A bulk extraction method to determine the stable isotope ratios of iron, nickel, copper, zinc, and cadmium in seawater using multi-collector inductively coupled plasma mass spectrometry
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Abstract: The oceanic trace metals iron (Fe), nickel (Ni), copper (Cu), zinc (Zn), and cadmium (Cd) are crucial to marine phytoplankton growth and global carbon cycle, and the analysis of their stable isotopes can provide valuable insights into their biogeochemical cycles within the ocean. However, the simultaneous isotopic analysis of multiple elements present in seawater is challenging because of their low concentrations, limited volumes of the test samples, and high salt matrix. In this study, we present the novel method developed for the simultaneous analysis of five isotope systems by 1 L seawater sample. In the developed method, the NOBIAS Chelate-PA1 resin was used to extract metals from seawater, the AG MP-1M anion-exchange resin to purify Cu, Fe, Zn, Cd, and the NOBIAS Chelate-PA1 resin to further extract Ni from the matrix elements. Finally, a multi-collector inductively coupled plasma mass spectroscope (MC-ICPMS) was employed for the isotopic measurements using a double-spike technique or sample-standard bracketing combined with internal normalization. This method exhibited low total procedural blanks (0.04 pg, 0.04 pg, 0.21 pg, 0.15 pg, and 3 pg for Ni, Cu, Fe, Zn, and Cd, respectively) and high extraction efficiencies (100.5% ± 0.3%, 100.2% ± 0.5%, 97.8% ± 1.4%, 99.9% ± 0.8%, and 100.1% ± 0.2% for Ni, Cu, Fe, Zn, and Cd, respectively). The external errors and external precisions of this method could be considered negligible. The proposed method was further tested on the seawater samples obtained from the whole vertical profile of a water column during the Chinese GEOTRACES GP09 cruise in the Northwest Pacific, and the results showed good agreement with previous related data. This innovative method will contribute to the advancement of isotope research and enhance our understanding of the marine biogeochemical cycling of Fe, Ni, Cu, Zn, and Cd.
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Key words:
- trace metal /
- stable isotopes /
- seawater /
- bulk extraction
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Figure 1. Elution scheme for sample purification using an AG MP-1M resin microcolumn (a) and a NOBIAS Chelate-PA1 resin microcolumn (b). For the detailed protocols, see Table 2.
Figure 2. δ56Fe, δ60Ni, δ65Cu, δ66Zn, and δ114Cd values in ultrapure water doped with varying concentrations of natural isotope standards (IRMM-524a Fe, NIST-986 Ni, NIST-647 Cu, NIST-3702 Zn, and NIST-3108 Cd) measured according to the proposed method. Each concentration measurement included five replicates. Error bars represent the internal errors (1σ).
Figure 3. Theoretical (gray line) versus measured (black points) 1σ internal errors of all samples for δ56Fe, δ60Ni, δ66Zn, and δ114Cd as compared to the MC-ICPMS signal. Theoretical lines were drawn based on Monte Carlo simulations. Vertical gray bars denote the seawater concentrations corresponding to 0.1‰ and 0.05‰ 1σ internal errors. Light blue rectangles indicate the range of signal intensities that correspond to 1 L nature seawater samples following their pretreatment based on the proposed method (de Baar et al., 1994; Moore and Braucher, 2007; Roshan et al., 2018; Richon and Tagliabue, 2019; John et al., 2022).
Figure 4. External precisions for δ56Fe, δ60Ni, δ65Cu, δ66Zn, and δ114Cd based on repeated pretreatment and analysis of a single seawater sample. The seawater sample was obtained at 34.88°N, 121.68°E from a depth of ~15 m during the Yellow Sea cruise (March/April 2022). Error bars represent the internal errors (1σ), while lines and gray bars depict the average isotope values and external precisions (average ± 1 SD), respectively.
Figure 5. Concentrations and stable isotope profiles of the samples collected at Station K9 (11°N, 150°E) along the GEOTRACES cruise GP09 in the Northwest Pacific compared with the GR19 and GR21 profiles obtained from the GEOTRACES Intermediate Data Product 2021 during the GP19 cruise (
https://www.bodc.ac.uk/geotraces/data/idp2021/ ), SAFe Station (30°N, 140°W) in the Northeast Pacific (Conway and John, 2015a), and GR03 Station (15°N, 165°E) in the Northwest Pacific (Takano et al., 2022). Error bars represent the 1σ internal errors of the isotopic analysis.Table 1. Protocol for preconcentration of Ni, Cu, Fe, Zn and Cd by NOBIAS Chelate-PA1 resin
Step Collection a. Add 61Ni–62Ni, 57Fe–58Fe, 64Zn–67Zn, 110Cd–111Cd double spikes to 1 L seawater sample (pH = 2; 1 mmol/L H2O2) 72 h before
extraction− b. Add 3 mL pre-cleaned resin in sample; shake for >5 h (Fe) − c. Adjust pH to 6.15 ± 0.2 with CH3CHOONH4 and NH3·H2O; shake for >5 h (Ni, Cu, Zn, Cd) − d. Load sample through filter to separate resin salts e. Rinse resin with 125 mL ultrapure water salts f. Elute metals with (5 × 5) mL 3 mol/L HNO3 metals g. Evaporate samples at 200℃; redigest using 100 µL 16 mol/L HNO3 and 100 µL 10 mol/L HCl to dissolve organics for >2 h − h. Evaporate samples at 200℃; redissolve in 200 μL 11 mol/L acetic acid + 4 mol/L HCl + 0.003% H2O2 for purification − Note: − represents no data. 
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Table 2. Protocol for purification of Ni, Cu, Fe, Zn and Cd for MC-ICPMS isotopic analysis
AG MP-1M purification step for Cu, Fe, Zn, Cd Step Reagent Volume/µL Collection Load AG MP-1M resin into PTFE microcolumns Milli-Q water 20 − Clean column 2 mol/L HNO3 250 × 4 − Rinse ultrapure water 100 × 5 − Condition 11 mol/L HAc + 4 mol/L HCl + 0.003% H2O2 100 × 2 − Load sample 11 mol/L HAc + 4 mol/L HCl + 0.003% H2O2 200 Ni, Cr, V, salts Elute Ni + salts 11 mol/L HAc + 4 mol/L HCl + 0.003% H2O2 20 × 7 Ni, Cr, V, salts Elute Cu 5 mol/L HCl + 0.003% H2O2 20 × 20 Cu, Mn, Pb, Co Elute Fe 1 mol/L HCl 20 × 9 Fe Elute Zn 2 mol/L HNO3 + 0.1 mol/L HBr 20 × 12 Zn Elute Cd 2 mol/L HNO3 20 × 10 Cd NOBIAS Chelate-PA1-Ni purification step Step Reagent Volume/µL Collection Load NOBIAS Chelate-PA1 resin into PTFE microcolumns Milli-Q water 20 − Clean column 2 mol/L HNO3 250 × 4 − Rinse ultrapure water 100 × 2 − Condition 0.05 mol/L NH4Ac (pH = 6) 100 × 2 − Load sample 0.05 mol/L NH4Ac (pH = 6) 200 salts, Cr Elute salts 0.006 mol/L NH4Ac (pH = 6) 20 × 7 salts Elute Ni 2 mol/L HNO3 20 × 7 Ni Note: Reconstitution steps: (1) evaporate; (2) redigest using 200 µL 16 mol/L HNO3 and 100 µL 30% H2O2 at 160℃ to dissolve organics for >6 h; (3) evaporate; (4) redissolve in 0.1 mol/L HNO3 in 15 mL LDPE tubes for isotopic analysis. LDPE: low-density polyethylene; PTFE: polytetrafluoroethylene. − represents no data.
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Table 3. Cup configurations for Ni, Cu, Fe, Zn, Cd, and Fe isotopic analysis by Neptune MC-ICPMS
Faraday cup position L4 L3 L2 L1 C H1 H2 H3 H4 Ni (HR) − 57Fe 58Ni − 60Ni 61Ni 62Ni − − Cu (LR) − − 63Cu 64Zn 65Cu 66Zn 67Zn 68Zn − Fe (HR) − 53Cr 54Fe − 56Fe 57Fe 58Fe − 60Ni Zn (HR) − 62Ni − 64Zn − 66Zn 67Zn 68Zn − Cd (LR) − 105Pd − 110Cd 111Cd 112Cd 114Cd − 117Sn Note: Isotopes used in isotope ratios are bolded, while spiked isotopes are underlined. − represents no data.
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Table 4. The blanks (ng) in pretreatment steps of NOBIAS Chelate-PA1 resin extraction, AG MP-1M resin purification, NOBIAS Chelate-PA1 resin Ni purification, and total procedure (±1SD, n = 5)
Element Extraction AG MP-1M purification NOBIAS Chelate-PA1-Ni purification Total procedure Reference comparison Ni 0.04 ± 0.04 0.022 ± 0.000 0.004 ± 0.002 0.04 ± 0.05 ≤ 1b; 0.22c Cu 0.05 ± 0.03 0.007 ± 0.001 − 0.04 ± 0.02 ≤ 1b; 0.29c Fe 0.18 ± 0.10 0.069 ± 0.016 − 0.21 ± 0.20 1.1 ± 0.6a; 0.3d Zn 0.16 ± 0.11 0.010 ± 0.002 − 0.15 ± 0.10 0.53c; 0.06d Cd 0.001 ± 0.001 0.006 ± 0.003 − 0.003 ± 0.003 0.004d Note: Total procedure blanks from recent studies are used for comparison. a John and Adkins (2010); b Yang et al. (2020); c Takano et al. (2017); d Conway et al. (2013). − represents no data.
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Table 5. The recoveries in pretreatment steps of NOBIAS Chelate-PA1 resin extraction, AG MP-1M resin purification, and NOBIAS Chelate-PA1 resin Ni purification (±1SD, n = 5)
Element Extraction AG MP-1M
purificationNOBIAS Chelate-PA1-Ni
purificationNi 100.5% ± 0.3% 99.8% ± 0.2% 99.7% ± 0.3% Cu 100.2% ± 0.5% 99.5% ± 0.6% − Fe 97.8% ± 1.4% 99.1% ± 1.1% − Zn 99.9% ± 0.8% 99.5% ± 0.6% − Cd 100.1% ± 0.2% 99.7% ± 0.6% − Note: − represents no data.
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