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LIBS

SciLIBS Modular Laser Induced Breakdown Spectrometry

What is LIBS?

LIBS is primarily an elemental analysis technique based on the high-temperature spark (plasma) produced by a sufficiently energetic laser pulse.

Light produced by the LIBS plasma is collected and spectrally dispersed in much the same manner as other analytical atomic methods (ICP-OES, spark-OES).

The LIBS technique can be used to essentially detect any element in the periodic table and is applicable to almost any sample type.

Laser Ablation History

Laser-based atomic spectrometry resulting from a fluence exceeding the ablation threshold of a wide range of sample matrices has been practiced for decades. The first of two currently popular applications for quantitative spectrochemistry was predicated on using the laser as a sampling tool to ablate samples and sweep the liberated particles into an inductively coupled plasma (ICP) where the dry aerosol experiences dissociation into atoms and ions and, in the case of emission spectrometry, thermal excitation to produce a laser ablation ICP emission spectrum (LA-ICP-ES).

LIBS Development

LIBS has also been practiced for decades and, in deja-vu parallel, also experienced an initial period of optimistic growth that triggered several commercial start-ups. Quantitative direct solid sampling LA-ICP-MS evolved to respect intrinsic issues like fractionation and limitations based on the availability of standards and found specific applications like mineral mapping and geochronology via isotope ratios. In similar fashion, LIBS has also found certain specific “killer apps” – one being the unique capabilities in the lithium-ion battery industry where elements like F, O, and H are very important and there is literally no other direct solid analytical method.

LIBS Evolution

There are a few major advantages that ought to emerge from the recent acceleration of LIBS research and development.

  • Since the sample or target is contained in a sample-cell that can be purged with inert gas (Ar, He), virtually the entire periodic table is accessible. In particular, the ability to determine H, C, N, and O is impossible by other conventional techniques (ICP-MS, ICP-ES, XRF) unless they are sample-type constrained (conductive only for spark-OES, GDS) or highly expensive (vacuum probes).
  • Also due to the closed sample cell design, LIBS provides the capability to simultaneously measure the complementary optical spectrum and the ICP-MS spectrum when virtually any ICP-MS instrument is properly triggered/synchronized and the aerosol provided by the LIBS excitation source is routed to the ICP-MS instrument via a simple tubing interface.
  • Many LIBS practitioners have employed chemometrics including principal component analysis (PCA) and many other algorithms to use most or all of the complex LIBS emission spectrum to improve accuracy, precision, and to extend the method to correlate analytical measurements for molecular, pH and other interesting metrics. This is not to say that the other popular elemental analysis techniques cannot enjoy chemometric advantages; but the LIBS community is well down the road to exploiting multivariate methods and it is becoming an acceptable processing method en-route to improved quantitative results.

Why Modular LIBS?

LIBS as a technique has unique characteristics when compared to traditional elemental analysis methods and a highly flexible yet standardized approach is necessary to address the wide range of potential applications.

Additionally, Modular LIBS allows you to:

  • Access a range of key components to best match the application.
  • Upgrade any module to provide enhanced capability.
  • Scale your system to meet your needs; expand easily.

The table below outlines different analytical elemental analysis techniques and their characteristics:

 

Table 1. Analytical Elemental Analysis Techniques and Characteristics
TechniqueLimitationsNot DetectedMinimum FeatureCost
Atomic Absorption Sample digestion H, C, N, O, F Bulk $
ICP-ES Sample digestion H, C, N, O, F Bulk $$
ICP-MS Sample digestion H, C, N, O, F Bulk $$$
Arc-Spark Conductive sample   Bulk/Surface $$
Glow Discharge Conductive sample   Bulk/Surface $$
X-ray Fluorescence Light elements H-F 50 mm $$
Laser Ablation ICP-MS/ES Cost H, Li-F 5-20 mm $$$
LIBS Sensitivity   20 mm $$
LIBS-LA-ICP Cost   20 mm $$$$
Femtosecond Laser Assisted Cost   1 mm $$$$$

SciLIBS System

Figure 1. SciLIBS MHE-266-RSH Modular High Energy Research-Grade LIBS System with Dual Beam for Sample Chamber and Stand-off Measurements
SciLIBS MHE-266-RSH

The SciLIBS MHE-266-RSV employs a high energy Nd:YAG pulsed laser to deliver 60 mJ of energy at 266 nm via the fundamental, frequency quadrupled beam. The Laser Excitation Module (LEM) can also accommodate lower energy primary laser sources as well as secondary lasers for double pulse (DP), laser induced fluorescence (LIF) and other scaleable modes of operation or experimentation.

The system employs three Sciencetech SC-12 sample chambers housing the energy delivery module (EDM), the sample/target module (STM), and for the large-sample stand-off module (SOM).

The EDM provides 3 X beam expansion, beam cleanup, and beam attenuation. The motorized beam attenuation module (BAM) can continuously vary the energy (0 -95%) of the primary 266 nm beam (PB) and simultaneously generate a secondary 266 nm beam (SB – alternate polarization) that is used for the Stand-off Module (SOM).

The second SC-12 is the STM and provides for XYZ translation control for research (small) samples. The STM contains the control and gas plumbing for air, helium or argon chamber environments. Low pressure chamber atmospheres are provided by optional vacuum accessories for more fundamental plasma studies.

Within the SC-12 STM, use of specialized reflective optics and lens configurations define the optical collection module (OCM). Off-axis parabolic UV-coated mirrors can provide 10 X to 100 X more light collection when compared with the usual objective-to-FOC method. However, in addition to a conventional spectrometer slit, it is possible to add FOC pickups to feed additional spectrometers

Selection Guide

Figure 2. Sample and Applications Profile Form
Elemental Analysis Detectable Elements
Elemental Analysis Detectable Elements

To determine which SciLIBS Product is right for you, contact Sciencetech's SciLIBS specialist at:

sales{at}sciencetech-inc.com

Sciencetech experts will help guide you through the selection process by gathering information on your:

  • Application (bulk analysis, depth profiling, feature mapping)
  • Scope of Application (R&D, an accredited contract laboratory, industrial site, combination)
  • Standard Methods/Quality Control (ISO 17025, CAN-P-1578, etc.)
  • Calibration Strategy
  • Sample Throughput and Precision Accuracy Requirements

We will also gather information on:

  • Detectable elements that may be present in your sample - analytes and matrix concomitants

    • Which of these are critical?
    • Which of these are analytes
    • What is the range of concentration expected? (major, minor, trace)
  • Sample Type (ore, alloy, artifact)
  • Sample Preparation (none, pressed disc, fusion, extraction, digestion)
  • Morphology (homo- or heterogeneous, size, distribution)
  • State of Original Sample (solid, liquid, gas)

All of this information can be gathered using Sciencetech's convenient Point and Click PDF Form (pictured right).