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A protocol for preparing subfossil chironomid head capsules (Diptera: Chironomidae) for stable isotope analysis in paleoclimate reconstruction and considerations of contamination sources

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Abstract

Several techniques are available to examine the isotopic composition of historic lake waters, providing data that can subsequently be used to examine environmental changes. A recently-developed technique is the stable oxygen isotope analysis of subfossil chironomid (Diptera: Chironomidae) head capsules (mostly chitin) preserved in lake sediments. This technique involves a high Temperature Conversion Elemental Analyzer (TC/EA), which has been a relatively recent addition to the suite of online peripherals for analyzing the stable isotopic composition of organic samples. The highly precise and accurate 18O/16O and D/H measurements obtainable using the TC/EA with samples in the microgram range make this instrumentation suitable for studying geochemical and biological processes. Preparation of organic samples for isotopic analysis typically requires first weighing each sample into silver/tin capsules. These capsules can introduce oxygen and hydrogen contamination (a “blank effect”), which is especially problematic for analysis of small organic samples (e.g. less than 100 μg). Here we tested tin and silver capsules from two manufacturers and a range of sizes to assess contamination to small organic samples on the TC/EA. We also assessed how a method for cleaning silver capsules affected our analysis of commercial chitin. In general, capsules made of silver have less detectible oxygen than those made of tin, and capsules from the two manufacturers varied in their detectible oxygen. There was no detectable H contamination from silver capsules. In addition to our empirical findings, we present a model demonstrating the influence that contaminant oxygen can have on the δ18O of small organic samples. Sample mass becomes an important issue for such analyses. In light of our findings, we recommend a minimum sample mass ≥50 μg (approximately 120 whole chironomid head capsules) on a TC/EA-IRMS (Deltaplus XP system). Finally, we present a detailed protocol for preparing and transferring chironomid head capsules into silver capsules that minimizes the influence of contaminant oxygen. This protocol provides the paleo-community with another potential method for reconstructing paleoenvironments.

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References

  • Anderson L, Abbott MB, Finney BP (2001) Holocene climate inferred from oxygen isotope ratios in lake sediments, central Brooks Range, Alaska. Quatern Res 55:313–321

    Article  Google Scholar 

  • Bowen GJ, Chesson L, Nielson K, Cerling TE., Ehleringer JR (2005) Treatment methods for the determination of delta H-2 and delta O-18 of hair keratin by continuous-flow isotope-ratio mass spectrometry. Rapid Commun Mass Spectrom 19:2371–2378

    Article  Google Scholar 

  • Farquhar GD, Henry BK, Styles JM (1997) A rapid on-line technique for determination of oxygen isotope composition of nitrogen-containing organic matter and water. Rapid Commun Mass Spectrom 11:1554–1560

    Article  Google Scholar 

  • Gannes LZ, O’Brien DM, delRio CM (1997) Stable isotopes in animal ecology: Assumptions, caveats, and a call for more laboratory experiments. Ecology 78:1271–1276

    Article  Google Scholar 

  • Gannon JE (1971) Two counting cells for the enumeration of zooplankton micro-crustacea. Trans Am Microsc Soc 90:486–490

    Article  Google Scholar 

  • Grocke DR, Schimmelmann A, Elias S, Miller RF (2006) Stable hydrogen-isotope ratios in beetle chitin: preliminary European data and re-interpretation of North American data. Quat Sci Rev 25:1850–1864

    Article  Google Scholar 

  • Hu FS, Kaufman D, Yoneji S, Nelson D, Shemesh A, Huang Y, Tian J, Bond G, Clegg B, Brown T (2003) Cyclic variation and solar forcing of Holocene climate in the Alaskan subarctic. Science 301:1890–1893

    Article  Google Scholar 

  • Huang YS, Shuman B, Wang Y, Webb T (2004) Hydrogen isotope ratios of individual lipids in Lake sediments as noval traces of climatic and environmental change: a surface sediment test. J Paleolimnol 31:363–375

    Article  Google Scholar 

  • ISOGEOCHEM Listserv archive (7/19/2006) Discussion on Silver/tin capsules on TC/EA, http://list.uvm.edu/cgi-bin/wa?A2=ind0607&L=ISOGEOCHEM&P=R9033&m=10516; Item number 014851-014857. Last accessed on September 24th 2007

  • ISOGEOCHEM Listserv archive (7/21/2006) Discussion on Silver/tin capsules on TC/EA, http://list.uvm.edu/cgi-bin/wa?A2=ind0607&L=ISOGEOCHEM&P=R10325&X=114D1F48358F04D4B1&Y=ftyw%40uaf.edu&m=14625; Item number 014870. Last accessed on September 24th 2007

  • Kelly SD, Parker IG, Sharman M, Dennis MJ (1998) On-line quantitative determination of H-2/H-1 isotope ratios in organic and water samples using an elemental analyzer coupled to an isotope ratio mass spectrometer. J Mass Spectrom 33:735–738

    Article  Google Scholar 

  • Kornexl BE, Gehre M, Hofling R, Werner RA (1999a) On-line delta O-18 measurement of organic and inorganic substances. Rapid Commun Mass Spectrom 13:1685–1693

    Article  Google Scholar 

  • Kornexl BE, Werner RA, Gehre M (1999b) Standardization for oxygen isotope ratio measurement – still an unsolved problem. Rapid Commun Mass Spectrom 13:1248–1251

    Article  Google Scholar 

  • Koziet J (1997) Isotope ratio mass spectrometric method for the on-line determination of oxygen-18 in organic matter. J Mass Spectrom 32:103–108

    Article  Google Scholar 

  • Kreuzer-Martin HW, Lott MJ, Dorigan J, Ehleringer JR (2003) Microbe forensics: Oxygen and hydrogen stable isotope ratios in Bacillus subtilis cells and spores. Proc Natl Acad Sci USA 100:815–819

    Article  Google Scholar 

  • Lamb AL, Leng MJ, Mohammed MU, Lamb HF (2004) Holocene climate and vegetation change in the Main Ethiopian Rift Valley, inferred from the composition (C/N and delta C-13) of lacustrine organic matter. Quat Sci Rev 23:881–891

    Article  Google Scholar 

  • Lamb AL, Leng MJ, Sloane HJ, Telford RJ (2005) A comparison of the palaeoclimate signals from diatom oxygen isotope ratios and carbonate oxygen isotope ratios from a low latitude crater lake. Palaeogeogr Palaeoclimatol Palaeoecol 223:290–302

    Article  Google Scholar 

  • Leng MJ, Barker PA (2006) A review of the oxygen isotope composition of lacustrine diatom silica for palaeoclimate reconstruction. Earth Sci Rev 75:5–27

    Article  Google Scholar 

  • Miller RF (1991) Chitin Paleoecology. Biochem Syst Ecol 19:401–411

    Article  Google Scholar 

  • Miller RF, Vossfoucart MF, Toussaint C, Jeuniaux C (1993) Chitin preservation in quaternary coleoptera—preliminary-results. Palaeogeogr Palaeoclimatol Palaeoecol 103:133–140

    Article  Google Scholar 

  • Sauer PE, Miller GH, Overpeck JT (2001) Oxygen isotope ratios of organic matter in arctic lakes as a paleoclimate proxy: field and laboratory investigations. J Paleolimnol 25:43–64

    Article  Google Scholar 

  • Schimmelmann A, DeNiro MJ (1986a) Stable isotopic studies on chitin, measurements on chitin/chitosan isolates and D-glucosamine hydrochloride from chitin. In: Muzzarelli RA, Jeuniaux AC, Gooday GW (eds) Chitin in nature and technology. Plenum Publishing Corporation, New York, pp 357–364

  • Sharp ZD, Atudorei V, Durakiewicz T (2001) A rapid method for determination of hydrogen and oxygen isotope ratios from water and hydrous minerals. Chem Geol 178:197–210

    Article  Google Scholar 

  • Walker IR (2001) Midges: Chironomidae and related diptera. In: Smol JP, Birks HJB, Last WM (eds) Tracking environmental change using lake sediments (Zoological indicators), vol 4. Kluwer Academic Publishers, Dordrecht, The Netherlands, pp 43–66

  • Wassenaar LI, Hobson KA (2002) Comparative equilibration and online technique for determination of non-exchangeable hydrogen of keratins for use in animal migration studies. Isotopes Environ Health Stud 39:211–217

    Article  Google Scholar 

  • Werner RA (2003) The online O-18/O-16 analysis: development and application. Isotopes Environ Health Stud 39:85–104

    Article  Google Scholar 

  • Werner RA, Brand WA (2001) Referencing strategies and techniques in stable isotope ratio analysis. Rapid Commun Mass Spectrom 15:501–519

    Article  Google Scholar 

  • Werner RA, Kornexl BE, Rossmann A, Schmidt HL (1996) On-line determination of delta O-18 values of organic substances. Anal Chim Acta 319:159–164

    Article  Google Scholar 

  • Wolfe BB, Edwards TWD, Aravena R, Forman SL, Warner BG, Velichko AA, MacDonald GM (2000) Holocene paleohydrology and paleoclimate at treeline, north-central Russia, inferred from oxygen isotope records in lake sediment cellulose. Quat Res 53:319–329

    Article  Google Scholar 

  • Wolfe BB, Edwards TWD, Elgood RJ, Beuning KR (2001) Carbon and oxygen isotope analysis of lake sediment cellulose: methods and applications. In: Last WM. Smol JP (eds) Tracking Environmental change using lake sediments (Physical and chemical techniques), vol 2. Kluwer Academic Publishers, Dordrecht, The Netherlands, pp 1–28

  • Wolfe BB, Falcone MD, Clogg-Wright KP, Mongeon CL, Yi Y, Brock BE, Amour NAS, Mark WA, Edwards TWD (2007) Progress in isotope paleohydrology using lake sediment cellulose. J Paleolimnol 37:221–231

    Article  Google Scholar 

  • Wooller MJ, Francis DR, Fogel ML, Miller GH, Walker IR, Wolfe AP (2004) Quantitative paleotemperature estimates from delta O-18 of chironomid head capsules preserved in arctic lake sediments. J Paleolimnol 31:267–274

    Article  Google Scholar 

  • Wooller MJ, Wang Y, Axford Y (2007) A multiple stable isotope record of Late Quaternary limnological changes and chironomid paleoecology from northeastern Iceland. J Paleolimnol, doi:10.1007/s10933-007-9144-8

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Acknowledgements

This research was supported by the National Science Foundation (NSF ESH-0317766 to Wooller) and the Alaska Stable Isotope Facility (ASIF) at the University of Alaska Fairbanks. The authors thank ASIF colleagues Tim Howe and Norma Haubenstock for their diligent work and valuable comments for experimental design and suggestions. We are grateful to participants and organizers, especially Dr. Ian Walker and Dr. Pete Landgon, at the international “Dead midges 2005 workshop” for stimulating encouragement for stable isotope applications on chironomid fossil heads. Thanks also to Dr. Yarrow Axford and Dr. Gifford Miller from the Institute for Arctic and Alpine Research (INSTAAR), Boulder, Colorado for valuable comments and support for method development in the early stages. We also thank Lena Krutikov and two anonymous reviewers for their constructive reviews of our paper.

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Authors and Affiliations

  1. Alaska Stable Isotope Facility, Water & Environmental Research Center, University of Alaska Fairbanks, Fairbanks, AK, 99775, USA

    Y. Wang & M. J. Wooller

  2. Department of Geology & Geophysics, University of Alaska Fairbanks, Fairbanks, AK, 99775, USA

    Y. Wang

  3. Department of Geosciences, University of Massachusetts Amherst, Amherst, MA, 01003, USA

    D. R. Francis

  4. Institute of Arctic Biology, University of Alaska Fairbanks, Fairbanks, AK, 99775, USA

    D. M. O’Brien

  5. School of Fisheries and Ocean Sciences, University of Alaska Fairbanks, Fairbanks, AK, 99775, USA

    M. J. Wooller

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  1. Y. Wang
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  2. D. R. Francis
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  4. M. J. Wooller
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Correspondence to Y. Wang.

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Wang, Y., Francis, D.R., O’Brien, D.M. et al. A protocol for preparing subfossil chironomid head capsules (Diptera: Chironomidae) for stable isotope analysis in paleoclimate reconstruction and considerations of contamination sources. J Paleolimnol 40, 771–781 (2008). https://doi.org/10.1007/s10933-008-9197-3

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  • DOI: https://doi.org/10.1007/s10933-008-9197-3

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