Equipment and newly developed methodological approaches for isotopic–geochemical studying fluid phases in rocks and minerals

Abstract

The paper presents data on an original equipment complex, consisting of two apparatuses, designed to prepare rock and mineral samples for the isotopic analysis of their fluid and/or gas inclusions. An example of samples from the Guli alkaline ultramafic massif in the Maimecha-Kutui province, northern central Siberia, is employed to demonstrate the capabilities of the technique of stepwise sample crushing and multiple-isotope analysis of the fluid phase.

An isotope ratio mass spectrometry‐based method for hydrogen isotopic analysis in sub‐microliter volumes of water: Application for multi‐isotope investigations of gases extracted from fluid inclusions

“…The samples (0.4–0.6 g) were washed in ethanol in an ultrasonic bath, dried, and then loaded into a homemade crushing tube connected to a vacuum line of the Gas Extraction System 34 (Figure 1, upper part; Figure S1, supporting information). The entire system was pumped out to a pressure of 10 −3 mbar and heated at ~120°C for 12 h to remove the gases adsorbed on the sample surface.…”

“…A Delta Plus isotope ratio mass spectrometer (Thermo Fisher Scientific) at Vernadsky Institute, Moscow, equipped with dual‐inlet system with microvolume option, was used to determine the 13 C/ 12 C isotopic ratios in CO 2 from fluid inclusions. A detailed description of the technique is presented in our earlier paper 34 . The carbon isotopic ratios in fluid inclusions are reported against VPDB (Vienna Pee Dee Belemnite).…”

“…A detailed description of the technique is presented in our earlier paper. 34 The carbon isotopic ratios in fluid inclusions are reported against VPDB (Vienna Pee Dee Belemnite).…”

“…We developed a sample preparation line for gases from fluid inclusions in rocks and minerals 32 and a technique for the preparation of micro-quantity water samples from fluid inclusions for isotope analysis. 33,34 While the noble gas, nitrogen and CO 2 data obtained with our crushing technique were successfully used to study mid ocean ridge basalt (MORB) glasses, 9,10,35 mantle xenoliths, 36 carbonatites 17,37,38 and meteorites, 39 the reliability of inclusion water analyses had to be proved. Based on the results of the study of hydrothermal quartz inclusions from the Solnechnoye tin ore deposit (Khabarovsk District), a δ 2 H reproducibility of ±4 ‰ (1σ, n = 5) was achieved.…”

“…Our goal was to elaborate the (stepwise) crushing technique for studying the isotope composition of different gas components, such as nitrogen, CO 2 , noble gases and micro‐quantities of water released from fluid inclusions in rocks and minerals. We developed a sample preparation line for gases from fluid inclusions in rocks and minerals 32 and a technique for the preparation of micro‐quantity water samples from fluid inclusions for isotope analysis 33,34 . While the noble gas, nitrogen and CO 2 data obtained with our crushing technique were successfully used to study mid ocean ridge basalt (MORB) glasses, 9,10,35 mantle xenoliths, 36 carbonatites 17,37,38 and meteorites, 39 the reliability of inclusion water analyses had to be proved.…”