Chromatographic NMR spectroscopy: the effect of hollow silica microspheres on magnetic field inhomogeneities and resonance lineshapes

2020 ◽  
Vol 22 (37) ◽  
pp. 21383-21392
Author(s):  
Federico De Biasi ◽  
Federico Moro ◽  
Diego Frezzato ◽  
Federico Rastrelli

We provide a description of the line broadening phenomenon observed in chromatographic NMR spectra with hollow silica microspheres.

1996 ◽  
Vol 74 (10) ◽  
pp. 1889-1895 ◽  
Author(s):  
Christopher Milne ◽  
John Milne

The oxidation of thiocyanic acid by selenous acid has been shown to take place in an analogous way to that found for selenous acid oxidation of most thiols and thiolates to give the corresponding selenotrisulfide and disulfide products[Formula: see text]The products of this reaction have been studied by IR, Raman, and Se-77, C-13, and N-15 NMR spectroscopy. The vibrational spectra of the solid Se(SCN)2 have been assigned based on S-bonded thiocyanate ligands and, through NMR and vibrational spectroscopy, both this linkage isomer and the isomer with N- and S-bonded thiocyanate have been identified and characterized in solutions of Se(SCN)2. A complex combination of scalar relaxation processes, involving chemical exchange and quadrupolar effects, accounts for the line broadening observed in the carbon-13 NMR spectra. Key words: selenite, thiocyanate, selenium dithiocyanate, Se-77, N-15, and C-13 NMR; Raman spectroscopy; linkage isomerism


2001 ◽  
Vol 79 (10) ◽  
pp. 1477-1482 ◽  
Author(s):  
Craig Anderson

2-Methylimidazole (2-MeIm) reacts with RuCl3 in aqueous acidic ethanolic medium to give (2-MeImH)2[RuCl5(2-MeIm)] (1) and (2-MeImH)[RuCl4(2-MeIm)2] (2) (2-MeImH = protonated 2-methylimidazole), the ratio depending on reaction conditions used. Molecule 1 crystallizes in the space group Pnma: a = 14.046(2), b = 17.294(2), and c = 8.2778(12) Å. The 1H NMR spectra of these ruthenium(III) complexes have been measured and show peaks with large isotropic shifts and large line broadening characteristic of such paramagnetic complexes. The aquation of complexes 1 and 2 were followed by proton NMR spectroscopy. 1,2-Dimethyl imidazole (1,2-diMeIm) reacts with RuCl3 in methanolic solution to give [RuCl3(1,2-diMeIm)(H2O)S] (S=H2O (3a) or CH3OH (3b)). The aquation reactions of complexes 3a and 3b were followed by 1H NMR.Key words: ruthenium, paramagnetic, antitumour, NMR.


1989 ◽  
Vol 54 (7) ◽  
pp. 1854-1869 ◽  
Author(s):  
Marián Schwarz ◽  
Petr Trška ◽  
Josef Kuthan

The 1H, 13C and 19F NMR spectra of photochromic p-substituted 2,4,4,6-tetraphenyl-1,4-dihydropyridines IIa-IIg, 1-methyl-2,4,4,6-tetraphenyl-1,4-dihydropyridines IIIa-IIIg, 2,4,4,6-tetraphenyl-4H-pyrans IVa-IVh, and 2,4,4,6-tetraphenyl-4H-thiopyran V were inspected; it was found that compounds IIa-IIg occur in a dynamic equilibrium with their dihydro tautomer VIa-VIg. Also deuteriodeprotonation of IIa and IIIa and their reaction with trifluoroacetic acid were investigated by NMR spectroscopy.


1997 ◽  
Vol 62 (5) ◽  
pp. 746-751 ◽  
Author(s):  
Andreas Franken ◽  
Jaromír Plešek ◽  
Christiane Nachtigal

On treatment of the [(1,2-C2B9H11)2Co]- ion with naphthalene in presence of AlCl3 a remarkably bridged [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- ion is obtained as a single isolated compound. The triatomic -CH2-C9H6- bridge is derived from the rearranged naphthalene nucleus. The mechanism of this reaction is obscure but it does resemble the "Electrophile-Induced Nucleophilic Substitution" reported earlier. The structure of the compound was established by multinuclear NMR spectroscopy and by single crystal X-ray diffraction.


1991 ◽  
Vol 56 (9) ◽  
pp. 1908-1915 ◽  
Author(s):  
Jaroslav Holeček ◽  
Antonín Lyčka ◽  
Milan Nádvorník ◽  
Karel Handlíř

Infrared spectroscopy and multinuclear (13C, 17O, and 119Sn NMR spectroscopy have been used to study the structure of bis(1-butyl)tin(IV) carboxylates of dicarboxylic acids (1-C4H9)2. Sn(X(COO)2), where X = (CH2)n (n = 0-8), CH=CH (cis and trans) and C6H4 (ortho and para).The crystalline compounds are formed by linear or cyclic oligomers or polymers whose basic building units represent a grouping composed of the central tin atom substituted by two 1-butyl groups and coordinated with both oxygen atoms of two anisobidentate carboxylic groups derived from different molecules of a dicarboxylic acid. The environment of the tin atom has a shape of a trapezoidal bipyramid. When dissolvet in non-coordinating solvents, the compounds retain the oligomeric character with unchanged structure of environment of the central tin atom. In the media of coordinating solvents the bis(1-butyl)tin(IV) carboxylates of dicarboxylic acids form complexes whose central hexacoordinated tin atom binds two molecules of the solvent trough their donor atoms. Carboxylic groups form monodenate linkages in these complexes.


Author(s):  
Anagha Sasikumar ◽  
Anouar Belhboub ◽  
Camille Bacon ◽  
Alexander C. Forse ◽  
John Griffin ◽  
...  

In situ NMR spectroscopy is a powerful technique to investigate charge storage mechanisms in carbon-based supercapacitors thanks to its ability to distinguish ionic and molecular species adsorbed in the porous...


2006 ◽  
Vol 182 (2) ◽  
pp. 343-347 ◽  
Author(s):  
Jeremy N. Robinson ◽  
Andrew Coy ◽  
Robin Dykstra ◽  
Craig D. Eccles ◽  
Mark W. Hunter ◽  
...  

2012 ◽  
Vol 159 ◽  
pp. 119-125 ◽  
Author(s):  
Pavel Kovačík ◽  
Zuzana Kremláčková ◽  
František Štěpánek

2005 ◽  
Vol 340 (7) ◽  
pp. 1343-1350 ◽  
Author(s):  
Yasuko Ishizuka ◽  
Kenji Takasugi ◽  
Yu Tsutsumi ◽  
Kenji Kanazawa ◽  
Tadashi Nemoto ◽  
...  

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