Oil shale retort water ammonia determination by titrimetry, phenate colorimetry, enzymatic analysis, and chromatographic fractionation/chemiluminescence

Journal Article · Sun Jun 01 00:00:00 EDT 1986 · Anal. Chem.; (United States)

DOI:https://doi.org/10.1021/ac00298a064· OSTI ID:5596532

Daughton, C G; Sakaji, R H; Langlois, G W

A statistical comparison was made of three modified standard methods and a new rapid estimator for determining ammoniac-N in oil shale retort waters. The modified standard methods were (1) distillation/acidimetric titration (automated), (2) phenate colorimetry, and (3) glutamate dehydrogenase enzymatic analysis. The fourth method, reverse-phase fractionation-combustion/chemiluminescence (RPF-C/Cl), used a reverse-phase chromatographic technique to separate polar from nonpolar nitrogenous compounds; combustion/chemiluminescence was then used to determine total-N in the polar fraction as a rapid estimate of ammoniac-N. Ammoniac-N for 12 retort waters ranged from 1 to 33 g/L. Precision was best for the titrimetric and colorimetric methods (relative standard deviations < 1.0%). For all waters, the colorimetric and RPF-C/CL methods yielded the lowest and highest concentrations, respectively. Paired comparisons and a sequentially rejective multiple test procedure showed that each pair of methods (with one exception) gave significantly different results for a majority of waters; none of the paired methods, however, gave significantly different results for a composite sample that comprised each of 12 waters. Fisher's test for combining probability values from independent significance tests showed no significant difference (P > 0.01) across all waters only when titrimetry was compared with enzymatic analysis. The RPF-C/CL method gave the most rapid estimate of ammonia and would be useful for spot monitoring or range finding for the other methods.

• Research Organization: Univ. of California (Berkeley), Richmond
• DOE Contract Number: AC03-76SF00098
• OSTI ID: 5596532
• Journal Information: Anal. Chem.; (United States), Vol. 58:7, Issue 7
• Country of Publication: United States
• Language: English

Related Subjects

04 OIL SHALES AND TAR SANDS
37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
AMMONIA
CHEMILUMINESCENCE
DISTILLATION
TITRATION
OIL SHALES
QUANTITATIVE CHEMICAL ANALYSIS
WASTE WATER
COMPARATIVE EVALUATIONS
EXPERIMENTAL DATA
RETORTING
BITUMINOUS MATERIALS
CARBONACEOUS MATERIALS
CHEMICAL ANALYSIS
CHEMICAL REACTIONS
DATA
DECOMPOSITION
ENERGY SOURCES
FOSSIL FUELS
FUELS
HYDRIDES
HYDROGEN COMPOUNDS
INFORMATION
LIQUID WASTES
LUMINESCENCE
MATERIALS
NITROGEN COMPOUNDS
NITROGEN HYDRIDES
NUMERICAL DATA
OXYGEN COMPOUNDS
SEPARATION PROCESSES
WASTES
WATER
040500* - Oil Shales &amp; Tar Sands- Properties &amp; Composition
400105 - Separation Procedures
400104 - Spectral Procedures- (-1987)
400102 - Chemical &amp; Spectral Procedures