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In this research, gas chromatography/chemical ionization/tandem mass spectrometry, coupled with direct aqueous derivatization, liquid-liquid extraction, and solid-phase extraction techniques, has been optimized for the analysis of selected hydrazines. A procedural calibration technique using an isotopically labeled internal standard was optimized for the analysis of hydrazine. Direct aqueous derivatization with 3,5- dinitrobenzoyl chloride was studied for the analysis of other selected hydrazines. The method accuracy, precision, sensitivity, and matrix effects were studied. Includes abstract only.