Spectrasol Applications
Sample Type: Coal & Fly Ash
|
 Preparation: |
Weigh 0.1 gm sample into 60 mls Teflon digestion vessel. Add 2
mls water + 0.5 ml HNO3 + 3 mls HF + 7 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 50 mls Spectrasol CFA-B reagent + 50 mls Spectrasol
CFA-C reagent. Dilute final solution weight to 250 gms with water.
|
| Results: |
Comparison of ICP results (n = 3) using Spectrasol Coal Fly Ash
(CFA) reagents for the NIST 1632b coal ash SRM. |
|
| Analyte |
ICP Analysis |
NIST Certified |
Recovery |
|
(%) |
(%) |
(%) |
|
| Si |
1.39 ± 0.01 |
(1.4) |
99 |
| Al |
0.864 ± 0.005 |
0.855 ± 0.019 |
101 |
| Ti |
0.0454 ± 0.0004 |
0.0454 ± 0.0017 |
100 |
| Fe |
0.759 ± 0.003 |
0.759 ± 0.045 |
100 |
| Ca |
0.208 ± 0.004 |
0.204 ± 0.006 |
102 |
| Mg |
0.0387 ± 0.0008 |
0.383 0 ± 0.0008 |
101 |
| Na |
0.0525 ± 0.0010 |
0.0515 ± 0.0011 |
102 |
|
| Discussion: |
The Spectrasol CFA-B reagent redissolves fluoride precipitates
such as CaF2. The CFA-C reagent deactivates free fluoride and neutralizes
the pH. The avoidance of fusions reduces the dissolved solids
in solution allowing for the use of a glass concentric nebulizer.
|
| Reference: |
Tatro, M.E., V.M. Giampa and R.J. Collins. Recent advances in the dissolution
of zeolites and coal ash for Flame AA and ICP analysis. Spectroscopy, 4, 2, 18 (1989). |