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Elementy walidacji metody oznaczania δ18O i δD próbek ciekłych (EA-IRMS)

Janiga M., Bieleń W.

Nafta-Gaz

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2017

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R. 73, nr 7

473--478

PL

Celem pracy było wykonanie elementów walidacji metodyki oznaczeń składu izotopowego tlenu i wodoru próbek ciekłych (wody) przy użyciu spektrometru masowego połączonego z analizatorem elementarnym (EA-IRMS). Zarówno w przypadku oznaczeń składu izotopowego wodoru, jak i tlenu wykonano kalibrację przy zastosowaniu wzorca VSMOW2 oraz wyznaczono stretching factor (wykorzystując wzorzec SLAP2). Dla obydwu pierwiastków metody są dokładne (wartości rzeczywiste wzorca znajdują się w wyznaczonych przedziałach). Odchylenia standardowe powtarzalności i odtwarzalności są na niskim poziomie (dla tlenu: 0,15‰ i 0,21‰; dla wodoru: 1,2‰ i 1,3‰). Wartość niepewności pomiaru w przypadku oznaczeń składu izotopowego tlenu wynosi 0,569885% (czyli 0,310644‰ po przeliczeniu dla wzorca SLAP2), a w przypadku wodoru: 0,479804% (czyli 2,022375‰ po przeliczeniu dla wzorca SLAP2).

EN

The aim of the study was to perform validation of a methodology of isotopic composition determinations of oxygen and hydrogen liquid samples (water) using a mass spectrometer combined with an elemental analyzer (EA-IRMS). For the determination of both the hydrogen and oxygen isotopic composition, calibration was performed by using VSMOW2 standard, and stretching factor was determined using the SLAP2 standard. For both elements methods are accurate (the actual value can be found at designated intervals). The standard deviations of repeatability and reproducibility are low (for oxygen 0.15‰ and 0.21‰, for hydrogen 1.2‰ and 1.3‰). The value of measurement uncertainty for the determination of the isotopic composition of oxygen is 0.569885% (or 0.310644‰ after calculation for the SLAP2 standard) and for hydrogen is 0.479804% (or 2.022375 ‰ after calculation for SLAP2 standard).

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Geological and geochemical implications of the genesis of the Qolqoleh orogenic gold mineralisation, Kurdistan Province (Iran)

Taghipour B., Ahmadnejad F.

Geologos

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2015

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Vol. 21, No. 1

31--57

EN

The Qolqoleh gold deposit is located in the northwestern part of the Sanandaj–Sirjan Zone (SSZ), within the NE–SW trending Qolqoleh shear zone. Oligocene granitoids, Cretaceous meta-limestones, schists and metavolcanics are the main lithological units. Chondrite-normalised REE patterns of the ore-hosting metavolcanics indicate REE enrichment relative to hanging wall (chlorite-sericite schist) and footwall (meta-limestone) rocks. The pattern also reflects an enrichment in LREE relative to HREE. It seems that the LREE enrichment is related to the circulation of SO42- and CO2-bearing fluids and regional metamorphism in the Qolqoleh shear zone. Both positive and negative Eu anomalies are observed in shear-zone metavolcanics. These anomalies are related to the degree of plagioclase alteration during gold mineralisation and hydrothermal alteration. In progressing from a metavolcanic protomylonite to an ultramylonite, significant changes occurred in the major/trace element and REE concentration. Utilising an Al-Fe-Ti isocon for the ore-hosting metavolcanics shows that Sc, Y, K, U, P, and M-HREE (except Eu) are relatively unchanged; S, As, Ag, Au, Ca, LOI, Rb and LREE are enriched, and Sr, Ba, Eu, Cr, Co and Ni decrease with an increasing degree of deformation. Based on geochemical features and comparison with other well-known shear zones in the world, the study area is best classified as an Isovolume-Gain (IVG) type shear zone and orogenic type gold mineralisation. Based on the number of phases observed at room temperature and their microthermometric behaviour, three fluid inclusion types have been recognised in quartz-sulphide and quartz-calcite veins: Type I monophase aqueous inclusions, Type II two-phase liquid-vapour (L-V) inclusions which are subdivided into two groups based on the homogenisation temperature (Th): a) L-V inclusions with Th from 205 to 255°C and melting temperature of last ice (Tm) from –3 to –9°C. b) L-V inclusions with higher Th from 335 to 385°C and Tm from –11 to –16°C. Type III three-phase carbonic-liquid inclusions (liquid water-liquid CO2-vapour CO2) with Th of 345–385°C. The mean values of the density of ore-forming fluids, pressure and depth of mineralisation have been calculated to be 0.79–0.96 gr/cm3, 2 kbar and 7 km, respectively. The δ18Owater and δD values of the gold-bearing quartz-sulphide veins vary from 7.2‰ to 8‰ and –40.24‰ to –35.28‰, respectively, which are indicative of an isotopically heavy crustal fluid and likely little involvement of meteoric fluid. The δ18Owater values of the quartz-calcite veins have a range of –5.31‰ to –3.35‰, and the δD values of –95.65‰ to –75.31‰, which are clearly lower than those of early-stage quartz-sulphide-gold veins, and are close to the meteoric water line. Based on comparisons of the D–O isotopic systematics, the Qolqoleh ore-mineralising fluids originated from metamorphic devolatilisation of Cretaceous volcano-sedimentary piles. Devolatilisation of these units occurred either synchronously with, or postdates, the development of penetrative (ductile) structures such as shear zones and during overprinting brittle deformation.

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Oznaczenie składu trwałych izotopów tlenu w kalcycie metodą termicznego rozkładu EA-IRMS

Janiga M.

Nafta-Gaz

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2013

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R. 69, nr 9

659--663

PL

Stosowaną zazwyczaj metodą dekompozycji kalcytu na potrzeby badań izotopowych jest trawienie kwasem ortofosforowym. Laboratorium Geochemii Nafty i Gazu wyposażone jest w izotopowy spektrometr masowy połączony on-line z analizatorem elementarnym, za pośrednictwem którego węglan wapnia może ulegać rozkładowi w temperaturze 1450°C. W celu oceny metody wykonano eksperyment walidacyjny. Termiczny rozkład kalcytu jest skuteczną metodą analizy składu izotopowego tlenu. δ18O w węglanach może być analizowana za pośrednictwem EA-IRMS, ale wymagane jest spełnienie odpowiednich warunków: próbki węglanu muszą być czyste (bez dodatku substancji organicznej), a na próbkę węglanu musi się składać wyłącznie kalcyt (bez udziału innych minerałów).

EN

The most commonly used method of calcium carbonate decomposition for isotopic studies is teatment with phosphoric acid. The Oil and Gas Geochemistry Laboratory is equipped with an elemental analyzer, through which calcite can undergo decomposition at a temperature of 1450°C. To evaluate the method, a validation experiment was performed. Thermal decomposition of calcite is an effective method to analyze the isotopic composition of oxygen. δ18O in carbonates can be analyzed using EA-IRMS but under specific conditions: carbonate samples must be pure (without the addition of organic matter) and carbonate samples must contain only calcite (without any content of other minerals).

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Oxygen isotope analysis of shark teeth phosphates from Bartonian (Eocene) deposits in Mangyshlak peninsula, Kazakhstan

Pelc A., Hałas S., Niedźwiedzki R.

Mineralogia

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2011

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Vol. 42, iss. 1

53--61

EN

We report the results of high-precision (±0.05‰) oxygen isotope analysis of phosphates in 6 teeth of fossil sharks from the Mangyshlak peninsula. This precision was achieved by the offline preparation of CO2 which was then analyzed on a dual-inlet and triple-collector IRMS. The teeth samples were separated from Middle- and Late Bartonian sediments cropping out in two locations, Usak and Kuilus. Seawater temperatures calculated from the δ18O data vary from 23–41oC. However, these temperatures are probably overestimated due to freshwater inflow. The data point at higher temperature in the Late Bartonian than in the Middle Bartonian and suggest differences in the depth habitats of the shark species studied.

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Note on the stable isotope values of vein calcite in the El-Seboah peralkaline granite (SW Egypt)

Hassan K. M.

Mineralogia

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2011

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Vol. 42, iss. 2/3

113--120

EN

Stable isotope data for carbon (δ13C) and oxygen (δ18O) are used to constrain the environments of calcite formation in two veins in the El-Seboah peralkaline granite in south-western Egypt. Vein I with calcitemagnetite-goethite-hematite-quartz, and vein II with calcite-magnetite-goethite-kaolinite-hematite-quartz are texturally distinct. The calcite of each vein has characteristic δ13C- and δ18O-values: + 0.32 and -7.28‰ for vein I and + 1.16 and - 1.21‰ for vein II, respectively. The observed differences between the δ13C values of the two veins indicate that they represent two separate systems of primary dissolved inorganic carbon formed at or near equilibrium with atmospheric CO2. The δ18O values, on the other hand, indicate calcite deposition from meteoric waters which were fresh for vein I and brackish for vein II.