This method is for the determination of chlorinated acids (herbicides) in drinking water, ground water, raw source water, and water at any intermediate treatment stage. Forty milliliters of samples is adjusted to pH 12 with 4N sodium hydroxide to hydrolize derivatives. After derivitization, the sample is extracted with methyl-tert-butyl-ether (MTBE). The chlorinated acids are converted to the methyl ester form by derivitizing with diazomethane or tetramethylammonium hydroxide followed by methyl iodide. The esters are then analyzed by capillary column gas chromatography with an electron capture detector (ECD).
The method strongly recommends that any positive detects are confirmed with analysis using a second column.
Phthalate esters are the source of major interferences with the elctron capture detector. Avoid use of any flexible tubing during sample collection.
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| Hold Times, Preservatives, Preps, Collection, Analytical & Documentation | |
|---|---|
| Holding Time: | 14 days from collection to extraction if the sample has been preserved and 14 days from extraction to analysis. |
| Preservatives: | If residual chlorine is present, add 4mg of sodium thiosulfate per 50mL to the bottle prior to collection. Samples must be iced or refrigerated at 4°C and kept away from light from the time of collection until extraction. |
| Required Preps: | 50mL Amber glass bottle with Teflon-lined cap |
| Collection Method: | Grab sampling |
| Analytical Methodology: | GC/ECD |
| Documentation: | 
515.3
|
| Analyte | Formula | CAS Number | Detection Limit | |
|---|---|---|---|---|
| 4-Nitrophenol | C6H5NO3 |
100-02-7 |
1.25 |
µg/L |
| Dichloroprop | C9H8Cl2O3 |
120-36-5 |
0.51 |
µg/L |
| Chloramben | C7H5Cl2NO2 |
133-90-4 |
0.25 |
µg/L |
| Dicamba | C8H6Cl2O3 |
1918-00-9 |
0.3 |
µg/L |
| Picloram | C6H3Cl3N2O2 |
1918-02-1 |
1 |
µg/L |
| Bentazon | C10H12N2O3S |
25057-89-0 |
1.25 |
µg/L |
| Acifluorfen | C14H7ClF3NO5 |
50594-66-6 |
0.47 |
µg/L |
| 3,5-Dichlorobenzoic acid | C7H4O2Cl2 |
51-36-5 |
0.625 |
µg/L |
| Dalapon | C3H4Cl2O2 |
75-99-0 |
1.25 |
µg/L |
| 5-Hydroxydicamba | C8H6Cl2O4 |
7600-50-2 |
0.625 |
µg/L |
| Pentachlorophenol | C6HCl5O |
87-86-5 |
0.085 |
µg/L |
| Dinoseb | C10H12N2O5 |
88-85-7 |
0.82 |
µg/L |
| 2,4,5-TP (Silvex) | C9H7Cl3O3 |
93-72-1 |
0.14 |
µg/L |
| 2,4,5-T | C8H5Cl3O3 |
93-76-5 |
0.2 |
µg/L |
| 2,4-D | C8H6Cl2O3 |
94-75-7 |
0.35 |
µg/L |
| 2,4-DB | C10H10Cl2O3 |
94-82-6 |
1.25 |
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.