United States
Environmental Protection
Agency
Environmental Monitoring
Systems Laboratory
Las Vegas, NV 89193-3478
Research and Development
EPA/600/S4-90/015 Sept. 1990
EPA Project Summary
Analysis of Solid Waste-
Performance Data for
SW-846 Methods
8270, 8081, and 81 41
Paul Marsden
The U.S. Environmental Protection
Agency (U.S. EPA) has developed a Best
Demonstrated Available Technology
(BOAT) list of specific chemicals to be
monitored in treated wastes before land
disposal. Reliable measurement of these
chemicals in wastes is a measurement
issue facing the Office of Solid Waste
and the Office of Research and Devel-
opment. This report provides data for
the precision and accuracy of recoveries
of BDAT chemicals from fly ash, sewage
sludge, and a petroleum still bottom.
Three SW-846 analytical methods
(8270 [semi-volatile organics], 8081 [or-
ganochlorine pesticides], and 8141 [or-
ganophosphorus insecticides]) can be
used in conjunction with extraction
procedures (Methods 3540 or 3550) and
sample clean-up (Methods 3640 and
draft-3670) to measure almost all of the
BDAT list chemicals in waste matrices.
Surrogates added at the time of sample
extraction provide a reliable measure of
method performance for measuring
analytes with similar chemical proper-
ties.
Analyte recoveries of 40-70 percent
were obtained for most analytes from fly
ash, sewage sludge, and petroleum still
bottom using Method 8270 (Table 1).
Strongly polar chemicals (2-picoline
[20-60 percent], phenol [20-60 percent],
the nitroso compounds [20-80 percent])
presented greater difficulties than most
neutral species. Several analytes are not
measured using Method 8270: toluene
di-isocyanate, the four diaminotoluene
isomers (2,4-, 2,3-, 2,6-, and 3,4-), and all
methylcyclohexylamine isomers. Ortho-
andpara-toluidine were not resolved and
must be measured as the sum of both
compounds. The high level of
co-extracted interferences in these ma-
trices caused quantitation problems in
the analysis of organochlorine pesti-
cides; a number of recoveries were >100
percent (Table 2). The spiking levels of
the organophosphorus pesticides were
relatively high, recoveries were
75-95 percent (Table 3).
It is clear that It may be difficult to
achieve BDAT target detection limits in
complex matrices without additional
cleanup of waste extracts.
This Project Summary was developed
by U.S. EPA's En vironmentalMonitoring
Systems Laboratory, Las Vegas, NV, to
announce key findings of the research
project that is fully documented in a
separate report of the same title (see
Project Report ordering information at
back).
-------
Sludge Sonication Soxhlet
Average Std Average Std
Surrogates
Z-Fluoropbanol
DS-Phenol
DS-Nitrobcnzene
2-FkJorobiphenyl
2,4,6-Tribromophenol
D14-Torphenyl
Analytos
N-Nitrosocffmothylamine
2-P'Kolins
S-Mothylcyclohexylamine
S-MolhylcyctohoxanonB
Phenol
Bis(2-CMoro!sopropyl)ether
Hoxachloroethane
o-Toltildina
Di-n-propylnitrosamine
Nitrobenzene
Toluene d<-lsocyanate
HexachtorobutadfenB
o-Nitrotoluone
m-Nitrotoluene
p-Nitrotoluene
2,3-DiaminotoluBna
2,6-Dlaminotoluene
Hsxachlorocyclopentadiene
2-Cbloronaphthalene
2,6-Dlnitrotoluene
2,4-Dinitrotoluene
1,2-Dlphonylbydrazine
4-Bromophonylphenylether
A-BHC
B-BHC
G-BHC
D-BHC
Pronamida
Hoptachlor
Atdrin
Hoptachlor epoxide
Endosulfan 1
Gamma-chhrdane
Alpha-chtordana
DDE
Dleldfln
Endrin
Endosulfan II
ODD
DDT
29
33
46
54
75
73
32
23
0
44
34
56
54
59
50
55
0
62
42
65
68
0
0
44
54
69
63
55
89
83
93
77
84
72
69
37
71
75
68
62
74
68
88
78
117
70
15
13
12
11
23
13
31
9
0
10
13
15
15
13
2
14
18
10
14
17
-
-
9
14
14
15
12
24
19
25
20
23
15
9
5
15
11
9
9
21
15
19
16
43
14
54
54
56
69
74
77
59
63
0
78
57
71
85
87
72
67
0
87
55
94
96
0
0
19
72
79
68
64
106
97
112
96
100
83
73
27
102
96
69
59
89
92
121
-102
97
70
1
2
5
3
11
6
51
6
0
2
2
6
9
6
- 9
4
4
1
4
2
-
-
4
9
4
2
5
10
9
12
9
9
5
3
8
10
8
7
6
9
4
17
11
52
24
Still Bottom Sonication Soxhlet
Average Std Average Std
46
41
50
56
37
86
37
50
0
60
38
65
58
25
62
64
0
65
45
70
69
0
0
11
51
62
49
51
78
70
75
62
58
70
63
44
58
63
54
44
48
53
71
59-
52
34
2
2
2
12
7
4
33
6
0
8
3
6
2
11
8
4
2
4
2
2
-
-
5
5
8
4
2
3
3
4
6
5
5
7
4
5
6
7
6
8
6
13
—-.....9 - -_- .
9
10
28
27
42
38
37
50
39
34
0
49
24
47
46
0
40
53
0
69
36
50
53
0
0
0
25
37
30
45
87
75
90
72
76
48
37
39
59
58
40
32
49
57
71
64
76
16
9
8
13
9
7
11
11
11
0
18
8
12
12
0
*~-1-1-~.
17
20
11
11
14
-
-
18
10
10
11
16
16
25
17
20
12
8
11
19
13
7
7
13
20
11
16
23
6
Fly Ash Sonication Soxhlet
Average Std Average Std
28
33
49
59
7
90
20
33
0
59
33
64
68
60
72.-
62
0
80
51
80
85
0
5
60
70
83
71
63
108
94
118
90
99
91
93
71
85
76
71
68
91
84
95
79
150
109
17
14
11
8
4
1
35
25
0
19
14
16
11
8
- 27
15
18
8
12
14
-
8
9
16
8
7
8
11
11
10
9
9
14
16
13
14
6
6
5
7
18
7
7
22
15
49
52
64
67
78
79
80
45
0
76
49
77
86
95
75
79
0
91
60
94
96
11
46
53
75
86
79
73
124
107
134
108
116
92
95
86
102
85
70
68
97
94
114
_,.- -~gy.~.
173
117
4
3
4
3
3
5
22
7
0
7
2
2
6
11
6 •
7
5
4
5
6
19
43
10
4
j
1
4
2
3
2
2
3
4
2
1
1
1
1
1
1
5
3
1
_. 3
15
5
-------
Table 2. Percent Recoveries of Organochlorine Pesticides
Sludge Sonication Soxhlet
A verage Std A verage Std
Surrogates
Tetra-cl-m-xylene
Decachlorobiphenyl
Analytes
Hexachloroethane
2-Chloronaphthalene
4-Br-diphenyIether
A-BHC
G-BHC
Heptachlor
Aldrin
B-BHC
D-BHC
Hept. epoxide
Endosulfan 1
G-Chhrdane
A-Chlordane
DDE
Dieldrin
Endrin
Endosulfan II
DDT
Endrin aldehyde
ODD
71
26
80
50
118
88
55
60
92
351
51
54
52
50
49
52
89
56
52
57
45
57
19
23
7
56
14
25
9
13
33
71
11
11
11
9
8
11
19
10
10
10
6
11
82
28
79
67
0
265
155
469
875
150
57
70
70
65
66
74
327
92
88
95
42
99
1
48
1
8
-
18
29
294
734
260
2
3
4
1
0
1
7
15
11
17
10
8
Still Bottom Sonication Soxhlet
Average Std Average Std
49
17
70
59
159
55
43
48
48
51
43
47
47
48
45
45
45
50
49
49
40
48
2
29
2
3
19
7
6
6
5
7
4
6
4
5
5
4
5
6
5
4
4
5
176
104
50
35
128
47
30
55
200
75
119
66
41
47
37
70
58
41
46
40
29
35
211
93
30
35
137
25
30
18
258
42
129
34
18
13
21
40
24
23
17
29
20
21
Fly Ash Sonication Soxhlet
Average Std Average Std
119
49
81
48
37
45
47
53
49
62
49
53
52
53
53
51
52
55
54
56
50
54
12
2
3
3
64
3
3
2
3
3
3
2
3
3
3
3
3
2
2
3
2
3
57
57
54
39
118
38
41
46
46
58
43
51
52
52
53
53
50
36
56
57
47
55
41
11
39
36
70
24
23
26
22
23
20
17
15
16
15
14
16
35
12
16
19
13
Table 3. Percent Recoveries of Organophosphorous Pesticides
Sludge Sonication Soxhlet
A verage Std A verage Std
Surrogates
Ethion
Analytes
Dichlorvos
Ethoprop
Phorate
Diazinon
Ethyl parathion
Tetrachlorvinphos
Bolstar
Fensulfothion
Methyl Azinophos
Coumaphos
78
74
76
74
79
78
62
77
82
82
81
4
4
4
5
4
4
27
4
5
8
3
85
93
88
83
85
87
74
88
136
72
83
4
10
4
1
4
<1
4
2
51
9
7
Still Bottom Sonication Soxhlet
A verage Std A verage Std
78
84
85
81
85
84
75
81
87
72
83
4
4
4
3
4
4
8
5
-------
PaulMarsden (also the U.S. EPA Project Officer, see below) is with the Environmental
Monitoring Systems Laboratory, Las Vegas, NV.
The complete report, entitled "Analysis of Solid Waste—Performance Data for SW-846
Methods 8270, 8081, and 8141" (Order No. PB 90-251 844: Cost $23.00, 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 Systems Laboratory
U. S. Environmental Protection Agency
Las Vegas, NV 89193-3478
United States
Environmental Protection
Agency
Center for Environmental Research
Information
Cincinnati, OH 45268
Official Business
Penalty for Private Use $300
EPA/600/S4-90/015
------- |