Overcoming the slow oxygen reduction reaction (ORR) kinetics at the cathode of the hydrogen fuel cells requires the use of electrocatalysts containing expensive and scare platinum to achieve reasonable performance, hampering widespread use of the technology due to high material costs and sustainability issues. One option available to tackle this issue is to use new designs to create nanomaterials which achieve excellent electrocatalytic performances and long-lasting stabilities whilst using less platinum than is currently required. Reliably producing nanomaterials with predictable activities and stabilities using simple, safe, and scalable methods is an important research topic to the advancement of fuel cell technologies.
View Article and Find Full Text PDFFormulating pharmaceutical cocrystals as inhalable dosage forms represents a unique niche in effective management of respiratory infections. Favipiravir, a broad-spectrum antiviral drug with potential pharmacological activity against SARS-CoV-2, exhibits a low aqueous solubility. An ultra-high oral dose is essential, causing low patient compliance.
View Article and Find Full Text PDFThe likelihood of finding intact cellular structures on the surface or in the near subsurface of the martian regolith is slim, due in part to the intense bombardment of the surface by ionizing radiation from outer space. Given that this radiation is predicted to be so intense that it would render a living cell inactive within minutes, it is logical to search for evidence of microbial life by looking for molecules produced by the breakdown of cellular matter. This "pool" of molecules, known as biomarkers, consists of a range of species with various functionalities that make them likely to interact with minerals in the martian regolith.
View Article and Find Full Text PDFThe design of a melt synthesis of the first air-stable formulation of the metastable form III of paracetamol is derived from thermo-spectroscopic and thermo-diffraction experiments. Melt crystallisation in the presence of β-1,4-saccharides produces form III selectively and the excipients appear to act as stabilising 'active' templates of the metastable polymorph.
View Article and Find Full Text PDFThree highly porous Zr(iv)-based metal-organic frameworks, UBMOF-8, UBMOF-9, and UBMOF-31, were synthesized by using 2,2'-diamino-4,4'-stilbenedicarboxylic acid, 4,4'-stilbenedicarboxylic acid, and combination of both linkers, respectively. The mixed-linker UBMOF-31 showed excellent hydrogen uptake of 4.9 wt% and high selectivity for adsorption of CO2 over N2 with high thermal stability and moderate water stability with permanent porosity and surface area of 2552 m(2) g(-1).
View Article and Find Full Text PDFActa Crystallogr B Struct Sci Cryst Eng Mater
February 2014
The creation of ternary multi-component crystals through the introduction of 18-crown-6 to direct the hydrogen-bonding motifs of the other molecular components was investigated for 3,5-dinitrobenzoic acid (3,5-dnba) with 4-aminobenzoic acid (4-aba). The creation of a binary complex between 18-crown-6 and 4-aba (C12H24O6·2C7H7NO2)2 and a ternary salt between 3,5-dnba, 18-crown-6 and 4-aba (C12H24O6·C7H8NO2(+)·C7H3N2O6(-)·C7H4N2O6) were confirmed by single-crystal structure determination. In both structures, the amino molecules bind to the crown ether through N-H.
View Article and Find Full Text PDFFour new ternary crystalline molecular complexes have been synthesised from a common 3,5-dinitrobenzoic acid (3,5-dnda) and 4,4'-bipyridine (bipy) pairing with a series of amino-substituted aromatic compounds (4-aminobenzoic acid (4-aba), 4-(N,N-dimethylamino)benzoic acid (4-dmaba), 4-aminosalicylic acid (4-asa) and sulfanilamide (saa)). The ternary crystals were created through the application of complementary charge transfer and hydrogen-bonding interactions. For these systems a dimer was created through a charge-transfer interaction between two of the components, while hydrogen bonding between the third molecule and this dimer completed the construction of the ternary co-crystal.
View Article and Find Full Text PDFGamma-hydroxybutyric acid (GHB) is a drug-of-abuse that has recently become associated with drug-facilitated sexual assault, known as date rape. For this reason the drug is commonly found 'spiked' in alcoholic beverages. When GHB is in solution it may undergo conversion into the corresponding lactone, Gamma-butyrolactone (GBL).
View Article and Find Full Text PDFRaman spectroscopy has proven to be a very effective approach for the detection of microorganisms colonising hostile environments on Earth. The ExoMars rover, due for launch in 2018, will carry a Raman laser spectrometer to analyse samples of the martian subsurface collected by the probe's 2-m drill in a search for similar biosignatures. The martian surface is unprotected from the flux of cosmic rays, an ionising radiation field that will degrade organic molecules and so diminish and distort the detectable Raman signature of potential martian microbial life.
View Article and Find Full Text PDFSpectrochim Acta A Mol Biomol Spectrosc
October 2011
Trace amounts of street samples of cocaine hydrochloride and N-methyl-3,4-methylenedioxy-amphetamine (MDMA) on natural and synthetic textiles were successfully detected in situ using confocal Raman microscopy. The presence of some excipient bands in the spectra of the drugs did not prevent the unambiguous identification of the drugs. Raman spectra of the drugs were readily obtained without significant interference from the fibre substrates.
View Article and Find Full Text PDFCycloaddition of 3-carbomethoxy-2H-pyran-2-one to a vinylated sugar followed by the loss of bridging CO(2) from the cycloadduct affords a cyclohexadiene which can be manipulated to a carbasugar-sugar pseudodisaccharide.
View Article and Find Full Text PDFA general method for the synthesis of a novel class of oligomers, comprising alpha-hydroxy phenylphosphinic acid building blocks, is reported. A series of dimeric alpha-hydroxy phenylphosphinates are analyzed by a combination of NMR spectroscopy, X-ray crystallography and computational methods.
View Article and Find Full Text PDFA general synthetic methodology for the synthesis of sugar-carbasugar pseudodisaccharides is described. The methodology is based on the cycloaddition of pyran-2-ones to vinylated sugars and the subsequent manipulation of the cycloadducts to construct the carbasugar component of the pseudodisaccharide.
View Article and Find Full Text PDFConfocal Raman microscopy is shown to detect picogram quantities of explosives in-situ on undyed natural and synthetic fibres, and coloured textile specimens leaving potentially evidential materials unaltered. Raman spectra were obtained from pentaerythritol tetranitrate (PETN), trinitrotoluene (TNT), and ammonium nitrate particles trapped between the fibres of the specimens. Despite the presence of spectral bands arising from the natural and synthetic polymers and dyed textiles, the explosive substances could be identified by their characteristic Raman bands.
View Article and Find Full Text PDFSpectrochim Acta A Mol Biomol Spectrosc
May 2009
For the manufacture of dosage forms all ingredients must be reliably identified. In this paper, the suitability of FT-NIR spectroscopy to identify potassium sorbate, sodium starch glycollate, calcium ascorbate, calcium carbonate, candelilla wax, maltosextrin, monohydrated and anhydrous lactose inside USP vials was investigated. Differentiation between the anhydrous and monohydrated forms of lactose was found to be possible by studying the regions of the near-infrared spectrum corresponding to the combination and first overtone stretching frequencies of water.
View Article and Find Full Text PDFKnowledge and control of the polymorphic phases of chemical compounds are important aspects of drug development in the pharmaceutical industry. Salmeterol xinafoate, a long acting beta-adrenergic receptor agonist, exists in two polymorphic Forms, I and II. Raman and near infrared spectra were obtained of these polymorphs at selected wavelengths in the range of 488-1064 nm; significant differences in the Raman and near-infrared spectra were apparent and key spectral marker bands have been identified for the vibrational spectroscopic characterisation of the individual polymorphs which were also characterised with X ray diffractometry.
View Article and Find Full Text PDFThis study describes the application of confocal Raman microscopy to the detection and identification of drugs-of-abuse in situ on undyed natural synthetic fibres, and coloured textile specimens. Raman spectra were obtained from drug particles trapped between the fibres of the specimens. Pure samples of cocaine hydrochloride and N-methyl-3,4-methylenedioxy-amphetamine HCl (MDMA-HCl) were used in this study.
View Article and Find Full Text PDFThis study describes the application of Raman spectroscopy to the detection of drugs of abuse and noncontrolled substances used in the adulteration of drugs of abuse on human nail. Contamination of the nail may result from handling or abusing these substances. Raman spectra of pure cocaine hydrochloride, a seized street sample of cocaine hydrochloride (77%), and paracetamol could be acquired from drug crystals on the surface of the nail.
View Article and Find Full Text PDFSpectrochim Acta A Mol Biomol Spectrosc
August 2003
Mosaic gold, tin (IV) sulphide, is a yellow pigment which was known in antiquity but whose use was superseded by other more easily obtainable yellow pigments by the Renaissance. The identification of mosaic gold residues in a burnished golden mirror decoration on a XIIIth Century Spanish polychrome statue is important in that the first reference to the use of mosaic gold in the European literature dates from the XIVth Century, although the use of this material in China had been recorded some time before. In this paper, Raman spectroscopy, XRD and SEM are used in the analysis of the conditions required for the formation of golden mirrors using tin (IV) sulphide in admixture with dilead (II) lead (IV) tetroxide and mercury (II) sulphide.
View Article and Find Full Text PDFTrimethylsilylation of 1,8-diaminonaphthalene gave 1,8-bis(trimethylsilylamino)naphthalene (1 a), which was in turn lithiated with two molar equivalents of n-butyllithium to give the tris(thf)-solvated dilithium diamide [1,8-[(Me(3)SiN)Li(thf)](2)C(10)H(6)](thf) (2 a). Metal exchange of 2 a with TlCl was carried out in two steps, via the previously characterized mixed-metal amide [1-[(Me(3)SiN)Li(thf)(2)]-8-[(Me(3)SiN)Tl]C(10)H(6)], to give the dithallium diamide [1,8-[(Me(3)SiN)Tl](2)C(10)H(6)] (3 a). Thermolysis of 3 a cleanly gave a 1:1 mixture of the 4,9-bis(trimethylsilylamino)perylenequinone-3,10-bis(trimethylsilylimine) (4 a) and 1 a.
View Article and Find Full Text PDFThe reaction of [MeSi{Me(2)SiN(Li)(p-tol)}(3)(Et(2)O)(2)] with SnCl(2) in a 1:1 molar ratio leads the tris(amido)stannate [MeSi{Me(2)SiN(p-tol)}(3)SnLi(Et(2)O)] (1), which further reacts with neutral [AuCl(PPh(3))] and anionic [PPN][AuCl(2)], PPN[AuRCl] (R = C(6)F(5), mes), and chlorogold(I) complexes yielding [Au(MeSi{Me(2)SiN(p-tol)}(3)Sn)(PPh(3))] (2) and [PPN][Au(MeSi{Me(2)SiN(p-tol)}(3)Sn)(2)] (3) and [Au(MeSi{Me(2)SiN(p-tol)}(3)Sn)(R)] (R = C(6)F(5), 4; R = mes, 5), respectively. The reaction of 1 with the dinuclear gold(II) derivative [Au(2)(CH(2)PPh(2)CH(2))(2)Cl(2)] in a 1:2 ratio affords [Au(2)(CH(2)PPh(2)CH(2))(2)(MeSi{Me(2)SiN(p-tol)}(3)Sn)(2)] (6). In a similar way but starting from PPN[Au(C(6)F(5))(3)Cl] and reacting with 1 in a 1:1 ratio, the Au(III) complex [PPN][Au(MeSi{Me(2)SiN(p-tol)}(3)Sn)(C(6)F(5))(3)] (7) has been obtained.
View Article and Find Full Text PDFThe stabilization of unsupported Ti-M (M = Fe, Ru, Co) heterodinuclear complexes has been achieved by use of amidotitanium building blocks containing tripodal amido ligands. Salt metathesis of H(3)CC(CH(2)NSiMe(3))(3)TiX (1) and C(6)H(5)C(CH(2)NSiMe(3))(3)TiX (2) as well as HC{SiMe(2)N(4-CH(3)C(6)H(4))}(3)TiX (3) (X = Cl, a; Br, b) with K[M(CO)(2)Cp] (M = Fe, Ru) and Na[Co(CO)(3)(PR(3))] (R = Ph, Tol) gave the corresponding stable heterobimetallic complexes of which H(3)CC(CH(2)NSiMe(3))(3)Ti-M(CO)(2)Cp (M = Fe, 6; Ru, 7) and HC{SiMe(2)N(4-CH(3)C(6)H(4))}(3)Ti-M(CO)(2)Cp (M = Fe, 12; Ru, 13) have been characterized by X-ray crystallography. 6: monoclinic, P2(1)/n, a = 15.
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