The sample is an intermediate product in the synthesis of CuO-doped TiO2 catalyst. Ethanoic acid is added and it reacts with copper nitrate to produce copper(II)acetate. A gel is prepared with sol gel method and calcined at 500°C
The temperature needed to ensure that all copper precursor are converted to copper(II)oxide CuO is 500°C. A sample is prepared by terminating the calcination at 300°C. At this stage the copper(II)acetate is almost completely converted to copper and copper(I)oxide Cu2O according to scientific literature.
The mole ratio of copper in comparison to titanium is very low and at 300°C the sample is almost completely amorphous. Therefore X-ray diffraction spectroscopy cannot be used to determine the exact composition of the sample.
Is there any analysis method to determine the exact composition of the sample? It is particularly important to find out what the copper-containing compounds are (Cu/Cu2O/CuO ?) and whether there are any copper-containing organics (Copper(II)acetate) left.
Could Raman spectroscopy work?
Hi Yu,
This is an interesting question and I would love to see it answered. Given the complexity of the problem I am inclined that any one characterization method would be insufficient. XPS is a good technique, however, the presence of C creates a problem and depth profiling would take ages. Same is the case with X-ray diffraction analysis. Volumetric determination is theoretically possible, but against the background of an amorphous sample it might be very difficult.
I wonder if there is a way to dissolve and separate the different species individually and then use GC-MS to quantify them.
XPS can help. Precipitation or complexation of Cu compounds selectively followed by estimation of organic content May be indirectly. Selective Complex formation and calib curve development may help in their determination using UV spectroscopy or if the Cu containg compounds are in the colloidal range then based on their SPR their amounts can be quantified in development of calib curve.
I have used xps as method to distinguish chemical bond of Cu element, it's really useful, but xps is test the surface element, if Cu element is under the suface of particle, you maybe have to destroy the particle so that the inner element will be tested. Best luck for you.
XPS is a good technique. If you are going to perform XPS, it is important that you pick up the Cu 2p and Cu KLMM lines. The identification of the chemical state of the sample depends on the binding energy and the distance between the peaks.
By performing C,H,N,S ICP-OES, TGA,-DTA and XRD you can get the composition.
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