A method is described for the modification and use of a gas chromatograph heated inlet for the preparation of trace vapor reference standards. A conventional GC-MS is used to validate the prepared vapor standards and an evaluation is provided on the reproducibility of replicate measurements made from a single sample as well as individual measurements made between replicate samples. The described method is applied to the preparation of single component trace organic vapors, complex vapor mixtures (containing >10 components over a concentration range spanning four orders of magnitude), and low vapor pressure analytes, which are solids under ambient conditions (e.g., ferrocene). Results demonstrate delivery of picomole quantities of single component organic vapors with a reproducibility of ca. 1% RSD.