These analytical methods have been used, sometimes in combination with other analytical methods, in analysis of volatiles from grapefruit (_Citrus paradise_ L.) [24], berry cactus (_Myrtillocatus geometrizans_) [25], Shine Muscat [9], Cabernet Sauvignon [4; 26], Zuoshanyi grapes [14], Muscat cultivars [27], Nero d'Avola and Fiano grapes [28], Monastrell wines [29], and selected cold-hardy grape cultivars and wine [16; 17] and cold-hardy wines [17; 30; 31; 32; 33; 34]. A review of SPME use for in-vivo and in-vitro in whole plant and plant organ analysis is found elsewhere [35]. It is clear that there is little research in cold-hardy wine grape cultivars when compared to _V. vinifera_. There is a need for a better understanding of these new cultivars in order to produce quality cold-climate wines that can compete in the world market. To date, this research is the first report of aroma compounds (1) emitted in-vivo from veraison to harvest using two novel sampling methods and collected by SPME and analyzed by GC-MS from Frontenac, Marquette, St. Croix, and La Crescent grape cultivars. In this research, we propose a novel concept for a non-destructive evaluation of volatiles emitted from ripening grapes using SPME. This concept is novel to both the traditional vinifera grapes and the cold-hardy cultivars. Our models are cold-hardy varieties in the upper Midwest for which many of the basic multiyear grape flavor and wine style data is needed. Research into aroma compounds present in cold-hardy cultivars is essential to the continued growth of the wine industry in cold climates and diversification of agriculture in the upper Midwestern area of the U.S. The need for data is confounded by the small resources available to conduct long-term research. If proven feasible, the concept of non-destructive analysis of ripening grapes presents a tantalizing possibility to investigate the effects of different viticulture practices throughout the stages of berry ripening on berry aroma. This, in turn, could be used to develop better quality wines. If volatile compounds emitted in-vivo could be identified as developmental biomarkers, portable target VOC detectors could then be developed. These detectors can give vineyards a real-time gauge to guide them in harvesting for flavor. The main objective was to develop the proof-of-concept for a non-destructive (in-vivo) sampling of volatile compounds from growing and ripening grapes. Specific objectives (1-4) were to (1) develop sampling devices to capture volatiles emitted from a whole cluster and single berry; (2) characterize the volatile compounds emitted in-vivo from four cold-hardy grape cultivars using: (2i) whole cluster analysis, (2 ii) single berry analysis; (3) compare volatile compounds emitted in-vivo (objective 1) with crushed berry (i.e., destructive analysis including skin, seeds, and pulp); (4) search for preliminary links between volatile compounds detected (objectives 1 and 2) and selected: (4i) microclimates (Iowa and South Dakota), (4 ii) the individual cultivars (i.e., Frontenac, Marquette, St. Croix, and La Crescent), and (4 iii) time stages of berry ripening. The working hypotheses were: (1) aroma compound development from veraison-to-harvest can be detected in-vivo by sampling volatile emissions from ripening grapes (from both a single berry and whole grape cluster) and (2) that the flavor accumulation (i.e., increasing concentration of VOCs) can be correlated with berry ripening in all four cultivars. Testing these hypotheses can potentially translate into improving viticulture practices that lead to timing the harvesting for flavor. This research aims at addressing the gap in knowledge for cold-hardy grape cultivars by cataloging VOCs from Frontenac, Marquette, St. Croix and La Crescent emitted in-vivo and whole crushed berries throughout berry ripening.