Semivolatile organic compounds (SVOCs) are present in many indoor materials. SVOC emissions can be characterized with a critical parameter, y , the gas-phase SVOC concentration in equilibrium with the source material. To reduce the required time and improve the accuracy of existing methods for measuring y , we developed a new method which uses solid-phase microextraction (SPME) to measure the concentration of an SVOC emitted by source material placed in a sealed chamber. Taking one typical indoor SVOC, di-(2-ethylhexyl) phthalate (DEHP), as the example, the experimental time was shortened from several days (even several months) to about 1 day, with relative errors of less than 5%. The measured y values agree well with the results obtained by independent methods. The saturated gas-phase concentration (y ) of DEHP was also measured. Based on the Clausius-Clapeyron equation, a correlation that reveals the effects of temperature, the mass fraction of DEHP in the source material, and y on y was established. The proposed method together with the correlation should be useful in estimating and controlling human exposure to indoor DEHP. The applicability of the present approach for other SVOCs and other SVOC source materials requires further study.