I need elemental analysis of individual ceramic powders and agglomerated fluxes (flux which comprise mixture of SiO2,TiO2,CaO,Al2O3,MgO costituents). For elemental analysis of these fluxes and individual powders by ICP-OES which Acid/acids required for dissolving all these elements??
I mean for dissolving fluxes and individual ceramic powders which acid required? plz suggest .
Try reference:
https://www.inorganicventures.com/sample-preparation
I have used concentrated H2SO4 to prepare sample of TiO2 (P25) for ICP-OES analysis. I hope it will work for your other materials also. Follow the below steps with full precautions with the reaction taking place only inside a hood having proper ventilation.
DIGESTION in acid
1. Take 5mg of your powder sample in a 20 ml vial with 2 ml conc. H2SO4 in it.
2. Stir the above mixture at 500 rpm @ 400 C.
3. You will observe an initial orange colour and acid starts to boil with fumes coming out ( WEAR MASK AND GLOVES, PROPER HOOD VENTILATION)
4. Stir the above solution until 1 ml acid is left and cool down.
5. If you observe powder suspended, then add more acid (around 2 ml) and again stir.
6. If the amount of acid left is 1 ml, cool down the acid to RT.
Filtration of sample
1.Filter the above solution using a 400 nm syringe filter by adding 10 ml DI water.
2. The pH of the solution SHOULD BE NUETRAL or it will damage the ICP-OES sensor.
3. Finally dilute your sample in 10 ml DI water.
4. Give your sample plus 10 ml DI water (background sample) to the operator for analysis.
NOTE: You must keep a note of all the calculation of acid added, sample taken in preparing your sample because the operator will ask so.
Good luck!
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