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PubMed1979

Analysis of the venom of the Sydney funnel-web spider, Atrax robustus using gas chromatography mass spectrometry.

Thirteen compounds have been identified using gas chromatography mass spectrometry in the venom of the Sydney funnel-web spider, Atrax robustus. The compounds were identified as their trimethylsilyl or pentafluoropropionate derivatives and were citric acid, lactic acid, phosphoric acid, glycerol, urea, glucose, gamma-aminobutyric acid, glycine, spermidine, spermine, tyramine and octopamine. Female venom contained trace quantities of 5-methyoxytryptamine which was not detected in male venom. Quantitative determination of tyramine and octopamine was achieved using chemical ionization (CH4) gas chromatography mass spectrometry and deuterated internal standards.

Arthropod Venoms↗

PubMed1985

Kinetics of phosphoramide mustard hydrolysis in aqueous solution.

Hydrolysis of phosphoramide mustard was investigated using HPLC, 31P NMR, and GC-MS with specific deuterium labels. The hydrolysis of phosphoramide mustard in sodium phosphate buffers was found to follow apparent first-order kinetics. The rate of hydrolysis was temperature and pH dependent, being slower under acidic conditions. The hydrolysis was not catalyzed by hydroxyl ion, and its pH dependence appeared to be the result of a change in the mechanism of hydrolysis at different pH values. At a pH value approximately above the pKa of the phosphoramide mustard nitrogen, the major hydrolytic pathway of phosphoramide mustard was via the formation of the aziridinium ion, followed by nucleophilic attack. At pH values below its pKa, cleavage of the P-N bond predominated. At pH 7.4, the formation of an aziridinium ion was followed by a rapid hydrolysis to yield the monohydroxy and, subsequently, the dihydroxy products. The hydrolysis at this pH was adequately described by consecutive first-order kinetics. Seven species in the hydrolytic mixture have been identified as intact phosphoramide mustard, N-(2-chloroethyl)-N-(2-hydroxyethyl)phosphorodiamidic acid, N,N-bis-(2-hydroxyethyl)phosphorodiamidic acid, phosphoramidic acid, phosphoric acid, N,N-bis-(2-chloroethyl)amine, and N-(2-chloroethyl)-N-(2-hydroxyethyl)amine by GC-MS with the aid of deuterium labels. Phosphoramide mustard was found to be stabilized by chloride ion. The stabilization was linearly related to the chloride ion concentration, and the mechanism was found to be via the formation of phosphoramide mustard from the aziridinium and chloride ions. Phosphoramide mustard was significantly more stable in human plasma and in 5% human serum albumin as compared to aqueous buffers, an observation that may be important in vivo.

Bromides↗

PubMed1998

High-pressure liquid chromatographic determination of toluene in urine as a marker of occupational exposure to toluene.

OBJECTIVE: To establish a convenient method by high-pressure liquid chromatography (HPLC) to measure toluene in urine as a marker of occupational exposure to toluene. METHODS: As soon after sampling as possible, 1 ml of urine was mixed with an equal volume of acetonitrile in a 2.2-ml HPLC glass bottle, and the bottle was tightly sealed and stored at 4 degrees C. Immediately before HPLC determination, 100 microl methanol was added to the mixture to prevent confounding effects of glycosuria, and the bottle was spun to remove any suspended matter. An aliquot of the supernate was introduced into the HPLC system and analyzed on a PRODIGY column, with an acetonitrile - perchloric acid phosphoric acid - water mixture serving as the mobile phase. The effluent was monitored at 191 nm. RESULTS: The method can measure toluene in urine every 20 min, the detection limit was 2 microg/l, the coefficient of variation was less than 5%, and the recovery rate was 100%. No significant reduction in toluene concentration was observed for 1 week after storage at 4 degrees C. When the method was applied to end-of-shift urine samples from 13 male workers exposed to toluene at 18-140 ppm and also to urine samples from 10 nonexposed male controls, toluene in urine was linearly related to toluene exposure concentration, with a regression line passing close to the origin. The correlation coefficient was as high as 0.97 (n=23). No toluene was detected in control urine samples. Calculations suggest that urinary toluene accounts for as little as less than 0.01% of the toluene absorbed via inhalation and that the absorbed toluene is converted almost quantitatively to hippuric acid and, by less than 0.1%, to o-cresol.

Adult↗

PubMed1980

Improvements in the determination of urea using diacetyl monoxime; methods with and without deproteinisation.

A rapid and reproducible method is described for measurement of urea in biological materials (after deproteinisation) and in serum (without deproteinisation). Urea is colorimetrically determined with diacetyl monoxime and thiosemicarbazide in the presence of sulphuric acid, phosphoric acid and ferric chloride. The sensitivity of the colorimetric reaction and stability of the colour are enhanced over existing related procedures and the serum blank diminished, enabling urea to be precisely measured in micro amounts (1--5 microliters) of serum.

Chromogenic Compounds↗

PubMed1980

Asthma caused by occupational exposure to a furan-based binder system.

A 50-yr-old mold maker developed severe asthma a few weeks after commencing work with a furan binder. Asthma recurred within hours of subsequent exposure and was confirmed by measurements every 2 hr of peak flow rate. The molds were prepared by mixing sand with a resin (containing furfuryl alcohol, paraformaldehyde, and xylene) and a catalyst (containing sulfuric acid, phosphoric acid, and butyl alcohol). Occupation-type exposure in the laboratory to the resin mixed with catalyst, and to pure furfuryl alcohol mixed with sulfuric acid or butyl alcohol, provoked late asthmatic responses and heightened nonallergic bronchial responsiveness to inhaled histamine. No changes were produced by the same exposures in an asthmatic volunteer with a similar degree of histamine bronchial responsiveness, or in the worker after exposure to resin alone and catalyst alone. Avoidance of exposure was followed by clearing of symptoms and return of histamine bronchial responsiveness towards normal. The findings identify the occurrence of specific bronchial responsiveness to volatile reaction product(s) of furfuryl alcohol following reaction with sulfuric acid or with butyl alcohol. The incidence of this problem needs investigation, especially since furan-based binder systems are replacing traditional methods.

Albuterol↗

PubMed2004

Activation of waste MDF sawdust charcoal and its reactive dye adsorption characteristics.

This paper reports an experimental investigation of converting waste medium density fibreboard (MDF) sawdust into chars and activated carbon using chemical activation and thermal carbonisation processes. The MDF sawdust generated during the production of architectural mouldings was characterised and found to have unique properties in terms of fine particle size and high particle density. It also has a high content of urea formaldehyde resin used as a binder in the manufacturing of MDF board. Direct thermal carbonisation and chemical activation of the sawdust by metal impregnation and acid (phosphoric acid) treatment prior to pyrolysis treatment were carried out. The surface morphology of the raw dust, its chars and activated carbon were examined using scanning electron microscopy (SEM). Adsorptive properties and total pore volume of the materials were also analysed using the BET nitrogen adsorption method. Liquid adsorption of a reactive dye (Levafix Brilliant red E-4BA) by the derived sawdust carbon was investigated in batch isothermal adsorption process and the results compared to adsorption on to a commercial activated carbon (Filtrasorb F400). The MDF sawdust carbon exhibited in general a very low adsorption capacity towards the reactive dye, and physical characterisation of the carbon revealed that the conventional chemical activation and thermal carbonisation process were ineffective in developing a microporous structure in the dust particles. The small size of the powdery dust, the high particle density, and the presence of the urea formaldehyde resin all contributed to the difficulty of developing a proper porous structure during the thermal and chemical activation process. Finally, activation of the dust material in a consolidated form (cylindrical pellet) only achieved very limited improvement in the dye adsorption capacity. This original study, reporting some unexpected outcomes, may serve as a stepping-stone for future investigations of recycle and reuse of the waste MDF sawdust which is becoming an increasing environmental and cost liability.

Adsorption↗

PubMed2002

Gas phase reactions of trimethyl borate with phosphates and their non-covalent complexes.

Using a quadrupole ion trap mass spectrometer, trimethyl borate was allowed to react with dihydrogen phosphate, deprotonated O-phosphoserine, and a set of hydrogen bonded complexes involving dihydrogen phosphate and neutral acids (phosphoric acid, acetic acid, serine, and O-phosphoserine). The reactions show a consistent pattern in which the initial attack leads to addition with the loss of one or two CH3OH molecules. Collision-activated dissociation (CAD) experiments on the reaction products generally lead to the loss of an additional CH3OH molecule. In no case is a partner from the original hydrogen-bonded complex lost. The results indicate that the reactions lead to structures where the phosphate and its complex partner are covalently bound to the boron. For each of the reactions, rate constants were determined. In the course of CAD experiments (up to MS5), several novel borophosphate structures were identified. The work is supported by ab initio calculations on selected species.

Borates↗

PubMed2003

Augmenting effect of acetic acid for acidification on bactericidal activity of hypochlorite solution.

AIMS: Bactericidal activity of chlorine solution is enhanced by weak acidification. We compared the effects of various acids on the bactericidal activity of hypochlorite solution to establish a method for safe and effective use of an acidic hypochlorite solution. METHODS AND RESULTS: The bactericidal activities of acidic hypochlorite solutions that had been adjusted to pH 5.0 with hydrochloric acid, acetic acid, citric acid, lactic acid, formic acid, phosphoric acid or sulphuric acid against Bacillus subtilis spores were compared. The acidic solutions prepared with hydrochloric acid and acetic acid showed the highest bactericidal activity, and all of the spores (5 x 106 cfu ml(-1)) were killed within 10 min. On the other hand, the solutions prepared with citric acid and lactic acid showed no bactericidal activity against any bacterial strains tested in this study despite the low pH. The amount of chlorine gas produced by the preparation using acetic acid was sixfold less than that produced from the preparation using hydrochloric acid. CONCLUSIONS: Acetic acid is the most suitable and safe acid for the preparation of an acidic hypochlorite solution. SIGNIFICANCE AND IMPACT OF THE STUDY: The results of this study provide useful information for establishing a method for safe and effective use of an acidic hypochlorite solution.

Acetic Acid↗

PubMed2001

Comparative study of influence on tensile bond strength of a composite to dentin using Er:YAG laser, air abrasion, or air turbine for preparation of cavities.

OBJECTIVES: The purpose of this study was to evaluate, in vitro, the tensile bond strength of the Single Bond (3M) adhesive system placed over dentin surfaces treated with air turbine, Er:YAG laser without contact and in focused or air abrasion. SUMMARY BACKGROUND DATA: The use of dentin adhesives is a well-established clinical routine among the dentists. However, there have been few reports comparing the influence of the Er:YAG laser, air abrasion, and air turbine on the Single Bond tensile bond strength of adhesives systems to dentin fact that could influence which tools dentists select for use in cavity preparations. METHODS: Twenty-three extracted retained human molars were used in this study. The coronal portion was divided in two parts and fixed in acrylic resin; the occlusal surface was abraded to a 2-mm width with a mechanic lathe until the dentin surface was completely exposed. The dental portions were divided into three groups of 15 each and treated with Er:YAG laser, air abrasion, or air turbine. A 3 mm hole in the center of each tooth was marked off using contact paper. Single Bond (3M) adhesive system was applied after acid phosphoric at 35% application for 15 sec over dentin surfaces. A resin composite cone was built into the delimited area to accomplish the tensile bond strength test on the EMIC universal test machine. The specimens were then evaluated by stereoscopy to determine the type of failures into the dentin-adhesive-resin composite surface. RESULTS: The tensile test was performed using the universal testing machine EMIC DL-2000 at a cross-head speed of 0.5 mm/min. The average results were: air turbine (17.52 MPa), Er:YAG laser (16.65 MPa) and air abrasion (15.83 MPa). Statistical treatment by ANOVA and Tukey's test (p < 0.01) showed no significant differences between the groups tested. The tensile bond strength test to the dentin showed no significant difference among the three groups when the Single Bond was used after the 35% phosphoric-acid conditioning. The stereoscopy showed a predominant adhesive failure in all groups. CONCLUSION: These results suggest that Single Bond tensile bond strength is the same as dentin prepared by Er:YAG laser, air abrasion, or air turbine.

Air Abrasion, Dental↗

PubMedDate not supplied

Method to detect minimal amounts of calcium dissolved in acidic solutions.

The study describes the application of the Arsenazo III method for detection of minimal amounts of calcium 12.4-49.4 micromol/l in different acidic solutions (hydrochloric acid, oxalic acid, maleic acid, phosphoric acid, tartaric acid, citric acid, lactic acid and acetic acid) adjusted to pH 2.0, 2.3 and 3.0. A mixture of the respective calcium concentrations with distilled water served as control. The experiments were run with ten repeats in series. Assessment of intra- and interassay coefficient of variation, and lower limit of quantification revealed that depending on the acid used, the Arsenazo III method is a reliable tool to quantify minimal calcium contents in acidic solutions.

Arsenazo III↗

PubMed2004

Derivatization in mass spectrometry-3. Alkylation (arylation).

The review is devoted to alkylation (arylation) as a widely employed derivatization procedure for the protection of OH (carboxylic acids, phosphoric acids, sulfonic acids, alcohols, polyols, phenols, enols), SH (thiols) and NH (amines, amides) groups in order to increase volatility, to improve the chromatographic properties and, if possible, mass spectral properties of derivatives. Chemical aspects of derivatization and various alkylation (arylation) reagents and reaction procedures are described. Specific mass spectral (electron ionization, chemical ionization) features of derivatives helpful in identification, structure elucidation, profiling and quantitative determination of the above-mentioned polar compounds by coupled gas chromatography or high-performance liquid chromatography are discussed. Some common analytical applications of the procedures in organic chemistry, clinical chemistry, environmental chemistry etc. are briefly summarized.

Acids↗

PubMed1991

[Blood biochemistry during acidosis associated with ATP-induced hypotensive anesthesia].

Several investigators reported metabolic acidosis during ATP-induced hypotensive anesthesia. To elucidate the etiology, we studied blood biochemistry during hypotensive anesthesia for tympanoplastic surgery. The blood concentration of lactic acid, uric acid, phosphoric acid and carbonic acid increased and their total amount coincided with the base excess change. We also found that metabolic intermediates of glycolysis and of the catabolic pathway of adenosine also increased proportionally. The result suggests that the metabolic change is caused by lactic acid produced from glycolysis promoted by ATP and by the catabolic products of administered ATP itself.

Acidosis↗

PubMed1996

Testing mode and surface treatment effects on dentin bonding.

The goal of this project was to evaluate the effect of the following variables on shear dentin-bonding test results: mode of testing (cyclic fatigue versus static loading), surface treatments (32% phosphoric acid, 10% phosphoric acid, and no treatment [unetched]), and type of shear test (traditional planar versus push-out). All teeth were stored in distilled water and tested in a shear mode at a loading rate of 2 mm/ min. The specimens were loaded in static or cycled for 1000 cycles using a staircase approach or until fracture, whichever occurred first. On samples with etched dentin surfaces, the push-out test did not demonstrate a significant difference in measured bond strength when compared with results from the planar test, although sample preparation was more labor-intensive. The bond strength resulting from cyclic fatigue of the etched specimens was approximately 51% of the static loading value. Ten percent phosphoric acid was as effective as 32% phosphoric acid for dentin bonding. Finite-element analysis indicated that the traditional planar shear test produces flexure of the specimen and high tensile stress magnitudes within the resin bonding layer. The push-out test produces elevated compressive stresses localized in the composite along the circumference of the punch. Shear stresses in the resin bonding layer are similar for both testing methods at the same loading element contact force.

Acid Etching, Dental↗

PubMed2006

Acid resistance of erbium-doped yttrium aluminum garnet laser-treated and phosphoric acid-etched enamels.

OBJECTIVE: To compare the effects of erbium-doped yttrium aluminum garnet (Er:YAG) laser ablation and of phosphoric acid etching on the in vitro acid resistance of bovine enamel. MATERIALS AND METHODS: Teeth were polished to make the surface flat. The polished enamel was either etched with 37% phosphoric acid for 30 seconds or ablated with a single 33 J/cm2 pulse from an Er:YAG laser. The control specimens were free from acid etching and laser ablation. Changes in crystal structure, dissolved mineral (calcium [Ca] and phosphorus [P]) contents, and calcium distribution in the enamel subsurface after a pH-cycling process were evaluated. RESULTS: After laser treatment, poor crystal structures improved without forming any new phases, such as tricalcium phosphates. Among the tested enamels, dissolved mineral contents were significantly different (P < .05). Er:YAG laser-treated enamels had the lowest mineral dissolution (Ca, 13.78 ppm; P, 6.33 ppm), whereas phosphoric acid-etched enamels had the highest (Ca, 15.90 ppm; P, 7.33 ppm). The reduction rate and reduced depth of calcium content along the subsurface were lowest in Er:YAG laser-treated enamels. CONCLUSION: The Er:YAG laser-treated enamels are more acid resistant to acid attack than phosphoric acid-etched enamels.

Animals↗

PubMed2003

Use of a self-etching primer in combination with a resin-modified glass ionomer: effect of water and saliva contamination on shear bond strength.

The purpose of this study was to evaluate the effects of 3 different enamel conditioners (10% polyacrylic acid, 37% phosphoric acid, and self-etching primer) on the shear bond strength and site of bond failure of a resin-modified glass ionomer (Fuji Ortho LC, GC Europe, Leuven, Belgium) bonded onto dry, water-moistened, and saliva-moistened enamel. One hundred eighty bovine permanent mandibular incisors were randomly divided into 12 groups; each group consisted of 15 specimens. Three different enamel surface conditions were studied: dry, soaked with water, soaked with saliva. One hundred eighty stainless steel brackets were bonded with the resin-modified glass ionomer. After bonding, all samples were stored in distilled water for 24 hours and then tested in a shear mode on a testing machine. After self-etching primer application, Fuji Ortho LC produced the highest shear bond strengths under all the different enamel surface conditions; these values were significantly higher than those achieved in the remaining groups, except when Fuji Ortho LC was used in combination with 37% phosphoric acid on dry enamel. Fuji Ortho LC bonded without enamel conditioning produced the lowest shear bond strengths. The bond strength of the groups conditioned with 10% polyacrylic acid was significantly lower than that of the groups etched with 37% phosphoric acid, except when both conditioners were used on enamel soaked with water.

Acid Etching, Dental↗

PubMed1999

In vitro shear bond strength of adhesive to normal and fluoridated enamel under various contaminated conditions.

OBJECTIVE: This study examined the shear bond strength of bonding agents to normal or fluoridated enamel following use of weak or strong acids to prepare enamel surfaces and after contamination with a measured amount of saliva at various stages of the bonding procedure. METHOD AND MATERIALS: One hundred extracted human third molar teeth were randomly separated into 2 basic groups (normal or fluoridated teeth), then divided into 5 subgroups. Group A specimens were not contaminated. After etching, enamel surfaces were dry and clean. Group B was left with wet surfaces after etching. Group C specimens were contaminated with artificial saliva and then dried. Group D specimens were contaminated with artificial saliva, rinsed, and then dried. In group E, all enamel surfaces were left contaminated with saliva after the etching procedures (with maleic acid or phosphoric acids). Adhesive resins were applied to all enamel surfaces according to the manufacturer's instructions. The specimens were then mounted and tested to determine shear bond strength. RESULTS: If normal enamel surfaces were rinsed and dried immediately after contamination, there was no significant reduction of shear bond strength of adhesive to enamel. Specimens in group E and group C had significantly lower bond strengths than did control specimens (group A). In the fluoridated groups etched with the phosphoric acid, statistically significant reductions in bond strengths were obtained in all contamination groups and in the control group. In the fluoridated specimens, there were no statistically significant differences between any of the contamination groups and the control group when maleic acid was used. CONCLUSION: Saliva contamination may not be a risk factor for successful bonding between bonding agent and dental tissues for normal or fluoridated enamel surfaces if they are rinsed and dried immediately after contamination. Etching of normal enamel surfaces with phosphoric acid in the presence of contamination may provide higher shear bond strength than etching with maleic acid.

Acid Etching, Dental↗

PubMed2001

Adhesion of a glass-ionomer root canal sealer to the root canal wall.

Glass-ionomer root canal sealer is commonly used because of its chemical bonding and favorable physical characteristics when bonding to dentin. This study was designed to determine the tensile bond strength of a glass-ionomer sealer (Ketac Endo, Espe, Seefeld, Germany) on root canal walls after pretreatment with different conditioners. Flat inner surfaces of root canal specimens were prepared. The specimens were divided into five groups of 10 teeth, and the groups were conditioned with one of the following smear layer removal solutions: 15% EDTA/NaOCl, 10% polyacrylic acid, 35% phosphoric acid, 6% citric acid, and 5.25% NaOCl as a control. Then the exposed root canal areas were coated with Ketac-Endo. Tensile bonding was measured using a universal testing machine until ultimate failure was obtained. The groups that were treated with phosphoric acid and citric acid showed significantly higher bond strengths than the groups that were treated with 15% EDTA and polyacrylic acid (p < 0.05). Bonding to dentin without smear layer removal (NaOCl group) was too low to be measured in the testing apparatus. Scanning electron microscopy confirmed that phosphoric and citric acids were more effective in removing smear layer than EDTA or polyacrylic acid. The result supported the view that pretreatment with phosphoric acid or citric acid should be used in association with glass-ionomer root canal sealer to achieve the most effective removal of the smear layer and to provide better adhesion.

Acid Etching, Dental↗

PubMed2006

Organogels with Fe(III) complexes of phosphorus-containing amphiphiles as two-component isothermal gelators.

The properties of thermally reversible organogels in which the gelators consist of a phosphonic acid monoester, phosphonic acid, or phosphoric acid monoester and a ferric salt are probed by IR and NMR spectroscopies, optical microscopy, X-ray diffraction, rheology, and light and small-angle neutron scattering (SANS) techniques. This is one of a small number of two-component molecular gelator systems in which gelation can be induced isothermally. The data indicate that complexation between the phosphonate moieties and Fe(III) is accompanied by their in situ polymerization to form self-assembled fibrillar networks that encapsulate and immobilize macroscopically the organic liquid component. From SANS measurements, the cross-sectional radii of the cyclindrical fibers are ca. 15 A. The efficiencies of the gelators (based on the diversity of the liquids gelated, the minimum concentration of gelator required to make a gel at room temperature, and the temporal and thermal stabilities of the gels) have been determined. With a common ferric salt and liquid component, phosphonic acid monoesters are generally more efficient than phosphinic acids or phosphoric acid esters. Of the phosphonic acid monoesters, monophosphonates are better gelator components than bisphosphonates, and introduction of an omega-hydroxy group on the alkyl chain directly attached to phosphorus reduces significantly gelation ability. Several of the gels are stable for very long periods at room temperature. When heated, they revert to sols over wide temperature ranges. The structures of the gelator complexes and the mechanism of their formation and transformation to gels in selected liquids are examined as well.

Journal Article↗