This method is used for sampling and analysis of a variety of common pesticides and polychlorinated biphenyls (PCBs) in ambient air using a high volume sampler. The procedure is based on the adsorption of chemicals from ambient air on polyurethane foam (PUF) cartridge and a quartz fiber filter. The samples are analyzed using gas chromatography combined with a variety of detectors that are suitable for analyzing pesticides and PCBs.
The high volume PUF sampling procedure is applicable to multicomponent atmospheres containing common pesticide concentrations from 0.001 to 50 µg/m3 over 4 to 24 hour sampling periods. A total sample volume of greater than 300 scm (standard cubic meters) is collected at a rate of 4-10 scfm(standard cubic feet per minute). The high volume method is used to collect a suffcient volume of sample in order to detect pesticides and PCBs during the analysis because of the relatively low levels of these compounds found in the environment. The PUFs must be precleaned prior to sampling and certified clean prior to use. One PUF in each preparation batch must be analyzed and contain less than 10ng of single component compounds and <100ng of multi-component compounds. The PUFs are inserted into the glass cartridge and wrapped in hexane rinsed aluminum foil. There is a 30 day holding time from the certification of the PUF until sampling.
The method calls for the collection of a field blank and a field spike. The field spike is a PUF spiked with target compounds prior to sampling and ships to the field with the blank PUFs, however, no sample is pulled through the spiked PUF. This spiked PUF is then analyzed with the field samples upon return to the laboratory.
After sampling the PUF and filter are Soxhlet extracted using 10% diethyl ether in hexane and analyzed using gas chromatography combined with a variety of suitable detectors. Types of detectors used are ECD (eletrochemical detector), FPD (flame photometric detector), NPD (nitrogen phosphorous detector), and HECD (Hall electrolytic conductivity detector). In some instances, it may also be suitable to use GC/MS and HPLC/UV for analysis.
The limits of detection will depend on the nature of the analyte and the length of the sampling period. Method TO-10A is similar, but can be used for a lower rate of volume on collection.
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| Hold Times, Preservatives, Preps, Collection, Analytical & Documentation | |
|---|---|
| Holding Time: | 7 days from collection to extraction and 40 days from extraction to analysis |
| Preservatives: | Keep at 4°C or less after sample collection and protect from UV light. |
| Required Preps: | A 102mm quartz fiber filter (baked) and a precleaned PUF. A 65 mm OD x 25 mm borosilicate glass sorbent cartridge is used to hold the PUF. 30 day hold time for preps (if stored in foil). |
| Collection Method: | TO-4A |
| Analytical Methodology: | GC/ECD, GC/FPD, GC/NPD, GC/HECD, GC/MS, or HPLC/UV |
| Documentation: | 
TO-4A
|
| Analyte | Formula | CAS Number | Detection Limit | |
|---|---|---|---|---|
| Heptachlor epoxide | C10H5Cl7O |
1024-57-3 |
0.1 |
µg |
| Resmethrin | C22H26O3 |
10453-86-8 |
0.1 |
µg |
| Aroclor-1260 | 11096-82-5 |
0.1 |
µg | |
| Aroclor-1254 | 11097-69-1 |
0.1 |
µg | |
| Propoxur (Baygon) | C11H15NO3 |
114-26-1 |
0.1 |
µg |
| Dicofol (Kelthane) | 115-32-2 |
0.1 |
µg | |
| Hexachlorobenzene | C6Cl6 |
118-74-1 |
0.1 |
µg |
| Pyrethrin | C22H28O5 |
121-29-9 |
0.1 |
µg |
| Malathion | C10H19O6PS2 |
121-75-5 |
0.1 |
µg |
| Simazine | C7H12ClN5 |
122-34-9 |
0.1 |
µg |
| Captan | C9H8Cl3NO2S |
133-06-2 |
0.1 |
µg |
| Folpet | C9H4Cl3NO2S |
133-07-3 |
0.1 |
µg |
| Polychlorinated Biphenyls | 1336-36-3 |
0.1 |
µg | |
| Propazine | C9H16ClN5 |
139-40-2 |
0.1 |
µg |
| Dicrotophos | C8H16NO5P |
141-66-2 |
0.1 |
µg |
| Monuron | C9H11ClN2O |
150-68-5 |
0.1 |
µg |
| Chlorotoluron | C10H13ClN2O |
15545-89-9 |
0.1 |
µg |
| Carbofuran | C12H15NO3 |
1563-66-2 |
0.1 |
µg |
| Trifluralin | C13H16F3N3O4 |
1582-09-8 |
0.1 |
µg |
| Alachlor (Lasso) | C14H20ClNO2 |
15972-60-8 |
0.1 |
µg |
| 2,3,5,6-Tetrachloro-1,4-benzenedicarboxylic acid dimethyl ester (Dacthal) | C10H6Cl4O4 |
1861-32-1 |
0.1 |
µg |
| Chlorothalonil (Bravo) | C8Cl4N2 |
1897-45-6 |
0.1 |
µg |
| Atrazine | C8H14ClN5 |
1912-24-9 |
0.1 |
µg |
| Fluometuron | C10H11F3N2O |
2164-17-2 |
0.1 |
µg |
| Bendiocarb | C11H13NO4 |
22781-23-3 |
0.1 |
µg |
| Mirex | C10Cl12 |
2385-85-5 |
0.1 |
µg |
| Oxychlordane | C10H4Cl8O |
27304-13-8 |
0.1 |
µg |
| Chlorpyrifos (Dursban) | C9H11Cl3NO3PS |
2921-88-2 |
0.1 |
µg |
| Methyl parathion | C8H10NO5PS |
298-00-0 |
0.1 |
µg |
| Phorate | C7H17O2PS3 |
298-02-2 |
0.1 |
µg |
| Ronnel | C8H8Cl3O3PS |
299-84-3 |
0.1 |
µg |
| Aldrin | C12H8Cl6 |
309-00-2 |
0.1 |
µg |
| Zectran (Mexacarbate) | C12H18N2O2 |
315-18-4 |
0.1 |
µg |
| alpha-BHC | C6H6Cl6 |
319-84-6 |
0.1 |
µg |
| beta-BHC | C6H6Cl6 |
319-85-7 |
0.1 |
µg |
| Diuron | C9H10Cl2N2O |
330-54-1 |
0.1 |
µg |
| Linuron | C9H10Cl2N2O2 |
330-55-2 |
0.1 |
µg |
| Diazinon | C12H21N2O3PS |
333-41-5 |
0.1 |
µg |
| Tebuthiuron | C9H16N4OS |
34014-18-1 |
0.1 |
µg |
| trans-Nonachlor | C10H5Cl9 |
39765-80-5 |
0.1 |
µg |
| 4,4'-DDT | C14H9Cl5 |
50-29-3 |
0.1 |
µg |
| Metolachlor | C15H22ClNO2 |
51218-45-2 |
0.1 |
µg |
| Fenvalerate | C25H22ClNO3 |
51630-58-1 |
0.1 |
µg |
| trans-Permethrin | C21H20Cl2O3 |
51877-74-8 |
0.1 |
µg |
| Aroclor-1242 | 53469-21-9 |
0.1 |
µg | |
| cis-Permethrin | C21H20Cl2O3 |
54774-45-7 |
0.1 |
µg |
| Ethyl parathion | C10H14NO5PS |
56-38-2 |
0.1 |
µg |
| Chlordane | C10H6Cl8 |
57-74-9 |
0.1 |
µg |
| Allethrin | C19H26O3 |
584-79-2 |
0.1 |
µg |
| gamma-BHC (Lindane) | C6H6Cl6 |
58-89-9 |
0.1 |
µg |
| Dieldrin | C12H8Cl6O |
60-57-1 |
0.1 |
µg |
| Pentachlorobenzene | C6HCl5 |
608-93-5 |
0.1 |
µg |
| Carbaryl (Sevin) | C12H11NO2 |
63-25-2 |
0.1 |
µg |
| Methoxychlor | C16H15Cl3O2 |
72-43-5 |
0.1 |
µg |
| 4,4'-DDE | C14H8Cl4 |
72-55-9 |
0.1 |
µg |
| Heptachlor | C10H5Cl7 |
76-44-8 |
0.1 |
µg |
| Pentachlorophenol | C6HCl5O |
87-86-5 |
0.1 |
µg |
| 2-Phenylphenol | C12H10O |
90-43-7 |
0.1 |
µg |
| 2,4-D | C8H6Cl2O3 |
94-75-7 |
0.1 |
µg |
| Dichloran (Botran) | C6H4Cl2N2O2 |
99-30-9 |
0.1 |
µg |
* 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.