A research program was designed and conducted to define the effect of organics in SSMS and to evaluate several sample preparation methods for their removal. Samples of known organic content were fabricated by diluting NBS SRM 1633 fly ash with a mixture of organic compounds. The SRM 1633 fly ash was spiked with several trace elements prior to this mixing. Samples containing 0. 10, 50, and 90 percent organic material were developed. These fabricated samples and NBS SRM 1632 coal were analyzed by three laboratories using SSMS without prior pretreatment (neat) and after processing by several preparation procedures. The effects of organic material on neat SSMS analysis were assessed for the various concentration levels. Samples containing <50 percent organic material could be successfully analyzed by SSMS without pretreatment. Difficulties were encountered with 90 percent organics. Four preparation procedures (Parr oxygen bomb, HF bomb, low temperature ashing, and mineral acid extraction) were evaluated for removal of organic interference and maintenance of sample integrity for SSMS, AAS (primarily Hg), and ICP analyses. Conclusions were drawn regarding their suitability for use in the Level 1 and/or Level 2 analysis schemes and the benefits of further research.