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University of California
Stable Isotope Laboratory
Earth and Planetary Sciences
1156 High Street Santa Cruz, CA 95064

Lab: (831) 459-5751
Office: (831) 459-5857
Fax: (831) 459-3074


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Dual-Inlet AutoCarbonate Device Overview

The Auto-Carbonate devices used at UCSC are either a common acid bath sampling peripheral or a individual sample acid-drip peripheral used to measure:

  • δ18O and δ13C of calcium carbonate.

  • At UCSC, the Auto-carbonate is primarily used to simultaneously measure δ18O and δ13C of calcium carbonate formainiferal tests and of bulk ocean sediments. The facility also regularly measures δ18O and δ13C of bioapatites (i.e., bone and teeth).



    Automated Carbonate Device Rates


    Dual Inlet: Automated Carbonate Device

      Isotope Phase Optimum
    Quantity
    Measurement
    Precision
    Cost per Sample
    Internal* External
    Carbonate Device δ13C Solid 50 µg ± 0.05 ‰ $13.00 $20.02
    δ18O Solid 50 µg ± 0.08 ‰ $13.00 $20.02
    δ18O, δ13C Solid 50 µg ± 0.08 ‰ $13.00 $20.02
    Sample Types: Biogenic and inorganic minerals (e.g., Calcium carbonate).
    * An additional 54% University of California overhead (indirect) charge is automatically taken
    from UC based grants when paying for these samples.
    For samples that require sample processing above normal an additional assisted rate of
    $4.50/sample ($6.91/sample external) may be charged.

    Analysis


    Prism Instrument:

    Solid samples are analyzed for δ18O and δ13C isotopes by acid digestion using an automated common acid bath carbonate device interfaced to either a Fisons Prism III dual-inlet isotope ratio mass spectrometer (IRMS). Samples are reacted at 90°C in orthophosphoric acid (specific gravity = 1.92 g/cm3) to generate carbon dioxide and water. Water is cryogenically removed from CO2 and non-condensible gases are pumped away, prior to introduction of the purified CO2 into the IRMS.

    During a run sequence, calibrated in-house standard Carrera Marble is used to correct the data including a drift correction. Two NBS-19 limestone samples are run "as-a-sample" to monitor quality control and long term performance. Carrera Marble has been extensively calibrated against NIST Standard Reference Materials (NBS-19, NBS-18, and LSVEC) and as part of intercomparison studies with other stable isotope laboratories.

    Kiel-253 Instrument:

    Solid samples are analyzed for δ18O and δ13C isotopes by acid digestion using an individual vial acid drop ThemoScientific Kiel IV carbonate device interfaced to ThermoScientific MAT-253 dual-inlet isotope ratio mass spectrometer (IRMS). Samples are reacted at 75°C in orthophosphoric acid (specific gravity = 1.92 g/cm3) to generate carbon dioxide and water. Water is cryogenically removed from CO2 and non-condensible gases are pumped away, prior to introduction of the purified CO2 into the IRMS.

    During a run sequence, calibrated in-house standard Carrera Marble is used to correct the data including a drift correction. Four NBS-18 limestone standards are used in conjunction with Carrera Marble to correct for instrument specific source ionization effects. Two NBS-19 limestone samples are run "as-a-sample" to monitor quality control and long term performance. Carrera Marble has been extensively calibrated against NIST Standard Reference Materials (NBS-19, NBS-18, and LSVEC) and as part of intercomparison studies with other stable isotope laboratories.

    Corrected delta values are expressed relative to international standards PDB (PeeDee Belemnite) for δ13C and δ18O.


    Sample Preparation Guidelines


    Sample Size: For pure calcium carbonate measurements sample sizes of 50-70 µg is optimal. Samples should be kept to under 200 µg and greater than 20 µg for best results. For smaller samples, contact the lab manager to discuss your circumstances. Samples as small as 5 µg have been reliably measured. For bulk sediment samples an estimate of percent inorganic carbon is useful to ensure a proper amount of sample is run.

    Submitting powdered samples: Static charge on fine grained powdered samples can be a problem because the static charges can make it difficult to remove powdered samples from plastic polyvials. Some people have found Eppendorf 0.2ml PCR tubes (thin walled, VWR # 951010006) work well. Alternatively, placing the samples in "origami" wrapped pouches eliminates the charge problem. HOWEVER: we have experienced issues with using weighing paper (sample loss) and strongly recommend aluminum foil packets instead, yet this approach does not always yield recovery. Pack samples in the dull side of the foil. The shiny side has oil resides and powders stick. View the wrapping technique here: Origami sample packets tutorial.


    Sample Submission:

    Two Steps:

    1) Contact the UCSC-SIL laboratory manager to discuss your analyses and whether the UCSC-SIL is an appropriate facility for your analysis needs (i.e., can we measure your samples in a reasonable time frame, do we have the expertise to properly measure your samples, etc...).
    2) Once confirmation with the laboratory manager has been arranged please fill out a sample submission form.

    Shipping Info:

    UCSC - Earth and Planetary Sciences
    Stable Isotope Laboratory
    1156 High Street, E&MS C512
    Santa Cruz, CA 95064
    Phone: 831-459-5857