An acid method for the volumetric estimation of water-soluble dithiocarbamates

Dithiocarbamates have been estimated previously by reaction with a strong acid, the carbon disulfide evolved being converted into a xanthate and the latter estimated iodimetrically. In the present method, a water-soluble dithiocarbamate is reacted with a decinormal mineral acid and the excess acid is determined to compute the amount of dithiocarbamate present. This method is applicable for the determination of a dithiocarbamate in a mixture containing thiuram disulfide.

Molecular Complexes of Alprazolam with Carboxylic Acids, Boric Acid, Boronic Acids, and Phenols. Evaluation of Supramolecular Heterosynthons Mediated by a Triazole Ring

A series of molecular complexes, both co-crystals and salts, of a triazole drug-alprazolam-with carboxylic acids, boric acid, boronic acids, and phenols have been analyzed with respect to heterosynthons present in the crystal structures. In all cases, the triazole ring behaves as an efficient hydrogen bond acceptor with the acidic coformers. The hydrogen bond patterns exhibited with aromatic carboxylic acids were found to depend on the nature and position of the substituents. Being a strong acid, 2,6-dihydroxybenzoic acid forms a salt with alprazolam. With aliphatic dicarboxylic acids alprazolam forms hydrates and the water molecules play a central role in synthon formation and crystal packing. The triazole ring makes two distinct heterosynthons in the molecular complex with boric acid. Boronic acids and phenols form consistent hydrogen bond patterns, and these are seemingly independent of the substitutional effects. Boronic acids form noncentrosymmetric cyclic synthons, while phenols form O-H center dot center dot center dot N hydrogen bonds with the triazole ring. (C) 2010 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 99:3743-3753, 2010.

Recuperação de cobre de rejeitos de galvanoplastia utilizando resinas de troca iônica

Neste estudo, a sorção e recuperação de íons metálicos de resíduos sólidos industriais provenientes de uma indústria de galvanoplastia situada no Rio de Janeiro (Brasil) foram investigadas através da utilização de duas resinas comerciais de troca iônica: Lewatit VPOC 1800 (fortemente ácida, tipo gel) e Lewatit VPOC 1960 (fortemente básica, tipo gel), produzidas pela Lanxess-Bayer Chemicals. As características físico-quimicas das resinas e do lodo galvânico foram determinadas. Os estudos de sorção das resinas foram conduzidos em batelada e em coluna. Baseado nesses estudos, os parâmetros de sorção e das curvas de ruptura foram determinados. Os estudos de equilíbrio e cinética de sorção também foram realizados. O resíduo de galvanoplastia era composto pelos metais: Cu2+, Fe3+, Al3+, Ni2+ e Cr3+. A capacidade de sorção qe das resinas Lewatit VPOC 1800 variou entre 0,1-1,9 mg g-1 para Cu2+, 0,01-0,6 mg g-1 para Fe3+ e 0,2-0,4 mg g-1 para Al3+. Enquanto que para a resina Lewatit VPOC 1960, os valores de qe variou entre 0,01-0,4 mg g-1 para Cu2+ e 0,01 0,2 mg g-1 para Fe3+ dependendo da concentração do metal e do tempo de contato. A capacidade de sorção para a resina Lewatit VPOC 1960 foi restrita para íons Cu2+ e Fe3+ os quais formam complexos aniônicos com íons Cl-. O modelo de Freundlich foi o mais adequado para descrever o equilíbrio de troca iônica de ambas as resinas. Já em relação ao mecanismo de sorção, o modelo pseudo-segunda ordem tipo 1 foi o mais aplicável. O ponto de ruptura das resinas Lewatit VPOC 1800 e Lewatit VPOC 1960 em relação aos íons Cu2+ocorreu quando passou através da coluna, 1860 cm3 e 2220 cm3 de solução de resíduo sólido respectivamente (20 g de resina, 100 mg L-1 de íons Cu2+, vazão de 60 cm3 min-1). Os íons metálicos Cu2+, Fe3+, Al3+, foram dessorvidos em alta proporção da resina Lewatit VPOC 1800 passando pela coluna solução aquosa de H2SO4 2,4 mol L-1. Já os metais Cu2+ e Fe3+ foram eluídos da resina Lewatit VPOC 1960 com solução aquosa de HCl 2,0 mol L-1. A recuperação seletiva de Cu2+ não foi alcançada porque Cu2+ e Fe3+ precipitam na mesma faixa de pH

Hydrodynamics in an expanded bed of large size ion-exchange resin, and natural product adsorption

Successful applications of expanded bed adsorption (EBA) technology have been widely reported in the literature for protein purification. Little has been reported on the recovery of natural products and active components of Chinese herbal preparations using EBA technology. In this study, the hydrodynamic behavior in an expanded bed of cation resin, 001 x 7 Styrene-DVB, was investigated. Ephedrine hydrochloride (EH) was used as a model natural product to test the dynamic binding capacity (DBC) in the expanded bed. EBA of EH directly from a feedstock containing powdered herbs has also been investigated. These particles are different from commercially available expanded bed adsorbents by virtue of their large size (20S to 1030 gm). When the adsorbent bed is expanded to approximately 1.3 to 1.5 times its settled bed height, the axial liquid-phase dispersion coefficient was found to be of the order 10(-5) m(2) s(-1), which falls into the range 1.0 x 10(-6) to 1.0 X 10(-5) m(2) s(-1) observed previously in protein purification. Because of the favorable column efficiency (low axial dispersion coefficient), the recovery yield and purification factor values of EH directly from a feedstock reached 86.5% and 18, respectively. The results suggest that EBA technology holds promise for the recovery of natural products and active components of Chinese herbal preparations.

Effect of acid strength distribution on conversion of FCC gasoline over a ZSM-5 zeolite catalyst

Acid strength distribution and the distribution of aromatics formed in the FCC gasoline conversion reaction on a ZSM-5 zeolite with different Na contents have been studied. With increasing Na content in the ZSM-5 zeolite, the acid sites determined by NH3-TPD technique, especially the strong acid sites, clearly decrease. When used as catalyst for the aromatization reaction, the transformation of olefins in the FCC gasoline into aromatics is governed directly by the strong acid sites on the ZSM-5 catalyst. Only under the conditions that a ZSM-5 catalyst possesses suitable strong acid sites is reaction temperature favorable for the aromatics formed.

The role of acid strength of zeolites in liquid-phase alkylation of benzene with ethylene

The role of acid strength of zeolites in liquid-phase alkylation of benzene with ethylene was studied over beta, MCM-22, and USY zeolites by means of adsorbing NH3 at different temperatures. The strong acid sites are active centers, while the weak acid sites are inactive. The selectivity behavior of the strong acid sites varies with the relative acid strength as well as the types of the zeolites.

Highly sensitive electrogenerated chemiluminescence produced at Ru(bpy)(3)(2+) in Eastman-AQ55D-carbon nanotube composite film electrode

The electrochemistry and electrogenerated chemilurninescence (ECL) of tris(2,2-bipyridyl)ruthenium(II) ion-exchanged in Eastman-AQ-carbon nanotube (CNT) composite films were investigated at a glassy carbon (GC) electrode. Eastman-AQ55D is a poly (ester sulfonic acid) cation exchanger available in a commercial dissolved form. It is much more hydrophilic than Nafion due to its unique structure, so Ru(bpy)(3)(2+) does not diffuse into the hydrophobic region where it may lose its electroactivity as that in Nafion. The interfused CNT could act as electronic wires that connect the electrode with Ru(bpy)(3)(2+), which made the composite film much more electronically which finally led to the increasing of Ru(bpy)(3)(2+) conductive. Besides, the negatively charged CNT could also absorb some Ru(bpy)(3)(2+). Moreover, the strong electrostatic interaction between AQ and Ru(bpy)(3)(2+) made the composite films much more stable. The combination of AQ and CNT brings excellent sensitivity with the detection limit as low as 3 x 10(-11) M for TPA.

Effect of variations in acid properties of HZSM-5 on the coking behavior and reaction stability in butene aromatization

In order to investigate the effect of acid properties on the coke behavior and stability of butene aromatization, we prepared the AHZSM-5 samples with various acid properties by the methods of hydrothernial treatment and K addition. The reaction of butene aromatization was carried out at 350 degrees C and 0.5 MPa in a continuous flow fixed bed. The characterization of the fresh/coked catalysts with NH3-TPD, N-2 adsorption-desorption measurement, and TG techniques has shown that a large amount of acid sites (high acid density) of the AHZMS-5 catalyst can cause a large quantity of coke deposit and serious channel blockage, and so result in a rapid loss of aromatization activity. On the contrary, after a great reduction in strong acid sites of AHZSM-5 catalyst resulting from some K-modification, the presence of only many weak acid sites also could not lessen the formation of coke nor improve the reaction stability of butene aromatization. Interestingly, the simultaneous reduction in the strong and weak acid sites to a desirable level by hydrothermal treating the AHZSM-5 catalyst at a proper temperature can effectively suppress the coke formation and channel blockage, and thus improve its olefin aromatization stability. (c) 2005 Elsevier B.V. All rights reserved.

A comparative study of chitin synthase activity in two Mortierella species

An in vitro investigation of some important factors controlling the activity of chitin synthase in cell-free extracts of two Mortierella species has been carried out. Mixed membrane fractions from mycelial homogenates of Mortierella candelabrum and Mortierella pusilla were found to catalyse the transfer of N-acetylglucosamine from UDP-N-acetylglucosamine into an insoluble product characterized as chitin by its insolubility in weak acid and alkali, and the release of glucosamine and diacetylchitobiose on hydrolysis with a strong acid and chitinase, respectively. Apparent Km values for UDP-GlcNAc were 1.8 mM and 2.0 mM for M. pusilla and ~ candelabrum, respectively. Polyoxin D was found to be a very potent competitive inhibitor with values of the constant of inhibition, Ki' for both species about three orders of magnitude lower than theKm for UDP-GlcNAc. A divalent cation, Mg+2 , Mn+2 or Co+2 , was required for activity. N-acetylglucosamine, the monomer of chitin, stimulated the activity of the enzyme. The crude enzyme preparation of ~ candelabrum, unlike that of ~ pusilla, showed an absolute requirement for both Mg+2 and N-acetylglucosamine. Large differences in response to exogenous proteases were noted in the ratio of active to inactive chitin synthase of the two species. A fifteen fold or greater increase was obtained after treatment with acid protease (from Aspergillussaitoi) as compared to a two- to four-fold activation of the M. pusilla membrane preparation treated similarly. During storage at 4°C over 48 hours, an endogenous activation of chitin synthase of ~ pus ilIa was achieved, comparable to that obtained by exogenous protease treatment. The high speed supernatant of both species inhibited the chitin synthase activity of the mixed membrane fractions. The inhibitor of ~ pus ilIa was effective against the pre-activated enzyme whereas that of M. candelabrum inhibited the activated enzyme. Several possibilities are discussed as to the role of the different factors regulating the enzyme activity. The suggestion is made from the properties of chitin synthase in the two species that in vivo a delicate balance exists between the activation and inactivation of the enzyme which is responsible for the pattern of wall growth of each fungus.

Extraction of copper(II) ions from aqueous solutions with a methimazole-based ionic liquid

The recently synthesized ionic liquid (IL) 2-butylthiolonium bis(trifluoromethanesulfonyl)amide, [mimSBu][NTf2], has been used for the extraction of copper(II) from aqueous solution. The pH of the aqueous phase decreases upon addition of [mimSBu]+, which is attributed to partial release of the hydrogen attached to the N(3) nitrogen atom of the imidazolium ring. The presence of sparingly soluble water in [mimSBu][NTf2] also is required in solvent extraction studies to promote the incorporation of Cu(II) into the [mimSBu][NTf2] ionic liquid phase. The labile copper(II) system formed by interacting with both the water and the IL cation component has been characterized by cyclic voltammetry as well as UV−vis, Raman, and 1H, 13C, and 15N NMR spectroscopies. The extraction process does not require the addition of a complexing agent or pH control of the aqueous phase. [mimSBu][NTf2] can be recovered from the labile copper−water−IL interacting system by washing with a strong acid. High selectivity of copper(II) extraction is achieved relative to that of other divalent cobalt(II), iron(II), and nickel(II) transition-metal cations. The course of microextraction of Cu2+ from aqueous media into the [mimSBu][NTf2] IL phase was monitored in situ by cyclic voltammetry using a well-defined process in which specific interaction with copper is believed to switch from the ionic liquid cation component, [mimSBu], to the [NTf2] anion during the course of electrochemical reduction from Cu(II) to Cu(I). The microextraction−voltammetry technique provides a fast and convenient method to determine whether an IL is able to extract electroactive metal ions from an aqueous solution.

THE EFFECT of DENTIN PRETREATMENT on THE MICROTENSILE BOND STRENGTH of SELF-ADHESIVE RESIN CEMENTS

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Bonding Efficacy of New Self-etching, Self-adhesive Dual-curing Resin Cements to Dental Enamel

Purpose: 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.Materials and Methods: 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-mm(2) 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 degrees C, the blocks were sectioned for obtaining microbar specimens with an adhesive area of 1 mm(2) (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 Tu key's test.Results: 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).Conclusion: 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.

Effect of surface conditioning methods on the microtensile bond strength of resin composite to composite after aging conditions

Objectives. This study evaluated the effect of two different surface conditioning methods on the repair bond strength of a bis-GMA-adduct/bis-EMA/TEGDMA based resin composite after three aging conditions.Methods. Thirty-six composite resin blocks (Esthet X, Dentsply) were prepared (5 mm x 6 mm x 6 mm) and randomly assigned into three groups for aging process: (a) immersion in citric acid (pH 3.0 at 37 degrees C, 1 week) (CA); (b) boiling in water for 8h (BW) and (c) thermocycling (x5000, 5-55 degrees C, dwell time: 30s) (TC). After aging, the blocks were assigned to one of the following surface conditioning methods: (1) silica coating (30 mu m SiOx) (CoJet, 3M ESPE) + silane (ESPE-Sil) (CJ), (2) phosphoric acid + adhesive resin (Single Bond, 3M ESPE) (PA). Resin composite (Esthet.X (R)) was bonded to the conditioned substrates incrementally and light polymerized. The experimental groups formed were as follows: Gr1:CA + PA; Gr2:CA + CJ Gr3:BW + PA; Gr4: BW + CJ; Gr5:TC + PA; Gr6: TC + CJ. The specimens were sectioned in two axes (x and y) with a diamond disc under coolant irrigation in order to obtain non-trimmed bar specimens (sticks, 10 mm x 1 mm x 1 mm) with 1 mm(2) of bonding area. The microtensile test was accomplished in a universal testing machine (crosshead speed: 0.5 mm min(-1)).Results. The means and standard deviations of bond strength (MPa +/- S.D.) per group were as follows: Gr1: 25.5 +/- 10.3; Gr2: 46.3 +/- 10.1; Gr3: 21.7 +/- 7.1; Gr4: 52.3 +/- 15.1; GrS: 16.1 +/- 5.1; Gr6, 49.6 +/- 13.5. The silica coated groups showed significantly higher mean bond values after all three aging conditions (p < 0.0001) (two-way ANOVA and Tukey tests, alpha = 0.05). The interaction effect revealed significant influence of TC aging on both silica coated and acid etched groups compared to the other aging methods (p < 0.032). Citric acid was the least aggressive aging medium.Significance. Chairside silica coating and silanization provided higher resin-resin bond strength values compared to acid etching with phosphoric acid followed by adhesive resin applications. Thermocycling the composite substrates resulted in the lowest repair bond strength compared to citric acid challenge or boiling in water. (C) 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of curing regime on the cytotoxicity of resin-modified glass-ionomer lining cements applied to an odontoblast-cell line

Objective: The aim of this in vitro study was to evaluate the cytotoxicity of resin-modified glass-ionomer lining cements submitted to different curing regimes and applied to an immortalized odontoblast-cell line (MDPC-23). Methods: Forty round-shaped specimens of each experimental material (Fuji Lining LC and Vitrebond) were prepared. They were light-cured for the manufacturers' recommended time (MRT = 30 s), under-cured (0.5 MRT = 15 s), over-cured (1.5 MRT = 45 s) or allowed to dark cure (0 MRT). Sterilized filter papers soaked with either 5 μL of PBS or HEMA were used as negative and positive control, respectively. After placing the specimens individually in wells of 24-well dishes, odontoblast-like cells MDPC-23 (30,000 cells/cm2) were plated in each well and incubated for 72 h in a humidified incubator at 37 °C with 5% CO2 and 95% air. The cytotoxicity was evaluated by the cell metabolism (MTT assay) and cell morphology (SEM). Results: Fuji Lining LC was less cytotoxic than Vitrebond (p < 0.05) in all the experimental conditions. However, the cytotoxicity of Fuji Lining LC was noticeably increased in the absence of light-curing while the same was not observed for Vitrebond. The length of light-curing (15, 30 or 45 s) did not influence the toxicity of both lining materials when they were applied on the odontoblast-cell line MDPC-23. Significance: The light-activation plays an important role in reducing the cytotoxicity of Fuji Lining LC. Following the manufacturer' recommendation regarding the light-curing regime may prevent toxic effect to the pulp cells. © 2005 Academy of Dental Materials.

Influence of brush type as a carrier of adhesive solutions and paper points as an adhesive-excess remover on the resin bond to root dentin

Purpose: To evaluate the influence of the brush type as a earner of priming adhesive solutions and the use of paper points as a remover of the excess of these solutions on the push-out bond strength of resin cement to bovine root dentin. The null hypotheses were that brush type and the use of paper points do not affect the bond strength. Materials and Methods: The canals of 80 single-root bovine roots (16 mm in length) were prepared at 12 mm using the preparation drill (FRC Postec Plus, Ivoclar). Half of each root was embedded in acrylic resin and the specimens were divided into 8 groups, considering the factors brush type (4 levels) and paper point (2 levels) (n = 10): Gr 1: small microbrush (Cavi-Tip, SDI); Gr 2: Microbrush (Dentsply); Gr 3: Endobrush (Bisco); Gr 4: conventional brush (Bisco); Gr 5: Cavi-Tip (SDI) + paper points; Gr 6: Microbrush (Dentsply) + paper points; Gr 7: Endobrush (Bisco) + paper points; Gr 8: conventional brush (Bisco) + paper points. The root dentin was treated with a multistep total-etch adhesive system (All Bond 2). The adhesive system was applied using each microbrush, with and without using paper points. One fiber post was molded with addition silicon and 80 posts were made of resin cement (Duolink), The resin posts were luted (Duolink resin cement), and the specimens were stored for 24 h in water at 37°C. Each specimen was cut into 4 disk-shaped samples (1.8 mm in thickness), which were submitted to the push-out test. Results: The brush type (p < 0.0001) (small microbrush > microbrush = endobrush = conventional brush) and the use of paper points (p = 0.0001) (with > without) influenced the bond strength significantly (two-way ANOVA). The null hypotheses were rejected. Conclusion: The smallest brush (Cavi-Tip) and the use of paper points significantly improved the resin bond to bovine root dentin.