Nuclear magnetic resonance spectroscopy sample preparation

Page RC, Moore JD, Nguyen HB, Shatma M, Chase R, Gao FP, Mobley CK, Sanders CR, Ma L, Sonnichsen FD, Lee S, Howell SC, Opella SJ, Cross TA (2006) Comprehensive evaluation of solution nuclear magnetic resonance spectroscopy sample preparation for helical integral membrane proteins. J Struct Funct Genomics 7 51-64... 

Other methods of identification include the customary preparation of derivatives, comparisons with authentic substances whenever possible, and periodate oxidation. Lately, the application of nuclear magnetic resonance spectroscopy has provided an elegant approach to the elucidation of structures and stereochemistry of various deoxy sugars (18). Microcell techniques can provide a spectrum on 5-6 mg. of sample. The practicing chemist is frequently confronted with the problem of having on hand a few milligrams of a product whose structure is unknown. It is especially in such instances that a full appreciation of the functions of mass spectrometry can be developed. 

To detect dynamic featnres of colloidal preparations, additional methods are required. Nuclear magnetic resonance spectroscopy allows a rapid, repeatable, and noninvasive measurement of the physical parameters of lipid matrices withont sample preparation (e.g., dilution of the probe) [26,27]. Decreased lipid mobility resnlts in a remarkable broadening of the signals of lipid protons, which allows the differentiation of SLN and supercooled melts. Because of the different chemical shifts, it is possible to attribute the nuclear magnetic resonance signal to particnlar molecnles or their segments. 

Like infrared spectroscopy, specific test methods for recording the nuclear magnetic resonance spectroscopy of coal do not exist. It is necessary, therefore, to adapt other methods to the task at hand, provided that the necessary sample preparation protocols and instrumental protocols for recording magnetic resonance spectra are followed to the letter as proposed and described for infrared spectroscopy (Section 9.1). 

Exploring various phenomena at metal/solution interfaces relates directly to heterogeneous catalysis and its applications to fuel cell catalysis. By the late 1980s, electrochemical nuclear magnetic resonance spectroscopy (EC-NMR) was introduced as a new technique for electrochemical smface science. (See also recent reviews and some representative references covering NMR efforts in gas phase surface science. ) It has been demonstrated that electrochemical nuclear magnetic resonance (EC-NMR) is a local surface and bulk nanoparticle probe that combines solid-state, or frequently metal NMR with electrochemistry. Experiments can be performed either under direct in situ potentiostatic control, or with samples prepared in a separate electrochemical cell, where the potential is both known and constant. Among several virtues, EC-NMR provides an electron-density level description of electrochemical interfaces based on the Eermi level local densities of states (Ef-LDOS). Work to date has been predominantly conducted with C and PtNMR, since these nuclei... 

Nuclear Magnetic Resonance Spectroscopy. Like IR spectroscopy, NMR spectroscopy requires little sample preparation, and provides extremely detailed information on the composition of many resins. The only limitation is that the sample must be soluble in a deuterated solvent (e.g., deuterated chloroform, tetrahydro-furan, dimethylformamide). Commercial pulse Fourier transform NMR spectrometers with superconducting magnets (field strength 4-14 Tesla) allow routine measurement of high-resolution H- and C-NMR spectra. Two-dimensional NMR techniques and other multipulse techniques (e.g., distortionless enhancement of polarization transfer, DEPT) can also be used [10.16]. These methods are employed to analyze complicated structures. C-NMR spectroscopy is particularly suitable for the qualitative analysis of individual resins in binders, quantiative evaluations are more readily obtained by H-NMR spectroscopy. Comprehensive information on NMR measurements and the assignment of the resonance lines are given in the literature, e.g., for branched polyesters [10.17], alkyd resins [10.18], polyacrylates [10.19], polyurethane elastomers [10.20], fatty acids [10.21], cycloaliphatic diisocyanates [10.22], and epoxy resins [10.23]. 

Abstract Stereocomplexes have been formed by mixing the two isotactic poly(a-methyl-a-cthyl-p-propriolactones) (PMEPL) of opposite chirality. This leads to an insoluble complex exhibiting a melting transition which is 40 C above that of the initial isotactic components. Structural differences between these samples have been determined by nuclear magnetic resonance spectroscopy and electron diffraction. It was found by NMR that the stereocomplex crystallizes in a 2 helical conformation whereas the corresponding isotactic chains exhibit a helical or extended chain conformation depending upon the method of sample preparation. Electron diffraction confirms these measurements with the determination of a,b and c dimensions of the orthorombic unit cells. 

Sample Handling. Forensic Sciences Blood Analysis Explosives Systematic Drug Identification. Nuclear Magnetic Resonance Spectroscopy Techniques Nuclear Overhauser Effect. Pharmaceutical Analysis Drug Purity Determination Sample Preparation. 

Combining separation and analysis techniques (hyphenated techniques) can produce powerful tools for chtiracteriz-ing viscous oils. Thus, liquid chromatography or gas chromatography can be used to separate a sample for subsequent characterization by mass spectrometry (LC/MS or GC/MS). Research into suitable methods for the analysis of viscous oils is underway, but no standard tests have yet been prepared. Extensive research on both proton and carbon-13 nuclear magnetic resonance spectroscopy shows promise as a tool for the analysis of lubricant base oils and other viscous oils. Both near-infrared spectroscopy (NIR) and Fourier-transform IR (FTIR) are the subjects of active research into methods to characterize hydrocarbons and for quality control during production of petroleum products. Standard test methods using these techniques should become available in the future. 

Modern spectroscopy plays an important role in pharmaceutical analysis. Historically, spectroscopic techniques such as infrared (IR), nuclear magnetic resonance (NMR), and mass spectrometry (MS) were used primarily for characterization of drug substances and structure elucidation of synthetic impurities and degradation products. Because of the limitation in specificity (spectral and chemical interference) and sensitivity, spectroscopy alone has assumed a much less important role than chromatographic techniques in quantitative analytical applications. However, spectroscopy offers the significant advantages of simple sample preparation and expeditious operation. 

GC and GC-MS (see Chapter 2), are ideal for the separation and characterization of individual molecular species. Characterization generally relies on the principle of chemotaxonomy, where the presence of a specific compound or distribution of compounds in the ancient sample is matched with its presence in a contemporary authentic substance. The use of such 6molecular markers is not without its problems, since many compounds are widely distributed in a range of materials, and the composition of ancient samples may have been altered significantly during preparation, use and subsequent burial. Other spectroscopic techniques offer valuable complementary information. For example, infrared (IR) spectroscopy and 13C nuclear magnetic resonance (NMR) spectroscopy have also been applied. 

Powdering, or grinding, of samples is a simple preparation method required in a number of spectrometric and spectroscopic techniques, such as x-ray diffraction (XRD), nuclear magnetic resonance (NMR), differential thermal analysis (DTA), thermogravimetric analysis (TG), or ATR-FTIR spectroscopy. Control of the particle size during grinding must be taken into account in attempting to obtain reliable results. 

Mass spectrometry (MS), infrared (IR) spectroscopy, and nuclear magnetic resonance (NMR) spectroscopy with their numerous applications are the main instrumental techniques for the detection and identification of CWC-related chemicals. During the last few years, however, less laborious techniques such as liquid chromatography (LC) and capillary electrophoresis (CE) have become attractive for the analysis of water samples and extracts where sample preparation is either not required or is relatively simple. 

Keywords Carotenoids analysis sample preparation UV/Visible spectroscopy geometrical isomers optical isomers HPLC mass spectrometry nuclear magnetic resonance metabolites. 

High-resolution nuclear magnetic resonance (NMR) spectroscopy is a relatively rapid technique and is highly robust in terms of reproducibility of results. The ubiquity of protons in cellular metabolites and the fact that other nuclei are observable by NMR (e.g., and mean that a relatively large number of different metabolites can be detected. Furthermore, the technique requires minimal sample preparation, and its nondestructive nature allows for more analyses to be... 

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