The report gives preliminary data on methodology for two groups of compounds: organometallics and other organic compounds difficult to measure by the generalized methods. Previous work (Contract 68-02-2685, Task 111, and Task 1 of this contract) involved the evaluation of generalized GC/FID, GC/MS, and HPLC/UV methods for determining approximately 170 compounds from the approximately 400 compounds in Appendix VIII, Part 261, 40 CFR. However, the survey analysis portion of waste characterization often targets specific compounds for determination in incinerator effluent that are not amenable to previously developed methods. Therefore current research involves the development of specific GC/FID, GC/MS, and HPLC/UV methods for the determination of several of these compounds. Organometallic compounds such as benzenearsonic acid, hydroxydimethylarsine oxide (cacodylic acid), phenylmercury acetate, selenourea, and tetraethyl lead were selected as candidate POHCs for this study. In support of the destruction and removal efficiency requirement, generalized GC/FID, GC/MS, and HPLC/UV analysis methods were evaluated and, when necessary, modified for the detemiination of 33 additional candidate POHCs.