Laser Induced Breakdown Spectroscopy

Diane M Wong, A3 Technologies LLC, Aberdeen, MD, USA

Alexander A Bol’shakov, A3 Technologies LLC, Aberdeen, MD, USA and Applied Spectra Inc., Fremont, CA, USA
Richard E Russo, A3 Technologies LLC, Aberdeen, MD, USA, Applied Spectra Inc., Fremont, CA, USA and
Lawrence Berkeley National Laboratory, Berkeley, CA, USA
& 2010 Elsevier Ltd. All rights reserved.

specific requirements for the sample to fluoresce, be

Abbreviations
IB inverse bremsstrahlung
Raman-active or infrared-sensitive. It is truly a universal
technique, where any sample type can yield a LIBS
ICP-AES inductively coupled plasma-atomic
spectrum.
emission spectrometry
ICP-MS inductively coupled plasma-mass
spectrometry
Theory of Laser-Induced Breakdown
LIBS laser-induced breakdown
Spectroscopy
spectroscopy
LSD laser-supported detonation
In practice, LIBS is a very simple spectroscopic techni-
LTE local thermodynamic equilibrium
que to implement. A high-powered laser beam (com-
MPI multiphoton ionization
monly 10-ns pulsed infrared 1.06 mm radiation) is focused
UV ultraviolet
through a lens to produce a plasma. The emitted light is
collected, often through a fiber optic cable, and directed
into a spectrometer (Figure 1). However, the physics and
chemistry of the plasma initiation, formation, lifetime,
Introduction
and decay are very complicated. Much progress has been
made in recent years toward elucidating the physics
Laser-induced breakdown spectroscopy (LIBS) is a
of the plasma generation processes. Studies that have
powerful analytical technique that can be used for the
been performed to characterize the LIBS plasma include
detection and characterization of materials. In LIBS, a
local thermodynamic equilibrium (LTE) models, hydro-
focused laser beam is used to generate a plasma plume on
dynamic and kinetic models, nonuniform plasmas, and
the surface of solid and liquid samples or inside the
plasmas generated in a vacuum.
sample volume of gases, liquids, and aerosols. Each ex-
There are two main processes that can initiate ion-
cited atom in the plasma emits a unique set of spectral
ization of atomic and molecular species in laser-induced
lines, particularly in the optical region of the spectrum.
breakdown. The first is the direct ionization of the
Therefore, this optical emission can be collected and
sample by multiphoton ionization (MPI), and the second
analyzed to determine the chemical composition of a
is the inverse bremsstrahlung (IB) absorption processes.
sample. A LIBS plasma can be generated as a single event
In MPI, atoms or molecules undergo simultaneous ab-
using just one laser pulse or using repetitive laser pulses.
sorption of sufficient numbers of photons to cause ion-
As a result, localized microanalysis with lateral and depth
ization (or the ejection of electrons from the valence to
profiling information is easily obtained. Remote sensing
the conduction band, in the case of metals) (eqn [1]).
of materials is also possible with LIBS, since only photons
need to come in direct contact with the sample. The
ability to perform analyses on samples at a standoff M þ mðhvÞ- M þ þ e  ½1
distance is especially important when dealing with
hazardous materials, samples located in a dangerous If EI is the ionization potential, then m, the number of
environment, or in physically inaccessible locations. photons, must be greater than the integer part of (EI/
LIBS has a distinct advantage over many other tech- hn þ 1). MPI is only significant at wavelengths that are
niques since little or no sample preparation is needed shorter than B1 mm and at high laser power, that is,
before analysis, and it can be used for rapid real-time greater than 1010 W/cm2. When the wavelength is sub-
analysis in field operations. Quantitative analytical results stantially longer than B1 mm, it is statistically unlikely
can be obtained from LIBS by using conventional (one- for an atom or molecule to absorb enough photons to
element) or multivariate calibration. Recently, cali- increase the energy of the neutral above its ionization
bration-free LIBS analysis has been demonstrated as the potential. This process is also important at low pressures,
semiquantitative determination of elements, based on when few collisions are occurring due to the low particle
theoretical plasma models. With LIBS, there are no density of the medium.

1281
1282 Laser Induced Breakdown Spectroscopy
Laser-induced breakdown spectroscopy
Laser
power supply
Laser head
Input optical fiber
PC
Figure 1 Schematic diagram of a typical lab bench LIBS setup.
IB processes involve the absorption of a photon by one
or more seed electrons present in the focal volume at the
beginning of the laser pulse. These initial free electrons
may be generated through the presence of cosmic rays, or
by the Earth’s natural radiation. The first few photons in
a laser pulse can also produce seed electrons from dust,
–
negative ions, such as O2, organic vapors, or from atoms
and molecules present in the atmosphere via MPI. Seed
electrons are not necessary for ‘pure’ MPI processes.
In IB, the absorption of a photon raises the electron
energy to a higher state in the continuum. This process
must occur in the vicinity of a heavy particle, such as an
atom, ion, or molecule so that momentum is conserved.
In normal bremsstrahlung processes, high-energy elec-
trons emit radiation as they slow down upon interacting
with a gas or a solid. This term comes from the German
words, bremsen, which means to slow down, and strah-
lung, which means radiation. Electrons will typically lose
energy by rotational and vibrational excitation of neutral
molecules, excitation of electronic states, and by attach-
ment of electrons. However, in IB processes, electrons
acquire energy from the absorbance of photons and
collisions with atoms, ions, and molecules. If the energy
of the free electron is greater than the ionization po-
tential of a neutral species, it can ionize a molecule (M)
by colliding with it. This produces two lower-energy free
electrons, which can gain more energy from the electric
field, causing ionization of other neutrals and two more
electrons (eqn [2]).
e  þ M- 2e  þ M þ
With the increase in the population of ions and electrons
in the focal volume, the probability of electron–photon
neutral collisions also increases, resulting in electron
multiplication and cascade growth. As more and more
electrons repeat the process, there is a geometric growth
(LIBS)
Focusing lens Laser spark
Unknown material
Collection lenses
Spectrograph
Delay generator
Detector controller
in the number of free electrons, resulting in cascade
ionization. IB processes can be so dramatic that all the
species ablated from the surface of the substrate can
be ionized causing such an increase in plasma growth
that the entire laser pulse can be coupled into the plasma.
This results in the plasma becoming so optically opaque
that the substrate becomes shielded from the remainder
of the laser pulse.
Both MPI and IB absorption can contribute to cascade
ionization. The dominant process will depend on the
wavelength of the laser radiation, laser intensity, and
density of the medium in which the laser breakdown
occurs. IB-dominated breakdown is important at high
pressures, when collisional effects are strong, and at
wavelengths longer than 1 mm. At shorter irradiation
wavelengths (o1 mm) or at low densities of molecules,
the possibility of electrons colliding with neutral species
is small. Therefore, MPI dominates usually at these
shorter wavelengths and in low-density media. Cascade
ionization continues throughout the duration of the laser
pulse and results in the ionization and dielectric break-
down of gases, vaporized particles, and the creation of a
plasma.
Plasma Life Cycle
The plasma generated by a focused laser beam in LIBS
has a distinct, time-dependent life cycle. For a plasma to
be created, the breakdown threshold must be reached.
½2 This breakdown threshold is usually defined qualita-
tively as the minimum irradiance needed to generate a
visible plasma. With the exponential increase in the
production of free electrons and ions by IB and MPI
processes, the plasma begins to expand from the initial
focal volume. Ablated materials, such as particulates,
ions, molecules, neutrals, and electrons, are also present

in the plasma that forms at the surface of the sample in
solids and liquids. The ionization potential of gases is
generally higher than that of liquids and solids, but they
too can be readily analyzed by LIBS. Using higher-
energy densities, gases can be ionized with a tightly
focused laser to produce a plasma in the sample volume.
A sonic boom is produced from the initial expansion of
the plasma. The compression wave front, or shock wave,
emanates from the focal volume of the plasma. The wave
front is traveling well above the speed of sound, on the
order of 105 ms–1. For comparison, the speed of sound in
air is B345 ms–1 at 211C. As the plasma expands, it
continuously emits spectroscopic signals from all con-
stituent components in the sample. When the plasma
cools through radiation and other loss mechanisms, the
ionized species recombine to form neutral atoms and
molecules.
Throughout the lifetime of the plasma, the emission
spectrum changes as a function of time. In the earliest
phase, there is a strong white light component, which
contains little useful spectroscopic information. This
continuum light consists mainly of bremsstrahlung
and recombination radiation. Recombination radiation is
caused by the recombination of free electrons and ions.
As stated earlier, bremsstrahlung radiation is caused by
the decrease in the translational energy that occurs when
ions and electrons slow down upon collision with a gas or
solid. This is in contrast to IB processes, which cause
cascade ionization during the initial breakdown event.
After the laser pulse, the continuum gradually fades
allowing the weaker spectroscopic signals from the
elements of interest to be detected. This occurs in a time
frame that is much longer than the laser pulse duration,
which in a nanosecond laser is on the order of 10 ns.
Since the weaker signals only appear as the continuum
fades, the collection of the spectroscopic signal of interest
should be delayed.
Time parameters in LIBS are important consider-
ations when obtaining emission spectra. At low laser
pulse energies, that is, several millijoules, the time
delay may need to be less than 1 ns in duration to ob-
tain an optimal signal. With higher laser powers, the
delay may be several microseconds. Too short a
gate width will not allow enough signal to be processed
across the detector. Too long a gate width will allow
too much ambient light to enter the detector thus ad-
versely affecting the signal to noise ratio. Optimization
of the time delay and gate width should be performed
on the individual samples to maximize the relative
intensities of the emission lines for the signatures
of interest. Sample properties, such as substrate, matrix,
and concentration, and experimental conditions such as
laser power, wavelength, and pulse width, can all influ-
ence the temperature and energy density of the plasma
(Figure 2).
Laser Induced Breakdown Spectroscopy 1283
LIBS Emission Signal Enhancement –
Background Gas Effects
Different background gases are often utilized to enhance
the quality and intensity of the LIBS plasma, especially
for the analysis of complicated or difficult samples. The
use of argon gas is a common technique to effectively
enhance the LIBS emission signal. In this method, a
steady stream of gas is directed toward the focal volume
of the plasma. This increases both the intensity and
quality of the signal by displacing the background air and
making it easier to generate a plasma. Calculations of
electron densities and plasma temperatures of plasmas
created in difference background gases show that argon
produces the highest temperatures and electron densities,
followed by ambient air. Helium is associated with the
lowest temperatures and densities.
When laser ablation is performed in a vacuum, lower
temperatures are attained and lower concentrations of
electrons are seen in the plasma volume than in a gaseous
environment. Since there is no pressure counteracting
free plasma expansion in the vacuum, the expansion rate
is increased whereas the cooling rate is decreased as
compared to expansion in a gas. This decrease in cooling
rate of the excited electrons can be explained by the
dominance of elastic collisions. Since cooling is inversely
proportional to the mass of the background gas, heavier
gases like argon have a less efficient cooling capacity than
helium or air. Therefore, using argon will produce higher
plasma temperatures with greater electron density than
one produced in ambient air or gases with lower atomic
masses, like helium. Argon also displaces the nitrogen
and oxygen molecules in the air. This effectively elim-
inates any interference from these molecules in the an-
alysis of species that contain nitrogen and oxygen atoms,
including organic compounds.
When argon gas is utilized, a laser-supported det-
onation (LSD) wave can be observed at the tip of the
vapor plume 3 ns after the laser pulse. An LSD wave
occurs when a shock wave front, expanding at supersonic
speeds, is transmissive enough to allow the incoming
laser energy to penetrate the boundary of the plasma
and the surrounding atmospheric gases. The shock wave
is powerful enough to compress and heat the gases
surrounding the plasma, thus allowing for strong optical
absorption of the incoming laser radiation. The com-
pression of background gases by the shock wave en-
hances the conversion of kinetic energy into thermal
energy in the vapor plume by slowing the rate of vapor
plume expansion. As a result, the vapor plume generated
with a background gas of argon continues to increase in
temperature and electron number density after the laser
pulse ends. The LSD is thought to create an area of high
temperature and low gas density above the vapor plume,
which allows the expansion of the plume to continue, in
1284 Laser Induced Breakdown Spectroscopy

(b)

(a)

(c) 500 000

Orange truck
(d)

400 000

LIBS emission
300 000

200 000 Pb

100 000

0
390 400 410 420
Wave length (nm)

Figure 2 (a) A commercial LIBS instrument (RT100 -HP) developed by A3 Technologies, LLC (Aberdeen, MD, USA) and Applied
Spectra, Inc. (Fremont, CA, USA). (b) The emission plasma can be seen underneath the focusing objective. (c) A spectrum was taken of
the paint used on a (d) toy truck. It clearly shows that the paint was contaminated with lead (Pb).

addition to supplying energy to the plume, which
is well after the end of the laser pulse. This contrasts
with the behavior of the plasma in helium where
the vapor plume electron number density reaches a
maximum at the end of the laser pulse. The phenom-
enological difference between the two gases can
be explained as a function of the mass and ionization
potential of the two gases. Argon has mass of 40 amu and
an ionization potential of 15.759 eV versus 4 amu and
24.587 eV for helium. The smaller atomic mass at
helium means that it is less efficient of preventing vapor
plume expansion since it creates less drag than the
heavier argon atoms. The higher ionization potential
also means the background gas is less ionized
during laser ablation so no LSD wave occurs. Since
there is no LSD wave, more laser energy is absorbed
by the vapor plume. As a result, the electron density
and temperature of the plume reach a maximum
at approximately the center of the pulse width of the
laser.
LIBS Emission Signal Enhancement –
Double Pulse
The use of double laser pulses is another method that has
been used to produce significant enhancements of the
LIBS signal. One limitation of the LIBS technique has
been its lower sensitivity compared to other spectro-
metric techniques such as atomic absorption and in-
ductively coupled plasma atomic emission and mass
spectrometry (ICP-AES and ICP-MS). Typically, single-
pulse nanosecond LIBS has limits of detection in the
parts-per-million range whereas other commonly used
elemental analysis methods can detect analytes in the
parts-per-billion range or lower. The use of double or
multiple laser pulses has developed as a strategy to
overcome this deficiency. The term, double pulse, is
defined as using two laser pulses to produce a LIBS
plasma that are separated in time by nanoseconds or
microseconds. Since a majority of the laser energy is
absorbed by the target sample and vapor plume,

successive laser strikes can be used to reheat the plasma
containing the ionized species, causing significant in-
creases in the emissions of the species present in the
plume. The first double-pulse experiments were con-
ducted in bulk aqueous solution by two overlapping,
laser-induced plasmas. Using this technique, detection
limits were improved by orders of magnitude over a
single-nanosecond pulse. In a dense medium, like water,
the first pulse forms a bubble in the solution, which
reduces the plasma quenching of the second pulse.
Temperature and signal enhancements seen in double-
pulse LIBS are probably due to (1) rarefaction of at-
mosphere by the first pulse creating a lower-pressure
volume where plasma excitation is more efficient and (2)
a larger portion of laser energy of the second pulse
being absorbed in the analyte containing plasma, instead
of being absorbed at the sample surface or in the
atmosphere.
There are many variations in the double-pulse
method. It has been used in liquids, on liquid surfaces,
with solids, gases, and thin films. Different pulse and laser
configurations have been studied including the use of
different laser wavelengths, energies, pulse widths, and
beam geometries. As with argon, the use of double-pulse
LIBS can be used to remove atmospheric nitrogen and
oxygen from the plasma volume. This allows the analysis
of nitrogen- and oxygen-containing compounds to pro-
ceed without interference from nitrogen and oxygen
atoms in the air. The initial laser pulse displaces the
ambient air whereas the emission from the second pulse
is used in the analysis of the compound of interest. Of
these two enhancement techniques, the double-pulse
technique has a major advantage over the use of argon
because it can be used in remote or standoff detection
applications.
LIBS Reproducibility and Accuracy
Enhancement
For analytical purposes, it is desirable that the extracted
mass is independent of possible heterogeneity in the
sample. Very short pulses can be used, for example, to
eliminate the effect of thermalization and heat transfer
across the sample. For pulses of B1000 fs and shorter, the
duration of the laser pulse is sufficient to heat up only the
electrons in the vicinity of the laser-illuminated spot on
the sample surface. An explosion-type ejection of these
electrons causes simultaneous destruction and ejection of
the cold lattice material due to the Coulomb forces.
Thus, in the femtosecond mode, the process of instant-
aneous vaporization and ionization of the sample can be
greatly simplified, without inducing heat transfer across
the sample and without shielding of the laser irradiation
by the plasma plume. Shielding is not relevant when
Laser Induced Breakdown Spectroscopy 1285
using femtosecond lasers since the formation of the
plasma plume occurs only after the laser pulse has ended.
These factors improve significantly the reproducibility of
the analysis.
Use of short-wavelength (ultraviolet, UV) lasers pro-
vides more efficient and reproducible ablation and hence
is more accurate than the infrared lasers. Advantages of
the UV irradiation are associated with more efficient
absorption in the sample bulk (i.e., smaller losses due to
reflection from the surface and less absorption in the
plume above the sample surface), as well as a lower
number of steps required for MPI as compared to the
laser-induced breakdown in the infrared. Because of
the higher photon energy, the UV radiation can break
lattice bonds even in a single-quantum absorption event.
Ablation by short-pulse UV lasers is a direct and very
efficient method of microextraction. Fractionation effects,
which can cause the ratios of elements in a plume to
differ from the stoichiometry of the sample, are min-
imized by utilizing this technique. Although fractionation
cannot be entirely avoided, ablation with short-pulse UV
lasers reduces the difficulties associated with calibration,
reproducibility, and accuracy of the analysis.
The elimination of heat transfer and meltdown effects
in the femtosecond mode becomes of particular signifi-
cance for local lateral and layer-by-layer analyses where
one must avoid thermal ‘mixing’ of neighboring areas in
the sample. The UV focus spot can be reduced to a
smaller size compared to the infrared. However, use of
short-wavelength lasers can result in the deterioration of
resolution in layer-by-layer analysis.
Standoff (Remote) Detection Using LIBS
One of the advantages of LIBS over other analytical
methods is the ability to analyze samples remotely.
Samples need not be placed inside the instrument, or
even be in the same proximity, for analysis to occur. The
only requirements are the abilities to direct photons to
the sample and collect the resulting emission spectrum. If
a medium is relatively transparent to the laser beam, and
the beam is able to strike its intended target with suf-
ficient energy to create an emitting plasma, LIBS analysis
is possible. This is extremely important when samples are
physically inaccessible, in a hazardous location or when
the substance to be analyzed is potentially dangerous
(Figure 3).
There are many examples of remote LIBS in the lit-
erature. Rapid analysis of metals including Cu, Zn, Al, Ni,
Mo, and Pb has been done at moderate distances of 0.5–
2.4 m to demonstrate the utility of this technique for
identification and sorting purposes in industrial appli-
cations. Remote LIBS in combination with specific laser
ablation techniques has also been shown to be of great
1286 Laser Induced Breakdown Spectroscopy
Standoff LIBS
Samples at 50 m
Collected light
Plasma
Laser beam
Figure 3 Schematics of the standoff LIBS system used as a 50-m remote detector of explosive materials in Mojave Desert. The
sensor concept and the chemometric identification algorithms were developed and successfully field-tested by A3 Technologies, LLC
(Aberdeen, MD, USA) and Applied Spectra, Inc. (Fremont, CA, USA) in collaboration with the US Army Research Laboratory (Aberdeen
Proving Ground, MD, USA).
value in the cleaning of cultural heritage objects, such as
statues, architectural structures, and other archeological
materials.
Since LIBS can be performed remotely and with no
part of the instrument coming in direct contact with the
specimen, it can be very useful in applications where
contamination of equipment is an issue. LIBS has been
used with success in spent nuclear fuel reprocessing plants
where a laser beam can be introduced into a highly
radioactive chamber through leaded glass to analyze both
radioactive and nonradioactive deposits coating a dissolver
basket. No decontamination of equipment is necessary
since the system does not come into physical contact with
the highly radioactive surfaces. Other industrial appli-
cations include the identification of carbon contamination
in molten steel, analysis of mineral melt at 1600 1C, and
remote analysis of high-voltage insulators. In summary,
remote LIBS is used for process control applications in
metallurgy, mineral, and coal industries, and also for en-
vironmental control, detection of explosive residues, cul-
tural heritage monitoring, and planetary exploration.
Conclusion
LIBS is a versatile spectroscopic tool that can be easily
implemented for the characterization and detection of
substances. Since excited atoms of all elements emit in
the optical segment of the spectrum, there are no re-
strictions on the type of samples to be analyzed. LIBS can
be used for real-time analysis of materials as a remote or
portable system. Little or no sample preparation is re-
quired and the technique is sensitive to residues in
High-resolution ICCD Spectral data for analysis
spectrograph system
Telescope
Chemometrics
Reference spectra
NO YES
Explosive detection
and identification
LIBS data are compared to a library of reference
spectra for identification of unknown samples
concentrations of parts-per-million. Enhancement of the
LIBS signal can be accomplished with the use of argon
gas that increases the temperature and the electron
density of the emission signal. The double-pulse laser
technique can also enhance signal quality by reheating
the plasma as well as displacing the oxygen and nitrogen
present in ambient air. Femtosecond UV laser pulses
offer advantages in accuracy and in reproducibility of
LIBS spectra due to the elimination of heat transfer,
shielding, and fractionation effects. Recent developments
in both laser technology and basic understanding of the
plasma physics have allowed LIBS to be used reliably and
with great sensitivity in a wide variety of analytical
applications.
See also: Atomic Absorption, Methods and
Instrumentation, Atomic Emission, Methods and
Instrumentation, Environmental and Agricultural
Applications of Atomic Spectroscopy, Laser Ablation ICP-
MS.
Further Reading
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