LEA-S500® Elemental Analyzer

LEA-S500 – is a modern powerful atomic – emission spectral instrument with multichannel spectrum registration, combining in itself innovation technologies in the area of laser, spectral, measuring, digital equipment and software and permitting elemental (chemical) analysis of a sample in minutes. The detectable elements are from H to U, measuring range is to 100%. Necessary weight of the analyzed material is from 50 nanograms. The time period of multi-element analysis including sample preparation is 1 – 15 minutes. 400 analyses on determination of material homogeneity take about 7 minutes.

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Description

Intuitive software of LEA-S500 guarantees operation of the instrument from the first opeartion. Only several hours and minimum special knowledge is needed to learn basic functions of the device.

Two-pulse nanosecond laser source of spectra excitation, due to high energy, power and temporal stability, provides a maximal reproducibility of the analysis results and low detection limits of chemical elements and compounds. Simultaneously it provides arc and spark modes of spectra excitation.

High-quality light throughput aberration-free high-resolution spectrograph provides accurate and reliable measurements.

Unique detection system of short pulsed light signals provides extremely low limits of elements detection and a linearity of concentration dependences in a wide range.

LEA S500 2018

SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. Laser S-pulse-mode eng orange

one-pulse spectra excitation mode

Two-pulse nanosecond laser
In the elemental analyzer LEA – S500 plasma of a sample material, arising due to the treatment of material with powerful light pulses, is used as a light source to obtain an atomic – emission spectrum.
It has been experimentally revealed, that when a sample is treated with two successive laser pulses (with time delay not exceeding the plasma lifetime) an essential growth of intensity and spectral lines stability in comparison with one-pulse excitation mode is provided. The given effect reduces substantially the lower limit of elements detection, increases measurements accuracy, extends analytical potential owing to excitation of lines with high ionization energy.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. Laser D-pulse -mode eng jrange

two-pulse spectra excitation mode

 

Our innovative solutions guarantee:

  • High accuracy and precision determination of elements and their compounds (oxides) in the samples
  • Low detection limit of elements (from 0.01 ppm to 1ppb)
  • Analysis of various elements in any conductive, nonconductive solid (monolithic and powder) samples
  • Use of analytic lines at the optimal concentration sensitivity, free from spectral overlaps
  • Maximal efficiency of analytical light signal
  • Ease at operation and service
  • Safe operation and protection of personnel from harmful factors
Detection system
Use of digital cameras with multi-element spectrum detection systems in spectral instruments is conditioned by a number of advantages before the traditional detection systems
(photo-electronic multipliers, photo-plates and etc.). The main of them are: the opportunity of simultaneous detection of a wide spectrum range; high-speed performance, providing detection of spectra excited with frequency pulsed sources, what allows one to make a large number of measurements per a time unit (in our case it is 20 times per second); wide range of spectral sensitivity; low dark signals (noise); wide dynamic range. As a radiation receiver in digital cameras matrix charge-coupled devices (CCD) are used, which are referred to the type of photosensitive (photoelectric)
charge-transfer devices (CTD). Quantum efficiency of modern semiconductor radiation receivers is 90% and higher.
Spectrograph
Spectrograph performs radiation spectral analysis.
This analysis is realized in optics by means of an element deviating the beams with various wavelengths to different angles.

 

Methods

Description of a method

LIBS (Laser-Induced Breakdown Spectroscopy) – is a modern analytical method of elemental analysis providing a high- precision multi-element real-time analysis of chemical composition of a sample.

The method is based on excitation of elements atoms of a sample with a laser radiation pulse, focused to sample surface, on spectral decomposition of radiation of element atoms, measurement of analytical signals proportional to the spectral lines intensity, and on subsequent detection of mass fractions of elements by means of calibration graphs.

 

Calibration graphs
Functional dependence of analytical signal on the content of the element, represented as a graph.
Spectrum

Atomic-emission spectrum is a registered as a graph or visually observed dependence of the intensity of radiation emitted by free atoms or ions on the radiation wavelength. Radiation intensity depends on the material temperature and number of emitting atoms or ions. The wavelength of a separate spectral line is defined with the difference of atom quantum transition energies from the excited state to a lower-energy state. The quantum levels structure is unique for each chemical element, and this fact allows one to identify the presence of an element in the substance according to the spectral line.

 

 

Sample chemical analysis diagram ( LIBS)

 

SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. opisanie metoda shema obsch eng

 

SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. blok shema LEA eng Spectral composition of laser plasma radiation of any chemical element is unique and this fact permits the identification of an element in a sample according to the spectrum and the its concentration detection according to the spectral line intensity. Therefore, a multi-component material spectrum includes spectral lines of all chemical elements it comprises.
The Analyzer consists of the following basic parts: a pulsed laser; a system of collection, transfer and spatial decomposition of optical radiation into monochromatic components – spectrograph;
a system of spectra detection (detector) – digital camera, a control unit, analysis data archiving.
 

 

There are several important stages of quantitative sample analysis:

 

Initial condition for a quantitative analysis is a response of the analytical instrument for the identified component in sample. Such response is called analytical signal, and a graph illustrating analytical signal dependence on concentration is called calibration curve (graph).  The form of calibration curves strongly depends on  a number of factors, which finally define
the reproducibility and measurement accuracy.At element concentration detection in a sample the calculated is executed according to the calibration curve which corresponds to the value of the analytical signal detected with the instrument.
Analytical signal

Signal contains quantitative information on value, functionally connected with the content of the element and registered during the material analysis.

 

Calibration curve

Element content functional dependence on the analytical signal expressed in the form of a graph.

 

Operation Conditions

Operating and service conditions:

The design of laser elemental analyzer LEA-S500 provides complete and reliable protection of personnel from harmful and physically dangerous factors during operation of the instrument.

Analyzer is aimed for the use indoors at ambient temperature from + 15 up to + 27 оС and relative humidity of not more than 80%
at 25 °С, moisture condensation is not allowed. Diurnal indoors temperature difference is not more than 3 °С; maximal allowable temperature difference within 2 hours is not more than 2°С.

Presence of corrosive media and conducting and fine-dispersed dust in the operative area is not allowed.
Power supply is (220±22) V, with (50±1) or (60±1) Hz frequency.

Minimal industrial facility area for exploitation of the analyzer cannot be less than 15 m2.

The following free-space standards should be followed at the analyzer exploitation while operating the instrument:

  • from back and lateral sides – not less than 1 meter
  • from front side – not less than 2 meters

 

 

Certification

LEA-S500 is included into the State Register of approved measuring instruments of Russian Federation.

Certification_2014

 

Analytical Capabilities

 

Multi-element quantitative sample analysis including sample preparation takes from 1 to 15 minutes.

Analysis of any solid-state or powder materials:
  • ceramics, glass, cement
  • metals and alloys
  • slags
  • rubbers, caoutchoucs, plastics
  • micro-elements and admixtures in pure materials
  • chemical agents
  • ores, minerals and mono-mineral inclusions
  • natural materials (clays, sands, dolomite, soda, salt and etc.)
  • ash of herbal and animal origin
  • wooden materials
  • solid residue of liquids
  • frozen liquids
  • soil
  • dry plant materials

and other materials.

Qualitative analysis – 50 elements per 5 minutes.

Laser elemental analyzer LEA-S500 permits chemical analysis of any solid-state samples without re-configuration of the equipment. The change of a sample type for analysis takes several seconds. 

 

Detection limits

Detection limit means a minimal content of the element in a sample, detected with the instrument.

Usually a concentration, at which the analytical signal detected with the instrument equals to a triple value of a standard deviation of noise signal, is taken for a detection limit. Obtaining of such signal is a sufficient reason for making a decision on presence of the searched component.

Detection limit is a parameter sensitive to measurement conditions and a sample characteristic.

 

H
100
Detectable Elements
with selected detection limits, ppm
1 ppm = 0.0001%
He
100
Li
0.01
Be
0.07
B
2
C
1
N
< 100
O
< 100
F
20
Ne
< 100
Na
0.05
Mg
0.1
Al
1
Si
3
P
20
S
10
Cl
100
Ar
< 100
K
0.06
Ca
0.1
Sc
10
Sc
10
Ti
0.3
V
1
Cr
1
Mn
0.2
Fe
0.5
Co
0.2
Ni
0.8
Cu
0.1
Zn
0.5
Ga
< 100
Ge
2
As
40
Se
< 100
Br
200
Kr
< 100
Rb
1
Sr
0.2
Y
10
Zr
1
Nb
5
Mo
1
Tc
< 100
Ru
< 100
Rh
< 100
Pd
< 100
Ag
0.1
Cd
0.2
In
5
Sn
10
Sb
10
Te
< 100
I
< 100
Xe
< 100
Cs
< 100
Ba
0.2
Lu
< 100
Hf
5
Ta
< 100
W
5
Re
< 100
Os
< 100
Ir
< 100
Pt
< 100
Au
1
Hg
< 100
Tl
1
Pb
0.3
Bi
5
Po
< 100
At
< 100
Rn
< 100
Fr
< 100
Ra
< 100
La
40
Ce
4
Pr
< 100
Nd
< 100
Pm
< 100
Sm
< 100
Eu
< 100
Gd
< 100
Tb
1
Dy
< 100
Ho
< 100
Er
10
Tm
< 100
Yb
1
Ac
< 100
Th
< 100
Pa
2
U
30

 

Advantages

  • Measuring of mass fraction (concentration) of chemical elements or their compounds (oxides) in a sample with minimal sample preparation
  • Express multi-element analysis
  • Multielement chemical analysis per one measurement
  • High sensitive and precise measurements in the wide concentration range
  • No change of a sample aggregate state
  • Sample analysis in the set points (areas) on the surface by means of positioning system and video surveillance
  • Layer-by-layer analysis of coatings, films, deposits, corrosion
  • Analysis of inclusions, flaws, defects
  • Analysis of elements distribution in a sample with the step from 30 mcm. Mapping of elements distribution over the surface, homogeneity control
  • No need in ultrapure reagents for a sample preparation
  • No need in expensive consumables
  • No need in inert gas to solve most of the tasks
  • Dirty sample surface is cleaned with the preliminary laser pulses
  • No need in re-configuration or modernization of the instrument to solve all the mentioned tasks
  • Analysis of conductive, non-conductive materials
  • Analysis of a wire of any diameter, balls, cylindrical details without additional processing using special
    adapters (included in the delivery set)
  • Uncompromising operation safety, complete protection of the personnel from harmful factors

ATILLA 2 Software

ATILLA 2 is a powerful intuitive software instrument for the instrument control and measurements automation.

ATILLA 2 contains:
  • Spectral lines database
  • Certified reference materials database
  • Analyzed samples database (archive)
ATILLA 2 provides:
  • Automatic sample analysis
  • Calibration and re-calibration
  • Graphical imaging of the obtained spectrum
  • Sample surface observation, selection of any point or area for the analysis
  • Possibility for development of analytical programs by a user (selection of spectra excitation and detection
    modes, selection of algorithms of spectral lines mathematical processing, calibration of the instrument)
  • Control of quality and reliability of the analysis results
  • Printing out the analysis results and their mathematical processing
  • Memory storage of unlimited number of analytical programs
  • Control over the instrument and the system state
  • Auto-calibration of a wavelength scale

Sample preparation

 

For analysis of solid-state, monolith materials (metals, alloys, glass, ceramics and etc.) no sample preparation is required or it lies in the obtaining of a plane section of a sample surface. For analysis of a transparent sample (glass, crystal) the area of analysis is additionally polished.

For the analysis of powdery samples (refractory components, slags, concentrates, sands, ash, etc.) the materials are ground with the subsequent pressing in tablets. Sample preparation of powder-state materials takes 10 – 40 min; with manual tools and 3 – 5 min; with the help of semi-automatic tools.

100 mg of a sample material is enough for the preparation of a tablet.

SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. metall

 

More capabilities

 

The types of analysis that require essential material and time costs if other methods of analysis are used, are considered.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. fig1 trubka 320x250

The inclusion in a tube made of medical glass (photo)

SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. fig2 trubka-monitor 320x250

The inclusion in a tube made of a medical glass
(monitor view), х100

Defectoscopy.
Analysis of inclusions and structural components

Material defect is a local change of chemical composition of the material affecting the properties of the material
Flaw (defect) detection is performed by means of comparison of pure glass spectra and the spectra of a defect. The positioning system of the LEA-S500 provides the pointing accuracy of 1 µm. For a qualitative analysis size of defect should be not less than 5 µm and for a quantitative analysis size of defect should be not less than 150 µm.
In the given case the zirconium inclusion indicates the destruction of the refractory laying in a glass-making furnace.
Diagnostics of destruction processes at initial stage allows to take preventive measures and to avoid expensive reconstructions. Time of analysis is about 2 min.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. spektr def chist stek eng
The spectrum of the defect and the pure glass

Distribution of elements over the surface, homogeneity control

The control of elements distribution over the material surface provides new information about the analyzed samples. LEA-S500 allows high accurate, fast and low cost analysis. It also allows to analyze materials with a step of 100 µm.
This type of the analysis is recommended for specification of homogeneity specification at the certification of composition of reference materials.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. fig4 map koncentr LEA 320x250
Concentration map of the element on the sample surface

Layer-by-layer analysis

Successive evaporation of sample material with the focused laser pulses provides elemental (chemical) analysis of composition and thickness of multi-layer coatings and thin films. Deposits, corrosion areas, sections with the damaged structure, composite materials, etc. can be investigated.

SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. fig5 zerk poverh LEA 320x250

Analysis of the mirror surface with minimal path of 2х2 mm, 400 points

Application

Application

Laser elemental analyzer LEA-S500 is applied for qualitative, semi-quantitative and quantitative elemental (chemical) analysis of raw material, components, additives, admixtures, inclusions at all stages of manufacturing process; for control of finished products at factories; for scientific investigations.

The instrument allows to perform both general averaged multi-element analysis of a sample and local analysis of small
volume and mass.

The instrument is of great importance for the organizations where much care is taken about their personnel health.

LEA-S500 provides safe chemical analysis of the materials and components. An operator is completely protected from
harmful factors connected with the analysis.

Only several hours are needed for the instrument operation training.

 

Procedures of measurement

Procedures of measurement is a set of operations and rules that provide the results of measurements with the set error (ambiguity) characteristics.

Generally procedures of measurement include:

  • name of the analyzed material(s), purpose, application
  • nomenclature of detectable elements (compounds)
  • ranges (intervals) of detectable concentrations of the elements (compounds)
  • nomenclature of the certified reference materials (CRM) or reference materials
  • necessary for calibration
  • measurement accuracy
  • safety requirements
  • selection and sample preparation for analysis
  • calibration
  • execution of measurements
  • processing of measurement results, estimation of the results, final results of measurements
  • control of accuracy of analysis results
  • Certified reference materials (CRM) or reference standards

For the control of a technological process, input and output inspection of goods and raw materials, for scientific research
application
of the techniques of analysis with the analytical programs, supplied with the instrument or developed by a user, is possible.

Analytical program is an integral multifunctional command of the software running a sequence of operations, programmed by the manufacturer (a user) of the analyzer. In the process of these operations the elemental (chemical) analysis of a sample placed in a sample chamber, documenting and archiving of the results is performed.

Analytical programs comprise:

  • excitation and detection modes of spectra (the parameters of laser, spectrograph, detection system, purification system)
  • basic list of spectral lines, providing the measurement of concentrations of the specified (set) elements and algorithms of
    intensity calculation
  • the list of certified reference samples (or materials) used for construction of calibration graphs
  • calibration curves (graphs)
  • methods of additional processing of the obtained results (if needed)

Metrological characteristics of the analytical programs for LEA-S500

SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500Primary aluminumAluminum alloys
Nomenclature of detectable elements, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500Iron ore
Nomenclature of detectable oxides, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Pure copperCopperbased alloys (brass, bronze)
Nomenclature of the detectable elements, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Mineral fertilizers
Nomenclature of detectable compounds, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Glass
Nomenclature of detectable oxides, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. High-alloy steel (stainless, high-speed)
Nomenclature of detectable elements, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Cement and slag
Nomenclature of detectable elements, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Low- and medium-alloy steel
Nomenclature of detectable elements, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Cast iron
Nomenclature of detectable elements, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Titanium. Titanium alloys
Nomenclature of detectable elements, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Raremetallic concentrates (rutile, zircon, ilmenite)
Nomenclature of detectable elements, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Refractories: aluminum silicate, low-cement products, magnesites
Nomenclature of detectable oxides, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Clay raw materials
Nomenclature of detectable oxides, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Quartz sand
Nomenclature of detectable oxides, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Rocks
Nomenclature of detectable elements, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Chalk, soda, dolomite
Nomenclature of detectable oxides, measurement ranges, errors of analysis.
SOL instruments: спектрометр, рамановский микроскоп, эмиссионный спектрометр. PDF Laser elemental analyzer LEA-S500. Magnesium. Magnesium-based alloys
Nomenclature of detectable elements, measurement ranges, errors of analysis.

 

Reference Materials

Certified reference materials (CRM) are samples of materials and components with certified elemental (chemical) composition intended for calibration of the instrument.

Name, field of application, certified concentrations of elements and errors of measurement are given in the certificate for any kit of certified reference materials.

The reference samples included in the State Register of approved measuring instruments have the status of the State Certified reference materials. The state certified reference materials can be used for the certification, verification and calibration.

 

Certified reference materials (CRM). Requirements

  • Chemical composition of any CRM kit should correspond to the composition of the analyzed samples.
  • Concentrations of elements in the CRM kit should cover the complete range of possible values of element
    composition in the analyzed samples.
  • CRM should provide reproducibility of the detected analytical signal.
  • The CRM kit and the analyzed samples should have the same structural (granulometric) composition and
    similar physical and chemical properties.
  • The CRM should keep the stability of metrological characteristics during the whole serviceable lifetime.
  • Optimally 3 – 7pcs of CRM samples with uniform concentration laying is required for the instrument calibration.

In many sectors of national economy samples and materials that meet the requirements to CRM, are widely used.