United States
Environmental Protection
Agency
Environmental Monitoring and
Support Laboratory
Cincinnati, Ohio 45268
Research and Development
EPA-600/S4-84-061 Aug. 1984
Project Summary
EPA Method Study 18
Method 608 — Organochlorine
Pesticides and PCB's
John D. Millar, Richard E. Thomas, and Herbert J. Schattenberg
This report describes the results ob-
tained and data analyses from an inter-
laboratory study of EPA Method 608
(Organochlorine Pesticides and PCB's).
The method is designed to analyze for
16 single-compound pesticides, chlor-
dane, toxaphene, and seven Aroclor
formulations in water and wastewater.
All were included in this study except
endrin aldehyde, sufficient quantities of
which could not be obtained. As tested
here, the method utilizes three 60-mL
extractions with dichloromethane,
cleanup/separation on a Florisil co-
lumn, and;injection into a gas chroma-
tog rap h equipped with an electron cap-.
ture detector.
The study design required the analyst
to dose six waters with eight analytical
groups, each at six levels. The six dosing
levels of each substance or combination
represented three Youden pairs, one
each at a low, an intermediate, and a
high level. The six waters used were a
laboratory pure water, a finished
drinking water, and a surf ace. water,
collected by the participant, and three
low-background industrial effluents
(SIC's 2869, 2869 and 2621) provided
by the prime contractor. A total of 22
laboratories participated in the study.
The method is assessed quantitatively
with respect to the accuracy and preci-
sion that can be expected. In addition,
results of method detection limit
studies are included as are qualitative
assessments of the method based upon
comments; by the participating labora-
tories. ;
This Project Summary was developed
by EPA's \ Environmental Monitoring
and Support Laboratory, Cincinnati,
Ohio, to announce key findings of the
research project that is fully docu-
mented in a separate report of the same
title (see Project Report ordering
information at back).
Introduction
EPA first promulgated guidelines
establishing test; procedures for the
analysis of pollutants in 1973, following
the passage of the Federal Water Pollu-
tion Control Act in 1972 by Congress.
Pursuant to the amendment and publica-
tion of these guidelines, EPA entered
into a Settlement Agreement—the Con-
sent Decree—which required the study
and, if necessary, regulation of 65
"priority" pollutants and classes of
pollutants of known or suspected toxicity
to the biota. Subsequently, Congress
passed the Clean Water Act of 1977,
mandating the control of toxic pollutants
discharged into ambient waters by
industry.
In order to facilitate the implementation
of the Clean Water Act, EPA selected 129
specific toxic pollutants, 113 organic and
16 inorganic, for initial study. The organic
pollutants were divided into 12 categor-
ies based on their chemical structure.
Analytical methods were developed by
EPA for these 12 categories through in-
house and contracted research. These
analytical methods may eventually be
required for the monitoring of 113 toxic
pollutants in industrial wastewater
effluents, as specified by the Clean Water
Act of 1977.
As a logical subsequence to the work
that produced proposed EPA Method 608
(Organochlorine Pesticides and PCB's),
an interlaboratory study was conducted
-------
to determine the precision and accuracy
of the proposed method. This report
describes the work performed, presents
the data acquired, and gives the conclu-
sions drawn from the collaborative effort.
Of the 25 priority pollutants named in
Method 608,24 were tested in this study.
Endrin aldehyde, which is included in
Method 608, was eliminated from this
study because it could not be obtained in
sufficient quantity for the study, except
through a costly synthesis effort.
The objective of this interlaboratory
study was to obtain information about the
accuracy and precision associated with
measurements generated by Method
608. This objective was met through the
use of statistical analysis techniques
designed to extract and summarize the
relevant information about accuracy and
precision from the data reported by the
participating laboratories. The statistical
techniques employed in the data reduc-
tion process are similar to the techniques
suggested in the ASTM Standard Practice
D2777-77.
The algorithms required to perform the
statistical analyses have been integrated
into a system of computer programs
referred to as IMVS (Interlaboratory
Method Validation Study). The analyses
performed by IMVS include several tests
for the rejection of outliers (laboratories
and individual data points), summary
statistics by concentration level for mean
recovery (accuracy), overall and single-
analyst standard deviation (precision),
determination of the linear relationship
between mean recovery and concentra-
tion level, determination of the linear
relationship between the precision
statistics and mean recovery, and a test
for the effect of water type on accuracy
and precision.
Procedure
The study design was based on You-
den's original plan for collaborative
evaluation of precision and accuracy for
analytical methods. According to You-
den's design, samples are analyzed in
pairs where each sample of a pair has a
slightly different concentration of the
constituent. The analyst is directed to do a
single analysis and report on value for
each sample, as if for a normal, routine
sample.
In this study, samples were prepared as
concentrates in sealed glass ampules and
shipped to the analyst with portions of
final effluents from manufacturing plants
from three relevant industries. Each
participating laboratory was responsible
for supplying laboratory pure water, a
finished drinking water and a surface
water, thus giving a total of six water
matrices involved in the study. The
analyst was required to add an aliquot of
each concentrate to a volume of water
from each of the six waters and submit
the spiked water to analysis. Three pairs
of samples were used. One pair contained
the substances at what was considered to
be equivalent to a low level for the
industrial effluents; a second pair con-
tained the substances at an intermediate
level; and the third pair contained the
substances at a high level.
Before the formal study began, each
participant was sent a pair of ampules
(not one of the pairs used in the study) for
a trial analysis by Method 608. After
submitting data from these analyses to
SwRI, all participants met in Cincinnati to
discuss problems encountered during the
trial run.
Results and Discussion
The accuracy of the method could
generally be expressed as a linear
function of the true concentration. The
regression equations are shown in Table
1.
The precision of the method could
generally be expressed as a linear
function of the mean recovery. These
regression equations are also shown in
Table 1.
Recoveries at the midrange concentra-
tion were similar to those obtained during
the developmental phase in many instan-
ces and lower in others, indicating
satisfactory method performance. The
recoveries ranged from 68 to 101% for
single-compound pesticides, 73 to 86%
for multiple-compound pesticides, and 69
to 101% for the PCB formulations in the
first five matrices. Lower recoveries were
obtained in the third industrial effluent
due to emulsion formation. Eighty-six
percent of the recoveries among the first
five matrices exceeded 80% and 12.5
exceeded 90%.
At the midrange concentration, overall
percent relative standard deviations of 12
to 45, 19 to 36, and 14 to 40% were
obtained for the three above groupings of
compounds among the first five matrices.
The single-analyst percent relative
standard deviations were from 11 to 33,
10 to 31, and 12 to 28%, respectively,
under the same conditions. Poorer
precision values were obtained for
industrial effluent 3, as expected, due to
the nature of the effluent.
Six water types were used in this study:
laboratory pure, finished drinking, sur-
face and three industrial effluents. The
only significant difference among the
results obtained was in the recovery of
the substances from the third industrial
effluent. This effluent gave a large
emulsion on extraction that resulted in
lowered extraction efficiency. With one
exception, there was no detectable
difference in precision among the results
from the six waters studied.
The principal problem area noted by
the participants was related to the
concentration of extracts with the
Kuderna-Danish apparatus.
Conclusions and
Recommendations
The participating laboratories in this
study were able to obtain results with
Method 608 that were comparable: to
those obtained during the single-labora-
tory evaluations conducted after method
development. The accuracy and precision
statements presented earlier apply only
to the range of concentrations studied
and should not be extrapolated beyond
those limits.
-------
Table 1 . Accuracy and Precision Equations
Water tvn* Aldrin
Range. ug/L
Laboratory Pure
Accuracy
Precision
Overall
Single analyst
Finished Drinking
Accuracy
Precision
Overall
Single analyst
Surface
Accuracy
Precision
Overall
Single analyst
Ind. Effluent J
Accuracy
Precision
Overall
Single analyst
Ind. Effluent 2
Accuracy
Precision
Overall
Single Analyst
Ind. Effluent 3
Accuracy
Precision
Overall
Single analyst
Table 1 . (Continued)
Water type
Range. ug/L
Laboratory Pure
Accuracy
Precision
Overall
Single analyst
Finished Drinking
Accuracy
Precision
Overall
Single analyst
Surface
Accuracy
Precision
Overall
Single analyst
Ind. Effluent 1
Accuracy
Precision
Overall
Single analyst
Ind. Effluent 2
Accuracy
Precision
Overall
Single analyst
Ind. Effluent 3
Accuracy
Precision
Overall
Single analyst
0.9444-5.60
X = 0.81 c + 0.04
S = O.20X - 0.01
SR = 0. 16X - 0.04
X = 0.81 c + 0.04
S = 0.1 8X + 0.11
SR = 0.09X + 0. 13
X = 0.82c + O.O5
S = 0.15X + 0.14
SR = 0.11X + 0. 10
X = 0.76c + O.O6
S = 0.22X 4- O.O3
SR = 0. 14X + 0.06
X =0.75c-0.03
S = 0.28X
SR = 0.24X - 0.07
X = 0.34c - 0.07
S = 0.63X + 0.02
SR = 0.37X + 0.01
4. 4' -DDE
1.31-9.84
X =0.85c + 0.14
S = 0.28X - 0.09
SR = 0. 13X + 0.06
X = 0.81 c + 0.17
S = O.2OX + O.O7
SR = 0. 10X + 0.23
X =0.84c + 0.10
S = 0.22X - 0.07
SR = 0.1 3X + 0.01
X =0.89c + 0.05
S = 0.23X - 0.09
SR = 0.23X - O.O8
X =0.74c + 0.11
S = 0.23X
SR = 0. 19X + 0. 12
X =0.52c-O.13
S = O.46X + 0.08
SR = 0.25X + 0. 12
alpha- '
BHC ,
0.470-3.96
X = 0.84c+0.03
S - 0.23X
SR=O.J3X + 0.04
X = 0.83C + 0.06
S = 0.21X
SR = O.O9X + 0.06
X = O.83C + 0.05
S = 0.21 X + 0.01
SR = 0.20X - 0.02
X =0.78c + 0.17
S = 0.28X + O.O5
SR = 0.25X
X = 0.83c + 6.04
S = 0.19X + 0.01
SR = 0. 14X + 6.O3
'
X = 0.63c,
S = 0.31X + 0.02
SR=0.11X + 0.07
4.4--DDT
3.64-22.2.
X = 0.93c - 6. 13
S = O.31X-O.21
SR =0.17X^0.39
X = 0.89c + 0,31
S =0.32X-0.01
SR = 0.1 3X + 0.73
X = 0.95c - 0.09
S = 0.29X - 6.34
SR = 0. 15X + 0. 13
X = 0.92c + 0,04
S = 0.28X -0.11
SR = 0.26X -0.11
X = 0.76c + 6.04
S = 0.2SX + 6. 16
SR = 0. 13X + 0,47
X = 0.55c - 0.64
S = 0.55X + 6, 16
SR = 0.28X + 0.29
beta-
BHC
0.864-9. 15
X = 0.81 c + 0.07
S -0.33X-O.OS
SR = 0.22X - O.02
X =0.85c + 0.17
S = 0.27X - 0.01
SR = O.09X + 0.22
X = O.SJc + 0. 12
S = 0.27X - 0.04
SR = 0.17X
X =0.79c + 0.'15
S = 0.25X - 0.03
SR = 0.17X + 0.01
X = O.SSc - 0.06
S = 0.27X
SR = 0.17X + O.01
X =0.66c
S = 0.26X - 0.01
SR = 0. 1 1X + 0. 12
Dieldrin
1.32-12.3
X = 0.90c + 0.02
S =0. 16X + 0. 16
SR = 0. 12X + 0. 19
X = 0.89c - 0.08
S =0. 15X + 0.24
SR = 0. 13X + 0. 14
X = O.SSc + O.01
S = 0.26X - 0.03-
SR = 0.24X - 0. 14
X = O.86c + 0. 12
S =0. 15X + 0.06
SR = 0. 18X - 0. 10
X = 0.90c - O.O8
S = 0. 13X + 0. 16
SR = 0. 12X + 0. 15
X = O.SSc
S = O.39X + 0.03
SR = 0.27X - 0.03
gamma-
BHC
0.476-3.34
X = 0.82c - 0.05
S = 0.22X + 0.04
SR = 0. 12X + 0.06
X =0.79c-0.02
S = 0.1 9X + 0,08
SR = O.08X + 0. 13
X = O.83c - O.O3
S = 0.1 5X + 0.09
SR = 0.04X + 0. 15
X = 0.81 c + 0.04
S = 0.05X + 0. 15
SR = 0.07X + 0. 1O
X = 0.83c - 0.07
S =0. 13X + 0.06
SR = O.O6X + O.O7
X = 0.63c - 0.03
S = 0.28X + 0.03
SR = 0. 19X + 0.05
Endosulfan
1
1.26-13.4
X = 0.97c + O.O4
S =0. 18X + 0.08
SR = 0. 10X + 0.07
X = O.90c + 0.02
S =0. 16X
SR = 0. 14X - O.O6
X = 0.90c + 0.38
S = 0.23X + 0. 18
SR = 0. 15X
X = 0.93c + 0.72
S =O. 12X + 0.02
SR = 0. 12X - O.O2
X = 0.89c - 0.01
S =0. 18X + 0.04
SR = 0.11X + 0.07
X = 0.57c + 0.05
S = 0.46X + 0.06
SR = 0. 16X + 0.30
sigma-
BHC
0.944-5.76
t
X = 0.81 c + 0.07
r
S = 0.25X + 0.03
SR = 0.18'X + O.09
1
X = 0.81 c + 0.03
S =O.32X-0.05
SR = 0. 14X + 0.09
\
X = 0.82c + 0.01
S = 0.31 X + 0.04
SR - 0. 16X + 0.11
X =0.75c + 0.08
S = 0.35.X - 0.03
SR = 0.20X + 0.05
X = O.SSc -0.01
S = 0.25X + 0.03
SR = 0.1 5X + 0.10
X = O.SSc - 0.03
i
S = 0.31 X + 0.09
SR = 0.22X + 0.06
Endosulfan
II
2.27-14.0
X = 0.93c + 0.34
S = 0.47X - 0.20
SR = 0.41 X - 0.65
X = O.SSc + 0. 1O
S = 0.28X + 0.37
SR = O.17X + O.3O
X = O.SSc + 0.03
S =0.24* +0.23
SR = 0.23X + 0.11
X = 0.97c + 0.32
S = 0.39* - 0.03
SR - 0.05X + 0.94
X = 0.84c + 0.45
S = 0.24X + O.61
SR = 0.02X + 0.94
X = O.SSc + 0. 16
S =0.69X-0.22
SR = 0. 14X + 0.26
4.4'-DDD
2.46-22.3
X = 0.84c + 0.30
S = 0.27X + 0. 14
SR = 0.20X - 0. 18
X = O.SSc + 0.32
S = 0.24X - 0. 16
SR = 0. 13X + 0. 14
X = O.SSc + 0.09
S = 0.22X - 0.05
SR = 0. 14X + 0.32
X = O.SSc + 0.06
S = O.22X - O.OS
SR = O.20X + 0.01
X =0.83c + 0.26
S =0.18X + 0. 13
SR = O.06X + O.56
X = O.SSc -0.1 3
S = 0.42X + 0. 13
SR = 0.23X + 0.24
Endosulfan
sulfate
3.86-29.7
.
X = O.SSc - 0.37
S =0.24X + 0.35
SR = 0. 13X + 0.33
X =0.87c + 0.11
S = 0.26X + 0.02
SR = 0. 15X + O.06
•-
X = 0.87c - 0.57
S =0.22X + 0.19
SR = 0. 1 1X + O.39
X =O.91c-0.46
S = 0.39X + 0.2S
SR = 0.24X + 1.04
X = 0.81 c- 0.17
S =0.32X-0.14
SR = 0.27X -0.16
X = O.SOc + 0.39
S = 0.36X + 0.42
SR = 0.1 8X + 0.31
3
-------
T* bit 1. (Continued)
Water type —
Range, ug/L
Laboratory Pure
Accuracy
Precision
Overall
Single analyst
Finished Drinking
Accuracy
Precision
Overall
Single analyst
Surface
Accuracy
Precision
Overall
Single analyst
Ind. Effluent 1
Accuracy
Precision
Overall
Single analyst
Ind. Effluent 2
Accuracy
Precision
Overall
Single Analyst
Ind. Effluent 3
Accuracy
Precision
Overall
Single analyst
Table 1. (Continued!
Water type
Range, ug/L
Laboratory Pure
Accuracy
Precision
Overall
Single Analyst
Finished Drinking
Accuracy
Precision
Overall
Single analyst
Surface
Accuracy
Precision
Overall
Single analyst
Ind. Effluent 1
Accuracy
Precision
Overall
Single analyst
Ind. Effluent 2
Accuracy
Precision
Overall
Single Analyst
Ind, Effluent 3
Accuracy
Precision
Overall
Single analyst
c - true concentration
X • mean concentration
Endrin
2.15-22.6
X =0.890-0.04
S =0.24X + 0.25
X =0.86c + 0.31
S =0.21X + 0.12
SR = 0.17X + 0.17
X =0.89c + 0.45
S = 0.31 X + 0.33
SR = 0.27X + 0.21
X =0.970 + 0.15
S = O.32X + 0.03
SR = 0.24X + 0.31
X = 0.94c
S =O.28X-0.01
SR = 0.23X-0.18
X =0.550 + 0.13
S =0.49X
SR = 0.29X + 0.04
Aroclor 1221
23.9-191
X =0.960 + 0.65
S =0.35X-0.62
SR=O.29X-0.76
X = 0.84c + 7.56
S =0.37X-0.95
SR = 0.31 X- 2.70
X =O.84c + 2.37
S =0.40X-0.18
SR = 0.22X + 3.93
X =0.84c + 6.78
S =O.19X + 9.76
SR = 0.07X + 9.70
X =0.76c + 4.92
S =0.37X-0.39
SR = 0.24X + 2.57
X =0.580 + 0.71
S = 0.57X - 1.78
SR = 0.45X - 1.80
Heptachlor
0.446-3.22
X =0.69c + 0.04
S = 0.1 6X + 0.08
SR = 0.06X + 0.13
X = 0.79c - 0.02
S = 0.24X + 0.06
SR = 0.14X + 0.07
X =0.750 + 0.02
S = 0.24X + 0.04
SR = 0.1 6X + 0.03
X =0.66c + 0.03 '
S = 0.21 X + 0.08
SR = 0.1 4X + 0.08
X =0.580 + 0.08
S =O.3OX + 0.11
SR = 0.22X + 0.07
X =0.280-0.01
S = 0.93X - 0.03
SR = 0.57X + 0.02
Aroclor 1232
24.8-185
X =0.910 + 10.79
S = 0.31 X + 3.50
SR = 0.21X - 1.93
X =0.910 + 2.06
S = 0.42X - 3.01
SR = 0.29X - 2.71
X =0.990 + 2.27
S = 0.35X - 1.50
SR = 0.25X - 1.92
X =0.880 + 7.65
S = 0.35X - 1.27
SR = 0.30X - 5.27
X = 0.91c + 1.94
S =0.44X-5.16
SR = 0.25X - 2.45
X =0.570-0.03
S = 0.52X - 0. 19
SR = 0.26X - 2.09
4
Heptachlor
epoxide
0.872-6.62
X =0.89c + 0.10
S = 0.25X - 0.08
SR=0.18X-0.11
X =0.830 + 0.09
S = 0.24X-0.05
SR = 0.1 4X + 0.07
X =0.84c + 0.11
S = 0.20X + 0.01
SR = 0.1 2X + 0.02
X =0.830 + 0.11
S = 0.1 9X- 0.04
SR = 0.1 5X + 0.01
X =0.87c + 0.08
S = 0.1 8X + 0.03
SR = 0.1 5X + 0.08
X = 0.54c
S =0.33X + 0.10
SR = 0.18X + 0.14
Aroclor 1242
13.0-106
X =0.930 + 0.70
S = 0.21 X + 1.52
SR = 0.11X+ 1.40
X = 1.00c - 1.09
S = 0.22X + 0.05
SR = 0.11X+ 1.20
X =O.93c + O.31
S = 0.28X + 0.55
SR = 0.1 4X + 0.57
X = 0.990 + 0.89
S = 0.22X + 1.87
SR = 0.04X + 2.54
X =0.900 + 0.43
S =0.17X+1.83
SR = 0.09X + 1.65
X =0.53c + 0.30
S = O.33X + 1.92
SR = 0.1 3X + 2.36
Chlordane
8.49-53.0
X = 0.82c - 0.04
S =0.18X + 0.18
SR = 0.13X + 0.13
X =0.790-0.37
S = 0.27X + 0.22
SR = 0.17X + 0.42
X =0.820-0.61
S =0.18X + 0.18
SR = 0.11X + 0.19
X = 0.82c - 0.43
S = 0.40X - 1. 14
SR = 0.28X - 0.85
X =0.740 + 0.13
S =0.27X-0.66
SR = 0.1 7X- 0.48
X =0.340-0.20
S = 0.42X + 0.23
SR = 0.34X - 0.20
Aroclor 1248
16.4-154
X = 0.97c + 1.06
S = 0.25X - 0.37
SR = 0.17X + 0.41
X = 0.90c + 1.96
S = 0.20X + 3.66
SR = 0. 12X + 4.58
X = 0.86o. + 1.72
S =0.22X-0.37
SR = 0. 10X + 1.80
X =0.910 + 0.85
S =0. 18X + 1.22
SR = 0.11X+ 1.78
X =0.82c + 3.72
S = 0.22X + 4.09
SR = 0.05X + 5.60
X = 0.52c + 0. 19
S = 0.49X + 0.30
SR = 0.35X - 0.26
Toxaphene
47.0-403
X =0.800 + 1.74
S = 0.20X +. 0.22
SR = 0.09X + 3.20
X =0.840 + 0.72
S = 0.20X + 1.55
SR = 0.1 OX + 3.96
X =0.790 + 2.03
S = 0.24X - 0.30
SR = 0.2OX - 0.53
X = O.SOc - 0.44
S = 0.21 X + 2.34
SR = 0.15X - 1.92
X =0.710 + 4.74
S = O.21X + 7.45
SR = 0.15X* 1.92
X =0.420 + 2.27
S = 0.44X + 0.43
SR = 0.23X + 3.04
Aroclor 1254
17.4-W8
X =0.760+2.07
S = 0.17X + 3.62
SR = 0.15X]+ 1.66
X = 0.83c + 1.28
S =0.77X!+2.04
SR = 0.1 3X\+ 0.87
X =0.770+1.81
S = 0.17X.+ 3.12
SR = 0. 12X + 0.51
X =0.880-1.41
S = 0.1 9X + 0.52
SR = 0.1OX,+ 1.66
X =0.750-1.74
S = 0.23X - 0.44
SR = 0.17X- 1.04
X = 0.48c - 0.26
S = 0.38X^1.12
SR = 0.22X + 1.85
Arocior 1016
10.2-88.3
X =0.81c + 0.50
S =0. 15X + 0.45
SR = 0. 13X + 0. 15
X = 0.870 - 0.39
S =0. 15X + 0. 18
SR = 0.1 OX + 0.77
X =0.800 + 0.90
S = 0.14X + 0.98
SR = 0.10X + O.77
X =0.8tc + 0.99
S =0.11X+1.69
SR = 0.1 2X + 0.43
X =0.750+1.10
S =0. 19X + O.28
SR = 0.20X -0.17
X =0.500 + 0.78
S = 0.48X - 0.40
SR = 0.36X - 0.94
Aroclor 126O
36.8-254
X =0.660 + 3.76
S = 0.3SX - 4.S6
SR = 0.22X - 2.37
X =0.780 + 3.87
S = 0.34X - 2.36
SR = 0.20X -2\12
X = 0.84c + 3, 1O
S = 0.27X-0.74
SR = 0.15X + 0.10
X =0.790 + 3.27
S =0.25X + 2.53
SR = 0. 1 1X + 2.50
X =0.800-1.84
S =0.33X-2.71
SR = 0.14X + 0.14
X = 0.56c - 0.24
S =0.44X + 0.70
SR = 0. 16X + 5.01
*OSGPO: ! 1984-759-102-10643
i 1
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i
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John D. Millar, Richard E. Thomas, and Herbert J. Schattenberg are with
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Robert L Graves and Edward L. Berg are the EPA Project Officers (see below).
The complete report, entitled "EPA Method Study 18, Method 608—Organo-
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subject to change) will be available only from:
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