Spectrasol Applications
Sample Type: Fluid Cracking Catalyst
|
 Preparation: |
Weigh 0.2 gm sample into 125 mls Teflon digestion vessel. Add
2 mls water + 0.5 ml HNO3 + 12 mls HF + 3 mls HCl.
Place the capped vessel in a hot water bath at 95ºC for 30 minutes.
Cool, open vessel and transfer contents to a pre-tared plastic
bottle.
Add 75 mls Spectrasol Z-B reagent. Dilute final solution weight
to 100 gms with water.
|
| Results: |
Correlation (n=50) of ICP results from the more laborious perchloric
acid-hydrofluoric acid-boric acid preparation of fluid cracking
catalysts with the Spectrasol preparation |
|
| Analyte |
Concentration |
Correlation (r)
|
|
| Al2O3 |
12.0 - 55.2% |
0.996 |
| CaO |
0.02 - 1.61% |
0.997 |
| Fe2O3 |
0.48 - 3.45% |
0.997 |
| MgO |
0.01 - 2.98% |
0.999 |
| Na2O |
0.00 - 1.07% |
0.998 |
| P2O5 |
0.01 - 1.32% |
0.989 |
| Re2O3 |
0.00 - 3.88% |
0.998 |
| SiO2 |
41.2 - 81.7% |
0.985* |
| TiO2 |
0.72 - 3.17% |
0.998 |
| Ni |
0 - 4100 ppm |
0.999 |
| Sb |
183 - 1900 ppm |
0.999 |
| V |
0 - 3200 ppm |
0.999 |
* The SiO2 results for the perchloric acid preparation are by difference.
|
| Discussion: |
The closed vessel Spectrasol method has replaced the perchloric
acid method that involves multiple evaporations and loss of silicon.
The avoidance of boric acid reduces the solids in the sample allowing
for the use of a glass concentric nebulizer. The batching of digests
in a hot water bath reduces analyst intervention and increases
productivity.
|
| Reference: |
Tatro, M.E. A novel dissolution technique for the preparation of zeolites
fluid cracking catalysts and clays. Spectroscopy, 5, 2, 16 (1990). 355, 793 (1996). |