Detector nuclear magnetic resonance

J. F. Haw, T. E. Glass, D. W. Hausler, E. Motell, and H. C. Dorn, Direct coupling of a liquid chromatograph to a continuous flow hydrogen nuclear magnetic resonance detector for analysis of petroleum and synthetic fuels. And. Chem. 52 (1980), 1135-1140. 

Other detectors, such as the flame ionization detector, atomic emission detector, Eourier transform infrared spectrometer and nuclear magnetic resonance detectors, have been used in GC for the... 

Initially, simple methods such as ultraviolet-visible (UV-Vis), fluorescence or infrared (IR) spectroscopy were proposed in order to estimate the total amount of antioxidants in various food samples. However, coupled methods such as gas chromatography-mass spectrometry (GC-MS), high performance liquid chromatography with ultraviolet-visible (HPLC-UV-Vis) or nuclear magnetic resonance detector (HPLC-NMR) and liquid chromatography-mass spectrometry (LC-MS) are employed more to quantify individual tocols or carotens from various corn-based food samples. In this chapter all these methods of analysis will be briefly described. 

The most common detectors in HPLC are ultraviolet, fluorescence, electrochemical detector and diffractometer. However, despite all improvements of these techniques it seems necessary to have a more selectivity and sensitivity detector for the purposes of the medical analysis. It should be therefore improvements to couple analytical techniques like infrared IR, MS, nuclear magnetic resonance (NMR), inductively coupled plasma-MS (ICP-MS) or biospecific detectors to the LC-system and many efforts have been made in this field. 

D2O = deutered water. HPLC = high performance liquid chromatography. IS = internal standard. MeOH = methanol. MS = mass spectrometry. NMR = nuclear magnetic resonance. PDA = photodiode array detector. TEA = triethylamine. MTBE = methyl tert-butyl ether. 

Perhaps the most revolutionary development has been the application of on-line mass spectroscopic detection for compositional analysis. Polymer composition can be inferred from column retention time or from viscometric and other indirect detection methods, but mass spectroscopy has reduced much of the ambiguity associated with that process. Quantitation of end groups and of co-polymer composition can now be accomplished directly through mass spectroscopy. Mass spectroscopy is particularly well suited as an on-line GPC technique, since common GPC solvents interfere with other on-line detectors, including UV-VIS absorbance, nuclear magnetic resonance and infrared spectroscopic detectors. By contrast, common GPC solvents are readily adaptable to mass spectroscopic interfaces. No detection technique offers a combination of universality of analyte detection, specificity of information, and ease of use comparable to that of mass spectroscopy. 

The basic instrumentation used for spectrometric measurements has already been described in Chapter 7 (p. 277). The natures of sources, monochromators, detectors, and sample cells required for molecular absorption techniques are summarized in Table 9.1. The principal difference between instrumentation for atomic emission and molecular absorption spectrometry is in the need for a separate source of radiation for the latter. In the infrared, visible and ultraviolet regions, white sources are used, i.e. the energy or frequency range of the source covers most or all of the relevant portion of the spectrum. In contrast, nuclear magnetic resonance spectrometers employ a narrow waveband radio-frequency transmitter, a tuned detector and no monochromator. 

Nuclear magnetic resonance and mass spectrometric detectors HPLC/NMR and HPLC/MS are popular techniques that combine the versatility of HPLC with the identification power of NMR or MS (see Chapters 11, 12, and 18). 

Non-specific sum parameter analysis [12,13], which is still used today, failed [14,15] in the analyses of some of these compounds. Chromatographic methods in combination with non-substance specific detectors, e.g. colorimetric and photometric [5] or with substance specific detectors such as IR (infrared spectroscopy), NMR (nuclear magnetic resonance spectroscopy) or MS (mass spectrometry), are applied increasingly nowadays. 

The recent improvements in the nuclear magnetic resonance (NMR) instrumentation allow its application as detectors in polymer HPLC [258,259,307], Modem NMR techniques namely work with the decreased sample concentrations and enable the application of eluents acceptable for polymer HPLC. 

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