The Qiyugou district is one of the most important gold deposit distribution areas in the Xiong'ershan region, North China Craton. These deposits are hosted in Archean Taihua Supergroup rocks as gold-bearing breccia pipes. Here, we report a detailed in situ analysis of trace elements and S-Pb isotopes in sulfides from different ore stages, in combination with electron probe microanalysis of ore minerals from the gold-bearing J4 breccia pipe in the Qiyugou district, to unravel the gold distribution and their textural relationships to pyrite, the metal sources and S-Pb isotopic composition variations during the ore-forming processes. The Qiyugou breccia pipes hosted gold ore (over 70 t Au, average grade of 2-5 g/t) that formed in four mineralization stages, i.e., an early K-feldspar-biotite-magnetite-quartz-pyrite (Py-1) stage (I) that can be further divided into two substages, namely the Ia K-feldspar-biotite-magnetite stage and the Ib quartz-pyrite stage; a gold-pyrite (Py-2)-quartz stage (II); a gold-quartz-polymetallic sulfide (Py-3) stage (III); and a late quartz-carbonate stage (IV). The visible native gold and electrum grains occur as small inclusions and disseminations in the fractures within Py-2 and Py-3. Tellurides and Bi-Pb-minerals are widespread in the stage II stockworks and veins, as is intergrowth with visible native gold and Py-2. In situ LA-ICP-MS trace element analysis reveals the presence of invisible gold hosted in three types of pyrite with extremely low Au content (Py-1 <= 0.05 ppm; Py-2 <= 0.03 ppm; Py-3 <= 0.02 ppm). Concentrations of Te, Bi, and Pb in pyrite are high and correlate well with Au concentrations, but As content is low. Therefore, the Te, Bi and Pb played a significant role in gold mineralization in As-deficient ore fluids in the J4 gold-bearing breccia pipe from the Qiyugou district. High-precision in situ laser ablation multiple collector inductively coupled mass spectrometry (LA-MC-ICP-MS) lead isotope analyses indicate that the sulfides have Pb-206/Pb-204, Pb-207/Pb-204, and Pb-208/Pb-204 ratios from 17.250 to 17.629, from 15.401 to 15.621, and from 37.649 to 38.290, respectively, which are similar to the granite porphyry in the district and indicative of their similar lead sources. High-precision in situ LA-MC-ICP-MS sulfur isotope analyses of pyrite show a large delta S-34 variation (e.g., from -18.1 to -11.1 per mil for Py-1, from -12.2 to - 6.6 per mil for Py-2, and from -4.9 to -1.6 per mil for Py-3) with a remarkable increasing trend from stage I, stage IIto stage III. This trend may record a decreasing oxygen fugacity of the ore-forming fluids during mineralization.
