The cooling history of granulite is crucial to understanding tectonic scenarios of the continental crust. Ti-in-quartz, a useful indicator of temperature, can decipher the thermal evolution of crustal rocks. Here we apply the Ti-in-quartz (TitaniQ) thermometer to ancient ultrahigh-temperature (UHT) granulites from the Khondalite Belt (KB) in the North China Craton (NCC) and young UHT granulites from the Mogok Metamorphic Belt (MMB), Myanmar. Ti content in quartz was analyzed using a highly precise method constructed in a CAMECA SXFive electron probe microanalyzer (EPMA). The granulites from the two localities show different quartz Ti contents with a constant deforced beam of 10 μm. Matrix quartz and quartz inclusions from the NCC granulites have 57–241 ppm and 65–229 ppm, respectively, corresponding to the TitaniQ temperatures of 653–810 °C and 666–807 °C. The calculated temperatures are significantly lower than the peak temperatures (850–1096 °C) obtained by other methods, due to the formation of abundant rutile exsolution rods in quartz during cooling. Thus, the low calculated temperatures for the NCC granulites reflect a cooling state near or after the exsolution of rutile from quartz, most likely caused by a slow cooling process. However, the matrix quartz from the MMB granulites is exsolution-free and records higher Ti contents of 207–260 ppm and higher metamorphic temperatures of 894–926 °C, close to the peak UHT conditions. This feature indicates that the MMB granulites underwent rapid cooling to overcome Ti loss from quartz. Therefore, determining the amount of Ti loss from quartz by diffusion can provide new insight into the cooling behavior of UHT granulites. When a large deforced beam of 50 μm was used to cover the rutile rods, the matrix quartz in the KB granulites could also yield the TitaniQ temperatures above 900 °C. Thus, our new data suggest that the TitaniQ thermometer could be useful for revealing UHT conditions.

Ruby (red corundum) is one of the most prominent colored gemstones in the world. The highest-quality ruby (“pigeon blood” ruby) comes from marbles of the Mogok Stone Tract in central Myanmar. Although Mogok ruby has been exploited since the 6th century AD, the formation time of this gemstone is ambiguous and controversial. In this paper, we describe a mineralogical, geochemical, and geochronological study of ruby and titanite in ruby-bearing marbles obtained from an outcrop in the Mogok Stone Tract, central Myanmar. Petrographic observations have shown that titanite generally occurs in the marble matrix or occurs as inclusions in ruby. These two types of titanite exhibit identical chemical compositions. In situ secondary ion mass spectrometer (SIMS) U–Pb dating of the separated titanite from two representative samples of ruby-bearing marbles yielded lower intercept ages of 25.15 ± 0.24 Ma (MSWD = 0.26) and 25.06 ± 0.22 Ma (MSWD = 0.15), respectively. Because the closure temperature of the U–Pb system in titanite is close to the temperature of ruby growth, the obtained U–Pb ages (~25 Ma) are suggested to represent the timing of the studied ruby formation in Mogok. The acquired ages are in agreement with the timing of post-collisional extension in the Himalaya related to the migration of the eastern Himalayan syntaxis. Combining our dating results with previous geochronological data from the Mogok Stone Tract, we suggest that the formation of the studied ruby is most likely related to the high-temperature metamorphic event in the marbles during the India–Asia collision. Our study not only confirms that texturally constrained titanite could be a precise geochronometer to date the mineralization of different types of ruby, but also provides important geochronological information linking gemstone formation to the India–Asia collision.

Orthopyroxene, an important phase in mantle-derived rocks, has become a powerful tool to unravel mantle nature and magma processes. However, the applications have been hindered by the lag in the development of analytical techniques, such as shortage of reference materials. Orthopyroxene grains derived from an ultramafic intrusion at the Mogok metamorphic belt (Myanmar) were evaluated for the potential use of orthopyroxene as a reference material for in-situ microanalysis. Approximately 20 g of 0.5–3 mm pure orthopyroxene grains were separated under binocular microscope and analyzed using EPMA, LA-ICPMS, and bulk analytical methods (XRD, XRF, and solution-ICPMS) for major and trace elements at four institutions. Eleven core-to-rim profiles carried out using EPMA and twelve core-to-rim profiles determined using LA-ICPMS suggest that MK-1 orthopyroxene grains are sufficiently homogeneous, with RSD < ±2% (1σ) for major elements (Mg, Si, and Fe) and RSD < ±10% (1σ) for trace elements (Na, Al, Ca, Ti, Cr, Co, Zn, Ni, Mn, Sc, and V). In addition, the composition of MK-1 orthopyroxene was also measured by XRF and solution-ICPMS measurements in two different laboratories, to compare with the results measured using EPMA and LA-ICPMS. The results indicated a good agreement with RSE < ±2% (1σ) for major elements and RSE < ±5% (1σ) for most trace elements, except for Na (±9.73%) and Ti (±6.80%). In an overall assessment of these data, MK-1 orthopyroxene can be considered as a reference material for in-situ microanalysis, which would provide solid trace elements data for a better understanding of mantle source and magmatic evolution.

The mineral beryl (Be₃Al₂(SiO₃)₆) has the most abundant phase with industrial value for extracting a critical metal—beryllium. Due to multi-stage, fluid-induced growth, individual beryl grains may yield complex geochemical records, revealing variations in the oxygen isotopes of the fluids from which they crystallize. Secondary ion mass spectrometry (SIMS) with high sensitivity and high spatial resolution represents a good tool for in situ isotopic analysis. SIMS oxygen analyses require matrix-matched reference materials to calibrate instrumental mass fractionations during measurement. In this work, the oxygen isotope homogeneities of six beryl samples with different compositions (BS1, BS2, BS3, BS4, BS5, and BS6) were documented by SIMS. These samples’ recommended oxygen isotope compositions were characterized by laser fluorination isotope ratio mass spectrometry (IRMS). This study suggests that there is no matrix effect related to composition variation in beryl SIMS oxygen isotope analysis. The recommended δ¹⁸O values of the four reference materials, BS1, BS2, BS4, and BS5, were 15.01 ± 0.34‰ (2 standard deviations, 2 SD), 7.53 ± 0.16‰ (2 SD), 2.38 ± 0.14‰ (2 SD), and 10.72 ± 0.44‰ (2 SD), respectively. Therefore, BS1, BS2, BS4, and BS5 are recommended as suitable reference materials for in situ mineral beryl oxygen isotope microanalysis.