Abstract

Laser-induced breakdown spectrometry (LIBS) with multiple pulse excitation has been applied for the multielemental analysis of liquid steel. The laser beam and the measuring radiation are guided inside a moveable lance to gain access to the melt surface from the top. Low-alloy steel grades were investigated with a focus on the light elements phosphorus, sulfur, and carbon by use of emission wavelengths in the vacuum ultraviolet. Calibration curves were determined for the elements carbon, phosphorus, sulfur, nickel, and chromium in steel melts of 100 kg. The estimated limits of detection for the light elements phosphorus, sulfur, and carbon are below 21 µg/g for direct analysis of liquid steel with LIBS. The results demonstrate the potential of the laser-based analysis to fulfill the requirements for a process integrated on-line analysis in the secondary metallurgy of steel works.

© 2003 Optical Society of America

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References

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  1. H. Richter, H. Rzepczyk, D. Tembergen, “Prozessteuerung sekundärmetallurgischer Verfahren,” Stahl und Eisen 114, 110–113 (1994), in German.
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    [CrossRef]
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    [CrossRef]
  7. R. Sattmann, V. Sturm, R. Noll, “Laser-induced breakdown spectroscopy of steel samples using multiple Q-switch Nd:YAG laser pulses,” J. Phys. D 28, 2181–2187 (1995).
    [CrossRef]
  8. R. Noll, R. Sattmann, V. Sturm, S. Lüngen, H.-J. von Wachtendonk, “Schnelle Multielement-Analyse in der Stahlschmelze mit laserinduzierter Emissionsspektrometrie,” Stahl und Eisen 117, 57–62 (1997), in German.
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    [CrossRef]
  10. M. Khater, J. Costello, E. Kennedy, “Optimization of the emission characteristics of laser-produced steel plasmas in the vacuum ultraviolet: significant improvements in carbon detection limits,” Appl. Spectrosc. 56, 970–984 (2002).
    [CrossRef]
  11. R. Noll, V. Sturm, L. Peter, R. Hakala, J. Viirret, H. W. Gudenau, K. Mavrommatis, L. Ernenputsch, “Sensitivity-enhanced laser analysis (SELA) of steel melts for a fast multi-element online analysis during ladle processing in secondary metallurgy,” in EUR 19411—Analytical Techniques for Processes, Products and the Environment, Technical Steel Research Series (European Commission Office for Official Publications of the European Communities, Luxembourg, 2001).
  12. V. N. Rai, F.-Y. Yueh, J. P. Singh, “Study of laser-induced breakdown emission from liquid under double pulse excitation,” Appl. Opt. 42, 2094–2101 (2003).
    [CrossRef] [PubMed]
  13. National Standard of Germany, DIN 32 645: Nachweis-, Erfassungs- und Bestimmungsgrenze (Beuth Verlag, Berlin, Germany, 1994).

2003 (1)

2002 (1)

2001 (1)

J. Gruber, J. Heitz, H. Strasser, D. Bäuerle, N. Ramaseder, “Rapid in situ analysis of liquid steel by laser-induced breakdown spectroscopy,” Spectrochim. Acta Part B 56, 685–693 (2001).
[CrossRef]

2000 (1)

1997 (1)

R. Noll, R. Sattmann, V. Sturm, S. Lüngen, H.-J. von Wachtendonk, “Schnelle Multielement-Analyse in der Stahlschmelze mit laserinduzierter Emissionsspektrometrie,” Stahl und Eisen 117, 57–62 (1997), in German.

1995 (2)

R. Sattmann, V. Sturm, R. Noll, “Laser-induced breakdown spectroscopy of steel samples using multiple Q-switch Nd:YAG laser pulses,” J. Phys. D 28, 2181–2187 (1995).
[CrossRef]

H. Richter, H. Rzepczyk, D. Tembergen, “Qualitätsbezogene Prozessteuerung in der Sekundärmetallurgie eines Oxygenstahlwerkes,” Stahl und Eisen 115, 83–87 (1995), in German.

1994 (1)

H. Richter, H. Rzepczyk, D. Tembergen, “Prozessteuerung sekundärmetallurgischer Verfahren,” Stahl und Eisen 114, 110–113 (1994), in German.

1993 (1)

1991 (1)

C. Carlhoff, “Laserinduzierte Emissionsspektroskopie für die Direktanalyse von flüssigem Stahl im Konverter,” Laser Optoelectron. 23, 50–52 (1991), in German.

Aguilera, J.

Aragon, C.

Bäuerle, D.

J. Gruber, J. Heitz, H. Strasser, D. Bäuerle, N. Ramaseder, “Rapid in situ analysis of liquid steel by laser-induced breakdown spectroscopy,” Spectrochim. Acta Part B 56, 685–693 (2001).
[CrossRef]

Campos, J.

Carlhoff, C.

C. Carlhoff, “Laserinduzierte Emissionsspektroskopie für die Direktanalyse von flüssigem Stahl im Konverter,” Laser Optoelectron. 23, 50–52 (1991), in German.

Costello, J.

Ernenputsch, L.

R. Noll, V. Sturm, L. Peter, R. Hakala, J. Viirret, H. W. Gudenau, K. Mavrommatis, L. Ernenputsch, “Sensitivity-enhanced laser analysis (SELA) of steel melts for a fast multi-element online analysis during ladle processing in secondary metallurgy,” in EUR 19411—Analytical Techniques for Processes, Products and the Environment, Technical Steel Research Series (European Commission Office for Official Publications of the European Communities, Luxembourg, 2001).

Gruber, J.

J. Gruber, J. Heitz, H. Strasser, D. Bäuerle, N. Ramaseder, “Rapid in situ analysis of liquid steel by laser-induced breakdown spectroscopy,” Spectrochim. Acta Part B 56, 685–693 (2001).
[CrossRef]

Gudenau, H. W.

R. Noll, V. Sturm, L. Peter, R. Hakala, J. Viirret, H. W. Gudenau, K. Mavrommatis, L. Ernenputsch, “Sensitivity-enhanced laser analysis (SELA) of steel melts for a fast multi-element online analysis during ladle processing in secondary metallurgy,” in EUR 19411—Analytical Techniques for Processes, Products and the Environment, Technical Steel Research Series (European Commission Office for Official Publications of the European Communities, Luxembourg, 2001).

Hakala, R.

R. Noll, V. Sturm, L. Peter, R. Hakala, J. Viirret, H. W. Gudenau, K. Mavrommatis, L. Ernenputsch, “Sensitivity-enhanced laser analysis (SELA) of steel melts for a fast multi-element online analysis during ladle processing in secondary metallurgy,” in EUR 19411—Analytical Techniques for Processes, Products and the Environment, Technical Steel Research Series (European Commission Office for Official Publications of the European Communities, Luxembourg, 2001).

Heitz, J.

J. Gruber, J. Heitz, H. Strasser, D. Bäuerle, N. Ramaseder, “Rapid in situ analysis of liquid steel by laser-induced breakdown spectroscopy,” Spectrochim. Acta Part B 56, 685–693 (2001).
[CrossRef]

Kennedy, E.

Khater, M.

Lüngen, S.

R. Noll, R. Sattmann, V. Sturm, S. Lüngen, H.-J. von Wachtendonk, “Schnelle Multielement-Analyse in der Stahlschmelze mit laserinduzierter Emissionsspektrometrie,” Stahl und Eisen 117, 57–62 (1997), in German.

Mavrommatis, K.

R. Noll, V. Sturm, L. Peter, R. Hakala, J. Viirret, H. W. Gudenau, K. Mavrommatis, L. Ernenputsch, “Sensitivity-enhanced laser analysis (SELA) of steel melts for a fast multi-element online analysis during ladle processing in secondary metallurgy,” in EUR 19411—Analytical Techniques for Processes, Products and the Environment, Technical Steel Research Series (European Commission Office for Official Publications of the European Communities, Luxembourg, 2001).

Noll, R.

V. Sturm, L. Peter, R. Noll, “Steel analysis with laser-induced breakdown spectrometry in the vacuum ultraviolet,” Appl. Spectrosc. 54, 1275–1278 (2000).
[CrossRef]

R. Noll, R. Sattmann, V. Sturm, S. Lüngen, H.-J. von Wachtendonk, “Schnelle Multielement-Analyse in der Stahlschmelze mit laserinduzierter Emissionsspektrometrie,” Stahl und Eisen 117, 57–62 (1997), in German.

R. Sattmann, V. Sturm, R. Noll, “Laser-induced breakdown spectroscopy of steel samples using multiple Q-switch Nd:YAG laser pulses,” J. Phys. D 28, 2181–2187 (1995).
[CrossRef]

R. Noll, V. Sturm, L. Peter, R. Hakala, J. Viirret, H. W. Gudenau, K. Mavrommatis, L. Ernenputsch, “Sensitivity-enhanced laser analysis (SELA) of steel melts for a fast multi-element online analysis during ladle processing in secondary metallurgy,” in EUR 19411—Analytical Techniques for Processes, Products and the Environment, Technical Steel Research Series (European Commission Office for Official Publications of the European Communities, Luxembourg, 2001).

R. Noll, V. Sturm, L. Peter, I. Whiteside, “Analysis using lasers,” in Proceedings of the 49th Chemists’ Conference, R. Jowitt, ed. (British Steel, Middlesbrough, U.K., 1997), pp. 22–27.

Peter, L.

V. Sturm, L. Peter, R. Noll, “Steel analysis with laser-induced breakdown spectrometry in the vacuum ultraviolet,” Appl. Spectrosc. 54, 1275–1278 (2000).
[CrossRef]

R. Noll, V. Sturm, L. Peter, I. Whiteside, “Analysis using lasers,” in Proceedings of the 49th Chemists’ Conference, R. Jowitt, ed. (British Steel, Middlesbrough, U.K., 1997), pp. 22–27.

R. Noll, V. Sturm, L. Peter, R. Hakala, J. Viirret, H. W. Gudenau, K. Mavrommatis, L. Ernenputsch, “Sensitivity-enhanced laser analysis (SELA) of steel melts for a fast multi-element online analysis during ladle processing in secondary metallurgy,” in EUR 19411—Analytical Techniques for Processes, Products and the Environment, Technical Steel Research Series (European Commission Office for Official Publications of the European Communities, Luxembourg, 2001).

Rai, V. N.

Ramaseder, N.

J. Gruber, J. Heitz, H. Strasser, D. Bäuerle, N. Ramaseder, “Rapid in situ analysis of liquid steel by laser-induced breakdown spectroscopy,” Spectrochim. Acta Part B 56, 685–693 (2001).
[CrossRef]

Richter, H.

H. Richter, H. Rzepczyk, D. Tembergen, “Qualitätsbezogene Prozessteuerung in der Sekundärmetallurgie eines Oxygenstahlwerkes,” Stahl und Eisen 115, 83–87 (1995), in German.

H. Richter, H. Rzepczyk, D. Tembergen, “Prozessteuerung sekundärmetallurgischer Verfahren,” Stahl und Eisen 114, 110–113 (1994), in German.

Rzepczyk, H.

H. Richter, H. Rzepczyk, D. Tembergen, “Qualitätsbezogene Prozessteuerung in der Sekundärmetallurgie eines Oxygenstahlwerkes,” Stahl und Eisen 115, 83–87 (1995), in German.

H. Richter, H. Rzepczyk, D. Tembergen, “Prozessteuerung sekundärmetallurgischer Verfahren,” Stahl und Eisen 114, 110–113 (1994), in German.

Sattmann, R.

R. Noll, R. Sattmann, V. Sturm, S. Lüngen, H.-J. von Wachtendonk, “Schnelle Multielement-Analyse in der Stahlschmelze mit laserinduzierter Emissionsspektrometrie,” Stahl und Eisen 117, 57–62 (1997), in German.

R. Sattmann, V. Sturm, R. Noll, “Laser-induced breakdown spectroscopy of steel samples using multiple Q-switch Nd:YAG laser pulses,” J. Phys. D 28, 2181–2187 (1995).
[CrossRef]

Singh, J. P.

Strasser, H.

J. Gruber, J. Heitz, H. Strasser, D. Bäuerle, N. Ramaseder, “Rapid in situ analysis of liquid steel by laser-induced breakdown spectroscopy,” Spectrochim. Acta Part B 56, 685–693 (2001).
[CrossRef]

Sturm, V.

V. Sturm, L. Peter, R. Noll, “Steel analysis with laser-induced breakdown spectrometry in the vacuum ultraviolet,” Appl. Spectrosc. 54, 1275–1278 (2000).
[CrossRef]

R. Noll, R. Sattmann, V. Sturm, S. Lüngen, H.-J. von Wachtendonk, “Schnelle Multielement-Analyse in der Stahlschmelze mit laserinduzierter Emissionsspektrometrie,” Stahl und Eisen 117, 57–62 (1997), in German.

R. Sattmann, V. Sturm, R. Noll, “Laser-induced breakdown spectroscopy of steel samples using multiple Q-switch Nd:YAG laser pulses,” J. Phys. D 28, 2181–2187 (1995).
[CrossRef]

R. Noll, V. Sturm, L. Peter, R. Hakala, J. Viirret, H. W. Gudenau, K. Mavrommatis, L. Ernenputsch, “Sensitivity-enhanced laser analysis (SELA) of steel melts for a fast multi-element online analysis during ladle processing in secondary metallurgy,” in EUR 19411—Analytical Techniques for Processes, Products and the Environment, Technical Steel Research Series (European Commission Office for Official Publications of the European Communities, Luxembourg, 2001).

R. Noll, V. Sturm, L. Peter, I. Whiteside, “Analysis using lasers,” in Proceedings of the 49th Chemists’ Conference, R. Jowitt, ed. (British Steel, Middlesbrough, U.K., 1997), pp. 22–27.

Tembergen, D.

H. Richter, H. Rzepczyk, D. Tembergen, “Qualitätsbezogene Prozessteuerung in der Sekundärmetallurgie eines Oxygenstahlwerkes,” Stahl und Eisen 115, 83–87 (1995), in German.

H. Richter, H. Rzepczyk, D. Tembergen, “Prozessteuerung sekundärmetallurgischer Verfahren,” Stahl und Eisen 114, 110–113 (1994), in German.

Viirret, J.

R. Noll, V. Sturm, L. Peter, R. Hakala, J. Viirret, H. W. Gudenau, K. Mavrommatis, L. Ernenputsch, “Sensitivity-enhanced laser analysis (SELA) of steel melts for a fast multi-element online analysis during ladle processing in secondary metallurgy,” in EUR 19411—Analytical Techniques for Processes, Products and the Environment, Technical Steel Research Series (European Commission Office for Official Publications of the European Communities, Luxembourg, 2001).

von Wachtendonk, H.-J.

R. Noll, R. Sattmann, V. Sturm, S. Lüngen, H.-J. von Wachtendonk, “Schnelle Multielement-Analyse in der Stahlschmelze mit laserinduzierter Emissionsspektrometrie,” Stahl und Eisen 117, 57–62 (1997), in German.

Whiteside, I.

R. Noll, V. Sturm, L. Peter, I. Whiteside, “Analysis using lasers,” in Proceedings of the 49th Chemists’ Conference, R. Jowitt, ed. (British Steel, Middlesbrough, U.K., 1997), pp. 22–27.

Yueh, F.-Y.

Appl. Opt. (1)

Appl. Spectrosc. (3)

J. Phys. D (1)

R. Sattmann, V. Sturm, R. Noll, “Laser-induced breakdown spectroscopy of steel samples using multiple Q-switch Nd:YAG laser pulses,” J. Phys. D 28, 2181–2187 (1995).
[CrossRef]

Laser Optoelectron. (1)

C. Carlhoff, “Laserinduzierte Emissionsspektroskopie für die Direktanalyse von flüssigem Stahl im Konverter,” Laser Optoelectron. 23, 50–52 (1991), in German.

Spectrochim. Acta Part B (1)

J. Gruber, J. Heitz, H. Strasser, D. Bäuerle, N. Ramaseder, “Rapid in situ analysis of liquid steel by laser-induced breakdown spectroscopy,” Spectrochim. Acta Part B 56, 685–693 (2001).
[CrossRef]

Stahl und Eisen (3)

H. Richter, H. Rzepczyk, D. Tembergen, “Prozessteuerung sekundärmetallurgischer Verfahren,” Stahl und Eisen 114, 110–113 (1994), in German.

H. Richter, H. Rzepczyk, D. Tembergen, “Qualitätsbezogene Prozessteuerung in der Sekundärmetallurgie eines Oxygenstahlwerkes,” Stahl und Eisen 115, 83–87 (1995), in German.

R. Noll, R. Sattmann, V. Sturm, S. Lüngen, H.-J. von Wachtendonk, “Schnelle Multielement-Analyse in der Stahlschmelze mit laserinduzierter Emissionsspektrometrie,” Stahl und Eisen 117, 57–62 (1997), in German.

Other (3)

R. Noll, V. Sturm, L. Peter, R. Hakala, J. Viirret, H. W. Gudenau, K. Mavrommatis, L. Ernenputsch, “Sensitivity-enhanced laser analysis (SELA) of steel melts for a fast multi-element online analysis during ladle processing in secondary metallurgy,” in EUR 19411—Analytical Techniques for Processes, Products and the Environment, Technical Steel Research Series (European Commission Office for Official Publications of the European Communities, Luxembourg, 2001).

National Standard of Germany, DIN 32 645: Nachweis-, Erfassungs- und Bestimmungsgrenze (Beuth Verlag, Berlin, Germany, 1994).

R. Noll, V. Sturm, L. Peter, I. Whiteside, “Analysis using lasers,” in Proceedings of the 49th Chemists’ Conference, R. Jowitt, ed. (British Steel, Middlesbrough, U.K., 1997), pp. 22–27.

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Figures (7)

Fig. 1
Fig. 1

Schematic setup for LIBS of liquid steel. M, mirror; L, lens; W1, W2, W3 windows; MH, mirror with a hole; OP, optical probe; PL, permanent part of measuring lance; T, tip of lance; MT, steel melt; P, platform; H, housing; ES, entrance slit of spectrometer; A, vertical axis; V, vacuum pump; BT, beam tube.

Fig. 2
Fig. 2

Schematic view of the lower part of the model lance. LB, laser beam; G, gas flow; WF, water flow. Further abbreviations: see Fig. 1.

Fig. 3
Fig. 3

Calibration curve of carbon in liquid steel.

Fig. 4
Fig. 4

Calibration curve of phosphorus in liquid steel.

Fig. 5
Fig. 5

Calibration curve of sulfur in liquid steel.

Fig. 6
Fig. 6

Calibration curve of nickel in liquid steel.

Fig. 7
Fig. 7

Calibration curve of chromium in liquid steel.

Tables (1)

Tables Icon

Table 1 Analyzed Elements, Estimated Limits of Detection, Background Equivalent Concentration, Concentration Range of Calibration, Concentration Range of Linear Fit, and Coefficient of Determination for the Linear Fitting Curve (r2) for LIBS On-Line Analysis of Liquid Steel

Metrics