Send to

Choose Destination
See comment in PubMed Commons below
Anal Chem. 2012 Jul 3;84(13):5548-55. doi: 10.1021/ac3003566. Epub 2012 Jun 18.

Determination of chemical oxygen demand in heterogeneous solid or semisolid samples using a novel method combining solid dilutions as a preparation step followed by optimized closed reflux and colorimetric measurement.

Author information

IRTA, GIRO Joint Research Unit IRTA-UPC, Torre Marimon, Barcelona, Spain.


This paper reports the development of an innovative sample preparation method for the determination of the chemical oxygen demand (COD) in heterogeneous solid or semisolid samples, with high suspended solids and COD concentrations, using an optimized closed reflux colorimetric method. The novel method, named solid dilution (SD), is based on a different technique of sample preparation, diluting the sample with magnesium sulfate (MgSO(4)) previous to COD determination. With this, it is possible to obtain a solid homogeneous mixture much more easily analyzable. Besides, a modification of concentration and ratio of reagents was optimized to make the closed reflux colorimetric method suitable for complex substrates with COD levels ranging from 5 to 2500 g O(2) kg(-1) TS. The optimized method has been tested with potassium hydrogen phthalate (KHP) as primary solid standard and using different solid or semiliquid substrates like pig slaughterhouse waste and sewage sludge, among others. Finally, the optimized method (SD/SM-CRC) was intensively tested in comparison to the standard titrimetric method (SM-ORT) using different certified reference materials (CRM). The developed method was found to give higher accuracy, 1.4% relative standard deviation (RSD) vs 10.4%, and bias of 2.8% vs 8.0%, in comparison to the standard open reflux titrimetric method.

[Indexed for MEDLINE]
PubMed Commons home

PubMed Commons

How to join PubMed Commons

    Supplemental Content

    Full text links

    Icon for American Chemical Society
    Loading ...
    Support Center