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Granite-related wolframite-quartz veins are the world's most important tungsten mineralization and production resource. Recent progress in revealing their hydrothermal processes has been greatly facilitated by the use of infrared microscopy and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) analysis of both quartz- and wolframite-hosted fluid inclusions. However, owing to the paucity of detailed petrography, previous fluid inclusion studies on coexisting wolframite and quartz are associated with a certain degree of ambiguity. To better understand the fluid processes forming these two minerals, free-grown crystals of intergrown wolframite and quartz from the giant Yaogangxian W deposit in South China were studied using integrated in situ analytical methods including cathodoluminescence (CL) imaging, infrared microthermometry, Raman microspectroscopy, and fluid inclusion LA-ICP-MS analysis. Detailed crystal-scale petrography with critical help from CL imaging shows repetition of quartz, wolframite, and muscovite in the depositional sequence, which comprises a paragenesis far more complex than previous comparable studies. The reconstruction of fluid history in coexisting wolframite and quartz recognizes at least four successive fluid inclusion generations, two of which were entrapped concurrently with wolframite deposition. Fluctuations of fluid temperature and salinity during precipitation of coexisting wolframite and quartz are reflected by our microthermometry results, according to which wolframite-hosted fluid inclusions do not display higher homogenization temperature or salinity than those in quartz. However, LA-ICP-MS analysis shows that both primary fluid inclusions in wolframite and quartz-hosted fluid inclusions associated intimately with wolframite deposition are characterized by strong enrichment in Sr and depletion in B and As compared to quartz-hosted fluid inclusions that are not associated with wolframite deposition. The chemical similarity between the two fluid inclusion generations associated with wolframite deposition implies episodic tungsten mineralization derived from fluids exhibiting distinct chemical signatures. Multiple chemical criteria including incompatible elements and Br/Cl ratios of fluid inclusions in both minerals suggest a magmatic-sourced fluid with the possible addition of sedimentary and meteoric water. Combined with microthermometry and Raman results, fluid chemical evolution in terms of B, As, S, Sr, W, Mn, Fe, and carbonic volatiles collectively imply fluid phase separation and mixing with sedimentary fluid may have played important roles in wolframite deposition, whereas fluid cooling and addition of Fe and Mn do not appear to be the major driving factor. This study also shows that fluid inclusions in both wolframite and coexisting quartz may contain a substantial amount of carbonic volatiles (CO2 ± CH4) and H3BO3. Ignoring the occurrence of these components can result in significant overestimation of apparent salinity and miscalculation of LA-ICP-MS elemental concentrations. We suggest that these effects should be considered critically to avoid misinterpretation of fluid inclusion data, especially for granite-related tungsten-tin deposits.

The study of fluid inclusions is important for understanding various geologic processes involving geofluids. However, there are a number of problems that are frequently encountered in the study of fluid inclusions, especially by beginners, and many of these problems are critical for the validity of the fluid inclusion data and their interpretations. This paper discusses some of the most common problems and/or pitfalls, including those related to fluid inclusion petrography, metastability, fluid phase relationships, fluid temperature and pressure calculation and interpretation, bulk fluid inclusion analysis, and data presentation. A total of 16 problems, many of which have been discussed in the literature, are described and analyzed systematically. The causes of the problems, their potential impact on data quality and interpretation, as well as possible remediation or alleviation, are discussed.

The Zhuangzi Au deposit in the world-class Jiaodong gold province hosts visible natural gold, and pyrite as the main ore mineral, making it an excellent subject for deciphering the complex hydrothermal processes and mechanisms of gold precipitation. Three types of zoned pyrite crystals were distinguished based on textural and geochemical results from EPMA, SIMS sulfur isotopic analyses and NanoSIMS mapping. Py0 has irregular shapes and abundant silicate inclusions and was contemporaneous with the earliest pyrite–sericite–quartz alteration. It has low concentrations of As (0–0.3 wt.%), Au and Cu. Py1 precipitated with stage I mineralization shows oscillatory zoning with the bright bands having high As (0.4–3.9 wt.%), Au and Cu contents, whereas the dark bands have low contents of As (0–0.4 wt.%), Au and Cu. The oscillatory zoning represents pressure fluctuations and repeated local fluid phase separation around the pyrite crystal. The concentration of invisible gold in Py1 is directly proportional to the arsenic concentration. Py1 is partially replaced by Py2 which occurs with arsenopyrite, chalcopyrite and native gold in stage II. The replacement was likely the result of pseudomorphic dissolution–reprecipitation triggered by a new pulse of Au-rich hydrothermal fluids. The δ34S values for the three types of pyrite are broadly similar ranging from + 7.1 to + 8.8‰, suggesting a common sulfur source. Fluid inclusion microthermometry suggests that extensive phase separation was responsible for the gold deposition during stage II mineralization. Uranium–Pb dating of monazite constrains the age of mineralization to ca. 119 Ma coincident with a short compressional event around 120 Ma linked to an abrupt change in the drift direction of the subducting Pacific plate.

“Multi-method-approach” has now been for many years the buzzword in marble provenance analysis. Nevertheless a true combination of the results of different analytical methods is rarely applied in the sense of the combined simultaneous use of a large number of analytically obtained numerical variables. It is demonstrated here that the combination of data from isotope analysis, chemical data, and data from the chemical analysis of inclusion fluids of an artefact and of course in combination with a corresponding database enhances substantially the accuracy of marble provenance analysis. It is explicitly pointed out that the unchallenged collection of data of the chemical composition of marbles from different sources (and different analytical procedures) most probably implies severe differences in their comparability. Exemplarily presented is the nearly perfect discrimination of the most important fine-grained marbles and furthermore the possibility of the intra-site discrimination of the three Carrara districts and the assignment of two portrait heads to the Carrara Torano quarries.

Transport and deposition of copper in the Earth’s crust are mainly controlled by the solubility of Cu-bearing phases and the speciation of Cu in magmatic-hydrothermal fluids. To improve our understanding of copper mobilization by hydrothermal fluids, we conducted an experimental study on the interaction between Cu-bearing phases (metallic copper, Cu O, CuCl) and aqueous chloride solutions (H O ± NaCl ± HCl; with Cl concentrations of 0 to 4.3 mol kg- ). The experiments were run in rapid heat/rapid quench cold-seal pressure vessels at 800 °C, 200 MPa, and logf ~ NNO+2.3. Either Cu or Au capsules were used as containers. The reaction products were sampled in situ by the entrapment of synthetic fluid inclusions in quartz. Fluid composition was subsequently determined by analyzing individual fluid inclusions using a freezing cell and laser ablation inductively coupled plasma-mass spectrometry. Our results show that large isolated and isometric inclusions, free of late-stage modifications, can be preserved after the experiment even when using a high cooling rate of 25 K s The obtained results demonstrate that: (1) reaction between native Cu, NaCl solution, and quartz (± silica gel) leads to the coexistence of fluid inclusions and Na-bearing silicate melt inclusions. Micrometer- to submicrometer-sized cuprite (Cu O) crystals have been observed in both types of the inclusions, and they are formed most probably due to the dissociation of CuOH. (2) When Cu reacts with HCl and CuCl solutions, or Cu reacts with NaCl solution, nantokite (CuCl) formed due to oversaturation has been found in fluid inclusion. Copper concentration in the fluid shows a strong positive dependence on the initial chlorine content, with Cu/Cl molal ratios varying from 1:9 to 1:1 in case 1 and case 2, respectively. When Cl is fixed to 1.5 m, initial fluid acidity has a major control on the Cu content, i.e., 0.17 ± 0.09 and 1.29 ± 0.57 m Cu were measured in fluids of case 1 and case 2, respectively. Cu solubility in pure water and in 1.5 m NaCl solutions are 0.004 ± 0.002 and 0.16 ± 0.07 m, respectively. The main responsible Cu-bearing complexes are CuOH(H O) in water, NaCuCl in NaCl solutions and HCuCl in alkali-free solutions. These results provide quantitative constraints on the mobility of Cu in hydrothermal solutions and confirm that Cl is a very important ligand responsible for Cu transport. The first observation that silicate melt can be generated in the fluid-dominated and native-copper-bearing system implies that transitional thermosilicate liquids can coexist with metal-rich fluids and may enhance Cu mobility in magmatic-hydrothermal systems. This may have important implications for the formation of Cu deposits in the systems with low S activities.

Fluids exsolved from mafic melts are thought to be dominantly CO2-H2O ± S fluids. Curiously, although CO2 vapor occurs in bubbles of mafic melt inclusions (MI) at room temperature (T), the expected accompanying vapor and liquid H2O have not been found. We reheated olivine-hosted MI from Mt. Somma-Vesuvius, Italy, and quenched the MI to a bubble-bearing glassy state. Using Raman spectroscopy, we show that the volatiles exsolved after quenching include liquid H2O at room T and vapor H2O at 150 °C. We hypothesize that H2O initially present in the MI bubbles was lost to adjacent glass during local, sub-micrometer-scale devitrification prior to sample collection. During MI heating experiments, the H2O is redissolved into the vapor in the bubble, where it remains after quenching, at least on the relatively short time scales of our observations. These results indicate that (1) a significant amount of H2O may be stored in the vapor bubble of bubble-bearing MI and (2) the composition of magmatic fluids directly exsolving from mafic melts at Mt. Somma-Vesuvius may contain up to 29 wt% H2O.

The origin, evolution, and interplay of brine and hydrocarbon fluid systems play a crucial role in the formation of deep sediment-hosted base metal ore deposits. Here we investigate ratios of halogens, noble gases, stable C and S isotopes, and metal budgets of aqueous brines, which deposited deep-seated and near-surface hydrothermal Zn-Pb mineralization hosted by Zechstein carbonates in the Lower Saxony Basin (North German Basin), by studies of fluid inclusions in sphalerite and quartz. Major and trace element geochemistry and noble gas isotopic signatures of brine inclusions revealed that the ore-forming fluids were highly reactive and experienced prolonged interactions with host rocks in the constricted, over-pressured metal source regions and consequently evolved from near-neutral, oxidized brines towards more reduced, acidic high-salinity brines. Quartz-hosted halite-saturated fluid inclusions with Th <200°C contain Zn and Pb concentrations up to ca. 9400 μg g-1 and 5200 μg g-1, respectively, and indicate the efficiency of metal scavenging processes. The interactions with Westphalian coals and Corg-rich shales influenced the redox state as well as the trace and critical element budget of the sphalerite-hosted fluid inclusions, with enrichment in Ge, Pd, Sb, Tl, Bi, and Ag. The salinities of metalliferous fluids originated primarily from seawater evaporation, however in addition a significant halite-dissolution component is present in the southern part of the Lower Saxony Basin. High concentrations of radiogenic noble gases and potassium in the sphalerite-hosted fluid inclusions are ascribed to strong interactions with the Paleozoic siliciclastic sedimentary pile and crystalline basement rocks. Reflux of the strongly modified, sulfur-poor, Zn-Pb-bearing acidic brines, proceeded via re-activated structurally controlled pathways into sour gas or gas-saturated brine pools in the Zechstein Ca2 carbonate unit. Here, mixing of the ascending metal-rich brines with H2S derived from thermochemical sulfate reduction (TSR), resulted in the deposition of deep-seated Zn-Pb ores in the Lower Saxony Basin. The overall timing of the Zn-Pb ore formation can be constrained to the Upper Cretaceous basin inversion.

Highly saline, deep‐seated basement brines are of major importance for ore‐forming processes, but their genesis is controversial. Based on studies of fluid inclusions from hydrothermal veins of various ages, we reconstruct the temporal evolution of continental basement fluids from the Variscan Schwarzwald (Germany). During the Carboniferous (vein type i), quartz–tourmaline veins precipitated from low‐salinity (<4.5wt% NaCl + CaCl2), high‐temperature (≤390°C) H2O‐NaCl‐(CO2‐CH4) fluids with Cl/Br mass ratios = 50–146. In the Permian (vein type ii), cooling of H2O‐NaCl‐(KCl‐CaCl2) metamorphic fluids (T ≤ 310°C, 2–4.5wt% NaCl + CaCl2, Cl/Br mass ratios = 90) leads to the precipitation of quartz‐Sb‐Au veins. Around the Triassic–Jurassic boundary (vein type iii), quartz–haematite veins formed from two distinct fluids: a low‐salinity fluid (similar to (ii)) and a high‐salinity fluid (T = 100–320°C, >20wt% NaCl + CaCl2, Cl/Br mass ratios = 60–110). Both fluids types were present during vein formation but did not mix with each other (because of hydrogeological reasons). Jurassic–Cretaceous veins (vein type iv) record fluid mixing between an older bittern brine (Cl/Br mass ratios ~80) and a younger halite dissolution brine (Cl/Br mass ratios >1000) of similar salinity, resulting in a mixed H2O‐NaCl‐CaCl2 brine (50–140°C, 23–26wt% NaCl + CaCl2, Cl/Br mass ratios = 80–520). During post‐Cretaceous times (vein type v), the opening of the Upper Rhine Graben and the concomitant juxtaposition of various aquifers, which enabled mixing of high‐ and low‐salinity fluids and resulted in vein formation (multicomponent fluid H2O‐NaCl‐CaCl2‐(SO4‐HCO3), 70–190°C, 5–25wt% NaCl‐CaCl2 and Cl/Br mass ratios = 2–140). The first occurrence of highly saline brines is recorded in veins that formed shortly after deposition of halite in the Muschelkalk Ocean above the basement, suggesting an external source of the brine's salinity. Hence, today's brines in the European basement probably developed from inherited evaporitic bittern brines. These were afterwards extensively modified by fluid–rock interaction on their migration paths through the crystalline basement and later by mixing with younger meteoric fluids and halite dissolution brines.

The Xianghualing large tin-polymetallic skarn deposit is located in the Nanling W-Sn metallogenic belt, South China, showing distinct spatial zoning of mineralization. From the contact between granite and carbonate rocks, the mineralization transitions from proximal skarn Sn ore to cassiterite-sulfide ore and more distal Pb–Zn-sulfide ore. This study reveals the fluid evolution and genetic links among these different ore types. The physical and chemical characteristics of fluid inclusions from each ore types indicate that the skarn Sn ore, cassiterite-sulfide ore, and Pb–Zn-sulfide ore all originated from the identical magmatic fluid exsolved from the Laiziling granite. Their formation, however, is controlled by diverse fluid evolutionary processes and host rock characteristics. The Sn–Pb-Zn-rich fluids were primarily derived from cooled and diluted magmatic brine, which is generated by boiling of initial single phase magmatic fluid. Mixing of magmatic brine with meteoric water is crucial to form skarn Sn ore. Redox reactions of aqueous Sn (II) complexes with As (III) species and/or minor CO2 during short cooling period of ore-forming fluid is likely an effective mechanism to form high-grade cassiterite-sulfide ores, accompanied by favorable pH conditions maintained through interaction with carbonate host rocks. The later stage addition of meteoric water prompts the formation of Pb–Zn-sulfide ore. Comparing these findings with the characteristics of initial or pre-ore magmatic fluids in both mineralized and barren granitic systems indicates that high Sn content in the pre-ore fluids and the suitable fractional crystallization degree of the parent magma may determine high Sn mineralization potential in granitic magmatic-hydrothermal systems.

Deep hydrothermal Mo, W, and base metal mineralization at the Sweet Home mine (Detroit City portal) formed in response to magmatic activity during the Oligocene. Microthermometric data of fluid inclusions trapped in greisen quartz and fluorite suggest that the early-stage mineralization at the Sweet Home mine precipitated from low- to medium-salinity (1.5–11.5 wt% equiv. NaCl), CO2-bearing fluids at temperatures between 360 and 415 °C and at depths of at least 3.5 km. Stable isotope and noble gas isotope data indicate that greisen formation and base metal mineralization at the Sweet Home mine was related to fluids of different origins. Early magmatic fluids were the principal source for mantle-derived volatiles (CO2, H2S/SO2, noble gases), which subsequently mixed with significant amounts of heated meteoric water. Mixing of magmatic fluids with meteoric water is constrained by δ2Hw–δ18Ow relationships of fluid inclusions. The deep hydrothermal mineralization at the Sweet Home mine shows features similar to deep hydrothermal vein mineralization at Climax-type Mo deposits or on their periphery. This suggests that fluid migration and the deposition of ore and gangue minerals in the Sweet Home mine was triggered by a deep-seated magmatic intrusion. The findings of this study are in good agreement with the results of previous fluid inclusion studies of the mineralization of the Sweet Home mine and from Climax-type Mo porphyry deposits in the Colorado Mineral Belt.