METHOD DESCRIPTION


KIEL IV Carbonate Device
Oxygen and carbon isotopes in carbonates
Stable isotopic composition of oxygen and carbon in carbonates is determined using a Thermo KIEL IV Carbonate Device connected to a Finnigan Delta Plus isotope ratio mass spectrometer in a Dual Inlet system. CO2 is extracted from carbonates using the method described by McCrea (1950). Sample (minimum weight 20 µg) is reacted with orthophosphoric acid (density 1.94 g/dm3) at 70 °C. International standard NBS 19 is analyzed per every ten samples. Isotope ratios are reported as delta (δ) values and expressed relative to VPDB standard.


Measurement precision:

Standard deviation (1σ) δ13C ± 0.03‰
Standard deviation (1σ) δ18O ± 0.07‰

McCrea, J.M. (1950): The isotopic chemistry of carbonates and a paleo-temperature scale. J. Chem. Phys. 18: 849-857.
Flash EA 1112HT
Nitrogen and carbon isotopes in organic and inorganic solid samples
Stable isotopic composition of nitrogen and carbon is determined using a Thermo Flash EA 1112HT elemental analyzer connected to a Thermo Delta V Advantage isotope ratio mass spectrometer in a Continuous Flow system. Minimal weight of samples depends on the wt% amount of both elements. Samples wrapped in tin capsules are combusted at 1020 °C. Released gases (CO2 and N2 ) split in a GC column are transferred to MS source through a capillary. Isotope ratios are reported as delta (δ) values and expressed relative to VPDB for δ13C and to atmospheric nitrogen for δ15N. Delta values are normalized to a calibration curve based on international standards USGS 40, USGS 41, IAEA 600.


Measurement precision:

Standard deviation (1σ) δ13C ± 0.33‰
Standard deviation (1σ) δ15N ± 0.43‰
Oxygen isotopes in phosphates
Stable isotope composition of oxygen in phosphates is determined using a Thermo Flash EA 1112HT elemental analyzer connected to a Thermo Delta V Advantage isotope ratio mass spectrometer in a Continuous Flow system. The minimal weight of sample is ca. 400 µg. Samples wrapped in silver capsules are pyrolyzed at 1450 °C. Released gas (CO) is transferred to MS source through a capillary. Isotope ratios are reported as delta (δ) values and expressed relative to VSMOW. Delta values are normalized to a calibration curve based on internal standards UMCS 1, UMCS 2 and international standard B 2207.


Measurement precision:

Standard deviation (1σ) δ18O ± 0.3‰
Sulfur isotopes in sulfates
Stable isotopic composition of sulfur in sulfates is determined using a Thermo Flash EA 1112HT elemental analyzer connected to a Thermo Delta V Advantage isotope ratio mass spectrometer in a Continuous Flow system. The minimal weight of sample is ca. 400 µg plus 10-fold quantity of V2O5. Samples wrapped in tin capsules are combusted at 1020 °C. Released gas (SO2) is transferred to MS source through a capillary. Isotope ratio is reported as delta (δ) values and expressed relative to VCDT. Delta values are normalized to a calibration curve based on international standards NBS 127, IAEA SO-5, IAEA SO-6.


Measurement precision:

Standard deviation (1σ) δ34S ± 0.3‰
Oxygen isotopes in sulfates
Stable isotopic composition of oxygen in sulfates is determined using a Thermo Flash EA 1112HT elemental analyzer connected to a Thermo Delta V Advantage isotope ratio mass spectrometer in a Continuous Flow system. The minimal weight of sample is ca. 400 µg. Samples wrapped in silver capsules are pyrolyzed at 1450 °C. Released gas (CO) is transferred to MS source through a capillary. Isotope ratios are reported as delta (δ) values and expressed relative to VSMOW. Delta values are normalized to a calibration curve based on international standards NBS 127, IAEA SO-5, IAEA SO-6.


Measurement precision:

Standard deviation (1σ) δ18O ± 0.5‰
Sulfur isotopes in sulfides
Stable isotopic composition of sulfur in sulfides is determined using a Thermo Flash EA 1112HT elemental analyzer connected to a Thermo Delta V Advantage isotope ratio mass spectrometer in a Continuous Flow system. The minimal weight of sample is ca. 400 µg plus 10-fold quantity of V2O5. Samples wrapped in tin capsules are combusted at 1020 °C. Released gas (SO2) is transferred to MS source through a capillary. Isotope ratios are reported as delta (δ) values and expressed relative to VCDT. Delta values are normalized to a calibration curve based on international standards IAEA S-1, IAEA S-2, IAEA S-3.


Measurement precision:

Standard deviation (1σ) δ34S ± 0.2‰
GasBench II
Isotopic composition of Dissolved Inorganic Carbon in water
Stable isotopic composition of Dissolved Inorganic Carbon in water is determined using a Thermo GasBench II connected to a Thermo MAT 253 isotope ratio mass spectrometer in a Continuous Flow system. 0,8 ml of sample is equilibrated during 18 hours at 70 °C prior to analysis. Isotope ratios are reported as delta (δ) values and expressed relative to VPDB for δ13C. Delta values are normalized to a calibration curve based on international standards NBS 19, NBS 18, LSVEC.


Measurement precision:

Standard deviation (1σ) δ13C ± 0.2‰
Oxygen isotopes in water
Isotopic composition of oxygen in water is determined using a Thermo GasBench II connected to a Thermo MAT 253 isotope ratio mass spectrometer in a Continuous Flow system. 0.5 ml of sample is equilibrated during 18 hours at 32 °C prior to analysis. Isotope ratios are reported as delta (δ) values and expressed relative to VSMOW for δ18O. Delta values are normalized to a calibration curve based on standards GISP, W6444, W 67400.


Measurement precision:

Standard deviation (1σ) δ18O ± 0.25‰
HDevice
Hydrogen isotopes in water
Stable isotopic composition of hydrogen in water is determined using a Thermo HDevice connected to a Thermo MAT 253 isotope ratio mass spectrometer in a Dual Inlet system. 1,2 µl of sample is reduced in chromium reactor at 850 °C prior to analysis. Isotope ratios are reported as delta (δ) values and expressed relative to VSMOW for δ2H. Delta values are normalized to a calibration curve based on standards GISP, W6444, W 67400. H3+ factor is determined every sequence run.


Measurement precision:

Standard deviation (1σ) δ2H ± 1‰
ORTEC Octete PC Alpha spectrometer
U-Th dating
Uranium and thorium activities are determined using an alpha spectrometer OCTETE-PC, ORTEC. The minimum weight of samples depends on uranium concentration. After chemical treatment, uranium and thorium are separated on chromatographic column filled with Dowex 1x8. Subsequently, the samples are electrodeposited on steel disk prior to the measurements. The age of samples is calibrated based on isotope ratios of 234U/238U, 230Th/234U, 230Th/232Th and uranium concentration (ppm). The maximum age range of the method is ca. 350 thousand years.
210Pb dating
210Pb activity is determined based on radioactive equilibrium with 210Po. Activity of 210Po is determined using an alpha spectrometer OCTETE-PC, ORTEC. 1 cm3 of sample undergoes chemical treatment. Subsequently, the sample is electrodeposited on silver disk and analyzed. The age of samples is calibrated based on 210Po activity (Bq/kg). The maximum age range of the method is ca. 150 years.
Ultra Low Level Liquid Scintillation β/α Spectrometer Quantulus 1220
Tritium activity in water


Tritium activity in water is determined using an QUANTULUS 1220 ultra-low level LSC-liquid scintillation counter. 0.5 l of sample is pre-distilled and after that 300 ml of each sample undergoes electrolytic enrichment in stable conditions (temperature 2 °C, current intensity 5.5 A) until the sample volume is reduced to 15 ml. Subsequently the sample is distilled and mixed with an Ultima GoldTM LLT scintillator in proportion 8 ml of sample per 12 ml of scintillator. Sample is equilibrated for 24 hours prior to analysis. Standard measurement is 85 cycles per 15 minutes. Results are calibrated using a 1224-534 EASY View and reported as TU or DPM units. Values are normalized to a Perkin Elmer tritiated water cat. number 6004052.


Measurement precision: 0.15 TU.
Gamma Spectrometer Be 5030
Short-lived isotope activity in solid samples
Short-lived isotope activity measurement is determined using gamma spectrometer Be 5030 with a low background shield of measurement chamber. 210Pb and 137Cs are analyzed in various kinds of samples, e.g. lake sediments, soil and peat. Sample is homogenized and dried at 60 °C until attains stable mass prior to analysis. Weight of sample is 2-3 grams. Data is calibrated using a GENIE 2000 and reported as Bq/kg units.
Elemental analyzer Vario MicroCUBE
Percent amount of nitrogen, hydrogen, carbon and sulfur in solid samples
Percent amount of nitrogen, hydrogen, carbon and sulfur is determined using a Vario MicroCUBE elemental analyzer. Minimal weight of sample depends on the wt% of every element. Samples wrapped in tin capsules are combusted at 1150 °C. Released gases (CO2, N2, H2O and SO2) are separated on GC column and determined by thermal conductivity detector. Percent amount values are normalized to a sulfanilic acid standard. Measurement results are reported as wt%.


Measurement precision:

Standard deviation (1σ) %C ± 0.6‰
Standard deviation (1σ) %N ± 0.18‰
Standard deviation (1σ) %H ± 0.21‰
Standard deviation (1σ) %S ± 0.43‰
Detection limit is 40 ppm for every element.