Posted in | Spectrometers

ARL OPTIM’X — WDXRF Spectrometer

One of the most flexible analytical techniques for the elemental analysis of solids and liquids is wavelength dispersive X-Ray fluorescence (WDXRF). High accuracy, precision, and dependability may be achieved in analyzing elements ranging from uranium to boron in diverse samples.

The analytical methods and techniques have reached a level of maturity that allows for the precise qualitative and quantitative characterization of a wide range of materials. Because of its cost, simplicity, flexibility, and dependability, WDXRF has been incorporated into standard test techniques for analytical laboratories (such as ASTM and ISO requirements), thanks to modern technical advancements.

The cost per analysis is unquestionably better compared to several conventional wet chemicals and other spectroscopic procedures.

A Compact and Independent WDXRF Instrument

Thermo Fisher, which has a history of innovation and leadership in WDXRF, introduces the Thermo ScientificTM ARLTM OPTIM'X spectrometer, a compact instrument with two power levels to choose from and notable analytical features.

  • A special WDXRF platform with the ability to operate sequentially or simultaneously
  • Unique compact SmartGonio device for sequential analysis.
  • Sequential-simultaneous configuration blending speed with analytical flexibility.
  • Element coverage from carbon to uranium, depending on the configuration.
  • Innovative UCCO technology (Ultra Closely Coupled Optics) for increased intensity, up to 210% higher than conventional geometry.
  • Multichromators for fast analysis
  • Superior spectral resolution from low Z elements to heavy elements compared to EDXRF (~15 eV at Ca Kα and ~30 eV at Mn Kα)
  • High precision (short-term and long-term repeatability) due to temperature management of spectrometer and crystals
  • The best design (in accordance with ISO or ASTM standards) for a given application with streamlined operation
  • Easy and direct sample introduction.
  • Automatic batch analysis with sample changer.
  • Stand-alone and autonomous operation without water cooling.
  • Dependent on configuration, no gas supply or compressed air is needed.
  • Compact footprint

Excellent resolution compared to EDXRF: Mg, Na and F peaks do not interfere on each other

Excellent resolution compared to EDXRF: Mg, Na and F peaks do not interfere with each other. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Configuration for Speed and Flexibility

  • Sequential analysis utilizing the SmartGonio for up to 8 components at once using 4 multichromators
  • SmartGonio and two elements are analyzed sequentially concurrently on a single multichromator
  • Using a 50 W basic or 200 W optional power source for 2.5 times faster analysis.

Configuration selected according to application needs

Configuration selected according to application needs. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers 

Large Variety of Samples

The ARL OPTIM'X spectrometer can evaluate various sample types, including liquids, conductive or non-conductive solids, loose powders, pressed pellets, fusion beads, pastes, granules, and coatings. The device is always tailored to the user's unique application requirements.

ARL OPTIM’X — WDXRF Spectrometer

Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Exclusive UCCO Technology

Ultra Closely Coupled Optics, or UCCO, can produce:

  • 200 W of power from 50 W of power
  • 500 W of power from 200 W of power.

Whole X-Ray beam exciting the full sample diameter for highest efficiency: no photon loss during irradiation. Compact X-Ray tube allowing close coupling with sample for optimized sensitivity

Whole X-Ray beam exciting the full sample diameter for highest efficiency: no photon loss during irradiation. Compact X-Ray tube allowing close coupling with sample for optimized sensitivity. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers 

Optimized for Specific Applications

  • S (ISO 14596 or ASTM D2622), Pb (ASTM D5059), and other element analyses in gasoline, fuels, oils, and catalysts are done in the petroleum sector. For concentrations ranging from ppm levels up to 5% (Figure 1), obtaining the calibration curve for sulfur in lubricants and gasoline is simple. The excellent detection limit of 1.4 ppm in 100 s (or 1 ppm in 200 s) is reached at 50 W. The reproducibility test demonstrates this positive outcome (Table 1). The same precision is attained in 50 s at 200 W power, and the detection limit drops to 0.8 ppm in 100 s. Turn-key solutions for the preconfigured ARL OPTIM'X Sulfur Analyzer are available.
  • Primary and secondary oxides found in unprocessed substances like limestone, sand, feldspar, bauxite, magnesite, and various mining materials, including raw meal, clinker, and cement, can be effectively analyzed using the ARL OPTIM’X analyzer. It demonstrates exceptional repeatability in analyzing these material types. Additionally, the prearranged ARL OPTIM’X Cement Analyzer is at your disposal for specialized cement analysis.
  • When analyzing metallurgical slag, the prearranged ARL OPTIM’X Slag Analyzer provides a ready-to-use solution. As illustrated by the calibration curve in Figure 2, fluorine (F) analysis can be seamlessly conducted using either the SmartGonio or a fixed channel. The outstanding precision of ARL OPTIM’X is evident in Table 2, which includes data for fluorine analysis.
  • Major and minor oxides in products such as glasses, ceramics, refractories
  • Monitoring major and minor elements is crucial in various industries, including polymers (Table 3), paints, pigments, paper, ferroalloys, silicon, metal sheets, and other related products.
  • The food industry for main and minor nutrients and other controlled ingredients found in cereals and milk powders. Typical concentration ranges and excellent detection limits in milk powders at 50 W (Table 4).
  • Provide the preconfigured ARL OPTIM'X Uniquantometer for additional wide-range and unknown material analysis.

ARL OPTIM’X — WDXRF Spectrometer

Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers 

Calibration curve for S in oils and gasoline at 50 W (low concentration range).

Fig. 1. Calibration curve for S in oils and gasoline at 50 W (low concentration range). Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

  Calibration curve for F in slags. The standard error of the estimate is 0.2% in a range from 0.1% to 17%.

Fig. 2. Calibration curve for F in slags. The standard error of the estimate is 0.2% in a range from 0.1% to 17%. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Table 1. Excellent reproducibility for sulfur in oils at 50 W (120 s). Source: Thermo Fisher Scientific - Elemental and Phase Analysis

Sample ppm
Cell 1 25.4
Cell 2 25.7
Cell 3 26.4
Cell 4 26.0
Cell 5 25.0
Cell 6 25.9
Cell 7 26.7
Average 25.9
Std. Dev. 0.58

 

Table 2. Repeatability test on a pressed slag sample at 200W (6 consecutive runs). Total counting time 230 s for 13 elements - Fluorine is measured on a fixed channel. Source: Thermo Fisher Scientific - Elemental and Phase Analysis

Run # CaO SiO2 Al2O3 Fe2O3 MnO MgO S V2O5 TiO2 K2O P2O5 Na2O F Mono
1 39.58 35.37 10.05 0.984 2.42 5.43 0.954 0.209 0.811 1.506 0.641 1.4 0.493
2 39.61 35.33 10.06 0.984 2.43 5.43 0.948 0.213 0.812 1.512 0.642 1.41 0.484
3 39.63 35.41 10.05 0.993 2.42 5.44 0.946 0.212 0.819 1.511 0.646 1.39 0.477
4 39.55 35.38 10.07 0.985 2.42 5.43 0.953 0.213 0.812 1.514 0.646 1.40 0.491
5 39.62 35.4 10.06 0.993 2.42 5.44 0.953 0.210 0.811 1.508 0.647 1.37 0.471
6 39.57 35.37 10.06 0.987 2.43 5.47 0.954 0.209 0.815 1.513 0.645 1.41 0.486
AVG 39.59 35.38 10.06 0.988 2.42 5.44 0.951 0.211 0.813 1.511 0.645 1.40 0.484
SD 0.031 0.028 0.008 0.004 0.005 0.015 0.003 0.002 0.003 0.003 0.002 0.015 0.008
Meas Time [s] 10 10 20 10 20 20 30 20 20 20 20 30 230

 

Table 3. Limits of detection for heavy elements in polymers at 200 W (100 s counting time). SEE: standard error of estimate with ranges from 0 to 500 ppm. Source: Thermo Fisher Scientific - Elemental and Phase Analysis

    LOD in 100 s SEE
Element Line [ppm] [ppm]
Ba 2.6 17
Br 1.0 6.1
Cr 0.5 3.6
Cu 0.5 5.6
Hg 1.2 20
Ni 0.3 16
Pb 0.9 24
Zn 0.3 6.2

 

Table 4. Limits of detection (LoD) at 50 W in milk powders prepared as pressed pellets. Source: Thermo Fisher Scientific - Elemental and Phase Analysis

Element Analytical device Typical ranges LoD (ppm in 60 s)
Na Fixed channel 0 – 0.03% 20 ppm*
Mg Fixed channel 0 – 0.12% 11 ppm*
P SmartGonio 0 – 1.1% 4.4 ppm
K SmartGonio 0 – 1% 2 ppm
Ca SmartGonio 0 – 1.6% 10 ppm
Fe SmartGonio 0 – 0.33% 2.1 ppm
Cu SmartGonio 0 – 0.012% 0.6 ppm
Zn SmartGonio 0 – 0.2% 2 ppm
Cl SmartGonio 0 – 0.48% 10 ppm
Mn SmartGonio 0 – 0.0023% 1.2 ppm
Se SmartGonio 0 – 3.4 ppm 0.24 ppm

(*-cumulative counting time of SmartGonio for Na and Mg)

Full automation with Thermo Scientific ARL SMS-Omega loading system connecting full automatic preparation machines.

Full automation with Thermo Scientific ARL SMS-Omega loading system connecting full automatic preparation machines. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Exclusive SmartGonio – Principle of Operation

  • Quantitative examination of every element, ranging from F to U, based on configuration
  • Moiré fringe optical encoders are utilized to achieve ϔ/2ɔ relationship between the crystal and detector by means of angular orientation.
  • Superior repeatability and angular accuracy
  • It requires no wear, friction, or maintenance. It regulates crystal temperature for optimal analytical stability. Its closest linkage to the X-Ray tube maximizes sensitivity.

ARL OPTIM’X — WDXRF Spectrometer

Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Top Analytical Software

Instrument Control and Data Handling

Thermo Scientific OXSASTM software is state-of-the-art and makes it easy to use the ARL OPTIM’X spectrometer and quickly generate highly accurate analytical findings. OXSAS software adapts to changing client needs throughout the instrument's lifespan, providing them with the most recent solutions, all while running on the Windows® 10 operating system. The product specification document for the OXSAS program contains all the features and information.

Uniquant

For the ARL OPTIM'X spectrometer, the well-known UniQuantTM application offers "standard-less" analysis for up to 73 elements when certain standards are unavailable, samples are only available in limited amounts, or the samples have irregular forms. It is possible to evaluate any solid, conductive, or non-conductive.

 It is simple to analyze loose powders, liquids, and pastes when the helium environment option is enabled. The Uniquant algorithm also determines the remaining unanalyzed components in the sample, such as organic and ultra-light components. Comparing analysis using peak-to-peak hopping to scan-based spectral processing yields various benefits:

  • Improved detection limits
  • Optimal timing for each element's counting
  • Sample spinning for non-uniform samples or to balance out effects from polishing grooves

Using the SmartGonio of the ARL OPTIM'X spectrometer, the Uniquant software is fully calibrated and pre-installed in the factory, making it ready for use immediately upon installation at the customer site. Included are stable samples for long-term setup and upkeep. The ARL Uniquantometer is the preset variant of the ARL OPTIM'X analyzer.

Uniquant uses ‘peak hopping’ to acquire intensities for more than 121 line positions.

Uniquant uses ‘peak hopping’ to acquire intensities for more than 121 line positions. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

UniQuant is the world’s most renowned standard-less package.

UniQuant is the world’s most renowned standard-less package.

UniQuant is the world’s most renowned standard-less package. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers 

Fast Qualitative Analysis

Step scanning offers 0.001° resolution, which allows for exact peak definition. Continuous digital scanning enables the quick capture of spectra at up to 327°/min for quick qualitative analysis. The peaks that correspond to the identified items are automatically identified.

Accuracy Made Easy

Analytical programs and calibrations can be quickly and accurately defined with the aid of the online analytical assistant. The different calibration curves are constructed using the multi-variable regression (MVR) tool.

The impact of interfering elements in multi-component matrices is reduced thanks to correction models, improving analysis accuracy. These models include

  • Line overlap correction
  • Additive correction on intensities
  • Multiplication of intensities
  • Multiplication of concentrations
  • Multiplication of additive and
  • Multiplicative corrections on concentrations.
  • The NBSGSC basic parameters program uses Comprehensive LAchance (COLA) with three-term alphas to simulate analytical calibrations for homogenous materials. The MVR uses the inter-element correction factors—theoretical alphas, now with matrix and LOI/GOI elimination—as known coefficients that are computed. As a result, fewer requirements are required to

Turnkey Calibrations

Ex-works calibrations can be provided for a range of materials, including:

  • Petroleum industry products using the PetroilQuant program and/or ASTM & ISO methods
  • Iron, hot metal, and slags
  • Copper, bronze, and brass,
  • Aluminum and alloys
  • Ferro-alloys
  • Cement and clinker
  • Various oxides through the General Oxide calibration
  • Traces in soils and sediments
  • Polymers and coatings
  • Minerals like lime, limestone, dolomite, and sands
  • Glasses
  • Milk powders and cereals S and Cl in catalysts
  • For each of the calibrations, as mentioned earlier, as well as for specially ordered calibrations, analytical specifications are available upon request.

The Analytical Assistant helps define analytical programs, calibration, and instrument use.

The Analytical Assistant helps define analytical programs, calibration, and instrument use. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

  Statistical Process Control – Typical screen.

Statistical Process Control – Typical screen. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

 MVR calibration curve: real concentration vs. intensities.

MVR calibration curve: real concentration vs. intensities. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers 

Specifications

Specifications of the Thermo Scientific ARL OPTIM’X XRF spectrometer. Source: Thermo Fisher Scientific - Elemental and Phase Analysis

. .
Element range Oxygen (Z=8) to uranium (Z=92) with 2 detectors fitted. Oxygen to Iron (Z=26) with FPC detector fitted (Carbon (Z=6) can be fitted as fixed channel)
Spectrometer environment Vacuum for solids, helium for liquids and loose powders
Spectrometer design Analysis devices contained in a temperature-controlled vacuum chamber made of grey cast iron
Spectrometer arrangement X-ray tube inclined at 66° under sample for optimum incidence
Spectrometer capacity Simultaneous configuration: Four Multichromators (covering eight elements)
Sim-seq configuration: SmartGonio + one Multichromator (covering two elements)
UCCO
technology
Ultra Closely Coupled Optics offering largest solid angle for most efficient irradiation of the total sample surface: 50 W power providing excitation similar to 200 W or 200 W power providing excitation similar to 500 W
X-ray excitation Air-cooled Rh anode end window tube with thin Be window (0.075 mm). Other anodes available on request. 50 W version: Solid-state high frequency generator of maximum voltage 50 kV and maximum current 2 mA (combinations to be chosen to be at 50 W) 200 W version: maximum voltage 50 kV and maximum current 10 mA (combinations to be chosen to be at 200 W). Max. line voltage variation 230 V -15% to +10%. Stability ± 0.0002% per 1% variation
SmartGonio Fully automatic, gearless, microprocessor-controlled compact goniometer using optical encoders
Total angle range: 0 ˚ -150 ˚ 2 θ (Flow proportional counter: 17 ˚ -150 ˚, Scintillation counter: 0 ˚- 90 ˚ ).
Continuous digital scans: from 0.25 ˚/min to 1200 ˚/min.
Multichromator Fixed channel using dual curved crystal optics allowing analysis of two elements simultaneously. Sealed detectors available for elements from sodium (Z=11). Flow proportional or scintillation detectors also available depending on element. Dual pulse height integration to discriminate and correct for 2nd order peaks. Note: some elements can only be fitted as single channel monochromator
Counting electronics Multi-channel analyzer to discriminate peaks of higher energies. Digital Automatic Gain Control (AGC) for pulse shrinking correction.
Automatic dead time correction ensures linearity of response up to 2 Mcps on flow proportional counter and 1.5 Mcps on scintillation counter
Sample loading Basic: 1 position for cassette or liquid cell. Optional: 13-position autosampler
Automation ARL SMS-Omega full automation with transport link from/to fully automatic sample preparation machines for pressed pellets or fused beads or solids
Sample holders Sample cassettes with maximum size of sample: height 26 mm, diameter 52 mm. Liquid cell: height 22 mm, external diameter 40 mm
Exposed opening: 29 mm diameter (basic). Rotation of sample holder in analysis position: 6 to 60 rpm
Dimensions and weight H 126 cm, W 88 cm, D 82 cm with basic sample loading. System weight: approximately 260 kg
Laboratory information Optional phone service support through modem connection
Power requirements 1.5 kVA single phase at 50 W; 1.7 kVA single phase at 200 W

 

Safety Standards. Source: Thermo Fisher Scientific - Elemental and Phase Analysis

. .
Electrical and protection EN IEC 61010-1 (Safety requirements for electrical equipment for measurement, control and laboratory use. Part 1: General requirements)
Radiation Full protection system: Swiss directive ORaP RS 814.501 and German directive RöV BGB1.IS.114
Electro-magnetic immunity EN CEI 61326-1 (Electrical equipment for measurement, control and laboratory use – EMC requirements – Part 1: General requirements)
European directives 2006/95/EC (LVD) Low Voltage Directive
2011/65/EC (RoHS) Restriction of Hazardous Substances Directive
2002/96/EC (WEEE) Waste Electrical and Electronic Equipment Directive

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