The most suitable instrument for quantitative element analysis is the electron microprobe, for example the JEOL JXA-8230 electron microprobe (WDS mode, 20 kV, 20 nA, 1-2 μm beam size) (JEOL Ltd., Akishima, Japa). Particular attention should be paid to the detection limits for the individual elements to be analyzed, it strongly depends of the composition of the alloy, and of the standards, emission lines, and analyzing crystals used. Here for example some detection limits in ppm (parts per million) for
Ag 250
Hg 1100
Pb 400
Fe 150
Ni 200
Bi 300
Best regards,
Guenter Grundmann
The best option would be microprobe for sure! In case you do not have one around, X-ray Microfluorescence with the right group of standards can reach good results.
Regards
I agree with the previous ones. An important thing is, that the standard EDS method can only show quantitative results for elements with atomic number >11.
Atom probe tomography (APT) is a technique that is very well suited for this task. The atom probe maps provide a great deal of insight into the levels and distribution of wt.% of elements in the various phases of an alloy. It is a powerful technique to study the local distribution of atoms in a small volume, e.g. 200 × 80 × 80 nm3, allowing the accurate determination of compositions as small as 50 ppm over interfaces with sub-nanometer resolution.
APT is a microstructural characterization technique that uses the principle of field ion evaporation to remove individual atoms from a sample by applying a high electric field to the region of interest, which is in the shape of a sharpened tip. Thus, the APT technology allows acquiring three-dimensional elemental mapping with nearly atomic resolution and provides information about internal interfaces and local chemical gradients. Due to this significant feature, it has showed a huge potential to characterize the composition difference in nanostructures.
All the techniques described above can provide quantitative analysis of the elements present in the alloys. But each one has its advantages and disadvantages. For example EDX can not measure low atomic number elements accurately. ICP-MS is sensitive but is time taking and needs sample preparation. Laser Induced Breakdown Spectroscopy can be fast and no sample preparation is needed. But the sensitivity may be comparatively low. So user has to decide about his priorities about the analysis.
As Professor Muhammad Aslam Baig said, Calibration-Free LIBS is a powerful tool to analyse alloys. For more info, you may have a look at the recent paper published by Hermann et al. “Analysis of Multi-elemental Thin Films via Calibration-Free Laser-Induced Breakdown Spectroscopy”, Anal. Chem. 2019, 91, 2544−2550 (DOI: 10.1021/acs.analchem.8b05780).
Best regards,
Emanuel
For the chemical composition and quantification of the elements in samples (for layers, coating, alloys, ultra pure industrial materials etc.), Glow Discharge Spectrometry (GDS) is the best technique. Using glow discharge optical emission spectroscopy (GD-OES), limit of detection can reach up to micro-gram/gram level. While glow discharge mass spectrometry (GD-MS) is a much sensitive analytical technique which is commonly used for elemental analysis of ultra-pure materials and limit of detection up to 50 ng/kg can be reached. :)
An Energy Dispersive X-Ray Analyzer (EDX ) is also provide elemental identification and quantitative compositional information.
Laser Induced Breakdown Spectroscopy (LIBS) is slowly and gradually replacing all other techniques for qualitative and quantitative elemental analysis but still require other standard techniques like ICP-MS, ICP-OES, GD, EDX, NAA, etc. for benchmarking.
LIBS mostly unsuccessful to detect trace elemental quantities in sub ppm level and completely futile in ppt level trace detection.
Dear Manas RANJAN Sahu,
You may have a look at the our recent published papers on comparative study of different CF-LIBS based techniques and other analytical techniques. These papers may help your understanding
Best Wishes
Nasar
ICPMS - Inductively coupled plasma mass spectrometry (ICP-MS) is a type of mass spectrometry that uses an Inductively coupled plasma to ionize the sample. It atomizes the sample and creates atomic and small polyatomic ions, which are then detected.
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