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1.
Molecules ; 20(12): 22757-66, 2015 Dec 19.
Article in English | MEDLINE | ID: mdl-26703538

ABSTRACT

OSU-6, an MCM-41 type hexagonal mesoporous silica with mild Brönsted acid properties, has been used as an efficient, metal-free, heterogeneous catalyst for the click synthesis of 5-benzyl and 5-aryl-1H-tetrazoles from nitriles in DMF at 90 °C. This catalyst offers advantages including ease of operation, milder conditions, high yields, and reusability. Studies are presented that demonstrate the robust nature of the catalyst under the optimized reaction conditions. OSU-6 promotes the 1,3-dipolar addition of azides to nitriles without significant degradation or clogging of the nanoporous structure. The catalyst can be reused up to five times without a significant reduction in yield, and it does not require treatment with acid between reactions.


Subject(s)
Metals/chemistry , Silicon Dioxide/chemistry , Tetrazoles/chemistry , Azides/chemistry , Calcium Compounds/chemistry , Catalysis , Click Chemistry/methods , Nanopores , Nitriles/chemistry , Silicates/chemistry
2.
Rev Sci Instrum ; 79(8): 083706, 2008 Aug.
Article in English | MEDLINE | ID: mdl-19044356

ABSTRACT

In order to address the issue of spring constant calibration in viscous fluids such as water, a new method is presented that allows for the experimental calibration of bimaterial cantilever spring constants. This method is based on modeling rectangular cantilever beam bending as a function of changing temperature. The temperature change is accomplished by heating water as it flows around the cantilever beams in an enclosed compartment. The optical static method of detection is used to measure the deflection of cantilever at the free end. Experimentally determined results are compared to Sader's method and to the Thermotune method most commonly used in cantilever calibrations. Results indicate that the new bimaterial thermal expansion method is accurate within 15%-20% of the actual cantilever spring constant, which is comparable to other nondestructive calibration techniques.

3.
Rev Sci Instrum ; 79(9): 096102, 2008 Sep.
Article in English | MEDLINE | ID: mdl-19044456

ABSTRACT

A thin film evaporation device has been developed to prepare energetic materials at atmospheric pressure. The device is intuitive, simple, and easy to manipulate. The application of the device is demonstrated for pentaerythritol tetranitrate but can be extended to other explosives and organic materials that have low saturation pressures.

4.
Langmuir ; 24(11): 5955-60, 2008 Jun 03.
Article in English | MEDLINE | ID: mdl-18471001

ABSTRACT

We have developed a flow cell that allows culturing adherent cells as well as suspended cells in a stable, homogeneous, and low-shear force environment. The device features continuous medium supply and waste exchange. In this paper, a simple and fast protocol for device design, fabrication, and assembly (sealing) based on a poly(dimethylsiloxane) (PMDS)/glass slide hybrid structure is described. The cell culture system performance was monitored, and the effective shear force inside the culture well was also determined. By manipulating the device dimensions and volumetric flow rate, shear stress was controlled during experiments. Cell adhesion, growth, proliferation, and death over long-term culture periods were observed by microscopy. The growth of both endothelial and suspension cells in this device exhibited comparable characteristics to those of traditional approaches. The low-shear culture device significantly reduced shear stress encountered in microfluidic systems, allowing both adherent and suspended cells to be grown in a simple device.


Subject(s)
Cell Culture Techniques/instrumentation , Endothelial Cells/cytology , Microfluidic Analytical Techniques/instrumentation , Animals , Cell Adhesion , Cell Culture Techniques/methods , Cell Line , Cell Proliferation , Mice , Microfluidic Analytical Techniques/methods , Shear Strength , Stress, Mechanical , Time Factors
5.
Scanning ; 30(2): 118-22, 2008.
Article in English | MEDLINE | ID: mdl-18241042

ABSTRACT

The removal behavior of self-assembled monolayers (SAMs) of thiol molecules on a gold substrate by an NH(4)OH-H(2)O(2)-H(2)O solution was studied using attenuated total reflectance infrared spectroscopy (ATR-IR) and atomic force microscopy (AFM). Furthermore, the impact of the concentration of NH(4)OH and H(2)O(2) in the solution and reaction temperature on the SAM removal rate and efficiency was explored. The SAM removal rate and efficiency were significantly influenced by the concentration of NH(4)OH rather than H(2)O(2). The solution containing the 2 : 1 molar ratio of NH(4)OH : H(2)O(2) among three different solutions showed the highest removal rate and efficiency in the removal of 11-mercapto-1-undecanol. The increase in the reaction temperature resulted in the enhancement on the SAM removal rate, but it led to the fast delamination of the gold layer. These results may be useful in the regeneration of sensor surfaces relying on gold/thiol chemistry.

6.
J Phys Chem B ; 111(31): 9182-5, 2007 Aug 09.
Article in English | MEDLINE | ID: mdl-17630792

ABSTRACT

Atomic force microscopy (AFM) has been successfully used to study the activation energy for evaporation of pentaerythritol tetranitrate (PETN) nanoislands formed by spin coating. These islands are annealed isothermally in the temperature range of 30-70 degrees C for a given time and are scanned with AFM in contact mode at room temperature. The volume of these islands does not change significantly up to about 35-40 degrees C indicating that sublimation is not significant below 40 degrees C. Above 40 degrees C, the islands start shrinking, and the rate of weight loss is analyzed as a function of temperature. The activation energy of evaporation using AFM was found to be similar to that for bulk PETN crystals using thermogravimetric analysis (TGA) at higher temperatures (110-135 degrees C). These results demonstrate that AFM is a useful tool to measure thermodynamic properties with a nanoscale probe.

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