Abstract

Laser-induced breakdown spectroscopy (LIBS) has been evaluated as a tool for monitoring trace levels of helium in gas mixtures consisting mostly of hydrogen. Calibration data for helium in hydrogen was investigated at different helium concentration levels. At high concentrations of helium (>7.25%), the LIBS signal is quenched due to Penning ionization. The hydrogen alpha line (656.28 nm) was observed to broaden as the concentration of helium impurities in the hydrogen gas mixture increased. The helium line at 587.56 nm was selected as the analyte line for helium impurity detection. The effects of laser energy, the delay time between the laser pulse and data acquisition, and the gas pressure on the LIBS signal of helium were investigated to determine the optimum conditions for helium detection. The LIBS signal from the helium line at 587.56 nm shows good linear correlation with helium concentration for He concentrations below 1%. Thus, LIBS can be reliably used to detect the low levels of helium. The limit of detection for helium was found to be 78 ppm.

© 2012 Optical Society of America

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References

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  5. K. E. Eseller, F.-Y. Yueh, and J. P. Singh, “Non-intrusive, on-line, simultaneous multi-species impurity monitoring in hydrogen using LIBS,” Appl. Phys. B 102, 963–969 (2011).
    [CrossRef]
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  14. M. Hanafi, M. M. Omar, and Y. E. E.-D. Gamal, “Study of laser-induced breakdown spectroscopy of gases,” Radiat. Phys. Chem. 57, 11–20 (2000).
    [CrossRef]
  15. C. A. Henry, P. K. Diwakar, and D. W. Hahn, “Investigation of helium addition for laser induced plasma spectroscopy of pure gas phase systems: analyte interactions and signal enhancement,” Spectrochim. Acta B 62, 1390–1398 (2007).
    [CrossRef]
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2011

K. E. Eseller, F.-Y. Yueh, and J. P. Singh, “Non-intrusive, on-line, simultaneous multi-species impurity monitoring in hydrogen using LIBS,” Appl. Phys. B 102, 963–969 (2011).
[CrossRef]

2010

2009

E. D. McNaghten, A. M. Parkes, B. C. Griffiths, A. I. Whitehouse, and S. Palanco, “Detection of trace concentrations of helium and argon in gas mixtures by laser-induced breakdown spectroscopy,” Spectrochim. Acta B 64, 1111–1118 (2009).
[CrossRef]

J. Camparo and G. Fathi, “Effects of rf power on electron density and temperature, neutral temperature, and T-e fluctuations in an inductively coupled plasma,” J. Appl. Phys. 105, 103302 (2009).
[CrossRef]

2007

C. A. Henry, P. K. Diwakar, and D. W. Hahn, “Investigation of helium addition for laser induced plasma spectroscopy of pure gas phase systems: analyte interactions and signal enhancement,” Spectrochim. Acta B 62, 1390–1398 (2007).
[CrossRef]

Y. Weijun, “Trace analysis of impurities in bulk gases by gas chromatography-pulsed discharge helium ionization detection with ‘heart-cutting’ technique,” J. Chromatogr. A 1167, 225–230 (2007).
[CrossRef]

2001

M. Tran, B. W. Smith, D. W. Hahn, and J. D. Winefordner, “Detection of gaseous and particulate fluorides by laser-induced breakdown spectroscopy,” Appl. Spectrosc. 55, 1455–1461 (2001).
[CrossRef]

R. Uhl, J. Franzke, and U. Haas, “Detection of argon and krypton traces in noble gases by diode laser absorption spectrometry,” Appl. Phys. B 73, 71–74 (2001).
[CrossRef]

2000

M. Hanafi, M. M. Omar, and Y. E. E.-D. Gamal, “Study of laser-induced breakdown spectroscopy of gases,” Radiat. Phys. Chem. 57, 11–20 (2000).
[CrossRef]

1999

1997

D. A. Rusak, B. C. Castle, B. W. Smith, and J. D. Winefordner, “Fundamentals and applications of laser-induced breakdown spectroscopy,” Crit. Rev. Anal. Chem. 27, 257–290 (1997).
[CrossRef]

1996

Abdulmadjid, S. N.

Camparo, J.

J. Camparo and G. Fathi, “Effects of rf power on electron density and temperature, neutral temperature, and T-e fluctuations in an inductively coupled plasma,” J. Appl. Phys. 105, 103302 (2009).
[CrossRef]

Carney, K. P.

Castle, B. C.

D. A. Rusak, B. C. Castle, B. W. Smith, and J. D. Winefordner, “Fundamentals and applications of laser-induced breakdown spectroscopy,” Crit. Rev. Anal. Chem. 27, 257–290 (1997).
[CrossRef]

Cremers, D. A.

D. A. Cremers and L. J. Radziemski, The Handbook of LIBS (Wiley, 2006).

Diwakar, P. K.

C. A. Henry, P. K. Diwakar, and D. W. Hahn, “Investigation of helium addition for laser induced plasma spectroscopy of pure gas phase systems: analyte interactions and signal enhancement,” Spectrochim. Acta B 62, 1390–1398 (2007).
[CrossRef]

Eseller, K. E.

K. E. Eseller, F.-Y. Yueh, and J. P. Singh, “Non-intrusive, on-line, simultaneous multi-species impurity monitoring in hydrogen using LIBS,” Appl. Phys. B 102, 963–969 (2011).
[CrossRef]

Fathi, G.

J. Camparo and G. Fathi, “Effects of rf power on electron density and temperature, neutral temperature, and T-e fluctuations in an inductively coupled plasma,” J. Appl. Phys. 105, 103302 (2009).
[CrossRef]

Franzke, J.

R. Uhl, J. Franzke, and U. Haas, “Detection of argon and krypton traces in noble gases by diode laser absorption spectrometry,” Appl. Phys. B 73, 71–74 (2001).
[CrossRef]

Fukumoto, K.

Gamal, Y. E. E.-D.

M. Hanafi, M. M. Omar, and Y. E. E.-D. Gamal, “Study of laser-induced breakdown spectroscopy of gases,” Radiat. Phys. Chem. 57, 11–20 (2000).
[CrossRef]

Griem, R.

R. Griem, Spectral Line Broadening by Plasmas (Academic, 1974).

Griffiths, B. C.

E. D. McNaghten, A. M. Parkes, B. C. Griffiths, A. I. Whitehouse, and S. Palanco, “Detection of trace concentrations of helium and argon in gas mixtures by laser-induced breakdown spectroscopy,” Spectrochim. Acta B 64, 1111–1118 (2009).
[CrossRef]

Haas, U.

R. Uhl, J. Franzke, and U. Haas, “Detection of argon and krypton traces in noble gases by diode laser absorption spectrometry,” Appl. Phys. B 73, 71–74 (2001).
[CrossRef]

Hahn, D. W.

C. A. Henry, P. K. Diwakar, and D. W. Hahn, “Investigation of helium addition for laser induced plasma spectroscopy of pure gas phase systems: analyte interactions and signal enhancement,” Spectrochim. Acta B 62, 1390–1398 (2007).
[CrossRef]

M. Tran, B. W. Smith, D. W. Hahn, and J. D. Winefordner, “Detection of gaseous and particulate fluorides by laser-induced breakdown spectroscopy,” Appl. Spectrosc. 55, 1455–1461 (2001).
[CrossRef]

Hanafi, M.

M. Hanafi, M. M. Omar, and Y. E. E.-D. Gamal, “Study of laser-induced breakdown spectroscopy of gases,” Radiat. Phys. Chem. 57, 11–20 (2000).
[CrossRef]

Hedwig, R.

Henry, C. A.

C. A. Henry, P. K. Diwakar, and D. W. Hahn, “Investigation of helium addition for laser induced plasma spectroscopy of pure gas phase systems: analyte interactions and signal enhancement,” Spectrochim. Acta B 62, 1390–1398 (2007).
[CrossRef]

Jobiliong, E.

Kagawa, K.

Kurniawan, K. H.

Lie, T. J.

Lie, Z. S.

McNaghten, E. D.

E. D. McNaghten, A. M. Parkes, B. C. Griffiths, A. I. Whitehouse, and S. Palanco, “Detection of trace concentrations of helium and argon in gas mixtures by laser-induced breakdown spectroscopy,” Spectrochim. Acta B 64, 1111–1118 (2009).
[CrossRef]

Miziolek, A.

A. Miziolek, V. Palleschi, and I. Schechter, Laser-Induced Breakdown Spectroscopy (LIBS): Fundamentals and Applications (Cambridge University, 2006).

Niki, H.

Omar, M. M.

M. Hanafi, M. M. Omar, and Y. E. E.-D. Gamal, “Study of laser-induced breakdown spectroscopy of gases,” Radiat. Phys. Chem. 57, 11–20 (2000).
[CrossRef]

Palanco, S.

E. D. McNaghten, A. M. Parkes, B. C. Griffiths, A. I. Whitehouse, and S. Palanco, “Detection of trace concentrations of helium and argon in gas mixtures by laser-induced breakdown spectroscopy,” Spectrochim. Acta B 64, 1111–1118 (2009).
[CrossRef]

Palleschi, V.

A. Miziolek, V. Palleschi, and I. Schechter, Laser-Induced Breakdown Spectroscopy (LIBS): Fundamentals and Applications (Cambridge University, 2006).

Pardede, M.

Parkes, A. M.

E. D. McNaghten, A. M. Parkes, B. C. Griffiths, A. I. Whitehouse, and S. Palanco, “Detection of trace concentrations of helium and argon in gas mixtures by laser-induced breakdown spectroscopy,” Spectrochim. Acta B 64, 1111–1118 (2009).
[CrossRef]

Radziemski, L. J.

D. A. Cremers and L. J. Radziemski, The Handbook of LIBS (Wiley, 2006).

Rusak, D. A.

D. A. Rusak, B. C. Castle, B. W. Smith, and J. D. Winefordner, “Fundamentals and applications of laser-induced breakdown spectroscopy,” Crit. Rev. Anal. Chem. 27, 257–290 (1997).
[CrossRef]

Schechter, I.

A. Miziolek, V. Palleschi, and I. Schechter, Laser-Induced Breakdown Spectroscopy (LIBS): Fundamentals and Applications (Cambridge University, 2006).

Singh, J. P.

Smith, B. W.

M. Tran, B. W. Smith, D. W. Hahn, and J. D. Winefordner, “Detection of gaseous and particulate fluorides by laser-induced breakdown spectroscopy,” Appl. Spectrosc. 55, 1455–1461 (2001).
[CrossRef]

D. A. Rusak, B. C. Castle, B. W. Smith, and J. D. Winefordner, “Fundamentals and applications of laser-induced breakdown spectroscopy,” Crit. Rev. Anal. Chem. 27, 257–290 (1997).
[CrossRef]

Thakur, S. N.

J. P. Singh and S. N. Thakur, Laser Induced Breakdown Spectroscopy (Elsevier Press, 2007).

Tjia, M. O.

Tran, M.

Uhl, R.

R. Uhl, J. Franzke, and U. Haas, “Detection of argon and krypton traces in noble gases by diode laser absorption spectrometry,” Appl. Phys. B 73, 71–74 (2001).
[CrossRef]

Weijun, Y.

Y. Weijun, “Trace analysis of impurities in bulk gases by gas chromatography-pulsed discharge helium ionization detection with ‘heart-cutting’ technique,” J. Chromatogr. A 1167, 225–230 (2007).
[CrossRef]

Whitehouse, A. I.

E. D. McNaghten, A. M. Parkes, B. C. Griffiths, A. I. Whitehouse, and S. Palanco, “Detection of trace concentrations of helium and argon in gas mixtures by laser-induced breakdown spectroscopy,” Spectrochim. Acta B 64, 1111–1118 (2009).
[CrossRef]

Winefordner, J. D.

M. Tran, B. W. Smith, D. W. Hahn, and J. D. Winefordner, “Detection of gaseous and particulate fluorides by laser-induced breakdown spectroscopy,” Appl. Spectrosc. 55, 1455–1461 (2001).
[CrossRef]

D. A. Rusak, B. C. Castle, B. W. Smith, and J. D. Winefordner, “Fundamentals and applications of laser-induced breakdown spectroscopy,” Crit. Rev. Anal. Chem. 27, 257–290 (1997).
[CrossRef]

Yueh, F.-Y.

Zhang, H.

Appl. Opt.

Appl. Phys. B

K. E. Eseller, F.-Y. Yueh, and J. P. Singh, “Non-intrusive, on-line, simultaneous multi-species impurity monitoring in hydrogen using LIBS,” Appl. Phys. B 102, 963–969 (2011).
[CrossRef]

R. Uhl, J. Franzke, and U. Haas, “Detection of argon and krypton traces in noble gases by diode laser absorption spectrometry,” Appl. Phys. B 73, 71–74 (2001).
[CrossRef]

Appl. Spectrosc.

Crit. Rev. Anal. Chem.

D. A. Rusak, B. C. Castle, B. W. Smith, and J. D. Winefordner, “Fundamentals and applications of laser-induced breakdown spectroscopy,” Crit. Rev. Anal. Chem. 27, 257–290 (1997).
[CrossRef]

J. Appl. Phys.

J. Camparo and G. Fathi, “Effects of rf power on electron density and temperature, neutral temperature, and T-e fluctuations in an inductively coupled plasma,” J. Appl. Phys. 105, 103302 (2009).
[CrossRef]

J. Chromatogr. A

Y. Weijun, “Trace analysis of impurities in bulk gases by gas chromatography-pulsed discharge helium ionization detection with ‘heart-cutting’ technique,” J. Chromatogr. A 1167, 225–230 (2007).
[CrossRef]

Radiat. Phys. Chem.

M. Hanafi, M. M. Omar, and Y. E. E.-D. Gamal, “Study of laser-induced breakdown spectroscopy of gases,” Radiat. Phys. Chem. 57, 11–20 (2000).
[CrossRef]

Spectrochim. Acta B

C. A. Henry, P. K. Diwakar, and D. W. Hahn, “Investigation of helium addition for laser induced plasma spectroscopy of pure gas phase systems: analyte interactions and signal enhancement,” Spectrochim. Acta B 62, 1390–1398 (2007).
[CrossRef]

E. D. McNaghten, A. M. Parkes, B. C. Griffiths, A. I. Whitehouse, and S. Palanco, “Detection of trace concentrations of helium and argon in gas mixtures by laser-induced breakdown spectroscopy,” Spectrochim. Acta B 64, 1111–1118 (2009).
[CrossRef]

Other

J. P. Singh and S. N. Thakur, Laser Induced Breakdown Spectroscopy (Elsevier Press, 2007).

A. Miziolek, V. Palleschi, and I. Schechter, Laser-Induced Breakdown Spectroscopy (LIBS): Fundamentals and Applications (Cambridge University, 2006).

D. A. Cremers and L. J. Radziemski, The Handbook of LIBS (Wiley, 2006).

NexAir website, http://www.nexair.com/ .

R. Griem, Spectral Line Broadening by Plasmas (Academic, 1974).

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Figures (5)

Fig. 1.
Fig. 1.

Schematic of the LIBS system for a hydrogen impurity monitor.

Fig. 2.
Fig. 2.

587.56 nm He line at different (a) laser energies, (b) gas pressures, and (c) gate delays (300 ns gate delay and a 1 µs gate width).

Fig. 3.
Fig. 3.

Signal-to-noise ratio for the He 587.56 nm line versus gate delay at different laser energies at 15.3 psi (791 Torr).

Fig. 4.
Fig. 4.

Calibration curve for helium in a hydrogen gas mixture. (Data recorded with a 300 ns gate delay and a 1 µs gate width.)

Fig. 5.
Fig. 5.

(a) Electron density as a function of helium concentration. (b) Hα line intensity as a function of helium concentration.

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