A preliminary assessment of environmental volatiles in water using static headspace analysis was performed using the Agilent 7697A Headspace Sampler, Agilent 7890B GC, and the Agilent 5977B GC/MSD system with high efficiency source (HES). The revolutionary design of the HES produces a higher ion currentyield for many compounds (greater sensitivity), which allows flexible approaches to sample analysis such as lowering detection limits, reducing sample size, speeding up analysis, and so forth. Volatile organic analysis (VOA) by static headspace is a widely applied technique, but it is also particularly challenging as the response factors for the many potential analytes vary widely. This application note presents a survey of select compounds of environmental interest as an indication of what may be achieved with the 5977B GC/MSD in this approach. Analysis was performed in selected ion monitoring mode of a mixture of VOA compounds spiked into reverse osmosis (RO) water over a calibration range of 0.0220 g/L. Replicate injections were made at 0.04 g/L to assess the method detection limits (MDL). A study of replicates of local tap water was used to demonstrate long-term stability for some naturally occurring compounds. Agilent 5977B 單四極桿氣質(zhì)聯(lián)用系統(tǒng)GC/MSD