A green two-step process for adipic acid production from cyclohexene. A study on parameters affecting selectivity

Energy Technology Data Exchange (ETDEWEB)

Cavani, F.; Macchia, F.; Pino, R.; Raabova, K.; Rozhko, E. [Bologna Univ. (Italy). Dipt. di Chimica Industriale e dei Materiali; Alini, S.; Accorinti, P.; Babini, G. [Radici Chimica SpA, Novara (Italy)

2011-07-01

In this paper, we report about the effect of reaction parameters on catalytic behavior in a twostep process aimed at the synthesis of adipic acid from cyclohexene. In the first step, cyclohexene reacts with an aqueous solution of hydrogen peroxide, under conditions leading to the formation of trans-1,2-cyclohexandiol as the prevailing product; the reaction is catalysed by tungstic acid, in the presence of phosphoric acid and of a PT agent. In the second step, 1,2-cyclohexandiol is oxidized with air, in the presence of an heterogeneous catalyst made of alumina-supported Ru(OH){sub 3}. This process is aimed at using the minimal amount of the costly hydrogen peroxide, since only one mole is theoretically needed per mole of cyclohexene. The first step afforded very high yield to the glycol, using only a slight excess of hydrogen peroxide. However, the second step turned out to be the more critical one, since the selectivity to adipic acid was very low because of the concomitant occurrence of several undesired side reactions. The latter were in part due to the reaction conditions used, which were necessary for the activation of cyclohexandiol. (orig.)

A bio-based ‘green’ process for catalytic adipic acid production from lignocellulosic biomass using cellulose and hemicellulose derived γ-valerolactone

International Nuclear Information System (INIS)

Han, Jeehoon

2016-01-01

Highlights: • A bio-based ‘green’ process for catalytic conversion of corn stover to adipic acid (ADA) is studied. • New separations for effective recovery of biomass derivatives are developed. • Separations are integrated with cellulose/hemicellulose-to-ADA conversions. • Proposed process can compete economically with the current petro-based process. - Abstract: A bio-based ‘green’ process is presented for the catalytic conversion of corn stover to adipic acid (ADA) based on experimental studies. ADA is used for biobased nylon 6.6 manufacturing from lignocellulosics as carbon and energy source. In this process, the cellulose and hemicellulose fractions are catalytically converted to γ-valerolactone (GVL), using cellulose and hemicellulose-derived GVL as a solvent, and subsequently upgrading to ADA. Experimental studies showed maximal carbon yields (biomass-to-GVL: 41% and GVL-to-ADA: 46%) at low concentrations (below 16 wt% solids) using large volumes of GVL solvents while requiring efficient interstage separations and product recovery. This work presents an integrated process, including catalytic conversion and separation subsystems for GVL and ADA production and recovery, and designs a heat exchanger network to satisfy the total energy requirements of the integrated process via combustion of biomass residues (lignin and humins). Finally, an economic analysis shows that 2000 metric tonnes (Mt) per day of corn stover feedstock processing results in a minimum selling price of $633 per Mt if using the best possible parameters.

Structure and properties of Al-MIL-53-ADP, a breathing MOF based on the aliphatic linker molecule adipic acid.

Science.gov (United States)

Reinsch, Helge; Pillai, Renjith S; Siegel, Renée; Senker, Jürgen; Lieb, Alexandra; Maurin, Guillaume; Stock, Norbert

2016-03-14

The new aluminium based metal-organic framework [Al(OH)(O2C-C4H8-CO2)]·H2O denoted as Al-MIL-53-ADP-lp (lp stands for large pore) was synthesised under solvothermal conditions. This solid is an analogue of the archetypical aluminium terephthalate Al-MIL-53 based on the aliphatic single-chain linker molecule adipic acid (H2ADP, hexanedioic acid). In contrast to its aromatic counterparts, Al-MIL-53-ADP exhibits a structural breathing behaviour solely upon dehydration/rehydration. The crystal structure of the anhydrous compound denoted as Al-MIL-53-ADP-np (np stands for narrow pore) was determined by a combination of forcefield-based computations and Rietveld refinement of the powder X-ray diffraction data while the structure of the hydrated form Al-MIL-53-ADP-lp was derived computationally by a combination of force field based methods and Density Functional Theory calculations. Both structures were further supported by (1)H, (13)C and (27)Al high-resolution NMR MAS 1D data coupled again with simulations. Al-MIL-53-ADP was further characterised by means of vibrational spectroscopy, elemental analysis, thermogravimetry and water vapour sorption.

Amended final report of the safety assessment of dibutyl adipate as used in cosmetics.

Science.gov (United States)

Andersen, Alan

2006-01-01

Dibutyl Adipate, the diester of butyl alcohol and adipic acid, functions as a plasticizer, skin-conditioning agent, and solvent in cosmetic formulations. It is reportedly used at a concentration of 5% in nail polish and 8% in suntan gels, creams, and liquids. Dibutyl Adipate is soluble in organic solvents, but practically insoluble in water. Dibutyl Adipate does not absorb radiation in the ultraviolet (UV) region of the spectrum. Dibutyl Adipate is not toxic in acute oral or dermal animal toxicity tests. In a subchronic dermal toxicity study, 1.0 ml/kg day-1 caused a significant reduction in body weight gain in rabbits, but 0.5 ml/kg/day1 was without effect. In a study with dogs, no adverse effects were observed when an emulsion containing 6.25% Dibutyl Adipate was applied to the entire body twice a week for 3 months. Dibutyl Adipate was tested for dermal irritation using rabbits and mice and a none to minimal irritation was observed. Dibutyl Adipate at a concentration of 25% was not a sensitizer in a guinea pig maximization study. Undiluted Dibutyl Adipate was minimally irritating to the eyes of rabbits and 0.1% was nonirritating. A significant increase in fetal gross abnormalities was observed in rats given intraperitoneal injections of Dibutyl Adipate at 1.75 ml/kg on 3 separate days during gestation, but no effect was seen in animals given 1.05 ml/kg. Dibutyl Adipate was not genotoxic in either bacterial or mammalian test systems. Clinical patch tests confirmed the absence of skin irritation found in animal tests. Clinical phototoxicity tests were negative. Dibutyl Adipate at 0.1% was not an ocular irritant in two male volunteers. In a clinical test of comedogenicity, Dibutyl Adipate produced no effect. The Cosmetic Ingredient Review (CIR) Expert Panel recognized that use of Dibutyl Adipate in suntan cosmetic products will result in repeated, frequent exposure in a leave-on product. The available data demonstrate no skin sensitization or cumulative skin

Supramolecular architecture in a co-crystal of the N(7—H tautomeric form of N6-benzoyladenine with adipic acid (1/0.5

Directory of Open Access Journals (Sweden)

Robert Swinton Darious

2016-06-01

Full Text Available The asymmetric unit of the title co-crystal, C12H9N5O·0.5C6H10O4, consists of one molecule of N6-benzoyladenine (BA and one half-molecule of adipic acid (AA, the other half being generated by inversion symmetry. The dihedral angle between the adenine and phenyl ring planes is 26.71 (7°. The N6-benzoyladenine molecule crystallizes in the N(7—H tautomeric form with three non-protonated N atoms. This tautomeric form is stabilized by intramolecular N—H...O hydrogen bonding between the carbonyl (C=O group and the N(7—H hydrogen atom on the Hoogsteen face of the purine ring, forming an S(7 ring motif. The two carboxyl groups of adipic acid interact with the Watson–Crick face of the BA molecules through O—H...N and N—H...O hydrogen bonds, generating an R22(8 ring motif. The latter units are linked by N—H...N hydrogen bonds, forming layers parallel to (10-5. A weak C—H...O hydrogen bond is also present, linking adipic acid molecules in neighbouring layers, enclosing R22(10 ring motifs and forming a three-dimensional structure. C=O...π and C—H...π interactions are also present in the structure.

Supra-molecular architecture in a co-crystal of the N(7)-H tautomeric form of N (6)-benzoyl-adenine with adipic acid (1/0.5).

Science.gov (United States)

Swinton Darious, Robert; Thomas Muthiah, Packianathan; Perdih, Franc

2016-06-01

The asymmetric unit of the title co-crystal, C12H9N5O·0.5C6H10O4, consists of one mol-ecule of N (6)-benzoyl-adenine (BA) and one half-mol-ecule of adipic acid (AA), the other half being generated by inversion symmetry. The dihedral angle between the adenine and phenyl ring planes is 26.71 (7)°. The N (6)-benzoyl-adenine mol-ecule crystallizes in the N(7)-H tautomeric form with three non-protonated N atoms. This tautomeric form is stabilized by intra-molecular N-H⋯O hydrogen bonding between the carbonyl (C=O) group and the N(7)-H hydrogen atom on the Hoogsteen face of the purine ring, forming an S(7) ring motif. The two carboxyl groups of adipic acid inter-act with the Watson-Crick face of the BA mol-ecules through O-H⋯N and N-H⋯O hydrogen bonds, generating an R 2 (2)(8) ring motif. The latter units are linked by N-H⋯N hydrogen bonds, forming layers parallel to (10-5). A weak C-H⋯O hydrogen bond is also present, linking adipic acid mol-ecules in neighbouring layers, enclosing R (2) 2(10) ring motifs and forming a three-dimensional structure. C=O⋯π and C-H⋯π inter-actions are also present in the structure.

Influence of the addition of bentonite clay in poli (butylene adipate co-terephthalic) / poly(lactic acid) membranes

International Nuclear Information System (INIS)

Morais, D.D.S.; Medeiros, K.M.; Araujo, E.M.; Melo, T.J.A.; Barbosa, R.

2014-01-01

The processes of membrane separation have been used in many different sectors of industrial activity, ranging from the chemical industry, food, pharmaceutical, medical and biotech. In this paper, a bentonite clay was added by melt intercalation in a poly(butylene adipate-co-terephthalic acid)/poly(lactic acid) blend at levels 1 and 3 wt% of clay. After that, membranes were produced by solvent evaporation technique. From the XRD results, it was verified the possible formation of exfoliated/partially exfoliated structures in the membranes. By DSC, it was observed that the addition of clay did not promote alterations in glass transition temperature and crystalline melting of the PBAT/PLA matrix. The morphology of the membranes were observed by SEM and it was verified the clay formation of porous membranes. (author)

Analysis of Adipate Ester Contents in PVC Plastics

DEFF Research Database (Denmark)

Berg, Rolf W.

2006-01-01

Plasticizers are needed in flexible PVC (PolyVinylChloride) products. There is serious concern that commonly used phthalate esters may harm life reproduction systems. To avoid the problems, instead adipate di-esters (AEs) of C8 to C10 alcohols are used as higher prized alternatives; e.g. di-2......-ethylhexyl adipate or DEHA [103-23-1], also known as Adimoll® or di-octyl adipate, DOA, see Fig. 1. A widely used plasticizer in food (cling) films is DEHA, often in combination with polymers, epoxidized soya-bean oil, etcetera. DEHA also occurs in children toys. We have previously shown that the presence...... of phthalate esters in PVC can be rapidly analyzed by Fourier transform (FT-) Raman spectroscopy excited with a 1064 nm laser. Here in this project we report a similar study. The aim was to find out whether FT-Raman spectroscopy can be used to determine the presence of adipate esters (AEs) as plasticizers...

Poly(glycerol adipate) - indomethacin drug conjugates - synthesis and in vitro characterization.

Science.gov (United States)

Wersig, T; Hacker, M C; Kressler, J; Mäder, K

2017-10-05

The linear biodegradable polyester poly(glycerol adipate) (PGA) was synthesized via enzymatic polycondensation using lipase B from Candida antarctica (CAL-B). Every monomer unit of PGA possesses a pendant hydroxyl group which is responsible for the hydrophilic character and moisture swelling. These OH groups were esterified to different degrees with the anti-inflammatory drug indomethacin in order to create a prodrug with a pH-sensitive linker for modified drug release. The structure of the conjugates was determined via ATR FT-IR spectroscopy, NMR spectroscopy, GPC and UV/VIS spectroscopy. The physical properties of polymers with different drug load were investigated using DSC, contact angle measurements and oscillatory rheology. Drug release was monitored over one month in vitro. A very slow, but continuous release was observed in PBS. Slightly acidic conditions and lipase activity are accelerating the indomethacin release. Therefore, poly(glycerol adipate) - indomethacin conjugates are promising prodrugs for the local sustained release of indomethacin. Copyright © 2017 Elsevier B.V. All rights reserved.

Effect of addition of lignin in physical-chemical properties of a polyesters based on glycerol, phthalic and adipic acids; Efeito da adicao de lignina nas propriedades fisico-quimicas de poliesteres a base de glicerol e acidos ftalico e adipico

Energy Technology Data Exchange (ETDEWEB)

Guimaraes, D.H.; Viana, A.P.M.; Lima, A.S.C.; Goncalves, A.P.B.; Miranda, C.S.; Jose, N.M., E-mail: dhanseng@yahoo.com.br [Universidade Federal da Bahia (UFBA), alvador, BA (Brazil)

2014-07-01

In this paper the study of different addition amounts of lignin in the physicochemical properties of polyesters made from glycerol and different amounts of phthalic and adipic acids have been proposed. The following characterizations were made: XRD, FTIR, TGA, DSC and SEM. The variation in the percentage of adipic and phthalic acids had a direct effect on thermal and morphological properties. The thermal analysis showed that there was miscibility between the polyester and lignin, by means of displacement related to the temperature of thermal degradation events. In FTIR analysis was noted displacements of characteristic bands of hydrogen bonds and specific carbonyl ester groups. These shifts were more pronounced as it has larger amounts of phthalic acid as monomer and larger amounts of lignin in the compositions. (author)

40 CFR 721.8079 - Isophorone diisocyanate neopentyl glycol adipate polyurethane prepolymer.

Science.gov (United States)

2010-07-01

... glycol adipate polyurethane prepolymer. 721.8079 Section 721.8079 Protection of Environment ENVIRONMENTAL... adipate polyurethane prepolymer. (a) Chemical substance and significant new uses subject to reporting. (1... polyurethane prepolymer (PMN P-94-1743) is subject to reporting under this section for the significant new uses...

Overview of MIT, ADIP irradiation experiments

International Nuclear Information System (INIS)

Kohse, G.; Harling, O.K.; Grant, N.J.

1985-06-01

Various rapidly solidified austenitic, ferritic and copper alloys have been produced at MIT for inclusion in ADIP neutron irradiation experiments. A brief summary of the alloys and their preparation and the achieved or projected irradiation parameters is provided

The liquid–liquid coexistence curves of {x dimethyl adipate + (1 − x) n-hexane} and {x dimethyl adipate + (1 − x) n-heptane} in the critical region

International Nuclear Information System (INIS)

Chen Zhiyun; Cai Li; Huang Meijun; Yin Tianxiang; An Xueqin; Shen Weiguo

2012-01-01

Highlights: ► Coexistence curves of (dimethyl adipate + n-hexane) (+n-heptane) were measured. ► The critical exponent β are consistent with the 3D-Ising value. ► The asymmetry of the coexistence curves were discussed by complete scaling theory. - Abstract: The liquid–liquid coexistence curves for (dimethyl adipate + n-hexane), (dimethyl adipate + n-heptane) have been measured, from which the critical amplitudes and the critical exponents are deduced. The critical exponent β corresponding to the coexistence curves are consistent with the 3D-Ising value. The experimental results have also been analyzed to determine the critical amplitudes of Wegner-correction terms when β and Δ are fixed at their theoretical values, and to examine the asymmetry of the diameters for the coexistence curves.

Preparation of deuteriated adipic [2H2]-, [2H4]-, [2H6]-, and [2H8]-acids by use of Kolbe electrolysis as a key reaction

International Nuclear Information System (INIS)

Tashiro, Masahi; Tsuzuki, Hirohisa; Mataka, Shuntaro; Goto, Hideyuki; Ogasahara, Shoji

1990-01-01

Using Kolbe electrolysis of methyl hydrogen [ 2 H 0 ]-, [ 2 H 2 ]-, and [ 2 H 4 ]-succinates as a key reaction, adipic [2,2- 2 H 2 ]-, [2,3- 2 H 2 ]-, [2,2,3,3- 2 H 4 ]-, [2,3,4,5- 2 H 4 ]-, [2,3,5,5- 2 H 4 ]-, [2,2,3,3,5,5- 2 H 6 ]-, and [2,2,3,3,4,4,5,5- 2 H 8 ]-acids were prepared in high deuterium contents. (author)

ANALYSIS OF ADIPATE ESTER CONTENTS IN POLY(VINYL CHLORIDE) PLASTICS

DEFF Research Database (Denmark)

Berg, Rolf W.; Otero, Amalia Dopazo

2006-01-01

Fourier transform (FT-) Raman spectroscopy excited with a 1064 nm laser can be used to determine the content of plasticizers in commercial flexible poly vinyl chloride (PVC) products. Our previous study [T. Nørbygaard, R.W. Berg, Analysis of phthalate ester content in PVC plastics by means of FT......-Raman Spectroscopy, Appl. Spectrosc. 58 (4) (2004) 410–413]—on detection of the presence of phthalate esters in PVC by FT-Raman spectroscopy — is here extended to the similar case of adipate esters (AEs) in samples of soft poly vinyl chloride plastics. Spectra of a range of adipate ester plasticizers (11 AEs......) in pure form are reported. We studied if qualitative and quantitative determination of the adipate ester content would be possible based on the use of proper reference samples. It was found that AEs as a group cannot be definitively identified by their characteristic Raman bands because other aliphatic...

Solid acid catalysis from fundamentals to applications

CERN Document Server

Hattori, Hideshi

2014-01-01

IntroductionTypes of solid acid catalystsAdvantages of solid acid catalysts Historical overviews of solid acid catalystsFuture outlookSolid Acids CatalysisDefinition of acid and base -Brnsted acid and Lewis acid-Acid sites on surfacesAcid strengthRole of acid sites in catalysisBifunctional catalysisPore size effect on catalysis -shape selectivity-Characterization of Solid Acid Catalysts Indicator methodTemperature programmed desorption (TPD) of ammoniaCalorimetry of adsorption of basic moleculesInfrare

Development of silver/titanium dioxide/chitosan adipate nanocomposite as an antibacterial coating for fruit storage

Science.gov (United States)

A novel nanocomposite of silver/titanium dioxide/chitosan adipate (Ag/TiO2/CS) was developed through photochemical reduction using a chitosan adipate template. Chitosan served as a reducing agent for the metal ions, and anchored metal ions by forming Ag–N coordination bonds and electrostatic attract...

Evolution of insoluble eutectic Si particles in anodic oxidation films during adipic-sulfuric acid anodizing processes of ZL114A aluminum alloys

Science.gov (United States)

Hua, Lei; Liu, Jian-hua; Li, Song-mei; Yu, Mei; Wang, Lei; Cui, Yong-xin

2015-03-01

The effects of insoluble eutectic Si particles on the growth of anodic oxide films on ZL114A aluminum alloy substrates were investigated by optical microscopy (OM) and scanning electron microscopy (SEM). The anodic oxidation was performed at 25°C and a constant voltage of 15 V in a solution containing 50 g/L sulfuric acid and 10 g/L adipic acid. The thickness of the formed anodic oxidation film was approximately 7.13 μm. The interpore distance and the diameters of the major pores in the porous layer of the film were within the approximate ranges of 10-20 nm and 5-10 nm, respectively. Insoluble eutectic Si particles strongly influenced the morphology of the anodic oxidation films. The anodic oxidation films exhibited minimal defects and a uniform thickness on the ZL114A substrates; in contrast, when the front of the oxide oxidation films encountered eutectic Si particles, defects such as pits and non-uniform thickness were observed, and pits were observed in the films.

New Glucopyranosylglyceryl-N-Octenyl Adipate and Bioactivity of ...

African Journals Online (AJOL)

1-(3-β-D-Glucopyranosylglycer-2-yl)-6-N-(oct-2-enyl)-adipate, [orientalin, 1] was isolated as a new metabolite from the polar leaf extracts of Toussaintia orientalis Verdc (Annonaceae), together with the glycoflavonoids afzelin and quercitrin, and the indolidinoids toussaintines A-C. The reversed chalcones 2-hydroxy-3,4 ...

Multifunctional nanobiocomposite of Poly[(butylene succinate)-co-adipate] and clay

CSIR Research Space (South Africa)

Al-Thabaiti, SA

2015-03-01

Full Text Available The processing and characterization of multifunctional nanobiocomposite of biodegradable poly[(butylene succinate)-co-adipate] (PBSA) and organically modified synthetic fluorine mica (OSFM) are reported. The nanobiocomposite of PBSA with OSFM...

Carbon-based strong solid acid for cornstarch hydrolysis

Energy Technology Data Exchange (ETDEWEB)

Nata, Iryanti Fatyasari, E-mail: yanti_tkunlam@yahoo.com [Chemical Engineering Study Program, Faculty of Engineering, Lambung Mangkurat University, Jl. A. Yani Km. 36 Banjarbaru, South Kalimantan 70714 (Indonesia); Irawan, Chairul; Mardina, Primata [Chemical Engineering Study Program, Faculty of Engineering, Lambung Mangkurat University, Jl. A. Yani Km. 36 Banjarbaru, South Kalimantan 70714 (Indonesia); Lee, Cheng-Kang, E-mail: cklee@mail.ntust.edu.tw [Department of Chemical Engineering, National Taiwan University of Science and Technology, 43 Keelung Rd. Sec.4, Taipei 106, Taiwan (China)

2015-10-15

Highly sulfonated carbonaceous spheres with diameter of 100–500 nm can be generated by hydrothermal carbonization of glucose in the presence of hydroxyethylsulfonic acid and acrylic acid at 180 °C for 4 h. The acidity of the prepared carbonaceous sphere C4-SO{sub 3}H can reach 2.10 mmol/g. It was used as a solid acid catalyst for the hydrolysis of cornstarch. Total reducing sugar (TRS) concentration of 19.91 mg/mL could be obtained by hydrolyzing 20 mg/mL cornstarch at 150 °C for 6 h using C4-SO{sub 3}H as solid acid catalyst. The solid acid catalyst demonstrated good stability that only 9% decrease in TRS concentration was observed after five repeat uses. The as-prepared carbon-based solid acid catalyst can be an environmentally benign replacement for homogeneous catalyst. - Highlights: • Carbon solid acid was successfully prepared by one-step hydrothermal carbonization. • The acrylic acid as monomer was effectively reduce the diameter size of particle. • The solid acid catalyst show good catalytic performance of starch hydrolysis. • The solid acid catalyst is not significantly deteriorated after repeated use.

Carbon-based strong solid acid for cornstarch hydrolysis

International Nuclear Information System (INIS)

Nata, Iryanti Fatyasari; Irawan, Chairul; Mardina, Primata; Lee, Cheng-Kang

2015-01-01

Highly sulfonated carbonaceous spheres with diameter of 100–500 nm can be generated by hydrothermal carbonization of glucose in the presence of hydroxyethylsulfonic acid and acrylic acid at 180 °C for 4 h. The acidity of the prepared carbonaceous sphere C4-SO 3 H can reach 2.10 mmol/g. It was used as a solid acid catalyst for the hydrolysis of cornstarch. Total reducing sugar (TRS) concentration of 19.91 mg/mL could be obtained by hydrolyzing 20 mg/mL cornstarch at 150 °C for 6 h using C4-SO 3 H as solid acid catalyst. The solid acid catalyst demonstrated good stability that only 9% decrease in TRS concentration was observed after five repeat uses. The as-prepared carbon-based solid acid catalyst can be an environmentally benign replacement for homogeneous catalyst. - Highlights: • Carbon solid acid was successfully prepared by one-step hydrothermal carbonization. • The acrylic acid as monomer was effectively reduce the diameter size of particle. • The solid acid catalyst show good catalytic performance of starch hydrolysis. • The solid acid catalyst is not significantly deteriorated after repeated use

Processing and rheological characterization of poly(butylene adipate co-terephalate)/montmorillonite nanocomposites

International Nuclear Information System (INIS)

Beatrice, Cesar A.G.; Marini, Juliano; Bretas, Rosario E.S.; Branciforti, Marcia C.; Favaro, Marcia M.

2009-01-01

The rheological steady state and the linear viscoelastic properties of poly(butylene adipate co-terephthalate) (PBAT) / nanoclay nanocomposites were investigated. For this study, nanocomposites of PBAT and a chemically modified montmorillonite (MMT) were prepared by melt blending in a Haake Rheomix 600p rheometer at 140 and 160 deg C. The concentration of nanoclay was 5wt%. The samples obtained were characterized by x-ray diffraction (WAXS) and rheological measurements in an ARES (Rheometric Scientific) and AR-G2 (TA) rheometers, both with parallel plates geometry. It was confirmed by WAXS that the platelets of the nanoclay were intercalated in all samples, as the discernible sharp reflection of the (001) clay's diffraction was found in the x-ray diffractions patterns. The storage moduli (G') and the loss moduli (G ) of the nanocomposites increased with nanoclay content, at low frequencies. The presence of nanoclay caused these nanocomposites melts to have solid-like behaviors, which can be explained in terms of the development of a percolated network structure. (author)

Carbon-based strong solid acid for cornstarch hydrolysis

Science.gov (United States)

Nata, Iryanti Fatyasari; Irawan, Chairul; Mardina, Primata; Lee, Cheng-Kang

2015-10-01

Highly sulfonated carbonaceous spheres with diameter of 100-500 nm can be generated by hydrothermal carbonization of glucose in the presence of hydroxyethylsulfonic acid and acrylic acid at 180 °C for 4 h. The acidity of the prepared carbonaceous sphere C4-SO3H can reach 2.10 mmol/g. It was used as a solid acid catalyst for the hydrolysis of cornstarch. Total reducing sugar (TRS) concentration of 19.91 mg/mL could be obtained by hydrolyzing 20 mg/mL cornstarch at 150 °C for 6 h using C4-SO3H as solid acid catalyst. The solid acid catalyst demonstrated good stability that only 9% decrease in TRS concentration was observed after five repeat uses. The as-prepared carbon-based solid acid catalyst can be an environmentally benign replacement for homogeneous catalyst.

Influence of the adipate and dissolved oxygen concentrations on the beta-lactam production during continuous cultivations of a Penicillium chrysogenum strain expressing the expandase gene from Streptomyces clavuligerus

DEFF Research Database (Denmark)

Robin, Jarno Jacky Christian; Bonneau, S.; Schipper, D.

2003-01-01

The influence of adipate concentration and dissolved oxygen on production of adipoyl-7-aminodeacetoxycephalosporanic acid (ad-7-ADCA) by a recombinant strain of Penicillium chrysogenum expressing the expandase gene from Streptomyces clavuligerus was studied in glucose-limited continuous cultures....... from 15 to 7%AS, r(p) (total) increased to 25 mumol g DW-1 h(-1), mainly due to a two-fold increase in the adipoyl-6-aminopenicillanic acid (ad-6-APA) specific productivity....

Fatty acids polymorphism and solid-state miscibility

Energy Technology Data Exchange (ETDEWEB)

Gbabode, Gabin [Centre de Physique Moleculaire Optique et Hertzienne, Universite Bordeaux I, 33405 Talence (France)], E-mail: ggbabode@ulb.ac.be; Negrier, Philippe; Mondieig, Denise [Centre de Physique Moleculaire Optique et Hertzienne, Universite Bordeaux I, 33405 Talence (France); Moreno, Evelyn; Calvet, Teresa; Cuevas-Diarte, Miquel Angel [Departament de Cristallografia, Mineralogia i Diposits Minerals, Universitat de Barcelona, 08028 Barcelona (Spain)

2009-02-05

The pentadecanoic acid-hexadecanoic acid (C{sub 15}H{sub 29}OOH-C{sub 16}H{sub 31}OOH) binary system is dealt with in this article. The polymorphism of 20 mixed materials has been investigated combining calorimetric measurements, isothermal and versus temperature X-ray powder diffraction and also FTIR spectroscopy. In particular, the cell parameters of the stable forms, temperatures and heats of phase changes for the two constituents and a proposal of phase diagram are given in this article. Three solid forms are created by mixing in addition with the four solid forms of the pure components. All these solid forms are stabilized on narrow domains of composition, implying a reduced solid-state miscibility of the pentadecanoic and hexadecanoic acids.

Self-aligned nanocrystalline ZnO hexagons by facile solid-state and co-precipitation route

International Nuclear Information System (INIS)

Thorat, J. H.; Kanade, K. G.; Nikam, L. K.; Chaudhari, P. D.; Panmand, R. P.; Kale, B. B.

2012-01-01

In this study, we report the synthesis of well-aligned nanocrystalline hexagonal zinc oxide (ZnO) nanoparticles by facile solid-state and co-precipitation method. The co-precipitation reactions were performed using aqueous and ethylene glycol (EG) medium using zinc acetate and adipic acid to obtain zinc adipate and further decomposition at 450 °C to confer nanocrystalline ZnO hexagons. XRD shows the hexagonal wurtzite structure of the ZnO. Thermal study reveals complete formation of ZnO at 430 °C in case of solid-state method, whereas in case of co-precipitation method complete formation was observed at 400 °C. Field emission scanning electron microscope shows spherical morphology for ZnO synthesized by solid-state method. The aqueous-mediated ZnO by co-precipitation method shows rod-like morphology. These rods are formed via self assembling of spherical nanoparticles, however, uniformly dispersed spherical crystallites were seen in EG-mediated ZnO. Transmission electron microscope (TEM) investigations clearly show well aligned and highly crystalline transparent and thin hexagonal ZnO. The particle size was measured using TEM and was observed to be 50–60 nm in case of solid-state method and aqueous-mediated co-precipitation method, while 25–50 nm in case of EG-mediated co-precipitation method. UV absorption spectra showed sharp absorption peaks with a blue shift for EG-mediated ZnO, which demonstrate the mono-dispersed lower particle size. The band gap of the ZnO was observed to be 3.4 eV which is higher than the bulk, implies nanocrystalline nature of the ZnO. The photoluminescence studies clearly indicate the strong violet and weak blue emission in ZnO nanoparticles which is quite unique. The process investigated may be useful to synthesize other oxide semiconductors and transition metal oxides.

Self-aligned nanocrystalline ZnO hexagons by facile solid-state and co-precipitation route

Energy Technology Data Exchange (ETDEWEB)

Thorat, J. H. [Mahatma Phule College, Department of Chemistry (India); Kanade, K. G. [Annasaheb Awate College (India); Nikam, L. K. [B.G. College (India); Chaudhari, P. D.; Panmand, R. P.; Kale, B. B., E-mail: kbbb1@yahoo.com [Center for Materials for Electronics Technology (C-MET) (India)

2012-02-15

In this study, we report the synthesis of well-aligned nanocrystalline hexagonal zinc oxide (ZnO) nanoparticles by facile solid-state and co-precipitation method. The co-precipitation reactions were performed using aqueous and ethylene glycol (EG) medium using zinc acetate and adipic acid to obtain zinc adipate and further decomposition at 450 Degree-Sign C to confer nanocrystalline ZnO hexagons. XRD shows the hexagonal wurtzite structure of the ZnO. Thermal study reveals complete formation of ZnO at 430 Degree-Sign C in case of solid-state method, whereas in case of co-precipitation method complete formation was observed at 400 Degree-Sign C. Field emission scanning electron microscope shows spherical morphology for ZnO synthesized by solid-state method. The aqueous-mediated ZnO by co-precipitation method shows rod-like morphology. These rods are formed via self assembling of spherical nanoparticles, however, uniformly dispersed spherical crystallites were seen in EG-mediated ZnO. Transmission electron microscope (TEM) investigations clearly show well aligned and highly crystalline transparent and thin hexagonal ZnO. The particle size was measured using TEM and was observed to be 50-60 nm in case of solid-state method and aqueous-mediated co-precipitation method, while 25-50 nm in case of EG-mediated co-precipitation method. UV absorption spectra showed sharp absorption peaks with a blue shift for EG-mediated ZnO, which demonstrate the mono-dispersed lower particle size. The band gap of the ZnO was observed to be 3.4 eV which is higher than the bulk, implies nanocrystalline nature of the ZnO. The photoluminescence studies clearly indicate the strong violet and weak blue emission in ZnO nanoparticles which is quite unique. The process investigated may be useful to synthesize other oxide semiconductors and transition metal oxides.

Biodegradation of poly(lactic acid, poly(hydroxybutyrate-co-hydroxyvalerate, poly(butylene succinate and poly(butylene adipate-co-terephthalate under anaerobic and oxygen limited thermophilic conditions

Directory of Open Access Journals (Sweden)

Jutakan Boonmee

2016-01-01

Full Text Available In order to study the biodegradation behavior of biodegradable plastics in landfill conditions, four types of biodegradable plastics including poly(lactic acid (PLA, poly(hydroxybutyrate-co-hydroxyvalerate (PHBV, poly(butylene succinate (PBS, and poly(butylene adipate-co-terephthalate (PBAT were tested by burying in sludge mixed soil medium under anaerobic and oxygen limited conditions. The experiments were operated at 52 ± 2ºC in dark conditions according to ISO15985. The degree of biodegradation after 75 days was investigated by weight loss determination, visual examination, and surface appearance by scanning electronic microscopy (SEM. Under both anaerobic and oxygen limited conditions, the complete degradation (100% weight loss was found only in PHBV after 75 days. The plastic degradations were ranked in the order of PHBV> PLA> PBS> PBAT. The percentage of weight losses were significantly different at p ≤ 0.05. However, for all studied plastics, the degradation under anaerobic and oxygen limited conditions did not significantly different at 95% confidence.

In vitro Dissolution Studies on Solid Dispersions of Mefenamic Acid.

Science.gov (United States)

Rao, K R S Sambasiva; Nagabhushanam, M V; Chowdary, K P R

2011-03-01

Solid dispersions of mefanamic acid with a water-soluble polymer polyvinyl pyrrolidine and a super disintegrant, primojel were prepared by common solvent and solvent evaporation methods employing methanol as the solvent. The dissolution rate and dissolution efficiency of the prepared solid dispersions were evaluated in comparison to the corresponding pure drug. Solid dispersions of mefenamic acid showed a marked enhancement in dissolution rate and dissolution efficiency. At 1:4 ratio of mefenamic acid-primojel a 2.61 fold increase in the dissolution rate of mefenamic acid was observed with solid dispersion. The solid dispersions in combined carriers gave much higher rates of dissolution than super disintegrants alone. Mefanamic acid-primojel-polyvinyl pyrrolidine (1:3.2:0.8) solid dispersion gave a 4.11 fold increase in the dissolution rate of mefenamic acid. Super disintegrants alone or in combination with polyvinyl pyrrolidine could be used to enhance the dissolution rate of mefenamic acid.

Dehydration of alcohols using solid acid catalysts

OpenAIRE

Cholerton, Mary

2014-01-01

Solid acid catalysts were prepared through silicon substitution into aluminophosphate frameworks. Silicon incorporation was confirmed using solid state nuclear magnetic resonance spectroscopy. The nature of the acid sites generated was determined using Fourier Transform infrared spectroscopy. These materials were tested as catalysts for the dehydration of ethanol to ethylene at low operating temperatures. The materials were active for dehydration of ethanol to ethylene with significant differ...

Formulation of itraconazole nanococrystals and evaluation of their bioavailability in dogs.

Science.gov (United States)

De Smet, Lieselotte; Saerens, Lien; De Beer, Thomas; Carleer, Robert; Adriaensens, Peter; Van Bocxlaer, Jan; Vervaet, Chris; Remon, Jean Paul

2014-05-01

The aim of the study is to increase the bioavailability of itraconazole (ITRA) using nanosized cocrystals prepared via wet milling of ITRA in combination with dicarboxylic acids. Wet milling was used in order to create a nanosuspension of ITRA in combination with dicarboxylic acids. After spray-drying and bead layering, solid state was characterized by MDSC, XRD, Raman and FT-IR. The release profiles and bioavailability of the nanococrystalline suspension, the spray-dried and bead layered formulation were evaluated. A monodisperse nanosuspension (549±51nm) of ITRA was developed using adipic acid and Tween®80. Solid state characterization indicated the formation of nanococrystals by hydrogen bounds between the triazole group of ITRA and the carboxyl group of adipic acid. A bioavailability study was performed in dogs. The faster drug release from the nanocrystal-based formulation was reflected in the in vivo results since Tmax of the formulations was obtained 3h after administration, while Tmax of the reference formulation was observed only 6h after administration. This fast release of ITRA was obtained by a dual concept: manufacturing of nanosized cocrystals of ITRA and adipic acid via wet milling. Formation of stable nanosized cocrystals via this approach seems a good alternative for amorphous systems to increase the solubility and obtain a fast drug release of BCS class II drugs. Copyright © 2013 Elsevier B.V. All rights reserved.

Radiation-induced reactions of amino acids adsorbed on solid surfaces

Energy Technology Data Exchange (ETDEWEB)

Lopez-Esquivel Kranksith, L.; Negron-Mendoza, A. [Instituto de Ciencias Nucleares, Universidad Nacional Autonoma de Mexico, UNAM. Cd. Universitaria, A.P. 70-543, 04510 Mexico D.F. (Mexico); Mosqueira, F.G. [Direcion General de Divulgacion de la Ciencia, Universidad Nacional Autonoma de Mexico, Cd. Universitaria, AP. 70-487 Mexico D.F. (Mexico); Ramos-Bernal, Sergio, E-mail: ramos@nucleares.unam.m [Instituto de Ciencias Nucleares, Universidad Nacional Autonoma de Mexico, UNAM. Cd. Universitaria, A.P. 70-543, 04510 Mexico D.F. (Mexico)

2010-07-21

The purpose of this work is to study the adsorption of compounds such as amino acids on clays and carbon nanotubes (CNTs) as a possible phase in the chemical evolution that may have occurred on the primitive Earth or in extraterrestrial environments. We further study the behavior of amino acids adsorbed on these solid surfaces at different conditions of pH and levels of irradiation, simulating a high-radiation field at early Earth conditions. The relevance of this work is to explain the possible contribution of solids (clays and CNTs) as promoters of polymerization and as shields for the adsorbed organic compounds against external sources of energy. To this end, tryptophan, aspartic acid, and glutamic acid were adsorbed on fixed amounts of solid surfaces and were irradiated by a {sup 60}Co source for different periods of time at fixed dose rates. After irradiation, the amino acids were extracted from the solid and analyzed with UV and IR spectroscopes and high-performance liquid chromatography. The most efficient surface for adsorption of amino acids was clay, followed by CNTs. Studies of the gamma irradiation of amino acids adsorbed on clay (in the solid phase) show a low yield of recovery of the amino acid.

Processing and characterization of solid and microcellular PHBV/PBAT blend and its RWF/nanoclay composites

Science.gov (United States)

Alireza Javadi; Yottha Srithep; Jungjoo Lee; Srikanth Pilla; Craig Clemons; Shaoqin Gong; Lih-Sheng Turng

2010-01-01

Solid and microcellular components made of poly (3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV)/ poly (butylenes adipate-co-terephthalate) (PBAT) blend (weight ration of PHBV:PBAT = 30:70), recycled wood fiber (RWF), and nanoclay (NC) were prepared via a conventional and microcellular-injection molding process, respectively. Morphology, thermal properties, and...

Determination of organic acids evolution during apple cider fermentation using an improved HPLC analysis method

NARCIS (Netherlands)

Zhang, H.; Zhou, F.; Ji, B.; Nout, M.J.R.; Fang, Q.; Zhang, Z.

2008-01-01

An efficient method for analyzing ten organic acids in food, namely citric, pyruvic, malic, lactic, succinic, formic, acetic, adipic, propionic and butyric acids, using HPLC was developed. Boric acid was added into the mobile phase to separate lactic and succinic acids, and a post-column buffer

Piezoelectric crystal microbalance measurements of enthalpy of sublimation of C2-C9 dicarboxylic acids

Science.gov (United States)

Dirri, F.; Palomba, E.; Longobardo, A.; Zampetti, E.

2016-02-01

We present here a novel experimental set-up that is able to measure the enthalpy of sublimation of a given compound by means of piezoelectric crystal microbalances (PCMs). The PCM sensors have already been used for space measurements, such as for the detection of organic and non-organic volatile species and refractory materials in planetary environments. In Earth atmospherics applications, PCMs can be also used to obtain some physical-chemical processes concerning the volatile organic compounds (VOCs) present in atmospheric environments. The experimental set-up has been developed and tested on dicarboxylic acids. In this work, a temperature-controlled effusion cell was used to sublimate VOC, creating a molecular flux that was collimated onto a cold PCM. The VOC recondensed onto the PCM quartz crystal, allowing the determination of the deposition rate. From the measurements of deposition rates, it has been possible to infer the enthalpy of sublimation of adipic acid, i.e. ΔHsub : 141.6 ± 0.8 kJ mol-1, succinic acid, i.e. 113.3 ± 1.3 kJ mol-1, oxalic acid, i.e. 62.5 ± 3.1 kJ mol-1, and azelaic acid, i.e. 124.2 ± 1.2 kJ mol-1. The results obtained show an accuracy of 1 % for succinic, adipic, and azelaic acid and within 5 % for oxalic acid and are in very good agreement with previous works (within 6 % for adipic, succinic, and oxalic acid and within 11 % or larger for azelaic acid).

Oxalic acid as a heterogeneous ice nucleus in the upper troposphere and its indirect aerosol effect

Directory of Open Access Journals (Sweden)

B. Zobrist

2006-01-01

Full Text Available Heterogeneous ice freezing points of aqueous solutions containing various immersed solid dicarboxylic acids (oxalic, adipic, succinic, phthalic and fumaric have been measured with a differential scanning calorimeter. The results show that only the dihydrate of oxalic acid (OAD acts as a heterogeneous ice nucleus, with an increase in freezing temperature between 2 and 5 K depending on solution composition. In several field campaigns, oxalic acid enriched particles have been detected in the upper troposphere with single particle aerosol mass spectrometry. Simulations with a microphysical box model indicate that the presence of OAD may reduce the ice particle number density in cirrus clouds by up to ~50% when compared to exclusively homogeneous cirrus formation without OAD. Using the ECHAM4 climate model we estimate the global net radiative effect caused by this heterogeneous freezing to result in a cooling as high as −0.3 Wm−2.

FORMULATION AND EVALUATION OF MEFENAMIC ACID SOLID DISPERSIONS USING PEG-4000

OpenAIRE

Shaik Jamal Shariff; Shaik Saleem; Alaparthi Naga Pavan Kumar; Bachupally Ajay Kumar; Punuru Madhusudhan

2013-01-01

Mefenamic acid (MA) solid Dispersions were prepared employing methanol as a common solvent using PEG-4000 as a drug carrier with two different techniques namely, melting method and solvent evaporation in varied ratios. The prepared solid dispersions were evaluated and compared with that of pure drug (mefenamic acid) in respect to the dissolution rate and dissolution efficiency. It is noted that solid dispersions of mefenamic acid showed a remarkable increase in dissolution rate and dissolutio...

Poly(butylene adipate-co-terephthalate) and sunflower head residue composites: Effects of composition and compatibilization on properties

Science.gov (United States)

Utilizing the abundant byproducts generated from processing of agricultural materials has sustainable and cost–saving potential benefits. In this work, Sunflower Head Residues (SHR) in 3 different compositions were introduced into biodegradable Poly(butylene adipate-co-terephthalate) (PBAT) matrices...

Hemicellulose hydrolysis catalysed by solid acids

NARCIS (Netherlands)

Carà, P.D.; Pagliaro, M.; Elmekawy, A.; Brown, D.R.; Verschuren, P.; Shiju, N.R.; Rothenberg, G.

2013-01-01

Depolymerising hemicellulose into platform sugar molecules is a key step in developing the concept of an integrated biorefinery. This reaction is traditionally catalysed by either enzymes or homogeneous mineral acids. We compared various solid catalysts for hemicellulose hydrolysis, running

Rheology of dilute acid hydrolyzed corn stover at high solids concentration.

Science.gov (United States)

Ehrhardt, M R; Monz, T O; Root, T W; Connelly, R K; Scott, C T; Klingenberg, D J

2010-02-01

The rheological properties of acid hydrolyzed corn stover at high solids concentration (20-35 wt.%) were investigated using torque rheometry. These materials are yield stress fluids whose rheological properties can be well represented by the Bingham model. Yield stresses increase with increasing solids concentration and decrease with increasing hydrolysis reaction temperature, acid concentration, and rheometer temperature. Plastic viscosities increase with increasing solids concentration and tend to decrease with increasing reaction temperature and acid concentration. The solids concentration dependence of the yield stress is consistent with that reported for other fibrous systems. The changes in yield stress with reaction conditions are consistent with observed changes in particle size. This study illustrates that torque rheometry can be used effectively to measure rheological properties of concentrated biomass.

Research into esterification of mixture of lower dicarboxylic acids by 2-ethylhexan-1-ol in the presence of p-toluensulfonic acid

OpenAIRE

Melnyk, Stepan; Melnyk, Yuriy; Nykulyshyn, Irena; Shevchuk, Liliya

2017-01-01

Regularities of esterification of the mixture of lower dicarboxylic acids (succinic, glutaric, adipic) by 2-ethylhexan-1-ol in the presence of catalysts – p-toluensulfonic and sulfuric acids under non-stationary conditions were studied. It was found that in the presence of mineral acid, the reaction flows at a lower rate. Application of benzene as a substance that facilitates separation of water, formed in the esterification reaction, makes it possible, due to a lower reaction temperature, to...

Enzymatic Synthesis and Characterization of Hydrophilic Sugar Based Polyesters and Their Modification with Stearic Acid

Directory of Open Access Journals (Sweden)

Muhammad Humayun Bilal

2016-03-01

Full Text Available Biodegradable and hydrophilic functional polyesters were synthesized enzymatically using xylitol or d-sorbitol together with divinyl adipate and lipase B from Candida antartica (CAL-B. The resulting polyesters had pendant OH-groups from their sugar units which were esterified to different degrees with stearic acid chloride. The structure and the degrees of polymerization of the resulting graft copolymers based on poly(xylitol adipate and poly(d-sorbitol adipate were characterized by 1H NMR spectroscopy and SEC. DSC, WAXS and SAXS measurements indicated that a phase separation between polymer backbone and stearoyl side chains occurred in the graft copolymers, and, additionally, the side chains were able to crystallize which resulted in the formation of a lamellar morphology. Additionally, nanoparticles of the graft copolymers in an aqueous environment were studied by DLS and negative stain TEM.

Solid-phase route to Fmoc-protected cationic amino acid building blocks

DEFF Research Database (Denmark)

Clausen, Jacob Dahlqvist; Linderoth, Lars; Nielsen, Hanne Mørck

2012-01-01

Diamino acids are commonly found in bioactive compounds, yet only few are commercially available as building blocks for solid-phase peptide synthesis. In the present work a convenient, inexpensive route to multiple-charged amino acid building blocks with varying degree of hydrophobicity...... was developed. A versatile solid-phase protocol leading to selectively protected amino alcohol intermediates was followed by oxidation to yield the desired di- or polycationic amino acid building blocks in gram-scale amounts. The synthetic sequence comprises loading of (S)-1-(p-nosyl)aziridine-2-methanol onto...... of simple neutral amino acids as well as analogs displaying high bulkiness or polycationic side chains was prepared. Two building blocks were incorporated into peptide sequences using microwave-assisted solid-phase peptide synthesis confirming their general utility....

Novel electrospun nanofibrous matrices prepared from poly(lactic acid)/poly(butylene adipate) blends for controlled release formulations of an anti-rheumatoid agent.

Science.gov (United States)

Siafaka, Panoraia I; Barmbalexis, Panagiotis; Bikiaris, Dimitrios N

2016-06-10

In the present work, a series of novel formulations consisting of poly(lactic acid)/poly(butylene adipate) (PLA/PBAd) electrospun blends was examined as controlled release matrices for Leflunomide's active metabolite, Teriflunomide (TFL). The mixtures were prepared using different ratios of PLA and PBAd in order to produce nanofibrous matrices with different characteristics. Miscibility studies of the blended polymeric fibers were performed through differential scanning calorimetry (DSC) and X-ray diffractometry (XRD). Hydrolytic degradation in the prepared fibers was evaluated at 37°C using a phosphate buffered saline solution. Different concentrations of (TFL) (5, 10, 15wt.%) were incorporated into nanofibers for examining the drug release behavior in simulated body fluids (SBF), at 37°C. The drug-loaded nanofibrous formulations were further characterized by Fourier Transform Infrared Spectroscopy (FTIR) spectroscopy, DSC and XRD. Gel permeation chromatography (GPC) analysis was used to evaluate the mechanism of TFL release. Artificial neural networks (ANN) and multi-linear-regression (MLR) models were used to evaluate the effect of % content of PBAd (X1) and TFL (X2) on an initial burst effect and a dissolution behavior. It was found that PLA/PBAd nanofibers have different diameters depending on the ratio of used polyesters and added drug. TFL was incorporated in an amorphous form inside the polymeric nanofibers. In vitro release studies reveal that a drug release behavior is correlated with the size of the nanofibers, drug loading and matrix degradation after a specific time. ANN dissolution modeling showed increased correlation efficacy compared to MLR. Copyright © 2016 Elsevier B.V. All rights reserved.

Complete doping in solid-state by silica-supported perchloric acid as dopant solid acid: Synthesis and characterization of the novel chiral composite of poly [(±)-2-(sec-butyl) aniline

Energy Technology Data Exchange (ETDEWEB)

Farrokhzadeh, Abdolkarim; Modarresi-Alam, Ali Reza, E-mail: modaresi@chem.usb.ac.ir

2016-05-15

Poly [(±)-2-(sec-butyl) aniline]/silica-supported perchloric acid composites were synthesized by combination of poly[(±)-2-sec-butylaniline] base (PSBA) and the silica-supported perchloric acid (SSPA) as dopant solid acid in solid-state. The X-ray photoelectron spectroscopy (XPS) and CHNS results confirm nigraniline oxidation state and complete doping for composites (about 75%) and non-complete for the PSBA·HCl salt (about 49%). The conductivity of samples was (≈0.07 S/cm) in agreement with the percent of doping obtained of the XPS analysis. Also, contact resistance was determined by circular-TLM measurement. The morphology of samples by the scanning electron microscopy (SEM) and their coating were investigated by XPS, SEM-map and energy-dispersive X-ray spectroscopy (EDX). The key benefits of this work are the preparation of conductive chiral composite with the delocalized polaron structure under green chemistry and solid-state condition, the improvement of the processability by inclusion of the 2-sec-butyl group and the use of dopant solid acid (SSPA) as dopant. - Highlights: • The solid-state synthesis of the novel chiral composites of poly[(±)-2-(sec-butyl)aniline] (PSBA) and silica-supported perchloric acid (SSPA). • It takes 120 h for complete deprotonation of PSBA.HCl salt. • Use of SSPA as dopant solid acid for the first time to attain the complete doping of PSBA. • The coating of silica surface with PSBA.

Environmentally Benign Bifunctional Solid Acid and Base Catalysts

NARCIS (Netherlands)

Elmekawy, A.; Shiju, N.R.; Rothenberg, G.; Brown, D.R.

2014-01-01

Solid bifunctional acid-​base catalysts were prepd. in two ways on an amorphous silica support: (1) by grafting mercaptopropyl units (followed by oxidn. to propylsulfonic acid) and aminopropyl groups to the silica surface (NH2-​SiO2-​SO3H)​, and (2) by grafting only aminopropyl groups and then

Morphology and mechanical properties of poly(butylene adipate-co-terephthalate)/potato starch blends in the presence of synthesized reactive compatibilizer or modified poly(butylene adipate-co-terephthalate).

Science.gov (United States)

Wei, Dafu; Wang, Hao; Xiao, Huining; Zheng, Anna; Yang, Yang

2015-06-05

The biodegradable poly(butylene adipate-co-terephthalate)(PBAT)/thermoplastic starch (TPS) composite has received considerable attention because of the environmental concerns raised by solid waste disposal. However, the application of PBAT/TPS blends was limited due to the poor mechanical properties originating from the incompatibility between PBAT and TPS. In this work, two approaches were developed to improve the mechanical properties of PBAT/TPS blends. One approach is to use compatibilizers, including the synthesized reactive compatibilizer - a styrene-maleic anhydride-glycidyl methacrylate (SMG) terpolymer, and the commercial compatibilizer (Joncryl-ADR-4368). The chemical structures of SMG were analyzed with (1)H NMR and FT-IR. The other approach is to use the modified PBAT (M-PBAT) to replace part of PBAT in the PBAT/TPS blends. M-PBATs with higher molecular weight were obtained via reactive extrusion of PBAT in the presence of a chain extender. The better dispersion of TPS in PBAT was observed in SEM images when using M-PBAT, leading to the higher tensile strength and elongation at break of PBAT/TPS blends. However, the elongation at break decreased in the presence of compatibilizer (SMG or 4368), though the tensile strength remained in a similar level or slightly higher. Overall, the tensile strength and the elongation at break of the resulting biodegradable PBAT/M-PBAT/TPS blends (TPS=40wt%) were above 27.0MPa and 500%, respectively, which is promising for various applications, including packaging and agricultural mulching films. Copyright © 2015 Elsevier Ltd. All rights reserved.

Polystyrene/TiO2 composite electrospun fibers as fillers for poly(butylene succinate-co-adipate): Structure, morphology and properties

CSIR Research Space (South Africa)

Neppalli, R

2014-01-01

Full Text Available In this work, composite polystyrene/titanium dioxide (PS/TiO(sub2)) electrospun fibers were used as a reinforcement for a poly(butylene succinate-co-adipate) (PBSA) matrix. The structure, morphology, mechanical properties and degradation behavior...

A fast and simple solid phase microextraction coupled with gas chromatography-triple quadrupole mass spectrometry method for the assay of urinary markers of glutaric acidemias.

Science.gov (United States)

Naccarato, Attilio; Gionfriddo, Emanuela; Elliani, Rosangela; Sindona, Giovanni; Tagarelli, Antonio

2014-10-30

The analysis of characteristic urinary acidic markers such as glutaric, 3-hydroxyglutaric, 2-hydroxyglutaric, adipic, suberic, sebacic, ethylmalonic, 3-hydroxyisovaleric and isobutyric acid constitutes the recommended follow-up testing procedure for glutaric acidemia type 1 (GA-1) and type 2 (GA-2). The goal of the work herein presented is the development of a fast and simple method for the quantification of these biomarkers in human urine. The proposed analytical approach is based on the use of solid phase microextraction (SPME) combined with gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS) afterward a rapid derivatization of acidic moieties by propyl chloroformate, propanol and pyridine. Trueness and precision of the proposed protocol, tested at 5, 30 and 80mgl -1 , provided satisfactory values: recoveries were in the range between 72% and 116% and the relative standard deviations (RSD%) were between 0.9% and 18% (except for isobutyric acid at 5mgl -1 ). The LOD values achieved by the proposed method ranged between 1.0 and 473μgl -1 . Copyright © 2014 Elsevier B.V. All rights reserved.

Biodegradação de alcoóis, ftalatos e adipatos em um solo tropical contaminado Biodegradation of alcohol, phthalates and adipates in a tropical soil

Directory of Open Access Journals (Sweden)

Ieda Domingues Ferreira

2010-01-01

Full Text Available The adipic and phthalic acid esters are plasticizers, have low water solubility, high partition octanol/water coefficients (Kow and accumulate in soil and sediments. These compounds are considered teratogenic, carcinogenic and endocrine disruptors chemicals. This study evaluated the bioremediation of tropical soil contaminated with plasticizers process wastes, in aerobic conditions, with and without introduction of acclimated bacteria. It was selected 200 kg of contaminated tropical soil for the biodegradation study. The plasticizers concentrations in soil ranged between 153 mgDOA/kg up to 15552 mgDIDP/kg and after 90 days of biodegradation, the lower removal efficiencies were 72% with a 1-2 log simultaneous bacterial growth.

SOLID AND LIQUID PINEAPPLE WASTE UTILIZATION FOR LACTIC ACID FERMENTATION USING Lactobacillus delbrueckii

Directory of Open Access Journals (Sweden)

Abdullah Abdullah

2012-01-01

Full Text Available The liquid and solid  pineapple wastes contain mainly sucrose, glucose, fructose and other nutrients. It therefore can potentially be used as carbon source for fermentation to produce organic acid. Recently, lactic acid has been considered to be an important raw material for production of biodegradable lactate polymer. The experiments were  carried out in batch fermentation using  the  liquid and solid pineapple wastes to produce lactic acid. The anaerobic fermentation of lactic acid were performed at 40 oC, pH 6, 5% inocolum and  50 rpm. Initially  results show that the liquid pineapple waste by  using Lactobacillus delbrueckii can be used as carbon source  for lactic acid fermentation. The production of lactic acid  are found to be 79 % yield, while only  56% yield was produced by using solid waste. 

All-solid-state potentiometric sensors for ascorbic acid by using a screen-printed compatible solid contact

International Nuclear Information System (INIS)

Veltsistas, Panayotis G.; Prodromidis, Mamas I.; Efstathiou, Constantinos

2004-01-01

The development of all-solid-state potentiometric ion selective electrodes for monitoring of ascorbic acid, by using a screen-printed compatible solid contact is described. The applied methodology is based on the use of PVC membrane modified with some firstly-tested ionophores (triphenyltin(IV)chloride, triphenyltin(IV)hydroxide and palmitoyl-L-ascorbic acid) and a novel one synthesized in our laboratory (dibutyltin(IV) diascorbate). Synthesis protocol and some preliminary identification studies are given. A conductive graphite-based polymer thick film ink was used as an internal solid contact between the graphite electrode and the PVC membrane. The presence and the nature of the solid contact (plain or doped with lanthanum 2,6-dichlorophenolindophenol (DCPI)) seem to enhance the analytical performance of the electrodes in terms of sensitivity, dynamic range, and response time. The analytical performance of the constructed electrodes was evaluated with potentiometry, constant-current chronopotentiometry and electrochemical impedance spectroscopy (EIS). The interference effect of various compounds was also tested. The potential response of the optimized Ph 3 SnCl-based electrode was linear against ascorbic acid concentration range 0.005-5.0 mM. The applicability of the proposed sensors in real samples was also tested. The detection limit was 0.002 mM ascorbic acid (50 mM phosphate, pH 5 in 50 mM KCl). The slope of the electrodes was super-Nernstian and pH dependent, indicating a mechanism involving a combination of charge transfer and ion exchange processes. Fabrication of screen-printed ascorbate ISEs has also been demonstrated

[*C]octanoic acid breath test to measure gastric emptying rate of solids.

Science.gov (United States)

Maes, B D; Ghoos, Y F; Rutgeerts, P J; Hiele, M I; Geypens, B; Vantrappen, G

1994-12-01

We have developed a breath test to measure solid gastric emptying using a standardized scrambled egg test meal (250 kcal) labeled with [14C]octanoic acid or [13C]octanoic acid. In vitro incubation studies showed that octanoic acid is a reliable marker of the solid phase. The breath test was validated in 36 subjects by simultaneous radioscintigraphic and breath test measurements. Nine healthy volunteers were studied after intravenous administration of 200 mg erythromycin and peroral administration of 30 mg propantheline, respectively. Erythromycin significantly enhanced gastric emptying, while propantheline significantly reduced gastric emptying rates. We conclude that the [*C]octanoic breath test is a promising and reliable test for measuring the gastric emptying rate of solids.

Aqueous Microwave-Assisted Solid-Phase Synthesis Using Boc-Amino Acid Nanoparticles

Directory of Open Access Journals (Sweden)

Yoshinobu Fukumori

2013-07-01

Full Text Available We have previously developed water-based microwave (MW-assisted peptide synthesis using Fmoc-amino acid nanopaticles. It is an organic solvent-free, environmentally friendly method for peptide synthesis. Here we describe water-based MW-assisted solid-phase synthesis using Boc-amino acid nanoparticles. The microwave irradiation allowed rapid solid-phase reaction of nanoparticle reactants on the resin in water. We also demonstrated the syntheses of Leu-enkephalin, Tyr-Gly-Gly-Phe-Leu-OH, and difficult sequence model peptide, Val-Ala-Val-Ala-Gly-OH, using our water-based MW-assisted protocol with Boc-amino acid nanoparticles.

Langzeitevaluation eines psychologischen Trainings für adipöse Kinder und ihre Eltern (TAKE)

OpenAIRE

Roth, Binia; Munsch, Simone; Meyer, Andrea H.

2011-01-01

Verhaltenstherapeutische Eltern-Kind-Programme haben bisher die besten Effekte bei der Behandlung kindlicher Adipositas gezeigt. Mit TAKE (Training adipöser Kinder und ihrer Eltern) stellen wir eine psychologiebasierte Behandlung vor, die nicht nur Bewegung, Ernährung und Essverhalten als Elemente einschließt, sondern auch psychische Faktoren wie Selbstwertgefühl, Körperbild, soziale Kompetenzen und Hänseleien sowohl mit den Eltern als auch mit den Kindern behandelt. Aktuell liegen die Langze...

Langzeitevaluation des psychologischen Trainings für adipöse Kinder und deren Eltern : TAKE

OpenAIRE

Roth, B.; Munsch, S.; Meyer, A. H.

2011-01-01

Cognitive-behavioral parent-child-programmes have shown the best effects in treating childhood obesity so far. With TAKE (Training adipöser Kinder und ihrer Eltern) we introduce a psychologically-informed training, that includes physical activity, nutrition and eating behavior but also addresses psychological issues like self-confidence, body image, social and anti-bullying skills. Long-term data from up to 64 month-follow-up showed moderate effects on body-mass index standard deviation score...

Flexible and strong ternary blends of poly(vinyl chloride), poly(butylene adipate)and nanoparticle-plasticizers

OpenAIRE

Yin, Bo; Hakkarainen, Minna

2013-01-01

Multiple property enhancement was achieved for ternary blends of PVC, poly(butylene adipate) (PBA) plasticizer and PBA-grafted nanofillers as compared to ternary blends with untreated nanofillers. The blends with surface modified halloysite, kaolin or silicon dioxide nanofillers all exhibited higher stress at break and higher strain at break as compared to the corresponding composites with untreated nanoparticles. The strain at break was similar or improved compared to binary PVC/PBA blends. ...

Investigation of solid-phase hydrogenation of amino acids and peptides

International Nuclear Information System (INIS)

Zolotarev, Yu.A.; Myasoedov, N.F.; Zajtsev, D.A.; Lubnin, M.Yu.; Tatur, V.Yu.; Kozik, V.S.; Dorokhova, E.M.; Rozenberg, S.N.

1990-01-01

The possibility of synthesizing amino acids and peptides multiply labelled with tritium or deuterium by the method of solid-phase isotopic exchange with gaseous hydrogen isotopes was verified. Establishment of the isotopic hydrogen equilibrium between the gaseous phase and the solid phase formed by the amino acid molecules was found experimentally. The activation energy of the isotopic exchange is 13 kcal/mol. A mathematical model was set up for the isotopic exchange with a probable substitution of hydrogen atoms. Uniformly labelled amino acids were obtained in a high optical purity and with 80 to 90% hydrogen substitution by deuterium and tritium. Tritiated peptides were prepared in high yields at molar activities of 1.5 to 3.7 TBq/mmol. (author). 4 tabs

Characterizing Corrosion Effects of Weak Organic Acids Using a Modified Bono Test

Science.gov (United States)

Zhou, Yuqin; Turbini, Laura J.; Ramjattan, Deepchand; Christian, Bev; Pritzker, Mark

2013-12-01

To meet environmental requirements and achieve benefits of cost-effective manufacturing, no-clean fluxes (NCFs) or low-solids fluxes have become popular in present electronic manufacturing processes. Weak organic acids (WOAs) as the activation ingredients in NCFs play an important role, especially in the current lead-free and halogen-free soldering technology era. However, no standard or uniform method exists to characterize the corrosion effects of WOAs on actual metallic circuits of printed wiring boards (PWBs). Hence, the development of an effective quantitative test method for evaluating the corrosion effects of WOAs on the PWB's metallic circuits is imperative. In this paper, the modified Bono test, which was developed to quantitatively examine the corrosion properties of flux residues, is used to characterize the corrosion effects of five WOAs (i.e., abietic acid, succinic acid, glutaric acid, adipic acid, and malic acid) on PWB metallic circuits. Experiments were performed under three temperature/humidity conditions (85°C/85% RH, 60°C/93% RH, and 40°C/93% RH) using two WOA solution concentrations. The different corrosion effects among the various WOAs were best reflected in the testing results at 40°C and 60°C. Optical microscopy was used to observe the morphology of the corroded copper tracks, and scanning electron microscopy (SEM) energy-dispersive x-ray (EDX) characterization was performed to determine the dendrite composition.

Enzymatically and reductively degradable α-amino acid-based poly(ester amide)s: Synthesis, cell compatibility, and intracellular anticancer drug delivery

NARCIS (Netherlands)

Sun, H.; Cheng, Ru; Deng, Chao; Meng, Fenghua; Dias, Aylvin A.; Hendriks, Marc; Feijen, Jan; Zhong, Zhiyuan

2015-01-01

A novel and versatile family of enzymatically and reductively degradable α-amino acid-based poly(ester amide)s (SS-PEAs) were developed from solution polycondensation of disulfide-containing di-p-toluenesulfonic acid salts of bis-l-phenylalanine diesters (SS-Phe-2TsOH) with di-p-nitrophenyl adipate

Solid-state actinide acid phosphites from phosphorous acid melts

International Nuclear Information System (INIS)

Oh, George N.; Burns, Peter C.

2014-01-01

The reaction of UO 3 and H 3 PO 3 at 100 °C and subsequent reaction with dimethylformamide (DMF) produces crystals of the compound (NH 2 (CH 3 ) 2 )[UO 2 (HPO 2 OH)(HPO 3 )]. This compound crystallizes in space group P2 1 /n and consists of layers of uranyl pentagonal bipyramids that share equatorial vertices with phosphite units, separated by dimethylammonium. In contrast, the reaction of phosphorous acid and actinide oxides at 210 °C produces a viscous syrup. Subsequent dilution in solvents and use of standard solution-state methods results in the crystallization of two polymorphs of the actinide acid phosphites An(HPO 2 OH) 4 (An=U, Th) and of the mixed acid phosphite–phosphite U(HPO 3 )(HPO 2 OH) 2 (H 2 O)·2(H 2 O). α- and β-An(HPO 2 OH) 4 crystallize in space groups C2/c and P2 1 /n, respectively, and comprise a three-dimensional network of An 4+ cations in square antiprismatic coordination corner-sharing with protonated phosphite units, whereas U(HPO 3 )(HPO 2 OH) 2 (H 2 O) 2 ·(H 2 O) crystallizes in a layered structure in space group Pbca that is composed of An 4+ cations in square antiprismatic coordination corner-sharing with protonated phosphites and water ligands. We discuss our findings in using solid inorganic reagents to produce a solution-workable precursor from which solid-state compounds can be crystallized. - Graphical abstract: Reaction of UO 3 and H 3 PO 3 at 100 °C and subsequent reaction with DMF produces crystals of (NH 2 (CH 3 ) 2 )[UO 2 (HPO 2 OH)(HPO 3 )] with a layered structure. Reaction of phosphorous acid and actinide oxides at 210 °C produces a viscous syrup and further solution-state reactions result in the crystallization of the actinide acid phosphites An(HPO 2 OH) 4 (An=U, Th), with a three-dimensional network structure, and the mixed acid phosphite–phosphite U(HPO 3 )(HPO 2 OH) 2 (H 2 O) 2 ·(H 2 O) with a layered structure. - Highlights: • U(VI), U(IV) and Th(IV) phosphites were synthesized by solution

Metabolic engineering of β-oxidation in Penicillium chrysogenum for improved semi-synthetic cephalosporin biosynthesis.

Science.gov (United States)

Veiga, Tânia; Gombert, Andreas K; Landes, Nils; Verhoeven, Maarten D; Kiel, Jan A K W; Krikken, Arjen M; Nijland, Jeroen G; Touw, Hesselien; Luttik, Marijke A H; van der Toorn, John C; Driessen, Arnold J M; Bovenberg, Roel A L; van den Berg, Marco A; van der Klei, Ida J; Pronk, Jack T; Daran, Jean-Marc

2012-07-01

Industrial production of semi-synthetic cephalosporins by Penicillium chrysogenum requires supplementation of the growth media with the side-chain precursor adipic acid. In glucose-limited chemostat cultures of P. chrysogenum, up to 88% of the consumed adipic acid was not recovered in cephalosporin-related products, but used as an additional carbon and energy source for growth. This low efficiency of side-chain precursor incorporation provides an economic incentive for studying and engineering the metabolism of adipic acid in P. chrysogenum. Chemostat-based transcriptome analysis in the presence and absence of adipic acid confirmed that adipic acid metabolism in this fungus occurs via β-oxidation. A set of 52 adipate-responsive genes included six putative genes for acyl-CoA oxidases and dehydrogenases, enzymes responsible for the first step of β-oxidation. Subcellular localization of the differentially expressed acyl-CoA oxidases and dehydrogenases revealed that the oxidases were exclusively targeted to peroxisomes, while the dehydrogenases were found either in peroxisomes or in mitochondria. Deletion of the genes encoding the peroxisomal acyl-CoA oxidase Pc20g01800 and the mitochondrial acyl-CoA dehydrogenase Pc20g07920 resulted in a 1.6- and 3.7-fold increase in the production of the semi-synthetic cephalosporin intermediate adipoyl-6-APA, respectively. The deletion strains also showed reduced adipate consumption compared to the reference strain, indicating that engineering of the first step of β-oxidation successfully redirected a larger fraction of adipic acid towards cephalosporin biosynthesis. Copyright © 2012 Elsevier Inc. All rights reserved.

Mixing Acid Salts and Layered Double Hydroxides in Nanoscale under Solid Condition.

Science.gov (United States)

Nakayama, Hirokazu; Hayashi, Aki

2014-07-30

The immobilization of potassium sorbate, potassium aspartate and sorbic acid in layered double hydroxide under solid condition was examined. By simply mixing two solids, immobilization of sorbate and aspartate in the interlayer space of nitrate-type layered double hydroxide, so called intercalation reaction, was achieved, and the uptakes, that is, the amount of immobilized salts and the interlayer distances of intercalation compounds were almost the same as those obtained in aqueous solution. However, no intercalation was achieved for sorbic acid. Although intercalation of sorbate and aspartate into chloride-type layered double hydroxide was possible, the uptakes for these intercalation compounds were lower than those obtained using nitrate-type layered double hydroxide. The intercalation under solid condition could be achieved to the same extent as for ion-exchange reaction in aqueous solution, and the reactivity was similar to that observed in aqueous solution. This method will enable the encapsulation of acidic drug in layered double hydroxide as nano level simply by mixing both solids.

Mixing Acid Salts and Layered Double Hydroxides in Nanoscale under Solid Condition

Directory of Open Access Journals (Sweden)

Hirokazu Nakayama

2014-07-01

Full Text Available The immobilization of potassium sorbate, potassium aspartate and sorbic acid in layered double hydroxide under solid condition was examined. By simply mixing two solids, immobilization of sorbate and aspartate in the interlayer space of nitrate-type layered double hydroxide, so called intercalation reaction, was achieved, and the uptakes, that is, the amount of immobilized salts and the interlayer distances of intercalation compounds were almost the same as those obtained in aqueous solution. However, no intercalation was achieved for sorbic acid. Although intercalation of sorbate and aspartate into chloride-type layered double hydroxide was possible, the uptakes for these intercalation compounds were lower than those obtained using nitrate-type layered double hydroxide. The intercalation under solid condition could be achieved to the same extent as for ion-exchange reaction in aqueous solution, and the reactivity was similar to that observed in aqueous solution. This method will enable the encapsulation of acidic drug in layered double hydroxide as nano level simply by mixing both solids.

Effect of nanoclay loading on the thermal and mechanical properties of biodegradable Polylactide/Poly[(butylene succinate)- co-adipate] blend composites

CSIR Research Space (South Africa)

Ojijo, Vincent O

2012-04-01

Full Text Available Polylactide/poly[(butylene succinate)-co-adipate] (PLA/PBSA)-organoclay composites were prepared via melt compounding in a batch mixer. The weight ratio of PLA to PBSA was kept at 70:30, while the weight fraction of the organoclay was varied from 0...

Radium desorption, manganese and iron dissolution from sand filters of a conventional ground water treatment plant under reductive conditions

International Nuclear Information System (INIS)

Al-Hobaib, A.S.; Al-Sulaiman, K.M.; Al-Dhayan, D.M.; Al-Suhybani, A.A.

2006-01-01

Sand filters are used as a filter bed in many ground water treatment plants to remove the physical contaminants and oxidation products. A build-up of radioactivity may take place on the granules, where iron and manganese oxides are deposited and form thin films on the surface of sand filter. The oxides of iron and manganese play an important role in adsorbing radium from ground water. The disposal of those granules makes a significant problem. A batch technique is used for solubilization of radium from sand filters in the presence of some organic acids, which act as reducing agents. These acids are formic acid, acetic acid, benzoic acid, succinic acid, oxalic acid, phthalic acid, and adipic acid. The data were obtained as a function of acidity, temperature, contact time and liquid/solid ratio particle size and shaking speed. It was found that oxalic acid was the best for radium removal. The effectiveness of these acids on radium removal was as follows: oxalic acid > phthalic acid > adipic acid > succinic acid > formic acid > acetic acid. The maximum removal obtained was 69.9% at 1M oxalic acid at 8 ml/g ratio. Reaction kinetics and mechanism parameters of the dissolution process were studied and compared with other published data. (author)

Production of Citric Acid from Solid State Fermentation of Sugarcane ...

African Journals Online (AJOL)

Aspergillus niger is the leading microorganism of choice for citric acid production. Sugarcane waste was used as substrate under solid state fermentation to comparatively evaluate the citric acid production capacity of Aspergillus niger isolates and the indigenous microflora in the sugarcane waste. Known optimal cultural ...

Solid Acid-Catalyzed Cellulose Hydrolysis Monitored by In Situ ATR-IR Spectroscopy

NARCIS (Netherlands)

Zakzeski, J.; Grisel, R.J.H.; Smit, A.T.; Weckhuysen, B.M.

2012-01-01

The solid acid-catalyzed hydrolysis of cellulose was studied under elevated temperatures and autogenous pressures using in situ ATR-IR spectroscopy. Standards of cellulose and pure reaction products, which include glucose, fructose, hydroxymethylfurfural (HMF), levulinic acid (LA), formic acid, and

Solid acid catalysts in heterogeneous n-alkanes hydroisomerisation ...

African Journals Online (AJOL)

As the current global environmental concerns have prompted regulations to reduce the level of aromatic compounds, particularly benzene and its derivatives in gasoline, ydroisomerisation of n-alkanes is becoming a major alternative for enhancing octane number. Series of solid acid catalysts comprising of Freidel crafts, ...

Structural diversity of solid dispersions of acetylsalicylic acid as seen by solid-state NMR

Czech Academy of Sciences Publication Activity Database

Policianová, Olivia; Brus, Jiří; Hrubý, Martin; Urbanová, Martina; Zhigunov, Alexander; Kredatusová, Jana; Kobera, Libor

2014-01-01

Roč. 11, č. 2 (2014), s. 516-530 ISSN 1543-8384 R&D Projects: GA ČR GPP106/11/P426 Institutional support: RVO:61389013 Keywords : solid dispersions * acetylsalicylic acid * polymers Subject RIV: FR - Pharmacology ; Medidal Chemistry Impact factor: 4.384, year: 2014

Phase diagrams in blends of poly(3-hydroxybutyric acid with various aliphatic polyesters

Directory of Open Access Journals (Sweden)

2011-07-01

Full Text Available Phase behavior with immiscibility, miscibility, crystalline morphology, and kinetic analysis in blends of poly(3-hydroxybutyric acid (PHB with aliphatic polyesters such as poly(butylene adipate (PBA, poly(ethylene adipate (PEA, poly(trimethylene adipate (PTA, or poly(ethylene succinate (PESu, respectively, were explored mainly using differential scanning calorimeter (DSC and polarized-light optical microscopy (POM. Immiscibility phase behavior with reversible upper-critical-solution-temperature (UCST is common in the PHB/polyester blends. The polyester/polyester blend of PHB/PTA is partially miscible with no UCST in melt and amorphous glassy states within a composition range of PTA less than 50 wt%. The miscible crystalline/crystalline blend exhibits ring-banded spherulites at Tc = 50~100°C, with inter-ring spacing dependent on Tc. All immiscible or partially miscible PHB/polyester blends, by contrast, exhibit disrupted ringbanded spherulites or discrete spherical phase domains upon cooling from UCST to crystallization. The blends of PHB with all other aliphatic polyesters, such as PESu, PEA, PBA, etc. are only partially miscible or immiscible with an upper critical solution temperature (UCST at 180~221°C depending on blend composition. UCST with reversibility was verified.

Studies on radiolysis of amino acids, 1

International Nuclear Information System (INIS)

Oku, Tadatake

1977-01-01

In order to elucidate the radiolysis of amino acid, peptide, protein and enzyme, the radiolytic mechanisms of neutral amino acids (glycine, L-alanine, L-valine, L-leucine, L-isoleucine, L-serine, and L-threonine) and acidic amino acids (L-aspartic acid, L-glutamic acid and DL-amino-n-adipic acid) were studied in the presence of air or in the atmosphere nitrogen. An aqueous solution of 1 mM. of each amino acid was sealed in a glass ampoule under air or nitrogen. Irradiation of amino acid solutions was carried out with γ-rays of 60 Co at doses of 4.4-2,640x10 3 rads. The amino acids and the radiolytic products formed were determined by ion-exchange chromatography. From the results of determining amino acids and the radiolytic products formed and their G-values, the radiolytic mechanisms of the amino acids were discussed. (auth.)

76 FR 64010 - Special Rules Governing Certain Information Obtained Under the Clean Air Act: Technical Correction

Science.gov (United States)

2011-10-17

... Indian Country. Adipic Acid Production 325199 Adipic acid manufacturing facilities. Aluminum Production 331312 Primary Aluminum production facilities. Ammonia Manufacturing 325311 Anhydrous and aqueous ammonia manufacturing facilities. Cement Production 327310 Portland Cement manufacturing plants. Electronics...

A triclinic polymorph of hexanedioic acid

Directory of Open Access Journals (Sweden)

2009-03-01

Full Text Available Hexanedioic acid (or adipic acid, C6H10O4, crystallizes with two crystallographically independent half-molecules in the asymmetric unit of the triclinic unit cell, space group Poverline{1}, as each molecule lies across a crystallographic inversion centre. A monoclinic polymorph has been reported previously, most recently by Ranganathan, Kulkarni & Rao [J. Phys. Chem. A, (2003, 107, 6073–6081]. The molecules adopt the expected zigzag structure and are linked via centrosymmetric pairs of O—H...O hydrogen bonds, forming infinite one-dimensional chains along [011]. These chains are stacked along the a axis. The crystal is further stabilized by weak C—H...O interactions.

Processing and characterization of recycled poly(ethylene terephthalate) blends with chain extenders, thermoplastic elastomer, and/or poly(butylene adipate-co-terephthalate)

Science.gov (United States)

Yottha Srithep; Alireza Javadi; Srikanth Pilla; Lih-Sheng Turng; Shaoqin Gong; Craig Clemons; Jun Peng

2011-01-01

Poly(ethylene terephthalate) (PET) resin is one of the most widely used thermoplastics, especially in packaging. Because thermal and hydrolytic degradations, recycled PET (RPET) exhibits poor mechanical properties and lacks moldability. The effects of adding elastomeric modifiers, chain extenders (CE), and poly(butylenes adipate-co-terephthalate), PBAT, as a toughener...

Ionic liquids as surfactants for layered double hydroxide fillers: effect on the final properties of poly(butylene adipate-co-terephthalate)

Czech Academy of Sciences Publication Activity Database

Livi, S.; Lins, L. C.; Peter, Jakub; Beneš, Hynek; Kredatusová, Jana; Donato, R. K.; Pruvost, S.

2017-01-01

Roč. 7, č. 10 (2017), s. 1-16, č. článku 297. ISSN 2079-4991 R&D Projects: GA ČR(CZ) GA17-08273S Institutional support: RVO:61389013 Keywords : ionic liquids * poly(butylene adipate-co-terephthalate) * layered double hydroxide Subject RIV: CD - Macromolecular Chemistry OBOR OECD: Polymer science Impact factor: 3.553, year: 2016

INVESTIGATION OF THE PHARMACO-TECHNOLOGICAL PROPERTIES OF SOLID DISPERSIONS OF THIOCTIC ACID, OBTAINED BY MICRONIZATION

Directory of Open Access Journals (Sweden)

Kovalevska, I. V.

2018-04-01

Full Text Available Introduction. Thioctic acid is used in the treatment of diseases that are characterized by lack of mitochondrial activity, which is responsible for the formation of free radicals. Widespread use of thioctic acid is due to the chemical structure. The thioctic acid exhibits biological activity in both hydrophilic and hydrophobic environments. Thioctic acid is an enzyme cofactor and a powerful antioxidant, it regulates the transcription of numerous genes, participates in regulation of glucose and lipid metabolism, increases insulin sensitivity, and forms complexes with heavy metals. Thioctic acid has a high pharmacological potential, which is confirmed by the evidence base of clinical trials. An analysis of the literature on the oral use of thioctic acid indicates that solid dosage forms can be used for long-term therapy. This route of administration is limited by factors such as reduced solubility in acidic environments and enzymatic degradation. For this reason, the search for various compositions of auxiliary substances and methods of obtaining drugs is an urgent task of pharmaceutical technology. Material & methods. Objects of study were solid dispersions of thioctic acid (SDTA on the basis of cellulose derivatives: microcrystalline (MCC, HPMC (hydroxypropyl methylcellulose and polyvinylpyrrolidone (PVP as compared to thioctic acid (TA. The samples were made by solid phase method using micronization in a laboratory shredder at a ratio of 1: 1. Pharmacological and technological parameters were determined according to generally accepted methods. Results & discussion. In appearance the resulting mixtures had lemon color, without inclusions and the formation of conglomerates, with homogeneous sized particles According to the pharmaco-technological studies, the samples do not have a satisfactory flowability. The values of the Carr index and the ratio of Hausner make it possible to conclude that there is a large force of cohesion between the

40 CFR 52.222 - Negative declarations.

Science.gov (United States)

2010-07-01

..., Utility Boilers, Cement Manufacturing Plants, Glass Manufacturing Plants, and Iron and Steel Manufacturing... Pollution Control District. (i) Nitric and Adipic Acid Manufacturing Plants, Cement Manufacturing Plants... Adipic Acid Manufacturing Plants, Utility Boilers, Cement Manufacturing Plants, Glass Manufacturing...

Biowaiver Monographs for Immediate-Release Solid Oral Dosage Forms: Folic Acid.

Science.gov (United States)

Hofsäss, Martin A; Souza, Jacqueline de; Silva-Barcellos, Neila M; Bellavinha, Karime R; Abrahamsson, Bertil; Cristofoletti, Rodrigo; Groot, D W; Parr, Alan; Langguth, Peter; Polli, James E; Shah, Vinod P; Tajiri, Tomokazu; Mehta, Mehul U; Dressman, Jennifer B

2017-12-01

This work presents a review of literature and experimental data relevant to the possibility of waiving pharmacokinetic bioequivalence studies in human volunteers for approval of immediate-release solid oral pharmaceutical forms containing folic acid as the single active pharmaceutical ingredient. For dosage forms containing 5 mg folic acid, the highest dose strength on the World Health Organization Essential Medicines List, the dose/solubility ratio calculated from solubility studies was higher than 250 mL, corresponding to a classification as "not highly soluble." Small, physiological doses of folic acid (≤320 μg) seem to be absorbed completely via active transport, but permeability data for higher doses of 1-5 mg are inconclusive. Following a conservative approach, folic acid is classified as a Biopharmaceutics Classification System class IV compound until more reliable data become available. Commensurate with its solubility characteristics, the results of dissolution studies indicated that none of the folic acid products evaluated showed rapid dissolution in media at pH 1.2 or 4.5. Therefore, according to the current criteria of the Biopharmaceutics Classification System, the biowaiver approval procedure cannot be recommended for immediate-release solid oral dosage forms containing folic acid. Copyright © 2017 American Pharmacists Association®. All rights reserved.

Solid-state NMR studies of nucleic acid components

Czech Academy of Sciences Publication Activity Database

Dračínský, Martin; Hodgkinson, P.

2015-01-01

Roč. 5, č. 16 (2015), s. 12300-12310 ISSN 2046-2069 R&D Projects: GA ČR GA13-24880S Institutional support: RVO:61388963 Keywords : NMR spectroscopy * nucleic acid s * solid-state NMR Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.289, year: 2015 http://pubs.rsc.org/en/content/articlepdf/2015/ra/c4ra14404j

Consequences of acid strength for isomerization and elimination catalysis on solid acids.

Science.gov (United States)

Macht, Josef; Carr, Robert T; Iglesia, Enrique

2009-05-13

We address here the manner in which acid catalysis senses the strength of solid acids. Acid strengths for Keggin polyoxometalate (POM) clusters and zeolites, chosen because of their accurately known structures, are described rigorously by their deprotonation energies (DPE). Mechanistic interpretations of the measured dynamics of alkane isomerization and alkanol dehydration are used to obtain rate and equilibrium constants and energies for intermediates and transition states and to relate them to acid strength. n-Hexane isomerization rates were limited by isomerization of alkoxide intermediates on bifunctional metal-acid mixtures designed to maintain alkane-alkene equilibrium. Isomerization rate constants were normalized by the number of accessible protons, measured by titration with 2,6-di-tert-butylpyridine during catalysis. Equilibrium constants for alkoxides formed by protonation of n-hexene increased slightly with deprotonation energies (DPE), while isomerization rate constants decreased and activation barriers increased with increasing DPE, as also shown for alkanol dehydration reactions. These trends are consistent with thermochemical analyses of the transition states involved in isomerization and elimination steps. For all reactions, barriers increased by less than the concomitant increase in DPE upon changes in composition, because electrostatic stabilization of ion-pairs at the relevant transition states becomes more effective for weaker acids, as a result of their higher charge density at the anionic conjugate base. Alkoxide isomerization barriers were more sensitive to DPE than for elimination from H-bonded alkanols, the step that limits 2-butanol and 1-butanol dehydration rates; the latter two reactions showed similar DPE sensitivities, despite significant differences in their rates and activation barriers, indicating that slower reactions are not necessarily more sensitive to acid strength, but instead reflect the involvement of more unstable organic

Sulfuric acid functional zirconium (or aluminum) incorporated mesoporous MCM-48 solid acid catalysts for alkylation of phenol with tert-butyl alcohol

International Nuclear Information System (INIS)

Jiang, Tingshun; Cheng, Jinlian; Liu, Wangping; Fu, Lie; Zhou, Xuping; Zhao, Qian; Yin, Hengbo

2014-01-01

Several zirconium (or aluminum) incorporated mesoporous MCM-48 solid acid catalysts (SO 4 2− /Zr-MCM-48 and SO 4 2− /Al-MCM-48) were prepared by the impregnation method and their physicochemical properties were characterized by means of XRD, FT-IR, TEM, NH 3 -TPD and N 2 physical adsorption. Also, the catalytic activities of these solid acid catalysts were evaluated by the alkylation of phenol with tert-butyl alcohol. The effect of weight hour space velocity (WHSV), reaction time and reaction temperature on catalytic properties was also studied. The results show that the SO 4 2− /Zr-MCM-48 and SO 4 2− /Al-MCM-48 still have good mesoporous structure and long range ordering. Compared with the Zr (or Al)–MCM-48 samples, SO 4 2− /Zr-MCM-48 and SO 4 2− /Al-MCM-48 solid acid catalysts have strong acidity and exhibit high activities in alkylation reaction of phenol with tert-butyl alcohol. The SO 4 2− /Zr-MCM-48-25 (molar ratio of Si/Zr=0.04) catalyst was found to be the most promising and gave the highest phenol conversion among all catalysts. A maximum phenol conversion of 91.6% with 4-tert-butyl phenol (4-TBP) selectivity of 81.8% was achieved when the molar ratio of tert-butyl alcohol:phenol is 2:1, reaction time is 2 h, the WHSV is 2 h −1 and the reaction temperature is 140 °C. - Highlights: • Sulfuric acid functional mesoporous solid acid catalysts were prepared via impregnation method. • The alkylation of phenol with tert-butyl alcohol was carried out over these solid acid catalysts. • The catalytic activity of SO 4 2− /Zr-MCM-48-25 catalyst is much higher than that of the others. • A maximum phenol conversion of 91.6% was achieved under optimum reaction conditions for SO 4 2− /Zr-MCM-48-25

Investigation of heterogeneous solid acid catalyst performance on low grade feedstocks for biodiesel production: A review

International Nuclear Information System (INIS)

Mansir, Nasar; Taufiq-Yap, Yun Hin; Rashid, Umer; Lokman, Ibrahim M.

2017-01-01

Highlights: • Solid acid catalysts are proficient to esterifying high free fatty acid feedstocks to biodiesel. • Heterogeneous catalysts have the advantage of easy separation and reusability. • Heterogeneous basic catalysts have limitations due to high FFA of low cost feedstocks. • Solid catalysts having acid and base sites reveal better catalyst for biodiesel production. - Abstract: The conventional fossil fuel reserves are continually declining worldwide and therefore posing greater challenges to the future of the energy sources. Biofuel alternatives were found promising to replace the diminishing fossil fuels. However, conversion of edible vegetable oils to biodiesel using homogeneous acids and base catalysts is now considered as indefensible for the future particularly due to food versus fuel competition and other environmental problems related to catalyst system and feedstock. This review has discussed the progression in research and growth related to heterogeneous catalysts used for biodiesel production for low grade feedstocks. The heterogeneous base catalysts have revealed effective way to produce biodiesel, but it has the limitation of being sensitive to high free fatty acid (FFA) or low grade feedstocks. Alternatively, solid acid catalysts are capable of converting the low grade feedstocks to biodiesel in the presence of active acid sites. The paper presents a comprehensive review towards the investigation of solid acid catalyst performance on low grade feedstock, their category, properties, advantages, limitations and possible remedy to their drawbacks for biodiesel production.

By-products from the biodiesel chain as a substrate to citric acid production by solid-state fermentation.

Science.gov (United States)

Schneider, Manuella; Zimmer, Gabriela F; Cremonese, Ezequiel B; de C de S Schneider, Rosana; Corbellini, Valeriano A

2014-07-01

In this study, we propose the use of tung cake for the production of organic acids, with an emphasis on citric acid by solid-state fermentation. We evaluated the conditions of production and the by-products from the biodiesel chain as raw materials involved in this bioprocess. First, we standardized the conditions of solid-state fermentation in tung cake with and without residual fat and with different concentrations of glycerine using the fungus Aspergillus niger The solid-state fermentation process was monitored for 7 days considering the biomass growth and pH level. Citric acid production was determined by high-performance liquid chromatography. Fungal development was better in the crude tung cake, consisting of 20% glycerine. The highest citric acid yield was 350 g kg(-1) of biomass. Therefore, the solid-state fermentation of the tung cake with glycerine led to citric acid production using the Aspergillus niger fungus. © The Author(s) 2014.

Effect of ammonia on the volatility of organic diacids.

Science.gov (United States)

Paciga, Andrea L; Riipinen, Ilona; Pandis, Spyros N

2014-12-02

The effect of ammonia on the partitioning of two dicarboxylic acids, oxalic (C2) and adipic (C6) is determined. Measurements by a tandem differential mobility analysis system and a thermodenuder (TD-TDMA) system are used to estimate the saturation vapor pressure and enthalpy of vaporization of ammonium oxalate and adipate. Ammonia dramatically lowered the vapor pressure of oxalic acid, by several orders of magnitude, with an estimated vapor pressure of 1.7 ± 0.8 × 10(–6) Pa at 298 K. The vapor pressure of ammonium adipate was 2.5 ± 0.8 × 10(–5) Pa at 298 K, similar to that of adipic acid. These results suggest that the dominance of oxalate in diacid concentrations measured in ambient aerosol could be attributed to the salt formation with ammonia.

Structural diversity of solid dispersions of acetylsalicylic acid as seen by solid-state NMR.

Science.gov (United States)

Policianova, Olivia; Brus, Jiri; Hruby, Martin; Urbanova, Martina; Zhigunov, Alexander; Kredatusova, Jana; Kobera, Libor

2014-02-03

Solid dispersions of active pharmaceutical ingredients are of increasing interest due to their versatile use. In the present study polyvinylpyrrolidone (PVP), poly[N-(2-hydroxypropyl)-metacrylamide] (pHPMA), poly(2-ethyl-2-oxazoline) (PEOx), and polyethylene glycol (PEG), each in three Mw, were used to demonstrate structural diversity of solid dispersions. Acetylsalicylic acid (ASA) was used as a model drug. Four distinct types of the solid dispersions of ASA were created using a freeze-drying method: (i) crystalline solid dispersions containing nanocrystalline ASA in a crystalline PEG matrix; (ii) amorphous glass suspensions with large ASA crystallites embedded in amorphous pHPMA; (iii) solid solutions with molecularly dispersed ASA in rigid amorphous PVP; and (iv) nanoheterogeneous solid solutions/suspensions containing nanosized ASA clusters dispersed in a semiflexible matrix of PEOx. The obtained structural data confirmed that the type of solid dispersion can be primarily controlled by the chemical constitutions of the applied polymers, while the molecular weight of the polymers had no detectable impact. The molecular structure of the prepared dispersions was characterized using solid-state NMR, wide-angle X-ray scattering (WAXS), and differential scanning calorimetry (DSC). By applying various (1)H-(13)C and (1)H-(1)H correlation experiments combined with T1((1)H) and T1ρ((1)H) relaxation data, the extent of the molecular mixing was determined over a wide range of distances, from intimate intermolecular contacts (0.1-0.5 nm) up to the phase-separated nanodomains reaching ca. 500 nm. Hydrogen-bond interactions between ASA and polymers were probed by the analysis of (13)C and (15)N CP/MAS NMR spectra combined with the measurements of (1)H-(15)N dipolar profiles. Overall potentialities and limitations of individual experimental techniques were thoroughly evaluated.

Recovery of Terephthalic Acid by employing magnetic nanoparticles as a solid support

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Elmira Ghamary

2018-03-01

Full Text Available Abstract The aim of this research work is focused on the improvement of Terephthalic acid recovery from PET wastes by using organically modified nano-Fe3O4@Cyanuric Chloride as the solid support. The performance of organically modified nano magnetic was examined in detail and the obtained results were compared with the unsupported reaction data. Required reaction time for complete glycolysis of the wastes, consumption of the solvent as well as catalyst decreases up 99%, 37.5% and 40% respectively. Result showed that nano-Fe 3O4@Cyanuric Chloride delivered good performance as solid support in depolymerizing of PET to the terephthalic acid.

Supported zirconium sulfate on carbon nanotubes as water-tolerant solid acid catalyst

International Nuclear Information System (INIS)

Juan, Joon Ching; Jiang Yajie; Meng Xiujuan; Cao Weiliang; Yarmo, Mohd Ambar; Zhang Jingchang

2007-01-01

A new solid acid of zirconium sulfate (CZ) was successfully supported on carbon nanotube (CNT) for esterification reaction. Preparation conditions of the supported CZ have been investigated, to obtain highest catalytic activity for esterification reaction. XRD, TEM, BET, X-ray photoelectron spectra (XPS) and in situ FTIR analysis has also been carried out to understand the characteristics of the catalyst. In the esterification of acrylic acid with n-octanol, the supported CZ exhibited high catalytic activity and stability. The catalytic activity was nearly unchanged during four times of reuse. XRD and TEM analysis indicated that CZ was finely dispersed on CNT. XPS analysis shows that the CZ species was preserved and the chemical environment of the CZ has changed after loaded on CNT. This finding show that CNT as CZ support is an efficient water-tolerant solid acid

Physicochemical pretreatments and hydrolysis of furfural residues via carbon-based sulfonated solid acid.

Science.gov (United States)

Ma, Bao Jun; Sun, Yuan; Lin, Ke Ying; Li, Bing; Liu, Wan Yi

2014-03-01

Potential commercial physicochemical pretreatment methods, NaOH/microwave and NaOH/ultrasound were developed, and the carbon-based sulfonated solid acid catalysts were prepared for furfural residues conversion into reducing sugars. After the two optimum pretreatments, both the content of cellulose increased (74.03%, 72.28%, respectively) and the content of hemicellulose (94.11%, 94.17% of removal rate, respectively) and lignin (91.75%, 92.09% of removal rate, respectively) decreased in furfural residues. The reducing sugar yields of furfural residues with the two physicochemical pretreatments on coal tar-based solid acid reached 33.94% and 33.13%, respectively, higher than that pretreated via NaOH alone (27%) and comparable to that pretreated via NaOH/H2O2 (35.67%). The XRD patterns, IR spectra and SEM images show microwave and ultrasound improve the pretreatment effect. The results demonstrate the carbon-based sulfonated solid acids and the physicochemical pretreatments are green, effective, low-cost for furfural residues conversion. Copyright © 2014 Elsevier Ltd. All rights reserved.

Sulfuric acid functional zirconium (or aluminum) incorporated mesoporous MCM-48 solid acid catalysts for alkylation of phenol with tert-butyl alcohol

Energy Technology Data Exchange (ETDEWEB)

Jiang, Tingshun, E-mail: tshjiang@mail.ujs.edu.cn; Cheng, Jinlian; Liu, Wangping; Fu, Lie; Zhou, Xuping; Zhao, Qian; Yin, Hengbo

2014-10-15

Several zirconium (or aluminum) incorporated mesoporous MCM-48 solid acid catalysts (SO{sub 4}{sup 2−}/Zr-MCM-48 and SO{sub 4}{sup 2−}/Al-MCM-48) were prepared by the impregnation method and their physicochemical properties were characterized by means of XRD, FT-IR, TEM, NH{sub 3}-TPD and N{sub 2} physical adsorption. Also, the catalytic activities of these solid acid catalysts were evaluated by the alkylation of phenol with tert-butyl alcohol. The effect of weight hour space velocity (WHSV), reaction time and reaction temperature on catalytic properties was also studied. The results show that the SO{sub 4}{sup 2−}/Zr-MCM-48 and SO{sub 4}{sup 2−}/Al-MCM-48 still have good mesoporous structure and long range ordering. Compared with the Zr (or Al)–MCM-48 samples, SO{sub 4}{sup 2−}/Zr-MCM-48 and SO{sub 4}{sup 2−}/Al-MCM-48 solid acid catalysts have strong acidity and exhibit high activities in alkylation reaction of phenol with tert-butyl alcohol. The SO{sub 4}{sup 2−}/Zr-MCM-48-25 (molar ratio of Si/Zr=0.04) catalyst was found to be the most promising and gave the highest phenol conversion among all catalysts. A maximum phenol conversion of 91.6% with 4-tert-butyl phenol (4-TBP) selectivity of 81.8% was achieved when the molar ratio of tert-butyl alcohol:phenol is 2:1, reaction time is 2 h, the WHSV is 2 h{sup −1} and the reaction temperature is 140 °C. - Highlights: • Sulfuric acid functional mesoporous solid acid catalysts were prepared via impregnation method. • The alkylation of phenol with tert-butyl alcohol was carried out over these solid acid catalysts. • The catalytic activity of SO{sub 4}{sup 2−}/Zr-MCM-48-25 catalyst is much higher than that of the others. • A maximum phenol conversion of 91.6% was achieved under optimum reaction conditions for SO{sub 4}{sup 2−}/Zr-MCM-48-25.

Synthesis of a nano-crystalline solid acid catalyst from fly ash and its catalytic performance

Energy Technology Data Exchange (ETDEWEB)

Chitralekha Khatri; Ashu Rani [Government P.G. College, Kota (India). Environmental Chemistry Laboratory

2008-10-15

The synthesis of nano-crystalline activated fly ash catalyst (AFAC) with crystallite size of 12 nm was carried out by chemical and thermal treatment of fly ash, a waste material generated from coal-burning power plants. Fly ash was chemically activated using sulfuric acid followed by thermal activation at 600{sup o}C. The variation of surface and physico-chemical properties of the fly ash by activation methods resulted in improved acidity and therefore, catalytic activity for acid catalyzed reactions. The AFAC was characterized by X-ray diffraction, FT-IR spectroscopy, N{sub 2}-adsorption-desorption isotherm, scanning electron microscopy, flame atomic absorption spectrophotometry and sulfur content by CHNS/O elemental analysis. It showed amorphous nature due to high silica content (81%) and possessed high BET surface area (120 m{sup 2}/g). The catalyst was found to be highly active solid acid catalyst for liquid phase esterification of salicylic acid with acetic anhydride and methanol giving acetylsalicylic acid and methyl salicylate respectively. A maximum yield of 97% with high purity of acetylsalicylic acid (aspirin) and a very high conversion 87% of salicylic acid to methyl salicylate (oil of wintergreen) was obtained with AFAC. The surface acidity and therefore, catalytic activity in AFAC was originated by increased silica content, hydroxyl content and higher surface area as compared to fly ash. The study shows that coal generated fly ash can be converted into potential solid acid catalyst for acid catalyzed reactions. Furthermore, this catalyst may replace conventional environmentally hazardous homogeneous liquid acids making an ecofriendly; solvent free, atom efficient, solid acid based catalytic process. 27 refs., 5 figs., 2 tabs.

Preparation and Characterization of a Solid Acid Catalyst from Macro Fungi Residue for Methyl Palmitate Production

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Min Wang

2015-07-01

Full Text Available During the process of fungal polysaccharide extraction for health care products and food factories, a large quantity of macro-fungi residues are produced, but most of the residues are abandoned and become environmental pollutants. A solid acid catalyst, prepared by sulfonating carbonized Phellinus igniarius residue, was shown to be an efficient and environmentally benign catalyst for the esterification of palmitate acid (PA and methanol. As a comparison, two types of common biomass catalysts, wheat straws and wood chips, were prepared. In this study, characterizations, including scanning electron microscopy, thermo-gravimetric analysis, Fourier transform infrared spectrometry, Brunauer-Emmett-Teller assays and elemental analysis, and reaction conditions for the synthesis of methyl palmitate (MP using solid acid catalysts were investigated. Experiments showed that the solid acid catalyst prepared from P. igniarius residue had a higher catalytic activity than the other two catalysts, and the highest yield of MP catalyzed by P. igniarius residue solid acid catalyst was 91.5% under the following optimum conditions: molar ratio of methanol/PA of 10:1, reaction temperature of 60 °C, mass ratio of catalyst/substrate of 2%, and a reaction time of 1.5 h. Thus, the use of this catalyst offers a method for producing MP.

Quantitative characterization of short- and long-chain perfluorinated acids in solid matrices in Shanghai, China.

Science.gov (United States)

Li, Fei; Zhang, Chaojie; Qu, Yan; Chen, Jing; Chen, Ling; Liu, Ying; Zhou, Qi

2010-01-01

Perfluorinated acids (PFAs) have been recognized as emerging environmental pollutants because of their widespread occurrences, persistence, and bioaccumulative and toxicological effects. PFAs have been detected in aquatic environment and biota in China, but the occurrences of these chemicals have not been reported in solid matrices in China. In the present study, short- and long-chain PFAs (C2-C14) have been quantitatively determined in solid matrices including sediments, soils and sludge collected in Shanghai, China. The results indicate that sludge contains more PFAs than sediments and soils, and the total PFAs concentrations in sediments, soil and sludge are 62.5-276 ng g(-1), 141-237 ng g(-1) and 413-755 ng g(-1), respectively. In most cases, trifluoroacetic acid was the major PFA and accounted for 22-90% of the total PFAs. Although the levels of perfluorooctanoate (PFOA) and perfluorooctanesulfonate (PFOS) were not only lower than trifluoroacetic acid, but also lower than some short-chain PFCAs (PFAs, respectively. Meanwhile, unlike previous studies, PFOS levels were not always higher than PFOA in solids collected in Shanghai, China. Given that some short-chain PFAs such as trifluoroacetic acid are mildly phytotoxic and their higher levels in solid matrices were collected in Shanghai, China, these chemicals should be included in future environmental monitoring efforts.

Avaliação citométrica dos adipócitos localizados no tecido subcutâneo da parede anterior do abdome após infiltração percutânea de CO2

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Célia Sampaio Costa

Full Text Available OBJETIVO: Avaliar os efeitos da infiltração de dióxido de carbono em adipócitos presentes na parede abdominal. MÉTODOS: Quinze voluntárias foram submetidas a sessões de infusão de CO2 durante três semanas consecutivas (duas sessões por semana com intervalos de dois a três dias entre cada sessão. O volume de gás carbônico infundido por sessão, em pontos previamente demarcados, foi sempre calculado com base na superfície da área a ser tratada, com volume infundido fixo de 250 mL/100cm² de superfície tratada. Os pontos de infiltração foram demarcados respeitando-se o limite eqüidistante 2cm entre eles. Em cada ponto se injetou 10mL, por sessão, com fluxo de 80mL/min. Foram colhidos fragmentos de tecido celular subcutâneo da parede abdominal anterior antes e após o tratamento. O número e as alterações histomorfológicas dos adipócitos (diâmetro médio, perímetro, comprimento, largura e número de adipócitos por campos de observação foram mensurados por citometria computadorizada. Os resultados foram analisados com o teste t de Student pareado, adotando-se nível de significância de 5% (p<0,05. RESULTADOS: Encontrou-se redução significativa no número de adipócitos da parede abdominal e na área, diâmetro, perímetro, comprimento e largura após o uso da hipercapnia (p=0,0001. CONCLUSÃO: A infiltração percutânea de CO2 reduz a população e modifica a morfologia dos adipócitos presentes na parede abdominal anterior.

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.

Chromium–tungsten–titanium mixed oxides solid catalyst for fatty acid methyl ester synthesis from palm fatty acid distillate

International Nuclear Information System (INIS)

Wan, Zuraida; Hameed, B.H.

2014-01-01

Highlights: • Chromium–tungsten–titanium mixed oxides as solid catalyst. • Catalyst used for esterification of palm fatty acid distillate to methyl esters. • The maximum methyl ester content is 83%. • Catalyst has shown good activity and can be recycled for 4 times. - Abstract: Chromium–tungsten–titanium mixed oxides solid catalysts were prepared and evaluated in the esterification of palm fatty acid distillate (PFAD) to produce fatty acid methyl ester (FAME). Esterification was conducted in a batch reactor at 110–200 °C temperature ranges. The catalysts were characterized by several techniques such as BET, TEM, FTIR, TGA, XRD, EDX and SEM. The treatment conditions during catalyst preparation, effect of reaction parameters, leaching of the active species and the recycled use of the catalyst were investigated. The catalyst with formula CrWTiO 2 was found to be the most active with maximum FAME content of 83% obtained at best reaction conditions of 170 °C for 3 h, 2:1 (methanol to oil molar ratio) and 2 wt.% catalyst dosage. The catalyst can be recycled for 4 times. The results revealed CrWTiO 2 good potentials for use in esterification of high acid value oil

Tunable pH and redox-responsive drug release from curcumin conjugated γ-polyglutamic acid nanoparticles in cancer microenvironment.

Science.gov (United States)

Pillarisetti, Shameer; Maya, S; Sathianarayanan, S; Jayakumar, R

2017-11-01

Tunable pH and redox responsive polymer was prepared using γ-polyglutamic acid (γ-PGA) with linker 3-mercaptopropionic acid (3-MPA) (γ-PGA_SH) via oxidation to obtain redox responsive disulfide (γ-PGA_SS) backbone and adipic acid dihydrazide (ADH) (γ-PGA_SS_ADH) with hydrazide functional group for pH responsiveness. Further curcumin (Cur) was conjugated through hydrazone bond of the γ-PGA_SS_ADH via Schiff base reaction to obtain (γ-PGA_SS_ADH_Cur). The prepared systems were characterized by Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Electrospray ionization quadrupole time-of-flight mass spectrometry (ESI-Qq-TOF-MS/MS) and Solid state nuclear magnetic resonance (SS NMR) techniques. γ-PGA_SS_ADH_Cur formed self-assembled core shell nanoparticles (NPs) in existence of stabilized aqueous medium. γ-PGA_SS_ADH_Cur NPs maintained its stability in physiological condition. NPs tunable Cur release and cytotoxicity were observed for γ-PGA_SS_ADH_Cur NPs in both acidic and redox conditions mimicking the cancer microenvironment. γ-PGA_SS_ADH_Cur NPs uptake study showed via endocytosis mechanism resulted in the lysosomal entrapment of these NPs within the cell. γ-PGA_SS_ADH_Cur NPs exhibited a dual stimuli responsive drug delivery and can be used as a smart and potential drug delivery system in cancer microenvironment. Copyright © 2017 Elsevier B.V. All rights reserved.

Characteristics of immobilized lactobacillus delbrueckii in a liquid-solid fluidized bed bioreactor for lactic acid production

Energy Technology Data Exchange (ETDEWEB)

Wang, Henian; Seki, M.; Furusaki, S. [The Univ. of Tokyo (Japan). Faculty of Engineering

1995-04-20

A fluidized bed bioreactor was employed for lactic acid production using immobilized cells. First, the cell release rate was discussed. A liquid-solid fluidized bed reactor with immobilized cells was used to perform continuous lactic acid fermentation without any operational problems. The performance of the reactor was investigated under different conditions. Cell release rate and contribution of free cells to lactic acid production were studied quantitatively. The results showed that under low gel holdup and low dilution rate conditions, free cells played a significant role in lactic acid production. However, increasing solid holdup decreased the free cell concentration in the broth due to high lactic acid concentration and also decreased the contribution of the free cells to lactic acid production. The effects of growth nutrients on reactor performance were investigated. 16 refs., 12 figs.

Development of starch biofilms using different carboxylic acids as plasticizers

International Nuclear Information System (INIS)

Cruz, L.C.; Miranda, C.S.; Santos, W.J. dos; Goncalves, A.P.B.; Oliveira, J.C.; Jose, N.M.

2014-01-01

Biodegradable films have become a widely exploited issue among scientists because of their positive environmental impact, besides their potential to promote better food conservation and an increase in shelf life. Starch has been studied in this field due to its availability, low cost and biodegradability. However, starch films tend to be brittle and they need addition of a plasticizer to enable their usage. In this work, starch films were synthesized with different carboxylic acids as plasticizers, aiming to observe the effect of the acids chain size in the final films properties. The acids used were: oxalic, succinic and adipic. The materials were produced by casting and characterized by DSC, TG, DRX e FTIR. It was observed that the acids chain size influenced on the thermal and structural properties of the films. (author)

Self-assembly in solvates of 2,4-diamino-6-(4-methyl- phenyl)-1,3,5-triazine and in its molecular adducts with some aliphatic dicarboxylic acids

Science.gov (United States)

Nandy, Purnendu; Nayak, Amrita; Biswas, Sharmita Nandy; Pedireddi, V. R.

2016-03-01

Solid state structures of 2,4-diamino-6-(4-methylphenyl)-1,3,5-triazine, 1, in the form of methanol and dimethylsulfoxide (DMSO) solvates, as well as supramolecular assemblies of 1 with various aliphatic dicarboxylic acids, oxalic (a), malonic (b), succinic (c), glutaric (d) and adipic (e) have been reported. Analysis of the assemblies has been carried out by single crystal X-ray diffraction and thermal methods. Triazine 1 yields anhydrous molecular adducts with acids a-d, upon co-crystallization either from CH3OH and DMSO solvents. However acid e gives anhydrous adduct from DMSO solvent, while it gives a methanol adduct from CH3OH. Structure determination reveals that molecular adducts 1a, 1d and 1e are in a 2:1 ratio of 1 and the corresponding acid. However the ratio is 1:1, in 1b, perhaps due to the involvement of one of the acid groups in the intramolecular hydrogen bonding and in adduct 1c the ratio observed is 3:2. Structural features in all these assemblies have been rationalised in terms of various recognition patterns formed between the acceptor and donor groups. A noteworthy feature is that -COOH groups in acid a establish interaction with 1 through amino groups, while such interactions are observed to be through hetero -N atoms in case of the acids b-e.

Mixing Acid Salts and Layered Double Hydroxides in Nanoscale under Solid Condition

OpenAIRE

Nakayama, Hirokazu; Hayashi, Aki

2014-01-01

The immobilization of potassium sorbate, potassium aspartate and sorbic acid in layered double hydroxide under solid condition was examined. By simply mixing two solids, immobilization of sorbate and aspartate in the interlayer space of nitrate-type layered double hydroxide, so called intercalation reaction, was achieved, and the uptakes, that is, the amount of immobilized salts and the interlayer distances of intercalation compounds were almost the same as those obtained in aqueous solution...

Starch/poly (butylene adipate-co-terephthalate/montmorillonite films produced by blow extrusion

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Rodrigo A. L. Santos

2014-07-01

Full Text Available This study aims to prepare biodegradable films from cassava starch, poly (butylene adipate-co-terephthalate (PBAT, and montmorillonite (MMT using blow-extrusion process and analyze the effects of different types and concentrations of MMT on the microstructure, physicochemical, and mechanical properties of the resulting films. The films were produced by blending 30% of PBAT with glycerol (17.5%, starch (49.0-52.5%, and four different types of montmorillonite (Cloisite® Na+, 10A, 15A, and 30B at two different concentrations (1.75% and 3.5%. All the films prepared in this study showed an increase in the basal spacing of MMT layers. In particular, the films with 10A and 30B showed the highest increase in intercalation basal spacing, suggesting the formation of intercalated composites. The addition of nanoclays decreased the elongation of films. The addition of Cloisite® 10A resulted in films with the lowest WVP values and the highest stability to water adsorption under different RH conditions.

Simultaneous Saccharification and Fermentation of Lactic Acid from Empty Fruit Bunch at High Solids Loading

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Nursia Hassan

2016-03-01

Full Text Available The production of value-added chemicals from the bioconversion of lignocellulose biomass has been considered a promising venture. In this study, microwave, alkali-pretreated empty fruit bunch (EFB was used as the substrate, utilizing pelletized filamentous Rhizopus oryzae NRRL 395 and cellulolytic enzymes for lactic acid production in a fed-batch simultaneous saccharification and fermentation (SSF process. Insoluble solids generally do not affect the SSF process until a certain concentration is exceeded. To achieve a high lactic acid concentration in the broth, a high solids loading was required to allow a higher rate of glucose conversion. However, the results revealed a decrease in the final lactic acid yield when running SSF at a massive insoluble solids level. High osmotic pressure in the medium led to poor cellular performance and caused the Rhizopus oryzae pellets to break down, affecting the lactic acid production. To improve the process performance, a fed-batch operation mode was used. The fed-batch operation was shown to facilitate higher lactic acid yield, compared with the SSF batch mode. Enzyme feeding, as well as substrate feeding, was also investigated as a means of enabling a higher dry matter content, with a high glucose conversion in SSF of cellulose-rich EFB.

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.

Micromachined Dense Palladium Electrodes for Thin-film Solid Acid Fuel Cells

NARCIS (Netherlands)

Unnikrishnan, S.

2009-01-01

This thesis paves the way towards the microfabrication of a solid acid electrolyte based fuel cell (µSAFC), which has a membrane electrode assembly (MEA) consisting of a thin-film of water soluble electrolyte encapsulated between two dense palladium electrode membranes. This project work

Two-stage medium chain fatty acid (MCFA) production from municipal solid waste and ethanol

NARCIS (Netherlands)

Grootscholten, T.I.M.; Strik, D.P.B.T.B.; Steinbusch, K.J.J.; Buisman, C.J.N.; Hamelers, B.

2014-01-01

Chain elongation is an anaerobic fermentation that produces medium chain fatty acids (MCFAs) from volatile fatty acids and ethanol. These MCFAs can be used as biochemical building blocks for fuel production and other chemical processes. Producing MCFAs from the organic fraction of municipal solid

Flow-induced crystallization of a nano composite of poly(butylene adipate-co-terephthalate)/montmorillonite

International Nuclear Information System (INIS)

Bonel, Alan B.; Rego, Bruna T.; Beatrice, Cesar A.G.; Marini, Juliano; Bretas, Rosario E.S.

2011-01-01

Poly(butylene adipate-co-terephthalate) (PBAT) with 5wt% of an organically modified montmorillonite with polar surfactant was prepared by melt blending in a co-rotational twin-screw extruder at 160 degree C. 100rpm and 1 kg/h. Both pure polymer and nano composite were characterized by wide measurements. The study of the flow-induced crystallization was also done by rheological measurements, monitoring the viscosity as a function of time. The nano clay's lamellas were intercalated in the polymer m loss moduli of the nano composite, at low frequencies, showed that the particles of the nano clay were well dispersed and distributed thru the PBAT matrix. Finally, the presence of the nano clay's particles reduced the induction tim crystals growth, due to the strong interactions with the PBAT chains. (author)

Effects of polyurethane matrices on fungal tannase and gallic acid production under solid state culture

Institute of Scientific and Technical Information of China (English)

无

2007-01-01

The influence of the physical structure of polyurethane matrix as a support in a solid state culture in tannase production and gallic acid accumulation by Aspergillus niger Aa-20 was evaluated. Three different polyurethane matrices were used as the support: continuous, semi-discontinuous and discontinuous. The highest tannase production at 2479.59 U/L during the first 12 h of culture was obtained using the discontinuous matrix. The gallic acid was accumulated at 7.64 g/L at the discontinuous matrix. The results show that the discontinuous matrix of polyurethane is better for tannase production and gallic acid accumulation in a solid state culture bioprocess than the continuous and semi-discontinuous matrices.

Solid Silica-based Sulphonic Acid as an Efficient Green Catalyst for ...

African Journals Online (AJOL)

NJD

Solid Silica-based Sulphonic Acid as an Efficient Green. Catalyst for the Selective Oxidation of Sulphides to. Sulphoxides using NaCIO in Aqueous Media. Ali Amoozadeh* and Firouzeh Nemati. Department of Chemistry, Faculty of Science, Semnan University, Semnan, Iran. Received 21 October 2008, revised 6 December ...

Study of Non-Isothermal Crystallization Kinetics of Biodegradable Poly(ethylene adipate/SiO2 Nanocomposites

Directory of Open Access Journals (Sweden)

M. R. Memarzadeh

2013-09-01

Full Text Available Poly(ethylene adipte and poly(ethylene adipate/silica nanocomposite (PEAd/SiO2 containing 3 wt. % SiO2  were prepared by an in situ method. The examinations on the non-isothermal crystallization kinetic behavior have been conducted by means of differential scanning calorimeter (DSC. The Avrami, Ozawa, and combined Avrami and Ozawa equations were applied to describe the crystallization kinetics and to determine the crystallization parameters of the prepared PEAd/SiO2 nanocomposites. It is found that the inclusion of the silica nanoparticles can accelerate the nucleation rate due to heterogeneous nucleation effect of silica on the polymer matrix. According to the obtained results, the combined Avrami and Ozawa equation shown that the better model for examination of this system.

Quantitative characterization of short- and long-chain perfluorinated acids in solid matrices in Shanghai, China

International Nuclear Information System (INIS)

Li, Fei; Zhang, Chaojie; Qu, Yan; Chen, Jing; Chen, Ling; Liu, Ying; Zhou, Qi

2010-01-01

Perfluorinated acids (PFAs) have been recognized as emerging environmental pollutants because of their widespread occurrences, persistence, and bioaccumulative and toxicological effects. PFAs have been detected in aquatic environment and biota in China, but the occurrences of these chemicals have not been reported in solid matrices in China. In the present study, short- and long-chain PFAs (C2-C14) have been quantitatively determined in solid matrices including sediments, soils and sludge collected in Shanghai, China. The results indicate that sludge contains more PFAs than sediments and soils, and the total PFAs concentrations in sediments, soil and sludge are 62.5-276 ng g -1 , 141-237 ng g -1 and 413-755 ng g -1 , respectively. In most cases, trifluoroacetic acid was the major PFA and accounted for 22-90% of the total PFAs. Although the levels of perfluorooctanoate (PFOA) and perfluorooctanesulfonate (PFOS) were not only lower than trifluoroacetic acid, but also lower than some short-chain PFCAs (< C8) in some individual cases, PFOA and PFOS were still the major pollution compounds in most cases and they constituted 2-34% and 1-9% of the total PFAs, respectively. Meanwhile, unlike previous studies, PFOS levels were not always higher than PFOA in solids collected in Shanghai, China. Given that some short-chain PFAs such as trifluoroacetic acid are mildly phytotoxic and their higher levels in solid matrices were collected in Shanghai, China, these chemicals should be included in future environmental monitoring efforts.

Anaerobic Fermentation for Production of Carboxylic Acids as Bulk Chemicals from Renewable Biomass.

Science.gov (United States)

Wang, Jufang; Lin, Meng; Xu, Mengmeng; Yang, Shang-Tian

Biomass represents an abundant carbon-neutral renewable resource which can be converted to bulk chemicals to replace petrochemicals. Carboxylic acids have wide applications in the chemical, food, and pharmaceutical industries. This chapter provides an overview of recent advances and challenges in the industrial production of various types of carboxylic acids, including short-chain fatty acids (acetic, propionic, butyric), hydroxy acids (lactic, 3-hydroxypropionic), dicarboxylic acids (succinic, malic, fumaric, itaconic, adipic, muconic, glucaric), and others (acrylic, citric, gluconic, pyruvic) by anaerobic fermentation. For economic production of these carboxylic acids as bulk chemicals, the fermentation process must have a sufficiently high product titer, productivity and yield, and low impurity acid byproducts to compete with their petrochemical counterparts. System metabolic engineering offers the tools needed to develop novel strains that can meet these process requirements for converting biomass feedstock to the desirable product.

Solid phase extraction of uranium from phosphoric acid. Kinetic and thermodynamic study

Energy Technology Data Exchange (ETDEWEB)

Abdel-Magied, Ahmed Fawzy [Nuclear Materials Authority, Cairo (Egypt); Stockholm Univ. (Sweden). Dept. of Organic Chemistry

2017-07-01

There is a high interest to develop suitable solid phase extractants for uranium separation from aqueous solutions in order to reduce cost and enhance the efficiency. This paper describes solid phase extraction of uranium(VI) from aqueous phosphoric acid solution using MCM-41 based D2HEPA-TOPO organophosphorous extractants. The mixture of D2HEPA (di-2-ethyl-hexylphosphoric acid) and TOPO (tri-n-octylphosphine oxide) was impregnated into the pores of MCM-41 and the synthesized sorbent was fully characterized. The influences of different factors such as synergistic mixture ratio, phosphoric acid concentration, mixing time and temperature were investigated. The results showed that 90% of uranium(VI) extraction can be achieved within 5 min, using D2HEPA-TOPO rate at MCM-41 (mass ratio 2:1 w/w) from 1 M phosphoric acid containing 64 ppm of uranium at room temperature. High adsorption capacity of uranium(VI) have been achieved at the mentioned conditions. The rate constant for the chemical adsorption of uranium(VI) was 0.988 g mg{sup -1} min{sup -1} calculated by the pseudo-second order rate equation. The obtained thermodynamics parameters showed that uranium(VI) adsorption from H{sub 3}PO{sub 4} is an exothermic and spontaneous process.

Consumption of a solid fat rich in lauric acid results in a more favorable serum lipid profile in healthy men and women than consumption of a solid fat rich in trans-fatty acids

NARCIS (Netherlands)

Roos, de N.M.; Schouten, E.G.; Katan, M.B.

2001-01-01

Solid fats are used in food manufacturing to provide texture and firmness to foods. Such fats are rich in either saturated or trans-fatty acids, both of which increase the risk of coronary heart disease. Epidemiological and experimental studies suggest that trans-fatty acids increase risk more than

Investigating tautomeric polymorphism in crystalline anthranilic acid using terahertz spectroscopy and solid-state density functional theory.

Science.gov (United States)

Delaney, Sean P; Witko, Ewelina M; Smith, Tiffany M; Korter, Timothy M

2012-08-02

Terahertz spectroscopy is sensitive to the interactions between molecules in the solid-state and recently has emerged as a new analytical tool for investigating polymorphism. Here, this technique is applied for the first time to the phenomenon of tautomeric polymorphism where the crystal structures of anthranilic acid (2-aminobenzoic acid) have been investigated. Three polymorphs of anthranilic acid (denoted Forms I, II and III) were studied using terahertz spectroscopy and the vibrational modes and relative polymorph stabilities analyzed using solid-state density functional theory calculations augmented with London dispersion force corrections. Form I consists of both neutral and zwitterionic molecules and was found to be the most stable polymorph as compared to Forms II and III (both containing only neutral molecules). The simulations suggest that a balance between steric interactions and electrostatic forces is responsible for the favoring of the mixed neutral/zwitterion solid over the all neutral or all zwitterion crystalline arrangements.

Mesoporous (Ta, Nb3W7 Modified with Stearic Acid Used as Solid Acids for Esterification

Directory of Open Access Journals (Sweden)

Fei Chang

2017-01-01

Full Text Available Mesoporous solid acids Ta3W7 and Nb3W7 were prepared from TaCl5 and NbCl5 with WCl6 in the presence of stearic acid (SA via a sol-gel method, respectively. For comparison, mesoporous Ta3W7-P123 mixed oxides and mesoporous Nb3W7-P123 mixed oxides were synthesized in the same way. The catalysts were characterized through TGA, XRD, SEM, TEM, BET, and NH3-TPD. Experimental results showed that Ta3W7-SA and Nb3W7-SA exhibited several advantages such as higher activity, shorter preparation period, lower cost, stronger acid sites, and higher surface area, which had potential to be used as mesoporous heterogeneous catalysts in biodiesel production.

Biodegradable starch-based films containing saturated fatty acids: thermal, infrared and raman spectroscopic characterization

Directory of Open Access Journals (Sweden)

Marcelo M. Nobrega

Full Text Available Biodegradable films of thermoplastic starch and poly (butylene adipate co-terephthalate (PBAT containing fatty acids were characterized thermally and with infrared and Raman spectroscopies. The symmetrical character of the benzene ring in PBAT provided a means to illustrate the difference between these spectroscopic techniques, because a band appeared in the Raman spectrum but not in the infrared. The thermal analysis showed three degradation stages related to fatty acids, starch and PBAT. The incorporation of saturated fatty acids with different molecular mass (caproic, lauric and stearic did not change the nature of the chemical bonds among the components in the blends of starch, PBAT and glycerol, according to the thermal analysis, infrared and Raman spectroscopies.

Acid functionalized, highly dispersed carbonaceous spheres: an effective solid acid for hydrolysis of polysaccharides

International Nuclear Information System (INIS)

Jiang Yijun; Li Xiutao; Cao Quan; Mu Xindong

2011-01-01

Highly dispersed carbonaceous spheres with sulfonic acid groups were successfully prepared from glucose by hydrothermal method. Transmission electron microscopy (TEM) showed the as-synthesized carbonaceous materials were uniform, spherical in shape with an average diameter of about 450 nm. Fourier transform infrared (FT-IR) proved that –SO 3 H, –COOH, OH groups were grafted on the surface of the carbonaceous spheres during the sulfonation. Interestingly, the functionalized carbonaceous spheres exhibited high dispersibility in the polar solvent due to the hydrophilic groups on the surface. The mechanism of the formation for the carbonaceous spheres was also discussed based on the analysis of structure and composition. At last, the functionalized carbonaceous spheres were employed as solid acid to hydrolyze starch and cellulose. By comparison, the as-synthesized catalyst showed considerable high yield of glucose.

Acid functionalized, highly dispersed carbonaceous spheres: an effective solid acid for hydrolysis of polysaccharides

Science.gov (United States)

Jiang, Yijun; Li, Xiutao; Cao, Quan; Mu, Xindong

2011-02-01

Highly dispersed carbonaceous spheres with sulfonic acid groups were successfully prepared from glucose by hydrothermal method. Transmission electron microscopy (TEM) showed the as-synthesized carbonaceous materials were uniform, spherical in shape with an average diameter of about 450 nm. Fourier transform infrared (FT-IR) proved that -SO3H, -COOH, OH groups were grafted on the surface of the carbonaceous spheres during the sulfonation. Interestingly, the functionalized carbonaceous spheres exhibited high dispersibility in the polar solvent due to the hydrophilic groups on the surface. The mechanism of the formation for the carbonaceous spheres was also discussed based on the analysis of structure and composition. At last, the functionalized carbonaceous spheres were employed as solid acid to hydrolyze starch and cellulose. By comparison, the as-synthesized catalyst showed considerable high yield of glucose.

A route to quantitative ¹³C NMR analysis of multicomponent polyesters

DEFF Research Database (Denmark)

Hvilsted, S.

1991-01-01

A protocol for quantitative sequential 13C NMR analysis is developed for polyesters composed of trimethylol propane (TMP), neopentyl glycol (NPG), and adipic and isophthalic acids. TMP centred, structural models with methyl adipate and isophthalate branches in all possible combinations...

Concentrations of higher dicarboxylic acids C5–C13 in fresh snow samples collected at the High Alpine Research Station Jungfraujoch during CLACE 5 and 6

Directory of Open Access Journals (Sweden)

K. Sieg

2009-03-01

Full Text Available Samples of freshly fallen snow were collected at the high alpine research station Jungfraujoch (Switzerland in February and March 2006 and 2007, during the Cloud and Aerosol Characterization Experiments (CLACE 5 and 6. In this study a new technique has been developed and demonstrated for the measurement of organic acids in fresh snow. The melted snow samples were subjected to solid phase extraction and resulting solutions analysed for organic acids by HPLC-MS-TOF using negative electrospray ionization. A series of linear dicarboxylic acids from C5 to C13 and phthalic acid, were identified and quantified. In several samples the biogenic acid pinonic acid was also observed. In fresh snow the median concentration of the most abundant acid, adipic acid, was 0.69 μg L−1 in 2006 and 0.70 μg L−1 in 2007. Glutaric acid was the second most abundant dicarboxylic acid found with median values of 0.46 μg L−1 in 2006 and 0.61 μg L−1 in 2007, while the aromatic acid phthalic acid showed a median concentration of 0.34 μg L−1 in 2006 and 0.45 μg L−1 in 2007. The concentrations in the samples from various snowfall events varied significantly, and were found to be dependent on the back trajectory of the air mass arriving at Jungfraujoch. Air masses of marine origin showed the lowest concentrations of acids whereas the highest concentrations were measured when the air mass was strongly influenced by boundary layer air.

Graphene oxide for solid-phase extraction of bioactive phenolic acids.

Science.gov (United States)

Hou, Xiudan; Wang, Xusheng; Sun, Yingxin; Wang, Licheng; Guo, Yong

2017-05-01

A solid-phase extraction (SPE) method for the efficient analysis of trace phenolic acids (PAs, caffeic acid, ferulic acid, protocatechuic acid, cinnamic acid) in urine was established. In this work, a graphene oxide (GO) coating was grafted onto pure silica to be investigated as SPE material. The prepared GO surface had a layered and wrinkled structure that was rough and well organized, which could provide more open adsorption sites. Owing to its hydrophilicity and polarity, GO showed higher extraction efficiency toward PAs than reduced GO did, in agreement with the theoretical calculation results performed by Gaussian 09 software. The adsorption mechanism of PAs on GO@Sil was also investigated through static state and kinetic state adsorption experiments, which showed a monolayer surface adsorption. Extraction capacity of the as-prepared material was optimized using the response surface methodology. Under the optimized conditions, the as-established method provided wide linearity range (2-50 μg L -1 for protocatechuic acid and 1-50 μg L -1 for caffeic acid, ferulic acid, and cinnamic acid) and low limits of detection (0.25-1 μg L -1 ). Finally, the established method was applied for the analysis of urine from two healthy volunteers. The results indicate that the prepared material is a practical, cost-effective medium for the extraction and determination of phenolic acids in complex matrices. Graphical Abstract A graphene oxide coating was grafted onto pure silica as the SPE material for the extraction of phenolic acids in urines and the extraction mechanism was also mainly investigated.

Proton-conducting solid acid electrolytes based upon MH(PO3H)

NARCIS (Netherlands)

Zhou, W.

2011-01-01

Solid acids, such as CsHSO4 and CsH2PO4, are a novel class of anhydrous proton-conducting compounds that can be used as electrolyte in H2/O2 and direct methanol fuel cells. The disordering of the hydrogen-bonded network above the so-called superprotonic phase transition results in an increase of the

Highly Selective Liquid-Phase Benzylation of Anisole with Solid-Acid Zeolite Catalysts

DEFF Research Database (Denmark)

Poreddy, Raju; Shunmugavel, Saravanamurugan; Riisager, Anders

2015-01-01

Zeolites were evaluated as solid acid catalysts for the liquid-phase benzylation of anisole with benzyl alcohol, benzyl bromide, and benzyl chloride at 80 °C. Among the examined zeolites, H-mordenite-10 (H-MOR-10) demonstrated particular high activity (>99 %) and excellent selectivity (>96...

Effect of Anorganic Substance on Physical Properties of Poly (Butylene Succinate -co- Adipate) Irradiated by Electron Beam

International Nuclear Information System (INIS)

Meri Suhartini

2004-01-01

Poly(butylene succinate-co-adipate), PBSA were electron beam irradiated in the presence of inorganic materials. The samples gave high gel fraction by irradiation in the presence of 2% silicon dioxide and 2% carbon black. It was found that addition of carbon black (CB) was effective for improving the heat stability of the sample. This is because of three-dimensional carbon black- polymer networks. Irradiated PBSA sheets broke immediately at 110 o C with load 6.67 kgf/cm 2 , while irradiated the same sample mixed with 2% carbon black did not break at the same condition. Biodegradability of crosslinked PBSA by soil burial tests was accelerated by addition of carbon black. (author)

Influence of lactose hydrolysis and solids concentration on alcohol production by yeast in acid whey ultrafiltrate

Energy Technology Data Exchange (ETDEWEB)

O' leary, V S; Sutton, C; Bencivengo, M; Sullivan, B; Holsinger, V H

1977-11-01

Alcohol yields of 6.5 percent were obtained with Saccharomyces cerevisiae in lactase-hydrolyzed acid whey permeate containing 30 to 35 percent total solids. Maximum alcohol yields obtained with Kluyveromyces fragilis were 4.5 percent in lactase-hydrolyzed acid whey permeate at a solids concentration of 20 percent and 3.7 percent in normal permeate at a solids concentration of 10 percent. Saccharomyces cerevisiae efficiently converted the glucose present in lactase-hydrolyzed whey permeates containing 5 to 30 percent total solids (2 to 13 percent glucose) to alcohol. However, the galactose, which comprised about half the available carbohydrate in lactase-hydrolyzed whey, was not utilized by S. cerevisiae, so that even though alcohol yields were higher when this organism was used, the process was wasteful in that a substantial proportion of the substrate was not fermented. For the process to become commercially feasible, an efficient means of rapidly converting both the galactose and glucose to alcohol must be found.

Both solubility and chemical stability of curcumin are enhanced by solid dispersion in cellulose derivative matrices.

Science.gov (United States)

Li, Bin; Konecke, Stephanie; Wegiel, Lindsay A; Taylor, Lynne S; Edgar, Kevin J

2013-10-15

Amorphous solid dispersions (ASD) of curcumin (Cur) in cellulose derivative matrices, hydroxypropylmethylcellulose acetate succinate (HPMCAS), carboxymethylcellulose acetate butyrate (CMCAB), and cellulose acetate adipate propionate (CAAdP) were prepared in order to investigate the structure-property relationship and identify polymer properties necessary to effectively increase Cur aqueous solution concentration. XRD results indicated that all investigated solid dispersions were amorphous, even at a 9:1 Cur:polymer ratio. Both stability against crystallization and Cur solution concentration from these ASDs were significantly higher than those from physical mixtures and crystalline Cur. Remarkably, curcumin was also stabilized against chemical degradation in solution. Chemical stabilization was polymer-dependent, with stabilization in CAAdP>CMCAB>HPMCAS>PVP, while matrices enhanced solution concentration as PVP>HPMCAS>CMCAB≈CAAdP. HPMCAS/Cur dispersions have useful combinations of pH-triggered release profile, chemical stabilization, and strong enhancement of Cur solution concentration. Copyright © 2013 Elsevier Ltd. All rights reserved.

Green synthesis of 3,4-dihydropyrimidinones using nano Fe3O4@meglumine sulfonic acid as a new efficient solid acid catalyst under microwave irradiation

Directory of Open Access Journals (Sweden)

Leila Moradi

2018-01-01

Full Text Available Design, synthesis and characterization of nano Fe3O4@meglumine sulfonic acid as a new solid acid catalyst for the simple and green one pot multicomponent synthesis of 3,4-dihydropyrimidin-2(1H-ones/thiones was studied. New solid acid catalyst was prepared through a clean and simple protocol and characterized using FTIR, VSM, TGA, SEM, elemental analysis (CHN and XRD techniques. Heterogenization of homogeneous catalyst as a green approach is a useful method for enhancing the efficiency of catalyst. Presented study was a new method for attachment of homogeneous highly soluble catalyst (meglumine sulfate to the magnetite nanoparticle surfaces for preparing a heterogeneous and effective catalyst. Obtained heterogeneous and reusable solid acid catalyst has high performance in the synthesis of Biginelli compounds. The reaction was performed under microwave irradiation as a rapid and green condition. Easy work up as well as excellent yield (90–98% of products in short reaction times (40–200 s and reusable catalyst are the main advantages of presented procedure. Reaction products were characterized in details using physical and chemical techniques such as melting point, 1H NMR, 13C NMR and FTIR.

Formation of 1,2-diaminomaleodinitrile crystals in radiolyzed solid hydrocyanic acid

International Nuclear Information System (INIS)

Mozhaev, P.S.; Kichigina, G.A.; Aliev, Z.G.; Kiryukhin, D.P.; Atovmyan, L.O.; Barkalov, I.M.

1994-01-01

Hydrocyanic molecules, HCN, are widely found in various extraterrestrial objects and have come to be regarded as the building blocks of chemical evolution, because they convert directly to more complex organic compounds, such as amino acids, nucleotides, and proteins. While observing the low-temperature conversion of radiolyzed solid HCN, the authors noted the formation of an amorphous polymer and the nucleation and growth of needle shaped crystals. The crystals were studied by X-ray diffraction methods and believed to be formed by 1,2-diaminomaleodinitrile, a tetramer of HCN, arising by recombination of aminocyanocarbene diradicals. Cobalt 60 was used as the radiation source, preirradiating with a 800 kGy dose a solid HCN sample at 77K

Poly(lactic acid) (PLA) Based Tear Resistant and Biodegradable Flexible Films by Blown Film Extrusion

OpenAIRE

Norma Mallegni; Thanh Vu Phuong; Maria-Beatrice Coltelli; Patrizia Cinelli; Andrea Lazzeri

2018-01-01

Poly(lactic acid) (PLA) was melt mixed in a laboratory extruder with poly(butylene adipate-co-terephthalate) (PBAT) and poly(butylene succinate) (PBS) in the presence of polypropylene glycol di glycidyl ether (EJ400) that acted as both plasticizer and compatibilizer. The process was then scaled up in a semi-industrial extruder preparing pellets having different content of a nucleating agent (LAK). All of the formulations could be processed by blowing extrusion and the obtained films showed me...

Consensus report on therapeutic drug monitoring of mycophenolic acid in solid organ transplantation

NARCIS (Netherlands)

D. Kuypers (Dirk); Y. le Meur (Yann); M. Cantarovich (Marcelo); M.J. Tredger (Michael); S.E. Tett (Susan); D. Cattaneo (Dario); B. Tönshoff (Burkhard); D.W. Holt (David); J. Chapman (Jeremy); T. van Gelder (Teun)

2010-01-01

textabstractWith the increasing use of mycophenolic acid (MPA) in solid organ transplantation, the need for more accurate drug dosing has become evident. Personalized immunosuppressive therapy requires better strategies for avoidance of drug-related toxicity while maintaining efficacy. Few studies

Decontamination of materials contaminated with Francisella philomiragia or MS2 bacteriophage using PES-Solid, a solid source of peracetic acid.

Science.gov (United States)

Buhr, T L; Young, A A; Johnson, C A; Minter, Z A; Wells, C M

2014-08-01

The aim of the study was to develop test methods and evaluate survival of Francisella philomiragia cells and MS2 bacteriophage after exposure to PES-Solid (a solid source of peracetic acid) formulations with or without surfactants. Francisella philomiragia cells (≥7·6 log10 CFU) or MS2 bacteriophage (≥6·8 log10 PFU) were deposited on seven different test materials and treated with three different PES-Solid formulations, three different preneutralized samples and filter controls at room temperature for 15 min. There were 0-1·3 log10 CFU (6 log10 CFU/PFU F. philomiragia cells and/or MS2 bacteriophage on different materials. Published 2014. This article is a U.S. Government work and is in the public domain in the USA.

Effects of inherent/enhanced solid acidity and morphology of diatomite templates on the synthesis and porosity of hierarchically porous carbon.

Science.gov (United States)

Liu, Dong; Yuan, Peng; Tan, Daoyong; Liu, Hongmei; Fan, Mingde; Yuan, Aihua; Zhu, Jianxi; He, Hongping

2010-12-21

The inherent or enhanced solid acidity of raw or activated diatomite is found to have significant effects on the synthesis of hierarchically porous diatomite-templated carbon with high surface area and special porous structure. The solid acidity makes raw/activated diatomite a catalyst for the generation of porous carbon, and the porous parameters of the carbon products are strongly dependent on the solid acidity of diatomite templates. The morphology of diatomite also dramatically affects the textural structure of porous carbon. Two types of macroporous structures in the carbon product, the partially solid pillars and the ordered hollow tubes, derive from the replication of the central and the edge pores of diatom shell, respectively. The hierarchically porous carbon shows good capability for the adsorption of solvent naphtha and H(2), enabling potential applications in adsorption and gas storage.

Study of the molecular mobility of methyl-methacrylate and methacrylic acid copolymers by solid state NMR

International Nuclear Information System (INIS)

Tavares, Maria Ines B.; Mansur, Claudia R.E.; Monteiro, Elisabeth E.C.

1997-01-01

Several methyl-methacrylate/methacrylic acid copolymers were prepared in the presence of concentrated nitric acid. The obtained copolymers were characterized by molecular weigh determination and hydrolization degree. The molecular mobility of these copolymers was studied by solid state nuclear magnetic resonance. Results are presented

Preparation of a novel carbon-based solid acid from cassava stillage residue and its use for the esterification of free fatty acids in waste cooking oil.

Science.gov (United States)

Wang, Lingtao; Dong, Xiuqin; Jiang, Haoxi; Li, Guiming; Zhang, Minhua

2014-04-01

A novel carbon-based solid acid catalyst was prepared by the sulfonation of incompletely carbonized cassava stillage residue (CSR) with concentrated sulfuric acid, and employed to catalyze the esterification of methanol and free fatty acids (FFAs) in waste cooking oil (WCO). The effects of the carbonization and the sulfonation temperatures on the pore structure, acid density and catalytic activity of the CSR-derived catalysts were systematically investigated. Low temperature carbonization and high temperature sulfonation can cause the collapse of the carbon framework, while high temperature carbonization is not conducive to the attachment of SO3H groups on the surface. The catalyst showed high catalytic activity for esterification, and the acid value for WCO is reduced to below 2mg KOH/g after reaction. The activity of catalyst can be well maintained after five cycles. CSR can be considered a promising raw material for the production of a new eco-friendly solid acid catalyst. Copyright © 2014 Elsevier Ltd. All rights reserved.

Preparation and physical properties of (PVA0.7(NaBr0.3(H3PO4xM solid acid membrane for phosphoric acid – Fuel cells

Directory of Open Access Journals (Sweden)

F. Ahmad

2013-03-01

Full Text Available A solid acid membranes based on poly (vinyl alcohol (PVA, sodium bromide (NaBr and phosphoric acid (H3PO4 were prepared by a solution casting method. The morphological, IR, electrical and optical properties of the (PVA0.7(NaBr0.3(H3PO4xM solid acid membranes where x = 0.00, 0.85, 1.7, 3.4, 5.1 M were investigated. The variation of film morphology was examined by scanning electron microscopy (SEM studies. FTIR spectroscopy has been used to characterize the structure of polymer and confirms the complexation of phosphoric acid with host polymeric matrix. The temperature dependent nature of ionic conductivity and the impedance of the polymer electrolytes were determined along with the associated activation energy. The ionic conductivity at room temperature was found to be strongly depends on the H3PO4 concentration which it has been achieved to be of the order 4.3 × 10−3 S/cm at ambient temperature. Optical measurements showed a decrease in optical band gap and an increase in band tail width with the increase of phosphoric acid. The data shows that the (PVA0.7(NaBr0.3(H3PO4xM solid acid membrane is promising for intermediate temperature phosphoric acid fuel cell applications.

Modeling of anaerobic degradation of solid slaughterhouse waste: inhibition effects of long-chain fatty acids or ammonia.

Science.gov (United States)

Lokshina, L Y; Vavilin, V A; Salminen, E; Rintala, J

2003-01-01

The anaerobic bioconversion of solid poultry slaughterhouse wastes was kinetically investigated. The modified version of simulation model was applied for description of experimental data in mesophilic laboratory digester and assays. Additionally, stages of formation and consumption of long chain fatty acids (LCFA) were included in the model. Batch data on volatile solids, ammonium, acetate, butyrate, propionate, LCFA concentrations, pH level, cumulative volume, and methane partial pressure were used for model calibration. As a reference, the model was used to describe digestion of solid sorted household waste. Simulation results showed that an inhibition of polymer hydrolysis by volatile fatty acids and acetogenesis by NH3 or LCFA could be responsible for the complex system dynamics during degradation of lipid- and protein-rich wastes.

Dissolution-modulating mechanism of pH modifiers in solid dispersion containing weakly acidic or basic drugs with poor water solubility.

Science.gov (United States)

Tran, Phuong Ha-Lien; Tran, Thao Truong-Dinh; Lee, Kyoung-Ho; Kim, Dong-Jin; Lee, Beom-Jin

2010-05-01

Although the solid dispersion method has been known to increase the dissolution rate of poorly water-soluble drugs by dispersing them in hydrophilic carriers, one obstacle of the solid dispersion method is its limited solubilization capacity, especially for pH-dependent soluble drugs. pH-modified solid dispersion, in which pH modifiers are incorporated, may be a useful method for increasing the dissolution rate of weakly acidic or basic drugs. Sufficient research, including the most recent reports, was undertaken in this review. How could the inclusion of the pH the pH modifiers in the solid dispersion system change drug structural behaviors, molecular interactions, microenvironmental pH, and/or release rate of pH modifiers, relating with the enhanced dissolution of weakly acidic or weakly basic drugs with poor water solubility? These questions have been investigated to determine the dissolution-modulating mechanism of pH modifiers in solid dispersion containing weakly acidic or basic drugs. It is believed that step-by-step mechanistic approaches could provide the ultimate solution for solubilizing several poorly water-soluble drugs with pH-dependent solubility from a solid dispersion system, as well as provide ideas for developing future dosage systems.

Automated solid-phase extraction of phenolic acids using layered double hydroxide-alumina-polymer disks.

Science.gov (United States)

Ghani, Milad; Palomino Cabello, Carlos; Saraji, Mohammad; Manuel Estela, Jose; Cerdà, Víctor; Turnes Palomino, Gemma; Maya, Fernando

2018-01-26

The application of layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks for solid-phase extraction is reported for the first time. Al 2 O 3 is embedded in a polymer matrix followed by an in situ metal-exchange process to obtain a layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disk with excellent flow-through properties. The extraction performance of the prepared disks is evaluated as a proof of concept for the automated extraction using sequential injection analysis of organic acids (p-hydroxybenzoic acid, 3,4-dihydroxybenzoic acid, gallic acid) following an anion-exchange mechanism. After the solid-phase extraction, phenolic acids were quantified by reversed-phase high-performance liquid chromatography with diode-array detection using a core-shell silica-C18 stationary phase and isocratic elution (acetonitrile/0.5% acetic acid in pure water, 5:95, v/v). High sensitivity and reproducibility were obtained with limits of detection in the range of 0.12-0.25 μg/L (sample volume, 4 mL), and relative standard deviations between 2.9 and 3.4% (10 μg/L, n = 6). Enrichment factors of 34-39 were obtained. Layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks had an average lifetime of 50 extractions. Analyte recoveries ranged from 93 to 96% for grape juice and nonalcoholic beer samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sum Frequency Generation Vibrational Spectroscopy of Adsorbed Amino Acids, Peptides and Proteins of Hydrophilic and Hydrophobic Solid-Water Interfaces

Energy Technology Data Exchange (ETDEWEB)

Holinga IV, George Joseph [Univ. of California, Berkeley, CA (United States)

2010-09-01

Sum frequency generation (SFG) vibrational spectroscopy was used to investigate the interfacial properties of several amino acids, peptides, and proteins adsorbed at the hydrophilic polystyrene solid-liquid and the hydrophobic silica solid-liquid interfaces. The influence of experimental geometry on the sensitivity and resolution of the SFG vibrational spectroscopy technique was investigated both theoretically and experimentally. SFG was implemented to investigate the adsorption and organization of eight individual amino acids at model hydrophilic and hydrophobic surfaces under physiological conditions. Biointerface studies were conducted using a combination of SFG and quartz crystal microbalance (QCM) comparing the interfacial structure and concentration of two amino acids and their corresponding homopeptides at two model liquid-solid interfaces as a function of their concentration in aqueous solutions. The influence of temperature, concentration, equilibration time, and electrical bias on the extent of adsorption and interfacial structure of biomolecules were explored at the liquid-solid interface via QCM and SFG. QCM was utilized to quantify the biological activity of heparin functionalized surfaces. A novel optical parametric amplifier was developed and utilized in SFG experiments to investigate the secondary structure of an adsorbed model peptide at the solid-liquid interface.

Decontamination of materials contaminated with Bacillus anthracis and Bacillus thuringiensis Al Hakam spores using PES-Solid, a solid source of peracetic acid.

Science.gov (United States)

Buhr, T L; Wells, C M; Young, A A; Minter, Z A; Johnson, C A; Payne, A N; McPherson, D C

2013-08-01

To develop test methods and evaluate survival of Bacillus anthracis Ames, B. anthracis ∆Sterne and B. thuringiensis Al Hakam spores after exposure to PES-Solid (a solid source of peracetic acid), including PES-Solid formulations with bacteriostatic surfactants. Spores (≥ 7 logs) were dried on seven different test materials and treated with three different PES-Solid formulations (or preneutralized controls) at room temperature for 15 min. There was either no spore survival or less than 1 log (<10 spores) of spore survival in 56 of 63 test combinations (strain, formulation and substrate). Less than 2.7 logs (<180 spores) survived in the remaining seven test combinations. The highest spore survival rates were seen on water-dispersible chemical agent resistant coating (CARC-W) and Naval ship topcoat (NTC). Electron microscopy and Coulter analysis showed that all spore structures were intact after spore inactivation with PES-Solid. Three PES-Solid formulations inactivated Bacillus spores that were dried on seven different materials. A test method was developed to show that PES-Solid formulations effectively inactivate Bacillus spores on different materials. Published 2013. This article is a U.S. Government work and is in the public domain in the USA.

Formation and reactions of free radicals in the radiolysis of organic materials by ion beams

International Nuclear Information System (INIS)

Koizumi, H.

2000-01-01

High-energy heavy ions deposit energy along ion tracks with high density. Chemical effects of the heavy ions may hence differ from that of γ-rays and fast electrons. We can utilize these effects for material modification and fabrication of microstructure. It is necessary to know the dependence of the effects on ion beams and the variation of the effects on materials for developing new application of ion beams. We then studied radical formation in organic solids of alanine and of adipic acid by ion beams irradiation. (author)

Thermal Properties of Polyurethane-Polyisocyanurate Foams Based on Poly(ethylene terephthalate) Waste

OpenAIRE

Irena VITKAUSKIENĖ; Ričardas MAKUŠKA; Uldis STIRNA; Ugis CABULIS

2011-01-01

A series of polyurethane-polyisocyanurate (PU-PIR) foams synthesized from PET-waste-derived aromatic polyester polyols (APP) was studied using thermogravimetric analysis, Cone calorimeter and burning tests. The effect of chemical structure of the APP containing fragments of glycerol, adipic acid, poly(propylene glycol) or hexanediol on thermal stability and flame resistance of the PU-PIR foams was elucidated. PU-PIR foams prepared from APP containing fragments of glycerol and/or adipic acid h...

Starch saccharification by carbon-based solid acid catalyst

Science.gov (United States)

Yamaguchi, Daizo; Hara, Michikazu

2010-06-01

The hydrolysis of cornstarch using a highly active solid acid catalyst, a carbon material bearing SO 3H, COOH and OH groups, was investigated at 353-393 K through an analysis of variance (ANOVA) and an artificial neural network (ANN). ANOVA revealed that reaction temperature and time are significant parameters for the catalytic hydrolysis of starch. The ANN model indicated that the reaction efficiency reaches a maximum at an optimal condition (water, 0.8-1.0 mL; starch, 0.3-0.4 g; catalyst, 0.3 g; reaction temperature, 373 K; reaction time, 3 h). The relationship between the reaction and these parameters is discussed on the basis of the reaction mechanism.

MESOPOROUS ACID SOLID AS A CARRIER FOR METALLOCENE CATALYST IN ETHYLENE POLYMERIZATION AND A CATALYST IN CATALYTIC DEGRADATION OF POLYETHYLENE

Institute of Scientific and Technical Information of China (English)

Wen-xi Cheng; Li-ya Shi; Shi-yun Li; Hui Chen; Tao Tang

2007-01-01

The possibility of mesoporous acid solid as a carrier for metallocene catalyst in ethylene polymerization and catalyst for polyethylene(PE)catalytic degradation was investigated.Here,HMCM-41 and AlMCM-41.and mesoporous silicoaluminophosphate molecular sieves(SAPO1 and SAPO2)were synthesized and used as acid solid.Much more gases were produced during catalytic degradation in PE/acid solid mixtures via in situ polymerization than those via physical mixing.The particle size distribution results exhibited that the particle size of SAPO1 in the PE/SAO1 mixture via in situ polymerization was about 1/14 times of that of the original SAPO1 or SAPO1.supported metallocene catalyst.This work shows a novel technology for chemical recycling of polyolefin.

Production of Biodiesel by Esterification of Free Fatty Acid over Solid Catalyst from Biomass Waste

Science.gov (United States)

Mukti, N. I. F.; Sutrisno, B.; Hidayat, A.

2018-05-01

Recently, low cost feedstocks have been utilized to replace vegetable oils in order to improve the economic feasibility of biodiesel. The esterification of free fatty acid (FFA) on Palm Fatty Acid Distillate (PFAD) with methanol using solid catalyst generated from bagasse fly ash is a promising method to convert FFA into biodiesel. In this research, the esterification of FFA on PFAD using the sulfonated bagasse fly ash catalyst was studied. The performances of the catalysts were evaluated in terms of the reaction temperatures, the molar ratios of methanol to PFAD, and the catalyst loading. The effects of the mass ratio of catalyst to oil (1-10%), the molar ratio of methanol to oil (6:1-12:1), and the reaction temperature (40-60°C) were studied for the conversion of PFAD to optimize the reaction conditions. The results showed that the optimum conditions were methanol to PFAD molar ratio of 12:1, the amount of catalyst of 10%wt. of PFAD, and reaction temperature of 6°C. The reusability of the solid acid carbon catalysts was also studied in this work. The catalytic activity decreased up to 38% after third cycle. The significant decline in catalyst esterification activity was due to acid site leaching. The physico-characteristics and acid site densities were analyzed by Nitrogen gas adsorption, surface functional groups by Fourier transform infrared spectroscopy (FT-IR), elemental analysis using X-ray fluorescent (XRF), and acid-base back titration methods for determination of acid density.

Biodiesel production from acid oils and ethanol using a solid basic resin as catalyst

International Nuclear Information System (INIS)

Marchetti, J.M.; Errazu, A.F.

2010-01-01

In the search of an alternative fuel to substitute diesel fuel, biodiesel appears as one of the most promising sources of energy for diesel engines because of its environmental advantages and also due to the evolution of the petroleum market. Refined oil is the conventional raw material for the production of this biofuel; however, its major disadvantage is the high cost of its production. Therefore, frying oils, waste oils, crude oils and/or acid oils are being tested as alternative raw materials; nevertheless, there will be some problems if a homogeneous basic catalyst (NaOH) is employed due to the high amount of free fatty acid present in the raw oil. In this work, the transesterification reaction of acid oil using solid resin, Dowex monosphere 550 A, was studied as an alternative process. Ethanol was employed to have a natural and sustainable final product. The reaction temperature's effects, the initial amount of free fatty acid, the molar ratio of alcohol/oil and the type of catalyst (homogeneous or heterogeneous) over the main reaction are analyzed and their effects compared. The results obtained show that the solid resin is an alternative catalyst to be used to produce fatty acid ethyl esters (FAEEs) by a transesterification reaction with a final conversion over 90%. On the other hand, the time required to achieve this conversion is bigger than the one required using conventional technology which employs a homogeneous basic catalyst. This reaction time needs to be optimized. (author)

Effect of Periodic Water Addition on Citric Acid Production in Solid State Fermentation

Science.gov (United States)

Utpat, Shraddha S.; Kinnige, Pallavi T.; Dhamole, Pradip B.

2013-09-01

Water addition is one of the methods used to control the moisture loss in solid state fermentation (SSF). However, none of the studies report the timing of water addition and amount of water to be added in SSF. Therefore, this work was undertaken with an objective to evaluate the performance of periodic water addition on citric acid production in SSF. Experiments were conducted at different moistures (50-80 %) and temperatures (30-40 °C) to simulate the conditions in a fermenter. Citric acid production by Aspergillus niger (ATCC 9029) using sugarcane baggase was chosen as a model system. Based on the moisture profile, citric acid and sugar data, a strategy was designed for periodic addition of water. Water addition at 48, 96, 144 and 192 h enhanced the citric acid production by 62 % whereas water addition at 72, 120, and 168 h increased the citric acid production by just 17 %.

Tritium labeling of amino acids and peptides with liquid and solid tritium

International Nuclear Information System (INIS)

Peng, C.T.; Hua, R.L.; Souers, P.C.; Coronado, P.R.

1988-01-01

Amino acids and peptides were labeled with liquid and solid tritium at 21 K and 9 K. At these low temperatures radiation degradation is minimal, and tritium incorporation increases with tritium concentration and exposure time. Ring saturation in L-phenyl-alanine does not occur. Peptide linkage in oligopeptides is stable toward tritium. Deiodination in 3-iodotyrosine and 3,5-diiodotyrosine occurs readily and proceeds in steps by losing one iodine atom at a time. Nickel and noble metal supported catalysts when used as supports for dispersion of the substrate promote tritium labeling at 21 K. Our study shows that both liquid and solid tritium are potentially useful agents for labeling peptides and proteins. 11 refs., 1 fig., 3 tabs

Tritium labeling of amino acids and peptides with liquid and solid tritium

International Nuclear Information System (INIS)

Souers, P.C.; Coronado, P.R.; Peng, C.T.; Hua, R.L.

1988-01-01

Amino acids and peptides were labeled with liquid and solid tritium at 21/degree/K and 9/degree/K. At these low temperatures radiation degradation is minimal, and tritium incorporation increases with tritium concentration and exposure time. Ring saturation in L-phenylalanine does not occur. Peptide linkage in oligopeptides is stable toward tritium. Deiodination in 3-iodotyrosine and 3,5-diiodotyrosine occurs readily and proceeds in steps by losing one iodine atom at a time. Nickel and noble metal supported catalysts when used as supports for dispersion of the substrate promote tritium labeling at 21 K. Our study shows that both liquid and solid tritiums are potentially useful agents for labeling peptides and proteins

Influence of solid loading on D-xylose production through dilute sulphuric acid hydrolysis of olive stones

Directory of Open Access Journals (Sweden)

Cuevas, M.

2015-09-01

Full Text Available The selective hydrolysis of hemicellulose from olive stones was attempted in order to achieve a maximum D-xylose yield. For this aim, batch hydrolysis was conducted under different operating conditions of temperature, acid concentration and solid loading. Firstly, distilled water, sulphuric acid and nitric acid were assessed as hydrolytic agents at different temperatures (200, 205, 210 and 220 °C and at a fixed acid concentration (0.025 M. Sulphuric acid and 200 °C were selected for the subsequent dilute acid hydrolysis optimization based on the obtained D-xylose yields. The combined influence of solid loading (from 29.3 to 170.7 g olive stones into 300 mL acid solution and sulphuric acid concentration (0.006–0.034 M on the release of D-xylose was then estimated by response surface methodology. According to a statistical analysis, both parameters had significant interaction effects on D-xylose production. The results illustrated that the higher the solid loading, the higher the required acid concentration. The decrease in the solid/liquid ratio in the reactor had a positive effect on D-xylose extraction and on the amount of acid used. The optimum solid loading and sulphuric acid concentration were determined to be 50 g (solid/liquid ratio 1/6 and 0.016 M, respectively. Under these conditions, the predicted D-xylose yield (expressed as g of sugar per 100 g of dry matter fed was 20.4 (87.2% of maximum attainable.Se ha desarrollado una hidrólisis selectiva de la fracción hemicelulósica del hueso de aceituna con el fin de obtener el máximo rendimiento de D-xilosa. Para ello las hidrólisis se llevaron a cabo en un reactor discontinuo a distintas condiciones de temperatura, concentración de ácido y carga de sólidos. En primer lugar se evaluó la capacidad hidrolítica del agua destilada y de los ácidos nítrico y sulfúrico a distintas temperaturas (200, 205, 210 y 220°C manteniendo fija la concentración de ácido (0,025 M. A partir de

A novel tandem differential mobility analyzer with organic vapor treatment of aerosol particles

Directory of Open Access Journals (Sweden)

J. Joutsensaari

2001-01-01

Full Text Available A novel method to characterize the organic composition of aerosol particles has been developed. The method is based on organic vapor interaction with aerosol particles and it has been named an Organic Tandem Differential Mobility Analyzer (OTDMA. The OTDMA method has been tested for inorganic (sodium chloride and ammonium sulfate and organic (citric acid and adipic acid particles. Growth curves of the particles have been measured in ethanol vapor and as a comparison in water vapor as a function of saturation ratio. Measurements in water vapor show that sodium chloride and ammonium sulfate as well as citric acid particles grow at water saturation ratios (S of 0.8 and above, whereas adipic acid particles do not grow at S S = 0.75 and S = 0.79, respectively. Citric acid particles grow monotonously with increasing saturation ratios already at low saturation ratios and no clear deliquescence point is found. For sodium chloride and ammonium sulfate particles, no growth can be seen in ethanol vapor at saturation ratios below 0.93. In contrast, for adipic acid particles, the deliquescence takes place at around S = 0.95 in the ethanol vapor. The recrystallization of adipic acid takes place at S The results show that the working principles of the OTDMA are operational for single-component aerosols. Furthermore, the results indicate that the OTDMA method may prove useful in determining whether aerosol particles contain organic substances, especially if the OTDMA is operated in parallel with a hygroscopicity TDMA, as the growth of many substances is different in ethanol and water vapors.

Solid state radiolysis of sulphur-containing amino acids. Cysteine, cystine and methionine

International Nuclear Information System (INIS)

Franco Cataldo; Pietro Ragni; Susana Iglesias-Groth; Arturo Manchado

2011-01-01

The sulphur-containing proteinaceous amino acids l-cysteine, l-cystine and l-methionine were irradiated in the solid state to a dose of 3.2 MGy. This dose corresponds to that delivered by radionuclide decay in a timescale of 1.05 x 10 9 years to the organic matter buried at a depth >20 m in comets and asteroids. The purity of the sulphur-containing amino acids was studied by differential scanning calorimetry (DSC) before and after the solid state radiolysis and the preservation of the chirality after the radiolysis was studied by chirooptical methods (optical rotatory dispersion, ORD) and by FT-IR spectroscopy. Although the high radiation dose of 3.2 MGy delivered, all the amino acids studied show a high radiation resistance. The best radiation resistance was offered by l-cysteine. The radiolysis of l-cysteine leads to the formation of l-cystine. The radiation resistance of l-methionine is not at the level of l-cysteine but also l-methionine is able to survive the dose of 3.2 MGy. Furthermore in all cases examined the preservation of chirality after radiolysis was clearly observed by the ORD spectroscopy although a certain level of radioracemization was measured in all cases. The radioracemization is minimal in the case of l-cysteine and is more pronounced in the case of l-methionine. In conclusion, the study shows that the sulphur-containing amino acids can survive for 1.05 x 10 9 years and, after extrapolation of the data, even to the age of the Solar System i.e. to 4.6 x 10 9 years. (author)

Antisolvent Precipitation for the Synthesis of Monodisperse Mesoporous Niobium Oxide Spheres as Highly Effective Solid Acid Catalysts

KAUST Repository

Li, Cheng Chao; Dou, Jian; Chen, Luwei; Lin, Jianyi; Zeng, Hua Chun

2012-01-01

We have developed a low-cost reaction protocol to synthesize mesoporous Nb 2O 5-based solid acid catalysts with external shape control. In the synthesis, monodisperse glycolated niobium oxide spheres (GNOS) were prepared by means of a simple antisolvent precipitation approach and subsequently converted to mesoporous niobium oxide spheres (MNOS) with a large surface area of 312m 2g -1 by means of the hydrothermal treatment. The antisolvent acetone used to obtain GNOS was recovered through distillation at high purity. The obtained mesoporous MNOS were functionalized further with sulfate anions at different temperatures or incorporated with tungstophosphoric acid to obtain recyclable solid acid catalysts. These MNOS-based catalysts showed excellent performance in a wide range of acid-catalyzed reactions, such as Friedel-Crafts alkylation, esterification, and hydrolysis of acetates. As they are monodisperse spheres with diameters in the submicrometer range, the catalysts can be easily separated and reused. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Antisolvent Precipitation for the Synthesis of Monodisperse Mesoporous Niobium Oxide Spheres as Highly Effective Solid Acid Catalysts

KAUST Repository

Li, Cheng Chao

2012-03-20

We have developed a low-cost reaction protocol to synthesize mesoporous Nb 2O 5-based solid acid catalysts with external shape control. In the synthesis, monodisperse glycolated niobium oxide spheres (GNOS) were prepared by means of a simple antisolvent precipitation approach and subsequently converted to mesoporous niobium oxide spheres (MNOS) with a large surface area of 312m 2g -1 by means of the hydrothermal treatment. The antisolvent acetone used to obtain GNOS was recovered through distillation at high purity. The obtained mesoporous MNOS were functionalized further with sulfate anions at different temperatures or incorporated with tungstophosphoric acid to obtain recyclable solid acid catalysts. These MNOS-based catalysts showed excellent performance in a wide range of acid-catalyzed reactions, such as Friedel-Crafts alkylation, esterification, and hydrolysis of acetates. As they are monodisperse spheres with diameters in the submicrometer range, the catalysts can be easily separated and reused. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A convenient procedure for the solid-phase synthesis of hydroxamic acids on PEGA resins

DEFF Research Database (Denmark)

Nandurkar, Nitin Subhash; Petersen, Rico; Qvortrup, Katrine

2011-01-01

An efficient method for the solid-phase synthesis of hydroxamic acids is described. The method comprises the nucleophilic displacement of esters immobilized on PEGA resins with hydroxylamine/sodium hydroxide in isopropanol. The hydroxyaminolysis protocol is compatible with a broad range of PEGA...

Effect of organo-modified montmorillonite on poly(butylene succinate/poly(butylene adipate-co-terephthalate nanocomposites

Directory of Open Access Journals (Sweden)

2010-07-01

Full Text Available The composite material based on poly(butylene succinate (PBS, poly(butylene adipate-co-terephthalate (PBAT and organo-modified montmorillonite (OMMT were prepared by melt blending technique and characterized. Sodium montmorillonite (Na-MMT was successfully modified by octadecylammonium (ODA and dimethyldioctadecylammonium (DDOA salts to become OMMT through cation exchange technique which is shown by the increase of basal spacing of clay by XRD. The addition of the OMMT to the PBS/PBAT blends produced nanocomposites which is proved by XRD and TEM. Tensile tests showed increase in tensile strength and modulus which is attributed to the existence of strong interactions between PBS/PBAT and clay, particularly with OMMT. Highest tensile strength of nanocomposite was observed at 1 wt% of OMMT incorporated. TGA study showed that the thermal stability of the blend increased after the addition of clays. SEM micrographs of the fracture surfaces show that the morphology of the blend becomes homogeneous and smoother with presence of OMMT.

Nitric-phosphoric acid oxidation of solid and liquid organic materials

International Nuclear Information System (INIS)

Pierce, R.A.; Smith, J.R.; Poprik, D.C.

1995-01-01

Nitric-phosphoric acid oxidation has been developed specifically to address issues that face the Savannah River Site, other defense-related facilities, private industry, and small-volume generators such as university and medical laboratories. Initially tested to destroy and decontaminate SRS solid, Pu-contaminated job-control waste, the technology has also exhibited potential for remediating hazardous and mixed-hazardous waste forms. The process is unique to Savannah River and offers a valuable alternative to other oxidation processes that require extreme temperatures and/or elevated pressures. To address the broad categories of waste, many different organic compounds which represent a cross-section of the waste that must be treated have been successfully oxidized. Materials that have been quantitatively oxidized at atmospheric pressure below 180 degrees C include neoprene, cellulose, EDTA, tributylphosphate, and nitromethane. More stable compounds such as benzoic acid, polyethylene, oils, and resins have been completely decomposed below 200 degrees C and 10 psig. The process uses dilute nitric acid in a concentrated phosphoric acid media as the main oxidant for the organic compounds. Phosphoric acid allow nitric acid to be retained in solution well above its normal boiling point. The reaction forms NOx vapors which can be reoxidized and recycled using air and water. The addition of 0.001M Pd(II) reduces CO generation to near 1% of the released carbon gases. The advantages of this process are that it is straightforward, uses relatively inexpensive reagents, operates at relatively low temperature and pressure, and produces final solutions which are compatible with stainless steel equipment. For organic wastes, all carbon, hydrogen, and nitrogen are converted to gaseous products. If interfaced with an acid recovery system which converts NOx back to nitric acid, the net oxidizer would be oxygen from air

Comparative histological evaluation of new tyrosine-derived polymers and poly (L-lactic acid) as a function of polymer degradation.

Science.gov (United States)

Hooper, K A; Macon, N D; Kohn, J

1998-09-05

Previous studies demonstrated that poly(DTE carbonate) and poly (DTE adipate), two tyrosine-derived polymers, have suitable properties for use in biomedical applications. This study reports the evaluation of the in vivo tissue response to these polymers in comparison to poly(L-lactic acid) (PLLA). Typically, the biocompatibility of a material is determined through histological evaluations as a function of implantation time in a suitable animal model. However, due to changes that can occur in the tissue response at different stages of the degradation process, a fixed set of time points is not ideal for comparative evaluations of materials having different rates of degradation. Therefore the tissue response elicited by poly(DTE carbonate), poly(DTE adipate), and PLLA was evaluated as a function of molecular weight. This allowed the tissue response to be compared at corresponding stages of degradation. Poly(DTE adipate) consistently elicited the mildest tissue response, as judged by the width and lack of cellularity of the fibrous capsule formed around the implant. The tissue response to poly(DTE carbonate) was mild throughout the 570 day study. However, the response to PLLA fluctuated as a function of the degree of degradation, exhibiting an increase in the intensity of inflammation as the implant began to lose mass. At the completion of the study, tissue ingrowth into the degrading and disintegrating poly(DTE adipate) implant was evident while no comparative ingrowth of tissue was seen for PLLA. The similarity of the in vivo and in vitro degradation rates of each polymer confirmed the absence of enzymatic involvement in the degradation process. A comparison of molecular weight retention, water uptake, and mass loss in vivo with two commonly used in vitro systems [phosphate-buffered saline (PBS) and simulated body fluid (SBF)] demonstrated that for the two tyrosine-derived polymers the in vivo results were equally well simulated in vitro with PBS and SBF. However

Degradation of L-Ascorbic Acid in the Amorphous Solid State.

Science.gov (United States)

Sanchez, Juan O; Ismail, Yahya; Christina, Belinda; Mauer, Lisa J

2018-03-01

Ascorbic acid degradation in amorphous solid dispersions was compared to its degradation in the crystalline state. Physical blends and lyophiles of ascorbic acid and polymers (pectins and polyvinylpyrrolidone [PVP]) were prepared initially at 50:50 (w/w), with further studies using the polymer that best inhibited ascorbic acid crystallization in the lyophiles in 14 vitamin : PVP ratios. Samples were stored in controlled environments (25 to 60 °C, 0% to 23% RH) for 1 mo and analyzed periodically to track the physical appearance, change in moisture content, physical state (powder x-ray diffraction and polarized light microscopy), and vitamin loss (high performance liquid chromatography) over time. The glass transition temperatures of select samples were determined using differential scanning calorimetry, and moisture sorption profiles were generated. Ascorbic acid in the amorphous form, even in the glassy amorphous state, was more labile than in the crystalline form in some formulations at the highest storage temperature. Lyophiles stored at 25 and 40 °C and those in which ascorbic acid had crystallized at 60 °C (≥70% ascorbic acid : PVP) had no significant difference in vitamin loss (P > 0.05) relative to physical blend controls, and the length of storage had little effect. At 60 °C, amorphous ascorbic acid lyophiles (≤60% ascorbic acid : PVP) lost significantly more vitamin (P vitamin loss significantly increased over time. In these lyophiles, vitamin degradation also significantly increased (P vitamins are naturally present or added at low concentrations and production practices may promote amorphization of the vitamin. Vitamin C is one of the most unstable vitamins in foods. This study documents that amorphous ascorbic acid is less stable than crystalline ascorbic acid in some environments (for example, higher temperatures within 1 wk), especially when the vitamin is present at low concentrations in a product. These findings increase the understanding of

Effect of total solids content on methane and volatile fatty acid production in anaerobic digestion of food waste.

Science.gov (United States)

Liotta, Flavia; d'Antonio, Giuseppe; Esposito, Giovanni; Fabbricino, Massimiliano; van Hullebusch, Eric D; Lens, Piet N L; Pirozzi, Francesco; Pontoni, Ludovico

2014-10-01

This work investigates the role of the moisture content on anaerobic digestion of food waste, as representative of rapidly biodegradable substrates, analysing the role of volatile fatty acid production on process kinetics. A range of total solids from 4.5% to 19.2% is considered in order to compare methane yields and kinetics of reactors operated under wet to dry conditions. The experimental results show a reduction of the specific final methane yield of 4.3% and 40.8% in semi-dry and dry conditions compared with wet conditions. A decreasing trend of the specific initial methane production rate is observed when increasing the total solids concentration. Because of lack of water, volatile fatty acids accumulation occurs during the first step of the process at semi-dry and dry conditions, which is considered to be responsible for the reduction of process kinetic rates. The total volatile fatty acids concentration and speciation are proposed as indicators of process development at different total solids content. © The Author(s) 2014.

Conductivity And Thermal Stability of Solid Acid Composites CsH2PO4 /NaH2PO4/ SiO2

International Nuclear Information System (INIS)

Norsyahida Mohammad; Abu Bakar Mohamad; Abu Bakar Mohamad; Abdul Amir Hassan Kadhum

2016-01-01

Solid acid composites CsH 2 PO 4 / NaH 2 PO 4 / SiO 2 with different mole ratios of CsH 2 PO 4 and NaH 2 PO 4 to SiO 2 were synthesized and characterized. Preliminary infrared measurements of CsH 2 PO 4 and its composites indicated that hydrogen bonds breaking and formation were detected between 1710 to 2710 cm -1 , while the rotation of phosphate tetrahedral anions occurred between 900 and 1200 cm -1 . The superprotonic transition of CsH 2 PO 4 / NaH 2 PO 4 / SiO 2 composite was identified at superprotonic temperatures between 230 and 260 degree Celcius, under atmospheric pressure. This study reveals higher conductivity values for composites with higher CsH 2 PO 4 (CDP) content. Solid acid composite CDP 613 appeared as the composite with the highest conductivity that is 7.2x10 -3 S cm -1 at 230 degree Celcius. Thermal stability of the solid acid composites such as temperature of dehydration, melting and decomposition were investigated. The addition of NaH 2 PO 4 lowers the dehydration temperature of the solid acid composites. (author)

Production of Mycophenolic Acid by Penicillium brevicompactum Using Solid State Fermentation.

Science.gov (United States)

Patel, Gopal; Patil, Mahesh D; Soni, Surbhi; Chisti, Yusuf; Banerjee, Uttam Chand

2017-05-01

Solid-state fermentation using the microfungus Penicillium brevicompactum for the production of mycophenolic acid is reported in this paper. Of the initial substrates tested (whole wheat, cracked wheat, long grain Basmati rice, and short grain Parmal rice), Parmal rice proved to be the best. Under initial conditions, using steamed Parmal rice with 80% (w/w) initial moisture content, a maximum mycophenolic acid concentration of 3.4 g/kg substrate was achieved in 12 days of fermentation at 25 °C. The above substrate was supplemented with the following additional nutrients (g/L packed substrate): glucose 40.0, peptone 54.0, KH 2 PO 4 8.0, MgSO4⋅7H 2 O 2.0, glycine 7.0, and methionine 1.65 (initial pH 5.0). A small amount of a specified trace element solution was also added. The final mycophenolic acid concentration was increased to nearly 4 g/kg substrate by replacing glucose with molasses. Replacing Parmal rice with rice bran as substrate further improved the mycophenolic acid production to nearly 4.5 g/kg substrate.

Effects of organic solvents on hyaluronic acid nanoparticles obtained by precipitation and chemical crosslinking.

Science.gov (United States)

Bicudo, Rafaela Costa Souza; Santana, Maria Helena Andrade

2012-03-01

Hyaluronic acid is a hydrophilic mucopolysaccharide composed of alternating units of D-glucuronic acid and N-acetylglucosamine. It is used in many medical, pharmaceutical, and cosmetic applications, as sponges, films, or particle formulations. Hyaluronic acid nanoparticles can be synthesized free of oil and surfactants by nanoprecipitation in organic solvents, followed by chemical crosslinking. The organic solvent plays an important role in particles size and structure. Therefore, this study aimed to investigate the influence of acetone, ethanol, and isopropyl alcohol on the synthesis and physico-chemical properties of hyaluronic acid nanoparticles. Particles were crosslinked with adipic hydrazide and chloride carbodiimide under controlled conditions. The nanoparticles obtained with all three studied solvents were moderately electrostatically stable. Experiments with acetone produced the smallest particle size (120.44 nm) and polydispersity (0.27). The size and polydispersity of hyaluronic acid nanoparticles correlated with the surface tension between water and the organic solvents, not with the thermodynamic affinity of water for the organic solvents.

Potentiometric studies on ternary complexes involving some divalent transition metal ions, gallic acid and biologically abundant aliphatic dicarboxylic acids in aqueous solutions

Directory of Open Access Journals (Sweden)

Abdelatty Mohamed Radalla

2015-06-01

Full Text Available Formation of binary and ternary complexes of the divalent transition metal ions, Cu2+, Ni2+, Co2+ and Zn2+ with gallic acid and the biologically important aliphatic dicarboxylic acids (adipic, succinic, malic, malonic, maleic, tartaric and oxalic acids were investigated by means of the potentiometric technique at 25 °C and I = 0.10 mol dm−3 NaNO3. The acid-base properties of the ligands were investigated and discussed. The acidity constants of gallic acid and aliphatic dicarboxylic acids were determined and used for determining the stability constants of the binary and ternary complexes formed in the aqueous medium under the above experimental conditions. The formation of the different 1:1 and 1:2 binary complexes and 1:1:1 ternary complexes are inferred from the corresponding potentiometric pH-metric titration curves. The ternary complex formation was found to occur in a stepwise manner. The stability constants of these binary and ternary systems were calculated. The values of Δ log K, percentage of relative stabilization (%R.S. and log X were evaluated and discussed. The concentration distribution of the various complex species formed in solution was evaluated and discussed. The mode of chelation of ternary complexes formed was ascertained by conductivity measurements.

Thermal Properties of Polyurethane-Polyisocyanurate Foams Based on Poly(ethylene terephthalate Waste

Directory of Open Access Journals (Sweden)

Irena VITKAUSKIENĖ

2011-09-01

Full Text Available A series of polyurethane-polyisocyanurate (PU-PIR foams synthesized from PET-waste-derived aromatic polyester polyols (APP was studied using thermogravimetric analysis, Cone calorimeter and burning tests. The effect of chemical structure of the APP containing fragments of glycerol, adipic acid, poly(propylene glycol or hexanediol on thermal stability and flame resistance of the PU-PIR foams was elucidated. PU-PIR foams prepared from APP containing fragments of glycerol and/or adipic acid had higher thermal stability and lower weight loss at 330 °C. The foams based on APP derived from industrial PET waste were characterized by relatively low heat release and low smoke production. The presence of the fragments of the functional additives glycerol and/or adipic acid in the structure of APP used for production of PU-PIR foams, marginally decreased the heat release and slightly increased the smoke production.http://dx.doi.org/10.5755/j01.ms.17.3.588

Synthesis of sulfonated porous carbon nanospheres solid acid by a facile chemical activation route

Energy Technology Data Exchange (ETDEWEB)

Chang, Binbin, E-mail: changbinbin806@163.com; Guo, Yanzhen; Yin, Hang; Zhang, Shouren; Yang, Baocheng, E-mail: baochengyang@yahoo.com

2015-01-15

Generally, porous carbon nanospheres materials are usually prepared via a template method, which is a multi-steps and high-cost strategy. Here, we reported a porous carbon nanosphere solid acid with high surface area and superior porosity, as well as uniform nanospheical morphology, which prepared by a facile chemical activation with ZnCl{sub 2} using resorcinol-formaldehyde (RF) resins spheres as precursor. The activation of RF resins spheres by ZnCl{sub 2} at 400 °C brought high surface area and large volume, and simultaneously retained numerous oxygen-containing and hydrogen-containing groups due to the relatively low processing temperature. The presence of these functional groups is favorable for the modification of –SO{sub 3}H groups by a followed sulfonation treating with sulphuric acid and organic sulfonic acid. The results of N{sub 2} adsorption–desorption and electron microscopy clearly showed the preservation of porous structure and nanospherical morphology. Infrared spectra certified the variation of surface functional groups after activation and the successful modification of –SO{sub 3}H groups after sulfonation. The acidities of catalysts were estimated by an indirect titration method and the modified amount of –SO{sub 3}H groups were examined by energy dispersive spectra. The results suggested sulfonated porous carbon nanospheres catalysts possessed high acidities and –SO{sub 3}H densities, which endowed their significantly catalytic activities for biodiesel production. Furthermore, their excellent stability and recycling property were also demonstrated by five consecutive cycles. - Graphical abstract: Sulfonated porous carbon nanospheres with high surface area and superior catalytic performance were prepared by a facile chemical activation route. - Highlights: • Porous carbon spheres solid acid prepared by a facile chemical activation. • It owns high surface area, superior porosity and uniform spherical morphology. • It possesses

Solid state radiolysis of amino acids in an astrochemical perspective

International Nuclear Information System (INIS)

Cataldo, Franco; Angelini, Giancarlo; Iglesias-Groth, Susana; Manchado, Arturo

2011-01-01

The aliphatic amino acids L-alanine and L-leucine and the aromatic amino acids L-phenylalanine, L-tyrosine and L-tryptophan were irradiated in the solid state to a dose of 3.2 MGy. The degree of decomposition was measured by differential scanning calorimetry (DSC). Furthermore the degree of radioracemization was measured by optical rotatory dispersion (ORD) spectroscopy. From the DSC measurement a radiolysis rate constant k and the half life T 1/2 for each amino acid have been determined and extrapolated to a dose of 14 MGy, which corresponds to the expected total dose delivered by the decay of radionuclides to the organic molecules present in comets and asteroids in 4.6x10 9 years, the age of the Solar System. It is shown that all the amino acids studied can survive a radiation dose of 14 MGy although they are reduced to 1/4-1/5 of their original value they had at the beginning of the history of the Solar System. Consequently, the amount of alanine or leucine found today in the meteorites known as carbonaceous chondrites is just 1/4-1/5 of the amount originally present at the epoch of the formation of the Solar System 4.6x10 9 years ago. Among the amino acids studied, tyrosine shows the highest radiation resistance while tryptophan does not combine its relatively high radiation resistance with an elevated level of radioracemization resistance. Apart from the exception of tryptophan, it is shown that the radiolysis rate constants k of all the amino acids studied are in reasonable agreement with the radioracemization rate constant k rac .

Solid state radiolysis of amino acids in an astrochemical perspective

Energy Technology Data Exchange (ETDEWEB)

Cataldo, Franco, E-mail: franco.cataldo@fastwebnet.i [Istituto Nazionale di Astrofisica-Osservatorio Astrofisica di Catania, Via S. Sofia 78, 95123 Catania (Italy); Lupi Chemical Research, Via Casilina 1626/A, 00133 Rome (Italy); Angelini, Giancarlo [Istituto di Metodologie Chimiche, CNR, Via Salaria Km 29300, 00016 Monterotondo Stazione, Rome (Italy); Iglesias-Groth, Susana [Instituto de Astrofisica de Canarias, Via Lactea s/n, E-38200, La Laguna, Tenerife (Spain); Manchado, Arturo [Instituto de Astrofisica de Canarias, Via Lactea s/n, E-38200, La Laguna, Tenerife (Spain) and CSIC (Spain)

2011-01-15

The aliphatic amino acids L-alanine and L-leucine and the aromatic amino acids L-phenylalanine, L-tyrosine and L-tryptophan were irradiated in the solid state to a dose of 3.2 MGy. The degree of decomposition was measured by differential scanning calorimetry (DSC). Furthermore the degree of radioracemization was measured by optical rotatory dispersion (ORD) spectroscopy. From the DSC measurement a radiolysis rate constant k and the half life T{sub 1/2} for each amino acid have been determined and extrapolated to a dose of 14 MGy, which corresponds to the expected total dose delivered by the decay of radionuclides to the organic molecules present in comets and asteroids in 4.6x10{sup 9} years, the age of the Solar System. It is shown that all the amino acids studied can survive a radiation dose of 14 MGy although they are reduced to 1/4-1/5 of their original value they had at the beginning of the history of the Solar System. Consequently, the amount of alanine or leucine found today in the meteorites known as carbonaceous chondrites is just 1/4-1/5 of the amount originally present at the epoch of the formation of the Solar System 4.6x10{sup 9} years ago. Among the amino acids studied, tyrosine shows the highest radiation resistance while tryptophan does not combine its relatively high radiation resistance with an elevated level of radioracemization resistance. Apart from the exception of tryptophan, it is shown that the radiolysis rate constants k of all the amino acids studied are in reasonable agreement with the radioracemization rate constant k{sub rac}.

The Effect of Acid Pre-Treatment using Acetic Acid and Nitric Acid in The Production of Biogas from Rice Husk during Solid State Anaerobic Digestion (SS-AD)

Science.gov (United States)

Nugraha, Winardi Dwi; Syafrudin; Keumala, Cut Fadhila; Matin, Hasfi Hawali Abdul; Budiyono

2018-02-01

Pretreatment during biogas production aims to assist in degradation of lignin contained in the rice husk. In this study, pretreatment which is used are acid and biological pretreatment. Acid pretreatment was performed using acetic acid and nitric acid with a variety levels of 3% and 5%. While biological pretreatment as a control variable. Acid pretreatment was conducted by soaking the rice straw for 24 hours with acid variation. The study was conducted using Solid State Anaerobic Digestion (SS-AD) with 21% TS. Biogas production was measured using water displacement method every two days for 60 days at room temperature conditions. The results showed that acid pretreatment gave an effect on the production of biogas yield. The yield of the biogas produced by pretreatment of acetic acid of 5% and 3% was 43.28 and 45.86 ml/gr.TS. While the results without pretreatment biogas yield was 29.51 ml/gr.TS. The results yield biogas produced by pretreatment using nitric acid of 5% and 3% was 12.14 ml/gr.TS and 21.85 ml/gr.TS. Results biogas yield with acetic acid pretreatment was better than the biogas yield results with nitric acid pretreatment.

Processing stability of cross-linked starches in acid sauce applications and identification of some of the molecular factors involved

NARCIS (Netherlands)

Steeneken, P.A.M.; Woortman, A.J.J.; Oudhuis, A.A.C.M.

2011-01-01

The thickening functionality of four acetylated di-starch adipates with variations in starch source and amylose and adipate contents was evaluated in a simplified small-scale model sauce system at fourteen processing conditions with variations in temperature, shear, and pH. A processing stability

A Linker for the Solid-Phase Synthesis of Hydroxamic Acids and Identification of HDAC6 Inhibitors

DEFF Research Database (Denmark)

Bang, Claus Gunnar; Jensen, Jakob Feldthusen; Cohrt, Anders Emil O'Hanlon

2017-01-01

We herein present broadly useful, readily available and nonintegral hydroxylamine linkers for the routine solid-phase synthesis of hydroxamic acids. The developed protocols enable the efficient synthesis and release of a wide range of hydroxamic acids from various resins, relying on high control...... and flexibility with respect to reagents and synthetic processes. A trityl-based hydroxylamine linker was used to synthesize a library of peptide hydroxamic acids. The inhibitory effects of the compounds were examined for seven HDAC enzyme subtypes using a chemiluminescence-based assay....

Optimisation of a wet FGD pilot plant using fine limestone and organic acids

DEFF Research Database (Denmark)

Frandsen, Jan; Kiil, Søren; Johnsson, Jan Erik

2001-01-01

, but the residual limestone content in the gypsum increased to somewhere between 19 and 30 wt%, making this pH range unsuitable for use in a full-scale plant. The investigations have shown that both the addition of organic acids and the use of a limestone with a fine PSD can be used to optimise wet FGD plants. (C......The effects of adding an organic acid or using a limestone with a fine particle size distribution (PSD) have been examined in a wet flue gas desulphurisation (FGD) pilot plant. Optimisation of the plant with respect to the degree of desulphurisation and the residual limestone content of the gypsum...... has been the aim of the work. In contrast to earlier investigations with organic acids, all essential process parameters (i.e. gas phase concentration profiles of SO(2), slurry pH profiles. and residual limestone in the gypsum) were considered. Slurry concentrations of adipic acid in the range of 0...

Direct Succinic Acid Production from Minimally Pretreated Biomass Using Sequential Solid-State and Slurry Fermentation with Mixed Fungal Cultures

Directory of Open Access Journals (Sweden)

Jerico Alcantara

2017-06-01

Full Text Available Conventional bio-based succinic acid production involves anaerobic bacterial fermentation of pure sugars. This study explored a new route for directly producing succinic acid from minimally-pretreated lignocellulosic biomass via a consolidated bioprocessing technology employing a mixed lignocellulolytic and acidogenic fungal co-culture. The process involved a solid-state pre-fermentation stage followed by a two-phase slurry fermentation stage. During the solid-state pre-fermentation stage, Aspergillus niger and Trichoderma reesei were co-cultured in a nitrogen-rich substrate (e.g., soybean hull to induce cellulolytic enzyme activity. The ligninolytic fungus Phanerochaete chrysosporium was grown separately on carbon-rich birch wood chips to induce ligninolytic enzymes, rendering the biomass more susceptible to cellulase attack. The solid-state pre-cultures were then combined in a slurry fermentation culture to achieve simultaneous enzymatic cellulolysis and succinic acid production. This approach generated succinic acid at maximum titers of 32.43 g/L after 72 h of batch slurry fermentation (~10 g/L production, and 61.12 g/L after 36 h of addition of fresh birch wood chips at the onset of the slurry fermentation stage (~26 g/L production. Based on this result, this approach is a promising alternative to current bacterial succinic acid production due to its minimal substrate pretreatment requirements, which could reduce production costs.

21 CFR 184.1009 - Adipic acid.

Science.gov (United States)

2010-04-01

... CONSUMPTION (CONTINUED) DIRECT FOOD SUBSTANCES AFFIRMED AS GENERALLY RECOGNIZED AS SAFE Listing of Specific....3 percent for meat products as defined in § 170.3(n)(29) of this chapter; 1.3 percent for snack...

Preparation, characterization and pharmacokinetics of enrofloxacin-loaded solid lipid nanoparticles: influences of fatty acids.

Science.gov (United States)

Xie, Shuyu; Zhu, Luyan; Dong, Zhao; Wang, Xiaofang; Wang, Yan; Li, Xihe; Zhou, WenZhong

2011-04-01

Enrofloxacin-loaded solid lipid nanoparticles (SLN) were prepared using fatty acids (tetradecanoic acid, palmitic acid, stearic acid) as lipid matrix by hot homogenization and ultrasonication method. The effect of fatty acids on the characteristics and pharmacokinetics of the SLN were investigated. The results showed that the encapsulation efficiency and loading capacity of nanoparticles varied with fatty acids in the order of stearic acid>palmitic acid>tetradecanoic acid. Furthermore, stearic acid-SLN had larger particle size, bigger polydispersity index (PDI) and higher zeta potential compared with the other two fatty acid formulated SLN. The SLN showed sustained releases in vitro and the released enrofloxacin had the same antibacterial activity as that of the native enrofloxacin. Although in vitro release exhibited similar patterns, within 24 h the releasing rates of the three formulations were significantly different (tetradecanoic acid-SLN>palmitic acid-SLN>stearic acid-SLN). Pharmacokinetic study after a single dose of intramuscular administration to mice demonstrated that tetradecanoic acid-SLN, palmitic acid-SLN, and stearic acid-SLN increased the bioavailability by 6.79, 3.56 and 2.39 folds, and extended the mean residence time (MRT) of the drug from 10.60 h to 180.36, 46.26 and 19.09 h, respectively. These results suggest that the enrofloxacin-fatty acid SLN are promising formulations for sustained release while fatty acids had significant influences on the characteristics and performances of the SLN. Copyright © 2010 Elsevier B.V. All rights reserved.

Synthesis of biodiesel from waste vegetable oil with large amounts of free fatty acids using a carbon-based solid acid catalyst

Energy Technology Data Exchange (ETDEWEB)

Shu, Qing; Gao, Jixian; Nawaz, Zeeshan; Liao, Yuhui; Wang, Dezheng; Wang, Jinfu [Beijing Key Laboratory of Green Chemical Reaction Engineering and Technology, Department of Chemical Engineering, Tsinghua University, Beijing 100084 (China)

2010-08-15

A carbon-based solid acid catalyst was prepared by the sulfonation of carbonized vegetable oil asphalt. This catalyst was employed to simultaneously catalyze esterification and transesterification to synthesis biodiesel when a waste vegetable oil with large amounts of free fatty acids (FFAs) was used as feedstock. The physical and chemical properties of this catalyst were characterized by a variety of techniques. The maximum conversion of triglyceride and FFA reached 80.5 wt.% and 94.8 wt.% after 4.5 h at 220 C, when using a 16.8 M ratio of methanol to oil and 0.2 wt.% of catalyst to oil. The high catalytic activity and stability of this catalyst was related to its high acid site density (-OH, Broensted acid sites), hydrophobicity that prevented the hydration of -OH species, hydrophilic functional groups (-SO{sub 3}H) that gave improved accessibility of methanol to the triglyceride and FFAs, and large pores that provided more acid sites for the reactants. (author)

Production and characterization of novel starch and poly(butylene adipate-co-terephthalate)-based materials and their applications

Science.gov (United States)

Stagner, Jacqueline Ann

This work focuses on the production and characterization of blends of maleated thermoplastic starch (MTPS) and poly(butylenes adipate-co-terephthalate) and their application for use as thermoformed objects, films, and foams. First, by the production and characterization of maleated thermoplastic starch (MTPS) synthesized by reactive extrusion in a twin-screw extruder, a better understanding of MTPS was gained. This reactive thermoplastic starch was prepared with glycerol as the plasticizer, maleic anhydride (MA), and free-radical initiator, 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane (Luperox 101). Dynamic light scattering (DLS), differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), soxhlet extraction in acetone, and environmental scanning electron microscopy (ESEM) were performed to determine the effect of maleation, extrusion temperature, initiator concentration, and maleic anhydride concentration on the resulting MTPS. Next, maleated thermoplastic starch (MTPS) and thermoplastic starch (TPS) were reactively blended in a twin-screw extruder with a biodegradable polyester, poly(butylene adipate-co-terephthalate) (PBAT). The blends were extruded to produce thermoformable sheets. The mechanical properties of the sheets were characterized by tensile and puncture tests. Proof of grafting was determined by soxhlet extraction in dichloromethane and FTIR analysis. Observations of the thermal properties were made using DSC, while the surface of the sheets was imaged using ESEM. Blends of MTPS and PBAT were also extruded to produce films. Mechanical testing (tensile and puncture tests) and barrier performance testing (carbon dioxide, oxygen, and water vapor permeability) were performed on the films. Transmission electron microscopy (TEM) was used to image the blends and to view the dispersion of the various phases. Finally, blends of MTPS and PBAT were extruded with an endothermic chemical blowing agent to produce foams. The foams were

Utilization of solid catfish manure waste as carbon and nutrient source for lactic acid production.

Science.gov (United States)

Shi, Suan; Li, Jing; Blersch, David M

2018-04-19

The aim of this work was to study the solid waste (manure) produced by catfish as a potential feedstock for the production of lactic acid (LA) via fermentation. The solid waste contains high levels of both carbohydrates and nutrients that are sufficient for LA bacteria. Simultaneous saccharification and co-fermentation (SSCF) was applied using enzyme and Lactobacillus pentosus, and different loadings of enzyme and solid waste were tested. Results showed LA concentrations of 35.7 g/L were obtained at 15% solids content of catfish waste. Because of the high nutrient content in the fish waste, it could also be used as supplementary substrate for nitrogen and carbon sources with other lignocellulosic materials. A combined feedstock of catfish waste and paper mill sludge was tested, increasing the final LA concentration to 43.1 g/L at 12% solids loading. The catfish waste was shown to be a potential feedstock to provide both carbon and nutrients for LA production, suggesting its use as a sole substrate or in combination with other lignocellulosic materials.

Cholesterylbutyrate Solid Lipid Nanoparticles as a Butyric Acid Prodrug

Directory of Open Access Journals (Sweden)

Alessandro Mauro

2008-02-01

Full Text Available Cholesterylbutyrate (Chol-but was chosen as a prodrug of butyric acid.Butyrate is not often used in vivo because its half-life is very short and therefore too largeamounts of the drug would be necessary for its efficacy. In the last few years butyric acid'santi-inflammatory properties and its inhibitory activity towards histone deacetylases havebeen widely studied, mainly in vitro. Solid Lipid Nanoparticles (SLNs, whose lipid matrixis Chol-but, were prepared to evaluate the delivery system of Chol-but as a prodrug and totest its efficacy in vitro and in vivo. Chol-but SLNs were prepared using the microemulsionmethod; their average diameter is on the order of 100-150 nm and their shape is spherical.The antineoplastic effects of Chol-but SLNs were assessed in vitro on different cancer celllines and in vivo on a rat intracerebral glioma model. The anti-inflammatory activity wasevaluated on adhesion of polymorphonuclear cells to vascular endothelial cells. In thereview we will present data on Chol-but SLNs in vitro and in vivo experiments, discussingthe possible utilisation of nanoparticles for the delivery of prodrugs for neoplastic andchronic inflammatory diseases.

Development of starch biofilms using different carboxylic acids as plasticizers; Desenvolvimento de biofilmes de amido utilizando como plastificantes diferentes acidos carboxilicos

Energy Technology Data Exchange (ETDEWEB)

Cruz, L.C.; Miranda, C.S.; Santos, W.J. dos; Goncalves, A.P.B.; Oliveira, J.C.; Jose, N.M., E-mail: uanaconceicaocruz@gmail.com [Universidade Federal da Bahia (GECIM/UFBA), Salvador, BA (Brazil). Programa de Pos-Graduacao em Engenharia Quimica. Grupo de Energia e Ciencias dos Materiais

2014-07-01

Biodegradable films have become a widely exploited issue among scientists because of their positive environmental impact, besides their potential to promote better food conservation and an increase in shelf life. Starch has been studied in this field due to its availability, low cost and biodegradability. However, starch films tend to be brittle and they need addition of a plasticizer to enable their usage. In this work, starch films were synthesized with different carboxylic acids as plasticizers, aiming to observe the effect of the acids chain size in the final films properties. The acids used were: oxalic, succinic and adipic. The materials were produced by casting and characterized by DSC, TG, DRX e FTIR. It was observed that the acids chain size influenced on the thermal and structural properties of the films. (author)

Separation of oils from solids

International Nuclear Information System (INIS)

Van Slyke, D.C.

1992-01-01

This patent describes a method for cleaning oil-contaminated particulate solids. It comprises: contacting contaminated solids with a non-aqueous liquid composition comprising a carboxylic acid; then contacting the solids with an aqueous wash containing a reagent for converting the carboxylic acid to a water-soluble carboxylate salt; and removing an aqueous phase containing carboxylate salt and entrained oil

Continuous synthesis of Oleyl Oleate in supercritical carbon oxide using solid p-Toluenesulfonic Acid as catalyst

International Nuclear Information System (INIS)

Ghaziaskar, H.; Ikushima, Y.

2000-01-01

Supercritical carbon dioxide (Sc-CO 2 ) was used as solvent to synthesize oleyl oleate as an analog of Jojoba oil from oleic acid and oleyl alcohol with high conversion (100%) of the acid into ester in a short time of 100 min. Utilizing a low cost solid catalyst, p-toluenesulfonic acid monohydrate , the esterification reaction was performed, without any prior preparation step, in a flow mode, at a pressure of 147 bar and a temperature of 60 d eg C. This method seems industrially suitable for the production of oleyl oleate. The solubility of a mixture of oleyl alcohol and oleic acid in Sc-CO 2 were also measured to calculate the alcohol to acid ratio and the esterification yield

Preparation and application of zirconium sulfate supported on SAPO-34 molecular sieve as solid acid catalyst for esterification

Energy Technology Data Exchange (ETDEWEB)

Xu, Dongyan, E-mail: xdy0156@sina.com; Ma, Hong; Cheng, Fei

2014-05-01

Graphical abstract: - Highlights: • SAPO-34 supported zirconium sulfate solid acid catalyst was prepared. • Esterification of acetic acid with ethanol can be catalyzed by ZS/SAPO-34. • The hydration of ZS is vital to the acidic property and catalytic performance. • The ZS/SAPO-34 catalyst treated at 200 °C shows good reusability. - Abstract: Zirconium sulfate (ZS) was supported on SAPO-34 molecular sieve by using an incipient wetness impregnation method with zirconium sulfate as the precursor. The as-prepared catalysts were used as solid acid catalyst for esterification reaction of acetic acid with ethanol. The influence of calcination temperature on the acidic property, catalytic activity, and reusability of ZS/SAPO-34 catalysts were mainly investigated. FT-IR, SEM, EDS and TG analysis have been carried out to demonstrate the characteristics of ZS/SAPO-34 catalysts. It was found that the 30 wt%ZS/SAPO-34 catalysts display the property of superacid irrespective of calcination temperature. The ZS/SAPO-34 catalyst treated at 200 °C can enhance the interaction between the supported ZS and SAPO-34 and keep the catalyst remaining substantially active after several reaction cycles. However, further increasing calcination temperature will cause the transfer of ZS from hydrate to anhydrous phase, and thus the decrease of activity.

Preparation and application of zirconium sulfate supported on SAPO-34 molecular sieve as solid acid catalyst for esterification

International Nuclear Information System (INIS)

Xu, Dongyan; Ma, Hong; Cheng, Fei

2014-01-01

Graphical abstract: - Highlights: • SAPO-34 supported zirconium sulfate solid acid catalyst was prepared. • Esterification of acetic acid with ethanol can be catalyzed by ZS/SAPO-34. • The hydration of ZS is vital to the acidic property and catalytic performance. • The ZS/SAPO-34 catalyst treated at 200 °C shows good reusability. - Abstract: Zirconium sulfate (ZS) was supported on SAPO-34 molecular sieve by using an incipient wetness impregnation method with zirconium sulfate as the precursor. The as-prepared catalysts were used as solid acid catalyst for esterification reaction of acetic acid with ethanol. The influence of calcination temperature on the acidic property, catalytic activity, and reusability of ZS/SAPO-34 catalysts were mainly investigated. FT-IR, SEM, EDS and TG analysis have been carried out to demonstrate the characteristics of ZS/SAPO-34 catalysts. It was found that the 30 wt%ZS/SAPO-34 catalysts display the property of superacid irrespective of calcination temperature. The ZS/SAPO-34 catalyst treated at 200 °C can enhance the interaction between the supported ZS and SAPO-34 and keep the catalyst remaining substantially active after several reaction cycles. However, further increasing calcination temperature will cause the transfer of ZS from hydrate to anhydrous phase, and thus the decrease of activity

Characterization and Design of Zeolite Catalysts Solid Acidity, Shape Selectivity and Loading Properties

CERN Document Server

Niwa, Miki; Okumura, Kazu

2010-01-01

Zeolites are microporous, aluminosilicate minerals commonly used as commercial adsorbents. Zeolite-based catalysts are used by industrial chemical companies in the interconversion of hydrocarbons and the alkylation of aromatic compounds. The current book deals with the characterization of specific properties of Zeolites and calculations for the design of catalysts. Measurements and utilization of solid acidity, shape selectivity, and loading properties, that are three prominent properties of a Zeolite catalyst, are treated in detail. These features concern chemical vapor deposition of silica, shape selectivity, loading properties, solid activity, Brønsted or Lewis character, ammonia temperature programmed desorption, control of the pore-opening size by chemical vapor deposition of silica and XAFS analysis of metals being highly dispersed inside and outside a framework.

Palm Frond and Spikelet as Environmentally Benign Alternative Solid Acid Catalysts for Biodiesel Production

Directory of Open Access Journals (Sweden)

Yahaya Muhammad Sani

2015-04-01

Full Text Available A carbonization-sulfonation method was utilized in synthesizing sulfonated mesoporous catalysts from palm tree biomass. Brunauer-Emmet-Teller (BET, powder X-ray diffraction (XRD, energy dispersive X-ray (EDX, and field emission scanning emission microscopy (FE-SEM analyses were used to evaluate the structural and textural properties of the catalysts. Further, Fourier transform infrared (FT-IR spectroscopy and titrimetric analyses measured the strong acid value and acidity distribution of the materials. These analyses indicated that the catalysts had large mesopore volume, large surface area, uniform pore size, and high acid density. The catalytic activity exhibited by esterifying used frying oil (UFO containing high (48% free fatty acid (FFA content further indicated these properties. All catalysts exhibited high activity, with sPTS/400 converting more than 98% FFA into fatty acid methyl esters (FAMEs. The catalyst exhibited the highest acid density, 1.2974 mmol/g, determined by NaOH titration. This is outstanding considering the lower reaction parameters of 5 h, 5:1 methanol-to-oil ratio, and a moderate temperature range between 100 and 200 °C. The study further illustrates the prospect of converting wastes into highly efficient, benign, and recyclable solid acid catalysts.

Surface acidity and solid-state compatibility of excipients with an acid-sensitive API: case study of atorvastatin calcium.

Science.gov (United States)

Govindarajan, Ramprakash; Landis, Margaret; Hancock, Bruno; Gatlin, Larry A; Suryanarayanan, Raj; Shalaev, Evgenyi Y

2015-04-01

The objectives of this study were to measure the apparent surface acidity of common excipients and to correlate the acidity with the chemical stability of an acid-sensitive active pharmaceutical ingredient (API) in binary API-excipient powder mixtures. The acidity of 26 solid excipients was determined by two methods, (i) by measuring the pH of their suspensions or solutions and (ii) the pH equivalent (pHeq) measured via ionization of probe molecules deposited on the surface of the excipients. The chemical stability of an API, atorvastatin calcium (AC), in mixtures with the excipients was evaluated by monitoring the appearance of an acid-induced degradant, atorvastatin lactone, under accelerated storage conditions. The extent of lactone formation in AC-excipient mixtures was presented as a function of either solution/suspension pH or pHeq. No lactone formation was observed in mixtures with excipients having pHeq > 6, while the lactone levels were pronounced (> 0.6% after 6 weeks at 50°C/20% RH) with excipients exhibiting pHeq 6, 3-6, and < 3) were consistent with the reported solution pH-stability profile of AC. In contrast to the pHeq scale, lactone formation did not show any clear trend when plotted as a function of the suspension/solution pH. Two mechanisms to explain the discrepancy between the suspension/solution pH and the chemical stability data were discussed. Acidic excipients, which are expected to be incompatible with an acid-sensitive API, were identified based on pHeq measurements. The incompatibility prediction was confirmed in the chemical stability tests using AC as an example of an acid-sensitive API.

Bacterial dynamics and metabolite changes in solid-state acetic acid fermentation of Shanxi aged vinegar.

Science.gov (United States)

Li, Sha; Li, Pan; Liu, Xiong; Luo, Lixin; Lin, Weifeng

2016-05-01

Solid-state acetic acid fermentation (AAF), a natural or semi-controlled fermentation process driven by reproducible microbial communities, is an important technique to produce traditional Chinese cereal vinegars. Highly complex microbial communities and metabolites are involved in traditional Chinese solid-state AAF, but the association between microbiota and metabolites during this process are still poorly understood. In this study, we performed amplicon 16S rRNA gene sequencing on the Illumina MiSeq platform, PCR-denaturing gradient gel electrophoresis, and metabolite analysis to trace the bacterial dynamics and metabolite changes under AAF process. A succession of bacterial assemblages was observed during the AAF process. Lactobacillales dominated all the stages. However, Acetobacter species in Rhodospirillales were considerably accelerated during AAF until the end of fermentation. Quantitative PCR results indicated that the biomass of total bacteria showed a "system microbe self-domestication" process in the first 3 days, and then peaked at the seventh day before gradually decreasing until the end of AAF. Moreover, a total of 88 metabolites, including 8 organic acids, 16 free amino acids, and 66 aroma compounds were detected during AAF. Principal component analysis and cluster analyses revealed the high correlation between the dynamics of bacterial community and metabolites.

Conversion of polar and non-polar algae oil lipids to fatty acid methyl esters with solid acid catalysts--A model compound study.

Science.gov (United States)

Asikainen, Martta; Munter, Tony; Linnekoski, Juha

2015-09-01

Bio-based fuels are becoming more and more important due to the depleting fossil resources. The production of biodiesel from algae oil is challenging compared to terrestrial vegetable oils, as algae oil consists of polar fatty acids, such as phospholipids and glycolipids, as well as non-polar triglycerides and free fatty acids common in vegetable oils. It is shown that a single sulphonated solid acid catalyst can perform the esterification and transesterification reactions of both polar and non-polar lipids. In mild reaction conditions (60-70 °C) Nafion NR50 catalyst produces methyl palmitate (FAME) from the palmitic acid derivatives of di-, and tri-glyceride, free fatty acid, and phospholipid with over 80% yields, with the glycolipid derivative giving nearly 40% yields of FAME. These results demonstrate how the polar and non-polar lipid derivatives of algal oil can be utilised as feedstocks for biodiesel production with a single catalyst in one reaction step. Copyright © 2015 Elsevier Ltd. All rights reserved.

The effect of the distance between acidic site and basic site immobilized on mesoporous solid on the activity in catalyzing aldol condensation

Science.gov (United States)

Yu, Xiaofang; Yu, Xiaobo; Wu, Shujie; Liu, Bo; Liu, Heng; Guan, Jingqi; Kan, Qiubin

2011-02-01

Acid-base bifunctional heterogeneous catalysts containing carboxylic and amine groups, which were immobilized at defined distance from one another on the mesoporous solid were synthesized by immobilizing lysine onto carboxyl-SBA-15. The obtained materials were characterized by X-ray diffraction (XRD), N 2 adsorption, Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), scanning electron micrographs (SEM), transmission electron micrographs (TEM), elemental analysis, and back titration. Proximal-C-A-SBA-15 with a proximal acid-base distance was more active than maximum-C-A-SBA-15 with a maximum acid-base distance in aldol condensation reaction between acetone and various aldehydes. It appears that the distance between acidic site and basic site immobilized on mesoporous solid should be an essential factor for catalysis optimization.

Meso- and macroporous sulfonated starch solid acid catalyst for esterification of palm fatty acid

Directory of Open Access Journals (Sweden)

Ibrahim M. Lokman

2016-03-01

Full Text Available In the present work, a heterogeneous solid acid catalyst was successfully developed from starch. The catalyst was prepared by a significant two-step process; the initial step was incomplete carbonization of starch (ICS at 400 °C for 12 h and consequently followed by sulfonation process using concentrated H2SO4 to produce sulfonated-incomplete carbonized starch (ICS-SO3H. The characterization of the ICS-SO3H catalyst was done for chemical and physical properties such as X-ray diffraction (XRD, ammonia-temperature programmed desorption (NH3-TPD, surface area analysis, thermal gravimetric analysis (TGA, elemental analysis and morphology analysis by scanning electron microscope (SEM. BET results showed the structure of ICS-SO3H consists of meso- and macro-porous properties, which allowed high density of the SO3H group attached on its carbon networks. The catalytic activity of ICS-SO3H catalyst was determined by analyzing the catalyst performance to esterify palm fatty acid distillate (PFAD and sequentially produced methyl ester. The maximum free fatty acid (FFA conversion and FAME yield were as high as 94.6% and 90.4%, respectively, at 75 °C using 10:1 methanol-to-PFAD molar ratio and 2 wt.% of catalyst within 3 h. The catalyst has sufficient potential to recycle up to 6 reactions without reactivation step and any remarkable loss of catalytic activity. It revealed that the heterogeneous ICS-SO3H catalyst exhibits high stability, reusability and catalytic activity.

Binary and ternary solid-liquid phase equilibrium for the systems formed by succinic acid, urea and diethylene glycol: Determination and modelling

International Nuclear Information System (INIS)

Li, Yanxun; Li, Congcong; Han, Shuo; Zhao, Hongkun

2017-01-01

Highlights: • Solubility of succinic acid in diethylene glycol was determined. • Solubility of succinic acid + urea + diethylene glycol was determined. • Three ternary phase diagrams were constructed for the ternary system. • The ternary phase diagrams were correlated using NRTL model. - Abstract: In this work, the solid-liquid phase equilibrium for binary system of succinic acid + diethylene glycol at the temperatures ranging from (298.15 to 333.15) K and ternary system of (succinic acid + urea + diethylene glycol) at 298.15 K, 313.15 K and 333.15 K was built by using the isothermal saturation method under atmospheric pressure (101.2 kPa), and the solubilities were determined by a high-performance liquid chromatography. The solid-phases formed in the ternary system of ((succinic acid + urea + diethylene glycol)) were confirmed by Schreinemaker’s method of wet residue, which corresponded to urea, succinic acid, and adduct 2:1 urea-succinic acid (mole ratio). Three isothermal phase diagrams for the ternary system were constructed based on the measured mutual solubility. Each isothermal phase diagram included six crystallization fields, three invariant curves, two invariant points and two co-saturated points. The crystalline region of adduct 2:1 urea-succinic acid is larger than those of the other two solids. The solubility of succinic acid in diethylene glycol was correlated with the modified Apelblat equation, λh equation and NRTL model; and the mutual solubility of the ternary ((succinic acid + urea + diethylene glycol)) system was correlated and calculated by the NRTL model. The interaction parameters’ values of succinic acid-urea were acquired. The value of RMSD was 7.11 × 10 −3 for the ternary system. The calculation results had good agreement with the experiment values. Furthermore, the densities of equilibrium liquid phase were acquired. The phase diagrams and the thermodynamic model of the ternary system could provide the basis for design of

Microwave-assisted solid phase conversion study of Meldrum's acid to ethylenetetracarboxylic dianhydride (C 6O 6)

Science.gov (United States)

Taherpour, Avat (Arman)

2010-01-01

Utilization of microwave irradiation provides an effective method for fast synthesizing of some important compounds. Microwave-assisted solid phase is an especial class in chemical synthesis. By the use of MW-irradiation on chemicals, sometimes interesting results can be seen. The synthesis of the interesting molecule ethylenetetracarboxylic dianhydride (C 6O 6) was attempted with a few different methods. In this study, the microwave-assisted solid phase conversion of Meldrum's acid to ethylenetetracarboxylic dianhydride was reported. This conversion was characterized by FT-IR, GC/MS and NMR spectroscopy results.

Hydrogen production by electrochemical decomposition of formic acid via solid polymer electrolyte

Energy Technology Data Exchange (ETDEWEB)

Kilic, Ebru Oender [KOSGEB Bursa Business Development Center, Besevler Kucuk Sanayi Sitesi 16149 Nilufer/Bursa (Turkey); Koparal, Ali Savas; Oeguetveren, Uelker Bakir [Anadolu University, Iki Eylul Campus, Applied Research Center for Environmental Problems 26555 Eskisehir (Turkey); Anadolu University, Iki Eylul Campus, Department of Environmental Engineering, 26555 Eskisehir (Turkey)

2009-01-15

The aim of this work is to investigate the feasibility of simultaneous hydrogen production by electrochemical decomposition of formic acid via solid polymer electrolyte (SPE) in an electrochemical reactor. Titanium oxide coated with iridium oxide as anode and carbon fibre with Pt catalyst as cathode were used in the experiments. Effects of applied current density, flow rates and temperature of formic acid solution, concentration of supporting electrolyte and pH of the solution on performance of the process have been investigated. The effect of membrane thickness has also been examined. The results suggest that electrolysis using SPE is a promising method for the treatment of organic pollutants. Hydrogen with purity of 99.999% at ambient temperature by using carbon fibre cathode with Pt catalyst can be produced simultaneously and COD removal efficiency of 95% has been achieved not requiring any chemical addition and temperature increase. Also complete electrochemical oxidation of formic acid at the original pH to CO{sub 2} and H{sub 2}O without production of intermediate has been proved by HPLC analysis. (author)

Heat capacity and thermodynamics of solid and liquid pyridine-3-carboxylic acid (nicotinic acid) over the temperature range 296 K to 531 K

International Nuclear Information System (INIS)

Joseph, Abhinav; Bernardes, Carlos E.S.; Minas da Piedade, Manuel E.

2012-01-01

Highlights: ► We determined the heat capacity of solid and liquid nicotinic acid by DSC. ► We determined Δ 357.8K 305.6K H m o (NA,crII) by Calvet microcalorimetry. ► We studied the thermodynamics of the cr II → cr I phase transition. ► We determined the Δ f G m o –T diagram of nicotinic acid for T = (296 to 531) K. - Abstract: The molar heat capacity of pyridine-3-carboxylic acid (nicotinic acid) for T = (296 to 531) K was investigated by differential scanning calorimetry (DSC) and Calvet-drop microcalorimetry. The measurements extended up to the liquid range and also covered the interval where a reversible and fast solid-solid (cr II → cr I) phase transition occurs. The molar enthalpies and entropies of that phase transition and of fusion were obtained as T trs = (455.0 ± 0.2) K, Δ trs H m o = (0.90 ± 0.10) kJ ⋅ mol −1 , Δ trs S m o = (1.98 ± 0.22) J ⋅ K −1 ⋅ mol −1 , T fus = (509.91 ± 0.04) K, Δ fus H m o = (28.2 ± 0.1) kJ ⋅ mol −1 , and Δ fus S m o = (55.30 ± 0.16) J ⋅ K −1 ⋅ mol −1 . By combining these experimental results with the previously reported Δ sub H m (NA,cr II) at T = 366.5 K, the corresponding entropy in the gaseous state calculated at the B3LYP/6-31+G(d,p) level of theory, and Δ f H m o (NA),cr II) at T = 298.15 K, it was possible to estimate the standard molar Gibbs energy of formation functions necessary for the construction of the Δ f G m ∘ vs. T diagram illustrating the enantiotropic nature of this system.

Polymer blends of polylactic acid (PLA) and polybutylene succinate-adipate

Science.gov (United States)

Ma, Wenguang

A series of blends consisting of polylactic acid (PLA) and aliphatic succinate polyester (BionolleRTM #3000) had been prepared and investigated. The results of mechanical property investigations showed that using 20 wt% Bionolle#3000 can significantly increase the toughness of PLA. BionolleRTM #3000 also reduces the physical aging rate of PLA so blends remain tough longer. Conversely, the stiffness of BionolleRTM #3000 can be significantly increased by blending in PLA. DMA and DSC results show that PLA/BionolleRTM 3000 blends are not thermodynamically miscible, but are compatible blends. Studies have also been performed to determine the amount and rate of aerobic biodegradation of PLA/aliphatic succinate polyester blends in biologically active composting, enzymatic, and soil environments. The changes in molecular weight, molecular structure and thermal properties in the composting environment were also studied by GPC, NMR and DSC analyses. The research results showed BionolleRTM #3000 had a high degradation rate, while PLA had a low degradation rate. PLA/BionolleRTM #3000 blends had moderate degradation rates that increased with BionolleRTM #3000 content. The melt flow behavior of PLA/BionolleRTM #3000 blends has been studied by capillary rheometry. The relationship of the blends' viscosity with their composition, shear stress, shear rate, and temperature has been investigated. Power law index and activation energy of PLA, BionolleRTM #3000 and their blends have been calculated. The experimental and theoretical data can let us understand the processability of PLA/BionolleRTM #3000 blends. A scanning electron microscope (SEM) was used to investigate the morphological structure of the PLA/BionolleRTM #3000 blends. Micrographs of the samples made from different methods (blown film, extrudate and compression molding sheet) were taken; their differences in morphology were compared. For comparison, the micrographs of blend PLA/BionolleRTM #6000 was also studied. The

Ethyl Carbamate Formation Regulated by Lactic Acid Bacteria and Nonconventional Yeasts in Solid-State Fermentation of Chinese Moutai-Flavor Liquor.

Science.gov (United States)

Du, Hai; Song, Zhewei; Xu, Yan

2018-01-10

This study aimed to identify specific microorganisms related to the formation of precursors of EC (ethyl carbamate) in the solid-state fermentation of Chinese Moutai-flavor liquor. The EC content was significantly correlated with the urea content during the fermentation process (R 2 = 0.772, P solid-state fermentation can be controlled using lactic acid bacteria and nonconventional yeasts.

Gallic Acid Production with Mouldy Polyurethane Particles Obtained from Solid State Culture of Aspergillus niger GH1.

Science.gov (United States)

Mata-Gómez, Marco; Mussatto, Solange I; Rodríguez, Raul; Teixeira, Jose A; Martinez, Jose L; Hernandez, Ayerim; Aguilar, Cristóbal N

2015-06-01

Gallic acid production in a batch bioreactor was evaluated using as catalytic material the mouldy polyurethane solids (MPS) obtained from a solid-state fermentation (SSF) bioprocess carried out for tannase production by Aspergillus niger GH1 on polyurethane foam powder (PUF) with 5 % (v/w) of tannic acid as inducer. Fungal biomass, tannic acid consumption and tannase production were kinetically monitored. SSF was stopped when tannase activity reached its maximum level. Effects of washing with distilled water and drying on the tannase activity of MPS were determined. Better results were obtained with dried and washed MPS retaining 84 % of the tannase activity. Maximum tannase activity produced through SSF after 24 h of incubation was equivalent to 130 U/gS with a specific activity of 36 U/mg. The methylgallate was hydrolysed (45 %) in an easy, cheap and fast bioprocess (30 min). Kinetic parameters of tannase self-immobilized on polyurethane particles were calculated to be 5 mM and 04.1 × 10(-2) mM/min for K M and V max, respectively. Results demonstrated that the MPS, with tannase activity, can be successfully used for the production of the antioxidant gallic acid from methyl-gallate substrate. Direct use of PMS to produce gallic acid can be advantageous as no previous extraction of enzyme is required, thus reducing production costs.

31P NMR Chemical Shifts of Phosphorus Probes as Reliable and Practical Acidity Scales for Solid and Liquid Catalysts.

Science.gov (United States)

Zheng, Anmin; Liu, Shang-Bin; Deng, Feng

2017-10-11

Acid-base catalytic reaction, either in heterogeneous or homogeneous systems, is one of the most important chemical reactions that has provoked a wide variety of industrial catalytic processes for production of chemicals and petrochemicals over the past few decades. In view of the fact that the catalytic performances (e.g., activity, selectivity, and reaction mechanism) of acid-catalyzed reactions over acidic catalysts are mostly dictated by detailed acidic features, viz. type (Brønsted vs Lewis acidity), amount (concentration), strength, and local environments (location) of acid sites, information on and manipulation of their structure-activity correlation are crucial for optimization of catalytic performances as well as innovative design of novel effective catalysts. This review aims to summarize recent developments on acidity characterization of solid and liquid catalysts by means of experimental 31 P nuclear magnetic resonance (NMR) spectroscopy using phosphorus probe molecules such as trialkylphosphine (TMP) and trialkylphosphine oxides (R 3 PO). In particular, correlations between the observed 31 P chemical shifts (δ 31 P) of phosphorus (P)-containing probes and acidic strengths have been established in conjuction with density functional theory (DFT) calculations, rendering practical and reliable acidity scales for Brønsted and Lewis acidities at the atomic level. As illustrated for a variety of different solid and liquid acid systems, such as microporous zeolites, mesoporous molecular sieves, and metal oxides, the 31 P NMR probe approaches were shown to provide important acid features of various catalysts, surpassing most conventional methods such as titration, pH measurement, Hammett acidity function, and some other commonly used physicochemical techniques, such as calorimetry, temperature-programmed desorption of ammonia (NH 3 -TPD), Fourier transformed infrared (FT-IR), and 1 H NMR spectroscopies.

Thermal decomposition of dimethoxymethane and dimethyl carbonate catalyzed by solid acids and bases

International Nuclear Information System (INIS)

Fu Yuchuan; Zhu Haiyan; Shen Jianyi

2005-01-01

The thermal decomposition of dimethoxymethane (DMM) and dimethyl carbonate (DMC) on MgO, H-ZSM-5, SiO 2 , γ-Al 2 O 3 and ZnO was studied using a fixed bed isothermal reactor equipped with an online gas chromatograph. It was found that DMM was stable on MgO at temperatures up to 623 K, while it was decomposed over the acidic H-ZSM-5 with 99% conversion at 423 K. On the other hand, DMC was easily decomposed on the strong solid base and acid. The conversion of DMC was 76% on MgO at 473 K, and 98% on H-ZSM-5 at 423 K. It was even easier decomposed on the amphoteric γ-Al 2 O 3 . Both DMM and DMC were relatively stable on SiO 2 possessing little surface acidity and basicity. They were even more stable on ZnO with the conversion of DMM and DMC of about 1.5% at 573 K. Thus, metal oxides with either strong acidity or basicity are not suitable for the selective oxidation of DMM to DMC, while ZnO may be used as a component for the reaction

The binary (solid + liquid) phase diagrams of (caprylic or capric acid) + (1-octanol or 1-decanol)

International Nuclear Information System (INIS)

Carareto, Natália D.D.; Castagnaro, Thamires; Costa, Mariana C.; Meirelles, Antonio J.A.

2014-01-01

Highlights: • SLE of mixtures of caprylic acid, (capric acid + 1-octanol), 1-decanol were studied. • Experimental data were obtained through DSC and Stepscan DSC. • Systems presented eutectic and peritectic points. • Liquidus line was modeled using Margules and NRTL models. • Solid phase was modeled using the Slaughter and Doherty approach. - Abstract: In the present study the phase diagrams of four (fatty acid + fatty alcohol) binary mixtures composed of caprylic (C8O2) or capric acid (C10O2) + 1-octanol (C8OH) or 1-decanol (C10OH) were obtained by differential scanning calorimetry (DSC). Eutectic and peritectic reactions occurred in the systems. In standard DSC analyses of the (C8O2 + C10OH) and (C10O2 + C8OH) systems, an exothermic transition occurs in association with the melting of a metastable phase. A Stepscan DSC method was used in order to avoid the formation of this metastable phase during the heating of the mixtures. The approach suggested by Slaughter and Doherty (1995) [24] was used for modeling the solid phase, and the Margules 2-suffix, Margules 3-suffix and NRTL models were applied for calculating the activity coefficients of the liquid phase. The best modeling results were obtained using the Margules-3-suffix with an average deviation between experimental and calculated values ranging from T = (0.3 to 0.9) K

Isoquercitrin Esters with Mono- or Dicarboxylic Acids: Enzymatic Preparation and Properties.

Science.gov (United States)

Vavříková, Eva; Langschwager, Fanny; Jezova-Kalachova, Lubica; Křenková, Alena; Mikulová, Barbora; Kuzma, Marek; Křen, Vladimír; Valentová, Kateřina

2016-06-07

A series of isoquercitrin (quercetin-3-O-β-d-glucopyranoside) esters with mono- or dicarboxylic acids was designed to modulate hydro- and lipophilicity and biological properties. Esterification of isoquercitrin was accomplished by direct chemoenzymatic reaction using Novozym 435 (lipase from Candida antarctica), which accepted C₅- to C12-dicarboxylic acids; the shorter ones, such as oxalic (C₂), malonic (C₃), succinic (C₄) and maleic (C₄) acids were not substrates of the lipase. Lipophilicity of monocarboxylic acid derivatives, measured as log P, increased with the chain length. Esters with glutaric and adipic acids exhibited hydrophilicity, and the dodecanedioic acid hemiester was more lipophilic. All derivatives were less able to reduce Folin-Ciocalteau reagent (FCR) and scavenge DPPH (1,1-diphenyl-2-picrylhydrazyl) than isoquercitrin; ABTS (2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid)) radical-scavenging activity was comparable. Dodecanoate and palmitate were the least active in FCR and ABTS scavenging; dodecanoate and hemiglutarate were the strongest DPPH scavengers. In contrast, most derivatives were much better inhibitors of microsomal lipoperoxidation than isoquercitrin; butyrate and hexanoate were the most efficient. Anti-lipoperoxidant activity of monocarboxylic derivatives, except acetates, decreased with increasing aliphatic chain. The opposite trend was noted for dicarboxylic acid hemiesters, isoquercitrin hemidodecanedioate being the most active. Overall, IQ butyrate, hexanoate and hemidodecanedioate are the most promising candidates for further studies.

Solid radiation curable polyene compositions containing liquid polythiols and solid styrene-allyl copolymer based polyenes

International Nuclear Information System (INIS)

Morgan, C.R.

1977-01-01

Novel styrene-allyl alcohol copolymer based solid polyene compositions which when mixed with liquid polythiols can form solid curable polyene-polythiol systems are claimed. These solid polyenes, containing at least two reactive carbon-to-carbon unsaturated bonds, are urethane or ester derivatives of styrene-allyl alcohol copolymers. The solid polyenes are prepared by treating the hydroxyl groups of a styrene-allyl alcohol copolymer with a reactive unsaturated isocyanate, e.g., allyl isocyanate or a reactive unsaturated carboxylic acid, e.g., acrylic acid. Upon exposure to a free radical generator, e.g., actinic radiation, the solid polyene-polythiol compositions cure to solid, insoluble, chemically resistant, cross-linked polythioether products. Since the solid polyene-liquid polythiol composition can be cured in a solid state, such a curable system finds particular use in preparation of coatings, imaged surfaces such as photoresists, particularly solder-resistant photoresists, printing plates, etc

High-efficiency removal of phytic acid in soy meal using two-stage temperature-induced Aspergillus oryzae solid-state fermentation.

Science.gov (United States)

Chen, Liyan; Vadlani, Praveen V; Madl, Ronald L

2014-01-15

Phytic acid of soy meal (SM) could influence protein and important mineral digestion of monogastric animals. Aspergillus oryzae (ATCC 9362) solid-state fermentation was applied to degrade phytic acid in SM. Two-stage temperature fermentation protocol was investigated to increase the degradation rate. The first stage was to maximize phytase production and the second stage was to realize the maximum enzymatic degradation. In the first stage, a combination of 41% moisture, a temperature of 37 °C and inoculum size of 1.7 mL in 5 g substrate (dry matter basis) favored maximum phytase production, yielding phytase activity of 58.7 U, optimized via central composite design. By the end of second-stage fermentation, 57% phytic acid was degraded from SM fermented at 50 °C, compared with 39% of that fermented at 37 °C. The nutritional profile of fermented SM was also studied. Oligosaccharides were totally removed after fermentation and 67% of total non-reducing polysaccharides were decreased. Protein content increased by 9.5%. Two-stage temperature protocol achieved better phytic acid degradation during A. oryzae solid state fermentation. The fermented SM has lower antinutritional factors (phytic acid, oligosaccharides and non-reducing polysaccharides) and higher nutritional value for animal feed. © 2013 Society of Chemical Industry.

Investigation on Polylactide (PLA)/Poly(butylene adipate-co-terephthalate) (PBAT)/Bark Flour of Plane Tree (PF) Eco-Composites

Science.gov (United States)

Dou, Qiang; Cai, Jun

2016-01-01

Polylactide (PLA)/poly(butylene adipate-co-terephthalate) (PBAT)/bark flour of plane tree (PF) eco-composites were prepared via melt blending. The morphologies, mechanical properties, crystal structures and melting and crystallization behaviors of the eco-composites were investigated by means of scanning electron microscopy (SEM), mechanical tests, polarized light microscopy (PLM), wide angle X-ray diffraction (WAXD) and differential scanning calorimetry (DSC), respectively. It is shown that the interfacial adhesion between PLA matrix and PF is weak and the mechanical properties of PLA/PF eco-composites are poor. The titanate treatment improves the adhesion between the matrix and the filler and enhances the stiffness of the eco-composites. The toughness is improved by PBAT and ductile fractured surfaces can be found. The spherulitic size of PLA is decreased by the addition of PF. The α crystalline form of PLA remains in the composites. Compared with PF, T-PF (PF treated by a titanate coupling agent) and PBAT have negative effects on the crystallization of PLA. PMID:28773515

Hollow nanoporous covalent triazine frameworks via acid vapor-assisted solid phase synthesis for enhanced visible light photoactivity

KAUST Repository

Huang, Wei

2016-04-11

Herein, we report a novel trifluoromethanesulfonic acid vapor-assisted solid phase synthetic method to construct nanoporous covalent triazine frameworks with highly ordered hollow interconnected pores under mild reaction conditions. This unique solid state synthetic route allows not only the avoidance of undesired side reactions caused by traditional high temperature synthesis, but also the maintaining of defined and precise optical and electronic properties of the nonporous triazine frameworks. Promising photocatalytic activity of the polytriazine networks was demonstrated in the photoreduction reaction of 4-nitrophenol into 4-aminophenol under visible light irradiation.

Hollow nanoporous covalent triazine frameworks via acid vapor-assisted solid phase synthesis for enhanced visible light photoactivity

KAUST Repository

Huang, Wei; Wang, Zi Jun; Ma, Beatriz Chiyin; Ghasimi, Saman; Gehrig, Dominik; Laquai, Fré dé ric; Landfester, Katharina; Zhang, Kai A. I.

2016-01-01

Herein, we report a novel trifluoromethanesulfonic acid vapor-assisted solid phase synthetic method to construct nanoporous covalent triazine frameworks with highly ordered hollow interconnected pores under mild reaction conditions. This unique solid state synthetic route allows not only the avoidance of undesired side reactions caused by traditional high temperature synthesis, but also the maintaining of defined and precise optical and electronic properties of the nonporous triazine frameworks. Promising photocatalytic activity of the polytriazine networks was demonstrated in the photoreduction reaction of 4-nitrophenol into 4-aminophenol under visible light irradiation.

Hydrolysis-acidogenesis of food waste in solid-liquid-separating continuous stirred tank reactor (SLS-CSTR) for volatile organic acid production.

Science.gov (United States)

Karthikeyan, Obulisamy Parthiba; Selvam, Ammaiyappan; Wong, Jonathan W C

2016-01-01

The use of conventional continuous stirred tank reactor (CSTR) can affect the methane (CH4) recovery in a two-stage anaerobic digestion of food waste (FW) due to carbon short circuiting in the hydrolysis-acidogenesis (Hy-Aci) stage. In this research, we have designed and tested a solid-liquid-separating CSTR (SLS-CSTR) for effective Hy-Aci of FW. The working conditions were pH 6 and 9 (SLS-CSTR-1 and -2, respectively); temperature-37°C; agitation-300rpm; and organic loading rate (OLR)-2gVSL(-1)day(-1). The volatile fatty acids (VFA), enzyme activities and bacterial population (by qPCR) were determined as test parameters. Results showed that the Hy-Aci of FW at pH 9 produced ∼35% excess VFA as compared to that at pH 6, with acetic and butyric acids as major precursors, which correlated with the high enzyme activities and low lactic acid bacteria. The design provided efficient solid-liquid separation there by improved the organic acid yields from FW. Copyright © 2015 Elsevier Ltd. All rights reserved.

Continuous cultivations of a Penicillium chrysogenum strain expressing the expandase gene from Streptomyces clavuligerus: Growth yields and morphological characterization

DEFF Research Database (Denmark)

Robin, Jarno Jacky Christian; Lettier, G.; Mcintyre, Mhairi

2003-01-01

and the mean total hyphal length and mean number of tips both increased with an increase in dilution rate from 0.015 to 0.065 h(-1). Both variables decreased when the dilution rate was increased above 0.065 h(-1). A correlation between mean total hyphal length and productivity of ad-7-ADCA was found....... it is fed with adipic acid. The biomass yield and maintenance coefficients for the strain were similar to those found for penicillin-producing strains of Penicillium chrysogenum. The maximum specific growth rate in the chemostat was found to be 0.11 h(-1). Metabolic degradation of adipate was found to take...... place in significant amounts only at dilution rates below 0.03 h(-1). After three to five residence times, adipate degradation and ad-7-ADCA production disappeared, and this allowed determination of the biomass yield coefficient on adipate. The morphology was measured at different dilution rates...

Molecular and Supramolecular Changes in Polybutylene Succinate (PBS and Polybutylene Succinate Adipate (PBSA Copolymer during Degradation in Various Environmental Conditions

Directory of Open Access Journals (Sweden)

Michał Puchalski

2018-03-01

Full Text Available In this paper, the influence of the various degradation conditions, on the molecular and supramolecular structure of polybutylene succinate (PBS and polybutylene succinate adipate (PBSA copolymer during degradation is described. The experiment was carried out by the use of injection molded samples and normalized conditions of biodegradation in soil, composting and artificial weathering. Materials were studied by size-exclusion chromatography (SEC coupled with multiangle laser light scattering (MALLS detection and wide-angle X-ray diffraction (WAXD. Additionally, the physical and mechanical properties of the samples were determined. The performed experiments clearly show difference impacts of the selected degradation conditions on the macroscopic, supramolecular and molecular parameters of the studied aliphatic polyesters. The structural changes in PBS and PBSA explain the observed changes in the physical and mechanical properties of the obtained injection molded samples.

Solid state fermentation studies of citric acid production

African Journals Online (AJOL)

SERVER

2008-03-04

Mar 4, 2008 ... solid waste management, biomass energy conservation, production of high value products and little risk ... The carrier, sugarcane bagasse for solid state fermentation was procured from National Sugar Institute ... constant weight and designated as dry solid residue (DSR). The filtrate (consisting of biomass, ...

Regulated and unregulated emissions from a diesel engine fueled with diesel fuel blended with diethyl adipate

Science.gov (United States)

Zhu, Ruijun; Cheung, C. S.; Huang, Zuohua; Wang, Xibin

2011-04-01

Experiments were carried out on a four-cylinder direct-injection diesel engine operating on Euro V diesel fuel blended with diethyl adipate (DEA). The blended fuels contain 8.1%, 16.4%, 25% and 33.8% by volume fraction of DEA, corresponding to 3%, 6%, 9% and 12% by mass of oxygen in the blends. The engine performance and exhaust gas emissions of the different fuels were investigated at five engine loads at a steady speed of 1800 rev/min. The results indicated an increase of brake specific fuel consumption and brake thermal efficiency when the engine was fueled with the blended fuels. In comparison with diesel fuel, the blended fuels resulted in an increase in hydrocarbon (HC) and carbon monoxide (CO), but a decrease in particulate mass concentrations. The nitrogen oxides (NO x) emission experienced a slight variation among the test fuels. In regard to the unregulated gaseous emissions, formaldehyde and acetaldehyde increased, while 1,3-butadiene, ethene, ethyne, propylene and BTX (benzene, toluene and xylene) in general decreased. A diesel oxidation catalyst (DOC) was found to reduce significantly most of the investigated unregulated pollutants when the exhaust gas temperature was sufficiently high.

Antiandrogenic effects in male rats perinatally exposed to a mixture of di(2-ethylhexyl) phthalate and di(2-ethylhexyl) adipate

DEFF Research Database (Denmark)

Jarfelt, K.; Dalgaard, M.; Hass, Ulla

2005-01-01

Di(2-ethylhexyl) phthalate (DEHP) is a well-known testicular toxicant inducing adverse effects in androgen responsive tissues. Therefore, di(2-ethylhexyl) adipate (DERA) is currently being evaluated as a potential substitute for DEHP. Similarities in structure and metabolism of DERP and DEHA have...... in the reproductive system than males receiving DERP alone. (c) 2004 Elsevier Inc. All rights reserved.......) and retention of nipples in male offspring were found in all three exposed groups. Dosed males exhibited decreased weights of ventral prostate and m. levator ani/bulbocavernosus. Histopathological investigations revealed alterations in testis morphology in both juvenile and adult animals. The litter size...... was decreased and postnatal mortality was increased in the combination group only, which is likely a combined effect of DEHP and DEHA. However, no combination effect was seen with respect to antiandrogenic effects, as males receiving DEHP in combination with DEHA did not exhibit more pronounced effects...

Solid phosphoric acid oligomerisation: Manipulating diesel selectivity by controlling catalyst hydration

International Nuclear Information System (INIS)

Prinsloo, Nicolaas M.

2006-01-01

Solid phosphoric acid (SPA) catalyst is traditionally used in crude oil refineries to produce unhydrogenated motor-gasoline by propene and butene oligomerisation. SPA is also used in High-Temperature Fischer-Tropsch refineries (HTFT) to produce synthetic fuels albeit with a different emphasis. The petrol/diesel ratio of an HTFT refinery is very different from crude refining and it is often necessary to shift this ratio depending on market requirements. The influence of hydration was investigated as a means of improving diesel selectivity. This was achieved by studying SPA over a hydration range of 99-110% H 3 PO 4 , a temperature range of 140-230 o C and using C 3 -C 6 model and synthetic FT-derived olefinic feedstocks. A direct correlation was found between the selectivity towards diesel range products and the distribution of the phosphoric acid species viz. H 3 PO 4 , H 4 P 2 O 7 and H 5 P 3 O 10 . For various olefinic feedstocks, diesel selectivity increased with decreasing catalyst hydration with a maximum around 108% H 3 PO 4 for propene oligomerisation. Commercial tests confirmed the increase in diesel selectivity with lowered catalyst hydration. (author)

Quantitative analysis of copolymers : influence of the structure of the monomer on the ionization efficiency in electrospray ionization FTMS

NARCIS (Netherlands)

Koster, S.; Mulder, B.; Duursma, M.C.; Boon, J.J.; Philipsen, H.J.A.; Velde, J.W.; Nielen, M.W.F.; Koster, de C.G.; Heeren, R.M.A.

2002-01-01

The influence of the ionization efficiency on the measured copolymer sequence distribution is presented. Large differences in ionization efficiency were observed for mixtures of homopolyesters containing dipropoxylated bisphenol A/adipic acid and dipropoxylated bisphenol A/isophthalic acid and the

Acidizing reservoirs while chelating iron with sulfosalicylic acid

Energy Technology Data Exchange (ETDEWEB)

McLaughlin, W A; Berkshire, D C

1980-09-30

A well treating process is described in which an aqueous solution of a strong acid capable of dissolving solids in a manner increasing the permeability of a subterranean earth formation is injected into a subterranean reservoir that contains an asphaltenic oil. At least the first injected portion of the aqueous acid and a solution or homogeneous dispersion of at least enough 5-sulfosalicylic acid to chelate with and prevent the formation of iron-asphaltene solids are included with substantially all of the ferric ions that become dissolved within the strong acid solution that enters the earth formation. 10 claims.

Saponification of esters of chiral alpha-amino acids anchored through their amine function on solid support.

Science.gov (United States)

Cantel, Sonia; Desgranges, Stéphane; Martinez, Jean; Fehrentz, Jean-Alain

2004-06-01

Anchoring an alpha-amino acid residue by its amine function onto a solid support is an alternative to develop chemistry on its carboxylic function. This strategy can involve the use of amino-acid esters as precursors of the carboxylic function. A complete study on the Wang-resin was performed to determine the non racemizing saponification conditions of anchored alpha-amino esters. The use of LiOH, NaOH, NaOSi(Me)3, various solvents and temperatures were tested for this reaction. After saponification and cleavage from the support, samples were examined through their Marfey's derivatives by reversed phase HPLC to evaluate the percentage of racemization.

The quantitative monitoring of mechanochemical reaction between solid L-tartaric acid and sodium carbonate monohydrate by terahertz spectroscopy

Science.gov (United States)

Liu, Xiaohong; Liu, Guifeng; Zhao, Hongwei; Zhang, Zengyang; Wei, Yongbo; Liu, Min; Wen, Wen; Zhou, Xingtai

2011-11-01

The solid-state reaction of chiral tartaric acid and alkali carbonate was studied by terahertz time-domain spectroscopy (THz-TDS). The sodium tartrate dihydrate was synthesized with high efficiency by mechanical grinding in the solid-state without waste that is particularly sustainable and environmentally benign. Distinct THz absorptions were observed for reactants and products. It indicates that THz spectroscopy is sensitive to different materials and crystal structures. The characteristic THz absorption peak at 1.09 THz of L (+)-Tartaric acid was selected for quantitative analysis. The reaction kinetics could be expressed by the Second-order equation and the Jander equation, which is consistent with a three-dimensional diffusion mechanism. The combination of multi-techniques including synchrotron radiation X-ray powder diffraction (SRXRPD), Fourier transform infrared (FT-IR) and scanning electron microscopy (SEM) was used to investigate the grinding process and presented supporting evidences. The results demonstrate that THz spectroscopy technique has great potential applications in process monitoring and analysis in pharmaceutical and chemical synthesis industry.

Determination of haloacetic acids in water using layered double hydroxides as a sorbent in dispersive solid-phase extraction followed by liquid chromatography with tandem mass spectrometry.

Science.gov (United States)

Alsharaa, Abdulnaser; Sajid, Muhammad; Basheer, Chanbasha; Alhooshani, Khalid; Lee, Hian Kee

2016-09-01

In the present study, highly efficient and simple dispersive solid-phase extraction procedure for the determination of haloacetic acids in water samples has been established. Three different types of layered double hydroxides were synthesized and used as a sorbent in dispersive solid-phase extraction. Due to the interesting behavior of layered double hydroxides in an acidic medium (pH˂4), the analyte elution step was not needed; the layered double hydroxides are simply dissolved in acid immediately after extraction to release the analytes which are then directly introduced into a liquid chromatography with tandem mass spectrometry system for analysis. Several dispersive solid-phase extraction parameters were optimized to increase the extraction efficiency of haloacetic acids such as temperature, extraction time and pH. Under optimum conditions, good linearity was achieved over the concentration range of 0.05-100 μg/L with detection limits in the range of 0.006-0.05 μg/L. The relative standard deviations were 0.33-3.64% (n = 6). The proposed method was applied to different water samples collected from a drinking water plant to determine the concentrations of haloacetic acids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Poly(ether amide) segmented block copolymers with adipicacid based tetra amide segments

NARCIS (Netherlands)

Biemond, G.J.E.; Feijen, Jan; Gaymans, R.J.

2007-01-01

Poly(tetramethylene oxide)-based poly(ether ester amide)s with monodisperse tetraamide segments were synthesized. The tetraamide segment was based on adipic acid, terephthalic acid, and hexamethylenediamine. The synthesis method of the copolymers and the influence of the tetraamide concentration,

Treatment of acid mine drainage with anaerobic solid-substrate reactors

Energy Technology Data Exchange (ETDEWEB)

Drury, W.J.

1999-10-01

Anaerobic solid-substrate reactors were used in a laboratory study of acid mine drainage treatment. Parallel systems were run continuously for 23 months, both containing a solid substrate of 2:1 (weight) cow manure and sawdust. One system had cheese whey added with the mine drainage to provide an additional electron donor source to simulate sulfate-reducing bacteria activity. Effluent pH from the reactor with whey addition was relatively constant at 6.5. Effluent pH from the reactor without whey addition dropped over time from 6.7 to approximately 5.5. Whey addition increased effluent alkalinity [550 to 700 mg/L as calcium carbonate (CaCO{sub 3}) versus 50 to 300 mg/L as CaCO{sub 3}] and sulfate removal (98 to 80% versus 60 to 40%). Sulfate removal rate with whey addition decreased over time from 250 to 120 mmol/m{sup 3}{center{underscore}dot}d, whereas it decreased from 250 to 40 mmol/m{sup 3}{center{underscore}dot}d without whey addition. Whey addition increased removal of dissolved iron, dissolved manganese, and dissolved zinc in the second part of the experiment. Copper and cadmium removals were greater than 99%, and arsenic removal was 84% without whey addition and 89% with whey addition. Effluent sulfide concentrations were approximately 1 order of magnitude greater with whey addition. A 63-day period of excessive loading permanently decreased treatment efficiency without whey addition.

UTILIZATION OF PINE NEEDLES AS BED MATERIAL IN SOLID STATE FERMENTATION FOR PRODUCTION OF LACTIC ACID BY LACTOBACILLUS STRAINS

Directory of Open Access Journals (Sweden)

Manoj Kumar Ghosh

Full Text Available Pine needles, which are abundantly found as underexploited biomass in coniferous forests, are responsible for fire hazards and air pollution. Utilization of pine needles as bed material in lactic acid production with solid state fermentation (SSF has been studied here. This investigation compared lactic acid production by pure strains of Lactobacilli, (1 L. delbrueckii (NCIM2025; (2 L. pentosus (NCIM 2912; (3 Lactobacillus sp. (NCIM 2734; (4 Lactobacillus sp. (NCIM2084; and a co-culture of the first two strains. The studies required 6 g per flask powdered dry pine needles as bed material, 2 g/L (inoculum, liquid production media based on pure glucose or whey substituted glucose, at 60, 80, and 120 g/L sugar levels, 37 oC, and an initial pH of 6.5. Co-culture attained a maximum lactic acid concentration of 45.10 g/L, followed by that of strain-1, 43.87 g/L and strain-4, 26.15 g/L, in 80 g/L pure glucose media. With 120g/L total sugar in whey-substituted media, the co-culture attained maximum lactic acid production of 44.88 g/L followed by that of strain-1, 43.67 g/L. The present experimental studies indicated better compatibility of pine needle bed with co-culture in solid state fermentation of lactic acid, which may prove to be an eco-friendly technology for utilization of biomass as well as minimizing fires in coniferous forests.

Isolation and surface modification of cellulose nanocrystals from sugarcane bagasse waste: From a micro- to a nano-scale view

Science.gov (United States)

Ferreira, F. V.; Mariano, M.; Rabelo, S. C.; Gouveia, R. F.; Lona, L. M. F.

2018-04-01

This work presents the isolation and functionalization of cellulose nanocrystals (CNCs) extracted from sugarcane bagasse (SCB). CNCs were obtained by acid hydrolysis of bleached bagasse pulp and functionalized with adipic acid. The results showed that unmodified CNCs exhibit both a high crystallinity index and a significant aspect ratio. Surface modification with adipic acid decreases the nanocrystal dimensions due to removal of the amorphous region between the crystalline domains and also changes the electrostatic repulsion and hydrophilic affinity of CNCs. Unmodified CNCs offer potential applications as reinforcing phase in hydrophilic polymeric matrices, while modified CNCs interact better with hydrophobic matrices. The use of CNCs as reinforcement in polymer nanocomposites expands the application of this renewable material and increases its added value, providing nonenergy-based markets for the main biomass of the sugarcane industry.

PdRu alloy nanoparticles of solid solution in atomic scale: outperformance towards formic acid electro-oxidation in acidic medium

International Nuclear Information System (INIS)

Miao, Kanghua; Luo, Yun; Zou, Jiasui; Yang, Jun; Zhang, Fengqi; Huang, Lin; Huang, Jie; Kang, Xiongwu; Chen, Shaowei

2017-01-01

Developing catalyst of high performance and low cost toward the electro-oxidation of formic acid on the anode of fuel cell is critical for the commercialization of direct formic acid fuel cells. Here we reported the synthesis of Pd x Ru 10-x (x = 1,3,5,7,9) nanoparticles (NPs) by concurrent reduction of Pd 2+ and Ru 2+ in polyol solution at 200 °C. The particle size of the obtained NPs was confined at 5–15 nm in diameter. X-ray diffraction (XRD) analysis revealed face-centered cubic (fcc) crystal structure for Pd x Ru 10-x (x = 3,5,7,9), with the lattice parameter proportional to the Pd content. The formation of the solid solution in atomic scale was confirmed for the alloy nanoparticles by XRD and the elemental mapping. Williamson-Hall method revealed that the stacking fault was dependent on the alloying extent of the alloy nanoparticles and reached the minimum for Pd 5 Ru 5 , which exhibited the highest activity towards formic acid oxidation among all these prepared samples, with mass activity of 12.6 times higher than that of commercial Pd/C. It was observed that the highest catalytic activity was in agreement with the minimum of the stacking fault of the alloy nanoparticles.

Production of itaconic acid by Ustilago maydis from agro wastes in solid state fermentation

Directory of Open Access Journals (Sweden)

MOKULA MD. RAFI

2014-08-01

Full Text Available Itaconic acid (IA is one of the hopeful substances within the cluster of organic acids. IA is used in artificial glass, bioactive compounds in pharmacy, medicine, agriculture, for the synthesis of fiber, resin, plastic, rubber, paints, surfactant, ion-exchange resins and lubricant. Most recurrently used microorganism for commercial production of IA is Aspergillus terreus. Some filamentous fungi belonging to Ustilaginales also produce IA. In the present work, an attempt was made to produce IA by Ustilago maydis employing Solid State Fermentation (SSF from various agro wastes like ground nut shells, rice bran, rice husk, orange pulp, ground nut oil cake, orange pulp and sugarcane bagasse as carbon substrates, which were used after pretreatment. 10 g of each substrate was taken in a 500 ml conical flasks separately and supplemented with 20 mL nutrient solution containing glucose, at pH 3. One milliliter inoculum containing 1×107 spores was added and moisture was maintained at 60%. After incubation at 32°C for 5 days, the acid production was estimated by spectrophotometric method and by HPLC analysis. Interestingly, the yield of itaconic acid was promising with all the above substrates, where orange pulp, sugarcane bagasse and rice bran supported higher yields.

Rheological Behavior, Granule Size Distribution and Differential Scanning Calorimetry of Cross-Linked Banana (Musa paradisiaca) Starch.

Science.gov (United States)

Núñez-Santiago, María C.; Maristany-Cáceres, Amira J.; Suárez, Francisco J. García; Bello-Pérez, Arturo

2008-07-01

Rheological behavior at 60 °C, granule size distribution and Differential Scanning Calorimetry (DSC) tests were employed to study the effect of diverse reaction conditions: adipic acid concentration, pH and temperature during cross-linking of banana (Musa paradisiaca) starch. These properties were determined in native banana starch pastes for the purpose of comparison. Rheological behavior from pastes of cross-linked starch at 60 °C did not show hysteresis, probably due the cross-linkage of starch that avoided disruption of granules, elsewhere, native starch showed hysteresis in a thixotropic loop. All pastes exhibited non-Newtonian shear thinning behavior. In all cases, size distribution showed a decrease in the median diameter in cross-linked starches. This condition produces a decrease in swelling capacity of cross-linked starch. The median diameter decreased with an increase of acid adipic concentration; however, an increase of pH and Temperature produced an increase in this variable. Finally, an increase in gelatinization temperature and entalphy (ΔH) were observed as an effect of cross-linkage. An increase in acid adipic concentration produced an increase in Tonset and a decrease in ΔH. pH and temperature. The cross-linked of banana starch produced granules more resistant during the pasting procedure.

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...

Co-production of bio-ethanol, xylonic acid and slow-release nitrogen fertilizer from low-cost straw pulping solid residue.

Science.gov (United States)

Huang, Chen; Ragauskas, Arthur J; Wu, Xinxing; Huang, Yang; Zhou, Xuelian; He, Juan; Huang, Caoxing; Lai, Chenhuan; Li, Xin; Yong, Qiang

2018-02-01

A novel bio-refinery sequence yielding varieties of co-products was developed using straw pulping solid residue. This process utilizes neutral sulfite pretreatment which under optimal conditions (160 °C and 3% (w/v) sulfite charge) provides 64.3% delignification while retaining 90% of cellulose and 67.3% of xylan. The pretreated solids exhibited excellent enzymatic digestibility, with saccharification yields of 86.9% and 81.1% for cellulose and xylan, respectively. After pretreatment, the process of semi-simultaneous saccharification and fermentation (S-SSF) and bio-catalysis was investigated. The results revealed that decreased ethanol yields were achieved when solid loading increased from 5% to 30%. An acceptable ethanol yield of 76.8% was obtained at 20% solid loading. After fermentation, bio-catalysis of xylose remaining in fermentation broth resulted in near 100% xylonic acid (XA) yield at varied solid loadings. To complete the co-product portfolio, oxidation ammoniation of the dissolved lignin successfully transformed it into biodegradable slow-release nitrogen fertilizer with excellent agricultural properties. Copyright © 2017 Elsevier Ltd. All rights reserved.

BIOREMEDIATION FOR ACID MINE DRAINAGE: ORGANIC SOLID WASTE AS CARBON SOURCES FOR SULFATE-REDUCING BACTERIA: A REVIEW

Directory of Open Access Journals (Sweden)

I. N. Jamil

2013-12-01

Full Text Available Biological sulfate reduction has been slowly replacing chemical unit processes to treat acid mine drainage (AMD. Bioremediations for AMD treatment are favored due to their low capital and maintenance cost. This paper describes the available AMD treatment, current SRB commercialization such as THIOPAQ® and BioSulphide® technologies, and also the factors and limitations faced. THIOPAQ® and BioSulphide® technologies use expensive carbon sources such as hydrogen as the electron donor. This paper discusses the possibility of organic solid waste as an alternative substrate as it is cheaper and abundant. A possible AMD treatment system setup was also proposed to test the efficiency of sulfate-reducing bacteria utilizing organic solid substrate.

Comparing peracetic acid and hypochlorite for disinfection of combined sewer overflows: Effects of suspended-solids and pH.

Science.gov (United States)

McFadden, M; Loconsole, J; Schockling, A J; Nerenberg, R; Pavissich, J P

2017-12-01

Peracetic acid (PAA) is an alternative disinfectant that may be effective for combined sewer overflow (CSO) disinfection, but little is known about the effect of particle size on PAA disinfection efficiency. In this work, PAA and hypochlorite were compared as disinfectants, with a focus on the effect of wastewater particles. Inactivation experiments were conducted on suspended cultures of Escherichia coli and wastewater suspended solids. Tested size fractions included particle diameters disinfection efficiency decreased with increasing solids size. However, solids size had little effect on PAA disinfection. The PAA disinfection efficiency decreased at pH values above 7.5. Live/dead staining revealed that PAA disinfection leaves most cells in a viable but non-culturable condition. Fourier transform infrared spectroscopy (FTIR) analyses suggests that PAA and hypochlorite may inactivate E. coli bacteria by similar mechanisms. Copyright © 2017 Elsevier B.V. All rights reserved.

Method of melting solid waste

International Nuclear Information System (INIS)

Ootsuka, Katsuyuki; Mizuno, Ryokichi; Kuwana, Katsumi; Sawada, Yoshihisa; Komatsu, Fumiaki.

1982-01-01

Purpose: To enable the volume reduction treatment of a HEPA filter containing various solid wastes, particularly acid digestion residue, or an asbestos separator at a relatively low temperature range. Method: Solid waste to be heated and molten is high melting point material treated by ''acid digestion treatment'' for treating solid waste, e.g. a HEPA filter or polyvinyl chloride, etc. of an atomic power facility treated with nitric acid or the like. When this material is heated and molten by an electric furnace, microwave melting furnace, etc., boron oxide, sodium boride, sodium carbonate, etc. is added as a melting point lowering agent. When it is molten in this state, its melting point is lowered, and it becomes remarkably fluid, and the melting treatment is facilitated. Solidified material thus obtained through the melting step has excellent denseness and further large volume reduction rate of the solidified material. (Yoshihara, H.)

Paper-based solid-phase nucleic acid hybridization assay using immobilized quantum dots as donors in fluorescence resonance energy transfer.

Science.gov (United States)

Noor, M Omair; Shahmuradyan, Anna; Krull, Ulrich J

2013-02-05

A paper-based solid-phase assay is presented for transduction of nucleic acid hybridization using immobilized quantum dots (QDs) as donors in fluorescence resonance energy transfer (FRET). The surface of paper was modified with imidazole groups to immobilize QD-probe oligonucleotide conjugates that were assembled in solution. Green-emitting QDs (gQDs) were FRET-paired with Cy3 acceptor. Hybridization of Cy3-labeled oligonucleotide targets provided the proximity required for FRET-sensitized emission from Cy3, which served as an analytical signal. The assay exhibited rapid transduction of nucleic acid hybridization within minutes. Without any amplification steps, the limit of detection of the assay was found to be 300 fmol with the upper limit of the dynamic range at 5 pmol. The implementation of glutathione-coated QDs for the development of nucleic acid hybridization assay integrated on a paper-based platform exhibited excellent resistance to nonspecific adsorption of oligonucleotides and showed no reduction in the performance of the assay in the presence of large quantities of noncomplementary DNA. The selectivity of nucleic acid hybridization was demonstrated by single-nucleotide polymorphism (SNP) detection at a contrast ratio of 19 to 1. The reuse of paper over multiple cycles of hybridization and dehybridization was possible, with less than 20% reduction in the performance of the assay in five cycles. This work provides an important framework for the development of paper-based solid-phase QD-FRET nucleic acid hybridization assays that make use of a ratiometric approach for detection and analysis.

Precise Measurement of Refractive Index and Absorption Coefficient of Near Millimeter Wave and Far Infrared Materials.

Science.gov (United States)

1987-06-01

polyethylene. The plexiglass is a polymethyl methacrylate and the acrylic is a polymethacrylate . The polyamide(nylon) is made with adipic acid and hexamethylene...are made with acrylic acid . It was not sur- prizing to see both exhibiting similar absorption characteristics atleast 30 times higher than

Selective synthesis of thioethers in the presence of a transition-metal-free solid Lewis acid

Directory of Open Access Journals (Sweden)

Federica Santoro

2016-12-01

Full Text Available The synthesis of thioethers starting from alcohols and thiols in the presence of amorphous solid acid catalysts is reported. A silica alumina catalyst with a very low content in alumina gave excellent results in terms of both activity and selectivity also under solvent-free conditions. The reaction rate follows the electron density of the carbinol atom in the substrate alcohol and yields up to 99% and can be obtained for a wide range of substrates under mild reaction conditions.

Synthesis and Characterization of Tin (IV Tungstate Nanoparticles – A Solid Acid Catalyst

Directory of Open Access Journals (Sweden)

Manoj Sadanandan

2012-12-01

Full Text Available Tin (IV tungstate, a tetravalent metal acid salt was synthesized in the nanoform by chemical coprecipitation method using EDTA as capping agent. The material was found to be stable in mineral acids, bases and organic solvents except  in HF and aquaregia. The material was characterized using EDS, TG/DTA, FTIR, XRD, SEM, HRTEM and BET surface area measurement. The molecular formula of the compound is 2SnO2 3WO3.5H2O determined from elemental analysis using TG/DTA. Surface morphology and particle size were obtained using SEM and HRTEM. The surface area was found to be 205-225m2/g. The Na+ exchange capacity found to be 3.8 meq/g, indicates the presence of surface hydroxyl group and hence the presence of Bronsted acid sites. The catalytic activity of the material was tested by using esterification and oxidation as model reactions. For the esterification of different alcohols, the percentage yield was found to be high for n-alcohol compared to isomeric alcohols. Oxidation of benzyl alcohol gives benzaldehyde and benzoic acid as the only products. Copyright © 2012 by BCREC UNDIP. All rights reservedReceived: 12nd June 2012, Revised: 23rd July 2012, Accepted: 29th July 2012[How to Cite: S. Manoj, R. Beena, (2012. Synthesis and Characterization of tin(IV Tungstate Nanoparticles – A Solid Acid Catalyst. Bulletin of Chemical Reaction Engineering & Catalysis, 7 (2: 105-111. doi:10.9767/bcrec.7.2.3622.105-111] [How to Link / DOI: http://dx.doi.org/10.9767/bcrec.7.2.3622.105-111 ] | View in 

78 FR 10583 - Approval and Promulgation of Air Quality Implementation Plans; Massachusetts; Reasonably...

Science.gov (United States)

2013-02-14

...-Density Polyethylene, Polypropylene and Polystyrene Resins; 7. Natural Gas/Gasoline Process Leaks; 8... adipic acid plants; cement plants; and iron and steel manufacturing facilities. Major NO X sources do...

Nature of the activates places of the acid solid catalysts of the sulphated metallic oxides type

International Nuclear Information System (INIS)

Gomez, Miguel A; Fontalvo Javier

1998-01-01

In this revision the state of the knowledge is presented with respect to the understanding of the nature of the active places for the strongly acid solid catalysts of the type sulphated metallic oxides. The results presented by means of models are based on the characterization of the properties physicochemical carried out by means of technical as XPS, to GO, NMR etc., and the evaluation of the catalytic activity in different applications

Solid emulsion gel as a vehicle for delivery of polyunsaturated fatty acids: implications for tissue repair, dermal angiogenesis and wound healing.

Science.gov (United States)

Shingel, Kirill I; Faure, Marie-Pierre; Azoulay, Laurent; Roberge, Christophe; Deckelbaum, Richard J

2008-10-01

The paper describes preparation and biological characterization of the solid hybrid biomaterial that was designed for cell-targeted lipid delivery in healing tissues. The material referred to as 'solid emulsion gel' combines a protein-stabilized lipid emulsion and a hydrogel structure in a single compartment. The potential of the omega-3 (n-3)-fatty acids rich solid emulsion gel for tissue repair applications was investigated at the macro-, micro-, molecular and gene expression levels, using human fibroblasts and endothelial cells and a porcine model of full-thickness wounds. Being non-cytotoxic in vitro and in vivo, the biomaterial was found to affect cell metabolism, modulate expression of certain genes, stimulate early angiogenesis and promote wound repair in vivo. The neovascular response in vivo was correlated with upregulated expression of the genes involved in lipid transport (e.g. adipophilin), anti-apoptosis (e.g. heat shock proteins, haem oxygenase 1) and angiogenesis (vascular endothelial growth factor, placental growth factor). Collectively, the results of this study provide first evidence that the angiogenic response provided by solid emulsion gel-mediated delivery of n-3 fatty acids is an alternative to the topical administration of exogenous growth factors or gene therapy, and can be advantageously used for the stimulation of tissue repair in complex wounds. Copyright (c) 2008 John Wiley & Sons, Ltd.

Characterization of Carbamazepine-Loaded Solid Lipid ...

African Journals Online (AJOL)

loaded solid lipid nanoparticles by RESS as well as their characterization has been achieved in this study. Keywords: Rapid expansion of supercritical fluid, Stearic acid, Solid lipid nanoparticles, Carbamazepine, Co-precipitation ...

Methyl vinyl glycolate as a diverse platform molecule

DEFF Research Database (Denmark)

Sølvhøj, Amanda Birgitte; Taarning, Esben; Madsen, Robert

2016-01-01

and various long-chain terminal olefins give unsaturated α-hydroxy fatty acid methyl esters in good yields. [3,3]-Sigmatropic rearrangements of MVG also proceed in good yields to give unsaturated adipic acid derivatives. Finally, rearrangement of the allylic acetate of MVG proceeds in acceptable yield...

Isotopic study on mechanism for skeletal isomerization of n-butane over solid acids

International Nuclear Information System (INIS)

Suzuki, Tetsuo; Okuhara, Toshio

2000-01-01

Reaction mechanism for skeletal isomerization of n-butane over typical strong solid acids were investigated by using 1,4- 13 C 2 -n-butane. We used FI MASS for the analysis of 13 C distribution to get the parent pattern. 13 C-distribution of isobutane formed at 423 K over SO 3 2- /ZrO 2 (SZ) and Cs 2.5 H 0.5 PW 12 O 40 (Cs2.5) were close to binomial distributions, indicating that the isomerization proceeded mainly via a bimolecular mechanism on these catalysts. On the other hand, at 523 K over Cs2.5, the isotopic distribution pattern in isobutane was quite different from the binomial one; the fraction of 13 C 2 -isobutane was much greater than the binomial distribution. This result demonstrates that an intramolecular (monomolecular) rearrangement became significant at 523 K over Cs2.5. The contribution of monomolecular pathway was higher on Cs2.5 than on SZ. We presumed that the contribution of mechanism is related to the acidic property and the dehydrogenation ability of the catalyst. (S.Y.)

Improvement of medium chain fatty acid content and antimicrobial activity of coconut oil via solid-state fermentation using a Malaysian Geotrichum candidum.

Science.gov (United States)

Khoramnia, Anahita; Ebrahimpour, Afshin; Ghanbari, Raheleh; Ajdari, Zahra; Lai, Oi-Ming

2013-01-01

Coconut oil is a rich source of beneficial medium chain fatty acids (MCFAs) particularly lauric acid. In this study, the oil was modified into a value-added product using direct modification of substrate through fermentation (DIMOSFER) method. A coconut-based and coconut-oil-added solid-state cultivation using a Malaysian lipolytic Geotrichum candidum was used to convert the coconut oil into MCFAs-rich oil. Chemical characteristics of the modified coconut oils (MCOs) considering total medium chain glyceride esters were compared to those of the normal coconut oil using ELSD-RP-HPLC. Optimum amount of coconut oil hydrolysis was achieved at 29% moisture content and 10.14% oil content after 9 days of incubation, where the quantitative amounts of the modified coconut oil and MCFA were 0.330 mL/g of solid media (76.5% bioconversion) and 0.175 mL/g of solid media (53% of the MCO), respectively. MCOs demonstrated improved antibacterial activity mostly due to the presence of free lauric acid. The highest MCFAs-rich coconut oil revealed as much as 90% and 80% antibacterial activities against Staphylococcus aureus and Escherichia coli, respectively. The results of the study showed that DIMOSFER by a local lipolytic G. candidum can be used to produce MCFAs as natural, effective, and safe antimicrobial agent. The produced MCOs and MCFAs could be further applied in food and pharmaceutical industries.

Prototype demonstration of dual sorbent injection for acid gas control on municipal solid waste combustion units

Energy Technology Data Exchange (ETDEWEB)

None

1994-05-01

This report gathered and evaluated emissions and operations data associated with furnace injection of dry hydrated lime and duct injection of dry sodium bicarbonate at a commercial, 1500 ton per day, waste-to-energy facility. The information compiled during the project sheds light on these sorbents to affect acid gas emissions from municipal solid waste combustors. The information assesses the capability of these systems to meet the 1990 Clean Air Act and 1991 EPA Emission Guidelines.

Preparation of a Carbon-Based Solid Acid Catalyst by Sulfonating Activated Carbon in a Chemical Reduction Process

Directory of Open Access Journals (Sweden)

Xiao-Yan Liu

2010-10-01

Full Text Available Sulfonated (SO3H-bearing activated carbon (AC-SO3H was synthesized by an aryl diazonium salt reduction process. The obtained material had a SO3H density of 0.64 mmol·g-1 and a specific surface area of 602 m2·g-1. The catalytic properties of AC-SO3H were compared with that of two commercial solid acid catalysts, Nafion NR50 and Amberlyst-15. In a 10-h esterification reaction of acetic acid with ethanol, the acid conversion with AC-SO3H (78% was lower than that of Amberlyst-15 (86%, which could be attributed to the fact that the SO3H density of the sulfonated carbon was lower than that of Amberlyst-15 (4.60 mmol·g-1. However, AC-SO3H exhibited comparable and even much higher catalytic activities than the commercial catalysts in the esterification of aliphatic acids with longer carbon chains such as hexanoic acid and decanoic acid, which may be due to the large specific surface area and mesoporous structures of the activated carbon. The disadvantage of AC-SO3H is the leaching of SO3H group during the reactions.

Ethanol production from residual wood chips of cellulose industry: acid pretreatment investigation, hemicellulosic hydrolysate fermentation, and remaining solid fraction fermentation by SSF process.

Science.gov (United States)

Silva, Neumara Luci Conceição; Betancur, Gabriel Jaime Vargas; Vasquez, Mariana Peñuela; Gomes, Edelvio de Barros; Pereira, Nei

2011-04-01

Current research indicates the ethanol fuel production from lignocellulosic materials, such as residual wood chips from the cellulose industry, as new emerging technology. This work aimed at evaluating the ethanol production from hemicellulose of eucalyptus chips by diluted acid pretreatment and the subsequent fermentation of the generated hydrolysate by a flocculating strain of Pichia stipitis. The remaining solid fraction generated after pretreatment was subjected to enzymatic hydrolysis, which was carried out simultaneously with glucose fermentation [saccharification and fermentation (SSF) process] using a strain of Saccharomyces cerevisiae. The acid pretreatment was evaluated using a central composite design for sulfuric acid concentration (1.0-4.0 v/v) and solid to liquid ratio (1:2-1:4, grams to milliliter) as independent variables. A maximum xylose concentration of 50 g/L was obtained in the hemicellulosic hydrolysate. The fermentation of hemicellulosic hydrolysate and the SSF process were performed in bioreactors and the final ethanol concentrations of 15.3 g/L and 28.7 g/L were obtained, respectively.

21 CFR 177.1500 - Nylon resins.

Science.gov (United States)

2010-04-01

... condensation of hexamethyl-enediamine, adipic acid, and terephthalic acid such that composition in terms of...), isophthalic acid (CAS Reg. No. 0121-91-5), and bis(4-amino-3-methylcycl-ohexyl)methane (CAS Reg. No. 6864-37-5) such that the composition in terms of ingredients is 34.4±1.5 weight percent omega-laurolactam, 26.8±0...

Influence of the microwave technology on solid dispersions of mefenamic acid and flufenamic acid.

Directory of Open Access Journals (Sweden)

Sultan Alshehri

Full Text Available The present studies were undertaken to develop solvent-free solid dispersions (SDs for poorly soluble anti-inflammatory drugs mefenamic acid (MA and flufenamic acid (FFA in order to enhance their in vitro dissolution rate and in vivo anti-inflammatory effects. The SDs of MA and FFA were prepared using microwaves irradiation (MW technique. Different carriers such as Pluronic F127® (PL, Eudragit EPO® (EPO, polyethylene glycol 4000 (PEG 4000 and Gelucire 50/13 (GLU were used for the preparation of SDs. Prepared MW irradiated SDs were characterized physicochemically using differential scanning calorimetry (DSC, thermogravimetric analysis (TGA, Fourier transform infra-red (FT-IR spectroscopy, powder X-ray diffraction (PXRD and scanning electron microscopy (SEM. The physicochemical characteristics and drug release profile of SDs were compared with pure drugs. The results of DSC, TGA, FT-IR, PXRD and SEM showed that SDs were successfully prepared. In vitro dissolution rate of MA and FFA was remarkably enhanced by SDs in comparison with pure MA and FFA. The SDs of MA and FFA prepared using PEG 400 showed higher drug release profile in comparison with those prepared using PL, EPO or GLU. The dissolution efficiency for MA-PEG SD and FFA-PEG SD was obtained as 61.40 and 59.18%, respectively. Optimized SDs were also evaluated for in vivo anti-inflammatory effects in male Wistar rats. The results showed significant % inhibition by MA-PEG (87.74% after 4 h and FFA-PEG SDs (81.76% after 4 h in comparison with pure MA (68.09% after 4 h and pure FFA (55.27% after 4 h (P<0.05. These results suggested that MW irradiated SDs of MA and FFA could be successfully used for the enhancement of in vitro dissolution rate and in vivo therapeutic efficacy of both drugs.

76 FR 64055 - Special Rules Governing Certain Information Obtained Under the Clean Air Act: Technical Correction

Science.gov (United States)

2011-10-17

... Production......... 325199 Adipic acid manufacturing facilities. Aluminum Production 331312 Primary Aluminum production facilities. Ammonia Manufacturing 325311 Anhydrous and aqueous ammonia manufacturing facilities. Cement Production 327310 Portland Cement manufacturing plants. Electronics Manufacturing...... 334111...

Fabrication and thermal stability studies of polyamide 66 containing ...

Indian Academy of Sciences (India)

Administrator

by two-step polymerization reaction with adipic acid hexamethylene salt (AH salt) and bis(4-carboxyphenyl) .... polymerization autoclave (Weihai-controlled reactor Ltd,. WHF-2) equipped ... After melt polymerization, the molten copolymer was.

Presidential Green Chemistry Challenge: 1998 Academic Award (Draths and Frost)

Science.gov (United States)

Presidential Green Chemistry Challenge 1998 award winners, Dr. Karen M. Draths and Professor John W. Frost, used benign, genetically engineered microbes and sugars (instead of benzene) to synthesize adipic acid and catechol.

Uranium (IV) carboxylates - I

Energy Technology Data Exchange (ETDEWEB)

Satpathy, K C; Patnaik, A K [Sambalpur Univ. (India). Dept. of Chemistry

1975-11-01

A few uranium(IV) carboxylates with monochloro and trichloro acetic acid, glycine, malic, citric, adipic, o-toluic, anthranilic and salicylic acids have been prepared by photolytic methods. The I.R. spectra of these compounds are recorded and basing on the spectral data, structure of the compounds have been suggested.

Direct solid surface fluorescence spectroscopy of standard chemicals and humic acid in ternary system.

Science.gov (United States)

Mounier, S; Nicolodelli, G; Redon, R; Milori, D M B P

2017-04-15

The front face fluorescence spectroscopy is often used to quantify chemicals in well-known matrices as it is a rapid and powerful technique, with no sample preparation. However it was not used to investigate extracted organic matter like humic substances. This work aims to fully investigate for the first time front face fluorescence spectroscopy response of a ternary system including boric acid, tryptophan and humic substances, and two binaries system containing quinine sulfate or humic substance in boric acid. Pure chemicals, boric acid, tryptophan, quinine sulfate and humic acid were mixed together in solid pellet at different contents from 0 to 100% in mass. The measurement of excitation emission matrix of fluorescence (3D fluorescence) and laser induced fluorescence were then done in the front face mode. Fluorescence matrices were decomposed using the CP/PARAFAC tools after scattering treatments. Results show that for 3D fluorescence there is no specific component for tryptophan and quinine sulfate, and that humic substances lead to a strong extinction effect for mixture containing quinine sulfate. Laser induced fluorescence gives a very good but non-specific related response for both quinine sulfate and tryptophan. No humic substances fluorescence response was found, but extinction effect is observed as for 3D fluorescence. This effect is stronger for quinine sulfate than for tryptophan. These responses were modeled using a simple absorbance versus emission model. Copyright © 2017 Elsevier B.V. All rights reserved.

Successive Recovery of Copper and Uranium From Carbonate-Rich Latosol, Um Bogma Formation, Abuthor Locality, South Western Sinai, Egypt

International Nuclear Information System (INIS)

El-Sheikh, E.M.; Amin, M.M.; Aita, S.K.; Rezk, A.A.

2013-01-01

A technological sample of a copper/ uranium mineralization in carbonate rich latosol rock sequence of Urn Bogma Formation Abu Thor locality at southwestern Sinai, Egypt, has been properly processed. The working sample assaying 12.5 % CuO and 875 ppm U was subjected to adipic acid leaching for copper followed by bioleaching of uranium in a manner to avoid excessive acid consumption in the classical leaching procedure. It is thus possible to achieve leaching efficiencies of 95% for Cu in the first stage and 82% for U in the second stage. From the two separately obtained leach liquors of Cu and uranium, pure products have conveniently been prepared. Accordingly, Cu adipate product was first prepared by crystallization,followed by acid dissolution and alkali precipitation of copper hydroxide. In case of uranium, the impure precipitate of the bioleach liquor is purified via Amberlite IRA-400 anion exchanger resin

Solid-phase extraction versus matrix solid-phase dispersion: Application to white grapes.

Science.gov (United States)

Dopico-García, M S; Valentão, P; Jagodziñska, A; Klepczyñska, J; Guerra, L; Andrade, P B; Seabra, R M

2007-11-15

The use of matrix solid-phase dispersion (MSPD) was tested to, separately, extract phenolic compounds and organic acids from white grapes. This method was compared with a more conventional analytical method previously developed that combines solid liquid extraction (SL) to simultaneously extract phenolic compounds and organic acids followed by a solid-phase extraction (SPE) to separate the two types of compounds. Although the results were qualitatively similar for both techniques, the levels of extracted compounds were in general quite lower on using MSPD, especially for organic acids. Therefore, SL-SPE method was preferred to analyse white "Vinho Verde" grapes. Twenty samples of 10 different varieties (Alvarinho, Avesso, Asal-Branco, Batoca, Douradinha, Esganoso de Castelo Paiva, Loureiro, Pedernã, Rabigato and Trajadura) from four different locations in Minho (Portugal) were analysed in order to study the effects of variety and origin on the profile of the above mentioned compounds. Principal component analysis (PCA) was applied separately to establish the main sources of variability present in the data sets for phenolic compounds, organic acids and for the global data. PCA of phenolic compounds accounted for the highest variability (77.9%) with two PCs, enabling characterization of the varieties of samples according to their higher content in flavonol derivatives or epicatechin. Additionally, a strong effect of sample origin was observed. Stepwise linear discriminant analysis (SLDA) was used for differentiation of grapes according to the origin and variety, resulting in a correct classification of 100 and 70%, respectively.

Uranium recovery from wet-process phosphoric acid

International Nuclear Information System (INIS)

McCullough, J.F.; Phillips, J.F. Jr.; Tate, L.R.

1979-01-01

A method of recovering uranium from wet-process phosphoric acid is claimed where the acid is treated with a mixture of an ammonium salt or ammonia, a reducing agent, and then a miscible solvent. Solids are separated from the phosphoric acid liquid phase. The solid consists of a mixture of metal phosphates and uranium. It is washed free of adhering phosphoric acid with fresh miscible solvent. The solid is dried and dissolved in acid whereupon uranium is recovered from the solution. Miscible solvent and water are distilled away from the phosphoric acid. The distillate is rectified and water discarded. All miscible solvent is recovered for recycle. 5 claims

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

Headspace solid-phase microextraction with 1-pyrenyldiazomethane on-fibre derivatisation for analysis of fluoroacetic acid in biological samples.

Science.gov (United States)

Sporkert, Frank; Pragst, Fritz; Hübner, Sandra; Mills, Graham

2002-05-25

A new and in part automated headspace solid-phase microextraction method for quantitative determination of the highly toxic rodenticide fluoroacetic acid (FAA) in serum and other biological samples has been developed. FAA and deuterated acetic acid (internal standard) were extracted from acidified samples by a StableFlex divinylbenzene-Carboxen on polydimethylsiloxane fibre. The acids were derivatised on the fibre in-situ with 1-pyrenyldiazomethane and detected using gas chromatography-mass spectrometry with electron impact ionisation and selected ion monitoring. The calibration curve for FAA in serum was linear over the range from 0.02 to 5 microg/ml, with limits of detection and quantification of 0.02 and 0.07 microg/ml, respectively. The method was also tested with spiked whole blood, urine, stomach contents and kidney samples. It was sufficiently reliable, reproducible and sensitive for use in routine forensic toxicology applications.

Co-Production of Nattokinase and Poly (γ-Glutamic Acid Under Solid-State Fermentation Using Soybean and Rice Husk

Directory of Open Access Journals (Sweden)

Guangjun Nie

2015-10-01

Full Text Available ABSTRACTThe aim of this work was to study the co-production of nattokinase and poly (γ-glutamic acid by Bacillus subtilis natto with soybean and rice husk under solid-state fermentation (SSF. The results showed that the size of soybean particle and rice husk significantly improved the co-production of nattokinase and poly (γ-glutamic acid, yielding 2503.4 IU/gs and 320 mg/gs, respectively in the improved culture medium composed of 16.7% soybean flour and 13.3% rice husk with 70% water content. The yields increased by approximate 7- and 2-fold factor relative to their original ones. Thus, the co-production of nattokinase and poly (γ-glutamic acid under SSF could be considered as an efficient method to exploit agro-residues for economical production of some higher-value products.

Improvement of Medium Chain Fatty Acid Content and Antimicrobial Activity of Coconut Oil via Solid-State Fermentation Using a Malaysian Geotrichum candidum

Directory of Open Access Journals (Sweden)

Anahita Khoramnia

2013-01-01

Full Text Available Coconut oil is a rich source of beneficial medium chain fatty acids (MCFAs particularly lauric acid. In this study, the oil was modified into a value-added product using direct modification of substrate through fermentation (DIMOSFER method. A coconut-based and coconut-oil-added solid-state cultivation using a Malaysian lipolytic Geotrichum candidum was used to convert the coconut oil into MCFAs-rich oil. Chemical characteristics of the modified coconut oils (MCOs considering total medium chain glyceride esters were compared to those of the normal coconut oil using ELSD-RP-HPLC. Optimum amount of coconut oil hydrolysis was achieved at 29% moisture content and 10.14% oil content after 9 days of incubation, where the quantitative amounts of the modified coconut oil and MCFA were 0.330 mL/g of solid media (76.5% bioconversion and 0.175 mL/g of solid media (53% of the MCO, respectively. MCOs demonstrated improved antibacterial activity mostly due to the presence of free lauric acid. The highest MCFAs-rich coconut oil revealed as much as 90% and 80% antibacterial activities against Staphylococcus aureus and Escherichia coli, respectively. The results of the study showed that DIMOSFER by a local lipolytic G. candidum can be used to produce MCFAs as natural, effective, and safe antimicrobial agent. The produced MCOs and MCFAs could be further applied in food and pharmaceutical industries.

Citric acid production by solid-state fermentation on a semi-pilot scale using different percentages of treated cassava bagasse

Directory of Open Access Journals (Sweden)

F. C. Prado

2005-12-01

Full Text Available Citric acid is commercailly important product used in several industrial processes. Solid-state fermentation (SSF has become an alternative method for citric acid production using agro-industrial residues such as cassava bagasse (CB. Use of CB as substrate can avoid the environmental problems caused by its disposal in the environment. The aim of this work was to verify the effect of different percentages of gelatinized starch in CB on production of citric acid by SSF in horizontal drum and tray-type bioreactors. Gelatinization was used in order to make the starch structure more susceptible to consumption by the fungus. The best results (26.9 g/100g of dry CB were obtained in horizontal drum bioreactor using 100% gelatinized CB, although the tray-type bioreactor offers advantages and shows promise for large-scale citric acid production in terms of processing costs.

New Micro-Method for Prediction of Vapor Pressure of Energetic Materials

Science.gov (United States)

2014-07-01

Sigma Aldrich (for calorimetric determination) Adipic acid Mettler certified thermometric standard Anthraquinone Mettler certified thermometric standard...Naphthalene Mettler certified thermometric standard Caffeine Arthur R Thomas Co thermometric standard Acetanilide Arthur R Thomas Co thermometric

Solid Obtained by Electrocoagulation of Vinasse, new Inhibitor for Acid Corrosion of Brass

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Elaine Ojeda-Armaignac

2016-07-01

Full Text Available This work is part of research related to obtaining a corrosion inhibitor from vinasse, whose basic advantages is the possibility of using an industrial waste from distilleries ethyl alcohol as raw material in the production of a solid corrosion inhibitor of national production by electrocoagulation, which implies import substitution and cost reductions. The inhibitory action of the solids obtained by electrocoagulation of vinasse was investigated by potentiodynamic polarization techniques and electrochemical impedance spectroscopy. It was found that the efficiencies of inhibition against the brass into the electrolyte solution were very good, behaving as an efficient inhibitor in acid medium. Inhibition efficiency increases with increasing concentration. The maximum inhibition efficiency was of 93,43 % for the concentration of 2 mg / L of vinasse. Thermodynamic parameters were obtained at the study temperature. It was found that the adsorption of inhibitor molecules on the surface of brass obey the Langmuir isotherm, and the values of adsorción free energy of - 23.06 kJ mol-1 show the spontaneity of adsorption and indicate that the inhibitor is strongly adsorbed on the surface of brass, study of potentiodynamic polarization curves confirmed that it is a mixed type inhibitor, with an anode predominance and there is a predominant mechanism of physical adsorption combined with a chemisorption.

Solid state fermentation with lactic acid bacteria to improve the nutritional quality of lupin and soya bean.

Science.gov (United States)

Bartkiene, Elena; Krungleviciute, Vita; Juodeikiene, Grazina; Vidmantiene, Daiva; Maknickiene, Zita

2015-04-01

The ability of bacteriocin-like inhibitory substance (BLIS)-producing lactic acid bacteria (LAB) to degrade biogenic amines as well as to produce L(+) and D(-)-lactic acid during solid state fermentation (SSF) of lupin and soya bean was investigated. In addition, the protein digestibility and formation of organic acids during SSF of legume were investigated. Protein digestibility of fermented lupin and soya bean was found higher on average by 18.3% and 15.9%, respectively, compared to untreated samples. Tested LAB produced mainly L-lactic acid in soya bean and lupin (D/L ratio 0.38-0.42 and 0.35-0.54, respectively), while spontaneous fermentation gave almost equal amounts of both lactic acid isomers (D/L ratio 0.82-0.98 and 0.92, respectively). Tested LAB strains were able to degrade phenylethylamine, spermine and spermidine, whereas they were able to produce putrescine, histamine and tyramine. SSF improved lupin and soya bean protein digestibility. BLIS-producing LAB in lupin and soya bean medium produced a mixture of D- and L-lactic acid with a major excess of the latter isomer. Most toxic histamine and tyramine in fermented lupin and soya bean were found at levels lower those causing adverse health effects. Selection of biogenic amines non-producing bacteria is essential in the food industry to avoid the risk of amine formation. © 2014 Society of Chemical Industry.

SOLIDS PRECIPITATION EVENT IN MCU CAUSAL ANALYSIS AND RECOMMENDATIONS FROM SOLIDS RECOVERY TEAM

Energy Technology Data Exchange (ETDEWEB)

Garrison, A.; Aponte, C.

2014-08-15

A process upset occurred in the Modular Caustic-Side Solvent Extraction Unit (MCU) facility on April 6th, 2014. During recovery efforts, a significant amount of solids were found in the Salt Solution Feed Tank (SSFT), Salt Solution Receipt Tanks (SSRTs), two extraction contactors, and scrub contactors. The solids were identified by Savannah River National Laboratory (SRNL) as primarily sodium oxalate and sodium alumina silicate (NAS) with the presence of some aluminum hydroxide. NAS solids have been present in the SSFT since simulant runs during cold chemical startup of MCU in 2007, and have not hindered operations since that time. During the process upset in April 2014, the oxalate solids partially blocked the aqueous outlet of the extraction contactors, causing salt solution to exit through the contactor organic outlet to the scrub contactors with the organic phase. This salt solution overwhelmed the scrub contactors and passed with the organic phase to the strip section of MCU. The partially reversed flow of salt solution resulted in a Strip Effluent (SE) stream that was high in Isopar™ L, pH and sodium. The primary cause of the excessive solids accumulation in the SSRTs and SSFT at MCU is attributed to an increase in the frequency of oxalic acid cleaning of the 512-S primary filter. Agitation in the SSRTs at MCU in response to cold weather likely provided the primary mechanism to transfer the solids to the contactors. Sources of the sodium oxalate solids are attributed to the oxalic acid cleaning solution used to clean the primary filter at the Actinide Removal Process (ARP) filtration at 512-S, as well as precipitation from the salt batch feed, which is at or near oxalate saturation. The Solids Recovery Team was formed to determine the cause of the solids formation and develop recommendations to prevent or mitigate this event in the future. A total of 53 recommendations were generated. These recommendations were organized into 4 focus areas: • Improve

Poly(lactic acid (PLA Based Tear Resistant and Biodegradable Flexible Films by Blown Film Extrusion

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Norma Mallegni

2018-01-01

Full Text Available Poly(lactic acid (PLA was melt mixed in a laboratory extruder with poly(butylene adipate-co-terephthalate (PBAT and poly(butylene succinate (PBS in the presence of polypropylene glycol di glycidyl ether (EJ400 that acted as both plasticizer and compatibilizer. The process was then scaled up in a semi-industrial extruder preparing pellets having different content of a nucleating agent (LAK. All of the formulations could be processed by blowing extrusion and the obtained films showed mechanical properties dependent on the LAK content. In particular the tearing strength showed a maximum like trend in the investigated composition range. The films prepared with both kinds of blends showed a tensile strength in the range 12–24 MPa, an elongation at break in the range 150–260% and a significant crystallinity.

Sterochemical consequences of hydrogen exchange as a result of tritium atom reactions on solid aliphatic amino acids

International Nuclear Information System (INIS)

Ehrenkaufer, R.L.E.; Hembree, W.C.; Lieberman, S.; Wolf, A.P.

1977-01-01

The products of stereochemistry resulting from radicals generated by the interaction of tritium atoms with L-isoleucine and L-alloisoleucine in the solid phase were determined. Among the four possible tritiated stereoisomers for each amino acid the major product was the parent L-amino acid (approximately 70 percent in each case) with the major fraction of the labeling being in positions other than the α position. Approximately 30 percent of the labeling resulted in the diastereomeric product by reaction at either the α or β position, with the major pathway being β-inversion. The yield of products from α-carbon attack of L-isoleucine was minor (7.9 percent) and occurred with net retention. Labeling at the α-carbon of alloisoleucine was less than 1 percent. Tritiated glycine was formed from both amino acids by cleavage of the alkyl side chain. This may result from the excitation decomposition of the intermediates formed from recombination of α (or β) amino acid radicals with tritium. Determination of the stereochemical and chemical consequences of radical formation at chiral centers provides a sensitive probe for studying the consequences of tritium (hydrogen or deuterium) atom reactions

Contacting particulate solids with liquids

International Nuclear Information System (INIS)

Hodgson, T.D.

1980-01-01

Apparatus is described for contacting particulate solids with a fluid. The particular applications described are 1) an acid dissolver for dissolving plutonium from plutonium contaminated ash produced by the incineration of waste such as rubber gloves, tissue paper etc. and 2) apparatus for dissolving gel spheres of nuclear fuel material. The liquid, e.g. acid for use in a leaching process flows through a vertical conduit and past a series of baffles spaced along the axis of the conduit. Each baffle defines a mixing chamber and provides a small gap around its perimeter between the baffle and the wall of the conduit. The baffles are provided with sloping top surfaces for preventing solid particles from settling on the baffles and sloping undersurfaces to improve mixing of the liquid and the solid particles. The liquid flows upwards in the conduit but solid particles may be fed from the top or from the bottom of the conduit to mix with the liquid. Gas may be introduced to promote improved flow conditions. (U.K.)

Synthesis of 1,2-Disubstituted Benzimidazoles in the Presence of SBA-Pr-SO3H as a Nano Solid Acid Catalyst

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G. Mohammadi Ziarani

2012-06-01

Full Text Available In this article, simple, convenient synthesis of 2-aryl-1- arylmethyl-1H-1,3-benzimidazole (1,2-disubstituted benzimidazoles via condensation of 1,2-phenylenediamine and aromatic aldehydes using SBA-Pr-SO3H as a nanoporous solid acid catalyst in green protocol was reported.

Well acidizing

Energy Technology Data Exchange (ETDEWEB)

Street, E H

1980-01-23

The apparatus relates in particular to a well-treating process in which an aqueous acid solution having a pH of < 2 is injected into a subterranean reservoir in a manner such that materials that contain ferric ions are present in the acid and, as the acid reacts within the reservoir and attains a pH exceeding 3, tend to be precipitated as ferric ion-containing solid materials that may plug the pores of the reservoir. Such a precipitation is prevented by dissolving in the acid solution an amount of 5-sulfosalicylic acid which is at least sufficient to sequester significant proportions of ferric ions when the pH of the acid is from 0.5 to 3 but is less than enough to cause a significant salting-out of solid materials, and an amount of citric acid which is at least sufficient to sequester significant proportions of ferric ions when the pH of the acid is from 3 to 6 but is less than enough to precipitate a significant amount of calcium citrate. The amount of the 5-sulfosalicylic acid may be from 0.01 to 0.05 moles/l and the amount of citric acid is from 0.001 to 0.009 moles/l. 11 claims.

Solid phase syntheses of oligoureas

Energy Technology Data Exchange (ETDEWEB)

Burgess, K.; Linthicum, D.S.; Russell, D.H.; Shin, H.; Shitangkoon, A.; Totani, R.; Zhang, A.J.; Ibarzo, J. [Texas A& M Univ., College Station, TX (United States)

1997-02-19

Isocyanates 7 were formed from monoprotected diamines 3 or 6, which in turn can be easily prepared from commercially available N-BOC- or N-FMOC-protected amino acid derivatives. Isocyanates 7, formed in situ, could be coupled directly to a solid support functionalized with amine groups or to amino acids anchored on resins using CH{sub 2}Cl{sub 2} as solvent and an 11 h coupling time at 25 {degree}C. Such couplings afforded peptidomimetics with an N-phthaloyl group at the N-terminus. The optimal conditions identified for removal of the N-phthaloyl group were to use 60% hydrazine in DMF for 1-3 h. Several sequences of amino acids coupled to ureas (`peptidic ureas`) and of sequential urea units (`oligoureas`) were prepared via solid phase syntheses and isolated by HPLC. Partition coefficients were measured for two of these peptidomimetics, and their water solubilities were found to be similar to the corresponding peptides. A small library of 160 analogues of the YGGFL-amide sequence was prepared via Houghten`s tea bag methodology. This library was tested for binding to the anti-{beta}-endorphin monoclonal antibody. Overall, this paper describes methodology for solid phase syntheses of oligourea derivatives with side chains corresponding to some of the protein amino acids. The chemistry involved is ideal for high-throughput syntheses and screening operations. 51 refs., 3 figs., 2 tabs.

A comparison study of rhodamine B photodegradation over nitrogen-doped lamellar niobic acid and titanic acid under visible-light irradiation.

Science.gov (United States)

Li, Xiukai; Kikugawa, Naoki; Ye, Jinhua

2009-01-01

A solid-state reaction method with urea as a nitrogen precursor was used to prepare nitrogen-doped lamellar niobic and titanic solid acids (i.e., HNb(3)O(8) and H(2)Ti(4)O(9)) with different acidities for visible-light photocatalysis. The photocatalytic activities of the nitrogen-doped solid acids were evaluated for rhodamine B (RhB) degradation and the results were compared with those obtained over the corresponding nitrogen-doped potassium salts. Techniques such as XRD, BET, SEM, X-ray photoelectron spectroscopy, and UV-visible diffuse reflectance spectroscopy were adopted to explore the nature of the materials as well as the characteristics of the doped nitrogen species. It was found that the intercalation of the urea precursor helped to stabilize the layered structures of both lamellar solid acids and enabled easier nitrogen doping. The effects of urea intercalation were more significant for the more acidic HNb(3)O(8) sample than for the less acidic H(2)Ti(4)O(9). Compared with the nitrogen-doped KNb(3)O(8) and K(2)Ti(4)O(9) samples, the nitrogen-doped HNb(3)O(8) and H(2)Ti(4)O(9) solid acids absorb more visible light and exhibit a superior activity for RhB photodegradation under visible-light irradiation. The nitrogen-doped HNb(3)O(8) sample performed the best among all the samples. The results of the current study suggest that the protonic acidity of the lamellar solid-acid sample is a key factor that influences nitrogen doping and the resultant visible-light photocatalysis.

Catalysis of a Nanometre Solid Super Acid of SO42-/TiO2 on the Thermal Decomposition of Ammonium Nitrate

OpenAIRE

Song, Xiaolan; Wang, Yi; Song, Dan; An, Chongwei; Wang, Jingyu

2016-01-01

Raw TiO2 nanoparticles were prepared using the hydroly‐ sis of TiCl4. The nanoparticles were subjected to a surface treatment in diluted sulphuric acid and, subsequently, calcined at different temperatures. Then, a type of super solid acid (SO42-/TiO2) with particle sizes of 20∼30 nm was fabricated. The catalysis of SO42-/TiO2 on the thermolysis of ammonium nitrate (AN) was probed using thermal analysis. For SO42-/TiO2 (AN doped with 3%SO42-/TiO2), the onset temperature decreased by 19°C and ...

Investigation of Di-ethylhexyl Phthalate Migration by Applying Magnetic Solid Phase Extraction Method Followed by GC-FID Determination

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Mohammad Faraji

2016-10-01

Full Text Available Background and Objectives: The addition of plasticizers (mainly phthalates and adipates makes plastic flexible and popular for packaging, storing and preserving food, water, and so on. The most widely used plasticizer in food contact applications is di-ethylhexyl phthalate (DEHP though being suspected to have carcinogenic and estrogenic properties. The aim of this study is application of magnetic solid phase extraction as new absorbent for determination of DEHP in water samples by gas chromatography (GC. Materials and Methods: Important factors in extraction, separation and determination processes were optimized using the one-variable-at-a-time method. For optimization, all tests were performed two times. Figures of merit of the proposed method were evaluated. The amount of DEHP in some water samples was determined using the proposed method. Results: The results showed that the obtained chromatogram of extract was free of significant interference. The preservatives’ recoveries ranged from 91.6% to 102.2%. Limit of detection and limit of quantitation were 0.1 mg kg-1 and 0.3 µg L-1, respectively. Concentration of DEHP in the studied samples was in the range of N.D-2.3 µg L-1. Conclusions: The acceptable performance and reliability of the proposed method were demonstrated. Temperature and time were fount as the most effective parameters in migration of DEHP. Keywords: Di-ethylhexyl phthalate, Magnetic solid phase extraction, Migration, Gas chromatography

Transport of Eu3+ through a Bis(2-ethylhexyl)-phosphoric acid, n-dodecane solid supported liquid membrane

International Nuclear Information System (INIS)

Danesi, P.R.; Horwitz, E.P.; Rickert, P.

1982-01-01

The coupled transpot of Eu 3 + and H + ions througn a solid supported liquid membrane consisting of a porous polypropylene film immobilizing an HDEHP solution in n-dodecane has been studied as a function of the membrane area, stirring speed of the aqueous solutions, membrane composition, and acidity of the feed solution. The experimental results are in agreement with predictions derived from a theoretical permeability coefficient equation which assumes that membrane diffusion and aqueous film diffusion are the only rate-controlling factors

Removing hydrochloric acid exhaust products from high performance solid rocket propellant using aluminum-lithium alloy

Energy Technology Data Exchange (ETDEWEB)

Terry, Brandon C., E-mail: terry13@purdue.edu [School of Aeronautics and Astronautics, Purdue University, Zucrow Laboratories, 500 Allison Rd, West Lafayette, IN 47907 (United States); Sippel, Travis R. [Department of Mechanical Engineering, Iowa State University, 2025 Black Engineering, Ames, IA 50011 (United States); Pfeil, Mark A. [School of Aeronautics and Astronautics, Purdue University, Zucrow Laboratories, 500 Allison Rd, West Lafayette, IN 47907 (United States); Gunduz, I.Emre; Son, Steven F. [School of Mechanical Engineering, Purdue University, Zucrow Laboratories, 500 Allison Rd, West Lafayette, IN 47907 (United States)

2016-11-05

Highlights: • Al-Li alloy propellant has increased ideal specific impulse over neat aluminum. • Al-Li alloy propellant has a near complete reduction in HCl acid formation. • Reduction in HCl was verified with wet bomb experiments and DSC/TGA-MS/FTIR. - Abstract: Hydrochloric acid (HCl) pollution from perchlorate based propellants is well known for both launch site contamination, as well as the possible ozone layer depletion effects. Past efforts in developing environmentally cleaner solid propellants by scavenging the chlorine ion have focused on replacing a portion of the chorine-containing oxidant (i.e., ammonium perchlorate) with an alkali metal nitrate. The alkali metal (e.g., Li or Na) in the nitrate reacts with the chlorine ion to form an alkali metal chloride (i.e., a salt instead of HCl). While this technique can potentially reduce HCl formation, it also results in reduced ideal specific impulse (I{sub SP}). Here, we show using thermochemical calculations that using aluminum-lithium (Al-Li) alloy can reduce HCl formation by more than 95% (with lithium contents ≥15 mass%) and increase the ideal I{sub SP} by ∼7 s compared to neat aluminum (using 80/20 mass% Al-Li alloy). Two solid propellants were formulated using 80/20 Al-Li alloy or neat aluminum as fuel additives. The halide scavenging effect of Al-Li propellants was verified using wet bomb combustion experiments (75.5 ± 4.8% reduction in pH, ∝ [HCl], when compared to neat aluminum). Additionally, no measurable HCl evolution was detected using differential scanning calorimetry coupled with thermogravimetric analysis, mass spectrometry, and Fourier transform infrared absorption.

Removing hydrochloric acid exhaust products from high performance solid rocket propellant using aluminum-lithium alloy

International Nuclear Information System (INIS)

Terry, Brandon C.; Sippel, Travis R.; Pfeil, Mark A.; Gunduz, I.Emre; Son, Steven F.

2016-01-01

Highlights: • Al-Li alloy propellant has increased ideal specific impulse over neat aluminum. • Al-Li alloy propellant has a near complete reduction in HCl acid formation. • Reduction in HCl was verified with wet bomb experiments and DSC/TGA-MS/FTIR. - Abstract: Hydrochloric acid (HCl) pollution from perchlorate based propellants is well known for both launch site contamination, as well as the possible ozone layer depletion effects. Past efforts in developing environmentally cleaner solid propellants by scavenging the chlorine ion have focused on replacing a portion of the chorine-containing oxidant (i.e., ammonium perchlorate) with an alkali metal nitrate. The alkali metal (e.g., Li or Na) in the nitrate reacts with the chlorine ion to form an alkali metal chloride (i.e., a salt instead of HCl). While this technique can potentially reduce HCl formation, it also results in reduced ideal specific impulse (I_S_P). Here, we show using thermochemical calculations that using aluminum-lithium (Al-Li) alloy can reduce HCl formation by more than 95% (with lithium contents ≥15 mass%) and increase the ideal I_S_P by ∼7 s compared to neat aluminum (using 80/20 mass% Al-Li alloy). Two solid propellants were formulated using 80/20 Al-Li alloy or neat aluminum as fuel additives. The halide scavenging effect of Al-Li propellants was verified using wet bomb combustion experiments (75.5 ± 4.8% reduction in pH, ∝ [HCl], when compared to neat aluminum). Additionally, no measurable HCl evolution was detected using differential scanning calorimetry coupled with thermogravimetric analysis, mass spectrometry, and Fourier transform infrared absorption.

Immobilization of metal-humic acid complexes in anaerobic granular sludge for their application as solid-phase redox mediators in the biotransformation of iopromide in UASB reactors.

Science.gov (United States)

Cruz-Zavala, Aracely S; Pat-Espadas, Aurora M; Rangel-Mendez, J Rene; Chazaro-Ruiz, Luis F; Ascacio-Valdes, Juan A; Aguilar, Cristobal N; Cervantes, Francisco J

2016-05-01

Metal-humic acid complexes were synthesized and immobilized by a granulation process in anaerobic sludge for their application as solid-phase redox mediators (RM) in the biotransformation of iopromide. Characterization of Ca- and Fe-humic acid complexes revealed electron accepting capacities of 0.472 and 0.556milli-equivalentsg(-1), respectively. Once immobilized, metal-humic acid complexes significantly increased the biotransformation of iopromide in upflow anaerobic sludge blanket (UASB) reactors. Control UASB reactor (without humic material) achieved 31.6% of iopromide removal, while 80% was removed in UASB reactors supplied with each metal-humic acid complex. Further analyses indicated multiple transformation reactions taking place in iopromide including deiodination, N-dealkylation, decarboxylation and deacetylation. This is the first successful application of immobilized RM, which does not require a supporting material to maintain the solid-phase RM in long term operation of bioreactors. The proposed redox catalyst could be suitable for enhancing the redox conversion of different recalcitrant pollutants present in industrial effluents. Copyright © 2016 Elsevier Ltd. All rights reserved.

Investigation of the behaviour of solid acid catalysts for acylations and cyanisations of aromatics. Final report; Untersuchungen zur Wirkungsweise von festen sauren Katalysatoren bei Acylierungen und Cyanierungen von Aromaten. Abschlussbericht

Energy Technology Data Exchange (ETDEWEB)

Kemnitz, E.

2002-01-01

The present state of the art in the field of FRIEDEL-CRAFTS-ACYLATIONS is characterized by the application of homogenous catalysts (at least stochiometric amounts) like AlCl{sub 3} or FeCl{sub 3}. Problems arising from this application are corrosions, difficult product separations from the catalyst and the origin of acid waste water. Hence, the aim of this project was the development of suitable solid catalysts which overcome the problems ascribed above. Sulfated zirconia (SZ) was found to be an excellent solid Br.o/nsted-acid to be used especially in their aerogel or cryogel form. Thus with this catalyst system, in the benzoylation of anisol nearly 100% conversion may be achieved. In this way it could be proved, that with SZ a solid Br.o/nsted-acid might be available which gives reasonable hope to substitute in a near future, at least for some reactions, the classical homogeneous catalysts and to overcome their problems in use. (orig.)

Synthesis and Properties of Some polyurethane/ Partially Aromatic Polyester Casting Samples

International Nuclear Information System (INIS)

Sadek, E.M.; Mazroua, A.M.; Emam, A.S.; Motawie, A.M.

2005-01-01

A series of partially aromatic terephthalate polyesters were synthesized by melt transesterification of dimethyl terephthalate with various types of aliphatic diol compounds in 1:1.1 molar ratio. Ethylene-, di-, tri-, tetra ethylene glycol and polyethylene glycol with different molecular weights 1000, 4000, 6000 as well as the prepared dihydroxy natural rubber were used. Another series of partially aromatic adipate and sebacate polyesters based on the prepared bisphenol A and its tetrabromo derivative were also synthesized by direct polycondensation esterification with adipic and sebacic acid. Polyurethane with NCO/OH ratio equal 4 was prepared from the reaction of 2,4 toluene diisocyanate with polyethylene glycol 1000. The prepared polyurethane was mixed with different weight percentages (2, 4, 6, 8, 10 or 12 % w/w) of the prepared partially aromatic polyesters to give polyurethane/polyester compositions. Mechanical and electrical properties as well as water and chemical resistance of the prepared film samples with thickness 3-4 mm were determined and compared with those of polyurethane film sample without polyester. The data indicate that 10 % w/w of the added partially aromatic polyester increases polyurethane tensile strength, improves its insulation properties and hydrolytic stability as well as its chemical resistance. Film samples based on bisphenol A impart excellent properties as compared with those based on aliphatic glycol species and dihydroxy natural rubber. Keywords: Partially aromatic polyesters, Dimethyl terephthalate, Glycols, Bisphenol A, Tetrabromo bisphenol A, Natural rubber, Adipic acid, Sebacic acid, Polyurethane, Casting

Comparative acid-base properties of the surface of components of the CdTe-ZnS system in series of substitutional solid solutions and their analogs

Science.gov (United States)

Kirovskaya, I. A.; Kasatova, I. Yu.

2011-07-01

The acid-base properties of the surface of solid solutions and binary components of the CdTe-ZnS system are studied by hydrolytic adsorption, nonaqueous conductometric titration, mechanochemistry, IR spectroscopy, and Raman scattering spectroscopy. The strength, nature, and concentration of acid centers on the original surface and that exposed to CO are determined. The changes in acid-base properties in dependence on the composition of the system under investigation in the series of CdB6, ZnB6 analogs are studied.

Specific bile acid radioimmunoassays for separate determinations of unconjugated cholic acid, conjugated cholic acid and conjugated deoxycholic acid in serum and their clinical application

International Nuclear Information System (INIS)

Matern, S.; Gerok, W.

1977-01-01

Specific radioimmunoassays for separate determinations of serum unconjugated cholic, conjugated cholic and conjugated deoxycholic acids have been developed. Prior to the radioimmunoassay, extraction of serum bile acids was performed with Amberlite XAD-2. Unconjugated cholic acid was separated from glyco- and taurocholic acids by thin-layer chromatography. At 50% displacement of bound labeled glyco[ 3 H]cholic acid using antiserum obtained after immunization with cholic acid-bovine serum albumin-conjugate the cross-reactivity of taurocholic acid was 100%, cholic acid 80%, glycochenodeoxycholic acid 10%, chenodeoxycholic acid 7%, conjugated deoxycholic acid 3%, and conjugated lithocholic acid 3 H]cholic acid was linear on a logit-log plot from 5 to 80 pmol of unlabeled glycocholic acid. Fasting serum conjugated cholic acid in healthy subjects was 0.68 +- 0.34 μmol/l. Unconjugated cholic acid was determined by a solid phase radioimmunoassay using the cholic acid antibody chemically bound to Sepharose. The displacement curve of [ 3 H]cholic acid in the solid phase radioimmunoassay was linear on a logit-log plot from 5 to 200 pmol of unlabeled cholic acid. The coefficient of variation between samples was 5%. Fasting serum conjugated deoxycholic acid concentrations in 10 healthy subjects ranged from 0.18 to 0.92 μmol/l determined by a radioimmunoassay using antiserum obtained after immunization with deoxycholic acid-bovine serum albumin-conjugate. The clinical application of these bile acid radioimmunoassays is shown by an 'oral cholate tolerance test' as a sensitive indicator of liver function and by an 'oral cholyglycine tolerance test' as a useful test for bile acid absorption. (orig.) [de

Analysis of non-esterified fatty acids in human samples by solid-phase-extraction and gas chromatography/mass spectrometry.

Science.gov (United States)

Kopf, Thomas; Schmitz, Gerd

2013-11-01

The determination of the fatty acid (FA) profile of lipid classes is essential for lipidomic analysis. We recently developed a GC/MS-method for the analysis of the FA profile of total FAs, i.e. the totality of bound and unbound FAs, in any given biological sample (TOFAs). Here, we present a method for the analysis of non-esterified fatty acids (NEFAs) in biological samples, i.e. the fraction that is present as extractable free fatty acids. Lipid extraction is performed according to Dole using 80/20 2-propanol/n-hexane (v/v), with 0.1% H2SO4. The fatty acid-species composition of this NEFA-fraction is determined as FAME after derivatization with our GC/MS-method on a BPX column (Shimadzu). Validation of the NEFA-method presented was performed in human plasma samples. The validated method has been used with human plasma, cells and tissues, as well as mammalian body fluids and tissue samples. The newly developed solid-phase-extraction (SPE)-GC-MS method allows the rapid separation of the NEFA-fraction from a neutral lipid extract of plasma samples. As a major advantage compared to G-FID-methods, GC-MS allows the use of stable isotope labeled fatty acid precursors to monitor fatty acid metabolism. Copyright © 2013 Elsevier B.V. All rights reserved.

Recovery of boric acid from nuclear waste

International Nuclear Information System (INIS)

Lahoda, E.J.

1985-01-01

Disclosed is a process for separating and recovering boric acid from water containing solids which include boric acid and radionuclides. In the first step, the water is separated from the solids by evaporation of the water at a temperature under 130 0 F In the second step, an alcohol selected from the group consisting of methanol, ethanol, propanol, isopropanol, and mixtures thereof is added to the remaining solids in the amount of at least 1.4 times that stoichiometrically required to react with the boric acid to form boron alkoxide and water to about 100 mole % in excess of stoichiometric. In the third step, the boron alkoxide is separated from the remaining solids by evaporation of the boron alkoxide. In the fourth step, water is added to the volatilized boron alkoxide to form boric acid and an alcohol. And finally, the alcohol is separated from the boric acid by evaporating the alcohol

Effect of total solid content and pretreatment on the production of lactic acid from mixed culture dark fermentation of food waste.

Science.gov (United States)

Yousuf, Ahasa; Bastidas-Oyanedel, Juan-Rodrigo; Schmidt, Jens Ejbye

2018-04-28

Food waste landfilling causes environmental degradation, and this work assesses a sustainable food valorization technique. In this study, food waste is converted into lactic acid in a batch assembly by dark fermentation without pH control and without the addition of external inoculum at 37 °C. The effect of total solid (TS), enzymatic and aeration pretreatment was investigated on liquid products concentration and product yield. The maximum possible TS content was 34% of enzymatic pretreated waste, and showed the highest lactic acid concentration of 52 g/L, with a lactic acid selectivity of 0.6 g lactic /g totalacids . The results indicated that aeration pretreatment does not significantly improve product concentration or yield. Non-pretreated waste in a 29% TS system showed a lactic acid concentration of 31 g/L. The results showed that enzymatic pretreated waste at TS of 34% results in the highest production of lactic acid. Copyright © 2018 Elsevier Ltd. All rights reserved.

Transformation of ferulic acid to vanillin using a fed-batch solid-liquid two-phase partitioning bioreactor.

Science.gov (United States)

Ma, Xiao-kui; Daugulis, Andrew J

2014-01-01

Amycolatopsis sp. ATCC 39116 (formerly Streptomyces setonii) has shown promising results in converting ferulic acid (trans-4-hydroxy-3-methoxycinnamic acid; substrate), which can be derived from natural plant wastes, to vanillin (4-hydroxy-3-methoxybenzaldehyde). After exploring the influence of adding vanillin at different times during the growth cycle on cell growth and transformation performance of this strain and demonstrating the inhibitory effect of vanillin, a solid-liquid two-phase partitioning bioreactor (TPPB) system was used as an in situ product removal technique to enhance transformation productivity by this strain. The thermoplastic polymer Hytrel(®) G4078W was found to have superior partitioning capacity for vanillin with a partition coefficient of 12 and a low affinity for the substrate. A 3-L working volume solid-liquid fed-batch TPPB mode, using 300 g Hytrel G4078W as the sequestering phase, produced a final vanillin concentration of 19.5 g/L. The overall productivity of this reactor system was 450 mg/L. h, among the highest reported in literature. Vanillin was easily and quantitatively recovered from the polymers mostly by single stage extraction into methanol or other organic solvents used in food industry, simultaneously regenerating polymer beads for reuse. A polymer-liquid two phase bioreactor was again confirmed to easily outperform single phase systems that feature inhibitory or easily further degraded substrates/products. This enhancement strategy might reasonably be expected in the production of other flavor and fragrance compounds obtained by biotransformations. © 2013 American Institute of Chemical Engineers.

Kinetic study of solid phase demineralization by weak acids in one-step enzymatic bio-refinery of shrimp cuticles

OpenAIRE

Baron, Regis; Socol, Marius; Arhaliass, A.; Bruzac, Sandrine; Le Roux, Karine; Del Pino, J. Rodriguez; Berge, Jean-pascal; Kaas, Raymond

2015-01-01

We describe a one-step bio-refinery process for shrimp composites by-products. Its originality lies in a simple rapid (6 h) biotechnological cuticle fragmentation process that recovers all major compounds (chitins, peptides and minerals in particular calcium). The process consists of a controlled exogenous enzymatic proteolysis in a food-grade acidic medium allowing chitin purification (solid phase), and recovery of peptides and minerals (liquid phase). At a pH of between 3.5 and 4, protease ...

Nitrate removal properties of solid-phase denitrification processes using acid-blended poly(L-lactic acid) as the sole substrate

International Nuclear Information System (INIS)

Yamada, T; Matsuoka, H; Sun, J; Tsuji, H; Hiraishi, A; Yoshikawa, S

2013-01-01

The large amount of waste that is discharged along with the diffusion of poly(L-lactic acid) (PLLA) articles in use is persistent concern. Previously, we studied solid-phase denitrification (SPD) processes using PLLA to establish an effective re-use of PLLA waste. We found that PLLA with a weight-average molecular weight (M w ) of approximately 10,000 was suitable for SPD processes; however, the recycling of PLLA waste consumes a high energy. A new PLLA plastic including 5% poly(ethylene oxalate) (PEOxPLLA) as a blend material has attracted attention because recycling of PEOxPLLA consumes less electricity than that of PLLA. In this study, our main objectives were to evaluate whether PEOxPLLA can be used for SPD processes by changing its M w and to investigate the bioavailability for denitrification of hydrolysates released from PEOxPLLA. The predicted hydrolysates, including oxalic acid, ethylene glycol, and lactate, are abiotically released, leading to different biological nitrate removal rates. Consequently, the nitrate removal rate of PEOxPLLA ranged from 0.9–4.1 mg-NO 3 − -N·g-MLSS·h −1 by changing the M w in the range of 8,500–238,000. In culture-dependent approaches, denitrifying bacteria using each substrate as an electron donor are found in activated sludge, suggesting that all hydrolysates functioned in the SPD processes using PEOxPLLA.

Combined use of titration calorimetry and spectrofluorimetry for the screening of the acidity of solid catalysts in different liquids

International Nuclear Information System (INIS)

Gervasini, Antonella; Auroux, Aline

2013-01-01

Graphical abstract: Measurements of acidity of oxides of catalytic importance in various liquids open the possibility to know their effective acidity, which is related with their activity in liquid-heterogeneous catalysis. Titration-calorimetry alone or in connection with spectrofluorimetry is efficient for this scope. - Highlights: • Measurements of acidity of oxides of catalytic importance in various liquids. • Titration-calorimetry alone or in connection with spectrofluorimetry is efficient for this scope. • Effective acidities are expressed by given sample in various liquids. • Nb-containing samples are able to maintain acidity in protic liquids. - Abstract: The effective acid and base surface properties of selected acidic and basic samples of catalytic interest (alumina, titania, zirconia, silica–alumina, niobium oxide, niobium phosphate, boron nitride, and hydrotalcite) were measured by titration with basic and acidic molecular probes (aniline, 2-phenylethylamine, and phenol) in various liquids (cyclohexane, 1,4-dioxane, isopropanol, n-decane, and toluene) with different polar and protic characteristics. The combined use of a reaction calorimeter and a spectrofluorimeter has been performed. The set-up of the coupled technique and the most interesting results are shown here. The study confirmed that the acid–base properties of solids are deeply affected by the nature and properties of the liquid surrounding the samples. Few oxides are able to maintain their surface acidity in highly polar and protic solvents, in particular whose containing niobium. In general, the solvating and coordinative ability of the most polar and protic liquids caused remarkable loss of acidity/basicity of the oxide surfaces

Combined use of titration calorimetry and spectrofluorimetry for the screening of the acidity of solid catalysts in different liquids

Energy Technology Data Exchange (ETDEWEB)

Gervasini, Antonella, E-mail: antonella.gervasini@unimi.it [Dipartimento di Chimica, Università degli Studi di Milano, via Camillo Golgi, 19, 20133 Milano (Italy); Auroux, Aline, E-mail: aline.auroux@ircelyon.univ-lyon1.fr [Université Lyon 1, CNRS, UMR 5256, Institut de Recherches sur la Catalyse et l‘Environnement de Lyon (IRCELYON), 2 Avenue A. Einstein, 69626 Villeurbanne (France)

2013-09-10

Graphical abstract: Measurements of acidity of oxides of catalytic importance in various liquids open the possibility to know their effective acidity, which is related with their activity in liquid-heterogeneous catalysis. Titration-calorimetry alone or in connection with spectrofluorimetry is efficient for this scope. - Highlights: • Measurements of acidity of oxides of catalytic importance in various liquids. • Titration-calorimetry alone or in connection with spectrofluorimetry is efficient for this scope. • Effective acidities are expressed by given sample in various liquids. • Nb-containing samples are able to maintain acidity in protic liquids. - Abstract: The effective acid and base surface properties of selected acidic and basic samples of catalytic interest (alumina, titania, zirconia, silica–alumina, niobium oxide, niobium phosphate, boron nitride, and hydrotalcite) were measured by titration with basic and acidic molecular probes (aniline, 2-phenylethylamine, and phenol) in various liquids (cyclohexane, 1,4-dioxane, isopropanol, n-decane, and toluene) with different polar and protic characteristics. The combined use of a reaction calorimeter and a spectrofluorimeter has been performed. The set-up of the coupled technique and the most interesting results are shown here. The study confirmed that the acid–base properties of solids are deeply affected by the nature and properties of the liquid surrounding the samples. Few oxides are able to maintain their surface acidity in highly polar and protic solvents, in particular whose containing niobium. In general, the solvating and coordinative ability of the most polar and protic liquids caused remarkable loss of acidity/basicity of the oxide surfaces.

Black liquor-derived carbonaceous solid acid catalyst for the hydrolysis of pretreated rice straw in ionic liquid.

Science.gov (United States)

Bai, Chenxi; Zhu, Linfeng; Shen, Feng; Qi, Xinhua

2016-11-01

Lignin-containing black liquor from pretreatment of rice straw by KOH aqueous solution was applied to prepare a carbonaceous solid acid catalyst, in which KOH played dual roles of extracting lignin from rice straw and developing porosity of the carbon material as an activation agent. The synthesized black liquor-derived carbon material was applied in catalytic hydrolysis of the residue solid from the pretreatment of rice straw, which was mainly composed of cellulose and hemicellulose, and showed excellent activity for the production of total reducing sugars (TRS) in ionic liquid, 1-butyl-3-methyl imidazolium chloride. The highest TRS yield of 63.4% was achieved at 140°C for 120min, which was much higher than that obtained from crude rice straw under the same reaction conditions (36.6% TRS yield). Overall, this study provides a renewable strategy for the utilization of all components of lignocellulosic biomass. Copyright © 2016 Elsevier Ltd. All rights reserved.

Preparation and Characterization of Waterborne Polyurethaneurea Composed of Dimer Fatty Acid Polyester Polyol

Directory of Open Access Journals (Sweden)

2006-01-01

Full Text Available A series of polyurethaneurea (PUU aqueous dispersions, which were stable at ambient temperature for more than 1 year, were prepared with C 36 -dimer-fatty-acid-based polyester polyol, isophorone diisocyanate, dimethylol propionic acid, and ethylenediamine. The particle size of all these PUU (DPU aqueous dispersions ( <100 nm was less than that of comparable specimens, that is, poly-(neopentyl glycol adipate polyester-polyol-based PUU (APU aqueous dispersions, and the polydispersity index was very narrow ( ≤1.13 . The films prepared with the DPU aqueous dispersions exhibited excellent waterproof performance, such as low amount of water absorption (1.3 wt%, and good mechanical properties (hardness and tensile strength, resulting from the strong hydrogen bonding in urea carbonyl groups and the perfect ordered structure of hard segments compared with those prepared with the APU aqueous dispersions. The surface hydrophobicity of the films prepared with modified DPU aqueous dispersions, which were modified with a fluorinated polyacrylate emulsion, was excellent, as the water contact angle on the surface of such films rose up to 100. The mechanical properties of such modified DPU films were further enhanced.

Preparation and investigation of mefenamic acid - polyethylene glycol - sucrose ester solid dispersions.

Science.gov (United States)

Fülöp, Ibolya; Gyéresi, Árpád; Kiss, Lóránd; Deli, Mária A; Croitoru, Mircea Dumitru; Szabó-Révész, Piroska; Aigner, Zoltán

2015-12-01

Mefenamic acid (MA) is a widely used non-steroidal antiinflammatory (NSAID) drug. The adverse effects typical of NSAIDs are also present in the case of MA, partly due to its low water solubility. The aim of this study was to increase the water solubility of MA in order to influence its absorption and bioavailability. Solid dispersions of MA were prepared by the melting method using polyethylene glycol 6000 and different types (laurate, D-1216; palmitate, P-1670; stearate, S-1670) and amounts of sucrose esters as carriers. The X-ray diffraction results show that MA crystals were not present in the products. Dissolution tests carried out in artificial intestinal juice showed that the product containing 10 % D-1216 increased water solubility about 3 times. The apparent permeability coefficient of MA across human Caco-2 intestinal epithelial cell layers was high and, despite the difference in solubility, there was no further increase in drug penetration in the presence of the applied additives.

Isobutane/butene alkylation on solid catalysts. Where do we stand?

Energy Technology Data Exchange (ETDEWEB)

Weitkamp, J.; Traa, Y. [Institute of Chemical Technology I, University of Stuttgart, D-70550 Stuttgart (Germany)

1999-02-24

Liquid-phase processes with concentrated sulfuric acid or hydrogen fluoride as catalysts are currently being used in petroleum refining for the manufacture of alkylation gasoline from isobutane and butenes. While the product, i.e., alkylate, is a most valuable gasoline component, the existing processes for its manufacture are less satisfactory. Replacement of the liquid catalysts by a solid acid is an important target of modern research. In the past two decades, a large number of solid acids have been scrutinized, and at least four developments were driven till the pilot plant stage. In this paper, an attempt is made to rationalize, on a mechanistic basis, the selectivity loss almost always encountered with solid acids after relatively short times-on-stream. Suggestions are made concerning a more target-oriented research on isobutane/alkene alkylation in the future

The preparation of solid acid and acid water reducing agent for slag is prepared by adsorption method

Science.gov (United States)

Zhao, Su; Wang, Jinpeng; Zhu, Xitong

2018-03-01

Solid polycarboxylate superplasticizer can not only solve the problems caused by water reducing agent in storage and transportation, but also meet the needs of some special projects. We can choose to use the mineral slag, which is larger than surface area and has stronger adsorption, as adsorbent to absorb liquid polycarboxylate superplasticizer and absorb its moisture, and then makes solid polycarboxylate superplasticizer after drying. It determines the solid-liquid ratio to prepare the solid polycarboxylate superplasticizer to be 3:1. The temperature change within 100°C will not cause changes in the functional group and structure of the water reducing agent molecule. The application of the solid polycarboxylate superplasticizer was basically unchanged compared with its liquid water reducing agent.

Tannase production by Aspergillus aculeatus DBF9 through solid-state fermentation.

Science.gov (United States)

Banerjee, D; Mondal, K C; Pati, B R

2007-06-01

Tannase an industrially important enzyme was produced by Aspergillus aculeatus DBF9 through a solid-state fermentation (SSF). The organism produced good amount of enzyme and gallic acid in wheat bran among the solid substrate used in SSF. Maximum enzyme and gallic acid production occurred in 5% tannic acid after 72 h. Eighty percent initial substrate moisture and 30 degrees C temperature was found suitable for tannase production.

Physicochemical characterization of some solid materials by inverse gas chromatography

International Nuclear Information System (INIS)

Hamieh, T.; Abdessater, S.

2004-01-01

Full text.New equations and models on two-dimensional state of solid surfaces were previously elaborated in many other studies. results obtained were used in this paper to the determination and the quantification of some physicochemical properties of some solid surfaces, and especially, to study the acid-base superficial characteristics of some solid substrates like oxides and/or polymer adsorbed on oxides, carbon fibers, cements, etc. The technique used was the inverse gas chromatography (CGI) at infinite dilution. The acid-base constants were calculated for many solid surfaces: Al 2 O 3 , SiO 2 , MgO, ZnO, some cements, textiles and carbon fibers

Étude de la technique d'échange ionique avec compétition. Cas du dépôt de platine sur support solide acide par échange cationique Research on the Ion Exchange Technique with Competition. Case of Platinum Deposit on a Solid Acid Support by Cation Exchange

Directory of Open Access Journals (Sweden)

Ribeiro F.

2006-11-01

Full Text Available Cet article présente une étude détaillée de la technique de dépôt de platine sur support acide par échange cationique avec compétition. Cette technique permet d'obtenir à la fois une dispersion quasi atomique et une répartition macroscopique homogène du métal sur la surface du solide. En l'absence de limitations diffusionnelles extra-granulaires, les résultats expérimentaux sont en bon accord avec les prévisions théoriques . This article is a detailed examination of the technique of depositing platinum on an acid support by cation exchange with compétition. This technique produces both a quasi-atomic dispersion and a homogeneous macroscopic distribution of the métal onthe surface of the solid. In the absence of extragranular diffusion limitations, experimental findings are in good agreement with theoretical predictions.

Fresh meat quality of pigs fed diets with different fatty acid profiles and supplemented with red wine solids

Directory of Open Access Journals (Sweden)

Pier Giorgio Peiretti

2015-01-01

Full Text Available AbstractThree groups of pigs were fed three different diets, namely a diet rich in saturated fatty acids (palm oil-based, PO, a polyunsaturated fatty acid (PUFA-rich diet (corn oil-based, CO, and a PUFA-rich diet (corn oil-based supplemented with red wine solids (RWS, which was added to the diet (CO+RWS in order to assess the protective effect on the oxidative status of the pork meat. The addition of corn oil favourably modulates the FAs profile of the backfat, and to a lesser extent of the intramuscular fat of semimembranosus muscle, without causing adverse effects on the meat quality or on its oxidative stability. Moreover, these parameters were not affected by the addition of the RWS in the CO+RWS diet.

Mechanism of formation of humus coatings on mineral surfaces 3. Composition of adsorbed organic acids from compost leachate on alumina by solid-state 13C NMR

Science.gov (United States)

Wershaw, R. L.; Llaguno, E.C.; Leenheer, J.A.

1996-01-01

The adsorption of compost leachate DOC on alumina is used as a model for elucidation of the mechanism of formation of natural organic coatings on hydrous metal oxide surfaces in soils and sediments. Compost leachate DOC is composed mainly of organic acid molecules. The solid-state 13C NMR spectra of these organic acids indicate that they are very similar in composition to aquatic humic substances. Changes in the solid-state 13C NMR spectra of compost leachate DOC fractions adsorbed on alumina indicate that the DOC molecules are most likely adsorbed on metal oxide surfaces through a combination of polar and hydrophobic interaction mechanisms. This combination of polar and hydrophobic mechanism leads to the formation of bilayer coatings of the leachate molecules on the oxide surfaces.

A novel mesoporous sulfated zirconium solid acid catalyst for Friedel-Crafts benzylation reaction

International Nuclear Information System (INIS)

Miao, Zhichao; Zhou, Jin; Zhao, Jinping; Liu, Dandan; Bi, Xu; Chou, Lingjun; Zhuo, Shuping

2017-01-01

Highlights: • A novel mesoporous ZrO_2/SO_4"2"− has been prepared via a facile one-pot EISA strategy. • The M-ZrO_2/SO_4"2"− exhibited excellent textural and acidic properties. • The introduced S species were homogeneously dispersed in mesoporous skeleton. • The M-ZrO_2/SO_4"2"− exhibited excellent catalytic performance and reusability. - Abstract: In this paper, a novel mesoporous sulfated zirconium (M-ZrO_2/SO_4"2"−) has been gotten by one-pot evaporation-induced self-assembly (one-pot EISA) strategy. The SXRD, N_2-physisorption and TEM characterization techniques indicated that M-ZrO_2/SO_4"2"− possessed distinct mesostructure with big specific surface area (133.5 m"2 g"−"1), large pore volume (0.18 cm"3 g"−"1) and narrow pore size distribution (4.90 nm). Moreover, the existing states and the influence in mesostructure of introduced S species were detailedly investigated by the XRD, N_2-physisorption, TEM, TG-DSC, FT-IR and XPS techniques and the results showed that the S species, which existed as the type of SO_4"2"−, improved the textural properties of prepared materials. In addition, the NH_3-TPD and IR spectra of adsorbed pyridine indicated the existence of strong Brønsted and Lewis acid sites in M-ZrO_2/SO_4"2"− even evacuated at 400 °C. Furthermore, the M-ZrO_2/SO_4"2"− was used as a promise solid acid catalyst and displayed excellent catalytic performance and reusability in Friedel-Crafts benzylation reaction.

Biodegradability of poly(butylene succinate-co-butylene adipate) (PBSA) controlled by temperature during the dried-gel process

Science.gov (United States)

Yamazaki, Hana; Maeda, Tomoki; Hotta, Atsushi

Currently there is a growing interest in biodegradable plastics that can be readily degraded into H2O and CO2. Among them, poly(butylene succinate-co-butylene adipate)(PBSA) is one of the mechanically attractive materials that can be biodegraded by surrounding water molecules and microorganisms after the disposal of the plastics. In order to expand the use of PBSA, the proper and effective control of the biodegradability of PBSA should be realized. In this work, the dried-gel process of the PBSA was carefully studied considering the temperature of the process. Three different types of dried PBSA gels were prepared at three different gel-process temperatures. From the biodegradability testing by immersing the PBSA samples in NaOH aq., it was found that the percentage of the weight loss of the PBSA was increased, indicating that the biodegradability was enhanced as the gel preparation temperature became lower. In fact, smaller spherocrystals were observed in PBSA dried at cooler temperature, studied by the scanning electron microscopy (SEM). It was therefore concluded that the microstructures of PBSA could be well controlled by changing the gel preparation temperatures for the precise control of the biodegradability of PBSA. This work was supported by a Grant-in-Aid for Scientific Research (A) (No. 15H02298 to A.H.) and a Grant-in-Aid for Research Activity Start-up (No.15H06586 to T.M.) from JSPS: KAKENHI\\x9D.

The effect of using solid-state fermented peeled and unpeeled cassava root tubers and limiting amino acid supplementation on metabolisable energy for meat-type cockerels

OpenAIRE

Oso, A.O.; Li, L; Zhang, B.; Liu, H.; Li, F; Osho, S.O.; Olayemi, W.A.; Pirgozliev, V.

2017-01-01

A preliminary in-vitro solid-state fermentation of peeled (PCRM) and unpeeled cassava root tuber meal (UCRM) using Aspergillus niger van Tieghem, was conducted, followed by a force-feeding experiment to investigate the effects of a diet of solid state fermented peeled (PCRM) and unpeeled (UPCRM) cassava root, supplemented with limiting amino acid, on metabolizable energy (ME) for meat-type cockerels. Forty eight, 84 d-old meat-type cockerels (Ross 308) were assigned to 8 treatments consisting...

Problem Definition Studies on Potential Environmental Pollutants. 4. Physical, Chemical, Toxicological, and Biological Properties of Benzene; Toluene; Xylenes; and para-Chlorophenyl Methyl Sulfide, Sulfoxide, and Sulfone

Science.gov (United States)

1976-06-01

microorganisms. The presence of nitro, amino or sulfonic acid groups or halogens on the ring will almost always render benzene and related compounds...benzoquinone --- muconic acid Their later experiments with tea and grape leaf homogenates support this * conclusion. 12 2 Tkhelidze 1 2 3 showed that grape ...of such chemicals as phenol, aniline, cumene, adipic acid , diphenyl, and ethyl- * benzene, each of which is a starting material for other products

Performance and techno-economic assessment of several solid-liquid separation technologies for processing dilute-acid pretreated corn stover.

Science.gov (United States)

Sievers, David A; Tao, Ling; Schell, Daniel J

2014-09-01

Solid-liquid separation of pretreated lignocellulosic biomass slurries is a critical unit operation employed in several different processes for production of fuels and chemicals. An effective separation process achieves good recovery of solute (sugars) and efficient dewatering of the biomass slurry. Dilute acid pretreated corn stover slurries were subjected to pressure and vacuum filtration and basket centrifugation to evaluate the technical and economic merits of these technologies. Experimental performance results were used to perform detailed process simulations and economic analysis using a 2000 tonne/day biorefinery model to determine differences between the various filtration methods and their process settings. The filtration processes were able to successfully separate pretreated slurries into liquor and solid fractions with estimated sugar recoveries of at least 95% using a cake washing process. A continuous vacuum belt filter produced the most favorable process economics. Copyright © 2014 Elsevier Ltd. All rights reserved.

Effect of Chain-Extenders on the Properties and Hydrolytic Degradation Behavior of the Poly(lactide/ Poly(butylene adipate-co-terephthalate Blends

Directory of Open Access Journals (Sweden)

Mingqing Chen

2013-10-01

Full Text Available Biodegradable poly(lactide/poly(butylene adipate-co-terephthalate (PLA/PBAT blends were prepared by reactive blending in the presence of chain-extenders. Two chain-extenders with multi-epoxy groups were studied. The effect of chain-extenders on the morphology, mechanical properties, thermal behavior, and hydrolytic degradation of the blends was investigated. The compatibility between the PLA and PBAT was significantly improved by in situ formation of PLA-co-PBAT copolymers in the presence of the chain-extenders, results in an enhanced ductility of the blends, e.g., the elongation at break was increased to 500% without any decrease in the tensile strength. The differential scanning calorimeter (DSC results reveal that cold crystallization of PLA was enhanced due to heterogeneous nucleation effect of the in situ compatibilized PBAT domains. As known before, PLA is sensitive to hydrolysis and in the presence of PBAT and the chain-extenders, the hydrolytic degradation of the blend was evident. A three-stage hydrolysis mechanism for the system is proposed based on a study of weight loss and molecular weight reduction of the samples and the pH variation of the degradation medium.

Silica sulfuric acid: a reusable solid catalyst for one pot synthesis of densely substituted pyrrole-fused isocoumarins under solvent-free conditions

Directory of Open Access Journals (Sweden)

Sudipta Pathak

2013-11-01

Full Text Available A convenient and efficient methodology for the synthesis of densely substituted pyrrole-fused isocoumarins, which employs solid-supported silica sulfuric acid (SSA as catalyst, has been developed. When the mixture of ninhydrin adducts of acetylacetone/ethyl acetoacetate and primary amines was heated on the solid surface of SSA under solvent-free conditions, the pyrrole-fused isocoumarins were formed in good yields. This synthetic method has several advantages such as the employment of solvent-free reaction conditions without the use of any toxic reagents and metal catalysts, the ease of product isolation, the use of a recyclable catalyst, the low cost, the easy availability of the starting materials, and the excellent yields of products.

Enhancement of carvedilol solubility by solid dispersion technique using cyclodextrins, water soluble polymers and hydroxyl acid.

Science.gov (United States)

Yuvaraja, K; Khanam, Jasmina

2014-08-05

Aim of the present work is to enhance aqueous solubility of carvedilol (CV) by solid dispersion technique using wide variety of carriers such as: β-cyclodextrin (βCD), hydroxypropyl-β-cyclodextrin (HPβCD), tartaric acid (TA), polyvinyl pyrrolidone K-30 (PVP K-30) and poloxamer-407 (PLX-407). Various products of 'CV-solid dispersion' had been studied extensively in various pH conditions to check enhancement of solubility and dissolution characteristics of carvedilol. Any physical change upon interaction between CV and carriers was confirmed by instrumental analysis: XRD, DSC, FTIR and SEM. Negative change of Gibb's free energy and complexation constants (Kc, 75-240M(-1), for cyclodextrins and 1111-20,365M(-1), for PVP K-30 and PLX-407) were the evidence of stable nature of the binding between CV and carriers. 'Solubility enhancement factor' of ionized-CV was found high enough (340 times) with HPβCD in presence of TA. TA increases the binding efficiency of cyclodextrin and changing the pH of microenvironment in dissolution medium. In addition, ionization process was used to increase the apparent intrinsic solubility of drug. In vitro, dissolution time of CV was remarkably reduced in the solid dispersion system compared to that of pure drug. This may be attributed to increased wettability, dispersing ability and transformation of crystalline state of drug to amorphous one. Copyright © 2014 Elsevier B.V. All rights reserved.

Solid-Liquid and Liquid-Liquid Equilibrium in the Ternary System Acetic Acid-Propanoic Acid-Formamide.

Czech Academy of Sciences Publication Activity Database

Sedláková, Zuzana; Malijevská, I.

2007-01-01

Roč. 261, 1-2 (2007) , s. 129-132 ISSN 0378-3812. [International Conference on Properties and Phase Equilibria for Product and Process Design PPEPPD 2007 /11./. Hersonissos, Crete, 20.05.2007-25.05.2007] Institutional research plan: CEZ:AV0Z40720504 Keywords : solid-liquid equilibrium * ternary system * solid adduct Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 1.506, year: 2007

Characterization of polyesters by matrix-assisted laser desorption/ionization and Fourier transform mass spectrometry.

Science.gov (United States)

Mize, Todd H; Simonsick, William J; Amster, I Jonathan

2003-01-01

Two homopolyesters, poly(neopentyl glycol-alt-isophthalic acid) and poly(hexanediol-alt-azelaic acid), and two copolyesters, poly(dipropoxylated bisphenol-A-alt-(isophthalic acid-co-adipic acid)) and poly(neopentyl glycol-alt-(adipic acid-co-isophthalic acid)) were analyzed by internal source matrix assisted laser desorption/ionization Fourier transform mass spectrometry (MALDI-FTMS). The high resolution and high mass accuracy provided by FTMS greatly facilitate the characterization of the polyester and copolyester samples. Isobaric resolution allows the ion abundances of overlapping isotopic envelopes to be assessed. Repeat units were confirmed and end functionality assigned. Single shot mass spectra of the entire polymeric distribution demonstrate that the dynamic range of this internal MALDI source instrument and the analyzer cell exceeds performance of those previously reported for higher field instruments. Corrections of space charge mass shift effects are demonstrated for the analytes using an external calibrant and (subsequent to confirmation of structure) via internal calibration which removes ambiguity due to space charge differences in calibrant and analyte spectra. Capillary gel permeation chromatography was used to prepare low polydispersity samples from a high polydispersity polyester, improving the measurement of molecular weight distribution two-fold while retaining the benefits of high resolution mass spectrometry for elucidation of oligomer identity.

Amino acids separation with the tetracarboxylic derived of the para-ter-butylcalix[4]arene by means of solid-liquid extraction assisted with lanthanides

International Nuclear Information System (INIS)

Bernal R, R. del C.

2014-01-01

The tetracarboxylic derived of the para-ter-butylcalix[4]arene (B 4 ACEbL 4 ) does not exist commercially for what was synthesized and characterized at laboratory level. The separation of the L-tyrosine amino acid was studied by means of a solid-liquid extraction system with the B 4 ACEbL 4 as solid phase, in function of ph (2.5-7.5) and contact time (5 and 15 hours) to temperature of 15-17 grades C. Resulted that the ph and the contact time were decisive in the extraction percentage of water tyrosine. The lowest percentage was 49% to ph 4 and the highest percentage was 61% to ph 7.5 with 15 hours of contact. In a contact time of 5 hours the extraction was inferior to 32% (ph 4) and of 47% to ph 6.5. The europium effect (Eu (III)) was studied to ph acid in the tyrosine separation and was found that the tyrosine extraction is not increased neither decomposes in europium presence, this is simultaneously extracted by the calixarene but it does not enter in competition for the calixarene with the amino acid. The separate solid phases: calixarene-tyrosine was analyzed by Far infrared radiation (Fir), Mid-Infrared (Mir) spectroscopy and luminescence to check the tyrosine presence in the separate solids as well as the nature of the connection calixarene-tyrosine. In this way was possible to check the tyrosine presence and to propose the formed molecular species tyrosine-calixarene, those which interact mainly by means of hydrogen connections and Van der Waals forces. The liquid phases before and after the extraction were analyzed by UV-Vis spectrophotometry and luminescence. The Neutron activation analysis was used to determine the europium content in the solid and liquid phases of extractions in europium presence. The tyrosine degradation also shows dependence with the ph, obtaining 88% degradation to the 24 hours to ph 7.5, while to ph 3 is degraded the 54% of tyrosine present in the sample. The europium presence does not affect the tyrosine extraction but if its photo

Study of the compatibilizer effect in the properties of starch/polyester blends

Directory of Open Access Journals (Sweden)

Juliana Bonametti Olivato

2013-01-01

Full Text Available The mechanical, viscoelastic and structural properties of starch/ poly (butylene adipate co-terephthalate (PBAT blown films produced by reactive extrusion were evaluated using citric acid (CA and maleic anhydride (MA as compatibilizers. Scanning electron microscopy images showed more homogeneous structure when CA and MA were included in the formulation. The tensile strength (MPa was improved with the inclusion of the highest proportion of both compatibilizers (1.5 %wt. A larger elastic component with values between 0.42-0.45 for the degree of solidity (1-c1 was observed for the intermediate concentration of compatibilizers. A high level of glycerol (10 %wt results in films with increased % elongation. Three partially miscible phases were observed in the blends. Biodegradable films of starch/PBAT with better properties could be produced by one-step reactive extrusion using CA and/or MA as compatibilizers.

Solid-to-solid oxidation of a vanadium(IV) to a vanadium(V) compound: chemisty of a sulfur-containing siderophore.

Science.gov (United States)

Chatterjee, Pabitra B; Crans, Debbie C

2012-09-03

Visible light facilitates a solid-to-solid photochemical aerobic oxidation of a hunter-green microcrystalline oxidovanadium(IV) compound (1) to form a black powder of cis-dioxidovanadium(V) (2) at ambient temperature. The siderophore ligand pyridine-2,6-bis(thiocarboxylic acid), H(2)L, is secreted by a microorganism from the Pseudomonas genus. This irreversible transformation of a metal monooxo to a metal dioxo complex in the solid state in the absence of solvent is unprecedented. It serves as a proof-of-concept reaction for green chemistry occurring in solid matrixes.

Biowaiver monograph for immediate-release solid oral dosage forms: acetylsalicylic acid.

Science.gov (United States)

Dressman, Jennifer B; Nair, Anita; Abrahamsson, Bertil; Barends, Dirk M; Groot, D W; Kopp, Sabine; Langguth, Peter; Polli, James E; Shah, Vinod P; Zimmer, Markus

2012-08-01

A biowaiver monograph for acetylsalicylic acid (ASA) is presented. Literature and experimental data indicate that ASA is a highly soluble and highly permeable drug, leading to assignment of this active pharmaceutical ingredient (API) to Class I of the Biopharmaceutics Classification System (BCS). Limited bioequivalence (BE) studies reported in the literature indicate that products that have been tested are bioequivalent. Most of the excipients used in products with a marketing authorization in Europe are not considered to have an impact on gastrointestinal motility or permeability. Furthermore, ASA has a wide therapeutic index. Thus, the risks to the patient that might occur if a nonbioequivalent product were to be incorrectly deemed bioequivalent according to the biowaiver procedure appear to be minimal. As a result, the BCS-based biowaiver procedure can be recommended for approval of new formulations of solid oral dosage forms containing ASA as the only API, including both multisource and reformulated products, under the following conditions: (1) excipients are chosen from those used in ASA products already registered in International Conference on Harmonization and associated countries and (2) the dissolution profiles of the test and the comparator products comply with the BE guidance. Copyright © 2012 Wiley Periodicals, Inc.

New concept bioceramics composed of octacalcium phosphate (OCP) and dicarboxylic acid-intercalated OCP via hydrothermal hot-pressing

Energy Technology Data Exchange (ETDEWEB)

Ishihara, Shiho [Graduate School of Engineering, Osaka Prefecture University (Japan); Matsumoto, Takuya [Graduate School of Dentistry, Osaka University (Japan); Onoki, Takamasa, E-mail: onoki@mtr.osakafu-u.ac.jp [Graduate School of Engineering, Osaka Prefecture University (Japan); Sohmura, Taiji [Graduate School of Dentistry, Osaka University (Japan); Nakahira, Atsushi [Graduate School of Engineering, Osaka Prefecture University (Japan)

2009-08-01

Octacalcium phosphate (OCP) and adipic acid-intercalated complexed OCP (Adi-OCP) were synthesized. Moreover, we made ceramic bodies out of them through a hydrothermal hot-pressing (HHP) method. Characteristic features of both the powder and ceramics were investigated by the X-ray diffraction method (XRD). Surface morphology of the ceramics was observed by scanning electron microscopy (SEM). Density, compressive strength and pore size distribution of the ceramics were measured. Crystalline structure of the newly developed OCP ceramics had no phase transformation from the starting materials. Moreover, the newly developed OCP ceramics had good mechanical properties only through the HHP treatment with a temperature as low as 110 deg. C. In order to evaluate bioactivity, the ceramics were immersed in simulating body fluid (SBF). It was predicted that OCP and Adi-OCP had better bioactivity than that of conventional HAp ceramics.

New concept bioceramics composed of octacalcium phosphate (OCP) and dicarboxylic acid-intercalated OCP via hydrothermal hot-pressing

International Nuclear Information System (INIS)

Ishihara, Shiho; Matsumoto, Takuya; Onoki, Takamasa; Sohmura, Taiji; Nakahira, Atsushi

2009-01-01

Octacalcium phosphate (OCP) and adipic acid-intercalated complexed OCP (Adi-OCP) were synthesized. Moreover, we made ceramic bodies out of them through a hydrothermal hot-pressing (HHP) method. Characteristic features of both the powder and ceramics were investigated by the X-ray diffraction method (XRD). Surface morphology of the ceramics was observed by scanning electron microscopy (SEM). Density, compressive strength and pore size distribution of the ceramics were measured. Crystalline structure of the newly developed OCP ceramics had no phase transformation from the starting materials. Moreover, the newly developed OCP ceramics had good mechanical properties only through the HHP treatment with a temperature as low as 110 deg. C. In order to evaluate bioactivity, the ceramics were immersed in simulating body fluid (SBF). It was predicted that OCP and Adi-OCP had better bioactivity than that of conventional HAp ceramics.

The enhancement of the hydrolysis of bamboo biomass in ionic liquid with chitosan-based solid acid catalysts immobilized with metal ions.

Science.gov (United States)

Cheng, Jie; Wang, Nan; Zhao, Dezhou; Qin, Dandan; Si, Wenqing; Tan, Yunfei; Wei, Shun'an; Wang, Dan

2016-11-01

Three kinds of sulfonated cross-linked chitosan (SCCR) immobilized with metal ions of Cu(2+), Fe(3+) and Zn(2+) individually were synthesized and firstly used as solid acid catalysts in the hydrolysis of bamboo biomass. FTIR spectra showed that metal ions had been introduced into SCCR and the N-metal ions coordinate bound was formed. The particle sizes of these catalysts were about 500-1000μm with a pore size of 50-160μm. All of the three kinds of catalysts performed well for bamboo hydrolysis with 1-butyl-3-methyl-imidazolium chloride used as solvent. The most effective one was sulfonated cross-linked chitosan immobilized with Fe(3+) (Fe(3+)-SCCR). TRS yields were up to 73.42% for hydrolysis of bamboo powder in [C4mim]Cl with Fe(3+)-SCCR at 120°C and 20RPM after 24h. These novel chitosan-based metal ions immobilized solid acid catalysts with ionic liquids as the solvent might be promising to facilitate cost-efficient conversion of biomass into biofuels and bioproducts. Copyright © 2016 Elsevier Ltd. All rights reserved.

A novel mesoporous sulfated zirconium solid acid catalyst for Friedel-Crafts benzylation reaction

Energy Technology Data Exchange (ETDEWEB)

Miao, Zhichao; Zhou, Jin; Zhao, Jinping; Liu, Dandan; Bi, Xu [School of Chemical Engineering, Shandong University of Technology, Zibo, 255049 (China); Chou, Lingjun, E-mail: ljchou@licp.cas.cn [State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou, 730000 (China); Zhuo, Shuping, E-mail: zhuosp_academic@yahoo.com [School of Chemical Engineering, Shandong University of Technology, Zibo, 255049 (China)

2017-07-31

Highlights: • A novel mesoporous ZrO{sub 2}/SO{sub 4}{sup 2−} has been prepared via a facile one-pot EISA strategy. • The M-ZrO{sub 2}/SO{sub 4}{sup 2−} exhibited excellent textural and acidic properties. • The introduced S species were homogeneously dispersed in mesoporous skeleton. • The M-ZrO{sub 2}/SO{sub 4}{sup 2−} exhibited excellent catalytic performance and reusability. - Abstract: In this paper, a novel mesoporous sulfated zirconium (M-ZrO{sub 2}/SO{sub 4}{sup 2−}) has been gotten by one-pot evaporation-induced self-assembly (one-pot EISA) strategy. The SXRD, N{sub 2}-physisorption and TEM characterization techniques indicated that M-ZrO{sub 2}/SO{sub 4}{sup 2−} possessed distinct mesostructure with big specific surface area (133.5 m{sup 2} g{sup −1}), large pore volume (0.18 cm{sup 3} g{sup −1}) and narrow pore size distribution (4.90 nm). Moreover, the existing states and the influence in mesostructure of introduced S species were detailedly investigated by the XRD, N{sub 2}-physisorption, TEM, TG-DSC, FT-IR and XPS techniques and the results showed that the S species, which existed as the type of SO{sub 4}{sup 2−}, improved the textural properties of prepared materials. In addition, the NH{sub 3}-TPD and IR spectra of adsorbed pyridine indicated the existence of strong Brønsted and Lewis acid sites in M-ZrO{sub 2}/SO{sub 4}{sup 2−} even evacuated at 400 °C. Furthermore, the M-ZrO{sub 2}/SO{sub 4}{sup 2−} was used as a promise solid acid catalyst and displayed excellent catalytic performance and reusability in Friedel-Crafts benzylation reaction.

Origins of hydration differences in homochiral and racemic crystals of aspartic acid.

Science.gov (United States)

Juliano, Thomas R; Korter, Timothy M

2015-02-26

The propensity for crystalline hydrates of organic molecules to form is related to the strength of the interactions between molecules, including the chiral composition of the molecular solids. Specifically, homochiral versus racemic crystalline samples can exhibit distinct differences in their ability to form energetically stable hydrates. The focus of the current study is a comparison of the crystal structures and intermolecular forces found in solid-state L-aspartic acid, DL-aspartic acid, and L-aspartic acid monohydrate. The absence of experimental evidence for the DL-aspartic acid monohydrate is considered here in terms of the enhanced thermodynamic stability of the DL-aspartic acid anhydrate crystal as compared to the L-aspartic acid anhydrate as revealed through solid-state density functional theory calculations and terahertz spectroscopic measurements. The results indicate that anhydrous DL-aspartic acid is the more stable solid, not due to intermolecular forces alone but also due to the improved conformations of the molecules within the racemic solid. Hemihydrated and monohydrated forms of DL-aspartic acid have been computationally evaluated, and in each case, the hydrates produce destabilized aspartic acid conformations that prevent DL-aspartic acid hydrate formation from occurring.

Purification and characterization of a novel tannase produced by Kluyveromyces marxianus using olive pomace as solid support, and its promising role in gallic acid production.

Science.gov (United States)

Mahmoud, Abeer E; Fathy, Shadia A; Rashad, Mona M; Ezz, Magda K; Mohammed, Amira T

2018-02-01

Tannase is considered one of the most important industrial enzymes that find great applications in various sectors. Production of tannases through solid state fermentation (SSF) using agro-industrial wastes is an eco-friendly and cheap technology. Tannase was produced by the yeast Kluyveromyces marxianus using olive pomace as a solid support under SSF. It was purified using ammonium sulfate fractional precipitation followed by Sephadex G-200 gel filtration resulting in 64.6% enzyme yield with 1026.12U/mg specific activity and 24.21 purification fold. Pure tannase had molecular weight of 65 KDa and 66.62 KDa by SDS-PAGE and gel filtration, respectively. It showed a maximal activity at 35°C having two different pH optima, one of which is acidic (4.5) and the other one is alkaline (8.5). The enzyme was stable in the acidic range of pH (4.0-5.5) for 30min, and thermostable within the temperature range 30-70°C. Using tannic acid, the enzyme had a Km value of 0.77mM and Vmax of 263.20μmolemin -1 ml -1 . The effect of different metal ions on enzymatic activity was evaluated. HPLC analysis data indicated that the purified enzyme could carry out 24.65% tannic acid conversion with 5.25 folds increase in gallic acid concentration within 30min only. Copyright © 2017 Elsevier B.V. All rights reserved.

Flow-induced crystallization of a nano composite of poly(butylene adipate-co-terephthalate)/montmorillonite; Cinetica de cristalizacao induzida por fluxo de nanocomposito de poli(butileno adipato-co-tereftalato)/montmorilonita

Energy Technology Data Exchange (ETDEWEB)

Bonel, Alan B [Universidade Federal de Sao Carlos. UFSCar, Departamento de Engenharia de Materiais DEMa, SP (Brazil); Rego, Bruna T; Beatrice, Cesar A.G.; Marini, Juliano; Bretas, Rosario E.S., E-mail: bretas@ufscar.br [Universidade Federal de Sao Carlos. UFSCar, Programa de Pos-Graduacao em Ciencia e Engenharia de Materiais, SP (Brazil)

2011-07-01

Poly(butylene adipate-co-terephthalate) (PBAT) with 5wt% of an organically modified montmorillonite with polar surfactant was prepared by melt blending in a co-rotational twin-screw extruder at 160 degree C. 100rpm and 1 kg/h. Both pure polymer and nano composite were characterized by wide measurements. The study of the flow-induced crystallization was also done by rheological measurements, monitoring the viscosity as a function of time. The nano clay's lamellas were intercalated in the polymer m loss moduli of the nano composite, at low frequencies, showed that the particles of the nano clay were well dispersed and distributed thru the PBAT matrix. Finally, the presence of the nano clay's particles reduced the induction tim crystals growth, due to the strong interactions with the PBAT chains. (author)

Catalytic conversion of xylose and corn stalk into furfural over carbon solid acid catalyst in γ-valerolactone.

Science.gov (United States)

Zhang, Tingwei; Li, Wenzhi; Xu, Zhiping; Liu, Qiyu; Ma, Qiaozhi; Jameel, Hasan; Chang, Hou-min; Ma, Longlong

2016-06-01

A novel carbon solid acid catalyst was synthesized by the sulfonation of carbonaceous material which was prepared by carbonization of sucrose using 4-BDS as a sulfonating agent. TEM, N2 adsorption-desorption, elemental analysis, XPS and FT-IR were used to characterize the catalyst. Then, the catalyst was applied for the conversion of xylose and corn stalk into furfural in GVL. The influence of the reaction time, temperature and dosage of catalyst on xylose dehydration were also investigated. The Brønsted acid catalyst exhibited high activity in the dehydration of xylose, with a high furfural yield of 78.5% at 170°C in 30min. What's more, a 60.6% furfural yield from corn stalk was achieved in 100min at 200°C. The recyclability of the sulfonated carbon catalyst was perfect, and it could be reused for 5times without the loss of furfural yields. Copyright © 2016 Elsevier Ltd. All rights reserved.

Production of poly(β-l-malic acid) by Aureobasidium pullulans HA-4D under solid-state fermentation.

Science.gov (United States)

Xia, Jun; Li, Rongqing; He, Aiyong; Xu, Jiaxing; Liu, Xiaoyan; Li, Xiangqian; Xu, Jiming

2017-11-01

Poly(β-l-malic acid) (PMA) production by Aureobasidium pullulans HA-4D was carried out through solid-state fermentation (SSF) using agro-industrial residues. Maximum PMA production (75.4mg/g substrate) was obtained from a mixed substrate of sweet potato residue and wheat bran (1:1, w/w) supplemented with NaNO 3 (0.8%, w/w) and CaCO 3 (2%, w/w), with an initial moisture content of 70% and inoculum size of 13% (v/w) for 8days. Repeated-batch SSF was successfully conducted for 5 cycles with a high productivity. The scanning electron microscopy showed that the yeast-like cells of A. pullulans HA-4D could grow well on the solid substrate surface. Moreover, the cost analysis showed that the unit price of PMA in SSF was much lower than that of SmF. This is the first report on PMA production via SSF, and this study provided a new method to produce PMA from inexpensive agro-industrial residues. Copyright © 2017 Elsevier Ltd. All rights reserved.

Controlling the biodegradability of poly(butylene succinate-co-butylene adipate) (PBSA) by solvents used in the dried-gel process

Science.gov (United States)

Yamazaki, Hana; Kamitabira, Saya; Maeda, Tomoki; Hotta, Atsushi

Considering an environmentally friendly material, poly(butylene succinate-co-butylene adipate)(PBSA) is one of the attractive biodegradable plastics that can be eventually degraded into H2O and CO2 by neighboring water molecules and microorganisms after the disposal. In order to expand the application of PBSA, the precise control of the biodegradability of PBSA is necessary. In this study, the dried-gel process was introduced to control the biodegradability of PBSA. The dried PBSA gels were prepared by using three different solvents (toluene, cyclohexanone, and o-dichlorobenzene). The scanning electron microscopy (SEM) micrographs revealed that the PBSA prepared by toluene had smaller spherocrystals than the other PBSA dried-gels prepared by cyclohexanone or o-dichlorobenzene. The biodegradability testing by immersing the three types of PBSA in NaOH aq. showed that the percentage of the weight loss of the PBSA produced by toluene was the highest. The results indicated that the microstructures of PBSA could be controlled by changing solvents during the gel preparations, and that the biodegradability of PBSA could therefore be efficiently modified by changing solvents. This work was supported by a Grant-in-Aid for Scientific Research (A) (No. 15H02298 to A.H.) and a Grant-in-Aid for Research Activity Start-up (No.15H06586 to T.M.) from JSPS: KAKENHI\\x9D.

A study of low-energy ion induced radiolysis of thiol-containing amino acid cysteine in the solid and aqueous solution states

Energy Technology Data Exchange (ETDEWEB)

Ke Zhigang [Key Laboratory of Ion Beam Bio-engineering, Institute of Plasma Physics of Chinese Academy of Sciences, 350 Shushanhu Road, P.O. Box 1126, Hefei 230031 (China); Huang Qing, E-mail: huangq@ipp.ac.c [Key Laboratory of Ion Beam Bio-engineering, Institute of Plasma Physics of Chinese Academy of Sciences, 350 Shushanhu Road, P.O. Box 1126, Hefei 230031 (China); Dang Bingrong [Institute of Modern Physics, Chinese Academy of Sciences, 509 Nanchang Road, Lanzhou 730000 (China); Lu Yilin [Key Laboratory of Ion Beam Bio-engineering, Institute of Plasma Physics of Chinese Academy of Sciences, 350 Shushanhu Road, P.O. Box 1126, Hefei 230031 (China); Department of Physics, Anhui University, Hefei 230031 (China); Yuan Hang; Zhang Shuqing; Yu Zengliang [Key Laboratory of Ion Beam Bio-engineering, Institute of Plasma Physics of Chinese Academy of Sciences, 350 Shushanhu Road, P.O. Box 1126, Hefei 230031 (China)

2010-09-15

The radiolysis of cysteine under plasma discharge and irradiation of low-energy ion beam was investigated. The damage of cysteine in aqueous solution under discharge was assessed via the acid ninhydrin reagent and the yield of cystine produced from the reaction was analyzed by FTIR. In addition, the generation of hydrogen sulfide was also identified. The destruction of solid cysteine under low-energy ion beam irradiation was estimated via monitoring IR bands of different functional groups (-SH, -NH{sub 3}, -COO{sup -}) of cysteine, and the production of cystine from ion-irradiated solid cysteine after dissolution in water was also verified. These results may help us to understand the inactivation of sulphydryl enzymes under direct and indirect interaction with the low-energy ion irradiation.

A solid-state sensor based on ruthenium (II) complex immobilized on polytyramine film for the simultaneous determination of dopamine, ascorbic acid and uric acid

International Nuclear Information System (INIS)

Khudaish, Emad A.; Al-Ajmi, Khawla Y.; Al-Harthi, Salim H.

2014-01-01

A solid-state sensor based on a polytyramine (Pty) film deposited on a glassy carbon electrode doped with a tris(2,2′-bipyridyl)Ru(II) complex (Ru/Pty/GCE) was constructed electrochemically. The surface morphology of the film modified electrode was characterized using electrochemical and surface scanning techniques. A redox property represented by a [Ru(bpy) 3 ] 3+/2+ couple immobilized at the Pty moiety was characterized using typical voltammetric techniques. A distinct Ru 3d peak obtained at 280.9 eV confirms doping of the Ru species onto the Pty moiety characterized by X-ray photoelectron (XPS). Atomic force microscopy (AFM) images demonstrate that incorporation of Ru decreases the surface roughness of the native Pty film modified electrode. The Ru/Pty/GCE exhibits efficient electrochemical sensing toward the oxidation of dopamine (DA), ascorbic acid (AA) and uric acid (UA) in their mixture. Three well-defined peaks were resolved with a large peak to peak separation and the detection limits of AA, DA and UA are brought down to 0.31, 0.08 and 0.58 μM, respectively. Interference studies and application for DA determination in real samples were conducted with satisfactory results. - Highlights: • XPS data confirm doping of ruthenium onto the polytyramine moiety. • The voltammetric signals of ascorbic acid, dopamine and uric acid are well defined. • The sensor is stable and offers a large adsorption facility for all species. • The sensor is highly sensitive to dopamine oxidation. • The sensor is applied to a real sample with a satisfactory recovery percentage

A solid-state sensor based on ruthenium (II) complex immobilized on polytyramine film for the simultaneous determination of dopamine, ascorbic acid and uric acid

Energy Technology Data Exchange (ETDEWEB)

Khudaish, Emad A., E-mail: ejoudi@squ.edu.om [Sultan Qaboos University, College of Science, Chemistry Department, PO Box 36, PC 123 Muscat (Oman); Al-Ajmi, Khawla Y. [Sultan Qaboos University, College of Science, Chemistry Department, PO Box 36, PC 123 Muscat (Oman); Al-Harthi, Salim H. [Sultan Qaboos University, College of Science, Department of Physics, PO Box 36, PC 123 Muscat (Oman)

2014-08-01

A solid-state sensor based on a polytyramine (Pty) film deposited on a glassy carbon electrode doped with a tris(2,2′-bipyridyl)Ru(II) complex (Ru/Pty/GCE) was constructed electrochemically. The surface morphology of the film modified electrode was characterized using electrochemical and surface scanning techniques. A redox property represented by a [Ru(bpy){sub 3}]{sup 3+/2+} couple immobilized at the Pty moiety was characterized using typical voltammetric techniques. A distinct Ru 3d peak obtained at 280.9 eV confirms doping of the Ru species onto the Pty moiety characterized by X-ray photoelectron (XPS). Atomic force microscopy (AFM) images demonstrate that incorporation of Ru decreases the surface roughness of the native Pty film modified electrode. The Ru/Pty/GCE exhibits efficient electrochemical sensing toward the oxidation of dopamine (DA), ascorbic acid (AA) and uric acid (UA) in their mixture. Three well-defined peaks were resolved with a large peak to peak separation and the detection limits of AA, DA and UA are brought down to 0.31, 0.08 and 0.58 μM, respectively. Interference studies and application for DA determination in real samples were conducted with satisfactory results. - Highlights: • XPS data confirm doping of ruthenium onto the polytyramine moiety. • The voltammetric signals of ascorbic acid, dopamine and uric acid are well defined. • The sensor is stable and offers a large adsorption facility for all species. • The sensor is highly sensitive to dopamine oxidation. • The sensor is applied to a real sample with a satisfactory recovery percentage.

Salt and cocrystals of sildenafil with dicarboxylic acids: solubility and pharmacokinetic advantage of the glutarate salt.

Science.gov (United States)

Sanphui, Palash; Tothadi, Srinu; Ganguly, Somnath; Desiraju, Gautam R

2013-12-02

Sildenafil is a drug used to treat erectile dysfunction and pulmonary arterial hypertension. Because of poor aqueous solubility of the drug, the citrate salt, with improved solubility and pharmacokinetics, has been marketed. However, the citrate salt requires an hour to reach its peak plasma concentration. Thus, to improve solubility and bioavailability characteristics, cocrystals and salts of the drug have been prepared by treating aliphatic dicarboxylic acids with sildenafil; the N-methylated piperazine of the drug molecule interacts with the carboxyl group of the acid to form a heterosynthon. Salts are formed with oxalic and fumaric acid; salt monoanions are formed with succinic and glutaric acid. Sildenafil forms cocrystals with longer chain dicarboxylic acids such as adipic, pimelic, suberic, and sebacic acids. Auxiliary stabilization via C-H···O interactions is also present in these cocrystals and salts. Solubility experiments of sildenafil cocrystal/salts were carried out in 0.1N HCl aqueous medium and compared with the solubility of the citrate salt. The glutarate salt and pimelic acid cocrystal dissolve faster than the citrate salt in a two hour dissolution experiment. The glutarate salt exhibits improved solubility (3.2-fold) compared to the citrate salt in water. Solubilities of the binary salts follow an inverse correlation with their melting points, while the solubilities of the cocrystals follow solubilities of the coformer. Pharmacokinetic studies on rats showed that the glutarate salt exhibits doubled plasma AUC values in a single dose within an hour compared to the citrate salt. The high solubility of glutaric acid, in part originating from the strained conformation of the molecule and its high permeability, may be the reason for higher plasma levels of the drug.

Influence of solvent on the poly (acrylic acid)-oligo-(ethylene glycol) polymer gel electrolyte and the performance of quasi-solid-state dye-sensitized solar cells

International Nuclear Information System (INIS)

Wu, Jihuai; Lan, Zhang; Lin, Jianming; Huang, Miaoliang; Hao, Shancun; Fang, Leqing

2007-01-01

The influence of solvents on the property of poly (acrylic acid)-oligo-(ethylene glycol) polymer gel electrolyte and photovoltaic performance of quasi-solid-state dye-sensitized solar cells (DSSCs) were investigated. Solvents or mixed solvents with large donor number enhance the liquid electrolyte absorbency, which further influences the ionic conductivity of polymer gel electrolyte. A polymer gel electrolyte with ionic conductivity of 4.45 mS cm -1 was obtained by using poly (acrylic acid)-oligo-(ethylene glycol) as polymer matrix, and absorbing 30 vol.% N-methyl pyrrolidone and 70 vol.% γ-butyrolactone with 0.5 M NaI and 0.05 M I 2 . By using this polymer gel electrolyte coupling with 0.4 M pyridine additive, a quasi-solid-state dye-sensitized solar cell with conversion efficiency of 4.74% was obtained under irradiation of 100 mW cm -2 (AM 1.5)

New methods to the determination of acid-base constants of solid substrates (oxides and carbon fibres) and of the transition temperatures of polymers adsorbed on oxides

International Nuclear Information System (INIS)

Hamieh, Tayssir

2000-01-01

Full text.Inverse gas chromatography technique at infinite dilution was used to calculate the acidic and basic surface characteristics of some solid substrates like oxides: Mono gal, MgO, ZnO, SiO 2 and Al 2 O 3 , four different carbon fibres and polymers as PMMA at various tacticities. We determined the specific interactions between them and model organic molecules and showed the amphoteric feature of such solids. We proved that the usual relation giving the specific enthalpy of adsorption (ΔH s P) of a polar molecule adsorbed on a solid: (-ΔH s P) = (K A DN + K D AN) was not correct for oxides and carbon fibres. We proposed a new relashionship by adding a third parameter K reflecting the amphoteric character of the solid according to: (-ΔH s P) = K A .DN + K D .AN - K. AN.DN. On the other hand, we used the inverse gas chromatography (IGC) at infinite dilution to determine the glass transition temperatures and other transitions of the systems PMMA/SiO 2 and PMMA/Al 2 O 3 , at various covered surface fractions and for various tacticities of the polymer (atactic, isotactic and syndiotactic). The maxima of the dispersive component of the surface energy γ s d of our two systems, obtained by IGC at infinite dilution, indicated clearly the presence of transition temperatures (glass or local transitions). The study of the chemical physical properties of PMMA/SiO 2 and PMMA/Al 2 O 3 , revealed an important difference in the acidic and basic behaviour, in Lewis terms, of oxide covered by various concentrations of PMMA. This study also highlighted an important effect of the tacticity of the polymer on the acidic basic character of PMMA adsorbed on oxides

PLGA and PHBV Microsphere Formulations and Solid-State Characterization

DEFF Research Database (Denmark)

Yang, Chiming; Plackett, David; Needham, David

2009-01-01

To develop and characterize the solid-state properties of poly(DL-lactic-co-glycolic acid) (PLGA) and poly(3-hydroxybutyric acid-co-3-hydroxyvaleric acid) (PHBV) microspheres for the localized and controlled release of fusidic acid (FA). The effects of FA loading and polymer composition on the me...... of a DCM-FA-rich phase in the forming microsphere....

Microwave Effect for Glycosylation Promoted by Solid Super Acid in Supercritical Carbon Dioxide

Directory of Open Access Journals (Sweden)

Takahiko Maeda

2009-12-01

Full Text Available The effects of microwave irradiation (2.45 GHz, 200 W on glycosylation promoted by a solid super acid in supercritical carbon dioxide was investigated with particular attention paid to the structure of the acceptor substrate. Because of the symmetrical structure and high diffusive property of supercritical carbon dioxide, microwave irradiation did not alter the temperature of the reaction solution, but enhanced reaction yield when aliphatic acceptors are employed. Interestingly, the use of a phenolic acceptor under the same reaction conditions did not show these promoting effects due to microwave irradiation. In the case of aliphatic diol acceptors, the yield seemed to be dependent on the symmetrical properties of the acceptors. The results suggest that microwave irradiation do not affect the reactivity of the donor nor promoter independently. We conclude that the effect of acceptor structure on glycosylation yield is due to electric delocalization of hydroxyl group and dielectrically symmetric structure of whole molecule.

Chemical digestion of low level nuclear solid waste material

International Nuclear Information System (INIS)

Cooley, C.R.; Lerch, R.E.

1976-01-01

A chemical digestion for treatment of low level combustible nuclear solid waste material is provided and comprises reacting the solid waste material with concentrated sulfuric acid at a temperature within the range of 230 0 --300 0 C and simultaneously and/or thereafter contacting the reacting mixture with concentrated nitric acid or nitrogen dioxide. In a special embodiment spent ion exchange resins are converted by this chemical digestion to noncombustible gases and a low volume noncombustible residue. 6 claims, no drawings

Topochemical approach to efficiently produce main-chain poly(bile acid)s with high molecular weights.

Science.gov (United States)

Li, Weina; Li, Xuesong; Zhu, Wei; Li, Changxu; Xu, Dan; Ju, Yong; Li, Guangtao

2011-07-21

Based on a topochemical approach, a strategy for efficiently producing main-chain poly(bile acid)s in the solid state was developed. This strategy allows for facile and scalable synthesis of main-chain poly(bile acid)s not only with high molecular weights, but also with quantitative conversions and yields.

Effects of pharmaceutical processing on pepsin activity during the formulation of solid dosage forms.

Science.gov (United States)

Kristó, Katalin; Pintye-Hódi, Klára

2013-02-01

The main aim of this study was to investigate the effects of pharmaceutical technological methods on pepsin activity during the formulation of solid dosage forms. The circumstances of direct compression and wet granulation were modeled. During direct compression, the heat and the compression force must be taken into consideration. The effects of these parameters were investigated in three materials (pure pepsin, and 1:1 (w/w) pepsin-tartaric acid and 1:1 (w/w) pepsin-citric acid powder mixtures). It was concluded that direct compression is appropriate for the formulation of solid dosage forms containing pepsin through application without acids or with acids at low compression force. The effects of wet granulation were investigated with a factorial design for the same three materials. The factors were time, temperature and moisture content. There was no significant effect of the factors when acids were not applied. Temperature was a significant factor when acids were applied. The negative effect was significantly higher for citric acid than for tartaric acid. It was found that wet granulation can be utilized for the processing of pepsin into solid dosage forms under well-controlled circumstances. The application of citric acid is not recommended during the formulation of solid dosage forms through wet granulation. A mathematically based optimization may be necessary for preformulation studies of the preparation of dosage forms containing sensitive enzymes.

Biodegradable composites from polyester and sugar beet pulp with antimicrobial coating for food packaging

Science.gov (United States)

Totally biodegradable, double-layered antimicrobial composite Sheets were introduced for food packaging. The substrate layers of the sheets were prepared from poly (lactic acid) (PLA) and sugar beet pulp (SBP) or poly (butylene adipate-co-terephthalate (PBAT) and SBP by a twin-screw extruder. The ac...

Physicochemical characterization of tacrolimus-loaded solid dispersion with sodium carboxylmethyl cellulose and sodium lauryl sulfate.

Science.gov (United States)

Park, Young-Joon; Ryu, Dong-Sung; Li, Dong Xun; Quan, Qi Zhe; Oh, Dong Hoon; Kim, Jong Oh; Seo, Youn Gee; Lee, Young-Im; Yong, Chul Soon; Woo, Jong Soo; Choi, Han-Gon

2009-06-01

To develop a novel tacrolimus-loaded solid dispersion with improved solubility, various solid dispersions were prepared with various ratios of water, sodium lauryl sulfate, citric acid and carboxylmethylcellulose-Na using spray drying technique. The physicochemical properties of solid dispersions were investigated using scanning electron microscopy, differential scanning calorimetery and powder X-ray diffraction. Furthermore, their solubility and dissolution were evaluated compared to drug powder. The solid dispersion at the tacrolimus/CMC-Na/sodium lauryl sulfate/citric acid ratio of 3/24/3/0.2 significantly improved the drug solubility and dissolution compared to powder. The scanning electron microscopy result suggested that carriers might be attached to the surface of drug in this solid dispersion. Unlike traditional solid dispersion systems, the crystal form of drug in this solid dispersion could not be converted to amorphous form, which was confirmed by the analysis of DSC and powder X-ray diffraction. Thus, the solid dispersion system with water, sodium lauryl sulfate, citric acid and CMC-Na should be a potential candidate for delivering a poorly water-soluble tacrolimus with enhanced solubility and no convertible crystalline.

Migration of additives from poly(vinyl chloride) (PVC) tubes into aqueous media

DEFF Research Database (Denmark)

Wang, Qian; Storm, Birgit Kjærside

2005-01-01

The stability and migration product of medical PVC tubes plasticized with polyadipates were investigated by ageing in phosphate buffer at pH 1.679 and water at different temperatures. Changes in the PVC tubes were studied by wtaer absorption, weight loss, Fourier infrared spectroscopy (FTIR.......5% and only a small amount of adipic acid migrated when a tube was aged at 37 C in water and phosphate buffer (pH 1.679), and at 70 C in water after 56 days. However, when aged at 70 and 110 C, gradual deactivation of heat stabilizer after 21 days of ageing in buffer solution and separation of plasticizer...... from PVC matrix occurred. When the tube was aged at 110 C, significant degradation of both polyadipates and PVC were observed. Adipic acid and 1,4-butanediol monomers and oligomers of polyadipate were the major migration products from polyadipates in the water ageing solution, while only a relatively...

Peanut Shell-Derived Carbon Solid Acid with Large Surface Area and Its Application for the Catalytic Hydrolysis of Cyclohexyl Acetate

Directory of Open Access Journals (Sweden)

Wei Xue

2016-10-01

Full Text Available A carbon solid acid with large surface area (CSALA was prepared by partial carbonization of H3PO4 pre-treated peanut shells followed by sulfonation with concentrated H2SO4. The structure and acidity of CSALA were characterized by N2 adsorption–desorption, scanning electron microscopy (SEM, X-ray powder diffraction (XRD, 13C cross polarization (CP/magic angle spinning (MAS nuclear magnetic resonance (NMR, X-ray photoelectron spectroscopy (XPS, Fourier transform-infrared spectroscopy (FT-IR, titration, and elemental analysis. The results demonstrated that the CSALA was an amorphous carbon material with a surface area of 387.4 m2/g. SO3H groups formed on the surface with a density of 0.46 mmol/g, with 1.11 mmol/g of COOH and 0.39 mmol/g of phenolic OH. Densities of the latter two groups were notably greater than those observed on a carbon solid acid (CSA with a surface area of 10.1 m2/g. The CSALA catalyst showed better performance than the CSA for the hydrolysis of cyclohexyl acetate to cyclohexanol. Under optimal reaction conditions, cyclohexyl acetate conversion was 86.6% with 97.3% selectivity for cyclohexanol, while the results were 25.0% and 99.4%, respectively, catalyzed by CSA. The high activity of the CSALA could be attributed to its high density of COOH and large surface area. Moreover, the CSALA showed good reusability. Its catalytic activity decreased slightly during the first two cycles due to the leaching of polycyclic aromatic hydrocarbon-containing SO3H groups, and then remained constant during following uses.

Functionalized carbon nanofibers as solid acid catalysts for transesterification

NARCIS (Netherlands)

Stellwagen, D.R.; van der Klis, Frits; van Es, D.S.; de Jong, K.P.; Bitter, J.H.

2013-01-01

Carbon nanofibers (CNFs) were functionalized with aryl sulfonic acid groups using in situ diazonium coupling. The use of diazonium coupling yielded an acidic carbon material, in which the introduced acidic groups are readily accessible to the triglyceride substrate. The material is an efficient

Functionalized carbon nanofibers as solid-acid catalysts for transesterification

NARCIS (Netherlands)

Stellwagen, D.R.; Klis, van der F.; Es, van D.S.; Jong, de K.P.; Bitter, J.H.

2013-01-01

Carbon nanofibers (CNFs) were functionalized with aryl sulfonic acid groups using in situ diazonium coupling. The use of diazonium coupling yielded an acidic carbon material, in which the introduced acidic groups are readily accessible to the triglyceride substrate. The material is an efficient

Recovery of metal values and hydrofluoric acid from tantalum and columbium waste sludge

International Nuclear Information System (INIS)

Bielecki, E.; Romberger, K.; Bakke, B.; Hobin, M.A.; Clark, C.

1992-01-01

A metallurgical processing system for economically recovering metal values, such as columbium, tantalum, thorium, and uranium from dilute source solids, such as digestion sludges, by a series of steps including: (1) slurrying the source solids with dilute hydrofluoric acid to produce a solid phase and a liquid phase containing dissolved tantalum and columbium, then extracting tantalum and/or columbium from the liquid phase by means of a liquid ion-exchange process and then, additionally; (2) roasting the solid phase with sulfuric acid to recover and recycle hydrofluoric acid, leaching the roasted solids with dilute sulfuric acid to produce a disposable solid phase and a liquid phase containing thorium and uranium, and extracting thorium and uranium from the liquid phase by means of a liquid-liquid amine extraction process

Conversion of agroindustrial residues for high poly(γ-glutamic acid) production by Bacillus subtilis NX-2 via solid-state fermentation.

Science.gov (United States)

Tang, Bao; Xu, Hong; Xu, Zongqi; Xu, Cen; Xu, Zheng; Lei, Peng; Qiu, Yibin; Liang, Jinfeng; Feng, Xiaohai

2015-04-01

Poly(γ-glutamic acid) (γ-PGA) production by Bacillus subtilis NX-2 was carried out through solid-state fermentation with dry mushroom residues (DMR) and monosodium glutamate production residues (MGPR; a substitute of glutamate) for the first time. Dry shiitake mushroom residue (DSMR) was found to be the most suitable solid substrate among these DMRs; the optimal DSMR-to-MGPR ratio was optimized as 12:8. To increase γ-PGA production, industrial waste glycerol was added as a carbon source supplement to the solid-state medium. As a result, γ-PGA production increased by 34.8%. The batch fermentation obtained an outcome of 115.6 g kg(-1) γ-PGA and 39.5×10(8) colony forming units g(-1) cells. Furthermore, a satisfactory yield of 107.7 g kg(-1) γ-PGA was achieved by compost experiment on a scale of 50 kg in open air, indicating that economically large-scale γ-PGA production was feasible. Therefore, this study provided a novel method to produce γ-PGA from abundant and low-cost agroindustrial residues. Copyright © 2015 Elsevier Ltd. All rights reserved.

A novel ionic liquid-modified organic-polymer monolith as the sorbent for in-tube solid-phase microextraction of acidic food additives.

Science.gov (United States)

Wang, Ting-Ting; Chen, Yi-Hui; Ma, Jun-Feng; Hu, Min-Jie; Li, Ying; Fang, Jiang-Hua; Gao, Hao-Qi

2014-08-01

A novel ionic liquid-modified organic-polymer monolithic capillary column was prepared and used for in-tube solid-phase microextraction (SPME) of acidic food additives. The primary amino group of 1-aminopropyl-3-methylimidazolium chloride was reacted with the epoxide group of glycidyl methacrylate. The as-prepared new monomer was then copolymerized in situ with acrylamide and N,N'-methylenebisacrylamide in the presence of polyethylene glycol (PEG)-8000 and PEG-10,000 as porogens. The extraction performance of the developed monolithic sorbent was evaluated for benzoic acid, 3-hydroxybenzoic acid, cinnamic acid, 2,4-dichlorophenoxyacetic acid, and 3-(trifluoromethyl)-cinnamic acid. Such a sorbent, bearing hydrophobic and anion-exchange groups, had high extraction efficiency towards the test compounds. The adsorption capacities for the analytes dissolved in water ranged from 0.18 to 1.74 μg cm(-1). Good linear calibration curves (R(2) > 0.99) were obtained, and the limits of detection (S/N = 3) for the analytes were found to be in the range 1.2-13.5 ng mL(-1). The recoveries of five acidic food additives spiked in Coca-Cola beverage samples ranged from 85.4 % to 98.3 %, with RSD less than 6.9 %. The excellent applicability of the ionic liquid (IL)-modified monolithic column was further tested by the determination of benzoic acid content in Sprite samples, further illustrating its good potential for analyzing food additives in complex samples.

Removing hydrochloric acid exhaust products from high performance solid rocket propellant using aluminum-lithium alloy.

Science.gov (United States)

Terry, Brandon C; Sippel, Travis R; Pfeil, Mark A; Gunduz, I Emre; Son, Steven F

2016-11-05

Hydrochloric acid (HCl) pollution from perchlorate based propellants is well known for both launch site contamination, as well as the possible ozone layer depletion effects. Past efforts in developing environmentally cleaner solid propellants by scavenging the chlorine ion have focused on replacing a portion of the chorine-containing oxidant (i.e., ammonium perchlorate) with an alkali metal nitrate. The alkali metal (e.g., Li or Na) in the nitrate reacts with the chlorine ion to form an alkali metal chloride (i.e., a salt instead of HCl). While this technique can potentially reduce HCl formation, it also results in reduced ideal specific impulse (ISP). Here, we show using thermochemical calculations that using aluminum-lithium (Al-Li) alloy can reduce HCl formation by more than 95% (with lithium contents ≥15 mass%) and increase the ideal ISP by ∼7s compared to neat aluminum (using 80/20 mass% Al-Li alloy). Two solid propellants were formulated using 80/20 Al-Li alloy or neat aluminum as fuel additives. The halide scavenging effect of Al-Li propellants was verified using wet bomb combustion experiments (75.5±4.8% reduction in pH, ∝ [HCl], when compared to neat aluminum). Additionally, no measurable HCl evolution was detected using differential scanning calorimetry coupled with thermogravimetric analysis, mass spectrometry, and Fourier transform infrared absorption. Copyright © 2016 Elsevier B.V. All rights reserved.

Effect of total solids content on biohydrogen production and lactic acid accumulation during dark fermentation of organic waste biomass.

Science.gov (United States)

Ghimire, Anish; Trably, Eric; Frunzo, Luigi; Pirozzi, Francesco; Lens, Piet N L; Esposito, Giovanni; Cazier, Elisabeth A; Escudié, Renaud

2018-01-01

Production of biohydrogen and related metabolic by-products was investigated in Solid State Dark Fermentation (SSDF) of food waste (FW) and wheat straw (WS). The effect of the total solids (TS) content and H 2 partial pressure (pp H2 ), two of the main operating factors of SSDF, were investigated. Batch tests with FW at 10, 15, 20, 25 and 30% TS showed considerable effects of the TS on metabolites distribution. H 2 production was strongly inhibited for TS contents higher than 15% with a concomitant accumulation of lactic acid and a decrease in substrate conversion. Varying the pp H2 had no significant effect on the conversion products and overall degradation of FW and WS, suggesting that pp H2 was not the main limiting factor in SSDF. This study showed that the conversion of complex substrates by SSDF depends on the substrate type and is limited by the TS content. Copyright © 2017 Elsevier Ltd. All rights reserved.

Formation and filtration characteristics of solids generated in a high level liquid waste treatment process. Filtration characteristics of solids formed in simulated high level liquid waste

International Nuclear Information System (INIS)

Kondo, Y.; Kubota, M.

1997-01-01

The filtration characteristics of solids generated in a simulated high level liquid waste (HLLW) were experimentally examined, when the simulated HLLW was processed according to the ordinary way of actual HLLW treatment process. The filtration characteristics of solids depended on the particle size. The phosphomolybdic acid, which was very fine particle with about 0.1 μm diameter, made slurry a 'difficult-to-filter' slurry, if the phosphomolybdic acid content (wt%) to the whole solids in a slurry exceeded 50wt%. On the contrary, the zirconium compounds (zirconium molybdate and zirconium telluride) had positive effect on filtration characteristics because of their relatively large particle size of about 3 to 5 μm. When the zirconium compounds content was above 50 wt%, slurry became a 'easy-to-filter' slurry. A centrifugal sedimentation was discussed as a solid/liquid separation technique for very fine particles such as phosphomolybdic acid. The theoretical feed flow rate corresponded to 0.1 μm diameter particles was about 20 1/h at the centrifugal acceleration of about 8000 G. (author)

40 CFR 98.54 - Monitoring and QA/QC requirements.

Science.gov (United States)

2010-07-01

... accounting purposes. (d) You must conduct all required performance tests according to the methods in § 98.54... requirements. (a) You must conduct a new performance test and calculate a new facility-specific emissions...) Conduct the performance test annually. (2) Conduct the performance test when your adipic acid production...

Decolorization of the azo dye Acid Orange 51 by laccase produced in solid culture of a newly isolated Trametes trogii strain

OpenAIRE

Daâssi, Dalel; Zouari-Mechichi, Héla; Frikha, Fakher; Martínez, María Jesús; Nasri, M.; Mechichi, Tahar

2013-01-01

This study concerns the decolorization and detoxification of the azo dye Acid Orange 51 (AO51) by crude laccase from Trametes trogii produced in solid culture using sawdust as support media. A three-level Box?Behnken factorial design with four factors (enzyme concentration, 1-hydroxybenzotriazole (HBT) concentration, dye concentration and reaction time) combined with response surface methodology was applied to optimize AO51 decolorization. A mathematical model was developed showing the effect...

Graphene quantum dots as the electrolyte for solid state supercapacitors

Science.gov (United States)

Zhang, Su; Li, Yutong; Song, Huaihe; Chen, Xiaohong; Zhou, Jisheng; Hong, Song; Huang, Minglu

2016-01-01

We propose that graphene quantum dots (GQDs) with a sufficient number of acidic oxygen-bearing functional groups such as -COOH and -OH can serve as solution- and solid- type electrolytes for supercapacitors. Moreover, we found that the ionic conductivity and ion-donating ability of the GQDs could be markedly improved by simply neutralizing their acidic functional groups by using KOH. These neutralized GQDs as the solution- or solid-type electrolytes greatly enhanced the capacitive performance and rate capability of the supercapacitors. The reason for the enhancement can be ascribed to the fully ionization of the weak acidic oxygen-bearing functional groups after neutralization. PMID:26763275

Zeolite-catalysed preparation of alpha-hydroxy carboxylic acids and esters thereof

DEFF Research Database (Denmark)

2010-01-01

A process for the production of lactic acid and 2-hydroxy-3-butenoic acid or esters thereof by conversion of glucose, fructose, sucrose, xylose and glycolaldehyde dissolved in a solvent in presence of a solid Lewis acidic catalyst.......A process for the production of lactic acid and 2-hydroxy-3-butenoic acid or esters thereof by conversion of glucose, fructose, sucrose, xylose and glycolaldehyde dissolved in a solvent in presence of a solid Lewis acidic catalyst....

Thermal decomposition of lanthanides (III) and yttrium (III) solid complexes from ethyl ene diamine tetraacetic acid

International Nuclear Information System (INIS)

Mercadante, A.

1991-01-01

Solid state compounds of lanthanides (III) and yttrium derived from ethyl ene diamine tetraacetic acid were prepared from respective basic carbonates, that were neutralized with EDTA stoichiometry quantities. Complexometry with EDTA, thermogravimetry (TG), differential thermal analysis (DTA) and X-ray diffraction have been used in the study of these compounds. The results of complexometry with EDTA as well as TG and DTA curves bed to the stoichiometry of these compounds the following general formula is obeyed: H[Ln(EDTA]. n H 2 O. X-ray powder patterns of these compounds permitted to establish two isomorphous series. The DTA ant TG curves allowed us to study the dehydration process, the thermal stability and thermal decomposition of these compounds. (C.G.C.)

Semi-Batch Reactive Distillation of Consecutive Reaction : The Saponification Reaction of Diethyl Adipate with Sodium Hydroxide Solution

Directory of Open Access Journals (Sweden)

Raghad Fareed Kasim

2016-03-01

Full Text Available This research presents a new study in reactive distillation by using consecutive reaction: the saponification reaction of diethyl adipate (DA with sodium hydroxide solution . The effect of three parameters were studied through a design of experiments applying 23 factorial design . These parameters were : the mole ratio of DA to NaOH solution (0.1 and 1 , NaOH solution concentration (3 N and 8 N , and batch time (1.5 hr. and 3.5 hr. . The conversion of DA to sodium monoethyladipate(SMA(intermediate product was the effect of these parameters which was detected . Also , the percentage purity of the intermediate product was recorded . The results showed that increasing mole ratio of DA to NaOHsolution increases the conversion and percentage purity to a maximum value within the range of study . The effect of NaOH solution concentration decreases the conversion and percentage purity to specified value within the range of study . The effect of batch time on conversion and percentage purity , when NaOH solution concentration (3 N is as follows : the increasing in batch time decreases the conversion and percentage purity to specified value within the range of study . When NaOH solution concentration (8 N increasing batch time decreases the conversion , while percentage purity increases with increasing batch time to a maximum value within the range of study . The maximum attainable conversion within the studied range of parameters was eighteen fold of the base case , while the maximum percentage purity was (99.40 % . Empirical equation was obtained using statistical analysis of experimental results . The empirical results of relative conversion was drawn . The empirical graphs showed linear variation .

Investigations on dendrimer space reveal solid and liquid tumor growth-inhibition by original phosphorus-based dendrimers and the corresponding monomers and dendrons with ethacrynic acid motifs.

Science.gov (United States)

El Brahmi, Nabil; Mignani, Serge M; Caron, Joachim; El Kazzouli, Saïd; Bousmina, Mosto M; Caminade, Anne-Marie; Cresteil, Thierry; Majoral, Jean-Pierre

2015-03-07

The well-known reactive diuretic ethacrynic acid (EA, Edecrin), with low antiproliferative activities, was chemically modified and grafted onto phosphorus dendrimers and the corresponding simple branched phosphorus dendron-like derivatives affording novel nanodevices showing moderate to strong antiproliferative activities against liquid and solid tumor cell lines, respectively.

Pyridoxine-dependent epilepsy owing to antiquitin deficiency - mutation in the ALDH7A1 gene

NARCIS (Netherlands)

Jagadeesh, S.; Suresh, B.; Murugan, V.; Suresh, S.; Salomons, G.S.; Struys, E.A.; Jacobs, C.

2013-01-01

Pyridoxine-dependent epilepsy (PDE) is an inborn error of metabolism resulting from antiquitin deficiency. There is marked elevation of a-amino adipic semi-aldehyde (aAASA), piperidine-6-carboxylate (P6C) and pipecolic acid. The diagnosis can be confirmed by identifying the mutation in the ALDH7A1

Nuclear dynamics in the metastable phase of the solid acid caesium hydrogen sulfate.

Science.gov (United States)

Krzystyniak, Maciej; Drużbicki, Kacper; Fernandez-Alonso, Felix

2015-12-14

High-resolution spectroscopic measurements using thermal and epithermal neutrons and first-principles calculations within the framework of density-functional theory are used to investigate the nuclear dynamics of light and heavy species in the metastable phase of caesium hydrogen sulfate. Within the generalised-gradient approximation, extensive calculations show that both 'standard' and 'hard' formulations of the Perdew-Burke-Ernzerhof functional supplemented by Tkatchenko-Scheffler dispersion corrections provide an excellent description of the known structure, underlying vibrational density of states, and nuclear momentum distributions measured at 10 and 300 K. Encouraged by the agreement between experiment and computational predictions, we provide a quantitative appraisal of the quantum contributions to nuclear motions in this solid acid. From this analysis, we find that only the heavier caesium atoms reach the classical limit at room temperature. Contrary to naïve expectation, sulfur exhibits a more pronounced quantum character relative to classical predictions than the lighter oxygen atom. We interpret this hitherto unexplored nuclear quantum effect as arising from the tighter binding environment of this species in this technologically relevant material.

Humic acid-bonded silica as a novel sorbent for solid-phase extraction of benzo[a]pyrene in edible oils

International Nuclear Information System (INIS)

Luo Dan; Yu Qiongwei; Yin Hongrui; Feng Yuqi

2007-01-01

A novel solid-phase extraction (SPE) sorbent, humic acid-bonded silica (HAS), was prepared. Humic acids (HAs) were grafted onto silica matrices via an amide linkage between humyl chloride and the amido terminus of 3-aminopropyltrimethoxysilane (APTS)-silica gel. The resulting material was characterized by Fourier transform infrared spectrometer, elemental analysis, and nitrogen adsorption analysis. This sorbent exhibits an excellent adsorption capacity for some electron-abundant analytes owing to its peculiar structure. In this paper, we choose benzo[a]pyrene (BaP) in oil as a probe to validate the adsorption capacity of the material. Thus a fast, cheap and simple SPE method with humic acid-bonded silica cartridge for edible oil clean-up, followed by high-performance liquid chromatography (HPLC) with fluorescence detection was established. The effects of experimental variables, such as washing and elution solvents, and the amount of sorbents have been studied. The recoveries of BaP in edible oils spiked at 0.2-100 μg kg -1 were in the range of 78.8-102.7% with relative standard deviations ranging between 1.3 and 9.3%; the limit of detection was -0.06 μg kg -1

Production of furfural from xylose, water-insoluble hemicelluloses and water-soluble fraction of corncob via a tin-loaded montmorillonite solid acid catalyst.

Science.gov (United States)

Li, Huiling; Ren, Junli; Zhong, Linjie; Sun, Runcang; Liang, Lei

2015-01-01

The conversion of xylose, water-insoluble hemicelluloses (WIH) and water-soluble fraction (WSF) of corncob to furfural was performed using montmorillonite with tin ions (Sn-MMT) containing double acid sites as a solid acid catalyst. The co-existence of Lewis acids and Brønsted acids in Sn-MMT was shown to improve the furfural yield and selectivity. 76.79% furfural yield and 82.45% furfural selectivity were obtained from xylose using Sn-MMT as a catalyst in a biphasic system with 2-s-butylphenol (SBP) as the organic extracting layer and dimethyl sulfoxide (DMSO) as the co-solvent in contact with an aqueous phase saturated with NaCl (SBP/NaCl-DMSO) at 180°C for 30min. Furthermore, Sn-MMT also demonstrated the excellent catalytic performance in the conversion of pentose-rich materials of corncob and 39.56% and 54.15% furfural yields can be directly obtained from WIH and WSF in the SBP/NaCl-DMSO system, respectively. Copyright © 2014 Elsevier Ltd. All rights reserved.

Preparation and investigation of mefenamic acid – polyethylene glycol – sucrose ester solid dispersions

Directory of Open Access Journals (Sweden)

Fülöp Ibolya

2015-12-01

Full Text Available Mefenamic acid (MA is a widely used non-steroidal antiinflammatory (NSAID drug. The adverse effects typical of NSAIDs are also present in the case of MA, partly due to its low water solubility. The aim of this study was to increase the water solubility of MA in order to influence its absorption and bioavailability. Solid dispersions of MA were prepared by the melting method using polyethylene glycol 6000 and different types (laurate, D-1216; palmitate, P-1670; stearate, S-1670 and amounts of sucrose esters as carriers. The X-ray diffraction results show that MA crystals were not present in the products. Dissolution tests carried out in artificial intestinal juice showed that the product containing 10 % D-1216 increased water solubility about 3 times. The apparent permeability coefficient of MA across human Caco-2 intestinal epithelial cell layers was high and, despite the difference in solubility, there was no further increase in drug penetration in the presence of the applied additives.

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

Science.gov (United States)

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

2008-03-03

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

[Determination of fatty acid esters of chloropropanediols in diet samples by gas chromatography-mass spectrometry coupled with solid-supported liquid-liquid extraction].

Science.gov (United States)

Gao, Jie; Liu, Qing; Han, Feng; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

2014-05-01

To establish a method for the determination of fatty acid esters of 3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD) in diet samples by gas chromatography-mass spectrometry (GC-MS) with solid-supported liquid-liquid extraction (SLE). Diet samples were ultrasonically extracted by hexane, followed by ester cleavage reaction with sodium methylate in methanol, and then purified by solid-supported liquid-liquid extraction. (SLE) using diatomaceous earth as the sorbent. After derivatization with heptafluorobutyrylimidazole, the analytes were detected by GC-MS and quantified by the deuterated internal standards. The limits of detection (LODs) of 3-MCPD esters and 2-MCPD esters in different diet samples were 0.002 - 0.005 mg/kg and 0.002 - 0.006 mg/kg. The average recoveries of 3-MCPD esters and 2-MCPD esters at the spiking levels of 0.05 and 0.1 mg/kg in the diet samples were in the range of 65.9% - 104.2% and 75.4% - 118.0%, respectively, with the relative standard deviations in the range of 2.2% - 14.2% and 0.8% - .13.9%. The method is simple, accurate and rugged for the determination of fatty acid esters of 3-MCPD and 2-MCPD in diet samples.

Viability of lactobacillus acidophilus in various vaginal tablet formulations

Directory of Open Access Journals (Sweden)

Fazeli M.R.

2006-07-01

Full Text Available The lactobacilli which are present in vaginal fluids play an important role in prevention of vaginosis and there are considerable interests in formulation of these friendly bacteria into suitable pharmaceutical dosage forms. Formulating these microorganisms for vaginal application is a critical issue as the products should retain viability of lactobacilli during formulation and also storage. The aim of this study was to examine the viability and release of Lactobacillus acidophilus from slow-release vaginal tablets prepared by using six different retarding polymers and from two effervescent tablets prepared by using citric or adipic acid. The Carbomer–based formulations showed high initial viablility compared to those based on HPMC-LV, HPMC-HV, Polycarbophil and SCMC polymers which showed one log decrease in viable cells. All retarding polymers in slow release formulations presented a strong bacterial release at about 2 h except Carbomer polymers which showed to be poor bacterial releasers. Although effervescent formulations produced a quick bacterial release in comparison with polymer based slow-release tablets, they were less stable in cold storage. Due to the strong chelating characteristic of citric acid, the viability was quickly lost for aqueous medium of citric acid in comparison with adipic acid based effervescent tablets.

Pretreatment of various feedstocks for lactic acid production: detection of sugars, organic acids and furanics in liquid fractions

NARCIS (Netherlands)

Harmsen, P.F.H.; Lips, S.J.J.; Bakker, R.R.C.

2012-01-01

Barley straw, sugarcane bagasse and empty fruit bunches were pretreated under acid- and alkaline conditions. Solid phase was separated from the liquid phase and the concentration of dissolved monomeric sugars, organic acids and furanics was determined. Acid hydrolysis yielded monomeric xylose

Sequential batch anaerobic composting (SEBAC sup TM ) of solid wastes

Energy Technology Data Exchange (ETDEWEB)

Chynoweth, D.P.; O' Keefe, D.M.; Barkdoll, A.W.; Owens, J.M. (Department of Agricultural Engineering, University of Florida, Gainesville, Florida (US)); Legrand, R. (Radian Corporation, Austin, Texas (US))

1992-01-01

Anaerobic high-solids digestion (anaerobic composting) is an attractive option for treatment of organic wastes. The main advantages of anaerobic composting are the lack of aeration requirements and production of methane. An anaerobic composting design, sequential batch anaerobic composting (SEBAC{sup TM}), has been developed and demonstrated at the pilot scale which has proven to be stable and effective for treatment of the non-yeard waste and yard waste organic fractions of municipal solid waste (MSW). The design employs leachate recycle for wetting, inoculation, and removal of volatile organic acids during startup. Performance is similar to that of other designs requiring heavy solids inoculation and mixing and which do not have a mechanism for volatile organic acid removal during imbalance. (au) (12 refs.).

Synthesis of bio-based methacrylic acid by decarboxylation of itaconic acid and citric acid catalyzed by solid transition-metal catalysts.

Science.gov (United States)

Le Nôtre, Jérôme; Witte-van Dijk, Susan C M; van Haveren, Jacco; Scott, Elinor L; Sanders, Johan P M

2014-09-01

Methacrylic acid, an important monomer for the plastics industry, was obtained in high selectivity (up to 84%) by the decarboxylation of itaconic acid using heterogeneous catalysts based on Pd, Pt and Ru. The reaction takes place in water at 200-250 °C without any external added pressure, conditions significantly milder than those described previously for the same conversion with better yield and selectivity. A comprehensive study of the reaction parameters has been performed, and the isolation of methacrylic acid was achieved in 50% yield. The decarboxylation procedure is also applicable to citric acid, a more widely available bio-based feedstock, and leads to the production of methacrylic acid in one pot in 41% selectivity. Aconitic acid, the intermediate compound in the pathway from citric acid to itaconic acid was also used successfully as a substrate. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Municipal solid waste compost as a novel sorbent for antimony(V): adsorption and release trials at acidic pH.

Science.gov (United States)

Diquattro, Stefania; Garau, Giovanni; Lauro, Gian Paolo; Silvetti, Margherita; Deiana, Salvatore; Castaldi, Paola

2018-02-01

The ability of two municipal solid waste composts (MSW-Cs) to sorb antimony(V) in acidic conditions (pH 4.5) was investigated. Sorption isotherms and kinetics showed that both MSW-Cs could sorb antimony(V), even if in different amounts (~ 0.18 and 0.24 mmol g -1 of Sb(V) by MSW-C1 and MSW-C2, respectively). These differences were ascribed to the chemical composition of composts, as well as to the total acidity of their humic substances. The Sb(V) sorption by both MSW-Cs followed a pseudo-second-order kinetic model, while the sorption isotherms data fitted the Freundlich model better than the Langmuir one. The humic acids extracted from composts contributed to 4.26 and 8.24% of Sb(V) sorption by MSW-C1 and MSW-C2 respectively. SEM-EDX spectra of the MSW-C+Sb(V) systems showed a certain association of Ca(II) with Sb(V), while sequential extraction procedures indicated that more than 80% of the Sb(V) sorbed was strongly retained by MSW-Cs. On the other hand, treatment with oxalic acid at pH 4.5 favored the release of more than 98 and 65% of the Sb(V) sorbed by MSW-C1 and MSW-C2 respectively, supporting a possible role of calcium in Sb(V) retention. The results from this study suggest that MSW-Cs could be used as amendments for the in-situ immobilization of Sb(V) in acidic-polluted soils.

Recovering folic acid and its identification on mixed pastes of tempeh and fermented vegetable as natural source of folic acid

Science.gov (United States)

Susilowati, Agustine; Aspiyanto, Maryati, Yati; Melanie, Hakiki; Lotulung, Puspa D.

2017-11-01

Mixing between tempeh and both fermented broccoli (Brassica oleracea) and spinach (Amaranthus sp.) were conducted to achieve mixed pastes as natural source of folic acid for 'smart food'. Mixing was performed on soy, mung bean, and kidney bean tempehs with both fermented broccoli and spinach at ratio of 1 : 1, 1 : 2, 1 : 3, 1 : 4, 1 : 5 and 1 : 6, respectively. Result of experimental activity showed that pulverizing ratio becoming more and more low will decrease total solids, soluble protein and N-Amino, but fluctuates on folic acid in mixed paste. Based on folic acid equivalent and the best fermented vegetable efficiency, optimization condition was reached in paste with combination between mung beans tempeh and fermented spinach at ratio of 1 : 2 by increasing folic acid concentration of 83.18 % (0.83 times), dissolved protein 432.29 % (4.32 times) and N-amino 55.36 % (0,55 times). While, it is occurred a lowering total solids 22.16 % (0.22 times) when compared with folic acid, soluble protein, N-amino, and total solids on initial materials of mung bean tempeh. In this condition, it is achieved folic acid monomer with molecular weight (MW) 148.14 Da. with relative intensity 100 %, and glutamic acid monomer 443.50 Da.with relative intensity 0.07 %.

Mechanochemically assisted solid-state and citric acid complex syntheses of Cu-doped sodium cobaltite ceramics

International Nuclear Information System (INIS)

Pršić, S.; Savić, S.M.; Branković, Z.; Vrtnik, S.; Dapčević, A.; Branković, G.

2015-01-01

Highlights: • Sodium cobaltite was synthesized by mechanochemically assisted solid-state reaction and citric acid complex (CAC) method. • We investigated effect of Cu-doping in NaCo 2−x Cu x O 4 (x = 0, 0.01, 0.03, 0.05). • ICP analysis showed that the controlling of the samples composition is easier by the CAC method. • The Seebeck coefficient in Cu-doped samples was higher compared to the undoped one. • The highest figure of merit was observed in the sample with the lowest Cu concentration. - Abstract: In the last decade, the sodium cobaltite ceramic became a promising candidate for potential thermoelectric applications, because of its large thermopower and low resistivity. In this work, polycrystalline samples of NaCo 2−x Cu x O 4 (x = 0, 0.01, 0.03, 0.05) were prepared using mechanochemically assisted solid-state reaction method (MASSR) and the citric acid complex method (CAC). Bulk samples were prepared by pressing into disc-shaped pellets and subsequently subjected to a thermal treatment at 880 °C in inert argon atmosphere. Changes in structural and microstructural characteristics of the samples, caused by the substitution of Cu for Co, were characterized using X-ray diffraction (XRD) analysis, and scanning electron microscopy (SEM), respectively. The results of inductively coupled plasma (ICP) analysis showed that the compositions of the final products correspond to γ-NaCo 2 O 4 and confirmed that desired compound was obtained in both syntheses procedures. The advantages and disadvantages of these two syntheses procedures have been observed and discussed: the CAC method enabled obtaining samples with higher density and fine microstructure compared to the MASSR method, thus better thermoelectric properties. The Cu 2+ substitution led to the increase in Seebeck coefficient in both synthesis routes. The highest figure of merit of 0.022 at 300 K was observed for the sample doped with 1 mol% Cu, obtained by the CAC method, and it was almost twice

Mechanochemically assisted solid-state and citric acid complex syntheses of Cu-doped sodium cobaltite ceramics

Energy Technology Data Exchange (ETDEWEB)

Pršić, S., E-mail: sanjaprsic@imsi.bg.ac.rs [Institute for Multidisciplinary Research, University of Belgrade, Kneza Višeslava 1, 11030 Belgrade (Serbia); Savić, S.M., E-mail: slavicas@imsi.bg.ac.rs [Institute for Multidisciplinary Research, University of Belgrade, Kneza Višeslava 1, 11030 Belgrade (Serbia); Branković, Z., E-mail: zorica.brankovic@imsi.bg.ac.rs [Institute for Multidisciplinary Research, University of Belgrade, Kneza Višeslava 1, 11030 Belgrade (Serbia); Vrtnik, S., E-mail: stane.vrtnik@ijs.si [Institute Jožef Stefan, Condensed Matter Physics, Jamova cesta 39, 1000 Ljubljana (Slovenia); Dapčević, A., E-mail: hadzi-tonic@tmf.bg.ac.rs [Department of General and Inorganic Chemistry, Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, 11120 Belgrade (Serbia); Branković, G., E-mail: goran.brankovic@imsi.bg.ac.rs [Institute for Multidisciplinary Research, University of Belgrade, Kneza Višeslava 1, 11030 Belgrade (Serbia)

2015-08-15

Highlights: • Sodium cobaltite was synthesized by mechanochemically assisted solid-state reaction and citric acid complex (CAC) method. • We investigated effect of Cu-doping in NaCo{sub 2−x}Cu{sub x}O{sub 4} (x = 0, 0.01, 0.03, 0.05). • ICP analysis showed that the controlling of the samples composition is easier by the CAC method. • The Seebeck coefficient in Cu-doped samples was higher compared to the undoped one. • The highest figure of merit was observed in the sample with the lowest Cu concentration. - Abstract: In the last decade, the sodium cobaltite ceramic became a promising candidate for potential thermoelectric applications, because of its large thermopower and low resistivity. In this work, polycrystalline samples of NaCo{sub 2−x}Cu{sub x}O{sub 4} (x = 0, 0.01, 0.03, 0.05) were prepared using mechanochemically assisted solid-state reaction method (MASSR) and the citric acid complex method (CAC). Bulk samples were prepared by pressing into disc-shaped pellets and subsequently subjected to a thermal treatment at 880 °C in inert argon atmosphere. Changes in structural and microstructural characteristics of the samples, caused by the substitution of Cu for Co, were characterized using X-ray diffraction (XRD) analysis, and scanning electron microscopy (SEM), respectively. The results of inductively coupled plasma (ICP) analysis showed that the compositions of the final products correspond to γ-NaCo{sub 2}O{sub 4} and confirmed that desired compound was obtained in both syntheses procedures. The advantages and disadvantages of these two syntheses procedures have been observed and discussed: the CAC method enabled obtaining samples with higher density and fine microstructure compared to the MASSR method, thus better thermoelectric properties. The Cu{sup 2+} substitution led to the increase in Seebeck coefficient in both synthesis routes. The highest figure of merit of 0.022 at 300 K was observed for the sample doped with 1 mol% Cu, obtained by

The Effects of Cobalt-60 Gamma Radiation on Vitamin B{sub 6} and Folic Acid; Effets des rayons gamma (cobalt-60) sur la vitamine B{sub 6} et l’acide folique

Energy Technology Data Exchange (ETDEWEB)

Galatzeanu, I.; Antoni, F. [International Atomic Energy Agency, Vienna (Austria)

1967-09-15

A study has been made of the behaviour of pyridoxine and folic acid, including structural changes, after {sup 60}Co gamma irradiation. The irradiation of pyridoxine (vitamin B{sub 6}) and folic acid in aqueous solutions leads to their partial or total destruction, depending on the dose. The irradiation of pyridoxine and folic acid in the solid state mainly results in the elimination of hydrogen atoms (free radicals). After dissolving the irradiated samples in acid solutions it was observed that the irradiated molecule was renewed through replacement of the eliminated hydrogen atoms, which depend on the pH-value of the solution. This gives the possibility of sterilizing both pyridoxine and folic acid in the solid state by irradiation at 2 Mrad. Most of the radiolysis products of pyridoxine and folic acid irradiated in solution and in the solid state have been separated and identified by means of chromatography (paper and thin layer) and cellulose column electrophoresis. Electron spin resonance was used to determine the concentration and nature of the free radicals after irradiation of pyridoxine and folic acid in the solid state. (author) [French] On a Studie le comportement de la pyridoxine et de l'acide folique apres exposition aux rayons gamma ({sup 60}Co) et les changements dans leurs structures. L'irradiation de la pyridoxine (Vitamine B{sub 6}) et de l'acide folique en solutions aqueuses enttarne leur destruction partielle ou totale selon la dose. L'irradiation de la pyridoxine et de l'acide folique á l'etat solide enttarne principalement l'elimination d'atomes d'hydrogene (radicaux libres). Par dissolution des echanrilions irradies dans des solutions acides, on a observe un renouvellement de la molecule irradiee par remplacement des atomes d'hydrogene elimines qui est fonction du pH de la solution, ce qui permet de radiosteriliser a 2 Mrad á l'etat solide tant la pyridoxine que l'acide folique. On a separe et identifie la majorite des produits de radiolyse

Interaction of acid mine drainage with Ordinary Portland Cement blended solid residues generated from active treatment of acid mine drainage with coal fly ash.

Science.gov (United States)

Gitari, Wilson M; Petrik, Leslie F; Key, David L; Okujeni, Charles

2011-01-01

Fly ash (FA) has been investigated as a possible treatment agent for Acid mine drainage (AMD) and established to be an alternative, cheap and economically viable agent compared to the conventional alkaline agents. However, this treatment option also leads to generation of solid residues (SR) that require disposal and one of the proposed disposal method is a backfill in coal mine voids. In this study, the interaction of the SR with AMD that is likely to be present in such backfill scenario was simulated by draining columns packed with SR and SR + 6% Ordinary Portland Cement (OPC) unsaturated with simulated AMD over a 6 month period. The evolving geochemistry of the liquid/solid (L/S) system was evaluated in-terms of the mineral phases likely or controlling contaminants attenuation at the different pH regimes generated. Stepwise acidification of the percolates was observed as the drainage progressed. Two pH buffer zones were observed (7.5-9 and 3-4) for SR and (11.2-11.3 and 3.5-4) for SR + 6% OPC. The solid residue cores (SR) appeared to have a significant buffering capacity, maintaining a neutral to slightly alkaline pH in the leachates for an extended period of time (97 days: L/S 4.3) while SR + 6% OPC reduced this neutralization capacity to 22 days (L/S 1.9). Interaction of AMD with SR or SR + 6% OPC generated alkaline conditions that favored precipitation of Fe, Al, Mn-(oxy) hydroxides, Fe and Ca-Al hydroxysulphates that greatly contributed to the contaminants removal. However, precipitation of these phases was restricted to the pH of the leachates remaining at neutral to circum-neutral levels. Backfill of mine voids with SR promises to be a feasible technology for the disposal of the SR but its success will greatly depend on the disposal scenario, AMD generated and the alkalinity generating potential of the SR. A disadvantage would be the possible re-dissolution of the precipitated phases at pH water column. However extrapolation of this concept to a field

Heat-shrink tubing as a solid-phase microextraction coating for the enrichment and determination of phthalic acid esters.

Science.gov (United States)

Luo, Xi; He, Chengxia; Zhang, Feifang; Wang, Hailong; Yang, Bingcheng; Liang, Xinmiao

2014-12-01

Heat-shrink tubing, which shrinks in one plane only (its diameter) when heated, commonly used for sealing protection in electrical engineering, was found to be able to function as a solid-phase microextraction coating. Its utility was demonstrated for the determination of phthalic acid esters in an aqueous solution combined with high-performance liquid chromatography equipped with a UV absorbance detector. The preparation procedure was rather simple and only ∼10 min was needed. The fiber cost is extremely low (∼10 cent each). The parameters affecting the extraction were optimized. Heat-shrink tubing fiber exhibited a significant enrichment effect for the three examined phthalic acid esters and up to 931-fold enrichment factor was obtained. The limit of detection was <10 μg/L for all analytes. The operation repeatability and fiber-to-fiber reproducibility were 1.2-8.3 and 5.4-9.1%, respectively. It was successfully applied for the analysis of bottled drinking water with recoveries ranging from 90.1-100.5%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of initial total solids concentration on volatile fatty acid production from food waste during anaerobic acidification.

Science.gov (United States)

Wang, Quan; Jiang, Jianguo; Zhang, Yujing; Li, Kaimin

2015-01-01

The effect of initial total solids (TS) concentration on volatile fatty acid (VFAs) production from food waste under mesophilic conditions (35 °C) was determined. VFAs concentration and composition, biogas production, soluble chemical oxygen demand concentration, TS and volatile solids (VS) reduction, and ammonia nitrogen [Formula: see text] release were investigated. The VFAs concentrations were 26.10, 39.68, 59.58, and 62.64 g COD/L at TS contents of 40, 70, 100, and 130 g/L, respectively. While the VFAs' yields ranged from 0.467 to 0.799 g COD/g VSfed, decreased as initial TS increased. The percentage of propionate was not affected by TS concentration, accounting for 30.19-34.86% of the total VFAs, while a higher percentage of butyrate and lower percentage of acetate was achieved at a higher TS concentration. Biogas included mainly hydrogen and carbon dioxide and the maximum hydrogen yield of 148.9 ml/g VSfed was obtained at 130 g TS/L. [Formula: see text] concentration, TS and VS reductions increased as initial TS increased. Considering the above variables, we conclude that initial TS of 100 g/L shall be the most appropriate to VFAs production.

The solid-state structures of organic salts formed by calix[4]arene dihydroxyphosphonic acid with nucleic bases cations: adeninium, cytosinium, guaninium and uracilium

KAUST Repository

Shkurenko, Aleksander

2018-02-19

Calix[4]arene dihydroxyphosphonic acid has been demonstrated to possess an interesting range of biological properties, including atypical anti-cancer activity. The robustness of calix[4]arene dihydroxyphosphonic acid and its ubiquitous dimeric motif offers perspectives for pre-defined solid state complexation with small molecules. In the current article we describe co-crystals (organic salts) of calix[4]arene dihydroxyphosphonic acid with four nucleic base cations: adeninium, cytosinium, guaninium and uracilium. A number of characteristic interactions between the components in the four co-crystals are pointed out also using the Hirshfeld surface analysis. All the four co-crystals are based on layers of calix[4]arene dimers, alternating with layers of nucleic acid molecules. Two of the reported crystal structures (cytosinium and guaninium) are 1D channel-type structures, while the two others (adeninium and uracilium) represent 2D channel-type structures. In three out of four reported structures, interactions between the cations of nucleic bases are present generating 1D chains of cations. A constant motif is that the nucleic base is present in a type of cavity formed by one aromatic ring and a phosphonic acid moiety.

A phase I pharmacokinetic study of ursolic acid nanoliposomes in healthy volunteers and patients with advanced solid tumors

Directory of Open Access Journals (Sweden)

Ying G

2013-01-01

Full Text Available Zhongling Zhu,1,4 Zhengzi Qian,2,4 Zhao Yan,1,4 Cuicui Zhao,2,4 Huaqing Wang,2,4 Guoguang Ying3,41Department of Clinical Pharmacology, 2Department of Lymphoma, 3Laboratory of Tumor Cell Biology, Tianjin Medical University Cancer Institute and Hospital, Tianjin, People's Republic of China; 4Key Laboratory of Cancer Prevention and Therapy, Tianjin, People’s Republic of ChinaBackground: Ursolic acid is a promising anticancer agent. The current study aims to evaluate the single- and multiple-dose pharmacokinetics (PK as well as the safety of ursolic acid nanoliposomes (UANL in healthy volunteers and in patients with advanced solid tumors.Methods: Twenty-four healthy volunteers in the single-dose PK study were divided into three different groups, which received 37, 74, and 98 mg/m2 of UANL. Eight patients in the multiple-dose PK study were administered with 74 mg/m2 of UANL daily for 14 days. The UA plasma concentrations were determined using ultra-performance liquid chromatograph-tandem mass spectrometry.Results: The plasma concentration profiles of all subjects were characterized by a biexponential decline after infusion. The mean peak plasma concentration (Cmax increased linearly as a function of the dose (r = 0.999. The mean area under the plasma concentration-time curve (AUC from 0 to 16 hours also increased proportionally with dose escalation (r = 0.998. However, the clearance was constant over the specific dose interval. In the multiple-dose PK study, the trough and average concentrations remained low. The mean AUC, half-life, Cmax, time to Cmax, and the volume of distribution on the first day were similar to those on the last day. All subjects tolerated the treatments well. Most UANL-associated adverse events varied from mild to moderate.Conclusions: UANL exhibits relatively linear PK behavior with dose levels from 37 mg/m2 to 98 mg/m2. No drug accumulation was observed with repeated doses of UANL. The intravenous infusion of UANL was well

SOLID-PHASE PEPTIDE SYNTHESIS OF ISOTOCIN WITH AMIDE ...

African Journals Online (AJOL)

SOLID-PHASE PEPTIDE SYNTHESIS OF ISOTOCIN WITH AMIDE OF ASPARAGINE PROTECTED WITH 1-TETRALINYL. TRIFLUOROMETHANESULPHONIC ACID (TFMSA) DEPROTECTION, CLEAVAGE AND AIR OXIDATION OF MERCAPTO GROUPS TO DISULPHIDE.

Osteoconductive bio-based meshes based on Poly(hydroxybutyrate-co-hydroxyvalerate) and poly(butylene adipate-co-terephthalate) blends

International Nuclear Information System (INIS)

Nar, Mangesh; Staufenberg, Gerrit; Yang, Bing; Robertson, Lesli; Patel, Rinkesh H.; Varanasi, Venu G.; D'Souza, Nandika Anne

2014-01-01

Poly(butylene adipate-co-terephthalate) (PBAT) and Poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV) are biopolymers that have the potential to be used in applications of bone healing. In this study, it is hypothesized that the polymer blend has the combined strength and osteoconductivity to support osteoblast collagen formation. PBAT (PBAT 100), and a blend with 20% PHBV (PBAT 80) were extruded in the form of fibers and then knitted in the form of mesh. These were tested in the warp as well as weft direction for the tensile properties; these showed that the weft direction had higher performance than the warp. The individual fibers were kept in phosphate buffered saline (PBS) over the period of 8 weeks and were tested for the storage and loss modulus using a dynamic mechanical analyser (DMA). The results indicated that mechanical relaxation strength showed a decrease and then an increase. In vitro osteoconductivity studies were done by using differentiating osteoblasts (MC3T3-E1 subclone 4 cells). Environmental Scanning Electron Microscopy (ESEM) showed that pre-soaking the samples in α-MEM for two weeks resulted in cell attachment and growth. X-ray diffraction (XRD) was used to determine the change in structure of polymers due to in vitro degradation for two weeks. Raman spectroscopy showed that all scaffolds supported the formation of a collagenous network over the scaffold surfaces. For a combination of knittable manufacturing, mechanical performance and osteoconductivity, blends offer an effective route. - Highlights: • PBAT and PHBV blend can be knitted to form mesh with good mechanical properties. • PBAT and PHBV blend do not show significant weight loss over a period of 8 weeks in PBS. • Osteoblast cell culture was done on these samples. • They support extracellular matrix and growth and hence are osteoconductive

Osteoconductive bio-based meshes based on Poly(hydroxybutyrate-co-hydroxyvalerate) and poly(butylene adipate-co-terephthalate) blends

Energy Technology Data Exchange (ETDEWEB)

Nar, Mangesh; Staufenberg, Gerrit; Yang, Bing [Department of Material Science and Engineering, University of North Texas, 1155 Union Circle #305310, Denton, TX 76203-5017 (United States); Robertson, Lesli [Department of Fibers, College of Visual Arts and Design, 1155 Union Circle #305100, Denton, TX 76203-5017 (United States); Patel, Rinkesh H. [Department of Biomedical Sciences and Center for Craniofacial Research and Diagnosis, Texas A and M University Baylor College of Dentistry, Dallas, TX 75246 (United States); Varanasi, Venu G., E-mail: vvaranasi@bcd.tamhsc.edu [Department of Biomedical Sciences and Center for Craniofacial Research and Diagnosis, Texas A and M University Baylor College of Dentistry, Dallas, TX 75246 (United States); D' Souza, Nandika Anne, E-mail: nandika.dsouza@unt.edu [Department of Material Science and Engineering, University of North Texas, 1155 Union Circle #305310, Denton, TX 76203-5017 (United States); Department of Mechanical and Energy Engineering, University of North Texas, 1155 Union Circle # 311098, Denton, TX 76203-5017 (United States)

2014-05-01

Poly(butylene adipate-co-terephthalate) (PBAT) and Poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV) are biopolymers that have the potential to be used in applications of bone healing. In this study, it is hypothesized that the polymer blend has the combined strength and osteoconductivity to support osteoblast collagen formation. PBAT (PBAT 100), and a blend with 20% PHBV (PBAT 80) were extruded in the form of fibers and then knitted in the form of mesh. These were tested in the warp as well as weft direction for the tensile properties; these showed that the weft direction had higher performance than the warp. The individual fibers were kept in phosphate buffered saline (PBS) over the period of 8 weeks and were tested for the storage and loss modulus using a dynamic mechanical analyser (DMA). The results indicated that mechanical relaxation strength showed a decrease and then an increase. In vitro osteoconductivity studies were done by using differentiating osteoblasts (MC3T3-E1 subclone 4 cells). Environmental Scanning Electron Microscopy (ESEM) showed that pre-soaking the samples in α-MEM for two weeks resulted in cell attachment and growth. X-ray diffraction (XRD) was used to determine the change in structure of polymers due to in vitro degradation for two weeks. Raman spectroscopy showed that all scaffolds supported the formation of a collagenous network over the scaffold surfaces. For a combination of knittable manufacturing, mechanical performance and osteoconductivity, blends offer an effective route. - Highlights: • PBAT and PHBV blend can be knitted to form mesh with good mechanical properties. • PBAT and PHBV blend do not show significant weight loss over a period of 8 weeks in PBS. • Osteoblast cell culture was done on these samples. • They support extracellular matrix and growth and hence are osteoconductive.

Heavy metal extraction from PCB wastewater treatment sludge by sulfuric acid

International Nuclear Information System (INIS)

Kuan, Yu-Chung; Lee, I-Hsien; Chern, Jia-Ming

2010-01-01

Heavy metals contaminated wastewater sludge is classified as hazardous solid waste and needs to be properly treated to prevent releasing heavy metals to the environment. In this study, the wastewater treatment sludge from a printed circuit board manufacturing plant was treated in a batch reactor by sulfuric acid to remove the contained heavy metals. The effects of sulfuric acid concentration and solid to liquid ratio on the heavy metal removal efficiencies were investigated. The experimental results showed that the total and individual heavy metal removal efficiencies increased with increasing sulfuric acid concentration, but decreased with increasing solid to liquid ratio. A mathematical model was developed to predict the residual sludge weights at varying sulfuric concentrations and solid to liquid ratios. The trivalent heavy metal ions, iron and chromium were more difficult to be removed than the divalent ions, copper, zinc, nickel, and cadmium. For 5 g/L solid to liquid ratio, more than 99.9% of heavy metals can be removed from the sludge by treating with 0.5 M sulfuric acid in 2 h.

Catalytic reduction of NH4NO3 by NO. Effects of solid acids and implications for low temperature DeNOx processes

International Nuclear Information System (INIS)

Savara, Aditya; Li, Mei-Jun; Sachtler, Wolfgang M.H.; Weitz, Eric

2008-01-01

Ammonium nitrate is thermally stable below 250 C and could potentially deactivate low temperature NO x reduction catalysts by blocking active sites. It is shown that NO reduces neat NH 4 NO 3 above its 170 C melting point, while acidic solids catalyze this reaction even at temperatures below 100 C. NO 2 , a product of the reduction, can dimerize and then dissociate in molten NH 4 NO 3 to NO + + NO 3 - , and may be stabilized within the melt as either an adduct or as HNO 2 formed from the hydrolysis of NO + or N 2 O 4 . The other product of reduction, NH 4 NO 2 , readily decomposes at ≤100 C to N 2 and H 2 O, the desired end products of DeNO x catalysis. A mechanism for the acid catalyzed reduction of NH 4 NO 3 by NO is proposed, with HNO 3 as an intermediate. These findings indicate that the use of acidic catalysts or promoters in DeNO x systems could help mitigate catalyst deactivation at low operating temperatures (<150 C). (author)

21 CFR 186.1093 - Sulfamic acid.

Science.gov (United States)

2010-04-01

... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Sulfamic acid. 186.1093 Section 186.1093 Food and... Substances Affirmed as GRAS § 186.1093 Sulfamic acid. (a) Sulfamic acid (H3NO3S, CAS Reg. No. 5329-14-6) is a white crystalline solid manufactured from urea, sulfur trioxide, and sulfuric acid. It is soluble and...

Synthesis, characterization, and thermochemistry of the solid state coordination compound Zn(Nic){sub 2} . H{sub 2}O(s) (Nic = nicotinic acid)

Energy Technology Data Exchange (ETDEWEB)

Di Youying [College of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, Shandong (China)], E-mail: yydi@lcu.edu.cn; Hong Yuanping; Kong Yuxia; Yang Weiwei [College of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, Shandong (China); Tan Zhicheng [Thermochemistry Laboratory, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023 (China)

2009-01-15

A novel compound, viz. zinc nicotinate monohydrate, was synthesized by the method of room temperature solid phase synthesis. The techniques of FT-IR chemical and elemental analyses and X-ray powder diffraction were applied to characterise the structure and composition of the complex. In accordance with Hess' law, a thermochemical cycle was designed and the enthalpy change of the solid phase reaction of nicotinic acid with hydrated zinc acetate was determined to be {delta}{sub r}H{sub m}{sup 0}=(46.71{+-}0.21)kJ.mol{sup -1} by use of an isoperibol solution-reaction calorimeter. The standard molar enthalpy of formation of the title complex Zn(Nic){sub 2} . H{sub 2}O(s) was calculated as -(1062.3 {+-} 2.0) kJ . mol{sup -1} by use of the enthalpies of dissolution and other auxiliary thermodynamic data.

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.

Acid-functionalized polyolefin materials and their use in acid-promoted chemical reactions

Science.gov (United States)

Oyola, Yatsandra; Tian, Chengcheng; Bauer, John Christopher; Dai, Sheng

2016-06-07

An acid-functionalized polyolefin material that can be used as an acid catalyst in a wide range of acid-promoted chemical reactions, wherein the acid-functionalized polyolefin material includes a polyolefin backbone on which acid groups are appended. Also described is a method for the preparation of the acid catalyst in which a precursor polyolefin is subjected to ionizing radiation (e.g., electron beam irradiation) of sufficient power and the irradiated precursor polyolefin reacted with at least one vinyl monomer having an acid group thereon. Further described is a method for conducting an acid-promoted chemical reaction, wherein an acid-reactive organic precursor is contacted in liquid form with a solid heterogeneous acid catalyst comprising a polyolefin backbone of at least 1 micron in one dimension and having carboxylic acid groups and either sulfonic acid or phosphoric acid groups appended thereto.

Catalytic decomposition of N2O over CeO2 supported Co3O4 catalysts

Indian Academy of Sciences (India)

N2O is a potent greenhouse gas.2 About 40% of global. N2O emissions are a result of human activities. Major sources are agriculture, transportation, combustion of fossil fuels and industries involved in preparation of adipic aid, nitric acid, etc. Apart from these, many natural processes like nitrogen cycle and breakdown.

Solid-phase reduction of silico-12-molybdic acid H4SiMo12O40 by some organic oxygen containing compounds

International Nuclear Information System (INIS)

Chuvaev, V.F.; Pinchuk, I.N.; Spitsyn, V.I.

1982-01-01

A study is made on reduction reactions of anhydrous silico-12-molybdic acid by vapors of organic oxygen-containing compounds at 170 deg C: alcohols, simple carbonyl compounds. Methods of thermal analysis, electron paramagnetic resonance, paramagnetic resonance were used to established that depending on the nature of organic reagent and temperature, H 6 SiMo 2 5 Mo 10 6 O 40 two-electron or H 8 SiMo 4 5 Mo 8 6 O 40 four-electron flues form. It is shown that the increase of heterogeneous reduction temperature can lead to formation of anhydrous phases of SiMo 12 O 38 -(n/2), able to attach water reversibly with formation of corresponding blue. Characteristics of blues, prepared during solid-phase reduction of silico-12-molybdic acid and mixed valent forms with corresponding reduction degree, separated from water solutions, were compared

Sustained Cytotoxicity of Wogonin on Breast Cancer Cells by Encapsulation in Solid Lipid Nanoparticles

Directory of Open Access Journals (Sweden)

Jong-Suep Baek

2018-03-01

Full Text Available While wogonin has been known to have cytotoxicity against various cancer cells, its bioavailability and cytotoxicity are low due to its low water solubility. Therefore, wogonin-loaded solid lipid nanoparticles were fabricated using a hot-melted evaporation technique. The highest solubility of wogonin was observed in stearic acid. Hence, wogonin-loaded solid lipid nanoparticles were composed of stearic acid as the lipid matrix. The physicochemical properties of the wogonin-loaded solid lipid nanoparticles were evaluated by dynamic laser scattering and scanning electron microscopy. The wogonin-loaded solid lipid nanoparticles exhibited sustained and controlled release up to 72 h. In addition, it was observed that the wogonin-loaded solid lipid nanoparticles exhibited enhanced cytotoxicity and inhibited poly (ADP-ribose polymerase in MCF-7 breast cancer cells. Overall, the results indicate that wogonin-loaded solid lipid nanoparticles could be an efficient delivery system for the treatment of breast cancer.

Exploring the Degradation of Gallotannins Catalyzed by Tannase Produced by Aspergillus niger GH1 for Ellagic Acid Production in Submerged and Solid-State Fermentation.

Science.gov (United States)

Chávez-González, Mónica L; Guyot, Sylvain; Rodríguez-Herrera, Raul; Prado-Barragán, Arely; Aguilar, Cristóbal N

2018-06-01

Due to great interest on producing bioactive compounds for functional foods and biopharmaceuticals, it is important to explore the microbial degradation of potential sources of target biomolecules. Gallotannins are polyphenols present in nature, an example of them is tannic acid which is susceptible to enzymatic hydrolysis. This hydrolysis is performed by tannase or tannin acyl hydrolase, releasing in this way, biomolecules with high-added value. In the present study, chemical profiles obtained after fungal degradation of tannic acid under two bioprocesses (submerged fermentation (SmF) and solid state fermentation (SSF)) were determined. In both fermentation systems (SmF and SSF), Aspergillus niger GH1 strain and tannic acid as a sole carbon source and inducer were used (the presence of tannic acid promotes production of enzyme tannase). In case of SSF, polyurethane foam (PUF) was used like as support of fermentation; culture medium only was used in case of submerged fermentation. Fermentation processes were monitored during 72 h; samples were taken kinetically every 8 h; and all extracts obtained were partially purified to obtain polyphenolic fraction and then were analyzed by liquid chromatography-mass spectrometry (LC-MS). Molecules like gallic acid and n-galloyl glucose were identified as intermediates in degradation of tannic acid; during SSF was identified ellagic acid production. The results obtained in this study will contribute to biotechnological production of ellagic acid.

Catalytic Upgrading of Bio-Oil by Reacting with Olefins and Alcohols over Solid Acids: Reaction Paths via Model Compound Studies

Directory of Open Access Journals (Sweden)

Qingwen Wang

2013-03-01

Full Text Available Catalytic refining of bio-oil by reacting with olefin/alcohol over solid acids can convert bio-oil to oxygen-containing fuels. Reactivities of groups of compounds typically present in bio-oil with 1-octene (or 1-butanol were studied at 120 °C/3 h over Dowex50WX2, Amberlyst15, Amberlyst36, silica sulfuric acid (SSA and Cs2.5H0.5PW12O40 supported on K10 clay (Cs2.5/K10, 30 wt. %. These compounds include phenol, water, acetic acid, acetaldehyde, hydroxyacetone, d-glucose and 2-hydroxymethylfuran. Mechanisms for the overall conversions were proposed. Other olefins (1,7-octadiene, cyclohexene, and 2,4,4-trimethylpentene and alcohols (iso-butanol with different activities were also investigated. All the olefins and alcohols used were effective but produced varying product selectivities. A complex model bio-oil, synthesized by mixing all the above-stated model compounds, was refined under similar conditions to test the catalyst’s activity. SSA shows the highest hydrothermal stability. Cs2.5/K10 lost most of its activity. A global reaction pathway is outlined. Simultaneous and competing esterification, etherfication, acetal formation, hydration, isomerization and other equilibria were involved. Synergistic interactions among reactants and products were determined. Acid-catalyzed olefin hydration removed water and drove the esterification and acetal formation equilibria toward ester and acetal products.

Dissolution of Simulated and Radioactive Savannah River Site High-Level Waste Sludges with Oxalic Acid & Citric Acid Solutions

International Nuclear Information System (INIS)

STALLINGS, MARY

2004-01-01

This report presents findings from tests investigating the dissolution of simulated and radioactive Savannah River Site sludges with 4 per cent oxalic acid and mixtures of oxalic and citric acid previously recommended by a Russian team from the Khlopin Radium Institute and the Mining and Chemical Combine (MCC). Testing also included characterization of the simulated and radioactive waste sludges. Testing results showed the following: Dissolution of simulated HM and PUREX sludges with oxalic and citric acid mixtures at SRTC confirmed general trends reported previously by Russian testing. Unlike the previous Russian testing six sequential contacts of a mixture of oxalic acid citric acids at a 2:1 ratio (v/w) of acid to sludge did not produce complete dissolution of simulated HM and PUREX sludges. We observed that increased sludge dissolution occurred at a higher acid to sludge ratio, 50:1 (v/w), compared to the recommended ratio of 2:1 (v/w). We observed much lower dissolution of aluminum in a simulated HM sludge by sodium hydroxide leaching. We attribute the low aluminum dissolution in caustic to the high fraction of boehmite present in the simulated sludge. Dissolution of HLW sludges with 4 per cent oxalic acid and oxalic/citric acid followed general trends observed with simulated sludges. The limited testing suggests that a mixture of oxalic and citric acids is more efficient for dissolving HM and PUREX sludges and provides a more homogeneous dissolution of HM sludge than oxalic acid alone. Dissolution of HLW sludges in oxalic and oxalic/citric acid mixtures produced residual sludge solids that measured at higher neutron poison to equivalent 235U weight ratios than that in the untreated sludge solids. This finding suggests that residual solids do not present an increased nuclear criticality safety risk. Generally the neutron poison to equivalent 235U weight ratios of the acid solutions containing dissolved sludge components are lower than those in the untreated

Nitrosation and Nitration of Fulvic Acid, Peat and Coal with Nitric Acid.

Directory of Open Access Journals (Sweden)

Kevin A Thorn

Full Text Available Nitrohumic acids, produced from base extraction of coals and peats oxidized with nitric acid, have received considerable attention as soil ammendments in agriculture. The nitration chemistry however is incompletely understood. Moreover, there is a need to understand the reaction of nitric acid with natural organic matter (NOM in general, in the context of a variety of environmental and biogeochemical processes. Suwannee River NOM, Suwannee River fulvic acid, and Pahokee Peat fulvic acid were treated with 15N-labeled nitric acid at concentrations ranging from 15% to 22% and analyzed by liquid and solid state 15N NMR spectroscopy. Bulk Pahokee peat and Illinois #6 coal were also treated with nitric acid, at 29% and 40% respectively, and analyzed by solid state 15N NMR spectroscopy. In addition to nitro groups from nitration of aromatic carbon, the 15N NMR spectra of all five samples exhibited peaks attributable to nitrosation reactions. These include nitrosophenol peaks in the peat fulvic acid and Suwannee River samples, from nitrosation of phenolic rings, and N-nitroso groups in the peat samples, from nitrosation of secondary amides or amines, the latter consistent with the peat samples having the highest naturally abundant nitrogen contents. Peaks attributable to Beckmann and secondary reactions of the initially formed oximes were present in all spectra, including primary amide, secondary amide, lactam, and nitrile nitrogens. The degree of secondary reaction product formation resulting from nitrosation reactions appeared to correlate inversely with the 13C aromaticities of the samples. The nitrosation reactions are most plausibly effected by nitrous acid formed from the reduction of nitric acid by oxidizable substrates in the NOM and coal samples.

Comparative Analysis of Performance and Microbial Characteristics Between High-Solid and Low-Solid Anaerobic Digestion of Sewage Sludge Under Mesophilic Conditions.

Science.gov (United States)

Lu, Qin; Yi, Jing; Yang, Dianhai

2016-01-01

High-solid anaerobic digestion of sewage sludge achieves highly efficient volatile solid reduction, and production of volatile fatty acid (VFA) and methane compared with conventional low-solid anaerobic digestion. In this study, the potential mechanisms of the better performance in high-solid anaerobic digestion of sewage sludge were investigated by using 454 high-throughput pyrosequencing and real-time PCR to analyze the microbial characteristics in sewage sludge fermentation reactors. The results obtained by 454 high-throughput pyrosequencing revealed that the phyla Chloroflexi, Bacteroidetes, and Firmicutes were the dominant functional microorganisms in high-solid and low-solid anaerobic systems. Meanwhile, the real-time PCR assays showed that high-solid anaerobic digestion significantly increased the number of total bacteria, which enhanced the hydrolysis and acidification of sewage sludge. Further study indicated that the number of total archaea (dominated by Methanosarcina) in a high-solid anaerobic fermentation reactor was also higher than that in a low-solid reactor, resulting in higher VFA consumption and methane production. Hence, the increased key bacteria and methanogenic archaea involved in sewage sludge hydrolysis, acidification, and methanogenesis resulted in the better performance of high-solid anaerobic sewage sludge fermentation.

Identification of three new phase II metabolites of a designer drug methylone formed in rats by N-demethylation followed by conjugation with dicarboxylic acids.

Science.gov (United States)

Židková, Monika; Linhart, Igor; Balíková, Marie; Himl, Michal; Dvořáčková, Veronika; Lhotková, Eva; Páleníček, Tomáš

2018-06-01

1. Methylone (3,4-methylenedioxy-N-methylcathinone, MDMC), which appeared on the illicit drug market in 2004, is a frequently abused synthetic cathinone derivative. Known metabolic pathways of MDMC include N-demethylation to normethylone (3,4-methylenedioxycathinone, MDC), aliphatic chain hydroxylation and oxidative demethylenation followed by monomethylation and conjugation with glucuronic acid and/or sulphate. 2. Three new phase II metabolites, amidic conjugates of MDC with succinic, glutaric and adipic acid, were identified in the urine of rats dosed subcutaneously with MDMC.HCl (20 mg/kg body weight) by LC-ESI-HRMS using synthetic reference standards to support identification. 3. The main portion of administered MDMC was excreted unchanged. Normethylone, was a major urinary metabolite, of which a minor part was conjugated with dicarboxylic acids. 4. Previously identified ring-opened metabolites 4-hydroxy-3-methoxymethcathinone (4-OH-3-MeO-MC), 3-hydroxy-4-methoxymeth-cathinone (3-OH-4-MeO-MC) and 3,4-dihydroxymethcathinone (3,4-di-OH-MC) mostly in conjugated form with glucuronic and/or sulphuric acids were also detected. 5. Also, ring-opened metabolites derived from MDC, namely, 4-hydroxy-3-methoxycathinone (4-OH-3-MeO-C), 3-hydroxy-4-methoxycathinone (3-OH-4-MeO-C) and 3,4-dihydroxycathinone (3,4-di-OH-C) were identified for the first time in vivo.

Classification of bacteria by simultaneous methylation-solid phase microextraction and gas chromatography/mass spectrometry analysis of fatty acid methyl esters.

Science.gov (United States)

Lu, Yao; Harrington, Peter B

2010-08-01

Direct methylation and solid-phase microextraction (SPME) were used as a sample preparation technique for classification of bacteria based on fatty acid methyl ester (FAME) profiles. Methanolic tetramethylammonium hydroxide was applied as a dual-function reagent to saponify and derivatize whole-cell bacterial fatty acids into FAMEs in one step, and SPME was used to extract the bacterial FAMEs from the headspace. Compared with traditional alkaline saponification and sample preparation using liquid-liquid extraction, the method presented in this work avoids using comparatively large amounts of inorganic and organic solvents and greatly decreases the sample preparation time as well. Characteristic gas chromatography/mass spectrometry (GC/MS) of FAME profiles was achieved for six bacterial species. The difference between Gram-positive and Gram-negative bacteria was clearly visualized with the application of principal component analysis of the GC/MS data of bacterial FAMEs. A cross-validation study using ten bootstrap Latin partitions and the fuzzy rule building expert system demonstrated 87 +/- 3% correct classification efficiency.

Bacteria-mediated in vivo delivery of quantum dots into solid tumor

International Nuclear Information System (INIS)

Liu, Ying; Zhou, Mei; Luo, Dan; Wang, Lijun; Hong, Yuankai; Yang, Yepeng; Sha, Yinlin

2012-01-01

Highlights: ► New approach using the probiotic Bifidobacterium bifidum as a vehicle to deliver QDs into the deep tissue of solid tumors in vivo was achieved. ► Bifidobacterium bifidum delivery system has intrinsic biocompatibility. ► The targeting efficacy was improved by folic acids. -- Abstract: Semiconductor nanocrystals, so-called quantum dots (QDs), promise potential application in bioimaging and diagnosis in vitro and in vivo owing to their high-quality photoluminescence and excellent photostability as well as size-tunable spectra. Here, we describe a biocompatible, comparatively safe bacteria-based system that can deliver QDs specifically into solid tumor of living animals. In our strategy, anaerobic bacterium Bifidobacterium bifidum (B. bifidum) that colonizes selectively in hypoxic regions of animal body was successfully used as a vehicle to load with QDs and transported into the deep tissue of solid tumors. The internalization of lipid-encapsuled QDs into B. bifidum was conveniently carried by electroporation. To improve the efficacy and specificity of tumor targeting, the QDs-carrying bacterium surface was further conjugated with folic acids (FAs) that can bind to the folic acid receptor overexpressed tumor cells. This new approach opens a pathway for delivering different types of functional cargos such as nanoparticles and drugs into solid tumor of live animals for imaging, diagnosis and therapy.

Active biodegradable films produced with blends of rice flour and poly(butylene adipate co-terephthalate): effect of potassium sorbate on film characteristics.

Science.gov (United States)

Sousa, G M; Soares Júnior, M S; Yamashita, F

2013-08-01

The objective of work was to produce and characterize biodegradable films from rice flour, poly(butylene adipate co-terephthalate) (PBAT), glycerol and potassium sorbate, for application as active packaging for fresh lasagna pasta. The films were evaluated with respect to their optical, water vapor barrier, mechanical and microstructural properties. The mechanical properties and microstructure were evaluated after use as packaging material for fresh pasta for 45 days at 7°C. The blends of rice flour, PBAT, glycerol and potassium sorbate showed good processability and allowed for the pilot scale production of films by blow extrusion process. The addition of 1 to 5% potassium sorbate as plasticizer agent of films in place of glycerol did not alter the film mechanical properties and a sorbate concentration greater or equal than 3% reduced the opacity, although increasing the water vapor permeability. The films could be used as active packaging for fresh food pasta, since they remained integral and easy to handle after application. The rice flour was shown to be an excellent material for the formulation of biodegradable films, since it is a low-cost raw material from a renewable source. The addition of potassium sorbate did not affect the extrusion process, and could be used in the production of packaging for use with foods. Copyright © 2013 Elsevier B.V. All rights reserved.

Hydrochloric acid leach of Agnew Lake uranium concentrate

International Nuclear Information System (INIS)

Haque, K.E.; Ipekoglue, B.

1981-10-01

Hydrochloric acid leaching was conducted on the radioactive mineral concentrate separated from the Agenw Lake uranium ore. Leach tests conducted at the optimum conditions (75 0 C; 36 hours; 66.0 Kg HCl/tonne; solid:liquid -1:1) resulted in the extraction of 87% uranium and 84% radium. The radionuclide level of the residue was U-0.016%, Th-0.24% and Ra-65 pCi/g solids. However to obtain a residue almost free of radium (i.e., Ra level at the detection limit: 4-6 pCi/g solids), the first stage leach residue was further treated with hydrochloric acid. The radium level in the best second stage leach residue was also above the target level. Therefore, multistage (3 or 4) hydrochloric acid and/or neutral chloride leaching is recommended to obtain tailings almost free of radionuclide

Solid state radiolysis of non-proteinaceous amino acids in vacuum. Astrochemical implications

International Nuclear Information System (INIS)

Franco Cataldo; Giancarlo Angelini; Yaser Hafez; Susana Iglesias-Groth

2013-01-01

The analysis of the amino acids present in Murchison meteorite and in other carbonaceous chondrites has revealed the presence of 66 different amino acids. Only eight of these 66 amino acids are proteinaceous amino acids used by the present terrestrial biochemistry in protein synthesis, the other 58 amino acids are somewhat 'rare' or unusual or even 'unknown' for the current terrestrial biochemistry. For this reason in the present work a series of 'uncommon' non-proteinaceous amino acids, namely, l-2-aminobutyric acid, R(-)-2-aminobutyric acid, 2-aminoisobutyric acid (or α-aminoisobutyric acid), l-norleucine, l-norvaline, l-β-leucine, l-β-homoalanine, l-β-homoglutamic acid, S(-)-α-methylvaline and dl-3-aminoisobutyric acid were radiolyzed in vacuum at 3.2 MGy a dose equivalent to that emitted in 1.05 x 10 9 years from the radionuclide decay in the bulk of asteroids or comets. The residual amount of each amino acid under study remained after radiolysis was determined by differential scanning calorimetry in comparison to pristine samples. For optically active amino acids, the residual amount of each amino acid remained after radiolysis was also determined by optical rotatory dispersion spectroscopy and by polarimetry. With these analytical techniques it was possible to measure also the degree of radioracemization undergone by each amino acid after radiolysis. It was found that the non-proteinaceous amino acids in general do not show a higher radiation and radioracemization resistance in comparison to the common 20 proteinaceous amino acids studied previously. The unique exception is represented by ?-aminoisobutyric acid which shows an extraordinary resistance to radiolysis since 96.6 % is recovered unchanged after 3.2 MGy. Curiously α-aminoisobutyric acid is the most abundant amino acid found in carbonaceous chondrites. In Murchison meteorite α-aminoisobutyric acid represents more than 20 % of the total 66 amino acids found in this meteorite. (author)

Magnetic silica nanomaterials for solid-phase extraction combined with dispersive liquid-liquid microextraction of ultra-trace quantities of plasticizers

International Nuclear Information System (INIS)

Yamini, Yadollah; Faraji, Mohammad; Adeli, Mahnaz

2015-01-01

We are presenting surface modified magnetic silica nanoparticles (m-Si-NPs) for use in solid-phase extraction combined with dispersive liquid-liquid microextraction (DLLME). The m-Si-NPs were surface-functionalized with octadecyl groups to give a material for the extraction of the plasticizers dibutyl phthalate, di(2-ethylhexyl) adipate and di(2-ethylhexyl) phthalate from water samples. The functionalized m-Si-NPs were characterized by scanning electron microscopy, FTIR spectroscopy, thermal gravimetric analysis, and vibrating sample magnetometry. The results showed that the m-Si-NPs were well functionalized with octadecyl groups. The effects of various experimental variables on the extraction efficiencies were investigated. The analytes were quantified by GC/FID. Under optimal conditions, the calibration plots are linear in the range from 0.01 to 100 μg∙L -1 , and very high enrichment factors (mean value ∼20,000) were obtained. As a result of the high enrichment factors, the detection limits are as low as 2–3 ng∙L -1 . The method was successfully employed to the extraction of the plasticizers from (spiked) water samples, and recoveries are in the order of 93.9 to 106.7 %. The method is low cost, fast, and very sensitive (author)

Physico-chemical analysis of tannery solid waste and structural characterization of its isolated humic acids after composting.

Science.gov (United States)

Amir, Soumia; Benlboukht, Fatima; Cancian, Nadia; Winterton, Peter; Hafidi, Mohamed

2008-12-30

In Marrakech, solid by-products from tanneries are highly polluting, generating large amounts of nitrogenous and organic matter. In the present study composting is tested as a cost-effective method for waste management to overcome many of the environmental hazards and produce a stable, rich material for soil fertilization. Two composting trials were conducted after neutralization by ammonia or lime. The aim of the neutralization was to avoid the antimicrobial effects of the acidity in the tannery waste, thus ensuring correct composting. Different techniques such as elemental analysis and 13C NMR spectroscopy were applied to analyse humic acids isolated from raw and composted materials, and to monitor the process of tannery waste composting, and the stability and maturity of the final product according to the means of neutralization. Comparison of data showed similar behaviour in both trials, but the composting process appeared to be more complete following neutralization with lime. The C, H and N content decreased, while the O increased. The FTIR and 13C NMR spectra show the decrease of aliphatic compounds demonstrated by the reduction of absorbance around 2922cm(-1) and of the resonance in the C-alkyl area around 0-55ppm. The humic acids newly formed during composting were richer in the O-N alkyl and oxidized aromatic structures that increased almost twofold on composting after neutralization with lime. The first principal component axis PC1 (54%) separated C-aliphatic, C-carboxylic and other less stable and less polycondensed compounds such as polyphenols from the more polycondensed O-N alkyl and oxidized C-aromatic compounds.

Lead sulfate nano- and microparticles in the acid plant blow-down generated at the sulfuric acid plant of the El Teniente mine, Chile.

Science.gov (United States)

Barassi, Giancarlo M; Klimsa, Martin; Borrmann, Thomas; Cairns, Mathew J; Kinkel, Joachim; Valenzuela, Fernando

2014-12-01

The acid plant 'blow-down' (also called weak acid) produced at El Teniente mine in Chile was characterized. This liquid waste (tailing) is generated during the cooling and cleaning of the smelter gas prior to the production of sulfuric acid. The weak acid was composed of a liquid and a solid phase (suspended solids). The liquid phase of the sample analyzed in this study mainly contained Cu (562 mg L(-1)), SO4(2-) (32 800 mg L(-1)), Ca (1449 mg L(-1)), Fe (185 mg L(-1)), As (6 mg L(-1)), K (467 mg L(-1)) and Al (113 mg L(-1)). Additionally, the sample had a pH-value and total acidity of 0.45 and 2970 mg L(-1) as CaCO3, respectively. Hence, this waste was classified as extremely acidic and with a high metal content following the Ficklin diagram classification. Elemental analysis using atomic absorption, inductively coupled plasma, X-ray diffraction and electron microscopy showed that the suspended solids were anglesite (PbSO4) nano- and microparticles ranging from 50 nm to 500 nm in diameter.

Incineration of alpha-active solid waste by microwaves

Energy Technology Data Exchange (ETDEWEB)

Mallik, G K; Bhargava, V K; Kamath, H S; Purushotham, D S.C. [Bhabha Atomic Research Centre, Tarapur (India). Advanced Fuel Fabrication Facility

1996-12-31

The conventional techniques for treatment of alpha-active compressible solid waste involve incineration using electrically heated incinerators and subsequent recovery of special nuclear materials (SNM) from the ash by acid leaching. A microwave incineration followed by microwave digestion and SNM recovery from ash has specific advantages from maintenance and productivity consideration. The paper describes a preliminary work carried out with simulated uranium containing compressible solid waste using microwave heating technique. (author). 3 refs., 1 tab.

Synthesis and properties of hydroxy acrylic resin with high solid content

Science.gov (United States)

Yu, Zhen; Hu, Mingguang; Cui, Han; Xiao, Jijun

2017-10-01

Manufacturers of automotive repair finishes are tending to reduce more and more the level of volatile organic compounds in their paints in order to comply with increasingly strict environmental legislation. A high solid hydroxy acrylic resin was synthesised using CARDURA E10 and a type of hydroxyacrylic acid resin, its' acid value, hydroxylvalue, viscosity, structure, morphology was measured and film-forming properties after curing were characterised. The results show that the addition of CARDURA E10 in the copolymer composition significantly reduced the viscosity of the polymer system, improved the solid content of the resin and the physical properties of the coating. The hydroxyl acrylate resin with solid content of 90% and excellent comprehensive performance were successfully prepared by controlling the initiator dosage, polymerization temperature and monomer ratio.

Indigenous microbial capability in solid manure residues to start-up solid-phase anaerobic digesters.

Science.gov (United States)

Yap, S D; Astals, S; Jensen, P D; Batstone, D J; Tait, S

2017-06-01

Batch solid-phase anaerobic digestion is a technology for sustainable on-farm treatment of solid residues, but is an emerging technology that is yet to be optimised with respect to start-up and inoculation. In the present study, spent bedding from two piggeries (site A and B) were batch digested at total solids (TS) concentration of 5, 10 and 20% at mesophilic (37°C) and thermophilic (55°C) temperatures, without adding an external inoculum. The results showed that the indigenous microbial community present in spent bedding was able to recover the full methane potential of the bedding (140±5 and 227±6L CH 4 kgVS fed -1 for site A and B, respectively), but longer treatment times were required than for digestion with an added external inoculum. Nonetheless, at high solid loadings (i.e. TS level>10%), the digestion performance was affected by chemical inhibition due to ammonia and/or humic acid. Thermophilic temperatures did not influence digestion performance but did increase start-up failure risk. Further, inoculation of residues from the batch digestion to subsequent batch enhanced start-up and achieved full methane potential recovery of the bedding. Inoculation with liquid residue (leachate) was preferred over a solid residue, to preserve treatment capacity for fresh substrate. Overall, the study highlighted that indigenous microbial community in the solid manure residue was capable of recovering full methane potential and that solid-phase digestion was ultimately limited by chemical inhibition rather than lack of suitable microbial community. Copyright © 2017 Elsevier Ltd. All rights reserved.

Anaerobic degradation of diethyl phthalate and phthalic acid during incubation of municipal solid waste from a biogas digestor

Energy Technology Data Exchange (ETDEWEB)

Ejlertsson, J.; Houwen, F.P.; Svensson, B.H. [Swedish Univ. of Agricultural Sciences, Uppsala (Sweden). Dept. of Microbiology

1996-11-01

Degradation of diethyl phthalate (DEP) and phthalic acid (PA) was investigated in diluted and homogenized municipal solid waste treated in a biogas digester. Complete degradation for both DEP and PA occurred at the concentrations investigated (50-250 mg/l). PA was shown to form an obligatory intermediate in stoichiometric amounts during DEP transformation. Mono-ethyl phthalate was also observed as an intermediate, though in concentrations below 40 mg/l. The formation of methane (and carbon dioxide) from DEP and PA took place within 80-100 days of incubation, of which at least 75% or more of the maximally expected methane was recovered. Two analytical procedures were compared in this paper: PAE-analysis by spectrophotometer and HPLC. 12 refs, 3 figs, 1 tab

Profiling the Fatty Acids Content of Ornamental Camellia Seeds Cultivated in Galicia by an Optimized Matrix Solid-Phase Dispersion Extraction

Directory of Open Access Journals (Sweden)

Carmen Garcia-Jares

2017-10-01

Full Text Available Camellia (genus of flowering plants of fam. Theaceae is one of the main crops in Asia, where tea and oil from leaves and seeds have been utilized for thousands of years. This plant is excellently adapted to the climate and soil of Galicia (northwestern Spain and northern Portugal where it is grown not only as an ornamental plant, but to be evaluated as a source of bioactive compounds. In this work, the main fatty acids were extracted from Camellia seeds of four varieties of Camellia: sasanqua, reticulata, japonica and sinensis, by means of matrix-solid phase dispersion (MSPD, and analyzed by gas chromatography (GC with MS detection of the corresponding methyl esters. MSPD constitutes an efficient and greener alternative to conventional extraction techniques, moreover if it is combined with the use of green solvents such as limonene. The optimization of the MSPD extraction procedure has been conducted using a multivariate approach based on strategies of experimental design, which enabled the simultaneous evaluation of the factors influencing the extraction efficiency as well as interactions between factors. The optimized method was applied to characterize the fatty acids profiles of four Camellia varieties seeds, allowing us to compare their fatty acid composition.

Profiling the Fatty Acids Content of Ornamental Camellia Seeds Cultivated in Galicia by an Optimized Matrix Solid-Phase Dispersion Extraction

Science.gov (United States)

Garcia-Jares, Carmen; Sanchez-Nande, Marta; Lamas, Juan Pablo; Lores, Marta

2017-01-01

Camellia (genus of flowering plants of fam. Theaceae) is one of the main crops in Asia, where tea and oil from leaves and seeds have been utilized for thousands of years. This plant is excellently adapted to the climate and soil of Galicia (northwestern Spain) and northern Portugal where it is grown not only as an ornamental plant, but to be evaluated as a source of bioactive compounds. In this work, the main fatty acids were extracted from Camellia seeds of four varieties of Camellia: sasanqua, reticulata, japonica and sinensis, by means of matrix-solid phase dispersion (MSPD), and analyzed by gas chromatography (GC) with MS detection of the corresponding methyl esters. MSPD constitutes an efficient and greener alternative to conventional extraction techniques, moreover if it is combined with the use of green solvents such as limonene. The optimization of the MSPD extraction procedure has been conducted using a multivariate approach based on strategies of experimental design, which enabled the simultaneous evaluation of the factors influencing the extraction efficiency as well as interactions between factors. The optimized method was applied to characterize the fatty acids profiles of four Camellia varieties seeds, allowing us to compare their fatty acid composition. PMID:29039745

Development of solid lipid nanoparticles for enhanced solubility of poorly soluble drugs

DEFF Research Database (Denmark)

Potta, Sriharsha Gupta; Minemi, Sriharsha; Nukala, Ravi Kumar

2010-01-01

Cyclosporine (CyA) solid lipid nanoparticles were prepared by using a solvent free high pressure homogenization process. CyA was incorporated into SLNs that consisted of stearic acid, trilaurin or tripalmitin lipid solid cores in order to enhance drug solubility. The process was conducted...

Use of the 2-chlorotrityl chloride resin for microwave-assisted solid phase peptide synthesis.

Science.gov (United States)

Ieronymaki, Matthaia; Androutsou, Maria Eleni; Pantelia, Anna; Friligou, Irene; Crisp, Molly; High, Kirsty; Penkman, Kirsty; Gatos, Dimitrios; Tselios, Theodore

2015-09-01

A fast and efficient microwave (MW)-assisted solid-phase peptide synthesis protocol using the 2-chlorotrityl chloride resin and the Fmoc/tBu methodology, has been developed. The established protocol combines the advantages of MW irradiation and the acid labile 2-chlorotrityl chloride resin. The effect of temperature during the MW irradiation, the degree of resin substitution during the coupling of the first amino acids and the rate of racemization for each amino acid were evaluated. The suggested solid phase methodology is applicable for orthogonal peptide synthesis and for the synthesis of cyclic peptides. © 2015 Wiley Periodicals, Inc.

Evaluation of the effect of process variables on the fatty acid profile of single cell oil produced by Mortierella using solid-state fermentation.

Science.gov (United States)

Asadi, Seyedeh Zeinab; Khosravi-Darani, Kianoush; Nikoopour, Houshang; Bakhoda, Hossein

2015-03-01

This article reviews some of the aspects of single cell oil (SCO) production using solid-state fermentation (SSF) by fungi of the genus Mortierella. This article provides an overview of the advantages of SSF for SCO formation by the aforementioned fungus and demonstrates that the content of the polyunsaturated fatty acids (PUFA) depend on the type of fermentation media and culture conditions. Process variables that influence lipid accumulation by Mortierella spp. and the profile of the fatty acids are discussed, including incubation temperature, time, aeration, growth phase of the mycelium, particle size of the substrate, carbon to nitrogen ratio, initial moisture content and pH as well as supplementation of the substrate with nitrogen and oil. Finally, the article highlights future research trends for the scaled-up production of PUFAs in SSF.

Novel Proton Conducting Solid Bio-polymer Electrolytes Based on Carboxymethyl Cellulose Doped with Oleic Acid and Plasticized with Glycerol

Science.gov (United States)

Chai, M. N.; Isa, M. I. N.

2016-06-01

The plasticized solid bio-polymer electrolytes (SBEs) system has been formed by introducing glycerol (Gly) as the plasticizer into the carboxymethyl cellulose (CMC) doped with oleic acid (OA) via solution casting techniques. The ionic conductivity of the plasticized SBEs has been studied using Electrical Impedance Spectroscopy. The highest conductivity achieved is 1.64 × 10-4 S cm-1 for system containing 40 wt. % of glycerol. FTIR deconvolution technique had shown that the conductivity of CMC-OA-Gly SBEs is primarily influenced by the number density of mobile ions. Transference number measurement has shown that the cation diffusion coefficient and ionic mobility is higher than anion which proved the plasticized polymer system is a proton conductor.

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

Energy Technology Data Exchange (ETDEWEB)

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

1997-06-24

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

Solid-state interactions between trimethoprim and parabens

DEFF Research Database (Denmark)

Pedersen, S.; Kristensen, H. G.; Cornett, Claus

1994-01-01

by differential scanning calorimetry, X-ray powder diffraction, Fourier transform infrared spectroscopy, and solid-state C-13-NMR. Interactions between trimethoprim and 4-hydroxybenzoic acid and its ethyl,propyl and butyl esters were not observed. The nature of the trimethoprim and methyl parahydroxybenzoate...

The resistance of Bacillus atrophaeus spores to the bactericidal activity of peracetic acid is influenced by both the nature of the solid substrates and the mode of contamination.

Science.gov (United States)

Grand, I; Bellon-Fontaine, M-N; Herry, J-M; Hilaire, D; Moriconi, F-X; Naïtali, M

2010-11-01

To evaluate the impact of the mode of contamination in relation with the nature of solid substrates on the resistance of spores of Bacillus atrophaeus -selected as surrogates of Bacillus anthracis- to a disinfectant, peracetic acid. Six materials confronted in urban and military environments were selected for their different structural and physicochemical properties. In parallel, two modes of contamination were examined, i.e. deposition and immersion. Deposition was used to simulate contamination by an aerosol and immersion by an extended contact with liquids. A pronounced difference in the biocontamination levels and spatial organization of spores was observed depending on the mode of contamination and the nature of the solid substrate considered, with consequences on decontamination. Contamination by immersion led to lower efficiency of peracetic acid decontamination than contamination by deposition. Infiltration of spores into porous materials after immersion is one reason. In contrast, the deposition mode aggregates cells at the surface of materials, explaining the similar disinfecting behaviour of porous and nonporous substrates when considering this inoculation route. The inoculation route was shown to be as influential a parameter as material characteristics (porosity and wettability) for decontamination efficacy. These results provide comparative information for the decontamination of B. atrophaeus spores in function of the mode of contamination and the nature of solid substrates. Journal of Applied Microbiology © 2010 The Society for Applied Microbiology. No claim to French government works.

Biochemical changes in low-salt solid-state fermented soy sauce ...

African Journals Online (AJOL)

Results showed that after a 15-day aging period, the contents of total nitrogen, formol titration nitrogen, free amino acids, reducing sugar, total sugar and the brown color were increased. However, pH was decreased during the fermentation period. Furthermore, contents of total free amino acids in low-salt solid-state ...

Acid-base interactions and secondary structures of poly-L-lysine probed by 15N and 13C solid state NMR and Ab initio model calculations.

Science.gov (United States)

Dos, Alexandra; Schimming, Volkmar; Tosoni, Sergio; Limbach, Hans-Heinrich

2008-12-11

The interactions of the 15N-labeled amino groups of dry solid poly-L-lysine (PLL) with various halogen and oxygen acids HX and the relation to the secondary structure have been studied using solid-state 15N and 13C CPMAS NMR spectroscopy (CP = cross polarization and MAS = magic angle spinning). For comparison, 15N NMR spectra of an aqueous solution of PLL were measured as a function of pH. In order to understand the effects of protonation and hydration on the 15N chemical shifts of the amino groups, DFT and chemical shielding calculations were performed on isolated methylamine-acid complexes and on periodic halide clusters of the type (CH3NH3(+)X(-))n. The combined experimental and computational results reveal low-field shifts of the amino nitrogens upon interaction with the oxygen acids HX = HF, H2SO4, CH3COOH, (CH3)2POOH, H3PO4, HNO3, and internal carbamic acid formed by reaction of the amino groups with gaseous CO2. Evidence is obtained that only hydrogen-bonded species of the type (Lys-NH2***H-X)n are formed in the absence of water. 15N chemical shifts are maximum when H is located in the hydrogen bond center and then decrease again upon full protonation, as found for aqueous solution at low pH. By contrast, halogen acids interact in a different way. They form internal salts of the type (Lys-NH3(+)X(-))n via the interaction of many acid-base pairs. This salt formation is possible only in the beta-sheet conformation. By contrast, the formation of hydrogen-bonded complexes can occur both in beta-sheet domains as well as in alpha-helical domains. The 15N chemical shifts of the protonated ammonium groups increase when the size of the interacting halogen anions is increased from chloride to iodide and when the number of the interacting anions is increased. Thus, the observed high-field 15N shift of ammonium groups upon hydration is the consequence of replacing interacting halogen atoms by oxygen atoms.

Bacteria-mediated in vivo delivery of quantum dots into solid tumor

Energy Technology Data Exchange (ETDEWEB)

Liu, Ying [Single-molecule and Nanobiology Lab., Dept. of Biophysics, School of Basic Medical Sciences, Peking University, No. 38 Xue Yuan Road, Beijing 100091 (China); Zhou, Mei [Dept. of Radiation Medicine, School of Basic Medical Sciences, Peking University, No. 38 Xue Yuan Road, Beijing 100091 (China); Luo, Dan; Wang, Lijun; Hong, Yuankai [Single-molecule and Nanobiology Lab., Dept. of Biophysics, School of Basic Medical Sciences, Peking University, No. 38 Xue Yuan Road, Beijing 100091 (China); Yang, Yepeng, E-mail: yangyepeng@bjmu.edu.cn [Dept. of Radiation Medicine, School of Basic Medical Sciences, Peking University, No. 38 Xue Yuan Road, Beijing 100091 (China); Sha, Yinlin, E-mail: shyl@hsc.pku.edu.cn [Single-molecule and Nanobiology Lab., Dept. of Biophysics, School of Basic Medical Sciences, Peking University, No. 38 Xue Yuan Road, Beijing 100091 (China); Biomed-X Center, Peking University, Peking University, No. 38 Xue Yuan Road, Beijing 100091 (China)

2012-09-07

Highlights: Black-Right-Pointing-Pointer New approach using the probiotic Bifidobacterium bifidum as a vehicle to deliver QDs into the deep tissue of solid tumors in vivo was achieved. Black-Right-Pointing-Pointer Bifidobacterium bifidum delivery system has intrinsic biocompatibility. Black-Right-Pointing-Pointer The targeting efficacy was improved by folic acids. -- Abstract: Semiconductor nanocrystals, so-called quantum dots (QDs), promise potential application in bioimaging and diagnosis in vitro and in vivo owing to their high-quality photoluminescence and excellent photostability as well as size-tunable spectra. Here, we describe a biocompatible, comparatively safe bacteria-based system that can deliver QDs specifically into solid tumor of living animals. In our strategy, anaerobic bacterium Bifidobacterium bifidum (B. bifidum) that colonizes selectively in hypoxic regions of animal body was successfully used as a vehicle to load with QDs and transported into the deep tissue of solid tumors. The internalization of lipid-encapsuled QDs into B. bifidum was conveniently carried by electroporation. To improve the efficacy and specificity of tumor targeting, the QDs-carrying bacterium surface was further conjugated with folic acids (FAs) that can bind to the folic acid receptor overexpressed tumor cells. This new approach opens a pathway for delivering different types of functional cargos such as nanoparticles and drugs into solid tumor of live animals for imaging, diagnosis and therapy.

Effect of solids, caloric content on dual-phase gastric emptying

Energy Technology Data Exchange (ETDEWEB)

Van Den Maegdenbergh, V.; Urbain, J.L.; Siegel, J.A.; Mortelmans, L.; De Roo, M. (Univ. Hospital Gasthuisberg, Leuven (Belgium) Temple Univ. Hospital, Philadelphia, PA (USA))

1990-03-01

The dual-phase gastric emptying technique is routinely employed to determine the differential emptying of solids and liquids in a wide spectrum of gastrointestinal diseases. Composition, acidity, volume, caloric density, physical form and viscosity of the test means have been shown to be important determinants for the quantitative evaluation of gastric emptying. In this study, the authors have evaluated the effect of increasing the caloric content of the solid portion of a physiologic test mean on both solid and liquid emptying kinetics in health male volunteers. They observed that increasing solid caloric content delayed emptying of both solids and liquids. For the solid phase, the delay was accounted for by a longer lag phase and decrease in emptying rate; for liquids a longer emptying rate was also obtained. They conclude that modification of the caloric content of the solid portion of a meal not only affects the emptying of the solid phase but also alters the emptying of the liquid component of the meal.

Enhanced solubility and bioavailability of sibutramine base by solid dispersion system with aqueous medium.

Science.gov (United States)