I have a question, I stirred the sugarcane biomass with ruthenium, added sodium alginate and gelled in an iron solution. Soon after, pyrolysis at 700ºC. I'm having this DRX profile, I'm suspicious that I have amorphous zero-valent iron particles, so I don't see spikes at 45° as expected. It would be possible?
Dear Joao Carlos
thank you for posting this interesting question on RG. I'm wondering what the goal of your experiment was. Especially the role of ruthenium is absolutely not clear to me. I assume that in the end you want to prepare some sort of biosorbents, right? For a potentially useful overview about this topic I suggest to have a look at the following review article:Sugarcane bagasse: a potential low-cost biosorbent for the removal of hazardous materials
Article Sugarcane bagasse: a potential low-cost biosorbent for the r...
This paper is freely available as public full text on RG.
For some good informantion about the full characterization of biosorbents using e.g. scanning electron microscopy (SEM), XRD (X-ray diffraction, not XDR or DRX 😎) and FTIR spectroscopy please also see the following instructive reference:
Chemical, Structural and Elemental Characterization of Biosorbents Using FE-SEM, SEM-EDX, XRD/XRPD and ATR-FTIR Techniques
https://www.longdom.org/open-access/chemical-structural-and-elemental-characterization-of-biosorbents-usingfesem-semedx-xrdxrpd-and-atrftir-techniques-2157-7048-1000295.pdf
This paper has been published Open Access and is freely available as public full text (see attached pdf file).
I assume that further details should better be discussed with your supervisor. In any case I would not expect to find anything crystalline in the XRD pattern when you start with sugarcane biomass.
Good luck with your work and best wishes, Frank Edelmann
Dear Joao Carlos
,in addition to the comments of Frank T. Edelmann with respect to the chemical/preparation aspects of your query,
I will comment on experimental XRD issues for your case.
a) You have got iron in your sample. Performing XRD with a Cu source ( Cu K-alpha radiation at about 1,54A in wavelength or about 8,04keV in photon energy) will give you in case of Fe as part of your sample a lot of Fe K-fluorescence radiation (Fe K-edge is at about 7,1keV). Your huge background is due to Fe K-fluorescence.
In order to avoid this background you should use a Co source. Co K-alpha is at about 1,79A or 6,93keV and is not able to excite Fe K-fluorescence.
The Fe 110 peak, which should show up for Cu radiation at about 45° in 2theta (you mentioned that angular position above), will show up at about 52,3° in 2theta for the Co radiation.
b) You i) neither see any narrow 'crystalline' peak at 45° nor ii) any broad amorphous peak there. The strong increase of your background may mask the amorphous peak when it is small compared to the background.
c) I have got the impression, that your height adjustment of your sample with respect to the center of your XRD imaging system has failed. You should play around with the height position and 'see', whether you can establish any structure around 45° (despite the increasing background there). However, as mentioned above; via the application of a Co source the background will be removed.
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