This method is for the determination of certain chlorinated herbicides from municipal and industrial wastewater. One liter of sample is acidified and the acid herbicides and their esters and salts are extracted with ethyl ether using a separatory funnel. The derivatives are hydrolyzed with potassium hydroxide and extraneous organic material is removed by a solvent wash. After acidification, the acids are extracted and converted to their methyl esters using diazomethane as the derivatizing agent. Excess reagent is removed, and the esters are analyzed by gas chromatography with and electron capture detector (GC/ECD).
This method is also applicable to the determination of salts and esters of these compounds. These include, but are not limited to: the isobutyl and isooctyl esters of 2,4-D; the isobutyl and isooctyl esters of 2,4-DB; the isooctyl ester of MCPA; and the isooctyl ester of 2,4,5-TP.
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| Hold Times, Preservatives, Preps, Collection, Analytical & Documentation | |
|---|---|
| Holding Time: | 7 days from sample collection to extraction and 40 days from sample extraction to analysis. |
| Preservatives: | The samples must be iced or refrigerated at 4°C from the time of collection until extraction. |
| Required Preps: | 1L amber glass bottle |
| Collection Method: | Grab sampling |
| Analytical Methodology: | GC/ECD |
| Documentation: | 
615
|
| Analyte | Formula | CAS Number | Detection Limit | |
|---|---|---|---|---|
| Dichloroprop | C9H8Cl2O3 |
120-36-5 |
0.65 |
µg/L |
| Dicamba | C8H6Cl2O3 |
1918-00-9 |
0.27 |
µg/L |
| MCPP | C10H11ClO3 |
7085-19-0 |
192 |
µg/L |
| Dalapon | C3H4Cl2O2 |
75-99-0 |
5.8 |
µg/L |
| Dinoseb | C10H12N2O5 |
88-85-7 |
0.07 |
µg/L |
| 2,4,5-TP (Silvex) | C9H7Cl3O3 |
93-72-1 |
0.17 |
µg/L |
| 2,4,5-T | C8H5Cl3O3 |
93-76-5 |
0.2 |
µg/L |
| MCPA | C9H9ClO3 |
94-74-6 |
249 |
µg/L |
| 2,4-D | C8H6Cl2O3 |
94-75-7 |
1.2 |
µg/L |
| 2,4-DB | C10H10Cl2O3 |
94-82-6 |
0.91 |
µg/L |
* The analytes and detection limits listed for each method represent the typical detection limits and analytes reported for that particular method. Keep in mind that analyte lists may vary from laboratory to laboratory. Detection limits may also vary from lab to lab and are dependent upon the sample size, matrix, and any interferences that may be present in the sample.