United States
Environmental Protection
Agency
Environmental Monitoring and
Support Laboratory
Cincinnati OH 45268
Research and Development
EPA/600/S4-85/050 Sept. 1985
v°/EPA Project Summary
Evaluation of 10 Pesticide
Methods
T. M. Engel, J. S. Warner, and W. M. Cooke
Ten pesticide analysis methods were
evaluated. The compounds listed in
each method were analyzed in tripli-
cate at two concentration levels in
reagent water and POTW effluent. Each
method was performed as written with
only minor modifications. If a cleanup
procedure was included in the analysis
method, all analyses were performed
with and without the cleanup step.
Resultant data reported included es-
timated detection limits (EDLs) in
reagent water and recovery data from
reagent water and POTW effluent for
each compound. Suggestions for
method improvements were included
in the report where necessary.
This Project Summary was devel-
oped by EPA's Environmental Monitor-
ing and Support Laboratory, Cincinnati,
OH, to announce key findings of the re-
search project that is fully documented
in a separate report of the same title
(see Project Report ordering informa-
tion at back).
Introduction
Ten pesticide analysis methods were
evaluated; a description of the methods
and the compounds included in those
methods are listed in Table 1. The com-
pounds included in each method were
analyzed in triplicate at two concentra-
tion levels in reagent water and POTW
effluent. Each method was performed
as written with only minor modifica-
tions as approved by the EPA Project
Officer. If a cleanup procedure was in-
cluded in the analysis method, all analy-
ses were performed with and without
the cleanup step.
Resultant data reported included esti-
mated detection limits (EDLs) in reagent
water and recovery data from reagent
water and POTW effluent for each com-
pound before and after the optional
cleanup step. Suggestions for method
improvements were offered where
warranted.
Results
A summary of the EDL and recovery
data obtained during the evaluation of
the 10 pesticide methods is given in
Table 2. Methods 641, 643, and 645
were found to yield acceptable results
as written. Method 641.1 was not ac-
ceptable due to low recoveries of
ethoxyquin, presumably due to adsorp-
tion of the ethoxyquin to paniculate ma-
terial prior to filtration of the sample for
HPLC analysis. Method 642 was mar-
ginally acceptable; recoveries of bi-
phenyl and o-phenylphenol were low,
possibly due to the rigorous conditions
needed to concentrate sample extracts.
Method 632.1 was acceptable for two of
the compounds, napropamide and
propanil, but was not acceptable for the
determination of carbaryl (carbaryl re-
coveries were low and dependent upon
sample matrix and carbaryl concentra-
tion). Method 644 was not acceptable;
picloram recoveries were low, pre-
sumably due to incomplete extraction
of the picloram from the water matrix.
The extraction and analysis portions of
Method 614.1 were found to be accept-
able for dioxathion, EPN, ethion, and
terbufos. The silica gel cleanup proce-
dure included in Method 614.1 was not
acceptable; compound recoveries were
decreased by 50 percent or more when
the cleanup procedure was used.
Method 646 was found to be acceptable
for the determination of basalin and
marginally acceptable for the determi-
nation of CDNB and dinocap. Method
-------
Table 1. Pesticide Method Information
Method
Number
641
647.7
642
642
643
632.7
632.7
632.7
632.7
644
614.1
614.1
674.7
674.7
645
645
645
645
645
645
646
646
646
608.2
608.2
608.2
608.2
608.2
Compound(s)
Thiabendazole
Ethoxyquin
Biphenyl
0-Phenylphenol
Bentazon
Carbaryl
Napropamide
Propanil
Vacor
Picloram
Dioxathion
EPN
Ethion
Terbufos
Alachlor
Butachlor
Diphenamid
Lethane
Norflurazon
Fluridone
Basalin
CDNB
Dinocap
Chlorothalonil
DCPA
Dichloran
Methoxychlor
Permethrin
Extraction
Method
None
None
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
None
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Separatory funnel
Cleanup
Method
Filtration
Filtration
None
None
None
None
None
None
None
Backextraction
with base
Silica gel
Silica gel
Silica gel
Silica gel
Florisil
Florisil
Florisil
Florisil
None
None
Florisil
Florisil
Florisil
Silica gel
Florisil
Florisil
Silica gel
Silica gel
Analysis
Method
HPLC-Fluorescence
HPLC-Fluorescence
HPLC-UV
HPLC-UV
HPLC-UV
HPLC-UV
HPLC-UV
HPLC-UV
None
HPLC-UV
GC-NPD
GC-NPD
GC-NPD
GC-NPD
GC-NPD
GC-NPD
GC-NPD
GC-NPD
GC-NPD
GC-NPD
GC-ECD
GC-ECD
GC-ECD
GC-ECD
GC-ECD
GC-ECD
GC-ECD
GC-ECD
A standard of vacor could not be obtained; Method 5 was not evaluated for vacor.
608.2 was found to be acceptable for
cis- and trans-permethrin, but was not
acceptable for the determination of
DCPA, methoxychlor, chlorothalonil,
and dicloran. Recoveries of DCPA and
methoxychlor were low and concentra-
tion and matrix dependent. Recoveries
of chlorothalonil and dicloran could not
be determined because of the presence
of interferences.
-------
Table 2. Summary of Data from Evaluation of W Pesticide Analysis Methods
Recovery from Reagent Water. %ldl
Recovery from POTW Effluentldl
Method
Number Compound
641
641.1
642
642
643
632.1
632.1
632.1
644
614.1
614.1
614.1
614.1
645
645
645
645
645
645
646
646
646
608.2
608.2
608.2
608.2
608.2
608.2
Thiabendazole
Ethoxyquin
Biphenyl
O-Phenylphenol
Bentazon
Carbaryl
Napropamide
Propanil
Picloram
Dioxathion
EPN
Ethion
Terbufos
Alachlor
Butachlor
Diphenamid
Lethane
Norflurazon
Fluridone
Basalin
CDNB
Dinocap
Chlorothalonil
DCPA
Dicloran
Methoxychlor
Cis-permethrin
Trans-permethrin
EDL,
1.7
6.3
0.04
0.01
1.1
1.2
0.02
0.3
0.3
0.5
12
0.3
0.02
0.2
0.2
0.2
0.1
0.02
0.6
0.0005
0.0005
0.1
0.001
0.003
0.002
0.4
0.2
0.2
Spike Level, pg/L
Low
10
6.2
2.5
5.0
10
2.0
6.0
0.2
3.0
10
10
10
10
10
10
10
10
10
10
0.1
0.1
0.1
0.02
0.02
0.01
0.1
1.0
1.0
High
100
62
25
50
100
20
60
2
30
100
100
100
100
100
100
100
100
100
100
1
1
1
0.2
0.2
0.1
7
70
10
Before Cleanup
Low
93 ± 3
100 + 32
74+2
73 ± 4
92+2
52+ 10
103 ± 2
79+6
N.D.
76+ 10
120+ 6
120+ 5
90+3
96+3
96+4
93+6
93 ± 6
69 ± 10
49 ± 76
738 ± 12
91+8
78+7
llcl
128 + 18
1
57+ 1
94+9
111 ± 4
High
81+5
82+6
51 + 11
60+5
81 + 10
83+ 13
102 + 2
99+3
N.D.
78+2
120+ 4
95+2
84+ 1
94+2
93+ 1
94+2
100+ 1
92+ 1
81 + 15
113+ 4
69+5
77+4
1
94+11
1
106 + 12
91+2
98+3
After Cleanup
Low
N.C.ia>
N.C.
N.C.
N.C.
N.C.
N.C.
N.C.
N.C.
N.D.
43+ 7
N.D.
54 ± 8
N.D.
96 ± 3
95+3
95+2
97+2
69 ± 6
N.C.
126 ± 8
89 ± 6
26+3
1
73 + 25
1
37+8
91+6
83+ 72
High
N.C.
N.C.
N.C.
N.C.
N.C.
N.C.
N.C.
N.C.
N.D.
58+6
65+ 14
78+ 11
42+ 13
94+3
93+2
97 ± 3
99' ± 4
60+6
N.C.
109 ± 10
71 + 5
72+ 14
1
62+5
1
86+ 72
128 ± 77
108 ± 13
Before Cleanup
Low
96+5
19 + 14
56+4
69+2
94+7
N.D.
96+7
85+11
52+9
87 ± 15
85+2
94+5
94 ± 5
109 ± 1
103+ 1
105+ 1
120 ± 2
107 ± 1
124+ 6
94+6
78+2
76 ±40
1
N.D.
1
47 + 72
89 ± 8
85+2
High
100 ±
58 +
61 +
82 +
76 +
28 +
94 +
77 +
71 ±
91 ±
110±
86 +
77 +
102 ±
100 ±
103 +
123 ±
108 ±
777 ±
773 ±
71 ±
72 +
1
62 +
1
99 +
85 +
90 ±
2
1
1
15
2
16
3
7
0
3
6
5
3
1
1
1
1
2
2
2
2
3
5
2
3
2
After Cleanup
Low
N.C.
N.C.
N.C.
N.C.
N.C.
N.C.
N.C.
N.C.
58+4
67+6
N.D.
59+ 72
57+4
105 ± 3
104 ± 5
95+3
108+ 4
76 ±77
N.C.
74+3
76+4
123 ± 53
1
71 + 5
1
40 + 27
97 ± 14
41 + 11
High
N.C.
N.C.
N.C.
N.C.
N.C.
N.C.
N.C.
N.C.
68+3
74+3
62+4
79+3
54+8
97+3
95+2
94+4
106+ 3
65+ 17
N.C.
108+ 3
70+2
80+ 10
1
76+2
1
90 + 14
98 + 27
95 + 29
(alN.C. = No cleanup procedure included in this method.
N.D. = Not detected.
MI - Presence of interferences precluded determination of compound in sample.
ld>Standard deviation is included.
-------
Tina M. Engel, J. Scott Warner, and W. Marcus Cooke are with Battelle Columbus
Laboratories, Columbus, OH 43201.
Thomas A. Presshy is the EPA Project Officer (see below).
The complete report, entitled "Evaluation of 10 Pesticide Methods," (Order No. PB
85-238 608/AS; Cost: $14.50, subject to change) will be available only from:
National Technical Information Service
5285 Port Royal Road
Springfield, VA 22161
Telephone: 703-487-4650
The EPA Project Officer can be contacted at:
Environmental Monitoring and Support Laboratory
U.S. Environmental Protection Agency
Cincinnati, OH 45268
United States
Environmental Protection
Agency
Center for Environmental Research
Information
Cincinnati OH 45268
Official Business
Penalty for Private Use $300
EPA/600/S4-85/050
0000329 PS
AGENCY
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