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J Chromatogr A ; 1217(3): 348-52, 2010 Jan 15.
Article in English | MEDLINE | ID: mdl-20004902

ABSTRACT

A practical gas chromatographic procedure has been developed and implemented for the measurement of arsine and phosphine in hydrocarbons such as propylene at the part-per-billion level. The successful measurement of arsine and phosphine at the level mentioned was attained by incorporating a large volume injection technique to increase the mass of solutes delivered for sensitivity improvement, capillary flow technology to keep the matrix from entering the detector by either back-flushing through the inlet vent, or by heart-cutting if required, and dielectric barrier discharge detector operating in argon mode for sensitivity enhancement, as well as offering improved selectivity towards the solutes cited. Using the technique described a complete analysis can be conducted in less than 4 min. A relative standard precision of less than 1.7% was achieved with repeated injections at the concentration level of 25 and 125 ppb (v/v) each of arsine and phosphine in nitrogen with a practical detection limit at the 5 ppb (v/v) level. Correlation coefficients of greater than 0.9999 were obtained for arsine and phosphine over a range from 10 to 2500 ppb (v/v). The analytical methodology was proven to be reliable in continuous operation during the first 6 months of deployment.


Subject(s)
Arsenicals/analysis , Chromatography, Gas/methods , Flow Injection Analysis/methods , Hydrocarbons/chemistry , Phosphines/analysis , Alkenes/chemistry , Chromatography, Gas/instrumentation , Flow Injection Analysis/instrumentation , Sensitivity and Specificity
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