This is a gas chromatographic (GC) method applicable to the determination of nitrosamines in municipal and industrial discharges as provided under 40 CFR 136.1. A measured volume of sample, approximately 1 L, is extracted with methylene chloride using a separatory funnel. The methylene chloride extract is washed with dilute hydrochloric acid to remove free amines, dried, and concentrated to a volume of 10 mL or less. After the extract has been exchanged to methanol, it is separated by gas chromatography and the parameters are then measured with a nitrogen-phosphorus detector. The method provides Florisil and alumina column cleanup procedures to separate diphenylamine from the nitrosamines and to aid in the elimination of interferences that may be encountered.
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| Hold Times, Preservatives, Preps, Collection, Analytical & Documentation | |
|---|---|
| Holding Time: | All samples must be extracted within seven days of collection and completely analyzed within 40 days of extraction. |
| Preservatives: | All samples must be iced or refrigerated at 4°C from the time of collection until extraction. Samples should be stored in amber or foil-wrapped bottles in order to minimize photolytic decomposition. If residual chlorine is present, add 80 mg of sodium thiosulfate per liter of sample and mix well. |
| Required Preps: | Glass bottle |
| Collection Method: | Grab or composite sampling |
| Analytical Methodology: | GC/NPD (Nitrogen Phosphorous Detection) |
| Documentation: | 
607
|
| Analyte | Formula | CAS Number | Detection Limit | |
|---|---|---|---|---|
| N-Nitrosodipropylamine | C6H14N2O |
621-64-7 |
0.46 |
µg/L |
| N-Nitrosodimethylamine | C2H6N2O |
62-75-9 |
0.15 |
µg/L |
| N-Nitrosodiphenylamine | C12H10N2O |
86-30-6 |
0.81 |
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.