PB 84-2 11614
EPA-600/4-84-063
June 1984
EPA METHOD STUDY 20,
METHOD 610PNA's
by
Glenn Kinzer, Ralph Riggin, Thomas Bishop,
Michelle A. Birts and Paul Strup
BATTELLE
Columbus Laboratories
505 King Avenue
Columbus, Ohio 43201
EPA Contract So. 68-03-2624
Project Officers
Edward L. Berg and Robert L. Graves
Quality Assurance Branch
Environmental Monitoring and Support Laboratory
Cincinnati, Ohio 45268
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
-------
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1. REPORT NO. 2.
EPA-600/4-84-063
3. RECIPIENT'S ACCESSION NO.
pm ^ 2 11614
4. TITLE AND SUBTITLE
EPA METHOD STUDY 20, METHOD 610--PNA's
S. REPORT DATE
June 1984
fi. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
Glenn Kinzer, Ralph Riggin, Thomas Bishop,
Michelle A. Blrts, and Paul Strup
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING organization name and address
Battelle Columbus Laboratories
505 King Avenue
Columbus, Ohio 43201-2693
10. PROGRAM ELEMENT NO.
CBSDIA, BEBIC
11. CONTRACT/(ShANT NO.
68-03-2624
12. sponsoring agency name and address
Quality Assurance Branch
Environmental Monitoring and Support Laboratory
Cincinnati, Ohio 45268
13. TYPE OF REPORT AND PERIOD COVERED
Final; 9/20/78-10/31/84
14. SPONSORING AGENCY CODE
EPA/600/06
IB. supplementary notes
16. ABSTRACT
Sixteen laboratories participated in an interlaboratory study conducted to provide
precision and accuracy statements for the proposed EPA Method 610 for 16 selected poly
nuclear aromatic hydrocarbons(PNA's) which may be present in municipal and industrial
aqueous discharges. Method 610 involves extraction of the pollutants with methylene
chloride and subsequent analysis of the subject compounds by high performance liquid
chromatography utilizing fluorescence and ultraviolet detection of the PNA's.
The study design was based on Youden's plan for collaborative tests of analytical
methods. Three Youden pair samples of the test compounds were spiked into six types o
test waters and then analyzed. The resulting data were statistically analyzed using
the computer program entitled "Interlaboratory Method Validation Study" (IMVS). Mean
recoveries of the PNA's were in the range of 41-100 percent. Overall precision was in
the range of 23-91 percent and single-analyst precision was in the range of 11-48
percent.
A statistically significant effect due to water type was established for six of
the sixteen PNA compounds for which recoveries from distilled water were generally
lower than from wastewaters. The effect was judged to be due to the analytical learn-
ing process and, therefore, of no practical importance. For the other 10 PNA's, there
were no differences of practical significance due to water types among mean recoveries
overall precisions, or single-analyst precisions,
17. KEY WORDS AND DOCUMENT ANALYSIS
a- DESCRIPTORS
b.IDENTIFIERS/OPEN ENDED TERMS
c. COSATi Field/Croup
18. DISTRIBUTION STATEMENT
19. SECURITY CLASS f
20. SECURITY CLASS ,
tPA Pwm 2320-1 (R»». 4-77) previous edition ¦ oiioliti
i
-------
DISCLAIMER
The information in this document has been funded wholly or in part
by the United States Environmental Protection Agency under Contract No. 68-
03-2624 to Battelle's Columbus Laboratories. It has been subject to the
Agency's peer and administrative review, and it has been approved for
publication as an EPA document. Mention of trade names or commercial
products does not constitute endorsement or recommendation for use.
ii
-------
FOREWORD
Environmental measurements are required to determine the quality of
ambient waters and the character of waste effluents. The Environmental
Monitoring and Support Laboratory (EMSL)-Cincinnati conducts research to:
Develop and evaluate techniques to measure the presence and
concentration of physical, chemical, and radiological
pollutants in water, wastewater, bottom sediments, and
solid waste.
Investigate methods for the concentration, recovery, and
identification of viruses, bacteria, and other micro-
organisms in water.
Determine the responses of aquatic organisms to water
quality.
Support an Agency-wide quality assurance program to assure
standardization and quality control of systems for
monitoring waste and wastewater.
This publication reports the results of EPA's interlaboratory
method study for the following priority pollutants:
Naphthalene (91-10-3)*
Acenaphthylene (203-96-8)
Benzo(a)anthracene (56-55-3)
Chrysene (218-01-9)
Phenanthrene (85-01-8)
Anthracene (120-12-7)
Fluoranthene (146-44-0)
Pyrene (129-00-0)
Acenaphthene (83-32-9)
Fluorene (86-73-7)
Benzo(b)fluoranthene (205-99-2)
Benzo(k)fluoranthene (207-08-9)
Benzo(a)pyrene (50-32-8)
Dibenzo(a,h)anthracene (53-70-3)
Benzo(g,h,i)perylere (191-24-2)
Indeno(l,2,3-cd)pyrene (193-39-5)
iii
-------
Federal agencies, states, municipalities, universities, private
laboratories, and industry should find this evaluative study of assistance in
monitoring and controlling pollution in the environment.
Robert L. Booth
__________________ Acting Director, EMSL-Cincinnati
*CAS Registry Number
iv
-------
ABSTRACT
The U.S. Environmental Protection Agency (USEPA) sponsored an
interlaboratory study conducted to provide precision and accuracy statements
for the proposed USEPA Method 610 for the 16 selected polynuclear aromatic
hydrocarbons (PNA's) comprising Category 9 of the priority pollutants which
may be present in municipal and industrial aqueous discharges. Method 610
involves extraction of the pollutants with methylene chloride followed by
silica gel cleanup and subsequent analysis by high performance liquid
chromatography (HPLC) utilizing fluorescence and ultraviolet detection (UV).
The study design was based on Youden's plan for collaborative tests of
analytical methods. Three Youden pair ampules of the test compounds were
spiked into six types of test waters and analyzed. The test waters were
distilled water, tap water, a surface water, and three different industrial
wastewater effluents. The resulting data were analyzed statistically using
the USEPA computer program entitled "Interlaboratory Method Validation Study"
(IMVS). Mean recoveries of the PNA's based upon inserting specific analyte
concentrations into the regression equations ranged from 43-110 percent.
Overall precision ranged from 16-91 percent and single-analyst precision
ranged from 11-50 percent.
The study was conducted at the request of the Environmental Protection
Agency, Quality Assurance Branch, EMSL - Cincinnati, Ohio under EPA Contract
No. 68-03-2624. This report covers a period from September 13, 1978 to
October 31, 1983, and work was completed as of December 31, 1982.
v
-------
CONTENTS
Page
Disclaimer ii
Foreword iii
Abstract v
Figures vii
Tables vii
Acknowledgement ix
1. Introduction 1
2. Summary 3
3. Description of Study 10
Selection of Participating Laboratories 10
Test Design 11
4. Experimental Procedures 13
Preparation of Youden Pair Concentrates . 13
Stability of Youden Pair Concentrates 13
Collection of Industrial Wastewater Effluents 14
Distribution of Samples 17
Treatment of Data 18
Rejection of Outliers 18
Youden's Laboratory Ranking Procedures 19
Individual Outliers 20
Statistical Summaries Data 20
Statement of Method Accuracy. . 22
Statement of Method Precision 24
Comparison of Accuracy and Precision Across
Water Types 25
5. Results and Discussions 31
Statistical Summaries . 31
Regression Equations 31
Effects of Water Type 31
General Discussion of Method Performance 49
Accuracy of the Method 54
Precision of the Method 55
Operational Problems 55
References 57
Appendices
A. Method 610 58
B. Instructions to Analyst 71
C. Saw Data . 74
D. Effect of Water Types on PNA Analyses 122
vi
-------
CONTENTS (Continued)
FIGURES
Page
A-l HPLC-Fluorescence of PNAs on reverse phase column, HC-ODS
Sil-X, 250 mm x 2.6 mm ID
70
TABLES
Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
Statistical
Statistical
Regression Equations for Accuracy and Precision of
Method 610 by Compound and Water Type
Calculated Concentrations of Category 9 Compounds in
Ampules, ug/mL
Background Analyses of Wastewater Samples for
Category 9 Compounds, yg/L
Statistical Summary for Naphthalene Analyses by Water Type.
Statistical Summary for Acenaphthylene Analyses by
Water Type
Statistical Summary of Acen&phthene Analysis by Water Type.
Statistical Summary of Fluorene Analyses by Water Type. . .
Summary of Phenanthrene Analyses by Water Type.
Summary of Anthracene Analyses by Water Type. .
Statistical Summary of Fluoranthene Analyses by Water Type.
Statistical Summary of Pyrene Analyses by Water Type. . . .
Statistical Summary of Benzo(a)anthracene Analyses by
Water Type
Statistical Summary of Chrysene Analyses by Water Type. . .
Statistical Summary of Benzo(b)fluoranthene Analyses by
Water Type
Statistical Summary of Benzo(k)fluoranthene Analyses by
Water Type
Statistical Summary of BenzoCa)pyrene Analyses by
Water Type
Statistical Summary of Dibenzo(a,h)anthracene Analyses
by Water Type
Statistical Summary of Benzo(g,h,i)perylene analyses by
by Water Type
Statistical Summary of Indeno(l,2,3-cd)pyrene Analyses
by Water Type
Summary of the Tests for the Differences Across
Water Types ............ .
Percent Recovery for Various Water Types
5
14
16
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
51
vix
-------
TABLES (Continued)
Page
Number
22 Overall Percent Relative Standard Deviation for Various
Water Types 52
23 Single-Analyst Percent Relative Standard Deviation
for various water types 53
A-l High Performance Liquid Chromatography of PNAs 60
viii
-------
ACKNOWLEDGMENT
The authors appreciate the cooperation of all Battelle Columbus
Laboratories' staff members who participated in this study. In particular,
we thank Mr. Fleet Girod and Mr. Carl Mullins for collecting and distributing
the industrial wastewater samples and handling ampule concentrate shipments.
The authors acknowledge the sincere efforts by the participating laboratories
to provide viable data for this study. Their patience and many helpful
suggestions were instrumental in resolving the problems which arose during
the course of the study.
Gratitude is also expressed to various industries for their interest in
the study and willingness to provide samples of appropriate wastewater efflu-
ents without which the program's objectives could not have been realized.
Lastly, we thank Mr. Edward L. Berg and Mr. Robert Graves, USEPA Project
Officers, whose guidance and intense interest in the study contributed to the
successful completion of a difficult and sometimes frustrating task.
ix
-------
SECTION 1
INTRODUCTION
USEPA first promulgated guidelines (1) establishing test procedures for
the analysis of pollutants in 1973, following the passage of the Federal
Water Pollution Control Act in 1972 by Congress. Pursuant to the amendment
and publication of these guidelines, USEPA entered into a Settlement
Agreementthe Consent Decreewhich 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(2), mandating the control of toxic pollutants discharged
into ambient waters by industry.
In order to facilitate the implementation of the Clean Water Act, USEPA
selected 129 specific toxic pollutants, 113 organic and 16 inorganic, for
initial study. The organic pollutants were divided into 12 categories based
on their chemical structure. Analytical methods were developed by USEPA for
these 12 categories through in-house and contracted research. These anal-
ytical methods are currently under review by USEPA and may eventually be
required for the monitoring of the 113 toxic pollutants in industrial waste
water effluents, as specified by the Clean Water Act of 1977. Upon
completion of the review, USEPA will promulgate a final rule.
This report describes the interlaboratory study of Method 610 proposed
for the Category 9 chemicals listed below:
Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo(a)anthrac ene
Chrysene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
Dibenzo(a,h)anthracene
Benzo(g,h,i)perylene
Indeno(1,2,3-cd)pyrene
1
-------
The primary objective of the study was to characterize the behavior of
Method 610 in terms of 1) accuracy; 2) overall precision; 3) single-
analyst precision; and 4) effect of water type on accuracy and precision.
The study was conducted with the cooperation of 16* participating labora-
tories under the auspices of the EMSL-Cincinnati.
Each of the laboratories was supplied with six samples of the Category 9
chemicals as solutions in acetone packaged in flame-sealed glass ampules.
One-mL aliquots of the solutions were added to six types of test waters
according to instructions. Water samples were then analyzed with and without
the increment, and the added level of pollutant determined by the difference.
Concentrations were reported in jjg/L with only one value reported for each
sample.
The data were collected from the 16 laboratories according to
Youden's(3) collaborative testing design. Formal statistical techniques
compatible with the Youden design were used to identify outliers, estimate
the method's accuracy and precision, and test for the effect of water type.
The formal statistical analyses were carried out using the USEPA's I MVS
computer program(4). The information obtained from the statistical analyses
was summarized and reduced to a descriptive form for interpretation and
presentation.
Method 610 was developed in the Battelle-Columbus Laboratories (BCL)
under a contract with the Physical and Chemical Methods Branch, Environmental
Monitoring and Support Laboratory-Cincinnati. Method 610 is presented in
Appendix A. Briefly, the method requires extraction of the pollutants from
the aqueous sample using methylene chloride. The extract is then subjected
to silica gel chromatographic cleanup. The PNA fraction is concentrated
using Kuderna Danish (K-D) evaporation, exchanged to acetonitrile and ana-
lyzed by HPLC with UV and fluorescence detection.
* Three additional laboratories which participated in the study did not
follow the approved .analytical procedure (Method 610) and their results
were not used in the statistical evaluation of the data.
2
-------
SECTION 2
SUMMARY
The interlaboratory study of an analytical method such as Method 610,
involves characterizing the accuracy and precision of the method over a wide
range of working conditions. Accuracy is directly related to mean recovery
and precision is related to both the overall variation and the single-analyst
variation of the method.
A range of typical working conditions was introduced into the study by
varying both the concentration levels of the analytes spiked into the sample
test water and by changing the type of test water. For each analyte, three
concentration levels (low, medium, and high) were used with each of six dif-
ferent test waters (distilled water, tap water, surface water, and three
industrial wastewater effluents).
To summarize the accuracy of Method 610, the following equation was
determined for each effluent:
X - a + b C
where X denotes the mean recovery and C the concentration level of the
analyte. The precision was summarized for each effluent by the equations
S ¦ d + e X and SR ¦ f + g X
where S denotes the overall standard deviation and SR the single-analyst
standard deviation.
The data reported by the 16 participating laboratories were used to
estimate the coefficients a, b, d, e, f, and g for these equations for each
3
-------
effluent. These equations were calculated for each effluent used in this
study, and the results are summarized in Table 1.
In addition to summarizing the accuracy and precision of Method 610, the
following observations were made based on the data:
The method has a pronounced negative bias for most compounds.
Twenty percent of the total data for all sixteen PNA's were
rejected by the outlier test.
The percentage recovery of the sixteen PNA's for a specific
analyte concentration in a water type ranged from 43-110
percent. The recoveries were significantly lower than those
reported by Battelle Columbus Laboratories and obtained during
the development of the method.
The overall and single-analyst percent relative standard
deviations ranged from 16-91 percent and 11-50 percent,
respectively, (see Tables 21 and 22).
A statistically significant effect due to water type was
established for 6 of the 16 PNA's. However, because distilled
water had consistently lower recoveries than the wastewaters,
and the distilled waters were the first samples to be analyzed,
the statistical effect was judged to be due to the analytical
learning process and, therefore, of no practical importance.
4
-------
TABLE 1. REGRESSION EQUATIONS FOR ACCURACY AND PRECISION
OF METHOD 610 BY COMPOUND AND WATER TYPE
WATER TYPE
NAPHTHALENE
ACENAPHTHYLENE
ACENAPHTHENE
FLUORENE
APPLICABLE CONC. RANGE
( 10
00 - 375.00)
( 10
00 - 425.00 I
( 10
00 - 260.00)
( to
.00 - 463.00)
DISTILLED WATER
SINGLE-ANALYST PRECISION
SR
* 0 39*
- 0. 18
SR
= 0.36X
~ 0.29
SR
= 0 39X
~ 0. 76
SR =
¦ 0.44X
- 1.12
OVERALL PRECISION
S *
O 411 ~
0 74
S =
0 42*
0 52
S =
0 53X
1 . 32
s =
0.63X -
0 65
ACCURACY
X =
0.57C -
0.70
X =
0 69C -
t .89
X =
0 52C «
0 .54
x -
0.56C -
0.52
TAP WATER
SINGLE-ANALYST PRECISION
SR
= 0.38X
~ 0.24
SR
x 0 38*
- 0.01
SR
= 0 29*
~ 0.27
SR »
= 0.25X
~ 1.16
OVERALL PRECISION
S =
0.39X
0. 73
S ¦
0.44X -
0 . 03
S »
0.47X '
0.45
s «
0 50* -
0. 16
ACCURACY
X =
o.eoc -
0.62
X =
0.7IC -
2.58
X =
0.5IC -
1 .55
X «
0 59C -
1 30
SURFACE WATER
SINGLE-ANALYST PRECISION
OVaRALL PRECISION
SR
- 0.24*
1 .94
SB
= 0.27X
« 0.30
SR
= 0 1 7 X
1.48
SR <
= 0 40*
- 0 . 93
S =
0.4IX ~
1 . 07
s =
0 30*
0 08
s =
0 48X
0. 23
S -
0.52X -
0 74
ACCURACY
X !
o.eoc -
0. 82
X !
0.74C -
2 . 07
X =
0.53C -
0.59
X «
0.57C -
0 25
WASTEWATER
SINGLE-ANALYST PRECISION
SR
= 0.I9X
1 . 34
SR
- 0 19*
~ 1 . 02
SR -
= 0.35X
- 0. 79
SR <
= 0.25X
~ 1. 60
OVERALL PRECISION
S !
0 36X <
0. 26
S =
0 32X -
0 01
s =
0 50X -
0.21
s =
0.52X -
1 26
ACCURACY
X '
0.62C *
0.72
* =
0 83C -
1 16
X =
0.59C -
0 . 46
X >
0.60C -
0 03
WASTEWATER
SINGLE-ANALYST PRECISION
SR
' 0.23X
- 0.48
SR
= 0.32X
- 0.81
SR »
> 0.24X
0.33
SR >
» 0.2IX
~ 2 56
OVERALL PRECISION
S =
0 32 X -
1 .09
S =
0.36X -
0 13
s =
0.471
0. 08
s =
0 471 -
0 44
ACCURACY
X =
0.58C
1 . 04
X =
0.75C -
0 80
X =
0 57C '
0 . 30
X =
0 53C ~
0. 73
WASTEWATER (C-96)
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR
S -
X =
¦ 0.31*
0.4IX -
0.65C -
0 . 26
0. IS
0 . 76
SR
s =
X =
= 0. 17 X
0 23X
0 83C -
' O. 57
1 . 09
t 89
SR =
S :
X =
: 0 28*
0 43X -
0.62C <
0. 34
0. 54
0 12
SR ¦
S
X =
- 0.35X
0.49X -
0 54C ~
~ 0. 10
0.39
0 . 36
X " MEAN RECOVERY
C * TRUE VALUE FOR THE CONCENTRATION
-------
TABLE 1 (Cont inued)
WATER TYPE
PHENANTHRENE
<5.00 - 200.00)
ANTHRACENE
(10 00 - 400 00 >
FLUORANTHENE
(0 30 - 15 001
PYRENE
(2 00 - 90.001
APPLICABLE CONC RANGE
OISTILLED WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
TAP MATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SURFACE MATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
WASTEWATER (C-94)
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
MASTEWATER (C-9S)
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
WASTEWATER (C-9BI
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR - 0.28 X 0.05
S = 0.47* - 0 25
X = 0.72C - 0 95
SR - 0.26* 0.10
S = 0 35X - 0.16
X * 0.7IC - 0.71
SR = 0.23X - 0.34
S = 0.37X - 0.62
X = 0.70C - 0.26
SR = 0. I IX < 0.47
S = 0 26X - 0.22
X = 0 79C - 0.61
SR = 0.I5X - 0.03
S - 0 28X - 0 03
X = 0.73C - 0 48
SR = 0.35X - 0.50
S - 0.38X - 0 28
X = 0.70C - 0.47
SR : 0.23X ~ 1.16
S - 0.4IX ~ O 45
X = 0 63C - I 26
SR = 0.22X ~ 0.06
S = 0 32X 0.03
X = 0 68C ~ 0 07
SR » 0.22X 0.61
S * 0 4 IX * 0.10
X = 0 63C - 2 05
SR » 0.23 X 0.01
S = 0 32X 0.01
X = 0.7IC - 0.03
SR = 0. 19 X 0.22
S = 0 34X - 0.69
X = 0.64C - 0.45
SR = O 2 7 X - 0 04
S = O 44 X - 0 01
X = 0 59C ~ 0.05
SR = 0.I9X » 0.99
S * 0.39X - 0 4 1
X * 0.69C - 0.26
SR = O 12 X 0.03
S * 0 35* - 0.01
X = 0.75C - 0.00
SR : 0.I9X ' 0.10
S « 0.33X - 0.31
X = 0 64C - 0.34
SR = 0.I7X - 0.01
S * 0.29X ~ 0.02
X = 0 7OC * 0.02
SR - 0.24X - 0.29
S * 0 35X - 0.91
X = 0 66C 0.08
SR = 0.40X - 0.06
S = 0 38X 0 03
X = 0.75C 0.01
SR * 0.25X 0.14
S = 0.42X - 0 00
X * 0.69C - 0.12
SR = 0.25X ~ 0.02
S ; 0.39X 0.09
X : 0 68C * 0.09
SR « 0.22 X - 0.10
S = O 301 -0.12
X ' 0.74C - 0 08
SR = 0. 17 X 0 15
S = 0 26X - 0 02
X = 0.71C ' 0 02
SR = 0.27X - 0 04
S = 0 34X - 0. 19
X = 0.66C ~ 0 25
SR * 0.20X - 0.00
S » 0.25k O 14
X = 0 77C ~ 0.01
X * MEAN RECOVERY
C = TRUE VALUE FOR THE CONCENTRATION
-------
TABLE 1. (Continued)
WATER TYPE BENZOIA I ANTHRACENE CHRYSENE BENZOIB)FLUORANTHENE BENZOtKIFl UORANTHENE
APPLICABLE CONC. RANGE 10.50 - IS 00) i 2 00 - 60.001 <0.20 - II 00) (0 12 - 6 00)
DISTILLEO MATER
SINGLE-ANALVST PRECISION SR * 0.28* ~ 0.04 SR = 0.32X - 0.18 SR = 0.2IX > 0.01 SR = 0.44X - O.Ot
OVERALL PRECISION S * 0 341 * 0 02 S = 0 58* - 0 22 S - 0 38X - 0 00 S - 0 69* <- 0 01
ACCURACY X = 0.73C ~ 0 05 X = 0.77C - 0 18 X = 0.78C 0 01 X = 0.59C « 0 00
TAP WATER
SINGLE-ANALYST PRECISION SR - 0.23X 0.13 SR = 0 40X - 0 37 SR - 0 24X - 0.00 SR = 0.48X 0.06
OVERALL PRECISION S - 0.37X « 0 05 S » O 55* - 0.10 S - 0 32* ¦ 0 01 S = 0 SIX - 0 01
ACCURACY X = 0.77C ~ 0.05 X = O 82C - 0 09 X = 0 83C 0.00 X - 0.98C - 0.03
SURFACE WATER
SINGLE-ANALYST PRECISION SR = 0.I8X - 0.01 SR - 0.39X - 0.51 SR - 0.26X - 0.01 SR - 0.I9X ~ 0 IB
OVERALL PRECISION S = 0.34X - 0.05 S = 0.50X - 0 20 S = 0 48X - 0.03 S = 0 76X 0 01
ACCURACY X * 0.76C - 0.02 X * 0.77C ~ 0. 39 X - 0 . 73C '0.01 X = I . 02C ~ 0 04
WASTEWATER (C-94)
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR
S =
X =
' 0.24X
0.32 X ~
0.73C ~
~ 0.03
0 . OS
0. 12
SR * 0.29X
S * 0 44 X -
X « 0 97C -
- 0 . 06
0 09
0.28
SR
S =
X =
= O . 2 1 X
0 391 -
0 80C -
- 0. 00
0 . 02
0.01
SR
s =
X =
= 0.I8X - 0.01
0 471 » 0 01
0 BIC « 0 03
WASTEWATER IC-95)
SINGLE-ANALYST PRECISION
SR
= 0.28X
-0.04
SR * 0 25*
' 0.42
SR
= 0 28X
- 0.01
SR ¦
= 0.46X - 0.07
OVERALL PRECISION
S -
0.43X -
0. 04
S ¦ 0.48X
0 10
s =
0 . 42X -
0 . 02
s =
0 B8X - 0.0 1
ACCURACY
X =
0.69C ~
0.03
X » I.22C -
0 56
X =
0 90C -
0 . 00
X =
1.09C ' 0 03
WASTEWATER (C-961
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR
s *
X *
* o.tax
0 32X ~
0.76C ~
0. 00
0.04
0 . 00
SR * 0.24X
S < 0 45* ~
X » 1 .OIC -
0 02
0. 14
0 . 07
SR
S =
X =
= 0.26X
0 37 X -
0 90C >
- 0.01
0 01
0. 00
SR
S *
X *
= 0.22X - 0.00
0 69* - 0.03
0 99C - 0.05
X * MEAN RECOVERY
C * TRUE VALUE FOR THE CONCENTRATION
-------
TABLE 1. (Continued)
MATER TYPE
BENZOIA tPYRENE
0IBEN7O
( 1 .
00 - 50
00)
(0
75 - 22
00)
DISTILLED WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR
S =
* =
- 0 36*
0.53X -
0.56C *
- 0.01
0 01
0.01
SR
s =
X *
* 0.24 X
0 45*
0 4 IC
« 0 . 02
> 0 03
~ 0.11
SR
S =
X =
= 0 25X
0 58X
: 0 44C
0. 04
~ 0. 10
~ 0.30
SR
S =
X =
= 0 29*
0.42X ~
0 54C <
'>.02
0.01
0 06
TAP WATER
SINCIE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR
S =
X *
= 0.29X
0 SIX -
0.54C -
- 0.01
o oo
0 02
SR
s *
X ¦¦
= 0.42X
0 44*
O.BSC
- 0.01
« 0 04
0 09
SR
S =
X =
* 0 24X
0.29X
0 71C
- 0.06
0 00
- 0 . 07
SR
S =
X =
* 0 33X
0 38* ~
0.70C -
- 0.04
0 . 02
0 05
SURFACE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR
s *
X =
= 0 24*
0 47X -
0.65C ~
- 0.01
0 . 00
0.01
SR
s =
X *
* 0.34X
0 49*
0. 7 IC
« 0. 04
- 0 02
- 0 03
SR
S =
X =
= 0 40X
0 60X
0 67C
- 0.16
- 0 12
0 05
SR
S =
X ¦
= 0.27X
0 421 -
0.60C »
- 0 04
0 06
0 02
WASTEWATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR
s =
X =
= O.30X
0 44X -
0.67C ~
- O.OI
0 0 1
0. 02
SR
s =
X =
= 0.24 X
0 35*
0 . 7 IC
~ 0. 00
~ 0 00
- 0 05
SR
S =
x =
= 0.25X
0 36X
0 72C
- 0 . 04
0 08
- 0 . 05
SR
S *
X :
= 0.25X
0 . 42X -
0.67C ~
- 0 . 06
0 04
0 0 1
WASTEWATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR
s =
X =
= 0 31*
0 40X -
0.72C -
0.01
0 00
0.01
SR
S =
x =
= 0.25X
0 39*
0 . 77C
0.12
0 00
0 . 02
SR
S =
X =
= 0 2 7 X
0 48*
0 7 IC
~ 0.01
- 0 17
> 0 14
SR
S =
X =
= 0 39*
0.501 »
0.95C -
- 0.01
0 04
0 . 05
WASTEWATER (C-96)
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR
s =
X =
- 0.20X
0.4IX -
0.7OC ~
- 0. oo
0 . 02
0.01
SR
S »
X ¦-
* 0.36X
0 45*
0 . 7 IC
- 0.07
0 OS
0. 18
SR
S =
X =
= 0.341
0 42*
0 69C
- 0.17
- 0 04
0 20
SR
S =
x --
= 0.37X
0.44X -
0 83C -
- 0.07
0 05
Oil
X * MEAN RECOVERY
c TRUE VALUE FOR THE CONCENTRATION
-------
Operational problems included variable HPLC column performance
and differences in fluorescence detector response for the
general types of detectors employed. Some of the PNA's are
light sensitive, in particular, dibenzo(a,h)anthracene and
benzo(g,h,i)perylene, thus exposure to light should be
m-initniKed.
9
-------
SECTION 3
DESCRIPTION OF STUDY
SELECTION OF PARTICIPATING LABORATORIES
Potential participants identified from a list of 100 laboratories pro-
vided by USEPA were informed of the impending study. Forty-one laboratories
responded to the request for technical and cost proposals. Proposals were
carefully reviewed and then ranked on the basis of technical experience and
facilities. The laboratories selected for awards represented a mix of those
showing average to above average analytical capabilities and are listed
below:
Analytical Development Company
1875 Willow Park Way
P.O. Box 744
Monument, CO 80132
Arthur D. Little, Inc.
25 Acorn Pike
Cambridge, MA 02140
Environmental Research Group, Inc.
117 N. First
Ann Arbor, MI 48103
Environmental Science and Engineering
P.O. Box 13454
Gainesville, FL 32604
Foremost Foods Inc.
6363 Clark Avenue
Dublin, CA 94566
Gulf South Research Institute
P.O. Box 26518
New Orleans, LA 70186
Hydroscience, Inc.
9041 Executive Park Drive
Knoxville, TN 37919
ITT Research Institute
10 West 35th Street
Chicago, IL 60616
Mead Technology Laboratories
P.O. Box 12652
Research Triangle Park, NC 27709
Metpath
One Malcom Avenue
Teterboro, NJ 07608
Midwest Research Institute
425 Volker Boulevard
Kansas City, MO 64110
Monsanto Research Corporation
P.O. Box 8, Sta. B
Dayton, OH 45407
10
-------
Southern Research Institute U.S. Coast Guard Research &
2000 Ninth Avenue, S. Development Center
Birmingham, AL 35205 Avery Point
Groton, CT 06340
Southwest Research Institute
8500 Culebra Road U.S. Environmental Protection
P.O. Drawer 25810 Agency
San Antonio, TX 78284 EMSL
Cincinnati, OH 45268
SRI International
333 Ravenswood Avenue West Coast Technical Service
Menlo Park, CA 94025 17605 Fabrica Way, Suite D
Cerritos, CA 90701
Systems, Science, and Software
3398 Carmel Mountain road
San Diego, CA 92121
TEST DESIGN
The test design was patterned after Youden's non-replicate design(3) for
collaborative evaluation of precision and accuracy for analytical methods.
According to Youden's design, samples are analyzed in pairs, with each sample
of a pair having a slightly different concentration of the constituent of
interest. The analyst is directed to do a single analysis and report one
value for each sample, as if for a normal routine sample.
Prior to the start of the formal interlaboratory study, a preliminary
study was conducted to enable the participants to gain experience with the
analytical and sample handling procedures. Each analyst analyzed one trial
Youden pair sample and then attended a prestudy conference at USEPA in
Cincinnati, Ohio, to discuss the findings, the method, and the factors that
could affect the quality of data. The major discussions concerned cleanup of
solvent extracts, HPLC conditions, and problems with the UV and fluorescence
detectors. A number of recommendations were offered for improving method
performance, and these are summarized in Appendix B.
Test samples were prepared as liquid concentrates in sealed glass
ampules and presented to the analyst with complete instructions. The analyst
was required to add an aliquot of each concentrate to a volume of distilled
water and to a volume of each of the five water types described below. The
analysis in distilled water was used to evaluate the analyst's ability to use
11
-------
the method on a sample free of interferences. Analyses in other water types
were intended to reveal effects of various chemical matrices on the method's
performance. Major elements of the test design were:
1. Three Youden pairs of samples were analyzed for each parameter
and the concentrations within each pair deviated at least + 5
percent but no more than + 20 percent from the mean of the pair.
The three Youden pairs were spread over a usable and realistic
range, the lowest pair being somewhat above the minimum
detection limit.
2. Samples of approximately 2 mL were supplied as liquid
concentrates in acetone contained in 10-mL glass ampules. One
-mL aliquots of the concentrates were added to the test waters
according to the instructions. Water samples including
distilled water were analyzed with and without added increment
and the added level determined by difference. Concentrations
were reported in terms of ug/L with only one value reported for
each sample.
3. Analyses were conducted in six types of water as follows:
a. Distilled water
b. A municipal drinking water
c. A surface water vulnerable to synthetic chemical contami-
nation, as from a river
d. Three industrial wastewaters from industries that normally
would be regulated for the priority pollutants under study.
4. The participating laboratories were provided with a write-up
of method of analysis, chemical standards required for cali-
bration, and samples of the three industrial wastewaters. Each
participating laboratory was responsible for securing samples
of the other three test waters.
12
-------
SECTION 4
EXPERIMENTAL PROCEDURES
PREPARATION OF YOUDEN PAIR CONCENTRATES
Stock solutions o£ the Category 9 compounds were prepared by dissolving
accurately weighed amounts of the chemicals in acetone. The sample concen-
trates were then prepared by diluting measured amounts of the stock solutions
to larger volumes. As noted, the concentration of a given compound in each
Youden pair was adjusted so that it differed by at least + 5 percent, but was
no greater than + 20 percent from the mean of the pair.
The concentrations of the diluted solutions were confirmed by liquid
chromatographic analysis. Chromatographic conditions were the same as those
described in Method 610. Sample concentrates of approximately 2 mL of the
diluted solutions were then prepared in 10-mL glass ampules and flame-sealed.
The concentrations, ug/mL, of the Category 9 compounds in the ampules are
given in Table 2.
STABILITY OF YOUDEN PAIR CONCENTRATES
The stability of the Youden pairs of Category 9 compounds was studied
over a 90-day period. Triplicate samples of each Youden pair concentrate
were selected at random from the lot of ampules and analyzed at 0, 45, and 90
days. The stability of the samples was considered satisfactory. With the
exception noted for fluorine ampules Numbers 2 and 6 (see Table 2 footnote),
deviation of the analyzed values from the true values did not exceed _+ 17
percent at the end of the 90-day period.
13
-------
TABLE 2. CALCULATED CONCENTRATIONS OF CATEGORY 9
COMPOUNDS IN AMPULES, ug/mL
Ampule Number
Component
1
2
3
4
5
6
Naphthalene
10.0
13.0
110.0
90.0
335.0
375.0
Acenaphthylene
10.0
15.0
110.0
90.0
425.0
375.0
Acenaphthene
10.0
12.0
120.0
95.0
235.0
260.0
Fluorene
10.0
13.0*
90.0
115.0
270.0
175*
Phenanthrene
5.0
6.0
60.0
50.0
205.0
280.0
Anthracene
10.0
14.0
70.0
85.0
400.0
350.0
Fluoranthene
0.30
0.4
4.0
3.0
15.0
12.0
Pyrene
2.0
2.6
24.0
28.0
90.0
75.0
Benz o(a)anthrac ene
0.50
0.60
6.0
5.0
12.0
16.0
Chrysene
2.0
3.0
20.0
28.0
60.0
40.0
Benzo(b)fluoranthene
0.20
0.30
3.0
2.0
8.0
11.0
Benzo(k)fluoranthene
0.12
0.15
1.4
1.1
4.0
6.0
Benzo(a)pyrene
0.20
0.30
2.0
2.8
12.0
15.0
D ibenzo(a,h)anthrac ene
0.50
0.70
6.5
5.0
24.0
20.0
Benzo(g,h,i)perylene
1.00
1.40
14.0
10.0
35.0
50.0
Indeno(1,2,3-cd)pyrene
0.75
1.0
5.0
6.0
22.0
15.0
* Fluorene analyses for these ampule samples indicate that the calculated
concentrations are incorrect. The analyzed values are approximately 25.4
and 463.0 ug/mL, respectively, for ampules 2 and 6 and were used in the
statistical analyses in lieu of the calculated values.
COLLECTION OF INDUSTRIAL WASTEWATER EFFLUENTS
Chemical industries producing Category 9 compounds or utilizing them in
chemical processes were identified from Synthetic Organic Chemicals - U.S.
Production and Sales 1974-77, U.S. International Trade Commission, and the
1979 Directory of Chemical Producers in the United States.
Since Method 610 may eventually be used by industries seeking permits
issued by the National Pollutant Discharge Elimination System under the Clean
14
-------
Water Act, plants using good technology in their wastewater treatment
facilities were selected for sampling. Attempts were made to obtain
wastewater samples from both users and producers of the various category
compounds. The appropriateness of a particular company's wastewater was
first assessed by discussions with technical personnel of that company. If
on the basis of these discussions, it appeared that the plant's effluent
might be suitable for the program, a 1-gallon sample of the effluent was sent
to BCL for a preliminary analysis. The effluent was judged to be suitable
for the method study if the analysis showed no major interferences or high
background of the chemical parameters of interest that might nullify analyt-
ical data obtained for the lowest Youden pair concentrates. Approximately 55
gallons of acceptable wastewater effluents were collected in stainless steel
drums at the plant sites by plant or BCL personnel and delivered to BCL by
truck. Samples of wastewater were analyzed at BCL before and after spiking
with the various Category 9 compounds. If the results of these analyses were
satisfactory, 1-quart samples of the effluent were prepared for shipment to
the participating laboratories. The contents of the drums were stirred vig-
orously during the bottling operation to ensure sample homogeneity. Samples
were identified by coded labels as C-94, C-95, or C-96. A brief description
of plant source and methods of wastewater treatments are given below. The
results of BCL's analysis of the wastewater samples are given in Table 3.
Wastewater C-94 (SIC Code #2911*)Effluent from a large oil
refinery. Wastewater stream is treated in a biological treatment
plant, clarified and then discharged into a river.
Wastewater C-95 (SIC Code #3312*)Effluent from a blast furnace
producing molten hot metal. Wastewater treatment scheme consists
of coagulation, sedimentation, and recycle. Chemicals are added to
the water to agglomerate the small suspended solids into larger
particles. The solids settle to the bottom of the clarifiers, and
this sludge is removed and dewatered. The clean effluent is cooled
and 95 percent is recycled for top gas scrubbing and 5 percent is
blown down to a river.
15
-------
Wastewater C-96 (SIC Code #3112*)Wastewater stream is the
combined effluents from a coke oven and blast furnace operation.
The waste stream is treated to agglomerate suspended solids and
sent to settling ponds. Effluent from the ponds is clarified and
then discharged into a river.
TABLE 3. BACKGROUND ANALYSES OF WASTEWATER
SAMPLES FOR CATEGORY 9 COMPOUNDS,
Ug/L
Oil
Blast
Coke
Refinery
Furnace,
Oven
Compound
C-94
C-95
C-96
Naphthalene
< 1
<1
<1
Acenaphthylene
<1
<1
<1
Acenaphthene
9.4
<1
<1
Fluorene
2.7
ND
0.9
Phenanthrene
<1
3.3
1.0
Anthracene
<1
4.1
ND
Fluoranthene
0.6
0.4
0.1
Pyrene
4.2
2.7
0.28
Benzo(a)anthracene
1.0
0.08
ND
Chrysene
<0.1
ND
0.32
Benzo(b)fluoranthene
<0.1
ND
0.06
Benzo(k)fluoranthene
<0.1
ND
0.03
Benzo(a)pyrene
<0.2
ND
0.08
D ibenzo(a,h)anthr ac ene
<0.1
0.04
0.09
Benzo(g,h,i)perylene
<0.2
ND
0.21
Indeno(1,2,3-cd)pyrene
<0.1
ND
0.07
* Standard Industrial Classification Code Number.
16
-------
DISTRIBUTION OF SAMPLES
Each laboratory was provided with the following materials:
(1) Six Youden pair ampules of each of three concentration levels, for
a total of 36 ampule for preparation of samples;
(2) Seven 1-quart samples of three types of industrial wastewater
effluents, a total of 21 samples;
(3) Standards of the 16 PNA's;
(4) A copy of Method 610;
(5) A form for reporting data; and
(6) A questionnaire requesting description of difficulties
encountered with the analytical method and suggestions for
improvement of the method.
The laboratories were instructed to add a measured quantity of the
contents of the ampules to test waters by the following procedure:
Place a magnetic stirbar in the sample bottle, add 1 mL of the
solution in the ampule, cap and stir 15 minutes using a magnetic
stirrer. Transfer the contents of the bottle to a 2-liter separa-
tor/ funnel and proceed with the analysis as described in Method
610. In calculating results, assume the volume of the sample to be
one liter.
Standards of the PNA's were supplied to the laboratories because of the
difficulty of obtaining PNA's of known purity and chemical structure. Some
of the more complex PNA's were not readily available in this country at the
time of the study and extensive delays in the program may have occured if
each laboratory had been required to procure their PNA standards. The
purities and structure identities of the standards supplied to the labora-
tories were confirmed by HPLC-fluorescence and GC-MS techniques.
17
-------
treatment of data
The study's 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 labor-
atories. The statistical techniques employed in the data reduction process
are similar to ASTM techniques.
The algorithms required to perform the statistical analyses have been
integrated into a system of computer programs referred to as IMVS. The
analyses performed by IMVS include tests for the rejection of outliers
(laboratories and individual data points), summary statistics by con-
centration level for mean recovery (accuracy), overall and single-analyst
standard deviation (precision), determination of the linear relationship
between mean recovery and concentration 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.
A detailed description of each of the statistical analysis procedures
is presented below.
REJECTION OF OUTLIERS
Since the objective of the statistical analyses is to summarize the
general behavior of the method in terms of accuracy and precision, it is
important to identify data points which are inconsistent with the majority
of the data. These data points should be deleted from the analysis because
they can lead to values of summary statistics which are not representative
of the general behavior of the method. However, some erratic behavior in
the data may be directly related to some facet of the method under the
study. Therefore, inconsistent data points should not be removed indis-
criminately, and any points that are removed should be clearly identified
since further investigation of the analytical conditions related to the
outliers might be of value. In some cases the data points which are deleted
may actually be closer to the true value than the retained data. This is
consistent since outliers are judged relative to the average value of the
data and not with respect to the true value. Data rejected as
18
-------
outliers for this study as a result of any of the following tests for
outliers have been identified by the symbol in the raw data tables.
Youden's Laboratory Ranking Procedure
In some cases, the analytical values reported by a specific laboratory
are so consistently high or low that a large systematic error may be attri-
buted to that laboratory. These data are not representative of the method
and should be rejected. Youden's(3) ranking test for outlying laboratories
was applied separately to data from each of the waters used in this study.
Since six water types were used in this study, the laboratory ranking pro-
cedure was applied to these six different subsets of the data. Each labora-
tory ranking test was performed at the 5 percent level of significance.
The Youden laboratory ranking procedure requires a complete set of data
from every laboratory within a given water type. Missing data from labora-
tory "i" for water type "j" were replaced by the following procedure.
Letting denote the reported measurement from laboratory "i" for water
type "j" and concentration level C^, it is assumed that
y.
*ijk " Pj Cjt J. Lj . eijit
where $j and Yj are fixed parameters which determine the effect of water
type "j", Li is the systematic error due to laboratory "i" and eijk is the
random within laboratory error. Taking natural logarithms, it follows that
in X£jfc - in 8j + Yj in * in Lf + in eijk
which is a linear regression model with dependent variable in Xjjk and
independent variable in C^. Details and justification for this model are
discussed in the section "Comparison of Accuracy and Precision Across Water
Types."
The natural logarithms of the individual laboratory's data were regres-
sed against the natural logarithms of the true concentration levels for the
six ampules in each water type. The predicted values in were obtained
from the regression equation, and the missing values for X^j^ were estimated
by Xjjk - exp(in X^j^), where exp(x) denotes the constant e raised to the
power X.
19
-------
If the ranking test rejected a laboratory for a specific water type,
then all the laboratory's data for that water type were rejected as
outliers. The rejected values were excluded from all the remaining
analyses. In addition, after completion of the laboratory ranking proced-
ure, the predicted values created to fill in for the missing data were
rejected and excluded from further analyses for all laboratories.
Individual Outliers
The data remaining after the laboratory ranking procedure were grouped
by water type. For each water type, the data were broken down into six sub-
sets defined by the six concentration levels (ampules) used in the study.
For each subset of the data, all missing, zero, "less than," and "nondetect"
data were rejected. Next, the test for individual outliers constructed by
Thompson(5), and suggested in the ASTM Standard Practice D2777-77, was
applied to the data using a 5-percent significance level. If an individual
data point was rejected based on this test, it was removed from the subset,
and the test was repeated using the remaining data in the subset. This pro-
cess was continued until no additional data could be rejected.
STATISTICAL SUMMARIES DATA
Several summary statistics were calculated using the data remaining for
each concentration level after the outlier rejection tests were performed.
These sunmary statistics include: the number of retained data points, the
mean recovery, accuracy as a percent relative error, the absolute overall
standard deviation, the percent relative overall standard deviation, the
absolute single-analyst standard deviation, and the percent relative single-
analyst standard deviation. The basic formulas used to calculate these sta-
tistics are presented below (X}, X2,..., Xn denote the values of the n
retained data points for a specific concentration level):
Mean Recovery (X):
*4 i
i=l
20
-------
The usual concentration notation for mean recovery is X. However, the
symbol X is used in this report to be consistent with the IMVS output.
Accuracy as a Percent Relative Error:
Percent RE - X - True Value x 100
True Value
Overall Standard Deviation:
S =
4
ftZ
-------
The percent relative single-analyst standard deviation was calculated
by
Percent RSD-SR - SR x 100
X*
where X* is the average of the two mean recovery statistics corresponding to
the two concentration levels defining the particular Youden pair.
These summary statistics provide detailed information on the accuracy
and precision of the data obtained for each concentration level. One objec-
tive of the statistical analysis of the data is to summarize the information
about accuracy and precision which is contained in the statistics.
A systematic relationship often exists between the mean recovery (X)
and the true concentration level (C) of the analyte in the sample. In
addition there are often systematic relationships between the precision
statistics (S and SR) and the mean recovery (X). Usually these systematic
relationships can be adequately approximated by a linear relationship (i.e.
by a straight line). Once these straight lines are established, they can be
used to conveniently summarize the behavior of the method within a water
type, and they can aid in comparing the behavior of the method across water
types. In addition they can be used to obtain estimates of the accuracy and
precision at any concentration level within the applicable range studied.
They can also be used to predict the behavior of the method when used under
similar conditions. These important relationships are discussed below.
STATEMENT OF METHOD ACCURACY
The accuracy of the method is characterized by the relationship of the
mean recovery (X) to the true concentration (C) of the analyte in the water
sample. In order to obtain a mathematical expression for this relationship,
a regression line of the form
X ¦ a + b C (1)
was fitted to the data by regression techniques.
The true concentration values often vary over a wide range. In such
cases, the mean recovery statistics associated with the larger concentration
values tend to dominate the fitted regression line producing relatively
22
-------
larger errors in the estimates of mean recovery at the lower concentration
values. In order to eliminate this problem, a weighted least squares
technique was used to fit the mean recovery data to the true concentration
values. The weighted least-squares technique was performed by dividing both
sides of Equation (1) by C resulting in Equation (2)
(2)
The (X/C) values were regressed against the (1/C) values using ordinary
least squares to obtain estimates for the values of a and b. (This is
equivalent to performing a weighted least squares with weights w ¦ 1/C2; see
Reference (6), page 108 for details.) Equation (2) can easily be converted
to the desired relationship given by Equation (1). The intercept (b) from
Equation (2) becomes the slope (b) for Equation (1) and slope (a) from
Equation (2) becomes the intercept (a) for Equation (1). Equation (1) can
be used to calculate the percent recovery over the applicable range of
concentrations used in the study.
The percent recovery is given by
Percent Recovery ¦
a + b
x 100
1 + b
C
x 100
If the absolute value of the ratio (a/G) is small relative to the slope (b)
for the low concentration levels used in the study, then the percent
recovery can be approximated by b x 100. For example, suppose the true
concentration values range from 25 yg/L to 515 vg/L, and the fitted line is
given by X ¦ 0.20 + 0.85 C. The percent recovery would be approximated by
0.85 x 100 ¦ 85 percent over the specified range of 25 pg/L to 515 yg/L.
If the ratio (a/C) is not small relative to the slope (b), then the
percent recovery depends upon Che true concentration (C), and it oust be
evaluated at each concentration value within the specified range.
23
-------
STATEMENT OF METHOD PRECISION
The precision of the method is characterized by the relationships
between precision statistics (S and SR) and mean recovery (X). In order to
obtain a mathematical expression for these relationships, regression lines
of the form
S » d + e X (4)
and
SR « f + g X* (5)
were fitted to the data by regression techniques.
As discussed previously with respect to accuracy, the values of X and
X* often vary over a wide range. In such cases, the standard deviation
statistics associated with the larger mean recovery values will dominate the
regression lines. This will produce relatively larger errors in the
estimates of S and SR at the lower mean recovery values. Therefore, a
weighted least squares technique was also used to establish the values of
the parameters d, e, f, and g in Equations (4) and (5). The weighted least
squares technique was performed by dividing both sides of Equation (4) by X
resulting in Equation (6)
(6)
and by dividing both sides of Equation (5) by X* resulting in Equation (7)
« . £ . i + g (7)
X* X*
The (S/X) values were regressed against the (1/X) values and the (SR/X*)
values were regressed against the (1/X*) values using ordinary least squares
to obtain estimates for the parameters d, e, f, and g.
Equations (4) and (5) were obtained from Equations (6) and (7) in a
manner similar to that discussed for mean recovery. The slope (d) for
Equation (6) is the intercept (d) for Equation (4), and the intercept (e) for
Equation (6) is the slope (e) for Equation (4). Similarly, the slope (f) for
Equation (7) is the intercept (f) for Equation (5), and the intercept (g) for
Equation (7) is the slope (g) for Equation (5).
24
-------
Given Equations (4) and (5), the percent relative overall standard
deviation and the percent relative single-analyst standard deviation are
Percent RSD
£ + e
x 100
and
Percent RSD-SA
!~ s
x*
x 100
(8)
(9)
respectively. If the absolute value of the ratio (d/X) is small relative to
the slope (e), then the percent relative overall standard deviation can be
approximated by (e x 100) over the applicable range of mean recovery values.
Similarly if the ratio (f/X*) is small relative to the slope (g), then the
percent relative single-analyst standard deviation can be approximated by (g
x 100) over the applicable range of mean recovery values. If the ratios
(d/X) and (f/X*) are not small relative to the slopes (e) and (f), then the
percent relative standard deviations depend upon the values of the mean
recovery statistics X and X*, and they should be evaluated separately for
each value of X and X*.
COMPARISON OF ACCURACY AND PRECISION ACROSS WATER TYPES
It is possible that the accuracy and precision of Method 610 depend
upon the type of water being analyzed. The summary statistics X, S, and SR
are calculated separately for each concentration level within each water
type. They can be compared across water types in order to obtain
information about the effects of water type on accuracy and precision.
However, the use of these summary statistics in this manner has several
disadvantages. First, it is cumbersome since there are 36 mean recovery
statistics (X) (6 concentrations x 6 waters), 36 precision statistics (S),
and 18 precision statistics (SR) calculated for each compound. Comparison
of these statistics across concentration levels and across water types
becomes unwieldy. Second, the statistical properties of this type of
comparison procedure are difficult to determine. Finally, due to variation
associated with X, S, and SR, comparisons based on these statistics can lead
to inconsistent conclusions about the effect of water type. For example,
25
-------
distilled water may produce a significantly lower value than surface water
for the precision statistic S at a high concentration, but a significantly
higher value for S at a low concentration.
An alternative approach, described in detail(7) has been developed to
test for the effects of water type. This alternative approach is based on
the concept of summarizing the average effect of water type across concen-
tration levels rather than studying the local effects at each concentration
level. If significant differences are established by this alternative tech-
nique, then the summary statistics can be used for further local analysis.
The test for the effect of water type is based on the following statis-
tical model. If Xijfc denotes the measurement reported by laboratory "i",
for water type "j", and ampule k, then
a C|^ j I>i £ ijk * i " 1,2,..., n (10)
j - 1,2,..., 6
k ¦ 1,2,..., 6
The model components 8j and Yj are fixed parameters which determine the
effect of water type "j" on the behavior of the observed measurements
(^ijk)* parameter is the true concentration level associated with
ampule k. If the observed measurements are plotted versus concentration on
a log-log scale, the data will plot approximately along a straight line.
The intercept for the line is log Sj and the parameter Yj is the slope of
the line. The model component is a random factor which accounts for the
systematic error associated with laboratory "i". The model component e^j^
is the random factor which accounts for the intralaboratory error.
The model is designed to approximate the global behavior of the data.
The multiplicative structure was chosen because of two important properties.
First, since the model describes a straight line relationship on a log-log
scale, it allows for a possible curvilinear relationship between the data
(Xijk) and the true concentration level Cfc through the use of the exponent Yj
on Cfc. This makes the model more flexible in comparison to straight line
models. Second, as will be seen below, there is an inherent increasing
relationship between the variability in the data and the concentration level
Cjj in this model. This property is important because it is typical of
26
-------
interlaboratory data collected under conditions where the true concentration
levels vary widely.
Accuracy is related directly to the mean recovery or expected value of
the measurements (Xijfc). The expected value for the data modeled by
Equation (10) is
E(*ijk) ¦ 3j . . E(Li . eijk) (11)
Precision is related to the variability in the measurements (Xijfc).
The variance of the data modeled by Equation (10) is
w awy 2
Var(3!ijlt) * K Ck vj| Var(Lt tljk) (12)
which is an increasing function of Cfc.
The effect of water type on the accuracy and precision of Method 610 is
determined by the values of the parameters (6j) and (Yj) in Equations (11)
and (12). If the (Bj) and (Yj) vary with j (i.e. vary across water type),
then the accuracy and precision of the method also vary across water type. .
In order to determine if these parameters do vary across water type and
to compare their values, they must be estimated from the laboratory data
using regression techniques. Equation (10) represents the basic model.
However, taking natural logarithms of both sides of Equation (10), the
following straight line regression model is obtained
in Xijfc ¦ an £3j + Yj fcn + in Li + An eijfc (13)
which can be analyzed using standard linear model analysis techniques. The
parameter Ln Bj is the intercept and Yj the slope of the regression line
associated with water type "j". It is assumed that An is normally dis-
2
tributed with mean 0 and variance ai> and that £n eijk is normally distri-
buted with mean 0 and variance o^, and that the (in L^) and (in eijk) terms
are independent.
Based on Equation (13), the comparison of water types reduces to the
comparison of straight lines. Distilled water is viewed as a control, and
each of the remaining lines is compared directly to the line for distilled
water.
27
-------
Using the data on the log-log scale and regression techniques, the
parameters An Bj (and hence 6j) and Yj can be estimated. The estimates are
then used to test the null hypothesis that there is no effect due to water
type. The formal null and alternative statistical hypotheses Ho and a**e
given by
Hq: An - in - 0 and Yj - Yj » 0 for j * 2,3,4,5,6
versus
An f?j - An 4 0 and/or Yj - Yj » 0 for some j » 2,3,4,5,6
The test of null hypothesis Hq against the alternative hypothesis Ha. is
based on an F-statistic derived from standard linear model theory. The pro-
bability of obtaining a value of an F-statistic as large as the value which
was actually observed (T OBS), denoted by P(F >F OBS), is calculated under
the assumption that Hq is true. The null hypothesis Ho is rejected in favor
of Ha if P(F > F OBS) is less than 0.05.
If Hq is rejected, then some linear combination of the differences
An 6j _ £n an
-------
not necessarily mean that the effect is of practical importance. Practical
importance is related to the size and interpretation of the difference.
The interpretation of the differences involves comparing the mean
recovery and standard deviation of the (Xijfc) data for each water type to
the mean recovery and standard deviation obtained for distilled water.
These comparisons are made on a relative basis. The mean recovery for water
type "j" is given by Equation (11). The mean recovery for water type "j" is
compared to that for distilled water (j»»l) on a relative basis by the ratio
E<*iik) 6jcwTj ECl-i . 0.38 and
the confidence interval for an 85 - In is (-0.69, -0.07). Suppose the
point estimate for Y5 - Yj is 0.07, and the confidence interval for Y5 -Y^
is (-0.04, 0.18). In this case, a statistically significant effect due to
water type has been established which involves only water type 5. The
practical significance of this effect is judged by considering Equation
29
-------
(14). The ratio of mean recoveries for water type 5 and distilled water is
given by
Enisle) «f5 y5 - yx
ECXilk) 61 Ck (15)
and the ratio of the standard deviations is given by
/Var(Xi5k) ^ ^5 *5 - Yi (16)
V Var(Xiik) * 8 x ck
Since the confidence interval for Y5 - Yj contains zero, this difference is
assumed to be insignificant and is set to zero. Therefore, Equations (15)
and (16) reduce to ^5/&x. The point estimate for An 85 - in $1 was -0.38.
Therefore, the point estimate for 65/ is 0.68, and the mean recovery for
water type 5 is estimated to be 68 percent of the mean recovery for
distilled water. Similarly, the standard deviation for the data for water
type 5 is estimated to be 68 percent of the standard deviation for distilled
water. Since the 95 percent confidence interval for An S5 - in Si was
(-0.69,-0.07), any value in the interval (0.50, 0.93) is a reasonable estimate
for 65/61, and the mean recovery (standard deviation) for water type 5 can
be claimed to be from 50 percent to 93 percent of the mean recovery
(standard deviation) for distilled water. The practical significance of the
effect due to water type 5 would depend upon the importance of a mean
recovery (standard deviation) which is between 50 percent and 93 percent of
the mean recovery (standard deviation) observed for distilled water.
The comparison of accuracy and precision across water types just
discussed, is based on the assumption that Equation (10) approximately
models the data. It is clear that in practical monitoring programs of this
type such models cannot represent the data completely in every case. This
analysis, therefore, is viewed as a screening procedure which identifies
those cases where differences in water types are likely to be present. A
more detailed, local analysis can then be pursued using the basic summary
statistics for precision and accuracy.
30
-------
SECTION 5
RESULTS AND DISCUSSION
The statistical analysis procedures described in Section 4 have been
applied to the raw data shown in Appendix C for the 16 laboratories par-
ticipating in this interlaboratory study. The results of those analyses with
respect to the performance of Method 610 are discussed in this section.
STATISTICAL SUMMARIES
The basic summary statistics discussed in Section 4 were calculated for
each of the 16 FNAs and are summarized in Tables 4-19. The number of out-
liers for each data set as determined by the ranking and individual outlier
test ranged from zero to eight, and averaged about three outliers per data
set. For all data for the sixteen compounds, 20 percent of the data was
rejected.
REGRESSION EQUATIONS
Using the values contained in the summary statistics for the true con-
centrations, mean recoveries(X and X*), overall standard deviations (S), and
single-analyst standard deviations (SR), the regression lines given by
Equations 1, 4, and 5 were obtained for each compound and water type. These
regression lines were summarized in Table 1 (see Section 2, pages 5-8).
Effects of Water Type
The multiplicative model (Equation 10) was fitted separately to the data
for each compound in order to test for the effects due to water type. These
analyses are summarized in Table 20. The detailed analysis of variance
tables supporting these results are presented in Appendix D.
31
-------
TABLE 4. STATISTICAL SUMMARY FOR NAPHTHALENE ANALYSES BY WATER TYPE
WATER 1
WATER 2
WATER
3
WATER
4
WATER 5
WATER 6
LOW YOUDEN PAIR
I
2
1
2
1
2
1
2
1 2
1
2
NUMBER OF DATA POINTS
13
12
12
12
13
13
13
14
It 12
13
13
TRUE CONC UG/L
10.00
13 00
10 00
13 . 00
10
00
13
00
10
00
13
00
to
00 13.00
10 00
13 00
MEAN RECOVERY
5 07
6 45
5 16
7 34
5
32
6
St
7
62
7
57
6
14 9 . 76
5 71
7 60
ACCURACY(%REL ERROR)
-49.33
-50.35
-48.38
-43.53
-46
83
-47
59
- 23
76
-4 1
77
-38
61 -24 92
-42.92
-4I.5J
OVERALL STB DEV
3 28
2 68
2 . 40
4 . 26
3
09
4
06
3
45
2
59
0
95 1.78
2 . 50
2 32
OVERALL REL STD DEV. %
64 .64
4 1.51
46 55
58 . 07
58
19
59
54
45
27
34
19
15
43 18.20
43 85
30.45
SINGLE STD DEV. (SR>
2 .
12
2
47
3
42
2
8 1
1 30
2 34
ANALYST REL DEV, %
36.
75
39
53
56
43
36
97
16 40
35 13
MEDIUM YOUDEN PAIR
3
4
3
4
3
4
3
4
3 4
3
4
NUMBER OF DATA POINTS
13
14
13
13
14
1 4
14
15
2 12
15
15
TRIJE CONC UG/L
110 00
90 00
MO 00
90 00
1 10
00
90
00
1 10
00
90
00
1 10
00 90.00
1 10 00
90 00
MEAN RECOVERY (X)
55 St
56 29
61 . 38
59 . 29
62
76
54
97
67
23
65
04
66
15 57 15
61 25
63 . 67
ACCURACY(XREL ERROR)
-49.26
-37 46
-44.20
-34 . 12
-42
95
-38
92
-38
aa
-27
73
-39
87 -36.50
-44.32
-29.26
OVERALL STO DEV
24 .58
26 03
24 .90
22 32
22
49
27
. 12
29
00
20
. 18
25
.40 15.04
31 00
29. 10
OVERALL REL STD DEV, X
44 . 04
46 24
40 . 57
37 65
35
83
49
34
43
13
3 1
02
38
.40 26 3 1
50.61
45 . 70
SINGLE STD DEV.
IS
4 1
2 1
29
15
82
14
28
17 . 06
20. 03
ANALYST REL DEV. *
32
85
35
28
26
88
2 1
59
27 67
32 . 07
HIGH YOUDEN PAIR
5
6
5
6
5
6
5
6
5 6
5
6
NUMBER OF DATA POINTS
14
14
13
13
14
13
15
15
11 II
15
15
TRUE CONC 4C> UG/L
335.00
375.00
335.00
375 00
335
00
375
00
335
00
375
00
335
,00 375.00
335 00
375.00
MEAN RECOVERY (X>
196.37
200.58
1 74.4 1
235 IB
20 1
.62
227
67
207
. to
22 1
. 12
188
.54 202.24
206.46
256.65
ACCURACY(%REL ERROR I
-41.36
-46.51
-47 94
-37 29
-39
.81
-39
29
-38
18
-4 1
04
-43
72 -46.07
-38 37
-31 56
OVERALL STD DEV (S>
79.4 1
82 95
7 1 52
84 45
72
10
103
99
77
65
76
67
59
57 56 36
58.98
107.36
OVERALL REL STD DEV. %
40 44
4 1 . 35
4 1.01
35 91
35
. 76
45
68
37
49
34
67
3 1
60 27.87
28.56
4 1 83
SINGLE STO DEV. (SR>
89
59
74
39
55
88
42
20
34 71
71 87
ANALYST REL DEV, %
45
14
36
32
26
03
19
7 t
17 76
30 95
WATER LEGEND
« - DISTILLED WATER
2 - TAP WATER
3 - SURFACE WATER
4 - WASTEWATER (C-94)
5 - WASTEWATER
-------
TABLE 5. STATISTICAL SUMMARY FOR ACENAPHTHYLENE ANALYSES BY WATER TYPE
MATER
I
WATER
WATER
WATER
WATER
LOW YOUOEN PAIR I 2 I 2 2 ( 2
NUMBER OF DATA POINTS 14 13 12 12 It 12 13 13
TRUE COMC UG/L 10 00 15 00 10.00 15 00 10 00 15 00 10 00 15.00
MEAN RECOVERY (K( 5 37 7.71 4.57 7.92 5 30 8 87 7 44 10 60
ACCURACY<%REL ERROR) -48.28 -48.57 -54.31 -47.23 -47.01 -40.89 -25.55 -29 32
OVERALL STO OEV (S) 2.95 3.42 2.02 3.31 I 65 2.83 2.32 3 42
OVERALL REL STO DEV. % 54.93 44.34 44.17 4 1.87 3110 31.93 31.17 32.25
I
13
10. 00
8 79
-32 06
2.61
38 40
2
13
15 00
10.44
-30.40
2 79
26.68
I
12
10 00
6 79
-32. I 1
2 80
4 1 . 19
2
13
15 . 00
9 72
-35.22
2.86
29 . 48
SINGLE
ANALYST
STD DEV. (SR)
REL DEV. %
2 . 66
40.68
2. 35
37 . 61
2 21
3 I 22
2 81
3 112
I 88
2 I .82
t 93
23.41
£ ANALYST REL DEV. * 27.44 48.36 32.52 13 45
MEDIUM YOUOEN PAIR
NUMBER OF DATA POINTS
TRt|F COMC UO/L
MEAN RECOVERY (X>
ACCURACY(UREL ERROR )
OVERALL STD DEV (S)
OVERALL REL STO OEV. K
3
15
1 IO . 00
62 54
-43.15
29 . 03
46.42
4
14
90. 00
59.93
-33.41
29.27
48.85
3
16
HO. 00
74.98
-31.84
41 .51
55.36
4
16
90 . 00
70.97
-21 . 14
37 . 49
52 . 82
3
13
I 10 . 00
77.22
-29.80
29. 14
37 74
4
13
90 00
68 . 07
-24 36
20 05
29.46
3
13
I 10.00
84 07
-23.58
29 27
34 81
4
13
90. 00
78.58
- 12 . 69
25.67
32 92
3
IS
110 00
73 75
-32 95
28 39
38 50
4
15
90 . 00
7 I . 40
-20.67
32 . 66
45 . 75
3
14
IIO.00
73 78
-32 93
16 98
23 02
4
15
90. 00
87 20
-3.11
36.61
4 I 98
SINGLE
STO OEV. (SR)
16.80
35 . 29
23.63
10 94
31 03
42 75
19 51
24 24
HIGH YOUOEN PAIR
NUMBER Of DATA POINTS
TRUE COMC
5 - WASTEWATER (C-951
6 - WASTEWATER IC-96)
-------
TABLE 6. STATISTICAL SUMMARY OF ACENAPHTHENE ANALYSES BY WATER TYPE
WATER 1
WATER
2
WATER 3
WATER 4
WATER 5
WATER 6
LOM YOUDEN PAIR
1 2
1
2
1 2
1 2
1 2
1 2
NUMBER OF OATA POINTS
11 9
10
8
9 10
8 1 1
10 10
10 9
TRUE CONC
5.40 3.66
2
. 26 2
36
2
13 3.71
2
37 3 37
3 12 3 05
3 39 0 78
OVERALL REL STD DEV. X
89.40 56.45
63
. 63 52
. 70
51
II 56 35
43
43 5 1 . 54
51 86 43.57
54.51 10.22
SINGLE STD DEV. (SR)
3 24
1 44
2 36
1 30
1 . 85
2 23
ANALYST REL DEV, %
51 .64
35.94
44 . 00
2 1 .65
28 45
32 08
MED IUM YOUOEN PAIR 3 4 3 4 3 4 3 4 3 4 3 4
NUMBER OF DATA POINTS 13 13 13 12 12 12 14 12 12 13 15 14
TRUE CONC UG/l 120.00 95 00 120.00 95.00 120.00 95 00 120 00 95 00 120 00 95.00 120.00 95 00
MEAN RECOVERY (X) 59.41 39.82 59.53 48.83 82.21 53.51 67.24 54 53 62 56 54.74 65.66 54.28
ACCURACY(%REl ERROR ) -50 49 -58.29 -SO.40 -48 60 -48 16 -43 67 -43.96 -42 60 -47 87 -42.38 -45.28 -42 86
OVERALL STD DEV (S) 33 .47 29 32 24.26 22 81 27 .56 19 30 35 57 20 .30 34 26 21 99 30 .50 24 81
OVERALL REL STD DEV. X 56 34 73 99 40.76 46.71 44.30 36 07 52 90 37 23 54 77 40.17 48.45 45.70
U>
C-
SINGLE
ANALYST
STD DEV. (SR)
REL DEV. %
17 . 24
34 .81
17 II
31 .58
1 I 97
20.69
18 01
29 57
17.77
30. 29
2 I 30
35 5 I
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (XI
ACCURACY(XREL ERROR!
OVERALL STD DEV (SI
OVERALL REL STD DEV. X
5 6
13 13
235.00 260.00
153.57 137.92
-34 65 -46.96
67 90 68.67
44 22
49 . 79
5
13
235.00
I 10.69
-52.90
67.57
61 . 04
e
13
260 00
131 88
-49.28
56 68
42 98
5
1 I
235 00
I 16 2 I
-50 55
69.61
59 90
6
12
260 00
136.50
-47 50
67 99
49 81
5
14
235 00
142 79
-39 24
79 12
55 . 4 I
6
14
260.00
154 88
-40 43
82 62
53 35
5
13
235 00
145 05
-38 27
68 14
46 98
6
I I
260 00
143 99
-44 62
66.45
46. 15
5
15
235.00
159 46
32 14
64 . 37
40 36
6
14
260 00
17 I 22
-34. 15
73.29
42 80
SINGLE
ANALYST
STD DEV. (SR)
REL DEV. X
65. 24
44 . 77
33 71
27 79
20 65
16 34
55 8S
37 54
26 . 59
18 40
35 39
2 1 4 1
HATER LEGEND
1 - DISTILLED WATER
2 - TAP MATER
3 - SURFACE MATER
4 - WASTEWATER (C-941
5 - WASTEHATER (C-951
6 - WASTEWATER (C-961
-------
TABLE 7. STATISTICAL SUMMARY OF FLUORENE ANALYSES BY WATER TYPE
WATER 1
WATER 2
WATER 3
WATER 4
WATER 5
WATER 6
LOW YOUDEN PAIR
1 2
1 2
1
2
1
2
1
2
1
2
NUMBER OF DATA POINTS
tS 14
12 12
1 1
12
12
12
1 I
1 1
1 1
10
TRUE CONC UG/L
(0 00 35 40
10.00 25.40
10 00
25 40
10 00
25 40
10
00
25 40
10 . 00
25 40
MEAN RECOVERY (X)
5 IB 12 96
4 56 14.12
5.52
13 10
5 88
15 86
6
25
12 11
5 . 83
13 71
ACCURACY(XREL ERROR)
-48.22 -48.98
-54.42 -44.42
-44.80
-48 43
-4 1 15
-37.55
-37
47
-52 32
-41.68
-46 0 1
OVERALL STD DEV (SI
2.92 5.77
2 18 6 67
2 . 09
6 94
1 92
7 00
2
18
6 44
2 .94
4 15
OVERALL REL STD DEV. X
56.42 44 52
47 75 47.27
37 . 82
52 98
32 56
44 14
34
92
53 20
50 35
30.24
SINGLE STD DEV.
2.91
3 55
2 86
4
37
4 57
3 60
ANALYST REL DEV, %
32 . 06
38. 00
30 . 76
40
1 7
49 76
36 . 88
MEDIUM YOUDEN PAIR
3 4
3 4
3
4
3
4
3
4
3
4
NUMBER OF OATA POINTS
IS 15
13 13
13
13
12
12
1 1
1 1
12
12
TRUE CONC (C> UG/L
90.00 115.00
90.00 115.00
90 . 00
115.00
90. 00
1 15 . 00
90
. 00
115.00
90 00
1 15 00
MEATt RECOVERY «X >
46.92 61.59
54.97 65.51
59 97
67 52
56 88
7 1 65
51
.48
62 . 27
49 04
67 22
ACCURACY(XREL ERROR )
-47.B7 -46.44
-38 92 -43.04
-33.37
-4 1 28
-38 80
-37.69
42
80
-45.86
-45 51
-41.54
OVERALL STD DEV (S)
26 26 40.79
19.29 3 1.62
20.63
33. 47
20.39
34 . 12
24
. 71
27 58
20.39
29.27
OVERALL REL STD DEV. X
55.98 66.22
35.10 48 27
34 40
49 56
35.85
4 7 63
48
00
44 30
4 1 .57
43 54
SINGLE STD >>EV. (SR)
21.96
15.03
17 56
16
82
9. 17
15 72
ANALYST REL DEV. %
40 . 48
24 96
27 .55
26
17
16 13
27 . 04
HIGH YOUDEN PAIR
5 B
5 6
5
6
5
6
5
6
5
6
NUMBER OF OATA POINTS
14 IS
13 13
13
13
13
13
9
10
12
1 1
TRUE CONC (CI UG/L
270.00 463.00
270 00 463 00
270.00
463.00
270.00
463 00
270
00
463.00
2 70.00
463 00
MEAN RECOVERY (XI
167.96 253 71
152.04 272.36
136.80
254 35
159 60
257 81
139
53
253.09
138 69
254 B5
ACCURACY(XREL ERROR)
-37 79 -45.20
-43.69 -4 117
-49.33
-45 08
-40 89
-44 32
-48
32
-45 34
-48.63
-44.96
OVERALL STD DEV (S)
102.42 190.62
93.29 147.9B
69.08
170 63
91 .96
161.38
59
.61
1 15 29
75 92
184.62
OVERALL REL STD DEV. X
60.98 75 13
61.36 54.33
50 50
67 08
57 . 62
62 . 60
42
. 72
45.55
54 74
64 . 59
SINGLE STD DEV. (SRI
95 25
59 09
95 (4
57
08
59 28
82 53
ANALYST REL DEV, X
45 18
27 85
48 65
27
35
30 20
4 1 . 94
WATER LEGEND
1 - DISTILLED MATER
2 - TAP WATER
3 - SURFACE WATER
4 - WASTEWATER IC-94)
5 - WASTEWATER (C-95)
0 WASTEWATER (C-96)
-------
TABLE 8. STATISTICAL SUMMARY OF PHENANTHRENE ANALYSES BY WATER TYPE
WATER I WATER 2 WATER 3 WATER 4 WATER S WATER 6
LOW YOUDEN PAIR
1 2
1
2
1
2
1
2
,
2
1 2
NUMBER OF DATA POINTS
15 15
13
12
12
13
13
14
12
1 1
14 14
TRUE CONC (C) UG/L
5 00 6 00
5 00
6 00
5
00 6
00
5
00
6
00
5
00
6.00
5
.00 6.00
MEAN RECOVERY IIG/L 205.00 280.00 205 00 280 00 205.00 280 00 205 00 280 00 205 00 280.00 205 00 260 00
MEAN RECOVERY (X) 158 01 199 17 148.86 207 43 128.73 204 81 167.69 213 19 163 83 203.43 141.03 216 25
ACCURACY(XREL ERROR) -22.63 -28 87 -28.36 -25 92 -38.18 -26 85 -18 10 -23 86 -20 08 -27.35 -31 20 -22 77
OVERALL STP DEV 65.07 93.58 51.44 74.71 64 93 84 06 31 73 34 .82 4 I 05 49.56 55 95 97 18
OVERALL REL STD DEV. * 4 1.02 46 98 35.02 36 02 51.24 4 I 04 18 90 16 33 25 05 24 .36 39 67 44 94
SINGLE STD DEV, (SR) 51.09 36 62 37.37 16 94 23 60 51 01
ANALYST REL DEV. % 28.56 20 67 22 54 8 69 12 85 2B 55
WATER LEGEND
- DISTILLED MATER
2 - TAP WATER
3 - SURFACE WATER
4 - WASTEWATER (C-94)
5 - WASTEWATER (C-95)
6 - WASTEWATER (C-96)
-------
TABLE 9. STATISTICAL SUMMARY OF ANTHRACENE ANALYSES BY WATER TYPE
MATER 1
MATER 2
MATER 3
WA1ER 4
WATER 5
WAFER 6
LOM VOUDEN PAIR
1 2
1
2
1
2
1
2
|
2
1
2
NUM0ER OF DATA POINTS
13 13
13
12
13
10
13
13
13
13
14
13
TRUE CONC UG/L
10.00 14.00
10 00
14 00
10 00
14 00
10
00
14 00
10
00
14 00
10 00
14 00
MEAN RECOVERY (X)
513 7.54
4 .36
0. 75
6 13
8 00
6
91
0 89
6
00
8 66
6 56
9 47
ACCURACY(XREL ERROR)
-40.07 -40.10
-50.45
-5 1 82
-38 74
-42 82
-30
85
-36 49
-39
97
-38 15
-34 36
-32 35
OVERALL STK DEV (S)
2 32 4 11
2 . 00
2 64
1 64
1 83
2
28
3 00
1
56
2 07
1 94
I 4 t
OVERALL REL STO DEV. X
45 25 54.51
45 .96
39 12
26 82
22 88
32
95
33 78
26
04
33 IS
29 53
14 88
SINGLE STD DEV. (SR)
2 S3
1
80
1 59
2 50
1 49
1
53
ANALYST REL OEV. X
4 1 .54
33
44
22 . 50
3 1 . 89
20 . 34
19
13
MEDIUM YOUDEN PAIR
3 4
3
4
3
4
3
4
3
4
3
4
NUM0ER OF DATA POINTS
13 13
13
13
13
12
13
13
13
13
14
14
TRUE CONC
vl
HIGH VOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY(XREL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD DEV. X
5 e
13 13
4 00 00 350.00
250.47 235.14
-3588 -32.02
100.92 90.01
42.47
38.54
SINGLE
ANALYST
STD DEV. (SRI
REL OEV. X
07.03
27.51
5 0
13 13
400.00 350 00
253.90 220.92
-30.52 -34 59
109.05 105 20
43.26 45 99
50 77
23 .52
5
<2
400.00
343.58
-39 10
109 70
45 . 03
0
13
350 OO
220 02
-37 14
93 52
42.51
5
13
400 00
289 69
-27 58
133 00
45 . 93
0
13
350.00
223 00
-36 29
72 08
32 32
5
13
400 00
258 05
-35 49
00 88
33 . 67
0
12
350.00
230.15
-34 24
75.53
32 .82
5
14
400.00
203 35
-34 . 10
107 19
40 . 70
6
13
350 00
230.45
-34. 10
SO 4 1
34 . 89
57 42
24 . 77
S3 43
20.84
45 97
18 83
43 41
17.58
MATER LEGENO
1 - DISTILLED WATER
2 - TAP MATER
3 - SURFACE MATER
4 - MASTEMATER
-------
TABLE 10. STATISTICAL SUMMARY OF FLUORANTHENE ANALYSES BY WATER TYPE
WATER I WATER 2 WATER 3 WATER 4 WATER 5 WATER S
LOW VOUDEN PAIR
1 2
I
2
1
2
1
2
1
2
1
2
NUMBER OF DATA POINTS
II II
10
9
1 1
9
13
12
1 1
1 1
13
13
TRUE CONC (C) UG/L
0.30 0.40
0 . 30
0
40
0 30
0
40
0 30
0 40
0 30
0 40
0 30
0.40
MEAN RECOVERY (X)
0.30 0 29
0 18
0
27
0 23
0
28
0 2 1
0 32
0 23
0.32
0 25
0 . 30
ACCURACY(%REL ERROR )
1.07 -28 59
-39 37
-32
75
-24 24
-29
72
-28 59
-20 60
-24 97
- 19 70
- 16 56
-26 02
OVERALL STD DEV
0 50
0 69
0.31
0
25
0.47
0 49
ANALYST REL DEV, X
22. 18
28 . 03
14 . 28
9
60
19.60
20 36
HIGH YOUDEN PAIR
5 6
5
6
5
6
5
6
5
6
5
6
NUMBER OF DATA POINTS
II 11
12
10
12
1 1
13
12
12
to
13
1 1
TRUE CONC (CI UG/L
15.00 12 00
15 . 00
12
00
15 00
12
00
15 00
12 00
15 00
12 . 00
15 00
12 . 00
MEAN RECOVERY
3.05 2 73
3 50
2
68
4 32
3
35
3 27
3 05
3 66
2 13
9 61
2 29
OVERALL REL STD DEV. %
27.95 29 69
33. 3 1
30
94
51 30
47
40
30.42
32 07
34 . 24
23.52
69 . 56
25 91
SINGLE STD DEV.
2 50
1 89
2 82
1
62
1 44
6. 18
ANALYST REL DEV, X
24 .84
19 . 74
36 44
16
04
14 . 60
54 . 34
WATER LEGEND
DISTILLED WATER
TAP WATER
SURFACE WATER
WASTEWATER
WASTEWATER (C-95)
WASTEWATER
7 -
3 -
4 -
5 -
e -
-------
TABLE 11. STATISTICAL SUMMARY OF PYRENE ANALYSES BY WATER TYPE
WATER 1
WATER 2
WATER 3
WATER 4
WATER 5
WATER 6
LOW VOUDEN PAIR
1 2
1
2
1
2
1 2
1
2
1 2
NUMBER OF DATA POINTS
13 14
1 1
12
13
1 1
1 1 12
12
1 1
12 12
TRUE CONC UG/L
2 00 2.60
2 00
2 60
2 00
2 60
2.00 2 60
2 00
2 60
2 00 2.60
MEAN RECOVERY (X)
1.35 1.53
I 45
1 .86
1.51
1 68
1 37 2.01
1 55
1 .99
1 53 2 06
ACCURACY
0 44 0 77
0 68
0 77
0 50
0 19
0 34 0 48
0 27
0 57
0 53 0.61
OVERALL REL STD DEV. %
32.84 50.34
47 15
41 40
33 12
11.28
24.69 23.81
17 21
28 56
35 03 29 73
SINGLE STD DEV.
0.50
0
44
0.26
0 44
0 43
0 35
ANALYST REL DEV. X
34 .54
26
48
16.22
26 20
24 42
19 78
MEDIUM VOUDEN PAIR
3 4
3
4
3
4
3 4
3
4
3 4
NUMBER OF DATA POINTS
16 16
IS
14
13
14
13 13
14
14
13 .14
TRUE CONC (CI UG/L
24.00 26.00
24 00
28 00
24 00
26 00
24 00 28.00
24.00
28.00
24.00 28 00
MErfN RECOVERY (X)
14.46 16.63
16 37
18 . 15
17.62
2171
17.87 19 75
14.31
16 48
17 83 19 62
ACCURACY<%REL ERROR>
-39.74 -39.88
-31.77
-35. 18
-26 60
-22 45
-25.54 -29 46
-40.36
-4 1.16
-25 70 -29 92
OVERALL STD OEV (SI
7.43 7 34
5 71
6.98
4 61
6 33
5.58 6 39
6 42
5 93
4 34 5 80
OVERALL REL STD DEV, X
51.36 43.60
34 88
38.4 7
26 19
29 16
3 1 23 32.34
44 85
36. 00
24.36 29 54
SINGLE STD DEV.
3.45
4
25
3 25
3 28
5 IS
4 25
ANALYST REL DEV. X
22 . 06
24
. 63
16 55
17 .42
33 44
22 69
VO
HIGH VOUDEN PAIR
NUMBED OF DATA POINTS
TRUE COMC (C) UG/L
MEAN RECOVERY (*>
ACCURACY<%REL ERROR)
OVERALL STO DEV (S>
OVERALL REL STD DEV. 1
SINGLE
ANALYST
SIP DEV,
-------
TABLE 12. STATISTICAL SUMMARY OF BENZO(a)ANTHRACENE ANALYSES BY WATER TYPE
MATER I WATER 2 WATER 3 WATER 4 WATER 5 WATER 6
LOW YOUDEN PAIR
1 2
1 2
1
2
,
2
1
2
1
2
NUMBER OF DATA POINTS
II II
13 13
10
9
14
12
13
13
12
13
TRUE CONC (C) UG/L
0.50 0 80
0 50 0.60
0
50
0
60
0 50
0.60
0. 50
0.60
0 50
0 60
MEAN RECOVERY (X)
0 43 0 48
0 49 0.42
0
38
0
40
0 54
0.47
0 37
0.47
0.39
0.44
ACCURACY(XREL ERROR)
-14.82 -19 47
-2 17 -29.27
-24
56
-33
04
8 . 70
-22 44
-26 43
-2 1 .55
-22 12
-25.92
OVERALL STD DEV (S)
0.16 0 20
0 29 0.17
0
12
0
05
0 . 30
0 16
0 12
0. 17
0 19
0 16
OVERALL REL STO DEV, X
37 79 4 1 84
59.24 40.26
3 1
42
12
78
54 77
33 84
33 32
36 27
47 57
35. 17
SINGLE STD DEV. (SR I
0. 17
0 24
0 06
0
15
0. 07
0 08
ANALYST REL DEV, X
38. II
52 49
16 29
30
27
17.65
18 31
MEDIUM YOUDEN PAIR
3 4
3 4
3
4
3
4
3
4
3
4
NUMBER OF OATA POINTS
II II
13 13
1 1
12
13
13
13
13
13
14
TRUE CONC (C) UG/L
6.00 5.00
6 00 5.00
6
00
5
00
6. 00
5 . 00
6 00
5.00
6 . 00
5 . 00
MEAN RECOVERY (XI
3 88 3.46
4 56 3.88
4
38
4
1 1
4 15
4 35
3 97
2 87
4 7 1
3 . 86
ACCURACY(XREL ERROR)
-35.30 -30 87
-23.94 -22.37
-27
02
- 17
77
-30 79
- 13 03
-33 82
-42 66
-21.49
-22.79
OVERALL STD DEV (S>
1.02 101
1.92 1.99
t
15
1
25
. 55
1 46
1 74
III
1 . 57
1 . 54
OVERALL REL STD DEV. X
26.21 29 24
42.09 51.34
26
29
30
31
37 39
33 47
43 89
38 . 66
33 . 26
39 85
SINGLE STD DEV, (SRI
0.91
1 . 10
0 38
1
02
0 95
0 80
ANALYST REL DEV. X
24 . 75
25 . 98
9 05
23
99
27 92
18 56
HIGH YOUDEN PAIR
5 6
5 6
5
6
5
6
5
6
5
6
NUMBER OF DATA POINTS
12 12
13 13
12
1 1
13
12
14
13
14
13
TRUE CONC (CI UG/L
12.00 16 00
12 00 16.00
12
00
16
00
12 . 00
16 00
12 00
16 00
12 00
16 . 00
MEAN RECOVERY (X)
9.86 12.38
10 11 II 74
9
42
1 1
29
8 56
1187
9 88
1 1 . 34
9 . 34
11.40
ACCURACY(XREL ERROR 1
-17.82 -22 59
15 76 -26 62
-2 1
49
-29
. 42
-28 65
-25 83
- 1 7 68
-29 12
-22 16
-28 75
OVERALL STD DEV (S>
5.27 3 47
2 49 4.12
3
26
4
64
3 . 04
2 9 1
4 55
4 65
3 55
2 30
OVERALL REL STD DEV. X
53.49 27 98
24 65 35.12
34
62
4 1
05
35 5 1
24 54
46 10
4 1 . 00
38 06
20 IB
SINGLE STO DEV, (SR)
3.68
2 69
2 65
2
50
2 86
18 1
ANALYST REL DEV. X
33.05
24 . 67
25 56
24
44
28 93
17.45
WATER LEGEND
1 - DISTILLED HATER
2 - TAP WATER
3 - SURFACE WATER
4 - WASTEWATER
5 - WASTEWATER (C-951
6 - WASTEWATER (C-961
-------
TABLE 13. STATISTICAL SUMMARY OF CHRYSENE ANALYSES BY WATER TYPE
WATER 1
WATER 2
WATER 3
WATER 4
WATER 5
WATER 6
LOW YOUDEN PAIR
1 2
1
2
1 2
1
2
1 2
1
2
NUMBER OF DATA POINTS
II 12
12
13
1 1 It
1 1
12
13 13
14
14
TRUE CONC (C) UG/L
2.00 3 OO
2 . 00
3 . OO
2.00 3.00
2 . 00
3 . 00
2.00 3 . 00
2 . OO
3 00
MEAN RECOVERY
1.32 2.26
1 63
2.2 1
2.00 2.58
1 .57
2 90
1.89 3.06
2 03
2 77
ACCURACY <%REL ERROR»
-33.80 -24.54
- 18 45
-26.3 t
-0 13 - 13.65
- 2 1 . 64
-3 33
-5 35 1.95
I . 46
-7 69
OVERALL STD DEV
0.48 1.2 t
0 80
1 . 10
0 92 0.95
0 59
1 24
1.08 1.32
1 . 02
I 43
OVERALL REL STD DEV. X
35.94 53.24
49.26
49.59
46.01 36.73
37 52
42 78
57.OB 43 22
50.35
51 58
SINGLE STD DEV.
0 41
0
4 1
0 4 1
0
58
1 07
0 60
ANALYST REL DEV. X
22 .84
2 1
13
17 74
26
08
43 . 12
25 22
MEDIUM YOUDEN PAIR
3 4
3
4
3 4
3
4
3 4
3
4
NUMBER OF DATA POINTS
12 12
12
12
14 13
13
1 1
4 13
14
14
TRUE CONC (C) UG/L
20.00 28.00
20 . 00
28.00
20.OO 28.00
20 00
28 00
20.00 28.00
20.00
28 00
MEAN RECOVERY
15.00 19.50
15. 13
19.71
15 43 21 04
16 91
23 50
26.12 29.22
22 65
24 97
ACCURACY <%REL ERROR>
-24.97 -30 34
-24.36
-29.62
-22.86 -24.84
-15.46
- 16.06
30 60 4 37
13 26
- 10 83
OVERALL STD DEV (S)
8.21 11.03
7 46
10.87
6.56 7.92
7 00
8 23
13 52 14 60
12 OO
1 1 14
OVERALL REL STO DEV, %
54.71 56.55
49 46
54 . 15
42 49 37.66
4 1 .43
35 . 03
51 75 49 97
52 98
44 62
SINGLE STD DEV.
3 45
4
82
3 71
5
52
4 42
5 69
ANALYST REL DEV. X
19.99
26
54
20 37
27
32
15.96
23.91
HIGH YOUDEN PAIR
5 6
5
6
5 6
5
6
5 6
5
6
NUMBER OF DATA POINTS
13 13
*3
13
14 14
14
4
14 13
15
14
TRUE CONC (C> UG/L
60.00 40.00
60 00
40.00
80.OO 40.00
60 00
40 . 00
80 00 40.00
60.00
40 . 00
MEAN RECOVERY (X)
48.10 32.14
60.09
32.38
50.10 31 . 76
56.03
4 7.93
75 40 48.38
59.21
42 13
ACCURACY<*REL ERROR)
-19.83 -19.66
0. 15
- 19 . 04
-16.51 -20 81
-6 62
19 . 82
25 67 20.96
- 1 .32
5.32
OVERALL STD DEV (SI
27.74 15.70
32.40
19.44
29.98 18.65
2 1 84
27.52
34 38 22.74
28.21
15.41
OVERALL REL STO DEV. %
57.67 48.84
53.92
60.03
59.85 58.72
38 .98
57 . 43
45 60 47 00
47 66
36.57
SINGLE STD DEV. ISR)
16. 78
22
70
21 . 28
15
25
22 . 64
12 47
ANALYST REL DEV, %
4 1 .82
49
10
52 . 01
29
34
36.58
24 . 61
WATER LEGEND
1 - DISTILLED HATER
2 - TAP WATER
3 - SURFACE HATER
4 - HASTEHATER (C-Q4)
5 - HASTEHATER (C-95)
6 - WASTEWATER IC-96)
-------
TABLE 14. STATISTICAL SUMMARY OF BENZO(b)FLUORANTHENE ANALYSES BY WATER TYPE
HATER 1
WATER 2
WATER 3
WATER 4
WATER 5
WATER 6
LOM YOUDEN PAIR
1 2
1 2
1
2
1
2
1
2
1
2
NUMBER OF DATA POINTS
II II
12 13
13
13
13
14
12
(2
13
12
TRUE CONC < C» UC/L
0.20 0 30
0 20 0.30
0.20
0 30
0 . 20
0 . 30
0
20
0.30
0 . 20
0 30
MEAN RECOVERY
0. 06
0 . 05
0 . 04
0
04
0 06
0 04
ANALYST REL DEV. X
26 . 00
2 2 05
19.11
19
44
25 54
20 85
MEDIUM YOUDEN PAIR
3 4
3 4
3
4
3
4
3
4
3
4
NUMBER OF DATA POINTS
12 13
13 <2
15
14
15
13
13
14
14
14
TRUE CONC (C> UG/L
3 00 2 00
3.00 2 00
3 00
2 00
3 . 00
2 . 00
3
00
2 . 00
3 00
2 00
MEAN RECOVERY (X)
2.24 1.48
2.41 1 . 64
2 22
1 47
2 03
1.81
2
.41
I .69
2 58
1 .84
ACCURACY(XREL ERROR)
-25.17 -25 89
-19.81 -18 04
-25 86
-26 28
-32.22
-9 32
- 19
51
- 15.86
- 14 10
-8 00
OVERALL STD DEV (S)
0.73 0 62
0.91 0 65
0 89
0 47
0 . 70
0. 76
0
48
0 . 76
0. 79
0 72
OVERALL REL STD DEV. X
32.48 4 1 64
38.01 39.70
40 10
3 177
34 62
4 1 . 74
20
02
44 .93
30 . 70
39 33
SINGLE STD DEV. ISR)
0.39
0 51
0 . 29
0
30
0 42
0 62
ANALYST REL DEV. %
20 99
24 99
15 . 59
15
85
20 . 38
28 . 10
HIGH YOUOEN PAIR
5 6
5 6
5
6
5
8
5
6
5
6
NUMBER OF DATA POINTS
13 13
12 13
15
15
15
15
14
12
14
14
TRUE CONC (C) UG/L
8.00 1100
8 00 II 00
8 00
1 1 . 00
e. oo
1 1 . 00
8
. 00
1 1 . 00
8 00
1 1 . 00
MEAN RECOVERY
7.14 8.26
6 99 9.4 7
5 98
8 30
8 27
9 30
8
74
9 94
7 21
10.49
ACCURACY(XREL ERROR)
-10.73 -24 92
-12 56 -13 89
-25.25
-24 54
-21 57
- 15 45
9
20
-9.66
-9.91
-4 64
OVERALL STD DEV (S)
2.85 3 30
2 . 02 2 19
3 18
4 99
2 .35
3 85
4
69
4 39
3 . 12
3 . 85
OVERALL REL STD DEV. X
39.98 39 92
28 86 23 17
53 16
80 . 08
37 50
4 14 1
53
67
44 16
43 22
36 89
SINGLE STD DEV. (SR)
1 74
1 82
2 51
1
97
3 18
2 03
ANALYST REL DEV, X
22 82
22 09
35 . 22
25 .
30
34 . 04
22 96
MATER LEGEND
1 - DISTILLED MATER
2 - TAP MATER
3 - SURFACE MATER
4 - WASTEWATER (C-94)
5 - MASTEMATER IC-95)
0 - MASTEMATER
-------
TABLE 15. STATISTICAL SUMMARY OF BENZO( k)FLUORANTHENE ANALYSES BY WATER TYPE
WATER I WATER 2 WATER 3 WATER 4 WATER 5 WATER 6
LOM VOUDEN PAIR
1 2
1 2
1
2
1
2
1
2
1
2
NUMBER OF DATA POINTS
12 1 1
12 12
1 t
12
1 1
9
9
13
10
9
TRUE CONC IC) UG/L
0 12 0 15
0.12 0.15
0. 12
0 15
0 12
0. 15
0
12
0 15
0 12
0 . 15
MEAN RECOVERY (X)
0.07 0 10
0. 06 0 17
Oil
0 27
0 12
0 10
0
08
0 30
0 07
0 10
ACCURACY(XREL ERROR 1
-40.83 -33.70
-49.53 10 83
-7 65
83 22
-3 4 1
-34 67
-33
96
103 09
-39.08
-35 94
OVERALL STD DEV (S>
0.06 0.07
0.04 0 18
0 . 08
0 32
0.1!
0 03
0
03
0 30
0. 03
0 . 03
OVERALL REL STD DEV. *
85. 19 66.92
63.59 107.4 7
74 . 74
1 15 7 1
93 85
27 27
43
78
99 . 02
4 125
27.33
SINGLE STD DEV. (SR)
0.03
0.11
0 20
0.01
o
o
M
0 03
ANALYST REL DEV. %
38.33
95.00
10 1.91
1172
11.81
20 . 1 1
MEOIUM YOUDEN PAIR
3 4
3 4
3
4
3
4
3
4
3
4
NUMBER OF DATA POINTS
12 12
13 14
13
3
10
10
12
13
1 1
13
TRUE CONC (C> UC/L
1 40 1.10
1 40 110
1 40
1 . 10
1 40
1 10
1
.40
1 . 10
I 40
1 . 10
MEAN RECOVERY
0.63 0.42
0.68 1 28
1 . 32
0 93
0 30
0 . 28
1
30
0 . 83
0 83
101
OVERALL REL STD DEV. %
64.75 75.59
63.56 102.17
73.42
73 66
40 22
42.21
70
18
64 .45
51 05
85 17
SINGLE STD DEV.
0 22
0 87
0 32
0 13
0 69
0 28
ANALYST REL DEV. %
29.23
76.09
20 . 88
18 07
44 20
23.43
HIGH VOUDEN PAIR
5 8
5 6
5
6
5
6
5
6
5
6
NUMBER OF DATA POINTS
1 1 12
14 13
12
13
10
13
12
10
13
12
TRUE CONC (C> UG/L
4.00 6 00
4.00 6 00
4.00
6.00
4 . 00
6 00
4
.00
6.00
4 00
6.00
MEAN RECOVERY (XI
2.07 3.03
4 34 4.97
3. 16
5. 16
2 24
4 97
3
55
5.26
4 . 29
5.06
ACCURACY(%REL ERROR)
-48.38 -38 24
8 . 44 -17.21
-20.96
- 14 03
-44 06
- 17 13
- 1 1
25
- 12.30
7 35
- 15.58
OVERALL STD DEV (SI
126 3.12
4.4 1 3.90
2. 19
3 49
0.82
3. 19
1
80
3.01
3 70
2.63
OVERALL REL STD DEV. %
60.89 81.65
lot.73 78.57
69.34
67 . 73
36 53
64 . 2 1
SO
77
57.21
86 22
5191
SINGLE STD DEV, (SR)
1 .64
1 30
25
0 61
1 .89
0.99
ANALYST REL DEV. %
55.53
28 . 02
30 05
16 83
42 90
2 122
MATER LEGEND
1 - DISTILLED MATER
2 - TAP MATER
3 - SURFACE MATER
4 - MASTEMATER (C-94)
5 - MASTEMATER
-------
TABLE 16. STATISTICAL SUMMARY OF BENZO(a)PYRENE ANALYSES BY WATER TYPE
MATER 1
MATER 2
MATER 3
MATER 4
MATER 5
MATER 6
LOM YOUDEN PAIR
1 2
1 2
1
2
,
2
1
2
1
2
NUMBER OF DATA POINTS
13 12
13 13
15
15
14
14
13
14
13
12
TRUE CONC (C) UG/L
0.20 0 30
0.20 0.30
0
20
0 30
0.20
0 . 30
0 20
0 30
0 20
0 30
MEAN RECOVERY (X)
0. 12 0. IS
0.09 0 14
0
. 14
0 20
0. 15
0. 23
0. 14
0.2 1
0 15
0 2 1
ACCURACY(XREL ERROR)
-40.15 -40.94
-53.6» -53 96
-27
85
-33 09
-25 79
-24 62
-31 40
-29 62
-22.66
-31 08
OVERALL STD DEV (SI
0 0! 0.07
0 05 0 06
0
07
0 09
0 05
0 09
0 04
O il
0 06
0 . 04
OVERALL REL STD DEV, %
44 51 40.9B
55.95 43.69
49
. 03
4 2 60
34 50
39 68
30 94
51 IS
38.91
20 It
SINGLE STD DEV. (SR)
0. 05
0 03
0 04
0
04
0. 06
0 03
ANALYST REL DEV. *
34 . SO
23 . 93
2 1 53
23
49
33 90
19.33
MEDIUM YOUDEN PAIR
3 4
3 4
3
4
3
4
3
4
3
4
NUMBER OF DATA POINTS
13 14
14 14
15
16
15
14
15
14
14
15
TRUE CONC UG/L
12.00 15.00
12.00 15 00
12
00
15 00
12 . 00
15 00
12 00
15 00
12 00
15 00
MEAN RECOVERY (XI
B.43 7.35
7.16 8.51
7
32
9 75
7 7 1
9 88
9 28
10 54
7 67
10 32
ACCURACY(XREL ERROR)
-48 45 -50 90
-40.37 -43.25
-39
02
-34 99
-35 73
-34. 14
-22 66
-29 72
-36 11
31 22
OVERALL STD DEV
-------
TABLE 17. STATISTICAL SUMMARY OF DIBENZO(a,h)ANTHRACENE ANALYSES BY WATER TYPE
WATER 1
WATER 2
WATER 3
WATER 4
WATER 5
WATER 6
LOW YOUDEN PAIR
1
2
1 2
1 2
1 2
1
2
1
2
NUMBER OF DATA POINTS
1 1
12
12 1 1
12 13
II II
1 1
1 1
14
13
TRUE CONC
0.11
0 19
0. 18
0.09
0 24
0 14
ANALYST REL DEV. X
28.57
39 56
43 . 55
24 80
48 . 28
23 65
MEDIUM YOUDEN PAIR
3
4
3 4
3 4
3 4
3
4
3
4
NUMBER OF DATA POINTS
13
14
13 12
13 14
14 13
12
14
14
15
TRUE CONC (C) UG/L
e so
5 . 00
6 50 5.00
8.50 5 00
6 50 5 00
6
SO
5 . 00
a so
5 00
ME/m RECOVERY
1 . 10
0.99
2.55 0.97
2 10 2 02
2.18 1 32
1
16
2 . 00
2 . 43
1 32
OVERALL REL STD DEV, %
42.24
53.46
64.25 33.84
4 1 93 55.81
48 2 1 38.45
25
47
59.65
49. 76
42 75
SINGLE STD DEV.
0.46
1 .65
0.99
1 05
III
1 . 42
ANALYST REL DEV. X
20.77
48 . 19
22 .95
26 29
27.99
35.64
HIGH YOUDEN PAIR
5
6
.5 6
5 6
5 6
5
6
5
6
NUMBER OF DATA POINTS
13
14
13 13
14 14
14 13
12
12
15
IS
TRUE CONC UO/L
24 .00
20. 00
24 OO 20.00
24.00 20.00
24.00 20.00
24
OO
20 . 00
24 00
20. 00
MEAN RECOVERY (1)
9.85
9.24
19.79 15 35
14.80 13.66
16 81 14.90
21
76
14 82
16.52
16. 54
ACCURACY<«REL ERROR*
-58.99
-53.78
-17.56 -23.24
-38.32 -31.71
-29.97 -25 50
-9
32
-25 89
-31.18
- 17 30
OVERALL STD DEV (SI
4.39
3 . 72
10 01 4.31
8.55 5 18
5 77 2 56
7
78
4 88
7 40
7.40
OVERALL REL STO DEV. *
44.57
40 . 25
50.58 28.07
57.79 37 90
34 . 34 17.17
35
73
32.92
44 .81
44. 76
SINGLE STD DEV, (SRI
2 57
6.40
6. 39
3 43
4 66
5 53
ANALYST REL DEV. %
26.89
36.43
44 . 94
2 1 66
25 . 49
33.46
WATER LEGEND
1 - OISTILLED HATER
2 - TAP WATER
3 - SURFACE MATER
4 - WASTEWATER IC-94)
5 - WASTEWATER
8 - WASTEWATER (C-981
-------
2
1 2
40
18
03
31
3 I
4
13
00
. 4 t
89
15
60
6
4
00
46
08
91
27
18. STATISTICAL SUMMARY OF BENZO( g.h,i)PERYLENE ANALYSES BY WATER TYPE
MATER 1
HATER 2
WATER 3
WATER 4
WATER 5
1 2
1
2
1 2
1 2
1
2
13 13
10
1 I
15 14
II II
1
1 I
1.00 t 40
1
00
1 . 40
1
00 1 40
1
00 1 40
1
00
1 .40
0 73 0 93
0
66
0 89
0
82 0 80
0
66 0 98
0
85
1 14
26.88 -33 28
-33
81
-36 75
- 18
37 -43 11
-33
96 -29 82
- 15
35
- 18.57
0 60 0 55
0
30
0 24
0
48 0 26
0
17 0.23
0
27
0 . 30
82 01 59 13
30
16
26 62
58
88 32 72
25
94 23 86
32
16
26 4R
0 . 25
0 13
0. 18
0 17
0 28
?9 . 79
16 . 28
22 50
?0 29
28 32
3 4
3
4
3 4
3 4
3
4
14 14
1
10
14 15
12 10
12
13
14.00 10 00
14
00
10 00
14
00 10 00
14
00 10 00
14
00
10 00
5.58 4 36
10
00
6. 18
9
61 6 47
10
06 7 13
9
85
6 97
60.12 -56.35
-28
.55
-38 23
-31
33 -35 34
-28
17 -28 69
-29
62
-30.26
2.66 2 40
3
54
2 33
5
10 3 28
3
8 1 2 53
3
67
3 42
48.06 54 95
35
37
37 . 80
53
07 50 74
37
93 35 49
37
29
49 . 01
1 . 14
2 03
1 45
t 60
2 13
22 .88
25 . 06
18 07
18 68
25 . 32
5 6
5
6
5 6
5 6
5
6
14 14
9
1 1
16 16
12 12
13
1 1
35.00 50.00
35
00
50 00
35
00 50 00
35
00 50 00
35
00
50.00
19.52 20.33
25
07
39 05
2 1
79 38 34
23
65 38 67
28
90
32 28
44.23 -59 33
-28
38
-2 J 89
-37
75 -23 32
-32
43 -22 67
- 17
42
-35.43
14.t7 12.75
3
59
12 05
12
91 2 7 03
7
33 14 66
15
88
14 .96
72.59 62.71
14
3 1
30 . 84
59
2B 70 50
3 1
01 37.92
54
96
46. 35
5.37
7 05
17 . 62
9 50
8 92
26 93
2 1 . 99
58 . 6 1
30 49
29. 14
-------
TABLE 19. STATISTICAL SUMMARY OF INDEN0O,2,3-cd)PYRENE ANALYSES BY WATER TYPE
MATER I
MATER
MATER
MATER
MATER
MA TER
LOW VOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C> UC/l
MEAN RECOVERY (X)
ACCURACY(%REL ERROR I
OVERALL STO DEV 4 S >
OVERALL REL STD DEV. *
I 2
12 13
0.75 1.00
0.40 0.70
-46.99 -30.22
0 18 0.35
40.34 49.92
I 2
II 12
0.75 I 00
0.43 0.74
-42 I I -25 83
0 17 0.36
38 29 48 01
t 2
13 14
0 75 I 00
0 . 44 0 69
-41.22 -31.41
0 .13 0 . 26
28.91 37 83
I 2
12 13
0 75 I 00
0 47 0 77
-37.74 -23 25
0 17 0 28
35.77 36.16
I 2
II II
0 75 I 00
0 62 I 03
- 17 88 2 91
0 31 0 73
50 24 71 31
I 2
10 I I
0 75 I 00
0 48 0 80
-36 52 -19.69
0 15 0.34
31.93 42 83
SINGLE
ANALYST
STO DEV, (SRI
REL DEV. X
0 19
34 31
0 15
25.95
0. 12
2 1.19
0 10
16. 76
0 33
40 4 1
0 17
26 .82
MEDIUM YOUDEN PAIR
3 4
3 4
3
4
3
4
3
4
3 4
NUMBER OF DATA POINTS
13 12
II II
13
13
13
12
10
12
12 12
TRUE CONC (C) UQ/L
5.00 6.00
5 00 6.00
5 00
6 00
5 00
6 00
5
00
6 . 00
5
.00 6.00
MEA* RECOVERY (X)
3.05 3.11
3.49 3 95
3.33
3 52
3 09
3 . 50
4
32
5 24
4
25 3.93
ACCURACY(%R£L ERROR)
-3903 -48.21
-30 17 -34 12
-33 34
-41.37
-38 II
-41.74
- 13
64
-12.71
- 14
90 -34.47
OVERALL STD DEV
1 . 66 1.31
1 74 1 68
1 22
0 91
0 98
12 1
1
10
2 81
1
80 1.29
OVERALL REL STD DEV. %
54 40 42.17
49.85 42.42
36. 72
25 94
31 68
34 63
25
. 44
53 64
42
.28 32.83
SINGLE STD DEV. (SR)
0.59
1 .30
0.40
0
49
0 93
1 .27
ANALYST REL DEV. %
9.21
34 . 95
II 80
14
77
19.37
31.11
HIGH YOUDEN PAIR
5 6
5 6
5
6
5
6
5
6
5 6
NUMBER OF DATA POINTS
12 11
II II
13
13
14
14
12
10
12 13
TRUE CONC IC> UG/L
22.00 15.00
22 00 15.00
22 . 00
15 00
22 00
15 00
22
00
15.00
22
00 15.00
MEAN RECOVERY (X>
10.66 6.11
!556 10.45
12 . 39
9.01
14 . 16
12 00
26
39
12.08
16
.03 15 06
ACCURACY<%REL ERROR!
-51 53 -45.92
-29.25 -30 32
-43 67
-39 92
-35 63
-20 01
19
95
-19.48
-27
15 0 39
OVERALL STD DEV (S)
5 53 1.4 1
6 46 1.90
6.41
4 32
5.81
6 74
17
67
5.71
5
99 8 43
OVERALL REL STD DEV. %
51 82 17.38
4 1 . 53 18.14
51 . 72
47 . 97
4 1 . 04
56 . 1 7
60
. 94
4 7 . 26
37
37 55.99
SINGLE STD DEV. (SR)
3.56
3 86
4 16
4
09
10 77
6 17
ANALYST REL DEV. *
37.69
29.67
38.89
3 1
29
56 00
39 70
P-
vj
WATER LEGEND
1 - DISTILLED WATER
2 - TAP WATER
3 - SURFACE WATER
4 - WASTEWATER (C-94 1
5 - WASTEWATER (C-951
8 - WASTEWATER (C-961
-------
TABLE 20. SUMMARY OF THE TESTS FOR THE DIFFERENCES ACROSS HATER TYPES
Significance
F-Test
Effect Established
Statistically
by the 95Z
Water Type
Practical
Observed
Significant at
Confidence
Showing
Significance
Compound
F-Value
P[F>F OBS]
the 5Z Level?
Intervals?
Effect
Established
Naphtalene
2.18
0.02
Yes
No
No
Acenaphthylene
2.80
0.00
Yes
Yes
4
Yes
"Acenaphthene
1.94
0.04
Yes
No
No
Fluorene
0.54
0.86
No '
No
No
Phenanthrene
2.00
0.03
Yes
No
No
Anthracene
3.25
0.00
Yes
Yes
3,4,6
Yes
Fluoranthene
2.28
0.01
Yes
No
No
Pyrene
00
0.06
No
No
No
Benzo(a)anthrac ene
0.72
0.71
No
No
No
Chrysene
4.36
0.00
Yes
No
No
Benzo(b)fluoranthene
2.25
0.02
Yes
No
No
Benzo(k)fluoranthene
3.76
0.00
Yes
Yes
3,5,6
Yes
Benzo(a)pyrene
4.50
0.00
Yes
No
No
Dibenzo(a,h)anthracene
8.90
0.00
Ye9
Yes
5,6
Yes
Benzo(g,h,i)perylene
7.92
0.00
Yes
Yes
2,5
Yes
Indeno(l,2,3-cd)pyrene
6.00
0.00
Yes
Yes
5
Yes
-------
For six of the sixteen PNA compounds, a statistically significant effect
due to water type was established since the P[F>F OBS]<0.05 and zero was
contained within the 95 percent confidence interval for a specific water
type. As indicated in Section 4, the multiplicative model is a statistical
screening procedure and a detailed study of the regression equations, the
statistical summary, and raw data must be conducted to determine if there is
any effect of practical importance. The results of the examination of the
data for the 6 PNA compounds are summarized below:
A. Acenaphthylene - Wastewater C-94 was the only water type
to show statistical significence (intercept).
Comparison of the percent recoveries in Table 21 shows
68 and 83 for distilled and C-94 Wastewater,
respectively. As indicated previously, this difference
is due largely to the fact that all analysts analyzed
the distilled water samples first, and with added
experience, become more proficient with Wastewater C-94
(learning experience). This conclusion is further
reinforced by comparing the overall percent RSD of
distilled (42) and C-94 (32) and single-analyst percent
RSD of distilled (36) and C-95 (20), in Tables 22 and
23, respectively. Therefore, it was judged that the
statistical effect was of no practical importance.
B. Anthracene - Surface, and Wastewaters C-94 and C-96
indicated a statistically significant effect (inter-
cepts). Comparison of the percentage recovery shows
distilled water (50 percent) significantly lower than
these water types (^60 percent). Comparison of the
summary statistics for the low Youden pair show poorer
recovery and larger overall and single-analyst percent
RSD for distilled water. Significantly lower recovery
was also experienced at the middle Youden pair. Due to
the learning experience previously mentioned, it is
judged that the statistical significance is of no
49
-------
practical importance for these water types.
C. Benzo(k)fluoranthene - Surface, and Wastewaters C-95 and
C-96 were the water types that indicated statistical
significance. Examination of the percentage recoveries
in Table 21 show that the recovery of 59 percent for
this PNA in distilled water is much lower than for
surface water (103 percent), C-95 (110 percent) and C-96
(97 percent). This was attributed to the learning
experience previously mentioned. Therefore, it was
judged that the statistical significance was of no
practical importance.
D. Dibenzo(a,h)anthracene, benzo(g,h,i)perylene, and indeno
-(1,2,3-c, d)pyrene all show the same phenomenon of low
recoveries from distilled water which is attributed to
the learning effect. Therefore, it was concluded that
the observed statistical effects for these 3 PNA's were
of no practical importance.
A significant factor in the results obtained in this study is the
relative inexperience most of the analysts had in HPLC analysis. While gas
chromatography is widely used in commercial analytical laboratories
conducting environmental analysis, HPLC is used only to a limited extent.
The lack of HPLC experience, coupled with limited experience in conducting
Method 610 probably contributed to the poorer recovery and precision
encountered in the round robin study compared to the previous single
laboratory evaluation.
GENERAL DISCUSSION OF METHOD PERFORMANCE
The percentage recovery, overall percent RSD, and single-analyst percent
RSD are shovn in Tables 21-23. These values were calculated by inserting
specific analyte concentrations into the respective regression equations.
For comparison, the specific values chosen were the average of the
concentration range that BCL studied during the development of Method 610(8).
This interpretative approach has been taken due to the non-zero intercepts in
-50
-------
TABLE 21. PERCENT RECOVERY FOR VARIOUS UATER TYPES
Percent Recovery in Given Water Types Average Recovery BCL
Concentrations** Wastewater For All Recovery
Coapound ug/L Distilled Tap Surface C-94 C-95 C-96 Water Types Data^*)
Naphthalene
45
55
59
58
64
60
63
60
78
Acenaphthylene(c)
350
68
70
73
83*
75
82
75
93
Acenaphthenelc)
25
54
45
51
57
58
62
55
88
Fluorene^c-
14
52
50
55
60
58
57
55
90
Phenanthrene
4.5
51
55
64
65
62
60
60
98
Anthracene
10
50
43
60*
66*
61
67*
58
93
£luoranthene
1.5
73
69
62
75
71
76
71
116
Pyrene
4.5
66
70
72
71
72
77
71
96
Benzo(a)anthrac ene
0.6
81
85
93
93
74
76
84
89
Chrysene
4.0
73
80
87
90
108
99
90
88
Benzo(b)fluoranthene
0.3
81
83
76
77
90
90
83
97
Benzo(k)fluoranthene
3.0
59
97
103*
62
110*
97*
88
94
Benzo(a)pyrene
0.3
59
47
68
74
69
73
65
94
Dibenzo(a,h)anthracene
1.0
52
77
68
66
79*
87*
72
87
Benso(gth,i)perylene
2.0
59
68*
70
70
78*
79
71
86
Indeno(l,2,3-cd)pyrene
1.0
60
65
62
68
90*
72
70
94
(a) Percent recovery ia defined aa 100^*^* where b and a are the slope and intercept, respectively, in the regression
equation Y » bx + a; Y » mean recovery and X " true concentration.
(b) Data obtained during method development study, see reference (8).
(c) Laboratories were instructed co determine these PNA compounds using UV detection and the remaining compounds using
fluorescence detection.
* Recovery for waters which indicated statistically significant matrix effects.
** The specific analyte concentration inserted into the regression equation and approximates the average concentration
used by BCL to obtain recovery data during method development.
-------
TABLE 22. OVERALL PERCENT RELATIVE STANDARD DEVIATION
FOR VARIOUS WATER TYPES
Compound
Overall
Percent
RSD(«) in
Given Water Types
Average
For All
Water Types
Distilled
Tap
Surface
C-94
Wastewater
C-95
C-96
Naphthalene
44
42
45
37
28
40
39
Acenaphthylene
42
44
30
32*
36
23
34
Acenaphthene
63
51
50
49
48
40
50
Fluorene
29
48
42
37
42
44
40
Phenanthrene
36
29
16
19
27
28
26
Anthracene
50
43
22*
33*
28
21*
33
Fluoranthene
35
33
43
34
31
41
36
Pyrene
42
42
26
25
28
29
33
Benso(a)anthracene
38
47
23
43
34
41
38
Chrysene
48
52
44
42
50
49
48
Benso(b)fluoranthene
38
28
61
30
35
33
38
Bens o(k)f1uoranthene
70
91
76*
48
68*
68*
70
Benso(a)pyrene
47
53
47
39
40
32
43
Dibenzo(a,h)anthracene
51
49
46
35
39*
54*
46
Benzo (g, h, i) pery lene
66
29*
51
30
37*
39
42
Indeno(1,2,3-cd)pyrene
44
41
32
36
54*
37
41
(a) Overall percent relative standard deviation is defined aa 100^bx^* in the regression
equation Y bz ~ a, where X is mean recovery and Y ia total interlaboratory standard
deviation. Analyte concentrations inserted into the regression equation for overall
RSD were the mean recoveries shown in Table 21.
* Recovery for waters which indicated statistically signficant matrix effects.
52
-------
TABLE 23. SINGLE-ANALYST PERCENT RELATIVE STANDARD DEVIATION
FOR VARIOUS WATER TYPES
Compound
Distilled
Tap
Surface
C-94
Wastewater
C-95 C-96
For All
Water Typea
Naphthalene
38
37
31
24
21
32
31
Acenaphthylene
36
38
27
20*
31
17
28
Acenaphthene
45
31
29
29
26
30
32
Fluorene
54
42
28
44
52
36
43
Phenanthrene
30
30
11
27
14
16
21
Anthracene
46
36
23*
34*
21
20*
30
Fluoranthene
28
24
23
15
16
35
24
Pyrene
30
26
19
22
26
20
24
Benzo(«)anthracene
36
48
16
29
19
18
28
Chrysene
26
28
24
27
35
25
28
Benzo(b)fluoranthene
30
CM
22
21
24
22
24
Benzo(k)fluoranthene
43
50
24*
17
44*
22*
33
Benzo(a)pyrene
32
22
19
25
36
20
26
Dibenzo(a,h)anthracene
28
41
40
24
40*
28*
34
Benzo(g,h,i)perylene
28
20*
28
22
28*
23
25
Indeno(l,2,3-cd)pyrene
32
27
21
16
38*
27
27
(a) Single analyat percent relative atandard deviation ia defined aa 100<»» c) in the
regression equation Y - dx + c, where X ia mean recovery and Y ia aingle-analyat
atandard deviation. Analyte concentrations inaerted into the regreaaion equation for
single-analyat RSD were the mean recoveries shown in Table 21.
* Precision for waters which indicted statiatical significant matrix effects.
53
-------
the regression equations for several of the compounds.
Accuracy of the Method
The percentage recovery of all PNA's for a specific water type ranged
from 43-110 percent. The average recovery for all water types for each PNA
ranged from 55-90 percent with acenaphthene and chrysene exhibiting the
lowest and highest recovery, respectively.
During the method development phase, BCL determined the percentage
recovery for each of the PNA's (8). These recoveries (Table 21) were
generally at the lower end of the concentration range of the method
validation study, and were obtained from spiked wastewater samples.
Comparing these results with the average percent recovery for all water types
at similar concentrations, it is evident that the percentage recoveries for
the method study are significantly lower than the method development
recoveries for most PNA's. Chrysene and benzo(k)fluoranthene appear to be
the exceptions, however, it should be noted that chrysene and
benzo(k)fluoranthene have excessively high recoveries of 108 and 110 percent,
respectively, for Wastewater C-95. Examination of the summary statistics for
chrysene indicates an excessive positive bias for the medium and high Youden
pairs. Further examination of the chrysene raw data for these Youden pairs
indicates that Laboratories #108, #110, and #113 reported data as high as 285
percent of the true value for the middle Youden pair and Laboratories #103,
#110, and #117 as high as 252 percent of the true values for the high Youden
pair. Such data is not rejected by the outlier test, therefore, they tend to
distort the percentage recovery (bias) in the summary statistics and
subsequently the slope of the regression equation. Also, since there appears
to be no significant background contamination in this water type, the random
errors are probably due to dilution, calibration or calculation errors. A
similar situation exists for benzo(k)fluoranthene, Wastewater C-95, low
Youden pair, in which the percentage recoveries were as high as 673 percent,
and for surface water in which the low Youden pair recovery was as high as
693 percent.
The reason for the overall lower recoveries compared to the single
laboratory data obtained during method development is not clear. However, it
54
-------
should be noted that the recoveries of the PNA's for distilled water were
generally lower than for wastewater samples, and especially pronounced for
those PNAs eluting after benzo(a)anthracene. Intuitively, one would
anticipate that the data would be somewhat better for distilled water, since
there is little chance of interferences or matrix effects. Since the
distilled water data were in all cases collected prior to wastewater data,
the analyst were more experienced in utilizing the method when they analyzed
the wastewater samples. This may have resulted in a learning curve effect
which improved the data for wastewater as compared to distilled water. This
effect may have been a result of a general lack of familiarity with HPLC as
well as the details of Method 610.
Precision of the Method
The overall and single operator percent relative standard deviations, in
general, for a specific PNA were similar for the various water types. The
overall and single-analyst percent relative standard deviations ranged from
16-91 percent and 11-50 percent, respectively.
Based upon the average percent overall relative standard deviation for
al-1 water types, acenaphthylene was the most precise (34 percent RSD) and
benzo(k)fluoranthene the least precise (70 percent RSD). The average single-
analyst percent Relative Standard Deviation for all water types ranged from
21-34 percent. Anthracene was the most precise and dibenzo(a,h)anthracene
the least precise.
Operational Problems
Several operational problems were reported by the laboratories while
conducting Method 610 analyses, the most relevant of which were:
Concentration of the acetonitrile to a final volume of
1 mL was time consuming. Concentration to approximately
2 mL was found to be much more appropriate by some of
the laboratories. In addition, several laboratories
reported "bumping" problems during the concentration
step which led to significant loss of all analytes.
55
-------
Bubbles (due Co solvent evaporation) were found in the
silica gel column, although this did not appear to
distort the elution pattern.
HPLC column performance was found to be somewhat
variable. Some laboratories had to try two or three
reverse phase HPLC columns* supplied by Perkin-Elmer
before they found one that would adequately separate
benzo(g,h,Operylene and dibenzo(a,h)anthracene. Perkin
-Elmer's current QA procedures supposedly will eliminate
this problem. Other compounds were generally well
resolved on these reversed phase columns.
Some of the older HPLC systems did not deliver stable
gradients and, therefore, retention times for the PNA's
were variable.
Fluorescence detector response for the various compounds
was quite different from one type to the next. Two
laboratories used filter type excitation, rather than a
grating monochrometor, which produces a much higher
relative response for anthracene causing it to interfere
with fluoranthene. Mercury vapor lamps were found to
give a low output at 280 nm, resulting in low response
for all compounds. Use of a phosphor coated lamp
improved the situation somewhat. In general, fluores-
cence detectors employing deuterium lamps and grating
monochrooators for excitation gave consistent results.
However, close inspection of the data did not reveal any
systematic differences between deuterium source/grating
instruments and mercury source/filter instruments.
* Reverse phase column, HC ODS SilX, 250 mm x 2.6 mnt ID.
*56
-------
REFERENCES
1. Code of Federal Regulations, 40: Part 136, October 16, 1973.
2. U.S. Code Congressional and Administrative News, 2> 1977, 95th Congress,
First Session 1977.
3. Youden, W. J., Statistical Techniques for Collaborative Tests.
Statistical Manual of the Association of Official Analytical Chemists,
1975.
4. Outler, E. C. and McCreery, J. H., Interlaboratory Method Validation
Study: Program Documentation. Battelle Columbus Laboratories, 1982.
5. Thompson, W. R., Annals of Mathematical Statistics, Vol. 6, 1935, p. 214.
6. Draper, N. R. and Smith, H., Applied Regression Analysis, 2nd Edition,
John Wiley and Sons, New York, 1981.
7. Bishop, T., Brydon, F. and Outler, E. C., Battelle Report for EPA
contract 68-03-2624, Development of Statistical Technique to Compare
Analytical Methods Across Wastewaters.
8. Riggin, R. and Cole, T. F., "Determination of Method Detection Limits and
Analytical Curve for EPA Method 610-PAH", EPA Contract NO. 68-03-2624.
57
-------
APPENDIX A
POLYNUCLEAR AROMATIC HYDROCARBONS
METHOD 610
1. Scope and Application
1.1 This method covers the determination of certain polynuclear
aromatic hydrocarbons (PAH). The following parameters may be
determined by this method:
Parameter
Storet No.
Parameter
Storet No.
Acenaphthene
34205
Chrysene
34320
Acenaphthylene
34200
DibenzoCah)anthracene
34556
Anthracene
34220
Fluoranthene
34376
Benzo(a)anthrac ene
34526
Fluorene
34381
Benzo(a)pyrene
34247
Indeno(l,2,3-cd)pyrene
34403
Benzo(b)fluoranthene
34230
Naphthalene
34696
Benz o(gh i)pery1ene
34521
Phenanthrene
34461
Benzo(k)fluoranthene
34242
Pyrene
34469
1.2 This method is applicable to the determination of these compounds
in municipal and industrial discharges. It is designed to be used
to meet the monitoring requirements of the National Pollutant
Discharge Elimination System (NPDES). As such, it presupposes a
high expectation of finding the specific compounds of interest. If
the user is attempting to screen samples for any or all of the
compounds above, he must develop independent protocols for the
verification of identity.
58
-------
1.3 The sensitivity of this method is usually dependent upon the level
of interferences rather than instrumental limitations. The limits
of detection listed in Table A-l represent sensitivities that can
be achieved in wastewaters.
1.4 This method is recommended for use only by experienced residue
analysts familiar with High Performance Liquid Chromatography
(HPLC) or under the close supervision of such qualified persons.
Summary of Method
2.1 A 1-liter sample of wastewater is extracted with methylene chloride
using separatory funnel techniques. The extract is dried and con-
centrated to a volume of 10 mL or less. HPLC conditions are des-
cribed which allow for the accurate measurement of the compounds in
the extract.
2.2 If interferences are encountered, the method provides a selected
general purpose cleanup procedure to aid the analyst in their
elimination.
Interferences
3.1 Solvents, reagents, glassware, and other sample processing hardware
may yield discrete artifacts and/or elevated baselines causing mis-
interpretation of chromatograms. All of these materials must be
demonstrated to be free from interferences under the conditions of
the analysis. Specific selection of reagents and purification of
solvents by distillation in all-glass systems may be required.
3.2 Interferences coextracted from the samples will vary considerably
from source to source, depending upon the diversity of the
industrial complex or municipality being sampled. While general
cleanup techniques are provided as part of this method, unique
samples may require additional cleanup approaches to achieve the
sensitivities stated in Table A-l.
59
-------
TABLE A-l. HIGH PERFORMANCE LIQUID CHROMATOGRAPHY(a) OF PNAs
Retention Time Detection Limit,Pg/L^b)
Compound (minutes) UV Fluorescence
Naphthalene
16.17
2.5
20.0
Acenaphthylene
18.10
5.0
100.0
Acenaphthene
20.14
3.0
4.0
Fluorene
20.89
0.5
2.0
Phenanthrene
22.32
0.25
1.2
Anthracene
23.78
0.10
1.5
Fluoranthene
25.00
0.50
0.05
Pyrene
25.94
0.10
0.05
Benzo(a)anthr acene
29.26
0.20
0.04
Chrysene
30.14
0.20
0.5
Benzo(b)fluoranthene
32.44
1.0
0.04
Benzo(k)fluoranthene
33.91
0.30
0.04
Benzo(a)pyrene
34.95
0.25
0.04
Dibenzo(a,h)anthracene
37.06
1.0
0.08
Benzo(g,h,i)perylene
37.82
0.75
0.2
Indeno(1,2,3-cd)pyrene
39.21
0.30
0.1
( fl)
HPLC conditions: Reverse phase HC-ODS Sil-X 2.6 x 250 mm Perkin-Elmer
column; isocratic elution for 5 min. using 40% acetonitrile/60%
water, then linear gradient elution to 100% acetonitrile over 25
minutes; flow rate is 0.5 mL/min.
Detection limit is calculated from the minimum detectable HPLC response
being equal to five times the background noise, assuming an
equivalent of a 2-mL final volume of the 1-liter sample extract, and
assuming an HPLC injection of 2 uL.
60
-------
3.3 The extent of interferences that may be encountered using liquid
chromatographic techniques has not been fully assessed. Although
the chromatographic conditions described allow for a unique
resolution of the specific PAH compounds covered by this method,
other PAH compounds may interfere.
4. Apparatus and Materials
4.1 Sampling equipment, for discrete or composite sampling.
4.1.1 Grab sample bottle - amber glass, pint or quart volume.
French or Boston Round design is recommended. The con-
tainer must be washed and solvent rinsed before use to
minimize interferences.
4.1.2 Bottle caps - Threaded to screw on sample bottles. Caps
oust be lined with Teflon. Foil may be substituted if
sample is not corrosive.
4.1.3 Compositing equipment - Automatic or manual compositing
system. Must incorporate glass sample containers for the
collection of a minimum of 250 mL. Sample containers must
be kept refrigerated during sampling. No tygon or rubber
tubing may be used in the system.
4.2 Separatory funnel - 2000 mL, with Teflon stopcock.
4.3 Drying column - A 20 mm ID pyrex chromatographic column with coarse
frit.
4.4 Kuderna-Danish (K-D) Apparatus
4.4.1 Concentrator tube - 10 mL, graduated (Rontes K-570050-1025
or equivalent). Calibration must be checked. Ground glass
stopper (size 19/22 joint) is used to prevent evaporation
of extracts.
4.4.2 Evaporative flask - 500 mL (Rontes R-57001-0500 or
equivalent). Attach to concentrator tube with springs.
(Rontes R-662750-0012).
61
-------
4.4.3 Snyder column - three-ball macro (Kontes K-50300-0121 or
equivalent.
4.4.4 Snyder column - two-ball micro (Kontes K-569001-0219 or
equivalent).
4.4.5 Boiling chips - extracted, approximately 10/40 mesh.
4.5 Water bath - Heated, with concentric ring cover, capable of temp-
erature control ( + 2°C). The bath should be used in a hood.
4.6 HPLC Apparatus:
4.6.1 Gradient pumping system, constant flow.
4.6.2 Reverse phase column, HC-ODS Sil-X, 250 mm x 2.6 mm ID
(Perkin Elmer No. 809-0716 or equivalent).
4.6.3 Fluorescence detector, Aex 280 nm and Xem 389 ran.
4.6.4 UV detector, 254 nm, coupled to fluorescence detector.
4.6.5 Strip chart recorder compatible with detectors, 250 mm (A
data system for measuring peak areas is recommended).
4.7 Chromatographic column - 250 mm long x 10 mm ID with coarse fritted
disc at bottom and Teflon stopcock.
5. Reagents
5.1 Preservatives:
5.1.1 Sodium hydroxide - (ACS) 10 N in distilled water.
5.1.2 Sulfuric acid - (ACS) Mix equal volumes of conc. H2SO4
with distilled water.
5.1.3 Sodium thiosulfate - (ACS) granular.
5.2 Methylene chloride, Pentane, Cyclohexane, High Purity Water-HPLC
quality, distilled in glass.
5.3 Sodium Sulfate - (ACS) Granular, anhydrous (purified by heating at
400°C for 4 hrs.).
62
-------
5.4 Stock standards - Prepare stock standard solutions at a concentra-
tion of 1.00 ug/uL by dissolving 0.100 grams of assayed reference
material in pesticide quality isooctane or other appropriate sol-
vent and diluting to volume in a 100mL ground glass stoppered
volumetric flask. The btock solution is transfered to ground glass
stoppered reagent bottles, stored in a refrigerator, and checked
frequently for signs of degradation or evaporation, especially just
prior to preparing working standards from them.
5.5 Acetonitrile - Spectral quality.
5.6 Silica gel - 100/200 mesh desiccant (Davison Chemical grade 923 or
equivalent). Before use, activate for at least 16 hours at 130°C
in a foil covered glass container.
6.Calibration
6.1 Prepare calibration standards that contain the compounds of inter-
est, either singly or mixed together. The standards should be
prepared at concentrations covering two or more orders of magnitude
that will completely bracket the working range of the chromato-
graphic system. If the sensitivity of the detection system can be
calculated from Table A-l as 100 ug/L in the final extract, for
example, prepare standards at 10 ug/L, 50 ug/L, 100 yg/L, 500 Mg/l>,
etc., so that injections of 1-5 yL of each calibration standard
will define the linearity of the detector in the working range.
6.2 Assemble the necessary liquid chromatographic apparatus and
establish operating parameters equivalent to those indicated in
Table A-l. By injecting calibration standards, establish the
sensitivity limit of the detectors and the linear range of the
analytical systems for each compound.
6.3 Before using any cleanup procedure, the analyst must process a
series of calibration standards through the system to validate
elution patterns and the absence of interferences from the
reagents.
63
-------
7. Quality Control
7.1 Before processing any samples, the analyst should demonstrate
through the analysis of a distilled water method blank, that all
glassware and reagents are interference-free. Each time a set of
samples is extracted or there is a change in reagents, a method
blank should be processed as a safeguard against laboratory
contamination.
7.2 Standard quality assurance practices should be used with this
method. Field replicates should be collected to validate the
precision of the sampling technique. Laboratory replicates should
be analyzed to validate the precision of the analysis. Fortified
samples should be analyzed to validate the accuracy of the
analysis. Where doubt exists over the identification of a peak on
the chromatogram, confirmatory techniques such as fraction collec-
tion and GC-tnass spectroscopy should be used.
8. Sample Collection, Preservation, and Handling
8.1 Grab samples must be collected in glass containers. Conventional
sampling practices should be followed, except that the bottle must
not be prewashed with sample before collection. Composite samples
should be collected in refrigerated glass containers in accordance
with the requirements of the program. Automatic sampling equipment
must be free of tygon and other potential sources of contamination.
8.2 The samples must be iced or refrigerated from the time of collect-
tion until extraction. Chemical preservatives should not be used
in the field unless more than 24 hours will elapse before delivery
to the laboratory. If the samples will not be extracted within 48
hours of collection, adjust the sample to a pH range of 6.0-8.0
with sodium hydroxide or sulfuric acid and add 35 mg sodium thio-
sulfate part-per-million of free chlorine per liter.
8.3 All samples must be extracted within 7 days and completely analyzed
within 30 days of collection.
64
-------
9. Sample Extraction
9.1 Mark the water meniscus on the side of the sample bottle for later
determination of sample volume. Quantitatively pour the entire
sample into a two-liter separatory funnel. Check the pH with wide-
range paper and adjust to within the range of 5-9 with sodium
hydroxide or sulfuric acid.
9.2 Add 60 mL methylene chloride to the sample bottle, and shake 30
seconds to rinse the walls. Transfer the solvent into the
separatory funnel, and extract the sample by shaking the funnel for
two minutes with periodic venting to release vapor pressure. Allow
the organic layer to separate from the water phase for a minimum of
ten minutes. If the emulsion interface between layers is more than
one-third the size of the solvent layer, the analyst must employ
mechanical techniques to complete the phase separation. The
optimum technique depends upon the sample, but may include stir-
ring, filtration of the emulsion through glass wool, or centri-
fugation. Collect the methylene chloride extract in a 250-mL
Ehrlenmeyer flask.
9.3 Add a second 60-mL volume of methylene chloride to the sample
bottle and complete the extraction procedure a second time,
combining the extracts in the Ehrlenmeyer flask.
9.4 Perform a third extraction in the same manner. Pour the combined
extract through a drying column containing 3-4 inches of anhydrous
sodium sulfate, and collect it in a 500-mL Kuderna-Daniah (K-D)
flask equipped with a 10 mL concentrator tube. Rinse the
Ehrlenmeyer flask and column with 20-30 mL methylene chloride to
complete the quantitative transfer.
9.5 Add 1-2 clean boiling chips to the flask and attach a three-ball
Snyder column. Prewet the Snyder column by adding about 1 mL
methylene chloride to the top. Place the K-D apparatus on a
steaming hot (60-6S°C) water bath so that the concentrator tube is
partially immersed in the hot water, and the entire lower rounded
65
-------
surface of the flask is bathed in steam. Adjust the vertical
position of the apparatus and the water temperature as required to
complete the concentration in 15-20 minutes. At the proper rate of
distillation the balls of the column will actively chatter but the
chambers will not flood. When the apparent volume of liquid
reaches 1 mL, remove the K-D apparatus and allow it to drain for at
least 10 minutes while cooling. Remove the Snyder column and rinse
the flask and its lower joint into the concentrator tube with 1-
2 mL of methylene chloride. A 5-mL syringe is recommended for this
operation. Stopper the concentrator tube and store refrigerated if
further processing will not be performed immediately.
9.6 Determine the original sample volume by refilling the sample bottle
to the mark and transferring the liquid to a 1000 mL graduated
cylinder. Record the sample volume to the nearest 5 mL.
9.7 If the sample requires cleanup before chromatographic analysis,
proceed to Section 10. If the sample does not require cleanup, or
if the need for cleanup is unknown, analyze an aliquot of the
extract according to Section 11.
10. Cleanup and Separation
10.1 Before the silica gel cleanup technique can be utilized, the
extract solvent must be exchanged to cyclohexane. Add a 1-10-mL
aliquot of sample extract (in methylene chloride) and a boiling
chip to a clean K-D concentrator tube. Add 4 mL cyclohexane and
attach a micro-Snyder column. Prewet the micro-Snyder column by
adding 0.5 mL methylene chloride to the top. Place the micro K-D
apparatus on a boiling (100°C) water bath so that the concentrator
tube is partially immersed in the hot water. Adjust the vertical
position of the apparatus and the water temperature as required to
complete concentration in 5-10 minutes. At the proper rate of
distillation the balls of the column will actively chatter but the
chambers will not flood. When the apparent volume of the liquid
reaches 0.5 mL, remove the K-D apparatus and allow it to drain for
66
-------
at least 10 minutes while cooling. Remove the micro-Snyder column
and rinse its lower joint into the concentrator tube with a minimum
of cyclohexane. Adjust the extract volume to about 2 mL.
10.2.1 Prepare a slurry of lOg activated silica gel in methylene
chloride and place this in a 10 mm ID chromatography
column. Gently tap the column to settle the silica gel and
elute the methylene chloride.
10.2.2 Preelute the column with 40 mL pentane. Discard the eluate
and just prior to exposure of the sodium sulfate layer to
the air, transfer the 2 mL cyclohexane sample extract onto
the column, using an additional 2 mL of cyclohexane to com-
plete the transfer.
10.2.3 Just prior to exposure of the sodium sulfate layer to the
air, add 25 mL pentane and continue elution of the column.
Discard the pentane eluate.
10.2.4 Elute the column with 25 mL of 402 methylene chloride/60%
pentane and collect the eluate in a 500 mL K-D flask
equipped with a 10 mL concentrator tube. Elution of the
column should be at a rate of about 2 mL/min.
10.2.5 Concentrate the collected fraction to less than 10 mL by K-
D techniques as in 9,5, using pentane to rinse the walls of
the glassware. Proceed with HPLC analysis.
High Performance Liquid Chromatography HPLC
11.1 Table A-l summarizes the recommended HPLC column materials and
operating conditions for the instrument. Included in this table
are estimated retention times and sensitivities that should be
achieved by this method. An example of the separation achieved by
this column is shown in Figure A-l. Calibrate the system daily
with a minimum of three injections of calibration standards.
67
-------
11.2 To the extract, add A mL acetonitrile and a new boiling chip, then
attach a micro-Snyder column. Increase the temperature of the hot
water bath to 95-100°C. Concentrate the solvent as above. After
cooling, remove the micro-Snyder column and rinse its lower joint
into the concentrator tube with about 0.2 mL acetonitrile. Adjust
the extract volume to 1.0 mL.
11.3 Inject 2-5 pL of the sample extract with a high pressure syringe.
Smaller Cl.O uL) volumes can be injected in automatic devices are
employed. Record the volume injected to the nearest 0.05 pL, and
the resulting peak size, in area units.
11.4 If the peak area exceeds the linear range of the system, dilute the
extract and reanalyze.
11.5 If the peak area measurement is prevented by the presence of inter-
ferences, further cleanup is required.
11.6. The UV detector is recommended for the determination of naphthalene
and acenaphthylene and the fluorescence detector is recommended for
the remaining PAHs.
12. Calculations
11.1 Determine the concentration of individual compounds according to
the formula:
where A * Calibration factor for chromatographic system, in
namograms material per unit peak height.
B " Peak size in injection of sample extract, in area units
Vi « Volume of extract injected (yL)
Vfc Volume of total extract (uL)
Vs * Volume of water extracted (mL).
11.2 Report results in micrograms per liter without correction for
recovery data. When duplicate and spiked samples are analyzed, all
data obtained should be reported.
Concentration, pg/L «*
68
-------
12. Accuracy and Precision
12.1 Data is not available at this time.
69
-------
s
I
cr
x
M
PAII MIXTURE
a
i
Z
If
*
c
«/
u
<
U-V ^ fil'jf i{M
<1
c
- If
< I !? C
fr
X
U
d <
x
3 a
CP
u*
A A
10
20
30
40 min.
Figure A-l. HPLC-Fluorescence of PNAs on reverse phase
column, HC-ODS Sil-X, 250 mm x 2.6 mm ID
(Perkin Elmer No. 809-0716 or equivalent).
For conditions, see Table A-l.
70
Reproduced from
best available copy.
-------
APPENDIX B
INSTRUCTIONS TO ANALYST
The following instructions were sent to the analyst prior to the
start of the method study.
The PNA procedure is rather straighforward and easy to conduct.
However, some of the compounds are light sensitive and thus exposure to light
should be kept at a minimum. All sample extracts should be stored in the
dark prior to analysis. The column clean-up step should be checked to make
sure that proper elution is occurring.
The HPLC system performance is important since a large number of
compounds must be separated. The equilibration time (at 40% acetonitrile/60%
water) between runs should be at least 25 minutes and should be consistent
from run to run. Solvents for HPfcC must be filtered through a submicron
filter and then degassed, either by heating or by a helium purge, to prevent
bubble formation.
The sensitivity of the detectors should be checked daily. The
following amounts of materials on column give a 1/2 scale peak at 0.5% full
scale noise;
Naphthalene - 100 ng
Acenaphylene - 150 ng
Acenaphthene - 100 ng
Fluorene - 80 ng
Phenanthrene - 50 ng
Anthracene - 60 ng
Fluoranthene - 2 ng
Pyrene - 20 ng
Benzo(a)anthracene - 1.6 ng
Benzo(k)fluoranthene - 1.6 ng
Benzo(a)pyrene - 1.6 ng
Dibenzo(a,h)anthracene - 32. ng
Benzo(ghi)perylene - 8 ng
Indeno(l,2,3-cd)pyrene - 4 ng
71
-------
Procedure for Spiking Water Samples
All wastewater samples for all categories will be supplied in one
(l)-quart bottles with Teflon screw caps. To spike the sample, place a
magnetic stirbar in the bottle, add 1 mL of the ampule concentrate, then cap
and stir 15 minutes using a magnetic stirrer. Transfer the contents of the
bottle to a 2-liter separatory funnel and proceed with the analysis as des-
cribed in Method 610, PNAs. In calculating results, assume the volume of the
sample to be one liter.
Chrysene Impurity
The impurity present in most of the chrysene standards and which
was discussed at the prestudy conference has been determined to have the
following characteristics:
It co-elutes with fluorene on most HC-ODS columns.
It has strong fluorescence but relatively weak UV absorbance
under the detector conditions specified in Method 610. (i.e.,
it does not interfere with the determination of fluorene by
UV).
It is removed by the silica gel cleanup procedure specified in
Method 610.
A satisfactory chrysene standard may be prepared by the
following procedure:
A column containing 50 grams of silica gel (activated at
130°C) was eluted with 100 mL of methylene chloride and then
100 mL of petroleum ether. A solution (25 mL) of 40%
methylene chloride in petroleum ether containing 25 mg of
chrysene was applied to the column. The chrysene was then
eluted with 50 mL of 40% methylene chloride in petroleum
ether. This eluate was then evaporated just to dryness. The
product melted sharply at 252°C (literature value 254°C).
Both fluorescence and UV/HPLC gave a single peak. The peak
72
-------
areas obtained for chrysene before and after cleanup agree
within 2X (experimental error), thus indicating that the
impurity is present at less than 2%,
Since the impurity is not present at a significant level (i.e.
2% or less), and does not interfere with the fluorene
determination by UV, it would be best simply to determine
fluorene by UV.
Alternatively, since the impurity is removed by the silica gel
cleanup, fluorescence detection may be used for the fluorene
determination, provided an interference free chrysene standard
is used for calibration of the instrument.
73
-------
APPENDIX C
TABLE
C-l.
RAM
DATA FOR NAPTHALENE ANALYSIS
BY
WATER
TYPE
LOW
YOUDEN
PAIR,
UG/L
DISTILLED
water
TAP
WATER
SURFACE
WATER
WASTEWATER
-------
APPENDIX C (Continued)
TABLE C-l. RAW DATA FOR NAPTHALENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
OISTIILEO HATER
TAR
MATER
SURFACE
MATER
WASTEWATER
(C-94)
WASTEWATER
tC-95)
WASTEWATER
t C - 90
AMPUL NO:
3
4
3
4
3
4
3
4
3
4
3
4
TRUE CONC:
110.00
90 . OO
1 10. 00
90 . 00
MO . 00
90 . 00
t10.00
90 . 00
I 10.00
90 . 00
110 00
90 . 00
LAB NUMSE*
101
99 00*
240.00*
104 00*
100 00
86 . 00
74 . 00
78 . 00
74 00
34 00
59 00
58 . 00
50 . 00
102
45. SO
47.30
82 10
14 30
55 30
2. to
76 . 80
51 60
82 10
44 .60
5. 15
45 20
103
1200*
10 00*
6.60
62 00
30.00*
28.00*
24 . 00
60 . 00
20¦00*
0 00*
23 . 00
4 7 00
104
57.00
52.00
52.00
02 . 00
54.00
48 . 00
77 00
44 00
74 . 00
48 . 00
60.00
72 .00
108
62.30
64.50
75.20
87 40
90.20*
94 . 00*
106.00
102.00
36 70
65. 10
8 1 .90
126.00
1 10
60.00
96.00
22.00
50 00
25.00
40. 00
t32.00*
44 . 00
30 00
52.00
30 . 00
62 .00
Ui
50.90
43 62
46 II
52 78
50 00
65 78
IS 37
34 .67
89 97
84 . 88
103.53
04 . 50
1 to
26 . 00
92.00
0 00*
0 00*
100 00
66 00
1 17. 00
too.00
O.OO'
0 00*
1 to.00
104.00
lis
7.40
84.30
93 90
83 20
90 10
82 20
64 70
82 60
80 00*
98.70*
97 70
86 60
ne
77. 70
85 50
69.40
49.90
49.60
77.60
60 80
78. 70
92 40
54 .40
46 20
4 1 90
117
*
24.80
77 80
47 70
53.60
16.70
29 60
48.90
78 50
72 50
71 .90
12 00
119
40.00
46.70
94 .50
96.60
82.70
81 30
87. 40
68.60
47 60
29-90
57.00
45 60
122
6.90
9 . 70
9.30*
1 .30*
27.50
17 40
10. 70*
40.80*
I 1 .40*
5.30*
39.40*
19. to-
123
1 24
63.80
62.63
61 . 00
68 . 20
81 .90
78. 00
61 .80
86 60
54 60
81.10
75.50
124
90.00
45.00
67 . 00
71 .00
78 00
71 00
72 . 00
73 . 00
97 00
74 . 00
66 00
87 . 00
123
40.30
32.80
58.00
32 .90
58.60
45 . 60
53.60
51 .80
44 . 90
46. 80
27 20
35 70
Ul
-------
LAB
101
102
103
104
I OS
1 10
1 12
Hi
1 15
I IS
117
I 19
122
123
I24
125
90
e
oo
00
00
00
00
00
00
00
00
00
00
00
00
20
00
00
70
APPENDIX C (Continued)
TABLE C-l. RAW DATA FOR NAPTHALENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED WATER TAP WATEH SURFACE WATER WASTEWATER (C-94) WASTEWATER
5 056 565656
335.00 375.00 335.00 375 00 335 00 375.00 335.00 375.00 335.00 375.00
580.00*
440.00*
230.00«
360
00*
300 00
340.00
300 00
200.00
96 00
130 00
88 . 30
207.00
181.00
270
00
187 00
832.00*
211 00
207 00
185.00
236 00
33.00*
54 .00*
1 10 00
80
00
35 00*
29 00 *
22 00
92 . 00
80 00*
100.00*
140.00
200.00
170.00
140
00
140 00
170 00
260 00
270 00
290 00
~
177.00
200.00
150 00
250
00
240.00*
410.00*
257 00
303.00
158 00
220 00
388.00
88 .00
70 . 00
330
00
274 00
326.00
243 00
220 00
130.00
214 00
138.58
271.58
70.29
187
00
79 04
2 14 00
1 10 56
90 56
204 88
122 00
178.00
79 .00
122.00*
33
00*
198.00
253.00
223.00
327 00
0 00*
173.50*
279.00
248.00
277.00
268
00
2 10 00
315 00
271.00
3 15 00
248 00*
281 00*
183.00
241.00
98 . 00
374
00
297.00
3 14 00
152 00
120 00
109 00
171 00
91 .40
199.00
238 00
107
00
100 00
191.00
129.00
223.00
544 00*
294 00
223.00
203 00
258.00
295
00
298 . 00
339 00
294 00
1 70 00
194 00
209 00
101.00
9.70
23 90'
20
60'
140 80
21.40
112 90*
77 60*
98.70*
2 73.00
202.00
231.00
280
00
222.00
246.00
21 1 00
277 00
262 00
278.00
2 00 00
209.00
254 . 00
270
oo
202.00
59 . 00
259 00
251.00
248.00
206 00
226.90
210.90
144 10
I4R
30
174 . 90
171.30
163 90
191.20
137 10
144.60
-------
APPENDIX C (Continued)
TABLE C-2. RAW DATA FOR ACENAPH7HYLENE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UG/L
0I5TILLCD
WATER
TAP
WATER
SURFACE
WATER
WASTEWATER
(C
94 >
WASTEWATER
-------
APPENDIX C (Continued)
TABLE C-2. RAW DATA FOR ACENAPHTHYLENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DISTILLED MATER
TAP
WATER
SURFACE
WATER
WASTEWATER
(C
94 )
WASTEWATER
(C-95)
WASTEWATER
tC-96)
AMPUL NO:
3
4
3
4
3
4
3
4
3
4
3
4
TRUE CONC:
110 00
90 . 00
t to.00
90
00
1 10 00
90
00
1 10 00
90
00
t 10 . 00
90 00
110 00
«>0. 00
LAB NUMBER
tot
96. 00
94 00
180.00
170
00
94 00*
Bl
00*
290 00*
130
00*
120 00
130.00
66 00
91 00
102
69 30
56 60
84 40
31
70
89 40
88
90
85 70
73
00
90 70
63 40
74 70
62 70
103
13.00*
19.00*
39 00
98
00
50.00'
61
00*
4 40*
85
00*
0 74 ~
48.00*
0 . 74*
70.00*
104
ea.oo
62 . 00
57 00
78
00
88 . 00
65
00
89 . 00
56
00
83 00
48 00
70 00
90 . 00
tOB
65.90
67 . 00
64 00
81
50
III 00*
4
14 1 00
132
00
89 . 60
98 50
88 60
159 00
1 10
32 .80
27 00
13 00
86
00
16 00
32
80
108 00*
44
60
31 60
40 40
40 60
1 1 00
112
55.56
51.81
54.03
63
18
63 89
84
07
3 1 66
44
38
77 06
92 I 1
72 5 1
69 75
t <1
60 . 00
98.00
45 00
27
00
too.00
S3
00
121.00
1 16
00
80 00
43 00
102 OO
21.00
115
100 20
102.70
98 20
94
90
95 30
97
50
79 80
94
90
88 00
101 70
93 80
104.60
t IB
74 .30
92.80
58 90
50
40
95 00
83
00
77 90
85
70
101 00
86. 30
68 70
88 80
1 17
8.40
9.80
74 60
67
00
55 70
80
30
54 70
60
50
99 10
24 60
94 70
54 40
t 19
74 . 10
45 . 70
82 40
83
30
66 70
73
30
58 60
83
40
89 00
47 20
64 90
66.50
122
12 10 <
1 .40*
155.40
1
70
140 90
27
20
1 18 20
704
30*
2 90
127.20
247 30*
139.50
<23
78.00
66.20
54 90
66
10
67 60
86
10
S3 50
89
20
78 00
66 10
79 40
85.30
124
90 00
26 . 00
86 00
86
00
80 00
80
00
80 00
64
00
74 00
85 00
66 00
106 00
125
34 . 00
37.40
72 80
50-
80
85 40
83
80
7 1 80
75
90
82 30
39.50
5 I OO
58 40
00
-------
LAB
101
102
103
104
100
I 10
I 12
M*
I IS
i ie
I 17
I <9
122
123
124
125
96
e
00
oo
oo
oo
oo
00
00
00
00
00
00
00
00
eo
00
00
60
APPENDIX C (Continued)
TABLE C-2. RAW DATA FOR ACENAPHTHYLENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED MATER TAP WATER SURFACE WATER WASTEWATER (C-9 WASTEWATER
-------
APPENDIX C (Continued)
TABLE C-3. RAW DATA FOR ACENAPHTHENE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UG/L
DISTILLED WATER TAP WATER SURTACE WATER WASTEWATER (C-941 WASTEWATER IC-951 WASTEWATER (C-961
AMPUL NO: I 2 I 2 ) 2 I 2 I 2 I 2
TRUE CONC: 10.00 (2.00 10.00 12 OO 10.00 12 00 10.00 12.00 10. 00 12 00 10 00 12 00
LAB NUMBER
101
5 . 00*
5 80*
12.00*
13 00*
4 10*
7.90*
7 40
1 I 00
6 60
9. 10
6 80
7.80
102
1. 70
13 . 10
2 19
6 35
3 00
6 79
5 32
7 79
1 82
6. 20
3 28
7 09
103
0. 00*
0.00*
0. 00*
1 . 00
0 . 00*
4 00
0 00<
2 00
0 00*
0 . 00*
0 . 00*
0 . 00*
104
4. 10
4 60
5.80
4 90
6 70
8 70
6 80
10 00
6 . 30
9.80
6. 20
9. 10
106
4 81
~
4 95
~
2 75
3 99
*
4 56
~
4 .04
~
0 00*
110
te.oo <
10 00* <
10.00* <
10 00* <
10 00* <
10 00* <
10 00* <
10.OO* <
10 00* <
10.00* <
10.00* <
10 00*
112
2.55
5. 14
4 . 14
5 38
3.53
6.93
6.66
9.52
6.90
9.61
5 11
7 45
II ?
0.00*
0 . 00»
0 . 00*
0 00*
0 . 00*
0. 00*
0 00*
0. OO*
0 00'
O 00'
0 00*
0. 00*
1 IS
0.90
8.60
7.00*
9 . 60*
6. 20*
8 10*
7 . 30*
10.60*
6 . 10
7 10
6.90
7.50
1 IB
0 . 29*
0.51*
0. 18*
0 71*
0 28*
0 . 30*
0 40*
0 48*
0 . 60«
0.68*
0 62*
0 61*
1 17
1.83
2.44
4 .62
6 43
3 78
6 30
3 58
8.58
8 19*
9 56*
0 . 00*
8 58
119
3.99
2.63
4.90
6 54
6 . 23
7.62
6.31
7.62
5 .44
5.94
5 31
7 97
122
2.40
5.30
0. 20 c
0 50* <
0.50* <
0 50* <
0 50* <
0. 50*
7.40 <
0.50*
9 30
3 50*
123
0.60*
0.62*
0.56
0 70
0 34
0 83
0 45
0 86
0 56
0.40
0 18
0 64*
124
17. 00
1 1 . 00
1 .50
16 00*
4 . 30
15 00
17 00*
3 50
12 00
7 . 70
13 00
6 70
125
5.40
5 60
6.60
4 50
6 80
5. 70
7 20
6 50
7 10
10 20
6. 10
6 90
OO
O
-------
101
102
103
104
108
I 10
I 12
"I
IIS
i te
117
119
122
123
124
125
96
4
00
00
40
00
00
10
00
78
00
50
20
20
eo
30
13
00
00
APPENDIX C (Continued)
TABLE C-3. RAW DATA FOR ACENAPHTHENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DISTILLED MATER TAP MATED SURFACE MATER MASTEMATER
-------
TRU(
LAB
101
102
103
104
108
I 10
I 12
I Id
I 15
1 16
117
f 19
122
123
124
125
96
6
00
00
00
00
00
00
00
30
00
00
20
00
00
70
70
00
40
APPENDIX C (Continued)
TABLE C-3. RAW DATA FOR ACENAPHTHENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED WATER TAP WATER SURFACE WATER WASTEWATER (C-94) WASTEWATER (C-95)
5 850505650
235.00 260.OO 235.00 260.00 235 00 260.00 235.00 260.00 235.00 260.00
350.00*
660.00»
220.00*
290
00*
230 00*
270.00*
220 00
2 10
00
83 00
t to 00
60.50
199 . 00
144 . 00
201
00
165 00
160 00
178 00
143
00
159 00
133.00
75 . 00
85.00
95.00
78
00
68 . 00
84 . 00
28 . 00
85
00
74 00
58 00
100.00
140 . 00
120.00
97
00
100.00
130 00
200 00
190
00
220 00
~
67 . 00
88 .60
56.40
89
50
76 80
142.00
86 70
310
00
84 00
127 00
f 04 . 00
30.00
56.00
1 10
00
11.00
26 00
1 7 . 00
22
00
28.00*
12 00*
127.00
219.00
68 . 05
158
00
133 25
172 87
III 00
129
00
170 21
135.00
177.00
145.00
140 . 00
140
00
222 00
222 00
208 00
200
00
108 00
200 00
229 00
175.00
213 00*
203
00«
143.00*
243.00*
234 00*
246
00*
227 00
742 00
10.30*
16.20*
I 1 40*
27
70*
14.80*
14.20*
12 10*
10
10*
7 . 05*
12.SO*
257.00
97.60
196 00
140
00
126 00
210 00
1 14 00
2 14
00
546 00'
259 00*
2 19 00
2 19.00
2 16 00
239
00
2 10 00
210.00
229.00
191
00
237 00
2 1 7.00
218. 10
18.40
1 .90
1 17
40
35 60*
< 0 50*
192 70
65
60
152 70
*
18.40*
14.70*
17 10
20
00
18 . 70
15 80
17 80
17
40
12 50
~ 9 . 70
177.00
203.00
168 00
179
00
416 00*
103 00
220 00
199
00
188 00
163.00
<85.00
173.30
(60.50
147
60
147.6 0
ISO 30
176.90
192
30
170.30
179.20
-------
LAS
101
102
103
104
108
I 10
112
118
IIS
its
117
M»
122
123
124
96
2
40
00
20
00
IB
50
00
04
00
90
83
60
70
90
40
80
40
APPENDIX C (Continued)
TABLE C-4. RAW DATA FOR FLUORENE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UG/L
DISTILLED WATER TAP WATER SURFACE WATER WASTEWATER (C-94> WASTEWATER WASTEWATER
t 2 I 2 I 2 I 2 I 2 I
10.00 25.40 10.00 25.40 10.00 25 40 10.00 25 40 10.00 25.40 10 00
4 . 70
8.02
3.80
0.04*
5.24
12 . 00
2.85
3.60
7 00
9.80
I . 18
5.27
3. 10
7.01
4.80
1.50
t2 00
IB. 80
7.50
0. 07
13.94
5.00*
14 .40
17.00
18.80
20.80
3.27
12 .40
9.80
17 20
17 . 00
I . 10
12 00*
4 73
90
10*
.38
00'
52
.80
50
.48
05
97
60
78
20
50*
30.00~
4 40*
19
00'
8 70'
24
00
9 60
24 . 00
640
14 . 80
8.52
14
80
5.39
18
40
4 . 43
17.90
4.81
5 SO
4 50
8
70
2 30
15
00
2 40
6 00
5 20
0 09 ~ <
0 06'
0
15' <
0 03'
0
33' <
0 . 03 *
0.18* <
0.O8*
15 90
6 30
142
00*
5 88
10
70
5 10
8 61
3 88
5 00 * <
5 00' <
5
00' <
5 00* <
5
00' <
5.00' <
5 00' <
5 00« <
14 33
5 65
17
88
6 28
23
65
7 46
16.42
6 50
23.00
0 00'
22
00
9 10
24
00
7 . 00
9 50
7 00'
20 . 60
6 80
17
80
8.00
20
60
6 . 80 *
18 60 ~
7 . 50*
23 10
9 01
18
10
7 06
24
60
11.70'
264 00*
1 1 .40
17 . 60
4 17
10
20
4 . 15
17
10
6 . 68
16 50
o. at
B . 19
4 45
1 1
70
7 06
10
40
5 57
II 70
3 97
1 40
1 30
0
50
5 . 20'
9
60*
9 . 70
0.10
10 20
12 70
7 . 72
18
80
6 60
18
40
6 14
1 1 50
6 41
12 00
4 30
16
00
5 30
5
50
4 70
II oo
4 50
1.70* -
0 19'
0
90
3.50
4
00
0 70'
0 70*
0 10*
-------
APPENDIX C (Continued)
TABLE C-4. RAW DATA FOR FLUORENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DIST1
LLEO MATER
TAP
MATER
SURFACE
WATER
WASTEWATER
tc
94)
WASTEWATER
(C-95)
WASTEWATER
-------
APPENDIX C (Continued)
TABLE C-4. RAW DATA FOR FLUORENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED WATER TAP WATER SURF ACE WATER WASTEWATER (C-941 WASTEWATER WASTEWATER
AMPUL NO: 5 0 9 0 5 6 5 6 5 6 5 6
TRUE COHC: 270.00 403.00 270 00 403.00 270.00 483.00 270.00 463.00 270 00 403.00 270.00 463.00
LAB NUMBER
101
310.00
B30 00
220 00*
430.00*
360.00*
102
OS.00
408.00
210 00
428 00
71100
103
69 00
7< .00
73.00
MO 00
7 100
<04
< .30*
2.20*
I 40*
1 . 30»
< .20*
IOB
<13.00
<93.00
84.70
200 00
140.00
1 10
48. 00
80 00
23 00
120 00
<4 00*
112
52.88
to.82
55 72
5 59
95 75
119
203.00
405.00
137.00
340.00
108.00
<19
229.00
285.00
212.00
305.00
174.00
i ie
24 7.00
399.00
2<8.00
405 . 00
203.00
117
<81.00
208.00
304.00
335.00
<08.00
110
208.00
444.00
250.00
458.00
24 < 00
<22
< 0.04*
24 90
15 <0
05 <0
80 . 00
123
329.00
<0B-00
191 .00
355.00
232 00
124
184.00
400.00
<97.00
356.00
93 . 00
25
<3.50
20.90
9.20*
16 40*
21 . 70
550.00*
300 00*
440.00*
120 00
220 00
190 00
330.00
355 00
210.00
34100
195.00
300.00
202 00
392 00
79.00
59.00
03 . 00
91 .00
75.00
75 00
70.00
2 . 00*
< 0.08*
3 . 00*
< 1.20*
< 1 20*
4 . 30*
348 00
13100
309 . 00
151 00
299.00
106.00
107.00
38.00*
58.00
22 00
55.00*
24.00*
82.00
144.00
1 1 .40
36 46
6.83
28.76
27 90
4 00
7 36
400.00
194.00
4 14 . 00
147.00
324.00
200.00*
380.00*
380.00
249.00
378 00
250 00*
429.00'
235.00*
420.00*
388.00
221.00
375.00
226 00*
437.00*
139 00
258 . 00
407.00
185.00
292 00
554 00*
370 00
185 00
591.00
365 00
288.00
427 00
194 . 00
317.00
188 00
304.00
0 50
< 0. 04 *
< 0 04*
< 0 04 *
*
39 30
< 0 . 04 *
319.00
222.00
359 00
110 00
348 00
222 00
306.00
168 00
235.00
328 00
2 19 00
250.00
234 00
288 00
25.70
6.40
36. 70
7.10*
12.90*
7 . 60*
13.50*
00
in
-------
APPENDIX C (Continued)
TABLE C-5. RAW DATA FOR PHENANTHRENE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UG/L
DISTILLED
MATER
TAP
MATER
SURFACE
WATER
WASTEWATER
(C-94)
MASTEMATER
(C-95)
MASTEMATER
(C-96)
AMPUL NO:
1
2
1
2
1
2
1
2
t
2
1
2
TRUE CONC:
5 00
6. 00
5 . 00
6 00
5 . 00
6 00
5 00
6 . 00
5 . 00
6 00
5 . 00
6 . 00
LAB NUMBER
101
3.50
3. 10
B. 70»
7 10*
2 50
3 80
4 OQ
4 70
3.50
4 70
3 70
4 30
102
3 . 35
5 . 35
2.71
4 37
3.62
4 .84
2.86
4 38
2 . 73
5 16
2 . 77
4 . 45
103
2.80
2. BO
0.00*
2 50*
0.00*
4 10
0 00*
5 10
0 91*
2 90*
2.80
2 . 70
04
1 .90
1.90
2.50
2 20
3. 10
3 90
3 20
4 . 10
2.90
4 . 00
2 80
4 . 10
108
2 97
0.99
2.57
4 48
3 . 23
3 .97
2 7 1
4 60
2 . 10
2 27
1 9b
4 . 80
1 10
1 . 60
2 . 00
1 .40
3 50
2 40
3 54
3 60
4 40
2 . 40
2 60
2 60
3 . 40
1 12
2 05
8.80*
2 63
11 56»
5. 74*
16 00*
3 38
2 64
3 29
4 44
2 00
4 2 1
11?
3 . 10
4 .80
3 20
5 60
4 60
5.10
3 80
5 00
3 80
3 70
4 20
5 BO
1 15
4 30
4 . 70
3 00
4 50
4 70*
5. 10*
4 20*
5 10*
3 80*
5 . 80*
4 60*
5 20*
1 IB
2 97
5.25
2.37
5 05
2 76
2 76 ,
2 83
4 8 1
4 38
5 24
4 96
5 55
1 17
0.68
1.81
3.27
4 . 34
2 . 86
3 30
2 67
5 91
4.31*
5.49*
1 .34
4.56
1 19
3.84
3.34
2.71
2 71
3. 16
2 98
2 76
3.4 1
2 31
2.81
2 on
3 22
122 <
2.50*
3.00 <
2 .50*
< 2 50* <
2 50* <
2¦50* <
2 50* <
2 . 50*
4 50 <
2 50*
< 2 50* <
2 . 50*
123
2.84
3.45
2 13
3 40
2 . 79
3 51
3 27
3 52
1 84*
2.24*
3 13
3 . 70
124
2 . 80
2 . 00
0.61
4 . 60
3.40
5 30
3 40
1 90
2 . 60
2 .90
2 30
2 . 60
125
4 . 10
2 . 80
4 . 00
3 40
4 . 20
3 80
4 00
4 00
3 . 70
5. 10
3 00
3 . 60
00
-------
LAB
101
102
103
104
IOS
I 10
I 12
llfl
115
I IB
117
119
122
123
124
IU
...3
4
00
oo
20
00
00
70
60
09
00
10
30
40
40
90
00
00
30
APPENDIX C (Continued)
TABLE C-5. RAW DATA FOR PHENANTHRENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DISTILLEO MATER TAP HATER SURFACE WATER WASTEWATER (C-9^) WASTEWATER
3434343434
60 00 50.00 80.00 50 00 80.00 50.00 60.00 50 00 BO 00 50.00
55 . 00
64 . 00
63.00*
44 00*
47 00
38 . 00
59 00
38 . 00
30 00
34 00
49.90
30 30
48 40
17 90
47.60
39 . 00
4 7 90
37 20
49 80
33 40
24 . 00
16. 00
30.00*
24.00*
27 00
24 . 00
0 . 00*
25.00
27 00*
25 00*
28 . 00
22.00
22 00
26 00
29 00
24 00
38 00
21.00
34.00
16 00
21 . 20
39-90
25.30
20 90
40 50
42 20
4 1 90
33 30
17 70
21 60
91 .00
55.00
48.40
48 60
47 00
63.00
78.40
68 00
70 00
52 60
30. 64
25.81
46.30
35 03
43 65
30 80
18 .95
22.87
37 88
29 5 1
55.00
54.00
56 00
29.00
48.00
39.00
58.00
67 00
45 . 00
37.00
64 .40
53. 10
58.80
47 10
61.70*
48.60*
54 50*
50 60*
56 (0*
50.70*
43.90
42.60
31 . 10
36 90
42 80
45 .40
47 80
40 20
48 00
23 . 40
20.40
12.80
49.30
40.80
32 90
33.60
34 70
26 10
52 40*
44 00*
55. 10
31 .60
51 .00
40 80
43 70
36 . 20
54 90
39.80
53 60
32 .90
6.90
13.90
57.90
3 60
49.80
9 90
19.20'
83 40* <
2 50*
27 50
35 20
22.60
16.60
19.50
57.00
91.60*
35 60
35 60
33 20*
23.00*
47. 00
20. 00
40.00
4 1 00
47. 00
37 . 00
4 7 00
34 . 00
43 00
39 00
35.20
39.20
43 30
33.00
46.30
33 10
48 60
37 no
44 . 20
38 .50
-------
APPENDIX C (Continued)
TABLE C-5. RAW DATA FOR PHENANTHRENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED MATER
TAP
WATER
SURFACE
WATER
WASTEWA
TER (C-94)
WASTEWATER
1C-95)
WASTEWATER
(C-961
AMPUL NO:
5
6
5
6
5
e
5
6
5
6
5
8
TRUE CONC:
205.00
280.00
205.00
280
00
205.00
280 00
205.00
280 00
205 00
2B0.00
205.00
280 00
LAB NUMBER'
101
240.00
370.00
180.00*
310
00*
180 00
250 00
190 00
230 00
80 00
130.00
120 00
200.OO
102
91 .50
269.00
165.00
276
00
169 00
220 00
ISO 00
210.00
158 00
192.00
169.00
240.00
103
28 . 00
24 .00
26.00*
32
00*
26 . 00
31 00
24 00*
24 00*
37 00*
33 00*
31.00
29 00
104
78 00
120 00
79.00
79
00
76 00
110 00
140 00
180 00
180.00
*
150.OO
220 00
108
157.00
146.00
138 00
150.
00
115.00
206.00
106 00
174.00
113.00
169 00
102 00
1 1 1 00
1 to
275.00
269 00
207.00
342
00
210.00
342 00
207 00
292 00
2 1 1 00
266 00
253 00
342.00
1 12
81 . 79
194.20
75 18
165
00
28 .64
139 00
185 67
231.00
194 93
248 00
130.05
184 00
1 tft
217.00
200.00
120 00
200
00
65.00
2 14 00
173.00
224.00
150 00
195 00
189.00
266.00
f 15
209.00
228.00
197 00
227
00
175.00*
275 00*
192 00*
315 00*
199 00*
266 00*
220 00*
281 00*
1 16
188.00
280.00
167.00
323
00
193.00
250 00
208.00
228 00
161.00
285 00
117.00
229 00
1 17
190.00
187.00
211.00
191
00
90.30
268 00
135 00
226 00
480.00*
247.00*
18 1 00
462.00
1 19
183.00
264.00
190.00
264
oo
175.00
229 00
193 00
2 10 00
169.00
203 00
130 00
189.00
122
127.90
35.90
60.00
135
00
81 70 <
2 50*
147.60*
188 20*
230 00
*
49 80
2 18 20
123
148.00
114.00
102.00
142
00
232.00
31900
150.00
176 00
58.30*
154 00*
167.00
186 00
124
163.00
284 . 00
181.00
231
00
129.00
133 00
194 00
231 00
192 00
199 00
192 00
2 12 00
125
162.50
199.60
163.90
179
00
130.30
156.40
140 90
159 50
147.00
149 30
134.60
155 60
oo
oo
-------
APPENDIX C (Continued)
TABLE C-6. RAW DATA FOR ANTHRACENE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UG/L
DISTILLED
MATER
TAP
HATER
SURFACE
MATER
WASTEWATER
( C - 94 >
WASTEWATER
WASTEWATER
(C-96)
AMPUL NO:
1
2
1
2
1
2
1
2
|
2
1
2
TRUE CONC:
10 00
14 . 00
10. 00
14 . 00
10 . 00
14 00
O
o
©
14 . OO
10.00
14 00
o
o
o
14 00
LAB NUMBER
101
10.00*
13.00*
9.30*
15 00*
7.40*
1 1 00*
10 00*
14.00*
7 30
13 00
9 20
12 00
102
6 S3
IS.80
1.97
6 72
7 43
21 10*
6 86
II .30
5 74
12 00
4 .62
9 80
103
2 . 70*
1.50*
1.30*
3 .90*
1 .50*
2 80*
0.95*
0 . 00*
0 00*
0 00*
0.00*
0 . 00*
104
2 90
4 .30
3 . 70
4 10
5 30
7 90
5. 70
7 60
5 20
8 40
5.20
8 30
108
5. 77
2 36
4.50
6 74
6.57
8 18
4 44
7.92
3.87
5 35
4 . 04
10.40
t 10
6 . 80
6 00
6 . 40
II .80
8.40
6.67
II 70
12.50
7 20
7. 60
9.50
8 . 60
' "2
2 . 30
11.31
3.43
102 81*
S.39
107 7 1 *
6. 13
10 61
7 02
1173
8 40
8 48
1 IS
7 . 00
9.90
6 . 00
10 50
8 . 20
12 00
7 90
1 1 .60
7.20
7 . 50
7 . 80
10 . 80
1 IS
3 10
7.50
5 . 00
7 40
2 . 70
8 30
6 . 50
10 10
4 . 20
7 . 80
6. 30
8 . 40
1 IS
5 29
9.94
3.30
9 10
4 .98
5 24
5 51
9 32
8 57
10 60
9 00
II 00
1 17
0.40
0. IS
3.26
4 95
5 50
7 51
1100
3 43
7 50'
10. 70*
4 21
10 90
1 19
6.69
6.43
4 42
6 16
4 97
7 74
7 . 09
8 50
5 42
6 7 1
4 .51
7 45
123
1 .80*
4.80* <
0 90*
< 0 90* <
0.90* <
0.90*
2.50*
3.50*
5.30~ <
0. 90*
6 60
3 . 40*
123
8. 14
10.90
6 87
3 98
6.80
9.71
4 86
I 1 20
6 02
7.48
6 . 72
8 . 69
124
4 50
6 20
0.37
3 20
5.30
4 . 40
2 60
3 . 30
3. 20
3 60*
2.90*
125
7.30
7 . 20
7 . 40
6 30
8. 10
6 80
7 . 80
8.90
7 00
1 1 . 20
5 80
8 . 30
00
vO
-------
LAB
101
102
103
104
I OB
I 10
M2
I IB
I 15
i ie
117
119
122
123
124
98
4
00
oo
so
oo
oo
BO
20
IS
00
30
50
80
90
40
40
00
70
APPENDIX C (Continued)
TABLE C-6. RAW DATA FOR ANTHRACENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
OISTfllEO MATER TAP WATER SURFACE WATER WASTEWATER (C-94) WASTEWATER 10-951
3434343434
70.00 85.00 70.00 85.00 70.00 85 00 70.00 85 00 70 00 85 00
76.00*
77.00*
76.00*
102 00*
69.00*
78 00*
92.00*
89.00*
45 00
77 00
03 .80
57 . 10
82 .60
39 20
58 .90
69.40
64 . 70
65 50
59 40
60 90
14.00*
9 . 70*
14 00*
15 00*
t1.00*
13.00*
1 80*
15 00*
0 00*
15 00*
27. 00
34 .00
22 00
40 . 00
31 00
38 00
<100
32 . 00
36 00
23 00
25 90
17.30
27 90
25 80
43 . 40
64 . 10
48.50
33 . 30
28 90
25 20
57.20
49.60
45 80
38 80
38 . 20
49 80
33. 20
54 . 80
47 40
48 40
43.50
SI .46
45 17
62 03
50.89
51.41
26 69
40 05
4 7.88
59 27
55 . 00
83 .00
06 00
78 00
59 . 00
83 . 00
69. 00
8 1 . 00
57 00
SB 00
53 40
63.30
50.80
62 90
54 40
64 .80
53 30
67.30
50 80
66 50
52 40
7 1 .60
38 60
65 80
44 . 30
75 80
57. 10
74 80
59 .50
44 .60
4 . 78
9.67
44 40
54 20
38 . 50
56.30
88.90
98 40
6110*
*
56 30
47.60
57.20
71 60
50.80
58.20
66. 30
65 60
59.30
49 00
I 10*
9 .90*
24 70*
3 40*
J3.80-
1 1 to*
13.10*
100.50*
7 70*
24 70*
45. SO
49.00
28 10
18 80
4 1 .90
62.30
67 10
4 1 30
48.80
48 30
21 .00
35 00
10.00
35 00
16 00
<8 00*
32 00
16 00
19 00
19 00
38.00
83.50
46 00
53 40
45.50
48 . 60
50 80
56 . 40
46 . 00
38 70
-------
LAB
101
102
103
104
108
MO
I 12
;»
«ie
117
i ta
122
123
124
125
APPENDIX C (Continued)
TABLE C-6. RAW DATA FOR ANTHRACENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED MATER TAP WATER SURFACE WATER WASTEWATER WASTEWATER (C-95) WASTEWATER
505656565656
400.00 350.00 400.00 350.00 400 00 350.00 400 00 350 00 400.00 350.00 400.00 350.00
360.00*
2 OS 00
22.00*
120.00
170.00
82.40
215.87
342.00
355.00
35 I . 00
443.00
364.00
127.90*
240.00
<62.00
279.80
290.OO*
358 .00
15.OO*
120 00
136.OO
65.40
293.00
277.00
219.00
346.OO
202.OO
312.00
30.80*
286.00
177.00
265.40
390.00*
334.00
17.00*
140 00
125.00
72 00
123.71
232 00
332.00
323.00
430.00
372.00
142.90*
295.00
243 00
279.00
400 00*
365 00
14 00*
87 00
148 00
48 60
190 03
288 00
228.00
415.00
225 00
334 . 00
83.80*
259 00
169 00
219.30
500.00*
361.00
19.00*
140 00
226.00
80.40
71
348 .
271 .
368.00
191 .00
356.00
108.00*
320.00
*
190.30
. 26
.00
. 00
390.00*
280.00
IS 00*
120.00
235 00
61 .00
224.00
290 00
270.00
303 00
34 0 00
284.00
17.10*
233 00
44 00
176.30
480.00*
328.00
I I 00*
260 00
168.00
61.20
244. 14
394 00
325.00
388 00
583.00
391.00
165.70*
175 00
249 00
199.60
34 0.00~
258. 00
I 1.00*
190 00
178 00
60. 80
203 21
300 00
287.00
274 00
3 16 00
286 00
137.60*
205.00
160 00
181 00
200 00
339 00
I 2.00*
300 00
197 00
64 80
32 I 75
336.00
327 00
308.00
1045 00*
34 I 00
90.60*
147 00
249.00
224 10
220.00
222.00
7 . 60*
~
192 00
78 00
256 4 I
27 I.00
269 00
390 00
344 00*
277.OO
*
236 00
163 00
187.40
320 00
328 00
16 00*
260 00
180.00
7 I 00
245 8 I
387 00
301
267 .
426.00
261.00
59 30
366 00
160.00*
214.80
00
. OO
320.00
301.00
8.50*
24 0 00
125 00
52 60
2 17 00
26 I.00
265.00
342.00
64 I 00~
251 00
165 . 00
202 00
163.00*
194.30
-------
APPENDIX C (Continued)
TABLE C-7. RAW DATA FOR FLUORANTHENE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UG/L
AMPUL NO:
TRUE CONC:
DISTILLED MATER
O . 30
2
O . 40
TAP WATER
I
0 30
2
O A 0
SURFACE WATER
O 30
2
0.40
WASTEWATER (C-94)
1
O 30
2
0 40
WASTEWATER
I
O 30
2
O 40
WASTEWATER (C-96)
0 . 30
2
O . 40
LAB NUMBER
101
102
103
104
108
I IO
I ia
lift
I 15
I IS
I 17
I 19
12a
t23
124
125
0 03*
0.05*
0.01*
0
00*
0 04*
0.00*
0 04*
0 . 06*
0 03'
0 03*
0. 00*
0 04*
0. 24
0.43
0 20
0
39
0 27
0 38
0 22
0 38
0 2 1
0 40
0 19
0.36
0. 00*
0.24
59 00*
0
00*
16 00*
0.00*
0 30
0 61
2 60*
0 . 00*
0. 37
0 00*
0.06*
0.07*
0 07*
0
08*
0 10
0 15
o. to
0 14
0 10
0 15
0.10
0 15
0 . 54
0 66'
1 62*
0
69*
0 35*
1 00*
0.21
0. 86*
*
0 53
~
0 02
0.34*
0 46*
0. 70*
0
53*
0.46*
« 36*
0.41*
0.77'
0 4t»
0 59*
0 55
0. 54
0.53
0 . 20
0 16
1
35*
0 16
1 08*
0 22
0 27
0 18
0.26
0. 18
0 28
0 . 00*
0.00*
0 00*
0
00*
0 00*
0 00*
0 00*
0 00*
0 00
0 . 00*
0. 00*
0 . 00*
0.31
0.35
0 25
0 .
33
0 27
0 33
0 26
0. 39
0 25
0.32
0 26
0.38
0 27
0 . 45
0 25
0
43
0 27
« 35,
0 2 1
0 42
0 36
0 49
0 37
0 . 49
0. 07
0. 12
0 19
0
25
0 17
0 19
0 16
0 29
0 26
0.38
0 10
0 30
0. 28
0.30
0. 15
0
19
0 23
0 28
0 29
0. 36
0 21
0 26
0.17
0 26
0 . 20
0.30
0 . 07
0
20
0 10
0 06
0 20
0 30
0 30 <
0.02*
0.40
0 30
0.24
0.31
0. IB
0
23
0.39
0 48
0 25
0 30
0 2 1
0 . 24
0. 23
0 28
0. IS
0 23
0.06
0
20
0.23
»
0 17
0. 15
0 09
0. 20
0. 14
0 18
0.50
0. 20
0.30
0
20
0 30
0 30
0.20
0. 20
0 30
0 . 30
0. 20
0 30
v£>
K>
-------
APPENDIX C (Continued)
TABLE C-7. RAW DATA FOR FLUORANTHENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DISTILLED
MATER
TAP
WATER
SURFACE
WATER
WASTEWATER
(C-94)
WASTEWATER
< C-951
WASTEWATER
(C
AMPUL NO:
3
4
3
4
3
4
3
4
3
4
3
TRUE CONC:
4 . 00
3 . 00
4 . 00
3 . 00
4 00
3 . 00
4 . 00
3 . 00
4 00
3 . 00
4 . 00
3
LAB NUMBER*
101
0.35*
0 . 08»
0. 38«
0 19
0 33*
0 18*
0 43*
0 22»
0 J2<
0 24«
0. 09*
0
102
3.38
2. 12
3.42
1 49
3 27
2 45
3 53
2 80
3 71
2 4 1
3 32
2
103
2.40
1 . 10
3.00
4 . 00
1 . 20
0 30
4 20
3.80
3 80
2 00
2 80
2
104
0.92*
0 70*
0. 70*
0 75*
1 . to
0 84
1 .40
0 71
1 30
0 4 1
1 . I0«
1
10*
2.08
2 51
4. 1 I*
3 3I»
8 58*
5 78*
4 92
3.51
3 53
1 28
2 . 83
1
1 10
7.90*
8. 20»
4.88 ~
28¦00*
4 . 30*
4 98 ~
14.40*
8 20*
to.00*
8 44'
8 78 +
0
112
2.07
1 55
2.58
2. 10
2 08
t 42
t 38
1 28
2 19
t 77
2 . 67
0
1 W
1 .40*
0.00*
2.80
1 80
0 00*
0 00 ~
0.00*
0 00»
0.00*
0 00»
0.00*
0
IIS
4 . 20
3 30
3 70
2 80
4 . 00
2 80
3.20
2 90
3 80
3 00
3 .50
2
1 IB
2.85
2 58
1 .93
2 03
3.41
2.73
2.99
2 57
3 33
1 24
3.88
2
117
1 48
0.71
2.88
2 23
1 93
1 .87
I .94
1 22
3 . 18
2.27
2 .50
t
II*
3.88
2.37
335
2 88
3.08
2 32
3 05
2 59
3.30
2.17
2.75
2
122
1 80
1 . 20
3.80
0.50
2.80
1 10
1 .80
7 . 00*
1 80
1 .80
3.00
t
123
2.92
1 84
1. 13
1 .43
2.50
2 28
2.87
2 54
2 88
1 87
3. 13
2
124
3 00
0.98
2.30
1 . 90
2 50
1 . 70
2. 70
1 90
2 90
2.00
2.70
2
125
2.30
2 . 40
2.80
2 10
MO
2 . 00
2 . 70
2 30
2 .50
2 00
2.40
2
W
90)
4
00
to»
23
SO
00
07
79
87
00*
70
78
44
14
00
71
40
20
-------
APPENDIX C (Continued)
TABLE C-7. RAW DATA FOR FLUORANTHENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED MATER TAP WATER SURFACE WATER WASTEWATER (C-941 WASTEWATER (C-951 WASTEWATER (C-98)
AMPUL NO: 5 8 5 6 5 6 5 0 5 8 5 6
TRUE CONC: 15.OO 12.00 15.00 12.00 15 00 12.00 15.00 12.00 15.00 12 00 15.00 12 00
LAB NUMBER
101
0.
37*
0
28*
0
95*
1
20*
1
30*
0
86*
0
93*
0
09*
0
42*
0
. 48*
0.
7/*
0
57*
102
a.
OB
12
. 10
12
. 80
12
20
13
20
9
33
1 1
80
9.
17
12
10
8
50
12
20
10
40
103
14
00
9
.30
1 1
00
6
40
5
20
5
50
5
50
8
70
14
00
8
30
12
00
12
00
104
3.
00*
2
. 70*
2
90*
1
70*
3
00
2
80
5
80
4
20
B.
80
~
5.
80
5 .
10
108
26
70*
10
50
24
00*
15
50*
IB
00*
23
20*
13
90
15.
50
7.
30
8
72
33.
30
7 .
22
1 10
35
00*
IB
20*
30
00*
49
40*
25
70*
29
00*
23
40*
24
40*
30
90*
25
10*
35
00
25
40*
1 12
B .
98
10
20
4
12
8
52
2
14
7
92
9
84
7 .
39
10
88
8
05
85
22*
7 .
31
t vs
0
00*
0
00*
5
50
0
00*
0
00*
0
00*
0
00*
0.
00*
0
00*
0
00*
0
00*
0
00*
1 15
14
. 70
9.
OO
13
eo
8
90
12
50
10
90
13
60
1 I
50
14
20
1 1
10
14
90
1 1
50
1 IB
14
.90
12
30
14
10
12
90
13
40
8
93
15
00
1 1
30
14
20
13
80
8.
10
10
40
1 17
12
.00
B.
4B
14
40
7
38
4
39
10
10
8
00
9.
90
33
70*
9
23
12
90
17
80*
1 19
13
.80
1 1
50
13
90
1 1
90
13
80
10
70
14
40
12
50
13
00
9
85
10
50
9
55
122
9.
.40
3 .
10
10
10
8
40
8
30
0
90
1 1
50
10
20
14
eo
~
3
50
10
20
123
7
27
85.
30*
8.
56
75.
50*
12.
00
82
30*
I 1
50
83
90 ~
3
91
74
90*
12
90
90
70*
124
8.
SO
9.
30
1 1
00
7 .
70
7 .
to
5
10
12
00
7
80
1 1
00
7
80
12
00
7
70
125
7.
70
7.
30
7.
20
6
20
6
30
5
80
7
00
S.
00
6
BO
5
60
6.
50
6
00
vO
-C*
-------
APPENDIX C (Continued)
TABLE C-8. RAW DATA FOR PYRENE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UG/L
01 STILLED
WATER
TAP
MATER
SURFACE
WATER
WASTEWATER
(C-94 »
WASTEWATER
(C-951
WASTEWATER
(C-961
AMPUL NO:
1
2
2
1
2
1
2
1
2
1
2
TRUE CONC:
2.00
2 00
2 .00
2 60
2 . OO
2 .60
2 . 00
2 . 60
2 00
2 .60
2 00
2 60
LAB NUMBER
101
2 . 10
1 .50
2.80
3 30
1 30
1 80
1 60
2 . 20
i eo
2 20
1 50
1 90
102
1 . 73
3. 12
1 42
2 70
1 . 90
2 . 96«
1 37
2 . 50
1 55
2 . 89
1 43
2 45
103
t .00
1. 20
0.00*
1 80
0.41
3 . 60 ~
0.00'
2.40
0.00*
0 00«
0 00*
0 00*
104
0.84
0.90
0.98
0 97
1 . 40
1 .80
1 50
1 . 80
1 30
1 90
1 20
1 . 80
108
1 . 18
0.37
2.80
t 82
1 55
1 .56
1 77
1 29
1 84
0 85
1 46
3 17
1 10
1 .40
2 . 20
2 .80*
3 50»
2 20
1 85
3 . 06*
4 . 32 *
2 . 66
3 90*
2 . 70
2 . 96
1 <2
1 14
I . 08
0 71
0 91
III
1 86
1 37
2 M
2 16
2.17
1 16
1 15
MS
0.00*
0.00*
0.00»
0. 00«
0. 00~
0. 00*
0.00*
0 . 00»
0 00*
0 . 00*
0.00*
0.00*
113
1 . 70
2 . 10
1 . 10
1 . 60
1 . 70
1 .90
1 .50
2 . 20
1 40
2.20
1 .60
2 . 00
11S
1 . 16
2.44
t 19
1 97
1 12
1 29
0.97
1 . 89
1 .69
2 23
2 30
2 . 60
117
0.40
0.43
1 .28
1 42
1 . 28
I 46
0 . 79
1 65
1 14
1 . 54
0.64
1 52
111
f eo
1 53
0 96
1 .38
1 .50
1 80
1 .03
2 83
1 . 38
1 90
1 23
1 86
122 <
0.80*
1 .40 <
0.80*
< 0.80» <
0.80» <
0. 80 ~
< 0.80* <
0.80*
1 . 60 <
0 . 80*
< 0.80* <
0. 80»
123
11.70«
13 SO*
1 1 00«
16 30'
12.20*
15 90*
17.10'
15. 70»
13 . 40*
15 70*
15 30*
20 I0»
124
1 . 10
1 90
1 . 10
1 40
2 00
1 70
1 30
1 . 20
1 40
1 40
1 70
1 .50
125
1 .60
1 .20
1 .80
3 00
2.20
1 70
1 .90
2.00
1 .60
2 80
1 .40
1 . 80
NO
w
-------
APPENDIX C (Continued)
TABLE C-8. RAW DATA FOR PYRENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DISTILLED MATER
TAP
WATER
SURFACE
WATER
WASTEWATER
(C
-94 )
WASTEWATER
-------
LAB
101
102
103
104
108
110
1 12
110
IIS
116
117
119
<22
123
124
125
-96
6
00
00
40
00
00
50
00
so
00'
30
30
10
40
eo<
30
00
BO
APPENDIX C (Continued)
TABLE C-8. RAW DATA FOR PYRENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED MATER TAP WATER SURFACE WATER WASTEWATER IC-94) WASTEWATER (C-951
3650565658
90.00 75.OO 90.00 75.00 90.00 75.00 90.00 75.00 90.00 75.00
62 . 00
77. 00
79.00
ee oo
75 . 00
63.00
72 . 00
66. 00
38 00
39.00
52 .00
81 . 70
77 10
a? 90
88 40
58 50
77 20
55 . 20
80 30
50.30
110.00
66. 00
t 16 00
50 00
89.00
74 00
28. 00
53 . 00
270 00'
42 . 00
32 00
33.00
38 . 00
22 00
34 00
32 00
66 00
5 1 . 00
75 00
~
7 1 .30
48.60
49. 20
30 . 70
34 40
73 20
4 1.10
4 1 . 20
90 60
4 7 . 00
136.00
57.60
85.40*
150.00*
103.00
115 00*
90 . 60*
96 40*
121 00*
116.00*
59.56
58 . OO
33.59
242 93*
12.66
49 00
68 14
53 00
53 64
40 . 90
0.00*
34.00
51 .00
4 40
24.00*
0 00*
0. 00*
0.00*
0 00*
0 . 00«
67. 10
56.90
76.00
54 00
82 60
65 00
75.60
84.30*
77 70
62.00
75 90
69.60
49 . 20
56.90
73.90
56 00
58. 30
41 40
60 30
63 40
65 00
41.00
80.30
43. 10
35.90
64 40
34 .50
50 20
73 90
05 10
77.60
67.20
7.9. 20
71 00
82 80
68 30
78 60
60 90
84 40
60.90
38.20
14 . 70
44 .50
26 70
35.40*
3 90*
51.90*
51 .90*
48 30
~
36. 70
46 70
39.30
32 90
64 . 10
45.60
61.60
47 BO
2 1 .30
38 20
69.00
64.00
63.00
61 . 00
50.00
34.00
81 . 00
56 00
96.00
60 00
86.50
65.60
82.30
55 BO
77 .80
57.80
71 . 40
55 50
02 90
61 . 50
-------
LAB
101
102
f 03
104
108
( 10
I 12
t IS
I 15
I IS
117
119
122
123
124
96 >
2
SO
43
44
00*
35
27
74 *
51
39
73
79
24
42
00*
4 I
40
40
APPENDIX C (Continued)
TABLE C-9. RAW DATA FOR BENZO(A)ANTHRACENE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UG/L
DISTILLED WATER TAP HATER SURFACE WATER WASTEWATER (C-94) WASTEWATER (C-95)
21212(2)2
0.50 0.60 0.50 O 60 0.50 0.60 0.50 0 60 0.50 0 60
0.2B 0 36
0.39 0 53
0 00* 0.00*
0 13* O IB*
0 75 0.13
0.70* 0.48*
0.55 0.70
0.22 0.37
0 84 0.81
O 43 0 71
0.06* 0.08*
0.39 0.48
1.40* 2.60*
0.32 0.39
0.33 0.55
0.40 0.30
0 59 0 84
0.31 0 47
0.87 0 32
O.I3» 0 I5»
0 81 0 60
0 78* 0 72'
1.11 0 13
0.29 0 40
0 58 0 88
0.47 O 62
0 13 0 17
0.29 0 34
0.80* I 00*
0.32 0 34
0.20 0 43
0.40 0 40
0 27 0 35
0.30 0.30
0 00* 0 00*
0 28* O.34~
1 08* 0 43
0 82* 0 68*
0 26 1 . 63 ~
0 31 0 42
0 58 0.67'
O 38 0 47
O 22* 0 22*
0 32 0.38
0 90« 0 80*
0 30 0.41
0.59 0.45
0 40 0.40
0.40 0 53
0 35 0 47
1 20 0.00*
0.29 0.35
0 83 0.31
0 60* I 00*
0 53 0.60
0.32 0.39
0.5B 0.8 1
0 33 0.65
0 I5> 0 29«
0.34 0 44
1 . 10 I.4 0*
0 60 0 44
0 35 0.30
0.40 0.30
0.27 0 38
O 35 0 48
0 00* 0.00*
O 27 0 37
0 19 0 42
O 70* 0 82*
O 58 0 76
0 45 0 32
0 52 0 79
O 55 O 73
O 26 0 32
0 34 0 39
2 30* I 20*
0 31 0 35
0 29 0 41
0.40 0.40
-------
LAB
101
102
103
104
108
no
I 12
nd
IIS
tie
117
n«
122
123
124
I2S
98
4
00
40
77
70
90
f 9
40
02
20
SO
31
80
97
30
39
40
40
APPENDIX C (Continued)
TABLE C-9. RAW DATA FOR BENZO(A)ANTHRACENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DISTILLED WATER TAP WATER SURFACE WATER WASTEWATER (C-94> WASTEWATER
3434343434
8.00 5.00 8.00 5.00 8.00 5.00 6.00 5.00 8 00 5.00
2.20
4 . 00
8.00
5.30
4 . 70
S. 25
3.80
5.27
2 72
4.71
2 80
i .40
5.50
6.50
4.40
1 .40*
1.60*
1 .80*
1 80*
2.50*
4.33
4.29
5.21
0 36
6.93
18.00*
10.40*
11.80*
9.80*
10 20*
4 38
3.55
8.35
5.87
3.83
3.20
4.80
4.70
4 70
3.40
8 80*
7 50*
830
6 90
9 . 00*
3.40
3.88
2. ta
2 83
4 . 70
1 .03*
0.63*
2.84
2. 10
2.42*
4.89
4.22
4.59
4 23
4.51
13.90*
8.20*
21 .80*
4 .90*
18.80*
4.27
2. 10
1 .28
1 .85
3.09
5.00
350
4 .50
4 . 70
5.20
3.20
2.70
2.80
2.80
2.70
3 . 70
5.30
4 . 20
2 80
3 50
3 88
5.59
4 . 10
5 48
3 93
4 80
3 . 20
5 80
0 00«
4 50
2 20'
2.80
2 00
3 10
0 70
625
2.98
6 00
1 06
1 . 86
1 1 .20*
12 40*
1 1 20*
13 80*
8 . 80*
3 35
1 .44
3 00
4 05
3 74
350
4 . 70
4 .60
4 20
3.20
8 80
8 . 50
7 10
7 80
7.10*
3 89
3.31
4 .03
4 . 78
1 .55
2.53*
2.39*
1 .57*
1 80
2 .80
3 81
8 25
5.46
4 81
3 08
9 40*
13.80*
38.30*
27 80»
15.60*
3 18
4.31
4 04
4 34
2.11
4 . 00
5.00
3 80
5 00
4 . 00
2 80
2.60
2.40
2.60
2.30
-------
APPENDIX C (Continued)
TABLE C-9. RAM DATA FOR BENZO(A)ANTHRACENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED WATER TAP MATER SURFACE WATER WASTEWATER IC-94) WASTEWATER IC-95) WASTEWATER (C-98>
AMPUL NO: 5 6 5 0 5 0 5 6 5 6 5 6
TRUE CONC: 12.00 18.00 12.00 (6.00 12 00 10.00 12.00 IB 00 12 00 18 00 12.00 IB 00
LAB NUMBER
101
7 .
30
12
. 00
10
. 00
ie
00
10
.00
14
00
8.
60
12
00
4 .
40
8
80
6
40
1 1 .
00
102
0
37
15
.30
9
82
<5
80
10
80
1 1
80
9.
88
1 1
70
10
00
1 1
20
10
20
13 .
20
103
12
00
12
.00
10
00
8
90
6
80
9
50
2
70
1 1
00
7
30
5 .
60
7
80
6
60
104
2
30*
3
20»
2
90*
3
20*
3
70*
4
80*
7
. 40
8
90
8
.90
~
7
80
t 1
00
108
22
. 10
12
10
13
40
10
10
1 1
60
31
90*
4
92
17
80
9
.75
8
33
10
30
13
30
1 10
30
.80*
25
. 40*
25
00*
32
40*
28
40*
3 1
50»
23
20«
33
00*
25
40*
30
80*
27
20*
37
00*
' '2
8
.97
14
.90
7 .
83
9
88
3
35
14
10
9
05
1 1
90
1 1
54
14
10
8
. 72
12
30
1 IS
4
. 10
1 1
90
7.
30
14
00
9
00
7
80
8.
50
13
SO
7
10
13
80
7
. 10
10
90
1 IS
17
. 10
18
30
15 .
80
17
30
IB
30
22
00
14
70
25
20*
16
50
21
50
18
or
22
40*
t IS
12
.70
15
.80
10.
20
13
70
10
40
8.
52
10
30
12
50
1 1
70
IS
90
5
. 50
1 1
40
1 17
9
18*
5.
92*
9.
15
7 .
22
3
63*
to
30»
5
28*
7
07*
19
10
10
90
8
19
14
90
t 19
9
.36
12
20
11 .
30
15
10
10
90
13
30
1 1
30
14
90
1 1
30
12
80
10
00
12
60
122
30
.40'
24
. 30*
39
50*
35
40*
32
80*
10
50*
46
10*
56
4 0*
58
50*
~
14
30*
81
40*
123
7
.94
6
22
8
91
7
83
10
40
1 1
40
9
88
to
80
2
30
8
21
10
80
10
50
124
5
90
1 1
00
12
00
1 1
00
7 .
30
7
20
9
20
1 1
00
13
00
12
00
15
00
13
00
125
B
50
8.
90
8
10
8
00
B.
40
5
00
5
30
6
10
5
40
5 .
30
5
10
7
50
O
O
-------
LAB
101
102
103
104
I OS
110
112
"J
IIS
tie
117
119
122
123
124
125
96)
2
00
50
5 1
20
20*
40*
34
86
80
10
55
34
72
50
85
80
70
APPENDIX C (Continued)
. TABLE C-10. RAW DATA FOR CHYRSENE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UG/L
DISTILLED MATER TAP WATER SURFACE MATER WASTEWATER
-------
APPENDIX C (Continued)
TABLE C-10. RAW DATA FOR CHYRSENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DISTILLED WATER
TAP
WATER
SURFACE
WATER
WASTEWATER
«C
94 )
WASTEWATER
1 C-95 >
WASTEWATER
(C-96)
AMPUL NO:
3
4
3
4
3
4
3
4
3
4
3
4
TRUE CONC:
20 . 00
28.00
20 . 00
28
00
20 00
28 00
20 . 00
28
00
20 00
28 00
20 00
28 00
LAB NUMBER
101
IS 00
30 . 00
22 . 00*
35
00*
17 00
22 00
2 1 00
25
00
15 00
25 00
13 00
23 00
102
20.60
2 1 .90
20.00
IB
90
18 . 00
26.30
26 90
28
10
20.70
24 . 60
19. 70
23 70
103
0. 00*
0.00*
55 . 00*
96
00*
0.47
94 00*
69 00*
103
00*
39 00
100 00*
0 . 00*
10. 00*
104
3.90*
5 . 20*
3 .80*
4
70*
7 30*
10 00*
7 50*
7
00*
7 I0»
2 40*
6 . 50*
12 00«
108
4 .38
2 .98
3 33
2
2 1
17.30
II 80
27 00
19
90
57 00
64 00
52.00
46 00
1 10
34 . 00
39.40
29 . 00
40
60
24 40
37 40
28 40
55
40 ~
47 40
47 80
4 0 00
33 60
1 12
8.99
9.88
17 . 00
23
35
12.69
15 27
8 45
1 1
78
12 77
18 42
15 88
8 75
27.00*
60.00*
38.00*
55
00*
30.00*
47 00*
38 00*
53
00*
34 00
44 00
38 00
28 00
115
24 .30
33.20
23 . 00
32
50
24 . 20
3 1.10
15 60
30
70
20 20
3 110
18 30
29 50
116
16.30*
26 30*
10.20
19
30
22 40
28 10
15 70
35
00
24 90
12 80
28 10
39 20
117
7.79
6.00
11.10
16
40
8 75
15.20
8 38
8
84
12 .80
15 60
9.65
11.10
1 IS
14 . 10
23.50
17.80
25
70
19 20
21 60
15 60
31
70
18.30
25 50
17 . 70
22 80
122
10.30
13.60
18 .30
8
to
16 . 70
13 10
11.40
43
50*
22 .80
19 80
16 10
7 00
123
12.40
13.80
3.61
9
82
9.89
16. 20
13 60
21
40
1 1 80*
14 . 10*
15 10
22 40
124
5.00
18.00
13-00
2 1
00
13 . 00
13 00
14 . 00
19
00
15 00
2 1 00
15 . 00
22 00
125
10. 20
2 1.80
15.20
20
BO
12 00
22 50
15 80
27
10
25 80
30.30
22 . 60
32 . 70
o
N>
-------
101
102
103
104
108
I 10
( 12
lift
I IS
116
117
119
122
123
124
I2S
APPENDIX C (Continued)
TABLE C-10. RAW DATA FOR CHYRSENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED MATER TAP MATCH SURFACE WATER WASTEWATER
-------
APPENDIX C (Continued)
TABLE C-ll. RAW DATA FOR BENZO(B)FLUORANTHENE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UG/L
DISTILLED
WATER
TAP
WATER
SURFACE
WATER
WASTEWATER
-------
IAS
101
103
103
104
108
ItO
;k
I IS
i is
117
«19
122
123
124
APPENDIX C (Continued)
TABLE C-ll. RAW DATA FOR BENZO(B)FLUORANTHENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DISTILLED WATER TAP WATER SURFACE WATER WASTEWATER (C-94) WASTEWATER WASTEWATER tC-96>
34 34343434 34
3.00 2.00 3.00 2 00 3.00 2.00 3.00 2 00 3.00 2.00 3.00 7 00
1.90 0.70
7.It* 4.82*
2.10 0.05
9.SI* 0.66*
0.13* 0.05*
3.64 2.12
13.20* 1-00
1.90 2.00
3.50 2.60
1.81 I.59
1.21 0.48
2.12 1-86
1.70 0.90
2.66 137
2.60 140
1.80 180
2. 10 I 30
7. 17* 3 71*
3.90 5 80*
0.72* 0 57*
0.I7» 0.18*
3. 16 2 24
313 2 63
2.20 2 00
3.20 2 60
I.06 I 18
1 86 I 20
2.32 I 90
3.00 0.00
0. 54 1.04
2.40 I 20
2.40 I 80
I 70 I 20
6 76* 5 ¦ 12
4 40 4 10'
1 40 100
0.92 0.47
2.42 2 08
I 96 117
2.10 I 70
3.70 2. 10
2.27 1 57
1.20 1 09
2.47 181
2.70 1.50
2.12 2 . 05
2.00 130
2.00 160
2 08 I 40
7.52* 5 29*
3 80 3 10
I.60 0.86
0.84 0.49
2 69 2 47
1.44 13.06*
2.20 200
1.90 2.20
150 2 03
1.34 0 75
2.28 2.50
1.60 5.50*
2 63 2 08
1 .40 I . 70
2.00 2.00
I 00' 1.20*
7 48~ 5 10*
2.70 2 60
» BO O 23
1 96 I 84
4.44~ 2 88
2 43 2 02
1.90 0.48
2 80 7 30
2 68 0 7 1
2 20 I 46
2 52 2 25
3 50 2 10
2 40 I 44
2 60 I 70
2.10 I 80
l.}0< I 20*
7.17* 4 93*
1 60 3 00
I.4C 1.30
3 66 2 . 75
3.95 2.16
2.76 0 97
2.40 1.00
2 .50 2 30
3. 18 2.25
1 29 0.79
2.75 2.19
2.90 0.90
2.87 2 35
2 80 2 00
2 00 .80
-------
LAB
«01
102
103
104
(OS
I to
1 12
H8
115
116
I 17
119
122
123
124
APPENDIX C (Continued)
TABLE C-ll. RAW DATA FOR BENZO(B)FLUORANTHENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED MATER
5
8 . 00
6
1100
TAP WATER
5
8 00
6
I I 00
SURFACE WATER
5
8 . 00
e
II oo
WASTEWATER (C-94) WASTEWATER (C-951 WASTEWATER
5
e oo
e
1100
5
8 00
e
II oo
5
8 00
2 SO
13 70*
II 00
I .50*
0. 02*
10. 70
5.52
5.70
10. 70
9 88
4.75
6 97
6 10
7.54
4.30
B. 10
3.00
26.50*
14 00
2 . 00*
0. 08*
9.20
12.92
9.00
10. 10
11.23
BO
07
50
75
90
10
4 .80
20 50*
15 00*
I .90*
0. 10*
8 78
3.64
3 80
9 10
9 29
7 30
8 23
8 60
6 80
7.40
6.40
8 70
26 80*
12 00
2 20*
06*
I I 70
10. 05
50
60
12 5 1
5 88
12 40
7 20
8 10
8 70
6 80
5 50
19 70*
9 90
2 60
0 . 67
10 40
57
40
00
77
50
73
20
76
00
70
6 80
2 I.60
16.00
3 20
0.31
17 70
I I 07
10 70
II 90
6 04
7 88
I t 10
2 30
10 40
4 10
5 00
4 70
17.40*
3.60
5 . 20
0.48
7 31
7 3 1
7 . 00
7 .90
8.57
4 32
9 45
8 . 00
8 37
6 70
5 20
6 60
2 I 20*
12 00
6 30
0 39
15 50
9 51
tO 50
13 10
I I 00
8 11
12 60
13 11
7 29
8 10
5 40
2 70*
18.00'
12 00
6 60
I . 13
12 80
9 50
5 60
9 80
9 12
18.80
9 95
12 50
I 40
8 . 00
5 tO
4 . 00*
20.30*
11 00
~
I 09
te to
11.97
9 40
12 60
14 40
7 80
I I . 30
7 29
8 80
5 50
3 70*
18 10*
9 90
5 60
2 I t
13 20
7 69
7 20
10 00
4 . 08
6 29
7 82
2.90
9 51
9 70
4 90
-------
LAB
101
tOl
103
104
108
110
112
II*
IIS
tie
117
119
(23
<23
124
APPENDIX C (Continued)
TABLE C-12. RAW DATA FOR BENZO(K)FLUORANTHENE ANALYSIS BY MATER TYPE
LOW YOUDEN PAIR, UG/L
DISTILLED WATER TAP WATER SURFACE WATER WASTEWATER
-------
AMPt
TRUI
LftB
101
102
103
104
108
110
112
IIS
I IS
I te
117
119
122
123
124
96)
4
to
36*
71
to
62
74
70
48
31
89
92*
27
75
30
14*
40
10
APPENDIX C (Continued)
TABLE C-12. RAW DATA FOR BENZO(K)FLUORANTHENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DISTILLED WATER TAP MATER SURFACE WATER WASTEWATER
0 24*
0 37*
1 85*
2 65
1 . 76
2 52
0 80
0 00*
2 50
0 00*
0 42
0 80
0 12
0. 75
0 39
2.07
2.54
2 . 20
0 84
1 .42
0 80
1 .22
0 19
14 1
I 12
1 . 38
0 62
0. 70*
0 48*
0.80
0 91
1 20
0 94
1 . 00
3 54*
4 74
1 28
5 . 70*
0 25*
0 75
0 50
0 43
0 90
0 92
0 80
0 97
1 . 70*
1 to
0.70
0.90
9 27*
10 90*
6 15*
12.10*
2 60«
4 00
2.70
4 50*
1 00
1 20
t .00
t . 30
-------
APPENDIX C (Continued)
TABLE C-12. RAW DATA FOR BENZO(K)FLUORANTHENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTI
LLED HATER
TAP
WATER
SURFACE
MATER
WASTEWATER
1C-94 >
WASTEWATER
(C- 95 >
WASTEWATER
AMPUL NO:
S
S
5
6
5
6
5
0
5
6
5
0
TRUE COttC:
4.00
6 . 00
4.00
BOO
4 . 00
o
c
e
4 00
6 00
4 . 00
6. 00
4 . 00
n. oo
LAB NUMBER
I0»
0.43
0.53
1.30
J 70
1.60'
2 00*
1 30
2. 10
0 . 70«
1 . 20*
1 00*
2 . to*
102
3.96
10.20
6.33
1 1 . 30
7. 17
8.68
6.31*
8 55
6.53
7.90
6 45
9.49
103
7 70*
9.30
9 . 20
7 90
6.20
1100
23 00*
9 . 30
t . 70
92.00*
1 1 00
72.00*
104
0.52
0.63
0. 86*
1 . 10*
1 .20
1 . 60
2 40
3 . 20
3 . 00
2 . 60
4 . 20
108
*
0. 06*
0 to
0. 06
0 . 49
0 64
0 . 50
0.37
2 . 22
2.68
2.11
2 05
1 10
3.35
3.46
2 . 75
4.56
3.35
5 78
2.48
5. 16
3 96
5.56
3.88
5.34
fa
0.44
5.58
©36
4.81
1 . 00
5 . 74
2 75
4 . 14
0 . 42
5 . 96
3.51
5 . 54
til
1 .50
2 90
1 .20
3. 20
2. 10
3 20
1 .80
3. 20
1 .50*
2 . 80*
t .80
3 . 10
tts
3. IO
4 . 00
3 20
3.90
3. 10
5 OO
3. IO
5. 10
3 60
5. 10
3.60
5 . 00
its
14.60*
17.20*
14 .90
22.00*
12.00*
1100 ,
13.70*
19.70*
14 . 40*
26.00*
6.50*
16 20*
117
2.75
1 .38
2.00
1.81
0. 73*
2 . 84*
1.28*
1.38*
6 . 08
I .32
1. 86
4 17
119
1.97
2.93
2.69
4 .33
2 73
3 82
2 .95
4.22
3.06
3.97
2.41
3 59
122
1.70
1. 70
2 50
2.40
1.90
0 80
2 30
4.30
3.50
~
0.80
4 00
123
30.10*
20.70*
26 70*
33.20*
33.50*
42.30*
34 10*
40.10*
5 . 63
5 03
35.00*
44 70*
124
4.40*
9 90*
1 1 00
14 . 00
6. 10
6 80
9 . 80*
12.00
11.00*
12 . 00
13.00
1 1 . 00
t25
3.00
3.30
3.20
3.60
2.60
3.00
2.80
3.00
2 90
3. 10
2.80
3 30
o
VO
-------
APPENDIX C (Continued)
TABLE C-13. RAW DATA FOR BENZO(A)PYRENE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UG/L
DISTILLED
WATER
TAP
WATER
SURFACE
WATER
WASTEWATER
(C-94 >
WASTEWATER
(C-95)
WASTEWATER
< C-98 >
AMPUL NO:
1
2
1
2
1
2
1
2
1
2
1
2
TRUE CONC:
0.20
0 . 30
0 . 20
0 30
o
o
0 30
0 . 20
0 . 30
o
w
o
0 30
0 . 20
0 . 30
LAB NUMBER
0 34*
101
0 25
0 59*
0 17*
0 30*
0 19
0 . 24
0. 22*
0 38*
0 18
0 38
0 22*
102
0. (3
0.27
0 . 05
0. 13
0 19
0. 25
0 14
0 25
0. 13
0 . 28
0.11
0 24
103
0 . 00*
0. 00*
0. 00»
0 00*
0.00*
0 . 00*
0 . 00*
o.oo*
0 00*
0.00*
0 00*
0 00*
104
O.OB
0.01
0 09
0 12
0 17
0 24
0 19
0 32
0 18
0 3 1
0 18
0 29
108
0. 13
0.11
0 10
0 10
0 30
0 38
0 26
0 4 1
1 98*
2 01*
2 20*
2 .85*
1 10
0 10
0 13
0 04
0 14
0 09
0 14
0 09
0 18
0 13
0 23
0 18
0 18
' 'I
O il
0.25
0(1
0 88 ~
0 14
0 27
0 18
0 24
0 10
0 02
0. 13
0 16
1 10
0.09
0.17
0 08
0 17
Oil
0 16
0. 12
0 22
0 13
Oil
0. 13
0 25
1 19
0 . 05
0. 17
0 OB
0 09
0 06
0. 18
0 18
0 20
0 09
0 21
0 18
0 23
1 16
0.17*
0.35*
0 17
0 . 26
0 . 19
0 . 25
0 17
0.37
0 33*
0 . 40
0 . 29
0.44 ~
117 <
0.00* <
0.00*
0 . 05
0 . 07
0.04
0 04
0 08
0. 14
0. 07
0.12
0. 04
0. 16
1 19
0. 14
0.21
0. 14
0 19
0. 19
0. 24
0 12
0 14
0 14
0. 22
0. 15
0 23
122
O.OB
0.20 <
0.01*
0 03
0.04
0. 08
0 . 09
0. 10
0 20
0 10
0 20
0 . 20
123
0. II
0. IB
0 10
0 IB
0. 12
0 . 20
0. to
0 18
0.09
0. 13
Oil
0 16
124
009
0.25
0 02
0 13
0. 14
0 2 1
0. 18
0. 15
0 14
0 19
0 14
0 19
125
0.20
0.20
0 . 20
0 70
0 20
0 10
0 20
0 20
0.20
0 30
0 20
0.20
-------
APPENDIX C (Continued)
TABLE C-13. RAW DATA FOR BENZO(A)PYRENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DISTILLED WATER TAP MATER SURFACE WATER WASTEWATER WASTEWATER
-------
APPENDIX C (Continued)
TABLE C-13. RAW DATA FOR BENZO(A)PYRENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED WATER TAP WATER SURFACE WATER WASTEWATER WASTEWATER (C-95) WASTEWATER
AMPUL NO: 5 65656585650
TRUE CONC: 12.00 15.00 12 00 15 00 12.00 15 00 12.00 15 00 12 00 15.00 12.00 15 00
LAB NUMBER
101
3.
70
4
. 30
13
. 00»
24
00
5
80
17
00
14
00«
18
00»
4 .
60
1 1 .
00
1 1
0O»
18
00'
102
5.
51
12
.80
9
39
14
00
10
10
1 1
00
9
02
10
70
9
54
9
69
9
68
12
10
103
14
00
3
.30
17
00
1 1
00
15
00
IB
00
2
70
1
30
5.
70*
1
00*
0
13
1
30
104
2 .
90
3
. 20
4 .
00
4
40
5 .
20
6.
20
1 1
00
13
00
15
00
~
12
00
18
00
I0B
0
. IB
0
12
0.
1 1
0
09
0
50
0
47
0
59
0
43
1
82
1
19
1
17
1
55
110
1 1
32
12
50
8
42
12
00
1 1
84
IB
70
9
96
15
50
14
36
16
50
14
50
17
10
1 12
5
. 33
12
, 40
3.
64
9
44
2 .
13
1 I
90
7
88
9
70
9
92
1 1
60
8
38
1 1
20
"»
6
. 20
9
80
4 .
00
8
90
8
60
1 1
20
7
60
t 1
90
6
20
to
70
7
80
1 1
80
MS
9
. 10
9.
30
6.
60
7
20
9
40
1 I
80
8
50
14
50
9
. 20
1 1 .
40
1 1
10
12
50
116
13
.90*
14 .
50*
1 1 .
20
15.
00
to
90
8
44
I 1
50
*3
80
12
80
17.
30
6
43
10.
70
117
3
. 88*
1 .
94 »
4 .
61
2
64
2
51
8
43
4 .
25
8 .
61
18
20
7 .
52
6
78
12
00
1 19
7
.61
9.
92
10
40
14
20
10
60
13
00
1 1
00
13
70
12
10
12 .
90
8
78
10
70
122
5
.90
4 .
50
6.
80
5
30
5.
50
1
90
7
80
12
00
9
50
~
2
20
9
30
123
5
.43
5.
09
5.
17
5
82
8 .
1 1
8
59
8
79
8 .
84
1
28
28.
70*
9
05
10
0 1
124
3
.80
8.
60
6.
30
8
00
4 .
70
4 .
70
8 .
60
7 .
50
8.
50
9.
50
10
00
8
70
125
9
. 00
9.
10
9.
70
9
70
6
20
6
70
6
50
0
70
6
20
7 .
20
7
00
7
80
-------
APPENDIX C (Continued)
TABLE C-14. RAW DATA FOR DIBENZO(A,H)ANTHRACENE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UG/L
DISTILLED
WATER
TAP
MATER
SURFACE
WATER
WASTEWATER
(C 94 )
WASTEWATER
-------
LAB
101
102
103
104
108
I 10
I 12
It?
I 15
I IS
I 17
I 19
122
123
124
90)
4
00
20
25
30
60
49
te
39
10*
30
03
44
94
10
10
10
80
APPENDIX C (Continued)
TABLE C-14. RAW DATA FOR DIBENZO(A,H)ANTHRACENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DISTILLED WATER TAP WATER SURFACE WATER WASTEWATER (C-94) WASTEWATER
-------
APPENDIX C (Continued)
TABLE C-14. RAW DATA FOR DIBENZO(A,H)ANTHRACENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
OISTI
ILED MATER
TAP
MATER
SURFACE
MATER
MASTEMATER
(C 94 >
MASTEMATER
(C-95)
MASTEMATER
(C-96 I
AMPUL NO:
5
6
S
6
5
6
5
6
5
6
5
6
TRUE CONC:
24 .00
o
©
e
-------
LAB
101
102
103
104
108
1 10
I 12
11*
I 15
116
117
119
122
123
124
96)
2
40
10
20
00*
8 1
27»
SB*
62
30
08
54
76
95
70
32 *
95
10
APPENDIX C (Continued)
TABLE C-15. RAW DATA FOR BENZO(G,H,I)PERYLENE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UG/L
DISTILLED MATER TAP WATER SURFACE WATER WASTEWATER (C-94) WASTEWATER (C-951
1 2 12 12 12 12
I 00 1 40 1.00 I 40 1.00 1.40 1.00 1.40 1.00 1.40
2.00 2.20
0.92 I 23
0.00* 0.00*
0.23 0.23
0 24* 0.24*
1.20 I 04
1.49* 2.99'
0.60 1.00
0.70 1.12
0.59 I 27
O.lf 004
0.40 0.S7
0.30 0.80
0.24 0 34
0.41 I.00
1.80 1.20
0.72 0 99
0 72 1 25
0.00* 0 87
0.28* 0 32*
0.23* 0 23»
I.50* I 90*
1.48* 2 03*
0.57 0 90
0.75 0 91
0.97 I 21
0.26 0 38
0.62 0.80
0.60 0 70
0.36* 0 22 ~
0.51 0 93
0.90 C 80
0 52 0 65
O 82 0 97
0.00* 0.00*
0 .56 0 69
0 87 0 74
1 26 O 94
1.77 3 53*
0 78 1.20
0.78 O 84
0.52 0 83
0 47 0 46
0 81 0.90
0 40 0 50
0 23 0 39
0.55 0 73
I.90 I 30
0.66 1.00
0 84 I 22
0 00* 0 00«
0 53 0.80
0 40* 0.30*
1 05* 2.07*
1.45* 2 29*
0.71 I 30
0.82 I 09
0.58 I 28
0 52 0 83
0 44 I.00
0 50 0 70
0 14* 0 44*
0.60 0.59
I.00 I 00
0 67 1.20
0 81 I.27
3.30* 0.00*
0 52 0.82
2 04* 1.50
I.64* JOB'
1 83* I 75*
I 20 0 60
0.70 1.28
I 05 1.46
0.68 2 46*
0 57 0.87
140 I . 10
0 4 7* 0.58*
0 81 O 94
0 90 I 50
-------
APPENDIX C (Continued)
TABLE C-15. RAW DATA FOR BENZO(G,H,I)PERYLENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DISTILLED
MATER
TAP
MATER
SURFACE
WATER
WASTEWATER
(C-94)
WASTEWATER
(C-95)
WASTEWATER
(C
AMPUL NO:
3
4
3
4
3
4
3
4
3
4
3
TRUE CONC:
14 . 00
10 . 00
14 . 00
10 00
14 . 00
to oo
14 00
10 00
14 00
10 00
14 . 00
to
LAB NUMBER
101
4 .00
1 .50
8.40
5 50
9.50
6 40
1 1 00
7 70
6 40
7 . 20
5.00
6
102
6.52
5.07
12 . 70
6 37
12 20
8 30
IS 40
9.51
14 20
8 47
13 50
8
103
5 .40
3.50
17.00
3O 00*
13 .00
72.00*
15 00
20 00*
0 00"
15 . 00
0 00*
ta
104
3.80
2.40
2.80*
t 80*
5 . 70
4 10
6 . 60
3 50
8 70
0.91
8 00
5
108
0.23*
0. 22*
0. 2 !~
0.27«
tot
0 77
0.41*
0 32*
2 32
4 19
5 45
3
1 10
10 . 80
7 00
15.60*
10 4 0*
13.40
10 20
13 4 0*
II 30*
19 40*
9.60*
18.40*
8
* '2
0 . 97
6. 36*
23.24*
19 76*
21 .48
14 33
7 70*
10.51 *
19 73*
15.60*
5.49
8
i ra
5.20
8 20
1100
10 00
It .00
9 . 20
14 10
1 I . 00
10 20
7 10
12.80
5
1 IS
7.60
5.30
11 . 40
8 40
13.20
7 00
780
7.30
10.60
7 70
9. 10
7
t IB
4.91
3.St
4 .04
4 47
8. 18
5 57
5 89
7 54
10 70
2 50
It 90
7
1 17
0.64
0 64
7.64
4.50
6.40
6 00
5 78
2 88
9 89
8 . 50
5 47
2
1 19
5.54
5.20
8.85
5.03
9.38
6.40
9 50
7 48
8.43
7 64
to 10
7
122
4 .60
2.90
11 .80
2 30
106.00*
5.40
7. 10
20 10*
15.20
9 30
12 80
3
123
2.59
1.78
0.64*
1 . 29*
3. 15
2 . 32
4 . 36*
3.42*
3 74*
2 23*
4 37*
4
124
to. 00
7.50
7.50
6 40
7.00
4 . 00
7 . 70
5.80
9 60
8 00
8. 80
6
125
8.80
6.60
11 . 70
8 . §0
39.50*
7 . 00
14 .80
8.80
14 20
8 . 20
13 80
10
98)
4
00
30
25
00*
50
48
00*
37
00
70
81
91
52
90
26*
50
10
-------
LAB
101
102
103
104
108
110
112
IIP
115
i ie
117
119
122
123
124
125
96
6
00
00
70
00
00
1 I
00
50
00
40
00
00
40
70
70
00
60
APPENDIX C (Continued)
TABLE C-15. RAW DATA FOR BENZO(G,H,I)PERYLENE ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED WATER TAP WATER SURFACE WATER WASTEWATER WASTEWATER IC 951
5 650565666
35 00 50 00 35.00 50 00 35 00 50 00 35 00 50 00 35 00 50 00
B. 10
B . 00
28.00
44
00
29 00
38 00
24 . 00
35
00
13
00
21.00
12 30
30. 30
30 . 00
55
20
35.30
4 1 10
3 120
4 1
10
32
40
38 10
54 00
52.00
67.00*
59
00
4 7.00
83 00
9.80
55
00
8
70
13.00
3 . 40
2 SO
6.60*
8
60*
9 60
12 00
20 00
36
00
76
00
~
*
0. 24*
~
0
21*
0 91
0 . 54
0 28*
0
38*
3
. 43
1 52
25.60
27.60
39.20*
5 1
60*
29. 40
57 60
34.20*
53
00*
43
20*
63 20*
33. IB*
91 .30*
29.34*
82
10*
16 12
100 00
98 05 ~
79
00«
78
62*
103.60 »
8. 00
15 . 20
19 00
42
00
4 00
54 00
30 00
5 1
00
24
00
49 00
2 ! . 40
19.60
27 . 10
31
60
34 70
39 . 70
23.90
48
30
29
50
40 70
3 1 70
28. 00
24.90
34
40
29 1 1
20 . 60
25 91
34
10
33
80
42 20
35.30
18.80
21 .50
24
10
8 67
43 00
12 70
10
50
62
30
35 00
IB 40
24 . 90
23.80
40
00
28 10
37.90
24 . 20
33
60
29
80
35 . 30
19 40
19. 20
28.30
24
00
22 70
8 . 60
28 . 60
60.
90
49
70
7.49
8. 08
9.07*
1 1
20*
13.60
15 70
12.80*
12
90*
1
61 «
11.60*
6.60
7. 50
23.00
27
00
12 . 00
14 00
19 . 00
22
00
25
00
30 00
25.40
24 . 90
41.00*
48
30
28 . 40
47.70
34 50
46.
50
38
10
49 30
-------
toi
102
103
104
108
I 10
112
1l6
I IS
IIS
117
i ia
122
123
124
125
96)
2
00
49*
00*
00*
89
58*
33
66
81
90
31*
98
44
80
53
00
70
APPENDIX C (Continued)
TABLE C-16. RAW DATA FOR INDEN0(1,2,3-CD)PYRENE ANALYSIS BY MATER TYPE
LOW YOUDEN PAIR, UG/L
01 ST I LIED WATER TAP WATER SURFACE WATER WASTEWATER WASTEWATER (C-95) WASTEWATER
12 12 12(2121
0.75 1.00 0.75 1.00 0.75 1.00 0.75 1.00 0 75 1.00 0.75
0.33
0.94
0.50
0 . 68
0.33
0 45
0 35
0 . 48
0. 33*
0 . 56«
0 . 33*
1 .54*
2.23*
1 18*
J . 06 »
1.71*
2 10*
1 37»
1 96*
1 40*
2 . 14 ~
1 . 1 1*
I . 10*
0 80
0 . 00*
100
0 . 00*
0 00*
0 00*
0 00 ~
1 30
0. 00*
0. 00*
0.30
0. 33
0. 29*
0.35*
0 53
0 75
0 . 62
0.97
0 55
0 92
0. 60
0.28*
0. 19*
0. 13*
0 24 »
1 40*
1 22
1 . 52»
1 .34
3 90'
2 . 75
4 . 00*
0 40
0.34
0 40
0.53
0 40
0 24
0 30
0 53
0 35
0 56
0 . 36
0.27
0.84
0.27
0 96
0 43
0 97
0 41
0.51
0 29
0.51
0 69
0.29
0 58
0 34
0.50
0 32
0. 65
0.43
0. 76
0 48
0 37
0 41
0. 62
0 . 93
0.65
0 81
0.66
0 94
0. 74
1 26
0.7 1
1.01
0. 59
0 54*
1.06*
0.67*
1 . 20*
0.42
0 73
0. 52»
1 20*
1 . (5*
1 15*
0.96*
0. 15
0.20
0. 19
0 34
0 30
0 33
0 42
0.68
0 51
2 05
0 22
0. 28
0.47
0.33
0 . 43
0 31.
0 . 49
0. 28
0.56
0 . 23
0.45
0 . 38
o.eo
1 .30
0.70
0.80
0.40
0.60
0.50
0 70
0 90
0. 70
1.40*
0.38
0. 56
0.31
0.43
0.42
0. 75
0 25
0 68
0. 34 ~
0 39*
0 34
0.65
1 .30
0.49
t 10
0 51
0 67
0 61
0.60
0 66
1 . 00
0 57
0.50
o eo
0.60
0. 70
0 . 70
0. 80
0 70
0.90
0.80
1 . 00
0 60
-------
LAB
101
102
103
104
108
110
1 12
MC
1 15
i te
117
1 19
122
123
124
90)
4
00
50*
70»
00*
70
39
20
72
40
10
40*
32
53
90
82
20
90
APPENDIX C (Continued)
TABLE C-16. RAW DATA FOR IN0EN0(1,2,3-CD)PYRENE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UG/L
DISTILLED WATER TAP WATFR SURFACE WATER WASTEWATER (C-9*> WASTEWATER (C-95)
3434343434
5 eo 8.00 5.00 6 00 5.00 8 00 5.00 6 00 5 00 8 00
2 . 00
2 .50
2 70
3
40
2.40
2 . 70
2.50
3. 10
1 .50*
2 . 70*
9. 70*
9.45*
10 30*
8
56*
9. 72*
1 1 90*
I 1 .30*
12 60«
11.10'
1 2.30*
8. 80
0.00*
13.00*
33
00*
0 . 00*
23.00 *
9 . 80
18 00*
0 00*
12.00
1 . 90
2.20
1 . 80*
1
60*
3 . 20
3 60
3 40
3 00
3 70
0 67
0. 45*
0. 28*
0. 50
0
19*
1 . 70
1 90
2.46
1 77
5 80
4 .46
3 . 84
3 54
4 32
4
70
3.44
4 48
3 78
4 . 76
5 54
5 04
1 . 52
1 .53
3.02
4
27
2.69
3.05
0.84
2 02
3 00
3 99
2 . 50
4 .30
2 .90
4
30
3. 10
3 90
3 60
4 50
2 90
3 40
4.50
4 80
4 70
8
50
5.40
4 . 60
3 20
4 80
4 . 00
5.30
1 1 .40*
11.80*
6.99*
1 1
70*
14 . 80*
15.00*
9 11*
22 40'
22.40*
7.39*
0. 97
0 . 77
2 88
2
55
1 .96
2 .69
2 27
1 87
4 70
4 51
1.99
2.87
1 90
2
37
3.08
3 . 17
2 38
2 79
3 24
4 . 08
3.30
4.80
7 10
2
. 30
8. 10
5 . 10
4 10
19 B0<
1 1 00«
8 80
2 . 74
2 . 28
0.51
1
81
3.00
3 . 06
3 30
3 94
2.82*
3 . 00*
5.50
4.50
4 .80
6
60
3.60
3 .30
4 50
4 . 80
5 50
5 10
2.60
3.80
3.80
4
80
3.60
4 00
3.90
4 60
4 80
5 50
-------
APPENDIX C (Continued)
TABLE C-16. RAW DATA FOR INDENO(l,2,3-CD)PYRENE ANALYSIS BY MATER TYPE
HIGH YOUDEN PAIR, UG/L
DISTILLED WATER TAP WATER SURFACE WATER WASTEWATER WASTEWATER (C-95) WASTEWATER (C-96)
AMPUL NO: 505650595650
TRUE CONC: 22.00 15 00 22 . OO 15.00 22.00 15.00 22.00 15.00 22 00 15.00 22.00 15.00
LAB NUMBER
«0I
5
40
7 .
90
12
00
9
50
12
00
7 .
70
10
00
7
80
5.
40«
4 .
00*
~
5
.50*
102
23
. I0»
31.
90*
42
40*
38
70*
48.
20*
27
50 ~
42
50*
27
30*
44
50*
25
80 ~
44
I0»
31
00*
103
69
.00*
40
00«
77
00*
30
00*
54
.00*
40
00
13
00
28
00
48
00
25
00
41
. 00*
30
. 00
104
3
.40
1
80*
6
10*
4
00*
8
80
5.
20
18
00
12 .
00
23
00
~
19
00
15
00
I0S
0
I0»
0
15*
*
0
25»
0
83
0
76
1
42
1
66
3
77
2 .
73
3
73
4 .
22
110
16
. 00
8.
78
16.
90
12
10
18.
90
1.7
50
14 .
10
15
60
25
20
15
60
25.
70
15
20
112
7
.43
9.
62
6.
31
8
56
3
.25
10
20
t 1
93
8
03
16
20
10
57
13
70
10
30
11/8
e
. 20
7 .
40
8.
30
9 .
40
15
.00
1 1
SO
13
00
1 t
20
10
10
10
20
13
00
10
70
115
18
10
9.
10
<8.
90
to.
40
18
.90
12
80
IB
60
13
40
20
50
14
10
20
00
13
30
I 16
00
50*
47 .
60*
90
19*
71
I0»
70.
I0»
32.
10*
90
20*
7 1
. 90*
90
10*
95
10*
34 .
90*
42.
20*
117
1 1
90
3.
29
15.
60
6
82
5
.41
1 1
to
10
40
9
.43
60
80
9
08
16
20
18.
10
119
8.
83
6.
31
11.
10
11
10
14
.30
to
30
1 1
20
9
68
15
90
10
30
12
20
8
65
122
21 .
00
9.
70
29.
70
13
20
21
40
4 .
40
27
60
23
70
52
50
«
12
50
34
70
123
e.
31
9.
33
13
60
10
40
17
30
10.
40
IS
70
7
27
1
84*
8.
68*
14 .
50
I 1 .
10
124
7.
20
7.
50
20.
00
13
00
9
90
5.
20
17
00
10
00
22
00
13
00
25
00
12
00
125
14 .
20
8 .
30
18 .
80
10
50
15
. 10
9.
80
18.
30
10
20
18 .
90
10
20
16
80
12
50
-------
APPENDIX D
TABLE D-l. EFFECT OF WATER TYPE ON NAPHTHALENE ANALYSIS
~~ POINT ESTIMATES ~«
DISTILLED WATER SLOPE:GAMMA(I) - t.04424
WATER INTERCEPT(WATER-DISTILLEDl SLOPE
N1
REG(OISTILLED) I 956 47452 958.47452
REGIWATER/DISTILLED) 10 5 09192 56919
ERROR 450 117.61589 76137
2.18 .018 1
TOTAL
461
I08t 78234
TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
MATER
INTERCEPT(WATER-DISTILL ED I
ESTIMATE INTERVAL
SLOPE
ESTIMATE INTERVAL
0261
0277
55 10
7 182
268 I
. 7748
. 7672
. 1764
0447
4651
7226)
7 118)
2783)
48 10)
.0013)
0233
0190
. 0744
. I 148
02 08
1402
. 1426
2327
2825
1799
1868)
1805)
0839)
0530)
1382)
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AND THE CORRESPONDING WASTE WATER TOR THE ASSOCIATED PARAMETFR
-------
APPENDIX D (Continued)
TABLE D-2. EFFECT OF WATER TYPE ON ACENAPHTHYLENE ANALYSIS
~~ POINT ESTIMATES ~~
DISTILLED WATER SLOPE:GAMMA(I) - 112589
MATER INTERCEPT
2
.2900
-.0485
3
473 1
- 0507
4
9936
- 1542
5
661 1
- 0971
6
5758
-.0583
~ ~ ANALYSIS OF VARIANCE ~~
SOURCE
OF
SUM OF SQUARES MEAN SQUARE
PROB
is)
REGIDIST ILLED) I 1057 6634 1 1057 08341
REG(WATER/OIST ILLEOI 10 9 22423 .92242
ERROR 459 153 95890 .33542
2 75
. 002 7
TOTAL
470
1220 80860
TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES ~ ~
WATER
INTERCEPT(WATER-DISTILLED)
ESTIMATE INTERVAL
SLOPE I WATER-DISTILLED)
ESTIMATE INTERVAL
. 2960
4 731
.9936
.6611
. 5758
.5323
. 373 I
. 17 13
. 1599
. 2529
1243)
3194)
8 159)
482 I )
4044 )
0485
0507
1542
. 097 I
0583
2254
2330
3323
2751
2374
. 1285)
1316)
0240)
0808)
1209)
NOTE:
IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED MATER AND THE CORRESPONDING WASTE WATER FOR THE ASSOCIATED PARAMETFR(INTERCEPT/SLOPE)
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
TABLE
APPENDIX D (Continued)
D-3. EFFECT OF WATER TYPE ON ACENAPHTHENE ANALYSIS
POINT ESTIMATES
DISTILLED WAIER SLOPE : GAMMA ( I I -- I 03H34
WATER INTERCEPTIWATER-DISTILLED) SLOPE IWA T( R-Dl S11 LI ED I
2
- 4 209
1022
3
1432
0022
4
24 19
001 1
5
2686
0281
8
092 1
0374
to
*»
SOURCE
ANALYSIS OF VARIANCE
DF SUM OF SQUARES Mf AN SQUARE
HEO(DISTILLED) I 709 001*9 709 00189
RtGIMATE R/DISTIL(EO) 10 9 15317 91532
ERROR 400 III 90601 78227
I 83
PROS
0545
TOTAL
82 7.OS 107
TABLE OF 95% CONFIDENCE INTERVAI S FOR THE 01FF ERENCE S BETWEEN INTERCEPTS AND IMF DIFFERENCES BETWEEN SLOPES
WATER
INTERCEPT(WATER-DISTILLED)
ESTIMATE INTERVAL
SLOPE(WATER -DISTI LIED)
ESTIMATE INTERVAI
2
3
4
5
6
4209
. 1432
24 19
2688
0921
I 3330
-.7848
- 8840
- 8280
-.8060
4913)
I 0510)
I 14 781
I 1833)
9901 I
1022
0022
001 I
028 I
0374
098 I
1987
1972
2284
1594
3024 )
2031 )
1994 I
1702)
2342 )
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AND THE CORRESPONDING WASTE WATER FOR THE ASSOCIATED PARAMETERI INTERCEPT/SLOPE).
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARIIFR.
-------
APPENDIX D (Continued)
TABLE D-4. EFFECT OF WATER TYPE ON FLUORENE ANALYSIS
~~ POINT ESTIMATES
DISTILLED HATER SLOPE:GAMMA'I I = 95503
MATER INTERCEPT!MATER-OISTILLEDI SLOPE(MATER-DI ST ILLED I
2 -.3059 0752
3 1989 - 0350
4 .3383 - 04 88
5 .0125 - 0134
B .2853 - 0461
SOURCE
~~ ANALYSIS OF VARIANCE ~«
OF SUM OF SQUARES
N)
Ln
REGIDISTILLED) I 668 93203
REG!WATER/DISTILLED) 10 2 53991
ERROR 4 18 196 08694
MEAN SQUARE
868 93203
25399
4 691 I
54
PROB
8806
TOTAL
429
885.55888
TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS ANO THE DIFFERENCES BETWEEN SLOPES
MATER
2
3
4
5
8
INTERCEPT!WATER-DISTILLED I
ESTIMATE
3059
1989
3383
0125
2853
INTERVAL
- I 3757
- 8848
- 7320
- I 0975
- 82 17
7840)
I 2827)
I 4085)
I 1224)
I.3924 I
SLOPE(WATER-DISTILLEO)
ESTIMATE INTERVAL
0752
-.035O
- 0488
- 0 134
- 0*61
- 1558
- 2682
- 2798
- 2558
- 2848
3059)
1982 I
1820)
229 1 I
1927)
"°Te! BIST irLFBSWATCBAi!!n0TUt 'rnnsr rr N£! '2T"V*L THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER ANO THE CORRESPONDING WASTE WATER FOR THE ASSOCIATED PARAMETER
-------
APPENDIX D (Continued)
TABLE D-5. EFFECT OF WATER TYPE ON PHENANTHRENE ANALYSIS
POINT ESTIMATES ~~
DISTILLED WATER SLOPE:GAMMA I I> - 1088 IB
WATER INTERCEPT(WATER-DISI III ED) SLOPE TABLE or 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
WATER
INTERCEPT(WATER-DISTILLED I
ESTIMATE INTERVAL
SLOPE
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER
-------
APPENDIX D (Continued)
TABLE D-6. EFFECT OF WATER TYPE ON ANTHRACENE ANALYSIS
« POINT ESTIMATES ~~
DISTILLED WATER SLOPE:GAMMA ItI * 1.10903
WATER INTERCEPTtWATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 .0255 - 0052
3 .6925 - 1295
4 .7203 - I 128
5 .5613 - 1019
8 .7495 -.1291
ANALYSIS OF VARIANCE
SOURCE DF SUM OF QUAKES MEAN SQUARE F PROB
I-*
K) RECIDISTILLED) I 983.92303 983.92383
REG
5
.5813 1
-.0850 .
1.2077)
-.1019 (
- 2464 .
0426)
8
. 7495 1
1112 ,
1.3879)
-.1291 (
-.2718 .
.0134)
NOTE:
IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AND THE CORRESPONDING WASTE WATER FOR THE ASSOCIATED PARAME TF.R < INTERCEPT/SLOPE )
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
APPENDIX D (Continued)
TABLE D-7. EFFECT OF WATER TYPE ON FLUORANTHENE ANALYSIS
POINT ESTIMATES
DISTILLED WATER SLOPE:GAMMA(I) = .96753
WATER INTERCEPT(WATER-DISTILLED) SLOPE
-------
APPENDIX D (Continued)
TABLE D-8. EFFECT OF WATER TYPE ON PYRENE ANALYSIS
POINT ESTIMATES
DISTILLED WATER SLOPE:GAMMA(1 I = 1.06892
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLEDI
2 .2620 - 0634
3 2757 - 05*8
4 .3354 - 0696
5 3735 - 1022
6 .3063 - 0446
SOURCE
~ ~ ANALYSIS OF VARIANCE *
OF SUM OF SQUARES
fO
VO
REC(DISTILLED) I 1012.98007
REG(WATER/DISTILLED! 10 2 46146
ERROR 449 62 04649
MEAN SQUARE
1012.98007
24615
13019
PBOB
I 78 .0617
TOTAL
460
1077.48801
~~ TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
WATER
INTERCEPT(WATER-DISTILLED)
ESTIMATE INTERVAL
SLOPE(WATER-DISTILLED)
ESTIMATE INTERVAL
. 2620
2757
.3354
3735
3063
- 1021
- 0838
-.0300
0088
- 0546
.6262)
6351 I
7007)
738 I I
667 I I
0634
0548
0696
1022
- .0446
. 1740
. (650
18 18
.2141
(555
047 I >
05551
0426)
0097)
0664 )
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AND THE CORRESPONDING WASTE WATER FOR THE ASSOCIATED PARAMETEN(INTERCEPT/SLOPE) .
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
ANO ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
APPENDIX D (Continued)
TABLE D-9. EFFECT OF WATER TYPE ON BENZO(A)ANTHRACENE ANALYSIS
POINT ESTIMATES ~~
DISTILLED MATER SLOPE:GAMMA(I) = 982B8
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 OOOI 0128
3 - 0143 0139
4 IOSO - 0335
5 - 0244 - 0154
S . 0149 0294
SOURCE
ANALYSIS OF VARIANCE *
DF SUM OF SQUARES MEAN SQUARE
U>
O
REGIOI STILLED) 1
REG(WA TER/DISTILLED) 10
ERROR 420
TOTAL 43 1
777 58379
.94034
54.85436
833 37850
777 58379
09403
<3081
72
PROB
7058
» TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS ANO THE DIFFERENCES BETWEEN SLOPES »~
WATER
INTERCEPT(WATER-DISTILLED)
ESTIMATE
INTERVAL
SLOPE!WATER-DISTILLED)
ESTIMATE INTERVAL
2
. OOOI
3
- 0143
4
1050
5
- 0244
8
. 0 149
- 2309
- 2615
- 1277
- 2560
- 2 188
231 I )
.2329)
3376)
.207 I I
.2484)
0128
0139
0335
O 154
0294
1110
I 174
1583
1388
094 7
1366)
1453)
.0913)
1079)
1535)
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AND THE CORRESPONDING WASTE WATER FOR THE ASSOCIATED PARAMETER!INTERCEPT/SLOPE).
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
APPENDIX D (Continued)
TABLE D-10. EFFECT OF WATER TYPE ON CHRYSENE ANALYSIS
~~ POINT ESTIMATES ~~
DISTILLED WATER SLOPE:GAMMA(I) ' 98722
WATER INTERCEPTIWATER-DISTILLED) SLOPE 4WATFft - 01 ST ILLED>
2 .0168 0057
3 .2407 - 0580
4 .0887 0653
5 0998 1046
6 .1565 .0454
SOURCE
~* ANALYSI
OF
OJ
REC4DIST1LLED) I
REG(WATER/DISTILLEO) 10
ERROR 439
S OF VARIANCE '«
SUM OF SQUARES
772.59992
I I.04269
1*1.14149
MEAN SQUARE
772 59992
I.10427
253 17
4 36
PROB
. 0000
TOTAL
450
894 78410
TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
WATER
INTERCEPT(WATER-DISTILLED)
ESTIMATE INTERVAL
SLOPE(WATER-DISTILLED I
ESTIMATE INTERVAL
2
0168
3
. 2407
4
.0887
5
. 0998
6
. 1565
- 5237
- 314 I
- 4608
- 4367
- 3704
5574 )
.7954 )
.6383)
.6362)
6834 )
0057
- 0586
0653
. 1046
.0454
1754
2420
I 172
0744
1309
1868)
1248)
2478)
2836)
2216)
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AND THE CORRESPONDING WASTE WATER FOR THE ASSOCIATED PARAMETER(INTERCEPT/SLOPF)
THE SLOPE ANO INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
APPENDIX D (Continued)
TABLE D-ll. EFFECT OF WATER TYPE ON BENZO(B)FLUORANTHENE ANALYSIS
~ ~ POINT EST(MATES ~»
DISTILLED WATER SLOPE:GAMMA II) = 99154
WATER INTERCEPT) WATE R-DISTILLED) SLOPE
to
REQ(DISTILLED) I 1040 46326
REGtWATER/DISTILLED) 10 3 54982
ERROR 450 71 1543?
MEAN SOUARE
1046 40326
35498
. 158 11
2 25
PROB
0146
TOTAL 461
1121.16740
»~ TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES ~«
WATER
INTERCEPTIWATER-DISTILLF.D)
ESTIMATE INTERVAL
SLOPE(WATER-DISTILLED)
ESTIMATE INTERVAL
2
.0754 (
- - 124 1 ,
. 2748)
01 16 (
- 1 107 .
1338)
3
.0033 (
-.1934 .
.2000)
- 0258 (
- 1453 .
0937)
4
054 7 I
- 14 15 .
2508)
0103 <
- 1087 .
1293)
5
.1B65 <
- . 0344 .
3874 (
0153 <
-.1075 .
.1380)
6
.1821 <
-.0172 ,
3813)
0369 (
-.084 0 .
1578 )
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AND THE CORRESPONDING WASTE WATER FOR THE ASSOCIATED PARAMETFR
-------
APPENDIX D (Continued)
TABLE D-12. EFFECT OF WATER TYPE ON BENZO(K)FLUORANTHENE ANALYSIS
POINT ESTIMATES
DISTILLED WATER SLOPE:GAMMA_. REC(WATER/DISTILLED) 10 13 73283 1.37328 3 75 0001
OJ ERROR 395 144 54 I II 3*593
U>
TOTAL 400 1002.10208
~~ TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
INTERCEPT (WATER-DISTILLED) SLOPE < WA TER-01 ST I LLEI>)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .1088 I 1704 . 3939) 0359 < -.1040 . 2158)
3 .3319 I 0397 , .024 1) - 0549 I -.2472 . .1375)
4 2500 < - 04 20 . .5558) - 0220 < - 2191 . .1751)
5 .4977 < .1990 . .7905) - 0400 ( - 2435 . 1510)
0 .4208 ( .1274 . .7142) 0748 ( -I234 . 2730)
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AND THE CORRESPONDING WASTE WATER FOR THE ASSOCIATED PARAMETER.
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
APPENDIX D (Continued)
TABLE D-13. EFFECT OF WATER TYPE ON BENZO(A)PYRENE ANALYSIS
~* POINT ESTIMATES ~~
DISTILLED WATER SLOPE:GAMMA
2 1848 0958
3 2000 0339
4 2919 0128
5 2210 0979
6 .2897 .0320
»~ ANALYSIS OF VARIANCE ~
SOURCE
DF
SUM OF SQUARES
MEAN SQUARE
F PROB
REG(DISTILLED)
1
1247 92405
1247 92405
REGtWATER/DISTILLED)
10
15 58327
1.55833
4.12 0000
ERROR
484
183 02680
37815
TOTAL
495
1446.53392
TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES ~ ~
INTERCEPT(WATER-DISTILLED I SLOPE
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2
-.1848
<
.4861 .
1166)
0958 1
- 0689 .
2606)
3
2000
(
- . 0912 .
4912)
0339 (
-. 1267 .
.1944)
4
2919
(
-.0049 .
5888)
0128 (
- 1502 .
1759)
5
. 22 10
<
-0773 .
5192)
0979 <
- 0686 .
.2645)
6
2897
(
-0125 ,
.5918)
0370 (
-.1335 .
. 1975)
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AND THE CORRESPONDING WAS1E WATER FOR THE ASSOCIATED PARAMETER(I NTERCEPT/SLOPE».
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER
-------
APPENDIX D (Continued)
TABLE D-14. EFFECT OF WATER TYPE ON DIBENZO(A,H)ANTHRACENE ANALYSIS
POINT ESTIMATES *~
DISTILLED WATER SLOPE:GAMMA(t) * .90229
WATER INTERCEPT!WATER-OISTILLED) SLOPE(WATER-DlST 1LLED)
2 .3208 0873
3 2894 . 0706
4 .2778 I2S9
5 4474 0838
8 .6825 .0412
~ ~ ANALYSIS OF VARIANCE ~ »
SOURCE
DF
SUM OF SQUARES MEAN SQUARE
PROB
CO
Ui
REG(DISTILLED) I
REG1WATER/DIST ILLED) 10
ERROR 439
TOTAL 450
091.53070
22 23987
109 26783
1023.0384 t
891.53070
2.22399
.24890
8 94
0000
TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SICES
WATER
INTERCEPT(WATER-DISTILLED)
ESTIMATE INTERVAL
SLOPE(WATER-DISTILLEO)
ESTIMATE
INTERVAL
2
3208 (
-.0084 .
.8499)
.0873 (
-.0878 ,
2424 1
3
2894 (
-.0328 .
.6116)
.0766 (
-.0758 .
2290)
4
2778 <
-.0533 .
6089)
.1259 (
- 0297 .
.2815)
5
.4474 (
.1159 .
.7790)
.0838 I
- 0739 .
. 2414 )
6
.8825 (
.3635 .
1.0014)
-.04 12 (
-.1907 .
1082 )
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLEO WATER AND THE CORRESPONDING WASTE WATER FOR THE ASSOCIATED PARAMETFR(INTERCEPT/SLOPE>
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER
-------
APPENDIX D (Continued)
TABLE D-15. EFFECT OF WATER TYPE ON BENZO(G,H,I)PERYLENE ANALYSIS
~~ POINT ESTIMATES »~
DISTILLED WATER SLOPE:GAMMA SLOPE(WATFR-DISTILI ED)
2
. 0904
1558
3
3177
0313
4
2502
1 104
5
.5014
0319
6
3848
0728
SOURCE
»* ANALYSIS OF VARIANCE *
OF SUM OF SQUARES MEAN SQUARE
UJ
REGIDISTILLED) I 87} 64349 972 84349
REGIWATER/DISTILLEDt 10 18 76459 I 87046
ERROR 423 100 26381 .73703
7 92
PROB
0000
TOTAL
434
991.67189
~~ TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS ANO THE DIFFERENCES BETWEEN SLOPES <
WATER
INTERCEPTIWATER-DISTILLED)
ESTIMATE INTERVAL
SLOPE!WATER-DISTILLED)
ESTIMATE INTERVAL
. 0904
3177
. 2502
5014
.3848
- 3174
-.0545
- 1510
1008
- . 0083
498 I )
6898 >
.6513)
9020)
. 7778)
1558
. 03 13
. I 104
03 19
. 0728
0002
1097
04 I 1
I 199
0749
3 115)
I 724 }
2818)
1838)
2205 )
NOTE:
IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AND THE CORRESPONDING WASTE WATER FOR THE ASSOCIATED PARAME»FR<1NTERCEPT/SI OPE) .
THE SLOPE ANO INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER
-------
APPENDIX D (Continued)
TABLE D-16. EFFECT OF WATER TYPE ON INDENO(l,2,3-CD)PYRENE ANALYSIS
~~ POINT ESTIMATES ~~
DISTILLED MATER SLOPE:GAMMA(I) - 95662
WATER INTERCEPT(MATER-DISTILLED* SLOPE(MATER-DISTILLEDI
2 .0842 .0849
3 .(842 0227
4 .2239 0108
5 .3636 .0727
6 .2579 0858
CO
~~ TABLE OF 95% CONFIDENCE INTERVAIS FOR THE DIFFERENCES RETMEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
INTERCEPT I WATER-DISTILL ED) SLOPE(MATER-01 ST ILLEOI
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2
0842 <
- 2268 .
.3952)
0849 <
- 0762 .
.2461 I
3
. 1842 I
- I 198 .
4880)
0227 (
- 1792 .
1337)
4
2239 (
-.0802 .
5280)
0 108 (
- 1449 .
1666)
5
3636 (
0487 .
6784 )
0727 (
- 0892 .
2346)
e
2579 1
- 0597 .
5755)
.0858 (
-.0759 .
2475)
~ ANALYSIS OF VARIANCE ~
SOURCE
OF
SUM OF SQUARES MEAN SQUARE
PROB
REC(DISTILLEO) I 668 27649 668 27649
REG(WATER/DISTILLEO) 10 10 89425 I 08943
ERROR 407 74.20686 18233
5.98
0000
TOTAL
416
753 37760
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AND THE CORRESPONDING WASTE WATER FOR THE ASSOCIATED PARAMITER(INTERCEPT/SLOPE)
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER
-------
------- |