Method TO-4A

Pesticides/PCBs in Ambient Air Using High Volume PUFs Sampling


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.


(EPA 600/4-89-017)

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Method Data

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 List*

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.