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1.
Anal Chem ; 89(11): 5882-5890, 2017 06 06.
Article in English | MEDLINE | ID: mdl-28497696

ABSTRACT

A new approach to achieving chemical mapping on a nanoscale is described that can provide 2D and tomographic images of surface and near-surface structure. The method comprises dissolving material from the surface of the sample by applying a series of aliquots of solvent, then analyzing their contents after removing them; in between exposures, the surface is imaged with atomic force microscopy. This technique relies on being able to compensate for any drift between images by use of software. It was applied to a blend of two polymers, PMMA and PS. The analytical data identified the material that was dissolved, and the topography images enabled the location of the various materials to be determined by analyzing local dissolution kinetics. The prospects for generalizing the approach are discussed.

2.
Chem Commun (Camb) ; 50(79): 11742-5, 2014 Oct 11.
Article in English | MEDLINE | ID: mdl-25144908

ABSTRACT

Here we describe a simple route to creating conformal sulphated zirconia monolayers throughout an SBA-15 architecture that confers efficient acid-catalysed one-pot conversion of glucose to ethyl levulinate.


Subject(s)
Glucose/chemistry , Levulinic Acids/chemical synthesis , Silicon Dioxide/chemistry , Sulfates/chemistry , Zirconium/chemistry , Catalysis
3.
Phys Chem Chem Phys ; 8(24): 2893-902, 2006 Jun 28.
Article in English | MEDLINE | ID: mdl-16775645

ABSTRACT

Highly dispersed H(3)PW(12)O(40)/SiO(2) catalysts with loadings between 3.6 and 62.5 wt% have been synthesised and characterised. The formation of a chemically distinct interfacial HPW species is identified by XPS, attributed to pertubation of W atoms within the Keggin cage in direct contact with the SiO(2) surface. EXAFS confirms the Keggin unit remains intact for all loadings, while NH(3) adsorption calorimetery reveals the acid strength >0.14 monolayers of HPW is loading invariant with initial DeltaH(ads) = approximately -164 kJ mol(-1). Lower loading catalysts exhibit weaker acidity which is attributed to an inability of highly dispersed clusters to form crystalline water. For reactions involving non-polar hydrocarbons the interfacial species where the accessible tungstate is highest confer the greatest reactivity, while polar chemistry is favoured by higher loadings which can take advantage of the H(3)PW(12)O(40) pseudo-liquid phase available within supported multilayers.


Subject(s)
Oxides/chemistry , Phosphorus/chemistry , Silicon Dioxide/chemistry , Tungsten/chemistry , Catalysis , Chemical Phenomena , Chemistry, Physical , Molecular Structure , Sensitivity and Specificity , Spectrometry, X-Ray Emission/methods , Temperature
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