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ICP-MS > Inductively Coupled Plasma Mass Spectrometer

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  • Trace metal concentrations are reported in micrograms per gram of sediment in core C012-PC05 (64⁰ 40.517’ S, 119⁰ 18.072’ E, water depth 3104 m). Each sediment sample (100-200mg) was ground using a pestle and mortar and digested following an initial oxidation step (1:1 mixture of H2O2 and HNO3 acid) and open vessel acid on a 150 degree C hotplate using 2:5:1 mixture of concentrated distilled HCl, HNO3 and Baseline Seastar HF acid. After converting the digested sample to nitric acid, an additional oxidation step was performed with 1:1 mixture of concentrated distilled HNO3 and Baseline Seastar HClO4 acid. A 10% aliquot of the final digestion was sub-sampled for trace metal analyses. Trace metal concentrations were determined by external calibration using an ELEMENT 2 sector field ICP-MS from Thermo Fisher Scientific (Bremen, Germany) at Central Science Laboratory (University of Tasmania). The following elements were analysed in either low (LR) or medium resolution (MR): Sr88(LR), Y89(LR), Mo95(LR), Ag107(LR), Cd111(LR), Cs133(LR), Ba137(LR), Nd146(LR), Tm169(LR), Yb171(LR), Tl205(LR), Pb208(LR), Th232(LR), U238(LR), Na23(MR), Mg24(MR), Al27(MR), P31(MR), S32(MR), Ca42(MR), Sc45(MR), Ti47(MR), V51(MR), Cr52(MR), Mn55(MR), Fe56(MR), Co59(MR), Ni60(MR), Cu63(MR), Zn66(MR).

  • Samples were collected from the East Antarctic margin, aboard the Australian Marine National Facility R/V Investigator from January 14th to March 5th 2017 (IN2017_V01; Armand et al., 2018). This marine geoscience expedition, named the “Sabrina Sea Floor Survey”, focused notably on studying the interactions of the Totten Glacier with the Southern Ocean through multiple glacial cycles. Ten litres seawater samples were collected using a CTD rosette equipped with Niskin® bottle and filtered through a 0.45µm Acropak® capsule filter directly into acid-cleaned 10 L polyethylene jerrycans. Samples were then acidified to pH 2 with 2 mL/L of distilled 6M HCl in a laminar flow hood. These samples were analysed for neodymium (Nd) isotopes, a tracer of ocean circulation. In the home laboratory (IMAS Trace-Metal Lab, UTAS, Hobart, Australia), seawater samples were pre-concentrated using pre-packed Nobias® PA1L (Hitachi Technologies, Japan) chelating resin cartridges following the method of Pérez-Tribouillier et al., (2019). Rare Earth Elements were separated using anion-exchange chromatography (Anderson et al., 2012) and cation-exchange chromatography (Struve et al., 2016). Finally, Nd isotopes were isolated using LN-Spec column chemistry (Pin and Zalduegui, 1997). Purified seawater sample Nd concentrations were checked prior to isotopic analysis using Sector Field Inductively Coupled Mass Spectrometry (ICP-MS) at the Central Science Laboratory (UTAS, Hobart, Australia). Nd isotope ratio measurements were then carried out at the Geochemistry Laboratory of the School of Geography, Environment and Earth Sciences of Victoria University of Wellington, New Zealand, using a Thermo Finnigan Triton thermal ionization mass spectrometer (TIMS). Data were reduced offline for outlier rejection and corrected using 146Nd/144Nd = 0.7219 for mass fractionation using the exponential law, and 144Sm/147Sm = 0.20667 for the Sm interference correction on mass 144. JNdi standard data produced for two load sizes using two amplifier configurations were identical: 143Nd/144Nd = 0.512110 ± 24 2sd (46 ppm 2rsd, n = 16) for 1 ng loads using 1013Ω amplifiers, vs. 143Nd/144Nd = 0.512112 ± 3 2sd (6 ppm 2rsd, n = 6) for 100 ng loads using 1011Ω amplifiers. The corrected 143Nd/144Nd were normalised to the JNdi standard with the published value of 0.512115 (Tanaka et al., 2000). Nd isotopic compositions are reported as eNd = [(143Nd/144Nd)sample / (143Nd/144Nd)CHUR - 1]x10,000 , where CHUR is the Chondritic Uniform Reservoir with 143Nd/144Nd)CHUR = 0.512638 (Jacobsen and Wasserburg, 1980). References - Anderson R. F., Fleisher M. Q., Robinson L. F., Edwards R. L., Hoff J. A., Moran S. B., van der Loeff M. R., Thomas A. L., Roy-Barman M. and Francois R. (2012) GEOTRACES intercalibration of 230Th, 232Th, 231Pa, and prospects for 10Be. Limnol. Oceanogr. Methods 10, 179–213. A - Armand L. K., O’Brien P. E., Armbrecht L., Baker H., Caburlotto A., Connell T., Cotterle D., Duffy M., Edwards S., Evangelinos D., Fazey J., Flint A., Forcardi A., Gifford S., Holder L., Hughes P., Lawler K.-A., Lieser J., Leventer A., Lewis M., Martin T., Morgan N., López-Quirós A., Malakoff K., Noble T., Opdyke B., Palmer R., Perera R., Pirotta V., Post A., Romeo R., Simmons J., Thost D., Tynan S. and Young A. (2018) Interactions of the Totten Glacier with the Southern Ocean through multiple glacial cycles (IN2017-V01): Post-survey report. ANU Res. Publ. - Jacobsen S. B. and Wasserburg G. J. (1980) Sm-Nd isotopic evolution of chondrites. Earth Planet. Sci. Lett. 50, 139–155. - Pérez-Tribouillier H., Noble T. L., Townsend A. T., Bowie A. R. and Chase Z. (2019) Pre-concentration of thorium and neodymium isotopes using Nobias chelating resin: Method development and application to chromatographic separation. Talanta, 1–10. - Pin C. and Zalduegui J. F. S. (1997) Sequential separation of light rare-earth elements , thorium and uranium by miniaturized extraction chromatography: Application to isotopic analyses of silicate rocks. Anal. Chim. Acta 339, 79–89. - Struve T., Van De Flierdt T., Robinson L. F., Bradtmiller L. I., Hines S. K., Adkins J. F., Lambelet M., Crocket K. C., Kreissig K., Coles B. and Auro M. E. (2016) Neodymium isotope analyses after combined extraction of actinide and lanthanide elements from seawater and deep-sea coral aragonite. Geochemistry, Geophys. Geosystems 17, 232–240. - Tanaka T., Togashi S., Kamioka H., Amakawa H., Kagami H., Hamamoto T., Yuhara M., Orihashi Y., Yoneda S., Shimizu H., Kunimaru T., Takahashi K., Yanagi T., Nakano T., Fujimaki H., Shinjo R., Asahara Y., Tanimizu M. and Dragusanu C. (2000) JNdi-1: A neodymium isotopic reference in consistency with LaJolla neodymium. Chem. Geol. 168, 279–281.

  • This data describes the cellular metal concentrations of Phaeocystis antarctica and Cryothecomonas armigera following exposure to metals singly and in mixtures in laboratory studies. Microalgae were cultured in 80 mL of filtered (less than 0.45 um) seawater and low concentrations of nutrients supplemented with metal stocks to give a range of single and mixture exposures to the metals cadmium, copper, nickel, lead, and zinc. The cellular accumulation and partitioning are used to explain the metal's toxicity (cellular metal fractions are compared to the toxicity data provided in 10.4225/15/5ae93ff723ff8) and assess the risk bioaccumulation of metals to Antarctic marine microalgae may pose in the Southern Ocean food web.

  • Sediment cores were collected from the East Antarctic margin, aboard the Australian Marine National Facility R/V Investigator from January 14th to March 5th 2017 (IN2017_V01; (Armand et al., 2018). This marine geoscience expedition, named the “Sabrina Sea Floor Survey”, focused notably on studying the interactions of the Totten Glacier with the Southern Ocean through multiple glacial cycles. The cores were collected using a multi-corer (MC), were sliced every centimetre, wrapped up in plastic bags, and stored in the fridge. Back at the home laboratory (IMAS, UTAS, Hobart, Australia), sediment samples were dried in an oven at 40°C. Three hundred mg of dry sediment was then homogenised and vortexed for 10-sec with 12 mL of a reductive solution of 0.005M hydroxylamine hydrochloride (HH) / 1.5% Acetic Acid (AA) / 0.001M Na-EDTA / 0.033M NaOH, at pH 4 (Huang et al., 2021). The sediment was then leached a second time (to ensure the removal of all oxides and excess minerals, i.e. to isolate the detrital fraction) with 15 mL of 0.02M HH, 25% AA solution and agitated using a rotisserie (20 rpm) overnight (Wilson et al., 2018). Samples were then centrifuged, rinsed with Milli-Q water 3 times, and dried in an oven at 50°C. About 50 mg of resulting dry (detrital) sediment was ground, weighed into a Teflon vial, and digested with a strong acid mixture. First, the sediment was oxidized with a mixture of concentrated HNO3 and 30% H2O2 (1:1). Samples were then digested in open vials using 10 mL HNO3, 4 mL HCl, and 2 mL HF, at 180°C until close to dryness. Digested residues were converted to nitric form before being oxidised with a mixture of 1 mL HNO3 and 1 mL HClO4 at 220°C until fully desiccated. Samples were finally re-dissolved in 4 mL 7.5 M HNO3. A 400 μL aliquot was removed from the 4 mL digest solution and diluted ~2500 times in 2% HNO3 for trace metals analysis by Sector Field Inductively Coupled Mass Spectrometry (SF-ICP-MS, Thermo Fisher Scientific, Bremen, Germany) at the Central Science Laboratory (UTAS, Hobart, Australia). Indium was added as internal standard (In, 100 ppb). 88Sr, 89Y, 95Mo, 107Ag, 109Ag, 111Cd, 133Cs, 137Ba, 146Nd, 169Tm, 171Yb, 185Re, 187Re, 205Tl, 208Pb, 232Th, 238U, 23Na, 24Mg, 27Al, 31P, 32S, 42Ca, 47Ti, 51V, 52Cr, 55Mn, 56Fe, 59Co, 60Ni, 63Cu and 66Zn were analysed using multiple spectral resolutions. Element quantification was performed via external calibration using multi-element calibration solutions (MISA suite, QCD Analysts, Spring Lake, NJ, USA). Raw intensities were blank and dilution corrected. References Armand, L. K., O’Brien, P. E., Armbrecht, L., Baker, H., Caburlotto, A., Connell, T., … Young, A. (2018). Interactions of the Totten Glacier with the Southern Ocean through multiple glacial cycles (IN2017-V01): Post-survey report. ANU Research Publications Huang, H., Gutjahr, M., Kuhn, G., Hathorne, E. C., and Eisenhauer, A. (2021). Efficient Extraction of Past Seawater Pb and Nd Isotope Signatures From Southern Ocean Sediments. Geochemistry, Geophysics, Geosystems, 22(3), 1–22. Wilson, D. J., Bertram, R. A., Needham, E. F., van de Flierdt, T., Welsh, K. J., McKay, R. M., … Escutia, C. (2018). Ice loss from the East Antarctic Ice Sheet during late Pleistocene interglacials. Nature, 561(7723), 383.

  • Sediment cores were collected from the East Antarctic margin, aboard the Australian Marine National Facility R/V Investigator from January 14th to March 5th 2017 (IN2017_V01; Armand et al., 2018). This marine geoscience expedition, named the “Sabrina Sea Floor Survey”, focused notably on studying the interactions of the Totten Glacier with the Southern Ocean through multiple glacial cycles. The cores were collected using a multi-corer (MC) and a Kasten corer (KC). The MC were sliced every centimetre, wrapped up in plastic bags, and stored in the fridge. The KC was sub-sampled using an u-channel; and sliced every centimetre once back the home laboratory (IMAS, UTAS, Hobart, Australia). This dataset presents concentrations of major and trace elements measured in bulk multi-cores sediment samples collected during the IN2017_V01 voyage. The data include the sampling date (day/month/year), the latitude and longitude (in decimal degrees), the seafloor depth (in meter), the sediment core ID, the sediment depth (in cm), and the concentrations (in ppm or μg/g) of a suite of elements. This dataset presents concentrations of major and trace elements measured in bulk sediment samples collected during the IN2017_V01 voyage. The data include the sampling date (day/month/year), the latitude and longitude (in decimal degrees), the seafloor depth (in meter), the sediment core ID (KC14), the sediment depth (in cm), and the concentrations (in ppm or μg/g) of a suite of elements. About 200 mg of dried and ground sediment were weighed into a clean Teflon vial and oxidized with a mixture of concentrated HNO3 and 30% H2O2 (1:1). Samples were then digested in open vials using an acid mixture comprising 10 mL HNO3, 4 mL HCl, and 2 mL HF, at 180°C until close to dryness. Digested residues were converted to nitric form before being oxidised with a mixture of 1 mL HNO3 and 1 mL HClO4 at 220°C until fully desiccated. Samples were finally re-dissolved in 4 mL 7.5 M HNO3. A 400 μL aliquot was removed from the 4 mL digest solution and diluted ~2500 times in 2% HNO3 for trace metals analysis by Sector Field Inductively Coupled Mass Spectrometry (SF-ICP-MS, Thermo Fisher Scientific, Bremen, Germany) at the Central Science Laboratory (UTAS, Hobart, Australia). Indium was added as internal standard (In, 100 ppb). 88Sr, 89Y, 95Mo, 107Ag, 109Ag, 111Cd, 133Cs, 137Ba, 146Nd, 169Tm, 171Yb, 185Re, 187Re, 205Tl, 208Pb, 232Th, 238U, 23Na, 24Mg, 27Al, 31P, 32S, 42Ca, 47Ti, 51V, 52Cr, 55Mn, 56Fe, 59Co, 60Ni, 63Cu and 66Zn were analysed using multiple spectral resolutions. Element quantification was performed via external calibration using multi-element calibration solutions (MISA suite, QCD Analysts, Spring Lake, NJ, USA). Raw intensities were blank and dilution corrected. References L.K. Armand, P.E. O’Brien and On-board Scientific Party. 2018. Interactions of the Totten Glacier with the Southern Ocean through multiple glacial cycles (IN2017-V01): Post-survey report, Research School of Earth Sciences, Australian National University: Canberra.

  • These data describe the field deployments of the trace-metal passive sampling tools, diffusive gradients in thin-films (DGT). Deployments occurred over the summer 2017/2018 season in the coastal region adjacent to Casey and Wilkes stations. Deployments of DGT to the nearshore marine environment was achieved with small watercraft and shallow (less than 5m deep) moorings, which were left in situ for 21-37 days, depending on the site.

  • This study assessed the performance of diffusive gradients in thin-films (DGT) with a binding resin that used Chelex-100 (iminodiacetic acid functional groups) to measure cadmium, copper, nickel, lead, and zinc contaminants in Antarctic marine conditions. To do this, three sets of experiments were done: (I) the uptake of metals to DGT samplers was assessed over time when deployed to three metal mixtures of known concentrations (DGT performance page). This allowed for the determination of metal diffusion coefficients in Antarctic marine conditions and demonstrated when metal competition for binding sites were likely to occur. (II) the DGT were deployed in the presence of the microalga Phaeocystis antarctica at a concentration of 1000-3000 cells/mL to investigate how environmentally realistic concentrations of an Antarctic marine microalgae affect the uptake of metals (DGT uptake with algae page). Finally, the DGT-labile concentrations from part (II) were used in reference toxicity mixture models to predict toxicity to the microalgae so they could be compared to a previous study that investigated the toxicity of metal mixtures to Phaeocystis antarctica and Cryothecomonas armigera (DGT toxicity modelling page).

  • Sediment cores were collected from the East Antarctic margin, aboard the Australian Marine National Facility R/V Investigator from January 14th to March 5th 2017 (IN2017_V01; (Armand et al., 2018). This marine geoscience expedition, named the “Sabrina Sea Floor Survey”, focused notably on studying the interactions of the Totten Glacier with the Southern Ocean through multiple glacial cycles. The cores were collected using a multi-corer (MC), sliced every centimetre, wrapped up in plastic bags, and stored in the fridge. Back at the home laboratory (IMAS, UTAS, Hobart, Australia), sediment samples were dried in an oven at 40°C. Three hundred mg of dry sediment was then homogenised and vortexed for 10-sec with 12 mL of a reductive solution of 0.005M hydroxylamine hydrochloride (HH) / 1.5% Acetic Acid (AA) / 0.001M Na-EDTA / 0.033M NaOH, at pH 4 (Huang et al., 2021). The sediment was then leached a second time (to ensure the removal of all oxides and excess minerals, i.e. to isolate the detrital fraction) with 15 mL of 0.02M HH, 25% AA solution and agitated using a rotisserie (20 rpm) overnight (Wilson et al., 2018). Sample residues were then centrifuged, rinsed with Milli-Q water 3 times, and dried in an oven at 50°C. About 50 mg of resulting dry (detrital) sediment was ground, weighed into a Teflon vial, and digested with a strong acid mixture. First, the sediment was oxidized with a mixture of concentrated HNO3 and 30% H2O2 (1:1). Samples were then digested in open vials using 10 mL HNO3, 4 mL HCl, and 2 mL HF, at 180°C until close to dryness. Digested residues were converted to nitric form before being oxidised with a mixture of 1 mL HNO3 and 1 mL HClO4 at 220°C until fully desiccated. Samples were finally re-dissolved in 4 mL 7.5 M HNO3. A 400 μL aliquot was removed from the 4 mL digest solution and diluted ~2500 times in 1% HNO3 for rare earth elements (REE) analysis by Sector Field Inductively Coupled Mass Spectrometry (SF-ICP-MS, Thermo Fisher Scientific, Bremen, Germany) at the Central Science Laboratory (UTAS, Hobart, Australia). Element quantification was performed via external calibration using multi-element calibration solutions (MISA-5, QCD Analysts, Spring Lake, NJ, USA). Samples were introduced to the instrument using an Aridius® II desolvating nebulizer (CETAC Technologies, USA). The DSN was tuned daily, and oxide formation for a range of test analytes (Ba, Ce, U etc) was always less than 0.05%. Isotopes 137Ba, 139La, 140Ce, 141Pr, 146Nd, 150Nd, 147Sm, 153Eu, 158Gd, 159Tb, 163Dy, 165Ho, 166Eu, 169Tm, 172Yb and 175Lu were monitored in low resolution mode. Raw intensities were blank and dilution corrected. References - Armand, L. K., O’Brien, P. E., Armbrecht, L., Baker, H., Caburlotto, A., Connell, T., … Young, A. (2018). Interactions of the Totten Glacier with the Southern Ocean through multiple glacial cycles (IN2017-V01): Post-survey report. ANU Research Publications - Huang, H., Gutjahr, M., Kuhn, G., Hathorne, E. C., and Eisenhauer, A. (2021). Efficient Extraction of Past Seawater Pb and Nd Isotope Signatures From Southern Ocean Sediments. Geochemistry, Geophysics, Geosystems, 22(3), 1–22. - Wilson, D. J., Bertram, R. A., Needham, E. F., van de Flierdt, T., Welsh, K. J., McKay, R. M., … Escutia, C. (2018). Ice loss from the East Antarctic Ice Sheet during late Pleistocene interglacials. Nature, 561(7723), 383.

  • Zooplankton were collected during the winter-spring transition during two cruises of the Aurora Australis: SIPEX in 2007 and SIPEX II in 2012. As part of the collections sea ice cores were collected to describe the ice habitat during the period of zooplankton collections. Ice cores were taken with a 20 cm diameter SIPRE corer and sectioned in the field with an ice core. Particulate organic matter (POM) and animals from the zooplankton (water column) and the sea ice cover (meiofauna) were processed for stable isotopes - delta 13 Carbon and delta 15 Nitrogen.

  • The heavy metal content of whole Paramoera walkeri (Eusiridae, Amphipoda) were measured from specimens collected and deployed in experimental mesocosms around Casey station during the summer of 2003/04. Data are the parts per million (ppm) concentrations of 45 heavy metals measured via acid digestion and ICP-MS analysis. P.walkeri were collected from an intertidal area on the northern side of O'Brien Bay and deployed in mesocosms (perforated sample jars housed within perforated 20 litre food buckets) suspended approximately three metres below the sea ice at four sites; two potentially impacted sites in Brown Bay and two control sites, O'Brien Bay and McGrady Cove. The experiment was run on three occasions during the summer each lasting two weeks. These data were collected as part of ASAC project 2201 (ASAC_2201 - Natural variability and human induced change in Antarctic nearshore marine benthic communities). See also other metadata records by Glenn Johnstone for related information.