Nuclear magnetic resonance spectrometry scale

Field desorption mass spectrometry [1606], C nuclear magnetic resonance, and fourier-transform infrared spectroscopy [1337] have been used to characterize oil field chemicals, among them, scale inhibitors. Ion... 

A reevaluation of molecular structure of humic substances based on data obtained primarily from nuclear magnetic resonance spectroscopy, X-ray absorption near-edge structure spectroscopy, electrospray ionization-mass spectrometry, and pyrolysis studies was presented by Sutton and Sposito (2005). The authors consider that humic substances are collections of diverse, relatively low molecular mass components forming dynamic associations stabilized by hydrophobic interactions and hydrogen bonds. These associations are capable of organizing into micellar structures in suitable aqueous environments. Humic components display contrasting molecular motional behavior and may be spatially segregated on a scale of nanometers. Within this new structural context, these components comprise any molecules... 

Several methods are available in the literature for the measurement of aliphatic amines in biological samples [28]. Problems with specificity and separation and cumbersome derivatisation and/or extraction procedures have limited the use of these techniques on a larger scale in clinical practice. The lack of a simple analytical method may have led to an underestimation of the incidence of the fish odour syndrome. For diagnosing the syndrome, an analytical technique should be used that is able to simultaneously and quantitatively measure TMA and its N-oxide in the complex matrix of human urine. Two such methods are currently available for this purpose proton nuclear magnetic resonance (NMR) spectroscopy and head-space gas analysis with gas chromatography or direct mass spectrometry (see below). 

From a medicinal chemist s perspective, nuclear magnetic resonance (NMR) was still the analytical tool of choice, whereas mass spectrometry, infrared (IR), and elemental analyses completed the necessary ensemble of analytical structure confirmation. Synthesis routines were capable of generating several milligrams of product, which is more than adequate for proton and carbon NMR experiments. For analyses that involved natural products, metabolites, or synthetic impurities, time-consuming and often painstaking isolation methods were necessary, followed by expensive scale-up procedures, to obtain the necessary amount of material for an NMR experiment. In situations that involved trace-mixture analysis, radiolabeling approaches were often used in conjunction with various formats of chromatographic separation. 

Although several metal-containing heterocyclic compounds (such as porphyrins, phthalocyanines, naphthenates) are present in oil fractions most of the bench-scale research has been based on relatively rapid Ni, V, or Ni/V deposition procedures in which experimental FCC formulations have been artificially metal contaminated with solutions of Ni and/or V naphthenate dissolved in benzene (or toluene) (24). Metal levels in these novel FCC are usually above 0.5% that is well above the concentration that today exist on equilibrium FCC, see Figure 1. High metal concentration facilitate the study and characterization of Ni and V effects by modern characterization techniques such as X-ray photoelectron spectroscopy (XPS), Laser Raman spectroscopy (LRS), X-ray diffraction (XRD), electron microscopy, secondary ion mass spectrometry (SIMS), and 51V nuclear magnetic resonance (NMR). 

Although the determination of HA or HB selectivity is relatively straightforward the techniques for isolation of pyridine nucleotides from the reaction mixtures are tedious and time consuming. Two more recent techniques use either proton magnetic resonance or electron impact and field desorption mass spectrometry. The technique of Kaplan and colleagues requires a 220 MHz nuclear magnetic resonance spectrometer interfaced with a Fourier transform system [104], It allows the elimination of extensive purification of the pyridine nucleotide, is able to monitor the precise oxidoreduction site at position 4, can be used with crude extracts, and can be scaled down to /nmole quantities of coenzyme. The method can distinguish between [4-2H]NAD+ (no resonance at 8.95 8) and NAD+ (resonance at 8.95—which is preferred) or between [4A-2H]NADH (resonance at 2.67 8, 75 4B = 3.8 Hz) and [4B-2H]NADH (resonance at 2.77 8, J5 4A = 3.1 Hz). 

One possible solution to the above problem is to fractionate the polymer using preparative-scale SEC, then examine the fractions with powerful off-line techniques such as mass spectrometry, Fourier transform infrared and nuclear magnetic resonance. This technique can also be used to isolate pure polymer fractions for subsequent use in SEC calibration. 

Chemists can legitimately ask the question whether the / values of photo-electron signals really give information about the molecule or the solid itself. Many other experimental techniques perturb the electronic structure of the groundstate much less, such as Mossbauer spectrometry, nuclear magnetic or quadrupolar resonance, or to a certain extent vibrational spectra obtained by infra-red or Raman methods. Further on, the time-scale of the other techniques tends to be much longer (22) than 10 17 sec of the photo-electron spectra. 

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