Absolute hydrogen determination in coal-derived heavy distillate samples
Organic elemental hydrogen analysis is routinely performed with an automated analyzer having a high temperature combustion zone that is connected to a detector which measures the response of the product water. With the advent of instrumental electronics, automated microanalysis gradually replaced the gravimetric techniques mainly because of increased analysis speed. Modern automated organic elemental analysis consists of combusting the sample in the presence of a solid oxidant and sweeping the products into a thermal conductivity of infrared detector [4,5]. An alternative technique for the detection of hydrogen is to react the product water with carbonyldiimidazole to generate a quantitative amount of carbon dioxide which is measured by a coulometric tritration [6]. The development of Proton Nuclear Magnetic Nuclear Resonance Spectroscopy has led to the description and qualitative classification of hydrogen in organic compounds. These techniques have been especially helpful in describing hydrogen as it is classified into aliphatic, aromatic and hydroaromatic groupings [1,2,3]. In addition, low resolution proton {sup 1}H-NMR has been sucessfully used to determine absolute amounts of hydrogen in a variety of petroleum fractions [7,8]. Our technique involves simple integration of high resolution {sup 1}H-NMR spectra with careful attention given to sample preparation and spectral integration.
- Research Organization:
- Sandia National Labs., Albuquerque, NM (United States)
- Sponsoring Organization:
- USDOE, Washington, DC (United States)
- DOE Contract Number:
- AC04-94AL85000
- OSTI ID:
- 10160225
- Report Number(s):
- SAND-94-1084C; CONF-940813-11; ON: DE94013779; BR: GB0103012
- Resource Relation:
- Conference: 208. American Chemical Society (ACS) national meeting,Washington, DC (United States),21-26 Aug 1994; Other Information: PBD: [1994]
- Country of Publication:
- United States
- Language:
- English
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