nanocrystalline ordering with a particle diameter of 3.5(5) nm, similar to a size-broadened 1.1 nm tobermorite crystal structure. The CSH component in hydrated tricalcium silicate is found to be similar to CSH(I). Only a slight bend and additional disorder within the CaO sheets is required to explain its nanocrystalline structure. © 2010 The American Physical Society.

  8. Nanostructure of Calcium Silicate Hydrates in Cements

    KAUST Repository

    Skinner, L. B.

    2010-05-11

    Calcium silicate hydrate (CSH) is the major volume phase in the matrix of Portland cement concrete. Total x-ray scattering measurements with synchrotron x rays on synthetic CSH(I) shows nanocrystalline ordering with a particle diameter of 3.5(5) nm, similar to a size-broadened 1.1 nm tobermorite crystal structure. The CSH component in hydrated tricalcium silicate is found to be similar to CSH(I). Only a slight bend and additional disorder within the CaO sheets is required to explain its nanocrystalline structure. © 2010 The American Physical Society.

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

    Energy Technology Data Exchange (ETDEWEB)

    Deng, Li [Iowa State Univ., Ames, IA (United States)

    1998-03-27

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

  10. A novel liquid chromatography/tandem mass spectrometry (LC-MS/MS) based bioanalytical method for quantification of ethyl esters of Eicosapentaenoic acid (EPA) and Docosahexaenoic acid (DHA) and its application in pharmacokinetic study.

    Science.gov (United States)

    Viswanathan, Sekarbabu; Verma, P R P; Ganesan, Muniyandithevar; Manivannan, Jeganathan

    2017-07-15

    Omega-3 fatty acids are clinically useful and the two marine omega-3 fatty acids eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) are prevalent in fish and fish oils. Omega-3 fatty acid formulations should undergo a rigorous regulatory step in order to obtain United States Food and Drug Administration (USFDA) approval as prescription drug. In connection with that, despite quantifying EPA and DHA fatty acids, there is a need for quantifying the level of ethyl esters of them in biological samples. In this study, we make use of reverse phase high performance liquid chromatography coupled with mass spectrometry (RP-HPLC-MS)technique for the method development. Here, we have developed a novel multiple reaction monitoring method along with optimized parameters for quantification of EPA and DHA as ethyl esters. Additionally, we attempted to validate the bio-analytical method by conducting the sensitivity, selectivity, precision accuracy batch, carryover test and matrix stability experiments. Furthermore, we also implemented our validated method for evaluation of pharmacokinetics of omega fatty acid ethyl ester formulations. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Crystallochemical characteristics of alkali calcium silicates from charoitites

    International Nuclear Information System (INIS)

    Rozhdestvenskaya, I.V.; Nikishova, L.V.

    2002-01-01

    The characteristic features of the crystal structures of alkali calcium silicates from various deposits are considered. The structures of these minerals, which were established by single-crystal X-ray diffraction methods, are described as the combinations of large construction modules, including the alternating layers of alkali cations and tubular silicate radicals (in canasite, frankamenite, miserite, and agrellite) and bent ribbons linked through hydrogen bonds in the layers (in tinaksite and tokkoite). The incorporation of impurities and the different ways of ordering them have different effects on the structures of these minerals and give rise to the formation of superstructures accompanied by a change of the space group (frankamenite-canasite), leading, in turn, to different mutual arrangements of the layers of silicate tubes and the formation of pseudopolytypes (agrellites), structure deformation, and changes in the unit-cell parameters (tinaksite-tokkoite)

  12. Energetic Processing of Interstellar Silicate Grains by Cosmic Rays

    Energy Technology Data Exchange (ETDEWEB)

    Bringa, E M; Kucheyev, S O; Loeffler, M J; Baragiola, R A; Tielens, A G Q M; Dai, Z R; Graham, G; Bajt, S; Bradley, J; Dukes, C A; Felter, T E; Torres, D F; van Breugel, W

    2007-03-28

    While a significant fraction of silicate dust in stellar winds has a crystalline structure, in the interstellar medium nearly all of it is amorphous. One possible explanation for this observation is the amorphization of crystalline silicates by relatively 'low' energy, heavy ion cosmic rays. Here we present the results of multiple laboratory experiments showing that single-crystal synthetic forsterite (Mg{sub 2}SiO{sub 4}) amorphizes when irradiated by 10 MeV Xe{sup ++} ions at large enough fluences. Using modeling, we extrapolate these results to show that 0.1-5.0 GeV heavy ion cosmic rays can rapidly ({approx}70 Million yrs) amorphize crystalline silicate grains ejected by stars into the interstellar medium.

  13. Use of reversed-phase gel partition chromatography for the purification of chemically synthesized (5,6,8,9,11,12,14,15(n)) octadeuterium- and octatritium-labelled arachidonic acid

    Energy Technology Data Exchange (ETDEWEB)

    Wollard, P M; Lascelles, P T [Department of Chemical Pathology, Institute of Neurology, London, Great Britain; Hensby, C N [Hammersmith Hospital, London (UK). Postgraduate Medical School

    1978-12-11

    The development of a method is described for the preparation and purification of (5,6,8,9,11,12,14,15(n)-/sup 2/H)arachidonic acid (/sup 2/H/sub 8/-AA). The /sup 2/H/sub 8/-AA was chemically synthesised by the selective reduction of 5,8,11,14-eiconsatetraynoic acid (ETYA) with deuterium gas. Using reversed-phase partition chromatography on a Lipidex 5000 column support, it was shown that: (1) The reaction products could readily be separated from each other to yield /sup 2/H/sub 8/-AA of greater than 98% mass purity by gas chromatography. (2) Closely related C20 cis-ethylenic fatty acids differing only in the degree of unsaturation are efficiently separated. The resolution increases exponentially on saturation of double bonds. (3) Commercially available (5,6,8,9,11,12,14,15(n))octatritium-labelled arachidonic acid (/sup 3/H/sub 8/-AA) was readily purified. Both (/sup 3/H/sub 8/)- and (1-/sup 14/C)arachidonic acid (/sup 14/C-AA) co-chromatographed with /sup 2/H/sub 8/-AA. (4) The mass spectra of the methyl ester and trimethylsilyl ester of the purified /sup 2/H/sub 8/-AA showed molecular ions at m/e 326 and 384, respectively.

  14. Profile of Fatty Acids, Amino Acids, Carotenoid Total, and α-Tocopherol from Flying Fish Eggs

    Directory of Open Access Journals (Sweden)

    Aulia Azka

    2015-12-01

    Full Text Available Flying fish are found in waters of eastern Indonesia, which until now is still limited information about nutritional content. The purpose of this research was determine the composition of fatty acids, amino acids, total carotenoids, α-tocopherol flying fish eggs (Hyrundicthys sp.. The composition of fatty acid was measured by gas chromatography (GC, while amino acids, total carotenoids, α-tocopherol was measured by High performanced Liquid Chromatography (HPLC. Egg contained 22 fatty acids such as saturated fatty acid 29.71%, monounsaturated fatty acid 7.86%, and polysaturated fatty acid 13.64%. The result showed that eggs flying fish contained 17 amino acids, such as essential amino acid 14.96% and non-essential amino acids 20.27%. Eggs contained a total carotenoid of 245.37 ppm. α-tocopherol content of flying fish eggs by 1.06 ppm.

  15. Gas chromatography/isotope ratio mass spectrometry: analysis of methanol, ethanol and acetic acid by direct injection of aqueous alcoholic and acetic acid samples.

    Science.gov (United States)

    Ai, Guomin; Sun, Tong; Dong, Xiuzhu

    2014-08-15

    Methanol, ethanol, and acetic acid are not easily extracted from aqueous samples and are susceptible to isotope fractionation in gas chromatography/isotope ratio mass spectrometry (GC/IRMS) analysis. Developing a direct dilution GC/IRMS method for aqueous samples, by adjusting the sample concentrations in common solvents to be similar to each other and using a fixed GC split ratio, is very convenient and important because any linearity effects caused by amount-dependent isotope fractionation can be avoided. The suitability of acetonitrile and acetone solvents for the GC/IRMS analysis of pure methanol, ethanol and acetic acid, and commercial liquor and vinegar samples was evaluated using n-hexane and water as control solvents. All the solvents including water were separated from the analyte on a HP-INNOWAX column and were diverted away from the combustion interface. The influence of liquor matrix on the ethanol GC/IRMS analyses was evaluated by adding pure ethanol to liquor samples. Acetonitrile and acetone gave similar δ(13) C values for pure ethanol and pure acetic acid to those obtained in water and n-hexane, and also gave similar δ(13) C values of ethanol in liquor and acetic acid in white vinegar to that obtained in water. For methanol analysis, acetonitrile and refined acetone gave similar δ(13) C values to that obtained in water, but n-hexane was not a suitable solvent. In addition, isotopic fractionation caused by solvent and solute interactions was observed. We recommend using acetonitrile for the GC/IRMS analysis of aqueous alcoholic samples, and acetone for the analysis of aqueous acetic acid samples. This direct dilution method can provide high accurate and precise GC/IRMS analysis of the relative changes in δ(13) C values of methanol, ethanol, and acetic acid. Copyright © 2014 John Wiley & Sons, Ltd.

  16. Prediction of Molar Extinction Coefficients of Proteins and Peptides Using UV Absorption of the Constituent Amino Acids at 214 nm To Enable Quantitative Reverse Phase High-Performance Liquid Chromatography-Mass Spectrometry Analysis

    NARCIS (Netherlands)

    Kuipers, B.J.H.; Gruppen, H.

    2007-01-01

    The molar extinction coefficients of 20 amino acids and the peptide bond were measured at 214 nm in the presence of acetonitrile and formic acid to enable quantitative comparison of peptides eluting from reversed-phase high-performance liquid chromatography, once identified with mass spectrometry

  17. Schinus terebinthifolius countercurrent chromatography (Part III): Method transfer from small countercurrent chromatography column to preparative centrifugal partition chromatography ones as a part of method development.

    Science.gov (United States)

    das Neves Costa, Fernanda; Hubert, Jane; Borie, Nicolas; Kotland, Alexis; Hewitson, Peter; Ignatova, Svetlana; Renault, Jean-Hugues

    2017-03-03

    Countercurrent chromatography (CCC) and centrifugal partition chromatography (CPC) are support free liquid-liquid chromatography techniques sharing the same basic principles and features. Method transfer has previously been demonstrated for both techniques but never from one to another. This study aimed to show such a feasibility using fractionation of Schinus terebinthifolius berries dichloromethane extract as a case study. Heptane - ethyl acetate - methanol -water (6:1:6:1, v/v/v/v) was used as solvent system with masticadienonic and 3β-masticadienolic acids as target compounds. The optimized separation methodology previously described in Part I and II, was scaled up from an analytical hydrodynamic CCC column (17.4mL) to preparative hydrostatic CPC instruments (250mL and 303mL) as a part of method development. Flow-rate and sample loading were further optimized on CPC. Mobile phase linear velocity is suggested as a transfer invariant parameter if the CPC column contains sufficient number of partition cells. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Fluorescence of soil humic acids and their fractions obtained by tandem size exclusion chromatography-polyacrylamide gel electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Trubetskaya, O. [Russian Academy of Sciences, Moscow Region (Russian Federation). Shemyakin and Ovchinnikov Inst. of Bioorganic Chemistry; Trubetskoj, O. [Russian Academy of Sciences, Moscow Region (Russian Federation). Inst. of Basic Biological Problems; Guyot, G.; Richard, C. [UMR CNRS 6505, Aubiere (France). Lab. de Photochimie Moleculaire et Macromoleculaire; Andreux, F. [Centre des Sciences de la Terre, Dijon (France)

    2002-07-01

    Humic acids (HAs) extracted from soils of different origin (chernozem, ferralsol and ranker) and their fractions (A, B and C+D) obtained by tandem size exclusion chromatography-polyacrylamide gel electrophoresis were investigated by steady-state fluorescence spectroscopy in the emission mode. Independently of HA source, high molecular size fractions A and B are shown to be weakly fluorescent. The main fluorophores, especially those emitting at long wavelength (around 500-510 nm), are contained in the polar and low molecular size fractions C+D. As indicated by the observed pH effect, aromatic structures bearing carboxylate and OH substituents may be involved in these longer wavelength emissions. [author].

  19. Deep-Earth Equilibration between Molten Iron and Solid Silicates

    Science.gov (United States)

    Brennan, M.; Zurkowski, C. C.; Chidester, B.; Campbell, A.

    2017-12-01

    Elemental partitioning between iron-rich metals and silicate minerals influences the properties of Earth's deep interior, and is ultimately responsible for the nature of the core-mantle boundary. These interactions between molten iron and solid silicates were influential during planetary accretion, and persist today between the mantle and liquid outer core. Here we report the results of diamond anvil cell experiments at lower mantle conditions (40 GPa, >2500 K) aimed at examining systems containing a mixture of metals (iron or Fe-16Si alloy) and silicates (peridotite). The experiments were conducted at pressure-temperature conditions above the metallic liquidus but below the silicate solidus, and the recovered samples were analyzed by FIB/SEM with EDS to record the compositions of the coexisting phases. Each sample formed a three-phase equilibrium between bridgmanite, Fe-rich metallic melt, and an oxide. In one experiment, using pure Fe, the quenched metal contained 6 weight percent O, and the coexisting oxide was ferropericlase. The second experiment, using Fe-Si alloy, was highly reducing; its metal contained 10 wt% Si, and the coexisting mineral was stishovite. The distinct mineralogies of the two experiments derived from their different starting metals. These results imply that metallic composition is an important factor in determining the products of mixed phase iron-silicate reactions. The properties of deep-Earth interfaces such as the core-mantle boundary could be strongly affected by their metallic components.

  20. Carbonation of metal silicates for long-term CO.sub.2 sequestration

    Energy Technology Data Exchange (ETDEWEB)

    Blencoe, James G.; Palmer, Donald A.; Anovitz, Lawrence M.; Beard, James S.

    2017-08-01

    In a preferred embodiment, the invention relates to a process of sequestering carbon dioxide. The process comprises the steps of: (a) reacting a metal silicate with a caustic alkali-metal hydroxide to produce a hydroxide of the metal formerly contained in the silicate; (b) reacting carbon dioxide with at least one of a caustic alkali-metal hydroxide and an alkali-metal silicate to produce at least one of an alkali-metal carbonate and an alkali-metal bicarbonate; and (c) reacting the metal hydroxide product of step (a) with at least one of the alkali-metal carbonate and the alkali-metal bicarbonate produced in step (b) to produce a carbonate of the metal formerly contained in the metal silicate of step (a).

  1. Carbonation of metal silicates for long-term CO.sub.2 sequestration

    Science.gov (United States)

    Blencoe, James G [Harriman, TN; Palmer, Donald A [Oliver Springs, TN; Anovitz, Lawrence M [Knoxville, TN; Beard, James S [Martinsville, VA

    2012-02-14

    In a preferred embodiment, the invention relates to a process of sequestering carbon dioxide. The process comprises the steps of: (a) reacting a metal silicate with a caustic alkali-metal hydroxide to produce a hydroxide of the metal formerly contained in the silicate; (b) reacting carbon dioxide with at least one of a caustic alkali-metal hydroxide and an alkali-metal silicate to produce at least one of an alkali-metal carbonate and an alkali-metal bicarbonate; and (c) reacting the metal hydroxide product of step (a) with at least one of the alkali-metal carbonate and the alkali-metal bicarbonate produced in step (b) to produce a carbonate of the metal formerly contained in the metal silicate of step (a).

  2. Isotachophoresis. The separation of amino acids

    NARCIS (Netherlands)

    Everaerts, F.M.; Put, van der A.J.M.

    1970-01-01

    There are several instrumental methods of analysis available for amino acids. The most important ones are ion-exchange chromatography (Stein and Moore), gas chromatography and paper chromatography. These techniques all have various disadvantages; the time for analysis may be long or the sample

  3. Rapid and precise measurement of serum branched-chain and aromatic amino acids by isotope dilution liquid chromatography tandem mass spectrometry.

    Directory of Open Access Journals (Sweden)

    Ruiyue Yang

    Full Text Available BACKGROUND: Serum branched-chain and aromatic amino acids (BCAAs and AAAs have emerged as predictors for the future development of diabetes and may aid in diabetes risk assessment. However, the current methods for the analysis of such amino acids in biological samples are time consuming. METHODS: An isotope dilution liquid chromatography tandem mass spectrometry (ID-LC/MS/MS method for serum BCAAs and AAAs was developed. The serum was mixed with isotope-labeled BCAA and AAA internal standards and the amino acids were extracted with acetonitrile, followed by analysis using LC/MS/MS. The LC separation was performed on a reversed-phase C18 column, and the MS/MS detection was performed via the positive electronic spray ionization in multiple reaction monitoring mode. RESULTS: Specific analysis of the amino acids was achieved within 2 min. Intra-run and total CVs for the amino acids were less than 2% and 4%, respectively, and the analytical recoveries ranged from 99.6 to 103.6%. CONCLUSION: A rapid and precise method for the measurement of serum BCAAs and AAAs was developed and may serve as a quick tool for screening serum BCAAs and AAAs in studies assessing diabetes risk.

  4. Fast simultaneous analysis of caffeine, trigonelline, nicotinic acid and sucrose in coffee by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Perrone, Daniel; Donangelo, Carmen Marino; Farah, Adriana

    2008-10-15

    A rapid liquid chromatography-mass spectrometry method for the simultaneous quantification of caffeine, trigonelline, nicotinic acid and sucrose in coffee was developed and validated. The method involved extraction with hot water, clarification with basic lead acetate and membrane filtration, followed by chromatographic separation using a Spherisorb(®) S5 ODS2, 5μm chromatographic column and gradient elution with 0.3% aqueous formic acid/methanol at a flow rate of 0.2mL/min. The electrospray ionization source was operated in the negative mode to generate sucrose ions and in the positive mode to generate caffeine, trigonelline and nicotinic acid ions. Ionization suppression of all analytes was found due to matrix effect. Calibrations curves prepared in green and roasted coffee extracts were linear with r(2)>0.999. Roasted coffee was spiked and recoveries ranged from 93.0% to 105.1% for caffeine, from 85.2% to 116.2% for trigonelline, from 89.6% to 113.5% for nicotinic acid and from 94.1% to 109.7% for sucrose. Good repeatibilities (RSDcoffee samples (regular or decaffeinated green, ground roasted and instant) gave results in agreement with the literature. The method showed to be suitable for different types of coffee available in the market thus appearing as a fast and reliable alternative method to be used for routine coffee analysis. Copyright © 2008 Elsevier Ltd. All rights reserved.

  5. Q-Speciation and Network Structure Evolution in Invert Calcium Silicate Glasses.

    Science.gov (United States)

    Kaseman, Derrick C; Retsinas, A; Kalampounias, A G; Papatheodorou, G N; Sen, S

    2015-07-02

    Binary silicate glasses in the system CaO-SiO2 are synthesized over an extended composition range (42 mol % ≤ CaO ≤ 61 mol %), using container-less aerodynamic levitation techniques and CO2-laser heating. The compositional evolution of Q speciation in these glasses is quantified using (29)Si and (17)O magic angle spinning nuclear magnetic resonance spectroscopy. The results indicate progressive depolymerization of the silicate network upon addition of CaO and significant deviation of the Q speciation from the binary model. The equilibrium constants for the various Q species disproportionation reactions for these glasses are found to be similar to (much smaller than) those characteristic of Li (Mg)-silicate glasses, consistent with the corresponding trends in the field strengths of these modifier cations. Increasing CaO concentration results in an increase in the packing density and structural rigidity of these glasses and consequently in their glass transition temperature Tg. This apparent role reversal of conventional network-modifying cations in invert alkaline-earth silicate glasses are compared and contrasted with that in their alkali silicate counterparts.

  6. Phytochemical analyses of Ziziphus jujuba Mill. var. spinosa seed by ultrahigh performance liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Bao; Yang, Hongshun; Chen, Feng; Hua, Yanglin; Jiang, Yueming

    2013-11-21

    Ziziphus jujuba Mill. var. spinosa (Z. jujuba) seeds have attracted much attention within the field of medicine due to their significant effects against disturbances of the central nervous system. Secondary metabolites composition is key to the influence of the pharmaceutical and commercial qualities of this plant. In this work, the phytochemical profile of Z. jujuba seeds was analysed by ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and gas chromatography-mass spectrometry (GC-MS). The UPLC-MS/MS information identified the main secondary metabolites in Z. jujuba seeds, including flavonoid C-glycosides, triterpene acids and unsaturated fatty acids. The leading chemical identified by UPLC-MS/MS was betulinic acid, and oleic acid was the leading volatile from the GC-MS results. All the samples tested showed similar phytochemical profiles, but levels of the chemical compounds varied. Principal component analysis revealed the principal secondary metabolites that could define the differences in quality. It was confirmed that the combination of UPLC-MS/MS and GC-MS was an effective technique to demonstrate the pharmaceutical quality of Z. jujuba seeds.

  7. Profile of Fatty Acids, Amino Acids, Carotenoid Total, and α-Tocopherol from Flying Fish Eggs

    Directory of Open Access Journals (Sweden)

    Aulia Azka

    2015-12-01

    Full Text Available Flying fish are found in waters of eastern Indonesia, which until now is still limited informationabout nutritional content. The purpose of this research was determine the composition offatty acids, amino acids, total carotenoids, α-tocopherol flying fish eggs (Hyrundicthys sp..The composition of fatty acid was measured by gas chromatography (GC, while amino acids,total carotenoids, α-tocopherol was measured by High performanced Liquid Chromatography(HPLC. Egg contained 22 fatty acids such as saturated fatty acid 29.71%, monounsaturated fattyacid 7.86%, and polysaturated fatty acid 13.64%. The result showed that eggs flying fish contained17 amino acids, such as essential amino acid 14.96% and non-essential amino acids 20.27%. Eggscontained a total carotenoid of 245.37 ppm. α-tocopherol content of flying fish eggs by 1.06 ppm.Keywords: Amino acids, carotenoid total, fatty acid, flying fish egg, α-tocopherol

  8. Development and validation of an ultra-performance liquid chromatography quadrupole time of flight mass spectrometry method for rapid quantification of free amino acids in human urine.

    Science.gov (United States)

    Joyce, Richard; Kuziene, Viktorija; Zou, Xin; Wang, Xueting; Pullen, Frank; Loo, Ruey Leng

    2016-01-01

    An ultra-performance liquid chromatography quadrupole time of flight mass spectrometry (UPLC-qTOF-MS) method using hydrophilic interaction liquid chromatography was developed and validated for simultaneous quantification of 18 free amino acids in urine with a total acquisition time including the column re-equilibration of less than 18 min per sample. This method involves simple sample preparation steps which consisted of 15 times dilution with acetonitrile to give a final composition of 25 % aqueous and 75 % acetonitrile without the need of any derivatization. The dynamic range for our calibration curve is approximately two orders of magnitude (120-fold from the lowest calibration curve point) with good linearity (r (2) ≥ 0.995 for all amino acids). Good separation of all amino acids as well as good intra- and inter-day accuracy (amino acids in the prepared urine samples was found to be stable for 72 h at 4 °C, after one freeze thaw cycle and for up to 4 weeks at -80 °C. We have applied this method to quantify the content of 18 free amino acids in 646 urine samples from a dietary intervention study. We were able to quantify all 18 free amino acids in these urine samples, if they were present at a level above the LOD. We found our method to be reproducible (accuracy and precision were typically <10 % for QCL, QCM and QCH) and the relatively high sample throughput nature of this method potentially makes it a suitable alternative for the analysis of urine samples in clinical setting.

  9. Chromatography.

    Science.gov (United States)

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

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

  10. The stable Cr isotopic compositions of chondrites and silicate planetary reservoirs

    Science.gov (United States)

    Schoenberg, Ronny; Merdian, Alexandra; Holmden, Chris; Kleinhanns, Ilka C.; Haßler, Kathrin; Wille, Martin; Reitter, Elmar

    2016-06-01

    The depletion of chromium in Earth's mantle (∼2700 ppm) in comparison to chondrites (∼4400 ppm) indicates significant incorporation of chromium into the core during our planet's metal-silicate differentiation, assuming that there was no significant escape of the moderately volatile element chromium during the accretionary phase of Earth. Stable Cr isotope compositions - expressed as the ‰-difference in 53Cr/52Cr from the terrestrial reference material SRM979 (δ53/52CrSRM979 values) - of planetary silicate reservoirs might thus yield information about the conditions of planetary metal segregation processes when compared to chondrites. The stable Cr isotopic compositions of 7 carbonaceous chondrites, 11 ordinary chondrites, 5 HED achondrites and 2 martian meteorites determined by a double spike MC-ICP-MS method are within uncertainties indistinguishable from each other and from the previously determined δ53/52CrSRM979 value of -0.124 ± 0.101‰ for the igneous silicate Earth. Extensive quality tests support the accuracy of the stable Cr isotope determinations of various meteorites and terrestrial silicates reported here. The uniformity in stable Cr isotope compositions of samples from planetary silicate mantles and undifferentiated meteorites indicates that metal-silicate differentiation of Earth, Mars and the HED parent body did not cause measurable stable Cr isotope fractionation between these two reservoirs. Our results also imply that the accretionary disc, at least in the inner solar system, was homogeneous in its stable Cr isotopic composition and that potential volatility loss of chromium during accretion of the terrestrial planets was not accompanied by measurable stable isotopic fractionation. Small but reproducible variations in δ53/52CrSRM979 values of terrestrial magmatic rocks point to natural stable Cr isotope variations within Earth's silicate reservoirs. Further and more detailed studies are required to investigate whether silicate

  11. The role of humic acid on the formation of HAS (hydroxy-aluminosilicate) colloid-borne actinides

    Energy Technology Data Exchange (ETDEWEB)

    Priemyshev, A.; Kim, M.A. [Inst. fuer Radiochemie, Technische Universitaet Muenchen, D-85748 Garching (Germany); Breban, D.; Panak, P.J.; Yun, J.I.; Kim, J.I.; Fanghanel, Th. [Inst. fuer Nukleare Entsorgung, Forschungszentrum Karlsruhe, D-76021 Karlsruhe (Germany); Mansel, A. [Inst. fuer Interdisziplinaere Isotopenforschung, Georadiochemie, Leipzig, D-04318 Leipzig (Germany)

    2005-07-01

    Full text of publication follows: One of the major unknowns in the process of actinide migration is the formation of their colloid-borne species. Previous studies have been directed to the incorporation of actinides into HAS (hydroxy-aluminosilicate) colloids generated by the nucleation of Si and Al. The present work further pursues the behaviour of actinides at HAS colloid formation but in the presence of humic acid that is known to be an ubiquitous groundwater constituent. The formation and degree of stability of the aluminosilicate binding for the generation of HAS colloids are investigated at first in the absence of actinides. Free and complexed Al resulting from ligand competitions reactions for the complexation of Al with mono-silicic acid, poly-silicic acid and EDTA are monitored spectroscopically by colour reaction. The second part of the study concentrates on the formation and stability of humic colloids using {sup 14}C-labeled humic acid. The activity distribution is ascertained in the ionic, colloidal and precipitated fractions under different conditions of colloid formation, e.g. as a function of pH, time, humic acid and Al concentration. The third part follows the appraisal of appropriate conditions under which stable HAS and humic colloids are formed, and their interaction with actinides, either separately or in competition. Trace actinides of different oxidation states {sup 241}Am(III), {sup 234}Th(IV) and {sup 233}U(VI) are taken for the purpose. HAS colloids generated from poly-silicic acid at neutral pH show EDTA-resistance, whereas HAS colloids formed from mono-silicic acid become EDTA-resistant only by aging (> one month). Humic acid appears to stabilize HAS colloids, unless the loading capacity of humic acid for the Al ion is exceeded. The incorporation of actinides into the colloidal phase is generally enhanced in the presence of humic acid. Synergic effects produce chimeric HAS-humic colloids into which tri-, tetra- and hexavalent actinides

  12. Non-conservative controls on distribution of dissolved silicate in Cochin Backwaters

    Digital Repository Service at National Institute of Oceanography (India)

    Balachandran, K.K.; Sankaranarayanan, V.N.; Joseph, T.; Nair, M.

    Cochin backwater system was studied with regard to dissolved silicate (DSi) to understand its seasonal distribution and behaviour during estuarine mixing. Silicate had a linear relationship with salinity during the high river discharge period...

  13. E-Beam-Cured Layered-Silicate and Spherical Silica Epoxy Nanocomposites (Preprint)

    National Research Council Canada - National Science Library

    Chen, Chenggang; Anderson, David P

    2007-01-01

    .... The nanofillers can be two dimensional (layered-silicate) and zero dimensional (spherical silica). Both the spherical silica epoxy nanocomposite and the layered-silicate epoxy nanocomposite can be cured to a high degree of curing...

  14. [Measurement of sialic acid from lipoproteins and human plasma by liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Guo, Shoudong; Sang, Hui; Yang, Nana; Kan, Yujie; Li, Fuyu; Li, Yu; Li, Fangyuan; Qin, Shucun

    2014-11-01

    A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was established to quantify sialic acid (N-acetylneuraminic acid, NANA) from lipoproteins and human plasma. The method was used to investigate the different contents of NANA from lipoproteins between diabetic with an average age of 51.6 years and healthy participants with an average age of 50.7 years. The NANA from lipoprotein samples was hydrolyzed by acetic acid (pH = 2) at 80 °C for 2 h and analyzed by the optimized LC-MS/MS method after high speed centrifugation and filtration. The limits of detection and quantification of NANA were 7.4 and 24.5 pg, respectively. The linear range was 2.5-80 ng/mL for NANA and the correlation coefficient (R2) was more than 0.998. The levels of NANA in the plasma of type II diabetics and healthy participants were (548.3 ± 88.9) and (415.3 ± 55.5) mg/L, respectively; and the levels of NANA from very low density lipoproteins (VLDL), low density lipoproteins (LDL), and high density lipoproteins (HDL) of the type II diabetics and the healthy participants were (4.91 ± 0.19), (6.95 ± 0.28), (3.61 ± 0.22) μg/mg and (2.90 ± 0.27), (7.03 ± 0.04), (2.40 ± 0.09) μg/mg, respectively. The sialic acid levels of VLDL and HDL from the type II diabetics were markedly higher than those of the corresponding healthy participants with the similar ages (P lipoproteins, and is reproducible and time saving.

  15. SOFT X-RAY IRRADIATION OF SILICATES: IMPLICATIONS FOR DUST EVOLUTION IN PROTOPLANETARY DISKS

    Energy Technology Data Exchange (ETDEWEB)

    Ciaravella, A.; Cecchi-Pestellini, C.; Jiménez-Escobar, A. [INAF—Osservatorio Astronomico di Palermo, P.za Parlamento 1, I-90134 Palermo (Italy); Chen, Y.-J.; Huang, C.-H. [Department of Physics, National Central University, Jhongli City, Taoyuan County 32054, Taiwan (China); Muñoz Caro, G. M. [Centro de Astrobiología (INTA-CSIC), Carretera de Ajalvir, km 4, Torrejón de Ardoz, E-28850 Madrid (Spain); Venezia, A. M., E-mail: aciaravella@astropa.unipa.it [ISMN—CNR, Via Ugo La Malfa 153, I-90146 Palermo (Italy)

    2016-09-01

    The processing of energetic photons on bare silicate grains was simulated experimentally on silicate films submitted to soft X-rays of energies up to 1.25 keV. The silicate material was prepared by means of a microwave assisted sol–gel technique. Its chemical composition reflects the Mg{sub 2}SiO{sub 4} stoichiometry with residual impurities due to the synthesis method. The experiments were performed using the spherical grating monochromator beamline at the National Synchrotron Radiation Research Center in Taiwan. We found that soft X-ray irradiation induces structural changes that can be interpreted as an amorphization of the processed silicate material. The present results may have relevant implications in the evolution of silicate materials in X-ray-irradiated protoplanetary disks.

  16. Pore solution in alkali-activated slag cement pastes. Relation to the composition and structure of calcium silicate hydrate

    International Nuclear Information System (INIS)

    Puertas, F.; Fernandez-Jimenez, A.; Blanco-Varela, M.T.

    2004-01-01

    In this work, the relationship between the composition of pore solution in alkali-activated slag cement (AAS) pastes activated with different alkaline activator, and the composition and structure of the main reaction products, has been studied. Pore solution was extracted from hardened AAS pastes. The analysis of the liquids was performed through different techniques: Na, Mg and Al by atomic absorption (AA), Ca ions by ionic chromatography (IC) and Si by colorimetry; pH was also determined. The solid phases were analysed by XRD, FTIR, solid-state 29 Si and 27 Al NMR and BSE/EDX. The most significant changes in the ionic composition of the pore solution of the AAS pastes activated with waterglass take place between 3 and 24 h of reaction. These changes are due to the decrease of the Na content and mainly to the Si content. Results of 29 Si MAS NMR and FTIR confirm that the activation process takes place with more intensity after 3 h (although at this age, Q 2 units already exist). The pore solution of the AAS pastes activated with NaOH shows a different evolution to this of pastes activated with waterglass. The decrease of Na and Si contents progresses with time. The nature of the alkaline activator influences the structure and composition of the calcium silicate hydrate formed as a consequence of the alkaline activation of the slag. The characteristic of calcium silicate hydrate in AAS pastes activated with waterglass is characterised by a low structural order with a low Ca/Si ratio. Besides, in this paste, Q 3 units are detected. The calcium silicate hydrate formed in the pastes activated with NaOH has a higher structural order (higher crystallinity) and contains more Al in its structure and a higher Ca/Si ratio than those obtained with waterglass

  17. Rapid Determination of Two Triterpenoid Acids in Chaenomelis Fructus Using Supercritical Fluid Extraction On-line Coupled with Supercritical Fluid Chromatography.

    Science.gov (United States)

    Zhang, Xiaotian; Ji, Feng; Li, Yueqi; He, Tian; Han, Ya; Wang, Daidong; Lin, Zongtao; Chen, Shizhong

    2018-01-01

    In this study, an on-line supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) method was developed for the rapid determination of oleanoic acid and ursolic acid in Chaenomelis Fructus. After optimization of the conditions, the two triterpenoid acids was obtained by SFE using 20% methanol as a modifier at 35°C in 8 min. They were resolved on a Shim-pack UC-X Diol column (4.6 × 150 mm, 3 μm) in 14 min (0 - 10 min, 5 - 10%; 10 - 14 min, 10% methanol in CO 2 ) with a backpressure of 15 MPa at 40°C. The on-line SFE-SFC method could be completed within 40 min (10.79 mg/g dry plant, R s = 2.36), while the ultrasound-assisted extraction and HPLC method required at least 90 min (3.55 mg/g dry plant, R s = 1.92). This on-line SFE-SFC method is powerful to simplify the pre-processing and quantitative analysis of natural products.

  18. Application of cyanuric chloride-based six new chiral derivatizing reagents having amino acids and amino acid amides as chiral auxiliaries for enantioresolution of proteinogenic amino acids by reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Bhushan, Ravi; Dixit, Shuchi

    2012-04-01

    Six dichloro-s-triazine (DCT) reagents having L-Leu, D-Phg, L-Val, L-Met, L-Ala and L-Met-NH(2) as chiral auxiliaries in cyanuric chloride were introduced for enantioseparation of 13 proteinogenic amino acids. Four other DCTs and six monochloro-s-triazine (MCT) reagents having amino acid amides as chiral auxiliaries were also synthesized. These 16 chiral derivatizing reagents (CDRs) were used for synthesis of diastereomers of all the 13 analytes using microwave irradiation, which were resolved by reversed-phase high-performance liquid chromatography (RP-HPLC) using C18 column and gradient eluting mixture of aqueous TFA and acetonitrile with UV detection at 230 nm. It required only 60-90 s for derivatization using microwave irradiation. Better resolution and lower retention times were observed for the diastereomers prepared with CDRs having amino acids as chiral auxiliaries as compared to counterparts prepared with reagents having amino acid amides as chiral auxiliaries. As the best resolution of all the 13 analytes was observed for their diastereomers prepared using the DCT reagent having L-Leu as chiral auxiliary, this CDR was further employed for derivatization of Lys, Tyr, His and Arg followed by RP-HPLC analysis of resulting diastereomers. The results are discussed in light of acid and amide groups of chiral auxiliaries constituting CDRs, electronegativities of the atoms of achiral moieties constituting CDRs and hydrophobicities of side chains of amino acids constituting CDRs and analytes.

  19. Extraction chromatography of Am (III), Eu (III), Zn (II), and Cs (I), Using chromo sorb impregnated by 0..01 m 2-heptyl-2-methyl-nonanoic acid in benzene. Vol. 3

    Energy Technology Data Exchange (ETDEWEB)

    El-naggar, H A; Ramadan, A; Abdel-Fattah, A [Nuclear chemistry Department, Hot laboratories Center, Atomic Energy Authority, Cairo (Egypt)

    1996-03-01

    Extraction chromatography studies were carried out for Am(III), Eu(III), Zn(II), and Cs(I) using long carboxylic acid, 2-heptyl-2-methyl nonanoic acid in benzene as an extractant chromo sorb. This was selected to act as a solid support and it was impregnated with the extractant to obtain the stationary phase. The eluting agent used was 0.1 m H N O{sub 3}. The investigation included primarily the extraction chromatography of the individual elements concerned and their elution peaks which were plotted. Group separation of the four elements into two pairs was obtained Am-Eu, and Zn-Cs. A mixture of the four elements was loaded on the column to achieve practically such promising group separations. 5 figs.

  20. Extraction chromatography of Am (III), Eu (III), Zn (II), and Cs (I), Using chromo sorb impregnated by 0..01 m 2-heptyl-2-methyl-nonanoic acid in benzene. Vol. 3

    International Nuclear Information System (INIS)

    El-naggar, H.A.; Ramadan, A.; Abdel-Fattah, A.

    1996-01-01

    Extraction chromatography studies were carried out for Am(III), Eu(III), Zn(II), and Cs(I) using long carboxylic acid, 2-heptyl-2-methyl nonanoic acid in benzene as an extractant chromo sorb. This was selected to act as a solid support and it was impregnated with the extractant to obtain the stationary phase. The eluting agent used was 0.1 m H N O 3 . The investigation included primarily the extraction chromatography of the individual elements concerned and their elution peaks which were plotted. Group separation of the four elements into two pairs was obtained Am-Eu, and Zn-Cs. A mixture of the four elements was loaded on the column to achieve practically such promising group separations. 5 figs

  1. Improved fatty acid detection in micro-algae and aquatic meiofauna species using a direct thermal desorption interface combined with comprehensive gas chromatography-time-of-flight mass spectrometry

    NARCIS (Netherlands)

    Akoto, L.; Stellaard, F.; Irth, H.; Vreuls, R.J.J.; Pel, R.

    2008-01-01

    Comprehensive two-dimensional gas chromatography (GC × GC) with time-of-flight mass spectrometry detection is used to profile the fatty acid composition of whole/intact aquatic microorganisms such as the common fresh water green algae Scenedesmus acutus and the filamentous cyanobacterium Limnothrix

  2. Improved fatty acid detection in micro-algae and aquatic meiofauna species using a direct thermal desorption interface combined with comprehensive gas chromatography-time-of-flight mass spectrometry

    NARCIS (Netherlands)

    Akoto, Lawrence; Stellaard, Frans; Irth, Hubertus; Vreuls, Rene J. J.; Pel, Roel

    2008-01-01

    Comprehensive two-dimensional gas chromatography (GC x GC) with time-of-flight mass spectrometry detection is used to profile the fatty acid composition of whole/intact aquatic microorganisms such as the common fresh water green algae Scenedesmus acutus and the filamentous cyanobacterium Limnothrix

  3. Sorption of Europium in zirconium silicate

    International Nuclear Information System (INIS)

    Garcia R, G.

    2004-01-01

    Some minerals have the property of sipping radioactive metals in solution, that it takes advantage to manufacture contention barriers that are placed in the repositories of nuclear wastes. The more recent investigations are focused in the development of new technologies guided to the sorption of alpha emissors on minerals which avoid their dispersion in the environment. In an effort to contribute to the understanding of this type of properties, some studies of sorption of Europium III are presented like homologous of the americium, on the surface of zirconium silicate (ZrSiO 4 ). In this work the results of sorption experiences are presented as well as the interpretation of the phenomena of the formation of species in the surface of the zirconium silicate. (Author)

  4. Effects of ionization on silicate glasses

    International Nuclear Information System (INIS)

    Primak, W.

    1982-02-01

    This evaluation of radiation effects in silicate glasses caused by ionization is based on our own investigations, on material collected in our files (reports, articles, and notes), and on a computer literature search through recent issues of Physics Abstracts and Chemical Abstracts (and the apparently pertinent references which appeared). Some of our recent results, available heretofore only in internal correspondence, are presented in some detail. It is concluded that research into the behavior of silicate glasses generally will be required before the specific effects in the radioactive waste storage glasses can be properly understood and evaluated. Two particular neglected areas of investigation are targeted for immediate concern: a kinetic analysis of annealing data and the acquisition of data on effects of irradiation at controlled elevated temperatures

  5. Analysis of oak tannins by liquid chromatography-electrospray ionisation mass spectrometry.

    Science.gov (United States)

    Mämmelä, P; Savolainen, H; Lindroos, L; Kangas, J; Vartiainen, T

    2000-09-01

    Extractable tannins were analysed by liquid chromatography-electrospray ionisation mass spectrometry in two oak species, North American white oak (Quercus alba) and European red oak (Quercus robur). They mainly included various glucose gallic and ellagic acid esters. The structures were partially determined, and they included grandinin/roburin E, castalagin/vescalagin, gallic acid, valoneic acid bilactone, monogalloyl glucose, digalloyl glucose, trigalloyl glucose, ellagic acid rhamnose, quercitrin and ellagic acid.

  6. Non-polar lipids characterization of Quinoa (Chenopodium quinoa) seed by comprehensive two-dimensional gas chromatography with flame ionization/mass spectrometry detection and non-aqueous reversed-phase liquid chromatography with atmospheric pressure chemical ionization mass spectrometry detection.

    Science.gov (United States)

    Fanali, Chiara; Beccaria, Marco; Salivo, Simona; Tranchida, Peter; Tripodo, Giusy; Farnetti, Sara; Dugo, Laura; Dugo, Paola; Mondello, Luigi

    2015-07-08

    A chemical characterization of major lipid components, namely, triacylglycerols, fatty acids and the unsaponifiable fraction, in a Quinoa seed lipids sample is reported. To tackle such a task, non-aqueous reversed-phase high-performance liquid chromatography with mass spectrometry detection was employed. The latter was interfaced with atmospheric pressure chemical ionization for the analysis of triacylglycerols. The main triacylglycerols (>10%) were represented by OLP, OOL and OLL (P = palmitoyl, O = oleoyl, L = linoleoyl); the latter was present in the oil sample at the highest percentage (18.1%). Furthermore, fatty acid methyl esters were evaluated by gas chromatography with flame ionization detection. 89% of the total fatty acids was represented by unsaturated fatty acid methyl esters with the greatest percentage represented by linoleic and oleic acids accounting for approximately 48 and 28%, respectively. An extensive characterization of the unsaponifiable fraction of Quinoa seed lipids was performed for the first time, by using comprehensive two-dimensional gas chromatography with dual mass spectrometry/flame ionization detection. Overall, 66 compounds of the unsaponifiable fraction were tentatively identified, many constituents of which (particularly sterols) were confirmed by using gas chromatography with high-resolution time-of-flight mass spectrometry. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Modern Aspects Of Fluorometric Detection In Liquid-Phase Chromatography

    Science.gov (United States)

    Bousquet, Bernard; Garnier, Jean P.; Dreux, Claude

    1983-10-01

    Recent advances are described in the combined use of fluorometric derivatization and high performance liquid chromatography (HPLC) for clinical chemistry determinations. Derivatives (especially dansyl derivatives) can be formed prior to chromatography in the case of estrogens, amino acids, and catecholamines. In post-column reactions, we preferred to use air-segmented reactions as they conform better to all the optimized chromatographic and spectrofluorometric parameters. Fluorescent derivatives produced from cate-cholamines, tryptophan and its metabolites, hydroxyindoles, tryptamine, amino acids, sugars, polyamines, and other substances are often sufficiently sensitive to be detected in picogram quantities by HPLC. Their reaction principle and some of their applications to samples are described. Recently, chemical excitation of fluorophore-like dansyl amino acid was proposed as a detection system for HPLC. By a post-column reaction, a fluorophore can be made to emit light by its reaction with trichlorophenyl oxalate (TCPO) and hydrogen peroxide. The detection limit of this system is about 10 fmol for each dansyl amino acid. Application of this new reaction to catecholamines opens up new prospects for fluorometric detection.

  8. Nicotine–magnesium aluminum silicate microparticle surface modified with chitosan for mucosal delivery

    Energy Technology Data Exchange (ETDEWEB)

    Kanjanakawinkul, Watchara [Faculty of Pharmaceutical Sciences, Khon Kaen University, Khon Kaen 40002 (Thailand); Rades, Thomas [School of Pharmacy, University of Otago, Dunedin 9054 (New Zealand); Department of Pharmacy, Faculty of Health and Medical Sciences, University of Copenhagen, DK-2100 Copenhagen (Denmark); Puttipipatkhachorn, Satit [Department of Manufacturing Pharmacy, Faculty of Pharmacy, Mahidol University, Bangkok 10400 (Thailand); Pongjanyakul, Thaned, E-mail: thaned@kku.ac.th [Faculty of Pharmaceutical Sciences, Khon Kaen University, Khon Kaen 40002 (Thailand)

    2013-04-01

    Magnesium aluminum silicate (MAS), a negatively charged clay, and nicotine (NCT), a basic drug, can interact electrostatically to form microparticles. Chitosan (CS) was used for the surface modification of the microparticles, and a lyophilization method was used to preserve the original particle morphology. The microparticles were characterized in terms of their physicochemical properties, NCT content, mucoadhesive properties, and release and permeation across porcine esophageal mucosa. The results showed that the microparticles formed via electrostatic interaction between MAS and protonated NCT had an irregular shape and that their NCT content increased with increasing NCT ratios in the microparticle preparation solution. High molecular weight CS (800 kDa) adsorbed to the microparticle surface and induced a positive surface charge. CS molecules intercalated into the MAS silicate layers and decreased the crystallinity of the microparticles, leading to an increase in the release rate and diffusion coefficient of NCT from the microparticles. Moreover, the microparticle surface modified with CS was found to have higher NCT permeation fluxes and mucoadhesive properties, which indicated the significant role of CS for NCT mucosal delivery. However, the enhancement of NCT permeation and of mucoadhesive properties depended on the molecular weight and concentration of CS. These findings suggest that NCT-MAS microparticle surface modified with CS represents a promising mucosal delivery system for NCT. Highlights: ► Nicotine–magnesium aluminum silicate microparticles were prepared using electrostatic interaction. ► Lyophilization was used for drying and maintaining an original morphology of the microparticles. ► Chitosan (CS) was used for surface modification of the microparticles at acidic pH. ► Surface modification using CS caused an increase in release and permeation of nicotine. ► Microparticle surface-modified with CS presented better mucoadhesive properties.

  9. Nicotine–magnesium aluminum silicate microparticle surface modified with chitosan for mucosal delivery

    International Nuclear Information System (INIS)

    Kanjanakawinkul, Watchara; Rades, Thomas; Puttipipatkhachorn, Satit; Pongjanyakul, Thaned

    2013-01-01

    Magnesium aluminum silicate (MAS), a negatively charged clay, and nicotine (NCT), a basic drug, can interact electrostatically to form microparticles. Chitosan (CS) was used for the surface modification of the microparticles, and a lyophilization method was used to preserve the original particle morphology. The microparticles were characterized in terms of their physicochemical properties, NCT content, mucoadhesive properties, and release and permeation across porcine esophageal mucosa. The results showed that the microparticles formed via electrostatic interaction between MAS and protonated NCT had an irregular shape and that their NCT content increased with increasing NCT ratios in the microparticle preparation solution. High molecular weight CS (800 kDa) adsorbed to the microparticle surface and induced a positive surface charge. CS molecules intercalated into the MAS silicate layers and decreased the crystallinity of the microparticles, leading to an increase in the release rate and diffusion coefficient of NCT from the microparticles. Moreover, the microparticle surface modified with CS was found to have higher NCT permeation fluxes and mucoadhesive properties, which indicated the significant role of CS for NCT mucosal delivery. However, the enhancement of NCT permeation and of mucoadhesive properties depended on the molecular weight and concentration of CS. These findings suggest that NCT-MAS microparticle surface modified with CS represents a promising mucosal delivery system for NCT. Highlights: ► Nicotine–magnesium aluminum silicate microparticles were prepared using electrostatic interaction. ► Lyophilization was used for drying and maintaining an original morphology of the microparticles. ► Chitosan (CS) was used for surface modification of the microparticles at acidic pH. ► Surface modification using CS caused an increase in release and permeation of nicotine. ► Microparticle surface-modified with CS presented better mucoadhesive properties

  10. Detection of lysergic acid diethylamide (LSD) in urine by gas chromatography-ion trap tandem mass spectrometry.

    Science.gov (United States)

    Sklerov, J H; Kalasinsky, K S; Ehorn, C A

    1999-10-01

    A confirmatory method for the detection and quantitation of lysergic acid diethylamide (LSD) is presented. The method employs gas chromatography-tandem mass spectrometry (GC-MS-MS) using an internal ionization ion trap detector for sensitive MS-MS-in-time measurements of LSD extracted from urine. Following a single-step solid-phase extraction of 5 mL of urine, underivatized LSD can be measured with limits of quantitation and detection of 80 and 20 pg/mL, respectively. Temperature-programmed on-column injections of urine extracts were linear over the concentration range 20-2000 pg/mL (r2 = 0.999). Intraday and interday coefficients of variation were LSD-positive samples in this laboratory. Comparisons with alternate GC-MS methods and extraction procedures are discussed.

  11. Optimal design and experimental validation of a simulated moving bed chromatography for continuous recovery of formic acid in a model mixture of three organic acids from Actinobacillus bacteria fermentation.

    Science.gov (United States)

    Park, Chanhun; Nam, Hee-Geun; Lee, Ki Bong; Mun, Sungyong

    2014-10-24

    The economically-efficient separation of formic acid from acetic acid and succinic acid has been a key issue in the production of formic acid with the Actinobacillus bacteria fermentation. To address this issue, an optimal three-zone simulated moving bed (SMB) chromatography for continuous separation of formic acid from acetic acid and succinic acid was developed in this study. As a first step for this task, the adsorption isotherm and mass-transfer parameters of each organic acid on the qualified adsorbent (Amberchrom-CG300C) were determined through a series of multiple frontal experiments. The determined parameters were then used in optimizing the SMB process for the considered separation. During such optimization, the additional investigation for selecting a proper SMB port configuration, which could be more advantageous for attaining better process performances, was carried out between two possible configurations. It was found that if the properly selected port configuration was adopted in the SMB of interest, the throughout and the formic-acid product concentration could be increased by 82% and 181% respectively. Finally, the optimized SMB process based on the properly selected port configuration was tested experimentally using a self-assembled SMB unit with three zones. The SMB experimental results and the relevant computer simulation verified that the developed process in this study was successful in continuous recovery of formic acid from a ternary organic-acid mixture of interest with high throughput, high purity, high yield, and high product concentration. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. A Search for Amino Acids and Nucleobases in the Martian Meteorite Roberts Massif 04262 Using Liquid Chromatography-Mass Spectrometry

    Science.gov (United States)

    Callahan, Michael P.; Burton, Aaron S.; Elsila, Jamie E.; Baker, Eleni M.; Smith, Karen E.; Glavin, Daniel P.; Dworkin, Jason P.

    2013-01-01

    The investigation into whether Mars contains signatures of past or present life is of great interest to science and society. Amino acids and nucleobases are compounds that are essential for all known life on Earth and are excellent target molecules in the search for potential Martian biomarkers or prebiotic chemistry. Martian meteorites represent the only samples from Mars that can be studied directly in the laboratory on Earth. Here, we analyzed the amino acid and nucleobase content of the shergottite Roberts Massif (RBT) 04262 using liquid chromatography-mass spectrometry. We did not detect any nucleobases above our detection limit in formic acid extracts; however, we did measure a suite of protein and nonprotein amino acids in hot-water extracts with high relative abundances of beta-alanine and gamma-amino-eta-butyric acid. The presence of only low (to absent) levels of several proteinogenic amino acids and a lack of nucleobases suggest that this meteorite fragment is fairly uncontaminated with respect to these common biological compounds. The distribution of straight-chained amine-terminal eta-omega-amino acids in RBT 04262 resembled those previously measured in thermally altered carbonaceous meteorites. A carbon isotope ratio of -24(0/00) +/- 6(0/00) for beta-alanine in RBT 04262 is in the range of reduced organic carbon previously measured in Martian meteorites (Steele et al. 2012). The presence of eta-omega-amino acids may be due to a high temperature Fischer-Tropschtype synthesis during igneous processing on Mars or impact ejection of the meteorites from Mars, but more experimental data are needed to support these hypotheses.

  13. Brain aluminium accumulation and oxidative stress in the presence of calcium silicate dental cements.

    Science.gov (United States)

    Demirkaya, K; Demirdöğen, B Can; Torun, Z Öncel; Erdem, O; Çırak, E; Tunca, Y M

    2017-10-01

    Mineral trioxide aggregate (MTA) is a calcium silicate dental cement used for various applications in dentistry. This study was undertaken to test whether the presence of three commercial brands of calcium silicate dental cements in the dental extraction socket of rats would affect the brain aluminium (Al) levels and oxidative stress parameters. Right upper incisor was extracted and polyethylene tubes filled with MTA Angelus, MTA Fillapex or Theracal LC, or left empty for the control group, were inserted into the extraction socket. Rats were killed 7, 30 or 60 days after operation. Brain tissues were obtained before killing. Al levels were measured by atomic absorption spectrometry. Thiobarbituric acid reactive substances (TBARS) levels, catalase (CAT), superoxide dismutase (SOD) and glutathione peroxidase (GPx) activities were determined using spectrophotometry. A transient peak was observed in brain Al level of MTA Angelus group on day 7, while MTA Fillapex and Theracal LC groups reached highest brain Al level on day 60. Brain TBARS level, CAT, SOD and GPx activities transiently increased on day 7 and then returned to almost normal levels. This in vivo study for the first time indicated that initial washout may have occurred in MTA Angelus, while element leaching after the setting is complete may have taken place for MTA Fillapex and Theracal LC. Moreover, oxidative stress was induced and antioxidant enzymes were transiently upregulated. Further studies to search for oxidative neuronal damage should be done to completely understand the possible toxic effects of calcium silicate cements on the brain.

  14. Obtainment and characterization of pure and doped gadolinium oxy ortho silicates with terbium III, precursor of luminescent silicates with sulphur

    International Nuclear Information System (INIS)

    Simoneti, J.A.

    1992-01-01

    Silicate and sulfide lattices are uniquely efficient luminescent materials to excitation by cathodic rays and furthermore the cathodoluminescence study of these compounds have been few investigated. In this work it has been prepared, characterized and investigated some spectroscopic properties of pure and Tb a+ - activated Gd 2 Si O 3 system and it has been tried to substitute oxygen by sulphur in order to obtain this or sulfide-silicate lattices. Products were characterized by vibrational infrared spectroscopy, powder X-ray diffraction patterns and electronic emission in UV-VIS region. (author)

  15. Wind-Eroded Silicate as a Source of Hydrogen Peroxide on Mars

    Science.gov (United States)

    Bak, E. N.; Merrison, J. P.; Jensen, S. K.; Nørnberg, P.; Finster, K.

    2014-07-01

    Laboratory simulations show that wind-eroded silicate can be a source of hydrogen peroxide. The ubiquitous, fine-grained silicate dust might thus explain the oxidizing properties of the martian soil and affect the preservation of organic compounds.

  16. Application of Sodium Silicate Enhances Cucumber Resistance to Fusarium Wilt and Alters Soil Microbial Communities

    Directory of Open Access Journals (Sweden)

    Xingang Zhou

    2018-05-01

    Full Text Available Exogenous silicates can enhance plant resistance to pathogens and change soil microbial communities. However, the relationship between changes in soil microbial communities and enhanced plant resistance remains unclear. Here, effects of exogenous sodium silicate on cucumber (Cucumis sativus L. seedling resistance to Fusarium wilt caused by the soil-borne pathogen Fusarium oxysporum f.sp. cucumerinum Owen (FOC were investigated by drenching soil with 2 mM sodium silicate. Soil bacterial and fungal community abundances and compositions were estimated by real-time PCR and high-throughput amplicon sequencing; then, feedback effects of changes in soil biota on cucumber seedling resistance to FOC were assessed. Moreover, effects of sodium silicate on the growth of FOC and Streptomyces DHV3-2, an antagonistic bacterium to FOC, were investigated both in vitro and in the soil environment. Results showed that exogenous sodium silicate enhanced cucumber seedling growth and resistance to FOC. In bare soil, sodium silicate increased bacterial and fungal community abundances and diversities. In cucumber-cultivated soil, sodium silicate increased bacterial community abundances, but decreased fungal community abundances and diversities. Sodium silicate also changed soil bacterial and fungal communality compositions, and especially, decreased the relative abundances of microbial taxa containing plant pathogens but increased these with plant-beneficial potentials. Moreover, sodium silicate increased the abundance of Streptomyces DHV3-2 in soil. Soil biota from cucumber-cultivated soil treated with sodium silicate decreased cucumber seedling Fusarium wilt disease index, and enhanced cucumber seedling growth and defense-related enzyme activities in roots. Sodium silicate at pH 9.85 inhibited FOC abundance in vitro, but did not affect FOC abundance in soil. Overall, our results suggested that, in cucumber-cultivated soil, sodium silicate increased cucumber seedling

  17. Experimental evidence for Mo isotope fractionation between metal and silicate liquids

    Science.gov (United States)

    Hin, Remco C.; Burkhardt, Christoph; Schmidt, Max W.; Bourdon, Bernard; Kleine, Thorsten

    2013-10-01

    Stable isotope fractionation of siderophile elements may inform on the conditions and chemical consequences of core-mantle differentiation in planetary objects. The extent to which Mo isotopes fractionate during such metal-silicate segregation, however, is so far unexplored. We have therefore investigated equilibrium fractionation of Mo isotopes between liquid metal and liquid silicate to evaluate the potential of Mo isotopes as a new tool to study core formation. We have performed experiments at 1400 and 1600 °C in a centrifuging piston cylinder. Tin was used to lower the melting temperature of the Fe-based metal alloys to double spike technique. In experiments performed at 1400 °C, the 98Mo/95Mo ratio of silicate is 0.19±0.03‰ (95% confidence interval) heavier than that of metal. This fractionation is not significantly affected by the presence or absence of carbon. Molybdenum isotope fractionation is furthermore independent of oxygen fugacity in the range IW -1.79 to IW +0.47, which are plausible values for core formation. Experiments at 1600 °C show that, at equilibrium, the 98Mo/95Mo ratio of silicate is 0.12±0.02‰ heavier than that of metal and that the presence or absence of Sn does not affect this fractionation. Equilibrium Mo isotope fractionation between liquid metal and liquid silicate as a function of temperature can therefore be described as ΔMoMetal-Silicate98/95=-4.70(±0.59)×105/T2. Our experiments show that Mo isotope fractionation may be resolvable up to metal-silicate equilibration temperatures of about 2500 °C, rendering Mo isotopes a novel tool to investigate the conditions of core formation in objects ranging from planetesimals to Earth sized bodies.

  18. Polymer/Silicate Nanocomposites Developed for Improved Strength and Thermal Stability

    Science.gov (United States)

    Campbell, Sandi G.

    2003-01-01

    Over the past decade, polymer-silicate nanocomposites have been attracting considerable attention as a method of enhancing polymer properties. The nanometer dimensions of the dispersed silicate reinforcement can greatly improve the mechanical, thermal, and gas barrier properties of a polymer matrix. In a study at the NASA Glenn Research Center, the dispersion of small amounts (less than 5 wt%) of an organically modified layered silicate (OLS) into the polymer matrix of a carbon-fiber-reinforced composite has improved the thermal stability of the composite. The enhanced barrier properties of the polymer-clay hybrid are believed to slow the diffusion of oxygen into the bulk polymer, thereby slowing oxidative degradation of the polymer. Electron-backscattering images show cracking of a nanocomposite matrix composite in comparison to a neat resin matrix composite. The images show that dispersion of an OLS into the matrix resin reduces polymer oxidation during aging and reduces the amount of cracking in the matrix significantly. Improvements in composite flexural strength, flexural modulus, and interlaminar shear strength were also obtained with the addition of OLS. An increase of up to 15 percent in these mechanical properties was observed in composites tested at room temperature and 288 C. The best properties were seen with low silicate levels, 1 to 3 wt%, because of the better dispersion of the silicate in the polymer matrix.

  19. Relationships between mineralization and silicic volcanism in the central Andes

    Energy Technology Data Exchange (ETDEWEB)

    Francis, P.W.; Halls, C.; Baker, M.C.W.

    1983-10-01

    Studies of late Tertiary silicic volcanic centers in the Western and Eastern Cordilleras of the Central Andes show that three volcanic environments are appropriate sites for mineralization: (1) ring-fracture extrusions post-dating large calderas; (2) similar extrusions within ignimbrite shields; and (3) isolated, small silicic volcanoes. Subvolcanic tin mineralization in the Eastern Cordillera is located in silicic stocks and associated breccias of Miocene age. The Cerro Rico stock, Potosi, Bolivia, contains tin and silver mineralization and has an intrusion age apparently millions of years younger than that of the associated Kari Kari caldera. Similar age relationships between mineralization and caldera formation have been described from the San Juan province, Colorado. The vein deposits of Chocaya, southern Bolivia, were emplaced in the lower part of an ignimbrite shield, a type of volcanic edifice as yet unrecognized in comparable areas of silicic volcanism. The El Salvador porphyry copper deposit, Chile, is related to silicic stocks which may have been intruded along a caldera ring fracture. Existing models for the genesis of porphyry copper deposits suggest that they formed in granodioritic stocks located in the infrastructure of andesitic stratovolcanoes. The dome of La Soufriere, Guadeloupe is proposed as a modern analog for the surface expression of subvolcanic mineralization processes, the phreatic eruptions there suggesting the formation of hydrothermal breccia bodies in depth.

  20. Synthesis, characterization and modelling of zinc and silicate co-substituted hydroxyapatite.

    Science.gov (United States)

    Friederichs, Robert J; Chappell, Helen F; Shepherd, David V; Best, Serena M

    2015-07-06

    Experimental chemistry and atomic modelling studies were performed here to investigate a novel ionic co-substitution in hydroxyapatite (HA). Zinc, silicate co-substituted HA (ZnSiHA) remained phase pure after heating to 1100 °C with Zn and Si amounts of 0.6 wt% and 1.2 wt%, respectively. Unique lattice expansions in ZnSiHA, silicate Fourier transform infrared peaks and changes to the hydroxyl IR stretching region suggested Zn and silicate co-substitution in ZnSiHA. Zn and silicate insertion into HA was modelled using density functional theory (DFT). Different scenarios were considered where Zn substituted for different calcium sites or at a 2b site along the c-axis, which was suspected in singly substituted ZnHA. The most energetically favourable site in ZnSiHA was Zn positioned at a previously unreported interstitial site just off the c-axis near a silicate tetrahedron sitting on a phosphate site. A combination of experimental chemistry and DFT modelling provided insight into these complex co-substituted calcium phosphates that could find biomedical application as a synthetic bone mineral substitute. © 2015 The Author(s) Published by the Royal Society. All rights reserved.

  1. Synthesis, characterization and modelling of zinc and silicate co-substituted hydroxyapatite

    Science.gov (United States)

    Friederichs, Robert J.; Chappell, Helen F.; Shepherd, David V.; Best, Serena M.

    2015-01-01

    Experimental chemistry and atomic modelling studies were performed here to investigate a novel ionic co-substitution in hydroxyapatite (HA). Zinc, silicate co-substituted HA (ZnSiHA) remained phase pure after heating to 1100°C with Zn and Si amounts of 0.6 wt% and 1.2 wt%, respectively. Unique lattice expansions in ZnSiHA, silicate Fourier transform infrared peaks and changes to the hydroxyl IR stretching region suggested Zn and silicate co-substitution in ZnSiHA. Zn and silicate insertion into HA was modelled using density functional theory (DFT). Different scenarios were considered where Zn substituted for different calcium sites or at a 2b site along the c-axis, which was suspected in singly substituted ZnHA. The most energetically favourable site in ZnSiHA was Zn positioned at a previously unreported interstitial site just off the c-axis near a silicate tetrahedron sitting on a phosphate site. A combination of experimental chemistry and DFT modelling provided insight into these complex co-substituted calcium phosphates that could find biomedical application as a synthetic bone mineral substitute. PMID:26040597

  2. High-throughput and sensitive analysis of 3-monochloropropane-1,2-diol fatty acid esters in edible oils by supercritical fluid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Hori, Katsuhito; Matsubara, Atsuki; Uchikata, Takato; Tsumura, Kazunobu; Fukusaki, Eiichiro; Bamba, Takeshi

    2012-08-10

    We have established a high-throughput and sensitive analytical method based on supercritical fluid chromatography (SFC) coupled with triple quadrupole mass spectrometry (QqQ MS) for 3-monochloropropane-1,2-diol (3-MCPD) fatty acid esters in edible oils. All analytes were successfully separated within 9 min without sample purification. The system was precise and sensitive, with a limit of detection less than 0.063 mg/kg. The recovery rate of 3-MCPD fatty acid esters spiked into oil samples was in the range of 62.68-115.23%. Furthermore, several edible oils were tested for analyzing 3-MCPD fatty acid ester profiles. This is the first report on the analysis of 3-MCPD fatty acid esters by SFC/QqQ MS. The developed method will be a powerful tool for investigating 3-MCPD fatty acid esters in edible oils. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. AC electrical breakdown phenomena of epoxy/layered silicate nanocomposite in needle-plate electrodes.

    Science.gov (United States)

    Park, Jae-Jun; Lee, Jae-Young

    2013-05-01

    Epoxy/layered silicate nanocomposite for the insulation of heavy electric equipments were prepared by dispersing 1 wt% of a layered silicate into an epoxy matrix with a homogenizing mixer and then AC electrical treeing and breakdown tests were carried out. Wide-angle X-ray diffraction (WAXD) analysis and transmission electron microscopy (TEM) observation showed that nano-sized monolayers were exfoliated from a multilayered silicate in the epoxy matrix. When the nano-sized silicate layers were incorporated into the epoxy matrix, the breakdown rate in needle-plate electrode geometry was 10.6 times lowered than that of the neat epoxy resin under the applied electrical field of 520.9 kV/mm at 30 degrees C, and electrical tree propagated with much more branches in the epoxy/layered silicate nanocomposite. These results showed that well-dispersed nano-sized silicate layers retarded the electrical tree growth rate. The effects of applied voltage and ambient temperature on the tree initiation, growth, and breakdown rate were also studied, and it was found that the breakdown rate was largely increased, as the applied voltage and ambient temperature increased.

  4. Optimization and validation of liquid chromatography and headspace-gas chromatography based methods for the quantitative determination of capsaicinoids, salicylic acid, glycol monosalicylate, methyl salicylate, ethyl salicylate, camphor and l-menthol in a topical formulation.

    Science.gov (United States)

    Pauwels, Jochen; D'Autry, Ward; Van den Bossche, Larissa; Dewever, Cédric; Forier, Michel; Vandenwaeyenberg, Stephanie; Wolfs, Kris; Hoogmartens, Jos; Van Schepdael, Ann; Adams, Erwin

    2012-02-23

    Capsaicinoids, salicylic acid, methyl and ethyl salicylate, glycol monosalicylate, camphor and l-menthol are widely used in topical formulations to relieve local pain. For each separate compound or simple mixtures, quantitative analysis methods are reported. However, for a mixture containing all above mentioned active compounds, no assay methods were found. Due to the differing physicochemical characteristics, two methods were developed and optimized simultaneously. The non-volatile capsaicinoids, salicylic acid and glycol monosalicylate were analyzed with liquid chromatography following liquid-liquid extraction, whereas the volatile compounds were analyzed with static headspace-gas chromatography. For the latter method, liquid paraffin was selected as compatible dilution solvent. The optimized methods were validated in terms of specificity, linearity, accuracy and precision in a range of 80% to 120% of the expected concentrations. For both methods, peaks were well separated without interference of other compounds. Linear relationships were demonstrated with R² values higher than 0.996 for all compounds. Accuracy was assessed by performing replicate recovery experiments with spiked blank samples. Mean recovery values were all between 98% and 102%. Precision was checked at three levels: system repeatability, method precision and intermediate precision. Both methods were found to be acceptably precise at all three levels. Finally, the method was successfully applied to the analysis of some real samples (cutaneous sticks). Copyright © 2011 Elsevier B.V. All rights reserved.

  5. New Silicate Phosphors for a White LED(Electronic Displays)

    OpenAIRE

    Toda, Kenji; Kawakami, Yoshitaka; Kousaka, Shin-ichiro; Ito, Yutaka; Komeno, Akira; Uematsu, Kazuyoshi; Sato, Mineo

    2006-01-01

    We focus on the development of new silicate phosphors for a white LED. In the europium doped silicate system, four LED phosphor candidates-Li_2SrSiO_4:Eu^, Ba_9Sc_2Si_6O_:Eu^, Ca_3Si_2O_7:Eu^ and Ba_2MgSi_2O_7:Eu^ were found. Luminescent properties under near UV and visible excitation were investigated for the new Eu^ doped LED silicate phosphors. These new phosphors have a relatively strong absorption band in a long wavelength region.

  6. Development of Li+ alumino-silicate ion source

    International Nuclear Information System (INIS)

    Roy, P.K.; Seidl, P.A.; Waldron, W.; Greenway, W.; Lidia, S.; Anders, A.; Kwan, J.

    2009-01-01

    To uniformly heat targets to electron-volt temperatures for the study of warm dense matter, one strategy is to deposit most of the ion energy at the peak of energy loss (dE/dx) with a low (E < 5 MeV) kinetic energy beam and a thin target. Lower mass ions have a peak dE/dx at a lower kinetic energy. To this end, a small lithium (Li+) alumino-silicate source has been fabricated, and its emission limit has been measured. These surface ionization sources are heated to 1000-1150 C where they preferentially emit singly ionized alkali ions. Alumino-silicates sources of K+ and Cs+ have been used extensively in beam experiments, but there are additional challenges for the preparation of high-quality Li+ sources: There are tighter tolerances in preparing and sintering the alumino-silicate to the substrate to produce an emitter that gives uniform ion emission, sufficient current density and low beam emittance. We report on recent measurements ofhigh ( up to 35 mA/cm2) current density from a Li+ source. Ion species identification of possible contaminants is being verified with a Wien (E x B) filter, and via time-of-flight.

  7. Analysis of Phenolic Acids of Jerusalem Artichoke (Helianthus tuberosus L. Responding to Salt-Stress by Liquid Chromatography/Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Fujia Chen

    2014-01-01

    Full Text Available Plant phenolics can have applications in pharmaceutical and other industries. To identify and quantify the phenolic compounds in Helianthus tuberosus leaves, qualitative analysis was performed by a reversed phase high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS and quantitative analysis by HPLC. Ten chlorogenic acids (CGAs were identified (3-o-caffeoylquinic acid, two isomers of caffeoylquinic acid, caffeic acid, p-coumaroyl-quinic acid, feruloylquinic acid, 3,4-dicaffeoyquinic acid, 3,5-dicaffeoylquinic acid, 1,5-dicaffeoylquinic acid, and 4,5-dicaffeoylquinic acid by comparing their retention times, UV-Vis absorption spectra, and MS/MS spectra with standards. In addition, four other phenolic compounds, including caffeoyl glucopyranose, isorhamnetin glucoside, kaempferol glucuronide, and kaempferol-3-o-glucoside, were tentatively identified in Helianthus tuberosus leaves for the first time. The 3-o-caffeoylquinic acid (7.752 mg/g DW, 4,5-dicaffeoylquinic acid (5.633 mg/g DW, and 3,5-dicaffeoylquinic acid (4.900 mg/g DW were the major phenolic compounds in leaves of Helianthus tuberosus cultivar NanYu in maturity. The variations in phenolic concentrations and proportions in Helianthus tuberosus leaves were influenced by genotype and plant growth stage. Cultivar NanYu had the highest concentration of phenolic compounds, in particular 3-o-caffeoylquinic acid and 4,5-dicaffeoylquinic acid compared with the other genotypes (wild accession and QingYu. Considering various growth stages, the concentration of total phenolics in cultivar NanYu was higher at flowering stage (5.270 mg/g DW than at budding and tuber swelling stages. Cultivar NanYu of Helianthus tuberosus is a potential source of natural phenolics that may play an important role in the development of pharmaceuticals.

  8. Confined Water in Layered Silicates: The Origin of Anomalous Thermal Expansion Behavior in Calcium-Silicate-Hydrates

    International Nuclear Information System (INIS)

    Krishnan, N. M. Anoop; Wang, Bu; Falzone, Gabriel; Le Pape, Yann; Neithalath, Narayanan

    2016-01-01

    Water, under conditions of nanoscale confinement, exhibits anomalous dynamics, and enhanced thermal deformations, which may be further enhanced when such water is in contact with hydrophilic surfaces. Such heightened thermal deformations of water could control the volume stability of hydrated materials containing nanoconfined structural water. Understanding and predicting the thermal deformation coefficient (TDC, often referred to as the CTE, coefficient of thermal expansion), which represents volume changes induced in materials under conditions of changing temperature, is of critical importance for hydrated solids including: hydrogels, biological tissues, and calcium silicate hydrates, as changes in their volume can result in stress development, and cracking. By pioneering atomistic simulations, we examine the physical origin of thermal expansion in calcium-silicate-hydrates (C–S–H), the binding agent in concrete that is formed by the reaction of cement with water. We report that the TDC of C–S–H shows a sudden increase when the CaO/SiO_2 (molar ratio; abbreviated as Ca/Si) exceeds 1.5. This anomalous behavior arises from a notable increase in the confinement of water contained in the C–S–H’s nanostructure. We identify that confinement is dictated by the topology of the C–S–H’s atomic network. Altogether, the results suggest that thermal deformations of hydrated silicates can be altered by inducing compositional changes, which in turn alter the atomic topology and the resultant volume stability of the solids.

  9. Confined Water in Layered Silicates: The Origin of Anomalous Thermal Expansion Behavior in Calcium-Silicate-Hydrates.

    Science.gov (United States)

    Krishnan, N M Anoop; Wang, Bu; Falzone, Gabriel; Le Pape, Yann; Neithalath, Narayanan; Pilon, Laurent; Bauchy, Mathieu; Sant, Gaurav

    2016-12-28

    Water, under conditions of nanoscale confinement, exhibits anomalous dynamics, and enhanced thermal deformations, which may be further enhanced when such water is in contact with hydrophilic surfaces. Such heightened thermal deformations of water could control the volume stability of hydrated materials containing nanoconfined structural water. Understanding and predicting the thermal deformation coefficient (TDC, often referred to as the CTE, coefficient of thermal expansion), which represents volume changes induced in materials under conditions of changing temperature, is of critical importance for hydrated solids including: hydrogels, biological tissues, and calcium silicate hydrates, as changes in their volume can result in stress development, and cracking. By pioneering atomistic simulations, we examine the physical origin of thermal expansion in calcium-silicate-hydrates (C-S-H), the binding agent in concrete that is formed by the reaction of cement with water. We report that the TDC of C-S-H shows a sudden increase when the CaO/SiO 2 (molar ratio; abbreviated as Ca/Si) exceeds 1.5. This anomalous behavior arises from a notable increase in the confinement of water contained in the C-S-H's nanostructure. We identify that confinement is dictated by the topology of the C-S-H's atomic network. Taken together, the results suggest that thermal deformations of hydrated silicates can be altered by inducing compositional changes, which in turn alter the atomic topology and the resultant volume stability of the solids.

  10. Tip-induced nanoreactor for silicate

    Science.gov (United States)

    Gao, Ming; Ma, Liran; Liang, Yong; Gao, Yuan; Luo, Jianbin

    2015-09-01

    Nanoscale scientific issues have attracted an increasing amount of research interest due to their specific size-effect and novel structure-property. From macro to nano, materials present some unique chemical reactivity that bulk materials do not own. Here we introduce a facile method to generate silicate with nanoscale control based on the establishment of a confined space between a meso/nanoscale tungsten tip and a smooth silica/silicon substrate. During the process, local water-like droplets deposition can be obviously observed in the confinement between the Si/SiO2 surfaces and the KOH-modified tungsten tip. By the combination of in-situ optical microscopy and Raman spectroscopy, we were able to take a deep insight of both the product composition and the underlying mechanism of such phenomena. It was indicated that such nanoreactor for silicate could be quite efficient as a result of the local capillarity and electric field effect, with implications at both nano and meso scales.

  11. Radiation effects in silicate glasses

    International Nuclear Information System (INIS)

    Bibler, N.E.; Howitt, D.G.

    1988-01-01

    The study of radiation effects in complex silicate glasses has received renewed attention because of their use in special applications such as high level nuclear waste immobilization and fiber optics. Radiation changes the properties of these glasses by altering their electronic and atomic configurations. These alterations or defects may cause dilatations or microscopic phase changes along with absorption centers that limit the optical application of the glasses. Atomic displacements induced in the already disordered structure of the glasses may affect their use where heavy irradiating particles such as alpha particles, alpha recoils, fission fragments, or accelerated ions are present. Large changes (up to 1%) in density may result. In some cases the radiation damage may be severe enough to affect the durability of the glass in aqueous solutions. In the paper, the authors review the literature concerning radiation effects on density, durability, stored energy, microstructure and optical properties of silicate glasses. Both simple glasses and complex glasses used for immobilization of nuclear waste are considered

  12. Carbon nanoparticles from corn stalk soot and its novel application as stationary phase of hydrophilic interaction chromatography and per aqueous liquid chromatography

    International Nuclear Information System (INIS)

    Li Yuanyuan; Xu Luan; Chen Tong; Liu Xiaoyan; Xu Zhigang; Zhang Haixia

    2012-01-01

    Highlights: ► Carbon nanoparticles (6–18 nm in size) were prepared from corn stalk soot. ► CNPs-based silica were used as novel chromatography stationary phase. ► The new phase shows good separation selectivity for polar compounds. ► The new phase had the similar retention for polar probes in HILIC and PALC modes. ► In contrast to PALC, under HILIC conditions high efficiencies were achieved. - Abstract: Carbon nanoparticles (CNPs) (6–18 nm in size) were prepared by refluxing corn stalk soot in nitric acid. The obtained acid-oxidized CNPs are soluble in water due to the existence of carboxylic and hydroxyl groups. 13 C NMR measurement shows the CNPs are mainly of sp 2 and sp 3 carbon structure different from CNPs obtained from candle soot and natural gas soot. Furthermore, these CNPs exhibit unique photoluminescence properties. Interestingly, the CNPs might be exploited to immobilize on the surface of porous silica particles as chromatographic stationary phase. The resultant packing material was evaluated by high-performance liquid chromatography, indicating that the new stationary phase could be used in hydrophilic interaction liquid chromatography (HILIC) and per aqueous liquid chromatography (PALC) modes. The separation of five nucleosides, four sulfa compounds and safflower injection was achieved by using the new column in the HILIC and PALC modes, respectively.

  13. In situ intercalative polymerization of poly (ε-caprolactone)/ 12-amino lauric acid-modified clay nano composites

    International Nuclear Information System (INIS)

    Reyes, Larry; Monserate, Juvy J.; Sumera, Florentino

    2013-01-01

    Polymer/layered silicate nano composites were prepared by in situ intercalative polymerization method from from ε-caprolactone (ε-CL) and 12-amino lauric acid modified montmorillonite (AMMT). The organo-modified clay was investigated for its capacity to facilitate ring-opening polymerization of ε-caprolactone within its silicate layers. The effect of varying the organo-modified clay loading (5%, 10% and 15% by weight) on the molecular weight of the poly (ε-caprolactone) (PCL) product was assessed by gel-permeation chromatography. The molecular weight of the polymer with different clay loadings ranged from ∼30,000 g/mo to ∼70,000 g/mol, where the 10% loading produced the highest molecular weight. Fourier Transform infrared (FTIR), and 1 H and 13 C Nuclear Magnetic Resonance (NMR) Spectroscopy were conducted to probe the composition of the polymer and the catalytic activity of AMMT to polymerize ε-CL. FTIR analyses showed two medium intensity and narrow CO-O stretching vibrations for the PCL products at around 1240 cm-1 and 1160 cm-1, which are attributed to ester skeletal backbone. 1 HNMR spectroscopic analysis revealed signals at 4.07 ppm and 3.66 ppm which can be attributed to εmethylene of caprolactone and methyl of ending ester group, respectively. The formation of the nano composites were assessed by X-ray Diffraction (XRD) and Transmission Electron Microscopy (TEM), XRD analyses showed a broadening and disappearance of diffraction peak of AMMT in the nana composite which may indicate the formation of the intercalated and partially exfoliated PCVL/AMMT nana composites. TEM observations corroborated the presence of intercalated and exfoliated layers of AMMT after polymerization. The present work demonstrates that AMMT can be used as an alternative g reen catalyst's for the production of biodegradable polymers, where the in situ intercalative polymerization was employed as a direct method of preparing polymer/layered silicates (author)

  14. The analysis of aqueous mixtures using liquid chromatography-electrospray mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, Steven [Iowa State Univ., Ames, IA (United States)

    1999-02-12

    The focus of this dissertation is the use of chromatographic methods coupled with electrospray mass spectrometry (ES-MS) for the determination of both organic and inorganic compounds in aqueous solutions. The combination of liquid chromatography (LC) methods and ES-MS offers one of the foremost methods for determining compounds in complex aqueous solutions. In this work, LC-ES-MS methods are devised using ion exclusion chromatography, reversed phase chromatography, and ion exchange chromatography, as well as capillary electrophoresis (CE). For an aqueous sample, these LC-ES-MS and CE-ES-MS techniques require no sample preparation or analyte derivatization, which makes it possible to observe a wide variety of analytes as they exist in solution. The majority of this work focuses on the use of LC-ES-MS for the determination of unknown products and intermediates formed during electrochemical incineration (ECI), an experimental waste remediation process. This report contains a general introduction to the project and the general conclusions. Four chapters have been removed for separate processing. Titles are: Chapter 2: Determination of small carboxylic acids by ion exclusion chromatography with electrospray mass spectrometry; Chapter 3: Electrochemical incineration of benzoquinone in aqueous media using a quaternary metal oxide electrode in the absence of a soluble supporting electrolyte; Chapter 4: The determination of electrochemical incineration products of 4-chlorophenol by liquid chromatography-electrospray mass spectrometry; and Chapter 5: Determination of small carboxylic acids by capillary electrophoresis with electrospray mass spectrometry.

  15. Investigation of folic acid stability in fortified instant noodles by use of capillary electrophoresis and reversed-phase high performance liquid chromatography.

    Science.gov (United States)

    Hau Fung Cheung, Rodney; Morrison, Paul D; Small, Darryl M; Marriott, Philip J

    2008-12-05

    A single enzyme treatment with alpha-amylase, prior to the quantification of added folic acid (FA) in fortified instant fried Asian noodles with analysis performed by capillary zone electrophoresis (CZE) and reversed-phase high performance liquid chromatography (RP-HPLC) with UV detection, is described. The method was validated and optimized for capillary electrophoresis (CE) with separation achieved using a 8 mM phosphate-12 mM borate run buffer with 5% MeOH at pH 9.5. FA was well separated from matrix components with nicotinic acid (NA) employed as an internal standard. In a comparative study, separation of FA was performed using HPLC with a mobile phase consisting of 27% MeOH (v/v) in aqueous potassium phosphate buffer (3.5 mM KH(2)PO(4) and 3.2 mM K(2)HPO(4)), pH 8.5, and containing 5 mM tetrabutylammonium dihydrogen phosphate as an ion-pairing agent. For both methods, excellent results were obtained for various analytical parameters including linearity, accuracy and precision. The limit of detection was calculated to be 2.2 mg/L for CE without sample stacking and 0.10 mg/L with high performance liquid chromatography (HPLC). Sample extraction involved homogenization and enzymatic extraction with alpha-amylase. Results indicated that FA was stable during four main stages of instant fried noodle manufacturing (dough crumbs, cut sheets, steaming and frying).

  16. Simultaneous Analysis of Ursolic Acid and Oleanolic Acid in Guava Leaves Using QuEChERS-Based Extraction Followed by High-Performance Liquid Chromatography

    Science.gov (United States)

    Xu, Chang; Liao, Yiyi; Fang, Chunyan; Zhang, Yingxia

    2017-01-01

    In this paper, a novel method of QuEChERS-based extraction coupled with high-performance liquid chromatography has been developed for the simultaneous determination of ursolic acid (UA) and oleanolic acid (OA) in guava leaves. The QuEChERS-based extraction parameters, including the amount of added salt, vortex-assisted extraction time, and absorbent amount, and the chromatographic conditions were investigated for the analysis of UA and OA in guava leaves. Under the optimized conditions, the method showed good linearity over a range of 1–320 μg mL−1, with correlation coefficients above 0.999. The limits of detection of UA and OA were 0.18 and 0.36 μg mL−1, respectively. The intraday and interday precision were below 1.95 and 2.55%, respectively. The accuracies of the UA and OA determinations ranged from 97.4 to 111.4%. The contents of UA and OA in the guava leaf samples were 2.50 and 0.73 mg g−1, respectively. These results demonstrate that the developed method is applicable to the simultaneous determination of UA and OA in guava leaves. PMID:28781908

  17. Vitamins in fruits and vegetables of the Amazon. 1. Methods for the determination of β—carotene, tocopherol and ascorbic acid with high performance liquid chromatography (HPLC)

    OpenAIRE

    Marx, F.; Maia, J.G.S.

    1983-01-01

    Summary At the beginning of on inventory of the chemical composition of regional fruits and vegetables of the Amazon, analytical methods were adapted for the high performance liquid chromatography (HPLC) determination of pro-vitamin A (β—carotene), vitamin C (ascorbic acid) and vitamin E (tocopherol) The first analyses indicate as excellent sources of β—carotene, Mauritia flexuosa L., Astrocaryum tucuma Mart. and Cucurbita pepa L.; of asco bic acid Theobroma grandiflorum (Culis ex Spreng.) Sc...

  18. Preparation of silica nanoparticles through microwave-assisted acid-catalysis.

    Science.gov (United States)

    Lovingood, Derek D; Owens, Jeffrey R; Seeber, Michael; Kornev, Konstantin G; Luzinov, Igor

    2013-12-16

    Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan δ solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials' morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by Stöber's methods, which have smooth surfaces.

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

    Science.gov (United States)

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

    2003-03-01

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

  20. Enantioselective determination of methylphenidate and ritalinic acid in whole blood from forensic cases using automated solid-phase extraction and liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Thomsen, Ragnar; B. Rasmussen, Henrik; Linnet, Kristian

    2012-01-01

    A chiral liquid chromatography tandem mass spectrometry (LC–MS-MS) method was developed and validated for quantifying methylphenidate and its major metabolite ritalinic acid in blood from forensic cases. Blood samples were prepared in a fully automated system by protein precipitation followed...... methylphenidate was not determined to be related to the cause of death, the femoral blood concentration of d-methylphenidate ranged from 5 to 58 ng/g, and from undetected to 48 ng/g for l-methylphenidate (median d/l-ratio 5.9). Ritalinic acid was present at concentrations 10–20 times higher with roughly equal...

  1. Natural penetrating radiation inside silicate dwellings in Chengdu and recommendation on permissible limits for radioactivity of building material made of silicate cinders

    International Nuclear Information System (INIS)

    Li Guangzao

    1984-01-01

    This paper reports the results of external exposure rate of penetrating radiation inside silicate dwellings in Chengdu. The average exposure rate was 24.3+-3.5 R/h. It was evidently higher than of red brick dwellings. The average effective equivalent of the population in silicate dwellings was 123.4+-10.4 mrem/y and the average additional dose was 29.5+-12.5 mrem/y. The permissible limits recommended for silicate building material would be 6 pCi/g, 7 pCi/g and 102 pCi/g for 226 Ra, 232 Th and 40 K, respectively. The total activity must fulfill the formula of Csub(Ra)/6 + Csub(Th)/7 + Csub(k)/102 1. Under ordinary condition the exposure rate (10+background) R/h of penetrating radiation from the surface of dry building material might be taken as the permissible limit for dwellings and other public buildings

  2. Calcium and magnesium silicate hydrates

    International Nuclear Information System (INIS)

    Lothenbach, B.; L'Hopital, E.; Nied, D.; Achiedo, G.; Dauzeres, A.

    2015-01-01

    Deep geological disposals are planed to discard long-lived intermediate-level and high-level radioactive wastes. Clay-based geological barriers are expected to limit the ingress of groundwater and to reduce the mobility of radioelements. In the interaction zone between the cement and the clay based material alteration can occur. Magnesium silicate hydrates (M-S-H) have been observed due to the reaction of magnesium sulfate containing groundwater with cements or in the interaction zone between low-pH type cement and clays. M-S-H samples synthesized in the laboratory showed that M-S-H has a variable composition within 0.7 ≤ Mg/Si ≤ 1.5. TEM/EDS analyses show an homogeneous gel with no defined structure. IR and 29 Si NMR data reveal a higher polymerization degree of the silica network in M-S-H compared to calcium silicate hydrates (C-S-H). The presence of mainly Q 3 silicate tetrahedrons in M-S-H indicates a sheet like or a triple-chain silica structure while C-S-H is characterised by single chain-structure. The clear difference in the silica structure and the larger ionic radius of Ca 2+ (1.1 Angstrom) compared to Mg 2+ (0.8 Angstrom) make the formation of an extended solid solution between M-S-H and C-S-H gel improbable. In fact, the analyses of synthetic samples containing both magnesium and calcium in various ratios indicate the formation of separate M-S-H and C-S-H gels with no or very little uptake of magnesium in CS-H or calcium in M-S-H

  3. Enantioselective micellar electrokinetic chromatography of dl-amino acids using (+)-1-(9-fluorenyl)-ethyl chloroformate derivatization and UV-induced fluorescence detection.

    Science.gov (United States)

    Prior, Amir; van de Nieuwenhuijzen, Erik; de Jong, Gerhardus J; Somsen, Govert W

    2018-05-22

    Chiral analysis of dl-amino acids was achieved by micellar electrokinetic chromatography coupled with UV-excited fluorescence detection. The fluorescent reagent (+)-1-(9-fluorenyl)ethyl chloroformate was employed as chiral amino acid derivatizing agent and sodium dodecyl sulfate served as pseudo-stationary phase for separating the formed amino acid diastereomers. Sensitive analysis of (+)-1-(9-fluorenyl)ethyl chloroformate-amino acids was achieved applying a xenon-mercury lamp for ultraviolet excitation, and a spectrograph and charge-coupled device for wavelength-resolved emission detection. Applying signal integration over a 30-nm emission wavelength interval, signal-to-noise ratios for derivatized amino acids were up to 23 times higher as obtained using a standard photomultiplier for detection. The background electrolyte composition (electrolyte, pH, sodium dodecyl sulfate concentration, and organic solvent) was studied in order to attain optimal chemo- and enantioseparation. Enantioseparation of twelve proteinogenic dl-amino acids was achieved with chiral resolutions between 1.2 and 7.9, and detection limits for most derivatized amino acids in the 13-60 nM range (injected concentration). Linearity (coefficients of determination > 0.985) and peak-area and migration-time repeatabilities (relative standard deviations lower than 2.6 and 1.9%, respectively) were satisfactory. The employed fluorescence detection system provided up to 100-times better signal-to-noise ratios for (+)-1-(9-fluorenyl)ethyl chloroformate-amino acids than ultraviolet absorbance detection, showing good potential for d-amino acid analysis. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  4. Studies on chemical constituents of Polygala japonica Houtt.

    Institute of Scientific and Technical Information of China (English)

    LI Ting-zhao; ZHANG Wei-dong; LIU Run-hui; CHEN Hai-sheng; ZHANG Chuan; SU Juan; XU Xi-ke

    2006-01-01

    Objective:To investigate the chemical constituents of Polygala japonica Houtt.. Methods:The constituents were separated and purified by column chromatographies with silical gel, RP-silical gel and Sephadex LH-20. Their structures were elucidated on the basis of spectral data (IR, MS, 1H-NMR, 13C-NMR, HMQC and HMBC). Results: Totally 15 compounds were obtained from Polygala japonica Houtt. And their structures were identified as castaprenol-12 (Ⅰ), β-sitosterol (Ⅱ), stigmasterol (Ⅲ),stigmasta-7,22-di-ene-3-one (Ⅳ), n-dotriacontanol ( Ⅴ ), n-hexadecanol ( Ⅵ ), arachidic acid (Ⅶ), erogosterol (Ⅷ), kaempferol (Ⅸ), quercetin (Ⅹ), daucosterol (Ⅺ), p-hydroxybenzoic acid (Ⅻ),coumaric acid (ⅩⅢ), rhamnocitrin 3-O-β-D-galactopyranoside (ⅪⅤ), quercetin 3-O-β-D-glucopyranoside (ⅩⅤ). Conclusion: Compounds Ⅰ , Ⅲ , Ⅳ, Ⅴ , Ⅵ, Ⅶ, Ⅷ, Ⅻ , ⅩⅢ and ⅩⅣ were obtained from this plant for the first time.

  5. Rapid, Sensitive and Validated Ultra-Performance Liquid Chromatography/Mass Spectrometric Method for the Determination of Fenofibric Acid and its Application to Human Pharmacokinetic Study

    Directory of Open Access Journals (Sweden)

    Sunil K. Dubey

    2010-01-01

    Full Text Available The first, rapid and sensitive ultra performance liquid chromatography mass spectrometric method for the determination of fenofibric acid, the active metabolite of fenofibrate, a lipid regulating agent, in human EDTA plasma has been developed and validated using fenofibric d6 acid as internal standard and Waters LC-MS/MS. Negative ions of fenofibric acid and fenofibric d6 acid were detected in multiple reaction-monitoring (MRM mode. The method was validated over a concentration range of 0.176 μg/mL to 19.837 μg/mL (r ≥ 0.99. It took only 1.5 minute to analyse a sample. Intra- and inter-run precision of fenofibric acid assay at four concentrations ranged from 0.5% to 4.3% with accuracy varied from 93.1 to 108.1% indicating good precision and accuracy. Analytical recoveries of fenofibric acid and internal standard in plasma were less than 90%. This method was successfully applied for evaluation of pharmacokinetics of fenofibric acid after a single oral dose of 145 mg fenofibrate to 10 Indian healthy volunteers

  6. Effect of additives on eremomycin sorbent selectivity in separation of salbutamol enantiomers using supercritical fluid chromatography

    Science.gov (United States)

    Pokrovskiy, O. I.; Kayda, A. S.; Usovich, O. I.; Parenago, O. O.; Lunin, V. V.

    2017-11-01

    A regime is found in which chiral stationary phase based on macrocyclic glycopeptide eremomycin allows separation of salbutamol sulfate enantiomers in supercritical fluid chromatography. Enantioseparation occurs only when two dynamic modifiers are used simultaneously: isopropylamin + trifluoroacetic acid or isopropylamin + ammonium acetate. Amine molar concentration in mobile phase has to be higher than acid molar concentration, otherwise enantiomers coelute. We suppose that with amine excess a mechanism of enantiorecognition is realized which involves ionic sorbent-sorbate interactions. Such mechanism is well-known for glycopeptide chiral selectors in liquid chromatography, but for supercritical fluid chromatography it is reported for the first time.

  7. Isolation and purification of six iridoid glycosides from gardenia jasminoides fruit by medium-pressure liquid chromatography combined with macroporous resin chromatography.

    Science.gov (United States)

    Wang, Yun; Liu, Hui; Shen, Lifeng; Yao, Lan; Ma, Yinlian; Yu, Dingrong; Chen, Jianhong; Li, Puling; Chen, Ying; Zhang, Cun

    2015-12-01

    Gardeniae fructus is one of the most frequently used herbs in traditional Chinese medicine. In the present study, a process for the enrichment of six iridoid glycosides from Gardeniae fructus was developed using medium-pressure liquid chromatography combined with macroporous resin and reversed-phase chromatography. The purities of different fractions from Gardeniae fructus were assessed using quantitative high-performance liquid chromatography. After fractionation using HPD-100 column chromatography, a 30% ethanol fraction was selected based on high-performance liquid chromatography and liquid chromatography with mass spectrometry qualitative analysis to separate and purify. Based on the orientation analysis results, six compounds-deacetyl asperulosidic acid methyl ester, gardenoside, ixoroside, scandoside methyl ester, genipin-1-O-β-d-gentiobioside, and geniposide-were successfully isolated and purified in three to four combined steps from Gardeniae fructus. The purities of these compounds were found by high-performance liquid chromatography analysis to be 97.9, 98.1, 95.5, 96.3, 97.1, and 98.7%, respectively. Moreover, their structures were elucidated by NMR spectroscopy and liquid chromatography with tandem mass spectrometry. The separation process was highly efficient, rapid, and accurate, making it a potential approach for the large-scale production of iridoids in the laboratory and providing several marker compounds for quality control. This procedure may be meaningful for the purification of other natural products used in traditional Chinese medicine. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Silicate Phases on the Surfaces of Trojan Asteroids

    Science.gov (United States)

    Martin, Audrey; Emery, Joshua P.; Lindsay, Sean S.

    2017-10-01

    Determining the origin of asteroids provides an effective means of constraining the solar system’s dynamic past. Jupiter Trojan asteroids (hereafter Trojans) may help in determining the amount of radial mixing that occurred during giant planet migration. Previous studies aimed at characterizing surface composition show that Trojans have low albedo surfaces and are spectrally featureless in the near infrared. The thermal infrared (TIR) wavelength range has advantages for detecting silicates on low albedo asteroids such as Trojans. The 10 μm region exhibits strong features due to the Si-O fundamental molecular vibrations. Silicates that formed in the inner solar system likely underwent thermal annealing, and thus are crystalline, whereas silicates that accreted in the outer solar system experienced less thermal processing, and therefore are more likely to have remained in an amorphous phase. We hypothesize that the Trojans formed in the outer solar system (i.e., the Kuiper Belt), and therefore will have a more dominant amorphous spectral silicate component. With TIR spectra from the Spitzer Space Telescope, we identify mineralogical features from the surface of 11 Trojan asteroids. Fine-grain mixtures of crystalline pyroxene and olivine exhibit a 10 μm feature with sharp cutoffs between about 9 μm and 12 μm, which create a broad flat plateau. Amorphous phases, when present, smooth the sharp emission features, resulting in a dome-like shape. Preliminary results indicate that the surfaces of analyzed Trojans contain primarily amorphous silicates. Emissivity spectra of asteroids 1986 WD and 4709 Ennomos include small peaks in the 10 μm region, diagnostic of small amounts of crystalline olivine. One explanation is that Trojans formed in the same region as Kuiper Belt objects, and when giant planet migration ensued, they were swept into Jupiter’s stable Lagrange points where they are found today. As such, it is possible that an ancestral group of Kuiper Belt

  9. Incorporation of oxygen into abscisic acid and phaseic acid for molecular oxygen

    International Nuclear Information System (INIS)

    Creelman, R.A.; Zeevaart, J.A.D.

    1984-01-01

    Abscisic acid accumulates in detached, wilted leaves of Xanthium strumariu. When these leaves are subsequently rehydrated, phaseic acid, a catabolite of abscisic acid, accumulates. Analysis by gas chromatography-mass spectrometry of phaseic acid isolated from stressed and subsequently rehydrated leaves placed in an atmosphere containing 20% 18 O 2 and 80% N 2 indicates that one atom of 18 O is incorporated in the 6'-hydroxymethyl group of phaseic acid. This suggests that the enzyme that converts abscisic acid to phaseic acid is an oxygenase. Analysis by gas chromatography-mass spectrometry of abscisic acid isolated from stressed leaves kept in an atmosphere containing 18 O 2 indicates that one atom of 18 O is presented in the carboxyl group of abscisic acid. Thus, when abscisic acid accumulates in water-streesed leaves, only one of the four oxygens present in the abscisic acid molecule is derived from molecular oxygen. This suggest that either (a) the oxygen present in the 1'-, 4'-, and one of the two oxygens at the 1-position of abscisic acid arise from water, or (b) there exists a stored precursor with oxygen atoms already present in the 1'- and 4'-positions of abscisic acid which is converted to abscisic acid under conditions of water stress. 17 references, 2 figures, 1 tables

  10. Incorporation of oxygen into abscisic Acid and phaseic Acid from molecular oxygen.

    Science.gov (United States)

    Creelman, R A; Zeevaart, J A

    1984-05-01

    Abscisic acid accumulates in detached, wilted leaves of Xanthium strumarium. When these leaves are subsequently rehydrated, phaseic acid, a catabolite of abscisic acid, accumulates. Analysis by gas chromatography-mass spectrometry of phaseic acid isolated from stressed and subsequently rehydrated leaves placed in an atmosphere containing 20% (18)O(2) and 80% N(2) indicates that one atom of (18)O is incorporated in the 6'-hydroxymethyl group of phaseic acid. This suggests that the enzyme that converts abscisic acid to phaseic acid is an oxygenase.Analysis by gas chromatography-mass spectrometry of abscisic acid isolated from stressed leaves kept in an atmosphere containing (18)O(2) indicates that one atom of (18)O is present in the carboxyl group of abscisic acid. Thus, when abscisic acid accumulates in water-stressed leaves, only one of the four oxygens present in the abscisic acid molecule is derived from molecular oxygen. This suggests that either (a) the oxygen present in the 1'-, 4'-, and one of the two oxygens at the 1-position of abscisic acid arise from water, or (b) there exists a stored precursor with oxygen atoms already present in the 1'- and 4'-positions of abscisic acid which is converted to abscisic acid under conditions of water stress.

  11. Hydrophilic interaction liquid chromatography of anthranilic acid-labelled oligosaccharides with a 4-aminobenzoic acid ethyl ester-labelled dextran hydrolysate internal standard.

    Science.gov (United States)

    Neville, David C A; Alonzi, Dominic S; Butters, Terry D

    2012-04-13

    Hydrophilic interaction liquid chromatography (HILIC) of fluorescently labelled oligosaccharides is used in many laboratories to analyse complex oligosaccharide mixtures. Separations are routinely performed using a TSK gel-Amide 80 HPLC column, and retention times of different oligosaccharide species are converted to glucose unit (GU) values that are determined with reference to an external standard. However, if retention times were to be compared with an internal standard, consistent and more accurate GU values would be obtained. We present a method to perform internal standard-calibrated HILIC of fluorescently labelled oligosaccharides. The method relies on co-injection of 4-aminobenzoic acid ethyl ester (4-ABEE)-labelled internal standard and detection by UV absorption, with 2-AA (2-aminobenzoic acid)-labelled oligosaccharides. 4-ABEE is a UV chromophore and a fluorophore, but there is no overlap of the fluorescent spectrum of 4-ABEE with the commonly used fluorescent reagents. The dual nature of 4-ABEE allows for accurate calculation of the delay between UV and fluorescent signals when determining the GU values of individual oligosaccharides. The GU values obtained are inherently more accurate as slight differences in gradients that can influence retention are negated by use of an internal standard. Therefore, this paper provides the first method for determination of HPLC-derived GU values of fluorescently labelled oligosaccharides using an internal calibrant. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Topotactic condensation of layer silicates with ferrierite-type layers forming porous tectosilicates.

    Science.gov (United States)

    Marler, B; Wang, Y; Song, J; Gies, H

    2014-07-21

    Five different hydrous layer silicates (HLSs) containing fer layers (ferrierite-type layers) were obtained by hydrothermal syntheses from mixtures of silicic acid, water and tetraalkylammonium/tetraalkylphosphonium hydroxides. The organic cations had been added as structure directing agents (SDA). A characteristic feature of the structures is the presence of strong to medium strong hydrogen bonds between the terminal silanol/siloxy groups of neighbouring layers. The five-layered silicates differ chemically only with respect to the organic cations. Structurally, they differ with respect to the arrangement of the fer layers relative to each other, which is distinct for every SDA-fer-layer system. RUB-20 (containing tetramethylammonium) and RUB-40 (tetramethylphosphonium) are monoclinic with stacking sequence AAA and shift vectors between successive layers 1a0 + 0b0 + 0.19c0 and 1a0 + 0b0 + 0.24c0, respectively. RUB-36 (diethyldimethylammonium), RUB-38 (methyltriethylammonium) and RUB-48 (trimethylisopropylammonium) are orthorhombic with stacking sequence ABAB and shift vectors 0.5a0 + 0b0± 0.36c0, 0.5a0 + 0b0 + 0.5c0 and 0.5a0 + 0b0± 0.39c0, respectively. Unprecedented among the HLSs, two monoclinic materials are made up of fer layers which possess a significant amount of ordered defects within the layer. The ordered defects involve one particular Si-O-Si bridge which is, to a fraction of ca. 50%, hydrolyzed to form nests of two ≡Si-OH groups. When heated to 500-600 °C in air, the HLSs condense to form framework silicates. Although all layered precursors were moderately to well ordered, the resulting framework structures were of quite different crystallinity. The orthorhombic materials RUB-36, -38 and -48, general formula SDA4Si36O72(OH)4, which possess very strong hydrogen bonds (d[O···O] ≈ 2.4 Å), transform into a fairly or well ordered CDO-type silica zeolite RUB-37. The monoclinic materials RUB-20 and -40, general formula SDA2Si18O36(OH)2OH, possessing

  13. A novel sol-gel-derived calcium silicate cement with short setting time for application in endodontic repair of perforations.

    Science.gov (United States)

    Lee, Bor-Shiunn; Lin, Hong-Ping; Chan, Jerry Chun-Chung; Wang, Wei-Chuan; Hung, Ping-Hsuan; Tsai, Yu-Hsin; Lee, Yuan-Ling

    2018-01-01

    Mineral trioxide aggregate (MTA) is the most frequently used repair material in endodontics, but the long setting time and reduced mechanical strength in acidic environments are major shortcomings. In this study, a novel sol-gel-derived calcium silicate cement (sCSC) was developed using an initial Ca/Si molar ratio of 3, with the most effective mixing orders of reactants and optimal HNO 3 catalyst volumes. A Fourier transform infrared spectrometer, scanning electron microscope with energy-dispersive X-ray spectroscopy, and X-ray powder diffractometer were used for material characterization. The setting time, compressive strength, and microhardness of sCSC after hydration in neutral and pH 5 environments were compared with that of MTA. Results showed that sCSC demonstrated porous microstructures with a setting time of ~30 min, and the major components of sCSC were tricalcium silicate, dicalcium silicate, and calcium oxide. The optimal formula of sCSC was sn200, which exhibited significantly higher compressive strength and microhardness than MTA, irrespective of neutral or pH 5 environments. In addition, both sn200 and MTA demonstrated good biocompatibility because cell viability was similar to that of the control. These findings suggest that sn200 merits further clinical study for potential application in endodontic repair of perforations.

  14. Characterization of goat colostrum oligosaccharides by nano-liquid chromatography on chip quadrupole time-of-flight mass spectrometry and hydrophilic interaction liquid chromatography-quadrupole mass spectrometry.

    Science.gov (United States)

    Martín-Ortiz, A; Salcedo, J; Barile, D; Bunyatratchata, A; Moreno, F J; Martin-García, I; Clemente, A; Sanz, M L; Ruiz-Matute, A I

    2016-01-08

    A detailed qualitative and quantitative characterization of goat colostrum oligosaccharides (GCO) has been carried out for the first time. Defatted and deproteinized colostrum samples, previously treated by size exclusion chromatography (SEC) to remove lactose, were analyzed by nanoflow liquid chromatography-quadrupole-time of flight mass spectrometry (Nano-LC-Chip-Q-TOF MS). Up to 78 oligosaccharides containing hexose, hexosamine, fucose, N-acetylneuraminic acid or N-glycolylneuraminic acid monomeric units were identified in the samples, some of them detected for the first time in goat colostra. As a second step, a hydrophilic interaction liquid chromatography coupled to mass spectrometry (HILIC-MS) methodology was developed for the separation and quantitation of the main GCO, both acidic and neutral carbohydrates. Among other experimental chromatographic conditions, mobile phase additives and column temperature were evaluated in terms of retention time, resolution, peak width and symmetry of target carbohydrates. Narrow peaks (wh: 0.2-0.6min) and good symmetry (As: 0.8-1.4) were obtained for GCO using an acetonitrile:water gradient with 0.1% ammonium hydroxide at 40°C. These conditions were selected to quantify the main oligosaccharides in goat colostrum samples. Values ranging from 140 to 315mgL(-1) for neutral oligosaccharides and from 83 to 251mgL(-1) for acidic oligosaccharides were found. The combination of both techniques resulted to be useful to achieve a comprehensive characterization of GCO. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Synthesis of yttrium silicate luminescent materials by sol-gel method

    International Nuclear Information System (INIS)

    Arkhipov, D.V.; Vasina, O.Yu.; Popovich, N.V.; Galaktionov, S.S.; Soshchin, N.P.

    1996-01-01

    Several yttrium-silicate composition with Y 2 O 3 content within 44-56% have been synthesized. it is ascertained that employment of sol-gel technique permits preparation of luminescent materials on yttrium silicate basis, which compare favourably with bath-produced specimens. The influence of phase composition of sol-gel phosphors on basic performance indices: intensity and luminescence spectrum, has been analyzed

  16. Development of Biomedical Polymer-Silicate Nanocomposites: A Materials Science Perspective

    Directory of Open Access Journals (Sweden)

    Chia-Jung Wu

    2010-04-01

    Full Text Available Biomedical polymer-silicate nanocomposites have potential to become critically important to the development of biomedical applications, ranging from diagnostic and therapeutic devices, tissue regeneration and drug delivery matrixes to various bio-technologies that are inspired by biology but have only indirect biomedical relation. The fundamental understanding of polymer-nanoparticle interactions is absolutely necessary to control structure-property relationships of materials that need to work within the chemical, physical and biological constraints required by an application. This review summarizes the most recent published strategies to design and develop polymer-silicate nanocomposites (including clay based silicate nanoparticles and bioactive glass nanoparticles for a variety of biomedical applications. Emerging trends in bio-technological and biomedical nanocomposites are highlighted and potential new fields of applications are examined.

  17. Simultaneous determination of wine sugars, glycerol and organic acids 13C/12C isotopic ratio by ion chromatography-co-IRMS

    Directory of Open Access Journals (Sweden)

    Guyon Francois

    2014-01-01

    Full Text Available Ion chromatography (IC isotope ratio mass spectrometry (IRMS coupling is possible using a liquid interface allowing chemical oxidation (co of organic compounds. Synthetic solutions containing a mixture of glycerol, sugars (sucrose, glucose and fructose and organic acids (gluconic, lactic, malic, tartaric, oxalic, fumaric, citric and isocitric were elaborated to estimate analytical applications of two different IC systems. It appears that the use of carbonated solution in the eluting phase is a perturbation for 13C isotope measurements as it creates a δ13C deviation from the expected values. A sample of authentic sweet wine was analyzed by IC-co-IRMS using KOH gradient. Ratios of isotopic, ratios of organic acids and glycerol was found to be, in average, equal 1.01 ± 0.04 that is in accordance with our previous results.

  18. Chemical evolution. XXI - The amino acids released on hydrolysis of HCN oligomers

    Science.gov (United States)

    Ferris, J. P.; Wos, J. D.; Nooner, D. W.; Oro, J.

    1974-01-01

    Major amino acids released by hydrolysis of acidic and basic HCN oligomers are identified by chromatography as Gly, Asp, and diaminosuccinic acid. Smaller amounts of Ala, Ile and alpha-aminoisobutyric acid are also detected. The amino acids released did not change appreciably when the hydrolysis medium was changed from neutral to acidic or basic. The presence of both meso and d, l-diaminosuccinic acids was established by paper chromatography and on an amino acid analyzer.

  19. Fast determination of phenoxy acid herbicides in carrots and apples using liquid chromatography coupled triple quadrupole mass spectrometry.

    Science.gov (United States)

    Santilio, Angela; Stefanelli, Patrizia; Dommarco, Roberto

    2009-08-01

    A fast, simple and inexpensive method has been developed for the analysis of phenoxy acid herbicides: 2,4-dichlorophenoxyacetic acid (2,4-D), 4-chloro-2-methylphenoxyacetic acid (MCPA), 2-(4-chloro-o-tolyloxy)propionic acid (MCPP), 2-(4-aryloxyphenoxy)propionic acid (Fluazifop) and 2-(4-aryloxyphenoxy)propionic acid (Haloxyfop) in carrots and apples by liquid chromatography coupled to triple quadrupole mass spectrometry (LC/MS/MS). The compounds were analyzed by QuEChERS (quick, easy, cheap, effective, rugged, safe) methodology without cleanup. The recoveries were performed at two spiked levels (0.05 and 0.5 mg/kg) for both matrices with six replicates for each level. The mean recoveries ranged from 70-92% for both apples and carrots. The precision of the method expressed as relative standard deviation (RSD%) was found to be in the range 3-15%. For all compounds, good linearity (r(2) > 0.99) was obtained over the range of concentration from 0.05 micro g/mL to 0.5 micro g/mL, corresponding to the pesticide concentrations of 0.05 mg/kg and 0.5 mg/kg, respectively. The determination limits (LOQs) ranged from 0.01 ng/mL to 1.3 ng/mL in solvent, whereas, the LOQs calculated in matrix ranged from 0.05 ng/g to 21.0 ng/g for apples and from 0.06 ng/g to 10.2 ng/g for carrots. The developed methodology combines the advantages of both QuEChERS and LC/MS/MS producing a very rapid, sensitive and cheap method useful for the routine analytical laboratories.

  20. The effect of conjugated linoleic acid on the fatty acid composition of ...

    African Journals Online (AJOL)

    rahim aydin

    Dietary conjugated linoleic acid (CLA) was reported to increase the levels of saturated fatty ... Hence, the objective of this study was to determine the effects of dietary CLA on the fatty acid ..... silver ion-high performance liquid chromatography.

  1. Enabling Microliquid Chromatography by Microbead Packing of Microchannels

    Science.gov (United States)

    Balvin, Manuel; Zheng, Yun

    2014-01-01

    The microbead packing is the critical element required in the success of on-chip microfabrication of critical microfluidic components for in-situ analysis and detection of chiral amino acids. In order for microliquid chromatography to occur, there must be a stationary phase medium within the microchannel that interacts with the analytes present within flowing fluid. The stationary phase media are the microbeads packed by the process discussed in this work. The purpose of the microliquid chromatography is to provide a lightweight, low-volume, and low-power element to separate amino acids and their chiral partners efficiently to understand better the origin of life. In order to densely pack microbeads into the microchannels, a liquid slurry of microbeads was created. Microbeads were extracted from a commercially available high-performance liquid chromatography column. The silica beads extracted were 5 microns in diameter, and had surface coating of phenyl-hexyl. These microbeads were mixed with a 200- proof ethanol solution to create a microbead slurry with the right viscosity for packing. A microfilter is placed at the outlet via of the microchannel and the slurry is injected, then withdrawn across a filter using modified syringes. After each injection, the channel is flushed with ethanol to enhance packing. This cycle is repeated numerous times to allow for a tightly packed channel of microbeads. Typical microbead packing occurs in the macroscale into tubes or channels by using highly pressurized systems. Moreover, these channels are typically long and straight without any turns or curves. On the other hand, this method of microbead packing is completed within a microchannel 75 micrometers in diameter. Moreover, the microbead packing is completed into a serpentine type microchannel, such that it maximizes microchannel length within a microchip. Doing so enhances the interactions of the analytes with the microbeads to separate efficiently amino acids and amino acid

  2. Carbonate formation in non-aqueous environments by solid-gas carbonation of silicates

    Science.gov (United States)

    Day, S. J.; Thompson, S. P.; Evans, A.; Parker, J. E.

    2012-02-01

    We have produced synthetic analogues of cosmic silicates using the Sol Gel method, producing amorphous silicates of composition Mg(x)Ca(1-x)SiO3. Using synchrotron X-ray powder diffraction on Beamline I11 at the Diamond Light Source, together with a newly-commissioned gas cell, real-time powder diffraction scans have been taken of a range of silicates exposed to CO2 under non-ambient conditions. The SXPD is complemented by other techniques including Raman and Infrared Spectroscopy and SEM imaging.

  3. Activation of Ca(OH){sub 2} using different siliceous materials

    Energy Technology Data Exchange (ETDEWEB)

    Karatepe, N.; Ersoy-Mericboyu, A.; Kucukbayrak, S. [Istanbul Technical University, Istanbul (Turkey)

    1999-04-01

    Siliceous materials such as silica fume, bentonite and diatomite were mixed with Ca(OH){sub 2} and hydrated at different conditions to produce reactive SO{sub 2} sorbents. Two different hydration methods were used, namely atmospheric and pressure hydration. The effects of the hydration temperature, time and siliceous material/Ca(OH){sub 2} weight ratio on the physical properties of the activated sorbents wereinvestigated. A statistical design technique was applied by use of a two-level factorial design matrix to interpret experimental results. In atmospheric hydration, it was found that increasing the temperature and hydration time caused an increase in the total surface area of the sorbents. But, increasing the siliceous material/Ca(OH){sub 2} weight ratio caused a decrease in the total surface area of the sorbents. In pressure hydration, mathematical analysis showed that the surface area of the activated sorbents was positively affected by the hydration variables. Thermogravimetric measurements showed that increasing the amount of reacted Ca(OH){sub 2} during hydration caused an increase in the surface area of the sorbent. X-ray diffraction studies also indicated that calcium silicate hydrates were the principal Ca-containing species formed during hydration.

  4. Analysis of Free Amino Acids in Different Extracts of Orthosiphon stamineus Leaves by High-Performance Liquid Chromatography Combined with Solid-Phase Extraction.

    Science.gov (United States)

    Shafaei, Armaghan; Halim, Nor Hidayah Ab; Zakaria, Norhidayah; Ismail, Zhari

    2017-10-01

    Orthosiphon stamineus (OS) Benth is a medicinal plant and native in Southeast Asia. Previous studies have shown that OS leaves possess antioxidant, cytotoxic, diuretic, antihypertensive, and uricosuric effects. These beneficial effects have been attributed to the presence of primary and secondary metabolites such as polyphenols, amino acids, and flavonoids. To develop and validate an high-performance liquid chromatography (HPLC)-diode array detector (DAD) method combined with solid-phase extraction that involves precolumn derivatization with O -phthaladehyde for simultaneous analysis of free amino acids in OS leaves extracts. OS leaves were extracted with water (OS-W), ethanol (OS-E), methanol (OS-M), 50% ethanol (OS-EW), and 50% methanol (OS-MW). The extracts were treated by C18 cartridge before derivatization, resulting in great improvement of separation by Zorbox Eclipse XDB-C 18 column. The HPLC-DAD method was successfully developed and validated for analyzing the contents of free amino acids in OS extracts. The results showed that l-aspartic acid with 0.93 ± 0.01 nmol/mg was the major free amino acid in OS-W extract. However, in OS-E, OS-M, OS-EW, and OS-MW, l-glutamic acid with 3.53 ± 0.16, 2.17 ± 0.10, 4.01 ± 0.12, and 2.49 ± 0.12 nmol/mg, respectively, was the major free amino acid. Subsequently, l-serine, which was detected in OS-W, OS-E, and OS-M, was the minor free amino acid with 0.33 ± 0.02, 0.12 ± 0.01, and 0.06 ± 0.01 nmol/mg, respectively. However, l-threonine with 0.26 ± 0.02 and 0.19 ± 0.08 nmol/mL in OS-EW and OS-MW, respectively, had the lowest concentration compared with other amino acid components. All validation parameters of the developed method indicate that the method is reliable and efficient to simultaneously determine the free amino acids content for routine analysis of OS extracts. The HPLC-DAD method combined with solid phase extraction was successfully developed and validated for simultaneous determination and

  5. Detection of radiation-induced hydrocarbons in irradiated fish and prawns by means of on-line coupled liquid chromatography-gas chromatography

    International Nuclear Information System (INIS)

    Schulzki, G.; Spiegelberg, A.; Bogl, K.W.; Schreiberg, G.A.

    1997-01-01

    Radiation-induced hydrocarbons were analyzed in a fatty (halibut) and a lean fish (cod) as well as in a prawn species by on-line coupled liquid chromatography (LC) -gas chromatography (GC) combined with mass spectrometry. In irradiated halibut which is known to contain mainly saturated and monounsaturated fatty acids, all expected radiolytic alkanes, alkenes, and alkadienes could be detected. The yields of the C(n-1) and C(n-2:1) hydrocarbons were comparable to those found in irradiated lipids of terrestrial animals and plants. However, in cod and prawns which contain high levels of polyunsaturated fatty acids (PUFA), the C(n-1) hydrocarbons were found in concentrations which were up to 10 times higher whereas the C(n-2:1) products were again comparable to those of terrestrial animals and plants. The identification of radiation-induced hydrocarbons in fish lipids was achieved by transfer of the hydrocarbons from the LC column to the gas chromatographic column in fractions differing in their degree of unsaturation. For the first time, radiation-induced hydrocarbons with more than four double bonds generated from polyunsaturated fatty acids (20:4 omega 6 and 20:5 omega 3) could be identified

  6. [Application of reversed-phase ion-pair chromatography for universal estimation of octanol-water partition coefficients of acid, basic and amphoteric drugs].

    Science.gov (United States)

    Zhu, Hui; Yang, Ri-Fang; Yun, Liu-Hong; Jiang, Yu; Li, Jin

    2009-09-01

    This paper is to establish a reversed-phase ion-pair chromatography (RP-IPC) method for universal estimation of the octanol/water partition coefficients (logP) of a wide range of structurally diverse compounds including acidic, basic, neutral and amphoteric species. The retention factors corresponding to 100% water (logk(w)) were derived from the linear part of the logk'/phi relationship, using at least four isocratic logk' values containing different organic compositions. The logk(w) parameters obtained were close to the corresponding logP values obtained with the standard "shake flask" methods. The mean deviation for test drugs is 0.31. RP-IPC with trifluoroacetic acid as non classic ion-pair agents can be applicable to determine the logP values for a variety of drug-like molecules with increased accuracy.

  7. Electrical conductivity studies of nanocrystalline lanthanum silicate synthesized by sol-gel route

    International Nuclear Information System (INIS)

    Nallamuthu, N.; Prakash, I.; Satyanarayana, N.; Venkateswarlu, M.

    2011-01-01

    Research highlights: → Nanocrystalline La 10 Si 6 O 27 material was synthesized by sol-gel method. → TG/DTA curves predicted the thermal behavior of the material. → FTIR spectra confirmed the formation of SiO 4 and La-O network in the La 10 Si 6 O 27 . → XRD patterns confirmed the formation of pure crystalline La 10 Si 6 O 27 phase. → The grain interior and the grain boundary conductivities are evaluated. - Abstract: Nanocrystalline apatite type structured lanthanum silicate (La 10 Si 6 O 27 ) sample was synthesized by sol-gel process. Thermal behavior of the dried gel of lanthanum silicate sample was studied using TG/DTA. The structural coordination of the dried gel of lanthanum silicate, calcined at various temperatures, was identified from the observed FTIR spectral results. The observed XRD patterns of the calcined dried gel were compared with the ICDD data and confirmed the formation of crystalline lanthanum silicate phase. The average crystalline size of La 10 Si 6 O 27 was calculated using the Scherrer formula and it is found to be ∼80 nm. The observed SEM images of the lanthanum silicate indicate the formation of the spherical particles and the existence of O, Si and La in the lanthanum silicate are confirmed from the SEM-EDX spectrum. The grain and grain boundary conductivities are evaluated by analyzing the measured impedance data, using winfit software, obtained at different temperatures, of La 10 Si 6 O 27 sample. Also, the observed grain and grain boundary conductivity behaviors of the La 10 Si 6 O 27 sample are analysed using brick layer model. The electrical permittivity and electrical modulus were calculated from the measured impedance data and were analyzed by fitting through the Havriliak and Negami function to describe the dielectric relaxation behavior of the nanocrystalline lanthanum silicate.

  8. Incorporation of Oxygen into Abscisic Acid and Phaseic Acid from Molecular Oxygen 1

    Science.gov (United States)

    Creelman, Robert A.; Zeevaart, Jan A. D.

    1984-01-01

    Abscisic acid accumulates in detached, wilted leaves of Xanthium strumarium. When these leaves are subsequently rehydrated, phaseic acid, a catabolite of abscisic acid, accumulates. Analysis by gas chromatography-mass spectrometry of phaseic acid isolated from stressed and subsequently rehydrated leaves placed in an atmosphere containing 20% 18O2 and 80% N2 indicates that one atom of 18O is incorporated in the 6′-hydroxymethyl group of phaseic acid. This suggests that the enzyme that converts abscisic acid to phaseic acid is an oxygenase. Analysis by gas chromatography-mass spectrometry of abscisic acid isolated from stressed leaves kept in an atmosphere containing 18O2 indicates that one atom of 18O is present in the carboxyl group of abscisic acid. Thus, when abscisic acid accumulates in water-stressed leaves, only one of the four oxygens present in the abscisic acid molecule is derived from molecular oxygen. This suggests that either (a) the oxygen present in the 1′-, 4′-, and one of the two oxygens at the 1-position of abscisic acid arise from water, or (b) there exists a stored precursor with oxygen atoms already present in the 1′- and 4′-positions of abscisic acid which is converted to abscisic acid under conditions of water stress. PMID:16663564

  9. Methylated silicates may explain the release of chlorinated methane from Martian soil

    Science.gov (United States)

    Bak, Ebbe N.; Jensen, Svend J. Knak; Nørnberg, Per; Finster, Kai

    2016-01-01

    The only organic compounds that have been detected in the Martian soil are simple chlorinated compounds released from heated surface material. However, the sources of the organic carbon are in dispute. Wind abraded silicates, which are widespread on the Martian surface, can sequester atmospheric methane which generates methylated silicates and thus could provide a mechanism for accumulation of reduced carbon in the surface soil. In this study we show that thermal volatilization of methylated silicates in the presence of perchlorate leads to the production of chlorinated methane. Thus, methylated silicates could be a source of the organic carbon released as chlorinated methane upon thermal volatilization of Martian soil samples. Further, our experiments show that the ratio of the different chlorinated compounds produced is dependent on the mass ratio of perchlorate to organic carbon in the soil.

  10. Chromatography Analysis of Jatropha Curcas L Oil Raw and Refined

    International Nuclear Information System (INIS)

    Chitue de Assuncao Nascimento, Juliano; Lafargue Perez, Francisco; Diaz Velazquez, Manuel

    2013-01-01

    The chromatography of gases is one of the most versatile methods utilized in the chemical laboratory, which permits the determinations of the percentages and types of fatty acids present in vegetable oils. The objective of this work was to carry out a comparative study of the composition of the fatty acids, of the mechanically extracted oil from the seed of the Jatropha curcas L plant in the raw and refined state, using the data obtained by gas chromatography. The fatty acids of the oil were determined as methylic esteres. The analyst was carried out in a gas chromatographer, with a detector of ionization by way of flame (FID), Agilent 7890A (Agilent, USA) coupled to HP Pentium 4 computer, with a data processing program. The temperatures of the injector and of the detector were 250 °C and 260 °C respectively. The data obtained chromatographically of the oil of Jatropha curcas L, raw and refined indicates that the refinery process did not vary the composition of the fatty acid, because there are no significant differences between them. Also, the results obtained by other investigators, showed that the predominant fatty acids obtained from the oil of the Jatropha curcas L were palmitic and stearic in the saturated fatty acids, and oleic and linoleic in the unsaturated fatty acids

  11. Chromatography analysis of Jatropha Curcas L oil raw and refined

    International Nuclear Information System (INIS)

    Chitue de Assuncao Nascimento, Juliano; Lafargue Perez, Francisco; Diaz Velazquez, Manuel

    2013-01-01

    The chromatography of gases is one of the most versatile methods utilized in the chemical laboratory, which permits the determinations of the percentages and types of fatty acids present in vegetable oils. The objective of this work was to carry out a comparative study of the composition of the fatty acids, of the mechanically extracted oil from the seed of the Jatropha curcas L plant in the raw and refined state, using the data obtained by gas chromatography. The fatty acids of the oil were determined as methylic esteres. The analyst was carried out in a gas chromatographer, with a detector of ionization by way of flame (FID), Agilent 7890A (Agilent, USA) coupled to HP Pentium 4 computer, with a data processing program. The temperatures of the injector and of the detector were 250℃ and 260℃ respectively. The data obtained chromatographically of the oil of Jatropha curcas L, raw and refined indicates that the refinery process did not vary the composition of the fatty acid, because there are no significant differences between them. Also, the results obtained by other investigators, showed that the predominant fatty acids obtained from the oil of the Jatropha curcas L were palmitic and stearic in the saturated fatty acids, and oleic and linoleic in the unsaturated fatty acids

  12. Detection of irradiation history for health foods. Calcium salt of organic acid and its basic ingredient

    International Nuclear Information System (INIS)

    Sekiguchi, Masayuki; Nakagawa, Seiko; Yunoki, Shunji; Ohyabu, Yoshimi

    2013-01-01

    Calcium carbonate and calcium salt of organic acid are well-known food additives used for the improvement of the shelf life and eating quality of health food. Calcium carbonate is a precursor in the synthesis of calcium salts of organic acid. Certain calcium carbonates made of natural limestone mined from very old stratum have silicate minerals exposed to a low level of natural radiation over a long period of time and food additives derived from calcium carbonates contained of such silicate minerals are possible to classify as irradiated foods by PSL and TL analysis in spite of non-irradiation. The study of calcium carbonates and calcium salts of organic acid obtained from different producers were allow to provided appropriate decisions by using the information of both the TL response (Glow1 peak temperature and TL ratio) and PSL ratio. ESR measurements of radicals in such food additives caused by gamma- irradiation were effective tool for correctly determining for irradiation history of those because the measurements were not affected by silicate minerals contained in those. (author)

  13. Liquid chromatography-tandem mass spectrometry assay for the quantification of free and total sialic acid in human cerebrospinal fluid.

    Science.gov (United States)

    van der Ham, Maria; de Koning, Tom J; Lefeber, Dirk; Fleer, André; Prinsen, Berthil H C M T; de Sain-van der Velden, Monique G M

    2010-05-01

    Analysis of sialic acid (SA) metabolites in cerebrospinal fluid (CSF) is important for clinical diagnosis. In the present study, a high-performance liquid chromatography-tandem mass spectrometry (HPLC/MS/MS) method for free sialic acid (FSA) and total sialic acid (TSA) in human CSF was validated. The method utilized a simple sample-preparation procedure of protein precipitation for FSA and acid hydrolysis for TSA. Negative electrospray ionisation was used to monitor the transitions m/z 308.2-->87.0 (SA) and m/z 311.2--> 90.0 ((13)C(3)-SA). Conjugated sialic acid (CSA) was calculated by subtracting FSA from TSA. We established reference intervals for FSA, TSA and CSA in CSF in 217 control subjects. The method has been applied to patients' samples with known differences in SA metabolites like meningitis (n=6), brain tumour (n=2), leukaemia (n=5), and Salla disease (n=1). Limit of detection (LOD) was 0.54 microM for FSA and 0.45 mM for TSA. Intra- and inter-assay variation for FSA (21.8 microM) were 4.8% (n=10) and 10.4% (n=40) respectively. Intra- and inter-assay variation for TSA (35.6 microM) were 9.7% (n=10) and 12.8% (n=40) respectively. Tested patients showed values of TSA above established reference value. The validated method allows sensitive and specific measurement of SA metabolites in CSF and can be applied for clinical diagnoses. 2010 Elsevier B.V. All rights reserved.

  14. Decomposition of silica-alumina ores of Afghanistan by sulfuric acid

    International Nuclear Information System (INIS)

    Khomidi, A.K.; Mamatov, E.D.

    2016-01-01

    Present article is devoted to decomposition of silica-alumina ores of Afghanistan by sulfuric acid. Physicochemical properties of initial silica-alumina ores were studied by means of X-ray phase, differential thermal and silicate analysis. The influence of temperature, process duration and acid concentration on extraction rate of valuable components was considered. The optimal conditions of decomposition of silica-alumina ores of Afghanistan by sulfuric acid were proposed.

  15. Silicates in Alien Asteroids

    Science.gov (United States)

    2009-01-01

    This plot of data from NASA's Spitzer Space Telescopes shows that asteroid dust around a dead 'white dwarf' star contains silicates a common mineral on Earth. The data were taken primarily by Spitzer's infrared spectrograph, an instrument that breaks light apart into its basic constituents. The yellow dots show averaged data from the spectrograph, while the orange triangles show older data from Spitzer's infrared array camera. The white dwarf is called GD 40.

  16. Targeted metabolomics analysis reveals the association between maternal folic acid supplementation and fatty acids and amino acids profiles in rat pups.

    Science.gov (United States)

    Liu, Zhipeng; Liu, Rui; Chou, Jing; Yu, Jiaying; Liu, Xiaowei; Sun, Changhao; Li, Ying; Liu, Liyan

    2018-07-15

    Maternal diet during pregnancy can influence offspring's health by affecting development and metabolism. This study aimed to analyze the influence of maternal folic acid (FA) supplementation on the metabolism of rat pups using targeted metabolomics. Twenty female rats were randomly assigned to a FA supplementation (FAS group, n = 10) or control group (n = 10), which were fed AIN93G diet with 2 or 10 mg/kg FA, respectively. We then measured amino acids and their derivatives, biogenic amines, and fatty acids in the female rats and their pups by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC/MS-MS) and gas chromatography-mass spectrometry (GC/MS-MS). In maternal rats, the significant changes of three metabolites (proline, γ-aminobutyric acid and esterified octadecatetraenoic acid, P acids (leucine, isoleucine, serine, proline) were obtained in FAS pups. Furthermore, there were the decreased esterified fatty acids (arachidonic acid, eicosapentaenoic acid, and docosatetraenoic acid) and free fatty acids (oleic acid, linoleic acid, γ-linolenic acid, octadecatetraenoic acid, arachidonic acid, eicosapentaenoic acid and selacholeic acid) in FAS pups. Metabolic changes in the FAS pups were characterized by changes in fatty acids and amino acids. These results suggested that FA supplementation during pregnancy influenced amino acids and fatty acids metabolism in rat pups. This study provides new insights into the regulation of amino acids and fatty acids metabolism during early life. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. Rapid Quantitative Analysis of Naringenin in the Fruit Bodies of Inonotus vaninii by Two-phase Acid Hydrolysis Followed by Reversed Phase-high Performance Liquid Chromatography-ultra Violet.

    Science.gov (United States)

    Guohua, Xia; Pan, Ruirong; Bao, Rui; Ge, Yanru; Zhou, Cunshan; Shen, Yuping

    2017-01-01

    Sanghuang is one of mystical traditional Chinese medicines recorded earliest 2000 years ago, that included various fungi of Inonotus genus and was well-known for antitumor effect in modern medicine. Inonotus vaninii is grown in natural forest of Northeastern China merely and used as Sanghuang commercially, but it has no quality control specification until now. This study was to establish a rapid method of two-phase acid hydrolysis followed by reversed phase-high performance liquid chromatography-ultra violet (RP-HPLC-UV) to quantify naringenin in the fruit body of I. vaninii . Sample solution was prepared by pretreatment of raw material in two-phase acid hydrolysis and the hydrolysis technology was optimized. After reconstitution, analysis was performed using RP-HPLC-UV. The method validation was investigated and the naringenin content of sample and comparison were determined. The naringenin was obtained by two-phase acid hydrolysis method, namely, 10.0 g of raw material was hydrolyzed in 200 mL of 1% sulfuric acid aqueous solution (v/v) and 400 mL of chloroform in oil bath at 110°C for 2 h. Good linearity ( r = 0.9992) was achieved between concentration of analyte and peak area. The relative standard deviation (RSD) of precision was 2.47% and the RSD of naringenin contents for repeatability was 3.13%. The accuracy was supported with recoveries at 96.37%, 97.30%, and 99.31%. The sample solution prepared using the proposed method contained higher content of naringenin than conventional method and was stable for 8 h. Due to the high efficiency of sample preparation and high reliability of the HPLC method, it is feasible to use this method for routine analysis of naringenin in the fungus. A convenient two-phase acid hydrolysis was employed to produce naringenin from raw material, and then an efficient and reliable reversed phase-high performance liquid chromatography-ultra violet method was established to monitor naringenin in the fruit bodies of Inonotus vaninii

  18. Influence of Surface Conditioning Protocols on Reparability of CAD/CAM Zirconia-reinforced Lithium Silicate Ceramic.

    Science.gov (United States)

    Al-Thagafi, Rana; Al-Zordk, Walid; Saker, Samah

    2016-01-01

    To test the effect of surface conditioning protocols on the reparability of CAD/CAM zirconia-reinforced lithium silicate ceramic compared to lithium-disilicate glass ceramic. Zirconia-reinforced lithium silicate ceramic (Vita Suprinity) and lithium disilicate glass-ceramic blocks (IPS e.max CAD) were categorized into four groups based on the surface conditioning protocol used. Group C: no treatment (control); group HF: 5% hydrofluoric acid etching for 60 s, silane (Monobond-S) application for 60 s, air drying; group HF-H: 5% HF acid etching for 60 s, application of silane for 60 s, air drying, application of Heliobond, light curing for 20 s; group CO: sandblasting with CoJet sand followed by silanization. Composite resin (Tetric EvoCeram) was built up into 4 x 6 x 3 mm blocks using teflon molds. All specimens were subjected to thermocycling (5000x, 5°C to 55°C). The microtensile bond strength test was employed at a crosshead speed of 1 mm/min. SEM was employed for evaluation of all the debonded microbars, the failure type was categorized as either adhesive (failure at adhesive layer), cohesive (failure at ceramic or composite resin), or mixed (failure between adhesive layer and substrate). Two-way ANOVA and the Tukey's HSD post-hoc test were applied to test for significant differences in bond strength values in relation to different materials and surface pretreatment (p ceramic types used (p ceramics and lithium-disilicate glass ceramic could be improved when ceramic surfaces are sandblasted with CoJet sand followed by silanization.

  19. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses.

    Science.gov (United States)

    Muthukrishnan, Suriyavathana; Palanisamy, Subha; Subramanian, Senthilkumar; Selvaraj, Sumathi; Mari, Kavitha Rani; Kuppulingam, Ramalingam

    2016-08-01

    Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV) were identified by using high-performance liquid chromatography (HPLC) and gas chromatography-mass spectroscopy (GC-MS) analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. The HPLC analysis of ELEV showed the presence of gallic and caffeic acids as the major components at concentrations of 2.0 ppm and 0.1 ppm, respectively, as well as other components. GC-MS analysis revealed the presence of 3-eicosyne; 3,7,11,15-tetramethyl-2-hexadecen-1-ol; butanoic acid, 3-methyl-3,7-dimethyl-6-octenyl ester; phytol; 1,2-benzenedicarboxylic acid, diundecyl ester; 1-octanol, 2-butyl-; squalene; and 2H-pyran, 2-(7-heptadecynyloxy) tetrahydro-derivative. Because pharmacopuncture is a new evolving natural mode that uses herbal extracts for treating patients with various ailments with minimum pain and maximum effect, the results of this study are particularly important and show that ELEV possesses a wide range of phytochemical constituents, as indicated above, as effective active principle molecules that can be used individually or in combination to treat patients with various diseases. Copyright © 2016. Published by Elsevier B.V.

  20. Monitoring utilizations of amino acids and vitamins in culture media and Chinese hamster ovary cells by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Qiu, Jinshu; Chan, Pik Kay; Bondarenko, Pavel V

    2016-01-05

    Monitoring amino acids and vitamins is important for understanding human health, food nutrition and the culture of mammalian cells used to produce therapeutic proteins in biotechnology. A method including ion pairing reversed-phase liquid chromatography with tandem mass spectrometry was developed and optimized to quantify 21 amino acids and 9 water-soluble vitamins in Chinese hamster ovary (CHO) cells and culture media. By optimizing the chromatographic separation, scan time, monitoring time window, and sample preparation procedure, and using isotopically labeled (13)C, (15)N and (2)H internal standards, low limits of quantitation (≤0.054 mg/L), good precision (culture media. In a fed-batch process of manufacturing scale bioreactors, two distinguished trends for changes in amino acid concentrations were identified in response to feeding. Ten essential amino acids showed a zigzag pattern with maxima at the feeding days, and 9 non-essential amino acids displayed a smoothly changing profile as they were mainly products of cellular metabolism. Five of 9 vitamins accumulated continuously during the culture period, suggesting that they were fed in access. The method serves as an effective tool for the development and optimization of mammalian cell cultures. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Synthesis and luminescence properties of erbium silicate thin films

    International Nuclear Information System (INIS)

    Miritello, Maria; Lo Savio, Roberto; Iacona, Fabio; Franzo, Giorgia; Bongiorno, Corrado; Priolo, Francesco

    2008-01-01

    We have studied the structure and the room temperature luminescence of erbium silicate thin films deposited by rf magnetron sputtering. Films deposited on silicon oxide layers are characterized by good structural properties and excellent stability. The optical properties of these films are strongly improved by rapid thermal annealing processes performed in the range of temperature 800-1250 deg. C. In fact through the reduction of the defect density of the material, a very efficient room temperature photoluminescence at 1535 nm is obtained. We have also investigated the influence of the annealing ambient, by finding that treatments in O 2 atmosphere are significantly more efficient in improving the optical properties of the material with respect to processes in N 2 . Upconversion effects become effective only when erbium silicate is excited with high pump powers. The evidence that all Er atoms (about 10 22 cm -3 ) in erbium silicate films are optically active suggests interesting perspectives for optoelectronic applications of this material

  2. Fast comprehensive two-dimensional gas chromatography method for fatty acid methyl ester separation and quantification using dual ionic liquid columns.

    Science.gov (United States)

    Nosheen, Asia; Mitrevski, Blagoj; Bano, Asghari; Marriott, Philip J

    2013-10-18

    Safflower oil is a complex mixture of C18 saturated and unsaturated fatty acids amongst other fatty acids, and achieving separation between these similar structure components using one dimensional gas chromatography (GC) may be difficult. This investigation aims to obtain improved separation of fatty acid methyl esters in safflower oil, and their quantification using comprehensive two-dimensional GC (GC×GC). Here, GC×GC separation is accomplished by the coupling of two ionic liquid (IL) column phases: the combination of SLB-IL111 with IL59 column phases was finally selected since it provided excellent separation of a FAME standard mixture, as well as fatty acids in safflower and linseed oil, compared to other tested column sets. Safflower oil FAME were well separated in a short run of 16min. FAME validation was demonstrated by method reproducibility, linearity over a range up to 500mgL(-1), and limits of detection which ranged from 1.9mgL(-1) to 5.2mgL(-1) at a split ratio of 20:1. Quantification was carried out using two dilution levels of 200-fold for major components and 20-fold for trace components. The fatty acids C15:0 and C17:0 were not reported previously in safflower oil. The SLB-IL111/IL59 column set proved to be an effective and novel configuration for separation and quantification of vegetable and animal oil fatty acids. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Virtual Practice of Biochemistry: Ascendant Chromatography on Paper of Amino acids.

    Directory of Open Access Journals (Sweden)

    G. Zanatta

    2010-05-01

    Full Text Available Chromatography is a method used for analyses of mixture components based on different criteria: adsorbility, solubility, molecular mass, ionic charge and affinity. It is an important subject of Biochemistry. This work reports the development and the validation of a software that simulated a laboratory activity named Ascendant Chromatography on Paper of Aminoacids. The organization and the multimedia material collection were done during the 2008/2 semester. The most representative images were inserted into the learning object. The tool used for the software development was Adobe® Flash® CS3. The first application of this object was in Biochemistry I (Pharmacy-UFRGS in 2009/1. Using this experience, a new version was developed which was tested by the students of the same subject in 2009/2. After a 50-minute class (theoretical-practical, the students of both semesters were divided in two groups. Group I answered a questionnaire about chromatography basic concepts and after used the software. Group II was submitted to an inverse protocol. The groups also evaluated the technical aspects of the software animation/simulation and the activity carried out. Associating both applications results (2009/1 and 2009/2, the present learning object can be valid as a support for practical teaching of basic biochemistry.

  4. Calc-silicate mineralization in active geothermal systems

    Energy Technology Data Exchange (ETDEWEB)

    Bird, D.K.; Schiffman, P.; Elders, W.A.; Williams, A.E.; McDowell, S.D.

    1983-01-01

    The detailed study of calc-silicate mineral zones and coexisting phase relations in the Cerro Prieto geothermal system were used as examples for thermodynamic evaluation of phase relations among minerals of variable composition and to calculate the chemical characteristics of hydrothermal solutions compatible with the observed calc-silicate assemblages. In general there is a close correlation between calculated and observed fluid compositions. Calculated fugacities of O{sub 2} at about 320{degrees}C in the Cerro Prieto geothermal system are about five orders of magnitude less than that at the nearby Salton Sea geothermal system. This observation is consistent with the occurrence of Fe{sup 3+} rich epidotes in the latter system and the presence of prehnite at Cerro Prieto.

  5. Insight into silicate-glass corrosion mechanisms

    Energy Technology Data Exchange (ETDEWEB)

    Cailleteau, C; Angeli, F; Gin, S; Jollivet, P [CEA VALRHO, DEN, Lab Etude Comportement Long Terme, F-30207 Bagnols Sur Ceze, (France); Devreux, F [Ecole Polytech, CNRS, Lab Phys Mat Condensee, F-91128 Palaiseau, (France); Jestin, J [CEA, CNRS, Lab Leon Brillouin, F-91191 Gif Sur Yvette, (France); Spalla, O [CEA, DSM, Lab Interdisciplinaire Org Nanometr et Supramol, F-91191 Gif Sur Yvette, (France)

    2008-07-01

    The remarkable chemical durability of silicate glass makes it suitable for a wide range of applications. The slowdown of the aqueous glass corrosion kinetics that is frequently observed at long time is generally attributed to chemical affinity effects (saturation of the solution with respect to silica). Here, we demonstrate a new mechanism and highlight the impact of morphological transformations in the alteration layer on the leaching kinetics. A direct correlation between structure and reactivity is revealed by coupling the results of several structure-sensitive experiments with numerical simulations at mesoscopic scale. The sharp drop in the corrosion rate is shown to arise from densification of the outer layers of the alteration film, leading to pore closure. The presence of insoluble elements in the glass can inhibit the film restructuring responsible for this effect. This mechanism may be more broadly applicable to silicate minerals. (authors)

  6. The preparation of zinc silicate/ZnO particles and their use as an efficient UV absorber

    Energy Technology Data Exchange (ETDEWEB)

    Podbrscek, Peter [National Institute of Chemistry, Hajdrihova 19, SI 1000 Ljubljana (Slovenia); Drazic, Goran [Department for Nanostructured Materials, Jozef Stefan Institute, Jamova 39, SI 1000 Ljubljana (Slovenia); Anzlovar, Alojz [National Institute of Chemistry, Hajdrihova 19, SI 1000 Ljubljana (Slovenia); Center of Excellence for Polymer Materials and Technologies, Tehnoloski Park 24, 1000 Ljubljana (Slovenia); Orel, Zorica Crnjak, E-mail: zorica.crnjak.orel@ki.si [National Institute of Chemistry, Hajdrihova 19, SI 1000 Ljubljana (Slovenia); Center of Excellence for Polymer Materials and Technologies, Tehnoloski Park 24, 1000 Ljubljana (Slovenia)

    2011-11-15

    Highlights: {yields} We used innovative gel-route in order to prepare zinc silicate/ZnO nano-particles. {yields} Continuous reactor was efficient for synthesizing ZnO and zinc silicate/ZnO precursors. {yields} Introduction of Si into reaction mixture influenced on particle size and their photoactivity. {yields} Prepared particles are appropriate for UV absorbers in polymers. -- Abstract: The formation of zinc silicate/ZnO particles synthesized by a two-step method and their incorporation into PMMA is presented. In the first step a segmented-flow tubular reactor was used for the continuous room-temperature preparation of a zinc silicate/Zn(OH){sub 2} gel that was thermally treated after rinsing and drying in the second step. The same preparation procedure was also employed for the synthesis of pure ZnO and pure zinc silicate particles. It was found that the presence of the zinc silicate phase significantly influenced the final particle size, decreased the degree of crystallization and reduced the particles' UV absorption capabilities. The reduced photocatalytic activity of the zinc silicate/ZnO particles indicated that the majority of ZnO crystallites were formed inside the zinc silicate matrix. The nanocomposite prepared from zinc silicate/ZnO particles (0.04 wt.%) and PMMA showed high UV shielding and at the same time sufficient transmittance in the visible-light region.

  7. The preparation of zinc silicate/ZnO particles and their use as an efficient UV absorber

    International Nuclear Information System (INIS)

    Podbrscek, Peter; Drazic, Goran; Anzlovar, Alojz; Orel, Zorica Crnjak

    2011-01-01

    Highlights: → We used innovative gel-route in order to prepare zinc silicate/ZnO nano-particles. → Continuous reactor was efficient for synthesizing ZnO and zinc silicate/ZnO precursors. → Introduction of Si into reaction mixture influenced on particle size and their photoactivity. → Prepared particles are appropriate for UV absorbers in polymers. -- Abstract: The formation of zinc silicate/ZnO particles synthesized by a two-step method and their incorporation into PMMA is presented. In the first step a segmented-flow tubular reactor was used for the continuous room-temperature preparation of a zinc silicate/Zn(OH) 2 gel that was thermally treated after rinsing and drying in the second step. The same preparation procedure was also employed for the synthesis of pure ZnO and pure zinc silicate particles. It was found that the presence of the zinc silicate phase significantly influenced the final particle size, decreased the degree of crystallization and reduced the particles' UV absorption capabilities. The reduced photocatalytic activity of the zinc silicate/ZnO particles indicated that the majority of ZnO crystallites were formed inside the zinc silicate matrix. The nanocomposite prepared from zinc silicate/ZnO particles (0.04 wt.%) and PMMA showed high UV shielding and at the same time sufficient transmittance in the visible-light region.

  8. Potassium silicate and calcium silicate on the resistance of soybean to Phakopsora pachyrhizi infection

    Directory of Open Access Journals (Sweden)

    Maria Fernanda Cruz

    2013-01-01

    Full Text Available The control of Asian Soybean Rust (ASR, caused by Phakopsora pachyrhizi, has been difficult due to the aggressiveness of the pathogen and the lack of resistant cultivars. The objective of this study was to evaluate the effects of spray of potassium silicate (PS and soil amendment with calcium silicate (CS on soybean resistance to ASR. The PS solution was sprayed to leaves 24 hours prior to fungal inoculation while CS was amended to the soil at thirty-five days before sowing. The infection process of P. pachyrhizi was investigated by scanning electron microscopy. The uredia on leaves of plants sprayed with PS were smaller and more compact than those observed on the leaves of plants grown in soil amended with CS or in soil non-amended with CS (control treatment. On leaves of plants from the control treatment, uredia produced many urediniospores at 9 days after inoculation, and the ASR severity was 15, 8 and 9%, respectively, for plants from control, PS and CS treatments. In conclusion, the spray of PS contributed to reduce the number of uredia per cm² of leaf area and both PS spray and CS resulted in lower ASR symptoms.

  9. Valence determination of rare earth elements in lanthanide silicates by L 3-XANES spectroscopy

    International Nuclear Information System (INIS)

    Kravtsova, Antonina N; Guda, Alexander A; Soldatov, Alexander V; Goettlicher, Joerg; Taroev, Vladimir K; Suvorova, Lyudmila F; Tauson, Vladimir L; Kashaev, Anvar A

    2016-01-01

    Lanthanide silicates have been hydrothermally synthesized using Cu and Ni containers. Chemical formulae of the synthesized compounds correspond to K 3 Eu[Si 6 O 15 ] 2H 2 O, HK 6 Eu[Si 10 O 25 ], K 7 Sm 3 [Si 12 O 32 ], K 2 Sm[AlSi 4 O 12 ] 0.375H 2 O, K 4 Yb 2 [Si 8 O 21 ], K 4 Ce 2 [Al 2 Si 8 O 24 ]. The oxidation state of lanthanides (Eu, Ce, Tb, Sm, Yb) in these silicates has been determined using XANES spectroscopy at the Eu, Ce, Tb, Sm, Yb, L 3 - edges. The experimental XANES spectra were recorded using the synchrotron radiation source ANKA (Karlsruhe Institute of Technology) and the X-ray laboratory spectrometer Rigaku R- XAS. By comparing the absorption edge energies and white line intensities of the silicates with the ones of reference spectra the oxidation state of lanthanides Eu, Ce, Tb, Sm, Yb has been found to be equal to +3 in all investigated silicates except of the Ce-containing silicate from the run in Cu container where the cerium oxidation state ranges from +3 (Ce in silicate apatite and in a KCe silicate with Si 12 O 32 layers) to +4 (starting CeO 2 or oxidized Ce 2 O 3 ). (paper)

  10. N-Acetyl-9-O-L-lactylneuraminic acid, a new acylneuraminic acid from bovine submandibular gland

    NARCIS (Netherlands)

    Vliegenthart, J.F.G.; Schauer, R.; Haverkamp, J.; Wember, M.; Kamerling, J.P.

    1976-01-01

    The acylneuraminic acid fraction, obtained on mild acid hydrolysis of glycoproteins from bovine submandibular glands, contains approximately 2 % N-acetyl-9-O-l-lactylneuraminic acid. The compound has been isolated and purified by ion-exchange and cellulose column chromatography. The structure has

  11. Metabolism of clofibric acid in zebrafish embryos (Danio rerio) as determined by liquid chromatography-high resolution-mass spectrometry.

    Science.gov (United States)

    Brox, Stephan; Seiwert, Bettina; Haase, Nora; Küster, Eberhard; Reemtsma, Thorsten

    2016-01-01

    The zebrafish embryo (ZFE) is increasingly used in ecotoxicology research but detailed knowledge of its metabolic potential is still limited. This study focuses on the xenobiotic metabolism of ZFE at different life-stages using the pharmaceutical compound clofibric acid as study compound. Liquid chromatography with quadrupole-time-of-flight mass spectrometry (LC-QToF-MS) is used to detect and to identify the transformation products (TPs). In screening experiments, a total of 18 TPs was detected and structure proposals were elaborated for 17 TPs, formed by phase I and phase II metabolism. Biotransformation of clofibric acid by the ZFE involves conjugation with sulfate or glucuronic acid, and, reported here for the first time, with carnitine, taurine, and aminomethanesulfonic acid. Further yet unknown cyclization products were identified using non-target screening that may represent a new detoxification pathway. Sulfate containing TPs occurred already after 3h of exposure (7hpf), and from 48h of exposure (52hpf) onwards, all TPs were detected. The detection of these TPs indicates the activity of phase I and phase II enzymes already at early life-stages. Additionally, the excretion of one TP into the exposure medium was observed. The results of this study outline the high metabolic potential of the ZFE with respect to the transformation of xenobiotics. Similarities but also differences to other test systems were observed. Biotransformation of test chemicals in toxicity testing with ZFE may therefore need further consideration. Copyright © 2016 Elsevier Inc. All rights reserved.

  12. Use of [18O4] phosphoric acid in the quantitation of phosphate by gas-liquid chromatography-mass spectrometry analysis

    International Nuclear Information System (INIS)

    Graff, G.; Krick, T.P.; Walseth, T.F.; Goldberg, N.D.

    1980-01-01

    A procedure is described to quantitate inorganic phosphate in the form of the tris(trimethylsilyl) (TMS) phosphate by gas-liquid chromatography-mass spectrometry (glc-ms) that increases the previously reported detection limit from the microgram to the nanogram range. The sensitivity for detecting TMS-phosphate by glc-ms analysis was shown to be limited by an increasing fractional loss with decreasing concentrations of TMS-phosphate analyzed due to its adsorption on different types of glc column supports. The method developed employs [ 18 O 4 ] phosphoric acid which serves as both an internal standard to permit quantitation and as a carrier to minimize sample adsorption on the glc column support

  13. Urinary Amino Acid Analysis: A Comparison of iTRAQ®-LC-MS/MS, GC-MS, and Amino Acid Analyzer

    OpenAIRE

    Kaspar, Hannelore; Dettmer, Katja; Chan, Queenie; Daniels, Scott; Nimkar, Subodh; Daviglus, Martha L.; Stamler, Jeremiah; Elliott, Paul; Oefner, Peter J.

    2009-01-01

    Urinary amino acid analysis is typically done by cation-exchange chromatography followed by post-column derivatization with ninhydrin and UV detection. This method lacks throughput and specificity. Two recently introduced stable isotope ratio mass spectrometric methods promise to overcome those shortcomings. Using two blinded sets of urine replicates and a certified amino acid standard, we compared the precision and accuracy of gas chromatography/mass spectrometry (GC-MS) and liquid chromatog...

  14. Carbonate-silicate liquid immiscibility in the mantle propels kimberlite magma ascent

    Science.gov (United States)

    Kamenetsky, Vadim S.; Yaxley, Gregory M.

    2015-06-01

    Kimberlite is a rare volcanic rock renowned as the major host of diamonds and originated at the base of the subcontinental lithospheric mantle. Although kimberlite magmas are dense in crystals and deeply-derived rock fragments, they ascend to the surface extremely rapidly, enabling diamonds to survive. The unique physical properties of kimberlite magmas depend on the specific compositions of their parental melts that, in absence of historical eruptions and due to pervasive alteration of kimberlite rocks, remain highly debatable. We explain exceptionally rapid ascent of kimberlite magma from mantle depths by combining empirical data on the essentially carbonatite composition of the kimberlite primary melts and experimental evidence on interaction of the carbonate liquids with mantle minerals. Our experimental study shows that orthopyroxene is completely dissolved in a Na2CO3 melt at 2.0-5.0 GPa and 1000-1200 °C. The dissolution of orthopyroxene results in homogeneous silicate-carbonate melt at 5.0 GPa and 1200 °C, and is followed by unmixing of carbonate and carbonated silicate melts and formation of stable magmatic emulsion at lower pressures and temperatures. The dispersed silicate melt has a significant capacity for storing a carbonate component in the deep mantle (13 wt% CO2 at 2.0 GPa). We envisage that this component reaches saturation and is gradually released as CO2 bubbles, as the silicate melt globules are transported upwards through the lithosphere by the carbonatite magma. The globules of unmixed, CO2-rich silicate melt are continuously produced upon further reaction between the natrocarbonatite melt and mantle peridotite. On decompression the dispersed silicate melt phase ensures a continuous supply of CO2 bubbles that decrease density and increase buoyancy and promote rapid ascent of the magmatic emulsion.

  15. Field and Experimental Constraints on the Dynamics of Replenished Silicic Magma Chambers

    Science.gov (United States)

    Bain, A. A.; Jellinek, M.

    2008-12-01

    The underlying causes of catastrophic caldera-forming volcanic eruptions remain poorly understood. However, the occurrence of magma mixing within bimodal systems has become increasingly linked with such eruptions. In particular, buoyancy effects related to unstable density contrasts arising as a result of silicic- basaltic magma interactions may play an important role in the growth, differentiation and catastrophic eruption of silicic magma chambers. Evidence of such magmatic interactions can be found in layered intrusions from the Coastal Maine Magmatic Province (USA), where well-exposed cross-sections reveal hundreds of laterally-extensive basaltic sheets, apparently injected as intrusive lava flows onto the growing floors of silicic magma chambers. Interfaces between mafic and silicic layers are commonly sharply defined and exhibit deformation parallel to the inferred direction of palaeo-gravity. Our field observations suggest that the cooling, settling and buckling of gravitationally-unstable mafic replenishments may have driven large-scale (basalt layer depth) and small- scale (crystal diameter) upwelling and/or overturning of underlying buoyant silicic cumulate material. In order to characterize the full range of buoyancy effects, we carried out extensive spectral analysis of high- resolution digital field measurements from the Pleasant Bay and Mount Desert Island intrusions. In many cases, Rayleigh-Taylor theory and the longest measured wavelength of deformation indicate that a large and potentially-quantifiable fraction of the original, pre-replenishment silicic cumulate thickness may be missing, implying that vertical mass transfer has occurred. In addition, the shortest wavelengths of deformation are generally consistent with observed length-scales of crystals and clumps of crystals at these localities. With the aim of understanding the initial conditions that gave rise to these field observations, we conduct a series of laboratory experiments in which we

  16. Determination of Fatty Acid in Asparagus by Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Zehra HAJRULAI-MUSLIU

    2016-05-01

    Full Text Available Asparagus contain a lot of macronutrients and micronutrients including folate, dietary fibre (soluble and insoluble and phenolic compounds. Also asparagus is a good source of unsaturated linoleic and linolenic fatty acids which are precursors for Eicosapentanoic acid (EPA and Docosahexanoic acid (DHA. Unsaturated fatty acids have important biological effects and they have important role in human health. The objective of this study was to analyze fatty acid composition of asparagus as a potential source of linoleic and linolenic acid - a precursor for EPA and DHA. For this reason we analyzed fifty seven samples of asparagus collected from the local market. We used AOAC 996.06 method and analyses were performed with gas chromatograph with flame-ionization detector (GC-FID. The highest concentration of fatty acid in the asparagus was linoleic acid (C18:2n6 which content in asparagus is 25.620±1.0%. Also, asparagus is good source of -linolenic fatty acid (C18:3n3 and content of this fatty acid in asparagus is 8.840±0.3%. The omega-6 to omega-3 (n6/n3 ratio in asparagus was 3.19. Polyunsaturated fatty acids (PUFAs were higher than monounsaturated fatty acids (MUFAs, and from saturated fatty acids, palmitic acid was most frequent with 24.324±1.0%. From our study we can conclude that asparagus is very good source of unsaturated fatty acids, especially linoleic and linolenic fatty acids.

  17. Silicate glasses

    International Nuclear Information System (INIS)

    Lutze, W.

    1988-01-01

    Vitrification of liquid high-level radioactive wastes has received the greatest attention, world-wide, compared to any other HLW solidification process. The waste form is a borosilicate-based glass. The production of phosphate-based glass has been abandoned in the western world. Only in the Soviet Union are phosphate-based glasses still being developed. Vitrification techniques, equipment and processes and their remote operation have been developed and studied for almost thirty years and have reached a high degree of technical maturity. Industrial demonstration of the vitrification process has been in progress since 1978. This chapter is a survey of world-wide research and development efforts in nuclear waste glasses and its production technology. The principal glasses considered are silicate glasses which contain boron, i.e., borosilicate glasses

  18. Determination of chloroacetanilide herbicide metabolites in water using high-performance liquid chromatography-diode array detection and high-performance liquid chromatography/mass spectrometry

    Science.gov (United States)

    Hostetler, K.A.; Thurman, E.M.

    2000-01-01

    Analytical methods using high-performance liquid chromatography-diode array detection (HPLC-DAD) and high-performance liquid chromatography/mass spectrometry (HPLC/MS) were developed for the analysis of the following chloroacetanilide herbicide metabolites in water: alachlor ethanesulfonic acid (ESA); alachlor oxanilic acid; acetochlor ESA; acetochlor oxanilic acid; metolachlor ESA; and metolachlor oxanilic acid. Good precision and accuracy were demonstrated for both the HPLC-DAD and HPLC/MS methods in reagent water, surface water, and ground water. The average HPLC-DAD recoveries of the chloroacetanilide herbicide metabolites from water samples spiked at 0.25, 0.5 and 2.0 ??g/l ranged from 84 to 112%, with relative standard deviations of 18% or less. The average HPLC/MS recoveries of the metabolites from water samples spiked at 0.05, 0.2 and 2.0 ??g/l ranged from 81 to 118%, with relative standard deviations of 20% or less. The limit of quantitation (LOQ) for all metabolites using the HPLC-DAD method was 0.20 ??g/l, whereas the LOQ using the HPLC/MS method was at 0.05 ??g/l. These metabolite-determination methods are valuable for acquiring information about water quality and the fate and transport of the parent chloroacetanilide herbicides in water. Copyright (C) 2000 Elsevier Science B.V.

  19. Polymer Analysis by Liquid Chromatography/Electrospray Ionization Time-of-Flight Mass Spectrometry.

    Science.gov (United States)

    Nielen, M W; Buijtenhuijs, F A

    1999-05-01

    Hyphenation of liquid chromatography (LC) techniques with electrospray ionization (ESI) orthogonal acceleration time-of-flight (oa-TOF) mass spectrometry (MS) provides both MS-based structural information and LC-based quantitative data in polymer analysis. In one experimental setup, three different LC modes are interfaced with MS:  size-exclusion chromatography (SEC/MS), gradient polymer elution chromatography (GPEC/MS), and liquid chromatography at the critical point of adsorption (LCCC/MS). In SEC/MS, both absolute mass calibration of the SEC column based on the polymer itself and determination of monomers and end groups from the mass spectra are achieved. GPEC/MS shows detailed chemical heterogeneity of the polymer and the chemical composition distribution within oligomer groups. In LCCC/MS, the retention behavior is primarily governed by chemical heterogeneities, such as different end group functionalities, and quantitative end group calculations can be easily made. The potential of these methods and the benefit of time-of-flight analyzers in polymer analysis are discussed using SEC/MS of a polydisperse poly(methyl methacrylate) sample, GPEC/MS of dipropoxylated bisphenol A/adipic acid polyester resin, LCCC/MS of alkylated poly(ethylene glycol), and LCCC/MS of terephthalic acid/neopentyl glycol polyester resin.

  20. Mid-infrared spectra of cometary dust: the evasion of its silicate mineralogy

    Science.gov (United States)

    Kimura, H.; Chigai, T.; Yamamoto, T.

    2008-04-01

    Infrared spectra of dust in cometary comae provide a way to identify its silicate constituents, and this is crucial for correctly understanding the condition under which our planetary system is formed. Recent studies assign a newly detected peak at a wavelength of 9.3 μm to pyroxenes and regard them as the most abundant silicate minerals in comets. Here we dispense with this pyroxene hypothesis to numerically reproduce the infrared features of cometary dust in the framework of our interstellar dust models. Presolar interstellar dust in a comet is modeled as fluffy aggregates consisting of submicrometer-sized organic grains with an amor