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Chitosan undergoes radical-induced depolymerization in the presence of potassium persulfate at 60 degrees C, leading to extensive crosslinking of the fragmented chains on subsequent cooling at 4 degrees C. As a result, a possible conformational change leading to higher crystallinity, as evidenced by IR, X-ray and 13C NMR was observed.
Using a catalytic amount of potassium persulfate (1.48 x 10(-4)M), eight different seed gums were fully hydrolyzed on alumina support under microwave irradiation. The hydrolysis time varied between 1.33 and 2.33 min depending upon the seed gum structure. The used solid support could be easily separated from the hydrolyzates and recycled. However, under microwave field in an aqueous medium, the same amount of persulfate was unable to hydrolyze the seed gums. Solid-supported microwave hydrolysis has been compared with the microwave-enhanced aqueous hydrolysis (using K2S2O8 or 0.1N H2SO4) and also with the conventional hydrolysis procedures.
Liquefaction of glucose into oil was examined in hot-compressed water at 300 degrees C and 30 or 60 min in a tumbling batch reactor. The effects of alkali (KHCO(3)), a hydrogenating agent (HCO(2)H), and a cobalt catalyst (Co(3)O(4)) were studied. Also the combinations of these additives were investigated. HCO(2)H and KHCO(3) showed a positive effect on oil formation. Co(3)O(4) was found to be an advantageous additive as well, increasing the oil formation from glucose, but the stability of this catalyst under reaction conditions was quite low.
In the plant, Pistia stratiotes L., the effect of different concentrations of chromium (0, 10, 40, 80 and 160 microM) applied for 48, 96 and 144 h was assessed by measuring changes in the chlorophyll, protein, malondialdehyde (MDA), cysteine, non-protein thiol, ascorbic acid contents and superoxide dismutase (SOD), ascorbate peroxidase (APX) and guiacol peroxidase (GPX) activity of the plants. Both in roots and leaves, an increase in MDA content was observed with increase in metal concentration and exposure periods. In roots, the activity of antioxidant enzymes viz. SOD and APX increased at all the concentrations of Cr at 144 h than their controls. The GPX activity of the treated roots increased with increase in Cr concentration at 48 and 96 h of exposures, however, at 144 h its activity was found declined beyond 10 microM Cr. The level of antioxidants in the roots of the treated plant viz. cysteine and ascorbic acid was also found increased at all the concentrations of Cr at 144 h than their respective controls, however, an increase in the non-protein thiol content was recorded up to 40 microM Cr followed by decrease. The chlorophyll content decreased with increase in Cr concentrations and exposure periods. However, the protein content of both roots and leaves were found decreased with increase in Cr concentrations at all the exposure periods except an increase was recorded at 10 microM Cr at 48 h. In Cr treated plants, the no observed effect concentration (NOEC) and lowest observed effect concentration (LOEC) for leaves chlorophyll and protein contents were 40 and 80 microM Cr, respectively after 48 h exposure while NOEC and LOEC for root protein content were 10 and 40 microM, respectively after 48 h. The analysis of correlation coefficient data revealed that the metal accumulation in the roots of the plant was found positively correlated with antioxidant parameters except SOD after 48 h of exposure, however, negatively correlated with most of all the parameters studied at 144 h in both part of the plant. It may be suggested from the present study that toxic concentrations of Cr cause oxidative damage as evidenced by increased lipid peroxidation and decreased chlorophyll and protein contents. However, the higher levels of enzymatic and non-enzymatic antioxidants suggest the reason for tolerating higher levels of metals.
In this study, we investigate pore scale morphology of nonaqueous phase liquids (NAPLs) trapped in different pore sizes using tracer techniques. Specific interfacial area and saturation of NAPL trapped in homogeneous sands were measured using the interfacial and partitioning tracer techniques. The observed NAPL-water interfacial areas increased in a log-linear fashion with decreasing sand grain size, but showed no clear trend with residual NAPL saturation formed in the various grain sizes. The measured values were used to calculate the NAPL morphology index, which characterizes the spatial NAPL distribution within the pore space. The NAPL morphology indices, increased exponentially with decreasing grain size, indicating that the NAPL becomes smaller, but more blobs. For a fixed grain size, the specific interfacial area and saturation of the NAPL were measured following changes caused by dissolution using alcohol. The observed interfacial areas showed a decrease linearly as a function of the NAPL saturation.
Desorption levels of soil-sorbed selenium (Se) were studied by adding phosphate to 22 typical Japanese agricultural soils. Soil-soil solution distribution coefficients of Se (Kd-Se) were measured using a batch process as an index of Se sorption level, adding 75Se as a tracer. After the Kd measurement, extraction of soil-sorbed 75Se with a 0.1 M or 1 M Na2HPO4 solution followed to determine the amount of 75Se desorbed by the phosphate. When the 0.1 M Na2HPO4 solution was used, 18-70% of soil-sorbed Se was extracted (average: 47%). However, when the 1 M Na2HPO4 solution was used, 27-83% of soil-sorbed Se was extracted (average: 57%). The observed 75Se desorption percentage indicated the maximum Se removability by phosphate addition. The desorption percentage of Se with 1 M Na2HPO4 correlated with Kd-Se values, suggesting that the soil sample with higher Kd-Se contained more reactive components for phosphate-sorption than the soil sample with lower Kd-Se. To evaluate the effect of phosphate concentration on the Se sorption, the Kd-Se was measured for two typical soils under different levels of phosphate (0.1-10 mM PO4). The Kd values were decreased by phosphate addition for both soils. The Kd decrease was observed even for just 1 mM PO4. The phosphate addition with 1 mM PO4 is the same level as in P fertilizer applied to paddy fields in Japan. Therefore, it was suggested that Se desorption should occur in Japanese soils due to the phosphate input.
An acetylation reaction for the derivatisation of the three chlorophenols involved in cork taint was optimised using a Doehlert design for direct application in wine samples. In this first step, the optimum reaction pH, by adding different amounts of KHCO3, and the required quantity of derivatisation reagent were fixed. Then a series of parameters relevant for the headspace solid-phase microextraction process, such as desorption conditions, salt addition and agitation sample were evaluated. A simultaneous study of the type of fibre and extraction temperature was performed at five levels and based on the results obtained the rest of factors (sample volume and exposition time) that could potentially affect the extraction yields were optimised by a central composite design. According to the validation of the method, we propose here, to our knowledge, the first application of solid-phase microextraction for the direct analysis of chlorophenols in red wine samples.
The aim of this work was to optimize an ultrasonic extraction procedure for the determination of polycyclic aromatic hydrocarbons (PAHs) in sediments and to compare it with the reflux procedure using methanolic potassium hydroxide. Sample extracts were purified with a miniaturized silica gel chromatographic column and analyzed by gas chromatography-mass spectrometry (GC-MS). Ultrasonication using n-hexane-acetone (1:1, v/v) solvent mixture on dried homogenized marine sediment gave better precision (smaller relative standard deviation (RSD) values) and comparable quantities of individual PAH's compared to the reflux procedure. Ultrasonication with the n-hexane-acetone (1:1, v/v) mixture, utilizing four 15 min extraction cycles, was found to be sufficient for extracting PAHs from wet sediments. The optimized ultrasonic extraction procedure extracted aliphatic and aromatic hydrocarbons from the National Institute of Standards and Technology SRM 1941a with recoveries greater than 90%. The major advantages of ultrasonication compared to the reflux method are the lower extraction times, simplicity of the apparatus and extraction procedure. The optimized ultrasonication procedure has been used in our laboratory to extract hydrocarbons from naturally wet sediments from rivers, and coastal and marine areas.
A new, improved method that only requires a potassium hydroxide extraction procedure is presented for the analysis of a full nucleotide pool in plant materials. Quantification was performed by high-pH anion-exchange chromatography (HPAEC) with UV detection after a potassium hydroxide extraction, and allowed the quantification of 13 linear ribonucleotides in a single run. The method has been validated by comparison of six extraction methods and also by measurement of the intracellular nucleotide levels of three plant species (cell cultures and leaves). The evolution of the nucleotide pool of Nicotiana tabacum cell culture during growth has also been measured, and showed an increase in the pool until the fifth day, where the growth rate reaches a maximum, after which a decrease was observed.
Conversions of statins, 3-hydroxy-3-methylglutaryl coenzyme A (HMG-CoA) reductase inhibitors, from lactone forms to their corresponding hydroxy acid form in 0.1 N NaOH or 0.05 N KOH (prepared with 25, 50, 75, 90% acetonitrile or methanol in water or 100% water) were evaluated. Results showed that lactone form statins could be transformed almost completely only in alkaline solutions prepared with 25 or 50% acetonitrile. In all methanolic alkaline solutions, lactone form statins could also be converted entirely, nevertheless, they would be further transformed to the methyl ester of the hydroxy acid form and the transformation increased as methanol rises. When lactone and hydroxy acid forms of statins were in methanol, ethyl acetate, 70% acetonitrile in water (with 0.5% acetic acid or no) for 0-48 h at room temperature or in 100 degrees C water for 0-2 h, lactone form statins were converted to their corresponding hydroxy acids, which were raised as time extends and the highest conversions of them were about 35% in 100 degrees C water and 70% acetonitrile, slightly transformed for lactone form statins in 70% acetonitrile (with 0.5% acetic acid) after 8 h, and the other treatments for all statins showed no significant changes. Interferences would be reduced efficiently when statins were extracted from Pu-Erh tea with methanol, ethyl acetate or 100 degrees C water followed by purifying through a C18 solid-phase extraction cartridge. Lovastatin was the only statin found in Pu-Erh tea and the highest content of it was found under ethyl acetate extraction. In ethyl acetate and methanol extracts, lovastatin existed merely as lactone form. The lowest content of lovastatin was found in the 100 degrees C water extract of Pu-Erh tea, however, both of lactone and hydroxy acid forms were found to exist in the extract.
Sub-micron sized polystyrene particles containing magnetite more than 30 wt.% were prepared by miniemulsion polymerization with commercially available ferricolloid. The effects of some water-soluble initiators and/or oil-soluble initiators on the particles characteristics, such as the size, morphology, magnetic properties and colloidal stability, were studied. The size of monomer droplets/polymer particles increased from 60 to 300 nm during polymerization, keeping magnetic in core when potassium persulfate (KPS) or ammonium persulfate (APS) was used as the sole initiator. These particles were easily separated from the medium within short time scale in external magnetic field, while such characteristics were controlled by the amount of persulfate used for the polymerization. In contrast, when 2,2'-azobis isobutyronitrile (AIBN) was used as the initiator, the size of droplets/particles was retained to be 90 nm at the most and magnetite nanoparticles located at the surface of polystyrene particles, which were so colloidally stable that they were not separated in external magnetic field. The above-mentioned effect of initiators on particle size in persulfate system was likely originated from the decrease of pH value and the increase of ionic strength, which induced the fusion of droplets/particles containing magnetite. Mixed-initiators system resulted in intermediate characteristics, compared with each initiator system. The location of magnetite in the particle seems to depend on where initiation/polymerization occurred in each initiator system.
OBJECTIVES: The goals of this study were to investigate the phase transformation and microstructure of dental porcelain bodies densified via a moving laser beam and to develop an understanding of how the microstructure of the dental porcelain varies with the laser processing condition and the position relative to the center of the laser beam. METHODS: A moving laser beam was used to scan and densify a commercial dental porcelain powder bed. The porcelain powder compact was also sintered using a furnace at different temperatures. The phase transformation and microstructure of these dental porcelain bodies were compared and investigated using a host of analytical instruments including scanning electron microscopy, X-ray diffraction, thermogravimetric analysis, and quantitative image analysis. RESULTS: Based on the temperature dependence of the leucite content in the dental porcelain derived from the furnace-sintered samples, the temperature distribution in the dental porcelain body during laser densification was established. The microstructure of the laser-densified porcelain body was found to be dependent of the location relative to the center of the laser beam and the average laser densification temperature. SIGNIFICANCE: The understanding of how the microstructure of dental porcelain bodies varies with the laser processing condition and the location with respect to the center of the laser beam was developed. Based on this understanding, the laser processing condition has been optimized to achieve the desired microstructure and densification of dental porcelain bodies simultaneously.
OBJECTIVES: The purpose of this study was to determine the validity and accuracy of mixing opaque feldspathic dental ceramic to obtain specific shades using two methods: (1) Concentration Additivity of Optical Parameters (CALAB) and (2) Concentration Additivity of Kubelka-Munk Optical Coefficients (CAK/S). METHODS: A total of 25 opaque feldspathic dental ceramic specimens were fabricated by mixing six different pure shades in different concentrations. The reflectance spectra were measured and the actual CIELAB L*, a* and b* coordinates were obtained for the 25 specimens. The CALAB and CAK/S methods were used to predict the L*, a* and b* values with reference to the concentrations of the pure shades. Correlation analysis was carried out between the actual and predicted L*, a* and b* values for both methods. The color differences (DeltaE*) between actual and predicted L*, a* and b* values were also calculated and analyzed using repeated measures ANOVA. RESULTS: Pearson's correlation coefficients between predicted and actual values for both methods were greater than 0.98. The mean DeltaE*s were 0.24 (0.11) for CALAB method and 0.21 (0.11) for the CAK/S method. The repeated measures ANOVA revealed a statistically significant difference (P=0.0213) between the mean DeltaE*s from the two methods. SIGNIFICANCE: Both methods produced mean DeltaE*s between the actual and predicted methods that were below the threshold of human perceptibility. The simpler CALAB method can be used to determine the opaque ceramic mixture for specific shades with accuracy.
OBJECTIVE: The aim of this study was to microstructurally characterize and to make comparisons of the physical properties of sintered dental porcelains prepared by mixing with distilled water and with their modeling liquid. METHODS: Six commercial porcelain powders: IPS Classic (Ivoclar Vivadent AG, Schaan, Liechtenstein), IPS d.SIGN (Ivoclar Vivadent AG), IPS InLine (Ivoclar Vivadent AG), Vita VMK95 (Vita Zahnfabrik, Bad Sackingen, Germany), Vita OMEGA 900 (Vita) and Ceramco III (Ceramco-Dentsply, Burlington, NJ, USA) were used as starting powders. Following particle size and BET analyses of starting powders, each porcelain powder was mixed with distilled water and with its own modeling liquid. Disc specimens were sintered in accordance with each manufacturer's instructions. Specimens were characterized using X-ray diffraction (XRD), optical microscopy and SEM analysis and their physical properties such as bulk density, microhardness and biaxial flexural strength were determined. RESULTS: The sintered dental porcelains premixed with modeling liquid had density, biaxial flexural strength and microhardness values slightly higher than those premixed with distilled water. Mixing with distilled water and modeling liquid caused statistically significant differences between the density values of Vita VMK 95 and microhardness values of IPS d.SIGN and IPS InLine. Characterization investigations (XRD and SEM) revealed the coexistence of the tetragonal leucite (1-3 microm) and hexagonal fluorapatite crystals (0.4-1.2 microm) in a feldspathic glassy matrix in the microstructure of IPS d.SIGN and only leucite crystals (3-6 microm) in the microstructures of other porcelains. SIGNIFICANCE: Mixing the porcelain powders with distilled water or modeling liquid prior to sintering has no effect on the resultant sintered crystalline microstructure. On the other hand, significant differences exist between the physical properties of some porcelains.
OBJECTIVES: The mechanical properties of zirconia ceramics are affected of stabilizing oxides and quality of sintering. The purpose of this study was to investigate the fracture resistance of frameworks manufactured using prefabricated zirconia blanks with differing stabilizing oxides and quality of sintering. METHODS: After dynamic loading in water, the fracture resistance was determined of stylized three-unit fixed partial dentures made of prefabricated homogenous ceramic green-body yttria-stabilized zirconia (Y-TZP) blanks (Vita YZ) or of densely-sintered magnesia partially stabilized zirconia (Mg-PSZ) blanks (Denzir-M); (i) as supplied from the manufacturer, (ii) after subjection to heat treatment in a way similar to veneering, and (Hi) after veneering with a feldspar-based ceramic. RESULTS: After veneering, the load at fracture of the Vita YZ specimens was significantly higher (p<0.05) than that of Denzir-M. The load necessary to fracture Denzir-M as supplied after machining was significantly (p<0.05) higher than that of heat-treated Denzir-M, Vita YZ as supplied and heat-treated Vita YZ specimens. There was no significant difference (p>0.05) between the heat-treated and veneered Denzir-M specimens. For Vita YZ the load at fracture of the veneered specimens was significantly (p<0.05) higher than of those as supplied or heat-treated, whereas no significant difference (p>0.05) was seen between heat-treated Vita YZ and Vita YZ specimens as supplied. SIGNIFICANCE: The fracture strength of the Vita YZ specimens increased considerably after veneering. Denzir-M and Vita YZ seem to be interesting alternatives for use as core materials in all-ceramic restorations. Long-term studies are, however, necessary before general clinical recommendations can be issued.
OBJECTIVE: The present study aimed at evaluating different restoring configurations of a crownless maxillary central incisor, in order to compare the biomechanical behavior of the restored tooth with that of a sound tooth. MATERIALS AND METHODS: A 3D FE model of a maxillary central incisor is presented. An arbitrary static force of 10 N was applied with an angulation of 125 degrees to the tooth longitudinal axis at level of the palatal surface of the crown. Different material configurations were tested: composite, syntered alumina, feldspathic ceramic endocrowns and glass post resorations with syntered alumina and feldspathic ceramic crown. RESULTS: High modulus materials used for the restoration strongly alter the natural biomechanical behavior of the tooth. Critical areas of high stress concentration are the restoration-cement-dentin interface both in the root canal and on the buccal and lingual aspects of the tooth-restoration interface. Materials with mechanical properties underposable to that of dentin or enamel improve the biomechanical behavior of the restored tooth reducing the areas of high stress concentration. SIGNIFICANCE: The use of endocrown restorations present the advantage of reducing the interfaces of the restorative system. The choice of the restorative materials should be carefully evaluated. Materials with mechanical properties similar to those of sound teeth improve the reliability of the restoartive system.
OBJECTIVES: This study evaluated the durability of bond strength between resin cement and a feldspathic ceramic submitted to different etching regimens with and without silane coupling agent application. METHODS: Thirty-two blocks (6.4 mm x 6.4 mm x 4.8 mm) were fabricated using a microparticulate feldspathic ceramic (Vita VM7), ultrasonically cleaned with water for 5 min and randomly divided into four groups, according to the type of etching agent and silanization method: method 1, etching with 10% hydrofluoric (HF) acid gel for 1 min + silanization; method 2, HF only; method 3, etching with 1.23% acidulated phosphate fluoride (APF) for 5 min + silanization; method 4, APF only. Conditioned blocks were positioned in their individual silicone molds and resin cement (Panavia F) was applied on the treated surfaces. Specimens were stored in distilled water (37 degrees C) for 24h prior to sectioning. After sectioning the ceramic-cement blocks in x- and y-axis with a bonded area of approximately 0.6mm(2), the microsticks of each block were randomly divided into two storage conditions: Dry, immediate testing; TC, thermal cycling (12,000 times)+water storage for 150 d, yielding to eight experimental groups. Microtensile bond strength tests were performed in universal testing machine (cross-head speed: 1mm/min) and failure types were noted. Data obtained (MPa) were analyzed with three-way ANOVA and Tukey's test (alpha=0.05). RESULTS: Significant influence of the use of silane (p<0.0001), storage conditions (p=0.0013) and surface treatment were observed (p=0.0014). The highest bond strengths were achieved in both dry and thermocycled conditions when the ceramics were etched with HF acid gel and silanized (17.4 +/- 5.8 and 17.4 +/- 4.8 MPa, respectively). Silanization after HF acid gel and APF treatment increased the results dramatically (14.5+/-4.2-17.4+/-4.8 MPa) compared to non-silanized groups (2.6 +/- 0.8-8.9 +/- 3.1 MPa) where the failure type was exclusively (100%) adhesive between the cement and the ceramic. SIGNIFICANCE: Silanization of the feldspathic ceramic surface after APF or HF acid etching increased the microtensile bond strength results significantly, with the latter providing higher results. Long-term thermocycling and water storage did not decrease the results in silanized groups.
Diabetic ketoacidosis (DKA) and hyperglycemic hyperosmolar state (HHS) potentially are fatal but largely preventable acute metabolic conditions of uncontrolled diabetes, the incidence of which continues to increase. Mortality from DKA has declined remarkably over the years because of better understanding of its pathophysiology and treatment. The mortality rate of HHS remains alarmingly high, however, owing to older age and mode of presentation of patients and associated comorbid conditions. DKA and HHS also are economically burdensome; therefore, any resources invested in their prevention would be rewarding.