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Psychophysiological studies of emotion have typically used static stimuli to elicit emotion (e.g. the International Affective Picture System). This work has shown positive correlations between skin conductance and activation ratings and negative correlations of corrugator electromyograph and pleasantness ratings (Lang, 1995). However, since emotional experience and associated physiological events are dynamic, it remains uncertain whether these same relationships are found over time. The current study examined this issue using music stimuli. Seventeen participants used a LabVIEW -based instrument to rate their emotional experience continuously on a two-dimensional space while listening to ten different instrumental excerpts; skin conductance and corrugator EMG were simultaneously measured. Second-by-second mean skin conductance and root mean square EMG were calculated and then averaged across participants. Cross correlation plots indicated a negative correlation of corrugator EMG and pleasantness for Rimsky-Korsakov’s “Scheherazade;†emotion lagged behind physiology by about eight seconds. Positive correlations between skin conductance and activation were shown for Coltrane’s “Alabama†and Tarrega’s “Gran jota†with no temporal lag between physiology and emotion. Two other excerpts actually produced a negative correlation of skin conductance and activation. Furthermore, time itself had a strong negative correlation with skin conductance (decline over time in all ten excerpts). Separate analyses for individual participants revealed more relationships consistent with the original hypothesis but also many instances of individualized responses to particular excerpts. Thus, averaging across participants obscures many relationships otherwise seen in individual analyses. It appears that skin conductance changes over time are not related so much to emotional activation as to habituation to the novelty of the stimuli.