Abstract

This experiment was carried out to address the need for overcoming the difficulties encountered in hydrogen analysis by means of plasma emission spectroscopy in atmospheric ambient gas. The result of this study on zircaloy-4 samples from a nuclear power plant demonstrates the possibility of attaining a very sharp emission line from impure hydrogen with a very low background and practical elimination of spectral contamination of hydrogen emission arising from surface water and water vapor in atmospheric ambient gas. This was achieved by employing ultrapure ambient helium gas as well as the proper defocusing of the laser irradiation and a large number of repeated precleaning laser shots at the same spot of the sample surface. Further adjustment of the gating time has led to significant reduction of spectral width and improvement of detection sensitivity to 50  ppm. Finally, a linear calibration curve was also obtained for the zircaloy-4 samples with zero intercept. These results demonstrate the feasibility of this technique for practical in situ and quantitative analysis of hydrogen impurity in zircaloy-4 tubes used in a light water nuclear power plant.

© 2007 Optical Society of America

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References

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  1. K. H. Kurniawan, M. Pardede, R. Hedwig, Z. S. Lie, T. J. Lie, D. P. Kurniawan, M. Ramli, K. Fukumoto, H. Niki, S. N. Abdulmadjid, N. Idris, T. Maruyama, K. Kagawa, and M. O. Tjia, "Quantitative hydrogen analysis of zircaloy-4 using low-pressure laser plasma technique," Anal. Chem. 79, 2703-2707 (2007).
    [CrossRef] [PubMed]
  2. G. Asimellis, S. Hamilton, A. Giannoudakos, and M. Compitsas, "Controlled inert gas environment for enhanced chlorine and fluorine detection in the visible and near-infrared by laser-induced breakdown spectroscopy," Spectrochim. Acta , Part B 60, 1132-1139 (2005).
    [CrossRef]
  3. G. Asimellis, A. Giannoudakos, and M. Kompitsas, "New near-infrared LIBS detection technique for sulphur," Anal. Bioanal. Chem. 385, 333-337 (2006).
    [CrossRef] [PubMed]
  4. G. Asimellis, A. Giannoudakos, and M. Kompitsas, "Near-IR bromine laser induced breakdown spectroscopy detection and ambient gas effects on emission line asymmetric Stark broadening and shift," Spectrochim. Acta , Part B 61, 1270-1278 (2006).
    [CrossRef]
  5. K. H. Kurniawan and K. Kagawa, "Hydrogen and deuterium analysis using laser-induced plasma spectroscopy," Appl. Spectrosc. Rev. 41, 99-130 (2006).
    [CrossRef]
  6. M. Tran, Q. Sun, B. W. Smith, and J. D. Winefordner, "Determination of F, Cl and Br in solid organic compounds by laser-induced plasma spectroscopy," Appl. Spectrosc. 55, 739-744 (2001).
    [CrossRef]
  7. S. N. Abdulmadjid, M. M. Suliyanti, K. H. Kurniawan, T. J. Lie, M. Pardede, R. Hedwig, K. Kagawa, and M. O. Tjia, "An improved approach for hydrogen analysis in metal samples using single laser-induced gas plasma and target plasma at helium atmospheric pressure," Appl. Phys. B 82, 161-166 (2006).
    [CrossRef]
  8. M. Pardede, R. Hedwig, M. M. Suliyanti, Z. S. Lie, T. J. Lie, D. P. Kurniawan, K. H. Kurniawan, M. Ramli, K. Fukumoto, H. Niki, S. N. Abdulmadjid, N. Idris, T. Maruyama, K. Kagawa, and M. O. Tjia, "Comparative study of laser-induced plasma emission of hydrogen from zircaloy-2 samples in atmospheric and low-pressure ambient helium gas," Appl. Phys. B (to be published).

2007 (1)

K. H. Kurniawan, M. Pardede, R. Hedwig, Z. S. Lie, T. J. Lie, D. P. Kurniawan, M. Ramli, K. Fukumoto, H. Niki, S. N. Abdulmadjid, N. Idris, T. Maruyama, K. Kagawa, and M. O. Tjia, "Quantitative hydrogen analysis of zircaloy-4 using low-pressure laser plasma technique," Anal. Chem. 79, 2703-2707 (2007).
[CrossRef] [PubMed]

2006 (4)

S. N. Abdulmadjid, M. M. Suliyanti, K. H. Kurniawan, T. J. Lie, M. Pardede, R. Hedwig, K. Kagawa, and M. O. Tjia, "An improved approach for hydrogen analysis in metal samples using single laser-induced gas plasma and target plasma at helium atmospheric pressure," Appl. Phys. B 82, 161-166 (2006).
[CrossRef]

G. Asimellis, A. Giannoudakos, and M. Kompitsas, "New near-infrared LIBS detection technique for sulphur," Anal. Bioanal. Chem. 385, 333-337 (2006).
[CrossRef] [PubMed]

G. Asimellis, A. Giannoudakos, and M. Kompitsas, "Near-IR bromine laser induced breakdown spectroscopy detection and ambient gas effects on emission line asymmetric Stark broadening and shift," Spectrochim. Acta , Part B 61, 1270-1278 (2006).
[CrossRef]

K. H. Kurniawan and K. Kagawa, "Hydrogen and deuterium analysis using laser-induced plasma spectroscopy," Appl. Spectrosc. Rev. 41, 99-130 (2006).
[CrossRef]

2005 (1)

G. Asimellis, S. Hamilton, A. Giannoudakos, and M. Compitsas, "Controlled inert gas environment for enhanced chlorine and fluorine detection in the visible and near-infrared by laser-induced breakdown spectroscopy," Spectrochim. Acta , Part B 60, 1132-1139 (2005).
[CrossRef]

2001 (1)

Anal. Bioanal. Chem. (1)

G. Asimellis, A. Giannoudakos, and M. Kompitsas, "New near-infrared LIBS detection technique for sulphur," Anal. Bioanal. Chem. 385, 333-337 (2006).
[CrossRef] [PubMed]

Anal. Chem. (1)

K. H. Kurniawan, M. Pardede, R. Hedwig, Z. S. Lie, T. J. Lie, D. P. Kurniawan, M. Ramli, K. Fukumoto, H. Niki, S. N. Abdulmadjid, N. Idris, T. Maruyama, K. Kagawa, and M. O. Tjia, "Quantitative hydrogen analysis of zircaloy-4 using low-pressure laser plasma technique," Anal. Chem. 79, 2703-2707 (2007).
[CrossRef] [PubMed]

Appl. Phys. B (2)

S. N. Abdulmadjid, M. M. Suliyanti, K. H. Kurniawan, T. J. Lie, M. Pardede, R. Hedwig, K. Kagawa, and M. O. Tjia, "An improved approach for hydrogen analysis in metal samples using single laser-induced gas plasma and target plasma at helium atmospheric pressure," Appl. Phys. B 82, 161-166 (2006).
[CrossRef]

M. Pardede, R. Hedwig, M. M. Suliyanti, Z. S. Lie, T. J. Lie, D. P. Kurniawan, K. H. Kurniawan, M. Ramli, K. Fukumoto, H. Niki, S. N. Abdulmadjid, N. Idris, T. Maruyama, K. Kagawa, and M. O. Tjia, "Comparative study of laser-induced plasma emission of hydrogen from zircaloy-2 samples in atmospheric and low-pressure ambient helium gas," Appl. Phys. B (to be published).

Appl. Spectrosc. (1)

Appl. Spectrosc. Rev. (1)

K. H. Kurniawan and K. Kagawa, "Hydrogen and deuterium analysis using laser-induced plasma spectroscopy," Appl. Spectrosc. Rev. 41, 99-130 (2006).
[CrossRef]

Spectrochim. Acta (2)

G. Asimellis, S. Hamilton, A. Giannoudakos, and M. Compitsas, "Controlled inert gas environment for enhanced chlorine and fluorine detection in the visible and near-infrared by laser-induced breakdown spectroscopy," Spectrochim. Acta , Part B 60, 1132-1139 (2005).
[CrossRef]

G. Asimellis, A. Giannoudakos, and M. Kompitsas, "Near-IR bromine laser induced breakdown spectroscopy detection and ambient gas effects on emission line asymmetric Stark broadening and shift," Spectrochim. Acta , Part B 61, 1270-1278 (2006).
[CrossRef]

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Figures (9)

Fig. 1
Fig. 1

Sketch of experimental setup.

Fig. 2
Fig. 2

Plasma photographs taken from zircaloy-4 sample containing 4300 ppm of hydrogen under laser irradiation with (a) tight focus, (b) defocus at + 10   mm , and (c) defocus at + 15   mm .

Fig. 3
Fig. 3

Emission spectra of zircaloy-4 samples containing hydrogen of (a) 0 and (b) 4300 ppm concentrations at tight focus condition. The laser energy was fixed at 100   mJ . The gate delay and gate width of the OMA system were set at 1 and 50 μ s , respectively.

Fig. 4
Fig. 4

Emission spectra of zircaloy-4 samples containing hydrogen of (a) 0 and (b) 4300 ppm concentrations at defocus + 10   mm condition. The laser energy was fixed at 100   mJ . The gate delay and gate width of the OMA system were set at 1 and 50 μ s , respectively.

Fig. 5
Fig. 5

Emission spectra of zircaloy-4 samples containing hydrogen of (a) 0 and (b) 4300 ppm concentrations at defocus + 15   mm condition. The laser energy was fixed at 100   mJ . The gate delay and gate width of the OMA system were set at 1 and 50 μ s , respectively.

Fig. 6
Fig. 6

Emission spectra of zircaloy-4 sample containing 0 ppm of hydrogen. Spectra were obtained for the (a) first 100 laser shots and (b) next 100 laser shots. The data were obtained under defocus + 10   mm condition. The gate delay and gate width of the OMA system were set at 1 and 50 μ s , respectively.

Fig. 7
Fig. 7

Emission spectra of zircaloy-4 sample containing 4300 ppm of hydrogen measured at different gating times of (a) 1, (b) 5, and (c) 10 μ s . The gate width was fixed at 1 μs. The data were taken under defocus + 10   mm condition.

Fig. 8
Fig. 8

Calibration curve from zircaloy-4 samples of 0, 161, 461, 1000, and 4300 ppm hydrogen concentrations with the data obtained from the averaged results over 100 shots under defocus + 10   mm condition. The gate delay and gate width of the OMA system were set at 5 and 50 μ s , respectively.

Fig. 9
Fig. 9

Emission spectra of zircaloy-4 sample containing 161 ppm of hydrogen measured at defocus + 10   mm condition. The gate delay and gate width of the OMA system were set at 5 and 50 μ s , respectively.

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