The development of liquid and gas chromatographic methods for the determination of water
Two liquid chromatographic (LC) methods and one gas chromatographic (GC) method for the determination of water are developed. In the LC methods, water in various analytical samples is separated from the sample matrices on either a single cation-exchange column or two cation-exchange columns via an ion-exclusion mechanism and determined using spectrophotometric detection. The detection system is based on a shift in the equilibrium between cinnamaldehyde and cinnamaldehyde dimethylacetal in the methanol eluent. The shift in equilibrium is linearly proportional to the amount of water present and occurs only in the presence of an acid catalyst. In the single-column LC method, a short column (2.5 cm {times} 2.1 mm i.d.) packed with cation-exchange resin in the H{sup +} form is used. Under favorable conditions, water in a wide variety of samples can be determined in as little as twenty seconds. A third water determining method is developed that is based on gas chromatographic (GC) technique. The amount of water in analytical samples is determined by reaction with an ortho ester (such as triethylorthoformate), followed by measurement of a product of the reaction by capillary-column GC. A low concentration of methanesulfonic acid is dissolved in the reagent to catalyze the reaction. 86 refs., 37 figs., 11 tabs.
- Research Organization:
- Ames Lab., IA (USA)
- Sponsoring Organization:
- USDOE; USDOE, Washington, DC (USA)
- DOE Contract Number:
- W-7405-ENG-82
- OSTI ID:
- 5619659
- Report Number(s):
- IS-T-1563; ON: DE91014504
- Resource Relation:
- Other Information: Thesis (Ph.D.)
- Country of Publication:
- United States
- Language:
- English
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