Derivatization procedure for gas chromatographic determination of hydroxylamine
Hydroxylamine has been of special interest recently because of the possibilities of manufacturing it by using electrochemical methods in which ammonia might also be formed. Its general chemistry and applications have been described elsewhere. Presently, there are two gas chromatographic methods reported for the determination of hydroxylamine in aqueous media. The first involves reacting the hydroxylamine to form acetone oxime and subsequently injecting the aqueous solution directly into a gas chromatograph equipped with nitrogen and flame ionization detectors. The second involves oxidizing hydroxylamine to nitrous oxide and trapping the gas for determination in an electron capture equipped gas chromatograph. Limits of detection are in the micromolar range for the former and the nanomolar range for the latter. Here, an alternate gas chromatographic procedure for determining hydroxylamine as the acetone oxime is described. Neither direct aqueous injection nor elaborate instrumentation is required. Extraction of the oxime into an ether phase allows for concentrating the analyte ad facilitates the use of an internal standard. The limitations and inconveniences of direct aqueous injection are avoided included column degradation and filament burnout in mass spectrometry detectors.
- Research Organization:
- Univ. of Wisconsin, Madison
- OSTI ID:
- 6804104
- Journal Information:
- Anal. Chem.; (United States), Vol. 59:8
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
10 SYNTHETIC FUELS
ACETONE
SOLVENT EXTRACTION
HYDROXYLAMINE
GAS CHROMATOGRAPHY
OXIMES
EXPERIMENTAL DATA
PH VALUE
QUANTITATIVE CHEMICAL ANALYSIS
AMINES
CHEMICAL ANALYSIS
CHROMATOGRAPHY
DATA
EXTRACTION
HYDROXY COMPOUNDS
INFORMATION
KETONES
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
SEPARATION PROCESSES
400102* - Chemical & Spectral Procedures
090320 - Inorganic Hydrogen Compound Fuels- Preparation- (1976-1989)
400105 - Separation Procedures