Hostname: page-component-76fb5796d-22dnz Total loading time: 0 Render date: 2024-04-25T21:48:58.928Z Has data issue: false hasContentIssue false

SEQUENTIAL THERMAL ANALYSIS OF COMPLEX ORGANIC MIXTURES: PROCEDURAL STANDARDS AND IMPROVED CO2 PURIFICATION CAPACITY

Published online by Cambridge University Press:  21 March 2023

Ulrich M Hanke*
Affiliation:
NOSAMS Laboratory, Geology and Geophysics, Woods Hole Oceanographic Institution, 266 Woods Hole Road, Woods Hole, MA, 02543 USA Marine Chemistry and Geochemistry, Woods Hole Oceanographic Institution, 266 Woods Hole Road, Woods Hole, MA, 02543 USA
Alan R Gagnon
Affiliation:
NOSAMS Laboratory, Geology and Geophysics, Woods Hole Oceanographic Institution, 266 Woods Hole Road, Woods Hole, MA, 02543 USA
Christopher M Reddy
Affiliation:
Marine Chemistry and Geochemistry, Woods Hole Oceanographic Institution, 266 Woods Hole Road, Woods Hole, MA, 02543 USA
Mary C Lardie Gaylord
Affiliation:
NOSAMS Laboratory, Geology and Geophysics, Woods Hole Oceanographic Institution, 266 Woods Hole Road, Woods Hole, MA, 02543 USA
Anne J Cruz
Affiliation:
NOSAMS Laboratory, Geology and Geophysics, Woods Hole Oceanographic Institution, 266 Woods Hole Road, Woods Hole, MA, 02543 USA
Valier Galy
Affiliation:
Marine Chemistry and Geochemistry, Woods Hole Oceanographic Institution, 266 Woods Hole Road, Woods Hole, MA, 02543 USA
Roberta L Hansman
Affiliation:
NOSAMS Laboratory, Geology and Geophysics, Woods Hole Oceanographic Institution, 266 Woods Hole Road, Woods Hole, MA, 02543 USA
Mark D Kurz
Affiliation:
NOSAMS Laboratory, Geology and Geophysics, Woods Hole Oceanographic Institution, 266 Woods Hole Road, Woods Hole, MA, 02543 USA Marine Chemistry and Geochemistry, Woods Hole Oceanographic Institution, 266 Woods Hole Road, Woods Hole, MA, 02543 USA
*
*Corresponding author. Email: uhanke@whoi.edu

Abstract

Sequential thermal analysis allows for deconvoluting the refractory nature and complexity of carbon mixtures embedded in mineral matrices for subsequent offline stable carbon and radiocarbon (14C) isotope analyses. Originally developed to separate Holocene from more ancient sedimentary organic matter to improve dating of marine sediments, the Ramped Pyrolysis and Oxidation (RPO) apparatus, or informally, the “dirt burner” is now used to address pressing questions in the broad field of biogeochemistry. The growing interest in the community now necessitates improved handling and procedures for routine analyses of difficult sample types. Here we report on advances in CO2 purification during sample processing, modifications to the instrumentation at the National Ocean Sciences Accelerator Mass Spectrometry (NOSAMS) facility, and introduce sodium bicarbonate procedural standards with differing natural abundance 14C signatures for blank assessment. Measurements from different environmental samples are used to compare the procedure to the different generations of sequential thermal analyses. With this study, we aim to improve the standardization of the procedures and prepare this instrumentation for innovations in online stable carbon isotopes and direct AMS-interface measurements in the future.

Type
Research Article
Copyright
© The Author(s), 2023. Published by Cambridge University Press for the Arizona Board of Regents on behalf of the University of Arizona

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

REFERENCES

Bao, R, McNichol, AP, Hemingway, JD, Lardie Gaylord, MC, Eglinton, TI. 2019. Influence of different acid treatments on the radiocarbon content spectrum of sedimentary organic matter determined by RPO/accelerator mass spectrometry. Radiocarbon 61(2):395413.CrossRefGoogle Scholar
Bao, RM, Strasser, M, McNichol, AP, Haghipour, N, McIntyre, C, Wefer, G, Eglinton, TI. 2018. Tectonically-triggered sediment and carbon export to the Hadal zone. Nature Communications 9(1):18.CrossRefGoogle Scholar
Cruz, AJ, Gagnon, AR, McNichol, AP, Burton, JR, Elder, KL, Lardie, GMC, Gospodinova, KD, Hlavenka, J, Kurz, MD, Longworth, BE, Roberts, ML, Trowbridge, NY, Walther, T, Xu, L. 2017. Advances in sample preparation at the National Ocean Sciences Accelerator Mass Spectrometry Facility (NOSAMS): Investigation of Carbonate Secondary Standards.Google Scholar
Currie, LA, Benner, BA, Cachier, HA, Cary, R, Chow, JC, Urban, DL, Eglinton, TI, Gustafsson, O, Hartmann, PC, Hedges, JI, et al. 2002. A critical evaluation of interlaboratory data on total, elemental, and isotopic carbon in the carbonaceous particle reference material, NIST SRM 1649a. Journal of Research of the National Institute of Standards and Technology 107(3):279298.CrossRefGoogle ScholarPubMed
Fernandez, A, Santos, GM, Williams, EK, Pendergraft, MA, Vetter, L, Rosenheim, BE. 2014. Blank corrections for ramped pyrolysis radiocarbon dating of sedimentary and soil organic carbon. Analytical Chemistry 86(24):1208512092.CrossRefGoogle ScholarPubMed
Grant, KE, Galy, VV, Chadwick, OA, Derry, LA. 2019. Thermal oxidation of carbon in organic matter rich volcanic soils: insights into SOC age differentiation and mineral stabilization. Biogeochemistry 144(3):291304.CrossRefGoogle Scholar
Haghipour, N, Ausin, B, Usman, MO, Ishikawa, N, Wacker, L, Welte, C, Ueda, K, Eglinton, TI. 2019. Compound-specific radiocarbon analysis by elemental analyzer-accelerator mass spectrometry: precision and limitations. Analytical Chemistry 91(3):20422049.CrossRefGoogle ScholarPubMed
Hanke, UM, Wacker, L, Haghipour, N, Schmidt, MWI, Eglinton, TI, McIntyre, CP. 2017. Comprehensive radiocarbon analysis of benzene polycarboxylic acids (BPCAs) derived from pyrogenic carbon in environmental samples. Radiocarbon 59(4):11031116.CrossRefGoogle Scholar
Hedges, JI, Eglinton, G, Hatcher, PG, Kirchman, DL, Arnosti, C, Derenne, S, Evershed, RP, Kögel-Knabner, I, De Leeuw, JW, Littke, R, Michaelis, W, Rullkötter, J. 2000. The molecularly-uncharacterized component of nonliving organic matter in natural environments. Organic Geochemistry 31(10):945958.CrossRefGoogle Scholar
Hemingway, JD, Galy, VV, Gagnon, AR, Grant, KE, Rosengard, SZ, Soulet, G, Zigah, PK, McNichol, AP. 2017a. Assessing the blank carbon contribution, isotope mass balance, and kinetic isotope fractionation of the ramped pyrolysis/oxidation instrument at nosams. Radiocarbon 59(1):179193.CrossRefGoogle Scholar
Hemingway, JD, Hilton, RG, Hovius, N, Eglinton, TI, Haghipour, N, Wacker, L, Chen, MC, Galy, VV. 2018. Microbial oxidation of lithospheric organic carbon in rapidly eroding tropical mountain soils. Science 360(6385):209212.CrossRefGoogle ScholarPubMed
Hemingway, JD, Rothman, DH, Grant, KE, Rosengard, SZ, Eglinton, TI, Derry, LA, Galy, VV. 2019. Mineral protection regulates long-term global preservation of natural organic carbon. Nature 570(7760):228231.CrossRefGoogle ScholarPubMed
Hemingway, JD, Rothman, DH, Rosengard, SZ, Galy, VV. 2017b. Technical note: an inverse method to relate organic carbon reactivity to isotope composition from serial oxidation. Biogeosciences 14(22):50995114.CrossRefGoogle Scholar
NIST. 2007. Certificate of Analysis Standard Reference Material 1649a. National Institute of Standards and Technology.Google Scholar
Peralta, O, Baumgardner, D, Raga, GB. 2007. Spectrothermography of carbonaceous particles. Journal of Atmospheric Chemistry 57(2):153169.CrossRefGoogle Scholar
Plante, A, Beaupré, SR, Robert, ML, Baisden, T. 2013. Distribution of radiocarbon ages in soil organic matter by thermal fractionation. Radiocarbon 55(2–3):10771083.CrossRefGoogle Scholar
Roberts, ML, Elder, KL, Jenkins, WJ, Gagnon, AR, Xu, L, Hlavenka, JD, Longworth, BE. 2019. 14C blank corrections for 25–100 μg samples at the National Ocean Sciences AMS Laboratory. Radiocarbon 61(5):14031411.CrossRefGoogle Scholar
Rogers, KL, Bosman, SH, Lardie-Gaylord, M, McNichol, A, Rosenheim, BE, Montoya, JP, Chanton, JP. 2019. Petrocarbon evolution: ramped pyrolysis/oxidation and isotopic studies of contaminated oil sediments from the Deepwater Horizon oil spill in the Gulf of Mexico. PLoS One 14(2):121.CrossRefGoogle ScholarPubMed
Rosenheim, BE, Day, MB, Domack, E, Schrum, H, Benthien, A, Hayes, JM. 2008. Antarctic sediment chronology by programmed-temperature pyrolysis: methodology and data treatment. Geochemistry, Geophysics, Geosystems 9(4):116.CrossRefGoogle Scholar
Sanderman, J, Grandy, SA. 2020. Ramped thermal analysis for isolating biologically meaningful soil organic matter fractions with distinct residence times. Soil 6(1):131144.CrossRefGoogle Scholar
Santos, GM, Southon, JR, Drenzek, NJ, Ziolkowski, LA, Druffel, ERM, Xu, X, Zhang, D, Trumbore, SE, Eglinton, TI, Hughen, KA. 2010. Blank assessment for ultra-small radiocarbon samples: chemical extraction and separation versus AMS. Radiocarbon 52(2–3):13221335.CrossRefGoogle Scholar
Santos, GM, Southon, JR, Griffin, S, Beaupre, SR, Druffel, ERM. 2007. Ultra small-mass AMS 14C sample preparation and analyses at KCCAMS/UCI facility. Nuclear Instruments and Methods in Physics Research B 259(1):293302.CrossRefGoogle Scholar
Slater, GF, White, HK, Eglinton, TI, Reddy, CM. 2005. Determination of microbial carbon sources in petroleum contaminated sediments using molecular 14C analysis, Environmental Science and Technology 39(8):25522558.CrossRefGoogle ScholarPubMed
Subt, C, Yoon, HI, Yoo, KC, Lee, JI, Leventer, A, Domack, EW, Rosenheim, BE. 2017. Publications, Geochemistry, Geophysics, Geosystems 18:14041418.CrossRefGoogle Scholar
Venturelli, RA, Siegfried, MR, Roush, KA, Li, W, Burnett, J, Zook, R, Fricker, HA, Priscu, JC, Leventer, A, Rosenheim, BE. 2020. Mid-Holocene grounding line retreat and readvance at Whillans Ice Stream, West Antarctica. Geophysical Research Letters 47(15):111.CrossRefGoogle Scholar
Walker, BD, Xu, X. 2019. An improved method for the sealed-tube zinc graphitization of microgram carbon samples and 14C AMS measurement, Nuclear Instruments and Methods in Physics Research, Section B 438:5865.CrossRefGoogle Scholar
White, HK, Xu, L, Hartmann, P, Quinn, JG, Reddy, CM. 2013. Unresolved complex mixture (UCM) in coastal environments is derived from fossil sources. Environmental Science and Technology 47(2):726731.CrossRefGoogle ScholarPubMed
White, HK, Xu, L, Lima, ALC, Eglinton, TI, Reddy, CM. 2005. Abundance, composition, and vertical transport of PAHs in marsh sediments. Environmental Science and Technology 39(21):82738280.CrossRefGoogle ScholarPubMed
Xu, L, Roberts, ML, Elders, KL, Kurz, MD, McNichol, AP, Reddy, CM, Ward, CP, Hanke, UM. 2021. Radiocarbon in dissolved organic carbon by UV oxidation: procedures and blank characterization at NOSAMS. Radiocarbon 63(1):357374.CrossRefGoogle Scholar
Zhang, X, Bianchi, TS, Cui, X, Rosenheim, BE, Ping, CL, Hanna, AJM, Kanevskiy, M, Schreiner, KM, Allison, MA. 2017. Permafrost organic carbon mobilization from the watershed to the Colville River delta: evidence from 14C ramped pyrolysis and lignin biomarkers, Geophysical Research Letters 44(22):11,491–11,500.CrossRefGoogle Scholar
Zigah, PK, Minor, EC, McNichol, AP, Xu, L, Werne, JP. 2017. Constraining the sources and cycling of dissolved organic carbon in a large oligotrophic lake using radiocarbon analyses. Geochimica et Cosmochimica Acta 208(April):102118.CrossRefGoogle Scholar
Supplementary material: File

Hanke et al. supplementary material

Hanke et al. supplementary material

Download Hanke et al. supplementary material(File)
File 352.2 KB