Our laboratory has three IRMS (Isotope Ratio Mass Spectrometer) units:
Mass spectrometers are coupled with peripheral devices in various configurations, either in continuous He flow or in dual inlet system.
Peripherals:
Kiel IV Carbonate Device + Delta Plus IRMS
Standard analysis:
δ13C and δ18O measurement of carbonates, with a carbonate content of at least 20 µg
Method description:
δ13C and δ18O measurement in carbonates
Analyses of the isotopic composition of carbon and oxygen (δ13C, δ18O) in carbonates are performed using KIEL IV Carbonate Device (Thermo Scientific) connected to Delta Plus mass spectrometer (Finnigan MAT) in a dual-inlet system. In the reaction of carbonate with anhydrous orthophosphoric acid at 70°C carbon dioxide is released, whose isotopic composition is then measured using a mass spectrometer. Three certified international reference materials are used for calibration: NBS 18, IAEA 610, and IAEA 603. The measurement results are reported in δ notation relative to VPDB. The measurement accuracy (1 SD) is ±0.03‰ and ±0.08‰ for δ13C i δ18O, respectively.
GasBench II, coupled with CTC PAL autosampler and MAT 253 IRMS
Standard analyses:
δ13C measurement of inorganic carbon dissolved in water (DIC); δ13C and δ18O measurement of carbonates, with a carbonate content of at least 300 µg, δ18O measurement of water with low mineralization.
Method description:
δ13C measurement of dissolved inorganic carbon (DIC)
Analyses of the isotopic composition of carbon (δ13C) in DIC are performed via GasBench II peripheral device coupled with MAT 253 mass spectrometer (Thermo Scientific) with He continuous flow. As a result of the reaction of anhydrous orthophosphoric acid with the sample (0.3 - 0.8 ml, depending on DIC concentration), carried out at 25°C for 18 hours, CO2 is released, whose isotopic composition is then measured using a mass spectrometer. Three certified international reference materials are used for calibration: NBS 18, IAEA 610 and IAEA 603. The measurement results are reported in δ notation relative to VPDB. The accuracy of the δ13C measurement (1 SD) is ±0.03‰.
δ13C and δ18O measurement of carbonates
Analyses of the isotopic composition of carbon and oxygen (δ13C, δ18O) in carbonates are performed using GasBench II peripheral device coupled with MAT 253 mass spectrometer (Thermo Scientific) with continous flow of He. In the reaction of anhydrous orthophosphoric acid with the carbonate sample, CO2 is released. The reaction takes place at 70°C for at least 2 hours. The isotopic composition is then measured using a mass spectrometer. Three certified international reference materials are used for calibration: NBS 18, IAEA 610, and IAEA 603. Measurement results are reported in δ notation relative to VPDB. The measurement accuracy (1 SD) is ±0.03‰ and ±0.08‰ for δ13C i δ18O, respectively.
δ18O measurement of waters
Analyses of the isotopic composition of oxygen (δ18O) contained in water are performed using GasBench II peripheral device coupled with MAT 253 mass spectrometer (Thermo Scientific) with He continuous flow. H2O-CO2 equilibration method is used for analysis of δ18O in waters. Water sample (0.5 ml) is equilibrated for 24 hours with CO2 gas at 25°C, after which the isotopic composition of the equilibrated CO2 is measured using a mass spectrometer. Three certified international reference materials are used for calibration: VSMOW2, GRESP, and SLAP2. Measurement results are reported in δ notation relative to VSMOW. Measurement accuracy for δ18O is (1 SD): ±0.1‰.
H-Device, coupled with CTC PAL autosampler and MAT 253 IRMS
Standard analyses:
δ2H measurement of low mineralized water
Method description:
δ2H measurement of waters
Analyses of the isotopic composition of hydrogen (δ2H) contained in water are performed using the H-Device peripheral device coupled with MAT 253 mass spectrometer (Thermo Scientific) in an He dual-inlet system. 1 µl of sample is introduced into a reactor filled with Cr, where it is reduced at 850°C; the resulting H2 is then introduced into the mass spectrometer, where its isotopic composition is measured. Three certified reference materials are used for calibration: VSMOW2, GRESP, and SLAP2. Measurement results are reported as δ relative to VSMOW. Measurement accuracy of δ2H is (1 SD) ±1‰.
Flash 1112 HT EA, coupled with MAS 200R autosampler, No Blank Device, ConFlo IV and DeltaV Advantage IRMS
Standard analyses:
δ13C and δ15N measurement of solid organic samples (e.g. soil humus, lake sediments, bone collagen, plant remains) and δ15N of inorganic solid samples (KNO3, NaNO3, AgNO3); δ18 measurement of BaSO4 and Ag3PO4; δ34S measurement of Ag2S and BaSO4
Method description:
δ13C and δ15N measurement of organics
Carbon and nitrogen isotopic analyses (δ13C and δ15N) of organic samples are performed using Flash EA 1112 HT elemental analyzer coupled with ConFlo IV and Delta V Advantage mass spectrometer (Thermo Scientific). The weighed amount of a sample depends on the percentage of individual components in the sample. Samples wrapped in a tin foil are combusted in O2 atmosphere at 1020°C. The obtained gases, N2 and CO2 are separated on a chromatographic column and sequentially introduced into a mass spectrometer, where their isotopic composition is measured. Three certified reference materials are used for calibration: USGS 41a, USGS 40, and IAEA 600. Results are reported in δ notation, for carbon - relative to the VPDB standard, for nitrogen - relative to atmospheric N2. The measurement accuracy (1 SD) is ±0.1‰ and ±0.3‰ for δ13C and δ15N, respectively.
δ34S measurement of sulfides (Ag2S)
Analyses of the isotopic composition of sulfur (δ34S) in Ag2S are performed using Flash 1112 HT elemental analyzer coupled with ConFlo IV and Delta V Advantage mass spectrometer (Thermo Scientific). Samples (approx. 400 µg of Ag2S and tenfold of V2O5) are wrapped in a tin foil and combusted in O2 atmosphere at 1020°C. The obtained SO2 is then introduced into the mass spectrometer, where its isotopic composition is measured. Three certified reference materials are used for calibration: IAEA S1, IAEA S2, and IAEA S3. Results are reported in δ notation, relative to the VCDT standard. The δ34S measurement accuracy: (1 SD) ±0.2‰.
δ34S measurement of sulfates (BaSO4)
Analyses of the isotopic composition of sulfur (δ34S) in sulfates (BaSO4) are performed using Flash 1112HT elemental analyzer coupled with ConFlo IV and Delta V Advantage mass spectrometer (Thermo Scientific). Samples (approx. 400 µg of BaSO4 and tenfold of V2O5) are combusted in O2 atmosphere at 1020°C. SO2 obtained from the reaction is then introduced into the mass spectrometer, where its isotopic composition is measured. Three certified reference materials are used for calibration: NBS 127, IAEA SO5, and IAEA SO6. Results are reported in δ notation, relative to the VCDT standard. The δ34S measurement accuracy (1 SD): ±0.2‰.
δ18O measurement of sulfates (BaSO4)
Analysis of the isotopic composition of oxygen (δ18O) in sulfates (BaSO4) is performed using Flash 1112 HT elemental analyzer coupled with ConFlo IV and Delta V Advantage mass spectrometer (Thermo Scientific). Approximately 400 µg of the sample, wrapped in silver foil, is decomposed at 1400°C in the presence of C. The obtained CO gas is introduced into the mass spectrometer, where its isotopic composition is measured. Three certified reference materials are used for calibration: NBS 127, IAEA SO5, and IAEA SO6. Results are reported in δ notation, relative to the VSMOW standard. Measurement accuracy for δ18O (1 SD): ±0.3‰.
δ18O measurement of phosphates (Ag3PO4)
Analysis of the isotopic composition of oxygen (δ18O) in phosphates (Ag3PO4) is performed using Flash 1112 HT elemental analyzer coupled with ConFlo IV and Delta V Advantage mass spectrometer (Thermo Scientific). Approximately 400 µg of the sample, wrapped in silver foil, is decomposed at 1400°C in the presence of C. The obtained CO is introduced into the mass spectrometer, where its isotopic composition is measured. Three certified reference materials are used for calibration: B 2207, USGS 80, and USGS 81. Results are reported in δ notation, relative to the VSMOW standard. Measurement accuracy for δ18O (1 SD): ±0.3‰.
δ15N and δ18O measurement of nitrates
Nitrogen isotopic composition (δ15N) analyses in nitrates are performed using Flash EA 1112HT elemental analyzer coupled with ConFlo IV and Delta V Advantage mass spectrometer (Thermo Scientific). Approximately 400 µg of sample, wrapped in a tin foil, is combusted in O2 atmosphere at 1020°C. The obtained N2 is then introduced into a mass spectrometer, where its isotopic composition is measured. Three certified reference materials are used for calibration: USGS 32, USGS 35, IAEA NO3. Results are reported in δ notation, relative to atmospheric N2. Measurement accuracy for δ15N (1 SD): ±0.2‰.
Analysis of the isotopic composition of oxygen (δ18O) in nitrates (AgNO3) is performed using Flash 1112 HT elemental analyzer coupled with ConFlo IV and Delta V Advantage mass spectrometer (Thermo Scientific). Approximately 400 µg of the sample, wrapped in silver foil, is decomposed at 1400°C in the presence of C. The obtained CO is introduced into the mass spectrometer, where its isotopic composition is measured. Three certified reference materials are used for calibration: USGS 32, USGS 35, and IAEA NO3. Results are reported in δ notation, relative to the VSMOW standard. Measurement accuracy for δ18O (1 SD): ±0.3‰.
