Pesticides in Wastewater Analysis by EPA 608.3
Summary
EPA 608.3 is used to determine the concentrations of Pesticides in wastewater.
Technique
EPA 608.3 is performed using separatory funnel liquid-liquid extraction and gas chromatography/electron capture detection (GC/ECD).
Holding Time
Samples must be extracted within 7-days of collection. Samples not extracted within this period must be discarded and replaced. If the sample will not be extracted within 72 hours of collection, check the pH and adjust to a range of 5.0 to 9.0; record the volume of sodium hydroxide (NaOH) or sulfuric acid (H2SO4) used. Sample extracts must be analyzed within 40 days of extraction.
Container and Preservative
Collect all samples in (2) 1-L amber glass bottles fitted with a fluoropolymer-lined screw cap. Bottles must NOT be rinsed with the sample before collection. Samples must be kept refrigerated at ≤6°C and protected from light during compositing. Ice or refrigerate samples at >0°C to ≤6°C from the time of collection, but do NOT freeze. If residual chlorine is present and aldrin is to be determined, add a dechlorinating agent (e.g., 80 mg/L sodium thiosulfate, ascorbic acid, or sodium sulfite) and mix well.
Shipping/Transport Instructions
Samples must be protected from light and chilled to >0°C to ≤6°C at collection and kept at >0°C to ≤6 °C until extracted. Field samples must be packaged for shipment with sufficient ice to ensure that they will be >0°C to ≤6 °C upon arrival at the laboratory.
Analytes and Reporting Limits
Analytes routinely reported are listed below.
| Analyte | CAS Number | Reporting Limit |
| alpha-BHC | 319-84-6 | 0.01 µg/L |
| Lindane (gamma-BHC) | 58-89-9 | 0.01 µg/L |
| beta-BHC | 319-85-7 | 0.01 µg/L |
| delta-BHC | 319-86-8 | 0.01 µg/L |
| Heptachlor | 76-44-8 | 0.01 µg/L |
| Aldrin | 309-00-2 | 0.01 µg/L |
| Heptachlor epoxide | 1024-57-3 | 0.01 µg/L |
| gamma-Chlordane | 5103-74-2 | 0.005 µg/L |
| alpha-Chlordane | 5103-71-9 | 0.005 µg/L |
| Endosulfan I | 959-98-8 | 0.01 µg/L |
| 4,4'-DDE | 72-55-9 | 0.01 µg/L |
| Dieldrin | 60-57-1 | 0.01 µg/L |
| Endrin | 72-20-8 | 0.01 µg/L |
| 4,4'-DDD | 72-54-8 | 0.01 µg/L |
| Endosulfan II | 33213-65-9 | 0.01 µg/L |
| 4,4'-DDT | 50-29-3 | 0.01 µg/L |
| Endrin aldehyde | 7421-93-4 | 0.01 µg/L |
| Endosulfan sulfate | 1031-07-8 | 0.01 µg/L |
| Methoxychlor | 72-43-5 | 0.01 µg/L |
| Endrin ketone | 53494-70-5 | 0.01 µg/L |
| Chlordane (as alpha- + gamma-) | 57-74-9 (a+g) | 0.01 µg/L |
| Chlordane, Technical | 57-74-9 (Tech) | 0.1 µg/L |
| Toxaphene | 8001-35-2 | 0.5 µg/L |