Quality assurance

Research enabled under the BIOGRIP facilities ensure strict quality control guidelines are adhered towards. This is to ensure the quality control standards upheld are set to internationally recognised standards.

Isotope Node

Laser Ablation and High-resolution Facility (LA-ICP-MS Lab)

The Laser Ablation and High-resolution Facility (LA-ICP-MS Lab) at the University of Cape Town specialises in high-precision elemental and isotopic analysis using laser ablation coupled with inductively coupled plasma mass spectrometry (LA-ICP-MS).

Trace element analysis

NIST SRM 610 is used as a calibration standard and various in-house standards (CPX, OPX, garnet) are analysed throughout laser sessions to ensure data accuracy. Sample standard bracketing at regular intervals allows for correction of instrumental drift. Data reduction is carried out in LADR (Danyushevsky & Norris 2018) which calculates the overall uncertainty budget and provides uncertainty estimates tailored for different applications, including intra-run, intra-laboratory, and inter-laboratory comparisons.

U-Pb carbonate geochronology

NIST612 or 614 (dependent on sample U concentrations) Matrix-matched reference materials (RM):  WC-1 (Roberts et al. 2017), ASH-15D (Nuriel et al. 2021) and RM RA138 (Guillong et al. 2024, under development in collaboration with ETH Zurich). NIST and RM sample blocks are analysed throughout each session to monitor accuracy and correct for instrumental drift and downhole fractionation. Data reduction is performed using Iolite software (Paton et al. 2011), utilising custom data reduction schemes that apply inter-element fractionation corrections (and common-Pb corrections where applicable). Instrument stability is monitored through session-specific metrics such as signal intensity and baseline stability, with documented logs maintained for all runs. All data are subject to internal review for concordance, precision, and comparison to expected values, ensuring that the laboratory delivers data of consistently high analytical quality.

References

Danyushevsky, L., & Norris, A. (2018). Software and protocols for improved accuracy of LA-ICP-MS analysis via quantification of matrix effects. Goldschmidt Conference Abstracts (Boston), 513.

Guillong, M., Samankassou, E., Müller, I. A., Szymanowski, D., Looser, N., Tavazzani, L., Merino-Tomé, Ó., Bahamonde, J. R., Buret, Y., & Ovtcharova, M. (2024). Technical note: RA138 calcite U–Pb LA-ICP-MS primary reference material. Geochronology, 6(3), 465–474. https://doi.org/10.5194/gchron-6-465-2024

Nuriel, P., Wotzlaw, J.-F., Ovtcharova, M., Vaks, A., Stremtan, C., Šala, M., Roberts, N. M. W., & Kylander-Clark, A. R. C. (2021). The use of ASH-15 flowstone as a matrix-matched reference material for laser-ablation U − Pb geochronology of calcite. Geochronology, 3(1), 35–47. https://doi.org/10.5194/gchron-3-35-2021

Paton, C., Hellstrom, J., Paul, B., Woodhead, J., & Hergt, J. (2011). Iolite: Freeware for the visualisation and processing of mass spectrometric data. Journal of Analytical Atomic Spectrometry, 26, 2508–2518. https://doi.org/10.1039/C1JA10172B

Roberts, N. M. W., Rasbury, E. T., Parrish, R. R., Smith, C. J., Horstwood, M. S. A., & Condon, D. J. (2017). A calcite reference material for LA‐ICP‐MS U‐Pb geochronology. Geochemistry, Geophysics, Geosystems, 18(7), 2807–2814. https://doi.org/10.1002/2016gc006784

Stable Light Isotope Lab

The Stable Light Isotope Laboratory at the University of Cape Town at the University of Cape Town is one of only a few on the African continent, provides state-of-the-art and routine stable light isotope analyses. The facility hosts three light isotope ratio mass spectrometers (IRMS), a Delta Plus XP and two Delta V instruments interfaced with peripherals such as elemental analysers and gas benches as well as a tunable infrared laser direct absorption spectrometer (Aerodyne Research, Inc., USA) (TILDAS) for high precision measurements of CO₂ isotopologues.

Delta XP

The Delta XP delivers high-precision isotope measurements, with 1σ (1 sigma) standard deviations of ±0.1‰ for δ¹³C and ±0.1‰ for δ¹⁸O, based on repeated analyses of a homogenous carbonate internal standard.

Delta V instruments

The Delta V delivers high-precision isotope measurements, with 1σ (1 sigma) standard deviations of ±0.2‰ for δ¹³C and ±0.2‰ for δ¹⁵N, based on repeated analyses of a homogenous protein internal standard.

TILDAS

Quality control protocols for TILDAS-based measurements of triple oxygen isotopes in CO₂ integrate emerging community standards and methodologies to ensure precision, accuracy, and long-term reproducibility. Every sixth sample run is a carbonate reference material—either NBS18 or IAEA603—interleaved systematically to monitor instrumental drift, facilitate correction of scale compression, and track analytical stability. This bracketing strategy is consistent with best practices reported by Hare et al. (2022), Perdue et al. (2022), and Bajnai et al (2023), who demonstrated that regular reference measurements are critical for achieving sub-per mil precision in Δ′¹⁷O determinations. Known-unknown materials with independently established δ¹⁸O and Δ′¹⁷O values are also run routinely to assess method accuracy and internal reproducibility over time, providing a second tier of quality control.

Corrections for the concentration dependence of isotopic measurements, particularly as it affects δ¹⁸O and δ¹⁷O via pressure broadening and baseline offsets, are implemented following approaches outlined in Hare et al. (2022), Steur et al. (2021) and Bajnai et al. (2023). These corrections are derived from in-house calibration curves using dilutions of reference CO₂ and are applied on a per-sample basis. In addition, UCT participates in international interlaboratory exercises, including IAEA-led triple oxygen isotope intercomparison campaigns, which help benchmark performance against global standards and ensure metrological traceability. This external validation complements internal data scrutiny—such as monitoring of acid digestion yields, spectral residuals and concentration-normalised Xp values (cf. Griffith, 2012)—to flag and exclude outliers and maintain the integrity of the analytical dataset.

References

Bajnai, D., Pack, A., Arduin Rode, F., Seefeld, M., Surma, J., & Di Rocco, T. (2023). A Dual Inlet System for Laser Spectroscopy of Triple Oxygen Isotopes in Carbonate‐Derived and Air CO2. Geochemistry, Geophysics, Geosystems, 24(10), e2023GC010976. https://doi.org/10.1029/2023GC010976

Griffith, D. W. T., Deutscher, N. M., Caldow, C., Kettlewell, G., Riggenbach, M., & Hammer, S. (2012). A Fourier transform infrared trace gas and isotope analyser for atmospheric applications. Atmospheric Measurement Techniques, 5(10), 2481-2498. https://doi.org/10.5194/amt-5-2481-2012

Hare, V. J., Dyroff, C., Nelson, D. D., & Yarian, D. A. (2022). High-precision triple oxygen isotope analysis of carbon dioxide by tunable infrared laser absorption spectroscopy. Analytical Chemistry, 94(46), 16023-16032. https://doi.org/10.1021/acs.analchem.2c03005

Perdue, N., Sharp, Z., Nelson, D., Wehr, R. and Dyroff, C., (2022). A rapid high‐precision analytical method for triple oxygen isotope analysis of CO2 gas using tunable infrared laser direct absorption spectroscopy. Rapid Communications in Mass Spectrometry, 36(21), p.e9391. https://doi.org/10.1002/rcm.9391

Steur, P.M., Scheeren, H.A., Nelson, D.D., McManus, J.B. and Meijer, H.A., (2021). Simultaneous measurement of δ 13 C, δ 18 O and δ 17 O of atmospheric CO 2–performance assessment of a dual-laser absorption spectrometer. Atmospheric Measurement Techniques, 14(6), pp.4279-4304. https://doi.org/10.5194/amt-14-4279-2021

Multicollector ICP-MS Lab

The Multicollector ICP-MS Lab is equipped with state-of-the-art instrumentation for high-precision isotopic and elemental analyses. All isotope data generated in are referenced to published value for bracketing analyses of international isotope standards: SRM987 87Sr/86Sr 0.710255 (Waight et al., 2022); JNdi-1 143Nd/144Nd 0.512115 (Tanaka et al., 2000); 208Pb/204Pb 36.7219, 207Pb/204Pb 15.4963, 206Pb/204Pb 16.9405 (Galer & Abouchami, 1998). In-house and international reference materials with known, published isotope compositions are processed as known unknowns with each batch of samples, and serves to assess data quality and accuracy.

Long-term results for selected materials

In-house carbonate material

NM95: 0.708909 ± 0.000038; n = 932

In-house ashed plant material

Namiso 316: 0.720503 ± 0.00003; n = 89

Laser ablation clinopyoxene reference

SRM 1400 : 0.713122 ± 0.000036; n = 53

SRM 1515: 0.713960 ± 0.000062; n = 38

JJG1424: 0.70482 ± 0.00029; n=155

Total procedural blanks are processed with every second batch of unknown samples, and the typical range of elemental background values are Sr < 250pg, Nd < 50pg and Pb < 200pg.

References

Galer, S. J. G., & Abouchami, W. (1998). Practical application of lead triple spiking for correction of instrumental mass discrimination. Mineral. Mag. A, 62, 491-492. Tanaka T, et al. (2000) JNdi-1: a neodymium isotopic reference in consistency with LaJolla neodymium. Chemical Geology, 168, 279–281

Waight, T., Baker, J., & Peate, D. (2002). Sr isotope ratio measurements by double-focusing MC-ICPMS: techniques, observations and pitfalls. International Journal of Mass Spectrometry, 221(3), 229-244. https://doi.org/10.1016/S1387-3806(02)01016-3