Despite several decades of study, the source(s) of gold and mineralizing fluids, and the mechanisms responsible for gold precipitation remain controversial. In particular, there is a need to improve: (i) the identification of secondary gold upgrading processes that lead to very highgrade gold zones; (ii) the understanding of precipitation mechanisms in carbonaceous material (CM)-bearing metasedimentary systems (i.e., slate belts); and (iii) the exploration criteria for the cryptic, finely disseminated gold mineralization in CM-bearing metamudstone lithologies. The combined results of an extensive in situ microanalytical protocol (SEM, confocal Raman microspectroscopy, microthermometry, decrepitate mound analysis, LA-ICP-MS, cathodoluminescence, SIMS) has idenitified evidence of secondary gold enrichment at the Madrid deposit, Hope Bay Greenstone Belt, NU, Canada, resulting from the addition of new gold onto an earlier orogenic quartz-carbonate vein deposit by magmatic-hydrothermal fluids. This conclusion is based on robust textural, mineralogical, and fluid inclusion evidence. The geological setting and mineral-chemical features suggest an intrusion-related (i.e., porphyry), or intermediate-sulfidation epithermal mineralization style for the later event. This work provides another example of the importance of compositionally distinct cumulative hydrothermal events in the development of high-grade gold deposits in orogenic settings. The Dufferin deposit, NS, Canada, is a vein-type system hosted in CM-bearing metasedimentary rocks. A detailed fluid inclusion study strongly suggests that Au mineralization occurred through coupled fluid fO2 reduction (via interaction with CM) and pH increase, leading to efficient Au precipitation from an Au-undersaturated aqueous-carbonic fluid. This study presents one of the few examples of measured Au concentrations in ore fluids in an economic orogenic Au deposit and reports direct evidence for the genetic relationship between Au and CM in metasedimentary lithologies. The results of this study show that, despite mineralizing fluids being Auundersaturated, they may still produce economic deposits through highly efficient precipitation processes. The Moose Rive anticline, NS, Canada, hosts a number of, commonly inconspicuous, metasediment-hosted disseminated Au deposits. An initial study using an on-line, rock-crushing gas chromatographic technique identified bulk fluid differences (CO2 and hydrocarbon abundances) between gold-bearing and gold-barren parcels of metasedimentary rock. This work suggests that bulk fluid characteristics may be a viable exploration vector for disseminated gold systems.