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NEMI Method Summary - 5220C

This method summary describes Standard Method 5220C for measuring chemical oxygen demand (COD) in water and wastewater samples. COD is measured by refluxing a sample with a known excess of potassium dichromate in an acid solution, which oxidizes organic matter. The remaining unreduced dichromate is then titrated to determine the amount consumed, and thus the amount of oxidizable organic matter present. Chloride, bromide, iodide, and other reagents that inactivate silver can interfere with the test. Nitrite also causes interference that can be eliminated by adding sulfamic acid. Reduced inorganic species are oxidized under test conditions. Sample handling and preparation procedures are described.

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52 views

NEMI Method Summary - 5220C

This method summary describes Standard Method 5220C for measuring chemical oxygen demand (COD) in water and wastewater samples. COD is measured by refluxing a sample with a known excess of potassium dichromate in an acid solution, which oxidizes organic matter. The remaining unreduced dichromate is then titrated to determine the amount consumed, and thus the amount of oxidizable organic matter present. Chloride, bromide, iodide, and other reagents that inactivate silver can interfere with the test. Nitrite also causes interference that can be eliminated by adding sulfamic acid. Reduced inorganic species are oxidized under test conditions. Sample handling and preparation procedures are described.

Uploaded by

Alberto VELOSA ROA
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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24/4/2020 NEMI Method Summary - 5220C

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Standard Methods: 5220C: COD by Closed Reflux, Titration


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Summary
Analytes
Revisions
Data and Sites

Official Method
Name 5220 C. Closed Reflux, Titrimetric Method

Current
Standard Methods 18th, 19th, 20th ed.
Revision
Media
WATER

Instrumentation
Not Applicable

Method
Subcategory Organic

Method Source
Standard Methods
Citation
Standard Methods Online - Standard Methods for the Examination of Water and Wastewater

Brief Method Most types of organic matter are oxidized by a boiling mixture of chromic and sulfuric acids. A sample is refluxed in strongly acid solution with a
Summary known excess of potassium dichromate (K2Cr2O7). After digestion, the remaining unreduced K2Cr2O7 is titrated with ferrous ammonium sulfate to
determine the amount of K2Cr2O7 consumed and the oxidizable organic matter is calculated in terms of oxygen equivalent.
Scope and
This parameter is generally of interest in wastewaters and natural waters. The closed reflux method (5220 C) is economical in the use of metallic salt
Application
reagents, but requires homogenization of samples containing suspended solids to obtain reproducible results.
Applicable
Concentration
40 to 400 mg/L
Range

The most common interferent is the chloride ion. Chloride reacts with silver ion to precipitate silver chloride, and thus inhibits the catalytic activity of
silver. Bromide, iodide, and any other reagent that inactivates the silver ion can interfere similarly. The difficulties caused by the presence of the
chloride can be overcome largely, though not completely, by complexing with mercuric sulfate (HgSO4) before the refluxing procedure. Halide
interferences may be removed by precipitation with silver ion and filtration before digestion. This approach may introduce substantial errors due to the
Interferences occlusion and carrydown of COD matter from heterogenous samples. Nitrite exerts a COD of 1.1 mg O2/mg NO2- -N. Because concentrations of NO2-
in waters rarely exceed 1 or 2 mg NO2- -N/L, the interference is considered insignificant and usually is ignored. To eliminate a significant interference
due to NO2-, add 10 mg sulfamic acid for each mg NO2- -N present in the sample volume used; add the same amount of sulfamic acid to the reflux
vessel containing the distilled water blank. Reduced inorganic species such as ferrous iron, sulfide, manganous manganese, etc., are oxidized
quantitatively under the test conditions.
Quality Control
Requirements See Section 5020 Quality Assurance/Quality Control

Preferably collect samples in glass bottles. Test unstable samples without delay. If delay before analysis is unavoidable, preserve sample by
Sample acidification to pH < or = 2 using conc H2SO4. Preferably acidify any sample that cannot be analyzed the same day it is collected. Blend samples
Handling
containing settleable solids with a homogenizer to permit representative sampling. Make preliminary dilutions for wastes containing a high COD to
reduce the error inherent in measuring small sample volumes.
Maximum
Holding Time 28 days (regulatory)

Relative Cost
$51 to $200
Sample
Preparation

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24/4/2020 NEMI Method Summary - 5220C
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