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1.
J Vis Exp ; (123)2017 05 11.
Article in English | MEDLINE | ID: mdl-28518076

ABSTRACT

An aqueous suspension of nanogibbsite was synthesized via the titration of aluminum aqua acid [Al(H2O)6]3+ with L-arginine to pH 4.6. Since the hydrolysis of aqueous aluminum salts is known to produce a wide array of products with a wide range of size distributions, a variety of state-of-the-art instruments (i.e., 27Al/1H NMR, FTIR, ICP-OES, TEM-EDX, XPS, XRD, and BET) were used to characterize the synthesis products and identification of byproducts. The product, which was comprised of nanoparticles (10-30 nm), was isolated using gel permeation chromatography (GPC) column technique. Fourier transform infrared (FTIR) spectroscopy and powder X-ray diffraction (PXRD) identified the purified material as the gibbsite polymorph of aluminum hydroxide. The addition of inorganic salts (e.g., NaCl) induced electrostatic destabilization of the suspension, thereby agglomerating the nanoparticles to yield Al(OH)3 precipitate with large particle sizes. By utilizing the novel synthetic method described here, Al(OH)3 was partially loaded inside the highly ordered mesoporous framework of MCM-41, with average pore dimensions of 2.7 nm, producing an aluminosilicate material with both octahedral and tetrahedral Al (Oh/Td = 1.4). The total Al content, measured using energy-dispersive X-ray spectrometry (EDX), was 11% w/w with a Si/Al molar ratio of 2.9. A comparison of bulk EDX with surface X-ray photoelectron spectroscopy (XPS) elemental analysis provided insight into the distribution of Al within the aluminosilicate material. Furthermore, a higher ratio of Si/Al was observed on the external surface (3.6) as compared to the bulk (2.9). Approximations of O/Al ratios suggest a higher concentration of Al(O)3 and Al(O)4 groups near the core and external surface, respectively. The newly developed synthesis of Al-MCM-41 yields a relatively high Al content while maintaining the integrity of the ordered silica framework and can be used for applications where hydrated or anhydrous Al2O3 nanoparticles are advantageous.


Subject(s)
Aluminum Hydroxide/chemical synthesis , Nanoparticles , Silicon Dioxide/chemistry , Aluminum Silicates , Chromatography, Gel , Microscopy, Electron, Transmission , Porosity , Spectroscopy, Fourier Transform Infrared , Thermodynamics , X-Ray Diffraction
2.
Inorg Chem ; 55(23): 12270-12280, 2016 Dec 05.
Article in English | MEDLINE | ID: mdl-27934402

ABSTRACT

We report solid-state 27Al NMR spectroscopic results for the sulfate salt of the γ-Al13 Keggin cluster, γ-[AlO4Al12(OH)25(OH2)11][SO4]3·[H2O]14, that provide a spectroscopic signature for partial hydrolysis of this Keggin-type cluster. In 27Al multiple-quantum magic-angle spinning NMR spectra, all 13 Al positions of the cluster are at least partially resolved and assigned with the aid of density functional theory (DFT) calculations of the 27Al electric field gradients. The isotropic chemical shift of the single tetrahedral site, 75.7 ppm, is nearly identical to that reported for solutions from which the cluster crystallizes. Reflecting broadly similar coordination environments, the octahedral Al show mostly small variations in isotropic chemical shift (+7 to +11 ppm) and quadrupolar coupling constant (CQ; 6-7.5 MHz), except for one resonance that exhibits a much smaller CQ and another site with a larger value. DFT calculations show that deprotonation of a terminal water ligand, to form an η-OH group, causes a large reduction in the 27Al CQ, allowing assignment of a distinct, narrow peak for octahedral Al to this hydroxyl-terminated site. This result suggests a relationship between octahedral 27Al NMR line width and hydrolysis for solids prepared from Keggin-type clusters.

3.
Appl Environ Microbiol ; 72(10): 6734-42, 2006 Oct.
Article in English | MEDLINE | ID: mdl-17021225

ABSTRACT

Clinical studies indicate relationships between dental plaque, a naturally formed biofilm, and oral diseases. The crucial role of nonmicrobial biofilm constituents in maintaining biofilm structure and biofilm-specific attributes, such as resistance to shear and viscoelasticity, is increasingly recognized. Concurrent analyses of the diverse nonmicrobial biofilm components for multiparameter assessments formed the focus of this investigation. Comparable numbers of Actinomyces viscosus, Streptococcus sanguinis, Streptococcus mutans, Neisseria subflava, and Actinobacillus actinomycetemcomitans cells were seeded into multiple wells of 96-well polystyrene plates for biofilm formation. Quantitative fluorescence and confocal laser scanning microscopy (CLSM) examined the influences of dietary sugars, incubation conditions, ingredients in oral hygiene formulations, and antibiotics on biofilm components. Biofilm extracellular polymeric substances (EPS) were examined with an optimized mixture of fluorescent lectins, with biofilm proteins, lipids, and nucleic acids detected with specific fluorescent stains. Anaerobic incubation of biofilms resulted in significantly more biofilm EPS and extractable carbohydrates than those formed under aerobic conditions (P < 0.05). Sucrose significantly enhanced biofilm EPS in comparison to fructose, galactose, glucose, and lactose (P < 0.05). CLSM demonstrated thicker biofilms under sucrose-replete conditions, along with significant increases in biofilm EPS, proteins, lipids, and nucleic acids, than under conditions of sucrose deficiency (P < 0.05). Agents in oral hygiene formulations (chlorhexidine, ethanol, and sodium lauryl sulfate), a mucolytic agent (N-acetyl-L-cysteine), and antibiotics with different modes of action (amoxicillin, doxycycline, erythromycin, metronidazole, and vancomycin) inhibited biofilm components (P < 0.05). Multiparameter analysis indicated a dose-dependent inhibition of biofilm EPS and protein by chlorhexidine and sodium lauryl sulfate, along with distinctive inhibitory patterns for subinhibitory concentrations of antibiotics. Collectively, these results highlight multiparameter assessments as a broad platform for simultaneous assessment of diverse biofilm components.


Subject(s)
Anti-Infective Agents/pharmacology , Biofilms/drug effects , Bioreactors , Carbohydrates/pharmacology , Biofilms/growth & development , Culture Media , Drug Administration Routes , Ecosystem
4.
J Clin Dent ; 15(2): 37-40, 2004.
Article in English | MEDLINE | ID: mdl-15359541

ABSTRACT

Colgate Simply White Toothpaste is a new advanced tooth whitening dentifrice that can be used every day. The synergy of abrasive stain removal with activated hydrogen peroxide delivers excellent performance in the removal of extrinsic and intrinsic tooth stain. Colgate Simply White Toothpaste provides other oral health benefits that have become the cost-of-entry into the toothpaste market: caries protection, tartar control, fresh breath, and a preferred flavor.


Subject(s)
Gluconates/chemistry , Hydrogen Peroxide/chemistry , Tooth Bleaching/methods , Toothpastes/chemistry , Biological Availability , Cariostatic Agents/chemistry , Chemistry, Pharmaceutical , Dental Calculus/prevention & control , Fluorides/chemistry , Humans , Oxidants/chemistry , Silicic Acid , Technology, Pharmaceutical , Tooth Discoloration/therapy , Toothpastes/classification
5.
Compend Contin Educ Dent ; 24(9 Suppl): 25-8; quiz 43, 2003 Sep.
Article in English | MEDLINE | ID: mdl-14692209

ABSTRACT

Volatile sulfur compounds are known to be major contributors to oral malodor, and their detection by gas chromatography (GC) is a commonly used method for evaluating breath odor in clinical trials. A custom-designed breath-sampling GC system was developed for this purpose. A clinical study was performed to compare the performance of this instrumental method to organoleptic evaluation by trained odor judges. A statistically significant correlation was found between the measured levels of volatile sulfurs and the ratings of the odor judges. Both methods performed similarly in evaluating the breath-freshening effects of two test products. These results demonstrate the strength of the GC method for evaluating breath odor and predicting the breath-freshening effects of oral-care products.


Subject(s)
Breath Tests/methods , Halitosis/therapy , Sulfur Compounds/analysis , Adult , Chromatography, Gas , Double-Blind Method , Humans , Middle Aged , Statistics, Nonparametric
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