Abstract

We present a first implementation of optical-frequency-comb-based rapid trace gas detection in the molecular fingerprint region in the mid-infrared. Near-real-time acquisition of broadband absorption spectra with 0.0056 cm−1 maximum resolution is demonstrated using a frequency comb Fourier transform spectrometer which operates in the 2100-to-3700-cm−1 spectral region. We achieve part-per-billion detection limits in 30 seconds of integration time for several important molecules including methane, ethane, isoprene, and nitrous oxide. Our system enables precise concentration measurements even in gas mixtures that exhibit continuous absorption bands, and it allows detection of molecules at levels below the noise floor via simultaneous analysis of multiple spectral features.

© 2010 OSA

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2010 (4)

F. Adler, M. J. Thorpe, K. C. Cossel, and J. Ye, “Cavity-enhanced direct frequency comb spectroscopy: technology and applications,” Annu Rev Anal Chem (Palo Alto Calif) 3(1), 175–205 (2010).
[CrossRef]

S. Kassi, K. Didriche, C. Lauzin, Xde. G. Vaernewijckb, A. Rizopoulos, and M. Herman, “Demonstration of cavity enhanced FTIR spectroscopy using a femtosecond laser absorption source,” Spectrochim. Acta A Mol. Biomol. Spectrosc. 75(1), 142–145 (2010).
[CrossRef]

B. Bernhardt, A. Ozawa, P. Jacquet, M. Jacquey, Y. Kobayashi, Th. Udem, R. Holzwarth, G. Guelachvili, T. W. Hänsch, and N. Picqué, “Cavity-enhanced dual-comb spectroscopy,” Nat. Photonics 4(1), 55–57 (2010).
[CrossRef]

M. El-Amraoui, J. Fatome, J. C. Jules, B. Kibler, G. Gadret, C. Fortier, F. Smektala, I. Skripatchev, C. F. Polacchini, Y. Messaddeq, J. Troles, L. Brilland, M. Szpulak, and G. Renversez, “Strong infrared spectral broadening in low-loss As-S chalcogenide suspended core microstructured optical fibers,” Opt. Express 18(5), 4547–4556 (2010), http://www.opticsexpress.org/abstract.cfm?URI=OPEX-18-5-4547 .
[CrossRef] [PubMed]

2009 (8)

A. Karpf and G. N. Rao, “Enhanced sensitivity for the detection of trace gases using multiple line integrated absorption spectroscopy,” Appl. Opt. 48(27), 5061–5066 (2009).
[CrossRef] [PubMed]

J. Mandon, G. Guelachvili, and N. Picqué, “Fourier transform spectrometry with a laser frequency comb,” Nat. Photonics 3(2), 99–102 (2009).
[CrossRef]

E. D. Schulze, S. Luyssaert, P. Ciais, A. Freibauer, I. A. Janssens et al, E. D. Schulze, J. F. Soussana, P. Smith, J. Grace, I. Levin, B. Thiruchittampalam, M. Heimann, A. J. Dolman, R. Valentini, P. Bousquet, P. Peylin, W. Peters, C. Rödenbeck, G. Etiope, N. Vuichard, M. Wattenbach, G. J. Nabuurs, Z. Poussi, J. Nieschulze, and J. H. Gash, “Importance of methane and nitrous oxide for Europe's terrestrial greenhouse-gas balance,” Nat. Geosci. 2(12), 842–850 (2009).
[CrossRef]

A. R. Ravishankara, J. S. Daniel, and R. W. Portmann, “Nitrous oxide (N2O): the dominant ozone-depleting substance emitted in the 21st century,” Science 326(5949), 123–125 (2009).
[CrossRef] [PubMed]

W. Lei, M. Zavala, B. de Foy, R. Volkamer, M. J. Molina, and L. T. Molina, “Impact of primary formaldehyde on air pollution in the Mexico City Metropolitan Area,” Atmos. Chem. Phys. 9(7), 2607–2618 (2009).
[CrossRef]

F. Adler, K. C. Cossel, M. J. Thorpe, I. Hartl, M. E. Fermann, and J. Ye, “Phase-stabilized, 1.5 W frequency comb at 2.8-4.8 microm,” Opt. Lett. 34(9), 1330–1332 (2009).
[CrossRef] [PubMed]

L. S. Rothman, I. E. Gordon, A. Barbe, D. Chris Benner, P. F. Bernath, M. Birk, V. Boudon, L. R. Brown, A. Campargue, J.-P. Champion, K. Chance, L. H. Coudert, V. Dana, V. M. Devi, S. Fally, J.-M. Flaud, R. R. Gamache, A. Goldman, D. Jacquemart, I. Kleiner, N. Lacome, W. J. Lafferty, J.-Y. Mandin, S. T. Massie, S. N. Mikhailenko, C. E. Miller, N. Moazzen-Ahmadi, O. V. Naumenko, A. V. Nikitin, J. Orphal, V. I. Perevalov, A. Perrin, A. Predoi-Cross, C. P. Rinsland, M. Rotger, M. Šimečková, M. A. H. Smith, K. Sung, S. A. Tashkun, J. Tennyson, R. A. Toth, A. C. Vandaele, and J. Vander Auwera, “The HITRAN 2008 molecular spectroscopic database,” J. Quant. Spectrosc. Radiat. Transf. 110(9-10), 533–572 (2009).
[CrossRef]

D. Richter, A. Fried, and P. Weibring, “Difference frequency generation laser based spectrometers,” Laser & Photon. Rev. 3(4), 343–354 (2009).
[CrossRef]

2008 (3)

M. J. Thorpe and J. Ye, “Cavity-enhanced direct frequency comb spectroscopy,” Appl. Phys. B 91(3-4), 397–414 (2008).
[CrossRef]

I. Coddington, W. C. Swann, and N. R. Newbury, “Coherent multiheterodyne spectroscopy using stabilized optical frequency combs,” Phys. Rev. Lett. 100(1), 013902 (2008).
[CrossRef] [PubMed]

P. Domachuk, N. A. Wolchover, M. Cronin-Golomb, A. Wang, A. K. George, C. M. B. Cordeiro, J. C. Knight, and F. G. Omenetto, “Over 4000 nm bandwidth of mid-IR supercontinuum generation in sub-centimeter segments of highly nonlinear tellurite PCFs,” Opt. Express 16(10), 7161–7168 (2008), http://www.opticsexpress.org/abstract.cfm?URI=OPEX-16-10-7161 .
[CrossRef] [PubMed]

2007 (6)

M. R. McCurdy, Y. Bakhirkin, G. Wysocki, R. Lewicki, and F. K. Tittel, “Recent advances of laser-spectroscopy-based techniques for applications in breath analysis,” J. Breath Res. 1(1), 014001 (2007).
[CrossRef] [PubMed]

W. Cao and Y. Duan, “Current status of methods and techniques for breath analysis,” Crit. Rev. Anal. Chem. 37(1), 3–13 (2007).
[CrossRef]

S. A. Diddams, L. Hollberg, and V. Mbele, “Molecular fingerprinting with the resolved modes of a femtosecond laser frequency comb,” Nature 445(7128), 627–630 (2007).
[CrossRef] [PubMed]

C. Gohle, B. Stein, A. Schliesser, Th. Udem, and T. W. Hänsch, “Frequency comb Vernier spectroscopy for broadband, high-resolution, high-sensitivity absorption and dispersion spectra,” Phys. Rev. Lett. 99(26), 263902 (2007).
[CrossRef]

L. W. Kornaszewski, N. Gayraud, J. M. Stone, W. N. Macpherson, A. K. George, J. C. Knight, D. P. Hand, and D. T. Reid, “Mid-infrared methane detection in a photonic bandgap fiber using a broadband optical parametric oscillator,” Opt. Express 15(18), 11219–11224 (2007), http://www.opticsexpress.org/abstract.cfm?URI=OPEX-15-18-11219 .
[CrossRef] [PubMed]

E. Sorokin, I. T. Sorokina, J. Mandon, G. Guelachvili, and N. Picqué, “Sensitive multiplex spectroscopy in the molecular fingerprint 2.4 µm region with a Cr2+:ZnSe femtosecond laser,” Opt. Express 15(25), 16540–16545 (2007), http://www.opticsexpress.org/abstract.cfm?URI=OPEX-15-25-16540 .
[CrossRef] [PubMed]

2006 (4)

T. H. Risby and S. F. Solga, “Current status of clinical breath analysis,” Appl. Phys. B 85(2-3), 421–426 (2006).
[CrossRef]

M. J. Thorpe, K. D. Moll, R. J. Jones, B. Safdi, and J. Ye, “Broadband cavity ringdown spectroscopy for sensitive and rapid molecular detection,” Science 311(5767), 1595–1599 (2006).
[CrossRef] [PubMed]

K. D. Skeldon, L. C. McMillan, C. A. Wyse, S. D. Monk, G. Gibson, C. Patterson, T. France, C. Longbottom, and M. J. Padgett, “Application of laser spectroscopy for measurement of exhaled ethane in patients with lung cancer,” Respir. Med. 100(2), 300–306 (2006).
[CrossRef]

Y. Qu, Z. H. Kang, Y. Jiang, and J. Y. Gao, “Multiline absorption spectroscopy for methane gas detection,” Appl. Opt. 45(33), 8537–8540 (2006).
[CrossRef] [PubMed]

2005 (2)

2004 (4)

K. A. Tillman, R. R. J. Maier, D. T. Reid, and E. D. McNaghten, “Mid-infrared absorption spectroscopy across a 14.4 THz spectral range using a broadband femtosecond optical parametric oscillator,” Appl. Phys. Lett. 85(16), 3366–3368 (2004).
[CrossRef]

S. W. Sharpe, T. J. Johnson, R. L. Sams, P. M. Chu, G. C. Rhoderick, and P. A. Johnson, “Gas-phase databases for quantitative infrared spectroscopy,” Appl. Spectrosc. 58(12), 1452–1461 (2004).
[CrossRef] [PubMed]

W. Miekisch, J. K. Schubert, and G. F. E. Noeldge-Schomburg, “Diagnostic potential of breath analysis--focus on volatile organic compounds,” Clin. Chim. Acta 347(1-2), 25–39 (2004).
[CrossRef] [PubMed]

Z. S. Li, M. Rupinski, J. Zetterberg, Z. T. Alwahabi, and M. Aldén, “Detection of methane with mid-infrared polarization spectroscopy,” Appl. Phys. B 79(2), (2004).
[CrossRef]

2003 (2)

T. N. Rosenstiel, M. J. Potosnak, K. L. Griffin, R. Fall, and R. K. Monson, “Increased CO2 uncouples growth from isoprene emission in an agriforest ecosystem,” Nature 421(6920), 256–259 (2003).
[CrossRef] [PubMed]

D. J. Karoly, K. Braganza, P. A. Stott, J. M. Arblaster, G. A. Meehl, A. J. Broccoli, and K. W. Dixon, “Detection of a human influence on North American climate,” Science 302(5648), 1200–1203 (2003).
[CrossRef] [PubMed]

2002 (2)

P. A. Stott and J. A. Kettleborough, “Origins and estimates of uncertainty in predictions of twenty-first century temperature rise,” Nature 416(6882), 723–726 (2002).
[CrossRef] [PubMed]

S. Schiller, “Spectrometry with frequency combs,” Opt. Lett. 27(9), 766–768 (2002).
[CrossRef]

2000 (2)

P. M. Cox, R. A. Betts, C. D. Jones, S. A. Spall, and I. J. Totterdell, “Acceleration of global warming due to carbon-cycle feedbacks in a coupled climate model,” Nature 408(6809), 184–187 (2000).
[CrossRef] [PubMed]

M. B. Esler, D. W. T. Griffith, S. R. Wilson, and L. P. Steele, “Precision Trace Gas Analysis by FT-IR Spectroscopy: 1. Simultaneous Analysis of CO2, CH4, N2O, and CO in Air,” Anal. Chem. 72(1), 206–215 (2000).
[CrossRef] [PubMed]

1995 (1)

D. Benner, C. P. Rinsland, V. M. Devi, M. A. H. Smith, and D. Atkins, “A multispectrum nonlinear least squares fitting technique,” J. Quant. Spectrosc. Radiat. Transf. 53(6), 705–721 (1995).
[CrossRef]

1976 (1)

C. Wieman and T. W. Hänsch, “Doppler-Free Laser Polarization Spectroscopy,” Phys. Rev. Lett. 36(20), 1170–1173 (1976).
[CrossRef]

1963 (1)

D. Marquardt, “An Algorithm for Least-Squares Estimation of Nonlinear Parameters,” SIAM J. Appl. Math. 11(2), 431–441 (1963).
[CrossRef]

Adler, F.

F. Adler, M. J. Thorpe, K. C. Cossel, and J. Ye, “Cavity-enhanced direct frequency comb spectroscopy: technology and applications,” Annu Rev Anal Chem (Palo Alto Calif) 3(1), 175–205 (2010).
[CrossRef]

F. Adler, K. C. Cossel, M. J. Thorpe, I. Hartl, M. E. Fermann, and J. Ye, “Phase-stabilized, 1.5 W frequency comb at 2.8-4.8 microm,” Opt. Lett. 34(9), 1330–1332 (2009).
[CrossRef] [PubMed]

Aldén, M.

Z. S. Li, M. Rupinski, J. Zetterberg, Z. T. Alwahabi, and M. Aldén, “Detection of methane with mid-infrared polarization spectroscopy,” Appl. Phys. B 79(2), (2004).
[CrossRef]

Alwahabi, Z. T.

Z. S. Li, M. Rupinski, J. Zetterberg, Z. T. Alwahabi, and M. Aldén, “Detection of methane with mid-infrared polarization spectroscopy,” Appl. Phys. B 79(2), (2004).
[CrossRef]

Arblaster, J. M.

D. J. Karoly, K. Braganza, P. A. Stott, J. M. Arblaster, G. A. Meehl, A. J. Broccoli, and K. W. Dixon, “Detection of a human influence on North American climate,” Science 302(5648), 1200–1203 (2003).
[CrossRef] [PubMed]

Atkins, D.

D. Benner, C. P. Rinsland, V. M. Devi, M. A. H. Smith, and D. Atkins, “A multispectrum nonlinear least squares fitting technique,” J. Quant. Spectrosc. Radiat. Transf. 53(6), 705–721 (1995).
[CrossRef]

Bakhirkin, Y.

M. R. McCurdy, Y. Bakhirkin, G. Wysocki, R. Lewicki, and F. K. Tittel, “Recent advances of laser-spectroscopy-based techniques for applications in breath analysis,” J. Breath Res. 1(1), 014001 (2007).
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M. B. Esler, D. W. T. Griffith, S. R. Wilson, and L. P. Steele, “Precision Trace Gas Analysis by FT-IR Spectroscopy: 1. Simultaneous Analysis of CO2, CH4, N2O, and CO in Air,” Anal. Chem. 72(1), 206–215 (2000).
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Annu Rev Anal Chem (Palo Alto Calif) (1)

F. Adler, M. J. Thorpe, K. C. Cossel, and J. Ye, “Cavity-enhanced direct frequency comb spectroscopy: technology and applications,” Annu Rev Anal Chem (Palo Alto Calif) 3(1), 175–205 (2010).
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T. H. Risby and S. F. Solga, “Current status of clinical breath analysis,” Appl. Phys. B 85(2-3), 421–426 (2006).
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J. Quant. Spectrosc. Radiat. Transf. (2)

L. S. Rothman, I. E. Gordon, A. Barbe, D. Chris Benner, P. F. Bernath, M. Birk, V. Boudon, L. R. Brown, A. Campargue, J.-P. Champion, K. Chance, L. H. Coudert, V. Dana, V. M. Devi, S. Fally, J.-M. Flaud, R. R. Gamache, A. Goldman, D. Jacquemart, I. Kleiner, N. Lacome, W. J. Lafferty, J.-Y. Mandin, S. T. Massie, S. N. Mikhailenko, C. E. Miller, N. Moazzen-Ahmadi, O. V. Naumenko, A. V. Nikitin, J. Orphal, V. I. Perevalov, A. Perrin, A. Predoi-Cross, C. P. Rinsland, M. Rotger, M. Šimečková, M. A. H. Smith, K. Sung, S. A. Tashkun, J. Tennyson, R. A. Toth, A. C. Vandaele, and J. Vander Auwera, “The HITRAN 2008 molecular spectroscopic database,” J. Quant. Spectrosc. Radiat. Transf. 110(9-10), 533–572 (2009).
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E. D. Schulze, S. Luyssaert, P. Ciais, A. Freibauer, I. A. Janssens et al, E. D. Schulze, J. F. Soussana, P. Smith, J. Grace, I. Levin, B. Thiruchittampalam, M. Heimann, A. J. Dolman, R. Valentini, P. Bousquet, P. Peylin, W. Peters, C. Rödenbeck, G. Etiope, N. Vuichard, M. Wattenbach, G. J. Nabuurs, Z. Poussi, J. Nieschulze, and J. H. Gash, “Importance of methane and nitrous oxide for Europe's terrestrial greenhouse-gas balance,” Nat. Geosci. 2(12), 842–850 (2009).
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Figures (6)

Fig. 1
Fig. 1

Schematic of the experimental setup; details on the OPO stabilization can be found in Ref [31]; SiPD, silicon photo diode; MCZT: mid-IR HgCdZnTe detector. Solid lines indicate optical paths, dotted lines represent electronic lines.

Fig. 2
Fig. 2

Collection of absorption spectra throughout the operating range of our mid-IR frequency comb Fourier transform spectrometer (black) and comparison to HITRAN or NWIR-based fits (purple, plotted negative for clarity). The trace concentration, nitrogen pressure, and spectral resolution are designated in the panels; (a) ν 3 band of nitrous oxide (N2O) at a concentration of 9 ppm, a pressure of 100 Torr N2, and a resolution of 0.014 cm−1; (b) formaldehyde (H2CO), 58 ppm, 600 Torr, 0.014 cm−1; (c) ethane (C2H6), 11 ppm, 600 Torr, 0.096 cm−1; (d) methane (CH4), 10 ppm, 100 Torr, 0.0056 cm−1; (e) isoprene (C5H8), 16 ppm, 600 Torr, 0.058 cm−1; (f) 2ν 2 + ν 3 and ν 1 + ν 3 band of N2O, 142 ppm, 600 Torr, 0.026 cm−1. All spectra are obtained with a single wavelength setting of the OPO except (a), which is a combination of two measurements at different central wavelengths.

Fig. 3
Fig. 3

(a) A zoom of the methane Q-branch spectrum at the system’s highest resolution of 0.0056 cm−1 (168 MHz) and an N2 pressure of 100 Torr. (b) A further magnified view of one of the line features; open circles in black are measured single data points; fitted HITRAN-based spectrum is shown in red and plotted negative for clarity.

Fig. 4
Fig. 4

(a) Measurement of CH4 at a highly diluted concentration of 275 ppb. Despite the low S/N ratio, the detection and fitting of multiple lines in the absorption band allow a reliable determination of the concentration with only 5 ppb uncertainty. The inset shows a comparison of measured data (black) and fit from HITRAN reference (red) at one single feature. (b) The residual of the multiple-line fit.

Fig. 5
Fig. 5

(a) Measured spectrum of a mixture of formaldehyde, methanol, and water at an N2 pressure of 600 Torr and a resolution of 0.014 cm−1 (black), as well as the fitted spectra based on HITRAN and NWIR of the three components (H2CO, magenta; CH3OH, green; H2O, blue) and their sum (gray). The fit gives abundances of (47.1 ± 0.1) ppm H2CO, (58.30 ± 0.04) ppm CH3OH, and (813 ± 7) ppm H2O. (b) The residual of the overall fit displays no remaining structure.

Fig. 6
Fig. 6

Measurement of laboratory air at 600 Torr recorded with a resolution of 0.014 cm−1 (black) containing 2.02 ppm of methane and 1.03% of water, as well as HITRAN-based fits of H2O (blue) and CH4 (red). (a) The full scale of absorbance displays mainly water lines, and the magnified scale in (b) reveals the weak methane lines among the much stronger water peaks.

Tables (1)

Tables Icon

Table 1 Detection limits for a collection of important molecules within the spectral range of our mid-IR FC-FTS. The third column shows the noise equivalent concentration (NEC) results, which are based on the measured absorption sensitivity of 3.8 × 10−8 cm−1 Hz-1/2 per spectral element under typical experimental conditions of 600 Torr N2 pressure, 0.014 cm−1 unapodized spectral resolution, and 30 s of total integration time (5 averages). The fourth column shows the theoretically estimated multiline detection limits (see Appendix) using the same noise and resolution conditions as those for column three. The fifth column displays the experimentally obtained concentration detection limits from the multi-line fits to measured spectra. The disagreement between the theoretical and experimental values is due to the fact that some spectra were not measured at the best possible noise performance of the system. Note that significantly lower detection limits are achievable with longer integration times (tested to at least 6 min).

Equations (7)

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F ( N ) = i = 1 k [ α ( ν i ) N α T ( ν i ) ] 2 = min ,
d F d N = i = 1 k 2 [ α ( ν i ) N α T ( ν i ) ]     [ α T ( ν i ) ] = 0.
N     =     ​ i = 1 k α ( ν i )     α T ( ν i ) i = 1 k α T 2 ( ν i ) .
S N 2 = i = 1 k [ N α ( ν i ) ] 2 S α 2 .
N α ( ν i ) = α T ( ν i ) i = 1 k α T 2 ( ν i ) ,
S N 2 = i = 1 k α T ( ν i ) 2 S α 2 [ i = 1 k α T 2 ( ν i ) ] 2 = S α 2 i = 1 k α T 2 ( ν i ) .
S N = S α [ i = 1 k α T 2 ( ν i ) ] 1 / 2 .

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