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Volume 18, Issue 2
(March 1990)
ISSN: 0090-3973
Development of Analytical Methodology and a Report on Collaborative Study on the Determination of Morpholine, Cyclohexylamine, and Diethylaminoethanol in Aqueous Samples by Direct Aqueous Injection Gas Chromatography A direct aqueous injection gas chromatographic procedure for the determination of morpholine, cyclohexylamine, and diethylaminoethanol has been developed. The method employs graphitized carbon B (60 to 80 mesh) coated with 4.8% polyethylene glycol 20 M + 0.4% potassium hydroxide and a flame ionization detection system. The detection limits (3 × signal-to-noise ratio) for morpholine, cyclohexylamine, and diethylaminoethanol were 55 ng, 52 ng, and 53 ng, respectively. Five spiked samples containing the three amines in concentrations ranging from 0.5 to 3.0 mg/mL after appropriate dilution have been analyzed by six laboratories. A duplicate of one concentration level has been separately spiked with 50 ppm of iron salts to study the influence of iron salts on the analytical technique. Statistical treatment complementary to that outlined in ASTM D 2777-86 was applied. Significant biases were observed at some spike levels for morpholine and cyclohexylamine; bias changes were not consistent with increasing concentration. No significant biases were noted for diethylaminoethanol. There was no evidence of interlaboratory variations for any concentrations of morpholine. Significant interlaboratory variability was observed for some concentrations of cyclohexylamine and diethylaminoethanol. Further, the presence of iron salts shows negligible influence on the analytical technique for the three amines.
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Paper ID: JTE12458J | ||
