Hostname: page-component-cd9895bd7-mkpzs Total loading time: 0 Render date: 2024-12-27T07:57:03.307Z Has data issue: false hasContentIssue false
  • English
  • Français

Conventionally Heated Microfurnace for the Graphitization of Microgram-Sized Carbon Samples

Published online by Cambridge University Press:  08 November 2016

Bin Yang  and
A M Smith Open the ORCID record for A M Smith [Opens in a new window]
Bin Yang*
Affiliation:
Australian Nuclear Science and Technology Organisation, New Illawarra Road, Lucas Heights, NSW 2234, Australia
A M Smith
Affiliation:
Australian Nuclear Science and Technology Organisation, New Illawarra Road, Lucas Heights, NSW 2234, Australia
*
*Corresponding author. Email: byz@ansto.gov.au.
Get access Rights & Permissions [Opens in a new window]

Abstract

A new type of miniaturized, externally heated graphitization reaction furnace, the microconventional furnace (MCF), was constructed following our development of the laser heated furnace (LHF). The MCF is comprised of a gas reactor, a cold finger cooling system, and a compact resistive heater, which can raise the temperature of the hot finger to 850°C. The gas reactor is provided with three integrated valves to connect with the hydrogen/vacuum manifold, to isolate the reactor, and to connect with sample vessels. We made two types of MCF: the type 1 furnace (volume of 0.9 mL), with an integral stainless steel cold finger, and the type 2 furnace (volume from 1.3 to 10 mL), with a changeable glass cold finger. The MCF is designed for above atmospheric pressure (up to 2500 mbar) operation to decrease the overall graphitization time and improve the carbon yield. The MCF provides an effective solution for producing graphite from carbon dioxide (CO2) sample gas from 5 to 2000 µg of carbon with only 0.083 μg of 100 pMC extraneous carbon added. Cross-contamination tests show that the MCFs have no memory effect from previous samples.

Keywords

Bosch reactiongraphitizationmicroconventional furnace
Type
Chemical Pretreatment Approaches
Information
Radiocarbon , Volume 59 , Special Issue 3: Proceedings of the 22nd International Radiocarbon Conference (Part 2 of 2) , June 2017 , pp. 859 - 873
Copyright
© 2016 by 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.)

Footnotes

Selected Papers from the 2015 Radiocarbon Conference, Dakar, Senegal, 16–20 November 2015

References

REFERENCES

Hua, Q, Zoppi, U, Williams, AA, Smith, AM. 2004. Small-mass AMS radiocarbon analysis at ANTARES. Nuclear Instruments and Methods in Physics Research B 223–224:284–292.Google Scholar
Liebl, J, Ortiz, RA, Golser, R, Handle, F, Kutschera, W, Steier, P, Wild, EM. 2010. Studies on the preparation of small 14C samples with an RGA and 13C-enriched material. Radiocarbon 52(2–3):1394–1404.CrossRefGoogle Scholar
Liebl, J, Steier, P, Golser, R, Kutschera, W, Mair, K, Priller, A, Vonderhaid, I, Wild, EM. 2013. Carbon background and ionization yield of an AMS system during 14C measurements of microgram-size graphite samples. Nuclear Instruments and Methods in Physics Research B 294:335–339.Google Scholar
Loyd, DH, Vogel, JS, Trumbore, S. 1991. Lithium contamination in AMS measurements of 14C. Radiocarbon 33(3):297–301.Google Scholar
Manning, MP, Reid, RC. 1977. C-H-O systems in the presence of an iron catalyst. Industrial & Engineering Chemistry Process Design and Development 16(3):358–361.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):293–302.CrossRefGoogle Scholar
Shah Walter, SR, Gagnon, AR, Roberts, ML, McNichol, AP, Gaylord, M, Klein, E. 2015. Ultra-small graphitization reactor for ultra-microscale 14C analysis at the National Ocean Sciences Accelerator Mass Spectrometry (NOSAMS) Facility. Radiocarbon 57(1):109–122.CrossRefGoogle Scholar
Smith, AM, Hua, Q, Levchenko, VA. 2007a. New developments in micro-sample 14C AMS at ANSTO. INQUA Abstracts. Quaternary International 167–168:390.Google Scholar
Smith, AM, Petrenko, VV, Hua, Q, Southon, J, Brailsford, G. 2007b. The effect of N2O on the graphitization of small CO2 samples. Radiocarbon 49(2):245–254.Google Scholar
Smith, AM, Hua, Q, Williams, A, Levchenko, V, Yang, B. 2010a. Developments in micro-sample 14C AMS at the ANTARES AMS facility. Nuclear Instruments and Methods in Physics Research B 268(7–8):919–923.Google Scholar
Smith, AM, Yang, B, Hua, Q, Mann, M. 2010b. Laser-heated microfurnace: gas analysis and graphite morphology. Radiocarbon 52(2–3):769–782.Google Scholar
Southon, J. 2007. Graphite reactor memory - where is it from and how to minimize it? Nuclear Instruments and Methods in Physics Research B 259(1):288–292.CrossRefGoogle Scholar
Vogel, JS, Southon, JR, Nelson, DE, Brown, TA. 1984. Performance of catalytically condensed carbon for use in accelerator mass spectrometry. Nuclear Instruments and Methods in Physics Research B 233(5):289–293.CrossRefGoogle Scholar
Yang, B, Smith, AM, Hua, Q. 2013. A cold finger cooling system for the efficient graphitisation of microgram-sized carbon samples. Nuclear Instruments and Methods in Physics Research B 294:262–265.Google Scholar
Yang, B, Smith, AM, Long, S. 2015. Second generation laser-heated microfurnace for the preparation of microgram-sized graphite samples. Nuclear Instruments and Methods in Physics Research B 361:363–371.CrossRefGoogle Scholar