Am currently working on a project on metal complexes and what to know NMR, XRF AND GC-MS which will give better results in characterization.
It really depends on what you want to know. If you are interested to know the morphology of your complexes, then you can go for SEM. Generally CHN, EDX and IR are reported are reported for the characterisation. NMR are also very helpful. For the thermal stability you should go for TGA analysis. And the most important technique is X-ray. The real structure and actual geometry of your complex can present by X-ray.
All the very best.
XRF, ICP-OES and TEM can be used for this purpose in addition to other technics
In general: FT-IR, UV-Vis, NMR, HPLC, HRMS or elemental analysis are the main requirements for the characterization of a new compound.
Other analysis are highly dependent on the materials you work on:
- NMR works well for diamagnetic metal complexes, paramagnetic complexes give broad signals with low S/N;
- X-Ray single crystal diffraction, if you manage to crystallize the compund and the crystals diffract;
- electrochemistry, spectroelectrochemistry, EPR for redox properties;
- for other techniques to highlight properties of your materials check the specific literature.
- check also this discussion:
https://www.researchgate.net/post/How_to_Analyze_Metal_Organic_Complexes_what_kind_of_characterization_do_I_need_to_use
General characterisation of ligand is report to IR, UV-Vis, CHN,Gc-MS, NMR and Xrd(crystal/powder). The metal complexes are characteristic of IR,UV-Vis, CHN,Gc-MS, magnetic,Tga-Dta,ESR,Electrochemical and Xrd(crystal/powder).
In addition to the above said, you have to make up your mind WHAT YOU WANT TO KNOW: a) basic characterisation, b) structural characterisation, or c) further characterisation
a) basic characterisation to satisfy the needs to publish your new complex in a chemical journal: elemental analysis (is a must), NMR (is a must), MS (is recommended), IR (helpful), EPR (for paramagnetic complexes) or magnetic data (helpful), Uv-vis (helpful) - these things are submitted in the Experimental Section of a paper.
b) structural characterisation: single crystal XRD or powder XRD. Single crystal XRD gives you also the molecular structure which you can compare with NMR or IR data.
c) further methods for characterisation: melting point, chromatography, DTA-TG, DSC (thinking these methods over you will easily see, that they are not unequivocal, e.g. DTA does not help if you do not konw the composition).
For further physicochemical characterisation there are many methods available, depending what you want to study: EPR, magnetic measurements, UV-vis absorption, emission, Moessbauer, ESCA, XAS, electrochemical methods ...
Importantly, all these physicochemical methods in c) CANNOT replace a thorough characterisation using the methods from a). E.g. a journal will not accept a new complex based on a UV-vis absorption spectrum and an IR spectrum or a DTA or a powder XRD.
Hope this helps through "the jungle" of characterisation.
AK
Thanks for your response. Have gotten idea of what to analyze. You answers are of great importance to my study. Love you guys
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