Systems and strippable coatings for decontaminating structures that include porous material

DOEpatents

Fox, Robert V [Idaho Falls, ID; Avci, Recep [Bozeman, MT; Groenewold, Gary S [Idaho Falls, ID

2011-12-06

Methods of removing contaminant matter from porous materials include applying a polymer material to a contaminated surface, irradiating the contaminated surface to cause redistribution of contaminant matter, and removing at least a portion of the polymer material from the surface. Systems for decontaminating a contaminated structure comprising porous material include a radiation device configured to emit electromagnetic radiation toward a surface of a structure, and at least one spray device configured to apply a capture material onto the surface of the structure. Polymer materials that can be used in such methods and systems include polyphosphazine-based polymer materials having polyphosphazine backbone segments and side chain groups that include selected functional groups. The selected functional groups may include iminos, oximes, carboxylates, sulfonates, .beta.-diketones, phosphine sulfides, phosphates, phosphites, phosphonates, phosphinates, phosphine oxides, monothio phosphinic acids, and dithio phosphinic acids.

Polyimides Containing Pendent Phosphine Oxide Groups for Space Applications

NASA Technical Reports Server (NTRS)

Thompson, C. M.; Smith, J. G., Jr.; Watson, K. A.; Connell, J. W.

2002-01-01

As part of an ongoing materials development activity to produce high performance polymers that are durable to the space environment, phosphine oxide containing polyimides have been under investigation. A novel dianhydride was prepared from 2,5-dihydroxyphenyldiphenylphosphine oxide in good yield. The dianhydride was reacted with commercially available diamines, and a previously reported diamine was reacted with commercially available dianhydrides to prepare isomeric polyimides. The physical and mechanical properties, particularly thermal and optical properties, of the polymers were determined. One material exhibited a high glass transition temperature, high tensile properties, and low solar absorptivity. The chemistry, physical, and mechanical properties of these resins will be discussed.

Comparative effects of gamma irradiation and phosphine fumigation on the quality of white ginseng

NASA Astrophysics Data System (ADS)

Kwon, J.-H. J.-H.; Byun, M.-W. M.-W.; Kim, K.-S. K.-S.; Kang, I.-J. I.-J.

2000-03-01

The hygienic, physicochemical, and organoleptic qualities of white ginseng were monitored during 6 months under accelerated conditions (40°C, 90% r.h.) by observing its microbial populations, disinfestation, and some quality attributes following either gamma irradiation at 2.5-10 kGy or commercial phosphine (PH 3) fumigation. In a comparative study, both treatments were found to be effective for disinfecting the stored samples. Phosphine showed no appreciable decontaminating effects on microorganisms contaminated including coliforms, while 5 kGy irradiation was sufficient to control all microorganisms related to the quality of the packed samples. Irradiation at 5 kGy caused negligible changes in physicochemical attributes of the samples, such as ginsenosides, amino acids, fatty acids, and organoleptic properties, whereas phosphine fumigation was found detrimental to sensory flavor ( P<0.01). Quality deterioration occurred in the commercially-packed samples was in the following order: the control, 10 kGy-, phosphine-, and 2.5-5 kGy-treated samples. Accordingly, irradiation at <5 kGy was found to be an effective alternative to phosphine fumigation for white ginseng.

Different in vitro and in vivo profiles of substituted 3-aminopropylphosphinate and 3-aminopropyl(methyl)phosphinate GABA(B) receptor agonists as inhibitors of transient lower oesophageal sphincter relaxation.

PubMed

Lehmann, A; Antonsson, M; Aurell-Holmberg, A; Blackshaw, L A; Brändén, L; Elebring, T; Jensen, J; Kärrberg, L; Mattsson, J P; Nilsson, K; Oja, S S; Saransaari, P; von Unge, S

2012-03-01

Gastro-oesophageal reflux is predominantly caused by transient lower oesophageal sphincter relaxation (TLOSR) and GABA(B) receptor stimulation inhibits TLOSR. Lesogaberan produces fewer CNS side effects than baclofen, which has been attributed to its affinity for the GABA transporter (GAT), the action of which limits stimulation of central GABA(B) receptors. To understand the structure-activity relationship for analogues of lesogaberan (3-aminopropylphosphinic acids), and corresponding 3-aminopropyl(methyl)phosphinic acids, we have compared representatives of these classes in different in vitro and in vivo models. The compounds were characterized in terms of GABA(B) agonism in vitro. Binding to GATs and cellular uptake was done using rat brain membranes and slices respectively. TLOSR was measured in dogs, and CNS side effects were evaluated as hypothermia in mice and rats. 3-Aminopropylphosphinic acids inhibited TLOSR with a superior therapeutic index compared to 3-aminopropyl(methyl)phosphinic acids. This difference was most likely due to differential GAT-mediated uptake into brain cells of the former but not latter. In agreement, 3-aminopropyl(methyl)phosphinic acids were much more potent in producing hypothermia in rats even when administered i.c.v. An enhanced therapeutic window for 3-aminopropylphosphinic acids compared with 3-aminopropyl(methyl)phosphinic acids with respect to inhibition of TLOSR was observed and is probably mechanistically linked to neural cell uptake of the former but not latter group of compounds. These findings offer a platform for discovery of new GABA(B) receptor agonists for the treatment of reflux disease and other conditions where selective peripheral GABA(B) receptor agonism may afford therapeutic effects. © 2011 The Authors. British Journal of Pharmacology © 2011 The British Pharmacological Society.

Different in vitro and in vivo profiles of substituted 3-aminopropylphosphinate and 3-aminopropyl(methyl)phosphinate GABAB receptor agonists as inhibitors of transient lower oesophageal sphincter relaxation

PubMed Central

Lehmann, A; Antonsson, M; Aurell-Holmberg, A; Blackshaw, LA; Brändén, L; Elebring, T; Jensen, J; Kärrberg, L; Mattsson, JP; Nilsson, K; Oja, SS; Saransaari, P; von Unge, S

2012-01-01

BACKGROUND AND PURPOSE Gastro-oesophageal reflux is predominantly caused by transient lower oesophageal sphincter relaxation (TLOSR) and GABAB receptor stimulation inhibits TLOSR. Lesogaberan produces fewer CNS side effects than baclofen, which has been attributed to its affinity for the GABA transporter (GAT), the action of which limits stimulation of central GABAB receptors. To understand the structure–activity relationship for analogues of lesogaberan (3-aminopropylphosphinic acids), and corresponding 3-aminopropyl(methyl)phosphinic acids, we have compared representatives of these classes in different in vitro and in vivo models. EXPERIMENTAL APPROACH The compounds were characterized in terms of GABAB agonism in vitro. Binding to GATs and cellular uptake was done using rat brain membranes and slices respectively. TLOSR was measured in dogs, and CNS side effects were evaluated as hypothermia in mice and rats. KEY RESULTS 3-Aminopropylphosphinic acids inhibited TLOSR with a superior therapeutic index compared to 3-aminopropyl(methyl)phosphinic acids. This difference was most likely due to differential GAT-mediated uptake into brain cells of the former but not latter. In agreement, 3-aminopropyl(methyl)phosphinic acids were much more potent in producing hypothermia in rats even when administered i.c.v. CONCLUSIONS AND IMPLICATIONS An enhanced therapeutic window for 3-aminopropylphosphinic acids compared with 3-aminopropyl(methyl)phosphinic acids with respect to inhibition of TLOSR was observed and is probably mechanistically linked to neural cell uptake of the former but not latter group of compounds. These findings offer a platform for discovery of new GABAB receptor agonists for the treatment of reflux disease and other conditions where selective peripheral GABAB receptor agonism may afford therapeutic effects. PMID:21950457

Preparation of polyvinyl alcohol graphene oxide phosphonate film and research of thermal stability and mechanical properties.

PubMed

Li, Jihui; Song, Yunna; Ma, Zheng; Li, Ning; Niu, Shuai; Li, Yongshen

2018-05-01

In this article, flake graphite, nitric acid, peroxyacetic acid and phosphoric acid are used to prepare graphene oxide phosphonic and phosphinic acids (GOPAs), and GOPAs and polyvinyl alcohol (PVA) are used to synthesize polyvinyl alcohol graphene oxide phosphonate and phosphinate (PVAGOPs) in the case of faint acidity and ultrasound irradiation, and PVAGOPs are used to fabricate PVAGOPs film, and the structure and morphology of GOPAs, PVAGOPs and PVAGOPs film are characterized, and the thermal stability and mechanical properties of PVAGOPs film are investigated. Based on these, it has been proved that GOPAs consist of graphene oxide phosphonic acid and graphene oxide phosphinic acid, and there are CP covalent bonds between them, and PVAGOPs are composed of GOPAs and PVA, and there are six-member lactone rings between GOPAs and PVA, and the thermal stability and mechanical properties of PVAGOPs film are improved effectively. Copyright © 2018 Elsevier B.V. All rights reserved.

40 CFR 721.10135 - Phosphinic acid, P,P-diethyl-, zinc salt (2:1).

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 32 2013-07-01 2013-07-01 false Phosphinic acid, P,P-diethyl-, zinc salt (2:1). 721.10135 Section 721.10135 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT SIGNIFICANT NEW USES OF CHEMICAL SUBSTANCES Significant New Uses for Specific Chemical Substances § 721.10135...

40 CFR 721.10135 - Phosphinic acid, P,P-diethyl-, zinc salt (2:1).

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Phosphinic acid, P,P-diethyl-, zinc salt (2:1). 721.10135 Section 721.10135 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT SIGNIFICANT NEW USES OF CHEMICAL SUBSTANCES Significant New Uses for Specific Chemical Substances § 721.10135...

40 CFR 721.10135 - Phosphinic acid, P,P-diethyl-, zinc salt (2:1).

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 32 2012-07-01 2012-07-01 false Phosphinic acid, P,P-diethyl-, zinc salt (2:1). 721.10135 Section 721.10135 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT SIGNIFICANT NEW USES OF CHEMICAL SUBSTANCES Significant New Uses for Specific Chemical Substances § 721.10135...

Methods for suppressing isomerization of olefin metathesis products

DOEpatents

Firth, Bruce E.; Kirk, Sharon E.; Gavaskar, Vasudeo S.

2015-09-22

A method for suppressing isomerization of an olefin metathesis product produced in a metathesis reaction includes adding an isomerization suppression agent to a mixture that includes the olefin metathesis product and residual metathesis catalyst from the metathesis reaction under conditions that are sufficient to passivate at least a portion of the residual metathesis catalyst. The isomerization suppression agent is phosphorous acid, a phosphorous acid ester, phosphinic acid, a phosphinic acid ester or combinations thereof. Methods of refining natural oils are described.

Method for separating metal chelates from other materials based on solubilities in supercritical fluids

DOEpatents

Wai, Chien M.; Smart, Neil G.; Phelps, Cindy

2001-01-01

A method for separating a desired metal or metalloi from impurities using a supercritical extraction process based on solubility differences between the components, as well as the ability to vary the solvent power of the supercritical fluid, is described. The use of adduct-forming agents, such as phosphorous-containing ligands, to separate metal or metalloid chelates in such processes is further disclosed. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is selected from the group consisting of .beta.-diketones; phosphine oxides, such as trialkylphosphine oxides, triarylphosphine oxides and alkylarylphosphine oxides; phosphinic acids; carboxylic acids; phosphates, such as trialkylphosphates, triarylphosphates and alkylarylphosphates; crown ethers; dithiocarbamates; phosphine sulfides; phosphorothioic acids; thiophosphinic acids; halogenated analogs of these chelating agents; and mixtures of these chelating agents. In especially preferred embodiments, at least one of the chelating agents is fluorinated.

Determination of polyfluoroalkyl phosphoric acid diesters, perfluoroalkyl phosphonic acids, perfluoroalkyl phosphinic acids, perfluoroalkyl carboxylic acids, and perfluoroalkane sulfonic acids in lake trout from the Great Lakes region.

PubMed

Guo, Rui; Reiner, Eric J; Bhavsar, Satyendra P; Helm, Paul A; Mabury, Scott A; Braekevelt, Eric; Tittlemier, Sheryl A

2012-11-01

A comprehensive method to extract perfluoroalkyl carboxylic acids, perfluoroalkane sulfonic acids, perfluoroalkyl phosphonic acids, perfluoroalkyl phosphinic acids, and polyfluoroalkyl phosphoric acid diesters simultaneously from fish samples has been developed. The recoveries of target compounds ranged from 78 % to 121 %. The new method was used to analyze lake trout (Salvelinus namaycush) from the Great Lakes region. The results showed that the total perfluoroalkane sulfonate concentrations ranged from 0.1 to 145 ng/g (wet weight) with perfluorooctane sulfonate (PFOS) as the dominant contaminant. Concentrations in fish between lakes were in the order of Lakes Ontario ≈ Erie > Huron > Superior ≈ Nipigon. The total perfluoroalkyl carboxylic acid concentrations ranged from 0.2 to 18.2 ng/g wet weight. The aggregate mean perfluorooctanoic acid (PFOA) concentration in fish across all lakes was 0.045 ± 0.023 ng/g. Mean concentrations of PFOA were not significantly different (p > 0.1) among the five lakes. Perfluoroalkyl phosphinic acids were detected in lake trout from Lake Ontario, Lake Erie, and Lake Huron with concentration ranging from non-detect (ND) to 0.032 ng/g. Polyfluoroalkyl phosphoric acid diesters were detected only in lake trout from Lake Huron, at levels similar to perfluorooctanoic acid.

Small Molecule Activation by Intermolecular Zr(IV)-Phosphine Frustrated Lewis Pairs.

PubMed

Metters, Owen J; Forrest, Sebastian J K; Sparkes, Hazel A; Manners, Ian; Wass, Duncan F

2016-02-17

We report intermolecular transition metal frustrated Lewis pairs (FLPs) based on zirconocene aryloxide and phosphine moieties that exhibit a broad range of small molecule activation chemistry that has previously been the preserve of only intramolecular pairs. Reactions with D2, CO2, THF, and PhCCH are reported. By contrast with previous intramolecular examples, these systems allow facile access to a variety of steric and electronic characteristics at the Lewis acidic and Lewis basic components, with the three-step syntheses of 10 new intermolecular transition metal FLPs being reported. Systematic variation to the phosphine Lewis base is used to unravel steric considerations, with the surprising conclusion that phosphines with relatively small Tolman steric parameters not only give highly reactive FLPs but are often seen to have the highest selectivity for the desired product. DOSY NMR spectroscopic studies on these systems reveal for the first time the nature of the Lewis acid/Lewis base interactions in transition metal FLPs of this type.

Special hydrogen bonds observed in two monovalent metal carboxylate-phosphinates: {NaH(Phsbnd PO2sbnd C2H4sbnd COOH)2}∞ and {[KH(Phsbnd PO2sbnd C2H4sbnd COOH)2]·H2O}∞

NASA Astrophysics Data System (ADS)

Zhao, Cui-Cui; Zhang, Jian-Wei; Zhou, Zhong-Gao; Du, Zi-Yi

2013-02-01

The addition of strong base such as sodium hydroxide or potassium hydroxide to the aqueous solution of (2-carboxyethyl)(phenyl)phosphinic acid afforded two novel monovalent metal carboxylate-phosphinates, namely, {NaH(Phsbnd PO2sbnd C2H4sbnd COOH)2}∞ (1) and {[KH(Phsbnd PO2sbnd C2H4sbnd COOH)2]·H2O}∞ (2). They represent the first examples of phosphinate containing short, symmetric or almost symmetric O⋯H⋯O hydrogen bonds.

Phosphine and methylphosphine production by simulated lightning—a study for the volatile phosphorus cycle and cloud formation in the earth atmosphere

NASA Astrophysics Data System (ADS)

Glindemann, Dietmar; Edwards, Marc; Schrems, Otto

Phosphine (PH 3), was recently found worldwide even in the remote atmosphere (Naturwissenschaften83(1996a)131; Atmos. Environ. 37(2003)24 29). It is of interest to find natural mechanisms which could produce phosphine gas and drive a volatile link of the atmospheric phosphorus cycle and the formation of phosphoric acid as possible condensation nuclei for clouds. Here, we report on simulated lightning exposing sodium phosphate in a reducing medium (methane model atmosphere or organic matter) for 5 s to a spark induced by microwave. The gas product analyzed by gas chromatography contained phosphine (yield up to 0.6 g kg -1 phosphate P) and methylphosphine (CH 3)PH 2 (yield up to 0.02 g kg -1 phosphate P). We suggest a plasma-chemical formation mechanism where organic compounds or methane or secondary hydrogen thereof reduce phosphate to phosphine of which a small fraction can subsequently react with methyl radicals to form methylphosphine. A small yield of 6 mg phosphine per kg phosphate P was even obtained in methane free medium, by simple plasmatic recombination of inorganic phosphorus. We believe that methane and hydrogen are useful model substances of pyrolytic gases with high reducing power which may form if lightning strikes biomass, soil and aerosol. These results suggest evidence that phosphine and methylphosphine (detectable in the field by intense garlic odor) are produced when atmospheric lightning strikes the ground or aerosol which is containing oxidized forms of phosphorus and chemical reductants. Additional reviewed data show that laboratory lightning was able to reduce a much more significant portion of phosphate to phosphite (up to 25% yield), methylphosphonic acid (up to 8.5% yield) and traces of hypophosphite in a matter of seconds.

Chemoselective ligation

DOEpatents

Saxon, Eliana [Albany, CA; Bertozzi, Carolyn Ruth [Berkeley, CA

2011-12-13

The present invention features a chemoselective ligation reaction that can be carried out under physiological conditions. In general, the invention involves condensation of a specifically engineered phosphine, which can provide for formation of an amide bond between the two reactive partners resulting in a final product comprising a phosphine moiety, or which can be engineered to comprise a cleavable linker so that a substituent of the phosphine is transferred to the azide, releasing an oxidized phosphine byproduct and producing a native amide bond in the final product. The selectivity of the reaction and its compatibility with aqueous environments provides for its application in vivo (e.g., on the cell surface or intracellularly) and in vitro (e.g., synthesis of peptides and other polymers, production of modified (e.g., labeled) amino acids).

Chemoselective ligation

DOEpatents

Saxon, Eliana; Bertozzi, Carolyn

2006-10-17

The present invention features a chemoselective ligation reaction that can be carried out under physiological conditions. In general, the invention involves condensation of a specifically engineered phosphine, which can provide for formation of an amide bond between the two reactive partners resulting in a final product comprising a phosphine moiety, or which can be engineered to comprise a cleavable linker so that a substituent of the phosphine is transferred to the azide, releasing an oxidized phosphine byproduct and producing a native amide bond in the final product. The selectivity of the reaction and its compatibility with aqueous environments provides for its application in vivo (e.g., on the cell surface or intracellularly) and in vitro (e.g., synthesis of peptides and other polymers, production of modified (e.g., labeled) amino acids).

Chemoselective ligation

DOEpatents

Saxon, Eliana [Albany, CA; Bertozzi, Carolyn R [Berkeley, CA

2011-05-10

The present invention features a chemoselective ligation reaction that can be carried out under physiological conditions. In general, the invention involves condensation of a specifically engineered phosphine, which can provide for formation of an amide bond between the two reactive partners resulting in a final product comprising a phosphine moiety, or which can be engineered to comprise a cleavable linker so that a substituent of the phosphine is transferred to the azide, releasing an oxidized phosphine byproduct and producing a native amide bond in the final product. The selectivity of the reaction and its compatibility with aqueous environments provides for its application in vivo (e.g., on the cell surface or intracellularly) and in vitro (e.g., synthesis of peptides and other polymers, production of modified (e.g., labeled) amino acids).

Chemoselective ligation

DOEpatents

Saxon, Eliana; Bertozzi, Carolyn Ruth

2010-11-23

The present invention features a chemoselective ligation reaction that can be carried out under physiological conditions. In general, the invention involves condensation of a specifically engineered phosphine, which can provide for formation of an amide bond between the two reactive partners resulting in a final product comprising a phosphine moiety, or which can be engineered to comprise a cleavable linker so that a substituent of the phosphine is transferred to the azide, releasing an oxidized phosphine byproduct and producing a native amide bond in the final product. The selectivity of the reaction and its compatibility with aqueous environments provides for its application in vivo (e.g., on the cell surface or intracellularly) and in vitro (e.g., synthesis of peptides and other polymers, production of modified (e.g., labeled) amino acids).

Chemoselective ligation

DOEpatents

Saxon, Eliana [Albany, CA; Bertozzi, Carolyn R [Berkeley, CA

2011-04-12

The present invention features a chemoselective ligation reaction that can be carried out under physiological conditions. In general, the invention involves condensation of a specifically engineered phosphine, which can provide for formation of an amide bond between the two reactive partners resulting in a final product comprising a phosphine moiety, or which can be engineered to comprise a cleavable linker so that a substituent of the phosphine is transferred to the azide, releasing an oxidized phosphine byproduct and producing a native amide bond in the final product. The selectivity of the reaction and its compatibility with aqueous environments provides for its application in vivo (e.g., on the cell surface or intracellularly) and in vitro (e.g., synthesis of peptides and other polymers, production of modified (e.g., labeled) amino acids).

Chemoselective ligation

DOEpatents

Saxon, Eliana; Bertozzi, Carolyn R.

2010-02-23

The present invention features a chemoselective ligation reaction that can be carried out under physiological conditions. In general, the invention involves condensation of a specifically engineered phosphine, which can provide for formation of an amide bond between the two reactive partners resulting in a final product comprising a phosphine moiety, or which can be engineered to comprise a cleavable linker so that a substituent of the phosphine is transferred to the azide, releasing an oxidized phosphine byproduct and producing a native amide bond in the final product. The selectivity of the reaction and its compatibility with aqueous environments provides for its application in vivo (e.g. on the cell surface or intracellularly) and in vitro (e.g., synthesis of peptides and other polymers, production of modified (e.g., labeled) amino acids).

Chemoselective ligation

DOEpatents

Saxon, Eliana [Albany, CA; Bertozzi, Carolyn [Berkeley, CA

2003-05-27

The present invention features a chemoselective ligation reaction that can be carried out under physiological conditions. In general, the invention involves condensation of a specifically engineered phosphine, which can provide for formation of an amide bond between the two reactive partners resulting in a final product comprising a phosphine moiety, or which can be engineered to comprise a cleavable linker so that a substituent of the phosphine is transferred to the azide, releasing an oxidized phosphine byproduct and producing a native amide bond in the final product. The selectivity of the reaction and its compatibility with aqueous environments provides for its application in vivo (e.g., on the cell surface or intracellularly) and in vitro (e.g., synthesis of peptides and other polymers, production of modified (e.g., labeled) amino acids).

An Infrared Spectroscopic Study Toward the Formation of Alkylphosphonic Acids and Their Precursors in Extraterrestrial Environments

NASA Astrophysics Data System (ADS)

Turner, Andrew M.; Abplanalp, Matthew J.; Blair, Tyler J.; Dayuha, Remwilyn; Kaiser, Ralf I.

2018-01-01

The only known phosphorus-containing organic compounds of extraterrestrial origin, alkylphosphonic acids, were discovered in the Murchison meteorite and have accelerated the hypothesis that reduced oxidation states of phosphorus were delivered to early Earth and served as a prebiotic source of phosphorus. While previous studies looking into the formation of these alkylphosphonic acids have focused on the iron–nickel phosphide mineral schreibersite and phosphorous acid as a source of phosphorus, this work utilizes phosphine (PH3), which has been discovered in the circumstellar envelope of IRC +10216, in the atmosphere of Jupiter and Saturn, and believed to be the phosphorus carrier in comet 67P/Churyumov–Gerasimenko. Phosphine ices prepared with interstellar molecules such as carbon dioxide, water, and methane were subjected to electron irradiation, which simulates the secondary electrons produced from galactic cosmic rays penetrating the ice, and probed using infrared spectroscopy to understand the possible formation of alkylphosphonic acids and their precursors on interstellar icy grains that could become incorporated into meteorites such as Murchison. We present the first study and results on the possible synthesis of alkylphosphonic acids produced from phosphine-mixed ices under interstellar conditions. All functional groups of alkylphosphonic acids were detected through infrared spectroscopically, suggesting that this class of molecules can be formed in interstellar ices.

Parameterization of phosphine ligands demonstrates enhancement of nickel catalysis via remote steric effects.

PubMed

Wu, Kevin; Doyle, Abigail G

2017-08-01

The field of Ni-catalysed cross-coupling has seen rapid recent growth because of the low cost of Ni, its earth abundance, and its ability to promote unique cross-coupling reactions. Whereas advances in the related field of Pd-catalysed cross-coupling have been driven by ligand design, the development of ligands specifically for Ni has received minimal attention. Here, we disclose a class of phosphines that enable the Ni-catalysed Csp 3 Suzuki coupling of acetals with boronic acids to generate benzylic ethers, a reaction that failed with known ligands for Ni and designer phosphines for Pd. Using parameters to quantify phosphine steric and electronic properties together with regression statistical analysis, we identify a model for ligand success. The study suggests that effective phosphines feature remote steric hindrance, a concept that could guide future ligand design tailored to Ni. Our analysis also reveals that two classic descriptors for ligand steric environment-cone angle and % buried volume-are not equivalent, despite their treatment in the literature.

Phosphine from rocks: mechanically driven phosphate reduction?

PubMed

Glindemann, Dietmar; Edwards, Marc; Morgenstern, Peter

2005-11-01

Natural rock and mineral samples released trace amounts of phosphine during dissolution in mineral acid. An order of magnitude more phosphine (average 1982 ng PH3 kg rock and maximum 6673 ng PH3/kg rock) is released from pulverized rock samples (basalt, gneiss, granite, clay, quartzitic pebbles, or marble). Phosphine was correlated to hardness and mechanical pulverization energy of the rocks. The yield of PH3 ranged from 0 to 0.01% of the total P content of the dissolved rock. Strong circumstantial evidence was gathered for reduction of phosphate in the rock via mechanochemical or "tribochemical" weathering at quartz and calcite/marble inclusions. Artificial reproduction of this mechanism by rubbing quartz rods coated with apatite-phosphate to the point of visible triboluminescence, led to detection of more than 70 000 ng/kg PH3 in the apatite. This reaction pathway may be considered a mechano-chemical analogue of phosphate reduction from lightning or electrical discharges and may contribute to phosphine production via tectonic forces and processing of rocks.

Parameterization of phosphine ligands demonstrates enhancement of nickel catalysis via remote steric effects

NASA Astrophysics Data System (ADS)

Wu, Kevin; Doyle, Abigail G.

2017-08-01

The field of Ni-catalysed cross-coupling has seen rapid recent growth because of the low cost of Ni, its earth abundance, and its ability to promote unique cross-coupling reactions. Whereas advances in the related field of Pd-catalysed cross-coupling have been driven by ligand design, the development of ligands specifically for Ni has received minimal attention. Here, we disclose a class of phosphines that enable the Ni-catalysed Csp3 Suzuki coupling of acetals with boronic acids to generate benzylic ethers, a reaction that failed with known ligands for Ni and designer phosphines for Pd. Using parameters to quantify phosphine steric and electronic properties together with regression statistical analysis, we identify a model for ligand success. The study suggests that effective phosphines feature remote steric hindrance, a concept that could guide future ligand design tailored to Ni. Our analysis also reveals that two classic descriptors for ligand steric environment—cone angle and % buried volume—are not equivalent, despite their treatment in the literature.

Iridium-Catalyzed Asymmetric Hydrogenation of Ketones with Accessible and Modular Ferrocene-Based Amino-phosphine Acid (f-Ampha) Ligands.

PubMed

Yu, Jianfei; Long, Jiao; Yang, Yuhong; Wu, Weilong; Xue, Peng; Chung, Lung Wa; Dong, Xiu-Qin; Zhang, Xumu

2017-02-03

A series of tridentate ferrocene-based amino-phosphine acid (f-Ampha) ligands have been successfully developed. The f-Ampha ligands are extremely air stable and exhibited excellent performance in the Ir-catalyzed asymmetric hydrogenation of ketones (full conversions, up to >99% ee, and 500 000 TON). DFT calculations were performed to elucidate the reaction mechanism and the importance of the -COOH group. Control experiments also revealed that the -COOH group played a key role in this reaction.

Methylene-bis[(aminomethyl)phosphinic acids]: synthesis, acid-base and coordination properties.

PubMed

David, Tomáš; Procházková, Soňa; Havlíčková, Jana; Kotek, Jan; Kubíček, Vojtěch; Hermann, Petr; Lukeš, Ivan

2013-02-21

Three symmetrical methylene-bis[(aminomethyl)phosphinic acids] bearing different substituents on the central carbon atom, (NH(2)CH(2))PO(2)H-C(R(1))(R(2))-PO(2)H(CH(2)NH(2)) where R(1) = OH, R(2) = Me (H(2)L(1)), R(1) = OH, R(2) = Ph (H(2)L(2)) and R(1),R(2) = H (H(2)L(3)), were synthesized. Acid-base and complexing properties of the ligands were studied in solution as well as in the solid state. The ligands show unusually high basicity of the nitrogen atoms (log K(1) = 9.5-10, log K(2) = 8.5-9) if compared with simple (aminomethyl)phosphinic acids and, consequently, high stability constants of the complexes with studied divalent metal ions. The study showed the important role of the hydroxo group attached to the central carbon atom of the geminal bis(phosphinate) moiety. Deprotonation of the hydroxo group yields the alcoholate anion which tends to play the role of a bridging ligand and induces formation of polynuclear complexes. Solid-state structures of complexes [H(2)N=C(NH(2))(2)][Cu(2)(H(-1)L(2))(2)]CO(3)·10H(2)O and Li(2)[Co(4)(H(-1)L(1))(3)(OH)]·17.5H(2)O were determined by X-ray diffraction. The complexes show unexpected geometries forming dinuclear and cubane-like structures, respectively. The dinuclear copper(II) complex contains a bridging μ(2)-alcoholate group with the (-)O-P(=O)-CH(2)-NH(2) fragments of each ligand molecule chelated to the different central ion. In the cubane cobalt(II) complex, one μ(3)-hydroxide and three μ(3)-alcoholate anions are located in the cube vertices and both phosphinate groups of one ligand molecule are chelating the same cobalt(II) ion while each of its amino groups are bound to different neighbouring metal ions. All such three metal ions are bridged by the alcoholate group of a given ligand.

Phosphazene diamines

NASA Technical Reports Server (NTRS)

Paciorek, K. L.; Harris, D. H.; Ito, T. I.; Kratzer, R. H.

1980-01-01

The synthesis of a specific phosphazene diamine was optimized, other phosphorus-containing diamines were prepared, and their effect upon certain characteristics of epoxy resins, prepared via reaction with MY 720, in particular, char yield at elevated temperatures was evaluated. The synthesis of the phosphazene diamine resulting from the interaction of methylenedianline with 4,4'-bis(diphenylphosphino)biphenyl was simplified into a one step process giving 77 percent yield of the pure product. Using this procedure, a related diamine containing bis(diphenylphosphino)methane was obtained in a 70 percent yield. Preparation of another class of phosphorus containing amines based upon p-aminophenyldiphenyl-phosphine was unsuccessful; the inability to produce p-aminophenylithlum was responsible for this failure. Seven epoxy resins employing Araldite MY 720, diaminodiphenylsulfone, and two of the phosphorus containing diamines were prepared, characterized, and their char yield capacity at elevated temperatures assessed. Based on these investigations, the resins containing phosphorus appear to exhibit significantly better char formation characteristics than materials hardened using conventional amines, without impairing the other properties measured.

The resolution of acyclic P-stereogenic phosphine oxides via the formation of diastereomeric complexes: A case study on ethyl-(2-methylphenyl)-phenylphosphine oxide.

PubMed

Bagi, Péter; Varga, Bence; Szilágyi, András; Karaghiosoff, Konstantin; Czugler, Mátyás; Fogassy, Elemér; Keglevich, György

2018-04-01

As an example of acyclic P-chiral phosphine oxides, the resolution of ethyl-(2-methylphenyl)-phenylphosphine oxide was elaborated with TADDOL derivatives, or with calcium salts of the tartaric acid derivatives. Besides the study on the resolving agents, several purification methods were developed in order to prepare enantiopure ethyl-(2-methylphenyl)-phenylphosphine oxide. It was found that the title phosphine oxide is a racemic crystal-forming compound, and the recrystallization of the enantiomeric mixtures could be used for the preparation of pure enantiomers. According to our best method, the (R)-ethyl-(2-methylphenyl)-phenylphosphine oxide could be obtained with an enantiomeric excess of 99% and in a yield of 47%. Complete racemization of the enantiomerically enriched phosphine oxide could be accomplished via the formation of a chlorophosphonium salt. Characterization of the crystal structures of the enantiopure phosphine oxide was complemented with that of the diastereomeric intermediate. X-ray analysis revealed the main nonbonding interactions responsible for enantiomeric recognition. © 2018 Wiley Periodicals, Inc.

A visible light-curable yet visible wavelength-transparent resin for stereolithography 3D printing

NASA Astrophysics Data System (ADS)

Park, Hong Key; Shin, Mikyung; Kim, Bongkyun; Park, Jin Woo; Lee, Haeshin

2018-04-01

Herein, a new polymeric resin for stereolithography (SLA) three-dimensional printing (SLA-3DP) is reported. An ultraviolet (UV) or visible (VIS) light source is critical for SLA printing technology. UV light can be used to manufacture 3D objects in SLA-3DP, but there are significant occupational safety and health issues (particularly for eyes). These issues prevent the widespread use of SLA-3DP at home or in the office. Through the use of VIS light, the safety and health issues can largely be solved, but only non-transparent 3D objects can be manufactured, which prevents the application of 3DP to the production of various common transparent consumer products. For these reasons, we developed a VIS light-curable yet visibly transparent resin for SLA-3DP, which also retains UV curability. The key was to identify the photoinitiator diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide (DPTBP). DPTBP was originally designed as a UV photoinitiator, but we found that VIS light irradiation is sufficient to split DPTBP and generate radicals due to its slight VIS light absorption up to 420 nm. The cured resin displays high transparency and beautiful transparent colors by incorporating various dyes; additionally, its mechanical properties are superior to those of commercial resins (Arario 410) and photoinitiators (Irgacure 2959).

Extracting metals directly from metal oxides

DOEpatents

Wai, Chien M.; Smart, Neil G.; Phelps, Cindy

1997-01-01

A method of extracting metals directly from metal oxides by exposing the oxide to a supercritical fluid solvent containing a chelating agent is described. Preferably, the metal is an actinide or a lanthanide. More preferably, the metal is uranium, thorium or plutonium. The chelating agent forms chelates that are soluble in the supercritical fluid, thereby allowing direct removal of the metal from the metal oxide. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is selected from the group consisting of .beta.-diketones, halogenated .beta.-diketones, phosphinic acids, halogenated phosphinic acids, carboxylic acids, halogenated carboxylic acids, and mixtures thereof. In especially preferred embodiments, at least one of the chelating agents is fluorinated. The method provides an environmentally benign process for removing metals from metal oxides without using acids or biologically harmful solvents. The chelate and supercritical fluid can be regenerated, and the metal recovered, to provide an economic, efficient process.

Extracting metals directly from metal oxides

DOEpatents

Wai, C.M.; Smart, N.G.; Phelps, C.

1997-02-25

A method of extracting metals directly from metal oxides by exposing the oxide to a supercritical fluid solvent containing a chelating agent is described. Preferably, the metal is an actinide or a lanthanide. More preferably, the metal is uranium, thorium or plutonium. The chelating agent forms chelates that are soluble in the supercritical fluid, thereby allowing direct removal of the metal from the metal oxide. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is selected from the group consisting of {beta}-diketones, halogenated {beta}-diketones, phosphinic acids, halogenated phosphinic acids, carboxylic acids, halogenated carboxylic acids, and mixtures thereof. In especially preferred embodiments, at least one of the chelating agents is fluorinated. The method provides an environmentally benign process for removing metals from metal oxides without using acids or biologically harmful solvents. The chelate and supercritical fluid can be regenerated, and the metal recovered, to provide an economic, efficient process. 4 figs.

Apparatus for purifying arsine, phosphine, ammonia, and inert gases to remove Lewis acid and oxidant impurities therefrom

DOEpatents

Tom, Glenn M.; Brown, Duncan W.

1991-01-08

An apparatus for purifying a gaseous mixture comprising arsine, phosphine, ammonia, and/or inert gases, to remove Lewis acid and/or oxidant impurities therefrom, comprising a vessel containing a bed of a scavenger, the scavenger including a support having associated therewith an anion which is effective to remove such impurities, such anion being selected from one or more members of the group consisting of: (i) carbanions whose corresponding protonated compounds have a pK.sub.a value of from about 22 to about 36; and (ii) anions formed by reaction of such carbanions with the primary component of the mixture.

Enzyme-Inspired Chiral Secondary-Phosphine-Oxide Ligand with Dual Noncovalent Interactions for Asymmetric Hydrogenation.

PubMed

Chen, Caiyou; Zhang, Zhefan; Jin, Shicheng; Fan, Xiangru; Geng, Mingyu; Zhou, Yan; Wen, Songwei; Wang, Xinrui; Chung, Lung Wa; Dong, Xiu-Qin; Zhang, Xumu

2017-06-06

Inspired by the unique character of enzymes, we developed novel chiral SPO (secondary-phosphine-oxide) ligand (SPO-Wudaphos) which can enter into both ion pair and H-bond noncovalent interactions. The novel chiral SPO-Wudaphos exhibited excellent results in the asymmetric hydrogenation of α-methylene-γ-keto carboxylic acids, affording the chiral γ-keto acids with up to over 99 % ee. A series of control experiments and DFT calculations were conducted to illustrate the critical roles of both the ion pair and H-bond noncovalent interactions. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of different photoinitiators and reducing agents on cure efficiency and color stability of resin-based composites using different LED wavelengths.

PubMed

de Oliveira, Dayane Carvalho Ramos Salles; Rocha, Mateus Garcia; Gatti, Alexandre; Correr, Americo Bortolazzo; Ferracane, Jack Liborio; Sinhoret, Mario Alexandre Coelho

2015-12-01

To evaluate the effect of photoinitiators and reducing agents on cure efficiency and color stability of resin-based composites using different LED wavelengths. Model resin-based composites were associated with diphenyl(2,4,6-trimethylbenzoyl) phosphine oxide (TPO), phenylbis(2,4,6-trimethylbenzoyl) phosphine oxide (BAPO) or camphorquinone (CQ) associated with 2-(dimethylamino) ethyl methacrylate (DMAEMA), ethyl 4-(dimethyamino) benzoate (EDMAB) or 4-(N,N-dimethylamino) phenethyl alcohol (DMPOH). A narrow (Smartlite, Dentisply) and a broad spectrum (Bluephase G2, Ivoclar Vivadent) LEDs were used for photo-activation (20 J/cm(2)). Fourier transform infrared spectroscopy (FT-IR) was used to evaluate the cure efficiency for each composite, and CIELab parameters to evaluated color stability (ΔE00) after aging. The UV-vis absorption spectrophotometric analysis of each photoinitiator and reducing agent was determined. Data were analyzed using two-way ANOVA and Tukey's test for multiple comparisons (α=0.05). Higher cure efficiency was found for type-I photoinitiators photo-activated with a broad spectrum light, and for CQ-systems with a narrow band spectrum light, except when combined with an aliphatic amine (DMAEMA). Also, when combined with aromatic amines (EDMAB and DMPOH), similar cure efficiency with both wavelength LEDs was found. TPO had no cure efficiency when light-cured exclusively with a blue narrowband spectrum. CQ-systems presented higher color stability than type-I photoinitiators, especially when combined with DMPOH. After aging, CQ-based composites became more yellow and BAPO and TPO lighter and less yellow. However, CQ-systems presented higher color stability than type-I photoinitiators, as BAPO- and TPO-, despite their higher cure efficiency when photo-activated with corresponding wavelength range. Color matching is initially important, but color change over time will be one of the major reasons for replacing esthetic restorations; despite the less yellowing of these alternative photoinitiators, camphorquinone presented higher color stability. Copyright © 2015 Elsevier Ltd. All rights reserved.

Site-specific incorporation of probes into RNA polymerase by unnatural-amino-acid mutagenesis and Staudinger-Bertozzi ligation

PubMed Central

Chakraborty, Anirban; Mazumder, Abhishek; Lin, Miaoxin; Hasemeyer, Adam; Xu, Qumiao; Wang, Dongye; Ebright, Yon W.; Ebright, Richard H.

2015-01-01

Summary A three-step procedure comprising (i) unnatural-amino-acid mutagenesis with 4-azido-phenylalanine, (ii) Staudinger-Bertozzi ligation with a probe-phosphine derivative, and (iii) in vitro reconstitution of RNA polymerase (RNAP) enables the efficient site-specific incorporation of a fluorescent probe, a spin label, a crosslinking agent, a cleaving agent, an affinity tag, or any other biochemical or biophysical probe, at any site of interest in RNAP. Straightforward extensions of the procedure enable the efficient site-specific incorporation of two or more different probes in two or more different subunits of RNAP. We present protocols for synthesis of probe-phosphine derivatives, preparation of RNAP subunits and the transcription initiation factor σ, unnatural amino acid mutagenesis of RNAP subunits and σ, Staudinger ligation with unnatural-amino-acid-containing RNAP subunits and σ, quantitation of labelling efficiency and labelling specificity, and reconstitution of RNAP. PMID:25665560

Discovery of potent and selective inhibitors of human aminopeptidases ERAP1 and ERAP2 by screening libraries of phosphorus-containing amino acid and dipeptide analogues.

PubMed

Węglarz-Tomczak, Ewelina; Vassiliou, Stamatia; Mucha, Artur

2016-08-15

A collection of fifty phosphonic and phosphinic acids was screened for inhibition of ERAP1 and ERAP2, the human endoplasmic reticulum aminopeptidases. The cooperative action of these enzymes is manifested by trimming a variety of antigenic precursors to be presented on the cell surface by major histocompatibility class I. The SAR studies revealed several potent compounds, particularly among the phosphinic dipeptide analogues, that were strong inhibitors of ERAP2 (Ki=100-350nM). A wide structural diversity of the applied organophosphorus compounds, predominantly non-proteinogenic analogues, allowed identification of representatives selective toward only one form of ERAP. For example, N'-substituted α,β-diaminophosphonates and phosphinates exhibited potency only toward ERAP2, which is in agreement with the P1 basic substrate-oriented specificity. Such discriminating ligands are invaluable tools for elucidating the precise role of a particular aminopeptidase in the concerted function of antigen processing and in human diseases. Copyright © 2016 Elsevier Ltd. All rights reserved.

Hydrogen storage and delivery: the carbon dioxide - formic acid couple.

PubMed

Laurenczy, Gábor

2011-01-01

Carbon dioxide and the carbonates, the available natural C1 sources, can be easily hydrogenated into formic acid and formates in water; the rate of this reduction strongly depends on the pH of the solution. This reaction is catalysed by ruthenium(II) pre-catalyst complexes with a large variety of water-soluble phosphine ligands; high conversions and turnover numbers have been realised. Although ruthenium(II) is predominant in these reactions, the iron(II) - tris[(2-diphenylphosphino)-ethyl]phosphine (PP3) complex is also active, showing a new perspective to use abundant and inexpensive iron-based compounds in the CO2 reduction. In the catalytic hydrogenation cycles the in situ formed metal hydride complexes play a key role, their structures with several other intermediates have been proven by multinuclear NMR spectroscopy. In the other hand safe and convenient hydrogen storage and supply is the fundamental question for the further development of the hydrogen economy; and carbon dioxide has been recognised to be a viable H2 vector. Formic acid--containing 4.4 weight % of H2, that is 53 g hydrogen per litre--is suitable for H2 storage; we have shown that in aqueous solutions it can be selectively decomposed into CO-free (CO < 10 ppm) CO2 and H2. The reaction takes place under mild experimental conditions and it is able to generate high pressure H2 (up to 600 bar). The cleavage of HCOOH is catalysed by several hydrophilic Ru(II) phosphine complexes (meta-trisulfonated triphenylphosphine, mTPPTS, being the most efficient one), either in homogeneous systems or as immobilised catalysts. We have also shown that the iron(II)--hydrido tris[(2-diphenylphosphino)ethyl]phosphine complex catalyses with an exceptionally high rate and efficiency (turnover frequency, TOF = 9425 h(-1)mol(-1); turnover number, TON = 92400) the formic acid cleavage, in environmentally friendly propylene carbonate solution, opening the way to use cheap, non-noble metal based catalysts for this reaction, too.

Curing and toughening of epoxy resins with phosphorus containing monomers and polymers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Park, Y.R.; Park, I.Y.; Yoon, T.H.

1996-12-31

Epoxy resins have been utilized in many areas, from house holds to airplanes, for the past several decades due to some exceptional properties such as low cost, good mechanical properties and excellent adhesive properties. However, low fracture toughness and flame resistance of epoxy resins have limited their applicability. Therefore, enhancing those properties have been of great interest to many researchers and scientists. As introduced by McGrath and co-workers in 1980s, the reactive thermoplastic polymers have proven to be an excellent toughener for improving not only fracture toughness but also adhesive properties without sacrificing thermo-mechanical properties and chemical resistance. Flame retardencymore » could be improved by adding flame retardent additives which are divided into two groups; additives and reactives. However, among the additives, halogen compounds are known to be toxic gas generator and ozone depleter. Moreover, additives could be potentially leached out of the material, while reactives are inferior to additives. Recently, a reactive type phosphine oxide containing flame retardants have been introduced by McGrath and co-workers and proven to be an excellent flame retardant. In this paper, phospine oxide containing monomers were prepared and utilized as curing agents for expoxy resins, and starting materials for the polymers.« less

40 CFR 721.10370 - Phosphonic acid, p-octyl-, lanthanum (3+) salt (2:1).

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 32 2013-07-01 2013-07-01 false Phosphonic acid, p-octyl-, lanthanum... New Uses for Specific Chemical Substances § 721.10370 Phosphonic acid, p-octyl-, lanthanum (3+) salt... substance identified as phosphinic acid, p-octyl-, lanthanum (3+) salt (2:1) (PMN P-10-99; CAS No. 1186211...

40 CFR 721.10370 - Phosphonic acid, p-octyl-, lanthanum (3+) salt (2:1).

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Phosphonic acid, p-octyl-, lanthanum... New Uses for Specific Chemical Substances § 721.10370 Phosphonic acid, p-octyl-, lanthanum (3+) salt... substance identified as phosphinic acid, p-octyl-, lanthanum (3+) salt (2:1) (PMN P-10-99; CAS No. 1186211...

40 CFR 721.10370 - Phosphonic acid, p-octyl-, lanthanum (3+) salt (2:1).

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 32 2012-07-01 2012-07-01 false Phosphonic acid, p-octyl-, lanthanum... New Uses for Specific Chemical Substances § 721.10370 Phosphonic acid, p-octyl-, lanthanum (3+) salt... substance identified as phosphinic acid, p-octyl-, lanthanum (3+) salt (2:1) (PMN P-10-99; CAS No. 1186211...

The betainic form of (imidazol-2-yl)phenylphosphinic acid hydrate

PubMed Central

Kunz, Peter C.; Frank, Walter

2010-01-01

Single crystals of the title compound, (imidazolium-2-yl)phenyl­phosphinate monohydrate, C9H9N2O2·H2O, were ob­tained from methanol/water after deprotection and oxidation of bis­(1-diethoxy­methyl­imidazol-2-yl)phenyl­phosphane. In the structure, several N–H⋯O and P—O⋯H–O hydrogen bonds are found. π–π inter­actions between the protonated imidazolyl rings [centroid–centroid distance = 3.977 (2) Å] help to establish the crystal packing. The hydrate water mol­ecule builds hydrogen bridges to three mol­ecules of the phosphinic acid by the O and both H atoms. PMID:21579513

Hydrogen generation at ambient conditions: application in fuel cells.

PubMed

Boddien, Albert; Loges, Björn; Junge, Henrik; Beller, Matthias

2008-01-01

The efficient generation of hydrogen from formic acid/amine adducts at ambient temperature is demonstrated. The highest catalytic activity (TOF up to 3630 h(-1) after 20 min) was observed in the presence of in situ generated ruthenium phosphine catalysts. Compared to the previously known methods to generate hydrogen from liquid feedstocks, the systems presented here can be operated at room temperature without the need for any high-temperature reforming processes, and the hydrogen produced can then be directly used in fuel cells. A variety of Ru precursors and phosphine ligands were investigated for the decomposition of formic acid/amine adducts. These catalytic systems are particularly interesting for the generation of H2 for new applications in portable electric devices.

Synthetic Analogs of Phospholipid Metabolites as Antimalarials.

DTIC Science & Technology

1979-07-01

phosphatidic acid analogs containing ether and phosphonate groups; completely non-hydrolyzable lecithin analogs containing phosphinate and ether groups...The phosphatidic acid and lecithin target compounds were successfully synthesized and submitted, together with a number of intermediates. A model of a... Phosphatidic acid analogs ......................... 5 Z.Z Lecithin Analogs .................................. 6 2.3 Analogs of Cytidine Diphosphate

RAILCAR4 Toxic Industrial Chemical Source Characterization Program (Software User’s Manual)

DTIC Science & Technology

2011-08-01

hydroxide (29%) boron trifluoride sulfur trioxide hydrogen chloride methyl bromide phosphine hydrochloric acid (39%) phosphoryl trichloride arsine...Data for Chlorine Trial 05-RC ...............................20 10 Nitric Acid Thermodynamic Properties...Table 1. TICs Available for RAILCAR Simulations chlorine hydrobromic acid (48%) acetylene tetrabromide ammonia OMPA o-anisidine ammonium

A structural insight into the P1S1 binding mode of diaminoethylphosphonic and phosphinic acids, selective inhibitors of alanine aminopeptidases

DOE Office of Scientific and Technical Information (OSTI.GOV)

Węglarz-Tomczak, Ewelina; Berlicki, Łukasz; Pawełczak, Małgorzata

N0 -substituted 1,2-diaminoethylphosphonic acids and 1,2-diaminoethylphosphinic dipeptides were explored to unveil the structural context of the unexpected selectivity of these inhibitors of M1 alanine aminopeptidases (APNs) versus M17 leucine aminopeptidase (LAP). The diaminophosphonic acids were obtained via aziridines in an improved synthetic procedure that was further expanded for the phosphinic pseudodipeptide system. The inhibitory activity, measured for three M1 and one M17 metalloaminopeptidases of different sources (bacterial, human and porcine), revealed several potent compounds (e.g., Ki ¼ 65 nM of 1u for HsAPN). Two structures of an M1 representative (APN from Neisseria meningitidis) in complex with N-benzyl-1,2-diaminoethylphosphonic acid and N-cyclohexyl-1,2-more » diaminoethylphosphonic acid were determined by the X-ray crystallography. The analysis of these structures and the models of the phosphonic acid complexes of the human ortholog provided an insight into the role of the additional amino group and the hydrophobic substituents of the ligands within the S1 active site region.« less

VIABILITY OF BACILLUS SUBTILIS SPORES IN ROCKET PROPELLANTS.

PubMed

GODDING, R M; LYNCH, V H

1965-01-01

The sporicidal activity of components used in liquid and solid rocket propellants was tested by use of spores of Bacillus subtilis dried on powdered glass. Liquid propellant ingredients tested were N(2)O(4), monomethylhydrazine and 1,1-dimethylhydrazine. N(2)O(4) was immediately sporicidal; the hydrazines were effective within several days. Solid propellants consisted of ammonium perchlorate in combination with epoxy resin (EPON 828), tris-1-(2-methyl) aziridinyl phosphine oxide, bis-1-(2-methyl) aziridinyl phenylphosphine oxide, and three modified polybutadiene polymers. There was no indication of appreciable sporicidal activity of these components.

Viability of Bacillus subtilis Spores in Rocket Propellants

PubMed Central

Godding, Rogene M.; Lynch, Victoria H.

1965-01-01

The sporicidal activity of components used in liquid and solid rocket propellants was tested by use of spores of Bacillus subtilis dried on powdered glass. Liquid propellant ingredients tested were N2O4, monomethylhydrazine and 1,1-dimethylhydrazine. N2O4 was immediately sporicidal; the hydrazines were effective within several days. Solid propellants consisted of ammonium perchlorate in combination with epoxy resin (EPON 828), tris-1-(2-methyl) aziridinyl phosphine oxide, bis-1-(2-methyl) aziridinyl phenylphosphine oxide, and three modified polybutadiene polymers. There was no indication of appreciable sporicidal activity of these components. PMID:14264838

Oxygen plasma resistant phosphine oxide containing imide/arylene copolymers

NASA Technical Reports Server (NTRS)

Jensen, Brian J.

1993-01-01

A series of oxygen plasma resistant imide/arylene ether copolymers were prepared by reacting anhydride-terminated poly(amide acids) and amine-terminated polyarylene ethers containing phosphine oxide units. Inherent viscosities for these copolymers ranged from 0.42 to 0.80 dL/g. After curing, the resulting copolymers had glass transition temperatures ranging from 224 C to 228 C. Solution cast films of the block copolymers were tough and flexible with tensile strength, tensile moduli, and elongation at break up to 16.1 ksi, 439 ksi, and 23 percent, respectively at 25 C and 9.1 ksi, 308 ksi and 97 percent, respectively at 150 C. The copolymers show a significant improvement in resistance to oxygen plasma when compared to the commercial polyimide Kapton. The imide/arylene ether copolymers containing phosphine oxide units are suitable as coatings, films, adhesives, and composite matrices.

Changes in fats and resins of Pinus radiata associated with heartwood formation

Treesearch

Richard W. Hemingway; W.E. Hillis

1971-01-01

In an analysis of Australian grown P. radiata marked changes were found in the relative proportions and compositions of the resin acids, fatty acids, and fatty acid esters associated with heartwood formation. While the proportion of resin acids increased substantially in the heartwood, there was little change in resin acid composition from outer...

21 CFR 175.260 - Partial phosphoric acid esters of polyester resins.

Code of Federal Regulations, 2011 CFR

2011-04-01

... 21 Food and Drugs 3 2011-04-01 2011-04-01 false Partial phosphoric acid esters of polyester resins... of polyester resins. Partial phosphoric acid esters of polyester resins identified in this section... prescribed conditions: (a) For the purpose of this section, partial phosphoric acid esters of polyester...

21 CFR 573.120 - Acrylamide-acrylic acid resin.

Code of Federal Regulations, 2010 CFR

2010-04-01

...) ANIMAL DRUGS, FEEDS, AND RELATED PRODUCTS FOOD ADDITIVES PERMITTED IN FEED AND DRINKING WATER OF ANIMALS Food Additive Listing § 573.120 Acrylamide-acrylic acid resin. Acrylamide-acrylic acid resin... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Acrylamide-acrylic acid resin. 573.120 Section 573...

21 CFR 573.120 - Acrylamide-acrylic acid resin.

Code of Federal Regulations, 2013 CFR

2013-04-01

...) ANIMAL DRUGS, FEEDS, AND RELATED PRODUCTS FOOD ADDITIVES PERMITTED IN FEED AND DRINKING WATER OF ANIMALS Food Additive Listing § 573.120 Acrylamide-acrylic acid resin. Acrylamide-acrylic acid resin... 21 Food and Drugs 6 2013-04-01 2013-04-01 false Acrylamide-acrylic acid resin. 573.120 Section 573...

21 CFR 573.120 - Acrylamide-acrylic acid resin.

Code of Federal Regulations, 2014 CFR

2014-04-01

...) ANIMAL DRUGS, FEEDS, AND RELATED PRODUCTS FOOD ADDITIVES PERMITTED IN FEED AND DRINKING WATER OF ANIMALS Food Additive Listing § 573.120 Acrylamide-acrylic acid resin. Acrylamide-acrylic acid resin... 21 Food and Drugs 6 2014-04-01 2014-04-01 false Acrylamide-acrylic acid resin. 573.120 Section 573...

21 CFR 573.120 - Acrylamide-acrylic acid resin.

Code of Federal Regulations, 2012 CFR

2012-04-01

...) ANIMAL DRUGS, FEEDS, AND RELATED PRODUCTS FOOD ADDITIVES PERMITTED IN FEED AND DRINKING WATER OF ANIMALS Food Additive Listing § 573.120 Acrylamide-acrylic acid resin. Acrylamide-acrylic acid resin... 21 Food and Drugs 6 2012-04-01 2012-04-01 false Acrylamide-acrylic acid resin. 573.120 Section 573...

21 CFR 573.120 - Acrylamide-acrylic acid resin.

Code of Federal Regulations, 2011 CFR

2011-04-01

...) ANIMAL DRUGS, FEEDS, AND RELATED PRODUCTS FOOD ADDITIVES PERMITTED IN FEED AND DRINKING WATER OF ANIMALS Food Additive Listing § 573.120 Acrylamide-acrylic acid resin. Acrylamide-acrylic acid resin... 21 Food and Drugs 6 2011-04-01 2011-04-01 false Acrylamide-acrylic acid resin. 573.120 Section 573...

Synthesis and Structural Studies of Calcium and Magnesium Phosphinate and Phosphonate Compounds

NASA Astrophysics Data System (ADS)

Bampoh, Victoria Naa Kwale

The work presented herein describes synthetic methodologies leading to the design of a wide array of magnesium and calcium based phosphinate and phosphonates with possible applications as bone scaffolding materials or additives to bone cements. The challenge to the chemistry of the alkaline earth phosphonate target compounds includes poor solubility of compounds, and poorly understood details on the control of the metal's coordination environment. Hence, less is known on phosphonate based alkaline earth metal organic frameworks as compared to transition metal phosphonates. Factors governing the challenges in obtaining crystalline, well-defined magnesium and calcium solids lie in the large metal diameters, the absence of energetically available d-orbitals to direct metal geometry, as well as the overall weakness of the metal-ligand bonds. A significant part of this project was concerned with the development of suitable reaction conditions to obtain X-ray quality crystals of the reaction products to allow for structural elucidation of the novel compounds. Various methodologies to aid in crystal growth including hydrothermal methods and gel crystallization were employed. We have used phosphinate and phosphonate ligands with different number of phosphorus oxygen atoms as well as diphosphonates with different linker lengths to determine their effects on the overall structural features. An interesting correlation is observed between the dimensionality of products and the increasing number of donor oxygen atoms in the ligands as we progress from phosphinic acid to the phosphorous acids. As an example, monophosphinate ligand only yielded one-dimensional compounds, whereas the phosphonates crystallize as one and two-dimensional compounds, and the di- and triphosphonate based compounds display two or three-dimensional geometries. This thesis provides a selection of calcium and magnesium compounds with one-dimensional geometry, as represented in a calcium phosphinate to novel two-dimensional sheets of magnesium and pillared calcium phosphonates. The preparation of these novel compounds has led to the establishment of synthetic protocols that allow for the direct preparation of compounds with defined structural features.

21 CFR 176.110 - Acrylamide-acrylic acid resins.

Code of Federal Regulations, 2011 CFR

2011-04-01

... 21 Food and Drugs 3 2011-04-01 2011-04-01 false Acrylamide-acrylic acid resins. 176.110 Section... Substances for Use Only as Components of Paper and Paperboard § 176.110 Acrylamide-acrylic acid resins. Acrylamide-acrylic acid resins may be safely used as components of articles intended for use in producing...

21 CFR 176.110 - Acrylamide-acrylic acid resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Acrylamide-acrylic acid resins. 176.110 Section 176... Substances for Use Only as Components of Paper and Paperboard § 176.110 Acrylamide-acrylic acid resins. Acrylamide-acrylic acid resins may be safely used as components of articles intended for use in producing...

Fixed-charge phosphine ligands to explore gas-phase coinage metal-mediated decarboxylation reactions.

PubMed

Vikse, Krista; Khairallah, George N; McIndoe, J Scott; O'Hair, Richard A J

2013-05-14

A combination of multistage mass spectrometry experiments and density functional theory (DFT) calculations were used to examine the decarboxylation reactions of a series of metal carboxylate complexes bearing a fixed-charge phosphine ligand, [(O3SC6H4)(C6H5)2PM(I)O2CR](-) (M = Cu, Ag, Au; R = Me, Et, benzyl, Ph). Collision-induced dissociation (CID) of these complexes using an LTQ linear ion mass spectrometer results in three main classes of reactions being observed: (1) decarboxylation; (2) loss of the phosphine ligand; (3) loss of carboxylic acid. The gas-phase unimolecular chemistry of the resultant decarboxylated organometallic ions, [(O3SC6H4)(C6H5)2PM(I)R](-), were also explored using CID experiments, and fragment primarily via loss of the phosphine ligand. Energy-resolved CID experiments on [(O3SC6H4)(C6H5)2PM(I)O2CR](-) (M = Cu, Ag, Au; R = Me, Et, benzyl, Ph) using a Q-TOF mass spectrometer were performed to gain a more detailed understanding of the factors influencing coinage metal-catalyzed decarboxylation and DFT calculations on the major fragmentation pathways aided in interpretation of the experimental results. Key findings are that: (1) the energy required for loss of the phosphine ligand follows the order Ag < Cu < Au; (2) the ease of decarboxylation of the coordinated RCO2 groups follows the order of R: Ph < PhCH2 < Me < Et; (3) in general, copper is best at facilitating decarboxylation, followed by gold then silver. The one exception to this trend is when R = Ph and M = Au which has the highest overall propensity for decarboxylation. The influence of the phosphine ligand on decarboxylation is also considered in comparison with previous studies on metal carboxylates that do not contain a phosphine ligand.

Development of a Lewis Base Catalyzed Selenocyclization Reaction

ERIC Educational Resources Information Center

Collins, William

2009-01-01

The concept of Lewis base activation of selenium Lewis acids has been effectively reduced to practice in the Lewis base catalyzed selenofunctionalization of unactivated olefins. In this reaction, the weakly acidic species, "N"-phenylselenyl succinimide, is cooperatively activated by the addition of a "soft" Lewis base donor (phosphine sulfides,…

Diphasic acido-basic properties of D(octylphenyl)phosphoric acid (DOPPA)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sella, C.; Cote, G.; Bauer, D.

1995-07-01

In the first part of this work, the diphasic acido-basic constant (pka*) of di(octylphenyl)phosphoric acid, denoted hereafter DOPPA or HL, is determined from its experimental diphasic neutralization curve. The pka* value of DOPPA appears to be equal to 2.6 in the presence of 1 mol/dm{sup 3} sodium salt. Such a value is significantly lower than that previously determined for di(2-ethylhexyl) phosphoric acid (DEHPA, pka* = 5.2), 2-ethylhexylphosphonic acid, mono-2-ethylhexyl ester (PC88A, pka* = 7.1) and di(2,4,4-trimethylpentyl)phosphinic acid (CYANEX 272, pka* = 8.7). DOPPA (HL) is definitely more acidic than the other organophosphorus acids because its acidic proton can be easilymore » exchanged with sodium cation to form Na{sup +}HL{sub 2}{sup -} species in organic phase. In the second and final part of the work, molecular modelling is used to model the dimers of various organophosphorus acids. A structure-activity relationship is obtained between the association energies of modelled dimers and their diphasic acido-basic constants. This relationship is then used for predicting the pka* values of DOPPOA and DOPPIA which are the phosphonic and phosphinic analogs of DOPPA, respectively. 16 refs., 5 figs., 4 tabs.« less

Biodegradation of resin acid sodium salts

Treesearch

Richard W. Hemingway; H. Greaves

1973-01-01

The sodium salts of resin acids were readily degraded by microflora from two types of river water and from an activated sewage sludge. A lag phase with little or no resin acid salt degradation but rapid bacterial development occurred which was greatly extended by a decrease in incubation temperature. After this initial lag phase, the resin acid salts were rapidly...

Automated protein hydrolysis delivering sample to a solid acid catalyst for amino acid analysis.

PubMed

Masuda, Akiko; Dohmae, Naoshi

2010-11-01

In this study, we developed an automatic protein hydrolysis system using strong cation-exchange resins as solid acid catalysts. Examining several kinds of inorganic solid acids and cation-exchange resins, we found that a few cation-exchange resins worked as acid catalysts for protein hydrolysis when heated in the presence of water. The most efficient resin yielded amounts of amino acids that were over 70% of those recovered after conventional hydrolysis with hydrochloric acid and resulted in amino acid compositions matching the theoretical values. The solid-acid hydrolysis was automated by packing the resin into columns, combining the columns with a high-performance liquid chromatography system, and heating them. The amino acids that constitute a protein can thereby be determined, minimizing contamination from the environment.

Inhibition of Xenobiotic-Degrading Hydrolases by Organophosphinates

DTIC Science & Technology

1985-07-01

transient increase in the salicylic acid hydrolysis product was observed. Pretreatment with 4-nitrophenyl methyl(phenyl)phosphinate had no significant...h. Hydroly- sis of aspirin was not reduced in pretreated mice, although a transient increase in the salicylic acid hydrolysis product was observed...26 Figure 1. Pathways of aspirin metabolism in mammals: CE is carboxylester hydrolase, SA is salicylic acid, SU is salicyluric

Synthesis of a Novel Phosphorus-Containing Flame Retardant Curing Agent and Its Application in Epoxy Resins.

PubMed

Zhang, Hongkun; Xu, Miaojun; Li, Bin

2016-03-01

A novel phosphorus-containing compound diphenyl-(2,5-dihydroxyphenyl)-phosphine oxide defined as DPDHPPO was synthesized and used as flame retardant and curing agent for epoxy resins (EP). The chemical structure was well characterized by Fourier transform infrared (FTIR) spectroscopy, 1H, 13C and 31P nuclear magnetic resonance. The flame retardant properties, combusting performances and thermal degradation behaviors of the cured epoxy resins were investigated by limiting oxygen index (LOI), vertical burning tests (UL-94), cone calorimeter and thermogravimetric analysis (TGA) tests. The morphologies and chemical compositions of char residues for cured epoxy resins were investigated by scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS), respectively. The water resistant properties were evaluated by putting the samples into distilled water at 70 degrees C for 168 h. The results revealed that the EP/40 wt% DPDHPPO/60 wt% PDA thermosets successfully passed UL-94 V-0 flammability rating and the LOI value was as high as 31.9%. The cone tests results revealed that the incorporation of DPDHPPO efficiently reduced the combustion parameters of epoxy resins thermosets, such as heat release rate (HRR), total heat release (THR) and so on. The TGA results indicated that the introduction of DPDHPPO promoted epoxy resins matrix decomposed ahead of time compared with that of pure EP and led to a higher char yield and thermal stability at high temperature. The morphological structures and analysis of XPS of char residues revealed that DPDHPPO benefited to the formation of a sufficient, compact and homogeneous char layer with rich flame retardant elements on the epoxy resins materials surface during combustion. After water resistance tests, EP/40 wt% DPDHPPO/60 wt% PDA thermosets still remained excellent flame retardancy, the moisture absorption of epoxy resins thermosets decreased with the increase of DPDHPPO contents in the thermosets due to the existing of P-C bonds and the rigid aromatic hydrophobic structure.

40 CFR 414.40 - Applicability; description of the thermoplastic resins subcategory.

Code of Federal Regulations, 2010 CFR

2010-07-01

... *Ethylene-Methacrylic Acid Copolymers *Ethylene-Vinyl Acetate Copolymers *Fatty Acid Resins *Fluorocarbon..., Acrylates (Latex) *PVC Copolymers, Ethylene-Vinyl Chloride *Rosin Derivative Resins *Rosin Modified Resins...

Homogeneous Palladium-Catalyzed Transfer Hydrogenolysis of Benzylic Alcohols Using Formic Acid as Reductant.

PubMed

Ciszek, Benjamin; Fleischer, Ivana

2018-04-12

Herein we report the first homogeneous palladium-based transfer hydrogenolysis of benzylic alcohols using an in situ formed palladium-phosphine complex and formic acid as reducing agent. The reaction requires a catalyst loading as low as only 1 mol% of palladium and just a slight excess of reductant to obtain the deoxygenated alkylarenes in good to excellent yields. Besides demonstrating the broad applicability for primary, secondary and tertiary benzylic alcohols, a reaction intermediate could be identified. Additionally, it could be shown that partial oxidation of the applied phosphine ligand was beneficial for the course of the reaction, presumably by stabilizing the active catalyst. Reaction profiles and catalyst poisoning experiments were used to characterize the catalyst, the results indicate a homogeneous metal complex as active species. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chemical Reaction between Boric Acid and Phosphine Indicates Boric Acid as an Antidote for Aluminium Phosphide Poisoning.

PubMed

Soltani, Motahareh; Shetab-Boushehri, Seyed F; Shetab-Boushehri, Seyed V

2016-08-01

Aluminium phosphide (AlP) is a fumigant pesticide which protects stored grains from insects and rodents. When it comes into contact with moisture, AlP releases phosphine (PH3), a highly toxic gas. No efficient antidote has been found for AlP poisoning so far and most people who are poisoned do not survive. Boric acid is a Lewis acid with an empty p orbital which accepts electrons. This study aimed to investigate the neutralisation of PH3 gas with boric acid. This study was carried out at the Baharlou Hospital, Tehran University of Medical Sciences, Tehran, Iran, between December 2013 and February 2014. The volume of released gas, rate of gas evolution and changes in pH were measured during reactions of AlP tablets with water, acidified water, saturated boric acid solution, acidified saturated boric acid solution, activated charcoal and acidified activated charcoal. Infrared spectroscopy was used to study the resulting probable adduct between PH3 and boric acid. Activated charcoal significantly reduced the volume of released gas (P <0.01). Although boric acid did not significantly reduce the volume of released gas, it significantly reduced the rate of gas evolution (P <0.01). A gaseous adduct was formed in the reaction between pure AlP and boric acid. These findings indicate that boric acid may be an efficient and non-toxic antidote for PH3 poisoning.

Bifunctional phenyl monophosphonic/sulfonic acid ion exchange resin and process for using the same

DOEpatents

Alexandratos, Spiro; Shelley, Christopher A.; Horwitz, E. Philip; Chiarizia, Renato

2001-01-01

A cross-linked water-insoluble ion exchange resin comprised of polymerized monomers having a phenyl ring is disclosed. A contemplated resin contains (i) polymerized phenyl ring-containing monomers having a phosphonic acid ligand linked to the phenyl ring, (ii) about 2 to about 5 millimoles per gram (mmol/g) of phosphorus as phosphonic acid ligands, and (iii) a sufficient amount of a sulfonic acid ligand such that the ratio of mmol/g of phosphonic acid to mmol/g sulfonic acid is up to 3:1. A process for removing polyvalent metal cations from aqueous solution, and a process for removing iron(III) cations from acidic copper(II) cation-containing solutions that utilize the contemplated resin or other resins are disclosed.

Bifunctional phenyl monophosphonic/sulfonic acid ion exchange resin and process for using the same

DOEpatents

Alexandratos, Spiro; Shelley, Christopher A.; Horwitz, E. Philip; Chiarizia, Renato; Gula, Michael J.; Xue, Sui; Harvey, James T.

2002-01-01

A cross-linked water-insoluble ion exchange resin comprised of polymerized monomers having a phenyl ring is disclosed. A contemplated resin contains (i) polymerized phenyl ring-containing monomers having a phosphonic acid ligand linked to the phenyl ring, (ii) about 2 to about 5 millimoles per gram (mmol/g) of phosphorus as phosphonic acid ligands, and (iii) a sufficient amount of a sulfonic acid ligand such that the ratio of mmol/g of phosphonic acid to mmol/g sulfonic acid is up to 3:1. A process for removing polyvalent metal cations from aqueous solution, and a process for removing iron(III) cations from acidic copper(II) cation-containing solutions that utilize the contemplated resin or other resins are disclosed.

Tailored Gallium(III) chelator NOPO: synthesis, characterization, bioconjugation, and application in preclinical Ga-68-PET imaging.

PubMed

Simeček, Jakub; Zemek, Ondřej; Hermann, Petr; Notni, Johannes; Wester, Hans-Jürgen

2014-11-03

The bifunctional chelator NOPO (1,4,7-triazacyclononane-1,4-bis[methylene(hydroxymethyl)phosphinic acid]-7-[methylene(2-carboxyethyl)phosphinic acid]) shows remarkably high Ga(III) complexation efficiency and comprises one carboxylic acid moiety which is not involved into metal ion coordination. An improved synthetic protocol affords NOPO with 45% overall yield. Stepwise protonation constants (log Ka), determined by potentiometry, are 11.96, 5.22, 3.77, and 1.54; the stability constant of the Ga(III) complex is log KGaL = 25.0. Within 5 min, (68)Ga(III) incorporation by NOPO is virtually quantitative at room temperature between pH 3 and 4, and at 95 °C at pH ranging from 0.5 to 7, at NOPO concentrations of 30 μM and 10 μM, respectively. During amide bond formation at the distant carboxylate using the HATU coupling reagent, an intramolecular phosphinic acid ester (phosphilactone) is formed, which is cleaved during (68)Ga complexation or in acidic media, such as trifluoroacetic acid (TFA). Phosphilactone formation can also be suppressed by complexation of Zn(2+) prior to conjugation, the resulting zinc-containing conjugates nevertheless being suitable for direct (68)Ga-labeling. In AR42J (rat pancreatic carcinoma) xenografted CD-1 nude mice, (68)Ga-labeled NOPO-NaI(3)-octreotide conjugate ((68)Ga-NOPO-NOC) showed high and fully blockable tumor uptake (13.9 ± 5% ID/g, 120 min p.i., compared to 0.9 ± 0.4% ID/g with 5 mg/kg of nonlabeled peptide). Uptake in other tissues was generally below 3% ID/g, except appearance of excretion-related activity accumulation in kidneys. NOPO-functionalized compounds tend to be more hydrophilic than the corresponding DOTA- and NODAGA-conjugates, thus promoting fast and extensive renal excretion of (68)Ga-NOPO-radiopharmaceuticals. NOPO-functionalized peptides provide suitable pharmacokinetics in vivo and meet all requirements for efficient (68)Ga-labeling even at room temperature in a kit-like manner.

Reaction catalysts of urea-formaldehyde resin, as related to strength properties of southern pine particleboard

Treesearch

C. -Y. Hse

1974-01-01

Twelve resins were formulated with factorial combinations of three alkaline catalysts (i.e., somdium hydroxide, hexamethylenetetramine, and triethanolamine) and four acidic catalysts (i.e., acetic acid, hydrochloric acid, ammonium chloride, and phosphoric acid). The resins were replicated.

Resin–dentin bonds to EDTA-treated vs. acid-etched dentin using ethanol wet-bonding

PubMed Central

Sauro, Salvatore; Toledano, Manuel; Aguilera, Fatima Sánchez; Mannocci, Francesco; Pashley, David H.; Tay, Franklin R.; Watson, Timothy F.; Osorio, Raquel

2013-01-01

Objective To compare resin–dentin bond strengths and the micropermeability of hydrophobic vs. hydrophilic resins bonded to acid-etched or EDTA-treated dentin, using the ethanol wet-bonding technique. Methods Flat dentin surfaces from extracted human third molars were conditioned before bonding with: 37% H3PO4 (15 s) or 0.1 M EDTA (60 s). Five experimental resin blends of different hydrophilicities and one commercial adhesive (SBMP: Scotchbond Multi-Purpose) were applied to ethanol wet-dentin (1 min) and light-cured (20 s). The solvated resins were used as primers (50% ethanol/50% comonomers) and their respective neat resins were used as the adhesive. The resin-bonded teeth were stored in distilled water (24 h) and sectioned in beams for microtensile bond strength testing. Modes of failure were examined by stereoscopic light microscopy and SEM. Confocal tandem scanning microscopy (TSM) interfacial characterization and micropermeability were also performed after filling the pulp chamber with 1 wt% aqueous rhodamine-B. Results The most hydrophobic resin 1 gave the lowest bond strength values to acid-etched dentin and all beams failed prematurely when the resin was applied to EDTA-treated dentin. Resins 2 and 3 gave intermediate bond strengths to both conditioned substrates. Resin 4, an acidic hydrophilic resin, gave the highest bond strengths to both EDTA-treated and acid-etched dentin. Resin 5 was the only hydrophilic resin showing poor resin infiltration when applied on acid-etched dentin. Significance The ethanol wet-bonding technique may improve the infiltration of most of the adhesives used in this study into dentin, especially when applied to EDTA-treated dentin. The chemical composition of the resin blends was a determining factor influencing the ability of adhesives to bond to EDTA-treated or 37% H3PO4 acid-etched dentin, when using the ethanol wet-bonding technique in a clinically relevant time period. PMID:20074787

Phosphinic acid functionalized polyazacycloalkane chelators for radiodiagnostics and radiotherapeutics: unique characteristics and applications.

PubMed

Notni, Johannes; Šimeček, Jakub; Wester, Hans-Jürgen

2014-06-01

Given the wide application of positron emission tomography (PET), positron-emitting metal radionuclides have received much attention recently. Of these, gallium-68 has become particularly popular, as it is the only PET nuclide commercially available from radionuclide generators, therefore allowing local production of PET radiotracers independent of an on-site cyclotron. Hence, interest in optimized bifunctional chelators for the elaboration of (68) Ga-labeled bioconjugates has been rekindled as well, resulting in the development of improved triazacyclononane-triphosphinate (TRAP) ligand structures. The most remarkable features of these ligands are unparalleled selectivity for Ga(III) , rapid Ga(III) complexation kinetics, extraordinarily high thermodynamic stability, and kinetic inertness of the respective Ga(III) chelates. As a result, TRAP chelators exhibit very favorable (68) Ga-labeling properties. Based on the scaffolds NOPO (1,4,7-triazacyclononane-1,4-bis[methylene(hydroxymethyl)phosphinic acid]-7-[methylene(2-carboxyethyl)phosphinic acid]) and TRAP-Pr, tailored for convenient preparation of (68) Ga-labeled monomeric and multimeric bioconjugates, a variety of novel (68) Ga radiopharmaceuticals have been synthesized. These include bisphosphonates, somatostatin receptor ligands, prostate-specific membrane antigen (PSMA)-targeting peptides, and cyclic RGD pentapeptides, for in vivo PET imaging of bone, neuroendocrine tumors, prostate cancer, and integrin expression, respectively. Furthermore, TRAP-based (68) Ga-labeled gadolinium(III) complexes have been proposed as bimodal probes for PET/MRI, and a cyclen-based analogue of TRAP-Pr has been suggested for the elaboration of targeted radiotherapeutics comprising radiolanthanide ions. Thus, polyazacycloalkane-based polyphosphinic acid chelators are a powerful toolbox for pharmaceutical research, particularly for the development of (68) Ga radiopharmaceuticals. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

21 CFR 175.260 - Partial phosphoric acid esters of polyester resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

... resins are prepared by the reaction of trimellitic anhydride with 2,2-dimethyl-1,3-propanediol followed by reaction of the resin thus produced with phosphoric acid anhydride to produce a resin having an...

Environmentally Friendly Bio-Based Vinyl Ester Resins for Military Composite Structures

DTIC Science & Technology

2008-12-01

composites, fatty acid , vinyl ester 9. Distribution $tatement (requr’iedl lsmanuscript subjectto export control? E ruo I yes Circfe appropriate l tter and...resins is to replace some or all of the styrene with fatty acid -based monomers. These fatty acid vinyl ester resins allow for the formulation of high...validation studies have been performed, showing that the fatty acid -based resins have sufficient, modulus, strength, glass transition temperature, and

Photooxidation of Mixed Aryl and Biarylphosphines

PubMed Central

Zhang, Dong; Celaje, Jeff A.; Agua, Alon; Doan, Chad; Stewart, Timothy; Bau, Robert; Selke, Matthias

2010-01-01

Aryl phosphines and dialkylbiaryl phosphines react with singlet oxygen to form phosphinate esters. For mixed arylphosphines, the most electron-rich aryl group migrates to form the phosphinate, while for dialkylbiaryl phosphines migration of the alkyl group occurs. Dialkylbiaryl phosphines also yield arene epoxides, especially in electron rich systems. Phosphinate ester formation is increased at high temperature while protic solvents increase the yield of epoxide. The product distribution provides evidence for Buchwald’s recent conformational model for the aerobic oxidation of dialkylbiaryl phosphines. PMID:20527907

A UV resonance Raman (UVRR) spectroscopic study on the extractable compounds of Scots pine ( Pinus sylvestris) wood . Part I: Lipophilic compounds

NASA Astrophysics Data System (ADS)

Nuopponen, M.; Willför, S.; Jääskeläinen, A.-S.; Sundberg, A.; Vuorinen, T.

2004-11-01

The wood resin in Scots pine ( Pinus sylvestris) stemwood and branch wood were studied using UV resonance Raman (UVRR) spectroscopy. UVRR spectra of the sapwood and heartwood hexane extracts, solid wood samples and model compounds (six resin acids, three fatty acids, a fatty acid ester, sitosterol and sitosterol acetate) were collected using excitation wavelengths of 229, 244 and 257 nm. In addition, visible Raman spectra of the fatty and resin acids were recorded. Resin compositions of heartwood and sapwood hexane extracts were determined using gas chromatography. Raman signals of both conjugated and isolated double bonds of all the model compounds were resonance enhanced by UV excitation. The oleophilic structures showed strong bands in the region of 1660-1630 cm -1. Distinct structures were enhanced depending on the excitation wavelength. The UVRR spectra of the hexane extracts showed characteristic bands for resin and fatty acids. It was possible to identify certain resin acids from the spectra. UV Raman spectra collected from the solid wood samples containing wood resin showed a band at ˜1650 cm -1 due to unsaturated resin components. The Raman signals from extractives in the resin rich branch wood sample gave even more strongly enhanced signals than the aromatic lignin.

A UV resonance Raman (UVRR) spectroscopic study on the extractable compounds of Scots pine (Pinus sylvestris) wood. Part I: lipophilic compounds.

PubMed

Nuopponen, M; Willför, S; Jääskeläinen, A-S; Sundberg, A; Vuorinen, T

2004-11-01

The wood resin in Scots pine (Pinus sylvestris) stemwood and branch wood were studied using UV resonance Raman (UVRR) spectroscopy. UVRR spectra of the sapwood and heartwood hexane extracts, solid wood samples and model compounds (six resin acids, three fatty acids, a fatty acid ester, sitosterol and sitosterol acetate) were collected using excitation wavelengths of 229, 244 and 257 nm. In addition, visible Raman spectra of the fatty and resin acids were recorded. Resin compositions of heartwood and sapwood hexane extracts were determined using gas chromatography. Raman signals of both conjugated and isolated double bonds of all the model compounds were resonance enhanced by UV excitation. The oleophilic structures showed strong bands in the region of 1660-1630 cm(-1). Distinct structures were enhanced depending on the excitation wavelength. The UVRR spectra of the hexane extracts showed characteristic bands for resin and fatty acids. It was possible to identify certain resin acids from the spectra. UV Raman spectra collected from the solid wood samples containing wood resin showed a band at approximately 1650 cm(-1) due to unsaturated resin components. The Raman signals from extractives in the resin rich branch wood sample gave even more strongly enhanced signals than the aromatic lignin.

Quantitative evaluation of XAD-8 and XAD-4 resins used in tandem for removing organic solutes from water

USGS Publications Warehouse

Malcolm, R.L.; MacCarthy, P.

1992-01-01

The combined XAD-8 and XAD-4 resin procedure for the isolation of dissolved organic solutes from water was found to isolate 85% or more of the organic solutes from Lake Skjervatjern in Norway. Approximately 65% of the dissolved organic carbon (DOC) was first removed on XAD-8 resin, and then an additional 20% of the DOC was removed on XAD-4 resin. Approximately 15% of the DOC solutes (primarily hydrophilic neutrals) were not sorbed or concentrated by the procedure. Of the 65% of the solutes removed on XAD-8 resin, 40% were fulvic acids, 16% were humic acids, and 9% were hydrophobic neutrals. Approximately 20% of the hydrophilic solutes that pass through the XAD-8 resin were sorbed solutes on the second resin, XAD-4 (i.e., they were hydrophobic relative to the XAD-4 resin). The fraction sorbed on XAD-4 resin was called XAD-4 acids because it represented approximately 85-90% of the hydrophilic XAD-8 acid fraction according to the original XAD-8 fractionation procedure. The recovery of hydrophobic acids (fulvic acids and humic acids) and the hydrophobic neutral fraction from XAD-8 resin was essentially quantitative at 96%, 98%, and 86%, respectively. The recovery of XAD-4 acids from the XAD-4 resin was only about 50%. The exact reason for this moderately low recovery is unknown, but could result from ??-?? bonding between these organic solutes and the aromatic matrix of XAD-4. The hydrophobic/hydrophilic solute separation on XAD-8 resin for water from background Side A and Side B of the lake was almost identical at 65 and 67%, respectively. This result suggested that both sides of the lake are similar in organic chemical composition even though the DOC variation from side to side is 20%.

Synthesis of monodentate ferrocenylphosphines and their application to the palladium-catalyzed Suzuki reaction of aryl chlorides.

PubMed

Pickett, Tom E; Roca, Francesc X; Richards, Christopher J

2003-04-04

Racemic and enantiopure ((p)()S)-1-bromo-2-methylferrocene 6 were synthesized in 4 steps from 2-(4,4-dimethyloxazolinyl)ferrocene and (S)-2-(4-methylethyloxazolinyl)ferrocene, respectively (46 and 81% overall yield). Bromolithium exchange and addition of ClPR(2) gave the corresponding racemic or enantiopure 2-methylferrocenyl phosphine ligands 2-MeFcPR(2) 11 (R = Ph), 12 (R = Cy), and 13 (R = (t)Bu) in 28-93% yield. Use of PCl(3) gave the C(3)-symmetric phosphine (2-MeFc)(3)P 5 from ((p)()S)-6(72% yield) but racemic 6 did not lead to the formation of triferrocenyl phosphines. Combination of 5 and Pd(2)(dba)(3) gave an active catalyst for the Suzuki reaction of aryl chlorides, for example, 4-chlorotoluene and phenylboronic acid reacted at only 60 degrees C in dioxane (86% yield). Other examples are reported together with the use of 12 in this same protocol. From the X-ray crystal structure of 5 the cone angle was determined as 211 degrees. With this, and the electronic character of 11, 12, and other phosphines (derived from nu(CO) of trans-[(R(3)P)(2)Rh(CO)Cl]), an analysis is made of the steric and electronic influences on ligand activity in the Suzuki reaction.

Design and development of novel linker for PbS quantum dots/TiO₂ mesoscopic solar cell.

PubMed

Etgar, Lioz; Park, Jinhyung; Barolo, Claudia; Nazeeruddin, Md K; Viscardi, Guido; Graetzel, Michael

2011-09-01

A novel bifunctional linker molecule, bis(4-mercaptophenyl)phosphinic acid, is designed to be used in a QDs solar cells. The linker anchors to TiO(2) mesoporous film through the phosphinic acid functional group and to the PbS QDs through the two thiol groups. The way of attachment of this new linker molecule in a photovoltaic PbS QDs/TiO(2) mesoporous device was studied by FTIR measurements. The photovoltaic performance of this new linker in a heterojunction PbS QDs solar cell show high V(oc) relative to QDs based solar cells, which will allow to receive high power conversion efficiency using this novel designed linker. This novel bifunctional linker molecule should pave the way for enhancing binding strength, and efficiency of QDs solar cells compared to the state-of-the-art linkers.

Phosphine-Catalyzed Doubly Stereoconvergent γ-Additions of Racemic Heterocycles to Racemic Allenoates: The Catalytic Enantioselective Synthesis of Protected α,α-Disubstituted α-Amino Acid Derivatives.

PubMed

Kalek, Marcin; Fu, Gregory C

2015-07-29

Methods have recently been developed for the phosphine-catalyzed asymmetric γ-addition of nucleophiles to readily available allenoates and alkynoates to generate useful α,β-unsaturated carbonyl compounds that bear a stereogenic center in either the γ or the δ position (but not both) with high stereoselectivity. The utility of this approach would be enhanced considerably if the stereochemistry at both termini of the new bond could be controlled effectively. In this report, we describe the achievement of this objective, specifically, that a chiral phosphepine can catalyze the stereoconvergent γ-addition of a racemic nucleophile to a racemic electrophile; through the choice of an appropriate heterocycle as the nucleophilic partner, this new method enables the synthesis of protected α,α-disubstituted α-amino acid derivatives in good yield, diastereoselectivity, and enantioselectivity.

Tall oil precursors and turpentine in Jack and Eastern White Pine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Conner, A.H.; Diehl, M.A.; Rowe, J.W.

1980-04-01

The tall oil precursors and turpentine from jack pine (Pinus banksiana Lamb.) and eastern white pine (Pinus strobus L.) were investigated. The tall oil precursors (resin acids, fatty acids, and unsaponifiables were determined by chemical fractionation of the nonvolatile diethyl ether extractives (NVEE) of these speices: (approximate % resin acids, % fatty acids, % unsaponifiables, and % acids other that fatty and resin acids) - jack pine sapwood (10, 60, 10, 20%), heartwood (38, 12, 6, 44%); eastern white pine sapwood (11, 57, 9, 22%), and heartwood (11, 18, 10, 62%). The resin acids were a mixture of the pimaricmore » and abietic acids common to pines. In addition, eastern white pine contained major amounts of the resin acid, anticopalic acid. The fatty acids were predominately oleic, linoleic, and 5, 9, 12-octadecatrienoic acids. The unsaponsiables were a complex mixture of diterpenes and sterols (mainly campesterol and sitosterol). On treating these species with paraquat, lightwood occurred in the sapwood but not in the heartwood areas as we have oberved with other pines. The NVEE of the lightwood areas contained increased amounts of resin acids, unsaponifiables, and acids other than fatty and resin acids. The total fatty acid content was essentially unchanged. Since fatty acid components are preferentially lost by esterification with neutral alcoholic constituents in the unsaponifiables during the distillation refining of crude tall oil, the increased unsaponifiables relative to the constant fatty acid content might result in a net reduction in fatty acid recovery from lightered trees. The turpentine content of both jack and eastern white pine increased on lightering and was primarily a mixture of ..cap alpha..- and ..beta..-pinene.« less

Chemical Reaction between Boric Acid and Phosphine Indicates Boric Acid as an Antidote for Aluminium Phosphide Poisoning

PubMed Central

Soltani, Motahareh; Shetab-Boushehri, Seyed F.; Shetab-Boushehri, Seyed V.

2016-01-01

Objectives: Aluminium phosphide (AlP) is a fumigant pesticide which protects stored grains from insects and rodents. When it comes into contact with moisture, AlP releases phosphine (PH3), a highly toxic gas. No efficient antidote has been found for AlP poisoning so far and most people who are poisoned do not survive. Boric acid is a Lewis acid with an empty p orbital which accepts electrons. This study aimed to investigate the neutralisation of PH3 gas with boric acid. Methods: This study was carried out at the Baharlou Hospital, Tehran University of Medical Sciences, Tehran, Iran, between December 2013 and February 2014. The volume of released gas, rate of gas evolution and changes in pH were measured during reactions of AlP tablets with water, acidified water, saturated boric acid solution, acidified saturated boric acid solution, activated charcoal and acidified activated charcoal. Infrared spectroscopy was used to study the resulting probable adduct between PH3 and boric acid. Results: Activated charcoal significantly reduced the volume of released gas (P <0.01). Although boric acid did not significantly reduce the volume of released gas, it significantly reduced the rate of gas evolution (P <0.01). A gaseous adduct was formed in the reaction between pure AlP and boric acid. Conclusion: These findings indicate that boric acid may be an efficient and non-toxic antidote for PH3 poisoning. PMID:27606109

Efficient in situ separation and production of L-lactic acid by Bacillus coagulans using weak basic anion-exchange resin.

PubMed

Zhang, Yitong; Qian, Zijun; Liu, Peng; Liu, Lei; Zheng, Zhaojuan; Ouyang, Jia

2018-02-01

To get rid of the dependence on lactic acid neutralizer, a simple and economical approach for efficient in situ separation and production of L-lactic acid was established by Bacillus coagulans using weak basic anion-exchange resin. During ten tested resins, the 335 weak basic anion-exchange resins demonstrated the highest adsorption capacity and selectivity for lactic acid recovery. The adsorption study of the 335 resins for lactic acid confirmed that it is an efficient adsorbent under fermentation condition. Langmuir models gave a good fit to the equilibrium data at 50 °C and the maximum adsorption capacity for lactic acid by 335 resins was about 402 mg/g. Adsorption kinetic experiments showed that pseudo-second-order kinetics model gave a good fit to the adsorption rate. When it was used for in situ fermentation, the yield of L-lactic acid by B. coagulans CC17 was close to traditional fermentation and still maintained at about 82% even after reuse by ten times. These results indicated that in situ separation and production of L-lactic acid using the 335 resins were efficient and feasible. This process could greatly reduce the dosage of neutralizing agent and potentially be used in industry.

Phosphonic acid based exchange resins

DOEpatents

Horwitz, E. Philip; Alexandratos, Spiro D.; Gatrone, Ralph C.; Chiarizia, Ronato

1995-01-01

An ion exchange resin for extracting metal ions from a liquid waste stream. An ion exchange resin is prepared by copolymerizing a vinylidene diphosphonic acid with styrene, acrylonitrile and divinylbenzene.

Synergistic effects in ambiphilic phosphino-borane catalysts for the hydroboration of CO2.

PubMed

Tlili, Anis; Voituriez, Arnaud; Marinetti, Angela; Thuéry, Pierre; Cantat, Thibault

2016-06-18

The benefit of combining both a Lewis acid and a Lewis base in a catalytic system has been established for the hydroboration of CO2, using ferrocene-based phosphine, borane and phosphino-borane derivatives.

Phosphonic acid based ion exchange resins

DOEpatents

Horwitz, E. Philip; Alexandratos, Spiro D.; Gatrone, Ralph C.; Chiarizia, Ronato

1994-01-01

An ion exchange resin for extracting metal ions from a liquid waste stream. An ion exchange resin is prepared by copolymerizing a vinylidene disphosphonic acid with styrene, acrylonitrile and divinylbenzene.

Phosphonic acid based ion exchange resins

DOEpatents

Horwitz, E. Philip; Alexandratos, Spiro D.; Gatrone, Ralph C.; Chiarizia, Ronato

1996-01-01

An ion exchange resin for extracting metal ions from a liquid waste stream. An ion exchange resin is prepared by copolymerizing a vinylidene diphosphonic acid with styrene, acrylonitrile and divinylbenzene.

Development of melamine modified urea formaldehyde resins based o nstrong acidic pH catalyzed urea formaldehyde polymer

Treesearch

Chung-Yun Hse

2009-01-01

To upgrade the performance of urea-formaldehyde (UF) resin bonded particleboards, melamine modified urea-formaldehyde (MUF) resins based on strong acidic pH catalyzed UF polymers were investigated. The study was conducted in a series of two experiments: 1) formulation of MUF resins based on a UF polymer catalyzed with strong acidic pH and 2) determination of the...

C6, C7, and C8 perfluoroalkyl-substituted phosphinic acids.

PubMed

Singh, R P; Shreeve, J M

2000-04-17

Reaction of red phosphorus with RfI in a 1:2 molar ratio at 230 degrees C led to the formation of a mixture of (Rf)2PI and (Rf)PI2 (Rf = C6F13, C7F15, C8F17) in about a 70:30 ratio, respectively. These mixtures were separated by vacuum distillation. (Rf)2PI (Rf = C6F13, C7F15) are yellow liquids whereas (C8F17)2PI is a yellow solid. Oxidation of (Rf)2PI with excess NO2 led to (Rf)2P(O)OH (Rf = C6F13, C7F15, C8F17) in > 90% isolated yields after aqueous hydrolysis of the anhydride intermediates. These highly fluorinated phosphinic acids are white solids with sharp melting points and are highly soluble in methyl sulfoxide (DMSO) and 1,1,2-trichlorotrifluoroethane. However, solubility in chloroform and methylene dichloride is low. These perfluoroalkylphosphinic acids were characterized by IR, NMR (1H, 19F, and 31P), and mass spectra and elemental analysis.

Process for separation of zirconium-88, rubidium-83 and yttrium-88

DOEpatents

Heaton, Richard C.; Jamriska, Sr., David J.; Taylor, Wayne A.

1994-01-01

A process for selective separation of strontium-82 and strontium-85 from proton irradiated molybdenum targets is provided and includes dissolving the molybdenum target in a hydrogen peroxide solution to form a first ion-containing solution, passing the first ion-containing solution through a first cationic resin whereby ions selected from the group consisting of molybdenum, niobium, technetium, selenium, vanadium, arsenic, germanium, zirconium and rubidium remain in the first ion-containing solution while ions selected from the group consisting of rubidium, zinc, beryllium, cobalt, iron, manganese, chromium, strontium, yttrium and zirconium are selectively adsorbed by the first resin, contacting the first resin with an acid solution capable of stripping adsorbed ions from the first cationic exchange resin whereby the adsorbed ions are removed from the first resin to form a second ion-containing solution, evaporating the second ion-containing solution for time sufficient to remove substantially all of the acid and water from the second ion-containing solution whereby a residue remains, dissolving the residue from the evaporated second-ion containing solution in a dilute acid to form a third ion-containing solution, said third ion-containing solution having an acid molarity adapted to permit said ions to be adsorbed by a cationic exchange resin, passing the third ion-containing solution through a second cationic resin whereby the ions are adsorbed by the second resin, contacting the second resin with a dilute sulfuric acid solution whereby the adsorbed ions selected from the group consisting of rubidium, zinc, beryllium, cobalt, iron, manganese, chromium, and zirconium are selectively removed from the second resin, and contacting the second resin with a dilute acid solution whereby the adsorbed strontium ions are selectively removed. Zirconium, rubidium, and yttrium radioisotopes can also be recovered with additional steps.

Enrichment and separation of chlorogenic acid from the extract of Eupatorium adenophorum Spreng by macroporous resin.

PubMed

Liu, Boyan; Dong, Beitao; Yuan, Xiaofan; Kuang, Qirong; Zhao, Qingsheng; Yang, Mei; Liu, Jie; Zhao, Bing

2016-01-01

A simple and efficient chromatographic method for separation of chlorogenic acid from Eupatorium adenophorum Spreng extract was developed. The adsorption properties of nine macroporous resins were evaluated. NKA-II resin showed much better adsorption/desorption properties. The adsorption of chlorogenic acid on NKA-II resin at 25°C was well fitted to Langmuir isotherm model and pseudo-second-order kinetic model. The dynamic adsorption and desorption experiments were carried out on columns packed with NKA-II resin to optimize the separation process. The content of chlorogenic acid in the product increased to 22.17%, with a recovery yield of 82.41%. Copyright © 2015 Elsevier B.V. All rights reserved.

Phosphonic acid based exchange resins

DOEpatents

Horwitz, E.P.; Alexandratos, S.D.; Gatrone, R.C.; Chiarizia, R.

1995-09-12

An ion exchange resin is described for extracting metal ions from a liquid waste stream. An ion exchange resin is prepared by copolymerizing a vinylidene diphosphonic acid with styrene, acrylonitrile and divinylbenzene. 10 figs.

Resin in bisulfite pulp from Pinus radiata wood and its relationship to pitch troubles

Treesearch

P.J. Nelson; Richard W. Hemingway

1971-01-01

The resin content of bisulfite pulp from Pinus radiata D. Don was determined at various stages in its manufacture and the changes in the composition of the resin studied. About 50% of the resin present in the wood was removed during cooking, an additional 11% by blowpit washing, and a further 8% by screening. Resin acids and fatty acids were...

Adsorbed States of phosphonate derivatives of N-heterocyclic aromatic compounds, imidazole, thiazole, and pyridine on colloidal silver: comparison with a silver electrode.

PubMed

Podstawka, Edyta; Olszewski, Tomasz K; Boduszek, Bogdan; Proniewicz, Leonard M

2009-09-03

Here, we report a systematic surface-enhanced Raman spectroscopy (SERS) study of the structures of phosphonate derivatives of the N-heterocyclic aromatic compounds imidazole (ImMeP ([hydroxy(1H-imidazol-5-yl)methyl]phosphonic acid) and (ImMe)(2)P (bis[hydroxy-(1H-imidazol-4-yl)-methyl]phosphinic acid)), thiazole (BAThMeP (butylaminothiazol-2-yl-methyl)phosphonic acid) and BzAThMeP (benzylaminothiazol-2-yl-methyl)phosphonic acid)), and pyridine ((PyMe)(2)P (bis[(hydroxypyridin-3-yl-methyl)]phosphinic acid)) adsorbed on nanometer-sized colloidal particles. We compared these structures to those on a roughened silver electrode surface to determine the relationship between the adsorption strength and the geometry. For example, we showed that all of these biomolecules interact with the colloidal surface through aromatic rings. However, for BzAThMeP, a preferential interaction between the benzene ring and the colloidal silver surface is observed more so than that between the thiazole ring and this substrate. The PC(OH)C fragment does not take part in the adsorption process, and the phosphonate moiety of ImMeP and (ImMe)(2)P, being removed from the surface, only assists in this process.

Phosphonic acid based ion exchange resins

DOEpatents

Horwitz, E.P.; Alexandratos, S.D.; Gatrone, R.C.; Chiarizia, R.

1996-07-23

An ion exchange resin is described for extracting metal ions from a liquid waste stream. An ion exchange resin is prepared by copolymerizing a vinylidene diphosphonic acid with styrene, acrylonitrile and divinylbenzene. 10 figs.

Phosphonic acid based ion exchange resins

DOEpatents

Horwitz, E.P.; Alexandratos, S.D.; Gatrone, R.C.; Chiarizia, R.

1994-01-25

An ion exchange resin is described for extracting metal ions from a liquid waste stream. An ion exchange resin is prepared by copolymerizing a vinylidene diphosphonic acid with styrene, acrylonitrile and divinylbenzene. 9 figures.

Method for digesting spent ion exchange resins and recovering actinides therefrom using microwave radiation

DOEpatents

Maxwell, III, Sherrod L.; Nichols, Sheldon T.

1999-01-01

The present invention relates to methods for digesting diphosphonic acid substituted cation exchange resins that have become loaded with actinides, rare earth metals, or heavy metals, in a way that allows for downstream chromatographic analysis of the adsorbed species without damage to or inadequate elution from the downstream chromatographic resins. The methods of the present invention involve contacting the loaded diphosphonic acid resin with concentrated oxidizing acid in a closed vessel, and irradiating this mixture with microwave radiation. This efficiently increases the temperature of the mixture to a level suitable for digestion of the resin without the use of dehydrating acids that can damage downstream analytical resins. In order to ensure more complete digestion, the irradiated mixture can be mixed with hydrogen peroxide or other oxidant, and reirradiated with microwave radiation.

Microbial activity in an acid resin deposit: biodegradation potential and ecotoxicology in an extremely acidic hydrocarbon contamination.

PubMed

Kloos, Karin; Schloter, Michael; Meyer, Ortwin

2006-11-01

Acid resins are residues produced in a recycling process for used oils that was in use in the forties and fifties of the last century. The resin-like material is highly contaminated with mineral oil hydrocarbons, extremely acidic and co-contaminated with substituted and aromatic hydrocarbons, and heavy metals. To determine the potential for microbial biodegradation the acid resin deposit and its surroundings were screened for microbial activity by soil respiration measurements. No microbial activity was found in the core deposit. However, biodegradation of hydrocarbons was possible in zones with a lower degree of contamination surrounding the deposit. An extreme acidophilic microbial community was detected close to the core deposit. With a simple ecotoxicological approach it could be shown that the pure acid resin that formed the major part of the core deposit, was toxic to the indigenous microflora due to its extremely low pH of 0-1.

Selection of anion exchangers for detoxification of dilute-acid hydrolysates from spruce.

PubMed

Horváth, Ilona Sárvári; Sjöde, Anders; Nilvebrant, Nils-Olof; Zagorodni, Andrei; Jönsson, Leif J

2004-01-01

Six anion-exchange resins with different properties were compared with respect to detoxification of a dilute-acid hydrolysate of spruce prior to ethanolic fermentation with Saccharomyces cerevisiae. The six resins encompassed strong and weak functional groups as well as styrene-, phenol-, and acrylic-based matrices. In an analytical experimental series, fractions from columns packed with the different resins were analyzed regarding pH, glucose, furfural, hydroxymethylfurfural, phenolic compounds, levulinic acid, acetic acid, formic acid, and sulfate. An initial adsorption of glucose occurred in the strong alkaline environment and led to glucose accumulation at a later stage. Acetic and levulinic acid passed through the column before formic acid, whereas sulfate had the strongest affinity. In a preparative experimental series, one fraction from each of six columns packed with the different resins was collected for assay of the fermentability and analysis of glucose, mannose, and fermentation inhibitors. The fractions collected from strong anion-exchange resins with styrene-based matrices displayed the best fermentability: a sevenfold enhancement of ethanol productivity compared with untreated hydrolysate. Fractions from a strong anion exchanger with acrylic-based matrix and a weak exchanger with phenol-based resin displayed an intermediate improvement in fermentability, a four- to fivefold increase in ethanol productivity. The fractions from two weak exchangers with styrene- and acrylic-based matrices displayed a twofold increase in ethanol productivity. Phenolic compounds were more efficiently removed by resins with styrene- and phenol-based matrices than by resins with acrylic-based matrices.

Metal-organophosphine and metal-organophosphonium frameworks with layered honeycomb-like structures.

PubMed

Humphrey, Simon M; Allan, Phoebe K; Oungoulian, Shaunt E; Ironside, Matthew S; Wise, Erica R

2009-04-07

Phosphanotriylbenzenecarboxylic acid (ptbcH(3); P(C(6)H(4)-p-CO(2)H)(3)) and its methyl phosphonium iodide derivative (mptbcH(3)I; {H(3)CP(C(6)H(4)-p-CO(2)H)(3)}I) have been used as organic building blocks in reaction with Zn(ii) salts to obtain a series of related two-dimensional coordination polymers with honeycomb-like networks. The variable coordination number and oxidation states available to phosphorus have been exploited to produce a family of related phosphine coordination materials (PCMs) using a single ligand precursor. The phosphine carboxylate trianion, ptbc(3-), reacted with Zn(ii) to form 3,3-connected undulating hexagonal sheets based on tetrahedral P and Zn nodes, where Zn-ptbc = 1 : 1. When hydroxide was used as an additional framework ligand, Zn(4)(OH)(2) clusters were obtained. The clusters support 6,3-connected bilayers that consist of pairs of fused hexagonal sheets (Zn-ptbc = 2 : 1) with intra-layer pore spaces. The Zn(4)(OH)(2) clusters are also coordinated by solvent, which was preferentially displaced when the bilayer material was synthesized in the presence of ethylene diamine. Treatment of ptbc(3-) with MeI resulted in methylation of the phosphine to give the P(v) phosphonium iodide salt derivative. The formally dianionic methylphosphonium tricarboxylate building block, mptbc(2-), has the same trigonal-pyramidal bridging geometry as the parent phosphine. However, mptbc(2-) reacted with Zn(ii) on a 1 : 1 stoichiometric ratio to give an unusual trilayer sheet polymer that is based exclusively on 3-connected nodes. Solid-state (31)P NMR studies confirmed that the phosphine ligands were resistant to oxidation upon solvothermal reaction under aerobic conditions.

21 CFR 175.260 - Partial phosphoric acid esters of polyester resins.

Code of Federal Regulations, 2012 CFR

2012-04-01

... resins are prepared by the reaction of trimellitic anhydride with 2,2-dimethyl-1,3-propanediol followed by reaction of the resin thus produced with phosphoric acid anhydride to produce a resin having an... conditions of time and temperature characterizing the conditions of its intended use, as determined from...

21 CFR 175.260 - Partial phosphoric acid esters of polyester resins.

Code of Federal Regulations, 2013 CFR

2013-04-01

... resins are prepared by the reaction of trimellitic anhydride with 2,2-dimethyl-1,3-propanediol followed by reaction of the resin thus produced with phosphoric acid anhydride to produce a resin having an... conditions of time and temperature characterizing the conditions of its intended use, as determined from...

Emission of volatile aldehydes and ketones from wood pellets under controlled conditions.

PubMed

Arshadi, Mehrdad; Geladi, Paul; Gref, Rolf; Fjällström, Pär

2009-11-01

Different qualities of biofuel pellets were made from pine and spruce sawdust according to an industrial experimental design. The fatty/resin acid compositions were determined by gas chromatography-mass spectrometry for both newly produced pellets and those after 2 and 4 weeks of storage. The aldehydes/ketones compositions were determined by high performance liquid chromatography at 0, 2, and 4 weeks. The designs were analyzed for the response variables: total fatty/resin acids and total aldehydes/ketones. The design showed a strong correlation between the pine fraction in the pellets and the fatty/resin acid content but the influence decreased over storage time. The amount of fatty/resin acids decreased approximately 40% during 4 weeks. The influence of drying temperature on the aldehyde/ketone emission of fresh pellets was also shown. The amounts of emitted aldehydes/ketones generally decreased by 45% during storage as a consequence of fatty/resin acid oxidation. The matrices of individual concentrations were subjected to multivariate data analysis. This showed clustering of the different experimental runs and demonstrated the important mechanism of fatty/resin acid conversion.

Isolation of hydrophilic organic acids from water using nonionic macroporous resins

USGS Publications Warehouse

Aiken, G.R.; McKnight, Diane M.; Thorn, K.A.; Thurman, E.M.

1992-01-01

A method has been developed for the isolation of hydrophilic organic acids from aquatic environments using Amberlite* * Use of trade names in this report is for identification purposes only and does not constitute endorsement by the U.S. Geological Survey. XAD-4 resin. The method uses a two column array of XAD-8 and XAD-4 resins in series. The hydrophobic organic acids, composed primarily of aquatic fulvic acid, are removed from the sample on XAD-8, followed by the isolation of the more hydrophilic organic acids on XAD-4. For samples from a number of diverse environments, more of the dissolved organic carbon was isolated on the XAD-8 resin (23-58%) than on the XAD-4 resin (7-25%). For these samples, the hydrophilic acids have lower carbon and hydrogen contents, higher oxygen and nitrogen contents, and are lower in molecular weight than the corresponding fulvic acids. 13C NMR analyses indicate that the hydrophilic acids have a lower concentration of aromatic carbon and greater heteroaliphatic, ketone and carboxyl content than the fulvic acid. ?? 1992.

Process for strontium-82 separation

DOEpatents

Heaton, Richard C.; Jamriska, Sr., David J.; Taylor, Wayne A.

1992-01-01

A process for selective separation of strontium-82 and strontium-85 from proton irradiated molybdenum targets comprises dissolving the molybdenum target in a hydrogen peroxide solution to form a first solution containing ions selected from a group consisting of molybdenum, niobium, technetium, selenium, vanadium, arsenic, germanium, zirconium, rubidium, zinc, beryllium, cobalt, iron, manganese, chromium, strontium, and yttrium; passing the solution through a first cationic resin whereby ions selected from a group consisting of zinc, beryllium, cobalt, iron, manganese, chromium, strontium, yttrium a portion of zirconium and a portion of rubidium are selectively absorbed by the first resin; contacting the first resin with an acid solution to strip and remove the absorbed ions from the first cationic exchange resin to form a second solution; evaporating the second solution for a time sufficient to remove substantially all of the acid and water from the solution whereby a residue remains; dissolving the residue in a dilute acid to form a third solution; passing the third solution through a second cationic resin whereby the ions are absorbed by the second resin; contacting the second resin with a dilute sulfuric acid solution whereby the absorbed ions selected from the group consisting of rubidium, zinc, beryllium, cobalt, iron, manganese, chromium and zirconium are selectively removed from the second resin; and contacting the second resin with a dilute acid solution whereby the absorbed strontium ions are selectively removed.

Process for strontium-82 separation

DOEpatents

Heaton, R.C.; Jamriska, D.J. Sr.; Taylor, W.A.

1992-12-01

A process for selective separation of strontium-82 and strontium-85 from proton irradiated molybdenum targets comprises dissolving the molybdenum target in a hydrogen peroxide solution to form a first solution containing ions selected from a group consisting of molybdenum, niobium, technetium, selenium, vanadium, arsenic, germanium, zirconium, rubidium, zinc, beryllium, cobalt, iron, manganese, chromium, strontium, and yttrium; passing the solution through a first cationic resin whereby ions selected from a group consisting of zinc, beryllium, cobalt, iron, manganese, chromium, strontium, yttrium a portion of zirconium and a portion of rubidium are selectively absorbed by the first resin; contacting the first resin with an acid solution to strip and remove the absorbed ions from the first cationic exchange resin to form a second solution; evaporating the second solution for a time sufficient to remove substantially all of the acid and water from the solution whereby a residue remains; dissolving the residue in a dilute acid to form a third solution; passing the third solution through a second cationic resin whereby the ions are absorbed by the second resin; contacting the second resin with a dilute sulfuric acid solution whereby the absorbed ions selected from the group consisting of rubidium, zinc, beryllium, cobalt, iron, manganese, chromium and zirconium are selectively removed from the second resin; and contacting the second resin with a dilute acid solution whereby the absorbed strontium ions are selectively removed. 1 fig.

2-Chlorotrityl chloride resin. Studies on anchoring of Fmoc-amino acids and peptide cleavage.

PubMed

Barlos, K; Chatzi, O; Gatos, D; Stavropoulos, G

1991-06-01

The esterification of 2-chlorotrityl chloride resin with Fmoc-amino acids in the presence of DIEA is studied under various conditions. High esterification yields are obtained using 0.6 equiv. Fmoc-amino acid/mmol resin in DCM or DCE, in 25 min, at room temperature. The reaction proceeds without by product formation even in the case of Fmoc-Asn and Fmoc-Gln. The quantitative and easy cleavage of amino acids and peptides from 2-chlorotrityl resin, by using AcOH/TFE/DCM mixtures, is accomplished within 15-60 min at room temperature, while t-butyl type protecting groups remain unaffected. Under these exceptionally mild conditions 2-chlorotrityl cations generated during the cleavage of amino acids and peptides from resin do not attack the nucleophilic side chains of Trp, Met, and Tyr.

Morphological and chemical characterization of the dentin/resin cement interface produced with a self-etching primer.

PubMed

Walker, Mary P; Wang, Yong; Spencer, Paulette

2002-01-01

The purpose of this study was to analyze a resin cement/dentin interface by comparing the diffusion of a resin cement into dentin surfaces pretreated with a self-etching primer with or without pretreatment by conventional acid etching. Dentin surfaces of 8 unerupted human third molars were treated with a self-etch primer (Panavia 21) with or without conventional phosphoric acid pretreatment. Panavia 21 resin cement was applied according to manufacturer's instructions. Dentin/resin cement interface sections from each tooth were examined with scanning electron microscopy and micro-Raman spectroscopy. When the self-etch primer was used following conventional acid pretreatment, the resin cement did not penetrate to the depth of the zone of demineralized dentin, leaving a substantial area of exposed dentin matrix at the dentin/cement interface. In contrast, there was substantial resin cement diffusion throughout the demineralized dentin when the self-etch primer was used without acid etching pretreatment. The in vitro evaluation of resin cement penetration throughout the zone of demineralized dentin is an important step in identifying sites of exposed dentin matrix that may promote postoperative sensitivity and may leave the dentin/resin cement interface vulnerable to premature degradation under clinical conditions. In this study, the self-etch primer used alone produced substantial resin cement penetration and left no exposed dentin matrix at the dentin/resin cement interface.

Effect of pore structure on the removal of clofibric acid by magnetic anion exchange resin.

PubMed

Tan, Liang; Shuang, Chendong; Wang, Yunshu; Wang, Jun; Su, Yihong; Li, Aimin

2018-01-01

The effect of pore structure of resin on clofibric acid (CA) adsorption behavior was investigated by using magnetic anion exchange resins (ND-1, ND-2, ND-3) with increasing pore diameter by 11.68, 15.37, 24.94 nm. Resin with larger pores showed faster adsorption rates and a higher adsorption capacity because the more opened tunnels provided by larger pores benefit the CA diffusion into the resin matrix. The ion exchange by the electrostatic interactions between Cl-type resin and CA resulted in chloride releasing to the solution, and the ratio of released chloride to CA adsorption amount decreased from 0.90 to 0.65 for ND-1, ND-2 and ND-3, indicating that non-electrostatic interactions obtain a larger proportional part of the adsorption into the pores. Co-existing inorganic anions and organic acids reduced the CA adsorption amounts by the competition effect of electrostatic interaction, whereas resins with more opened pore structures weakened the negative influence on CA adsorption because of the existence of non-electrostatic interactions. 85.2% and 65.1% adsorption amounts decrease are calculated for resin ND-1 and ND-3 by the negative influence of 1 mmol L -1 NaCl. This weaken effect of organic acid is generally depends on its hydrophobicity (Log Kow) for carboxylic acid and its ionization degree (pKb) for sulfonic acid. The resins could be reused with the slightly decreases by 1.9%, 3.2% and 5.4% after 7 cycles of regeneration, respectively for ND-1, ND-2 and ND-3, suggesting the ion exchange resin with larger pores are against its reuse by the brine solution regeneration. Copyright © 2017 Elsevier Ltd. All rights reserved.

Metabolism of aspirin and procaine in mice pretreated with O-4-nitrophenyl methyl(phenyl)phosphinate or O-4-nitrophenyl diphenylphosphinate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Joly, J.M.; Brown, T.M.

Concentrations of (carboxyl-/sup 14/C)procaine in blood of mice were increased threefold for 27 min by exposure to O-4-nitrophenyl diphenylphosphinate 2 hr prior to (carboxyl-/sup 14/C)procaine injection ip, while there was no effect of O-4-nitrophenyl methyl(phenyl)phosphinate pretreatment. There was no effect of either organophosphinate on the primary hydrolysis of (acetyl-l-/sup 14/C)aspirin when assessed by the expiration of (/sup 14/C)carbon dioxide; however, O-4-nitrophenyl diphenylphosphinate pretreatment produced transient increases in blood concentrations of both (carboxyl-/sup 14/C)aspirin and (carboxyl-/sup 14/C)salicylic acid following administration of (carboxyl-/sup 14/C)aspirin. Liver carboxylesterase activity in O-4-nitrophenyl diphenylphosphinate pretreated mice was 11% of control activity. These results indicate the potentialmore » for drug interaction with O-4-nitrophenyl diphenylphosphinate but not with O-4-nitrophenyl methyl(phenyl)phosphinate. It appears that liver carboxylesterase activity has a minor role in hydrolysis of aspirin in vivo, but may be more important in procaine metabolism.« less

METHOD OF SEPARATION

DOEpatents

Boyd, G.E.

1958-08-26

A process is presented fer separating uranium, plutonium, and fission products ions from uranyl nitrate solutions having a pH value between 1 and 3 obtained by dissolving neutron irradiated uranium. The method consists in passing such solutions through a bed of cation exchange resin, which may be a sulfonated phenol formaidehyde type. Following the adsorption step the resin is first treated with a solution of 0.2M to 0.3M sulfuric acid to desorb the uranium. Fission product ions are then desorbed by treating the resin in phosphoric acid and 1M in nitric acid. Lastly, the plutonium may be desorbed by treating the resin with a solution approximately 0.8M in phosphoric acid and 1M in nitric acid.

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

PubMed

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

2003-05-16

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

Stress pre-conditioning with temperature, UV and gamma radiation induces tolerance against phosphine toxicity.

PubMed

Alzahrani, Saad M; Ebert, Paul R

2018-01-01

Phosphine is the only general use fumigant for the protection of stored grain, though its long-term utility is threatened by the emergence of highly phosphine-resistant pests. Given this precarious situation, it is essential to identify factors, such as stress preconditioning, that interfere with the efficacy of phosphine fumigation. We used Caenorhabditis elegans as a model organism to test the effect of pre-exposure to heat and cold shock, UV and gamma irradiation on phosphine potency. Heat shock significantly increased tolerance to phosphine by 3-fold in wild-type nematodes, a process that was dependent on the master regulator of the heat shock response, HSF-1. Heat shock did not, however, increase the resistance of a strain carrying the phosphine resistance mutation, dld-1(wr4), and cold shock did not alter the response to phosphine of either strain. Pretreatment with the LD50 of UV (18 J cm-2) did not alter phosphine tolerance in wild-type nematodes, but the LD50 (33 J cm-2) of the phosphine resistant strain (dld-1(wr4)) doubled the level of resistance. In addition, exposure to a mild dose of gamma radiation (200 Gy) elevated the phosphine tolerance by ~2-fold in both strains.

Amino acid analysis

NASA Technical Reports Server (NTRS)

Winitz, M.; Graff, J. (Inventor)

1974-01-01

The process and apparatus for qualitative and quantitative analysis of the amino acid content of a biological sample are presented. The sample is deposited on a cation exchange resin and then is washed with suitable solvents. The amino acids and various cations and organic material with a basic function remain on the resin. The resin is eluted with an acid eluant, and the eluate containing the amino acids is transferred to a reaction vessel where the eluant is removed. Final analysis of the purified acylated amino acid esters is accomplished by gas-liquid chromatographic techniques.

Fatty Acid-Based Monomers as Styrene Replacements for Liquid Molding Resins

DTIC Science & Technology

2005-05-01

fatty acid length and unsaturation level on resin and polymer properties. Fig. 2. The addition of fatty acids ( oleic acid ) to glycidyl methacylate to...the synthetic route used to form the methacrylated fatty acids (MFA). The carboxylic acid of fatty acids undergoes a simple addition reaction with... form methacrylated fatty acid monomer

High Performance Fatty Acid-Based Vinyl Ester Resin for Liquid Molding

DTIC Science & Technology

2007-07-01

High Performance Fatty Acid -Based Vinyl Ester Resin for Liquid Molding by Xing Geng, John J. La Scala, James M. Sands, and Giuseppe R...it to the originator. Army Research Laboratory Aberdeen Proving Ground, MD 21005-5069 ARL-RP-184 July 2007 High Performance Fatty Acid ...CONTRACT NUMBER 5b. GRANT NUMBER 4. TITLE AND SUBTITLE High Performance Fatty Acid -Based Vinyl Ester Resin for Liquid Molding 5c. PROGRAM

Copper resinate: preparation, characterisation and study of degradation.

PubMed

Colombini, M P; Lanterna, G; Mairani, A; Matteini, M; Modugno, F; Rizzi, M

2001-01-01

This paper describes a method for the synthesis of Copper Resinate, which disappeared from artists' palettes in the eighteenth century. This was carried out by interpreting ancient recipes following a scientific approach. Its characterisation using Fourier Transform-Infrared Spectrometry and Gas Chromatography-Mass Spectrometry demonstrated that it is a mixture containing copper and oxidised abietic acids, mainly dehydroabietic and 7-oxo-dehydroabietic acids, formed during the preparation of the pigment and the curing of the paint layer. The composition of copper resinate paint layers, artificially aged by U.V. irradiation at 365 nm (UV), heating (T), and exposed to atmospheric pollutants (NOX) in a climatic chamber, was investigated. The combination of irradiation and temperature produced a change in colour along with a significant increase in the recovered amount of 7-oxo-dehydroabietic acid. The identification of copper resinate in a sample from an old painting should be related to the presence of the following resin compounds which are stable in the ageing process: dehydroabietic and 7-oxo-dehydroabietic acid pimaradienic acids. Photo-oxidation of the resin acids co-ordinated with copper seem to be the most probable decay mechanism responsible for the colour change in the pigment.

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

PubMed

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

2016-08-01

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

Inversion of Configuration at the Phosphorus Nucleophile in the Diastereoselective and Enantioselective Synthesis of P-Stereogenic syn-Phosphiranes from Chiral Epoxides.

PubMed

Muldoon, Jake A; Varga, Balázs R; Deegan, Meaghan M; Chapp, Timothy W; Eördögh, Ádám M; Hughes, Russell P; Glueck, David S; Moore, Curtis E; Rheingold, Arnold L

2018-04-23

Nucleophilic substitution results in inversion of configuration at the electrophilic carbon center (S N 2) or racemization (S N 1). The stereochemistry of the nucleophile is rarely considered, but phosphines, which have a high barrier to pyramidal inversion, attack electrophiles with retention of configuration at P. Surprisingly, cyclization of bifunctional secondary phosphine alkyl tosylates proceeded under mild conditions with inversion of configuration at the nucleophile to yield P-stereogenic syn-phosphiranes. DFT studies suggested that the novel stereochemistry results from acid-promoted tosylate dissociation to yield an intermediate phosphenium-bridged cation, which undergoes syn-selective cyclization. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Computational studies of complexation of nitrous oxide by borane-phosphine frustrated Lewis pairs.

PubMed

Gilbert, Thomas M

2012-08-14

Computational studies of complexes Ar(3)B-ONN-PR(3) derived from reactions between borane-phosphine frustrated Lewis pairs and N(2)O reveal several interesting facets. Natural resonance theory calculations support a change in the preferred resonance structure as the Lewis acidity of the borane increases. Potential constitutional isomers where phosphorus binds to oxygen and boron to nitrogen are predicted to be unstable with respect to loss of phosphine oxide and free N(2). Other constitutional isomers represent stationary points on the potential energy surface; most are considerably less stable than the observed complexes, but one is predicted to be as stable. This arises because the dominant resonance form combines alternating charge with the presence of a stabilizing NO double bond. The relationship between Lewis acidity and complex formation for a variety of boranes was explored; the results are consistent with the idea that greater Lewis acidity stabilizes both classical and frustrated Lewis acid-base pairs, but to differing degrees such that both types can entrap N(2)O. Calculations addressing the mechanism of complex formation suggest that N(2)O binds first through the nitrogen to the phosphine phosphorus of the FLP, whereupon boron coordinates the oxygen atom. Studies of the mechanism of the degenerate exchange reaction between (4-F-H(4)C(6))(3)B-ONN-P(t-Bu)(3) and B(C(6)H(4)-4-F)(3), involves a "transition state", with relatively short B-O distances, and so resembles a classical I(a) process. The process involves two barriers, one associated with bringing the incoming borane into proximity with the oxygen, and the other associated with isomerising from a ladle-shaped cis-trans ct conformer to the observed trans-trans tt-type structure. The overall barrier for degenerate exchange was predicted to be between 65 and 110 kJ mol(-1), in fair agreement with experiment. Similar studies of the reaction between (4-F-H(4)C(6))(3)B-ONN-P(t-Bu)(3) and B(C(6)F(5))(3) indicate that this process more closely resembles a classical I(d) process, in that the "transition state" involves long B-O distances. Derivatization of the complexed NNO fragment appears possible; interaction between (F(5)C(6))(3)B-ONN-P(t-Bu)(3) and MeLi suggests stability for the ion pairs (F(5)C(6))(3)B-ON(Me)N-P(t-Bu)(3)(-)/Li(+) and (F(5)C(6))(3)B-ONN(Me)-P(t-Bu)(3)(-)/Li(+).

Isolation of organic acids from large volumes of water by adsorption on macroporous resins

USGS Publications Warehouse

Aiken, George R.; Suffet, I.H.; Malaiyandi, Murugan

1987-01-01

Adsorption on synthetic macroporous resins, such as the Amberlite XAD series and Duolite A-7, is routinely used to isolate and concentrate organic acids from forge volumes of water. Samples as large as 24,500 L have been processed on site by using these resins. Two established extraction schemes using XAD-8 and Duolite A-7 resins are described. The choice of the appropriate resin and extraction scheme is dependent on the organic solutes of interest. The factors that affect resin performance, selectivity, and capacity for a particular solute are solution pH, resin surface area and pore size, and resin composition. The logistical problems of sample handling, filtration, and preservation are also discussed.

Inhibitory effect of resin composite containing S-PRG filler on Streptococcus mutans glucose metabolism.

PubMed

Kitagawa, Haruaki; Miki-Oka, Saeki; Mayanagi, Gen; Abiko, Yuki; Takahashi, Nobuhiro; Imazato, Satoshi

2018-03-01

Resin composites containing surface pre-reacted glass-ionomer (S-PRG) fillers have been reported to inhibit Streptococcus mutans growth on their surfaces, and their inhibitory effects were attributed to BO 3 3- and F - ions. The aim of this study was to evaluate S. mutans acid production through glucose metabolism on resin composite containing S-PRG fillers and assess inhibitory effects of BO 3 3- and F - on S. mutans metabolic activities. The pH change through S. mutans acid production on experimental resin composite was periodically measured after the addition of glucose. Inhibitory effects of BO 3 3- or F - solutions on S. mutans metabolism were evaluated by XTT assays and measurement of the acid production rate. The pH of experimental resin containing S-PRG fillers was significantly higher than that of control resin containing silica fillers (p < 0.05). OD 450 values by XTT assays and S. mutans acid production rates significantly decreased in the presence of BO 3 3- and F - compared with the absence of these ions (p < 0.05). pH reduction by S. mutans acid production was inhibited on resin composite containing S-PRG fillers. Moreover, S. mutans glucose metabolism and acid production were inhibited in the presence of low concentrations of BO 3 3- or F - . BO 3 3- or F - released from resin composite containing S-PRG fillers exhibits inhibitory effects on S. mutans metabolism at concentrations lower than those which inhibit bacterial growth. Copyright © 2017 Elsevier Ltd. All rights reserved.

Liner Technology Program. Volume 3. Liner Development Methodology Manual

DTIC Science & Technology

1982-05-01

derivative of trimesic acid, trimenoyl-l- (2-ethyl) aziridine BNO Hydroxyl ethyl ester of carboxy-terminated polybutadiene Catocene Liquid ferrocene ...diisocyanate MAPO rris-l-(2-methyl) aziridinyl phosphine oxide I.’ lNA Methyl nedic anhydride; methyl endo-cis-cicyolo-2,2,1-5- heptene-2,3-dicarboxylic

ADSORPTION PROCEDURE IN PREPARING U$sup 23$$sup 3$

DOEpatents

Stoughton, R.W.

1958-10-14

A process is presented for the separation of protoactinium and thorium from an aqueous nitric acid solution containing these metals. It comprises contacting the solution with a cation exchange phenol-formaldehyde resin containing sulfonic acid groups, and eluting the adsorbed thorium from the resin by means of aqueous nitric acid. Thereafter the adsorbed protoactinium is eluted from the resin by means of an aqueous solution of ammonium fluoride.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Torlakoglu, A.; Gueclue, G.

Waste polyethylene terephthalate (PET) flakes were depolymerized by using propylene glycol (PG) in the presence of zinc acetate as catalyst. Glycolysis reaction products of waste PET obtained by using PET/glycol molar ratio 1/2. Two short oil alkyd resins of high acid values (30-40 mgKOH/g) were prepared from phthalic anhydride (PA), glycerin (G), coconut oil fatty acids (COFA) and glycolyzed products of waste PET (PET-based alkyd resins) or glycols (PG) (reference alkyd resins). These alkyd resins were blended with 30%, 40%, and 50% of a commercial urea-formaldehyde, melamine-formaldehyde and urea-formaldehyde/melamine-formaldehyde mixture (1/1 weight ratio) and heated at 140 deg. C. Themore » physical and chemical properties such as drying time, hardness, abrasion resistance, adhesion strength, water resistance, alkaline resistance, acid resistance, gelation time, and thermal oxidative degradation resistance (with thermogravimetric analysis, TGA) of these alkyd-amino resins were investigated. The properties of the waste PET-based resins were found to be compatible with the properties of the reference resins.« less

Hydrolyzable polyester resins, varnishes and coating compositions containing the same

DOEpatents

Yamamori, Naoki; Yokoi, Junji; Yoshikawa, Motoyoshi

1984-01-01

Preparation of hydrolyzable polyester resin comprising reacting polycarboxylic acid and polyhydric alcohol components, which is characterized by using, as at least part of said polyhydric alcohol component, a metallic salt of hydroxy carboxylic acid of the formula defined and effecting the polycondensation at a temperature which is no more than the decomposition temperature of said metallic salt. The polyester resins are useful as resinous vehicle of varnishes and antifouling paints.

Method development for thermal analyses testing on Reillex HPQ resin using the advanced reactive system screening tool (ARSST)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Best, D.

Reillex™ HPQ resin was developed by Los Alamos Laboratory and Reilly Industries Inc. in an effort to increase safety and process efficiency during the recovery and purification of plutonium. Ionac™ A-641, another strong base macroporous anion exchange resin used in the nuclear industry, was known to undergo a runaway reaction in hot nitric acid solutions. Because of this, an extensive amount of thermal analyses testing on the Reillex™ HPQ resin in SRNL was performed in 1999-2001 prior to use. A report on the thermal stability qualification of the Reillex™ HPQ resin in 8M (35%) and 12M (53%) HNO 3 wasmore » reported in 2000. In 2001, the reactivity of Reillex™ HPQ resin in 14.4M (64%) HNO 3 was evaluated. In January of 2001, thermal stability scoping tests were performed on irradiated Reillex™ HPQ resin in 14.4M (64%) HNO 3 (as a worst case scenario) and the results sent to Fauske and Associates to calculate a rupture disk size for the HB-Line resin column. A technical report by Fauske and Associates was issued in February 2001 recommending a 2.0” vent line with a rupture disk set pressure of 60 psig. This calculation was based on ARSST thermal analyses scoping tests at SRNL in which 4 grams of dried resin and 6.0 grams of 64% nitric acid in a 10 gram test cell, produced a maximum pressure rate (dP/dt) of 720 psi/min (12 psi/sec) and a maximum temperature of 250 °C. In 2015, a new batch of Reillex™ HPQ resin was manufactured by Vertellus Industries. A test sample of the resin was sent to SRNL to perform acceptance and qualification thermal stability testing using the ARSST. During these tests, method development was performed to ensure that a representative resin to acid ratios were used while running the tests in the ARSST. Fauske and Associates recommended to either use a full test cell representative of the HB-Line column or a 10 gram sample in the test cell that was representative of the ratios of resin to nitric acid in the actual HB-Line column. An observation was made during method development testing that the 4 grams of resin to 6 grams of 64% acid ratio used in 2001 to determine the rupture disk size did not entirely wet the resin and was not representative of the actual HB-Line column. The results of this study raised questions as to whether the ratio of 4 grams of resin to 6 grams of 64% nitric acid recommended by Fauske and Associates in 2001 was the correct ratio.« less

Characteristics of Alcian-blue Dye Adsorption of Natural Biofilm Matrix

NASA Astrophysics Data System (ADS)

Kurniawan, A.; Yamamoto, T.; Sukandar; Guntur

2018-01-01

In this study, natural biofilm matrices formed on stones have been used for the adsorption of Alcian blue dye. Alcian blue is a member of polyvalent basic dyes that largely used from laboratory until industrial dying purposes. The adsorption of the dye onto the biofilm matrix has been carried out at different experimental conditions such as adsorption isotherm and kinetic of adsorption. The electric charge properties of biofilm matrix and its changes related to the adsorption of Alcian blue have been also investigated. Moreover, the results of Alcian blue adsorption to the biofilm were compared to those onto the acidic and neutral resin. The kinetics of adsorption result showed that the adsorption of the Alcian blue dye reached to a maximum adsorption amount within 60 minutes. The adsorption amount of Alcian blue to biofilm increased monotonously, and the maximum adsorption amount was greater compared to the resins. On the contrary, Alcian blue did not attach to the neutral resin having no electric charge. It seems that Alcian blue attached to the acidic resins due to electrostatic attractive force, and the same seems to be the case for adsorption of Alcian blue to biofilm. The adsorption of Alcian blue to the biofilm and acidic resins fitted to Langmuir type indicates that the binding of Alcian blue to the biofilm and acidic resins occurred in a monolayer like form. The maximum adsorption amount of Alcian blue on the biofilm (0.24 mmol/dry-g) was greater than those of acidic resin (0.025 mmol/dry-g). This indicates that the biofilm has many more sites for Alcian blue attachment than acidic resins. According to the result of this study, the biofilm matrix can be a good adsorbent for dye such as Alcian blue or other dyes that causing hazards in nature.

Occupational phosphine gas poisoning at veterinary hospitals from dogs that ingested zinc phosphide--Michigan, Iowa, and Washington, 2006-2011.

PubMed

2012-04-27

Zinc phosphide (Zn3P2) is a readily available rodenticide that, on contact with stomach acid and water, produces phosphine (PH3), a highly toxic gas. Household pets that ingest Zn3P2 often will regurgitate, releasing PH3 into the air. Veterinary hospital staff members treating such animals can be poisoned from PH3 exposure. During 2006-2011, CDC's National Institute for Occupational Safety and Health (NIOSH) received reports of PH3 poisonings at four different veterinary hospitals: two in Michigan, one in Iowa, and one in Washington. Each of the four veterinary hospitals had treated a dog that ingested Zn3P2. Among hospital workers, eight poisoning victims were identified, all of whom experienced transient symptoms related to PH3 inhalation. All four dogs recovered fully. Exposure of veterinary staff members to PH3 can be minimized by following phosphine product precautions developed by the American Veterinary Medical Association (AVMA). Exposure of pets, pet owners, and veterinary staff members to PH3 can be minimized by proper storage, handling, and use of Zn3P2 and by using alternative methods for gopher and mole control, such as snap traps.

Structure and magnetism of a new hydrogen-bonded layered cobalt(II) network, constructed by the unprecedented carboxylate-phosphinate ligand [O2(C6H5)PCH2CO2]2-.

PubMed

Midollini, Stefano; Orlandini, Annabella; Rosa, Patrick; Sorace, Lorenzo

2005-03-21

By hydrothermal reaction of CoCl2 x 6H2O with K2pcc (H2pcc = phenyl(carboxymethyl) phosphinic acid) at 423 K, a novel hybrid material of formula [Co2(pcc)2 (H2O)2] x H2O has been obtained. The compound, which is the first pcc/metal complex reported, exhibits a polymeric arrangement, where cobalt metal ions, linked together by bridging carboxylate and phosphinate oxygens, form infinite chains of edge-shared CoO6 octahedra. The cobalt chains are in turn linked together through important hydrogen-bonding interactions, which create an infinite 2D architecture. The two crystallographically independent cobalt centers, both displaying distorted octahedral coordination, present different environments as one is surrounded by six ligand oxygens and the other by four ligand oxygens and by two water oxygens. Careful magnetic studies performed by a home-built alternating current susceptometer reveal that the system undergoes an antiferromagnetic transition below 2.0 K leading to a canted structure. Field-dependent studies further indicate the occurrence of a metamagnetic transition at a critical field of 650 +/- 50 G.

Surface Engineering of PAMAM-SDB Chelating Resin with Diglycolamic Acid (DGA) Functional Group for Efficient Sorption of U(VI) and Th(IV) from Aqueous Medium.

PubMed

Ilaiyaraja, P; Deb, A K Singha; Ponraju, D; Ali, Sk Musharaf; Venkatraman, B

2017-04-15

A novel chelating resin obtained via growth of PAMAM dendron on surface of styrene divinyl benzene resin beads, followed by diglycolamic acid functionalization of the dendrimer terminal. Batch experiments were conducted to study the effects of pH, nitric acid concentration, amount of adsorbent, shaking time, initial metal ion concentration and temperature on U(VI) and Th(IV) adsorption efficiency. Diglycolamic acid terminated PAMAM dendrimer functionalized styrene divinylbenzene chelating resin (DGA-PAMAM-SDB) is found to be an efficient candidate for the removal of U(VI) and Th(IV) ions from aqueous (pH >4) and nitric acid media (>3M). The sorption equilibrium could be reached within 60min, and the experimental data fits with pseudo-second-order model. Langmuir sorption isotherm model correlates well with sorption equilibrium data. The maximum U(VI) and Th(IV) sorption capacity onto DGA-PAMAMG 5 -SDB was estimated to be about 682 and 544.2mgg -1 respectively at 25°C. The interaction of actinides and chelating resin is reversible and hence, the resin can be regenerated and reused. DFT calculation on the interaction of U(VI) and Th(IV) ions with chelating resin validates the experimental findings. Copyright © 2017 Elsevier B.V. All rights reserved.

Stereochemical investigations of a novel class of chiral phosphapalladacycle complexes derived from 1-[(2,5-dimethyl)phenyl]ethyldiphenylphosphine.

PubMed

Ng, Joseph Kok-Peng; Li, Yongxin; Tan, Geok-Kheng; Koh, Lip-Lin; Vittal, Jagadese J; Leung, Pak-Hing

2005-12-26

The phosphapalladacycle derived from 1-(2',5'-dimethylphenyl)ethyldiphenylphosphine has been prepared in the optically active and racemic forms. The phosphine was synthesized as a racemate by the treatment of 1-chloro-1-(2',5'-dimethylphenyl)ethane with sodium diphenylphosphide in THF. The racemic phosphapalladacycle was subsequently obtained as the chloro-bridged dimer by the treatment of the phosphine with palladium(II) acetate followed by anion metathesis with lithium chloride. Alternatively, the phosphine could be optically resolved via metal complexation using (R,R)-bis(mu-chloro)bis{1-[1-(N,N-dimethylamino)ethyl]naphthyl-C(2),N}dipalladium(II) as the resolving agent. An efficient separation of the resulting diastereomeric complexes was achieved by silica gel chromatography. The obtained optically resolved diastereomers were next subject to chemoselective removal of the (R)-N,N-(dimethylamino)-1-(1-naphthyl)ethylaminate auxiliary by treatment with concentrated hydrochloric acid. This process yielded the binuclear dimer complexes containing the resolved eta(1)-P ligand. Cyclopalladation of the coordinated phosphine could next be performed by treatment of its eta(1)-P binuclear dimer with silver(I) hexafluorophosphate(V) in a dichloromethane/water mixture followed by treatment with lithium chloride, giving rise to a pair of optically pure enantiomeric dimers with [alpha](D) -322 and +319 degrees in CH(2)Cl(2). Despite the possibilities of the phosphine to attain a five- membered structure by ortho-palladation or a six-membered ring formation by aliphatic C-H bond activation, only the former was observed. X-ray crystallographic data of the meso dimer and an acetylacetonate derivative indicated that the phosphapalladacycle alpha-C methyl substituent was axially located. The 2-D (1)H-(1)H ROESY spectrum of the acetylacetonate derivative further revealed that the phosphapalladacycle was conformationally rigid in CDCl(3).

Emission and distribution of phosphine in paddy fields and its relationship with greenhouse gases.

PubMed

Chen, Weiyi; Niu, Xiaojun; An, Shaorong; Sheng, Hong; Tang, Zhenghua; Yang, Zhiquan; Gu, Xiaohong

2017-12-01

Phosphine (PH 3 ), as a gaseous phosphide, plays an important role in the phosphorus cycle in ecosystems. In this study, the emission and distribution of phosphine, carbon dioxide (CO 2 ) and methane (CH 4 ) in paddy fields were investigated to speculate the future potential impacts of enhanced greenhouse effect on phosphorus cycle involved in phosphine by the method of Pearson correlation analysis and multiple linear regression analysis. During the whole period of rice growth, there was a significant positive correlation between CO 2 emission flux and PH 3 emission flux (r=0.592, p=0.026, n=14). Similarly, a significant positive correlation of emission flux was also observed between CH 4 and PH 3 (r=0.563, p=0.036, n=14). The linear regression relationship was determined as [PH 3 ] flux =0.007[CO 2 ] flux +0.063[CH 4 ] flux -4.638. No significant differences were observed for all values of matrix-bound phosphine (MBP), soil carbon dioxide (SCO 2 ), and soil methane (SCH 4 ) in paddy soils. However, there was a significant positive correlation between MBP and SCO 2 at heading, flowering and ripening stage. The correlation coefficients were 0.909, 0.890 and 0.827, respectively. In vertical distribution, MBP had the analogical variation trend with SCO 2 and SCH 4 . Through Pearson correlation analysis and multiple stepwise linear regression analysis, pH, redox potential (Eh), total phosphorus (TP) and acid phosphatase (ACP) were identified as the principal factors affecting MBP levels, with correlative rankings of Eh>pH>TP>ACP. The multiple stepwise regression model ([MBP]=0.456∗[ACP]+0.235∗[TP]-1.458∗[Eh]-36.547∗[pH]+352.298) was obtained. The findings in this study hold great reference values to the global biogeochemical cycling of phosphorus in the future. Copyright © 2017 Elsevier B.V. All rights reserved.

21 CFR 175.260 - Partial phosphoric acid esters of polyester resins.

Code of Federal Regulations, 2014 CFR

2014-04-01

... section, partial phosphoric acid esters of polyester resins are prepared by the reaction of trimellitic anhydride with 2,2-dimethyl-1,3-propanediol followed by reaction of the resin thus produced with phosphoric... characterizing the type of food and under the conditions of time and temperature characterizing the conditions of...

Extraction of High Quality DNA from Seized Moroccan Cannabis Resin (Hashish)

PubMed Central

El Alaoui, Moulay Abdelaziz; Melloul, Marouane; Alaoui Amine, Sanaâ; Stambouli, Hamid; El Bouri, Aziz; Soulaymani, Abdelmajid; El Fahime, Elmostafa

2013-01-01

The extraction and purification of nucleic acids is the first step in most molecular biology analysis techniques. The objective of this work is to obtain highly purified nucleic acids derived from Cannabis sativa resin seizure in order to conduct a DNA typing method for the individualization of cannabis resin samples. To obtain highly purified nucleic acids from cannabis resin (Hashish) free from contaminants that cause inhibition of PCR reaction, we have tested two protocols: the CTAB protocol of Wagner and a CTAB protocol described by Somma (2004) adapted for difficult matrix. We obtained high quality genomic DNA from 8 cannabis resin seizures using the adapted protocol. DNA extracted by the Wagner CTAB protocol failed to give polymerase chain reaction (PCR) amplification of tetrahydrocannabinolic acid (THCA) synthase coding gene. However, the extracted DNA by the second protocol permits amplification of THCA synthase coding gene using different sets of primers as assessed by PCR. We describe here for the first time the possibility of DNA extraction from (Hashish) resin derived from Cannabis sativa. This allows the use of DNA molecular tests under special forensic circumstances. PMID:24124454

Mass spectrometric methodology for the analysis of highly oxidized diterpenoid acids in Old Master paintings.

PubMed

Berg; Boon; Pastorova; Spetter

2000-04-01

Diterpenoid resins from larch and pine trees and the corresponding fractions in a >100-year-old wax-resin adhesive and varnish and a 200-year-old resin/oil paint sample were analysed with by gas chromatography/mass spectrometry (GC/MS) using several off-line and on-line derivatization methods. The main resin compounds were highly oxidized abietic acids. Important products found are hydroxydehydroabietic acids (OH-DHAs), 7-oxoDHA, di-OH-DHAs and 15-OH-7-oxoDHA. The last two compounds have not been reported to occur in artworks before. Larixyl acetate, an important marker from larch resins, was found to be still present in high amounts in the adhesive. A large number of mass spectra of the different oxidation products and larixol and larixyl acetate are presented and their fragmentation behaviour under electron impact conditions is discussed. An index for the degree of oxidation (IDOX) of the abietic acids is presented as an indicator of the degree of oxidation of the matrix in which the resin is present. The IDOX was 0.10, 0.67, 0.81 and 0.76 for the fresh resins, the dark-aged adhesive, the aged varnish and the resin/oil paint, respectively (measured with pyrolysis (Py)-tetramethylammonium hydroxide (TMAH)-GC/MS). Py-TMAH-GC/MS and direct temperature-resolved mass spectrometry are reliable, valuable and fast techniques for the assessment of the presence and degree of oxidation of diterpenoid resins. Copyright 2000 John Wiley & Sons, Ltd.

[The qualitative analysis and quantitative analysis of purification of salvianolic acids by macroreticular resin].

PubMed

Fang, Xin-sheng; Tan, Xiao-mei

2005-09-01

To purify salvianolic acids by macroreticular resin,then mensurate the contents of salvianolic acids and analyse the chromatogram with HPLC. Make salvianolic acids with macroreticular resin; mensurate the content of Salvianolic acids with UV spestrophotometry: the control compound is protocaechuic aldehyde, and the wavelength is 281 nm. Analysis the chromatogram with HPLC, and compare the chromatogram in different technics: zorbax ODS column (4.6 mm x 250 mm, 5 microm), mobilephase: 1% aceticacid-water and methanol in different proportions, the wavelength is 281 nm. The contents of salvianolic acids is 53.8%; HPLC chromatogram indicate that the method is reasonable to make salvianolic acids. Determination of contents and HPLC chromatogram can control the quality of Salvianolic acids more accurately.

Structure-Guided, Single-Point Modifications in the Phosphinic Dipeptide Structure Yield Highly Potent and Selective Inhibitors of Neutral Aminopeptidases

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vassiliou, Stamatia; Węglarz-Tomczak, Ewelina; Berlicki, Łukasz

Seven crystal structures of alanyl aminopeptidase from Neisseria meningitides (the etiological agent of meningitis, NmAPN) complexed with organophosphorus compounds were resolved to determine the optimal inhibitor–enzyme interactions. The enantiomeric phosphonic acid analogs of Leu and hPhe, which correspond to the P1 amino acid residues of well-processed substrates, were used to assess the impact of the absolute configuration and the stereospecific hydrogen bond network formed between the aminophosphonate polar head and the active site residues on the binding affinity. For the hPhe analog, an imperfect stereochemical complementarity could be overcome by incorporating an appropriate P1 side chain. The constitution of P1'-extendedmore » structures was rationally designed and the lead, phosphinic dipeptide hPhePψ[CH 2]Phe, was modified in a single position. Introducing a heteroatom/heteroatom-based fragment to either the P1 or P1' residue required new synthetic pathways. The compounds in the refined structure were low nanomolar and subnanomolar inhibitors of N. meningitides, porcine and human APNs, and the reference leucine aminopeptidase (LAP). The unnatural phosphinic dipeptide analogs exhibited a high affinity for monozinc APNs associated with a reasonable selectivity versus dizinc LAP. In conclusion, another set of crystal structures containing the NmAPN dipeptide ligand were used to verify and to confirm the predicted binding modes; furthermore, novel contacts, which were promising for inhibitor development, were identified, including a π–π stacking interaction between a pyridine ring and Tyr372.« less

Structure-Guided, Single-Point Modifications in the Phosphinic Dipeptide Structure Yield Highly Potent and Selective Inhibitors of Neutral Aminopeptidases

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vassiliou, Stamatia; Węglarz-Tomczak, Ewelina; Berlicki, Łukasz

2014-10-09

Seven crystal structures of alanyl aminopeptidase from Neisseria meningitides (the etiological agent of meningitis, NmAPN) complexed with organophosphorus compounds were resolved to determine the optimal inhibitor-enzyme interactions. The enantiomeric phosphonic acid analogs of Leu and hPhe, which correspond to the P1 amino acid residues of well-processed substrates, were used to assess the impact of the absolute configuration and the stereospecific hydrogen bond network formed between the aminophosphonate polar head and the active site residues on the binding affinity. For the hPhe analog, an imperfect stereochemical complementarity could be overcome by incorporating an appropriate P1 side chain. The constitution of P1'-extendedmore » structures was rationally designed and the lead, phosphinic dipeptide hPhePψ[CH2]Phe, was modified in a single position. Introducing a heteroatom/heteroatom-based fragment to either the P1 or P1' residue required new synthetic pathways. The compounds in the refined structure were low nanomolar and subnanomolar inhibitors of N. meningitides, porcine and human APNs, and the reference leucine aminopeptidase (LAP). The unnatural phosphinic dipeptide analogs exhibited a high affinity for monozinc APNs associated with a reasonable selectivity versus dizinc LAP. Another set of crystal structures containing the NmAPN dipeptide ligand were used to verify and to confirm the predicted binding modes; furthermore, novel contacts, which were promising for inhibitor development, were identified, including a π-π stacking interaction between a pyridine ring and Tyr372.« less

Structure-Guided, Single-Point Modifications in the Phosphinic Dipeptide Structure Yield Highly Potent and Selective Inhibitors of Neutral Aminopeptidases

DOE PAGES

Vassiliou, Stamatia; Węglarz-Tomczak, Ewelina; Berlicki, Łukasz; ...

2014-10-09

Seven crystal structures of alanyl aminopeptidase from Neisseria meningitides (the etiological agent of meningitis, NmAPN) complexed with organophosphorus compounds were resolved to determine the optimal inhibitor–enzyme interactions. The enantiomeric phosphonic acid analogs of Leu and hPhe, which correspond to the P1 amino acid residues of well-processed substrates, were used to assess the impact of the absolute configuration and the stereospecific hydrogen bond network formed between the aminophosphonate polar head and the active site residues on the binding affinity. For the hPhe analog, an imperfect stereochemical complementarity could be overcome by incorporating an appropriate P1 side chain. The constitution of P1'-extendedmore » structures was rationally designed and the lead, phosphinic dipeptide hPhePψ[CH 2]Phe, was modified in a single position. Introducing a heteroatom/heteroatom-based fragment to either the P1 or P1' residue required new synthetic pathways. The compounds in the refined structure were low nanomolar and subnanomolar inhibitors of N. meningitides, porcine and human APNs, and the reference leucine aminopeptidase (LAP). The unnatural phosphinic dipeptide analogs exhibited a high affinity for monozinc APNs associated with a reasonable selectivity versus dizinc LAP. In conclusion, another set of crystal structures containing the NmAPN dipeptide ligand were used to verify and to confirm the predicted binding modes; furthermore, novel contacts, which were promising for inhibitor development, were identified, including a π–π stacking interaction between a pyridine ring and Tyr372.« less

Use of the 2-chlorotrityl chloride resin for microwave-assisted solid phase peptide synthesis.

PubMed

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.

Novel unsymmetrical P/O substituted ferrocene ligands and the first structurally characterised hydroxyferrocene derivative.

PubMed

Atkinson, Robert C J; Gibson, Vernon C; Long, Nicholas J; White, Andrew J P; Williams, David J

2004-06-21

Two new unsymmetrical 1'-substituted hydroxyferrocene ligands featuring either phosphine or phosphine oxide substituents have been synthesised and the phosphine oxide derivative has been structurally characterised. A nickel complex of the hydroxyl/phosphine ligand has been formed, along with preliminary evaluation of the complex for catalysis of ethylene polymerisation.

Surfactant-controlled polymerization of semiconductor clusters to quantum dots through competing step-growth and living chain-growth mechanisms.

PubMed

Evans, Christopher M; Love, Alyssa M; Weiss, Emily A

2012-10-17

This article reports control of the competition between step-growth and living chain-growth polymerization mechanisms in the formation of cadmium chalcogenide colloidal quantum dots (QDs) from CdSe(S) clusters by varying the concentration of anionic surfactant in the synthetic reaction mixture. The growth of the particles proceeds by step-addition from initially nucleated clusters in the absence of excess phosphinic or carboxylic acids, which adsorb as their anionic conjugate bases, and proceeds indirectly by dissolution of clusters, and subsequent chain-addition of monomers to stable clusters (Ostwald ripening) in the presence of excess phosphinic or carboxylic acid. Fusion of clusters by step-growth polymerization is an explanation for the consistent observation of so-called "magic-sized" clusters in QD growth reactions. Living chain-addition (chain addition with no explicit termination step) produces QDs over a larger range of sizes with better size dispersity than step-addition. Tuning the molar ratio of surfactant to Se(2-)(S(2-)), the limiting ionic reagent, within the living chain-addition polymerization allows for stoichiometric control of QD radius without relying on reaction time.

Fourier transform infrared study on microemulsion system of potassium salt of bis(2-ethylhexyl) phosphinic acid (HA)

NASA Astrophysics Data System (ADS)

Zhou, Weijin; Shi, Nai; Wang, Yi; Chang, Zhiyuan; Wu, JinGuang

1994-01-01

To study microemulsion formation in a solvent extraction system is to probe into some basic principles of extraction chemistry in the light of combining extraction chemistry with surface chemistry. In our previous investigations, the microemulsions of the salts of HDEHP and PC88A have been studied systematically by FT-IR. In the experiment, we observed the change of peak positions and intensities of P equals O, P-O-C and P-O-H groups during saponification and hydration, and discovered that the peak of P-O-C splits apart into 1045 and 1075 cm-1. The vibration frequency of the P-O-C group in HDEHP and PC88A is quite close to the symmetric stretching frequency of the POO- group, and thus causes difficulties in the study of their peak position and absorbance variation. For this reason we synthesized bis(2-ethylhexyl) phosphinic acid without the P-O-C group. Infrared spectra in the range of 800 - 4000 cm-1 of this microemulsion system was studied.

Influence of phosphoproteins' biomimetic analogs on remineralization of mineral-depleted resin-dentin interfaces created with ion-releasing resin-based systems.

PubMed

Sauro, Salvatore; Osorio, Raquel; Watson, Timothy F; Toledano, Manuel

2015-07-01

The study aimed at evaluating the remineralization of acid-etched dentin pre-treated with primers containing biomimetic analogs and bonded using an ion-releasing light-curable resin-based material. An experimental etch-and-rinse adhesive system filled with Ca(2+), PO4(3-)-releasing Ca-Silicate micro-fillers was created along with two experimental primers containing biomimetic analogs such as sodium trimetaphosphate (TMP) and/or polyaspartic acid (PLA). Dentin specimens etched with 37% H3PO4 were pre-treated with two different aqueous primers containing the polyanionic biomimetic analogs or deionized water and subsequently bonded using the experimental resin-based materials. The specimens were sectioned and analyzed by AFM/nanoindentation to evaluate changes in the modulus of elasticity (Ei) across the resin-dentin interface at different AS storage periods (up to 90 days). Raman cluster analysis was also performed to evaluate the chemical changes along the interface. The phosphate uptake by the acid-etched dentin was evaluated using the ATR-FTIR. Additional resin-dentin specimens were tested for microtensile bond strength. SEM examination was performed after de-bonding, while confocal laser microscopy was used to evaluate the interfaces ultramorphology and micropermeability. Both biomimetic primers induced phosphate uptake by acid-etched dentin. Specimens created with the ion-releasing resin in combination with the pre-treatment primers containing either PLA and TMA showed the greatest recovery of the Ei of the hybrid layer, with no decrease in μTBS (p>0.05) after 3-month AS storage. The ion-releasing resin applied after use of the biomimetic primers showed the greatest reduction in micropermeability due to mineral precipitation; these results were confirmed using SEM. The use of the ion-releasing resin-based system applied to acid-etched dentin pre-treated with biomimetic primers containing analogs of phosphoproteins such as poly-l-aspartic acid and/or sodium trimetaphosphate provides a suitable bonding approach for biomimetic remineralization of resin-dentin interfaces. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Method of purifying neutral organophosphorus extractants

DOEpatents

Horwitz, E. Philip; Gatrone, Ralph C.; Chiarizia, Renato

1988-01-01

A method for removing acidic contaminants from neutral mono and bifunctional organophosphorous extractants by contacting the extractant with a macroporous cation exchange resin in the H.sup.+ state followed by contact with a macroporous anion exchange resin in the OH.sup.- state, whereupon the resins take up the acidic contaminants from the extractant, purifying the extractant and improving its extraction capability.

Influence of a peracetic acid-based immersion on indirect composite resin.

PubMed

Samuel, Susana Maria Werner; Fracaro, Gisele Baggio; Collares, Fabrício Mezzomo; Leitune, Vicente Castelo Branco; Campregher, Ulisses Bastos

2011-06-01

The aim of this study was to evaluate the influence of immersion in a 0.2% peracetic acid-based disinfectant on the three-point flexural strength, water sorption and water solubility of an indirect composite resin. Specimens were produced according to ISO 4049:2000 specifications and were divided in two groups: Control group, with no disinfection and Disinfected group, with three 10 min immersions in the peracetic acid intercalated with 10 min immersions in sterile distilled water. All evaluations were conducted in compliance with ISO specifications. Three-point flexural strength, water sorption and solubility of indirect composite resin before and after immersion showed no statistical significant differences (p > 0.05) and met ISO standard requirements. Immersion in peracetic acid solution showed no influence in indirect composite resin tested properties.

METHOD OF SEPARATING RARE EARTHS BY ION EXCHANGE

DOEpatents

Spedding, F.H.; Powell, J.E.

1960-10-18

A process is given for separating yttrium and rare earth values having atomic numbers of from 57 through 60 and 68 through 71 from an aqueous solution whose pH value can range from 1 to 9. All rare earths and yttrium are first adsorbed on a cation exchange resin, and they are then eluted with a solution of N-hydroxyethylethylenediaminetriacetic acid (HEDTA) in the order of decreasing atomic number, yttrium behaving like element 61; the effluents are collected in fractions. The HEDTA is recovered by elution with ammonia solution and the resin is regenerated with sulfuric acid. Rare earths are precipitated from the various effluents with oxalic acid, and each supernatant is passed over cation exchange resin for adsorption of HEDTA and nonprecipitated rare earths: the oxalic acid is not retained by the resin.

Experiments in Thermodynamics and Kinetics of Phosphine Substitution in (p-Cymene)RuCl[subscript 2](PR[subscript 3])

ERIC Educational Resources Information Center

Ozerov, Oleg V.; Fafard, Claudia M.; Hoffman, Norris W.

2007-01-01

This manuscript describes a set of three experiments that investigates the thermodynamic and kinetic aspects of phosphine substitution at a Ru center. In the first experiment, the students synthesize a Ru organometallic complex containing a phosphine ligand. In the second, equilibria for phosphine substitution involving several different…

Advances in Nucleophilic Phosphine Catalysis of Alkenes, Allenes, Alkynes, and MBHADs

PubMed Central

Fan, Yi Chiao

2014-01-01

In nucleophilic phosphine catalysis, tertiary phosphines undergo conjugate additions to activated carbon–carbon multiple bonds to form β-phosphonium enolates, β-phosphonium dienolates, β-phosphonium enoates, and vinyl phosphonium ylides as intermediates. When these reactive zwitterionic species react with nucleophiles and electrophiles, they may generate carbo- and heterocycles with multifarious molecular architectures. This Article describes the reactivities of these phosphonium zwitterions, the applications of phosphine catalysis in the syntheses of biologically active compounds and natural products, and recent developments in the enantioselective phosphine catalysis. PMID:24196409

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

PubMed

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

2017-10-01

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

Behavioral effects of gamma-hydroxybutyrate, its precursor gamma-butyrolactone, and GABA(B) receptor agonists: time course and differential antagonism by the GABA(B) receptor antagonist 3-aminopropyl(diethoxymethyl)phosphinic acid (CGP35348).

PubMed

Koek, Wouter; Mercer, Susan L; Coop, Andrew; France, Charles P

2009-09-01

Gamma-hydroxybutyrate (GHB) is used therapeutically and recreationally. The mechanism by which GHB produces its therapeutic and recreational effects is not entirely clear, although GABA(B) receptors seem to play an important role. This role could be complex, because there are indications that different GABA(B) receptor mechanisms mediate the effects of GHB and the prototypical GABA(B) receptor agonist baclofen. To further explore possible differences in underlying GABA(B) receptor mechanisms, the present study examined the effects of GHB and baclofen on operant responding and their antagonism by the GABA(B) receptor antagonist 3-aminopropyl(diethoxymethyl)phosphinic acid (CGP35348). Pigeons were trained to peck a key for access to food during response periods that started at different times after the beginning of the session. In these pigeons, GHB, its precursor gamma-butyrolactone (GBL), and the GABA(B) receptor agonists baclofen and 3-aminopropyl(methyl)phosphinic acid hydrochloride (SKF97541) decreased the rate of responding in a dose- and time-dependent manner. CGP35348 shifted the dose-response curve of each agonist to the right, but the magnitude of the shift differed among the agonists. Schild analysis yielded a pA(2) value of CGP35348 to antagonize GHB and GBL [i.e., 3.9 (3.7-4.2)] that was different (P = 0.0011) from the pA(2) value to antagonize baclofen and SKF97541 [i.e., 4.5 (4.4-4.7)]. This finding is further evidence that the GABA(B) receptor mechanisms mediating the effects of GHB and prototypical GABA(B) receptor agonists are not identical. A better understanding of the similarities and differences between these mechanisms, and their involvement in the therapeutic effects of GHB and baclofen, could lead to more effective medications with fewer adverse effects.

On the Chemical Emergence of Phosphate-Based Biochemistry

NASA Astrophysics Data System (ADS)

Kee, Terence

Contemporary organisms use orthophosphate derivatives (PO43-) in their cell biochemistry,1 yet questions remain as to how Nature was able to accumulate, activate and exploit the or-thophosphate group from geological sources with both poorly solubility and low chemical activ-ity.2 Gulick argued3 a central role for reduced oxidation state phosphorus (P) oxyacids such as H-phosphonates (H2PO3-) and especially H-phosphinates (H2PO2-) in prebiotic chemistry on account of the greater water solubility of their metal salts and, with the presence of P-H bonds, a different reactivity profile to that expected of orthophosphate. The recent demonstration that hydrothermal corrosion of P-rich mineral phases such as schreibersite (Fe,Ni)3P within iron meteorites leads to production of various P-oxyacids including H-phosphonic (H3PO3)4 and H-phosphinic5 acids as well as orthophosphate has reignited interest in reduced oxida-tion state P chemistry in prebiotic environments. We are examining the prebiotic potential of reduced oxidation state P-chemistry through reactions with carbonyl substrates with rea-sonable prebiotic provenance including formaldehyde glycolaldehyde, both intimately involved in the formose reaction for sugar synthesis6 and pyruvic acid,7 a product of glycolysis and feed-stock for the citric acid cycle, a fundamental cellular metablic process whose heritage is considered an ancient one. In this contribution we present some of our latest results on the H-phosphinate-pyruvate system. References: [1] Lodish H et al. (2000) Molecular Cell Biology, 4th Ed., W. H. Freeman Co., New York. [2] Gulick A. (1955) Am. Sci., 43, 479. [3] Gulick A. (1957) Ann. N. Y. Acad. Sci. 69, 309. [4] Pasek M. A. (2008) Proc. Nat. Acad. Sci. USA, 105, 853. [5] Bryant D. E.and Kee T. P. (2006) Chem. Commun. 2344. [6] Weber A. L. (2000) Origins of Life and Evol. Biosph., 30, 33. [7] Cody G. D. et. al. (2000) Science 289, 1337.

Biological activity of some naturally occurring resins, gums and pigments against in vitro LDL oxidation.

PubMed

Andrikopoulos, Nikolaos K; Kaliora, Andriana C; Assimopoulou, Andreana N; Papapeorgiou, Vassilios P

2003-05-01

Naturally occurring gums and resins with beneficial pharmaceutical and nutraceutical properties were tested for their possible protective effect against copper-induced LDL oxidation in vitro. Chiosmastic gum (CMG) (Pistacia lentiscus var. Chia resin) was the most effective in protecting human LDL from oxidation. The minimum and maximum doses for the saturation phenomena of inhibition of LDL oxidation were 2.5 mg and 50 mg CMG (75.3% and 99.9%, respectively). The methanol/water extract of CMG was the most effective compared with other solvent combinations. CMG when fractionated in order to determine a structure-activity relationship showed that the total mastic essential oil, collofonium-like residue and acidic fractions of CMG exhibited a high protective activity ranging from 65.0% to 77.8%. The other natural gums and resins (CMG resin 'liquid collection', P. terebinthus var. Chia resin, dammar resin, acacia gum, tragacanth gum, storax gum) also tested as above, showed 27.0%-78.8% of the maximum LDL protection. The other naturally occurring substances, i.e. triterpenes (amyrin, oleanolic acid, ursolic acid, lupeol, 18-a-glycyrrhetinic acid) and hydroxynaphthoquinones (naphthazarin, shikonin and alkannin) showed 53.5%-78.8% and 27.0%-64.1% LDL protective activity, respectively. The combination effects (68.7%-76.2% LDL protection) of ursolic-, oleanolic- and ursodeoxycholic- acids were almost equal to the effect (75.3%) of the CMG extract in comparable doses. Copyright 2003 John Wiley & Sons, Ltd.

Novel aqueous oil-in-water emulsions containing extracts of natural coniferous resins are strongly antimicrobial against enterobacteria, staphylococci and yeasts, as well as on bacterial biofilms.

PubMed

Haapakorva, E; Holmbom, T; von Wright, A

2018-01-01

The aim of this study was to examine the antimicrobial properties of novel aqueous natural rapeseed oil/saline emulsions containing different soluble components of spruce resin. The composition of aqueous resin emulsions was analysed by GC-MS and their antimicrobial properties were studied with challenge tests and with turbidometric assays. The emulsions were strongly antimicrobial against common Gram-positive and Gram-negative bacteria (including MRSA) as well as common yeasts. Furthermore, they inhibited the biofilm formation and eradicated the microbial biofilms on tested microbes. Characteristic for the emulsions was the presence of oxidized resin acids. Other main components present in emulsions, such as lignans and coumaric acids, were not antimicrobial, when tested separately. The results indicated that the oxidized resin acids were the antimicrobial components in the emulsions. Also, there appears to be a stoichiometric relationship between the number of resin acid molecules and the number microbe cells in the antimicrobial action. The fact that these solutions do not contain abietic acid, which is the main allergenic compound in resins, suggests that these solutions would be suitable, well-tolerated antimicrobials for various medical applications. The aqueous formulation will also allow the expansion of the use of these emulsions in from medical applications to the food preservatives and disinfectants. © 2017 The Authors. Journal of Applied Microbiology published by John Wiley & Sons Ltd on behalf of the Society for Applied Microbiology.

Significance of wood extractives for wood bonding.

PubMed

Roffael, Edmone

2016-02-01

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

Quantitative analysis of PMR-15 polyimide resin by HPLC

NASA Technical Reports Server (NTRS)

Roberts, Gary D.; Lauver, Richard W.

1987-01-01

The concentration of individual components and of total solids of 50 wt pct PMR-15 resin solutions was determined using reverse-phase HPLC to within + or - 8 percent accuracy. Acid impurities, the major source of impurities in 3,3', 4,4'-benzophenonetetracarboxylic acid (BTDE), were eliminated by recrystallizing the BTDE prior to esterification. Triester formation was not a problem because of the high rate of esterification of the anhydride relative to that of the carboxylic acid. Aging of PMR-15 resin solutions resulted in gradual formation of the mononadimide and bisnadimide of 4,4'-methylenedianiline, with the BTDE concentration remaining constant. Similar chemical reactions occurred at a reduced rate in dried films of PMR-15 resin.

Henry's law constant for phosphine in seawater: determination and assessment of influencing factors

NASA Astrophysics Data System (ADS)

Fu, Mei; Yu, Zhiming; Lu, Guangyuan; Song, Xiuxian

2013-07-01

The Henry's Law constant ( k) for phosphine in seawater was determined by multiple phase equilibration combined with headspace gas chromatography. The effects of pH, temperature, and salinity on k were studied. The k value for phosphine in natural seawater was 6.415 at room temperature (approximately 23°C). This value increases with increases in temperature and salinity, but no obvious change was observed at different pH levels. At the same temperature, there was no significant difference between the k for phosphine in natural seawater and that in artificial seawater. This implies that temperature and salinity are major determining factors for k in marine environment. Double linear regression with Henry's Law constants for phosphine as a function of temperature and salinity confirmed our observations. These results provide a basis for the measurement of trace phosphine concentrations in seawater, and will be helpful for future research on the status of phosphine in the oceanic biogeochemical cycle of phosphorus.

Theoretical study of adsorption of organic phosphines on transition metal surfaces

NASA Astrophysics Data System (ADS)

Lou, Shujie; Jiang, Hong

2018-04-01

The adsorption properties of organic phosphines on transition metal (TM) surfaces (Fe, Co, Ni, Cu, Ru, Rh, Pd, Ag, Ir, Pt, and Au) have been studied to explore the possibility of building novel heterogeneous chiral catalytic systems based on organic phosphines. Preferred adsorption sites, adsorption energies and surface electronic structures of a selected set of typical organic phosphines adsorbed on TM surfaces are calculated with density-functional theory to obtain a systematic understanding on the nature of adsorption interactions. All organic phosphines considered are found to chemically adsorb on these TM surfaces with the atop site as the most preferred one, and the TM-P bond is formed via the lone-pair electrons of the P atom and the directly contacted TM atom. These findings imply that it is indeed possible to build heterogeneous chiral catalytic systems based on organic phosphines adsorbed on TM surfaces, which, however, requires a careful design of molecular structure of organic phosphines.

7 CFR 160.3 - Rosin defined.

Code of Federal Regulations, 2010 CFR

2010-01-01

...) remains after distillation of the fatty acids from tall oil recovered from wood in the course of its chemical disintegration to produce cellulose. In addition to the free resin acids, rosin may contain relatively small proportions of fatty acids, resin esters and other esters, unsaponifiable resenes, and non...

7 CFR 160.3 - Rosin defined.

Code of Federal Regulations, 2011 CFR

2011-01-01

...) remains after distillation of the fatty acids from tall oil recovered from wood in the course of its chemical disintegration to produce cellulose. In addition to the free resin acids, rosin may contain relatively small proportions of fatty acids, resin esters and other esters, unsaponifiable resenes, and non...

Using Sr Resin with mixed acid matrices

DOE PAGES

McLain, Derek R.; Liu, Christine; Sudowe, Ralf

2018-03-02

Here, the quantification of radioactive material dispersed following the release of 90Sr, whether accidental or intentional, would be of high importance. Depending on the circumstances, it is possible that the contaminated materials would need to be completely digested prior to quantification. Many sample matrices require a mixture of different acids be employed to achieve total dissolution. Unfortunately, one the most common approaches for the separation of strontium, extraction chromatography with Sr Resin, has only been fully characterized in pure mineral acid solutions. This work shows that Sr Resin can be used effectively with high concentration mixtures of nitric and hydrochloricmore » acids in the presence or absence of hydrofluoric acid, thereby potentially negating the need for conversion to a pure mineral acid matrix.« less

Using Sr Resin with mixed acid matrices

DOE Office of Scientific and Technical Information (OSTI.GOV)

McLain, Derek R.; Liu, Christine; Sudowe, Ralf

Here, the quantification of radioactive material dispersed following the release of 90Sr, whether accidental or intentional, would be of high importance. Depending on the circumstances, it is possible that the contaminated materials would need to be completely digested prior to quantification. Many sample matrices require a mixture of different acids be employed to achieve total dissolution. Unfortunately, one the most common approaches for the separation of strontium, extraction chromatography with Sr Resin, has only been fully characterized in pure mineral acid solutions. This work shows that Sr Resin can be used effectively with high concentration mixtures of nitric and hydrochloricmore » acids in the presence or absence of hydrofluoric acid, thereby potentially negating the need for conversion to a pure mineral acid matrix.« less

Changes in properties of polyacid-modified composite resins (compomers) following storage in acidic solutions.

PubMed

Nicholson, J W; Gjorgievska, E; Bajraktarova, B; McKenzie, M A

2003-06-01

The interaction of three polyacid-modified composite resins (compomers) with various acidic storage solutions, and also water, over periods of time up to 6 months has been studied and compared with those of a glass-ionomer and a composite resin. This interaction has been shown to vary in a complex way with length of storage and nature of the acid, and citric acid was found to be the most aggressive storage medium for glass-ionomer cement, and also for the compomers. The pure composite resin, by contrast, was relatively unaffected by all of the acid solutions examined. In all acids, the compomers showed a distinct buffering effect, i.e. they increased the pH towards neutral, as did the glass-ionomer. The extent of this also varied with duration of storage and nature of the acid. The biaxial flexure strength was determined and found to be essentially unaffected by the complex chemical interactions with acidic storage solutions. Values obtained for the compomers were lower than those of the composite resin, but above those of the glass-ionomer. Fourier-transform infrared (FT-IR) spectroscopy was employed to study the changes in the compomers following storage in the aqueous media, but bands were broad and no detailed assignments could be made. There were changes in the region of the spectra associated with metal carboxylates however, and this indicates that the secondary acid-base reaction had occurred following water uptake.

Profiling secondary metabolites of needles of ozone-fumigated white pine (Pinus strobus) clones by thermally assisted hydrolysis/methylation GC/MS.

PubMed

Shadkami, F; Helleur, R J; Cox, R M

2007-07-01

Plant secondary metabolites have an important role in defense responses against herbivores and pathogens, and as a chemical barrier to elevated levels of harmful air pollutants. This study involves the rapid chemical profiling of phenolic and diterpene resin acids in needles of two (ozone-tolerant and ozone-sensitive) white pine (Pinus strobus) clones, fumigated with different ozone levels (control, and daily events peaking at 80 and 200 ppb) for 40 days. The phenolic and resin acids were measured using thermally assisted hydrolysis and methylation (THM) gas chromatography/mass spectrometry. Short-term fumigation affected the levels of two phenolic acids, i.e., 3-hydroxybenzoic and 3,4-dihydroxybenzoic acids, in that both showed a substantial decrease in concentration with increased ozone dose. The decrease in concentration of these THM products may be caused by inhibition of the plant's shikimate biochemical pathway caused by ozone exposure. The combined occurrence of these two ozone-sensitive indicators has a role in biomonitoring of ozone levels and its impact on forest productivity. In addition, chromatographic profile differences in the major diterpene resin acid components were observed between ozone-tolerant and ozone-sensitive clones. The resin acids anticopalic, 3-oxoanticopalic, 3beta-hydroxyanticopalic, and 3,4-cycloanticopalic acids were present in the ozone-sensitive pine; however, only anticopalic acid was present in the ozone-tolerant clone. This phenotypic variation in resin acid composition may be useful in distinguishing populations that are differentially adapted to air pollutants.

Photosensitive filler minimizes internal stresses in epoxy resins

NASA Technical Reports Server (NTRS)

Dillon, J. N.

1967-01-01

Photosensitive filler is added to curable epoxy resins to minimize stress from internal shrinkage during curing or polymerization. Cinnamic acid resins and cinnamal ketones may be added in the amount of 1 to 3 percent by weight of the resin mixture.

Wet spinning of solid polyamic acid fibers

NASA Technical Reports Server (NTRS)

Dorogy, William E., Jr. (Inventor); Saintclair, Anne K. (Inventor)

1989-01-01

The invention is a process for the production of solid aromatic polyamic acid and polyimide fibers from a wet gel or coagulation bath wet gel using N,N-dimethylacetamide (DMAc) solution of the polyamic acid derived from aromatic dianhydrides such as 3,3',4,4'-benzo phenone tetracarboxylic dianhydride (BTDA) and aromatic diamines such as 4,4'oxydianiline (4,4'-ODA). By utilizing the interrelationship between coagulation medium and concentration, resin inherent viscosity, resin percent solids, filament diameter, and fiber void content, it is possible to make improved polyamic acid fibers. Solid polyimide fibers, obtained by the thermal cyclization of the polyamic acid precursor, have increased tensile properties compared to fibers containing macropores from the same resin system.

Wet spinning of solid polyamic acid fibers

NASA Technical Reports Server (NTRS)

Dorogy, William E., Jr. (Inventor); St.clair, Anne K. (Inventor)

1991-01-01

The invention is a process for the production of solid aromatic polyamic acid and polyimide fibers from a wet gel or coagulation bath wet gel using N,N-dimethylacetamide (DMAc) solutions of the polyamic acid derived from aromatic dianhydrides such as 3,3',4,4' benzophenonetetra carboxylic dianhydride (BTDA) and aromatic diamines such as 4,4'-oxydianiline (4,4'-ODA). By utilizing the relationship among coagulation medium and concentration, resin inherent viscosity, resin percent solids, filament diameter, and fiber void content, it is possible to make improved polyamic acid fibers. Solid polyimide fibers, obtained by the thermal cyclization of the polyamic acid precursor, have increased tensile properties compared to fibers containing macropores from the same resin system.

Oxygen enhances phosphine toxicity for postharvest pest control.

PubMed

Liu, Yong-Biao

2011-10-01

Phosphine fumigations under superatmospheric oxygen levels (oxygenated phosphine fumigations) were significantly more effective than the fumigations under the normal 20.9% atmospheric oxygen level against western flower thrips [Frankliniella occidentalis (Pergande)] adults and larvae, leafminer Liriomyza langei Frick pupae, grape mealybug [Pseudococcus maritimus (Ehrhorn)] eggs, and Indianmeal moth [Plodia interpunctella (Hübner)] eggs and pupae. In 5-h fumigations with 1,000 ppm phosphine at 5 degrees C, mortalities of western flower thrips increased significantly from 79.5 to 97.7% when oxygen was increased from 20.9 to 40% and reached 99.3% under 80% O2. Survivorships of leafminer pupae decreased significantly from 71.2% under 20.9% O2 to 16.2% under 40% O2 and reached 1.1% under 80% O2 in 24-h fumigations with 500 ppm phosphine at 5 degrees C. Complete control of leafminer pupae was achieved in 24-h fumigations with 1,000 ppm phosphine at 5 degrees C under 60% O2 or higher. Survivorships of grape mealybug eggs also decreased significantly in 48-h fumigations with 1,000 ppm phosphine at 2 degrees C under 60% O2 compared with the fumigations under 20.9% O2. Indian meal moth egg survivorships decreased significantly from 17.4 to 0.5% in responses to an oxygen level increase from 20.9 to 40% in 48-h fumigations with 1,000 ppm phosphine at 10 degrees C and reached 0.2% in fumigations under 80% O2. When the oxygen level was reduced from 20.9 to 15 and 10% in fumigations, survivorships of Indianmeal moth eggs increased significantly from 17.4 to 32.9 and 39.9%, respectively. Increased O2 levels also resulted in significantly lower survival rates of Indianmeal moth pupae in response to 24-h fumigations with 500 and 1,000 ppm phosphine at 10 degrees C and a complete control was achieved in the 1,000 ppm phosphine fumigations under 60% O2. Oxygenated phosphine fumigations have marked potential to improve insecticidal efficacy. Advantages and limitations of oxygenated phosphine fumigation are discussed.

Ligand-Promoted Rh(III)-Catalyzed Coupling of Aryl C-H Bonds with Arylboron Reagents.

PubMed

Wang, Huai-Wei; Cui, Pei-Pei; Lu, Yi; Sun, Wei-Yin; Yu, Jin-Quan

2016-04-15

Rhodium(III)-catalyzed C-H arylation of arenes with phenylboronic acid pinacol esters has been achieved using a readily removable N-pentafluorophenylbenzamide directing group for the first time. The use of a bidentate phosphine ligand (Binap) significantly increased the yield of the cross-coupling of C-H bonds with organoboron reagents.

Effects of the peracetic acid and sodium hypochlorite on the colour stability and surface roughness of the denture base acrylic resins polymerised by microwave and water bath methods.

PubMed

Fernandes, Flavio H C N; Orsi, Iara A; Villabona, Camilo A

2013-03-01

This study evaluated the surface roughness (Ra) and color stability of acrylic resin colors (Lucitone 550, QC-20 and Vipi-Wave) used for fabricating bases for complete, removable dentures, overdentures and prosthetic protocol after immersion in chemical disinfectants (1% sodium hypochlorite and 2% peracetic acid) for 30 and 60 minutes. Sixty specimens were made of each commercial brand of resin composite, and divided into 2 groups according to the chemical disinfectants. Specimens had undergone the finishing and polishing procedures, the initial color and roughness measurements were taken (t=0), and after this, ten test specimens of each commercial brand of resin composite were immersed in sodium hypochlorite and ten in peracetic acid, for 30 and 60 minutes, with measurements being taken after each immersion period. These data were submitted to statistical analysis. There was evidence of an increase in Ra after 30 minutes immersion in the disinfectants in all the resins, with QC-20 presenting the highest Ra values, and Vipi-Wave the lowest. After 60 minutes immersion in the disinfectants all the resins presented statistically significant color alteration. Disinfection with 1% sodium hypochlorite and peracetic acid altered the properties of roughness and color of the resins. © 2012 The Gerodontology Society and John Wiley & Sons A/S.

Adsorptive separation in bioprocess engineering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang, E.W.Y.

1987-01-01

The invention and development of an energy-efficient separation technique for recovery of desired chemicals from biomass conversion would greatly enhance the economic viability of this bioprocess. Adsorptive separation of several chemicals from aqueous solution was studied in this thesis. The desired species were recovered from the dilute aqueous solution by using crosslinked polyvinylpyridine resin to effect selective sorption. The sorbed chemicals were then removed from the resin by either thermal regeneration or elution with some appropriate desorbents. The effects of temperature, pH value, and solute concentration on resin swelling were investigated. The adsorption equilibrium isotherms, resin capacities and resin selectivitiesmore » of methanol, ethanol, 1-propanol, isopropanol, glycerol, acetone, 1-butanol, tert-butanol, and 2,3-butanediol were determined to study the homologies. Furthermore, acetic acid, butyric acid, hydrochloric acid, lactic acid, and sulfuric acid were recovered from very dilute aqueous solutions. The concentration of the sorbed chemical in the stationary phase can be many times higher than in the mobile phase for some acids. Finally, different types of equilibrium isotherms were used to fit the experimental data. A mathematical model was developed by using the theory of interference to predict the breakthrough curves and the process efficiency to provide information for large-scale process design and development.« less

Resin-dentin bonds to EDTA-treated vs. acid-etched dentin using ethanol wet-bonding. Part II: Effects of mechanical cycling load on microtensile bond strengths.

PubMed

Sauro, Salvatore; Toledano, Manuel; Aguilera, Fatima Sánchez; Mannocci, Francesco; Pashley, David H; Tay, Franklin R; Watson, Timothy F; Osorio, Raquel

2011-06-01

To compare microtensile bond strengths (MTBS) subsequent to load cycling of resin bonded acid-etched or EDTA-treated dentin using a modified ethanol wet-bonding technique. Flat dentin surfaces were obtained from extracted human molars and conditioned using 37% H(3)PO(4) (PA) (15s) or 0.1M EDTA (60s). Five experimental adhesives and one commercial bonding agent were applied to the dentin and light-cured. Solvated experimental resins (50% ethanol/50% comonomers) were used as primers and their respective neat resins were used as the adhesives. The resin-bonded teeth were stored in distilled water (24h) or submitted to 5000 loading cycles of 90N. The bonded teeth were then sectioned in beams for MTBS. Modes of failure were examined by scanning electron microscopy. The most hydrophobic resin 1 gave the lowest bond strength values to both acid and EDTA-treated dentin. The hydrophobic resin 2 applied to EDTA-treated dentin showed lower bond strengths after cycling load but this did not occur when it was bonded to PA-etched dentin. Resins 3 and 4, which contained hydrophilic monomers, gave higher bond strengths to both EDTA-treated or acid-etched dentin and showed no significant difference after load cycling. The most hydrophilic resin 5 showed no significant difference in bond strengths after cycling loading when bonded to EDTA or phosphoric acid treated dentin but exhibited low bond strengths. The presence of different functional monomers influences the MTBS of the adhesive systems when submitted to cyclic loads. Adhesives containing hydrophilic comonomers are not affected by cycling load challenge especially when applied on EDTA-treated dentin followed by ethanol wet bonding. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Energy value of paraquat-treated and resin-soaked lobolly pine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kossuth, S.V.; Roberts, D.R.; Huffman, J.B.

1984-07-01

With a basal injector, loblolly pines were treated with 5% paraquat cation (weight/weight basis) and harvested after 18 months. The resin acid, turpentine, moisture content (MC) and energy value were measured in three bolts of the stem. In bolt 1, the first 152 cm above the injection site, the increase in resin acids was 392% and in turpentine, 564%. Within the whole stem (the first two 152 cm bolts and the third bolt to a 7.6 cm inside-bark diameter) resin acids and turpentine increased 203 and 296% respectively. Moisture content was reduced 9%, 8%, and 8% in bolts 1, 2more » and 3, respectively. Turpentine from treated and untreated trees had an average heating value of 19,369 cal/g. When weighted for volume, net energy content was 7.8% greater for treated than control trees because of the increase in resin, including turpentine and the lowered MC.« less

Analytical method for dissolved-organic carbon fractionation

USGS Publications Warehouse

Leenheer, Jerry A.; Huffman, Edward W. D.

1979-01-01

A standard procedure for analytical-scale dissolved organic carbon fractionation is presented, whereby dissolved organic carbon in water is first fractionated by a nonionic macroreticular resin into acid, base, and neutral hydrophobic organic solute fractions, and next fractionated by ion-exchange resins into acid, base, and neutral hydrophilic solute fractions. The hydrophobic solutes are defined as those sorbed on a nonionic, acrylic-ester macroreticular resin and are differentiated into acid, base, and nautral fractions by sorption/desorption controlled by pH adjustment. The hydrophilic bases are next sorbed on strong-acid ion-exchange resin, followed by sorption of hydrophilic acids on a strong-base ion-exchange resin. Hydrophilic neutrals are not sorbed and remain dissolved in the deionized water at the end of the fractionation procedure. The complete fractionation can be performed on a 200-milliliter filtered water sample, whose dissolved organic carbon content is 5-25 mg/L and whose specific conductance is less than 2,000 μmhos/cm at 25°C. The applications of dissolved organic carbon fractionation analysis range from field studies of changes of organic solute composition with synthetic fossil fuel production, to fundamental studies of the nature of sorption processes.

Hydrogenation of carboxylic acids with a homogeneous cobalt catalyst.

PubMed

Korstanje, Ties J; van der Vlugt, Jarl Ivar; Elsevier, Cornelis J; de Bruin, Bas

2015-10-16

The reduction of esters and carboxylic acids to alcohols is a highly relevant conversion for the pharmaceutical and fine-chemical industries and for biomass conversion. It is commonly performed using stoichiometric reagents, and the catalytic hydrogenation of the acids previously required precious metals. Here we report the homogeneously catalyzed hydrogenation of carboxylic acids to alcohols using earth-abundant cobalt. This system, which pairs Co(BF4)2·6H2O with a tridentate phosphine ligand, can reduce a wide range of esters and carboxylic acids under relatively mild conditions (100°C, 80 bar H2) and reaches turnover numbers of up to 8000. Copyright © 2015, American Association for the Advancement of Science.

Production of sodium-22 from proton irradiated aluminum

DOEpatents

Taylor, Wayne A.; Heaton, Richard C.; Jamriska, David J.

1996-01-01

A process for selective separation of sodium-22 from a proton irradiated minum target including dissolving a proton irradiated aluminum target in hydrochloric acid to form a first solution including aluminum ions and sodium ions, separating a portion of the aluminum ions from the first solution by crystallization of an aluminum salt, contacting the remaining first solution with an anion exchange resin whereby ions selected from the group consisting of iron and copper are selectively absorbed by the anion exchange resin while aluminum ions and sodium ions remain in solution, contacting the solution with an cation exchange resin whereby aluminum ions and sodium ions are adsorbed by the cation exchange resin, and, contacting the cation exchange resin with an acid solution capable of selectively separating the adsorbed sodium ions from the cation exchange resin while aluminum ions remain adsorbed on the cation exchange resin is disclosed.

Acid etching of titanium for bonding with veneering composite resins.

PubMed

Ban, Seiji; Taniki, Toshio; Sato, Hideo; Kono, Hiroshi; Iwaya, Yukari; Miyamoto, Motoharu

2006-06-01

Commercially pure titanium (cpTi) was etched using three concentrated acids: 18% HCl, 43% H3PO4, and 48% H2SO4. The bond strengths between five types of veneering composite resin and eight cpTi treatments (involving combinations of sandblasting, acid etching in 48% H2SO4, and vacuum firing) were determined before and after 10,000 and 20,000 thermal cycles. There were no significant differences in the bond strength of resin to cpTi after etching in 48% H2SO4 at 90 degrees C for 15 minutes, at 60 degrees C for 15, 30, or 60 minutes, and after sandblasting with and without vacuum firing (p > 0.05); moreover, these treatments yielded the highest values. As for vacuum firing, it had no significant effect on resin bond strength to cpTi before or after 10,000 and 20,000 thermal cycles. We therefore concluded that acid etching in concentrated H2SO4 is a simple and effective surface modification method of titanium for bonding to veneering composite resins.

Reusable chelating resins concentrate metal ions from highly dilute solutions

NASA Technical Reports Server (NTRS)

Bauman, A. J.; Weetal, H. H.; Weliky, N.

1966-01-01

Column chromatographic method uses new metal chelating resins for recovering heavy-metal ions from highly dilute solutions. The absorbed heavy-metal cations may be removed from the chelating resins by acid or base washes. The resins are reusable after the washes are completed.

Development of solvent-free offset ink using vegetable oil esters and high molecular-weight resin.

PubMed

Park, Jung Min; Kim, Young Han; Kim, Sung Bin

2013-01-01

In the development of solvent-free offset ink, the roles of resin molecular weight and used solvent on the ink performance were evaluated by examining the relationship between the various properties of resin and solvent and print quality. To find the best performing resin, the soy-oil fatty acid methyl ester (FAME) was applied to the five modified-phenolic resins having different molecular weights. It is found from the experimental results that the ink made of higher molecular weight and better solubility resin gives better printability and print quality. It is because larger molecular weight resin with better solubility gives higher rate of ink transfer. From the ink application of different esters to high molecular weight resin, the best printing performance was yielded from the soy-oil fatty acid butyl ester (FABE). It is due to its high kinematic viscosity resulting in the smallest change of ink transfer weight upon multiple number of printing, which improves the stability of ink quality.

21 CFR 177.2420 - Polyester resins, cross-linked.

Code of Federal Regulations, 2013 CFR

2013-04-01

... polyester resins are produced by the condensation of one or more of the acids listed in paragraph (a)(1) of.... Reinforcements: Asbestos Glass fiber Polyester fiber produced by the condensation of one or more of the acids...

21 CFR 177.2420 - Polyester resins, cross-linked.

Code of Federal Regulations, 2012 CFR

2012-04-01

... polyester resins are produced by the condensation of one or more of the acids listed in paragraph (a)(1) of.... Reinforcements: Asbestos Glass fiber Polyester fiber produced by the condensation of one or more of the acids...

Tall oil precursors of Douglas fir

Treesearch

Daniel O. Foster; Duane F. Zinkel; Anthony H. Conner

1980-01-01

The sapwood and heartwood extractives of Douglas fir [Pseudotsuga menziesii (Mirb.) Franco] and the tall oil in the kraft black liquor were characterized. On pulping, isomerization and conversion of conjugated resin acids to dehydroabietic acid was observed. Recovery of both fatty and resin acids from pulping was lower than predicted from the extractive composition....

Paraquat-induced lightwood in two European conifers - Scotch pine and Norway spruce

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wroblewska, H.; Conner, A.H.; Rowe, J.W.

1978-04-01

Paraquat treatment induced oleoresin-soaked lightwood in Scotch pine; borehole and ax-frill treatment methods were equally effective. Paraquat treatment of Norway spruce induced limited lightwood formation accompanied by heavy external oleoresin exudation. Thus paraquat treatment of Scotch pine and possibly Norway spruce could be commercially advantageous for increasing naval stores production from these species. Analysis of tall oil precursors (nonvolatile ether extractives) for resin acids, fatty acids, and nonsaponifiables showed that the increase from paraquat treatment was mainly from an increased resin acid content. The chemical composition of the resin acids from the lightwood and control wood areas was similar andmore » consisted of the usual pimaric and abietic type resin acids found in conifers. The fatty acids were predominately unsaturated C/sub 18/ isomers. Turpentine of both species consisted mainly of ..cap alpha..-pinene, ..beta..-pinene, and 3-carene. The composition of the turpentine from the Scotch pine lightwood did not differ from that of the control wood. However, turpentine from the Norway spruce lightwood had an increased 3-carene content compared to that from the control.« less

Separation of organic ion exchange resins from sludge -- engineering study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Duncan, J.B.

1998-08-25

This engineering study evaluates the use of physical separation technologies to separate organic ion exchange resin from KE Basin sludge prior to nitric acid dissolution. This separation is necessitate to prevent nitration of the organics in the acid dissolver. The technologies under consideration are: screening, sedimentation, elutriation. The recommended approach is to first screen the Sludge and resin 300 microns then subject the 300 microns plus material to elutriation.

SEPARATION OF PLUTONIUM FROM AQUEOUS SOLUTIONS BY ION-EXCHANGE

DOEpatents

Schubert, J.

1958-06-01

A process is described for the separation of plutonium from an aqueous solution of a plutonium salt, which comprises adding to the solution an acid of the group consisting of sulfuric acid, phosphoric acid, and oxalic acid, and mixtures thereof to provide an acid concentration between 0.0001 and 1 M, contacting the resultant solution with a synthetic organic anion exchange resin, and separating the aqueous phase and the resin which contains the plutonium.

A Cocatalytic Effect between Meldrum's Acid and Benzoxazine Compounds in Preparation of High Performance Thermosetting Resins.

PubMed

Chen, Yi; Lin, Liang-Kai; Chiang, Shu-Jen; Liu, Ying-Ling

2017-02-01

In this work, a cocatalytic effect between Meldrum's acid (MA) and benzoxazine (Bz) compounds has been explored to build up a self-promoting curing system. Consequently, the MA/Bz reactive blend exhibits a relatively low reaction temperature compared to the required temperatures for the cross-linking reactions of the pure MA and Bz components. This feature is attractive for energy-saving processing issues. Moreover, the thermosetting resins based on the MA/Bz reactive blends have been prepared. The MA component can generate additional free volume in the resulting resins, so as to trap air in the resin matrix and consequently to bring low dielectric constants to the resins. The MA-containing agent is an effective modifier for benzoxazine resins to reduce their dielectric constants. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Design and synthesis of bio-based UV curable PU acrylate resin from itaconic acid for coating applications

PubMed Central

Patil, Deepak M.; Phalak, Ganesh A.; Mhaske, S. T.

2017-01-01

Abstract UV curable PUA resin was successfully synthesized from polyol based on sustainable resource originated from itaconic acid (IA), isophorone diisocyanate (IPDI) and 2-hydroxyethyl methacrylate (HEMA). A polyol was synthesized by condensation reaction of IA with 16-hexanediol in the presence of p-Toluenesulfonic acid (pTSA). The synthesized PUA resin was characterized for its structural elucidation by using Fourier Transform Infrared Spectrophotometer (FTIR), 1H and 13C NMR spectroscopy. The synthesized UV curable PUA resin was incorporated in varying concentrations in conventional PUA coating system. The effects of varying concentration of synthesized UV curable PUA resin on rheology, crystallinity, thermal and coating properties were evaluated. The rheological behavior of the resins were evaluated at variable stress and result showed decrease in viscosity of resin as concentration of synthesized UV curable PUA resin increases in conventional PUA resin. The cured coatings have been evaluated for glass transition temperature (T g) and thermal behavior by differential scanning calorimeter and thermogravimetric analysis respectively. The degree of crystallinity of the coatings was determined from X-ray diffraction patterns using the PFM program. It was found that increase in the mass proportion of IA based PUA in coatings, the coating becomes more rigid and crystalline. The synthesized UV curable PUA coatings showed interesting mechanical, chemical, solvent and thermal properties as compared to the conventional PUA. Further, cured coatings were also evaluated for gel content and water absorption. PMID:29491798

Tall oil precursors in three western pines: ponderosa, lodgepole, and limber pine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Conner, A.H.; Diehl, M.A.; Rowe, J.W.

1980-01-01

The nonvolatile diethyl ether extracts (NVEE) from ponderosa, lodgepole, and limber pines were analyzed to determine the amounts and chemical composition of the tall oil precursors (resin acids, fatty acids, and nonsaponifiables) and turpentine precursors available from these species. The results showed that crude tall oil compositions would be approximately as follows (% resin acids, % fatty acids, % nonsaponifiables); ponderosa pine - sapwood (15, 75, 10), heartwood (78, 7, 15); lodgepole pine - sapwood (24, 57, 19), heartwood (51, 26, 23); limber pine - sapwood (10, 82, 8), heartwood (23, 60, 17). The larger nonsaponifiables content, as compared tomore » southern pines, is the major factor in explaining the greater difficulty in the distillative refining of tall oil from these western species. Eight resin acids were found in ponderosa and lodgepole pine: palustric, isopimaric, abietic, dehydroabietic, and neoabietic acids predominated. Seven resin acids were identified from limber pine: anticopalic, isopimaric, abietic, and dehydroabietic acids predominated. The free and esterfied fatty acids from these species contained predominantly oleic and linoleic acids. In addition limber pine contained major amounts of 5, 9, 12-octadecatrienoic acid. The nonsaponifiables contained mostly diterpenes and the sterols, sitosterol and campesterol. The major turpentine components were: ponderosa pine - ..beta..-pinene and 3-carene; lodgepole pine - ..beta..-phellandrene; and limber pine - 3-carene, ..beta..-phellandrene, ..cap alpha..-piene, and ..beta..-pinene.« less

Photooxidation of mixed aryl and biarylphosphines.

PubMed

Zhang, Dong; Celaje, Jeff A; Agua, Alon; Doan, Chad; Stewart, Timothy; Bau, Robert; Selke, Matthias

2010-07-02

Arylphosphines and dialkylbiarylphosphines react with singlet oxygen to form phosphine oxides and phosphinate esters. For mixed arylphosphines, the most electron-rich aryl group migrates to form the phosphinate, while for dialkylbiarylphosphines migration of the alkyl group occurs. Dialkylbiarylphosphines also yield arene epoxides, especially in electron-rich systems. Phosphinate ester formation is increased at high temperature, while protic solvents increase the yield of epoxide. The product distribution provides evidence for Buchwald's recent conformational model for the aerobic oxidation of dialkylbiarylphosphines.

Effect of sulfuric acid etching of polyetheretherketone on the shear bond strength to resin cements.

PubMed

Sproesser, Oliver; Schmidlin, Patrick R; Uhrenbacher, Julia; Roos, Malgorzata; Gernet, Wolfgang; Stawarczyk, Bogna

2014-10-01

To examine the influence of etching duration on the bond strength of PEEK substrate in combination with different resin composite cements. In total, 448 PEEK specimens were fabricated, etched with sulfuric acid for 5, 15, 30, 60, 90, 120, and 300 s and then luted with two conventional resin cements (RelyX ARC and Variolink II) and one self-adhesive resin cement (Clearfil SA Cement) (n = 18/subgroup). Non-etched specimens served as the control group. Specimens were stored in distilled water for 28 days at 37°C and shear bond strengths were measured. Data were analyzed nonparametrically using Kruskal-Wallis-H (p < 0.05). Non-etched PEEK demonstrated no bond strength to resin composite cements. The optimal etching duration varied with the type of resin composite: 60 s for RelyX ARC (15.3 ± 7.2 MPa), 90 s for Variolink II (15.2 ± 7.2 MPa), and 120 s for Clearfil SA Cement (6.4 ± 5.9 MPa). Regardless of etching duration, however, the self-etching resin composite cement showed significantly lower shear bond strength values when compared to groups luted with the conventional resin composites. Although sulfuric acid seems to be suitable and effective for PEEK surface pre-treatment, further investigations are required to examine the effect of other adhesive systems and cements.

Effect of acid and laser etching on shear bond strength of conventional and resin-modified glass-ionomer cements to composite resin.

PubMed

Navimipour, Elmira Jafari; Oskoee, Siavash Savadi; Oskoee, Parnian Alizadeh; Bahari, Mahmoud; Rikhtegaran, Sahand; Ghojazadeh, Morteza

2012-03-01

Success in sandwich technique procedures can be achieved through an acceptable bond between the materials. The aim of this study was to compare the effect of 35% phosphoric acid and Er,Cr:YSGG laser on shear bond strength of conventional glass-ionomer cement (GIC) and resin-modified glass-ionomer cement (RMGIC) to composite resin in sandwich technique. Sixty-six specimens were prepared from each type of glass-ionomer cements and divided into three treatment groups as follows: without pretreatment, acid etching by 35% phosphoric acid for 15 s, and 1-W Er,Cr:YSGG laser treatment for 15 s with a 600-μm-diameter tip aligned perpendicular to the target area at a distance of 1 mm from the surface. Energy density of laser irradiation was 17.7 J/cm(2). Two specimens in each group were prepared for evaluation under a scanning electron microscope (SEM) after surface treatment and the remainder underwent bonding procedure with a bonding agent and composite resin. Then the shear bond strength was measured at a crosshead speed of 0.5 mm/min. Two-factor analysis of variance and post-hoc Tukey test showed that the cement type, surface treatment method, and the interaction of these two factors significantly affect the shear bond strength between glass-ionomer cements and composite resin (p < 0.05). Surface treatment with phosphoric acid or Er,Cr:YSGG laser increased the shear bond strength of GIC to composite resin; however, in RMGIC only laser etching resulted in significantly higher bond strength. These findings were supported by SEM results. The fracture mode was evaluated under a stereomicroscope at ×20.

Modelling of the acid-base properties of natural and synthetic adsorbent materials used for heavy metal removal from aqueous solutions.

PubMed

Pagnanelli, Francesca; Vegliò, Francesco; Toro, Luigi

2004-02-01

In this paper a comparison about kinetic behaviour, acid-base properties and copper removal capacities was carried out between two different adsorbent materials used for heavy metal removal from aqueous solutions: an aminodiacetic chelating resin as commercial product (Lewatit TP207) and a lyophilised bacterial biomass of Sphaerotilus natans. The acid-base properties of a S. natans cell suspension were well described by simplified mechanistic models without electrostatic corrections considering two kinds of weakly acidic active sites. In particular the introduction of two-peak distribution function for the proton affinity constants allows a better representation of the experimental data reproducing the site heterogeneity. A priori knowledge about resin functional groups (aminodiacetic groups) is the base for preliminary simulations of titration curve assuming a Donnan gel structure for the resin phase considered as a concentrated aqueous solution of aminodiacetic acid (ADA). Departures from experimental and simulated data can be interpreted by considering the heterogeneity of the functional groups and the effect of ionic concentration in the resin phase. Two-site continuous model describes adequately the experimental data. Moreover the values of apparent protonation constants (as adjustable parameters found by non-linear regression) are very near to the apparent constants evaluated by a Donnan model assuming the intrinsic constants in resin phase equal to the equilibrium constants in aqueous solution of ADA and considering the amphoteric nature of active sites for the evaluation of counter-ion concentration in the resin phase. Copper removal outlined the strong affinity of the active groups of the resin for this ion in solution compared to the S. natans biomass according to the complexation constants between aminodiacetic and mono-carboxylic groups and copper ions.

Production of R-Mandelic Acid Using Nitrilase from Recombinant E. coli Cells Immobilized with Tris(Hydroxymethyl)Phosphine.

PubMed

Zhang, Xin-Hong; Liu, Zhi-Qiang; Xue, Ya-Ping; Wang, Yuan-Shan; Yang, Bo; Zheng, Yu-Guo

2018-03-01

Recombinant Escherichia coli cells harboring nitrilase from Alcaligenes faecalis were immobilized using tris(hydroxymethyl)phosphine (THP) as the coupling agent. The optimal pH and temperature of the THP-immobilized cells were determined at pH 8.0 and 55 °C. The half-lives of THP-immobilized cells measured at 35, 40, and 50 °C were 1800, 965, and 163 h, respectively. The concentration of R-mandelic acid (R-MA) reached 358 mM after merely 1-h conversion by the immobilized cells with 500 mM R,S-mandelonitrile (R,S-MN), affording the highest productivity of 1307 g L -1  day -1 and the space-time productivity of 143.2 mmol L -1  h -1  g -1 . The immobilized cells with granular shape were successfully recycled for 60 batches using 100 mM R,S-MN as substrate at 40 °C with 64% of relative activity, suggesting that the immobilized E. coli cells obtained in this study are promising for the production of R-MA.

Sand consolidation method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Young, B.M.

1965-10-05

This is a new and improved sand consolidation method wherein an in-situ curing of a resinous fluid is undertaken. This method does not require that the resinous fluids be catalyzed at the surface of the well or well bore as is the case in previous methods. This method consists of, first, pumping an acid-curable consolidating fluid into the unconsolidated sand or earth formation and, secondly, pumping an oil overflush solution containing a halogenated organic or other organic acid or delayed acid-producing chemical. A small quantity of diesel oilspacer may be used between the plastic catalyst solution. The overflush functions tomore » remove permeability, and its acid or acid producing component promotes subsequent hardening of the remaining film of consolidating fluid. Trichloroacetic acid and benzotrichloride are satisfactory to add to the overflush solution for curing the resins. (17 claims)« less

Chemical and biomedical motifs of the reactions of hydroxymethylphosphines with amines, amino acids, and model peptides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Berning, D.E.; Katti, K.V.; Barnes, C.L.

1999-03-03

The reactions of tris(hydroxymethyl)phosphine (THP, 1), 1,2-bis(bis(hydroxymethyl)phosphino)benzene (HMPB, 2), and 1,2-bis(bis(hydroxymethyl)phosphino)ethane (HMPE, 3) with various amines including amino acids and model peptides have been explored. The reactions of these multifunctional phosphines with excess amino acids unexpectedly produced monomeric products. The reaction of THP with excess glycine produced THP(glycine){sub 3} (4) in high yield. The reactions of HMPB with the secondary amines N-methylaniline and diethylamine produced the compounds HMPB(N-methylaniline){sub 4} (5) and HMPB(diethylamine){sub 4} (6), respectively. However, the reactions of HMPB and HMPE with excess glycine produced trans annular-bonded bicyclic compounds HMPB(glycine){sub 2} (7) and HMPE(glycine){sub 2} (10). The reactions ofmore » HMPB with excess alanine and glycylglycylglycine were also explored to determine the generality of the reactions and correspondingly yielded the novel heterocyclic compounds HMPB(alanine){sub 2} (8) and HMPB(gly-gly-gly){sub 2} (9), respectively. The products are oxidatively stable in air and under a wide pH range. All of the new compounds have been characterized by a combination of analytical and spectroscopic techniques, and the molecular structures of compounds 4, 5, 7, and 10 have been confirmed by single-crystal X-ray diffraction studies.« less

DOTA analogues with a phosphinate-iminodiacetate pendant arm: modification of the complex formation rate with a strongly chelating pendant.

PubMed

Procházková, Soňa; Kubíček, Vojtěch; Böhmová, Zuzana; Holá, Kateřina; Kotek, Jan; Hermann, Petr

2017-08-08

The new ligand H 6 do3aP ida combines the macrocyclic DOTA-like cavity and the open-chain iminodiacetate group connected through a coordinating phosphinate spacer. Its acid-base and coordination properties in solution were studied by potentiometry. Thermodynamic coordination characteristics of both chelating units are similar to those reported for H 4 dota and iminodiacetic acid themselves, respectively, so, macrocyclic and iminodiacetate units behave independently. The formation kinetics of the Ce(iii)-H 6 do3aP ida complex was studied by UV-Vis spectrophotometry. Various out-of-cage intermediates were identified with 1 : 1, 1 : 2 and 2 : 1 ligand-to-metal ratios. The presence of the strongly coordinating iminodiacetate group significantly slows down the metal ion transfer into the macrocyclic cavity and, so, the formation of the in-cage complex is two orders of magnitude slower than that reported for the Ce(iii)-H 4 dota system. The kinetic inertness of the [Ce(do3aP ida )] 3- complex towards acid-assisted dissociation is comparable to that of the [Ce(dota)] - complex. The coordination modes of the ligand are demonstrated in the solid-state structure of [Cu 4 (do3aP ida )(OH)(H 2 O) 4 ]Cl·7.5H 2 O.

Determination of airborne, volatile amines from polyurethane foams by sorption onto a high-capacity cation-exchange resin based on poly(succinic acid).

PubMed

Seeber, G; Buchmeiser, M R; Bonn, G K; Bertsch, T

1998-06-05

A high-capacity carboxylic acid-functionalized resin prepared by ring-opening metathesis polymerization based on cross-linked endo,endo-poly(norborn-2-ene-5,6-dicarboxylic acid) was used for the sampling of volatile, airborne amines from polyurethane (PU) foams. Six tertiary amines which represent commonly used promotors for the formation of PUs from diisocyanates and polyols, namely pentamethyldiethylenetriamine, diazabicyclooctane, N-methylmorpholine, N-ethylmorphine, 1,4-dimethylpiperazine and N,N-dimethylethanolamine, were sorbed onto the new resin. The sorption behavior of the new material was investigated in terms of loading capacities, the influence of concentration, flow-rate as well as of the amount of resin. Breakthrough curves were recorded from each single component as well as of mixtures thereof. Finally, the resin was used for the sampling of amines evaporating from PU foams applied in buildings. Further information about time dependent concentration profiles were obtained using a combination of GC-MS and Fourier transform IR spectroscopy.

Application of 2-chlorotrityl resin in solid phase synthesis of (Leu15)-gastrin I and unsulfated cholecystokinin octapeptide. Selective O-deprotection of tyrosine.

PubMed

Barlos, K; Gatos, D; Kapolos, S; Poulos, C; Schäfer, W; Yao, W Q

1991-12-01

The carboxyl terminal dipeptide amide, Fmoc-Asp-Phe-NH2, of gastrin and cholecystokinin (CCK) has been attached in high yield through its free side chain carboxyl group to the acid labile 2-chlorotrityl resin. The obtained peptide resin ester has been applied in the solid phase synthesis of partially protected (Leu15)-gastrin I utilising Fmoc-amino acids. Quantitative cleavage of this peptide from resin, with the t-butyl type side chain protection intact is achieved using mixtures of acetic acid/trifluoroethanol/dichloromethane. Under the same conditions complete detritylation of the tyrosine phenoxy function occurs simultaneously. Thus, the solid-phase synthesis of peptides selectively deprotected at the side chain of tyrosine is rendered possible by the use of 2-chlorotrityl resin and Fmoc-Tyr(Trt)-OH. The efficiency of this approach has been proved by the subsequent high-yield synthesis of three model peptides and the CCK-octapeptide.

Advances in developing alternative treatments for postharvest pest control

USDA-ARS?s Scientific Manuscript database

USDA-ARS made two significant advances in the last 10 years in the development of alternative treatments for postharvest pest control: oxygenated phosphine fumigation and nitric oxide fumigation. Oxygenated phosphine is phosphine fumigation in an oxygen enriched atmosphere. It is significantly more...

Convenient synthesis and diversification of dehydroalaninyl phosphinic peptide analogues.

PubMed

Matziari, M; Georgiadis, D; Dive, V; Yiotakis, A

2001-03-08

[structure: see text]. Dehydroalaninyl phosphinic dipeptide analogues were synthesized, via an efficient tandem Arbuzov addition/allylic rearrangement, in high yields. The susceptibility of the conjugate system to 1,4 nucleophilic additions was investigated. C-Elongation of the dipeptides was performed, and the efficiency of 1,4 addition to the resulting acrylamidic moiety was evaluated. Derivatization of such phosphinic templates is a powerful approach for rapid access to large number of phosphinic pseudopeptides bearing various side chains in the P1' position.

Action of phosphine on production of aflatoxins by various Aspergillus strains isolated from foodstuffs.

PubMed Central

Leitao, J; de Saint-Blanquat, G; Bailly, J R

1987-01-01

Phosphine is a food fumigant, used until now as an insecticide and rodenticide. The present work researches the action of phosphine treatment on growth and aflatoxin production of 23 Aspergillus strains. Production of aflatoxins B1, B2, G1, and G2 decreased in almost all cases by a ratio of 10 to 100. Phosphine treatment therefore seems favorable to prevent growth of various Aspergillus strains, in the context of keeping food safe. PMID:3426212

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

PubMed

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

2011-01-01

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

Humic Acid Isolations from Lignite by Ion Exchange Method

NASA Astrophysics Data System (ADS)

Kurniati, E.; Muljani, S.; Virgani, D. G.; Neno, B. P.

2018-01-01

The humic liquid is produced from lignite extraction using alkali solution. Conventional humic acid is obtained by acidifying a humic solution using HCl. The purpose of this research is the formation of solid humic acid from lignite by ion exchange method using cation resin. The results showed that the addition of cation resin was able to reduce the pH from 14 to pH 2 as well as the addition of acid (HCl), indicating the exchange of Na + ions with H + ions. The reduction of pH in the humic solution is influenced by the concentration of sodium ions in the humic solution, the weight of the cation resin, and the ion exchange time. The IR spectra results are in good agreement for humic acid from lignite characterization.

Analysis of diterpenoic compounds in natural resins applied as binders in museum objects by capillary electrophoresis.

PubMed

Findeisen, Anna; Kolivoska, Viliam; Kaml, Isabella; Baatz, Wolfgang; Kenndler, Ernst

2007-07-20

The exudates of conifers consist mainly of diterpenoic acids of the abietane and pimarane type (abietic, neoabietic, dehydroabietic, palustric, pimaric, isopimaric, levopimaric and sandaracopimaric acid) and larixol acetate. These natural resins were used as adhesives, coatings, varnishes or plasticizers in artistic and historic works since ancient times. For the purpose of conservation and restoration and for art historic examination of such museum objects the identification of the binding media used is undoubtedly of paramount importance. In the present paper, the characterization of these resins based on the pattern of their diterpenoid constituents is carried out by capillary electrophoresis. For separation a background electrolyte which has been initially introduced for the analysis of chlorinated and natural resin acids in waste water was modified and the experimental conditions were adjusted in terms of resolution and analysis time. Separation was carried out in borate buffer at pH 9.25 (ionic strength 20 mmol L(-1)) with methyl-beta-cyclodextrin and sulfobutylether-beta-cyclodextrin as additives to increase selectivity and enhance the solubility of the analytes. With this electrophoretic system the resin acids of interest and larixol acetate--all as anionic cyclodextrin complexes--were separated within 5 min and detected at 200, 250 and 270 nm with a diode array detector. The electrophoretic patterns served for the characterisation of the relevant diterpenoic resins, balsams and copals. Sample pre-treatment was limited to sonication in methanol at 55 degrees C for 30 min. This enables the identification of the resins in mixtures with other binders like plant gums, animal glues or drying oils, even when these media are present in excess. Colophony was identified as resinous constituent of a modelling mass for gilded frames originating from the 19th century.

Chemical Characterization of Beer Aging Products Derived from Hard Resin Components in Hops (Humulus lupulus L.).

PubMed

Taniguchi, Yoshimasa; Yamada, Makiko; Taniguchi, Harumi; Matsukura, Yasuko; Shindo, Kazutoshi

2015-11-25

The bitter taste of beer originates from resins in hops (Humulus lupulus L.), which are classified into two subtypes (soft and hard). Whereas the nature and reactivity of soft-resin-derived compounds, such as α-, β-, and iso-α-acids, are well studied, there is only a little information on the compounds in hard resin. For this work, hard resin was prepared from stored hops and investigated for its compositional changes in an experimental model of beer aging. The hard resin contained a series of α-acid oxides. Among them, 4'-hydroxyallohumulinones were unstable under beer storage conditions, and their transformation induced primary compositional changes of the hard resin during beer aging. The chemical structures of the products, including novel polycyclic compounds scorpiohumulinols A and B and dicyclohumulinols A and B, were determined by HRMS and NMR analyses. These compounds were proposed to be produced via proton-catalyzed cyclization reactions of 4'-hydroxyallohumulinones. Furthermore, they were more stable than their precursor 4'-hydroxyallohumulinones during prolonged storage periods.

Biomolecule conjugation strategy using novel water-soluble phosphine-based chelating agents

DOEpatents

Katti, Kattesh V.; Gali, Hariprasad; Volkert, Wynn A.

2004-08-24

This invention describes a novel strategy to produce phosphine-functionalized biomolecules (e.g. peptides or proteins) for potential use in the design and development of site-specific radiopharmaceuticals for diagnosis or therapy of specific cancers. Hydrophilic alkyl phosphines, in general, tend to be oxidatively unstable. Therefore, incorporation of such phosphine functionalities on peptide (and other biomolecule) backbones, without oxidizing the P.sup.III centers, is difficult. In this context this discovery reports on a new technology by which phosphines, in the form of bifunctional chelating agents, can be directly incorporated on biomolecular backbones using manual synthetic or solid phase peptide synthesis methodologies. The superior ligating abilities of phosphine ligands, with various diagnostically (e.g. TC-99m) or therapeutically (e.g. Re186/188, Rh-105, Au-199) useful radiometals, coupled with the findings that the resulting complexes demonstrate high in vivo stability makes this approach useful in the development of radiolabeled biomolecules for applications in the design of tumor-specific radiopharmaceuticals.

Building new discrete supramolecular assemblies through the interaction of iso-tellurazole N-oxides with Lewis acids and bases.

PubMed

Ho, Peter C; Jenkins, Hilary A; Britten, James F; Vargas-Baca, Ignacio

2017-10-13

The supramolecular macrocycles spontaneously assembled by iso-tellurazole N-oxides are stable towards Lewis bases as strong as N-heterocyclic carbenes (NHC) but readily react with Lewis acids such as BR 3 (R = Ph, F). The electron acceptor ability of the tellurium atom is greatly enhanced in the resulting O-bonded adducts, which consequently enables binding to a variety of Lewis bases that includes acetonitrile, 4-dimethylaminopyridine, 4,4'-bipyridine, triphenyl phosphine, a N-heterocyclic carbene and a second molecule of iso-tellurazole N-oxide.

Automated Desalting Apparatus

NASA Technical Reports Server (NTRS)

Spencer, Maegan K.; Liu, De-Ling; Kanik, Isik; Beegle, Luther

2010-01-01

Because salt and metals can mask the signature of a variety of organic molecules (like amino acids) in any given sample, an automated system to purify complex field samples has been created for the analytical techniques of electrospray ionization/ mass spectroscopy (ESI/MS), capillary electrophoresis (CE), and biological assays where unique identification requires at least some processing of complex samples. This development allows for automated sample preparation in the laboratory and analysis of complex samples in the field with multiple types of analytical instruments. Rather than using tedious, exacting protocols for desalting samples by hand, this innovation, called the Automated Sample Processing System (ASPS), takes analytes that have been extracted through high-temperature solvent extraction and introduces them into the desalting column. After 20 minutes, the eluent is produced. This clear liquid can then be directly analyzed by the techniques listed above. The current apparatus including the computer and power supplies is sturdy, has an approximate mass of 10 kg, and a volume of about 20 20 20 cm, and is undergoing further miniaturization. This system currently targets amino acids. For these molecules, a slurry of 1 g cation exchange resin in deionized water is packed into a column of the apparatus. Initial generation of the resin is done by flowing sequentially 2.3 bed volumes of 2N NaOH and 2N HCl (1 mL each) to rinse the resin, followed by .5 mL of deionized water. This makes the pH of the resin near neutral, and eliminates cross sample contamination. Afterward, 2.3 mL of extracted sample is then loaded into the column onto the top of the resin bed. Because the column is packed tightly, the sample can be applied without disturbing the resin bed. This is a vital step needed to ensure that the analytes adhere to the resin. After the sample is drained, oxalic acid (1 mL, pH 1.6-1.8, adjusted with NH4OH) is pumped into the column. Oxalic acid works as a chelating reagent to bring out metal ions, such as calcium and iron, which would otherwise interfere with amino acid analysis. After oxalic acid, 1 mL 0.01 N HCl and 1 mL deionized water is used to sequentially rinse the resin. Finally, the amino acids attached to the resin, and the analytes are eluted using 2.5 M NH4OH (1 mL), and the NH4OH eluent is collected in a vial for analysis.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lai, Yuet Fan

1977-10-01

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

Regeneration of strong-base anion-exchange resins by sequential chemical displacement

DOEpatents

Brown, Gilbert M.; Gu, Baohua; Moyer, Bruce A.; Bonnesen, Peter V.

2002-01-01

A method for regenerating strong-base anion exchange resins utilizing a sequential chemical displacement technique with new regenerant formulation. The new first regenerant solution is composed of a mixture of ferric chloride, a water-miscible organic solvent, hydrochloric acid, and water in which tetrachloroferrate anion is formed and used to displace the target anions on the resin. The second regenerant is composed of a dilute hydrochloric acid and is used to decompose tetrachloroferrate and elute ferric ions, thereby regenerating the resin. Alternative chemical displacement methods include: (1) displacement of target anions with fluoroborate followed by nitrate or salicylate and (2) displacement of target anions with salicylate followed by dilute hydrochloric acid. The methodology offers an improved regeneration efficiency, recovery, and waste minimization over the conventional displacement technique using sodium chloride (or a brine) or alkali metal hydroxide.

SEPARATION OF BARIUM VALUES FROM URANYL NITRATE SOLUTIONS

DOEpatents

Tompkins, E.R.

1959-02-24

The separation of radioactive barium values from a uranyl nitrate solution of neutron-irradiated uranium is described. The 10 to 20% uranyl nitrate solution is passed through a flrst column of a cation exchange resin under conditions favoring the adsorption of barium and certain other cations. The loaded resin is first washed with dilute sulfuric acid to remove a portion of the other cations, and then wash with a citric acid solution at pH of 5 to 7 to recover the barium along with a lesser amount of the other cations. The PH of the resulting eluate is adjusted to about 2.3 to 3.5 and diluted prior to passing through a smaller second column of exchange resin. The loaded resin is first washed with a citric acid solution at a pH of 3 to elute undesired cations and then with citric acid solution at a pH of 6 to eluts the barium, which is substantially free of undesired cations.

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

PubMed

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

2016-01-15

The effect of the molecular weight of polyethyleneimine (PEI), defined as a compound having two or more ethyleneamine units, and of its carboxymethylation rate (CM/N), represented by the ratio of ion-exchange capacity to the amount of N on the resin, on the selective solid-phase extraction ability of the chelating resin immobilizing carboxymethylated (CM) PEI was investigated. The chelating resins (24 types) were prepared by immobilization of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenehexamine, PEI300 (MW=ca. 300), and PEI600 (MW=ca. 600) on methacrylate resins, followed by carboxymethylation with various amounts of sodium monochloroacetate. When resins with approximately the same CM/N ratio (0.242-0.271) were used, the recovery of Cd, Co, Cu, Fe, Ni, Pb, Ti, Zn, and alkaline earth elements increased with increasing the molecular weight of PEIs under acidic and weakly acidic conditions; however, the extraction behavior of Mo and V was only slightly affected. This was probably due to the increase in N content of the resin, resulting in an increase in carboxylic acid groups; the difference in the molecular weight of PEIs immobilized on the resin exerts an insignificant influence on the selective extraction ability. The CM/N ratio considerably affected the extraction behavior for various elements. Under acidic and neutral conditions, the recovery of Cd, Co, Cu, Fe, Ni, Pb, Ti, and Zn increased with increasing CM/N values. However, under these conditions, the recovery of alkaline earth elements was considerably low when a resin with low CM/N ratio was used. This is presumably attributed to the different stability constants of the complexes of these elements with aminocarboxylic acids and amines, and to the electrostatic repulsion between the elements and the protonated amino groups in the CM-PEI. The recovery of Mo and V decreased or varied with increasing CM/N values, suggesting that the extraction of these elements occurred mainly by the anion-exchange reaction. For the separation and preconcentration of trace elements in samples containing large amounts of alkali and alkaline earth elements, the CM-PEI600 resin with CM/N=0.131 (Cu(II) extraction capacity, 0.37mmol g(-)(1)) was found to be the most suitable because it scarcely extracts alkali and alkaline earth elements under acidic and neutral conditions. This resin proved to be convenient for separating and preconcentrating Cd, Co, Cu, Fe, Mn, Mo, Ni, Pb, V, and Zn in the certified reference materials (EnviroMAT EU-L-1 wastewater and ES-L-1 ground water) and commercially available table salt. Copyright © 2015 Elsevier B.V. All rights reserved.

Bonding efficacy of new self-etching, self-adhesive dual-curing resin cements to dental enamel.

PubMed

Benetti, Paula; Fernandes, Virgílio Vilas; Torres, Carlos Rocha; Pagani, Clovis

2011-06-01

This study evaluated the efficacy of the union between two new self-etching self-adhesive resin cements and enamel using the microtensile bond strength test. Buccal enamel of 80 bovine teeth was submitted to finishing and polishing with metallographic paper to a refinement of #600, in order to obtain a 5-mm2 flat area. Blocks (2 x 4 x 4 mm) of laboratory composite resin were cemented to enamel according to different protocols: (1) untreated enamel + RelyX Unicem cement (RX group); (2) untreated enamel + Bifix SE cement (BF group); (3) enamel acid etching and application of resin adhesive Single Bond + RelyX Unicem (RXA group); (4) enamel acid etching and application of resin adhesive Solobond M + Bifix SE (BFA group). After 7 days of storage in distillated water at 37°C, the blocks were sectioned for obtaining microbar specimens with an adhesive area of 1 mm2 (n = 120). Specimens were submitted to the microtensile bond strength test at a crosshead speed of 0.5 mm/min. The results (in MPa) were analyzed statistically by ANOVA and Tukey's test. Enamel pre-treatment with phosphoric acid and resin adhesive (27.9 and 30.3 for RXA and BFA groups) significantly improved (p ≤ 0.05) the adhesion of both cements to enamel compared to the union achieved with as-polished enamel (9.9 and 6.0 for RX and BF). Enamel pre-treatment with acid etching and the application of resin adhesive significantly improved the bond efficacy of both luting agents compared to the union achieved with as-polished enamel.

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

PubMed

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

2003-05-16

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

Synthesis and properties of hydroxy acrylic resin with high solid content

NASA Astrophysics Data System (ADS)

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.

Method for the purification of bis (2-ethyl-hexyl)phosphoric acid

DOEpatents

Schulz, W.W.

1974-02-19

Foreign products including the neutral organophosphorous compounds and the iron salts normally present in commercial bis(2ethyl-hexyl) phosphoric acid(HDEHP), and the radiolytic degradation products of HDEHP on exposure of HDEHP to beta and gamma irradiation are removed from HDEHP containing one or more of such products by contacting the said foreign product containing HDEHP with a macroreticular anion exchange resin in base form whereby the DEHP- ion of HDEHP exchanges with the anion of the resin and is thus adsorbed on the resin and the said foreign products are not adsorbed and will pass through a bed of particles of the resin. The adsorbed DEHP- ion is then eluted from the resin and acidified to form and recover the purified HDEHP. (auth)

SURFACE DEGRADATION OF COMPOSITE RESINS BY ACIDIC MEDICINES AND pH-CYCLING

PubMed Central

Valinoti, Ana Carolina; Neves, Beatriz Gonçalves; da Silva, Eduardo Moreira; Maia, Lucianne Cople

2008-01-01

This study evaluated the effects of acidic medicines (Dimetapp® and Claritin®), under pH-cycling conditions, on the surface degradation of four composite resins (microhybrid: TPH, Concept, Opallis and Nanofilled: Supreme). Thirty disc-shaped specimens (Ø = 5.0 mm / thickness = 2.0 mm) of each composite were randomly assigned to 3 groups (n = 10): a control and two experimental groups, according to the acidic medicines evaluated. The specimens were finished and polished with aluminum oxide discs, and the surface roughness was measured by using a profilometer. After the specimens were submitted to a pH-cycling regimen and immersion in acidic medicines for 12 days, the surface roughness was measured again. Two specimens for each material and group were analyzed by scanning electron microscopy (SEM) before and after pH-cycling. Data were analyzed by the Student's-t test, ANOVA, Duncan's multiple range test and paired t-test (α=0.05). Significant increase in roughness was found only for TPH in the control group and TPH and Supreme immersed in Claritin® (p<0.05). SEM analyses showed that the 4 composite resins underwent erosion and surface degradation after being subjected to the experimental conditions. In conclusion, although the roughness was slightly affected, the pH-cycling and acidic medicines caused surface degradation of the composite resins evaluated. Titratable acidity seemed to play a more crucial role on surface degradation of composite resins than pH. PMID:19089257

A very simple, highly stereoselective and modular synthesis of ferrocene-based P-chiral phosphine ligands.

PubMed

Chen, Weiping; Mbafor, William; Roberts, Stanley M; Whittall, John

2006-03-29

A very simple, highly stereoselective and modular synthesis of ferrocene-based P-chiral phosphine ligands has been developed. On the basis of this new methodology, several new families of ferrocene-based phosphine ligands have been prepared coupling chirality at phosphorus with other, more standard stereogenic features. The introduction of P-chirality into ferrocene-based phosphine ligands enhances the enantioselective discrimination produced by the corresponding Rh catalyst when a matching among the planar chirality, carbon chirality, and the chirality of phosphorus is achieved.

Sustainable Phosphorus Chemistry: A Silylphosphide Synthon for the Generation of Value-Added Phosphorus Chemicals.

PubMed

Slootweg, J Chris

2018-05-07

Avoiding white phosphorus: Cummins and Geeson have recently described the conversion of phosphoric acid into the novel bis(trichlorosilyl)phosphide anion, which serves as a key intermediate in the synthesis of organophosphines, hexafluorophosphate, and phosphine gas in a reaction sequence that does not rely on white phosphorus. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

ELUTION OF URANIUM VALUES FROM ION EXCHANGE RESINS

DOEpatents

Kennedy, R.H.

1959-11-24

A process is described for eluting complex uranium ions absorbed on ion exchange resins. The resin is subjected to the action of an aqueous eluting solution contuining sulfuric acid and an alkali metal, ammonium, or magnesium chloride or nitrate, the elution being carried out until the desired amount of the uranium is removed from the resin.

Preventive effect of fluoridated orthodontic resins subjected to high cariogenic challenges.

PubMed

Passalini, Paula; Fidalgo, Tatiana Kelly da Silva; Caldeira, Erika Machado; Gleiser, Rogerio; Nojima, Matilde da Cunha Gonçalves; Maia, Lucianne Cople

2010-01-01

The aim of the present study was to evaluate the in vitro caries preventive effect of fluoridated orthodontic resins under pH cycling with two types of acid demineralizing saliva. Brackets were bonded to 60 bovine incisors, using either Transbond Plus Color Change (n=30) or Orthodontic Fill Magic (n=30) orthodontic resins. Each group of resin was divided into 3 subgroups (n=10): immersion in remineralizing artificial saliva for 14 days, pH cycling with high cariogenic challenge in acid saliva with pH 5.5, and acid saliva with pH 4.5. After 14 days of pH cycling, the caries preventive effect on the development of white spot lesion was evaluated considering the presence of inhibition zones to white spot lesions using two scores: 0= absence and 1= presence. Kruskal Wallis and Mann-Whitney tests (a=0.05) were used. Formation of white spot lesions was observed only under pH cycling using acid saliva with pH 4.5; with Transbond Plus Color Change being significantly more effective (p<0.05) in preventing the appearance of white spot lesions effect than Orthodontic Fill Magic. The acidity of the demineralizing solution influenced the formation of white spot lesions around orthodontic brackets under highly cariogenic conditions. Transbond Plus Color Change resin presented higher caries preventive effect than Orthodontic Fill Magic.

Low-Temperature Fumigation of Harvested Lettuce Using a Phosphine Generator.

PubMed

Liu, Yong-Biao

2018-02-28

A research-scale phosphine generator, QuickPHlo-R, from United Phosphorus Ltd. (Mumbai, India) was tested to determine whether it was suitable for low-temperature fumigation and oxygenated phosphine fumigation of harvested lettuce. Vacuum cooled Iceberg and Romaine lettuce (Lactuca sativa) were fumigated in 442-liter chambers at 2°C for 24 and 72 h for control of western flower thrips [Frankliniella occidentalis (Pergande) (Thysanoptera: Thripidae)] and lettuce aphid [Nasonovia ribisnigri (Mosely) (Homoptera: Aphididae)]. Oxygenated phosphine fumigation for 48 h under 60% O2 was also conducted at 2°C with Iceberg and Romaine lettuce for control of lettuce aphid. The generator completed phosphine generation in 60-90 min. Complete control of western flower thrips was achieved in 24-h treatment, and the 48-h oxygenated fumigation, and 72-h regular fumigation treatments completely controlled lettuce aphid. Lettuce quality was evaluated 14 d after fumigation. There was increased incidence of brown stains on fumigated Iceberg lettuce, and the increases were more obvious in longer (≥48 h) treatments. Both Iceberg and Romaine lettuce from all treatments and controls had good visual quality even though there was significantly higher brown stain incidence on fumigated Iceberg lettuce in ≥48-h treatment and significant differences in quality score for both Iceberg and Romaine lettuce in the 72-h treatment. The brown stains were likely due to the high sensitivity of lettuce to carbon dioxide. The study indicated that QuiPHlo-R phosphine generator has potential in low-temperature phosphine fumigation due to the quick establishment of desired phosphine levels, efficacy in pest control, and reasonable safety to product quality.

Ion exchange treatment of rinse water generated in the galvanizing process.

PubMed

Marañón, Elena; Fernández, Yolanda; Castrillón, Leonor

2005-01-01

A study was conducted of the viability of using the cationic exchange resins Amberlite IR-120 and Lewatit SP-112 to treat rinse water generated in the galvanizing process as well as acidic wastewater containing zinc (Zn) and iron (Fe). Solutions containing either 100 mg/L of Zn at pH 5.6 (rinse water) or Fe and Zn at concentrations of 320 and 200 mg/L at pH 1.5 (acidic water), respectively, were percolated through packed beds until the resins were exhausted. Breakthrough capacities obtained ranged between 1.1 and 1.5 meq metal/mL resin. The elution of metal and the regeneration of resins were performed with hydrochloric acid. The influence of the flowrate used during the loading stage was also studied, with 0.5 bed volumes/min (3.2 cm/min) found to be the optimum flowrate.

Preparation of phosphines through C–P bond formation

PubMed Central

Wauters, Iris; Debrouwer, Wouter

2014-01-01

Summary Phosphines are an important class of ligands in the field of metal-catalysis. This has spurred the development of new routes toward functionalized phosphines. Some of the most important C–P bond formation strategies were reviewed and organized according to the hybridization of carbon in the newly formed C–P bond. PMID:24991257

Effect of Silanization on Microtensile Bond Strength of Different Resin Cements to a Lithium Disilicate Glass Ceramic.

PubMed

Gré, Cristina Parise; de Ré Silveira, Renan C; Shibata, Shizuma; Lago, Carlo Tr; Vieira, Luiz Cc

2016-02-01

This study evaluated the influence of a silane-coupling agent on the bond strength of a self-adhesive cement and a conventional resin cement to a lithium disilicate glass ceramic. A total of eight ceramic blocks were fabricated and divided into four groups (n = 2). In groups 1 and 3, ceramic surfaces were etched with hydrofluoric acid 10% for 20 seconds, rinsed for 30 seconds, and air-dried. One layer of a silane agent was applied onto all ceramic specimens and air-dried for 30 seconds. In groups 2 and 4, ceramic surfaces were etched with hydrofluoric acid, rinsed, and air-dried without application of the silane-coupling agent. The ceramic blocks were bonded to a block of composite with a self-adhesive resin cement or with a conventional resin cement, according to the manufacturer's instructions. After 24 hours in distilled water at 37°C, the specimens were sectioned perpendicular to the bonding interface area to obtain beams with a bonding area of 0.8 mm(2) and submitted to a microtensile bond strength test at a crosshead speed of 0.5 mm/min. Data were statistically analyzed with one-way analysis of variance and the Games-Howell post hoc test (p = 0.05). Fractured specimens were examined under optical microscopy at 40x magnification. Silanization resulted in higher microtensile bond strength compared to groups without silane. No significant differences were found between the conventional resin cement and the self-adhesive resin cement with silane agent (p = 0.983), and without silane agent (p = 0.877). Silanization appears to be crucial for resin bonding to a lithium disilicate-based ceramic, regardless of the resin cement used. The self-adhesive resin cement performed as well as the conventional resin cement. Applying one layer of a silane-coupling agent after etching the ceramic surface with hydrofluoric acid 10% enhanced the bond strength between resin cements and a glass ceramic.

Study on the removal of iron impurities in methanesulfonic acid tin plating bath

NASA Astrophysics Data System (ADS)

Hou-li, LIU; Jian-Jun, CHEN; Hong-Liang, PAN

2018-03-01

This thesis investigated the the influence of sodium sulfite as reducing agent on the recovery rate of tin ion. The approach is that HZ016 type cation exchange resin was used to adsorb Sn2+ and Fe2+ in electroplated tin solution first. After adsorption, the resin was removed by sulfuric acid, which was added with NaOH to adjust pH value to form precipitation and separate tin. X-ray diffraction (XRD) and energy spectrum (EDS) method were used to analyze the composition of the precipitates adjusted by pH. The results show that when the mass ratio of resin to bath is 1:2, the adsorption efficiency of resin reaches 98.3% and 97.1% respectively, and the elution efficiency of tin and iron reaches 95.1% and 94% respectively when the mass ratio of resin to eluent sulfuric acid is 1:4. Sodium sulfite was added to increase the efficiency of tin recovery by 8.1%. EDS and XRD atlas showed that after pH regulation, the main composition of the filtration precipitation was the hydroxides of tin.

Interaction of some extreme-pressure type lubricating compounds with an iron surface

NASA Technical Reports Server (NTRS)

Buckley, D. H.

1973-01-01

An iron surface was exposed to the extreme-pressure type lubricant benzyl chloride, dichlorophenyl phosphine, dichlorophenyl phosphine sulfide, ophenyl phosphine oxide. Iron, in the sputter-cleaned state, was exposed to these materials statically and during dynamic friction experiments. With benzyl chloride only chlorine adsorbed to the surface, and with dichlorophenyl phosphine no adsorption occurred, while the addition of sulfur to that same molecular structure resulted in the promotion of carbon and chlorine adsorption. substitution of oxygen for sulfur in the dichlorobenzyl phosphine molecule resulted in carbon, chlorine, and oxygen adsorption. With none of the phosphorus containing molecules was phosphorus detected on the surface. Sliding in an atmosphere of benzyl chloride promoted adsorption of chlorine to the iron surface. Increases in load resulted in a decrease in the surface concentration of iron chloride.

Mysteries of TOPSe revealed: insights into quantum dot nucleation.

PubMed

Evans, Christopher M; Evans, Meagan E; Krauss, Todd D

2010-08-18

We have investigated the reaction mechanism responsible for QD nucleation using optical absorption and nuclear magnetic resonance spectroscopies. For typical II-VI and IV-VI quantum dot (QD) syntheses, pure tertiary phosphine selenide sources (e.g., trioctylphosphine selenide (TOPSe)) were surprisingly found to be unreactive with metal carboxylates and incapable of yielding QDs. Rather, small quantities of secondary phosphines, which are impurities in tertiary phosphines, are entirely responsible for the nucleation of QDs; their low concentrations account for poor synthetic conversion yields. QD yields increase to nearly quantitative levels when replacing TOPSe with a stoiciometric amount of a secondary phosphine chalcogenide such as diphenylphosphine selenide. Based on our observations, we have proposed potential monomer identities, reaction pathways, and transition states and believe this mechanism to be universal to all II-VI and IV-VI QDs synthesized using phosphine based methods.

Mysteries of TOPSe Revealed: Insights into Quantum Dot Nucleation

PubMed Central

Evans, Christopher M.; Evans, Meagan E.

2010-01-01

We have investigated the reaction mechanism responsible for QD nucleation using optical absorption and nuclear magnetic resonance spectroscopies. For typical II-VI and IV-VI quantum dot (QD) syntheses, pure tertiary phosphine selenide sources (e.g. trioctylphosphine selenide (TOPSe)) were surprisingly found to be unreactive with metal carboxylates and incapable of yielding QDs. Rather, small quantities of secondary phosphines, which are impurities in tertiary phosphines, are entirely responsible for the nucleation of QDs; their low concentrations account for poor synthetic conversion yields. QD yields increase to nearly quantitative levels when replacing TOPSe with a stoiciometric amount of a secondary phosphine chalcogenide such as diphenylphosphine selenide. Based on our observations, we have proposed potential monomer identities, reaction pathways and transition states, and believe this mechanism to be universal to all II-VI and IV-VI QDs synthesized using phosphine based methods. PMID:20698646

Affinity resins as new tools for identifying target proteins of ascorbic acid.

PubMed

Iwaoka, Yuji; Nishino, Kohei; Ishikawa, Takahiro; Ito, Hideyuki; Sawa, Yoshihiro; Tai, Akihiro

2018-02-12

l-Ascorbic acid (AA) has diverse physiological functions, but little is known about the functional mechanisms of AA. In this study, we synthesized two types of affinity resin on which AA is immobilized in a stable form to identify new AA-targeted proteins, which can provide important clues for elucidating unknown functional mechanisms of AA. To our knowledge, an affinity resin on which AA as a ligand is immobilized has not been prepared, because AA is very unstable and rapidly degraded in an aqueous solution. By using the affinity resins, cytochrome c (cyt c) was identified as an AA-targeted protein, and we showed that oxidized cyt c exhibits specific affinity for AA. These results suggest that two kinds of AA-affinity resin can be powerful tools to identify new target proteins of AA.

Affinity purification of the voltage-sensitive sodium channel from electroplax with resins selective for sialic acid

DOE Office of Scientific and Technical Information (OSTI.GOV)

James, W.M.; Emerick, M.C.; Agnew, W.S.

1989-07-11

The voltage-sensitive sodium channel present in the eel (Electrophorus electricus) has an unusually high content of sialic acid, including {alpha}-(2{yields}8)-linked polysialic acid, not found in other electroplax membrane glycopeptides. Lectins from Limax flavus (LFA) and wheat germ (WGA) proved the most effective of 11 lectin resins tried. The most selective resin was prepared from IgM antibodies against Neisseria meningitidis {alpha}-(2{yields}8)-polysialic acid which were affinity purified and coupled to Sepharose 4B. The sodium channel was found to bind to WGA, LFA, and IgM resins and was readily eluted with the appropriate soluble carbohydrates. Experiments with LFA and IgM resins demonstrated bindingmore » and unbinding rates and displacement kinetics, which suggest highly specific binding at multiple sites on the sodium channel protein. In preparative-scale purification of protein previously fractionated by anion-exchange chromatography, without stabilizing TTX, high yields were reproducibly obtained. Further, when detergent extracts were prepared from electroplax membranes fractionated by low-speed sedimentation, a single step over the IgM resin provided a 70-fold purification, yielding specific activities of 3,200 pmol of ({sup 3}H)TTX-binding sites/mg of protein and a single polypeptide of {approximately}285,000 Da on SDS-acrylamide gels. No small peptides were observed after this 5-h isolation. The authors describe a cation-dependent stabilization with millimolar levels of monovalent and micromolar levels of divalent species.« less

Zinc incorporation improves biological activity of beta-tricalcium silicate resin-based cement.

PubMed

Osorio, Raquel; Yamauti, Monica; Sauro, Salvatore; Watson, Tim F; Toledano, Manuel

2014-11-01

Matrix metalloproteinase (MMP) inhibition may improve endodontic treatment prognosis. The purpose of this study was to determine if zinc incorporation into experimental resin cements containing bioactive fillers may modulate MMP-mediated collagen degradation of dentin. Human dentin samples untreated and demineralized using 10% phosphoric acid or 0.5 mol/L EDTA were infiltrated with the following experimental resins: (1) unfilled resin, (2) resin with Bioglass 45S5 particles (OSspray, London, UK), (3) resin with beta-tricalcium silicate particles (βTCS), (4) resin with zinc-doped Bioglass 45S5, and (5) resin with zinc-doped βTCS particles. The specimens were stored in artificial saliva (for 24 hours, 1 week, and 4 weeks) and submitted to radioimmunoassay to quantify C-terminal telopeptide. Scanning electron microscopy analysis was also undertaken on dentin samples after 4 weeks of storage. Collagen degradation was prominent both in phosphoric acid and EDTA-treated dentin. Resin infiltration strongly reduced MMP activity in demineralized dentin. Resin containing Bioglass 45S5 particles exerted higher and stable protection of collagen. The presence of zinc in βTCS particles increases MMP inhibition. Different mineral precipitation was attained in dentin infiltrated with the resin cements containing bioactive fillers. MMP degradation of dentin collagen is strongly reduced after resin infiltration of dentin. Zinc incorporation in βTCS particles exerted an additional protection against MMP-mediated collagen degradation. However, it did not occur in resin containing Bioglass 45S5 particles, probably because of the formation of phosphate-zinc compounds. Copyright © 2014 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

The Mutagenic Potential of 4 nitrophenyl bis(2-thienyl)-phosphinate; 4-nitrophenyl 2-furyl(methyl)-phosphinates; 4-cyanophenyl bis(2-furyl)-phosphinate; 4-nitrophenyl bis(2-furyl)-phosphinate.

DTIC Science & Technology

1981-09-01

by an enzymatic process, a mammalian microsome system is incorporated. These microsomal enzymes are obtained from livers of rats induced with Aroclor...1254; the enzymes allow for the expression of the metabolites in the mammalian system. This activated rat liver microsomal enzyme homogenate is termed...C) NOME== - - c.J ~ -C) (n in C).*0 ’ r- 0 -0 -. -. : - kz ’.01. -C- - , C) ~~i - - o C40--. C) - ~ flj- ~ - - ~C) -* oj co 00 -r- -j P.. -C ’ opC

Asymmetric conjugate 1,4-addition of arylboronic acids to alpha, beta-unsaturated esters catalyzed by Rhodium(I)/(S)-binap

PubMed

Sakuma; Sakai; Itooka; Miyaura

2000-09-22

Arylboronic acids underwent the conjugate 1,4-addition to alpha, beta-unsaturated esters to give beta-aryl esters in high yields in the presence of a rhodium(I) catalyst. The addition of arylboronic acids to isopropyl crotonate resulted in high yields and high enantioselectivity exceeding 90% ee in the presence of 3 mol % of Rh(acac)(C(2)H(4))(2) and (S)-binap at 100 degrees C. The rhodium/(S)-binap complex provided (R)-3-phenylbutanoate in the addition of phenylboronic acid to benzyl crotonate. The effects on the enantioselectivity of chiral phosphine ligands, rhodium precursors, and substituents on alpha,beta-unsaturated esters are discussed, as well as the mechanistic aspect of the catalytic cycle.

Tensile bond strength of an aged resin composite repaired with different protocols.

PubMed

Celik, Esra Uzer; Ergücü, Zeynep; Türkün, L Sebnem; Ercan, Utku Kürșat

2011-08-01

To evaluate the effect of different surface treatments and bonding procedures on the tensile bond strength (TBS) of resin composites repaired 6 months after polymerization. Resin composite sticks were aged in distilled water at 37°C for 6 months. They were divided into 12 groups (n = 10) according to the combination of surface treatment/bonding procedures [none, only bur treatment, XP Bond (XPB/Dentsply/DeTrey) with/without bur, AdheSE (A-SE/Ivoclar/Vivadent) with/without bur, Composite Primer (CP/GC) with/without bur, CP after bur and acid-etching, XPB after acid etching and CP with bur, A-SE after bur and CP]. The ultimate tensile bond strength (UTS) of the resin composites was tested in intact but aged specimens. Tensile bond strengths were tested with a universal testing machine (Shimadzu). Data were analyzed using one-way ANOVA and Duncan Multiple Comparisons tests (p < 0.05). All repaired groups showed significantly higher TBS than the group without any sureface treatment (p < 0.05). Four groups resulted in TBS similar to those of intact resin composite UTS: A-SE, A-SE with bur, A-SE after CP with bur, and XPB after acid etching+CP with bur. Bur treatment, silane primer or etch-and-rinse adhesive application alone were not successful in the repair process of aged resin composite, whereas self-etching adhesive alone showed similar performance to the intact specimens. Combined procedures generally showed better performance: A-SE with bur, A-SE after CP with bur, and XPB after acid etching +CP with bur showed TBS similar to those of the intact specimens. It was concluded that bur roughening of the surfaces and rebonding procedures were essential for repairing aged resin composites.

Low dielectric polyimide fibers

NASA Technical Reports Server (NTRS)

Dorogy, William E., Jr. (Inventor); St.clair, Anne K. (Inventor)

1994-01-01

A high temperature resistant polyimide fiber that has a dielectric constant of less than 3 is presented. The fiber was prepared by first reacting 2,2-bis (4-(4aminophenoxy)phenyl) hexafluoropropane with 2,2-bis (3,4-dicarboxyphenyl) hexafluoropropane dianhydride in an aprotic solvent to form a polyamic acid resin solution. The polyamic acid resin solution is then extruded into a coagulation medium to form polyamic acid fibers. The fibers are thermally cured to their polyimide form. Alternatively, 2,2-bis(4-(4-aminophenoxy)phenyl) hexafluoropropane is reacted with 2,2-bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride to form a polyamic acid, and the polyamic acid is chemically converted to its polyimide form. The polyimide is then dissolved in a solvent to form a polyimide resin solution, and the polyimide resin is extruded into a coagulation medium to form a polyimide wet gel filament. In order to obtain polyimide fibers of increased tensile properties, the polyimide wet gel filaments are stretched at elevated temperatures. The tensile properties of the fibers were measured and found to be in the range of standard textile fibers. Polyimide fibers obtained by either method will have a dielectric constant similar to that of the corresponding polymer, viz., less than 3 at 10 GHz.

Versatile On-Resin Synthesis of High Mannose Glycosylated Asparagine with Functional Handles

PubMed Central

Chen, Rui; Pawlicki, Mark A.; Tolbert, Thomas J.

2013-01-01

Here we present a synthetic route for solid phase synthesis of N-linked glycoconjugates containing high mannose oligosaccharides which allows the incorporation of useful functional handles on the N-terminus of asparagine. In this strategy, the C-terminus of an Fmoc protected aspartic acid residue is first attached to a solid phase support. The side chain of aspartic acid is protected by a 2-phenylisopropyl protecting group, which allows selective deprotection for the introduction of glycosylation. By using a convergent on-resin glycosylamine coupling strategy, an N-glycosidic linkage is successfully formed on the free side chain of the resin bound aspartic acid with a large high mannose oligosaccharide, Man8GlcNAc2, to yield N-linked high mannose glycosylated asparagine. The use of on-resin glycosylamine coupling provides excellent glycosylation yield, can be applied to couple other types of oligosaccharides, and also makes it possible to recover excess oligosaccharides conveniently after the on-resin coupling reaction. Useful functional handles including an alkene (p-vinylbenzoic acid), an alkyne (4-pentynoic acid), biotin, and 5-carboxyfluorescein are then conjugated onto the N-terminal amine of asparagine on-resin after the removal of the Fmoc protecting group. In this way, useful functional handles are introduced onto the glycosylated asparagine while maintaining the structural integrity of the reducing end of the oligosaccharide. The asparagine side chain also serves as a linker between the glycan and the functional group and preserves the native presentation of N-linked glycan which may aid in biochemical and structural studies. As an example of a biochemical study using functionalized high mannose glycosylated asparagine, a fluorescence polarization assay has been utilized to study the binding of the lectin Concanavalin A (ConA) using 5-carboxyfluorescein labeled high mannose glycosylated asparagine. PMID:24326091

Comparison of microleakage of three acid-base luting cements versus one resin-bonded cement for Class V direct composite inlays.

PubMed

Piemjai, Morakot; Miyasaka, Kumiko; Iwasaki, Yasuhiko; Nakabayashi, Nobuo

2002-12-01

Demineralized dentin beneath set cement may adversely affect microleakage under fixed restorations. Microleakage of direct composite inlays cemented with acid-base cements and a methyl methacrylate resin cement were evaluated to determine their effect on the integrity of the underlying hybridized dentin. Sixty Class V box preparations (3 mm x 3 mm x 1.5 mm) were precisely prepared in previously frozen bovine teeth with one margin in enamel and another margin in dentin. Direct composite inlays (EPIC-TMPT) for each preparation were divided into 4 groups of 15 specimens each and cemented with 3 acid-base cements (control group): Elite, Ketac-Cem, Hy-Bond Carbo-Cem, and 1 adhesive resin cement: C&B Metabond. All specimens were stored in distilled water for 24 hours at 37 degrees C before immersion in 0.5% basic fuchsin for 24 hours. The dye penetration was measured on the sectioned specimens at the tooth-cement interface of enamel and cementum margins and recorded with graded criteria under light microscopy (Olympus Vanox-T) at original magnification x 50, 100, and 200. A Kruskal-Wallis and the Mann-Whitney test at P<.05 were used to analyze leakage score. All cementum margins of the 3 acid-base cements tested demonstrated significantly higher leakage scores than cementum margins for inlays cemented with the resin cement tested(P<.01). No leakage along the tooth-cement interface was found for inlays retained with the adhesive resin cement. Within the limitations of this study, the 3 acid-base cements tested exhibited greater microleakage at the cementum margins than did the adhesive resin cement that was tested.

A Convenient Approach to Synthesizing Peptide C-Terminal N-Alkyl Amides

PubMed Central

Fang, Wei-Jie; Yakovleva, Tatyana; Aldrich, Jane V.

2014-01-01

Peptide C-terminal N-alkyl amides have gained more attention over the past decade due to their biological properties, including improved pharmacokinetic and pharmacodynamic profiles. However, the synthesis of this type of peptide on solid phase by current available methods can be challenging. Here we report a convenient method to synthesize peptide C-terminal N-alkyl amides using the well-known Fukuyama N-alkylation reaction on a standard resin commonly used for the synthesis of peptide C-terminal primary amides, the PAL-PEG-PS (Peptide Amide Linker-polyethylene glycol-polystyrene) resin. The alkylation and oNBS deprotection were conducted under basic conditions and were therefore compatible with this acid labile resin. The alkylation reaction was very efficient on this resin with a number of different alkyl iodides or bromides, and the synthesis of model enkephalin N-alkyl amide analogs using this method gave consistently high yields and purities, demonstrating the applicability of this methodology. The synthesis of N-alkyl amides was more difficult on a Rink amide resin, especially the coupling of the first amino acid to the N-alkyl amine, resulting in lower yields for loading the first amino acid onto the resin. This method can be widely applied in the synthesis of peptide N-alkyl amides. PMID:22252422

Sampling and analysis of airborne resin acids and solvent-soluble material derived from heated colophony (rosin) flux: a method to quantify exposure to sensitizing compounds liberated during electronics soldering.

PubMed

Smith, P A; Son, P S; Callaghan, P M; Jederberg, W W; Kuhlmann, K; Still, K R

1996-07-17

Components of colophony (rosin) resin acids are sensitizers through dermal and pulmonary exposure to heated and unheated material. Significant work in the literature identifies specific resin acids and their oxidation products as sensitizers. Pulmonary exposure to colophony sensitizers has been estimated indirectly through formaldehyde exposure. To assess pulmonary sensitization from airborne resin acids, direct measurement is desired, as the degree to which aldehyde exposure correlates with that of resin acids during colophony heating is undefined. Any analytical method proposed should be applicable to a range of compounds and should also identify specific compounds present in a breathing zone sample. This work adapts OSHA Sampling and Analytical Method 58, which is designed to provide airborne concentration data for coal tar pitch volatile solids by air filtration through a glass fiber filter, solvent extraction of the filter, and gravimetric analysis of the non-volatile extract residue. In addition to data regarding total soluble material captured, a portion of the extract may be subjected to compound-specific analysis. Levels of soluble solids found during personal breathing zone sampling during electronics soldering in a Naval Aviation Depot ranged from below the "reliable quantitation limit" reported in the method to 7.98 mg/m3. Colophony-spiked filters analyzed in accordance with the method (modified) produced a limit of detection for total solvent-soluble colophony solids of 10 micrograms/filter. High performance liquid chromatography was used to identify abietic acid present in a breathing zone sample.

The effect of storage conditions, contamination modes and cleaning procedures on the resin bond strength to lithium disilicate ceramic.

PubMed

Klosa, Karsten; Wolfart, Stefan; Lehmann, Frank; Wenz, Hans-Jürgen; Kern, Matthias

2009-04-01

The purpose of this in-vitro study was to evaluate the resin bond strength to pre-etched lithium disilicate ceramic using different cleaning methods after two contamination modes (saliva or saliva and silicone). Plexiglas tubes filled with composite resin (MultiCore Flow) were bonded to etched and silanized ceramic disks made of lithium disilicate ceramic (IPS e.max Press) using a luting resin (Multilink Automix). Either etched or unetched ceramic surfaces were contaminated with saliva or with saliva followed by a disclosing silicone. Groups of 16 specimens each were bonded after pretreatment using 4 surface cleaning agents (37% phosphoric acid, 5% hydrofluoric acid, 96% isopropanol, air polishing device with sodium bicarbonate) in different combinations. Before measuring tensile bond strength, specimens were stored for 3 or 150 days with thermocycling. After 150 days of storage, etching of saliva-contaminated surfaces with 5% hydrofluoric acid and/or 37% phosphoric acid provided statistically significantly higher bond strengths (37.9 to 49.5 MPa) than the other cleaning methods (1.7 to 15.5 MPa). After saliva and silicone contamination, etching with 5% hydrofluoric acid provided statistically significantly higher bond strengths (44.5 to 50.3 MPa) than all other cleaning methods (0.3 to 13.5 MPa). Ceramic cleaning methods after try-in procedures have a significant influence on the resin bond strength and are dependent on the type of contamination. Re-etching lithium disilicate ceramic with 5% hydrofluoric acid is most effective in removing contamination with saliva and/or a silicone disclosing medium.

Phosphine resistance does not confer cross-resistance to sulfuryl fluoride in four major stored grain insect pests.

PubMed

Jagadeesan, Rajeswaran; Nayak, Manoj K

2017-07-01

Susceptibility to phosphine (PH 3 ) and sulfuryl fluoride (SF) and cross-resistance to SF were evaluated in two life stages (eggs and adults) of key grain insect pests, Rhyzopertha dominca (F.), Sitophilus oryzae (L.), Cryptolestes ferrugineus (Stephens), and Tribolium castaneum (Herbst). This study was performed with an aim to integrate SF into phosphine resistance management programmes in Australia. Characterisation of susceptibility and resistance to phosphine in eggs and adults showed that C. ferrugineus was the most tolerant as well as resistant species. Mortality responses of eggs and adults to SF at 25 °C revealed T. castaneum to be the most tolerant species followed by S. oryzae, C. ferrugineus and R. dominica. A high dose range of SF, 50.8-62.2 mg L -1 over 48 h, representing c (concentration) × t (time) products of 2438-2985 gh m -3 , was required for complete control of eggs of T. castaneum, whereas eggs of the least tolerant R. dominca required only 630 gh m -3 for 48 h (13.13 mg L -1 ). Mortality response of eggs and adults of phosphine-resistant strains to SF in all four species confirmed the lack of cross-resistance to SF. Our research concludes that phosphine resistance does not confer cross-resistance to SF in grain insect pests irrespective of the variation in levels of tolerance to SF itself or resistance to phosphine in their egg and adult stages. While our study confirms that SF has potential as a 'phosphine resistance breaker', the observed higher tolerance in eggs stresses the importance of developing SF fumigation protocols with longer exposure periods. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

URANIUM EXTRACTION PROCESS

DOEpatents

Baldwin, W.H.; Higgins, C.E.

1958-12-16

A process is described for recovering uranium values from acidic aqueous solutions containing hexavalent uranium by contacting the solution with an organic solution comprised of a substantially water-immiscible organlc diluent and an organic phosphate to extract the uranlum values into the organic phase. Carbon tetrachloride and a petroleum hydrocarbon fraction, such as kerosene, are sultable diluents to be used in combination with organlc phosphates such as dibutyl butylphosphonate, trlbutyl phosphine oxide, and tributyl phosphate.

A method for the production of weakly acidic cation exchange resins

NASA Astrophysics Data System (ADS)

Heller, H.; Werner, F.; Mitschker, A.; Diehl, H. V.; Schaefer, A.

1991-12-01

The invention relates to a nonpolluting method for the production of weakly acidic cation exchange resins by saponification of cross-linked acrylonitrile bead polymers, with an alkaline saponification agent at elevated temperature, according to which method the bead polymer and alkaline saponification agent are jointly added only at elevated temperature.

Diterpene resin acids in conifers.

PubMed

Keeling, Christopher I; Bohlmann, Jörg

2006-11-01

Diterpene resin acids are a significant component of conifer oleoresin, which is a viscous mixture of terpenoids present constitutively or inducibly upon herbivore or pathogen attack and comprises one form of chemical resistance to such attacks. This review focuses on the recent discoveries in the chemistry, biosynthesis, molecular biology, regulation, and biology of these compounds in conifers.

Solid lipid nanoparticles for the delivery of 1,3,5-triaza-7-phosphaadamantane (PTA) platinum (II) carboxylates.

PubMed

Sguizzato, Maddalena; Cortesi, Rita; Gallerani, Eleonora; Drechsler, Markus; Marvelli, Lorenza; Mariani, Paolo; Carducci, Federica; Gavioli, Riccardo; Esposito, Elisabetta; Bergamini, Paola

2017-05-01

The use of solid lipid nanoparticles (SLN) is a promising route for the delivery of platinum complexes aimed to anticancer activity. This paper describes the production and characterization of SLN suitable for the loading of Pt complexes containing the biocompatible phosphine 1,3,5-triaza-7-phosphaadamantane (PTA) as neutral ligand. After a screening of several lipidic phases, stearic acid-based SLN were identified as the most appropriate for the purpose. They were produced by emulsion-dilution method and then characterized in terms of dimension, polydispersity, time stability, pH balance and morphological aspect. Stearic acid SLN are designed as a system able to coordinate to platinum, acting as anionic carboxylic ligands, replacing the base carbonate of the Pt synthon [PtCO 3 (DMSO) 2 ], where also DMSO can subsequently be substituted by phosphinic ligands, namely PTA. SLN functionalised with Pt-PTA were produced and characterized by this synthetic route. The toxicity of plain SLN and the antiproliferative effect of SLN functionalised with Pt-PTA were evaluated on two human cancer cell lines K562 and A2780. The results indicate that SLN can be exploited as a delivery system for Pt complexes with potential anticancer activity. Copyright © 2016 Elsevier B.V. All rights reserved.

ANION EXCHANGE METHOD FOR SEPARATION OF METAL VALUES

DOEpatents

Hyde, E.K.; Raby, B.A.

1959-02-10

A method is described for selectively separating radium, bismuth, poloniums and lead values from a metallic mixture of thc same. The mixture is dissolved in aqueous hydrochloric acid and the acidity is adjusted to between 1 to 2M in hydrochloric acid to form the anionic polychloro complexes of polonium and bismuth. The solution is contacted with a first anion exchange resin such as strong base quaternary ammonia type to selectively absorb the polonium and bismuth leaving the radium and lead in the effluent. The effluent, after treatment in hydrochloric acid to increase the hydrochloric acid concentration to 6M is contacted with a second anion exchange iesin of the same type as the above to selectively adsorb the lead leaving the radium in the effluent. Radium is separately recovered from the effluent from the second exchange column. Lead is stripped from the loaded resin of the second column by treatment with 3M hydrochloric acid solution. The loaded resin of the first column is washed with 8M hydrochloric acid solution to recover bismuth and then treated with strong nitric acid solution to recover polonium.

Natural derivatives of diphenolic acid as substitutes for bisphenol-A

NASA Astrophysics Data System (ADS)

Ertl, Johanna; Cerri, Elisa; Rizzuto, Matteo; Caretti, Daniele

2014-05-01

Diphenolic acid had been originally used in the first epoxy resins and was later on forgotten as it was substituted by the cheaper bisphenol A. But in the recent years major health concerns have been raised as bisphenol A has a pseudo-hormonal effect on the body, playing the role of estrogen it can cause a severe impact on the organism, especially in males. Moreover it is produced from acetone and phenol, both from fossil, and thus limited resources. On the contrary, diphenolic acid is synthesized from levulinic acid and phenol. Levulinic acid being directly produced by hydrolysis of biomass. By substituting the fossil phenol with natural phenols from lignin or plant extraction we are able to synthesize a fully renewable substitute for bisphenol A. The reactions to yield an epoxy resin have been examined and the reactivity with epichlorohydrin is satisfying. Moreover, some of the derivatives of diphenolic acid have interesting curing properties and preliminary results show excellent properties of the cured resin, including thermal stability and pencil hardness.

Phosphine-free Stille-Migita chemistry for the mild and orthogonal modification of DNA and RNA.

PubMed

Krause, André; Hertl, Alexander; Muttach, Fabian; Jäschke, Andres

2014-12-08

An optimized catalyst system of [Pd2 (dba)3 ] and AsPh3 efficiently catalyzes the Stille reaction between a diverse set of functionalized stannanes and halogenated mono-, di- and oligonucleotides. The methodology allows for the facile conjugation of short and long nucleic acid molecules with moieties that are not compatible with conventional chemical or enzymatic synthesis, among them acid-, base-, or fluoride-labile protecting groups, fluorogenic and synthetically challenging moieties with good to near-quantitative yields. Notably, even azides can be directly introduced into oligonucleotides and (deoxy)nucleoside triphosphates, thereby giving direct access to "clickable" nucleic acids. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A nickel phosphine complex as a fast and efficient hydrogen production catalyst.

PubMed

Gan, Lu; Groy, Thomas L; Tarakeshwar, Pilarisetty; Mazinani, Shobeir K S; Shearer, Jason; Mujica, Vladimiro; Jones, Anne K

2015-01-28

Here we report the electrocatalytic reduction of protons to hydrogen by a novel S2P2 coordinated nickel complex, [Ni(bdt)(dppf)] (bdt = 1,2-benzenedithiolate, dppf = 1,1'-bis(diphenylphosphino)ferrocene). The catalysis is fast and efficient with a turnover frequency of 1240 s(-1) and an overpotential of only 265 mV for half activity at low acid concentrations. Furthermore, catalysis is possible using a weak acid, and the complex is stable for at least 4 h in acidic solution. Calculations of the system carried out at the density functional level of theory (DFT) are consistent with a mechanism for catalysis in which both protonations take place at the nickel center.

Strategies for improving production performance of probiotic Pediococcus acidilactici viable cell by overcoming lactic acid inhibition.

PubMed

Othman, Majdiah; Ariff, Arbakariya B; Wasoh, Helmi; Kapri, Mohd Rizal; Halim, Murni

2017-11-27

Lactic acid bacteria are industrially important microorganisms recognized for fermentative ability mostly in their probiotic benefits as well as lactic acid production for various applications. Fermentation conditions such as concentration of initial glucose in the culture, concentration of lactic acid accumulated in the culture, types of pH control strategy, types of aeration mode and different agitation speed had influenced the cultivation performance of batch fermentation of Pediococcus acidilactici. The maximum viable cell concentration obtained in constant fed-batch fermentation at a feeding rate of 0.015 L/h was 6.1 times higher with 1.6 times reduction in lactic acid accumulation compared to batch fermentation. Anion exchange resin, IRA 67 was found to have the highest selectivity towards lactic acid compared to other components studied. Fed-batch fermentation of P. acidilactici coupled with lactic acid removal system using IRA 67 resin showed 55.5 and 9.1 times of improvement in maximum viable cell concentration compared to fermentation without resin for batch and fed-batch mode respectively. The improvement of the P. acidilactici growth in the constant fed-batch fermentation indicated the use of minimal and simple process control equipment is an effective approach for reducing by-product inhibition. Further improvement in the cultivation performance of P. acidilactici in fed-bath fermentation with in situ addition of anion-exchange resin significantly helped to enhance the growth of P. acidilactici by reducing the inhibitory effect of lactic acid and thus increasing probiotic production.

Carbon dioxide capture using resin-wafer electrodeionization

DOEpatents

Lin, YuPo J.; Snyder, Seth W.; Trachtenberg, Michael S.; Cowan, Robert M.; Datta, Saurav

2015-09-08

The present invention provides a resin-wafer electrodeionization (RW-EDI) apparatus including cathode and anode electrodes separated by a plurality of porous solid ion exchange resin wafers, which when in use are filled with an aqueous fluid. The apparatus includes one or more wafers comprising a basic ion exchange medium, and preferably includes one or more wafers comprising an acidic ion exchange medium. The wafers are separated from one another by ion exchange membranes. The fluid within the acidic and/or basic ion exchange wafers preferably includes, or is in contact with, a carbonic anhydrase (CA) enzyme to facilitate conversion of bicarbonate ion to carbon dioxide within the acidic medium. A pH suitable for exchange of CO.sub.2 is electrochemically maintained within the basic and acidic ion exchange wafers by applying an electric potential across the cathode and anode.

Acrylic acid removal by acrylic acid utilizing bacteria from acrylonitrile-butadiene-styrene resin manufactured wastewater treatment system.

PubMed

Wang, C C; Lee, C M

2006-01-01

The aim of this study is to isolate the acrylic acid utilizing bacteria from the ABS resin manufactured wastewater treatment system. The bacteria should have the ability to remove acrylic acid and tolerate the acrylonitrile and acrylamide toxicity. The aim is also to understand the performance of isolated pure strain for treating different initial acrylic acid concentrations from synthetic wastewater. The results are: twenty strains were isolated from the ABS resin manufactured wastewater treatment system and twelve of them could utilize 600 mg/l acrylic acid for growth. Seven of twelve strains could tolerate the acrylonitrile and acrylamide toxicity, when the concentration was below 300 mg/l. Bacillus thuringiensis was one of the seven strains and the optimum growth temperature was 32 degrees C. Bacillus thuringiensis could utilize acrylic acid for growth, when the initial acrylic acid concentration was below 1,690.4 mg/l. Besides this, when the initial acrylic acid concentration was below 606.8 mg/l, the acrylic acid removal efficiency exceeded 96.3%. Bacillus thuringiensis could tolerate 295.7 mg/l acrylamide and 198.4 mg/l acrylonitrile toxicity but could not tolerate 297.3 mg/l epsilon-caprolactam.

Stereogenic phosphorus-induced diastereoselective formation of chiral carbon during nucleophilic addition of chiral H-P species to aldehydes or ketones.

PubMed

Zhang, He; Sun, Yong-Ming; Yao, Lan; Ji, Si-Yu; Zhao, Chang-Qiu; Han, Li-Biao

2014-05-01

P,C-stereogenic α-hydroxyl phosphinates or phosphine oxides were prepared from the additions of (RP)-phosphinate to ketones or (RP)-phosphine oxide to aldehydes, respectively, catalyzed by bases at room temperature in up to >99:1 diasteromeric ratio (d.r.P/d.r.C) and 99 % yields. The diastereoselectivity was induced by reversible equilibrium and different stabilities between two diastereomers of adduct, which was caused by the spatial interaction between menthoxyl or menthyl to alkyl groups of aldehydes or ketones. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chemoselective Polymerization of Polar Divinyl Monomers with Rare-Earth/Phosphine Lewis Pairs.

PubMed

Xu, Pengfei; Wu, Lei; Dong, Liqiu; Xu, Xin

2018-02-08

This work reports the chemoselective polymerization of polar divinyl monomers, including allyl methacrylate (AMA), vinyl methacrylate (VMA), and 4-vinylbenzyl methacrylate (VBMA), by using simple Lewis pairs comprised of homoleptic rare-earth (RE) aryloxide complexes RE(OAr)₃ (RE = Sc ( 1 ), Y ( 2 ), Sm ( 3 ), La ( 4 ), Ar = 2,6- t Bu₂C₆H₃) and phosphines PR₃ (R = Ph, Cy, Et, Me). Catalytic activities of polymerizations relied heavily upon the cooperation of Lewis acid and Lewis base components. The produced polymers were soluble in common organic solvents and often had a narrow molecular weight distribution. A highly syndiotactic poly(allyl methacrylate) (PAMA) with rr ~88% could be obtained by the scandium complex 1 /PEt₃ pair at -30 °C. In the case of poly(4-vinylbenzyl methacrylate) (PVBMA), it could be post-functionalized with PhCH₂SH. Mechanistic study, including the isolation of the zwitterionic active species and the end-group analysis, revealed that the frustrated Lewis pair (FLP)-type addition was the initiating step in the polymerization.

Telescoping Reactions with Trifluorodiazoethane-Derived Aza-Wittig Reagents and Allenyl esters.

PubMed

Zhang, Fa-Guang; Zeng, Jun-Liang; Tian, Yi-Qiang; Zheng, Yan; Cahard, Dominique; Ma, Jun-An

2018-05-28

A telescoping process involving the consecutive addition of four reagents (trifluorodiazoethane, phosphine, allenyl ester, and acetic acid) into a single reactor was developed for the novel functionalization of allenyl esters. First, new phosphazenes derived from trifluorodiazoethane and phosphines were generated and reacted with allenyl esters to give unexpected α-iminophosphoranes through the creation of C=P, C=N, and C-H bonds at the α-, β-, and γ-carbon atoms, respectively, of the allenyl esters. The α-iminophosphoranes did not react with aldehydes in a classic Wittig reaction, but instead β-enamino esters were obtained. The overall sequence of reactions offered a formal hydrohydrazonation of allenyl esters. The method was extended to other related diazo compounds and applied to the preparation of novel 5-pyrazolone derivatives. Not only is the telescoping process described herein an effective approach for truncating the multistep synthesis, but also each step has been dissected to understand and support the reaction mechanisms. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Reaction pH of urea-formaldehyde resins as related to strength properties of southern pine particleboard

Treesearch

C. -Y. Hse

1974-01-01

Twelve urea-formaldehyde resins were prepared with factorial combinations of 4 alkaline and 3 acidic reaction phases; i. e., the reaction mixture was adjusted to pH 7, 8, 9, or 10 for the first hour and then made weakly acid to pH 5.8, 4.8, or 3.8.

ION EXCHANGE PROCESS FOR THE RECOVERY AND PURIFICATION OF MATERIALS

DOEpatents

Long, R.S.; Bailes, R.H.

1958-04-15

A process for the recovery of certain metallic ions from aqueous solutions by ion exchange techniques is described. It is applicable to elements such as vanadium, chromium, nnanganese, and the like, which are capable of forming lower valent cations soluble in aqueous solutions and which also form ldgher valent anions soluble in aqueous acidic solutions. For example, small amounts of vanadium occurring in phosphoric acid prepared from phosphate rock may be recovered by reducing the vanadium to a trivalent cation adsorbing; the vanadium in a cationic exchange resin, then treating the resin with a suitable oxidizing agent to convert the adsorbed vanadium to a higher valent state, and finally eluting; the vanadium as an anion from the resin by means of an aqueous acidic solution.

Resin catalysts and method of preparation

DOEpatents

Smith, Jr., Lawrence A.

1986-01-01

Heat stabilized catalyst compositions are prepared from nuclear sulfonic acid, for example, macroporous crosslinked polyvinyl aromatic compounds containing sulfonic acid groups are neutralized with a metal of Al, Fe, Zn, Cu, Ni, ions or mixtures and alkali, alkaline earth metals or ammonium ions by contacting the resin containing the sulfonic acid with aqueous solutions of the metals salts and alkali, alkaline earth metal or ammonium salts. The catalysts have at least 50% of the sulfonic acid groups neutralized with metal ions and the balance of the sulfonic acid groups neutralized with alkali, alkaline earth ions or ammonium ions.

Resin catalysts and method of preparation

DOEpatents

Smith, L.A. Jr.

1986-12-16

Heat stabilized catalyst compositions are prepared from nuclear sulfonic acid, for example, macroporous crosslinked polyvinyl aromatic compounds containing sulfonic acid groups are neutralized with a metal of Al, Fe, Zn, Cu, Ni, ions or mixtures and alkali, alkaline earth metals or ammonium ions by contacting the resin containing the sulfonic acid with aqueous solutions of the metals salts and alkali, alkaline earth metal or ammonium salts. The catalysts have at least 50% of the sulfonic acid groups neutralized with metal ions and the balance of the sulfonic acid groups neutralized with alkali, alkaline earth ions or ammonium ions.

Unraveling aminophosphine redox mechanisms for glovebox-free InP quantum dot syntheses.

PubMed

Laufersky, Geoffry; Bradley, Siobhan; Frécaut, Elian; Lein, Matthias; Nann, Thomas

2018-05-10

The synthesis of colloidal indium phosphide quantum dots (InP QDs) has always been plagued by difficulties arising from limited P3- sources. Being effectively restricted to the highly pyrophoric tris(trimethylsilyl) phosphine (TMS3P) creates complications for the average chemist and presents a significant risk for industrially scaled reactions. The adaptation of tris(dialkylamino) phosphines for these syntheses has garnered attention, as these new phosphines are much safer and can generate nanoparticles with competitive photoluminescence properties to those from (TMS)3P routes. Until now, the reaction mechanics of this precursor were elusive due to many experimental optimizations, such as the inclusion of a high concentration of zinc salts, being atypical of previous InP syntheses. Herein, we utilize density functional theory calculations to outline a logical reaction mechanism. The aminophosphine precursor is found to require activation by a zinc halide before undergoing a disproportionation reaction to self-reduce this P(iii) material to a P(-iii) source. We use this understanding to adapt this precursor for a two-pot nanoparticle synthesis in a noncoordinating solvent outside of glovebox conditions. This allowed us to generate spherical InP/ZnS nanoparticles possessing fluorescence quantum yields >55% and lifetimes as fast as 48 ns, with tunable emission according to varying zinc halide acidity. The development of high quality and efficient InP QDs with this safer aminophosphine in simple Schlenk environments will enable a broader range of researchers to synthesize these nontoxic materials for a variety of high-value applications.

Bond strength of Bis-GMA and glass ionomer pit and fissure sealants using cyclic fatigue.

PubMed

Dewji, H R; Drummond, J L; Fadavi, S; Punwani, I

1998-02-01

The aim of the study was to determine the bond strength of glass ionomer and resin-modified glass ionomer sealants compared to Bis-GMA sealants using both static and cyclic fatigue shear testing. Four materials were evaluated: D, a Bis-GMA sealant with 10% phosphoric acid etchant; FC, a resin-modified glass ionomer sealant with 20% polyacrylic acid etchant; FD, a resin-modified glass ionomer sealant with 10% polyacrylic acid etchant; and FSC, a self-cured glass ionomer sealant with no etchant. Gelatin capsules filled with the sealant material were bonded to the enamel surfaces of bovine teeth after appropriate surface conditioning and then tested in shear static and cyclic fatigue. Static and cyclic shear bond strengths, respectively, for each group were (MPa): FC: 21.1+/-2.8 and 17.1+/-3.1; FD: 14.6+/-5.9 and 8.5+/-3.1; D: 10.8+/-4.9 and 4.7+/-2.6; FSC: 8.7 (1.0 and 2.9+/-0.6. The resin-modified glass ionomer sealants had better fatigue bond strength than both Bis-GMA and self-cured glass ionomer sealants with the surface conditioning affecting the bond strength of the resin-modified glass ionomer sealants.

Gastroprotective effect of the Mapuche crude drug Araucaria araucana resin and its main constituents.

PubMed

Schmeda-Hirschmann, Guillermo; Astudillo, Luis; Rodríguez, Jaime; Theoduloz, Cristina; Yáñez, Tania

2005-10-03

The resin from the tree Araucaria araucana (Araucariaceae) has been used since pre-columbian times by the Mapuche amerindians to treat ulcers. The gastroprotective effect of the resin was assessed in the ethanol-HCl-induced gastric ulcer in mice showing a dose-dependent gastroprotective activity at 100, 200 and 300 mg/kg per os. The main three diterpene constituents of the resin, namely imbricatolic acid, 15-hydroxyimbricatolal and 15-acetoxyimbricatolic acid were isolated and evaluated for gastroprotective effect at doses of 50, 100 and 200 mg/kg. A dose-related gastroprotective effect with highly significant activity (P<0.01) was observed at doses up to 200 mg/kg. At 100 mg/kg, the highest gastroprotective activity was provided by 15-hydroxyimbricatolal and 15-acetoxyimbricatolic acid, all of them being as active as the reference drug lansoprazole at 20 mg/kg. The cytotoxicity of the main diterpenes as well as lansoprazole was studied towards human lung fibroblasts (MRC-5) and determined by the MTT reduction assay. A concentration-dependent cell viability inhibition was found with IC50 values ranging from 125 up to 290 microM. Our results support the traditional use of the Araucaria araucana resin by the Mapuche culture.

[Bonding strength of resin and tooth enamel after teeth bleaching with cold plasma].

PubMed

Zhu, Meng-meng; Wang, Guo-min; Sun, Ke; Li, Ying-long; Pan, Jie

2016-02-18

To investigate the immediate bond strength and surface structure of resin and the tooth enamel which treated by cold plasma. In the study, 40 bovine incisors were divided into two equal parts. In this sense, all enamel adhesive samples were prepared and then randomly divided into 4 groups (n =20). group 1: acid + single bond 2+resin composite (control group); group 2:beyond bleaching+ acid+single bond 2+resin composite; group 3: treated by cold plasma for 5 minutes+ acid+single bond 2+resin composite; group 4: treated by cold plasma for 5 minutes+single bond 2+resin composite. Single bond 2 bonding system and Filtek Z250 resin were used in this experiment. The shear bond strength was tested by universal testing machine. The surface of the enamel in different processes was observed by scanning electron microscope (SEM). Statistical analyses by the single factor analysis of variance and multiple pairwise comparisons were performed with SPSS 17.0 . The shear bond strength of group 4 (8.60 MPa) was significantly lower than that of the other three groups (P<0.05). The shear bond strength of group 2 (17.89 MPa) was higher than that of group 4, but lower than group 1 and group 3 (P<0.05).There was no significant difference between group 1 (34.82 MPa) and group 3 (34.69 MPa). Scanning electron microscope indicated that the enamel treated by cold plasma had slight molten form, which was different from etched enamel surface.The fractured surface of group 3 was mix fracture, which was similar to the control group (group 1). Compared with the conventional clinic bleaching, immediate bond strength of resin-enamel that treated by cold plasma has not been affected.

International Traffic in Arms Regulations (ITAR), (22 CFR 120-130)

DTIC Science & Technology

1996-06-01

Butadienenitrileoxide (BNO); (6) Catocene, N-butyl- ferrocene and other ferrocene derivatives; (7) 3-nitraza-l,5 pentane diisocyanate; (8) Bis(2,2...Tris-l-(2-methyl)aziridinyl phosphine oxide (MAPO), bis(2-methyl aziridinyl) 2-(2-hydroxypropanoxy) propylamino phosphine oxide (BOBBA 8), and...other MAPO derivatives; (22) Bis(2-methyl aziridinyl) methylamino phosphine oxide (methyl BAPO); (23) Organo-metallic coupling agents, specifi

Multiphoton Production and Detection of Atoms.

DTIC Science & Technology

1985-04-01

photodissociation of metal ligand analogues of ferrocene would cleanly photodis- sociate to give metal atoms, producing atomic cobalt, ruthinium, nickel...in the exper- iments with triphenyl phosphine and phosphine , only at high I pressures, with a long-pulse (1 microsecond) laser. Sulphur atoms were...unassigned in our experiments. These probably originate in the poorly understood metastable SO state. Ashfold et.al., in their work on MPD/MPI on phosphine

Photochemically Induced Transformations of Transition Complexes.

DTIC Science & Technology

1993-05-17

simple Iron dinuclear species, the DPPM and DPPE phosphine bridged compounds undergo photolysis in CHCI3 to yield products containing formyl substitued...possible reaction pathway for the synthesis of these two monomers as byproducts In the ruthenium phosphine dimer preparation Is suggested. Full structural...DPPM dimer is also described. In contrast to the behavior of the simple iron dinuclear species, the DPPM and DPPE phosphine bridged compounds undergo

Synthesis, characterization and applications of a new cation exchanger tamarind sulphonic acid (TSA) resin.

PubMed

Singh, A V; Sharma, Naresh Kumar; Rathore, Abhay S

2012-01-01

A new composite cation exchanger, tamarind sulphonic acid (TSA) resin has been synthesized. The chemically modified TSA ion exchange resin has been used for the removal and preconcentration of Zn2+, Cd2+, Fe2+, Co2+ and Cu2+ ions in aqueous solution and effluent from the Laxmi steel plant in Jodhpur, India. This type of composite represents a new class of hybrid ion exchangers with good ion exchange capacity, stability, reproducibility and selectivity for toxic metal ions found in effluent from the steel industry. The characterization of the resin was carried out by determining the ion-exchange capacity, elemental analysis, pH titration, Fourier transform infrared spectra and thermal analysis. The distribution coefficients (K(d)) of toxic metal ions were determined in a reference aqueous solution and the steel plant effluent at different pH values; the absorbency of different metal ions on the TSA resin was studied for up to 10 cycles. The adsorption of different metal ions on TSA resin follows the order: Co2+ > Cu2+ > Zn2+ > Fe2+ > Cd2+. The ion exchange capacity of TSA resin is 2.87%.

Bond strength of orthodontic light-cured resin-modified glass ionomer cement.

PubMed

Cheng, Hsiang Yu; Chen, Chien Hsiu; Li, Chuan Li; Tsai, Hung Huey; Chou, Ta Hsiung; Wang, Wei Nan

2011-04-01

The purpose of this study was to compare the bond strengths and debonded interfaces achieved with light-cured resin-modified glass ionomer cement (RMGIC) and conventional light-cured composite resin. In addition, the effects of acid etching and water contamination were examined. One hundred human premolars were randomly divided into five equal groups. The mini Dyna-lock upper premolar bracket was selected for testing. The first four groups were treated with light-cured RMGIC with or without 15 per cent phosphoric acid-etching treatment and with or without water contamination preceding bracket bonding. The control samples were treated with the conventional light-cured Transbond composite resin under acid etching and without water contamination. Subsequently, the brackets were debonded by tensile force using an Instron machine. The modified adhesive remnant index (ARI) scores were assigned to the bracket base of the debonded interfaces using a scanning electron microscope. The bond strength and modified ARI scores were determined and analysed statistically by one-way analysis of variance and chi-square test. Under all four conditions, the bond strength of the light-cure RMGIC was equal to or higher than that of the conventional composite resin. The highest bond strength was achieved when using RMGIC with acid etching but without water contamination. The modified ARI scores were 2 for Fuji Ortho LC and 3 for Transbond. No enamel detachment was found in any group. Fifteen per cent phosphoric acid etching without moistening the enamel of Fuji Ortho LC provided the more favourable bond strength. Enamel surfaces, with or without water contamination and with or without acid etching, had the same or a greater bond strength than Transbond.

Assessment of microleakage of class V restored by resin composite and resin-modified glass ionomer and pit and fissure resin-based sealants following Er:YAG laser conditioning and acid etching: in vitro study

PubMed Central

Luong, Emilie; Shayegan, Amir

2018-01-01

Aim The aim of this study was to make a comparison between microleakage of conventionally restored class V cavities using acid etchant and the ones conditioned by erbium-doped yttrium aluminum garnet (Er:YAG) laser, and also to assess and compare the effectiveness of enamel surface treatments of occlusal pits and fissures by acid etching and conditioned by Er:YAG laser-etch. Materials and methods Seventy-two extracted third molars were used in this study. The samples were divided into two major groups: class V cavities and pit and fissure sealants. Each subgroup was divided into conventional acid etching, Er:YAG laser conditioning and conventional acid etching, and combination with Er:YAG laser conditioning (n=12). The teeth were placed in 2% methylene blue dye solution, were sectioned, and were evaluated according to the dye penetration criteria. Two samples per subgroup were chosen for scanning electron microscopic (SEM) analysis. Results There was a significant difference between occlusal and cervical margin groups. Laser conventional composite cementum group showed more microleakage values compared to other groups. There was no significant difference between occlusal margin groups. However, there was a significant difference between cervical margin groups in terms of microleakage. In sealant groups, there was a significant difference between laser and conventional with/without laser treatment groups in terms of microleakage. Conclusion Based on the results reported in this study, it can be concluded that the application of the Er:YAG laser beneath the resin composite, the resin-modified glass ionomers (GIs), and the fissure sealant placement may be an alternative enamel and dentin etching method to acid etching. PMID:29881311

Experimental resin cements containing bioactive fillers reduce matrix metalloproteinase-mediated dentin collagen degradation.

PubMed

Osorio, Raquel; Yamauti, Monica; Sauro, Salvatore; Watson, Thimoty F; Toledano, Manuel

2012-09-01

Collagen dentin matrix may represent a suitable scaffold to be remineralized in the presence of bioactive materials. The purpose of this study was to determine if experimental resin cements containing bioactive fillers may modulate matrix metalloproteinase-mediated collagen degradation of etched dentin. Human dentin beams demineralized using 10% phosphoric acid or 0.5 mol/L EDTA were infiltrated with the following experimental resins: (1) unfilled resin, (2) resin with Bioglass 45S5 particles (Sylc; OSspray Ltd, London, UK), and (3) resin with β-tricalcium phosphate-modified calcium silicate cement (HCAT-β) particles. The filler/resin ratio was 40/60 wt%. The specimens were stored in artificial saliva, and the determination of C-terminal telopeptide (ICTP) was performed by radioimmunoassay after 24 hours, 1 week, and 4 weeks. Scanning electron microscopic analysis of dentin surfaces after 4 weeks of storage was also executed. Collagen degradation was prominent both in phosphoric acid and EDTA-treated dentin. Resin infiltration strongly reduced the MMP activity in demineralized dentin. Resin-containing Bioglass 45S5 particles exerted higher and more stable protection of collagen at all tested dentin states and time points. HCAT-β induced collagen protection from MMPs only in EDTA-treated specimens. Dentin remineralization was achieved when dentin was infiltrated with the resin cements containing bioactive fillers. MMP degradation of dentin collagen is strongly reduced in resin-infiltrated dentin. The inclusion of Bioglass 45S5 particles exerted an additional protection of collagen during dentin remineralization. Copyright © 2012 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

Evaluation of polymeric adsorbent resins for efficient detoxification of liquor generated during acid pretreatment of lignocellulosic biomass.

PubMed

Sandhya, Soolamkandath Variem; Kiran, Kumar; Kuttiraja, Mathiyazhakan; Preeti, Varghese Elizabeth; Sindhu, Raveendran; Vani, Sankar; Kumar, Sukumaran Rajeev; Pandey, Ashok; Binod, Parameswaran

2013-11-01

Production of fuel ethanol from lignocellulosic biomass conventionally includes biomass pretreatment, hydrolysis, and fermentation. The liquor generated during dilute acid pretreatment of biomass contains considerable quantities of pentose sugars as well as various degradation products of sugars and lignin, like furfural, hydroxymethyl furfural (HMF), organic acids, aldehydes and others, which are known to be inhibitory for microbial growth. This pentose rich liquor is a potent resource which can be used to produce alcohol or other value added metabolites by microbial fermentation. However, the presence of these inhibitory compounds is a major hindrance and their removal is essential for efficient utilization of this byproduct stream. In the present work, the polymeric adsorbent resins, XAD-4, XAD-7 and XAD-16 were evaluated for their ability to adsorb fermentation inhibitors like furfural and HMF from the acid pretreated liquor. These resins could remove 55-75% of furfural and 100% of HMF and more than 90% sugar remained un-adsorbed in the pretreated liquor. Desorption of furfural from stationary phase was evaluated by using ethanol and hot water. The results suggest that these polymeric resins may be used for detoxification of acid pretreatment liquor with selective removal of sugar degradation products without affecting the sugar content in the solution.

Coinage metal coordination chemistry of stable primary, secondary and tertiary ferrocenylethyl-based phosphines.

PubMed

Azizpoor Fard, M; Rabiee Kenaree, A; Boyle, P D; Ragogna, P J; Gilroy, J B; Corrigan, J F

2016-02-21

Ferrocene-based phosphines constitute an important auxiliary ligand in inorganic chemistry. Utilizing the (ferrocenylethyl)phosphines (FcCH2CH2)3-nHnP (Fc = ferrocenyl; n = 2, 1; n = 1, 2; n = 0, 3) the synthesis of a series of coordination complexes [(FcCH2CH2)3-nHnPCuCl]4 (n = 2, 1-CuCl; n = 0, 3-CuCl), [(FcCH2CH2)2HPCuCl] (2-CuCl), {[(FcCH2CH2)H2P]2AgCl}2 (1-AgCl), [(FcCH2CH2)2HPAgCl] (2-AgCl), [(FcCH2CH2)3PAgCl]4 (3-AgCl), [(FcCH2CH2)3PM(OAc)]4 (M = Cu, 3-CuOAc M = Ag, 3-AgOAc), [(FcCH2CH2)3-nHnPAuCl] (n = 1, 2-AuCl; n = 0, 3-AuCl), via the reaction between the free phosphine and MX (M = Cu, Ag and Au; X = Cl, OAc), is described. The reaction between the respective phosphine with a suspension of metal-chloride or -acetate in a 1 : 1 ratio in THF at ambient temperature affords coordinated phosphine-coinage metal complexes. Varying structural motifs are observed in the solid state, as determined via single crystal X-ray analysis of 1-CuCl, 3-CuCl, 1-AgCl, 3-AgCl, 3-CuOAc, 3-AgOAc, 2-AuCl and 3-AuCl. Complexes 1-CuCl and 3-CuCl are tetrameric Cu(i) cubane-like structures with a Cu4Cl4 core, whereas silver complexes with primary and tertiary phosphine reveal two different structural types. The structure of 1-AgCl, unlike the rest, displays the coordination of two phosphines to each silver atom and shows a quadrangle defined by two Ag and two Cl atoms. In contrast, 3-AgCl is distorted from a cubane structure via elongation of one of the ClAg distances. 3-CuOAc and 3-AgOAc are isostructural with step-like cores, while complexes 2-AuCl and 3-AuCl reveal a linear geometry of a phosphine gold(i) chloride devoid of any aurophilic interactions. All of the complexes were characterized in solution by multinuclear (1)H, (13)C{(1)H} and (31)P NMR spectroscopic techniques; the redox chemistry of the series of complexes was examined using cyclic voltammetry. This class of complexes has been found to exhibit one reversible Fe(ii)/Fe(iii) oxidation couple, suggesting the absence of electronic communication between the ferrocenyl units on individual phosphine ligands as well as between different phosphines on the polymetallic cores.

Additives for High Temperature Hydraulic Fluids.

DTIC Science & Technology

HYDRAULIC FLUIDS, ADDITIVES, TRIAZINES, FERROCENES , PHOSPHINE , SULFOXIDES, SYNTHESIS(CHEMISTRY), SCIENTIFIC RESEARCH, FLUORINE COMPOUNDS, PHOSPHINE OXIDES, ORGANIC PHOSPHORUS COMPOUNDS, AMINES, HEAT RESISTANT MATERIALS.

Methods development for separation of inorganic anions, organic acids and bases, and neutral organic compounds by ion chromatography and capillary electrophoresis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Jie

1999-04-01

A novel anion-exchange resin containing three amine groups was prepared by reaction of a chloromethylated polystyrene-divinylbenzene (PS-DVB) resin with diethylenetriamine. After being protonated by contact with an aqueous acid, this resin can be used for ion chromatographic separation of anions. The charge on the resins can be varied from +1 to +3 by changing the mobile phase pH. The selectivity of the new ion exchangers for various inorganic anions was quite different from that of conventional anion exchangers. The performance of this new anion exchanger was studied by changing the pH and the concentration of the eluent, and several differentmore » eluents were used with some common anions as testing analytes. Conductivity detection and UV-visible detection were applied to detect the anions after separation. The new resin can also be used for HPLC separation of neutral organic compounds. Alkylphenols and alkylbenzenes were separated with this new polymeric resin, and excellent separations were obtained under simple conditions. This report contains Chapter 1: General introduction and Chapter 6: General conclusions.« less

Surface roughness of composite resins subjected to hydrochloric acid.

PubMed

Roque, Ana Carolina Cabral; Bohner, Lauren Oliveira Lima; de Godoi, Ana Paula Terossi; Colucci, Vivian; Corona, Silmara Aparecida Milori; Catirse, Alma Blásida Concepción Elizaur Benitez

2015-01-01

The purpose of this study was to determine the influence of hydrochloric acid on surface roughness of composite resins subjected to brushing. Sixty samples measuring 2 mm thick x 6 mm diameter were prepared and used as experimental units. The study presented a 3x2 factorial design, in which the factors were composite resin (n=20), at 3 levels: microhybrid composite (Z100), nanofilled composite (FiltekTM Supreme), nanohybrid composite (Ice), and acid challenge (n=10) at 2 levels: absence and presence. Acid challenge was performed by immersion of specimens in hydrochloric acid (pH 1.2) for 1 min, 4 times per day for 7 days. The specimens not subjected to acid challenge were stored in 15 mL of artificial saliva at 37 oC. Afterwards, all specimens were submitted to abrasive challenge by a brushing cycle performed with a 200 g weight at a speed of 356 rpm, totaling 17.8 cycles. Surface roughness measurements (Ra) were performed and analyzed by ANOVA and Tukey test (p≤0.05). Surface roughness values were higher in the presence (1.07±0.24) as compared with the absence of hydrochloric acid (0.72±0.04). Surface roughness values were higher for microhybrid (1.01±0.27) compared with nanofilled (0.68 ±0.09) and nanohybrid (0.48±0.15) composites when the specimens were not subjects to acid challenge. In the presence of hydrochloric acid, microhybrid (1.26±0.28) and nanofilled (1.18±0,30) composites presents higher surface roughness values compared with nanohybrid (0.77±0.15). The hydrochloric acid affected the surface roughness of composite resin subjected to brushing.

Phosphine polymerization by nitric oxide: experimental characterization and theoretical predictions of mechanism.

PubMed

Zhao, Yi-Lei; Flora, Jason W; Thweatt, William David; Garrison, Stephen L; Gonzalez, Carlos; Houk, K N; Marquez, Manuel

2009-02-02

A yellow solid material [P(x)H(y)] has been obtained in the reaction of phosphine (PH(3)) and nitric oxide (NO) at room temperature and characterized by thermogravimetric analysis mass spectrometry (TGA-MS) and attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy. In this work using complete basis set (CBS-QB3) methods a plausible mechanism has been investigated for phosphine polymerization in the presence of nitric oxide (NO). Theoretical explorations with the ab initio method suggest (a) instead of the monomer the nitric oxide dimer acts as an initial oxidant, (b) the resulting phosphine oxides (H(3)P=O <--> H(3)P(+)O(-)) in the gas phase draw each other via strong dipolar interactions between the P-O groups, and (c) consequently an autocatalyzed polymerization occurs among the phosphine oxides, forming P-P chemical bonds and losing water. The possible structures of polyhydride phosphorus polymer were discussed. In the calculations a series of cluster models was computed to simulate polymerization.

Chiral and achiral phosphine derivatives of alkylidyne tricobalt carbonyl clusters as catalyst precursors for (asymmetric) inter- and intramolecular Pauson-Khand reactions.

PubMed

Moberg, Viktor; Mottalib, M Abdul; Sauer, Désirée; Poplavskaya, Yulia; Craig, Donald C; Colbran, Stephen B; Deeming, Antony J; Nordlander, Ebbe

2008-05-14

Phosphine derivatives of alkylidyne tricobalt carbonyl clusters have been tested as catalysts/catalyst precursors in intermolecular and (asymmetric) intramolecular Pauson-Khand reactions. A number of new phosphine derivatives of the tricobalt alkylidyne clusters [Co3(micro3-CR)(CO)9] (R = H, CO2Et) were prepared and characterised. The clusters [Co3(micro3-CR)(CO)9-x(PR'3)x] (PR'3 = achiral or chiral monodentate phosphine, x = 1-3) and [Co3(micro3-CR)(CO)7)(P-P)] (P-P = chiral diphosphine; 1,1'- and 1,2-structural isomers) were assayed as catalysts for intermolecular and (asymmetric) intramolecular Pauson-Khand reactions. The phosphine-substituted tricobalt clusters proved to be viable catalysts/catalyst precursors that gave moderate to very good product yields (up to approximately 90%), but the enantiomeric excesses were too low for the clusters to be of practical use in the asymmetric reactions.

Determining resin/fiber content of laminates

NASA Technical Reports Server (NTRS)

Garrard, G. G.; Houston, D. W.

1979-01-01

Article discusses procedure where hydrazine is used to extract graphite fibers from cured polyimide resin. Method does not attack graphite fibers and is faster than hot-concentrated-acid digestion process.

A new configuration of membrane stack for retrieval of nickel absorbed in resins*

PubMed Central

Chen, Xue-fen; Wu, Zu-cheng

2005-01-01

A new configuration integrated ion exchange effect with both electro-migration and electrochemical reaction in a single cell was developed to effectively retrieve metal ions from simulated wastewater using ion exchange resins without additive chemicals. By simply assembling cation exchange resins and anion exchange resins separated by homogeneous membranes, we found that the system will always be acidic in the concentrate compartment so that ion exchange resins could be in-situ regenerated without hydroxide precipitation. Such a realizable design will be really suitable for wastewater purification. PMID:15909341

Resin-Bound Crypto-Thioester for Native Chemical Ligation.

PubMed

Naruse, Naoto; Ohkawachi, Kento; Inokuma, Tsubasa; Shigenaga, Akira; Otaka, Akira

2018-04-20

The resin-bound N-sulfanylethylanilide (SEAlide) peptide was found to function as a crypto-thioester peptide. Exposure of the peptide resin to an aqueous solution under neutral conditions in the presence of thiols affords thioesters without accompanying racemization of C-terminal amino acids. Furthermore, the resin-bound SEAlide peptides react with N-terminal cysteinyl peptides in the absence of phosphate salts to afford ligated products, whereas soluble SEAlide peptides do not. This unexpected difference in reactivity of the SEAlide peptides allows for a one-pot/three-fragment ligation using resin-bound and unbound peptides.

Electrochemistry of 1,1'-bis(2,4-dialkylphosphetanyl)ferrocene and 1,1'-bis(2,5-dialkylphospholanyl)ferrocene ligands: free phosphines, metal complexes, and chalcogenides.

PubMed

Mandell, Chelsea L; Kleinbach, Shannon S; Dougherty, William G; Kassel, W Scott; Nataro, Chip

2010-10-18

The oxidative electrochemistries of a series of chiral bisphosphinoferrocene ligands, 1,1'-bis(2,4-dialkylphosphetanyl)ferrocene (FerroTANE) and 1,1'-bis(2,5-dialkylphospholanyl)ferrocene (FerroLANE), were examined. The reversibility of the oxidation is sensitive to the steric bulk of the alkyl groups. New transition metal compounds and phosphine chalcogenides of these ligands were prepared and characterized. X-ray crystal structures of 10 of these compounds are reported. The percent buried volume (%V(bur)) is a recently developed measurement based on crystallographic data that examines the steric bulk of N-heterocyclic carbene and phosphine ligands. The %V(bur) for the FerroTANE and FerroLANE structures with methyl or ethyl substituents suggests these ligands are similar in steric properties to 1,1'-bis(diphenylphosphino)ferrocene (dppf). In addition the %V(bur) has been found to correlate well with the Tolman cone angle for phosphine chalcogenides. The oxidative electrochemistries of the transition metal complexes occur at more positive potentials than the free ligands. While a similar positive shift is seen for the oxidative electrochemistries of the phosphine chalcogenides, the oxidation of the phosphine selenides does not occur at the iron center, but rather oxidation occurs at the selenium atoms.

Effect of surface treatment methods on the shear bond strength of auto-polymerized resin to thermoplastic denture base polymer.

PubMed

Koodaryan, Roodabeh; Hafezeqoran, Ali

2016-12-01

Polyamide polymers do not provide sufficient bond strength to auto-polymerized resins for repairing fractured denture or replacing dislodged denture teeth. Limited treatment methods have been developed to improve the bond strength between auto-polymerized reline resins and polyamide denture base materials. The objective of the present study was to evaluate the effect of surface modification by acetic acid on surface characteristics and bond strength of reline resin to polyamide denture base. 84 polyamide specimens were divided into three surface treatment groups (n=28): control (N), silica-coated (S), and acid-treated (A). Two different auto-polymerized reline resins GC and Triplex resins were bonded to the samples (subgroups T and G, respectively, n=14). The specimens were subjected to shear bond strength test after they were stored in distilled water for 1 week and thermo-cycled for 5000 cycles. Data were analyzed with independent t-test, two-way analysis of variance (ANOVA), and Tukey's post hoc multiple comparison test (α=.05). The bond strength values of A and S were significantly higher than those of N ( P <.001 for both). However, statistically significant difference was not observed between group A and group S. According to the independent Student's t-test, the shear bond strength values of AT were significantly higher than those of AG ( P <.001). The surface treatment of polyamide denture base materials with acetic acid may be an efficient and cost-effective method for increasing the shear bond strength to auto-polymerized reline resin.

Control of resin production in Araucaria angustifolia, an ancient South American conifer.

PubMed

Perotti, J C; da Silva Rodrigues-Corrêa, K C; Fett-Neto, A G

2015-07-01

Araucaria angustifolia is an ancient slow-growing conifer that characterises parts of the Southern Atlantic Forest biome, currently listed as a critically endangered species. The species also produces bark resin, although the factors controlling its resinosis are largely unknown. To better understand this defence-related process, we examined the resin exudation response of A. angustifolia upon treatment with well-known chemical stimulators used in fast-growing conifers producing both bark and wood resin, such as Pinus elliottii. The initial hypothesis was that A. angustifolia would display significant differences in the regulation of resinosis. The effect of Ethrel(®) (ET - ethylene precursor), salicylic acid (SA), jasmonic acid (JA), sulphuric acid (SuA) and sodium nitroprusside (SNP - nitric oxide donor) on resin yield and composition in young plants of A. angustifolia was examined. In at least one of the concentrations tested, and frequently in more than one, an aqueous glycerol solution applied on fresh wound sites of the stem with one or more of the adjuvants examined promoted an increase in resin yield, as well as monoterpene concentration (α-pinene, β-pinene, camphene and limonene). Higher yields and longer exudation periods were observed with JA and ET, another feature shared with Pinus resinosis. The results suggest that resinosis control is similar in Araucaria and Pinus. In addition, A. angustifolia resin may be a relevant source of valuable terpene chemicals, whose production may be increased by using stimulating pastes containing the identified adjuvants. © 2014 German Botanical Society and The Royal Botanical Society of the Netherlands.

Oxygenated Phosphine Fumigation for Control of Light Brown Apple Moth (Lepidoptera: Tortricidae) Eggs on Cut-Flowers.

PubMed

Liu, Samuel S; Liu, Yong-Biao; Simmons, Gregory S

2015-08-01

Light brown apple moth, Epiphyas postvittana (Walker), eggs were subjected to oxygenated phosphine fumigation treatments under 70% oxygen on cut flowers to determine efficacy and safety. Five cut flower species: roses, lilies, tulips, gerbera daisy, and pompon chrysanthemums, were fumigated in separate groups with 2,500 ppm phosphine for 72 h at 5°C. Egg mortality and postharvest quality of cut flowers were determined after fumigation. Egg mortalities of 99.7-100% were achieved among the cut flower species. The treatment was safe to all cut flowers except gerbera daisy. A 96-h fumigation treatment with 2,200 ppm phosphine of eggs on chrysanthemums cut flowers also did not achieve complete control of light brown apple moth eggs. A simulation of fumigation in hermetically sealed fumigation chambers with gerbera daisy showed significant accumulations of carbon dioxide and ethylene by the end of 72-h sealing. However, oxygenated phosphine fumigations with carbon dioxide and ethylene absorbents did not reduce the injury to gerbera daisy, indicating that it is likely that phosphine may directly cause the injury to gerbera daisy cut flowers. The study demonstrated that oxygenated phosphine fumigation is effective against light brown apple moth eggs. However, it may not be able to achieve the probit9 quarantine level of control and the treatment was safe to most of the cut flower species. Published by Oxford University Press on behalf of Entomological Society of America 2015. This work is written by US Government employees and is in the public domain in the US.

Effect of surface treatments on the bond strength of soft denture lining materials to an acrylic resin denture base.

PubMed

Gundogdu, Mustafa; Yesil Duymus, Zeynep; Alkurt, Murat

2014-10-01

Adhesive failure between acrylic resin and resilient liner material is commonly encountered in clinical practice. The purpose of this study was to evaluate the effect of different surface treatments on the bond strength of 2 different resilient lining materials to an acrylic resin denture base. Ninety-six dumbbell-shaped specimens were fabricated from heat-polymerized acrylic resin, and 3 mm of the material was cut from the thin midsection. The specimens were divided into 6 groups according to their surface treatments: no surface treatment (control group), 36% phosphoric acid etching (acid group), erbium:yttrium-aluminum-garnet (Er:YAG) laser (laser group), airborne-particle abrasion with 50-μm Al2O3 particles (abrasion group), an acid+laser group, and an abrasion+laser group. The specimens in each group were divided into 2 subgroups according to the resilient lining material used: heat-polymerized silicone based resilient liner (Molloplast B) and autopolymerized silicone-based resilient liner (Ufi Gel P). After all of the specimens had been polymerized, they were stored in distilled water at 37°C for 1 week. A tensile bond strength test was then performed. Data were analyzed with a 2-way ANOVA, and the Sidak multiple comparison test was used to identify significant differences (α=.05). The effects of the surface treatments and resilient lining materials on the surface of the denture base resin were examined with scanning electron microscopy. The tensile bond strength was significantly different between Molloplast B and Ufi Gel P (P<.001). The specimens of the acid group had the highest tensile bond strength, whereas those of the abrasion group had the lowest tensile bond strength. The scanning electron microscopy observations showed that the application of surface treatments modified the surface of the denture base resin. Molloplast B exhibited significantly higher bond strength than Ufi Gel P. Altering the surface of the acrylic resin denture base with 36% phosphoric acid etching increased bond strength. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Cyclam Derivatives with a Bis(phosphinate) or a Phosphinato-Phosphonate Pendant Arm: Ligands for Fast and Efficient Copper(II) Complexation for Nuclear Medical Applications.

PubMed

David, Tomáš; Kubíček, Vojtěch; Gutten, Ondrej; Lubal, Přemysl; Kotek, Jan; Pietzsch, Hans-Jürgen; Rulíšek, Lubomír; Hermann, Petr

2015-12-21

Cyclam derivatives bearing one geminal bis(phosphinic acid), -CH2PO2HCH2PO2H2 (H2L(1)), or phosphinic-phosphonic acid, -CH2PO2HCH2PO3H2 (H3L(2)), pendant arm were synthesized and studied as potential copper(II) chelators for nuclear medical applications. The ligands showed good selectivity for copper(II) over zinc(II) and nickel(II) ions (log KCuL = 25.8 and 27.7 for H2L(1) and H3L(2), respectively). Kinetic study revealed an unusual three-step complex formation mechanism. The initial equilibrium step leads to out-of-cage complexes with Cu(2+) bound by the phosphorus-containing pendant arm. These species quickly rearrange to an in-cage complex with cyclam conformation II, which isomerizes to another in-cage complex with cyclam conformation I. The first in-cage complex is quantitatively formed in seconds (pH ≈5, 25 °C, Cu:L = 1:1, cM ≈ 1 mM). At pH >12, I isomers undergo nitrogen atom inversion, leading to III isomers; the structure of the III-[Cu(HL(2))] complex in the solid state was confirmed by X-ray diffraction analysis. In an alkaline solution, interconversion of the I and III isomers is mutual, leading to the same equilibrium isomeric mixture; such behavior has been observed here for the first time for copper(II) complexes of cyclam derivatives. Quantum-chemical calculations showed small energetic differences between the isomeric complexes of H3L(2) compared with analogous data for isomeric complexes of cyclam derivatives with one or two methylphosphonic acid pendant arm(s). Acid-assisted dissociation proved the kinetic inertness of the complexes. Preliminary radiolabeling of H2L(1) and H3L(2) with (64)Cu was fast and efficient, even at room temperature, giving specific activities of around 70 GBq of (64)Cu per 1 μmol of the ligand (pH 6.2, 10 min, ca. 90 equiv of the ligand). These specific activities were much higher than those of H3nota and H4dota complexes prepared under identical conditions. The rare combination of simple ligand synthesis, very fast copper(II) complex formation, high thermodynamic stability, kinetic inertness, efficient radiolabeling, and expected low bone tissue affinity makes such ligands suitably predisposed to serve as chelators of copper radioisotopes in nuclear medicine.

Technology development for phosphoric acid fuel cell powerplant, phase 2

NASA Technical Reports Server (NTRS)

Christner, L.

1979-01-01

A technique for producing an acid inventory control member by spraying FEP onto a partially screened carbon paper backing is discussed. Theoretical analysis of the acid management indicates that the vapor composition of 103% H3PO4 is approximately 1.0 ppm P4O10. An SEM evaluation of corrosion resistance of phenolic resins and graphite/phenolic resin composites in H3PO4 at 185 C shows specific surface etching. Carbonization of graphite/phenolic bipolar plates is achieved without blistering.

The effect of diamic acid additives on the dielectric constant of polyimides

NASA Technical Reports Server (NTRS)

Stoakley, Diane M.; St. Clair, Anne K.

1988-01-01

The effect of six selected diamic acids additives (including 2,2-prime bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride-aniline (An); 4,4-prime-oxydiphthalic anhydride-An, 3,3-prime diaminodiphenyl sulfone-phthalic anhydride (PA); 4,4-prime-oxydianiline-PA; 2,2-bis 4(4-aminophenoxy)phenyl hexafluoropropane-PA; and 2,2-bis 4(3-aminophenoxy)phenyl hexafluoropropane-PA) on the dielectric constants of low-dielectric-constant polyimide resins was evaluated. It was found that the effect of the incorporation of the diamic acids on reducing the dielectric constant of polyimides may be limited as the dielectric constant of the base resin itself becomes very low. The additives were found to lower the resin's values of glass transition temperature, with no effect on thermooxidative stability.

Commercial Ion Exchange Resin Vitrification in Borosilicate Glass

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cicero-Herman, C.A.; Workman, P.; Poole, K.

1998-05-01

Bench-scale studies were performed to determine the feasibility of vitrification treatment of six resins representative of those used in the commercial nuclear industry. Each resin was successfully immobilized using the same proprietary borosilicate glass formulation. Waste loadings varied from 38 to 70 g of resin/100 g of glass produced depending on the particular resin, with volume reductions of 28 percent to 68 percent. The bench-scale results were used to perform a melter demonstration with one of the resins at the Clemson Environmental Technologies Laboratory (CETL). The resin used was a weakly acidic meth acrylic cation exchange resin. The vitrification processmore » utilized represented a approximately 64 percent volume reduction. Glass characterization, radionuclide retention, offgas analyses, and system compatibility results will be discussed in this paper.« less

Comparing the variation of needle and wood terpenoids in Scots pine provenances.

PubMed

Manninen, A M; Tarhanen, S; Vuorinen, M; Kainulaine, P

2002-01-01

We determined variation in both the concentration and composition of terpenoids in needles and wood within nine Scots pine (Pinus sylvestris) provenances. Seedlings of different provenances representing a 1200-km N-S transect from Estonia to northern Finland were cultivated in Suonenjoki nursery field, central Finland, for seven years. Growth of seedlings and the number of vertical resin ducts in wood were also determined. alpha-Pinene and 3-carene were the major monoterpenes both in the needles and wood. The total monoterpene concentration was about five times higher in the needles than in the wood. A strong positive correlation was found between proportional quantities of several terpenes of the needles and wood, particularly for 3-carene, sabinene, and terpinolene. The needles contained both labdane-type and tricyclic resin acids, whereas the wood contained only tricyclic ones. The wood had a four times higher tricyclic resin acid concentration than the needles. The highest total monoterpene concentration in the needles and in the wood occurred in the most northern Muonio provenance and in the most southern Saaremaa provenance plants, respectively. The amount of high 3-carene genotype trees decreased among the northern provenances. The wood of the most northern Muonio provenance showed the lowest total resin acid concentration, but provenance did not affect total tricyclic resin acids in the needles. Korpilahti provenance trees from central Finland had the best growth in height. In addition, Korpilahti and Ruokolahti provenance trees showed largest radial growth of stem and smallest number of vertical resin ducts. The results suggest that especially the proportional quantity of 3-carene in the needles could be used in estimating the amount of this compound in the wood and vice versa.

Characterization of an anti-tuberculosis resin glycoside from the prairie medicinal plant Ipomoea leptophylla.

PubMed

Barnes, Curtis C; Smalley, Mary K; Manfredi, Kirk P; Kindscher, Kelly; Loring, Hillary; Sheeley, Douglas M

2003-11-01

The organic soluble extract from the leaves of the native North American prairie plant Ipomoea leptophylla (big root morning glory) showed in vitro activity against M. tuberculosis. Bioassay-guided fractionation of this extract resulted in the identification of two new resin glycosides (6, 7). Base-catalyzed hydrolysis of these glycosides gave operculinic acid (1) as the glycosidic acid component as well as trans-cinnamic acid, propanoic acid, and lauric acid. The complete structure elucidation was accomplished through derivatization, 1D and 2D NMR spectroscopy (TOCSY, ROESY, HSQC, HMBC), and MS/MS experiments on 6 and 7 as well as the permethylated derivative 8.

Human brain somatostatin release from isolated cortical nerve endings and its modulation through GABAB receptors.

PubMed Central

Bonanno, G.; Gemignani, A.; Schmid, G.; Severi, P.; Cavazzani, P.; Raiteri, M.

1996-01-01

1. The release of somatostatin-like immunoreactivity (SRIF-LI) in the human brain was studied in synaptosomal preparations from fresh neocortical specimens obtained from patients undergoing neurosurgery to remove deeply sited tumours. 2. The basal outflow of SRIF-LI from superfused synaptosomes was increased about 3 fold during exposure to a depolarizing medium containing 15 mM KCl. The K(+)-evoked overflow of SRIF-LI was almost totally dependent on the presence of Ca2+ in the superfusion medium. 3. The GABAB receptor agonist, (-)-baclofen (0.3 - 100 microM), inhibited the overflow of SRIF-LI in a concentration-dependent manner (EC50 = 1.84 +/- 0.20 microM; maximal effect: about 50%). The novel GABAB receptor ligand, 3-aminopropyl(difluoromethyl)phosphinic acid (CGP 47656) mimicked (-)-baclofen in inhibiting the SRIF-LI overflow (EC50 = 3.06 +/- 0.52 microM; maximal effect: about 50%), whereas the GABAA receptor agonist, muscimol, was ineffective up to 100 microM. 4. The inhibition by 10 microM (-)-baclofen of the K(+)-evoked SRIF-LI overflow was concentration-dependently prevented by two selective GABAB receptor antagonists, 3-amino-propyl (diethoxymethyl)-phosphinic acid (CGP 35348) (IC50 = 24.40 +/- 2.52 microM) and [3-[[(3,4-dichlorophenyl) methyl]amino]propyl] (diethoxymethyl) phosphinic acid (CGP 52432) (IC50 = 0.06 +/- 0.005 microM). 5. The inhibition of SRIF-LI overflow caused by 10 microM CGP 47656 was abolished by 1 microM CGP 52432. 6. When human synaptosomes were labelled with [3H]-GABA and depolarized in superfusion with 15 mM KCl, the inhibition by 10 microM (-)-baclofen of the depolarization-evoked [3H]-GABA overflow was largely prevented by 10 microM CGP 47656 which therefore behaved as an autoreceptor antagonist. 7. In conclusion: (a) the characteristics of SRIF-LI release from synaptosomal preparations of human neocortex are compatible with a neuronal origin; (b) the nerve terminals releasing the neuropeptide possess inhibitory receptors of the GABAB type; (c) these receptors differ pharmacologically from the GABAB autoreceptors present on human neocortex nerve terminals since the latter have been shown to be CGP 35348-insensitive but can be blocked by CGP 47656. PMID:8832070

Low Cost Aromatic Acetylene and Oligomeric Benzils and Their Conversion to Acetylene Terminated Quinoxalines

DTIC Science & Technology

1982-07-01

palladium acetate and the appropriate phosphine . This procedure is known to be effective for bromoarenes. In the early screen- ing runs, 4...Delaware), he indicated that he also had screened many phosphines , and the likelihood of success was very small. Dr. Heck reported that the palladium...any simple modification of the palla- dium phosphine catalyst system will effect the desired reaction. 5 III. PREPARATION OF OLIGOMERIC BENZILS AND

Photoinduced reductive perfluoroalkylation of phosphine oxides: synthesis of P-perfluoroalkylated phosphines using TMDPO and perfluoroalkyl iodides.

PubMed

Sato, Yuki; Kawaguchi, Shin-ichi; Ogawa, Akiya

2015-07-04

A photoinduced reaction between TMDPO (diphenyl(2,4,6-trimethylbenzoyl)-phosphine oxide) and perfluoroalkyl iodides successfully affords P-(perfluoroalkyl)diphenylphosphines as promising ligands for recyclable catalysts. Interestingly, the perfluoroalkylation reaction involves the reduction of phosphorus(V) compounds to phosphorus(III) species. The advantages of the present reaction include the use of an air-stable phosphorus source and good yields of P-perfluoroalkylphosphines in short reaction times.

[Study of purity tests for silicone resins].

PubMed

Sato, Kyoko; Otsuki, Noriko; Ohori, Akio; Chinda, Mitsuru; Furusho, Noriko; Osako, Tsutomu; Akiyama, Hiroshi; Kawamura, Yoko

2012-01-01

In the 8th edition of Japan's Specifications and Standards for Food Additives, the purity test for silicone resins requires the determination of the refractive index and kinetic viscosity of the extracted silicone oil, and allows for only a limited amount of silicon dioxide. In the purity test, carbon tetrachloride is used to separate the silicone oil and silicon dioxide. To exclude carbon tetrachloride, methods were developed for separating the silicone oil and silicon dioxide from silicone resin, which use hexane and 10% n-dodecylbenzenesulfonic acid in hexane. For silicone oil, the measured refractive index and kinetic viscosity of the silicone oil obtained from the hexane extract were shown to be equivalent to those of the intact silicone oil. In regard to silicon dioxide, it was confirmed that, following the separation with 10% n-dodecylbenzenesulfonic acid in hexane, the level of silicon dioxide in silicone resin can be accurately determined. Therefore, in this study, we developed a method for testing the purity of silicone resins without the use of carbon tetrachloride, which is a harmful reagent.

The management of defective resin composite restorations: current trends in dental school teaching in Japan.

PubMed

Lynch, C D; Hayashi, M; Seow, L L; Blum, I R; Wilson, N H F

2013-01-01

The aim of this article is to investigate the contemporary teaching of the management of defective direct resin composite restorations in dental schools in Japan. A questionnaire relating to the teaching of the management of defective resin composite restorations was developed and e-mailed to 29 dental schools in Japan in 2010. Completed responses were received from 19 of the 29 invited schools (response rate = 66%). Eighteen schools (95%) report that they included the teaching of repair of direct defective resin composite restorations in their dental school programs. Thirteen schools reported that they included both clinical and didactic instruction on the repair of direct resin composite restorations. Fourteen schools did not teach any mechanical roughening of the exposed resin composite restoration surface before undertaking a repair. The most commonly reported treatment was acid etching with phosphoric acid (12 schools). The most commonly taught material for completing repairs was a flowable resin composite (16 schools). The teaching of repair of defective resin composite restorations is well established within many Japanese dental schools, to a greater extent than in some other regions of the world. The impact of this teaching on subsequent clinical practices in Japan should be investigated. Furthermore, it is concluded that there is a need for much stronger leadership in operative and conservative dentistry, ideally at the global level, to resolve differences in key aspects of operative procedures such as repairs.

21 CFR 177.1655 - Polysulfone resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

...)(2) of this section. (c) Polysulfone resins, when extracted at reflux temperatures for 6 hours with... acetic acid in distilled water, and n-heptane, yield total extractives in each extracting solvent not to...

21 CFR 177.1655 - Polysulfone resins.

Code of Federal Regulations, 2012 CFR

2012-04-01

...)(2) of this section. (c) Polysulfone resins, when extracted at reflux temperatures for 6 hours with... acetic acid in distilled water, and n-heptane, yield total extractives in each extracting solvent not to...

21 CFR 177.1655 - Polysulfone resins.

Code of Federal Regulations, 2013 CFR

2013-04-01

...)(2) of this section. (c) Polysulfone resins, when extracted at reflux temperatures for 6 hours with... acetic acid in distilled water, and n-heptane, yield total extractives in each extracting solvent not to...

ADSORPTION METHOD FOR SEPARATING THORIUM VALUES FROM URANIUM VALUES

DOEpatents

Boyd, G.E.; Russell, E.R.; Schubert, J.

1959-08-01

An improved ion exchange method is described for recovery of uranium and thorium values as separate functions from an aqueous acidic solution containing less than 10/sup -3/ M thorium ions and between 0.1 and 1 M uranyl ions. The solution is passed through a bed of cation exchange resin in the acid form to adsorb all the thorium ions and a portion of the uranyl ions. The uranium is eluted by means of aqueous 0.1 to 0.4 M sulfuric acid. The thorium may then be stripped from the resin by elution with aqueous 0.5 M oxalic acid.

ADSORPTION METHOD FOR SEPARATING THORIUM VALUES FROM URANIUM VALUES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Boyd, G.E.; Russell, E.R.; Schubert, J.

An improved ion exchange method is described for recovery of uranium and thorium values as separate functions from an aqueous acidic solution containing less than 10/sup -3/ M thorium ions and between 0.1 and 1 M uranyl ions. The solution is passed through a bed of cation exchange resin in the acid form to adsorb all the thorium ions and a portion of the uranyl ions. The uranium is eluted by means of aqueous 0.1 to 0.4 M sulfuric acid. The thorium may then be stripped from the resin by elution with aqueous 0.5 M oxalic acid.

Self-etching adhesive on intact enamel, with and without pre-etching.

PubMed

Devarasa, G M; Subba Reddy, V V; Chaitra, N L; Swarna, Y M

2012-05-01

Bond strengths of composite resin to enamel using self-etch adhesive (SEA) Clearfil SE bond system on intact enamel and enamel pre-etched with phosphoric acid were compared. The objective was to determine if the pre-etching would increase the bond strengths of the SEA systems to intact enamel and to evaluate the effect of pre-etching on bond formation of self-etch adhesives on intact enamel. Labial surfaces of 40 caries free permanent upper central and lateral incisors were cleaned, sectioned of their roots. All specimens were mounted on acrylic block and divided randomly into four groups. In two groups the application of self-etch adhesive, Clearfil SE bond was carried as per manufacturer's instructions, composite cylinders were built, whereas in the other two groups, 37% phosphoric acid etching was done before the application of self-etching adhesives. Then the resin tags were analyzed using scanning electron microscope and shear bond strength was measured using Instron universal testing machine. When phosphoric acid was used, there was significant increase in the depth of penetration of resin tags and in the Shear Bond Strength of composite to enamel. The results indicate that out of both treatment groups, pre-etching the intact enamel with 37% phosphoric acid resulted in formation of longer resin tags and higher depth of penetration of resin tags of the Clearfil SE bond, and attaining higher bond strength of the Clearfil SE bond to intact enamel. Copyright © 2011 Wiley Periodicals, Inc.

Preparation of an amphiphilic resin-supported BINAP ligand and its use for rhodium-catalyzed asymmetric 1,4-addition of phenylboronic acid in water.

PubMed

Otomaru, Yusuke; Senda, Taichi; Hayashi, Tamio

2004-09-16

[reaction: see text] The axially chiral bisphosphine ligand, 2,2'-bis(diphenylphosphino)-1,1'-binaphthyl (binap), was supported on a polystyrene-poly(ethylene glycol) copolymer (PS-PEG) resin and was used successfully for the rhodium-catalyzed asymmetric 1,4-addition of phenylboronic acid to alpha,beta-unsaturated ketones in water.

Analysis of Commercial Unsaturated Polyester Repair Resins

DTIC Science & Technology

2009-07-01

resins utilizing renewable fatty acid -based monomers. 15. SUBJECT TERMS vinyl ester, styrene, fatty acid monomers, HAP, triglycerides 16. SECURITY...criteria for selecting the appropriate repair include whether the component can be removed and whether the back side is accessible. For a typical moderate...field repair, any remaining coating in the repair area is removed by hand sanding or portable tools. Damage is cut out in an appropriate

SPPS of protected peptidyl aminoalkyl amides.

PubMed

Karavoltsos, Manolis; Mourtas, Spyros; Gatos, Dimitrios; Barlos, Kleomenis

2002-11-01

Monophthaloyl diamines derived from naturally occurring amino acids were attached through their free amino functions to resins of the trityl type. The phthaloyl groups were removed by hydrazinolysis, and peptide chains were assembled using Fmoc/tBu-amino acids on the liberated amino functions. The peptidyl aminoalkyl amides obtained were cleaved from the resins by mild acidolysis, with the tBu-side chain protection remaining intact.

Improved bonding of adhesive resin to sintered porcelain with the combination of acid etching and a two-liquid silane conditioner.

PubMed

Kato, H; Matsumura, H; Ide, T; Atsuta, M

2001-01-01

This study determined the bond strengths of adhesive resins joined to a feldspathic porcelain (VMK 68) for the purpose of developing the most durable surface preparation for the porcelain. Three porcelain surfaces-ground, air-abraded with alumina, and etched with hydrofluoric acid-were prepared. A two-liquid porcelain conditioner that contained both 4-methacryloyloxyethyl trimellitate anhydride (4-META) and a silane coupler (Porcelain Liner M) was used as the priming agent. Each of the two liquid components of the conditioner was also used individually in order to examine the effects of the respective chemical ingredients on adhesive bonding. Two methyl methacrylate (MMA)-based resins initiated with tri-n-butylborane (TBB) either with or without 4-META (MMA-TBB and 4-META/MMA-TBB resins) were used as the luting agents. Shear bond strengths were determined both before and after thermocycling. Shear testing results indicated that thermocycling was effective for disclosing poor bonding systems, and that both mechanical and chemical retention were indispensable for bonding the porcelain. Of the combinations assessed, etching with hydrofluoric acid followed by two-liquid priming with the Porcelain Liner M material generated the most durable bond strength (33.3 MPa) for the porcelain bonded with the 4-META/MMA-TBB resin (Super-Bond C&B).

Reactions of nitroxides 15. Cinnamates bearing a nitroxyl moiety synthesized using a Mizoroki–Heck cross-coupling reaction

PubMed Central

Huras, Bogumiła

2015-01-01

Summary Cinnamic acid derivatives bearing a nitroxyl moiety (2,2,6,6-tetramethyl-1-oxyl-4-piperidyl 3-E-aryl acrylates) were synthesized in 30–100% yield using a Mizoroki–Heck cross-coupling reaction between 4-acryloyloxy-2,2,6,6-tetramethylpiperidine-1-oxyl and iodobenzene derivatives in the presence of palladium(II) acetate coordinated with a tri(o-tolyl)phosphine ligand immobilized in a polyurea matrix. PMID:26199672

21 CFR 177.2500 - Polyphenylene sulfone resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

... consist of basic resin produced by reacting polyphenylene sulfide with peracetic acid such that the... sanction or approval. (c) Specifications. The glass transition temperature of the polymer is 360±5 °C as...

21 CFR 177.2500 - Polyphenylene sulfone resins.

Code of Federal Regulations, 2011 CFR

2011-04-01

... consist of basic resin produced by reacting polyphenylene sulfide with peracetic acid such that the... sanction or approval. (c) Specifications. The glass transition temperature of the polymer is 360±5 °C as...

Rechargeable infection-responsive antifungal denture materials.

PubMed

Cao, Z; Sun, X; Yeh, C-K; Sun, Y

2010-12-01

Candida-associated denture stomatitis (CADS) is a significant clinical concern. We developed rechargeable infection-responsive antifungal denture materials for potentially managing the disease. Polymethacrylic acid (PMAA) was covalently bound onto diurethane dimethacrylate denture resins in the curing step. The PMAA resins bound cationic antifungal drugs such as miconazole and chlorhexidine digluconate (CG) through ionic interactions. The anticandidal activities of the drug-containing PMAA-resin discs were sustained for a prolonged period of time (weeks and months). Drug release was much faster at acidic conditions (pH 5) than at pH 7. Drugs bound to the denture materials could be "washed out" by treatment with EDTA, and the drug-depleted resins could be recharged with the same or a different class of anticandidal drugs. These results suggest clinical potential of the newly developed antifungal denture materials in the management of CADS and other infectious conditions.

Low-Melt Polyamic Acid Based Powder Coatings

NASA Technical Reports Server (NTRS)

Jolley, Scott T. (Inventor)

2017-01-01

The present invention is directed to a method for powder coating a metal substrate using a low-melt polyamic acid (PAA) polymer that readily imidizes to polyimides. These low-melt PAAs have been shown to be useful in resins applied as powder coatings to metal surfaces. The resin includes an end-capping material capable of providing crosslinking functionality to at least one end of the low-melt PAA polymer. The end-capping material functions dually as a polymerization chain terminator and crosslinking agent, thus producing resins that have molecular weights low enough to flow well and form good cured films applicable for use in powder coating.

ION EXCHANGE ADSORPTION PROCESS FOR PLUTONIUM SEPARATION

DOEpatents

Boyd, G.E.; Russell, E.R.; Taylor, M.D.

1961-07-11

Ion exchange processes for the separation of plutonium from fission products are described. In accordance with these processes an aqueous solution containing plutonium and fission products is contacted with a cation exchange resin under conditions favoring adsorption of plutonium and fission products on the resin. A portion of the fission product is then eluted with a solution containing 0.05 to 1% by weight of a carboxylic acid. Plutonium is next eluted with a solution containing 2 to 8 per cent by weight of the same carboxylic acid, and the remaining fission products on the resin are eluted with an aqueous solution containing over 10 per cent by weight of sodium bisulfate.

Purification of organic acids by chromatography with strong anionic resins: Investigation of uptake mechanisms.

PubMed

Lemaire, Julien; Blanc, Claire-Line; Lutin, Florence; Théoleyre, Marc-André; Stambouli, Moncef; Pareau, Dominique

2016-08-05

Bio-based organic acids are promising renewable carbon sources for the chemical industry. However energy-consuming purification processes are used, like distillation or crystallization, to reach high purities required in some applications. That is why preparative chromatography was studied as an alternative separation technique. In a previous work dealing with the purification of lactic, succinic and citric acids, the Langmuir model was insufficient to explain the elution profiles obtained with a strong anionic resin. Consequently the Langmuir model was coupled with a usual ion-exchange model to take into account the retention of their conjugate bases (<2%), which are commonly neglected at low pH (<1.5). Elution simulations with both uptake mechanisms fitted very well with experimental pulse tests. Only two parameters were optimized (equilibrium constant of acid uptake and ion-exchange selectivity coefficient of conjugate base) and their value were coherent with experimental and resin suppliers' data. These results confirmed that the singular tailing and apparent delay observed with succinic and citric acids can be explained by the high affinity of succinate and citrate for resin cationic sites. The model was implemented in a preparative chromatography simulation program in order to optimize operating parameters of our pilot-scale ISMB unit (Improved Simulated Moving Bed). The comparison with experimental ISMB profiles was conclusive. Copyright © 2016 Elsevier B.V. All rights reserved.

Secondary metabolite concentrations and terpene emissions of Scots pine xylem after long-term forest fertilization.

PubMed

Turtola, S; Manninen, A M; Holopainen, J K; Levula, T; Raitio, H; Kainulainen, P

2002-01-01

Secondary compounds are known to be associated with the resistance of conifer xylem against insects and fungi. The effects of long-term forest fertilization with nitrogen (N) or with N, calcium (Ca), and phosphorus (P) on secondary compounds in the xylem of 50-yr-old Scots pine (Pinus sylvestris L.) trees were examined. Xylem samples were collected from trees growing in three locations in southern Finland: Vilppula, Padasjoki, and Punkaharju. Forests were fertilized every fifth (Vilppula and Padasjoki) or tenth (Punkaharju) year since the 1950s. We compared concentrations of individual and total monoterpenes and resin acids in the heartwood and sapwood of Scots pine. Terpene emissions were analyzed from the sapwood and total phenolics from the heartwood. Fertilization did not have any significant effect on the concentrations and emissions of xylem monoterpenes. Concentrations of several individual terpenes in sapwood were positively correlated with the corresponding terpene emission. The concentrations of individual resin acids (i.e., abietic and dehydroabietic) decreased significantly in Punkaharju, but increased in the sapwood of N-fertilized trees compared with control ones at Padasjoki and Vilppula. The concentrations of resin acids in the heartwood were not significantly affected by fertilization. Both fertilization treatments decreased the total phenolic concentrations in the heartwood of trees growing in Padasjoki. There was a significant positive correlation between the total phenolics and total resin acid concentration. Overall, resin acids and phenolics seemed be more responsive than monoterpenes to N treatment. These results suggest that forest fertilization might cause slight changes in secondary compound concentrations of xylem, and thus might have significance in the decay resistance of wood.

Determining efficacy of monitoring devices on ceramic bond to resin composite

PubMed Central

Osorio, Estrella; Aguilera, Fátima S.; Osorio, Raquel; García-Godoy, Franklin; Cabrerizo-Vilchez, Miguel A.; Toledano, Manuel

2012-01-01

Objectives: This paper aims to assess the effectiveness of 3D nanoroughness and 2D microroughness evaluations, by their correlation with contact angle measurements and shear bond strength test, in order to evaluate the effect of two different acids conditioning on the bonding efficacy of a leucite-based glass-ceramic to a composite resin. Study Design: Ceramic (IPS Empress) blocks were treated as follows: 1) no treatment, 2) 37% phosphoric acid (H3PO4), 15 s, 3) 9% hydrofluoric acid (HF), 5 min. Micro- and nano-roughness were assessed with a profilometer and by means of an atomic force microscopy (AFM). Water contact angle (CA) measurements were determined to assess wettability of the ceramic surfaces with the asixymetric drop shape analysis contact diameter technique. Shear bond strength (SBS) was tested to a resin composite (Z100) with three different adhesive systems (Scotchbond Multipurpose Plus, Clearfil New Bond, ProBOND). Scanning electron microscopy (SEM) images were performed. Results: Nanoroughness values assessed in 50x50 μm areas were higher for the HF group, these differences were not detected by profilometric analysis. HF treatment created the nano- roughest surfaces and the smallest CA (p<0.05), producing the highest SBS to the composite resin with all tested adhesive systems (p<0.05). No differences existed between the SBS produced by the adhesive systems evaluated with any of the surface treatments tested. Conclusions: Nano-roughness obtained in a 50x50 µm scan size areas was the most reliable data to evaluate the topographical changes produced by the different acid treatments on ceramic surfaces. Key words:Dental ceramic, acid etching, bonding efficacy, resin composite, adhesive systems, contact angle, roughness. PMID:22549693

Flame retardant polyphosphazenes

NASA Technical Reports Server (NTRS)

Paciorek, K. L.; Karle, D. W.; Kratzer, R. H.

1973-01-01

Six polyphosphazene compositions were prepared by reaction of three bis-tertiary phosphines with two phenyl-s-triazine derived diazides. All six polyphosphazenes produced were completely characterized, four of them were furthermore subjected to isothermal gravimetric analysis, smoke density measurements, flammability and oxidative thermal degradation testing. The results of the characterization studies indicate that only low molecular weight oligomers, possibly of a cyclic structure, were obtained in the polymerization reactions. Despite this, however, two of the materials showed no weight loss after 96 hr at 200 C, one did not autoignite at 500 C in air, and all four self extinguished when exposed to a flame as soon as contact between flame and resin was lost. The only toxic decomposition products to be concerned about were found to be hydrogen cyanide and benzene. Under the conditions employed it was proven, however, that the quantities of toxic products are greatly reduced if no ignition takes place, e.g., if thermal decomposition proceeds at a sufficiently low rate.

Coordination chemistry with phosphine and phosphine oxide-substituted hydroxyferrocenes.

PubMed

Atkinson, Robert C J; Gibson, Vernon C; Long, Nicholas J; White, Andrew J P

2010-08-28

New unsymmetrical hydroxyferrocenes were synthesised from dibromoferrocene. The oxygen heteroatom was introduced via lithiation and quenching with bis-trimethylsilylperoxide followed by hydrolysis to unmask the hydroxyl functionality. The coordination chemistry of 1'-(diphenylphosphino)-1-hydroxyferrocene 2 was explored with palladium and rhodium precursors. A dinuclear palladium methyl complex with bridging ferrocenyloxo groups was obtained from the reaction between 2 and (cyclooctadiene)methylchloropalladium(II). With tetracarbonyldichlorodirhodium(I), two complexes were isolated. The major product was a bis ligand cis phosphine ligated complex with one ligand bound in a chelating mode and one with a pendant hydroxyl group. A minor product was crystallographically characterised as a dinuclear ferrocenyloxo-bridged rhodium carbonyl complex. The coordination chemistry of 2 and the corresponding phosphine oxide 3 was examined with group 4 metals and the resulting complexes examined as ethylene polymerisation catalysts. The ligands were found to bind in either a chelating fashion or with pendant phosphine donors. In all cases, low to moderately active ethylene polymerisation catalysts were found. The catalysts were very unstable and catalyst residues were observed in the isolated polymer indicating a short catalyst lifetime.

Integrated Extraction Chromatographic Separation of the Lithophile Elements Involved in Long-Lived Radiogenic Isotope Systems (Rb-Sr, U-Th-Pb, Sm-Nd, La-Ce, and Lu-Hf) Useful in Geochemical and Environmental Sciences.

PubMed

Pin, Christian; Gannoun, Abdelmouhcine

2017-02-21

A fast and efficient sample preparation method in view of isotope ratio measurements is described, allowing the separation of 11 elements involved, either as "parent" or as "daughter" isotopes, in six radiogenic isotope systems used as chronometers and tracers in earth, planetary, and environmental sciences. The protocol is based on small extraction chromatographic columns, used either alone or in tandem, through which a single nitric acid solution is passed, without any intervening evaporation step. The columns use commercially available extraction resins (Sr resin, TRU resin, Ln resin, RE resin, and again Ln resin for isolating Sr and Pb, LREE then La-Ce-Nd-Sm, Lu(Yb), and Hf, Th, and U, respectively) along with an additional, in-house prepared resin for separating Rb. A simplified scheme is proposed for samples requiring the separation of Sr, Pb, Nd, and Hf only. Adverse effects of troublesome major elements (Fe 3+ , Ti) are circumvented by masking with ascorbic acid and hydrofluoric acid, respectively. Typical recoveries in the 85-95% range are achieved, with procedural blanks of 10-100 pg, negligible with regard to the amounts of analytes processed. The fractions separated are suitable for high precision isotope ratio measurements by TIMS or MC-ICP-MS, as demonstrated by the repeat analyses of several international reference materials of basaltic composition for 87 Sr/ 86 Sr, 208,207,206 Pb/ 204 Pb, 143 Nd/ 144 Nd, 176 Hf/ 177 Hf, and 230 Th/ 232 Th. Concentration data could be obtained by spiking and equilibrating the sample with appropriate isotopic tracers before the onset of the separation process and, finally, measuring the isotope ratios modified by the isotope dilution process.

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

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

Study on dehydrochlorination of waste poly (vinyl chloride) resins by microwave irradiation

NASA Astrophysics Data System (ADS)

Moriwaki, Saburo; Qian, Qingrong; Sunohara, Satoshi; Machida, Motoi; Tatsumoto, Hideki

Waste poly (vinyl chloride: PVC) resins are experimentally dehydrochlorinated by microwave irradiation. The following unique results are obtained: (1) plasticizer in PVC resin absorbs microwave power more effectively than PVC polymer. The higher the plasticizer content in PVC resin, the higher is the dehydrochlorination reaction (2) low PVC polymer content materials such as cushion floor require high microwave irradiation power to secure a high dehydrochlorination yield, (3) calcium carbonate in PVC resin reacts with released hydrochloric acid gas and results calcium chloride during microwave irradiation, (4) additives in PVC resin strongly influence dehydrochlorination yield, (5) it is evidenced that the PVC copolymer is also dehydrochlorinated by microwave irradiation.

The effects of dentin and intaglio indirect ceramic optimized polymer restoration surface treatment on the shear bond strength of resin cement

NASA Astrophysics Data System (ADS)

Puspitarini, A.; Suprastiwi, E.; Usman, M.

2017-08-01

Ceramic optimized polymer (ceromer) bonds to the tooth substrate through resin cements. The bond strength between dentin, resin cement, and ceromer depends on the applied surface treatment. To analyze the effects of dentin and intaglio ceromer surface treatment on the shear bond strength self-adhesive resin cement. Forty-five dentin premolar and ceromer specimens were bonded with resin cement and divided into three groups as follows: in group 1, no treatment was applied; in group 2, dentin surface treatment was carried out with acid etching and a bonding agent; and in group 3, dentin surface treatment was carried out with acid etching, a bonding agent, and intaglio ceromer surface treatment with etching and silane. All specimens were incubated at 37 °C for 24 hours, and the shear bond strength was measured using a universal testing machine. Group 3 showed the highest shear bond strength, followed by group 2. The surface treatment of dentin and intaglio ceromer showed significantly improved shear bond strength in the group comparison. Dentin and intaglio ceromer surface treatment can improved the shear bond strength self-adhesive resin cement.

Structures of potent selective peptide mimetics bound to carboxypeptidase B.

PubMed

Adler, Marc; Buckman, Brad; Bryant, Judi; Chang, Zheng; Chu, Kieu; Emayan, Kumar; Hrvatin, Paul; Islam, Imadul; Morser, John; Sukovich, Drew; West, Christopher; Yuan, Shendong; Whitlow, Marc

2008-02-01

This article reports the crystal structures of inhibitors of the functional form of thrombin-activatable fibrinolysis inhibitor (TAFIa). In vivo experiments indicate that selective inhibitors of TAFIa would be useful in the treatment of heart attacks. Since TAFIa rapidly degrades in solution, the homologous protein porcine pancreatic carboxypeptidase B (pp-CpB) was used in these crystallography studies. Both TAFIa and pp-CpB are zinc-based exopeptidases that are specific for basic residues. The final development candidate, BX 528, is a potent inhibitor of TAFIa (2 nM) and has almost no measurable effect on the major selectivity target, carboxypeptidase N. BX 528 was designed to mimic the tripeptide Phe-Val-Lys. A sulfonamide replaces the Phe-Val amide bond and a phosphinate connects the Val and Lys groups. The phosphinate also chelates the active-site zinc. The electrostatic interactions with the protein mimic those of the natural substrate. The primary amine in BX 528 forms a salt bridge to Asp255 at the base of the S1' pocket. The carboxylic acid interacts with Arg145 and the sulfonamide is hydrogen bonded to Arg71. Isopropyl and phenyl groups replace the side chains of Val and Phe, respectively. A series of structures are presented here that illustrate the evolution of BX 528 from thiol-based inhibitors that mimic a free C-terminal arginine. The first step in development was the replacement of the thiol with a phosphinate. This caused a precipitous drop in binding affinity. Potency was reclaimed by extending the inhibitors into the downstream binding sites for the natural substrate.

21 CFR 177.2420 - Polyester resins, cross-linked.

Code of Federal Regulations, 2014 CFR

2014-04-01

... following prescribed conditions: (a) The cross-linked polyester resins are produced by the condensation of... fiber Polyester fiber produced by the condensation of one or more of the acids listed in paragraph (a)(1...

21 CFR 177.2500 - Polyphenylene sulfone resins.

Code of Federal Regulations, 2014 CFR

2014-04-01

... polyphenylene sulfide with peracetic acid such that the finished resins meet the specifications set forth in... glass transition temperature of the polymer is 360±5 °C as determined by the use of differential...

Separation of thorium and uranium in nitric acid solution using silica based anion exchange resin.

PubMed

Chen, Yanliang; Wei, Yuezhou; He, Linfeng; Tang, Fangdong

2016-09-30

To separate thorium and uranium in nitric acid solution using anion exchange process, a strong base silica-based anion exchange resin (SiPyR-N4) was synthesized. Batch experiments were conducted and the separation factor of thorium and uranium in 9M nitric acid was about 10. Ion exchange chromatography was applied to separate thorium and uranium in different ratios. Uranium could be eluted by 9M nitric acid and thorium was eluted by 0.1M nitric acid. It was proved that thorium and uranium can be separated and recovered successfully by this method. Copyright © 2016 Elsevier B.V. All rights reserved.

Advanced thermoplastic resins, phase 1

NASA Technical Reports Server (NTRS)

Hendricks, C. L.; Hill, S. G.; Falcone, A.; Gerken, N. T.

1991-01-01

Eight thermoplastic polyimide resin systems were evaluated as composite matrix materials. Two resins were selected for more extensive mechanical testing and both were versions of LaRC-TPI (Langley Research Center - Thermoplastic Polyimide). One resin was made with LaRC-TPI and contained 2 weight percent of a di(amic acid) dopant as a melt flow aid. The second system was a 1:1 slurry of semicrystalline LaRC-TPI powder in a polyimidesulfone resin diglyme solution. The LaRC-TPI powder melts during processing and increases the melt flow of the resin. Testing included dynamic mechanical analysis, tension and compression testing, and compression-after-impact testing. The test results demonstrated that the LaRC-TPI resins have very good properties compared to other thermoplastics, and that they are promising matrix materials for advanced composite structures.

Engineering and Design: Composite Materials for Civil Engineering Structures

DTIC Science & Technology

1997-03-31

the effects of acidic, salt, and fresh waters . Acidic, salt, and fresh waters are corrosive to ferrous metals. In Corps of Engineers structures, high...what is commonly called a toughened epoxy. (5) Polymeric resins will absorb moisture. Since many applications are in contact with water (at least...ultraviolet radiation. Some coatings can reduce the amount of moisture absorption by the structure. All polymeric resins will absorb water to some

The shear bond strength of self-adhesive resin cements to dentin and enamel: an in vitro study.

PubMed

Rodrigues, Raphaela F; Ramos, Carla M; Francisconi, Paulo A S; Borges, Ana Flávia S

2015-03-01

Clinicians continue to search for ways to simplify bonding procedures without compromising clinical efficacy. The purpose of this study was to evaluate the shear strength of self-adhesive cements RelyX U100 and RelyX U200, and conventional resin cement RelyX ARC to enamel and dentin after different surface treatments. The crowns of 120 bovine incisor teeth were separated from the roots and embedded in epoxy resin in polyvinyl chloride tubes. In each tooth, the area to be cemented was delimited with central holed adhesive tape. The teeth were distributed into 12 groups (n=10) according to the substrate; etched or not with 37% phosphoric acid; and cement type of enamel-U100, enamel-phosphoric acid-U100, enamel-U200, enamel-phosphoric acid-U200, enamel-ARC, enamel-phosphoric acid-ARC, dentin-U100, dentin-phosphoric acid-U100, dentin-U200, dentin-phosphoric acid-U200, dentin-ARC, and dentin-phosphoric acid-ARC. After 7 days of storage in artificial saliva, shear strength tests were performed by using a universal testing machine (0.5 mm/min). The data were analyzed with 3-way ANOVA and the Tukey test (α=.05). Fracture analysis was performed with a light microscope. Two specimens from each group were analyzed with a scanning electron microscope. In enamel, ARC (9.96 MPa) had higher shear strength (P=.038) than U100 (5.14 MPa); however, after surface etching, U100 (17.81 MPa) and U200 (17.52 MPa) had higher shear strength (P<.001). With dentin, no significant differences were observed (P=.999), except for dentin-ARC (0.34 MPa) (P=.001). Most fractures were of the adhesive type. U200 self-adhesive cement had similar bond strength to the ARC in enamel, but the combination with phosphoric acid had the best bond strength. For dentin, self-adhesive resin cements are equally effective alternatives to conventional resin cement. Copyright © 2015 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Enrichment and low-level determination of glyphosate, aminomethylphosphonic acid and glufosinate in drinking water after cleanup by cation exchange resin.

PubMed

Küsters, Markus; Gerhartz, Michael

2010-04-01

For the determination of glyphosate, aminomethylphosphonic acid and glufosinate in drinking water, different procedures of enrichment and cleanup were examined using anion exchange or SPE. In many cases interactions of, e.g. alkaline earth metal ions especially calcium could be observed during enrichment and cleanup resulting in loss of analytes. For that reason, a novel cleanup and enrichment procedure for the determination of these phosphonic acid herbicides has been developed in drinking water using cation-exchange resin. In summary, the cleanup procedure with cation-exchange resin developed in this study avoids interactions as described above and is applicable to calcium-rich drinking water samples. After derivatization with 9-fluorenylmethylchloroformate followed by LC with fluorescence detection, LOD of 12, 14 and 12 ng/L and mean recoveries from real-world drinking water samples of 98+/-9, 100+/-16 and 101+/-11% were obtained for glyphosate, aminomethylphosphonic acid and glufosinate, respectively. The low LODs and the high precision permit the analysis of these phosphonic acid herbicides according to the guidelines of the European Commission.

Phosphine/Sulfoxide-Supported Carbon(0) Complex.

PubMed

Lozano González, Mariana; Bousquet, Laura; Hameury, Sophie; Alvarez Toledano, Cecilio; Saffon-Merceron, Nathalie; Branchadell, Vicenç; Maerten, Eddy; Baceiredo, Antoine

2018-02-21

A new carbon(0) complex 2 with two different L ligands, a phosphine and a sulfoxide, was synthesized and fully characterized. This new type of carbone exhibits excellent coordination ability, in contrast to the related phosphine/sulfide-supported carbon(0) complexes. Several organometallic complexes were isolated and, of special interest, the ν av (CO) value of Rh I -dicarbonyl complex indicates that 2 has a donor capability superior to classical NHCs. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and structural characterisation of a novel phosphine-borane-stabilised dicarbanion and an unusual bis(phosphine-borane).

PubMed

Izod, Keith; McFarlane, William; Tyson, Brent V; Clegg, William; Harrington, Ross W

2004-03-07

The reaction between the phosphine-borane-substituted alkene [Pr(n)(2)P(BH(3))](Me(3)Si)C[double bond]CH(2) and elemental lithium in THF yields the complex [(pmdeta)Li[Pr(n)(2)P(BH(3))](Me(3)Si)CCH(2)](2)(2b) after recrystallisation; an X-ray crystallographic study of 2b reveals that the lithium is bound to the BH(3) hydrogens of the ligand, with no Li-C(carbanion) contact.

Recent Developments in the Addition of Phosphinylidene-Containing Compounds to Unactivated Unsaturated Hydrocarbons: Phosphorus-Carbon Bond-Formation via Hydrophosphinylation and Related Processes

PubMed Central

Coudray, Laëtitia

2012-01-01

Summary The reactions of phosphinylidene-containing compounds with unactivated unsaturated hydrocarbons are reviewed. The review is organized by phosphorus-containing functional group types. Free-radical and metal-catalyzed additions of R1R2P(O)H to alkenes, alkynes, and related compounds, deliver functionalized organophosphorus compounds RP(O)R1R2, including H-phosphinates, phosphinates, tertiary phosphine oxides, and phosphonates. The review covers the literature up to February 2008. PMID:23308039

Abietic acid isolated from pine resin (Resina Pini) enhances angiogenesis in HUVECs and accelerates cutaneous wound healing in mice.

PubMed

Park, Jun Yeon; Lee, Yun Kyung; Lee, Dong-Soo; Yoo, Jeong-Eun; Shin, Myoung-Sook; Yamabe, Noriko; Kim, Su-Nam; Lee, Seulah; Kim, Ki Hyun; Lee, Hae-Jeung; Roh, Seok Sun; Kang, Ki Sung

2017-05-05

Resin known as Resina Pini is listed in the Korean and Japanese pharmacopoeias and has been used for treating skin wounds and inflammation. Resin is composed of more than 50% abietic acid and 10% neutral substances. In the present study, the wound-healing effects of abietic acid and the possible underlying mechanism of action were investigated in various in vitro and in vivo models. The effects of abietic acid on tube formation and migration were measured in human umbilical vein vascular endothelial cells (HUVECs). Protein expression of mitogen-activated protein kinase (MAPK) activation was evaluated via Western blotting analysis. The wound-healing effects of abietic acid were assessed using a mouse model of cutaneous wounds. The results showed that abietic acid enhanced cell migration and tube formation in HUVECs. Abietic acid induced significant angiogenic potential, which is associated with upregulation of extracellular signal-regulated kinase (ERK) and p38 expression. Additionally, 0.8μM abietic acid-treated groups showed accelerated wound closure compared to the controls in a mouse model of cutaneous wounds. The current data indicate that abietic acid treatment elevated cell migration and tube formation in HUVECs by the activation of ERK and p38 MAPKs. We suggest that abietic acid can be developed as a wound-healing agent. Copyright © 2017 Elsevier Ltd. All rights reserved.

The Role of Nanobubbles in the Precipitation and Recovery of Organic-Phosphine-Containing Beneficiation Wastewater.

PubMed

Xiao, Wei; Ke, Shuo; Quan, Nannan; Zhou, Limin; Wang, Jun; Zhang, Lijuan; Dong, Yaming; Qin, Wenqing; Qiu, Guanzhou; Hu, Jun

2018-05-29

Dissolved air flotation (DAF) is broadly applied in wastewater treatment, especially for the recovery of organic pollution with low concentration. However, the mechanism of interaction between nanoscale gas bubbles and nanoparticles in the process of DAF remains unclear. Here, we investigated the role of nanobubbles in the precipitation of styryl phosphoric acid (SPA)-Pb particles and recovering organic phosphine containined in beneficiation wastewater by UV-vis (ultraviolet-visible) spectra, microflotation tests, nanoparticle tracking analysis, dynamic light scattering, and atomic force microscopy measurements. As suggested from the results, nanobubbles can inhibit the crystallization of SPA-Pb precipitation, which makes the sediment flotation recovery below 20%. After the precipitation crystallization is completed, nanobubbles can flocculate precipitated particles, which can promote the flotation recovery of precipitated particles to 90%. On the basis of the results, we proposed a model to explain the different roles of nanobubbles in the process of precipitation and flotation of SPA-Pb particles. This study will be helpful to understand the interaction between nanobubbles and nanoparticles in the application of flotation.

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

NASA Astrophysics Data System (ADS)

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

2016-11-01

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

Synthesis and characterization of bifunctional surfaces with tunable functional group pairs

NASA Astrophysics Data System (ADS)

Galloway, John M.; Kung, Mayfair; Kung, Harold H.

2016-06-01

Grafting of pairs of functional groups onto a silica surface was demonstrated by tethering both terminals of an organochlorosilane precursor molecule, Cl2(CH3)Si(CH2)4(CO)(OSi(i-Pr)2)(CH2)2Si(CH3)Cl2, that possess a cleavable silyl ester bond, onto a silica surface. Hydrolytic cleavage of the silyl ester bond of the grafted molecule resulted in the generation of organized pairs of carboxylic acid and organosilanol groups. This organosilanol moiety was easily transformed into other functional groups through condensation reactions to form, together with the neighboring acid group, pairs such as carboxylic acid/secondary amine, carboxylic acid/pyridine, and carboxylic acid/phosphine. In the case of carboxylic acid/amine pairing, there was evidence of the formation of amide. A sample grafted with amine-carboxylic acid pairs was three times more active (per free amine) than a sample without such pairs for the nitroaldol condensation of 4-nitrobenzaldehyde and nitromethane.

VALIDATION FOR THE PERMANGANATE DIGESTION OF REILLEX HPQ ANION RESIN

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kyser, E.

2009-09-23

The flowsheet for the digestion of Reillex{trademark} HPQ was validated both under the traditional alkaline conditions and under strongly acidic conditions. Due to difficulty in performing a pH adjustment in the large tank where this flowsheet must be performed, the recommended digestion conditions were changed from pH 8-10 to 8 M HNO{sub 3}. Thus, no pH adjustment of the solution is required prior to performing the permanganate addition and digestion and the need to sample the digestion tank to confirm appropriate pH range for digestion may be avoided. Neutralization of the acidic digestion solution will be performed after completion ofmore » the resin digestion cycle. The amount of permanganate required for this type of resin (Reillex{trademark} HPQ) was increased from 1 kg/L resin to 4 kg/L resin to reduce the amount of residual resin solids to a minimal amount (<5%). The length of digestion time at 70 C remains unchanged at 15 hours. These parameters are not optimized but are expected to be adequate for the conditions. The flowsheet generates a significant amount of fine manganese dioxide (MnO{sub 2}) solids (1.71 kg/L resin) and involves the generation of a significant liquid volume due to the low solubility of permanganate. However, since only two batches of resin (40 L each) are expected to be digested, the total waste generated is limited.« less

Extractive scintillating polymer sensors for trace-level detection of uranium in contaminated ground water.

PubMed

Duval, Christine E; DeVol, Timothy A; Husson, Scott M

2016-12-01

This contribution describes the synthesis of robust extractive scintillating resin and its use in a flow-cell detector for the direct detection of uranium in environmental waters. The base poly[(4-methyl styrene)-co-(4-vinylbenzyl chloride)-co-(divinylbenzene)-co-(2-(1-napthyl)-4-vinyl-5-phenyloxazole)] resin contains covalently bound fluorophores. Uranium-binding functionality was added to the resin by an Arbuzov reaction followed by hydrolysis via strong acid or trimethylsilyl bromide (TMSBr)-mediated methanolysis. The resin was characterized by Fourier-transform infrared spectroscopy and spectrofluorometry. Fluorophore degradation was observed in the resin hydrolyzed by strong acid, while the resin hydrolyzed by TMSBr-mediated methanolysis maintained luminosity and showed hydrogen bonding-induced Stokes' shift of ∼100 nm. The flow cell detection efficiency for uranium of the TMSBr-mediated methanolysis resin was evaluated at pH 4, 5 and 6 in DI water containing 500 Bq L -1 uranium-233 and demonstrated flow cell detection efficiencies of 23%, 16% and 7%. Experiments with pH 4, synthetic groundwater with 50 Bq L -1 uranium-233 exhibited a flow cell detection efficiency of 17%. The groundwater measurements show that the resins can concentrate the uranyl cation from waters with high concentrations of competitor ions at near-neutral pH. Findings from this research will lay the groundwork for development of materials for real-time environmental sensing of alpha- and beta-emitting radionuclides. Copyright © 2016 Elsevier B.V. All rights reserved.

Acidic resin-catalysed conversion of fructose into furan derivatives in low boiling point solvents.

PubMed

Zhu, Hong; Cao, Quan; Li, Chunhu; Mu, Xindong

2011-09-27

Conversion of fructose into furan derivatives 5-hydroxymethylfurfural (HMF) and 5-methoxymethylfurfural (MMF) is performed in tetrahydrofuran (THF) and methanol-organic solvent systems, catalysed by an acidic resin Amberlyst-15. The melted fructose can be converted into HMF on the surface of the solid resin catalyst in the presence of THF as an extracting phase, which is a good solvent for HMF and other by-products. The solid resin catalyst can be reused eleven times without losing its catalytic ability, with an average HMF yield of approximately 50%. Upon the addition of methanol, the generated HMF can further react with methanol to form MMF, and the total yield of HMF and MMF could be promoted to 65%. GC-MS analysis confirms the formation of a small amount of methyl levulinate in methanolorganic solvent system. Copyright © 2011 Elsevier Ltd. All rights reserved.

Attempt to induce lightwood in eastern hemlock by treating with paraquat

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kiatgrajai, P.; Rowe, J.W.; Conner, A.H.

1976-01-01

Treatment of eastern hemlock (Tsuga canadensis (L.) Carr.) with the herbicide paraquat did not induce formation of lightwood. However, a dead zone of phloem extended above the paraquat-treatment site. Traumatic resin ducts were observed in the wood immediately adjacent to this dead zone. Although some of these ducts were filled with resin, most were empty. A very small amount of resin soaking was observed at the edges of the dead phloem. Although there was an increase in the extractives content of the wood behind the dead phloem, this did not reach levels with commercial potential. The increase in turpentine levelmore » was mostly due to slightly volatile waxes. The nonvolatile ether extractives were predominately acids other than the fatty and resin acids typical of pines. Electron microscopy revealed fungal hyphae in the wood behind the dead phloem, and several species of fungi were cultured from the wood.« less

Rechargeable Infection-responsive Antifungal Denture Materials

PubMed Central

Cao, Z.; Sun, X.; Yeh, C.-K.; Sun, Y.

2010-01-01

Candida-associated denture stomatitis (CADS) is a significant clinical concern. We developed rechargeable infection-responsive antifungal denture materials for potentially managing the disease. Polymethacrylic acid (PMAA) was covalently bound onto diurethane dimethacrylate denture resins in the curing step. The PMAA resins bound cationic antifungal drugs such as miconazole and chlorhexidine digluconate (CG) through ionic interactions. The anticandidal activities of the drug-containing PMAA-resin discs were sustained for a prolonged period of time (weeks and months). Drug release was much faster at acidic conditions (pH 5) than at pH 7. Drugs bound to the denture materials could be “washed out” by treatment with EDTA, and the drug-depleted resins could be recharged with the same or a different class of anticandidal drugs. These results suggest clinical potential of the newly developed antifungal denture materials in the management of CADS and other infectious conditions. PMID:20940361

[Monitoring method for macroporous resin column chromatography process of salvianolic acids based on near infrared spectroscopy].

PubMed

Hou, Xiang-Mei; Zhang, Lei; Yue, Hong-Shui; Ju, Ai-Chun; Ye, Zheng-Liang

2016-07-01

To study and establish a monitoring method for macroporous resin column chromatography process of salvianolic acids by using near infrared spectroscopy (NIR) as a process analytical technology (PAT).The multivariate statistical process control (MSPC) model was developed based on 7 normal operation batches, and 2 test batches (including one normal operation batch and one abnormal operation batch) were used to verify the monitoring performance of this model. The results showed that MSPC model had a good monitoring ability for the column chromatography process. Meanwhile, NIR quantitative calibration model was established for three key quality indexes (rosmarinic acid, lithospermic acid and salvianolic acid B) by using partial least squares (PLS) algorithm. The verification results demonstrated that this model had satisfactory prediction performance. The combined application of the above two models could effectively achieve real-time monitoring for macroporous resin column chromatography process of salvianolic acids, and can be used to conduct on-line analysis of key quality indexes. This established process monitoring method could provide reference for the development of process analytical technology for traditional Chinese medicines manufacturing. Copyright© by the Chinese Pharmaceutical Association.

Impact of pH and application time of meta-phosphoric acid on resin-enamel and resin-dentin bonding.

PubMed

Cardenas, A F M; Siqueira, F S F; Bandeca, M C; Costa, S O; Lemos, M V S; Feitora, V P; Reis, A; Loguercio, A D; Gomes, J C

2018-02-01

To evaluate the immediate microshear resin-enamel bond strength (μSBS) and the immediate and 6-month microtensile bond strength (μTBS) and nanoleakage (NL) of the adhesive interface performed by different pHs of 40% meta-phosphoric acid (MPA) were compared with conventional 37% ortho-phosphoric acid (OPA) under different application times. Additionally, the enamel etching patterns were evaluated and the chemical/morphological changes induced by these differents groups were evaluated. One hundred and ninety-eight extracted human molars were randomly assigned into experimental groups according to the combination of independent variables: Acid [37% ortho-phosphoric acid (OPA), 40% meta-phosphoric acid (MPA) at pHs of: 0.5, 1 and 2] and Application Time [7, 15 and 30s]. Enamel-bond specimens were prepared and tested under μSBS. Resin-dentin beams were tested under μTBS tested immediately or after 6-months of water storage. Nanoleakage was evaluated using bonded-beams of each tooth/time-period. Enamel etching pattern and chemical and ultra-morphology analyses were also performed. The μSBS (MPa) data were subjected to a two-way repeated measures ANOVA (Acid vs. Application time). For μTBS, Acid vs application time vs storage time data were subjected to three-way ANOVA and Tukey's test (α = 0.05). MPA pH 0.5 showed μTBS similar to OPA, independently of the application time on enamel (p>0.05) or dentin (p>0.05). OPA provided higher nanoleakage values than MPA (p = 0.003). Significant decreases in TBS and increases in NL were only observed for OPA after 6 months (p = 0.001). An increase in the application time resulted in a more pronounced etching pattern for MPA. Chemical analysis showed that dentin demineralized by MPA depicted peaks of brushite and octacalcium phosphate. MPA exposed less collagen than OPA. However, optimal results for MPA were dependent on pH/application time. The use of 40% meta-phosphoric acid with a pH of 0.5 is an alternative acid-etching agent for dentin and enamel bonding. Furthermore, the use of MPA preserves the resin-dentin interface over a 6-months period, due to presence of brushite and octacalcium phosphate and a reduced demineralization pattern. Copyright © 2017 Elsevier Ltd. All rights reserved.

Feasibility study on the utilization of rubber latex effluent for producing bacterial biopolymers.

PubMed

Tang, S N; Fakhru'l-Razi, A; Hassan, M A; Karim, M I

1999-01-01

Rubber latex effluent is a polluting source that has a high biochemical oxygen demand (BOD). It is estimated that about 100 million liters of effluent are discharged daily from rubber processing factories. Utilization of this effluent such as the use of a coupled system not only can reduce the cost of treatment but also yield a fermentation feedstock for the production of bioplastic. This study initially was carried out to increase the production of organic acids by anaerobic treatment of rubber latex effluent. It was found that through anaerobic treatment the concentration of organic acids did not increase. Consequently, separation of organic acids from rubber latex effluent by anion exchange resin was examined as a preliminary study of recovering acetic and propionic acids. However, the suspended solids (SS) content in the raw effluent was rather high which partially blocked the ion-exchange columns. Lime was used to remove the SS in the rubber latex effluent. After the lime precipitation process, organic acids were found to adsorb strongly onto the anion exchange resin. Less adsorption of organic acids onto the resin was observed before the lime precipitation. This was probably due to more sites being occupied by colloidal particles on the resin thus inhibiting the adsorption of organic acids. The initial concentration of organic acids in the raw effluent was 3.9 g/L. After ion exchange, the concentration of the organic acids increased to 27 g/L, which could be utilized for production of polyhydroxyalkanoates (PHA). For PHA accumulation stage, concentrated rubber latex effluent obtained from ion exchange resins and synthetic acetic acid were used as the carbon source. Quantitative analyses from fed batch culture via HPLC showed that the accumulation of PHA in Alcaligenes eutrophus was maximum with a concentration of 1.182 g/L when cultivated on synthetic acetic acid, corresponding to a yield of 87% based on its cell dry weight. The dry cell weight increased from 0.71 to 1.67 g/L. On the other hand, using concentrated rubber latex effluent containing acetic and propionic acids resulted in reduced PHA content by dry weight (14%) but the dry cell weight increased from 0.49 to 1.30 g/L. The results clearly indicated that the cells grow well in rubber latex effluent but no PHA was accumulated. This could be due to the high concentration of propionic acid in culture broth or other factors such as heavy metals. Thus further work is required before rubber latex effluent can be utilized as a substrate for PHA production industrially.

Diclofenac removal in urine using strong-base anion exchange polymer resins.

PubMed

Landry, Kelly A; Boyer, Treavor H

2013-11-01

One of the major sources of pharmaceuticals in the environment is wastewater effluent of which human urine contributes the majority of pharmaceuticals. Urine source separation has the potential to isolate pharmaceuticals at a higher concentration for efficient removal as well as produce a nutrient byproduct. This research investigated the efficacy of using strong-base anion exchange polymer resins to remove the widely detected and abundant pharmaceutical, diclofenac, from synthetic human urine under fresh and ureolyzed conditions. The majority of experiments were conducted using a strong-base, macroporous, polystyrene resin (Purolite A520E). Ion-exchange followed a two-step removal rate with rapid removal in 1 h and equilibrium removal in 24 h. Diclofenac removal was >90% at a resin dose of 8 mL/L in both fresh and ureolyzed urine. Sorption of diclofenac onto A520E resin was concurrent with desorption of an equivalent amount of chloride, which indicates the ion-exchange mechanism is occurring. The presence of competing ions such as phosphate and citrate did not significantly impact diclofenac removal. Comparisons of three polystyrene resins (A520E, Dowex 22, Dowex Marathon 11) as well as one polyacrylic resin (IRA958) were conducted to determine the major interactions between anion exchange resin and diclofenac. The results showed that polystyrene resins provide the highest level of diclofenac removal due to electrostatic interactions between quaternary ammonium functional groups of resin and carboxylic acid of diclofenac and non-electrostatic interactions between resin matrix and benzene rings of diclofenac. Diclofenac was effectively desorbed from A520E resin using a regeneration solution that contained 4.5% (m/m) NaCl in an equal-volume mixture of methanol and water. The greater regeneration efficiency of the NaCl/methanol-water mixture over the aqueous NaCl solution supports the importance of non-electrostatic interactions between resin matrix and benzene rings of diclofenac. Experiments with ketoprofen, in addition to diclofenac, suggest that polystyrene anion exchange resins can be used to selectively remove other acidic pharmaceuticals from urine. Copyright © 2013 Elsevier Ltd. All rights reserved.

Identification of resinous materials on 16th and 17th century reverse-glass objects by gas chromatography/mass spectrometry

NASA Astrophysics Data System (ADS)

Baumer, Ursula; Dietemann, Patrick; Koller, Johann

2009-07-01

Objects of hinterglasmalerei, reverse-glass paintings, are painted on the back side of glass panels. Obviously, the paint layers are applied in reverse order, starting with the uppermost layer. The finished hinterglas painting is viewed through the glass, thus revealing an impressive gloss and depth of colour. The binding media of two precious objects of hinterglasmalerei from the 16th and 17th century have been identified as almost exclusively resinous. Identification was performed by a special optimised analysis procedure, which is discussed in this paper: solvent extracts are analysed by gas chromatography/mass spectrometry, both with and without derivatisation or hydrolysis. In an additional step, oxalic acid is added to the methanol extracts prior to injection. This attenuates the peaks of the non-acidic compounds, whereas the acids elute with good resolution. The non-acidic compounds are emphasised after injection of the underivatised extracts. This approach minimises compositional changes caused by the sample preparation and derivatisation steps. Chromatograms of aged samples with a very complex composition are simplified, which allows a more reliable and straightforward identification of significant markers for various materials. The binding media of the hinterglas objects were thus shown to consist of mixtures of different natural resins, larch turpentine, heat-treated Pinaceae resin or mastic. Typical compounds of dragon's blood, a natural red resin, were also detectable in red glazes by the applied analysis routine. Identification of the binding media provides valuable information that can be used in the development of an adequate conservation treatment.

Influence of surface conditions and silane agent on the bond of resin to IPS Empress 2 ceramic.

PubMed

Spohr, Ana Maria; Sobrinho, Lourenço Correr; Consani, Simonides; Sinhoreti, Mario Alexandre Coelho; Knowles, Jonathan C

2003-01-01

The aim of this study was to evaluate the effect of different ceramic surface treatments on the tensile bond strength between IPS Empress 2 ceramic framework and Rely X adhesive resin cement, with or without the application of a silane coupling agent. One hundred twenty disks were made, embedded in resin, and randomly divided into six groups: group 1 = sandblasting (100 microm), no silanation; group 2 = sandblasting (100 microm), silane treatment; group 3 = sandblasting (50 microm), no silanation; group 4 = sandblasting (50 microm), silane treatment; group 5 = hydrofluoric acid etching, no silanation; and group 6 = hydrofluoric acid etching, silane treatment. The disks were bonded into pairs with adhesive resin cement. All samples were stored in distilled water at 37 degrees C for 24 hours and then thermocycled. The samples were submitted to tensile testing. The use of silane improved the bond strength in relation to the groups in which silane was not applied (P < .05). The most effective surface treatment was etching with 10% hydrofluoric acid, both with (25.6 MPa) and without silane application (16.4 MPa); these values showed a statistically significant difference compared to sandblasting with 50- and 100-microm Al2O3. Sandblasting with 50-microm Al2O3, with (11.8 MPa) and without silane (5.4 MPa), demonstrated significantly higher tensile bond strength than sandblasting with 100-microm Al2O3, with (8.3 MPa) and without silane (3.8 MPa). Combined application of 10% hydrofluoric acid and silane enhanced the bond strength between the IPS Empress 2 ceramic framework and resin agent.

Characterization of the homologs of flerovium with crown ether based extraction chromatography resins: studies in nitric acid

DOE PAGES

Despotopulos, John D.; Kmak, Kelly N.; Gharibyan, Narek; ...

2016-09-17

Eichrom’s Pb resin, a crown-ether-based extraction chromatography resin, was characterized for separation of the flerovium (Fl) homologs, Pb and Sn. Batch uptake of Pb(II) and Sn(IV) radionuclides was determined from an HNO 3 matrix. Pb(II) was strongly retained on the resin at all HNO 3 concentrations, while Sn(IV) showed no uptake. Extraction kinetics for Pb(II) were examined and show suitable uptake on the second time scale. Here, separation methods for the isolation of individual homologs, Pb(II) and Sn(IV), have been established using 2 mL pre-packed vacuum flow Pb resin columns.

The biocompatability of mesoporous inorganic-organic hybrid resin films with ionic and hydrophilic characteristics.

PubMed

Kim, Gahee; Hong, Lan Young; Jung, Jungwoon; Kim, Dong-Pyo; Kim, Heesoo; Kim, Ik Jung; Kim, Jung Ran; Ree, Moonhor

2010-03-01

New mesoporous silicate-titania resin systems hybridized with 4,5-dihydroxy-m-benzenedisulfonic acid and poly(ethylene glycol)-dimethacrylate component were developed. These inorganic-organic hybrid resins were found to reveal highly controlled ionic and hydrophilic surface with excellent durability and adhesion onto various substrates. The resin films revealed high resistance to nonspecific adsorption of fibrinogen and to adherence by several bacterial pathogens such as Escherichia coli, Staphylococcus aureus, Staphylococcus epidermidis and Enterococcus faecalis. Furthermore, excellent biocompatibility of the developed resins was proved by both HEp-2 cell adhesion in vitro and subcutaneous implantation in mice. The inorganic-organic hybrid resins are strongly promising for biomedical applications including biomedical devices and biosensors. Copyright 2009 Elsevier Ltd. All rights reserved.

Bio-phenolic resin from oil palm empty fruit bunches

NASA Astrophysics Data System (ADS)

Zakaria, Zuhaili; Zakaria, Sarani; Roslan, Rasidi; Chia, Chin Hua; Jaafar, Sharifah Nabihah Syed; Amran, Umar Adli

2018-04-01

Utilization of oil palm empty fruit bunches (EFB) in the production of bio-phenolic resin is an alternative way to reduce the dependency of petroleum-based phenol. In this study, resol type bio-phenolic resin (BPR) was synthesized from EFB fibers using sulfuric acid as the catalyst to produce liquefied empty fruit bunches (LEFB) followed by resinification reaction with formaldehyde in alkaline condition. The SEM image of LEFB residue showed separation of fiber bundles into individual fibers. This indicate that lignin was destroyed during the liquefaction process. The increased of formaldehyde/LEFB molar ratio has resulted an increase of viscosity, solid content and pH of the resin. The obtained FTIR spectra confirmed that functional groups of BPR resins was almost similar with commercial resin.

Phenolic cation exchange resin material for recovery of cesium and strontium

DOEpatents

Ebra, Martha A.; Wallace, Richard M.

1983-01-01

A phenolic cation exchange resin with a chelating group has been prepared by reacting resorcinol with iminodiacetic acid in the presence of formaldehyde at a molar ratio of about 1:1:6. The material is highly selective for the simultaneous recovery of both cesium and strontium from aqueous alkaline solutions, such as, aqueous alkaline nuclear waste solutions. The organic resins are condensation polymers of resorcinol and formaldehyde with attached chelating groups. The column performance of the resins compares favorably with that of commercially available resins for either cesium or strontium removal. By combining Cs.sup.+ and Sr.sup.2+ removal in the same bed, the resins allow significant reduction of the size and complexity of facilities for processing nuclear waste.

Phenolic cation-exchange resin material for recovery of cesium and strontium. [Patent application

DOEpatents

Ebra, M.A.; Wallace, R.M.

1982-05-05

A phenolic cation exchange resin with a chelating group has been prepared by reacting resorcinol with iminodiacetic acid in the presence of formaldehyde at a molar ratio of about 1:1:6. The material is highly selective for the simultaneous recovery of both cesium and strontium from aqueous alkaline solutions, such as, aqueous alkaline nuclear wate solutions. The organic resins are condensation polymers of resorcinol and formaldehyde with attached chelating groups. The column performance of the resins compares favorably with that of commercially available resins for either cesium or strontium removal. By combining Cs/sup +/ and Sr/sup 2 +/ removal in the same bed, the resins allow significant reduction of the size and complexity of facilities for processing nuclear waste.

In vivo effects of two acidic soft drinks on shear bond strength of metal orthodontic brackets with and without resin infiltration treatment.

PubMed

Hammad, Shaza M; Enan, Enas T

2013-07-01

To evaluate the in vivo effects of two acidic soft drinks (Coca-Cola and Sprite) on the shear bond strength of metal orthodontic brackets with and without resin infiltration treatment. In addition, the enamel surface was evaluated, after debonding, using a scanning electron microscope. Sixty noncarious maxillary premolars, scheduled for extraction in 30 orthodontic patients, were used. Patients were randomly divided into two groups according to the soft drink tested (Coca-Cola or Sprite). In each group, application of resin infiltration (Icon. DMG, Hamburg, Germany) was done on one side only before bonding of brackets. Patients were told to rinse their mouth with their respective soft drink at room temperature for 5 minutes, three times a day for 3 months. Shear bond strength was tested with a universal testing machine. After shearing test, a scanning electron microscope was used to evaluate enamel erosion. Statistical analysis was performed by twoway analysis of variance followed by the least significant difference test. The Coca-Cola group without resin infiltration showed the lowest resistance to shearing forces. Scanning electron micrographs of both groups after resin application showed a significant improvement compared with results without resin use, as the enamel appeared smoother and less erosive. Pretreatment with the infiltrating resin has proved to result in a significant improvement in shear bond strength, regardless of the type of soft drink consumed.

Composite Properties of Polyimide Resins Made From "Salt-Like" Solution Precursors

NASA Technical Reports Server (NTRS)

Cano, Roberto J.; Weiser, Erik S.; SaintClair, Terry L.; Echigo, Yoshiaki; Kaneshiro, Hisayasu

1997-01-01

Recent work in high temperature materials at NASA Langley Research Center (LaRC (trademark)) have led to the development of new polyimide resin systems with very attractive properties. The majority of the work done with these resin systems has concentrated on determining engineering mechanical properties of composites prepared from a poly(amide acid) precursor. Three NASA Langley-developed polyimide matrix resins, LaRC (trademark) -IA, LaRC (trademark) -IAX, and LaRC (trademark) -8515, were produced via a salt-like process developed by Unitika Ltd. The 'salt-like' solutions (sixty-five percent solids in NMP) were prepregged onto Hexcel IM7 carbon fiber using the NASA LaRC Multipurpose Tape Machine. Process parameters were determined and composite panels fabricated. Mechanical properties are presented for these three intermediate modulus carbon fiber/polyimide matrix composites and compared to existing data on the same polyimide resin systems and IM7 carbon fiber manufactured via poly(amide acid) solutions (thirty-five percent solids in NMP). This work studies the effects of varying the synthetic route on the processing and mechanical properties of polyimide composites.

Antiinflammatory and antioxidant activities of gum mastic.

PubMed

Mahmoudi, M; Ebrahimzadeh, M A; Nabavi, S F; Hafezi, S; Nabavi, S M; Eslami, Sh

2010-09-01

Pistacia lentiscus has traditionally been used in the treatment of many diseases. Its resin was investigated for its mineral contents, anti-inflammatory and antioxidant activities in rats. Inhibition of carrageenan induced edema was used to evaluate anti-inflammatory activity. Fe2+ chelating ability, 1,1-diphenyl-2-picryl hydrazyl radical (DPPH) and nitric oxide scavenging activities were used to evaluate antioxidant activities and mineral contents were determined by atomic absorption spectroscopy. Gallic acid content was determined by HPLC. Resin produced statistically significant inhibition of edema at all doses when compared to the control groups. A 100% inhibition of inflammation was observed at 800 mg/kg i.p. Resin exhibit no toxicity up to 3 g/kg body weights i.p. in mice. Weak DPPH and nitric oxide scavenging activities were observed but showed good Fe2+ chelating ability (IC50 = 162 microg ml(-1)). The amount of elements was decreased in the order: Cu > Fe, Zn > Mn > Ni, Cd. Gallic acid content was 0.1 mg/g resin. These experimental data support the use of Pistacia lentiscus resin as an antiinflammatory and antioxidant agent.

Selective adsorption and recovery of Au(III) from three kinds of acidic systems by persimmon residual based bio-sorbent: a method for gold recycling from e-wastes.

PubMed

Fan, Ruiyi; Xie, Feng; Guan, Xueliang; Zhang, Qinglin; Luo, Zhengrong

2014-07-01

A low cost bio-sorbent, named "PPF resin", was prepared by crosslinking the persimmon residual with formaldehyde. The adsorption behavior of PPF resin towards Au(III) from varied HCl and HNO3 concentration solutions was studied. PPF resin could adsorb almost complete Au(III) from high acidic systems. The influence of dilution ratio, solid-liquid ratio and time towards Au(III) from aqua regia leached PCBs liquor was censored in detail by batch and continuous adsorption methods. The PPF resin before and after adsorption was characterized by FT-IR, XRD and XPS spectra which provided evidences for the reduction of Au(III) to Au(0) with a proposed mechanism of Au(III) adsorption-reduction process. After saturated column adsorption of 0.1g PPF resin, 0.0506 g gold (purity: 99.9%) was obtained by the method of incineration. The present results provide a new approach for gold recovery from the secondary resources. Copyright © 2014 Elsevier Ltd. All rights reserved.

Effect of EDTA and phosphoric Acid pretreatment on the bonding effectiveness of self-etch adhesives to ground enamel.

PubMed

Ibrahim, Ihab M; Elkassas, Dina W; Yousry, Mai M

2010-10-01

This in vitro study determined the effect of enamel pretreatment with phosphoric acid and ethylenediaminetetraacetic acid (EDTA) on the bond strength of strong, intermediary strong, and mild self-etching adhesive systems. Ninety sound human premolars were used. Resin composite cylinders were bonded to flat ground enamel surfaces using three self-etching adhesive systems: strong Adper Prompt L-Pop (pH=0.9-1.0), intermediary strong AdheSE (pH=1.6-1.7), and mild Frog (pH=2). Adhesive systems were applied either according to manufacturer instructions (control) or after pretreatment with either phosphoric acid or EDTA (n=10). After 24 hours, shear bond strength was tested using a universal testing machine at a cross-head speed of 0.5 mm/minute. Ultra-morphological characterization of the surface topography and resin/enamel interfaces as well as representative fractured enamel specimens were examined using scanning electron microscopy (SEM). Neither surface pretreatment statistically increased the mean shear bond strength values of either the strong or the intermediary strong self-etching adhesive systems. However, phosphoric acid pretreatment significantly increased the mean shear bond strength values of the mild self-etching adhesive system. SEM examination of enamel surface topography showed that phosphoric acid pretreatment deepened the same etching pattern of the strong and intermediary strong adhesive systems but converted the irregular etching pattern of the mild self-etching adhesive system to a regular etching pattern. SEM examination of the resin/enamel interface revealed that deepening of the etching pattern was consistent with increase in the length of resin tags. EDTA pretreatment had a negligible effect on ultra-morphological features. Use of phosphoric acid pretreatment can be beneficial with mild self-etching adhesive systems for bonding to enamel.

Effect of EDTA and Phosphoric Acid Pretreatment on the Bonding Effectiveness of Self-Etch Adhesives to Ground Enamel

PubMed Central

Ibrahim, Ihab M.; Elkassas, Dina W.; Yousry, Mai M.

2010-01-01

Objectives: This in vitro study determined the effect of enamel pretreatment with phosphoric acid and ethylenediaminetetraacetic acid (EDTA) on the bond strength of strong, intermediary strong, and mild self-etching adhesive systems. Methods: Ninety sound human premolars were used. Resin composite cylinders were bonded to flat ground enamel surfaces using three self-etching adhesive systems: strong Adper Prompt L-Pop (pH=0.9–1.0), intermediary strong AdheSE (pH=1.6–1.7), and mild Frog (pH=2). Adhesive systems were applied either according to manufacturer instructions (control) or after pretreatment with either phosphoric acid or EDTA (n=10). After 24 hours, shear bond strength was tested using a universal testing machine at a cross-head speed of 0.5 mm/minute. Ultra-morphological characterization of the surface topography and resin/enamel interfaces as well as representative fractured enamel specimens were examined using scanning electron microscopy (SEM). Results: Neither surface pretreatment statistically increased the mean shear bond strength values of either the strong or the intermediary strong self-etching adhesive systems. However, phosphoric acid pretreatment significantly increased the mean shear bond strength values of the mild self-etching adhesive system. SEM examination of enamel surface topography showed that phosphoric acid pretreatment deepened the same etching pattern of the strong and intermediary strong adhesive systems but converted the irregular etching pattern of the mild self-etching adhesive system to a regular etching pattern. SEM examination of the resin/enamel interface revealed that deepening of the etching pattern was consistent with increase in the length of resin tags. EDTA pretreatment had a negligible effect on ultra-morphological features. Conclusions: Use of phosphoric acid pretreatment can be beneficial with mild self-etching adhesive systems for bonding to enamel. PMID:20922162

Poly(ethylene imine)-based granular sorbents by a new process of templated gel-filling. High capacity and selectivity of copper sorption in acidic and alkaline media

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chanda, M.; Rempel, G.L.

A new process has been developed for making granular gel-type sorbents from chelating resins using metal ion as template. Named as templated gel-filling, the process uses the chosen metal as templating host ion on high-surface-area silica to build a templated gel layer from a solution of the chelating resin in a suitable solvent in which the resin is soluble but its metal complex is insoluble. After cross-linking the templated gel layer, the silica support is removed by alkali to produce a hollow shell of the templated gel. The shells are then soaked in a concentrated aqueous solution of the samemore » metal ion and suspended in the same resin solution to afford gel-filling. The shells thus filled with metal-templated gel are treated with cross-linking agent, followed by acid to remove the template ion and activate the resin for metal sorption. Poly(ethyleneimine) and its partially ethylated derivative have been used to produce granular gel-type sorbents by this process, with Cu(II) as the template ion. These sorbents are found to offer high capacity and selectivity for copper over nickel, cobalt, and zinc in both acidic and alkaline media. Containing a relatively high fraction of imbibed water, the sorbents exhibit markedly enhanced rate behavior, in both sorption and stripping.« less

Polyvinyl alcohol cross-linked with two aldehydes

NASA Technical Reports Server (NTRS)

Sheibley, D. W.; Rieker, L. L.; Hsu, L. C.; Manzo, M. A. (Inventor)

1982-01-01

A film forming polyvinyl alcohol resin is admixed, in aqueous solution, with a dialdehyde crosslinking agent which is capable of crosslinking the polyvinyl alcohol resin and a water soluble acid aldehyde containing a reactive aldehyde group capable of reacting with hydroxyl groups in the polyvinyl alcohol resin and an ionizable acid hydrogen atom. The dialdehyde is present in an amount sufficient to react with from 1 to 20% by weight of the theoretical amount required to react with all of the hydroxyl groups of the polyvinyl alcohol. The amount of acid aldehyde is from 1 to 50% by weight, same basis, and is sufficient to reduce the pH of the aqueous admixture to 5 or less. The admixture is then formed into a desired physical shape, such as by casting a sheet or film, and the shaped material is then heated to simultaneously dry and crosslink the article.

Energy efficient room temperature synthesis of cardanol-based novolac resin using acoustic cavitation.

PubMed

Jadhav, Nilesh L; Sastry, Sai Krishna C; Pinjari, Dipak V

2018-04-01

The present study deals with synthesis of cardanol-cased novolac (CBN) resin by the condensation reaction between cardanol and formaldehyde using acoustic cavitation. It is a step-growth polymerization which occurs in the presence of an acid catalyst such as adipic acid, citric acid, oxalic acid, sulphuric acid and hydrochloric acid. CBN was also synthesised by a conventional method for the sake of comparison of techniques. The effect of molar ratio, effect of catalyst, effect of different catalyst and effect of power on the conversion to CBN has been studied. The synthesised CBN was characterized using the Fourier Transform Infra Red Spectroscopy (FTIR), Gel Permeation Chromatography (GPC), Nuclear Magnetic Resonance (NMR) Spectroscopy and Thermogravimetric Analysis (TGA). The reaction was monitored by the Acid value, free formaldehyde content and viscosity of the synthesised product. The reaction time required for the conventionally synthesised CBN was 5 h (300 min) with 120 °C as an operating temperature while sonochemically the time reduced to 30 min at room temperature. The amount of time and energy saved can be quantified. Ultrasound facilitated synthesis was found to be an energy efficient and time-saving method for the synthesis of novolac resin. Copyright © 2017 Elsevier B.V. All rights reserved.

Transient and residual stresses in a pressable glass-ceramic before and after resin-cement coating determined using profilometry.

PubMed

Isgró, G; Addison, O; Fleming, G J P

2011-05-01

The effect of heat-pressing and subsequent pre-cementation (acid-etching) and resin-cementation operative techniques on the development of transient and residual stresses in different thicknesses of a lithium disilicate glass-ceramic were characterised using profilometry prior to biaxial flexure strength (BFS) determination. 60 IPS e.max Press discs were pressed and divested under controlled conditions. The discs were polished on one surface to thicknesses of 0.61±0.05, 0.84±0.08, and 1.06±0.07 mm (Groups A-C, respectively). The mean of the maximum deflection (acid-etching and resin-coating was determined using high resolution profilometery prior to BFS testing. Paired sample t-tests were performed (p<0.05) on the 20 individual samples in each group (Groups A-C) for each comparison. Differences between the baseline quantification and resin-cement coating deflection values and BFS values for Groups A-C were determined using a one-way ANOVA with post hoc Tukey tests (p<0.05). Baseline quantification for Groups A-C identified no significant differences between the group means of the maximum deflection values (p=0.341). Following HF acid-etching, a significant increase in deflection for all groups (p<0.001) was identified compared with the baseline quantification. Additionally, resin-cement coating significantly increased deflection for Group A (p<0.001), Group B (p<0.001) and Group C (p=0.001) specimens for the individual groups. The increased deflection from baseline quantification to resin-cement coating was significantly different (p<0.001) for the three specimen thicknesses, although the BFS values were not. The lower reported baseline quantification range of the mean of the maximum deflection for the IPS e.max(®) Press specimens was predominantly the result of specimen polishing regime inducing a tensile stress state across the surface defect integral which accounted for the observed surface convexity. Acid-etching and resin-cementation had a significant impact on the development and magnitude of the transient and residual stresses in the lithium disilicate glass-ceramic investigated. Copyright © 2011 Elsevier Ltd. All rights reserved.

Analysis of the critical step in catalytic carbodiimide transformation: proton transfer from amines, phosphines, and alkynes to guanidinates, phosphaguanidinates, and propiolamidinates with Li and Al catalysts.

PubMed

Rowley, Christopher N; Ong, Tiow-Gan; Priem, Jessica; Richeson, Darrin S; Woo, Tom K

2008-12-15

While lithium amides supported by tetramethylethylenediamine (TMEDA) are efficient catalysts in the synthesis of substituted guanidines via the guanylation of an amine with carbodiimide, as well as the guanylation of phosphines and conversion of alkynes into propiolamidines, aluminum amides are only efficient catalysts for the guanylation of amides. Density functional theory (DFT) calculations were used to explain this difference in activity. The origin of this behavior is apparent in the critical step where a proton is transferred from the substrate to a metal guanidinate. The activation energies of these steps are modest for amines, phosphines, and alkynes when a lithium catalyst was used, but are prohibitively high for the analogous reactions with phosphines and alkynes for aluminum amide catalysts. Energy decomposition analysis (EDA) indicates that these high activations energies are due to the high energetic cost of the detachment of a chelating guanidinate nitrogen from the aluminum in the proton transfer transition state. Amines are able to adopt an ideal geometry for facile proton transfer to the aluminum guanidinate and concomitant Al-N bond formation, while phosphines and alkynes are not.

Synthesis and Reactivity of a New (Methylene)Phosphine.

DTIC Science & Technology

1981-01-27

the synthesis of a variety of alkyl(silylamino)- 8phosphines Similarly, if two equivalents of the silylmethyl Grignard reagent were used (eq 3), the...n-BuLi (hexane solution), and t-BuLi (pentane solution). The Grignard reagent Me 3SiCH2 MgCl was prepared in Et 0 2 2 solution from Me3SiCH 2C and Mg...trimethylsilyl)amino] (chloro)- (trimethylsilylmethyl)phosphine (1) was prepared by the "one-pot" Grignard method (eqs 1 and 2) which we have used previously for

Patterned Functionalization of Gold and Single Crystal Silicon via Photochemical Reaction of Surface-Confined Derivatives of (Eta5-C5H5)MN(CO)3

DTIC Science & Technology

1990-11-01

output at -355 nm) until significant conversion of the tricarbonyl to the dicarbonyl phosphine was achieved, as determined by IR. The disubstitited product...forms rapidly once the dicarbonyl phosphine is present in solution so care was taken to stop the irradiation prior to extensive formation of...photochemical behavior and yields photoproducts analogous to those formed upon irradiation of (T5 -C 5 H4 )Mn(CO) 3 in the presence of phosphines . 7 UV

Studies on the application of temperature-responsive ion exchange polymers with whey proteins.

PubMed

Maharjan, Pankaj; Campi, Eva M; De Silva, Kirthi; Woonton, Brad W; Jackson, W Roy; Hearn, Milton T W

2016-03-18

Several new types of temperature-responsive ion exchange resins of different polymer composition have been prepared by grafting the products from the co-polymerisation of N-phenylacrylamide, N-iso-propylacrylamide and acrylic acid derivatives onto cross-linked agarose. Analysis of the binding isotherms for these different resins obtained under batch adsorption conditions indicated that the resin based on N-iso-propylacrylamide containing 5% (w/w) N-phenylacrylamide and 5% (w/w) acrylic acid resulted in the highest adsorption capacity, Bmax, for the whey protein, bovine lactoferrin, e.g. 14 mg bovine lactoferrin/mL resin at 4 °C and 62 mg bovine lactoferrin/mL resin at 40 °C, respectively. Under dynamic loading conditions at 40 °C, 94% of the loaded bovine lactoferrin on a normalised mg protein per mL resin basis was adsorbed by this new temperature-responsive ion-exchanger, and 76% was eluted by a single cycle temperature shift to 4 °C without varying the composition of the 10mM sodium dihydrogen phosphate buffer, pH 6.5, or the flow rate. The binding characteristics of these different ion exchange resins with bovine lactoferrin were also compared to results obtained using other resins based on N-isopropylacrylamide but contained N-tert-butylacrylamide rather than N-phenylacrylamide, where the corresponding dynamic capture and release properties for bovine lactoferrin required different temperature conditions of 20 °C and 50 °C, respectively for optimal desorption/adsorption. The cationic protein, bovine lactoperoxidase, was also adsorbed and desorbed with these temperature-responsive resins under similar conditions of changing temperature, whereas the anionic protein, bovine β-lactoglobulin, was not adsorbed under this regime of temperature conditions but instead eluted in the flow-through. Copyright © 2016 Elsevier B.V. All rights reserved.

Biologically Active Polymeric Coating Materials

DTIC Science & Technology

1975-04-01

unsaturated alkyds , or through a condensation reaction of an organometallic oxide and a resin containing carboxylic acid groups as side chains. The...extend the service life of antifouling coatings by means of polymerization of toxicant into paint resins . The coating binder is so constructed that the...from styrene (s6) and polyester (P54, figure 5) organometallic resins . To date, the antifouling performance of epoxy (WS 52B, figure 6) and

Detoxification of Organosolv-Pretreated Pine Prehydrolysates with Anion Resin and Cysteine for Butanol Fermentation.

PubMed

Li, Jing; Shi, Suan; Tu, Maobing; Via, Brain; Sun, Fubao Fuelbio; Adhikari, Sushil

2018-05-02

Bioconversion of lignocellulose to biofuels suffers from the degradation compounds formed during pretreatment and acid hydrolysis. In order to achieve an efficient biomass to biofuel conversion, detoxification is often required before enzymatic hydrolysis and microbial fermentation. Prehydrolysates from ethanol organosolv-pretreated pine wood were used as substrates in butanol fermentation in this study. Six detoxification approaches were studied and compared, including overliming, anion exchange resin, nonionic resin, laccase, activated carbon, and cysteine. It was observed that detoxification by anion exchange resin was the most effective method. The final butanol yield after anion exchange resin treatment was comparable to the control group, but the fermentation was delayed for 72 h. The addition of Ca(OH) 2 was found to alleviate this delay and improve the fermentation efficiency. The combination of Ca(OH) 2 and anion exchange resin resulted in completion of fermentation within 72 h and acetone-butanol-ethanol (ABE) production of 11.11 g/L, corresponding to a yield of 0.21 g/g sugar. The cysteine detoxification also resulted in good detoxification performance, but promoted fermentation towards acid production (8.90 g/L). The effect of salt on ABE fermentation was assessed and the possible role of Ca(OH) 2 was to remove the salts in the prehydrolysates by precipitation.

Phosphine Resistance in Adult and Immature Life Stages of Tribolium castaneum (Coleoptera: Tenebrionidae) and Plodia interpunctella (Lepidoptera: Pyralidae) Populations in California.

PubMed

Gautam, S G; Opit, G P; Hosoda, E

2016-12-01

Phosphine resistance in stored-product insects occurs worldwide and is a major challenge to continued effective use of this fumigant. We determined resistance frequencies and levels of resistance in Tribolium castaneum and Plodia interpunctella collected from California almond storage and processing facilities. Discriminating doses of phosphine were established for eggs and larvae of P. interpunctella and eggs of T. castaneum using laboratory susceptible strains of the two species. For T. castaneum and P. interpunctella eggs, discriminating doses were 62.4 and 107.8 ppm, respectively, over a 3-d fumigation period, and for P. interpunctella larvae, discriminating dose was 98.7 ppm over a 20-h fumigation period. Discriminating dose tests on adults and eggs showed that 4 out of 11 T. castaneum populations tested had resistance frequencies that ranged from 42 to 100% for adults and 54 to 100% for eggs. LC99 values for the susceptible and the most resistant adults of T. castaneum were 7.4 and 356.9 ppm over 3 d, respectively. LC99 values for T. castaneum eggs were 51.5 and 653.9 ppm, respectively. Based on adult data, the most resistant T. castaneum beetle population was 49× more resistant than the susceptible strain. Phosphine resistance frequencies in P. interpunctella eggs ranged from 4 to 20%. Results show phosphine resistance is present in both species in California. Future research will investigate phosphine resistance over a wider geographic area. In addition, the history of pest management practices in facilities where insects tested in this study originated will be determined in order to develop phosphine resistance management strategies for California almond storage and processing facilities. © The Authors 2016. Published by Oxford University Press on behalf of Entomological Society of America. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Fluid extraction using carbon dioxide and organophosphorus chelating agents

DOEpatents

Smart, N.G.; Wai, C.M.; Lin, Y.; Kwang, Y.H.

1998-11-24

Methods for extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical CO{sub 2}, and a chelating agent are described. The chelating agent forms a chelate with the species, the chelate being soluble in the fluid to allow removal of the species from the material. In preferred embodiments the extraction solvent is supercritical CO{sub 2} and the chelating agent comprises an organophosphorous chelating agent, particularly sulfur-containing organophosphorous chelating agents, including mixtures of chelating agents. Examples of chelating agents include monothiophosphinic acid, di-thiophosphinic acid, phosphine sulfite, phosphorothioic acid, and mixtures thereof. The method provides an environmentally benign process for removing metal and metalloids from industrial waste solutions, particularly acidic solutions. Both the chelate and the supercritical fluid can be regenerated and the contaminant species recovered to provide an economic, efficient process. 1 fig.

Fluid extraction using carbon dioxide and organophosphorus chelating agents

DOEpatents

Smart, Neil G.; Wai, Chien M.; Lin, Yuehe; Kwang, Yak Hwa

1998-01-01

Methods for extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical CO.sub.2, and a chelating agent are described. The chelating agent forms a chelate with the species, the chelate being soluble in the fluid to allow removal of the species from the material. In preferred embodiments the extraction solvent is supercritical CO.sub.2 and the chelating agent comprises an organophosphorous chelating agent, particularly sulfur-containing organophosphorous chelating agents, including mixtures of chelating agents. Examples of chelating agents include monothiophosphinic acid, di-thiophosphinic acid, phosphine sulfite, phosphorothioic acid, and mixtures thereof. The method provides an environmentally benign process for removing metal and metalloids from industrial waste solutions, particularly acidic solutions. Both the chelate and the supercritical fluid can be regenerated and the contaminant species recovered to provide an economic, efficient process.

Generator for gallium-68 and compositions obtained therefrom

DOEpatents

Neirinckx, Rudi D.; Davis, Michael A.

1981-01-01

A generator for obtaining radioactive gallium-68 from germanium-68 bound in a resin containing unsubstituted phenolic hydroxyl groups. The germanium-68 is loaded into the resin from an aqueous solution of the germanium-68. A physiologically acceptable solution of gallium-68 having an activity of 0.1 to 50 millicuries per milliliter of gallium-68 solution is obtained. The solution is obtained from the bound germanium-68 which forms gallium-68 in situ by eluting the column with a hydrochloric acid solution to form an acidic solution of gallium-68. The acidic solution of gallium-68 can be neutralized.

Phosphine

Integrated Risk Information System (IRIS)

Phosphine ; CASRN 7803 - 51 - 2 Human health assessment information on a chemical substance is included in the IRIS database only after a comprehensive review of toxicity data , as outlined in the IRIS assessment development process . Sections I ( Health Hazard Assessments for Noncarcinogenic Effect

Hydroxyalkyl phosphine compounds for use as diagnostic and therapeutic pharmaceuticals

DOEpatents

Katti, K.V.; Singh, P.R.; Reddy, V.S.; Katti, K.K.; Volkert, W.A.; Ketring, A.R.

1999-03-02

This research discloses a compound and method of making a compound for use as a diagnostic or therapeutic pharmaceutical comprises a functionalized hydroxyalkyl phosphine ligand and a metal combined with the ligand. 16 figs.

Control of morphology and crystal purity of InP nanowires by variation of phosphine flux during selective area MOMBE

NASA Astrophysics Data System (ADS)

Kelrich, A.; Dubrovskii, V. G.; Calahorra, Y.; Cohen, S.; Ritter, D.

2015-02-01

We present experimental results showing how the growth rate, morphology and crystal structure of Au-catalyzed InP nanowires (NWs) fabricated by selective area metal organic molecular beam epitaxy can be tuned by the growth parameters: temperature and phosphine flux. The InP NWs with 20-65 nm diameters are grown at temperatures of 420 and 480 °C with the PH3 flow varying from 1 to 9 sccm. The NW tapering is suppressed at a higher temperature, while pure wurtzite crystal structure is preferred at higher phosphine flows. Therefore, by combining high temperature and high phosphine flux, we are able to fabricate non-tapered and stacking fault-free InP NWs with the quality that other methods rarely achieve. We also develop a model for NW growth and crystal structure which explains fairly well the observed experimental tendencies.

An efficient synthetic method for organometallic radicals: structures and properties of gold(i)-(nitronyl nitroxide)-2-ide complexes.

PubMed

Suzuki, Shuichi; Kira, Sayaka; Kozaki, Masatoshi; Yamamura, Masaki; Hasegawa, Toru; Nabeshima, Tatsuya; Okada, Keiji

2017-02-21

One-pot synthesis of (nitronyl nitroxide)-gold(i)-phosphine (NN-Au-P) complexes has been developed using chloro(tetrahydrothiophene)gold(i), phosphine ligands, nitronyl nitroxide radicals, and sodium hydroxide. The NN-Au-P complexes can be easily handled because they were quite stable under aerated conditions in both solution and crystalline states. They showed weak absorption bands with vibrational structures in the 450-650 nm region. The oxidation potentials assigned to the NN moieties of NN-Au-P complexes with aromatic phosphines were observed around -0.1 V vs. Fc/Fc + (-0.11 V for NN-Au-1, -0.08 V for NN-Au-2, -0.13 V for NN-Au-5, and -0.07 V for NN-Au-6), somewhat lower than that of NN-Au-P complexes with aliphatic phosphines (-0.25 V for NN-Au-3 and -0.17 V for NN-Au-4).

Heliotropium huascoense resin exudate: chemical constituents and defensive properties.

PubMed

Villarroel, L; Torres, R; Urzúa, A; Reina, M; Cabrera, R; González-Coloma, A

2001-09-01

From the resinous exudate of Heliotropium huascoense a new compound, rel-(8R,9R)-carrizaloic acid, (1) (3-[rel-(8R,9R-9-hydroxy-9,13,13-trimethyl-12-oxo-10-cyclohexenyl)methyl]-4-methoxybenzoic acid), and three known flavonoids, [3-methylgalangin, 3,7-dimethylgalangin, and (-)-alpinone] have been isolated. The structure of 1 was determined by spectral and chemical methods. Several plant defensive properties of 1 (insecticidal and antifungal) have been evaluated.

Interaction of tertiary phosphines with lignin-type, alpha,beta-unsaturated aldehydes in water.

PubMed

Moiseev, Dmitry V; Patrick, Brian O; James, Brian R; Hu, Thomas Q

2007-10-29

To learn more about the bleaching action of pulps by (hydroxymethyl)phosphines, lignin chromophores, such as the alpha,beta-unsaturated aromatic aldehydes, sinapaldehyde, coniferylaldehyde, and coumaraldehyde, were reacted with the tertiary phosphines R2R'P [R = R' = Me, Et, (CH2)3OH, iPr, cyclo-C6H11, (CH2)2CN; R = Me or Et, R' = Ph; R = Ph, R' = Me, m-NaSO3-C6H4] in water at room temperature under argon. In all cases, initial nucleophilic attack of the phosphine occurs at the activated C=C bond to form a zwitterionic monophosphonium species. With the phosphines PR3 [R = Me, Et, (CH2)3OH] and with R2R'P (R = Me or Et, R' = Ph), the zwitterion undergoes self-condensation to give a bisphosphonium zwitterion that can react with aqueous HCl to form the corresponding dichloride salts (as a mixture of R,R- and S,S-enantiomers); X-ray structures are presented for the bisphosphonium chlorides synthesized from the Et3P and Me3P reactions with sinapaldehyde. With the more bulky phosphines, iPr3P, MePPh2, (cyclo-C6H11)3P, and Na[Ph2P(m-SO3-C6H4)], only an equilibrium of the monophosphonium zwitterion with the reactant aldehyde is observed. The weakly nucleophilic [NC(CH2)2]3P does not react with sinapaldehyde. An analysis of some exceptional 1H NMR data within the prochiral phosphorus centers of the bisphosphonium chlorides is also presented.

Total etch technique and cavity isolation.

PubMed

Fusayama, T

1992-01-01

In the total etch technique for chemically adhesive composite restorations, the phosphoric acid penetrates only 10 microns or less into the vital dentin with the dentinal tubules being filled with the odontoblast processes. The acid is completely removed by subsequent air-water jet spray washing. The tubule apertures are perfectly sealed by the protective bonding agent layer with the resin tags adhering to the tubule walls and the resin-impregnated dentin surface. Isolation of the cavity from moisture contamination is required for only less than a few seconds after drying the etched cavity until the bonding agent coating and after this coating until the composite resin placement. Such a short time for isolation is quite easy even without a rubber dam when a trained assistant is cooperating.

Method for the chemical separation of GE-68 from its daughter Ga-68

DOEpatents

Fitzsimmons, Jonathan M.; Atcher, Robert W.

2010-06-01

The present invention is directed to a generator apparatus for separating a daughter gallium-68 radioisotope substantially free of impurities from a parent gernanium-68 radioisotope, including a first resin-containing column containing parent gernanium-68 radioisotope and daughter gallium-68 radioisotope, a source of first eluent connected to said first resin-containing column for separating daughter gallium-68 radioisotope from the first resin-containing column, said first eluent including citrate whereby the separated gallium is in the form of gallium citrate, a mixing space connected to said first resin-containing column for admixing a source of hydrochloric acid with said separated gallium citrate whereby gallium citrate is converted to gallium tetrachloride, a second resin-containing column for retention of gallium-68 tetrachloride, and, a source of second eluent connected to said second resin-containing column for eluting the daughter gallium-68 radioisotope from said second resin-containing column.

21 CFR 177.1556 - Polyaryletherketone resins.

Code of Federal Regulations, 2012 CFR

2012-04-01

... molecular weight of 20,000 grams per mole, as determined by light scattering measurements in sulfuric acid at room temperature. (b) Optional adjuvant substances. The basic polyaryletherketone resins... centimeter) of food-contact surface, when extracted at reflux temperature for 2 hours with the following...

21 CFR 177.1556 - Polyaryletherketone resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

... molecular weight of 20,000 grams per mole, as determined by light scattering measurements in sulfuric acid at room temperature. (b) Optional adjuvant substances. The basic polyaryletherketone resins... centimeter) of food-contact surface, when extracted at reflux temperature for 2 hours with the following...

21 CFR 177.1556 - Polyaryletherketone resins.

Code of Federal Regulations, 2011 CFR

2011-04-01

... molecular weight of 20,000 grams per mole, as determined by light scattering measurements in sulfuric acid at room temperature. (b) Optional adjuvant substances. The basic polyaryletherketone resins... centimeter) of food-contact surface, when extracted at reflux temperature for 2 hours with the following...

21 CFR 177.1556 - Polyaryletherketone resins.

Code of Federal Regulations, 2013 CFR

2013-04-01

... molecular weight of 20,000 grams per mole, as determined by light scattering measurements in sulfuric acid at room temperature. (b) Optional adjuvant substances. The basic polyaryletherketone resins... centimeter) of food-contact surface, when extracted at reflux temperature for 2 hours with the following...

Reduction of non-enzymatic browning of orange juice and semi-concentrates by removal of reaction substrate.

PubMed

Sharma, Satish K; Juyal, Shashibala; Rao, V K; Yadav, V K; Dixit, A K

2014-07-01

A study was conducted to standardize the technology for the removal of amino acids (one of the browning reaction substrates) from sweet orange cv. Malta Common juice to reduce colour and quality deterioration in single strength juice and during subsequent concentration. Juice of sweet orange (Citrus sinensis) cv. Malta Common fruits was extracted by screw type juice extractor, preserved in 500 ppm SO2 and clarified by using "Pectinase CCM" enzyme (0.2% for 2 h at 50 ± 2 °C). For removal of amino acids juice was passed under gravity through a glass column packed with an acidic cation exchange resin (CER), Dowex-50 W and quantity to be treated in one lot was standardized. The CER treated and untreated juices were concentrated to 15 and 30°Brix in a rotary vacuum evaporator. Results indicate that 121 ml of orange juice when passed through a glass column (5 cm internal diameter) packed with cation exchange resin (Dowex-50 W) upto a height of 8 cm, could remove about 98.4% of the amino acids with minimum losses in other juice constituents. With cation exchange resin treatment, the non-enzymatic browning and colour deterioration of orange juice semi-concentrates was reduced to about 3 folds in comparison to untreated counterparts. The retention of vitamin C and sugars was also better in semi-concentrates prepared from cation exchange resin treated juice. Thus, cation exchange resin treatment of orange juice prior to concentration and storage is highly beneficial in reduction of non-enzymatic browning, colour deterioration and retention of nutritional, sensory quality of product during preparation and storage.

Nucleophilic Chiral Phosphines: Powerful and Versatile Catalysts for Asymmetric Annulations

PubMed Central

Xiao, Yumei; Guo, Hongchao; Kwon, Ohyun

2016-01-01

Recent advances in chiral-phosphine-catalyzed asymmetric annulation reactions; including annulations of allenes, alkynes, Morita–Baylis–Hillman (MBH) carbonates, and ketenes; and their applications in the synthesis of bioactive molecules and natural products are reviewed. PMID:28077882

Soil and sediment sample analysis for the sequential determination of natural and anthropogenic radionuclides.

PubMed

Michel, H; Levent, D; Barci, V; Barci-Funel, G; Hurel, C

2008-02-15

A new sequential method for the determination of both natural (U, Th) and anthropogenic (Sr, Cs, Pu, Am) radionuclides has been developed for application to soil and sediment samples. The procedure was optimised using a reference sediment (IAEA-368) and reference soils (IAEA-375 and IAEA-326). Reference materials were first digested using acids (leaching), 'total' acids on hot plate, and acids in microwave in order to compare the different digestion technique. Then, the separation and purification were made by anion exchange resin and selective extraction chromatography: transuranic (TRU) and strontium (SR) resins. Natural and anthropogenic alpha radionuclides were separated by uranium and tetravalent actinide (UTEVA) resin, considering different acid elution medium. Finally, alpha and gamma semiconductor spectrometer and liquid scintillation spectrometer were used to measure radionuclide activities. The results obtained for strontium-90, cesium-137, thorium-232, uranium-238, plutonium-239+240 and americium-241 isotopes by the proposed method for the reference materials provided excellent agreement with the recommended values and good chemical recoveries. Plutonium isotopes in alpha spectrometry planchet deposits could be also analysed by ICPMS.

Bilirubin and bile acids removal by haemoperfusion through synthetic resin "Persorb".

PubMed

Filip, K; Malý, J; Horký, J; Tlustáková, M; Kálal, J; Vrána, M

1990-01-01

A new type of styrene-divinylbenzene copolymer coated with polyhema was tested for biocompatibility and ability to remove bile acid, bilirubin, phenols and cholesterol in dogs with surgically induced biliary obstruction. After 4-hr hemoperfusion through a polypropylene column containing 325 g of resin, performed 7-10 days after the ligature of the cystic and common bile duct, the serum levels of bile acids, bilirubin, phenols and cholesterol decreased by 60.9 +/- 30.3% (p less than 0.001), 34.8 +/- 12.2% (p less than 0.001), 19.4 +/- 15.6% (p less than 0.001) and 15.3 +/- 4.2% (p less than 0.05), respectively. The procedure was well tolerated, no bleeding or other adverse reactions occurred. The average platelet count decreased by 19.4 +/- 15.6% (p less than 0.05). Hemoperfusion through the Czechoslovak resin coated with polyhema is safe and efficient for removal of bile acids and other protein-bound and lipid-soluble substances which accumulate in cholestatic syndromes and hepatic failure. Thus, it may play an important role in the treatment of such events as a method of artificial liver support.

Effect of different surface treatments on the shear bond strength of nanofilled composite repairs

PubMed Central

Ahmadizenouz, Ghazaleh; Esmaeili, Behnaz; Taghvaei, Arnica; Jamali, Zahra; Jafari, Toloo; Amiri Daneshvar, Farshid; Khafri, Soraya

2016-01-01

Background. Repairing aged composite resin is a challenging process. Many surface treatment options have been proposed to this end. This study evaluated the effect of different surface treatments on the shear bond strength (SBS) of nano-filled composite resin repairs. Methods. Seventy-five cylindrical specimens of a Filtek Z350XT composite resin were fabricated and stored in 37°C distilled water for 24 hours. After thermocycling, the specimens were divided into 5 groups according to the following surface treatments: no treatment (group 1); air abrasion with 50-μm aluminum oxide particles (group 2); irradiation with Er:YAG laser beams (group 3); roughening with coarse-grit diamond bur + 35% phosphoric acid (group 4); and etching with 9% hydrofluoric acid for 120 s (group 5). Another group of Filtek Z350XT composite resin samples (4×6 mm) was fabricated for the measurement of cohesive strength (group 6). A silane coupling agent and an adhesive system were applied after each surface treatment. The specimens were restored with the same composite resin and thermocycled again. A shearing force was applied to the interface in a universal testing machine. Data were analyzed using one-way ANOVA and post hoc Tukey tests (P < 0.05). Results. One-way ANOVA indicated significant differences between the groups (P < 0.05). SBS of controls was significantly lower than the other groups; differences between groups 2, 3, 4, 5 and 6 were not significant. Surface treatment with diamond bur + 35% phosphoric acid resulted in the highest bond strength. Conclusion. All the surface treatments used in this study improved the shear bond strength of nanofilled composite resin used. PMID:27092209

Green Thermosetting Factory: Novel Star-Shaped Biobased Systems and Their Thermosetting Resins; Synthesis and Characterization

NASA Astrophysics Data System (ADS)

Jahandideh, Arash

Increasing attentions toward sustainable development, economic and environmental issues have led to many attempts at replacing the petroleum-based materials with renewables. Substitution of petroleum-based platforms with green alternative technologies is beneficiary in different ways. Using bio-renewables reduces the dependency of the national plastic industry to the petroleum resources and substantially promotes the environmental profile and sustainability of the product. It is expected that the emergence of the corn-based thermosetting industry generates substantial profits for the corn production sector. Developments in the emerging biobased thermosets are spectacular from a technological point of view. However, there are still several disadvantages associated with the current biobased thermosetting resins, e.g. low processability, environmental issues, expensive sources and poor thermomechanical properties. Use of natural fibers not only contributes to the production of a more environmentally friendly product, but also has advantages such as low-weight product and low manufacturing costs. The results of this study show a possibility of production of biocomposites made from natural fibers and star-shaped resin, synthesized from corn-based materials (lactic acid and itaconic acid) and different multihydroxyl core molecules. These resins were synthesized via two-steps strategy: polycondensation of the monomers with the core molecules followed by end-functionalization of the branches by methacrylic anhydride or itaconic acid. The results have shown that these resin are capable of competing with or even surpassing fossil fuel based resins in terms of cost and eco-friendliness aspect. Inexpensive biobased raw material, better environmental profile, low viscosity, and better processability of the matrix along with better thermomechanical properties of the produced biocomposites are of advantages expected for these systems.

Effects of reaction pH on properties and performance of urea-formaldehyde resins

Treesearch

Chung-Yun Hse; Zhi-Yuan Xia; Bunchiro Tomita

1994-01-01

Urea formaldehyde resins were formulated with combination variables of three reaction pH (1.0, 4.8, and 8.0) and four molar ratios of formaldehyde to urea (2.5, 3.0, 3.5, and 4.0). The resins were prepared by placing all formaldehyde and water in reaction kettle and pH was adjusted with sulfuric acid and sodium hydroxide, respectively. Urea was added in 15 equal parts...

Sensomics analysis of key bitter compounds in the hard resin of hops (Humulus lupulus L.) and their contribution to the bitter profile of Pilsner-type beer.

PubMed

Dresel, Michael; Dunkel, Andreas; Hofmann, Thomas

2015-04-08

Recent brewing trials indicated the occurrence of valuable bitter compounds in the hard resin fraction of hop. Aiming at the discovery of these compounds, hop's ε-resin was separated by means of a sensory guided fractionation approach and the key taste molecules were identified by means of UV/vis, LC-TOF-MS, and 1D/2D-NMR studies as well as synthetic experiments. Besides a series of literature known xanthohumol derivatives, multifidol glucosides, flavon-3-on glycosides, and p-coumaric acid esters, a total of 11 bitter tastants are reported for the first time, namely, 1",2"-dihydroxanthohumol F, 4'-hydroxytunicatachalcone, isoxantholupon, 1-methoxy-4-prenylphloroglucinol, dihydrocyclohumulohydrochinone, xanthohumols M, N, and P, and isoxanthohumols M, N, and P, respectively. Human sensory analysis revealed low bitter recognition threshold concentrations ranging from 5 (co-multifidol glucopyranoside) to 198 μmol/L (trans-p-coumaric acid ethyl ester) depending on their chemical structure. For the first time, LC-MS/MS quantitation of these taste compounds in Pilsner-type beer, followed by taste re-engineering experiments, revealed the additive contribution of iso-α-acids and the identified hard resin components to be truly necessary and sufficient for constructing the authentic bitter percept of beer. Finally, brewing trails using the ε-resin as the only hop source impressively demonstrated the possibility to produce beverages strongly enriched with prenylated hop flavonoids.

Drought stress alters the concentration of wood terpenoids in Scots pine and Norway spruce seedlings.

PubMed

Turtola, Satu; Manninen, Anne-Marja; Rikala, Risto; Kainulainen, Pirjo

2003-09-01

Drought is known to have an impact on the resistance of conifers to various pests, for example, by affecting resin flow in trees. Little is known, however, about the quantitative and qualitative changes in resin when trees are growing in low moisture conditions. We exposed Scots pine (Pinus sylvestris L.) and Norway spruce (Picea abies (L.) Karst.) seedlings to medium and severe drought stress for two growing seasons and analyzed the monoterpenes and resin acids in the main stem wood after two years of treatment. In addition to secondary chemistry, we measured the level of nutrients in the needles and the growth response of seedlings. After the first year of treatment, drought stress did not affect the growth of seedlings, but in the second year, shoot growth was retarded, especially in Scots pine. In both conifer species, severe drought increased the concentrations of several individual monoterpenes and resin acids. Total monoterpenes and resin acids were 39 and 32% higher in severe drought-treated Scots pine seedlings than in the controls, and 35 and 45% higher in Norway spruce seedlings. In Scots pine needles, the concentrations of nitrogen and phosphorus increased, while magnesium and calcium decreased compared to controls. In Norway spruce needles, nutrient concentrations were not affected. The results suggest that drought stress substantially affects both the growth of conifers and the chemical quality of the wood. We discuss the potential trade-off in growth and defense of small conifer seedlings.

Parallel solid-phase synthesis and high-throughput 1H NMR evaluation of a 96-member 1,2,4-trisubstituted-pyrimidin-6-one-5-carboxylic acid library.

PubMed

Hamper, Bruce C; Kesselring, Allen S; Chott, Robert C; Yang, Shengtian

2009-01-01

A solid-phase organic synthesis method has been developed for the preparation of trisubstituted pyrimidin-6-one carboxylic acids 12, which allows elaboration to a 3-dimensional combinatorial library. Three substituents are introduced by initial Knoevenagel condensation of an aldehyde and malonate ester resin 7 to give resin bound 1. Cyclization of 1 with an N-substituted amidine 10, oxidation, and cleavage afforded pyrimidinone 12. The initial solid-phase reaction sequence was followed by gel-phase (19)FNMR and direct-cleavage (1)H NMR of intermediate resins to determine the optimal conditions. The scope of the method for library production was determined by investigation of a 3 x 4 pilot library of twelve compounds. Cyclocondensation of N-methylamidines and 7 followed by CAN oxidation gave mixtures of the resin bound pyrimidin-6-one 11 and the regioisomeric pyrimidin-4-one 15, which after cleavage from the resin afforded a nearly 1:1 mixture of pyrimidin-6-one and pyrimidin-4-one carboxylic acids 12 and 16, respectively. The regiochemical assignment was confirmed by ROESY1D and gHMBC NMR experiments. A library was prepared using 8 aldehydes, 3 nitriles, and 4 amines to give a full combinatorial set of 96 pyrimidinones 12. Confirmation of structural identity and purity was carried out by LCMS using coupled ELS detection and by high-throughput flow (1)H NMR.

Metal binding characterization and conformational studies using Raman microscopy of resin-bound poly(aspartic acid).

PubMed

Stair, Jacqueline L; Holcombe, James A

2007-03-01

The metal binding capacities, conditional stability constants, and secondary structure of immobilized polyaspartic acid (PLAsp) (n = 6, 20, and 30) on TentaGel resin were determined when binding Mg2+, Co2+, Cd2+, and Ni2+. Metal binding to the synthesized peptides was evaluated using breakthrough curves from a packed microcolumn and flame atomic absorption spectrophotometry (FAAS) detection. The metal capacities reached values of 590, 2160, and 3710 mumol of metal/g of resin for the 6-mer, 20-mer, and 30-mer, respectively, and this resulted in 2-3 residues per metal for all peptides and metals tested. Surprisingly, the concentrated environment of the resin along with the spatial distribution of attachment groups allowed for most residues to participate in metal binding regardless of the peptide length. Conditional stability constants calculated using single metal binding isotherms indicated that binding strength decreased as the chain length increased on the resin. Raman microscopy on single beads was used to determine PLAsp secondary structure, and all peptides were of a mixed conformation (i.e., beta-sheets, alpha-helices, random chain, etc.) during neutral conditioning and metal binding. Uniquely, the longer 20-mer and 30-mer peptides showed a distinct change from a mixed conformation to beta-sheets and alpha-helices during metal release with acid. This study confirms that metal release by longer immobilized peptides is often assisted by a conformational change, which easily spoils the binding cavity, while shorter peptides may release metal primarily by H+ displacement.

Marginal integrity of low-shrinkage and methacrylate-based composite resins: Effect of three different hemostatic agents

PubMed Central

Khoroushi, Maryam; Sahraneshin-Samani, Mahsa

2016-01-01

Background Moisture control is very important in restorative procedures in dentistry. Use of hemostatic agents helps control moisture; however, they might result in changes on enamel and dentin surfaces, affecting composite resin bond quality. The aim of this in vitro study was to evaluate the marginal microleakage of two different composite resins with the use of three different hemostatic agents. Material and Methods Standardized Class V cavities were prepared on the buccal and lingual surfaces of 48 premolars with cervical margins 1 mm apical to the cementoenamel junction (CEJ). The samples were randomly divided into 8 groups. In groups 1 to 4, an etch-and-rinse adhesive (Adper Single Bond) was applied as the bonding system, followed by exposure to different hemostatic agent: group 1: no hemostatic agent (control); group 2: ViscoStat; group 3: ViscoStat Clear; and group 4: trichloracetic acid, as hemostatic agents. The cavities were restored with Z-250 composite resin. In group 5 to 8 Silorane System Adhesive (Filtek P90 Adhesive) was applied as a bonding agent, followed by exposure to different hemostatic agents in a manner similar to that in groups 1to 4. The cavities were restored with Filtek P90, a low-shrinkage composite resin. The samples in each group were evaluated for dye penetration under a stereomicroscope at ×36 after 24 hours and a 500-round thermocycling procedure at enamel and dentin margins. Statistical analysis was carried out using Kruskal-Wallis and Mann-Whitney tests (α=0.05). Results Z-250 composite resin exhibited significantly higher dentin microleakage scores compared to Filtek P90 (P = 0.004). Trichloracetic acid increased dentin microleakage with Filtek P90 (P=0.033). Conclusions Under the limitations of this in vitro study, application of hemostatic agents did not affect microleakage of the two tested composite resins except for trichloracetic acid that increased marginal microleakage when used with Filtek P90. Key words:Composite resin, dental leakage, hemostatics, silorane system adhesive. PMID:27034759

Influence of laser structuring of PEEK, PEEK-GF30 and PEEK-CF30 surfaces on the shear bond strength to a resin cement.

PubMed

Henriques, Bruno; Fabris, Douglas; Mesquita-Guimarães, Joana; Sousa, Anne C; Hammes, Nathalia; Souza, Júlio C M; Silva, Filipe S; Fredel, Márcio C

2018-08-01

The aim of this study was to evaluate the influence of a surface conditioning technique using laser ablation and acid etching on PEEK substrate on its bonding strength to a resin cement. Cylindrical specimens of unfilled PEEK, 30% glass fiber reinforced PEEK and 30% carbon fiber reinforced PEEK were separated in four groups according to the following surface treatments: acid etching with H 2 SO 4 , laser ablation with 200 µm holes spaced 400 µm apart (D2E4), laser ablation with 200 µm holes spaced 600 µm apart (D2E6), and laser ablation (D2E4) followed by acid etching. A dual-curing resin cement (Allcem CORE) was then applied to the PEEK surface. Specimens were aged in distilled water at 37 °C for 24 h. Shear bond strength tests were performed to the fracture of the samples. Two-way ANOVA statistical analysis was performed with a significance level of 0.05. Scanning electron microscopy analysis was performed to analyse the conditioned and fracture surfaces. SEM images of the test interfaces showed that the resin cement could not flow in the holes designed by the laser ablation on the PEEK surface. The shear bond strength of PEEK to resin cement was not improved by the surface modification of the PEEK. Also, there was a statistically significant decrease in shear bond strength for unfilled PEEK specimens. On carbon or glass reinforced PEEK, the change was not significant. SEM images of the fracture surfaces revealed that the failure mode was mainly adhesive. Although laser ablation promoted the PEEK surface modification by the formation of retentive holes, the test resin cement could not thoroughly flow on the rough modified surfaces to establish an effective mechanical interlocking. That negatively affected the shear bonding strength of PEEK to the resin cement. Further studies should be carried out to increase the bonding between PEEK and resin cements. Copyright © 2018 Elsevier Ltd. All rights reserved.

Highly convergent synthesis of chiral bicyclophosphinates by domino hydrophosphinylation/Michael/Michael reaction.

PubMed

Fourgeaud, Pierre; Daydé, Bénédicte; Volle, Jean-Noël; Vors, Jean-Pierre; Van der Lee, Arie; Pirat, Jean-Luc; Virieux, David

2011-10-07

Diastereoselective domino reactions of iminoalcohols and allenyl H-phosphinates produce chiral phosphorus bicycles in a regio- and stereoselective fashion. A predictive model for diastereoselection is used for these new chiral phosphinic esters. © 2011 American Chemical Society

Evaluation of P1'-diversified phosphinic peptides leads to the development of highly selective inhibitors of MMP-11.

PubMed

Matziari, Magdalini; Beau, Fabrice; Cuniasse, Philippe; Dive, Vincent; Yiotakis, Athanasios

2004-01-15

Phosphinic peptides were previously reported to be potent inhibitors of several matrixins (MMPs). To identify more selective inhibitors of MMP-11, a matrixin overexpressed in breast cancer, a series of phosphinic pseudopeptides bearing a variety of P(1)'-side chains has been synthesized, by parallel diversification of a phosphinic template. The potencies of these compounds were evaluated against a set of seven MMPs (MMP-2, MMP-7, MMP-8, MMP-9, MMP-11, MMP-13, and MMP-14). The chemical strategy applied led to the identification of several phosphinic inhibitors displaying high selectivity toward MMP-11. One of the most selective inhibitors of MMP-11 in this series, compound 22, exhibits a K(i) value of 0.23 microM toward MMP-11, while its potency toward the other MMPs tested is 2 orders of magnitude lower. This remarkable selectivity may rely on interactions of the P(1)'-side chain atoms of these inhibitors with residues located at the entrance of the S(1)'-cavity of MMP-11. The design of inhibitors able to interact with residues located at the entrance of MMPs' S(1)'-cavity might represent an alternative strategy to identify selective inhibitors that will fully differentiate one MMP among the others.

Intumescent formulations based on lignin and phosphinates for the bio-based textiles

NASA Astrophysics Data System (ADS)

Mandlekar, N.; Cayla, A.; Rault, F.; Giraud, S.; Salaün, F.; Malucelli, G.; Guan, J.

2017-10-01

This study investigates new intumescent formulations based on lignin and phosphinates to improve the flame retardant properties of Polyamide 11, while preserving the bio-based characteristics of this latter. Lignin has the advantage of being a bio-based compound and can be effectively used as carbon source for the design of intumescent systems in combination with other flame retardant additives. Metal phosphinates belong to a novel class of phosphorus flame retardants. Despite their increasing use, there is lack of scientific understanding as far as their fire retardancy mechanism is considered, especially in char forming polymeric materials. In this context, Polyamide 11 was melt blended with lignin and metal phosphinates. The possibility of melt spinning the prepared blends were assessed through melt flow index (MFI) tests; thermogravimetric (TG) analyses and cone calorimetry tests were exploited for investigating the thermal stability and the combustion behaviour of the obtained products, respectively. MFI results indicate that some formulations are suitable for melt spinning processes to generate flame retardant multifilament. Furthermore, the combination of lignin and phosphinates provides charring properties to polyamide 11. Finally, cone calorimetry data confirmed that the designed intumescent formulations could remarkably reduce PHRR through formation of protective char layer, hence slowing down the combustion process.

Penguins significantly increased phosphine formation and phosphorus contribution in maritime Antarctic soils.

PubMed

Zhu, Renbin; Wang, Qing; Ding, Wei; Wang, Can; Hou, Lijun; Ma, Dawei

2014-11-14

Most studies on phosphorus cycle in the natural environment focused on phosphates, with limited data available for the reduced phosphine (PH3). In this paper, matrix-bound phosphine (MBP), gaseous phosphine fluxes and phosphorus fractions in the soils were investigated from a penguin colony, a seal colony and the adjacent animal-lacking tundra and background sites. The MBP levels (mean 200.3 ng kg(-1)) in penguin colony soils were much higher than those in seal colony soils, animal-lacking tundra soils and the background soils. Field PH3 flux observation and laboratory incubation experiments confirmed that penguin colony soils produced much higher PH3 emissions than seal colony soils and animal-lacking tundra soils. Overall high MBP levels and PH3 emissions were modulated by soil biogeochemical processes associated with penguin activities: sufficient supply of the nutrients phosphorus, nitrogen, and organic carbon from penguin guano, high soil bacterial abundance and phosphatase activity. It was proposed that organic or inorganic phosphorus compounds from penguin guano or seal excreta could be reduced to PH3 in the Antarctic soils through the bacterial activity. Our results indicated that penguin activity significantly increased soil phosphine formation and phosphorus contribution, thus played an important role in phosphorus cycle in terrestrial ecosystems of maritime Antarctica.

Penguins significantly increased phosphine formation and phosphorus contribution in maritime Antarctic soils

PubMed Central

Zhu, Renbin; Wang, Qing; Ding, Wei; Wang, Can; Hou, Lijun; Ma, Dawei

2014-01-01

Most studies on phosphorus cycle in the natural environment focused on phosphates, with limited data available for the reduced phosphine (PH3). In this paper, matrix-bound phosphine (MBP), gaseous phosphine fluxes and phosphorus fractions in the soils were investigated from a penguin colony, a seal colony and the adjacent animal-lacking tundra and background sites. The MBP levels (mean 200.3 ng kg−1) in penguin colony soils were much higher than those in seal colony soils, animal-lacking tundra soils and the background soils. Field PH3 flux observation and laboratory incubation experiments confirmed that penguin colony soils produced much higher PH3 emissions than seal colony soils and animal-lacking tundra soils. Overall high MBP levels and PH3 emissions were modulated by soil biogeochemical processes associated with penguin activities: sufficient supply of the nutrients phosphorus, nitrogen, and organic carbon from penguin guano, high soil bacterial abundance and phosphatase activity. It was proposed that organic or inorganic phosphorus compounds from penguin guano or seal excreta could be reduced to PH3 in the Antarctic soils through the bacterial activity. Our results indicated that penguin activity significantly increased soil phosphine formation and phosphorus contribution, thus played an important role in phosphorus cycle in terrestrial ecosystems of maritime Antarctica. PMID:25394572

Selective concentration of aromatic bases from water with a resin adsorbent

USGS Publications Warehouse

Stuber, H.A.; Leenheer, J.A.

1983-01-01

Aromatic bases are concentrated from water on columns of a resin adsorbent and recovered by aqueous-acid elution. The degree of concentration attainable depends on the ratio of the capacity factor (k) of the neutral form of the amine to that of the ionized form. Capacity factors of ionic forms of amines on XAD-8 resin (a methylacrylic ester polymer) are greater than zero, ranging from 20 to 250 times lower than those of their neutral forms; they increase with increasing hydrophobicity of the amine. Thus, desorption by acid is an edition (k during desorption >0) rather than a displacement (k during desorption = 0) process. The degree of concentration attainable on XAD-8 resin varies with the hydrophobicity of the amine, being limited for hydrophilic solutes (for example, pyridine) by small neutral-form k's, reaching a maximum for amines of intermediate hydrophobicity (for example, quinoline), and decreasing for more hydrophobc solutes (for example, acridine) because of their large ionic-form k's.

Biocatalytic Synthesis of Epoxy Resins from Fatty Acids as a Versatile Route for the Formation of Polymer Thermosets with Tunable Properties.

PubMed

Torron, Susana; Semlitsch, Stefan; Martinelle, Mats; Johansson, Mats

2016-12-12

The work herein presented describes the synthesis and polymerization of series of bio-based epoxy resins prepared through lipase catalyzed transesterification. The epoxy-functional polyester resins with various architectures (linear, tri-branched, and tetra-branched) were synthesized through condensation of fatty acids derived from epoxidized soybean oil and linseed oil with three different hydroxyl cores under bulk conditions. The selectivity of the lipases toward esterification/transesterification reactions allowed the formation of macromers with up to 12 epoxides in the backbone. The high degree of functionality of the resins resulted in polymer thermosets with T g values ranging from -25 to over 100 °C prepared through cationic polymerization. The determining parameters of the synthesis and the mechanism for the formation of the species were determined through kinetic studies by 1 H NMR, SEC, and molecular modeling studies. The correlation between macromer structure and thermoset properties was studied through real-time FTIR measurements, DSC, and DMA.

Preparative separation and purification of rosmarinic acid from perilla seed meal via combined column chromatography.

PubMed

Tang, Weizhuo; Sun, Baoshan; Zhao, Yuqing

2014-02-01

In this study, the preparative separation and purification of rosmarinic acid (RA) from perilla seed meal (PSM), which is a by-product of edible oil production, was achieved using combined column chromatography over macroporous and polyamide resins. To optimize the RA enrichment process, the performance and separation characteristics of nine selected macroporous resins with different chemical and physical properties were investigated. SP825 resin was the most effective: the content of RA increased from 0.27% in the original extract to 16.58% in the 50% ethanol fraction (a 61.4-fold increase). During further purification treatment on polyamide resin, 90.23% pure RA could be obtained in the 70% ethanol fraction. RA with a higher purity (>95%) could also be easily obtained using one crystallization operation. The proposed method is simple, easily operated, cost-effective, and environmentally friendly and is suitable for both large-scale RA production and waste management. Copyright © 2013 Elsevier B.V. All rights reserved.

Maintenance and Preservation of Concrete Structures. Report 3. Abrasion-Erosion Resistance of Concrete.

DTIC Science & Technology

1980-07-01

ORG. REPORT NUMBER 7. AUTH R(s) 11. CONTRACT OR GRANT NUMBER(&) Tony C Liu C I PERFORMING ORGANIZATION NAME AND ADDRESS 10. PROGRAM ELEMENT. PROJECT... organic acids, alkalis, solvents, etc. Polyurethane 25. Two types of elastomeric polyurethane systems were investi- gated: T19 and T21. a. The T19 specimens...polymer with a viscosity of about 450 cps at 250 C. The catalyst used to polymerize the resin is an organic acid. The mixing ratio of the resin to

Influence of caries infiltrant contamination on shear bond strength of different adhesives to dentin.

PubMed

Jia, Liuhe; Stawarczyk, Bogna; Schmidlin, Patrick R; Attin, Thomas; Wiegand, Annette

2013-03-01

To analyze whether the contamination with a caries infiltrant system impairs the adhesive performance of etch-and-rinse and self-etching adhesives on dentin. Dentin contamination with the caries infiltrant system (Icon, DMG) was simulated by applying either hydrochloric acid (15 % HCl, Icon Etch, 15 s), the resin infiltrant (Icon infiltrant, 4 min), or both prior to the application of the respective adhesives (each group n = 10). In the control groups, the etch-and-rinse adhesive (Optibond FL, Kerr) and the self-etching adhesive (iBOND Self Etch, Hereaus) were applied without former contamination with the infiltrant system. Additionally, the adhesive performance of the resin infiltrant alone was tested. Shear bond strength of a nano-hybrid composite was analyzed after thermocycling (5,000×, 5-55°C) of the specimens and analyzed by ANOVA/Scheffé post hoc tests (p < 0.05) and Weibull statistics. Failure mode was inspected under a stereomicroscope at × 25 magnification. Contamination with the resin infiltrant alone did not impair shear bond strength, while contamination with hydrochloric acid or with hydrochloric acid and the resin infiltrant reduced shear bond strength (MPa) of the adhesives (Optibond FL: 20.5 ± 3.6, iBOND Self Etch: 17.9 ± 2.6) significantly. Hydrochloric acid contamination increased the number of adhesive failures. The adhesive performance of the caries infiltrant system alone was insufficient. The contamination with the caries infiltrant system impaired the shear bond strength of conventional dental adhesives. Contamination of the caries infiltrant system on dentin should be avoided due to the detrimental effect of hydrochloric acid etching.

Determination of trace heavy metals in soil and sediments by atomic spectrometry following preconcentration with Schiff bases on Amberlite XAD-4.

PubMed

Kara, Derya; Fisher, Andrew; Hill, Steve J

2009-06-15

A matrix separation and analyte preconcentration system using Amberlite XAD copolymer resins functionalized by Schiff base reactions coupled with atomic spectrometry has been developed. Three different functionalized Amberlite XAD resins were synthesized using 4-phenylthiosemicarbazide, 2,3-dihydroxybenzaldehyde and 2-thiophenecarboxaldehyde as reagents. These resins could be used to preconcentrate transition and other trace heavy metal analytes from nitric acid digests of soil and sediment samples. Analyte retention was shown to work well at pH 6.0. After treatment of the digests with sodium fluoride and buffering to pH 6, samples that contain extremely large concentrations of iron were analysed for trace analytes without the excess iron overloading the capacity of the resin. The analytes Cd, Co, Cu, Ni and Pb were preconcentrated from acid extracts of certified soil/sediment samples and then eluted with 0.1M HNO(3) directly to the detection system. Flame atomic absorption spectrometry was used as a means of detection during the studies. The efficiency of the chelating resin and the accuracy of the proposed method were evaluated by the analysis of soil (SO-2) and sediment (LGC 6157 and MESS-3) certified reference materials.

Fatigue of the Resin-Enamel Bonded Interface and the Mechanisms of Failure

PubMed Central

Yahyazadehfar, Mobin; Mutluay, Mustafa Murat; Majd, Hessam; Ryou, Heonjune; Arola, Dwayne

2013-01-01

The durability of adhesive bonds to enamel and dentin and the mechanisms of degradation caused by cyclic loading are important to the survival of composite restorations. In this study a novel method of evaluation was used to determine the strength of resin-enamel bonded interfaces under both static and cyclic loading, and to identify the mechanisms of failure. Specimens with twin interfaces of enamel bonded to commercial resin composite were loaded in monotonic and cyclic 4-point flexure to failure within a hydrated environment. Results for the resin-enamel interface were compared with those for the resin composite (control) and values reported for resin-dentin adhesive bonds. Under both modes of loading the strength of the resin-enamel interface was significantly (p≤0.0001) lower than that of the resin composite and the resin-dentin bonded interface. Fatigue failure of the interface occurred predominately by fracture of enamel, adjacent to the interface, and not due to adhesive failures. In the absence of water aging or acid production of biofilms, the durability of adhesive bonds to enamel is lower than that achieved in dentin bonding. PMID:23571321

Method to upgrade bio-oils to fuel and bio-crude

DOEpatents

Steele, Philip H; Pittman, Jr., Charles U; Ingram, Jr., Leonard L; Gajjela, Sanjeev; Zhang, Zhijun; Bhattacharya, Priyanka

2013-12-10

This invention relates to a method and device to produce esterified, olefinated/esterified, or thermochemolytic reacted bio-oils as fuels. The olefinated/esterified product may be utilized as a biocrude for input to a refinery, either alone or in combination with petroleum crude oils. The bio-oil esterification reaction is catalyzed by addition of alcohol and acid catalyst. The olefination/esterification reaction is catalyzed by addition of resin acid or other heterogeneous catalyst to catalyze olefins added to previously etherified bio-oil; the olefins and alcohol may also be simultaneously combined and catalyzed by addition of resin acid or other heterogeneous catalyst to produce the olefinated/esterified product.

21 CFR 173.5 - Acrylate-acrylamide resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

... and acrylic acid, with the greater part of the polymer being composed of acrylamide units. (2) Sodium polyacrylate-acrylamide resin is produced by the polymerization and subsequent hydrolysis of acrylonitrile in a sodium silicate-sodium hydroxide aqueous solution, with the greater part of the polymer being composed of...

21 CFR 173.5 - Acrylate-acrylamide resins.

Code of Federal Regulations, 2011 CFR

2011-04-01

... and acrylic acid, with the greater part of the polymer being composed of acrylamide units. (2) Sodium polyacrylate-acrylamide resin is produced by the polymerization and subsequent hydrolysis of acrylonitrile in a sodium silicate-sodium hydroxide aqueous solution, with the greater part of the polymer being composed of...

ADSORPTION OF CERIUM VALUES FROM AQUEOUS SOLUTIONS

DOEpatents

Roberts, F.P.

1963-08-13

Cerium can be removed from aqueous nitric acid (2 to 13 M) solutions by passing the latter over a PbO/sub 2/-containing anion exchange resin. The cerium is taken up by the resin, while any lanthanides, yttrium, and strontium present remain in the solution. (AEC)

EVALUATION OF METHODS FOR THE ISOLATION OR CONCENTRATION OF ORGANIC SUBSTANCES FROM WATER USING XAD-4 QUATERNARY RESIN

EPA Science Inventory

A synthetic resin (Amberlite XAD-4 Quaternary in the OH- form) was evaluated as an adsorption medium for the concentration/isolation of acids, amines, aldehydes, carbohydrates, chlorobiphenyls, esters, hydrocarbons, ketones, phenols, polynuclear aromatic hydrocarbons, and trihalo...

Synthesis of cross-linked chitosan modified with the glycine moiety for the collection/concentration of bismuth in aquatic samples for ICP-MS determination.

PubMed

Oshita, Koji; Noguchi, Osamu; Oshima, Mitsuko; Motomizu, Shoji

2007-10-01

A chelating resin, cross-linked chitosan modified with the glycine moiety (glycine-type chitosan resin), was developed for the collection and concentration of bismuth in aquatic samples for ICP-MS measurements. The adsorption behavior of bismuth and 55 elements on glycine-type chitosan resin was systematically examined by passing a sample solution containing 56 elements through a mini-column packed with the resin (wet volume; 1 ml). After eluting the elements adsorbed on the resin with nitric acid, the eluates were measured by ICP-MS. The glycine-type chitosan resin could adsorb several cations by a chelating mechanism and several oxoanions by an anion-exchange mechanism. Especially, the resin could adsorb almost 100% Bi(III) over a wide pH region from pH 2 to 6. Bismuth could be strongly adsorbed at pH 3, and eluted quantitatively with 10 ml of 3 M nitric acid. A column pretreatment method with the glycine-type chitosan resin was used prior to removal of high concentrations of matrices in a seawater sample and the preconcentration of trace bismuth in river water samples for ICP-MS measurements. The column pretreatment method was also applied to the determination of bismuth in real samples by ICP-MS. The LOD of bismuth was 0.1 pg ml(-1) by 10-fold column preconcentration for ICP-MS measurements. The analytical results for bismuth in sea and river water samples by ICP-MS were 22.9 +/- 0.5 pg ml(-1) (RSD, 2.2%) and 2.08 +/- 0.05 pg ml(-1) (RSD, 2.4%), respectively.

Synthesis, characterization and application of ion exchange resin as a slow-release fertilizer for wheat cultivation in space

NASA Astrophysics Data System (ADS)

Li, Bowei; Dong, Chen; Chu, Zhengpei; Zhang, Weizhe; Wang, Minjuan; Liu, Hong; Xie, Beizhen

2016-10-01

In addition to the bio-regenerative air revitalization, water recycling and waste management systems and their associated challenges, enhancing the crop yield with less fertilizer input for sustainable food production in space is also a challenge that needs to be overcome. The purpose of this study is to investigate the feasibility of applying ion exchange resin as a slow-release fertilizer for wheat cultivation in space. Strong-acid cationic exchange resins and weak-base anion exchange resins soaked in 1X, 5X, 10X and 15X Hoagland nutrient solutions, respectively, were used as fertilizers in clinoptilolite to cultivate wheat plants, and the morphological and physiological characteristics of the wheat plants were studied and compared with that of the wheat planted in vermiculite and nutrient solutions. The results showed that more ions were attached on the surface of the ion exchange resins as the solution concentration increased. After 14 days, the fresh weight of wheat planted in the ion exchange resin-clinoptilolite (IER-clinoptilolite) treated with 10X and 15X solutions were 190% and 192% higher than that of wheat planted in nutrient solution with the same concentration. Chlorophyll content of wheat plants cultivated in the two kinds of solid medium is significantly higher than that of liquid cultivation. The lowest peroxidase (POD) activity and malondialdehyde (MDA) contents of wheat plants cultivated in the IER-clinoptilolite appeared on the 14th day. According to all the experimental data, it's promising to produce slow-release nutrient fertilizer by using strong-acid cationic exchange resins and weak-base anion exchange resins for wheat cultivation in space.

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

PubMed

Roane, J E; DeVol, T A

2002-11-01

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

Coordination chemistry and catalytic activity of N-heterocyclic carbene iridium(I) complexes.

PubMed

Fu, Ching-Feng; Chang, Yung-Hung; Liu, Yi-Hong; Peng, Shei-Ming; Elsevier, Cornelis J; Chen, Jwu-Ting; Liu, Shiuh-Tzung

2009-09-21

Iridium complexes [(CO)2Ir(NHC-R)Cl] (R = Et-, 3a; PhCH2-, 3b; CH3OCH2CH2-, 3c; o-CH3OC6H4CH2-, 3d; NHC: N-heterocyclic carbene) are prepared via the carbene transfer from [(NHC-R)W(CO)5] to [Ir(COD)Cl]2. By using substitution with 13CO, we are able to estimate the activation energy (G) of the CO-exchange in 3a-d, which are in the range of 12-13 kcal mol-1, significantly higher than those for the phosphine analog [(CO)2Ir(PCy3)Cl]. Reactions of 3b and 3d with an equimolar amount of PPh3 result in the formation of the corresponding [(NHC-R)Ir(CO)(PPh3)Cl] with the phosphine and NHC in trans arrangement. In contrast, the analogous reaction of 3a or 3c with phosphine undergoes substitution followed by the anion metathesis to yield the corresponding di-substituted [(NHC-R)Ir(CO)(PPh3)2]BF4 (5) directly. Treatment of 3b or 3d with excess of PPh3 leads to the similar product of disubstitution 5b and 5d. The analysis for the IR data of carbonyliridium complexes provides the estimation of electron-donating power of NHCs versus phosphines. The NHC moiety on the iridium center cannot be replaced by phosphines, even 1,2-bis(diphenylphohino)ethane (dppe). All the carbene moieties on the iridium complexes are inert toward sulfur treatment, indicating a strong interaction between NHC and the iridium centers. Complexes 3a-c are active on the catalysis of the oxidative cyclization of 2-(o-aminophenyl)ethanol to yield the indole compound. The phosphine substituted complexes or analogs are less active.

Studies on the effects of phosphine on Salmonella enterica serotype Enteritidis in culture medium and in black pepper (Piper nigrum).

PubMed

Castro, M F P M; Rezende, A C B; Benato, E A; Valentini, S R T; Furlani, R P Z; Tfouni, S A V

2011-04-01

The effect of phosphine on Salmonella enterica serotype Enteritidis inoculated in culture medium and in black pepper grains (Piper nigrum), as well as on the reduction of the microbial load of the dried and moisturized product, was verified. The postfumigation effect was verified in inoculated samples with 0.92 and 0.97 water activity (a(w)) exposed to 6 g/m(3) phosphine for 72 h, dried to 0.67 a(w), and stored for 24, 48, and 72 h. No decreases were observed in Salmonella Enteritidis populations in culture medium when fumigant concentrations up to 6 g/m(3) were applied for 48 h at 35°C. However, the colonies showed reductions in size and atypical coloration as the phosphine concentration increased. No reduction in Salmonella counts occurred on the inoculated dried samples after fumigation. On the other hand, when phosphine at concentrations of 6 g/m(3) was applied on moisturized black pepper for 72 h, decreases in Salmonella counts of around 80% were observed. The counts of total aerobic mesophilic bacterium populations of the dried and moisturized black pepper were not affected by the fumigant treatment. The results of the postfumigation studies indicated that Salmonella Enteritidis was absent in the fumigated grains after drying and storage for 72 h, indicating a promising application for this technique. It was concluded that for Salmonella Enteritidis control, phosphine fumigation could be applied to black pepper grains before drying and the producers should rigidly follow good agricultural practices, mainly during the drying process, in order to avoid product recontamination. Additional work is needed to confirm the findings with more Salmonella serotypes and strains.

Separation of arsenic(III) and arsenic(V) in ground waters by ion-exchange

USGS Publications Warehouse

Ficklin, W.H.

1983-01-01

The predominant species of arsenic in ground water are probably arsenite and arsenate. These can be separated with a strong anion-exchange resin (Dowex 1 ?? 8; 100-200 mesh, acetate form) in a 10 cm ?? 7 mm column. Samples are filtered and acidified with concentrated hydrochloric acid (1 ml per 100 ml of sample) at the sample site. Five ml of the acidified sample are used for the separation. At this acidity, As(III) passes through the acetate-form resin, and As(V) is retained. As(V) is eluted by passage of 0.12M hydrochloric acid through the column (resulting in conversion of the resin back into the chloride form). Samples are collected in 5-ml portions up to a total of 20 ml. The arsenic concentration in each portion is determined by graphite-furnace atomic-absorption spectrophotometry. The first two fractions give the As(III) concentration and the last two the As(V) concentration. The detection limit for the concentration of each species is 1 ??g l. ?? 1983.

Synthetic applications of hypophosphite derivatives in reduction.

PubMed

Guyon, Carole; Métay, Estelle; Popowycz, Florence; Lemaire, Marc

2015-08-07

The development of new tools for the reduction of organic functions to reach high chemo- and stereo-selectivity is an important research domain. Although, aluminum and boron hydrides are commonly used, they suffer from environmentally and safety issues. In particular, at industrial scale, the search for more specific and efficient reagents with a lower ecological impact remains one of the main objectives of organic chemists. This review captures highlights from literature concerning phosphonic and phosphinic acid derivatives as reducing agents and evaluates their potential as alternatives, in particular to boron and aluminum hydrides.

Chiral allene-containing phosphines in asymmetric catalysis

PubMed Central

Cai, Feng; Pu, Xiaotao; Qi, Xiangbing; Lynch, Vincent; Radha, Akella; Ready, Joseph M.

2011-01-01

Traditionally, ligands used in asymmetric catalysis have contained either stereogenic atoms or hindered single bonds (atropisomerism), or both. Here we demonstrate that allenes, chiral 1,2-dienes, appended with basic functionality can serve as ligands for transition metals. We describe an allene-containing bisphosphine that, when coordinated to Rh(I), promotes the asymmetric addition of aryl boronic acids to α-keto esters with high enantioselectivity. Solution and solid-state structural analysis reveals that one olefin of the allene can coordinate to transition metals generating bi- and tri-dentate ligands. PMID:21972824

Hydrometallurgical methods of recovery of scandium from the wastes of various technologies

NASA Astrophysics Data System (ADS)

Molchanova, T. V.; Akimova, I. D.; Smirnov, K. M.; Krylova, O. K.; Zharova, E. V.

2017-03-01

The recovery of scandium from the wastes of the production of uranium, titanium, iron-vanadium, and alumina is studied. The applied acid schemes of scandium transfer to a solution followed by ion-exchange recovery and extraction concentration of scandium ensure the precipitation of crude scandium oxides containing up to 5% Sc2O3. Scandium oxides of 99.96-99.99% purity are formed after additional refining of these crude oxides according to an extraction technology using a mixture 15% multiradical phosphine oxide or Cyanex-925 + 15% tributyl phosphate in kerosene.

Diaminophosphine oxide ligand enabled asymmetric nickel-catalyzed hydrocarbamoylations of alkenes.

PubMed

Donets, Pavel A; Cramer, Nicolai

2013-08-14

Chiral trivalent phosphorus species are the dominant class of ligands and the key controlling element in asymmetric homogeneous transition-metal catalysis. Here, novel chiral diaminophosphine oxide ligands are described. The arising catalyst system with nickel(0) and trimethylaluminum efficiently activates formamide C-H bonds under mild conditions providing pyrrolidones via intramolecular hydrocarbamoylation in a highly enantioselective manner with as little as 0.25% mol catalyst loading. Mechanistically, the secondary phosphine oxides behave as bridging ligands for the nickel center and the Lewis acidic organoaluminum center to give a heterobimetallic catalyst with superior reactivity.

Phenylethynyl Containing Reactive Additives

NASA Technical Reports Server (NTRS)

Connell, John W. (Inventor); Smith, Joseph G., Jr. (Inventor); Hergenrother, Paul M. (Inventor)

2002-01-01

Phenylethynyl containing reactive additives were prepared from aromatic diamines containing phenylethynyl groups and various ratios of phthalic anhydride and 4-phenylethynylphthalic anhydride in glacial acetic acid to form the imide in one step or in N-methyl-2-pyrrolidi none to form the amide acid intermediate. The reactive additives were mixed in various amounts (10% to 90%) with oligomers containing either terminal or pendent phenylethynyl groups (or both) to reduce the melt viscosity and thereby enhance processability. Upon thermal cure, the additives react and become chemically incorporated into the matrix and effect an increase in crosslink density relative to that of the host resin. This resultant increase in crosslink density has advantageous consequences on the cured resin properties such as higher glass transition temperature and higher modulus as compared to that of the host resin.

URANIUM RECOVERY AND PURIFICATION PROCESS AND PRODUCTION OF HIGH PURITY URANIUM TETRAFLUORIDE

DOEpatents

Bailes, R.H.; Long, R.S.; Grinstead, R.R.

1957-09-17

A process is described wherein an anionic exchange technique is employed to separate uramium from a large variety of impurities. Very efficient and economical purification of contamimated uranium can be achieved by treatment of the contaminated uranium to produce a solution containing a high concentration of chloride. Under these conditions the uranium exists as an aniomic chloride complex. Then the uranium chloride complex is adsorbed from the solution on an aniomic exchange resin, whereby a portion of the impurities remain in the solution and others are retained with the uramium by the resin. The adsorbed impurities are then removed by washing the resin with pure concentrated hydrochloric acid, after which operation the uranium is eluted with pure water yielding an acidic uranyl chloride solution of high purity.

Investigation of bracket bonding for orthodontic treatments using en-face optical coherence tomography

NASA Astrophysics Data System (ADS)

Sinescu, Cosmin; Negrutiu, Meda L.; Hughes, Michael; Bradu, Adrian; Todea, Carmen; Rominu, Roxana; Dodenciu, Dorin; Laissue, Philippe L.; Podoleanu, Adrian G.

2008-04-01

Despite good diagnosis and treatment planning, orthodontic treatment can fail if bonding fails. It is now common practice to address the aesthetic appearance of patients using aesthetic brackets instead of metal ones. Therefore, bonding aesthetic brackets has become an issue for orthodontists today. Orthodontic bonding is mainly achieved using composite resin but can also be performed with glass ionomer or resin cements. For improving the quality of bonding, the enamel is acid etched for 30 seconds with 38% phosphoric acid and then a bonding agent is applied. In our study we investigated and compared the quality of bonding between ceramic brackets, polymeric brackets and enamel, respectively using a new investigation method-OCT. The aim of our study was to evaluate the resin layer at the bracket base-tooth interface.

Phenylethynyl Containing Reactive Additives

NASA Technical Reports Server (NTRS)

Connell, John W. (Inventor); Smith, Joseph G., Jr. (Inventor); Hergenrother, Paul M. (Inventor)

2002-01-01

Phenylethynyl containing reactive additives were prepared from aromatic diamine, containing phenylethvnvl groups and various ratios of phthalic anhydride and 4-phenylethynviphthalic anhydride in glacial acetic acid to form the imide in one step or in N-methyl-2-pvrrolidinone to form the amide acid intermediate. The reactive additives were mixed in various amounts (10% to 90%) with oligomers containing either terminal or pendent phenylethynyl groups (or both) to reduce the melt viscosity and thereby enhance processability. Upon thermal cure, the additives react and become chemically incorporated into the matrix and effect an increase in crosslink density relative to that of the host resin. This resultant increase in crosslink density has advantageous consequences on the cured resin properties such as higher glass transition temperature and higher modulus as compared to that of the host resin.

ELUTION OF URANIUM FROM RESIN

DOEpatents

McLEan, D.C.

1959-03-10

A method is described for eluting uranium from anion exchange resins so as to decrease vanadium and iron contamination and permit recycle of the major portion of the eluats after recovery of the uranium. Diminution of vanadium and iron contamination of the major portion of the uranium is accomplished by treating the anion exchange resin, which is saturated with uranium complex by adsorption from a sulfuric acid leach liquor from an ore bearing uranium, vanadium and iron, with one column volume of eluant prepared by passing chlorine into ammonium hydroxide until the chloride content is about 1 N and the pH is about 1. The resin is then eluted with 8 to 9 column volumes of 0.9 N ammonium chloride--0.1 N hydrochloric acid solution. The eluants are collected separately and treated with ammonia to precipitate ammonium diuranate which is filtered therefrom. The uranium salt from the first eluant is contaminated with the major portion of ths vanadium and iron and is reworked, while the uranium recovered from the second eluant is relatively free of the undesirable vanadium and irons. The filtrate from the first eluant portion is discarded. The filtrate from the second eluant portion may be recycled after adding hydrochloric acid to increase the chloride ion concentration and adjust the pH to about 1.

Efficient one-step Suzuki arylation of unprotected halonucleosides, using water-soluble palladium catalysts.

PubMed

Western, Elizabeth C; Daft, Jonathan R; Johnson, Edward M; Gannett, Peter M; Shaughnessy, Kevin H

2003-08-22

Modification of nucleosides to give pharmaceutically active compounds, mutagenesis models, and oligonucleotide structural probes continues to be of great interest. The aqueous-phase modification of unprotected halonucleosides is reported herein. Using a catalyst derived from tris(3-sulfonatophenyl)phosphine (TPPTS) and palladium acetate, 8-bromo-2'-deoxyguanosine (8-BrdG) is coupled with arylboronic acids to give 8-aryl-2'-deoxyguanosine adducts (8-ArdG) in excellent yield in a 2:1 water:acetonitrile solvent mixture. The TPPTS ligand was found to be superior to water-soluble alkylphosphines for this coupling reaction. The coupling chemistry has been extended to 8-bromo-2'-deoxyadenosine (8-BrdA) and 5-iodo-2'-deoxyuridine (5-IdU), as well as the ribonucleosides 8-bromoguanosine and 8-bromoadenosine. Good to excellent yields of arylated adducts are obtained in all cases. With use of tri(4,6-dimethyl-3-sulfonatophenyl)phosphine (TXPTS), the Suzuki coupling of 8-BrdA and 5-IdU can be accomplished in less than 1 h at room temperature. This methodology represents an efficient and general method for halonucleoside arylation that does not require prior protection of the nucleoside.

Controlling the size of hot injection made nanocrystals by manipulating the diffusion coefficient of the solute.

PubMed

De Nolf, Kim; Capek, Richard K; Abe, Sofie; Sluydts, Michael; Jang, Youngjin; Martins, José C; Cottenier, Stefaan; Lifshitz, Efrat; Hens, Zeger

2015-02-25

We investigate the relation between the chain length of ligands used and the size of the nanocrystals formed in the hot injection synthesis. With two different CdSe nanocrystal syntheses, we consistently find that longer chain carboxylic acids result in smaller nanocrystals with improved size dispersions. By combining a more in-depth experimental investigation with kinetic reaction simulations, we come to the conclusion that this size tuning is due to a change in the diffusion coefficient and the solubility of the solute. The relation between size tuning by the ligand chain length and the coordination of the solute by the ligands is further explored by expanding the study to amines and phosphine oxides. In line with the weak coordination of CdSe nanocrystals by amines, no influence of the chain length on the nanocrystals is found, whereas the size tuning brought about by phosphine oxides can be attributed to a solubility change. We conclude that the ligand chain length provides a practical handle to optimize the outcome of a hot injection synthesis in terms of size and size dispersion and can be used to probe the interaction between ligands and the actual solute.

40 CFR 721.10087 - Substituted alkyl phosphine oxide (generic).

Code of Federal Regulations, 2010 CFR

2010-07-01

... are: (i) Industrial, commercial, and consumer activities. Requirements as specified in § 721.80(s... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Substituted alkyl phosphine oxide (generic). 721.10087 Section 721.10087 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED...

Cation exchange concentraion of the Americium product from TRUEX

DOE Office of Scientific and Technical Information (OSTI.GOV)

Barney, G.S.; Cooper, T.D.; Fisher, F.D.

1991-06-01

A transuranic extraction (TRUEX) process has been developed to separate and recover plutonium, americium, and other transuranic (TRU) elements from acid wastes. The main objective of the process is to reduce the effluent to below the TRU limit for actinide concentrations (<100 nCi/g of material) so it can be disposed of inexpensively. The process yields a dilute nitric acid stream containing low concentrations of the extracted americium product. This solution also contains residual plutonium and trace amounts of iron. The americium will be absorbed into a cation exchange resin bed to concentrate it for disposal or for future use. Themore » overall objective of these laboratory tests was to determine the performance of the cation exchange process under expected conditions of the TRUEX process. Effects of acid, iron, and americium concentrations on americium absorption on the resin were determined. Distribution coefficients for americium absorption from acide solutions on the resin were measured using batch equilibrations. Batch equilibrations were also used to measure americium absorption in the presence of complexants. This data will be used to identify complexants and solution conditions that can be used to elute the americium from the columns. The rate of absorption was measured by passing solutions containing americium through small columns of resin, varying the flowrates, and measuring the concentrations of americium in the effluent. The rate data will be used to estimate the minimum bed size of the columns required to concentrate the americium product. 11 refs. , 10 figs., 2 tabs.« less

Comparative assessment of different recycling methods of orthodontic brackets for clinical use.

PubMed

de Oliveira Correia, Ayla M; de Souza Matos, Felipe; Pilli Jóias, Renata; de Mello Rode, Sigmar; Cesar, Paulo F; Paranhos, Luiz R

2017-06-01

This study aimed to assess bond strength of the resin/bracket interface, under in-vitro shear stress, of metal brackets recycled by different clinical protocols. Sixty stainless steel orthodontic brackets were bonded on acrylic resin. The Transbond XT™ resin was applied at the base of the bracket aided by a matrix, obtaining 1 mm of thickness, and photoactivated with a LED device (40 s; 500 mW/cm2). Samples were randomly divided into four groups (N.=15) according to the reconditioning/recycling protocol: aluminum oxide (AO) 90 µm; hydrofluoric acid 60 s (HA60); hydrofluoric acid 120 s (HA120); hydrofluoric acid 60 s + silane (HA60S). After recycling, the resin was applied at the base of the bracket for shear testing in a universal testing machine (0.5 mm/min). After reconditioning/recycling, the surfaces were analyzed by Scanning Electron Microscopy. Data obtained after the shear test were subjected to ANOVA and Tukey's test (P<0.05). The AO group presented higher values of shear bond strength compared to the other reconditioning/recycling protocols (P<0.05). The HA120 and HA60S groups presented statistically similar results, but HA120 presented strength below the recommended limit. The recycling technique by aluminum oxide sandblasting was more effective for reconditioning orthodontic brackets when compared to the other protocols. The reconditioning technique with 10% hydrofluoric acid followed by the application of silane bonding agent may be used as an alternative protocol.

High-rate synthesis of phosphine-stabilized undecagold nanoclusters using a multilayered micromixer.

PubMed

Jin, Hyung Dae; Garrison, Anna; Tseng, T; Paul, Brian K; Chang, Chih-Hung

2010-11-05

Growth in the potential applications of nanomaterials has led to a focus on the development of new manufacturing approaches for these materials. In particular, an increased demand due to the unique properties of nanomaterials requires a substantial yield of high-performance materials and a simultaneous reduction in the environmental impact of these processes. In this paper, a high-rate production of phosphine-stabilized undecagold nanoclusters was achieved using a layer-up strategy which involves the use of microlamination architectures; the patterning and bonding of thin layers of material (laminae) to create a multilayered micromixer in the range of 25-250 µm thick was used to step up the production of phosphine-stabilized undecagold nanoclusters. The continuous production of highly monodispersed phosphine-stabilized undecagold nanoclusters at a rate of about 11.8 (mg s(-1)) was achieved using a microreactor with a size of 1.687 cm(3). This result is about 500 times over conventional batch syntheses based on the production rate per reactor volume.

High-rate synthesis of phosphine-stabilized undecagold nanoclusters using a multilayered micromixer

NASA Astrophysics Data System (ADS)

Jin, Hyung Dae; Garrison, Anna; Tseng, T.; Paul, Brian K.; Chang, Chih-Hung

2010-11-01

Growth in the potential applications of nanomaterials has led to a focus on the development of new manufacturing approaches for these materials. In particular, an increased demand due to the unique properties of nanomaterials requires a substantial yield of high-performance materials and a simultaneous reduction in the environmental impact of these processes. In this paper, a high-rate production of phosphine-stabilized undecagold nanoclusters was achieved using a layer-up strategy which involves the use of microlamination architectures; the patterning and bonding of thin layers of material (laminae) to create a multilayered micromixer in the range of 25-250 µm thick was used to step up the production of phosphine-stabilized undecagold nanoclusters. The continuous production of highly monodispersed phosphine-stabilized undecagold nanoclusters at a rate of about 11.8 (mg s - 1) was achieved using a microreactor with a size of 1.687 cm3. This result is about 500 times over conventional batch syntheses based on the production rate per reactor volume.

21 CFR 177.1500 - Nylon resins.

Code of Federal Regulations, 2013 CFR

2013-04-01

... condensation of adipic acid, 1,3-benzenedimethanamine, and alpha-(3-aminopropyl)-omega-(3-amino-propoxy)poly- oxyethylene under such conditions that the alpha-(3-amino-propyl)-omega-(3-aminopropoxy) polyoxyethylene... 21 Food and Drugs 3 2013-04-01 2013-04-01 false Nylon resins. 177.1500 Section 177.1500 Food and...

21 CFR 177.1500 - Nylon resins.

Code of Federal Regulations, 2011 CFR

2011-04-01

... condensation of adipic acid, 1,3-benzenedimethanamine, and alpha-(3-aminopropyl)-omega-(3-amino-propoxy)poly- oxyethylene under such conditions that the alpha-(3-amino-propyl)-omega-(3-aminopropoxy) polyoxyethylene... 21 Food and Drugs 3 2011-04-01 2011-04-01 false Nylon resins. 177.1500 Section 177.1500 Food and...

21 CFR 177.1500 - Nylon resins.

Code of Federal Regulations, 2012 CFR

2012-04-01

... condensation of adipic acid, 1,3-benzenedimethanamine, and alpha-(3-aminopropyl)-omega-(3-amino-propoxy)poly- oxyethylene under such conditions that the alpha-(3-amino-propyl)-omega-(3-aminopropoxy) polyoxyethylene... 21 Food and Drugs 3 2012-04-01 2012-04-01 false Nylon resins. 177.1500 Section 177.1500 Food and...

21 CFR 177.1500 - Nylon resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

... condensation of adipic acid, 1,3-benzenedimethanamine, and alpha-(3-aminopropyl)-omega-(3-amino-propoxy)poly- oxyethylene under such conditions that the alpha-(3-amino-propyl)-omega-(3-aminopropoxy) polyoxyethylene... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Nylon resins. 177.1500 Section 177.1500 Food and...

EFFECT OF THE DECHLORINATING AGENT, ASCORBIC ACID, ON THE MUTAGENICITY OF CHLORINATED WATER SAMPLES

EPA Science Inventory

XAD resin adsorption has been widely used to concentrate the organic compounds present in chlorinated drinking waters prior to mutagenicity testing. Previous work has shown that mutagenic artifcats can arise due to the reaction of residual chlorine with the resins. Althrough the ...

Synthesis of γ-hydroxypropyl P-chirogenic (±)-phosphorus oxide derivatives by regioselective ring-opening of oxaphospholane 2-oxide precursors

PubMed Central

Binyamin, Iris; Meidan-Shani, Shoval

2015-01-01

Summary The synthesis of P-chirogenic (±)-phosphine oxides and phosphinates via selective nucleophilic ring opening of the corresponding oxaphospholanes is described. Two representative substrates: the phosphonate 2-ethoxy-1,2-oxaphospholane 2-oxide and the phosphinate 2-phenyl-1,2-oxaphospholane 2-oxide were reacted with various Grignard reagents to produce a single alkyl/aryl product. These products may possess further functionalities in addition to the phosphorus center such as the γ-hydroxypropyl group which results from the ring opening and π-donor moieties such as aryl, allyl, propargyl and allene which originates from the Grignard reagent. PMID:26425187

Phosphine-catalyzed cycloadditions of allenic ketones: new substrates for nucleophilic catalysis.

PubMed

Wallace, Debra J; Sidda, Rachel L; Reamer, Robert A

2007-02-02

A range of phosphine-catalyzed cycloaddition reactions of allenic ketones have been studied, extending the scope of these processes from the more widely used 2,3-butadienoates to allow access to a number of synthetically useful products. Reaction of allenyl methyl ketone 4 with exo-enones afforded spirocyclic compounds in good regioselectivity and promising enantioselectivity via a [2 + 3] cycloaddtion. Aromatic allenyl ketones undergo a phosphine-promoted dimerization to afford functionalized pyrans, leading to a formal [2 + 4] Diels-Alder product, but did not react in the [2 + 3] cycloaddition. The results from other reactions that had found utility with 2,3-butadienoates are also reported.

Multielectron donors based on TTF-phosphine and ferrocene-phosphine hybrid complexes of a hexarhenium(III) octahedral cluster core.

PubMed

Perruchas, Sandrine; Avarvari, Narcis; Rondeau, David; Levillain, Eric; Batail, Patrick

2005-05-16

Electroactive molecular materials precursors are obtained through coordination chemistry of the hexarhenium cluster core [Re(6)Se(8)](2+) on the six available apical positions with redox-active phosphines bearing tetrathiafulvalene- or ferrocene-based moieties. Single-crystal X-ray diffraction study and electrospray mass spectrometry ascertain the synthesis of these hexasubstituted electroactive clusters, containing up to 12 redox active sites. Cyclic voltammetry experiments demonstrate that these compounds can be reversibly oxidized at rather low potentials, thus allowing an easy access to the corresponding radical species which should provide new conducting and/or magnetic molecular materials.

Amino acid sequences of peptides from a chymotryptic digest of a urea-soluble protein fraction (U.S.3) from oxidized wool

PubMed Central

Corfield, M. C.; Fletcher, J. C.

1969-01-01

1. A chymotryptic digest of the protein fraction U.S.3. from oxidized wool was separated into 51 peptide fractions by chromatography on a column of cation-exchange resin. 2. The less acidic fractions were separated into their component peptides by a combination of cation-exchange-resin chromatography, paper chromatography and paper electrophoresis. 3. The amino acid sequences of 34 of these peptides were elucidated, and those of 14 others partially determined. 4. Overlaps between the tryptic and chymotryptic peptides from fraction U.S.3 have enabled ten extended amino acid sequences to be deduced, the longest containing 20 amino acid residues. 5. The relevance of the results to the structures of the helical and non-helical regions of wool is discussed. PMID:5395876

Phosphazene additives

DOEpatents

Harrup, Mason K; Rollins, Harry W

2013-11-26

An additive comprising a phosphazene compound that has at least two reactive functional groups and at least one capping functional group bonded to phosphorus atoms of the phosphazene compound. One of the at least two reactive functional groups is configured to react with cellulose and the other of the at least two reactive functional groups is configured to react with a resin, such as an amine resin of a polycarboxylic acid resin. The at least one capping functional group is selected from the group consisting of a short chain ether group, an alkoxy group, or an aryloxy group. Also disclosed are an additive-resin admixture, a method of treating a wood product, and a wood product.

Analysis of potential hazards associated with 241Am loaded resins from nitrate media

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schulte, Louis D.; Rubin, Jim; Fife, Keith William

2016-02-19

LANL has been contacted to provide possible assistance in safe disposition of a number of 241Am-bearing materials associated with local industrial operations. Among the materials are ion exchange resins which have been in contact with 241Am and nitric acid, and which might have potential for exothermic reaction. The purpose of this paper is to analyze and define the resin forms and quantities to the extent possible from available data to allow better bounding of the potential reactivity hazard of the resin materials. An additional purpose is to recommend handling procedures to minimize the probability of an uncontrolled exothermic reaction.

Selected resin acids in effluent and receiving waters derived from a bleached and unbleached kraft pulp and paper mill

USGS Publications Warehouse

Quinn, B.P.; Booth, M.M.; Delfino, J.J.; Holm, S.E.; Gross, T.S.

2003-01-01

Water samples were collected on three dates at 24 sites influenced by effluent from Georgia-Pacific's Palatka Pulp and Paper Mill Operation, a bleached and unbleached kraft mill near Palatka, Florida, USA. The sampling sites were located within the mill retention ponds, Rice Creek, and the St. John's River. Samples were analyzed by gas chromatography-mass spectrometry for abietic, dehydroabietic, and isopimaric acids, all of which are potentially toxic by-products of pulp production. Isopimaric acid concentrations greater than 12 mg/L were measured at the mill's effluent outfall but were less than 20 ??g/L at the end of Rice Creek. This result indicates that the waters of Rice Creek provide dilution or conditions conducive for degradation or sorption of these compounds. Large differences in resin acid concentrations were observed between sampling events. In two sampling events, the maximum observed concentrations were less than 2 mg/L for each analyte. In a third sampling event, all of the compounds were detected at concentrations greater than 10 mg/L. Data from the three sample dates showed that resin acid concentrations were below 20 ??g/L before the confluence of Rice Creek and the St. John's River in all cases.

Gene disruption technologies have the potential to transform stored product insect pest control

USDA-ARS?s Scientific Manuscript database

Stored product insects feed on grains and processed commodities manufactured from grain post-harvest, reducing the nutritional value and contaminating food. Currently, the main defense against stored product insect pests is the pesticide fumigant phosphine. Phosphine is highly toxic to all animals, ...

Hydroxymethyl phosphine compounds for use as diagnostic and therapeutic pharmaceuticals and method of making same

DOEpatents

Katti, Kattesh V.; Karra, Srinivasa Rao; Berning, Douglas E.; Smith, C. Jeffrey; Volkert, Wynn A.; Ketring, Alan R.

1999-01-01

A compound and method of making a compound for use as a diagnostic or therapeutic pharmaceutical comprises at least one functionalized hydroxyalkyl phosphine donor group and one or more sulfur or nitrogen donor and a metal combined with the ligand.

Hydroxymethyl phosphine compounds for use as diagnostic and therapeutic pharmaceuticals and method of making same

DOEpatents

Katti, Kattesh V.; Karra, Srinivasa Rao; Berning, Douglas E.; Smith, C. Jeffrey; Volkert, Wynn A.; Ketring, Alan R.

2000-01-01

A compound and method of making a compound for use as a diagnostic or therapeutic pharmaceutical comprises at least one functionalized hydroxyalkyl phosphine donor group and one or more sulfur or nitrogen donor and a metal combined with the ligand.

LOW TEMPERATURE PHOSPHINE FUMIGATION FOR POSTHARVEST PEST CONTROL ON FRESH VEGETABLES

USDA-ARS?s Scientific Manuscript database

U.S. exported lettuce, broccoli, asparagus, and strawberries often harbor western flower thrips (Frankliniella occidentalis), a quarantined pest in Taiwan, and therefore require quarantine treatment. Fumigation with pure phosphine at a low temperature of 2°C was studied to control western flower t...

Development of critical molecular weight-property specifications for high performance polymers used as adhesives and composites

NASA Technical Reports Server (NTRS)

Kranbuehl, D. E.

1982-01-01

The polyimide resin, LARC-160, was prepared from diethyl-3, 3', 4,4'-benzophenone tetracarboxylate, ethyl-5-norbornene-2,3-dicarboxylate and Jeffamine AP-22. The imidization reactions of NE and BTDE were studied by HPLC, C-13-NMR and IR. NE imidizes slowly at 12 C; BTDE imidizes when the resin is heated above 100 C. Both imidization reactions proceed directly to the imide. Neither amic acid is present in significant quantities at any stage of the imidization reactions. The monomer mixture was stored at 12 C for periods up to 14 months. The effects of resin aging at this temperature on the chemical composition of the resin monomer mixture and the imidized polymer formed on curing were investigated. Aging the resin monomer mixture has the effect of partially advancing the imidization reaction. The average size of the cured polymer increases slightly with resin age.

Chemical affinities between the solvent extractable and the bulk organic matter of fossil resin associated with an extinct podocarpaceae

USGS Publications Warehouse

Grimalt, J.O.; Simoneit, B.R.T.; Hatcher, P.G.

1989-01-01

Analyses by GC-MS and GC-IR of resin associated to Dacridiumites mawsonii deposits, an extinct species of Podocarpaceae occurring on the South Island of New Zealand during the Bortonian (Middle Eocene), have revealed that dehydroabietic acid is the predominant component of the solvent soluble fraction. Accordingly, this diterpenoid has been selected as the principal component material for spectroscopic comparison with the bulk resin using IR and CP/MAS 13C NMR. ?? 1989.

40 CFR Appendix B to Subpart Nnn... - Free Formaldehyde Analysis of Insulation Resins by Hydroxylamine Hydrochloride

Code of Federal Regulations, 2011 CFR

2011-07-01

... 4.0 with pH 4.0 buffer and pH 7 with pH 7.0 buffer. 3.350-mL burette for 1.0 N sodium hydroxide. 3... hydrochloride solution, 100 grams per liter, pH adjusted to 4.00. 4.3Hydrochloric acid solution, 1.0 N and 0.1 N... magnetic stirrer. Confirm that the resin has dissolved. 5.4Adjust the resin/solvent solution to pH 4.0...

40 CFR Appendix B to Subpart Nnn... - Free Formaldehyde Analysis of Insulation Resins by Hydroxylamine Hydrochloride

Code of Federal Regulations, 2010 CFR

2010-07-01

... 4.0 with pH 4.0 buffer and pH 7 with pH 7.0 buffer. 3.350-mL burette for 1.0 N sodium hydroxide. 3... hydrochloride solution, 100 grams per liter, pH adjusted to 4.00. 4.3Hydrochloric acid solution, 1.0 N and 0.1 N... magnetic stirrer. Confirm that the resin has dissolved. 5.4Adjust the resin/solvent solution to pH 4.0...

CATALYTIC PROMOTION OF THE ADSORPTION OF VANADIUM ON AN ANIONIC EXCHANGE RESIN

DOEpatents

Bailes, R.H.; Ellis, D.A.

1958-08-26

An improvement in the process for the recovery of vanadium from acidic phosphatic solutions is presented. In this process the vanadium is first oxidized to the pentavaleat state, and is then separated by contacting such solutions with an anion exchange resin whereby adsorption of the complexed pentavalent vanadium is effected. The improvement lies in the fact that adsorp tion of the vanadium complex by the anion exchange resin is promoted and improved by providing fiuoride ions in solution to be contacted.

Liver histopathology of fatal phosphine poisoning.

PubMed

Saleki, Sepideh; Ardalan, Farid Azmoudeh; Javidan-Nejad, Abdullah

2007-03-02

Two commonly used pesticides in agriculture are phosphides of aluminium and zinc. Both of these metal phosphides act through elaboration of toxic phosphine gas. The poisoning in Iran is mostly oral and suicidal. Phosphine is rapidly absorbed throughout the gastrointestinal tract after ingestion and it is partly carried to the liver by the portal vein. In this study the liver histopathology of fatal poisoning is scrutinized. A descriptive, retrospective study was performed on 38 fatal phosphine poisonings. The slides of liver specimens of the cases were retrieved and studied separately by two pathologists. The poisoning was suicidal in 33 (86.5%) of cases. Portal inflammation was negligible in 37 cases and only in one of the cases, a moderate degree of chronic inflammation accompanied by granuloma formation was observed. Major histopathologic findings were as follows: mild sinusoidal congestion; 12 cases (31.6%), severe sinusoidal congestion; 25 cases (45.8%), central vein congestion; 23 cases (60.5%), centrilobular necrosis; 3 cases (7.9%), hepatocytes nuclear fragmentation; 6 cases (15.8%), sinusoidal clusters of polymorphonuclear leukocytes; 12 cases (31.6%), and mild macrovesicular steatosis; 5 cases (13.2%). Fine isomorphic cytoplasmic vacuoles were observed in 36 cases (94.7%). These vacuoles were distributed uniformly in all hepatic zones in the majority (75%) of cases. This study reveals that the main histopathologic findings of fatal phosphine poisoning in the liver are fine cytoplasmic vacuolization of hepatocytes and sinusoidal congestion.

Anticancer Agents: Does a Phosphonium Behave Like a Gold(I) Phosphine Complex? Let a "Smart" Probe Answer!

PubMed

Ali, Moussa; Dondaine, Lucile; Adolle, Anais; Sampaio, Carla; Chotard, Florian; Richard, Philippe; Denat, Franck; Bettaieb, Ali; Le Gendre, Pierre; Laurens, Véronique; Goze, Christine; Paul, Catherine; Bodio, Ewen

2015-06-11

Gold phosphine complexes, such as auranofin, have been recognized for decades as antirheumatic agents. Clinical trials are now underway to validate their use in anticancer or anti-HIV treatments. However, their mechanisms of action remain unclear. A challenging question is whether the gold phosphine complex is a prodrug that is administered in an inactive precursor form or rather that the gold atom remains attached to the phosphine ligand during treatment. In this study, we present two novel gold complexes, which we compared to auranofin and to their phosphonium analogue. The chosen ligand is a phosphine-based smart probe, whose strong fluorescence depends on the presence of the gold atom. The in vitro biological action of the gold complexes and the phosphonium derivative were investigated, and a preliminary in vivo study in healthy zebrafish larvae allowed us to evaluate gold complex biodistribution and toxicity. The different analyses carried out showed that these gold complexes were stable and behaved differently from phosphonium and auranofin, both in vitro and in vivo. Two-photon microscopy experiments demonstrated that the cellular targets of these gold complexes are not the same as those of the phosphonium analogue. Moreover, despite similar IC50 values in some cancer cell lines, gold complexes displayed a low toxicity in vivo, in contrast to the phosphonium salt. They are therefore suitable for future in vivo investigations.

Addition of phosphotungstic acid to ethanol for dehydration improves both the ultrastructure and antigenicity of pituitary tissue embedded in LR White acrylic resin.

PubMed

Sakai, Yuko; Hosaka, Masahiro; Hira, Yoshiki; Watanabe, Tsuyoshi

2005-12-01

Although hydrophilic acrylic resins including LR White have been widely utilized as embedding media for immunocytochemical use, the constituents of tissues are often extracted by the resin monomer during the infiltration process of the embedment, resulting in a discernible impairment of the ultrastructure when the tissue is weakly fixed only with aldehydes. To minimize the extraction by the resin monomer, the embedding procedure with LR White resin was reexamined in the present study. Among the treatments tested, a partial dehydration with 70% ethanol containing 2% phosphotungstic acid (PTA) well preserved the ultrastructure of the pituitary tissue without spoiling the antigenicity of LHbeta and other representative markers for the Golgi apparatus. In addition, treatment with 1% tannic acid (TA) prior to the dehydration described above synergistically improved both the ultrastructure and antigenicity of the tissue so that the orientation of the Golgi apparatus could be determined by double immunogold labeling with commercially available anti-GM130 and anti-TGN38 antibodies. The ultrathin sections from the LR White-embedded tissue treated with TA and dehydrated in 70% ethanol containing 2% PTA also enhanced contrast without conventional heavy-metal staining with uranyl acetate and lead citrate. Our findings further suggest that the precipitation of TA and PTA protected the tissue from being extracted during the embedment, probably because an insoluble complex was transiently formed with the constituents of the tissue. This simple modification of the LR White embedment can extend the application of post-embedding immunocytochemistry as an alternative to pre-embedding immunolabeling with frozen ultrathin sections.

Shear bond strength of a new self-adhering flowable composite resin for lithium disilicate-reinforced CAD/CAM ceramic material

PubMed Central

Sancakli, Hande Sar; Sancakli, Erkan; Eren, Meltem Mert; Ozel, Sevda; Yucel, Taner; Yildiz, Esra

2014-01-01

PURPOSE The purpose of this study was to evaluate and compare the effects of different surface pretreatment techniques on the surface roughness and shear bond strength of a new self-adhering flowable composite resin for use with lithium disilicate-reinforced CAD/CAM ceramic material. MATERIALS AND METHODS A total of one hundred thirty lithium disilicate CAD/CAM ceramic plates with dimensions of 6 mm × 4 mm and 3 mm thick were prepared. Specimens were then assigned into five groups (n=26) as follows: untreated control, coating with 30 µm silica oxide particles (Cojet™ Sand), 9.6% hydrofluoric acid etching, Er:YAG laser irradiation, and grinding with a high-speed fine diamond bur. A self-adhering flowable composite resin (Vertise Flow) was applied onto the pre-treated ceramic plates using the Ultradent shear bond Teflon mold system. Surface roughness was measured by atomic force microscopy. Shear bond strength test were performed using a universal testing machine at a crosshead speed of 1 mm/min. Surface roughness data were analyzed by one-way ANOVA and the Tukey HSD tests. Shear bond strength test values were analyzed by Kruskal-Wallis and Mann-Whitney U tests at α=.05. RESULTS Hydrofluoric acid etching and grinding with high-speed fine diamond bur produced significantly higher surface roughness than the other pretreatment groups (P<.05). Hydrofluoric acid etching and silica coating yielded the highest shear bond strength values (P<.001). CONCLUSION Self-adhering flowable composite resin used as repair composite resin exhibited very low bond strength irrespective of the surface pretreatments used. PMID:25551002

BisGMA/TEGDMA dental nanocomposites containing glyoxylic acid modified high-aspect ratio hydroxyapatite nanofibers with enhanced dispersion

PubMed Central

Chen, Liang; Xu, Changqi; Wang, Yong; Shi, Jian; Yu, Qingsong

2012-01-01

The purpose of this research was to investigate the influence of the glyoxylic acid (GA) modification of hydroxyapatite (HAP) nanofibers on their dispersion in bisphenol A glycidyl methacrylate (BisGMA)/triethylene glycol dimethacrylate (TEGDMA) dental composites and also investigate the mechanical properties, water absorption, and water solubility of the resulting dental resins and composites. Scanning/Transmission electron microscopy (STEM) images showed that microsized HAP nanofiber bundles could be effectively broken down to individual HAP nanofibers with an average length of ~15 μm after the surface modification process. Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and thermal gravimetric analysis (TGA) characterization confirmed glyoxylic acid was chemically grafted on the HAP nanofiber surface, hypothetically by reacting with the amine group on HAP nanofiber surface. The enhanced dispersion of HAP nanofibers in dental matrix led to increased biaxial flexural strength (BFS) compared with the corresponding dental resins and composites filled with untreated HAP nanofibers. In addition, impregnation of small mass fractions of the glyoxylic acid modified HAP nanofibers into the BisGMA/TEGDMA dental resins (5wt%, 10wt%) or composites (2wt%, 3wt%) could also substantially improve the BFS in comparison with the controls(pure resins or dental composites filled with silica particles alone). Larger mass fractions could not further increase the mechanical property or even degrade the BFS values. Water behavior testing results indicated that the addition of glyoxylic acid modified HAP nanofibers resulted in higher water absorption and water solubility values which is not preferred for clinical application. In summary, well dispersed HAP nanofibers and their dental composites with enhanced mechanical property have been successfully fabricated but the water absorption and water solubility of such dental composites need to be further improved. PMID:22689264

Antimicrobial activities of amphiphilic peptides covalently bonded to a water-insoluble resin.

PubMed Central

Haynie, S L; Crum, G A; Doele, B A

1995-01-01

A series of polymer-bound antimicrobial peptides was prepared, and the peptides were tested for their antimicrobial activities. The immobilized peptides were prepared by a strategy that used solid-phase peptide synthesis that linked the carboxy-terminal amino acid with an ethylenediamine-modified polyamide resin (PepsynK). The acid-stable, permanent amide bond between the support and the nascent peptide renders the peptide resistant to cleavage from the support during the final acid-catalyzed deprotection step in the synthesis. Select immobilized peptides containing amino acid sequences that ranged from the naturally occurring magainin to simpler synthetic sequences with idealized secondary structures were excellent antimicrobial agents against several organisms. The immobilized peptides typically reduced the number of viable cells by > or = 5 log units. We show that the reduction in cell numbers cannot be explained by the action of a soluble component. We observed no leached or hydrolyzed peptide from the resin, nor did we observe any antimicrobial activity in soluble extracts from the immobilized peptide. The immobilized peptides were washed and reused for repeated microbial contact and killing. These results suggest that the surface actions by magainins and structurally related antimicrobial peptides are sufficient for their lethal activities. PMID:7726486

BARIUM RECOVERY PROCESS

DOEpatents

Blanco, R.E.

1959-07-21

A method of separating barium from nuclear fission products is described. In accordance with the invention, barium may be recovered from an acidic solution of neutron-irradiated fissionable material by carrying ihe barium cut of solution as a sulfate with lead as a carrier and then dissolving the barium-containing precipitate in an aqueous solution of an aliphatic diamine chelating reagent. The barium values together with certain other metallic values present in the diamine solution are then absorbed onto a cation exchange resin and the barium is selectively eluted from the resin bed with concentrated nitric acid.

New Stable Cu(I) Catalyst Supported on Weakly Acidic Polyacrylate Resin for Green C-N Coupling: Synthesis of N-(Pyridin-4-yl)benzene Amines and N,N-Bis(pyridine-4-yl)benzene Amines.

PubMed

Kore, Nitin; Pazdera, Pavel

2016-12-22

A method for preparation of a new stable Cu(I) catalyst supported on weakly acidic polyacrylate resin without additional stabilizing ligands is described. A simple and efficient methodology for Ullmann Cu(I) catalyzed C-N cross coupling reactions using this original catalyst is reported. Coupling reactions of 4-chloropyridinium chloride with anilines containing electron donating (EDG) or electron withdrawing (EWG) groups, naphthalen-2-amine and piperazine, respectively, are successfully demonstrated.

Experiments on Anion Exchange with Amberlite Ir-120 Resin; ENSAYOS DE INTERCAMBIO ANIONICO CON RESINA AMBERLITA Ir-120

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cellini, R.F.; Palomino, J.V.

1956-01-01

The ion exchange of the uranyl ion on Amberlite Ir-120 resin was studied with different uranyl ion concentrations. Elution with sulfuric acid was investlgated and the elution curve for the experimental conditions was determined. From the concentrations of the ions of Cu/sup 2+/, Ni/sup 2+/, Fe/sup 3+/, Cd/sup 2+/, Mn/sup 2+/, and Cr/sup 3+/ the maximum exchange capacity was tested and elation curves with 4 N sulfuric acid were obtained. (tr-auth)

Process for the preparation of lactic acid and glyceric acid

DOEpatents

Jackson, James E [Haslett, MI; Miller, Dennis J [Okemos, MI; Marincean, Simona [Dewitt, MI

2008-12-02

Hexose and pentose monosaccharides are degraded to lactic acid and glyceric acid in an aqueous solution in the presence of an excess of a strongly anionic exchange resin, such as AMBERLITE IRN78 and AMBERLITE IRA400. The glyceric acid and lactic acid can be separated from the aqueous solution. Lactic acid and glyceric acid are staple articles of commerce.

The Resin-in-pulp Process and Its Application to Ores from Brosses "BRS 10"; LE PROCEDE "RESIN IN PULP" ET SON APPLICATION AUX MINERAIS DES BROSSES "BRS 10"

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kremer, M.

1959-03-01

The resin-in-pulp process is a technical variant of the recovery process of uranium in dilute solution by means of ion exchange resins. An anion resin, XE 123, of a welldefined grain size is placed in direct contact with the pulp produced by sulfuric acid attack on ore with a low uranium content. This process is of particular value in the treatment of pulps that cannot be filtered or decanted, such as those obtained with ore from Brosses. The preparation of the pulp, the elution of the uranium, and its fixation, as well as the various factors encountered in these operations,more » are discussed. (auth)« less

Separation and recovery of food coloring dyes using aqueous biphasic extraction chromatographic resins.

PubMed

Huddleston, J G; Willauer, H D; Boaz, K R; Rogers, R D

1998-06-26

Aqueous biphasic systems (ABS) and aqueous biphasic extraction chromatographic (ABEC) resins are currently under investigation for their utility in the removal of color from textile plant wastes. The structures of several widely used food colorings, suggest that these dyes would also be retained on the resins. In work currently in progress, we have begun to investigate the retention and resolution of several common food colorings including indigo carmine, amaranth, carminic acid. erythrosin B, tartrazine and quinoline yellow. The relationship between the uptake of these dyes on ABEC resins in terms of the binding strengths and capacities of the resins and their partitioning behavior in ABS is illustrated. Some possible theoretical and practical approaches to the prediction of the partitioning and retention behavior is discussed.

Separation of Be and Al for AMS using single-step column chromatography

NASA Astrophysics Data System (ADS)

Binnie, Steven A.; Dunai, Tibor J.; Voronina, Elena; Goral, Tomasz; Heinze, Stefan; Dewald, Alfred

2015-10-01

With the aim of simplifying AMS target preparation procedures for TCN measurements we tested a new extraction chromatography approach which couples an anion exchange resin (WBEC) to a chelating resin (Beryllium resin) to separate Be and Al from dissolved quartz samples. Results show that WBEC-Beryllium resin stacks can be used to provide high purity Be and Al separations using a combination of hydrochloric/oxalic and nitric acid elutions. 10Be and 26Al concentrations from quartz samples prepared using more standard procedures are compared with results from replicate samples prepared using the coupled WBEC-Beryllium resin approach and show good agreement. The new column procedure is performed in a single step, reducing sample preparation times relative to more traditional methods of TCN target production.

Conjugate and method for forming aminomethyl phosphorus conjugates

DOEpatents

Katti, Kattesh V.; Berning, Douglas E.; Volkert, Wynn A.; Ketring, Alan R.; Churchill, Robert

1999-01-01

A method of forming phosphine-amine conjugates includes reacting a hydroxymethyl phosphine group of an amine-free first molecule with at least one free amine group of a second molecule to covalently bond the first molecule with the second molecule through an aminomethyl phosphorus linkage and the conjugates formed thereby.

Hydroxymethyl phosphine compounds for use as diagnostic and therapeutic pharmaceuticals and method of making same

DOEpatents

Katti, K.V.; Karra, S.R.; Berning, D.E.; Smith, C.J.; Volkert, W.A.; Ketring, A.R.

1999-01-05

A compound and method of making a compound for use as a diagnostic or therapeutic pharmaceutical comprises at least one functionalized hydroxyalkyl phosphine donor group and one or more sulfur or nitrogen donor and a metal combined with the ligand. 21 figs.