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Microwave digestion of coal fly ash

Summary
Reference Material Coal Fly Ash NCS ZC 78001 is digested in a acid solution using a Analytik
Jena microwave digestion system (DIN EN 14385).

Equipment Type Manufacturer

TOPwave® Analytik Jena AG
CX 100 Analytik Jena AG

Reagents
HNO3 65% 7 ml
HF 40% 3 ml
H3BO3 saturated solution 20 ml

Procedure
1st step:
Weigh 500 mg of the sample into the digestion vessel. Add 7 ml of nitric acid and 3 ml of
hydrofluoric acid. Close the vessel and heat in the microwave oven with the following program.

Temperature Program Step 1 2 3 4

T [°C] 180 200
P [bar] 80 80
Power [%] 80 80
Ramp [min] 5 5
Time [min] 15 20
To avoid foaming and splashing wait until the vessels have cooled to room temperature (about 20 min). Carefully open
the digestion vessel in a fume hood wearing hand, eye and body protection since a large amount of gas will be produced
during the digestion process.

Microwave digestion of coal fly ash

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Reference: TOPwave_04_09_e | OB
2nd step:
Add 20 ml of boric acid solution or 0.5 g H3BO3, close the vessel and heat in the microwave oven
with program “complexation H3BO3”.
Temperature Program Step 1 2 3 4
T [°C] 190
P [bar] 50
Power [%] 90
Ramp [min] 5
Time [min] 10
Wait until the vessels have cooled to room temperature. Carefully open the digestion vessel in a fume hood wearing
hand, eye and body protection.

Transfer the solution to a volumetric flask and dilute with water.

Results
Clear solution

Validation
All elements were determined by AAS.

Element Result Certified Value

[µg/g] [µg/g]
Cr 58.0 60
Co 33.0 33
Cu 52.0 53
Zn 64.7 61

Notes: This application serves only as a guide line and may need to be optimized for your sample.

Chemicals of Sigma Aldrich® were used.

Printing and further use permitted with a reference to the source.

© 2009 Analytik Jena AG
Publisher:
Analytik Jena AG
Konrad-Zuse-Straße 1 Telephone +49 (0) 36 41 / 77-70 www.analytik-jena.com
07745 Jena Fax +49 36 41 77-92 79 info@analytik-jena.com

Microwave digestion of coal fly ash

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Reference: TOPwave_04_09_e | OB