Solvent liquid chromatography-nuclear magnetic

J. F. Haw, T. E. Glass, and H. C. Dorn, Analysis of coal conversion recycle solvent by liquid chromatography with nuclear magnetic resonance detection. Anal. Chem. 53 (1981), 2332-2336. 

The analysis of CAD and alkamides has been completed using a variety of analytical techniques that include high-performance liquid chromatography (HPLC), capillary electrophoresis, gas chromatography (GC), GC-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), and nuclear magnetic resonance (NMR). Sample preparation methodologies utilize hexane, methanol and ethanol as the primary extraction solvents. 

Attempts to optimize the yield were unsuccessful. The main parameters affecting the yield of the Fischer indole reaction are the added acid (AcOH > TFA > HCl > H2SO4) as well as the solvent composition, hi pure water, no reaction was observed, whereas in pure acetic acid, we mainly observed the degradation of the 4-methylhydrazine as evidenced by hydrogen nuclear magnetic resonance ( H NMR) and high-performance liquid chromatography (HPLC) analysis. The best compromise was to perform the Fischer indole reaction in a 75/25 ACOH/H2O mixture at 80°C (Table 6.1). 

Instmmental methods of analysis provide information about the specific composition and purity of the amines. Qualitative information about the identity of the product (functional groups present) and quantitative analysis (amount of various components such as nitrile, amide, acid, and determination of unsaturation) can be obtained by infrared analysis. Gas chromatography (gc), with a liquid phase of either Apiezon grease or Carbowax, and high performance Hquid chromatography (hplc), using silica columns and solvent systems such as isooctane, methyl tert-huty ether, tetrahydrofiiran, and methanol, are used for quantitative analysis of fatty amine mixtures. Nuclear magnetic resonance spectroscopy (nmr), both proton ( H) and carbon-13 ( C), which can be used for qualitative and quantitative analysis, is an important method used to analyze fatty amines (8,81). 

See also-. Extraction Solvent Extraction Principles. Gas Chromatography Mass Spectrometry High-Temperature Techniques. Liquid Chromatography Normal Phase Reversed Phase Liquid Chromatography-Mass Spectrometry. Nuclear Magnetic Resonance Spectroscopy - Applicable Elements Nitrogen-15. 

See also Extraction Solvent Extraction Principles. Infrared Spectroscopy Overview. Ion Exchange Overview Principles. Liquid Chromatography Overview Column Technology Normal Phase Reversed Phase. Nuclear Magnetic Resonance Spectroscopy-Applicable Elements Phosphorus-31. Thin-Layer Chromatography Overview. 

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