A protocol has been developed to enable source operators to comply with provisions of Title III of the Clean Air Act Amendments of 1990 which allows certain exemptions if reductions in emissions can be demonstrated and validated source emission test methods are not available. Essentially, the procedures consist in determining the method's bias and precision, the former by using known concentrations of analyte, and the latter by means of collocated sampling trains. The use of isotopically-labelled materials, comparisons with a validated method, or analyte spiking are techniques that may be employed. There is a requirement tht the analyst use an EPA audit material. Equations are given to calculate precision, to determine if bias is statistically significant, and to calculate correction factors if applicable. The protocol disallows the use of test methods having a bias greater than 30% or a precision greater than 50% at the level of the applicable standard.