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Microwave Digestion of Sediments III
Summary
Digestion of sediments according to EPA 3051 with an acid mixture using an Analytik Jena
microwave digestion system.

Equipment Type Manufacturer

®
TOPwave Analytik Jena AG
PM 60 Analytik Jena AG

Reagents
HNO3 65% 3 ml
HCl 37% 9 ml

Procedure
Weigh 0.5 to 1.0 g of the sample into the digestion vessel. The amount of organic material should
not exceed 500 mg. Add 3 ml of nitric acid and 9 ml of hydrochloric acid and shake the mixture
carefully or stir with a clean PTFE or a glass bar. Wait at least 2 min before the vessel is closed.
Heat in the microwave oven with the following program:

Temperature Program Step 1 2 3 4

T [°C] 175
P [bar] 40
Power [%] 90
Ramp [min] 1
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.

Microwave digestion of Sediments III

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Reference: TOPwave_17_09_e | OB
Results
Clear solution with white precipitate of SiO2.
Recoveries on CRM 044-050. All elements analysed by AAS.

Element Certified value [µg/g] Results [µg/g] Recovery [%]

As 52.3 56.6 108 %
Cd 71.6 64.3 90 %
Cr 88.5 86.5 98 %
Co 50.6 47.2 93 %
Pb 77.8 69.5 89 %
Mn 204.0 209.0 103 %
Ni 87.1 80.6 93 %
Zn 136.0 129.0 95 %

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 Sediments III

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Reference: TOPwave_17_09_e | OB