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This method is for determining trace arsine and phosphine in high purity polymer grade ethylene and propylene gas or liquid using a gas chromatograph equipped with a mass spectrometer run in selected ion monitoring mode. The specific instrument is preconfigured and is capable of determining typical impurities in polymer grade ethylene or propylene, however this method only outlines the procedure for determining arsine and phosphine. Arsine and phosphine are readily extracted as unique ions with selected ion monitoring. The lower limit of quantitation for arsine and phosphine is 0.02 mol-ppm and 0.20 mol-ppm respectively.