Measurement of 13C and 15N isotopic composition on nanomolar quantities of C and N

Pratigya J. Polissar, James M. Fulton, Christopher K. Junium, Courtney C. Turich, Katherine Haines Freeman

Research output: Contribution to journalArticle

55 Citations (Scopus)

Abstract

We describe a trapping and chromatography system that cryogenically removes CO 2 and N 2 generated from sample combustion in an elemental analyzer (EA) and introduces these gases into a low-flow helium carrier stream for isotopic analysis. The sample size required for measurement by this system (termed nano-EA/ IRMS) is almost 3 orders of magnitude less than conventional EA analyses and fills an important niche in the range of analytical isotopic methods. Only 25 nmol of N and 41 nmol of C are needed to achieve 1.0 % precision (2σ) from a single measurement while larger samples and replicate measurements provide better precision. Analyses of standards demonstrate that nano-EA measurements are both accurate and precise, even on nanomolar quantities of C and N. Conventional and nano-EA measurements on international and laboratory standards are indistinguishable within analytical precision. Likewise, nano-EA values for international standards do not differ statistically from their consensus values. Both observations indicate the nano-EA measurements are comparable to conventional EA analyses and accurately reproduce the VPDB and AIR isotopic scales. Critical to the success of the nano-EA system is the procedure for removing the blank contribution to the measured values. Statistical treatment of uncertainties for this procedure yields an accurate method for calculating internal and external precision.

Original languageEnglish (US)
Pages (from-to)755-763
Number of pages9
JournalAnalytical Chemistry
Volume81
Issue number2
DOIs
StatePublished - Jan 15 2009

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Chemical analysis
Helium
Carbon Monoxide
Chromatography
Gases

All Science Journal Classification (ASJC) codes

  • Analytical Chemistry

Cite this

Polissar, Pratigya J. ; Fulton, James M. ; Junium, Christopher K. ; Turich, Courtney C. ; Freeman, Katherine Haines. / Measurement of 13C and 15N isotopic composition on nanomolar quantities of C and N. In: Analytical Chemistry. 2009 ; Vol. 81, No. 2. pp. 755-763.
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abstract = "We describe a trapping and chromatography system that cryogenically removes CO 2 and N 2 generated from sample combustion in an elemental analyzer (EA) and introduces these gases into a low-flow helium carrier stream for isotopic analysis. The sample size required for measurement by this system (termed nano-EA/ IRMS) is almost 3 orders of magnitude less than conventional EA analyses and fills an important niche in the range of analytical isotopic methods. Only 25 nmol of N and 41 nmol of C are needed to achieve 1.0 {\%} precision (2σ) from a single measurement while larger samples and replicate measurements provide better precision. Analyses of standards demonstrate that nano-EA measurements are both accurate and precise, even on nanomolar quantities of C and N. Conventional and nano-EA measurements on international and laboratory standards are indistinguishable within analytical precision. Likewise, nano-EA values for international standards do not differ statistically from their consensus values. Both observations indicate the nano-EA measurements are comparable to conventional EA analyses and accurately reproduce the VPDB and AIR isotopic scales. Critical to the success of the nano-EA system is the procedure for removing the blank contribution to the measured values. Statistical treatment of uncertainties for this procedure yields an accurate method for calculating internal and external precision.",
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Measurement of 13C and 15N isotopic composition on nanomolar quantities of C and N. / Polissar, Pratigya J.; Fulton, James M.; Junium, Christopher K.; Turich, Courtney C.; Freeman, Katherine Haines.

In: Analytical Chemistry, Vol. 81, No. 2, 15.01.2009, p. 755-763.

Research output: Contribution to journalArticle

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