Quantitative elemental analysis of steel using calibration-free laser-induced breakdown spectroscopy

M. L. Shah; A. K. Pulhani; G. P. Gupta; B. M. Suri

doi:10.1364/AO.51.004612

Applied Optics
Vol. 51,
Issue 20,
pp. 4612-4621
(2012)
•https://doi.org/10.1364/AO.51.004612

Quantitative elemental analysis of steel using calibration-free laser-induced breakdown spectroscopy

M. L. Shah, A. K. Pulhani, G. P. Gupta, and B. M. Suri

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M. L. Shah, A. K. Pulhani, G. P. Gupta, and B. M. Suri, "Quantitative elemental analysis of steel using calibration-free laser-induced breakdown spectroscopy," Appl. Opt. 51, 4612-4621 (2012)

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Abstract

We report the quantitative elemental analysis of a steel sample using calibration-free laser-induced breakdown spectroscopy (CF-LIBS). A $Q$ -switched Nd:YAG laser (532 nm wavelength) is used to produce a plasma by focusing it onto a steel sample in air at atmospheric pressure. The time-resolved spectra from atomic and ionic emission lines of the steel elements are recorded by an echelle grating spectrograph coupled with a gated intensified CCD camera and are used for the plasma characterization and quantitative analysis of the sample. The time delay at which the plasma is in local thermodynamic equilibrium as well as optically thin, necessary for elemental analysis, is deduced. An algorithm for the CF-LIBS relating the experimentally measured spectral intensity values with the basic physics of the plasma is developed and used for the determination of Fe, Cr, Ni, Mg, and Si concentrations in the steel sample. The analytical results obtained from the CF-LIBS technique agree well with the certified values of the elements in the sample, with relative uncertainties of less than 5%.

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		Energy level (eV)
Species	Wavelength (nm)	Upper	Lower	Upper level degeneracy	Transition probability ( $s^{- 1}$ )
Fe I	346.59	3.686	0.110	3	$1.19 \times 10^{7}$
	355.49	6.319	2.832	13	$1.40 \times 10^{8}$
	361.88	4.415	0.990	7	$7.22 \times 10^{7}$
	396.93	4.608	1.485	7	$2.26 \times 10^{7}$
	425.08	4.473	1.557	7	$1.02 \times 10^{7}$
	426.05	5.308	2.399	11	$3.99 \times 10^{7}$
	432.58	4.473	1.608	7	$5.16 \times 10^{7}$
	492.05	5.352	2.832	9	$3.58 \times 10^{7}$
Fe II	233.28	5.361	0.048	6	$1.31 \times 10^{8}$
	233.80	5.408	0.107	4	$1.13 \times 10^{8}$
	241.33	5.257	0.121	4	$1.02 \times 10^{8}$
Cr I	520.84	3.321	0.941	7	$5.06 \times 10^{7}$
Ni I	352.45	3.542	0.025	5	$1.0 \times 10^{8}$
Mn I	404.14	5.181	2.114	10	$7.87 \times 10^{7}$
Si I	288.16	5.082	0.781	3	$2.17 \times 10^{8}$

Quantity	Value
$T$ (eV)	0.875
$n_{e} ({cm}^{- 3})$	$9.8 \times 10^{16}$
$n_{Cr I} / n_{Fe II}$	$3.24 \times 10^{- 2}$
$n_{Ni I} / n_{Fe II}$	$3.01 \times 10^{- 2}$
$n_{Si I} / n_{Fe II}$	$4.67 \times 10^{- 3}$
$n_{Mn I} / n_{Fe II}$	$5.80 \times 10^{- 3}$
$n_{Fe II} / n_{Fe I}$	6.7

	Concentration (wt. %)
Element	Certified	LIBS-determined	Relative uncertainty (%)
Fe	72.40	72.66	0.4
Cr	18.30	17.88	2.3
Ni	8.03	8.25	2.7
Mn	0.82	0.86	4.9
Si	0.33	0.34	3.0

		Energy level (eV)
Species	Wavelength (nm)	Upper	Lower	Upper level degeneracy	Transition probability ( $s^{- 1}$ )
Fe I	346.59	3.686	0.110	3	$1.19 \times 10^{7}$
	355.49	6.319	2.832	13	$1.40 \times 10^{8}$
	361.88	4.415	0.990	7	$7.22 \times 10^{7}$
	396.93	4.608	1.485	7	$2.26 \times 10^{7}$
	425.08	4.473	1.557	7	$1.02 \times 10^{7}$
	426.05	5.308	2.399	11	$3.99 \times 10^{7}$
	432.58	4.473	1.608	7	$5.16 \times 10^{7}$
	492.05	5.352	2.832	9	$3.58 \times 10^{7}$
Fe II	233.28	5.361	0.048	6	$1.31 \times 10^{8}$
	233.80	5.408	0.107	4	$1.13 \times 10^{8}$
	241.33	5.257	0.121	4	$1.02 \times 10^{8}$
Cr I	520.84	3.321	0.941	7	$5.06 \times 10^{7}$
Ni I	352.45	3.542	0.025	5	$1.0 \times 10^{8}$
Mn I	404.14	5.181	2.114	10	$7.87 \times 10^{7}$
Si I	288.16	5.082	0.781	3	$2.17 \times 10^{8}$

Quantity	Value
$T$ (eV)	0.875
$n_{e} ({cm}^{- 3})$	$9.8 \times 10^{16}$
$n_{Cr I} / n_{Fe II}$	$3.24 \times 10^{- 2}$
$n_{Ni I} / n_{Fe II}$	$3.01 \times 10^{- 2}$
$n_{Si I} / n_{Fe II}$	$4.67 \times 10^{- 3}$
$n_{Mn I} / n_{Fe II}$	$5.80 \times 10^{- 3}$
$n_{Fe II} / n_{Fe I}$	6.7

Abstract

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Equations (20)

Applied Optics