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TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1. REPORT NO.
EPA/600/4-85/070
2.
3. RECIPIENT'S ACCESSION NO.
1217 0 k
4. TITLE AND SUBTITLE
EPA Method Study 31: Trace Metals by Atomic
Absorption (Furnace Techniques)
5. REPORT DATE
October 1985
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
T. R. Copeland and J. P. Maney
8. PERFORMING ORGANIZATION REPORT MO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
ERCO/A Division of ENSECO
205 Alewife Brook Parkway
Cambridge, MA 02138
10. PROGRAM ELEMENT NO.
CBS D/A, BEBIC
11. CONTRACT/GRANT NO.
68-03-3092
12. SPONSORING AGENCY NAME AND ADDRESS
Quality Assurance Branch
Environmental Monitoring & Support Branch
U.S. Environmental Protection Agency
Cincinnati, Ohio 45268
13. TYPE OF REPORT AND PERIOD COVERED
Final 12/81-4/84
14. SPONSORING AGENCY CODE
EPA-ORD
15. SUPPLEMENTARY NOTES
16. ABSTRACT
An interlaboratory study in which 10 laboratories participated was conducted
to provide precision and accuracy statements for the analysis of 18 metals by
graphite furnace atomic absorption spectrometry. Samples were prepared and
analyzed using procedures specified in "Methods for Chemical Analysis of Water
and Wastes," EPA 600-4/79-020, U.S. Environmental Protection Agency, Environ-
mental Monitoring and Support Laboratory, Cincinnati, Ohio, March 1979.
The study design was based on Youden's non-replicate design for collaborative
tests of analytical methods. Three Youden pair samples of the test metals were
spiked into.six types of test waters and then analyzed. The test waters were
three industrial effluents supplied by ERGO and three waters supplied by the
subcontractor laboratories (laboratory pure water, finished drinking water, and
surface water). The resulting data were statistically analyzed using the
computer program entitled "Interlaboratory Method Validation Study" (IMVS).
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS c. COSATI Field/Group
18. DISTRIBUTION STATEMENT
Release to Public
19. SECURITY CLASS (This Report/
Unclassified
21. NO. OF PAGES
375"
20. SECURITY CLASS (This page)
Unclassified
22. PRICE
EPA F«rm 2220-1 (R«». 4-77) PREVIOUS EDITION is OBSOLETE
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DISCLAIMER
The information in this document has been funded wholly or in
part by the United States Environmental Protection Agency under
EPA Contract No. 68-03-3092 to Energy Resources Co. Inc. (ERGO).
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 names of commercially available products
does not constitute endorsement or recommendation for use.
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FOREWORD
Environmental measurements are required to determine the
quality of ambient waters and the character of waste effluents.
The Environmental Monitoring and Support Laboratory-Cincinnati
conducts research to:
Develop and evaluate methods 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 microbio-
logical organisms in water; and to determine the
responses of aquatic organisms to water quality.
Develop and operate an Agency-wide quality assurance
program to assure standardization and quality control of
systems for monitoring water and wastewater.
Develop and operate a computerized system for instrument
automation leading to improved data collection, analysis,
and quality control.
This publication reports the results of U.S. EPA's interlabo-
ratory Method Study 31, conducted to determine the accuracy and
precision of graphite furnace atomic absorption methods for the
analysis of 18 trace metals.
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Federal agencies, states, municipalities, universities,
private laboratories and industry should find this study of
assistance in monitoring trace metal pollution in the environment,
Robert L. booth
Director, EMSL-Cincinnat i
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ABSTRACT
An interlaboratory study in which 10 laboratories partici-
pated was conducted to provide precision and accuracy statements
for the analysis of 18 metals by graphite furnace atomic absorp-
tion spectrometry. Samples were prepared and analyzed usina
procedures specified in "Methods for Chemical Analysis of Water and
Wastes," EPA 600-4/79-020, U.S. Environmental Protection Agency,
Environmental Monitoring and Support Laboratory, Cincinnati, Ohio,
March 1979.
The study design was based on Youden's non-replicate design
for collaborative tests of analytical methods. Three Youden pair
samples of the test metals were spiked into six types of test
waters and then analyzed. The test waters were three industrial
effluents supplied by ERCO and three waters supplied by the
subcontractor laboratories (laboratory pure water, finished
drinking water, and surface water). The resulting data were
statistically analyzed using the computer program entitled
"Interlaboratory Method Validation Study" (IMVS).
This report was submitted in fulfillment of Contract No.
68-03-3092 by ERCO, Inc., Environmental Sciences Division. This
report covers a period from December 1981 to April 1984 and work
was completed as of April 1984.
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ACKNOWLEDGMENT
The authors appreciate the cooperation of all ERCO staff
members who participated in this study. The authors acknowledge
the sincere efforts of the participating laboratories to provide
viable data for this study.
Gratitude is also expressed to the industries for their
interest in the study and for their willingness to provide the
wastewater effluents. Lastly, we thank Mr. Edward L. berg and
Robert Graves, EPA Project Officers, and Theodore Martin of EMSL
(Cincinnati) whose guidance and intense interest in the study
contributed to the successful completion of a difficult task.
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CONTENTS
Section Page
Disclaimer ii
Foreword iii
Abstract v
Acknowledgment vi
Tables ix
1. Introduction 1
2. Conclusions and Recommendations ... 3
3. Description of Study 23
Preliminary Screening of Potential
Participating Laboratories 23
Performance Evaluation Study for
Participating Laboratories 24
Equipment and Methods Used in the Study ... 28
Effluents and Concentration Levels
Utilized in the Interlaboratory
Method Study 28
Method for Verification of True Values,
Homogeneity, and Stability of Sample
Containers 40
Analysis of Dosed Effluent and Water
Samples by Subcontractor Laboratories .... 40
Quality Assurance Requirements for
Participating Laboratories 48
Computer Processing of Laboratory Data ... 50
4. Treatment of Data 51
Rejection of Outliers 52
Youden's Laboratory Ranking Procedure . . 52
Individual Outliers 54
Statistical Summaries 54
Statement of Method Accuracy 57
Statement of Method Precision 59
Comparison of Accuracy and Precision
Across Water Types '. . 61
5. Results and Discussion 68
Rejection of Outliers 72
Statistical Summaries 79
Regression Equations 87
Effects of Water Types 87
References 96
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CONTENTS (Continued)
Section Page
Appendices
A. Sample Instructions Supplied to Laboratories . . . A-l
B. Trace Metals Laboratory Quality Assurance Plan . . B-l
C. Results of Interlaboratory Method Validation
Study C-l
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TABLES
Number Page
1 Regression equations 4
2 List of participating laboratories 25
3 Final results of performance evaluation study 26
4 Instrumentation used 29
5 Summary of homogeneity testing 32
6 Preliminary characterization of effluent samples
by ICAP 34
7 Concentrations in the spiked samples 36
8 Results of stability testing of spike ampules 41
9 Type and number of analyses 49
10 Effluent background concentrations determined by
the ten laboratories 69
11 Number of retained data points for lab pure water ... 73
12 Number of retained data points for drinking water ... 74
13 Number of retained data points for surface water ... 75
14 Number of retained data points for Effluent 1 76
15 Number of retained data points for Effluent 2 77
16 Number of retained data points for Effluent 3 78
17 Percentage of data rejected for each laboratory .... 80
18 Accuracy and precision summary table for lab
pure water 81
19 Accuracy and precision summary table for drinking
water 82
20 Accuracy and precision summary table for surface
water 83
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TABLES (Continued)
Number Page
21 Accuracy and precision summary table for Effluent 1 . . 84
22 Accuracy and precision summary table for Effluent 2 . . 85
23 Accuracy and precision summary table for Effluent 3 . . 86
24 Effect of water type 88
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SECTION 1
INTRODUCTION
The Safe Drinking Water Act (SDWA) and the National Pollu-
tant Discharge Elimination System (NPDES) require that waters and
waste be analyzed to determine their chemical content. The EPA
was given a mandate to prepare methods which would be approved
for the analysis of parameters of concern listed by these laws
and resulting regulations.
The EPA staff of the Environmental Monitoring and Support
Laboratory of Cincinnati, Ohio, provided the procedures for moni-
toring metal parameters in wastes and waters in the document
entitled , "Methods for Chemical Analysis of Water and Wastes" (1).
The second edition of this manual, which was published in March
1979, added atomic absorption furnace methods to guantitate lower
levels of metal parameters than those determinable by the flame
atomic absorption methods specified in the first edition.
Energy Resources Co. Inc. (ERCO) was contracted by EPA to
conduct a method study to define the accuracy and precision of
the atomic absorption furnace procedure for the following 18
trace metals:
Aluminum (Method 202.2) Iron (Method 236.2)
Antimony (Method 204.2) Lead (Method 239.2)
Arsenic (Method 206.2) Manganese (Method 243.2)
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Barium (Method 208.2) Nickel (Method 249.2)
Beryllium (Method 210.2) Selenium (Method 270.2)
Cadmium (Method 213.2) Silver (Method 272.2)
Chromium (Method 218.2) Thallium (Method 279.2)
Cobalt (Method 219.2) Vanadium (Method 286.2)
Copper (method 220.2) Zinc (Method 289.2)
Ten laboratories were selected by ERCO for participating
in the method study following their successful analysis of per-
formance evaluation samples. These laboratories then collected
drinking, surface, and laboratory pure waters while ERCO supplied
them with three different types of industrial effluents. These
waters and effluents were analyzed to determine background levels
of the elements of interest and subsequently specified volumes of
unknown metal concentrates were added and the samples reanalyzed.
The added level of each metal was determined by difference.
Youden's non-replicate (2) collaborative test design was
applied to 10 participating laboratories. 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 U.S. EPA's IMVS computer program (3).
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SECTION 2
CONCLUSIONS AND RECOMMENDATIONS
The primary objective of the study was to define the preci-
sion and accuracy of furnace atomic absorption procedures for the
analysis of 18 metals. The IMVS program regresses overall preci-
sion and single analyst precision against the mean recovery of a
particular element in a given water type and regresses accuracy
against the true concentration. The linear regression equations
best approximating these relationships are presented in Table 1.
These equations may be used to predict the precision and accuracy
of the methods at any concentration in the ranges investigated
in this study. Since the background levels of the metals ana-
lyzed varied among the six waters investigated, the applicable
ranges over which the equations are valid also vary. The exact
ranges over which the equations are valid are also presented in
Table 1.
Other conclusions which may be drawn from this study are as
follow:
Statistically significant effects across some water types
were found for As, Be, Cu, Fe, Mn, Ni, Se, Ag, Tl and Zn;
however the effect was not considered of practical impor-
tance for Cu, Fe, Mn, and Zn.
Ag, Be, Cd and Mn analyses near the recommended method
detection limits (1) were highly erratic and several
laboratories could not achieve the detection limits.
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TABLE 1.
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
HATER TYPE
_ __,-
APPLICABLE CONC. RANGE
ALUMINUM
» -.
(28.00 - 125.00) UQ/L
WATER TYPE
..____..___..___«______
APPLICABLE CONC. RANGE
ALUMINUM
__.. ___« .. __
(26.80 - 120.00)
LAB PURE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
DRINKING WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SURFACE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR - 0.23X + 6.45
S - 0.42X + 5.83
X = 0.70C +32.36
SR - 0.12X +21.97
S = 0.25X +14.45
X 1.10C +39.21
SR = 0.33X + 5.29
S = 0.80X - 0.27
X 0.34C+33.60
LAB PURE WATER
SINGLE-ANALYST PRECISION SR » 0.23X + 6.21
OVERALL PRECISION S - 0.42X * 5.80
ACCURACY X - 0.70C +31.13
EFFLUENT 3
SINGLE-ANALYST PRECISION SR » 0.24X + 3.18
OVERALL PRECISION S - 0.14X +26.59
ACCURACY X = 1.03C +32.88
WATER TYPE
APPLICABLE CONC. RANGE
LAB PURE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 1
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
ALUMINUM
(11.00 - 58
SR » 0.36X
S = 0.39X -
X = 0.85C +
SR = 0.16X
S « 0.26X +
X * 1.12C -
.30) mg/L
- 2.87
2.27
1.87
+ 0.88
2.24
2.89
WATER TYPE
APPLICABLE CONC. RANGE
LAB PURE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 2
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
ALUMINUM
(0.46 - 2.18) mg/L
SR = 0.39X - 0.14
S - 0.39X - 0.09
X = 0.85C + 0.08
SR =-0. 04X +0.16
S - 0.07X + 0.18
X = 0.85C + 0.12
X = MEAN RECOVERY
C = TRUE VALUE FOR THE CONCENTRATION
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TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
MATER TYPE ANTIMONY WATER TYPE ANTIMONY
APPLICABLrCONc""RANGE (10^50~-l30^0oTu9/L~ APPLICABLE CONC. RANGE (11.00 - 240.00) UQ/L
LAB PURE WATER LAB PURE WATER
SINGLE-ANALYST PRECISION SR 0.14X * 1.09 SINGLE-ANALYST PRECISION SR - 0.23X + 0.02
OVERALL PRECISION S - 0.40X + 0.88 OVERALL PRECISION S - 0.34X + 0.86
ACCURACY X - 0.65C + 0.56 ACCURACY X - 0.80C - 2.66
EFFLUENT 1 DRINKING WATER
SINGLE-ANALYST PRECISION SR 0.24X - 0.50 SINGLE-ANALYST PRECISION SR - 0.21X - 0.14
OVERALL PRECISION S 0.17X * 3.89 OVERALL PRECISION S - 0.18X + 0.73
ACCURACY X - 0.88C - 1.28 ACCURACY X - 0.87C - 2.14
EFFLUENT 2 SURFACE WATER
SINGLE-ANALYST PRECISION SR - 0.12X + 4.23 SINGLE-ANALYST PRECISION SR 0.16X * 0.14
OVERALL PRECISION S - 0.09X + 9.56 OVERALL PRECISION S 0.20X + 0.87
ACCURACY X - 0.73C + 5.80 ACCURACY X - 0.81C - 0.97
EFFLUENT 3
SINGLE-ANALYST PRECISION SR - 0.22X + 0.37
OVERALL PRECISION S - 0.33X + 0.87
ACCURACY X 0.61C +0.31
X - MEAN RECOVERY
C - TRUE VALUE FOR THE CONCENTRATION
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TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
I
cr.
I
HATER TYPE ARSENIC MATER TYPE ARSENIC
APPLICABLE CONC. RANGE (9.7B - 227.00) Ug/L APPLICABLE CONC. RANGE (10.20 - 237.00) UQ/L
LAB PURE WATER LAB PURE WATER
SINGLE-ANALYST PRECISION SR 0.08X + 2.82 SINGLE-ANALYST PRECISION SR - 0.10X + 0.70
OVERALL PRECISION S 0.17X + 1.98 OVERALL PRECISION S - 0.1IX + 1.98
ACCURACY X 1.02C + 3.30 ACCURACY X - 0.92C + 0.69
EFFLUENT 1 DRINKING WATER
SINGLE-ANALYST PRECISION SR 0.07X + 5.85 SINGLE-ANALYST PRECISION SR - 0.06X + 1.96
OVERALL PRECISION S 0.15X + 4.01 OVERALL PRECISION S » 0.12X + 1.49
ACCURACY X - 1.15C + 8.87 ACCURACY X - 0.93C * 0.62
EFFLUENT 2 SURFACE WATER
SINGLE-ANALYST PRECISION SR 0.16X « 0.91 SINGLE-ANALYST PRECISION SR 0.09X + 0.80
OVERALL PRECISION S 0.14X + 3.70 OVERALL PRECISION S - 0.13X + 2.75
ACCURACY X 0.94C - 0.68 ACCURACY X 0.91C - 1.29
EFFLUENT 3
SINGLE-ANALYST PRECISION SR 0.07X + 0.53
OVERALL PRECISION S - 0.15X * 2.56
ACCURACY X - 0.87C - 0.30
X MEAN RECOVERY
C - TRUE VALUE FOR THE CONCENTRATION
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TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
WATER TYPE BARIUM WATER TYPE BARIUM
APPLICABLE CONC. RANGE (56.50 - 418.00) Ug/L APPLICABLE CONC. RANGE (59.10 - 437.00) UQ/L
LAB PURE WATER LAB PURE WATER
SINGLE-ANALYST PRECISION SR - 0.12X + 4.80 SINGLE-ANALYST PRECISION SR - 0.15X - 1.72
OVERALL PRECISION S - 0.36X - 8.62 OVERALL PRECISION S 0.14X +15.63
ACCURACY X - 0.84C +83.71 ACCURACY X - 0.84C +30.67
EFFLUENT 1 DRINKING WATER
SINGLE-ANALYST PRECISION SR - 0.19X +10.20 . SINGLE-ANALYST PRECISION SR - 0.11X + 2.22
OVERALL PRECISION S 0.27X +32.68 OVERALL PRECISION S 0.37X -10.56
ACCURACY X - 0.97C +67.43 ACCURACY X 0.92C +36.50
I _ ^ _
71 EFFLUENT 2 SURFACE WATER
SINGLE-ANALYST PRECISION SR - 0.29X -13.14 SINGLE-ANALYST PRECISION SR - 0.20X - 0.16
OVERALL PRECISION S - 0.58X -27.91 OVERALL PRECISION S - 0.28X + 1.56
ACCURACY X - 0.84C +42.52 ACCURACY X - 0.93C +30.17
EFFLUENT 3
SINGLE-ANALYST PRECISION SR - 0.69X -39.17
OVERALL PRECISION S 0.34X + 9.88
ACCURACY X 0.24C +65.63
X - MEAN RECOVERY
C - TRUE VALUE FOR THE CONCENTRATION
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TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
I
CO
I
WATER TYPE BERYLLIUM WATER TYPE BERYLLIUM
APPLICABLE CONC. RANGE (0.45 - 10.90) Ug/L APPLICABLE CONC. RANGE (0.47 - 11.40) Ug/L
LAB PURE WATER LAB PURE WATER
SINGLE-ANALYST PRECISION SR - 0.12X * 0.05 SINGLE-ANALYST PRECISION SR - 0.10X + 0.08
OVERALL PRECISION S « 0.29X + O.OS OVERALL PRECISION S 0.11X + 0.18
ACCURACY X 1.15C - 0.25 ACCURACY X - 0.98C - 0.05
EFFLUENT 1 DRINKING WATER
SINGLE-ANALYST PRECISION SR 0.07X + 0.10 SINGLE-ANALYST PRECISION SR - 0.03X + 0.11
OVERALL PRECISION S - 0.19X + 0.20 OVERALL PRECISION S - 0.14X * 0.07
ACCURACY X 0.92C + 0.11 ACCURACY X - 1.01C - 0.07
EFFLUENT 2 SURFACE WATER
SINGLE-ANALYST PRECISION SR - 0.12X - 0.05 SINGLE-ANALYST PRECISION SR - 0.10X + 0.02
OVERALL PRECISION S 0.07X + 0.19 OVERALL PRECISION S 0.29X - 0.08
ACCURACY X - 1.08C + 0.01 ACCURACY X 0.90C +0.10
EFFLUENT 3
SINGLE-ANALYST PRECISION SR - 0.13X - 0.00
OVERALL PRECISION S 0.20X + 0.08
ACCURACY X 0.92C - 0.03
X - MEAN RECOVERY
C - TRUE VALUE FOR THE CONCENTRATION
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TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
WATER TYPE
CADMIUM
(0.43 - 12.00)
SR « 0.09X * 0.25
S = 0.17X + 0.20
X - 1.02C + 0.24
WATER TYPE
CADMIUM
(0.45 - 12.50)
SR * 0.10X + 0.05
S « 0.27X - 0.05
X * 0.95C + 0.09
I
vo
I
APPLICABLE CONC. RANGE
LAB PURE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 1
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 2
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 3
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR » 0.14X + 0.42
S * 0.32X * 0.15
X » 0.75C + 0.39
SR = 0.12X + 0.09
S = 0.23X t 0.07
X = 0.81C + 0.15
SR « 0.15X + 0.04
S = 0.27X + 0.14
X = 0.96C * 0.10
APPLICABLE CONC. RANGE.
LAB PURE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
DRINKING WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SURFACE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR = 0.17X + 0.11
S * 0.26X + 0.10
X = 0.92C « 0.24
SR 0.22X - 0. 13
S - 0.3BX + 0.10
X « 1.04C + 0.15
X = MEAN RECOVERY
C > TRUE VALUE FOR THE CONCENTRATION
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TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
o
I
WATER TYPE CHROMIUM WATER TYPE CHROMIUM
APPLICABLE CONC. RANGE (9.87 - 236*00) Ug/L APPLICABLE CONC. RANGE (10.30 - 246.00) ug/L
LAB PURE WATER LAB PURE WATER
SINGLE-ANALYST PRECISION SR = 0.18X + 0.73 SINGLE-ANALYST PRECISION SR » 0.12X - 0.41
OVERALL PRECISION S » 0.20X +1.14 OVERALL PRECISION S = 0.14X + 0.35
ACCURACY X ' 0.89C + 0.11 ACCURACY X = 0.94C + 0.40
EFFLUENT 1 DRINKING WATER
SINGLE-ANALYST PRECISION SR = 0.14X + 0.88 SINGLE-ANALYST PRECISION SR = 0.06X + 2.73
OVERALL PRECISION S - 0.21X + 3.87 OVERALL PRECISION S 0.12X + 4.14
ACCURACY X « 0.87C + 1.09 ACCURACY X = l.OOC + 0.89
EFFLUENT 2 SURFACE WATER
SINGLE-ANALYST PRECISION SR = 0.17X - 0.32 SINGLE-ANALYST PRECISION SR 0.12X - 0.12
OVERALL PRECISION S * 0.14X + 2.55 OVERALL PRECISION S = 0.26X - 0.04
ACCURACY X = 0.95C + 1.03 ACCURACY X = 0.91C + 0.47
EFFLUENT 3
SINGLE-ANALYST PRECISION SR = 0.08X + 0.28
OVERALL PRECISION S = 0.22X + 0.41
ACCURACY X » 0.92C - 0.68
X « MEAN RECOVERY
C * TRUE VALUE FOR THE CONCENTRATION
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TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
WATER TYPE COBALT HATER TYPE COBALT
APPLICABLE CONC. RANGE (29.70 - 420.00) Ug/L APPLICABLE CONC. RANGE (24.80 - 407.00) UQ/L
LAB PURE WATER LAB PURE WATER
SINGLE-ANALYST PRECISION SR - 0.09X + O.SO SINGLE-ANALYST PRECISION SR = 0.11X + 0.02
OVERALL PRECISION S * 0.25X - 2.99 OVERALL PRECISION S = 0.25X - 2.69
ACCURACY X « 0.8BC + 1.36 ACCURACY X - 0.89C * 1.11
DRINKING WATER EFFLUENT 1
SINGLE-ANALYST PRECISION SR = 0.12X * 1.60 SINGLE-ANALYST PRECISION SR = 0.16X + 0.58
OVERALL PRECISION S 0.23X + 1.24 OVERALL PRECISION S = 0.20X - 0.89
ACCURACY X 0.92C + 0.44 ACCURACY X - 0.88C » 4.50
SURFACE WATER
SINGLE-ANALYST PRECISION SR * 0.14X - 1.00
OVERALL PRECISION S - 0.18X - 0.14
ACCURACY X « 0.92C * 2.01
WATER TYPE COBALT WATER TYPE COBALT
APPLICABLE CONC. RANGE (21.10 - 461.00) UQ/L APPLICABLE CONC. RANGE (29.30 - 435.00) UQ/L
LAB PURE WATER LAB PURE WATER
SINGLE-ANALYST PRECISION SR - 0.09X * 0.03 SINGLE-ANALYST PRECISION SR * 0.09X + 0.16
OVERALL PRECISION S 0.2SX - 1.99 OVERALL PRECISION S - 0.25X - 3.31
ACCURACY X - 0.89C + 0.29 ACCURACY X - 0.88C * 1.32
EFFLUENT 2 EFFLUENT 3
SINGLE-ANALYST PRECISION SR 0.09X + 3.21 SINGLE-ANALYST PRECISION SR 0.06X + 2.06
OVERALL PRECISION S - 0.13X + 1.76 OVERALL PRECISION S - 0.15X * 1.28
ACCURACY X 0.95C + 0.43 ACCURACY X - 0.82C * 1.43
X - MEAN RECOVERY
C - TRUE VALUE FOR THE CONCENTRATION
-------
TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
NJ
I
MATER TYPE COPPER MATER TYPE COPPER
APPLICABLE CONC. RANGE (10.10 - 234.00) UQ/L APPLICABLE CONC. RANGE (0.30 - 1.67) Hig/L
LAB PURE MATER LAB PURE MATER
SINGLE-ANALYST PRECISION SR < 0.07X * 4.37 SINGLE-ANALYST PRECISION SR <- 0.13X - 0.02
OVERALL PRECISION S * 0.11X + 4.97 OVERALL PRECISION S = 0.13X - 0.00
ACCURACY X 0.92C - 0.81 ACCURACY X * 0.93C « 0.01
EFFLUENT 1 EFFLUENT 2
SINGLE-ANALYST PRECISION SR » 0.22X - 0.44 SINGLE-ANALYST PRECISION SR = 0.05X + 0.02
OVERALL PRECISION S 0.21X + 1.21 OVERALL PRECISION S - 0.13X * 0.01
ACCURACY X 0.96C - 0.10 ACCURACY X - 1.02C - 0.07
EFFLUENT 3
SINGLE-ANALYST PRECISION SR * 0.13X + 1.95
OVERALL PRECISION S 0.29X + 4.96
ACCURACY X O.B1C + 0.42
HATER TYPE COPPER
APPLICABLE CONC. RANGE (10.60 - 245.00) Ug/L
LAB PURE MATER
SINGLE-ANALYST PRECISION SR » 0.22X - 0.46
OVERALL PRECISION S - 0.21X + 1.29
ACCURACY X 0.96C - 0.11
DRINKING MATER
SINGLE-ANALYST PRECISION SR 0.15X + 2.63
OVERALL PRECISION S 0.34X + 3.39
ACCURACY X * 0.91C + 6.09
SURFACE MATER
SINGLE-ANALYST PRECISION SR - 0.06X > 1.81
OVERALL PRECISION S ° 0.18X + 1.44
ACCURACY X l.OOC - 0.26
X MEAN RECOVERY
C TRUE VALUE FOR THE CONCENTRATION
-------
TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
WATER TYPE
IRON
(26.10 - 455.00) Ug/L
WATER TYPE IRON
APPLICABLE CONC. RANGE (25.00 - 435.00) UQ/L
LAB PURE WATER
SINGLE-ANALYST PRECISION SR = 0.30X +25.23
OVERALL PRECISION S = 0.35X +12.73
ACCURACY X = 1.41C +11.24
ui
I
APPLICABLE CONC. RANGE
LAB PURE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
DRINKING WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SURFACE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR ° 0.30X +26.13
S = 0.35X +13.23
X - 1.40C +11.73
SR = 0.30X + 1.06
S - 0.36X + 9.15
X > 1.20C +10.35
SR = 0.35X - 3.95
S = 0.34X +37.42
X » 1.10C +96.38
EFFLUENT 3
SINGLE-ANALYST PRECISION SR - 0.23X +16.21
OVERALL PRECISION S " 0.31X +31.14
ACCURACY X 1.09C +37.18
WATER TYPE
IRON
(1.03 - 5.59) mg/L
SR = 0.04X + 0.13
S - 0.05X + 0.27
X « 1.01C + 0.07
SR - 0.28X + 0.04
S » 0.41X - 0.13
X = 1.16C - 0.25
WATER TYPE
APPLICABLE CONC. RANGE
IRON
(0.37 - 2.61)mg/L
APPLICABLE CONC. RANGE
LAB PURE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 1
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
LAB PURE WATER
SINGLE-ANALYST PRECISION SR = 0.06X + 0.03
OVERALL PRECISION S «= 0.07X + 0.08
ACCURACY X = 1.42C - 0.17
EFFLUENT 2
SINGLE-ANALYST PRECISION SR = 0.18X - 0.03
OVERALL PRECISION S » 0.22X - 0.01
ACCURACY X « l.OOC + 0.04
X = MEAN RECOVERY
C TRUE VALUE FOR THE CONCENTRATION
-------
TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
WATER TYPE LEAD WATER TYPE LEAD
APPLICABLE CONC. RANGE (10.40 - 243.00) Ug/L APPLICABLE CONC. RANGE (10.90 - 254.00)
LAB PURE WATER LAB PURE WATER
SINGLE-ANALYST PRECISION SR = 0.17X - 0.88 SINGLE-ANALYST PRECISION SR - 0.20X + 0.42
OVERALL PRECISION S = 0.17X + 1.36 OVERALL PRECISION S - 0.28X - 0.66
ACCURACY X = 1.06C - 2.26 ACCURACY X « 0.83C + 1.35
EFFLUENT 1 DRINKING WATER
SINGLE-ANALYST PRECISION SR » 0.22X - 0.14 SINGLE-ANALYST PRECISION SR = 0.07X * 1.39
OVERALL PRECISION S 0.23X - 0.06 OVERALL PRECISION S « 0.21X + 2.56
ACCURACY X « 0.81C + 2.05 ACCURACY X « 0.85C + 0.50
EFFLUENT 2 SURFACE WATER
SINGLE-ANALYST PRECISION SR » 0.14X + 1.00 SINGLE-ANALYST PRECISION SR = 0.19X + 0.11
OVERALL PRECISION S = 0.22X + 1.40 OVERALL PRECISION S = 0.18X + 1.73
ACCURACY X = 0.86C - 2.12 ACCURACY X « 0.92C - 0.96
EFFLUENT 3
SINGLE-ANALYST PRECISION SR = 0.22X + 1.48
OVERALL PRECISION S = 0.34X + 1.86
ACCURACY X 0.70C + 1.63
X = MEAN RECOVERY
C > TRUE VALUE FOR THE CONCENTRATION
-------
TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
HATER TYPE
MANGANESE
(0.44 - 14.80) ug/L
SR = 0.27X + 0.31
S 0.44X + 0.48
X - l.OOC + 1.46
SR = 0.16X + O.S1
S - 0.38X + 0.52
X - 0.90C + 1.38
WATER TYPE MANGANESE
APPLICABLE CONC. RANGE (91.00 - 484.00) UQ/L
LAB PURE HATER
SINGLE-ANALYST PRECISION SR = 0.03X +11.34
OVERALL PRECISION S - 0.05X +11.20
ACCURACY X = O.S5C X12.98
ui
I
APPLICABLE CONC. RANGE
LAB PURE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
DRINKING WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SURFACE HATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 1
SINGLE-ANALYST PRECISION SR = 0.04X +40.27
OVERALL PRECISION S - 0.11X +32.01
ACCURACY X = 0.97C - 6.66
HATER TYPE
MANGANESE
(111.00 - 666.00)
HATER TYPE MANGANESE
APPLICABLE CONC. RANGE (0.42 - 14.20) UQ/L
LAB PURE WATER
SINGLE-ANALYST PRECISION SR ' 0.27X + 0.31
OVERALL PRECISION S - 0.43X + 0.47
ACCURACY X » l.OOC +1.40
APPLICABLE CONC. RANGE
LAB PURE HATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 2
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR « 0.05X + 8.13
S 0.07X + 9.19
X » 0.93C + 9.38
SR = 0.26X + 3.47
S = 0.32X - 6.30
X 0.78C - 8.22
EFFLUENT 3
SINGLE-ANALYST PRECISION SR * 0.23X + 0.52
OVERALL PRECISION S = 0.48X - 0.2B
ACCURACY X * 0.46C + 2.56
X - MEAN RECOVERY
C » TRUE VALUE FOR THE CONCENTRATION
-------
TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
WATER TYPE NICKEL WATER TYPE NICKEL
APPLICABLE CONC. RANGE (26.20 - 461.00) Lig/L APPLICABLE CONC. RANGE (27.40 - 482.00) UQ/L
LAB PURE HATER LAB PURE WATER
SINGLE-ANALYST PRECISION SR « 0.17X + 0.34 SINGLE-ANALYST PRECISION SR - 0.21X - 2.45
OVERALL PRECISION S - 0.26X + 1.89 OVERALL PRECISION S * 0.23X + 1.98
ACCURACY X = 0.84C + 6.46 ACCURACY X - 0.93C - 2.02
EFFLUENT 1 DRINKING WATER
SINGLE-ANALYST PRECISION SR = 0.10X + 3.46 SINGLE-ANALYST PRECISION SR * 0.12X * 4.43
OVERALL PRECISION S - 0.16X + 4.72 OVERALL PRECISION S = 0.27X + 2.20
ACCURACY X » 0.67C +10.56 ACCURACY X = 0.81C + 0.75
I __
|± EFFLUENT 2 SURFACE HATER
I SINGLE-ANALYST PRECISION SR = 0.13X + 2.39 SINGLE-ANALYST PRECISION SR = 0.10X * 4.38
OVERALL PRECISION S - 0.24X + 5.60 OVERALL PRECISION S = 0.16X + 9.37
ACCURACY X = 0.85C - 4.74 ACCURACY X = 0.81C + 2.47
EFFLUENT 3
SINGLE-ANALYST PRECISION SR » 0.04X * 1.88
OVERALL PRECISION S = 0.18X + 9.11
ACCURACY X = 0.84C - 9.99
X < MEAN RECOVERY
C - TRUE VALUE FOR THE CONCENTRATION
-------
TABLE 1 (continued)
ENVIRONMENTAL MOM I TOR INC, AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
WATER TYPE SELENIUM WATER TYPE SELENIUM
APPLICABLE CONC. RANGE (10.00 - 235.00) Ug/L APPLICABLE CONC. RANGE (10.50 - 246.00) Lig/L
LAB PURE WATER LAB PURE WATER
SINGLE-ANALYST PRECISION SR = 0.06X + 0.65 SINGLE-ANALYST PRECISION SR = 0.10X + 0.50
OVERALL PRECISION S = 0.17X + 0.14 OVERALL PRECISION S = 0.14X + 2.18
ACCURACY X = 0.93C - 0.20 ACCURACY X « 0.98C + 1.28
EFFLUENT 1 DRINKING WATER
SINGLE-ANALYST PRECISION SR = 0.05X + 3.19 SINGLE-ANALYST PRECISION SR = 0.05X + 2.23
OVERALL PRECISION S = 0.19X + 1.76 OVERALL PRECISION S = 0.16X + 3.16
ACCURACY X = 0.88C - 2.45 ACCURACY X - 1.07C + 0.19
EFFLUENT 2 SURFACE WATER
SINGLE-ANALYST PRECISION SR = 0.11X + 3.14 SINGLE-ANALYST PRECISION SR = 0.15X + 0.25
OVERALL PRECISION S = 0.19X + 2.78 OVERALL PRECISION S = 0.17X + 1.64
ACCURACY X * 1.11C - 2.78 ACCURACY X = l.OOC - 0.66
EFFLUENT 3
SINGLE-ANALYST PRECISION SR = 0.17X + 0.20
OVERALL PRECISION S " 0.40X + 2.55
ACCURACY X = 0.84C - 2.14
X * MEAN RECOVERY
C = TRUE VALUE FOR THE CONCENTRATION
-------
TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
oo
I
WATER TYPE SILVER WATER TYPE SILVER
APPLICABLE CONC. RANGE (8.48 - 56.50) Ug/L APPLICABLE CONC. RANGE (0.45 - 13.60) Ug/L
LAB PURE WATER LAB PURE WATER
SINGLE-ANALYST PRECISION SR - 0.19X - 0.95 SINGLE-ANALYST PRECISION SR - 0.15X + 0.03
OVERALL PRECISION S 0.17X + 0.35 OVERALL PRECISION S 0.18X + 0.15
ACCURACY X 0.79C + 2.78 ACCURACY X - 0.96C + 0.17
EFFLUENT 1 DRINKING WATER
SINGLE-ANALYST PRECISION SR = 0.06X + 0.78 SINGLE-ANALYST PRECISION SR --0.02X + 0.77
OVERALL PRECISION S - 0.28X - 1.05 OVERALL PRECISION S = 0.20X * 0.17
ACCURACY X ' 0.90C + 0.96 ACCURACY X « 0.82C + 0.81
EFFLUENT 2 SURFACE WATER
SINGLE-ANALYST PRECISION SR = 0.28X + 1.11 SINGLE-ANALYST PRECISION SR 0.10X - 0.07
OVERALL PRECISION S ° 0.65X + 0.26 OVERALL PRECISION S - 0.56X + 0.06
ACCURACY X * 0.49C + 0.03 ACCURACY X - 0.87C + 2.46
EFFLUENT 3
SINGLE-ANALYST PRECISION SR = 0.34X - 2.10
OVERALL PRECISION S - 0.38X - 1.06
ACCURACY X » 0.70C + 4.27
X = MEAN RECOVERY
C = TRUE VALUE FOR THE CONCENTRATION
-------
TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
HATER TYPE
THALLIUM
(10.00 - 24i.oo) ug/L
SR = 0.15X * 0.03
S 0.12X + 0.96
X = 0.87C - 1.24
SR = 0.09X + 0.41
S = 0.30X - 0.04
X = 0.76C - 1.12
SR = 0.16X - 0.20
S = 0.14X + 1.58
X = 0.62C - 1.06
SR = 0.06X * 0.00
S = 0.19X + 0.33
X = 0.81C - 1.70
WATER TYPE
THALLIUM
(lo.so - 252.00) ug/L
SR = 0.06X + 0.41
S = O.llX + 0.13
X = 0.88C - 0.10
SR = 0.09X - 0.29
S = 0.26X - 1.14
X = 0.89C - 0.89
SR = 0.10X + 0.02
S » 0.25X - 0.14
X = 0.84C - 1.15
APPLICABLE CONC. RANGE
LAR PURE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 1
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 2
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 3
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
APPLICABLE CONC. RANGE
LAR PURE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
DRINKING WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SURFACE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
X = MEAN RECOVERY
C > TRUE VALUE FOR THE CONCENTRATION
-------
TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EQUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1
MATER TYPE VANADIUM WATER TYPE VANADIUM
APPLICABLE CONC. RANGE (151.00 - 902.00) ug/L APPLICABLE CONC. RANGE (144.00 - 939.00) UQ/L
LAB PURE WATER LAB PURE WATER
SINGLE-ANALYST PRECISION SR = 0.12X + 2.14 SINGLE-ANALYST PRECISION SR - 0.12X + 1.96
OVERALL PRECISION S = 0.53X -44.69 OVERALL PRECISION S « 0.53X -42.61
ACCURACY X = 0.75C +26.06 ACCURACY X = 0.75C +25.26
DRINKING WATER EFFLUENT 1
SINGLE-ANALYST PRECISION SR = 0.04X +21.95 SINGLE-ANALYST PRECISION SR - 0.04X +19.60
OVERALL PRECISION S = 0.1BX +14.92 OVERALL PRECISION S - 0.24X + 4.39
ACCURACY X l.OOC -14.73 ACCURACY X - 1.05C - 7.45
M SURFACE WATER EFFLUENT 2
<=> SINGLE-ANALYST PRECISION SR = 0.15X - 5.47 SINGLE-ANALYST PRECISION SR - 0.13X +14.33
1 OVERALL PRECISION S = 0.15X + 0.56 OVERALL PRECISION S 0.11X +19.77
ACCURACY X = 0.96C -11.91 ACCURACY X - 0.94C -17.68
WATER TYPE VANADIUM
APPLICABLE CONC. RANGE (1.36 - 6.03) IT1'J/L
LAB PURE WATER
SINGLE-ANALYST PRECISION SR = 0.05X + 0.01
OVERALL PRECISION S 0.1IX - 0.01
ACCURACY X » 0.96C + 0.04
EFFLUENT 3
SINGLE-ANALYST PRECISION SR 0.12X - 0.04
OVERALL PRECISION S » 0.21X - 0.13
ACCURACY X ' 0.99C - 0.18
X = MEAN RECOVERY
C « TRUE VALUE FOR THE CONCENTRATION
-------
TABLE 1 (continued)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
REGRESSION EOUATIONS FOR ACCURACY AND PRECISION FOR COMPOUND 1 - 1
WATER TYPE
ZINC
*...^~-~~^bK»^«^^«»K~~>--»*-*-
(0.54 - 17.40) UQ/L
SR = 0.56X - 1.19
S = 1.03X - 1.03
X = 2.93C + 1.02
SR = 0.31X + 6.80
S - 0.99X + 0.69
X = 1.29C +14.50
SR = 0.59X - 5.51
S = 1.06X - 0.04
X = 2.43C +7.16
MATER TYPE ZINC
~~~~~~- ~*->»~ ^'«>~~*I-*»^~B-»*»~^~^'~>*»^<^^~*»*-~^*~>^~'~~b>^*-~
APPLICABLE CONC. RANGE (1.31 - 6.41)fflg/L
APPLICABLE CONC. RANGE
LAR PURE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
DRINKING WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SURFACE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
LAB PURE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 1
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR = 0.24X + 0.04
S = 0.30X * 0.11
X = 1.18C - 0.31
SR
S
X
= 0.35X + 0.19
0.69X + 0.10
0.42C + 0.84
WATER TYPE
APPLICABLE CONC. RANGE
LAB PURE WATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 2
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
ZINC
(24.60 - 189.00) UQ/L
SR » 0.24X + 1.21
S = 0.31X + 1.45
X = 1.1 1C - 2.76
SR = 0.86X -19.95
S = 0.77X - 3.46
X = 1.04C + 9.58
WATER TYPE ZINC
APPUCABLE~CONc"~RANK (0.51 - 16.70) ug/L
LAB PURE MATER
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
EFFLUENT 3
SINGLE-ANALYST PRECISION
OVERALL PRECISION
ACCURACY
SR - 0.56X - 1.04
S l.OOX - 0.63
X 2.93C + 0.86
S « 1.27X -11.00
X 8.83C +54.05
X = MEAN RECOVERY
C * TRUE VALUE FOR THE CONCENTRATION
-------
Znf Al and Fe analyses were erratic with a high percentage
of outliers at all concentrations due to contamination.
This is most obvious in samples with low background con-
centrations (the waters as opposed to the industrial
effluents), but many data were rejected in all samples for
these elements.
On average 23% of the data were rejected. For four of the
six samples, zinc had the highest percentage of data
rejected.
For all six samples, more data were rejected for the low
spiking concentrations than for the high spiking concen-
trations.
For a single element in a single sample, the worst performer
was Mn in surface water where all the data were rejected
for one spiking level, again reflecting that for this
element the .method detection limits (1) cannot be achieved.
Recommendations for future research in this area are as
follow:
Surface and drinking water samples should be supplied
to the participating laboratories to assure uniformity of
the matrix elements.
The laboratories' method detection limits (MDLs) should be
reassessed since some were unable to obtain acceptable
accuracy and precision near the recommended MDL's.
The type of graphite used and parameters such as back-
ground correction, sheath gas, etc., should be specified
so that instrumental effects may be separated from matrix
or method effects.
-22-
-------
SECTION 3
DESCRIPTION OF STUDY
The objective of this study was to define the precision and
accuracy of atomic absorption furnace procedures for analysis
of 18 metals in three raw wastewater effluents aenerated by
regulated industries, as well as in samples of typical surface,
drinking, and laboratory-pure water supplied by ten subcontractor
laboratories. Samples were prepared and analyzed for total
metals according to atomic absorption furnace methods specified
by the U.S. EPA (1). The design of the interlaboratory method
study was based on the specific requirements of the Statement of
Work, Exhibit A contained in RFP CI-81-0270, as well as prece-
dents set by previous EPA-conducted interlaboratory evaluation
studies (3) and the recommendations of Youden (2).
PRELIMINARY SCREENING OF POTENTIAL PARTICIPATING LABORATORIES
An EPA-supplied list of laboratories and previous ERGO
experience were used to solicit interested laboratories. Selection
of laboratories during the initial screening was based on prior
experience of the laboratory in graphite furnace analysis, as-
surance of adeauate facilities, instrumentation, and personnel to
complete the required analysis within 45 days of sample receipt,
and fixed price cost estimates for the required analyses. Based on
-23-
-------
these criteria, ERGO selected the 10 lowest bidders for partici-
pation in the second phase (a performance evaluation study) of the
selection process. Two other laboratories were selected as backup
subcontractors pending the outcome of the performance evaluation
study. The names of the 10 laboratories selected for the perfor-
mance evaluation study were submitted to EPA for approval prior to
notification.
Performance Evaluation Study for Participating Laboratories
The final phase of subcontractor laboratory selection
included a performance evaluation study conducted by ERGO. Each
of the 10 laboratories selected during the initial screening was
required to analyze two ERCO-supplied test samples at their own
expense. Potential subcontractors were given 20 days from sample
receipt to complete the analyses and forward the results to ERGO.
Results of the laboratory analyses of the performance evaluation
samples were compared to the 95% confidence intervals for the
mean values for each element. Analyses falling outside the 95%
confidence interval were judged unacceptable and analysis of an
additional test sample was required. Failure to achieve accept-
able results on the second test sample disqualified the labora-
tory from participation in the study.
One laboratory failed to produce acceptable results on a
second attempt and a substitute was used. Selection and prep-
aration of the performance evaluation samples and analysis of
test results were performed in conjunction with the U.S. EPA
Project Officer. The laboratories finally selected for the study
are listed in Table 2. The order of appearance in the list has no
correlation to the "Laboratory Number" used throughout the report.
The final results for the performance evaluation study are compiled
in Table 3.
-24-
-------
Table 2. LIST OF PARTICIPATING LABORATORIES
Envirodyne Engineers
12161 Lackland Road
St. Louis, Missouri 63141
314-434-6960
Dr. Carol Byington
GCA Corporation
Technology Division
213 Burlington Road
Bedford, Massachusetts 01730
617-275-5444
Dr. Kenneth T. McGregor
PEDCo Environmental Inc.
11499 Chester Road
Cincinnati, Ohio 45246
513-782-4700
Mr. Craig Caldwell
Battelle Columbus Laboratories
505 King Avenue
Columbus, Ohio 43201
614-424-7941
Dr. Marvin Miller
Sverdrup Technology, Inc.
600 William Northern Blvd.
P.O. Box 884
Tullahoma, Tennessee 37388
615-455-6400 ext. 603
Dr. Charlotte Kimbrough
Research Triangle Institute
P.O. Box 12194
Research Triangle Park, North
Carolina 27709
919-541-6883
Dr. William F. Gutknecht
The University of Iowa
University Hygiene Laboratory
Des Moines Branch
H.A. Wallace Building
Des Moines, Iowa 50319
515-281-5371
Mr. Lee A. Friell
Radian Corporation
8501 Mo-Pac Blvd.
P.O.. Box 9948
Austin, Texas 78766
512-454-4797
Mr. Donnie Heinrich
EAL Corporation
2030 Wright Avenue
Richmond, California
415-235-2633
Mr. Larry E. Penfold
94804
Versar Inc.
6621 Electronic Drive
P.O. Box 1549
Springfield, Virginia 22151
703-750-3000
Mr. William Nivens
-25-
-------
Table 3.
FINAL RESULTS OF PERFORMANC1. VALUATION STUDY
Sample 1
1
to
CTl
1
Laboratory
1
2
3
4
5
6
7
8
9
10
11 (ERCO)
Mean and standard deviation
before rejection of outliers
Mean and standard deviation
after rejection of outliers
Theoretical Value
% of theoretical
% relative standard deviation
Acceptance Limits
(mean +; 95% confidence
interval )
As
28
37
37
40
48
22
33
42
30
35
37
35 + 7.1
35 + 7.1
42
83
20
21-79
Cd
3.7
4.1
5.3
4.6
2.4
5.0
3.8
5.1
2.7
4.0
3.5
4.0 + 0.9
4.0 +_ 0.9
3.6
111
23
2.2-5.8
Elemental Concentrations ( uq/L)
Cu Pb Ni Se
47
47
46
44
329
52
54
49
41
50
47
46 +_ 5.9
48 + 3.8
45
107
8
40-56
47
49
52
34b .
40
48
52
49
48
55
57
48 + 6.5
48 + 6.5
51
94
14
35-61
103
97
95
94
97
93
85
102
703
105
98
94 +_ 9.8
97 + 5.8
98
99
6
82-106
51
56
52
59
61
48
56
52
58
60
53
55 + 4.2
55 +_ 4.2
48
115
8
47-63
Tl
23
29
37
31
32
33
21
27
26
30
35
29 + 4.9
29 + 4.9
35
87
17
19-39
V
484
364
456
320
360
330
278
315
136
250
278
325 + 95
325 + 95
320
102
29
135-515
aOutlier
^Outside acceptance limits
-------
Table 3. (Continued)
Sample 1
1
M
1
F.aboratory
1
2
3
4
5
6
7
8
9
10
11 (ERCO)
Mean and standard deviation
before .reject ion of outliers
Mean and standard deviation
after rejection of outliers
Theoretical Value
% of theoretical
% relative standard deviation
Acceptance Limits
(mean + 95% confidence
interval )
As
21
26
25
32
36
18
28
37
26
40
30
29 + 6.8
29 + 6.8
34
85
23
15-43
Cd
3.0
4.5
5.0
6.4
3.8
5.6
4.4
5.6
3.4
4.5
4.0
4.6 + 1.0
4.6 + 1.0
4.4
105
22
2.6-6.6
Elemental Concentrations (uq/L)
Cu Pb Ni Se
52
52
72a
62
65
50
55
55
55
55
53
57 + 6.7
55 i 4.7
51
108
9
44-66
51
48
57
42
803
59
54
55
58
65
63
57 + 9.9
55 + 6.9
56
98
13
41-69
87
84
71
96b
84
84
87
89
60a
90
88
85 + 9.1
87 + 4.2
86
101
5
79-95
43
52
42
54
49
44
51
46
52
50
48
48 + 4.0
48 + 4.0
44
109
8
40-56
Tl
19
24
26
24
21
30
18
22
21
20
27
23 + 3.7
23 + 3.7
28
82
16
16-30
V
445
368
455
360
310
390
325
350
200b
300
324
348 + 71
348 + 71
359
97
20
206-490
aOutlier
^Outside acceptance limits
-------
EQUIPMENT AND METHODS USED IN THE STUDY
The methods utilized in the study were all U.S. EPA (1)
approved graphite furnace methods and are listed by method
number in the Introduction of this report. These methods
allow some latitude as to what type of instrument or type of
graphite is used. The instrumentation and graphite types are
listed by laboratory number in Table 4.
EFFLUENTS AND CONCENTRATION LEVELS UTILIZED IN THE
INTERLABORATORY METHOD STUDY
The initial consideration for design of the study was to
select suitable industrial wastewater effluents for analysis.
ERCO applied a number of criteria for selection of the effluents:
(1) the effluent must be from an industry regulated for trace
metals; (2) the effluents must represent an analytical challenge;
(3) at least one effluent must be high in suspended solids; (4)
concentration levels of the metals of interest must be suitable for
graphite furnace analysis; (5) a previous analytical history should
be available to provide a basis for determining likely spike
levels; and (6) sufficient quantities of effluent must be readily
obtainable. Based on these criteria, ERCO selected effluents from
three primary industries (paper and pulp, photographic, and steam
and electric) as the wastewater matrices for this study.
Previous analyses of effluents from these three industries
indicated that each of these wastewaters presented a unique analyti-
cal challenge that is widely applicable to other effluent samples.
Effluents from the paper and pulp industry are high in dissolved
and suspended solids and contain substantial amounts of potential
interferents (alkali and alkaline earth metals and anions such as
-28-
-------
Table 4. INSTRUMENTATION USED
Laboratory
Number
AAS*
1. IL251/257
2. PE
V
3. PE
PE
4. PE
5. PE
PE
6. PE
7. PE
PE
8. PE
PE
IL
9. PE
V
10. PE
PE
460
A A- 6
305
560
5000
560
2380
603
306
5000
403
503
351
373
1250
2380
703
Furnace
IL555CTF
HGA 2100
CRA 63
HGA 2000
HGA 2200
HGA 500
HGA 2200
HGA 2200
HGA 2100
HGA 2100
HGA 500
HGA 2200
HGA 2100
IL555CTF
HGA 2200
CRA 63
HGA 400
HGA 2100
Graphite
All pyrolytic
Pyrolytic for Ba,
V only
Pyrolytic for Ba,
V only
Pyrolytic for Ba,
V only
All pyrolytic
Pyrolytic for Ba,
V only
Pyrolytic for Ba,
V only
All non-pyrolytic
All non-pyrolytic
All pyrolytic
Pyrolytic for Ba,
V only
Pyrolytic for Ba,
V only
Ni,
Ni,
Ni,
Ni,
Ni,
Ni,
Ni,
*Abbreviations are as follows: IL=Instrumentation
Laboratory; PE=Perkin-Elmer; V=Varian.
-29-
-------
chloride or sulfate). Photographic industry wastewaters contain
variable amounts of suspended solids, and have considerable
amounts of dissolved organic compounds which act as effective
chelators in binding metals into non-labile complexes. These
sample types reauire great care in digestion and analysis.
Process waters from the «team and electric industry contain small
amounts of suspended solids and levels of trace elements near the
limit of detection.
Immediately upon contract award, the three selected waste
Generators were notified and arrangements were made to collect
adeauate auantities of each effluent. Personnel from ERGO super-
vised sample collection. Effluent samples were collected in
polyethylene-lined,. DOT-approved barrels and transported to ERGO's
laboratory. At the laboratory, each effluent was transferred to a
300-gallon polyethylene (Nalgene)1" tank and homogenized with a
Lightin model ND-1 mixer and aerator for 24 hours prior to sub-
sampling. The effluent was then subsampled into acid-rinsed,
1-gallon polyethylene bottles. Subsampling was accomplished using
subsurface grab sampler (Fisher #15-437) to collect discrete
samples at mid-depth in the tank. The discrete 1-liter samples
were transferred sequentially to the individual polyethylene
bottles. After each bottle received one aliquot of sample, the
tank was resampled and additional aliquots transferred sequentially
until all bottles were full. Each sample was then preserved with
equal amounts of concentrated Ultrex nitric acid to a pH of <2.
The effluents were continuously stirred during subsampling to
maximize homogeneity of suspended matter,in the effluents. Suf-
ficient effluent was collected to allow preparation of 100 1-gallon
aliquots. This provided enough discrete samples to supply each
subcontractor laboratory with 4 gallons of effluent and still have
a 4-gallon reserve for each, as well as providing 20 additional
gallons for homogeneity testing and background analysis.
-30-
-------
Following preparation of the effluent samples, 10 1-gallon
samples of each effluent were selected at random and analyzed in
triplicate by ERCO's Trace Metals Laboratory to determine homo-
geneity of the sample. The results of this analysis are summarized
in Table 5 where the range of analyte values for each effluent are
given.
Analysis of each of the ten 1-gallon aliquots was performed in
triplicate for all elements of interest using the graphite furnace
methods to be used by the collaborating laboratories. A simple
analysis of variance can then be used to demonstrate homogeneity of
each effluent for each element (4). If the ratio of the between-to-
within sample variances is less than the tabulated F statistic of
1.96 (F.01, 9, 20), the sample is homogeneous; the variation within
a single gallon is not significantly different from the variation
between bottles. All aliauots of each of the three effluents
analyzed were not significantly different from one another; i.e.,
they were homogeneous.
After verification of sample homogeneity, approval of
analytical data, and preparation of sample concentrates, 4
gallons of each effluent sample were shipped to each subcontrac-
tor. Samples were packaged and shipped according to DOT regula-
tions via air express carrier. In this manner, time delays were
minimized since samples were received one day following shipment
from ERCO, thus expediting chain-of-custody and resupply of lost
or broken samples.
The actual method study was based on analysis of spiked
and unspiked samples of each of the three raw wastewater efflu-
ents supplied by ERCO to each subcontractor laboratory, as well
as on analysis of spiked and unspiked surface, drinking, and
-31-
-------
Table 5. SUMMARY OF HOMOGENEITY TESTING
Analyte
Ag
Al
As
Ba
Be
Cd
Co
Cr
Cu
Pe
Mn
Ni
Pb
Sb
Se
Tl
V
Zn
Range
Effluent ia
<0.5-0.6
14,000-17,000
10-14
91-101
all <0.5
0.44-0.70
all <15
12-14
53-62
500-560
55-61
all <10
16-20
all <5
all <10
all <5
21-26
1,100-1,200
of Concentrations
Effluent 2t>
4.6-7.6
130-190
all <10
12-15
all <0.5
all <0.5
all <15
all <10
194-210
340-390
110-120
all <10
all <5
all <5
all <10
all <5
all <10
23-30
(ug/L)
Effluent 3C
<0.5-0.6
all <10
all <10
34-42
all <0.5
all <0.5
all <15
all <10
all <10
<20-21
2.8-5.5
53-70
all <5
all <5
all <10
all <5
770-880
all <10
aPaper industry effluent.
"Photographic industry effluent.
cSteam and electric industry effluent.
-32-
-------
laboratory-pure waters supplied by each of the ten subcontractor
laboratories. All spiked samples used by the ten laboratories were
prepared by the subcontractor laboratories according to instructions
supplied by ERGO using ERCO-prepared sample concentrates preserved
in sealed glass ampules and containing the 18 elements of interest.
Each sample of wastewater effluent was spiked at three concentration
levels, with each level constituting a Youden Pair (two similar, but
distinctly different concentrations). The spike (dosing) levels
were prepared to represent one, two, and five times the back-
ground concentration in the effluent. In all cases, the lowest
spike was at least twice the estimated detection limit of the
method (1).
Similarly, three samples, one each from surface, drinking, and
laboratory-pure water, were spiked at three levels (just above
the detection limit, in the middle of the linear range, and
near the upper limit of the linear range), with each spike level
constituting a Youden Pair. Using this nonreplicate technique,
precision for each laboratory was obtained as were estimates of
accuracy and precision for the different matrices.
The three industrial effluents were analyzed by inductively
coupled argon plasma emission spectrometry (ICAP) to provide
preliminary estimates of the background levels of each element of
interest and to provide estimates of possible interferences (Na,
Ca, Mg). The ICAP data is presented in Table 6. These levels
were used to calculate the spiking levels of the effluents.
The ICAP data were not in agreement with the homogeneity data
(AA) for several cases - aluminum and silver in effluent 2 and
silver in effluent 1. For effluent 2 the Al ICAP value was 410
ug/L while the AA range was 130 to 190 ug/L. This discrepancy is
most likely due to a positive spectral interference from a high Ca
-33-
-------
Table 6. PRELIMINARY CHARACTERIZATION OF EFFLUENT SAMPLES BY ICAP
Concentration (ug/L)
Element
Aluminum (Al)
Antimony (Sb)
Arsenic (As)
Barium (Ba)
Beryllium (Be)
Cadmium (Cd)
Chromium (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Nickel (Ni)
Selenium (Se)
Silver (Ag)
Thallium (Tl)
Vanadium (V)
Zinc (Zn)
Calcium (Ca)
Magnesium (Mg)
Sodium (Na)
Effluent la
16,600
<150
<10
145
<5
<10
25
<25
90
835
30
75
<25
<10
3.2
<10
25
1,430
42,600
1,240
311,000
Effluent 2b
410
<150
<10
12
<5
<10
<25
<25
291
380
<10
114
<25
<10
62
<10
<10
30
126,000
2,270
161,000
Effluent 3c
<50
<150
-------
concentration (126,000 ug/L) on the ICAP value. Consequently, the
Al spiking values for effluent 2 were slightly higher, twice those
called for by the original scheme discussed below. For effluent 1,
the AA values for silver were at or near the detection limit (0.5
ug/L) while the ICAP value was 3.2 ug/L (also near the detection
limit). The spike,levels were 10, 20, and 50 ug/L and recoveries
were good. For effluent 2, the AA values for silver were in the
range 4.6 to 7.6 ug/L while the ICAP value was 62 ug/L.. Effluent 2
was a photographic effluent containing complexed silver which was
not detected by the AA method. Spike recoveries were below 50% for
all spike levels. This is discussed further in the Results and
Discussion.
If an element was present in an effluent, the three pairs
of spiking concentrates were made so that the spikes would be near
the background concentration and at approximately two and five
times that concentration. If an element was not detected, the
pairs were prepared such that the spiked concentrations were near
the detection limit (at least twice the detection limit), in the
middle of the linear range and near the upper limit of the work-
ing range.
Three additional pairs of sample concentrates were prepared
for spiking the samples of drinking, surface and laboratory-pure
water. These concentrates were made so that the spiked water
concentrations were slightly above the detection limit, in the
center of the linear range and near the limit of the linear range.
The exact concentrations for all spikes are shown in Table 7.
Production of reliable, stable concentrates required strict
attention to purity and reactivity of metal-containing materials
and dissolution reagents used during sample preparation. For
production of sample concentrates for the interlaboratory
-35-
-------
Table 7. ''CONCENTRATIONS IN THE SPIKED SAMPLES (mq/L)
Element
Al
Sb
As
Ba
Be
Cd
Cr
Co
1
w Cu
(Tl
Fe
Pb
Mn
Ni
Se
Ag
Tl
V
Zn
Low
.028Q/.0335
.01 10/.0127
.0124/.0120
.0627/.0591
.00063/. 00047
.00045/. 00079
.0103/.0135
.0315/.0297
.0106/.0122
.0318/.0261
.0141/.0109
.00060/. 00044
.0274/.0311
.0121/.0105
.00045/. 00059
.0105/.0130
.175/.151
.00054/. 00075
Water Spikes
Medium
.0741/.0645
.0568/.0473
.0518/.0618
.165/.194
.00159/. 00191
.00455/. 00532
.113/.0959
.186/.216
.0727/.0973
.236/.200
.0555/.0473
.00500/. 00795
.200/.240
.0764/.0968
.00568/. 00409
.120/.0986
.404/.318
.00532/. 00614
Effluent One Spikes
High
.125/111
.240/.200
.237/.211
.S79/.437
.00909/.0114
.0125/.0101
.200/. 246
.420/. 314
.205/.245
.4557.389
.254/.211
.0148/.01 18
.402/. 482
.205/.246
.0114/.0136
.203/.252
.9827.855
.0139/. 0174
Low
12.6/11.0
.0105/.0122
.01 18/.0098
.060/.0565
.00064/. 00045
.00043/. 00076
.00987/.0129
.0302/.0248
.0101/.0117
1.03/1.22
.0135/.0104
.0910/.107
.0262/.0297
.0116/.0100
.00848/.0107
.0100/.0124
.167/.144
1.74/1 .31
Med i urn
21.7/25.7
.0543/.0452
.0496/.0591
.157/.185
.00152/. 00183
.00435/. 00509
.108/.0917
.230/.164
.0696/.0930
2.18/2.58
.0530/.0452
.192/.220
.191/.230
.0730/.0926
.0215/.0178
.115/.0943
.387/.304
3.40/2.83
High
58.3/49.6
.230/.191
.227/.202
.362/.418
.0087/.0109
.0120/.0097
.192/.236
.309/.407
.196/.234
4.78/5.59
.243/.202
.484/.420
.385/.461
.197/.235
.0427/.0565
.194/.241
.939/.817
5.19/6.41
-------
Table 7. (Continued)
Effluent Two Spikes
Al
Sb
As
Ba
Be
Cd
Cr
1 C°
Ul
-J Cu
1
Fe
Pb
Mn
Ni
Se
Ag
Tl
V
Zn
.46/.51
.0105/.0122
.0118/. 0098
.060/.0565
.00064/. 00045
.00043/. 00076
.00987/.0129
.0211/.0250
.36/.30
.42/.37
.0135/.0104
.151/.111
.0262/.0297
.0116/.0100
.00848/.0107
.0100/.0124
.167/.144
.0302/.0246
1.01/1 .11
.0543/.0452
.0496/.0591
.157/.185
.00152/. 00183
.00435/. 00509
.108/.0917
.250/.212
.65/.S5
.88/.9S
.0530/.0452
.227/.302
.191/.230
.0730/.0926
.0215/.0178
.115/.0943
.387/.304
.Q507/.0650
2.18/1.76
.230/.191
.227/.202
.362/.418
.0087/.0109
.0120/.0097
.192/.236
.461/.403
1.30/1.67
2.61/2.05
.243/.202
.666/.S77
.385/.461
.197/.235
.0427/.0565
.194/.241
.939/.817
.148/.189
Effluent Three Spikes
.0268/.0320
.0105/.0122
.0118/.0098
.060/.0565
. 0006 4/. 000 45
.00043/. 00076
.00987/.0129
.0293/.0347
.0101/.0117
.0304/.0250
.01357. 0104
.00057/. 00042
.0262/.0297
.0116/.0100
.00848/.0107
.0100/.0124
1.58/1 .36
.00051/. 00072
.0790/.0617
.0543/.0452
.0496/.0591
.157/.185
.00152/. 00183
.00435/. 00509
.108/.0917
.211/.166
.0696/.0930
.226/.191
.0530/.0452
.00478/. 00761
.191/.230
.0730/.0926
.0215/.0178
.115/.0943
2.34/2.70
.00509/. 00587
.120/.107
.230/.191
.227/.002
.362/.418
.0087/.0109
.0120/.0097
.192/.236
.43S/.326
.196/.234
.43S/.372
.243/.202
.0142/.0113
.385/.461
.197/.235
.0427/.0565
.194/.241
5.29/6.03
.0133/.0167
-------
method study, all reagents used for dissolution of pure metals or
metal compounds were Ultrex materials supplied by J.T. Baker Co.
Each lot number and the certified analysis for each reagent used
were recorded prior to use during the study. Ultra-pure water was
supplied by a Millipore Super-Q system containing an activated
charcoal bed, two mixed bed ion-exchange columns, and a 0.2-u final
filter. Water is supplied to the Super-Q system from a Millipore
RO system containing two prefilters and a 60-L/hr reverse osmosis
cartridge. Characteristics of the Super-Q water are as follows:
Total solids <1 mg/L
Total organic carbon <0.5 mg/L
Resistivity >18 megohms
Ammonia-N <0.01 mg/L
Total metals <10 ug/L
Ionized material <5 ug/L
This water was monitored continuously for the metals of interest
while it was being used for preparation of sample concentrates.
All substances used as starting materials for production
of sample concentrations were Spec-Pure (Spex Industries)
or Johnson-Matthey pure metals or metal compounds. The elements
were placed in five groups with each group ultimately comprising
a mixed standard stock solution. Element groupings and compound
selection were made utilizing the most recent recommendations of
EPA personnel familiar with multi-element standard production.
For preparation of these stocks, all weighings were per-
formed on a Mettler H51AR analytical balance capable of weighing
to 0.00001 g. All metals or metal compounds were desiccated as
-38-
-------
instructed by EPA (1) prior to weighing. During the dissolution
of the metals or metal compounds, the amount of Ultrex acids was
carefully recorded to allow precise adjustment of the final acid
concentration.
For preparation of the solutions to be used for preparation
of the sample concentrates, a given volume of each mixed standard
stock solution was transferred to a volumetric flask and diluted
to 1 liter with Super-Q water (all volumetric measurements were"
made with Class A pipettes and volumetrics). Prior to the final
dilution, Ultrex nitric acid was added so the final concentration
was 10 mL/L.
The solutions for each sample'concentrate were prepared
individually on a daily basis and the ampules for that concen- .
trate were filled during the same workday from the same solution.
Approximately 3 liters of solution were required for each concen-
trate. After preparation, the solution was transferred to a
Teflon container and continually mixed with a Teflon-coated
magnetic stirring bar. Approximately 23 mL of solution were
transferred to ampules (Wheaton #6620 BB or Kimble #12012 u) that
had been rinsed with cold tap water, hot tap water, and DIW
followed by drying and steam autoclaving for 15 min at 121° C.
The ampules were flame-sealed with a Carlisle ampule sealer. Two
individuals were present to verify all measurements and record-
ings performed during ampule production.
All ampules were packaged in shipping containers and kept
refrigerated. The ampules were shipped with the effluent samples
via air express carrier at the initiation of the analytical
portion of the interlaboratory method study.
-39-
-------
METHOD FOR VERIFICATION OF TRUE VALUES, HOMOGENEITY,
AND STABILITY OF SAMPLE CONTAINERS
After preparation of all sample concentrations, three
ampules of each concentrate were drawn at random and analyzed.
For each set of spike ampules, ten ampules were selected for
analysis at 0, 45, and 90 days following preparation. Ampules
were analyzed in duplicate by inductively coupled argon plasma
emission spectroscopy (ICP) or atomic absorption spectrophoteometry
(AAS). For each time interval (0, 45, and 90 days), the mean and
standard deviation of these analyses are presented in Table 8
along with the theoretical true value determined for each element.
There was no evidence of instability either through loss to the
glass or contamination from it» The average concentrations for
days 0, 45, and 90 were nearly all within 5% of the theoretical
value and all analyzed concentrations were within 10% of the
theoretical value. In fact, all analyses were within 5% of the
theoretical value except for the vanadium concentration in ampule
2a arid aluminum in Ib and 9b.
ANALYSES OF DOSED EFFLUENT AND WATER SAMPLES BY
SUBCONTRACTOR LABORATORIES
Following subsampling of effluent samples, preparation of
sample concentrates, and testing for homogeneity and stability,
4 gallons of each effluent and the appropriate sample concen-
trate were shipped to each laboratory for analyses. Instructions
for sample preparation and analysis were included as well as
requirements for data submittal (45 days) and quality control.
Each laboratory performed the following dosing scheme:
1. Samples were spiked with the metals of interest and
stirred with a magnetic mixer for 1 hr.
-40-
-------
Table 8. RESULTS OF STABILITY TESTING OP SPIKE AMPULES
Concentration (mg/L)
ELEMENT
Al
Sb
AS
Ba
Be
Cd
Cr
Cu
Fe
Pb
Mn
Ni
Se
Ti
V
Zn
Al
Sb
As
Ba
Be
Cd
Cr
Cu
Fe
Pb
Mn
Nl
Se
Ti
V
Zn
AMPULE
IDENTIFICATION
la
la
la
la
la
la
la
la
la
la
la
la
la
la
la
la
Ib
Ib
Ib
Ib
Ib
Ib
Ib
Ib
Ib
Ib
Ib
Ib
Ib
Ib
Ib
Ib
THEORETICAL
0.616
0.242
0.272
1.38
0.0139
0.0100
0.227
0.233
0.699
0.310
0.0131
0.603
0.266
0.230
3.84
0.0118
0.737
0.280
0.225
1.30
0.0103
0.0174
0.296
0.268
0.574
0.239
0.0097
0.684
0.230
0.286
3.32
0.0165
DAY 0
0.617+0.036
0.241+0.004
0.268+0.006
1.41+0.08
0.0140+0.0002
0.0105+0.0003
0.230+0.001
0.230+0.002
0.699+0.005
0.321+0.003
0.0126+0.0002
0.602+0.001
0.275+0.006
0.227+0.002
3.84+0.03
0.0120+0.0010
0.682+0.011
0.276+0.004
0.221+0.002
1.28+0.009
0.0104+0.0003
0.0176+0.0003
0.296+0.002
0.262+0.002
0.574+0.001
0.240+0.005
0.0093+0.0001
0.686+0.008
0.236+0.005
0.285+0
3.31+0.01
0.0166+0.0002
DAY 45
0.653+0.033
0.246+0.004
0.270+0.002
1.44+0.03
0.0137+0.0004
0.0103+0.0001
0.226+0.002
0.230+0.001
0.706+Q.003
0.322+0.006
0.0127+0.0002
0.603+0.003
0.272+0.005
0.233+0.002
3.83+0.01
0.0127+0.0020
0.742+0.041
0.276+0.003
0.219+0.011
1.35+0.04
0.0102+0.0004
0.0173+0.0003
0.295+0.002
0.265+0.001
0.580+0.002
0.250+0
0.0094+0.0002
0.688+0.009
0.243+0.002
0.297+0.006
3.33+0.03
0.0161+0.0009
DAY 90
0.641+0.041
0.239+0.002
0.279+0.002
1.37+0.05
0.0145+0.0002
0.0105+0.0003
0.229+0.002
0.239+0.002
0.719+0.005
0.295+0.008
0.0125+0.0001
0.609+0.008
0.272+0.003
0.232+0.007
3.93+0.01
0.0127+0.0010
0.786+0.013
0.284+0.011
0.233+0.006
1.33+0.09
0.0110+0.0004
0.0173+0.0003
0.300+0.004
0.274+0.001
0.591+0.007
0.249+0.004
0.0092+0
0.697+0.016
0.234+0.003
0.277+0.006
3.39+0.01
0.0172+0.0004
-------
Table 8 (CONT.)
Concentration (ng/L)
ELEMENT
Al
Sb
As
Ba
Be
Cd
Cr
Cu
Pe
Pb
Hn
Ni
Se
Ti
V
Zn
Al
Sb
As
Ba
Be
Cd
Cr
Cu
Pe
Pb
Mn
Nl
Se
Ti
V
Zn
AMPULE
IDENTIFICATION
2a
2a
2a
2a
2a
2a
2a
2a
2a
2a
2a
2a
2a
2a
2a
2a
2b
2b
2b
2b
2b
2b
2b
!2b
2b
2b
2b
2b
2b
2b
2b
2b
THEORETICAL
1.63
1.25
1.14
3.62
0.0350
0.100
2.49
1.60
5.20
1.22
0.110
4.40
1.68
2.64
8.89
0.117
1.42
1.04
1.36
4.26
0.042
0.117
2.11
2.14
4.39
1.04
0.175
5.29
2.13
2.17
6.99
0.1350
DAY 0
1.63+0.07
1.24+0.03
1.12+0.02
3.56+0.09
0.0346+0.0002
0.105+0.002
2.51+0.01
1.54+4.01
5.12+0.02
1.28+0.001
0.111+0.001
4.36+0.005
1.71+0.01
2.55+0.09
8.07+0.02
0.123+0.002
1.41+0.04
1.03+0.01
1.37+0.02
4.11+0.04
0.043+0.001
0.119+0.002
2.14+0.01
2.09+0.01
4.42+0.01
1.08+0.02
0.176+0.001
5.24+0.01
2.11+0.04
2.11+0.04
6.99+0.01
0.143+0.002
DAY 45
1.58+0.01
1.25+0.01
1.14+0.01
3.82+0.01
0.0347+0.0003
0.104+0.002
2.52+0.02
1.60+0.01
5.27+0.04
1.26+0.03
0.112+0.001
4.41+0.03
1.70+0.02
2.68+0.06
8.24+0.06
0.116+0.002
1.43+0.08
1.04+0.02
1.38+0.02
4.47+0.09
0.043+0.001
0.120+0.002
2.15+0.01
2.14+0.01
4.53+0.02
1.06+0.01
0.179+0.001
5.30+0.03
2.11+0.02
2.14+0.06
7.14+0.03
0.140+0.001
DAY 90
1.69+0.06
1.29+0.04
1.12+0.03
3.74+0.08
0.0357+0.0009
0.104+0.002
2.55+0.02
1.63+0.01
5.31+0.03
1.18+0.01
0.115+0.002
4.49+0.03
1.74+0.03
2.68+0.08
8.35+0.06
0.117+0.001
1.42+0.03
1.05+0.02
1.34+0.02
4.21+0.04
0.044+0.001
0.120+0.002
2.17+0.02
2.18+0.02
4.54+0.03
1.09+0.02
0.181+0.002
5.42+0.06
2.14+0.02
2.19+0.06
7.18+0.05
0.141+0.001
-------
Table 8 (CONT.)
Concentration (mg/L)
I
*>.
CO
I
ELEMENT
Al
Sb
As
Ba
Be
Cd
Cr
Cu
Fe
Pb
Hn
Ni
Se
Ti
V
Zn
Al
Sb
As
Ba
Be
Cd
Cr
Cu
Fe
Pb
Mn
Ni
Se
Ti
V
Zn
AMPULE
IDENTIFICATION
' 3a
3a
3a
3a
3a
3a
3a
3a
3a
3a
3a
3a
3a
3a
3a
3a
3b
3b
3b
3b
3b
3b
3b
3b
i
3b
3b
3b
3b
3b
3b
3b
3b
THEORETICAL
2.75
5.29
5.22
8.33
0.200
0.276
4.41
4.51
10.0
5.59
0.326
8.85
4.52
4.47
21.6
0.305
2.45
4.40
4.65
9.62
0.250
0.223
5.42
5.39
8.56
4.65
0.260
10.6
5.41
5.55
18.8
0.383
DAY 0
2.70+0.02
5.20+0.01
5.13+0.08
8.29+0.07
0.204^0.001
0.274+0.002
4.46+0.01
4.35+0.02
10.1+0.1
5.61+0.03
0.330+0.001
8.77+0.09
4.45+0.02
4.44+0.04
21.8+0.1
0.311+0.001
2.37+0.03
4.36+0.02
4.67+0.04
9.16+0.05
0.258+0.003
0.221+0.002
5.39+0.04
5.27+0.03
8.49+0.07
4.71+0.07
0.264+0.001
10.5+0.1
5.34+0.04
5.35+0.02
18.5+0.1
0.388+0.003
DAY 45
2.77+0.04
5.34+0.05
5.27+0.07
8.59^0.06
0.213+0.001
0.278+0.002
4.56+0.02
4.60+4.02
10.5+0.1
5.58+0.04
0.339+0.001
8.93+0.04
4.52+0.04
4.78+0.03
22.6+0.1
0.302+0.001
2.44+0.01
4.49+0.05
4.64+0.01
9.92+0.05
0.264+0.001
0.225+0.002
5.46+0.01
5.48+0.01
8.74+0.01
4.62+0.01
0.268+0.001
10.7+0.1
5.43+0.05
5.67+0.01
19.1+0.1
0.377+0.002
DAY 90
2.81+0.13
5.32+0.03
5.27+0.13
. 8.46+0.0.4
0.209+0.001
0.275+0
4.56+0.02
4.57+0.02
10.3+0.1
5.57+0.03
0.339+0.002
'8.90+0.02
4.57+0.02
4.65+0.02
22.6+0.1
0.305+0.005
2.53+0.07
4.39+0.02
4.62+0.04
9.78+0.18
0.257+0.002
0.224+0.002
5.42+0.03
5.43+0.03
8.44+0.09
4.60+0.01
0.266+0.002
10^5+0.1
5.41+0.06
5.63+0.05
18.9+0.2
0.384^0.019
-------
Table 8 (CONT.)
Concentration (mg/L)
I
*>.
ELEMENT
Al
Co
Pe
Mn
Zn
Al
Co
Pe
Mn
Zn
Al
Co
Fe
Mn
Zn
Al
Co
Fe
Mn
Zn
Al
Co
Fe
Mn
Zn
Al
Co
Fe
Mn
Zn
AMPULE
IDENTIFICATION
4a
4a
4a
4a
4a
4b
4b
4b
4b
4b
5a
5a
5a
5a
5a
5b
5b
5b
5b
5b
6a
6a
6a
6a
6a
6b
6b
6b
6b
6b
THEORETICAL
290
0.694
23.0
2.08
40.0
253
0.571
27.5
2.44
30.0
498
4.67
45.0
4.30
78.0
590
3.76
55.0
4.88
65.0
1,337
7.10
100
10.8
119
1,138
9.35
120
9.40
147
DAY 0
289+3.2
0.704+0.008
22.9+0.3
2.13+0.03
38.5+0.5
253+2
0.584+0.004
28 .1+0.2
2.51+0.02
29.6+0.2
494+1
4;71+_0.01
45.5+0.1
4.32+0.01
75.6+0.2
584+6
3.76+0.01
55 .3+0.4
4.94+0.03
64.4+0.4
1,228+8
7.14+0.05
101 + 1
10.9+0.1
119+1
1,140+14
9.37+0.13
122+2
9.39+_0.15
143+2
DAY 45
291+1
0.698+0.002
22.8+0.1
2.07+0.01
39.7+0.3
253+2
0.571+0.003
27.8+0.2
2.43+0.02
30 .1+0.1
508+3
4.73+0.17
45.7+0.2
4.24+0.02
80.3+0.2
605+1
3.67+0.06
55.8+0.1
4.87+0.01
65.5+0.1
1,360+28
6.97+0.17
99+2
10.5+0.2
119+2
1,154+17
9.22+0.14
121+2
9.09+0.15
145+2
DAY 90
290+4
0.679+0.004
24.0+0.2
2.18+0.03
39 .2+0.4
253+3
0.558+0.006
29,2+0.6
2.56+0.05
29.8+0.5
491+2
4.53+0.02
46.9+0.2
4.39+0.02
78 . 5+0 . 1
583+6
3.73+0.05
57.9+0.9
5.12+0.07
65.0+0.6
1,313+24
7.16+0.12
103+2
11.1+0.2
119+1
1,121+8
9.47+0.10
126+1
9.59+0.09
143+1
-------
Table 8 (CONT.)
Concentration (mg/L)
Ul
I
ELEMENT
Al
Co
Cu
Pe
Mn
Zn
Al
Co
Cu
Pe
Mn
Zn
Al
Co
Cu
Pe
Mn
Zn
Al
Co
Cu
Pe
Mn
Zn
AMPULE
IDENTIFICATION
7a
7a
7a
7a
7a
7a
7b
7b
7b
7b
7b
7b
8a
8a
8a
8a
8a
8a
8b
8b
8b
,8b
8b
8b
THEORETICAL
10.0
5.75
8.00
8.95
3.45
0.682
10.9
4.87
6.70
7.90
2.54
0.550
21.5
0.485
13.3
15.0
5.10
1.05
24.0
0.575
10.6
17.5
6.78
1.36
DAY 0
10.45*0.15
5.92+0.05
8.28+0.11
9.35+0.11
3.59+0.04
0.719+0.008
11.4+0.1
4.92+0.11
6.89+0.08
8.15+0.17
2.60+0.06
0.569+0.01
22.0+0.3
0.485+0.005
13.6+0.2
15.3+0.2
5.17+0.07
1.10+0.01
25.0+0.1
0.577+0.02
10.8+0.1
17.7+0.1
6.86+0.01
1.41+0.01
DAY 45
9.83+0.06
5.79+^0.01
7.94+0.02
8.83+0.03
3.42+0.01
0.676+0.002
lO.BjfO.l
4.96+0.02
6.72+0.01
7.88+0.02
2.53+0.01
0.550+0.01
20.8+0.1
0.493+0.004
13.3+0.1
14.8+0.1
5.12+0.02
1.07+0.01
23.7+0.2
0.586+0.006
10.6+0.1
17.2+0.2
6.81+0.04
1.38+0.01
DAY 90
9.51+0.01
5.55+0.02
7.70+0.01
8.66+0.01
3.36+0.01
0.652+0.004
10.9+0.4
4.74+0.02
6.484-0.04
7.70+0.07
2.49+0.01
0.532+0.01
20 .1+0.1
0.477+0.002
12.9+0.1
14.7+0.1
5.08+0.02
1.03^0.01
22.8+0.1
0.563+0.003
10.3+0.1
17.0+0.1
6.75+0.03
1.33+0.01
-------
Table 8 (CONT.)
Concentration (mg/L)
ELEMENT
Al
Co
Cu
Fe
Hn
Zn
Al
Co
Cu
Fe
Mn
Zn
Co
V
Co
V
Co
V
Co
V
Co
V
Co
V
AMPULE
IDENTIFICATION
9a
9a
9a
9a
9a
9a
9b
9b
9b
9b
9b
9b
lOa
lOa
lOb
lOb
lla
lla
lib
lib
12a
12a
12b
12b
THEORETICAL
47.5
10.6
25.5
50.0
15.0
3.10
38.0
9.27
33.0
38.7
13.0
3.96
0.675
32.5
0.797
28.0
4.85
45.0
3.82
55.0
10.0
100
7.50
120
DAY 0
49.5±0.2
10.7+0.1
26.6+0.1
51.0+0.3
15.4+0.1
3.26+0.01
39 . 9+0 . 3
9.38+0.07
34.4+0.3
39.9+0.5
13.5+0.1
4.15+0.02
0.675+0.004
34.0+0.2
0.806+0.008
28 . 8+0 . 3
4.86+0.01
46 .2+0.1
3.87+^0.01
56 . 5+0 . 1
9.86+0.15
101+2
7.36+0.08
122+2
DAY 45
48.3+0.4
10.7+0.1
25.2+0.2
49.0+0.3
14.6+0.1
3.07+0.02
38.9+0.2
9.35+0.02
32.5+0.1
38.4+0.2
12.8+0.1
3.87+0.01
0.681+0.002
32.8+0.2
0.797+0.006
27 . 4+0 . 3
4.90+0.09
44.7j+0.9
3.79+0.02
53.2+0.2
9.95+0.06
96.8+0.5
7.51+0.05
119+1
DAY 90
44.7+0.1
10.4+0.1
25.1+0.1
48.4+0.1
15.1+0.1
3.04+0.01
35.9+0.1
9.08+0.02
32.5+0.1
37.9+0.1
13.2+0.1
3.86+0.01
0.668+0.003
33.2+0.1
0.788+0.008
28.0+0.2
4.80+0.02
46.6+0.2
3.81+0.01
56.8+0.1
9.83+0.15
104+2
7.31+0.03
125+1
-------
Table 8 (CONT.)
Concentration (mg/L)
ELEHENT
CO
Ag
CO
Ag
Co
Ag
Co
Ag
Co
Ag
Co
Ag
Ag
Ag
Ag
Ag
Ag
Ag
AMPULE
IDENTIFICATION
13a
13a
13b
13b
14a
14a
14b
14b
15a
15a
15b
15b
16a
16b
17a
17b
18a
18b
THEORETICAL
0.693
0.010
0.653
0.013
4.10
0.125
4.75
0.090
9.24
0.250
6.90
0.300
0.195
0.245
0.495
0.410
0.982
1.30
DAY 0
0.696+0.009
0.0108+0
0.662+0.002
0.0127+0.0001
4.18+0.06
0.127+0.001
4.78+0.02
0.0875+0.001
9.38+0.06
0.245+0.001
6.95±0.03
0.305+0.002
0.195+0.003
0.243+0.003
0.490+0.002
0.409+4.003
0.961+0.002
1.27+0.001
DAY 45
0.682+0.006
0.0109+0.0001
0.643+0.002
0.0128+0
3.97+0.02
0.125+0.001
4.58+0.04
0.0879+0.001
9.04+0.05
0.253+0.001
6.79+0.03
0.314+0.001
0.195+0.003
0.248+0.001
0.501+0.002
0.420+0.001
0.993+0.005
1.33+0.01
DAY 90
0.700+0.005
0.0108+0.0002
0.653+0.003
0.0128+0.0002
4.14+0.03
0.130+0.001
4.80+0.04
0.0899+0.001
9.30+4.08
0.252+0.001
6.97+0.001
0.312+0.001
0.193+^0.003
0.244+0.001
0.497+0.002
0.412+0.001
0.992+0.002
1.31+0.01
-------
The samples were then capped and stored at room
temperature (approximately 20° C) for 1 week (7 days).
The pH was adjusted to pH of 2 or less with 1:1 nitric
acid and refrigerated for 24 hr.
The samples were then prepared and analyzed according
to the U.S. EPA Methods.
No deviations from the U.S. EPA methods were permitted
nor were further restrictions applied, i.e., use of
background correction, use of coated or treated.graphite
were not required or prohibited.
The type and number of analyses that were required of each
laboratory are shown in Table 9.
QUALITY ASSURANCE REQUIREMENTS FOR PARTICIPATING LABORATORIES
The quality assurance plan utilized to monitor the performance
of the subcontractor laboratories was based on the ongoing quality
assurance plan used routinely by ERCO's Trace Metals Laboratory for
all in-house work. At a minimum, all subcontractor laboratories
were required to adhere to the guidelines set forth in that plan.
The quality assurance plan for all participating laboratories
also contained the following elements:
1. As part of the preliminary screening phase, each
subcontractor laboratory was required to submit
detailed summaries of qualifications of all personnel
working on this project.
2. After the preliminary screening phase, each potential
subcontractor laboratory was required to participate
in an ERCO-conducted performance evaluation study.
3. Each subcontractor laboratory was required to
retain all pertinent raw data, finished data, and QC
data generated during this study until final disposi-
tion of the data is determined by EPA and/or ERGO.
-48-
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Table 9. TYPE AND NUMBER OF ANALYSES
Type of analysis Number of analyses3
Background analyses for 18
the metals of interest
in laboratory-pure water
(18 metals)
Background analyses for 18
the metals of interest
in drinking water
(18 metals)
Background analyses for 18
the metals of interest
in surface water
(18 metals)
Background analyses for 54
the metals of interest
in effluents
(18 metals x 3 effluents)
Analyses for the metals
of interest in the six
water types (laboratory-
pure water, drinking
water, surface water,
and the three industrial
effluents) dosed with
each of the sample
concentrates:
5 water typesb x 540
6 concentrates x
18 metals
1 water typec x 216
12 concentrates x
18 metals
Total number of analyses 864
aAn analysis is the determination of one metal in one
sample.
_ Surface water, drinking water, and three effluents.
cLaboratory-pure water.
-49-
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Each subcontractor laboratory'was required to adhere
to procedures for sample preparation and analysis
supplied by ERCO. At a minimum, calibration curves
consisted of a blank and four standards within the
appropriate linear ranqe. Instrument check standards
containing the element of interest at concentrations
approximating the midpoint of the calibration curve
were run at the beginning and end of the day and at
a frequency of 10% during sample analysis. If
results did not agree to within 10% of the true
value, analysis was terminated. After the problem
was resolved and the instrument.was recalibrated, all
samples analyzed since the last successful check
standard were reanalyzed.
COMPUTER PROCESSING OF LABORATORY DATA
The participating laboratories supplied data on forms provided
by ERCO. This data was then entered onto hard disc files from
which the data was processed by the IMVS program supplied by EPA.
All the raw data and the statistical summaries generated by the IMVS
program are included in Appendix C and summarized in sections 2
and 5 of this report.
-50-
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SECTION 4
TREATMENT OF DATA
The objective of this interlaboratory study was to obtain
information about the accuracy and precision associated with
measurements generated by the furnace methods. This objective was
met through the use of statistical analysis techniques designed to
extract and summarize the relevant information about accuracy and
precision from the data reported by the participating laboratories.
The statistical techniques employed in the data reduction process
are similar to the techniques suggested in the ASTM Standard
Practice D2777-77 (5).
The algorithms required to perform the statistical analyses
have been integrated into a U.S. EPA system of computer programs
referred to as IMVS. The analyses performed by IMVS include
several tests for the rejection of outliers (laboratories and
individual data points), summary statistics by concentration level
for mean recovery (accuracy), overall and single-analyst standard
deviation (precision), determination of the linear relationship
between mean recovery and 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 follows.
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REJECTION OF OUTLIERS
Since the objective of the statistical analysis 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 study. Therefore, incon-
sistent data points should not be removed indiscriminately, 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 not inconsistent since outliers are judged
relative to the average value of the data and not with respect to
the true value. Data rejected as 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 attributed to that laboratory. These data are not
representative of the method and should be rejected. Youden's (2)
ranking test for outlying laboratories was applied separately to
data from each of the waters used in this study.
The Youden laboratory ranking procedure requires a complete
set of data from every laboratory within a given water type.
Missing data from laboratory i for water type j were replaced by
-52-
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the following procedure. Letting Xijk denote the reported
measurement from laboratory i for water type j and concentration
level Ckf it is assumed that
xijk = Bj . CkvJ - Li . eijk
where Bj and vj are fixed parameters which determine the
effect of water type j, L± is the systematic error due to
laboratory i and eijk is the random within the laboratory
error. Taking natural logarithms, it follows that
Y. n A i T t ^* n P T * ^ T n t^ t * ^n LJ i * ^n ^i T t
^ J JX | J ^w X i I f^.
which is a linear regression model with dependent variable £n X^|k
and independent variable £n Ck. 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
regressed against the natural logarithms of the true concentration
levels for the six ampules in each water type. The predicted
values £nXijk were obtained from the regression equation, and the
missing values of X^k were estimated by Xijk = exp( £n Xijk) ,
where exp(x) denotes the constant e raised to the power X.
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 procedure, the predicted values created to fill
in for the missing data were rejected and excluded from further
analyses for all laboratories.
-53-
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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 subsets 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(6),
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 upon the basis of this test, it was removed
from the subset, and the test was repeated using the remaining
data in the subset. This process was continued until no additional
data could be rejected.
STATISTICAL SUMMARIES
Several summary statistics were calculated using the data
remaining for each concentration level after the outlier rejection
tests were performed: 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 statistics are presented below
(xlf X2,..., Xn denote the values of the n retained data
points for a specific concentration level):
Mean Recovery (X): n
X = J- V Xi
n 2-1
-54-
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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 100
True Value
Overall Standard Deviation:
:i - x)2
and
Percent Relative Overall Standard Deviation:
Percent RSD = - . 1QO
X
The overall standard deviation S indicates the precision
associated with measurements generated by a group of laboratories.
This represents the broad variation in the data collected in an
interlaboratory study. However, a measure of how well an individual
analyst can expect to perform in his own laboratory is another
important measure of precision. This single-analyst precision,
denoted by SR, was estimated for each Youden pair by
m
2(m -
-55-
-------
where
m = the number of complete sets of Youden pair observations
remaining after outliers have been removed,
Di = the difference between the observations in the ith
Youden pair
and
D = average of the DI values.
The percent relative single-analyst standard deviation was
calculated by
CD
Percent RSD-SR = . 100
X*
where X* is the average of the two mean recovery statistics corre-
sponding 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 objective 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).
-56-
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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 esti-
mates 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 con-
ditions. These important relationships are discussed below.
STATEMENT OF METHOD ACCURACY
The accuracy of the method is characterized by the relation-
ship 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 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)
XI
- = a - + b (2)
-57-
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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 (7), 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
a + b C a
Percent Recovery = ^ 100 = -= b 100 (3)
If the absolute value of the ratio (a/C) 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 100. For example,
suppose the true concentration values range from 25 ug/L to 515
ug/L, and the fitted line is given by X = 0.20 + 0.85 C. The
percent recovery would be approximated by 0.85 100 = 85%
over the specified range of 25 ug/L to .515 ug/L.
If the ratio (a/C) is not small relative to the slope (b),
then the percent recovery depends upon the true concentration (C),
and it must be evaluated at each concentration value within the
specified range.
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STATEMENT OF METHOD PRECISION
The precision of the method is characterized by the relation-
ships 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 + q 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)
S 1
-= d -+ e (6)
and by dividing both sides of Equation (5) by X* resulting in
Equation (7)
SR 1
= f ' + (7)
-59-
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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).
Given Equations (4) and (5), the percent relative overall
standard deviation and the percent relative single-analyst standard
deviation are
Percent RSD = ^ + e 100 (8)
and
Percent RSD-SA = + g 100 (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 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 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),
-60-
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then the percent relative standard deviations depend upon the
values of the mean recovery statistics X and X*f 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 the furnace
methods depend upon the type of water being analyzed. The summary
statistics X, S, and SR are calculated separately for each concen-
tration level within each water type. The summary statistics 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 disadvan-
tages. 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 element.
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, 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 (8), 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 concentration levels rather than studying the
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local effects at each concentration level. If sianifleant differ-.
ences are established by this alternative technique, then the
summary statistics can be used for further local analysis.
The test for the effect of water type is based on the following
statistical model. If Xijk denotes the measurement reported by
laboratory i, for water type j, and ampule k, then
xijk = Bj CkVJ Li . £ijk i = 1,2,..., n (10)
j - 1/2,...f 6
JC "~ _Lf^/...p D .
The model components gj and vj are fixed parameters which deter-
mine the effect of water type j on the behavior of the observed
measurements (X^j^). The parameter C^ is the true concentration
level associated with ampule k. The model component L^ is a
random factor which accounts for the systematic error associated
with laboratory i. The model component £ijk is the random factor
which accounts for the within-laboratory error.
The model is designed to approximate the global behavior of
the data. The multiplicative structure was chosen because of two
important properties. First, it allows for a possible curvilinear
relationship between the data (Xjik) and the true concentration
level Cfc through the use of the exponent vj on C]<. 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 concentra-
tion level Cfc in this model. This property is important because
it is typical of interlaboratory data collected under conditions
where the true concentration levels vary widely.
-62-
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Accuracy is related directly to the mean recovery or expected
value of the measurements (Xijk). The expected value for the
data modeled by Equation (10) is
E(Xijk) = Bj . ck vj . E(Li £ijk) (11)
Precision is related to the variability in the measurements
(xijk) The variance of the data modeled by Equation (10) is
Var(Xijk) = [6j Ck vj] Var(Li . £ijk) (12)
which is an increasing function of Ck.
The effect of water type on the accuracy and precision of the
methods is determined by the values of the parameters ( 3j) and
(Vj) in Equations (11) and (12). If the (6j) and (vj) 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) repre-
sents the basic model. However, taking natural logarithms of both
sides of Equation (10), the following straight line regression model
is obtained:
£n xijk = £n 6j + vj £n ck + £n Li + &n eijk (13)
which can be analyzed using standard linear model analysis tech-
niques. The parameter £n 6j is the intercept and vj the slope of
the regression line associated with water type j. It is assumed that
-63-
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£n Li is normally distributed with mean 0 and variance OL, and that
^n £ijk is normally distributed with mean 0 and variance o^, and that
the (in Ljj and ( in £ik) 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.
Using the data on the log-log scale and regression techniques,
the parameters in Bj (and hence 6 j ) and vj 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 HQ and HA are aiven by
H0: in Bj - in BI = 0 and vj - V]_ = 0 for j = 2,3,4,5,6
versus
H : £n 8. - in B, ^ 0 and/or v. - v, ^0
A J J. J J.
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 probability of obtaining a value of an
F-statistic as large -as the value which was actually observed
(Fobs)f denoted by P(F > Fobs)r is calculated under the assump-
tion that HO is true. The null hypothesis HO is rejected in
favor of HA if P(F > Fobs) is less than 0.05.
If HO is rejected, then some linear combination of the differ-
ences £n Bj - Jin BI and vj - vi is statistically different from zero
However, this does not guarantee there will be a statistically
-64-
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significant direct effect attributable to any specific water type
since the overall F test can be overly sensitive to minor systematic
effects common to several water types. The effect due to a specific
water type is judged to be statistically significant only if one of
the differences £n gj - £n $1 and/or vj - vi is statistically dif-
ferent from zero. This is determined by checking the simultaneous
95 percent confidence intervals which are constructed for each of
these differences. Each true difference can be stated to lie within
O
its respective confidence interval with 95 percent confidence. If
zero is contained within the confidence interval, then there is no
evidence that the corresponding difference is significantly different
from zero.
If at least one of the confidence intervals for the differences
£n Bj - &n BI or vj - v^ fails to include zero, then the statistical
significance of the effect due to water type has been established.
However, establishment of a statistically significant effect due to
water type does 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 (X^j^) 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 = 1) on a relative basis by the ratio
BjCkv E(Lj - _ __ c
"
E(Xilk) BI Ckv E(Li eUk) 61
-65-
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(The ratio of the standard deviations would be equivalent to Equa-
tion (14) and therefore the interpretation of the effect on precision
is the same as that for the effect on mean recovery.)
The ratio in Equation (14) is a measure of the relative differ-
ence in mean recovery between water type j and distilled water. It
is composed of two parts: (a) Bj/Si, which is independent of the
true concentration level (i.e. the constant bias), and (b) CKVJ ~v^
which depends upon the true concentration level (i.e. the concentra-
tion dependent bias). If vj - V]_ is zero, then the relative
difference in mean recovery is just Bj/3i, which is independent of
concentration level C^. It can then be stated that the mean
recovery of water type j is (6j/6i) x 100 percent of the mean
recovery for distilled water. If vj - vi is not zero, then the mean
recovery of water type j is ([3j/Bi] Cj^j ~ vl) x 100 percent
of that for distilled water, and therefore depends upon the true
concentration level C^.
In order to illustrate these points, consider the following
example. Suppose that a significant F-value has been obtained, and
the confidence intervals for all the differences contain zero except
for water type 5. Suppose for water type 5, the point estimate for
in 65 - in BI is -0.38 and the confidence interval for in 65 - in Bl
is (-0.69, -0.07). Suppose the point estimate for v5 - v^ is 0.07,
and the confidence interval for ^5 - v-j_ 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 (14).
The ratio of mean recoveries for water type 5 and distilled water
is given by
E 65 c (vs - vi)
el k (15)
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1
Var(Xijk)
Var(Xnk)
= S c
( V5 - vl )
-k
and the ratio of the standard deviations is aiven by
(16)
Since the confidence interval for vs - vi contains zero, this
difference is assumed to be insignificant and is set to zero.
Therefore, Equations (15) and (16) reduce to 65/61. The point
estimate for £n 65 - £n6i was -0.38. Therefore, the point
estimate for 65/61 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 £n 65 - £h 6]_ 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 model 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.
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SECTION FIVE
RESULTS AND DISCUSSION
The statistical analysis procedures described in the pre-
ceding section were applied to the raw data for the 10 labora-
tories. The results of those analyses are discussed below.
Prior to a discussion of the results of the recoveries
obtained by each of the laboratories, it is instructive to
examine the results of analyses for each element in each of the
three effluents. All of the data entered into the IMVS program
were for concentrations of the spikes determined in each of the
six waters, that is, the background level of each element in
each water or effluent was subtracted from the concentration of
the spiked water or effluent and the increase (amount recovered)
reported.
The three water samples (lab pure, drinking and surface) were
supplied by each individual laboratory and were consequently not
analyzed by ERCO or by any of the other nine laboratories. The
three effluents, however, were analyzed by all ten labs, by ERCO
using the same (AAS) methods and by ERCO using inductively
coupled plasma emission spectrometry (ICP). The results of these
analyses of the unspiked effluents are presented in Table 10.
These data clearly demonstrate problems with certain analyses
by certain laboratories. The most obvious discrepancies are for
Al and Zn in all effluents. The large range of results indicate
frequent and presumably reproducible errors. The results for Al
in effluent 1 range from not detected (<\>10 ug/L) to 29,240 ug/L.
Laboratory 5 was unable to detect Al in any of the effluents. For
effluent 3, which had low Al levels, one laboratory reported
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Table 10. EFFLUENT BACKGROUND CONCENTRATIONS DETERMINED BY THE TEN LABORATORIES
I
CTl
*£>
I
Effluent
Element
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Ag
Tl
V
Zn
1. (Concentrations in ug/L)
1
29,240
1.81
19.3
5,440
0.93
0.23
16.75
9.23
69.8
660
21.5
75.2
15.3
0.90
0.81
1.12
77.4
1,170
2
19,100
ND
ND
104
ND
9.3
13.2
19
52
491
ND
39
ND
ND
ND
ND
75
1,270
3
16,600
ND
43.7
112
ND
3.7
10.4
7.5
76.7
1,270
18.9
67.1
11
30.8
2.7
12.5
19.7
20,300
4
19.000
ND
5.0
140
ND
2.0
12
5.0
56
730
8.5
50
ND
ND
ND
ND
18
2,800
5
ND
19
10
10
ND
2
12
9
ND
1,460
12
62
4
6
1
ND
48
500
Labor atoiy
6
6,000
6
17
150
ND
2.3
51
7
56
790
31
77
62
23
ND
ND
ND
1,480
7
7,900
ND
20
79
ND
0.5
11
ND
62
480
ND
74
10
3
ND
ND
17
1,000
8
11,500
ND
ND
30
ND
ND
12
ND
51
950
20
51
30
6
ND
ND
ND
4,850
9
21,500
ND
38.2
74.9
ND
0.64
15.0
24.7
32.2
626
19.8
110
17.8
14.5
0.43
ND
26.9
1,670
10
15,000
ND
10
125
ND
0.6
20
ND
65
800
19
70
8
5
ND
1
25
2,000
ERCO AA*
14-17,000
<5
10-14
91-101
<0.5
0.44-0.70
12-14
<15
53-62
500-560
16-20
55-61
<10
<10
<0.5-0.6
<5
21-26
1,100-1,200
ERCO ICP**
16,600
<150
<10
145
<5
<10
25
<25
90
835
30
75
<25
<10
3.2
<10
25
1,430
ERCO data from the homogeneity testing (Table 5).
**ERCO data from the preliminary effluent characterization (Table 6).
-------
Table 10. (Continued)
O
I
Effluent
Element
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
re
Pb
Hn
Ni
Se
Ag
Tl
V
Zn
2. (Concentrations in ug/L)
1
31.5
1.85
ND
208
0.91
0.60
8.31
8.13
223
598
3.58
146
11.1
2.12
13.7
1.57
17.8
513
2
206
4
3
29
ND
ND
8
11
220
482
2
90
4
3
15.8
ND
112
20.6
3
291
ND
22.3
30.9
ND
1.70
ND
2.1
219
1,040
5.0
77.0
17
53.3
3.5
3.7
16.2
69.6
4
210
ND
ND
17
ND
0.6
ND
ND
240
360
5.0
120
6.0
ND
8.4
ND
ND
900
5
ND
12
ND
ND
ND
1
3
5
109
800
2
76
6
23
11
ND
32
390
Laboratory
6
120
2
15
20
0.1
2.6
106
ND
209
830
ND
274
21
8
1.2
ND
ND
1,360
7
760
ND
7
17
ND
0.4
8
ND
200
300
ND
144
12
3
15
ND
ND
16
8
170
ND
ND
226
ND
ND
5
ND
165
378
ND
107
30
12
6.9
ND
ND
510
9
142
0.9
12.2
ND
0.2
0.3
6.5
0.72
69.5
263
ND
90.5
9.9
28.8
1.18
0.34
7.26
39.6
10
300
ND
ND
25
ND
0.6
15
ND
200
500-
6
200
10
5
12
1
ND
20
ERCO AA*
130-900
<5
<10
12-15
<0.5
<0.5
<10
<15
194-210
340-390
<5
110-120
<10
-------
Table 10. (Continued)
Effluent
Element
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Nl
Se
Ag
Tl
V
Zn
3. (Concentrations in ug/L)
1
33.7
2.51
4.0
197
0.62
0.30
16.21
9.88
15.7
114
6.45
2.58
125.9
5.33
1.17
2.14
865
842
2
2
8
5
72
1.1
0.4
2
30
5
106
23
2
64
6
1.8
2
846
12
3
38.1
11.9
33.8
49.8
ND
1.20
13.0
7.7
20.9
57.0
7.1
1.2
107
73.1
4.1
21.8
1,020
58.0
4
ND
ND
ND
47
ND
ND
ND
ND
ND
110
ND
ND
74
ND
ND
ND
830
920
5
ND
16
ND
46
ND
1
2
2
1
107
ND
ND
92
20
ND
ND
1,480
320
Laboratory
6
260
3
9
42
ND
0.6
19
ND
2
ND
ND
ND
126
8
ND
ND
630
310
7
1,900
ND
13
34
ND
ND
3
ND
7
54
ND
ND
117
15
ND
ND
780
7
8
ND
ND
ND
53
ND
ND
4
ND
9.1
28
ND
ND
42
12
ND
ND
920
3
9
68:2
2.8
53.5
ND
ND
0.08
ND
2.7
20.0
46.5
3.7
8.8
74.2
140
ND
0.5
576
3.5
10
ND
ND
10
95
ND
ND
8
ND
2
26
3
1.2
60
20
ND
3
800
3.5
ERCO AA*
<10
<5
<10
34-42
<0.5
<0.5
<10
<15
<10
<20-21
<5
2.8-5.5
53-70
<10
<0.5-0.6
<5
770-880
<10
ERCO ICP**
<50
<150
<10
41
<5
<10
<25
<25
<10
<50
<10
<10
109
<10
<10
<10
918
<10
ERCO data from the homogeneity testing (Table 5).
'ERCO data from the preliminary effluent characterization (Table 6).
-------
1,900 ug/L. Both contamination and methodological difficulties
appear to be at fault. In fact, the spread of the values for Al
was so large that no statistically significant effects could be
established. Contamination appears also to have been a problem
with Zn analyses and, to a lesser extent, with Ba and Fe.
REJECTION OF OUTLIERS
The analytical data supplied by the ten participating labora-
tories were processed by the IMVS program to remove spurious results.
The processing of the data involved three steps. First,
the Youden's Laboratory Ranking Procedure (2) was used to detect
and reject data having a large systematic error associated with a
particular laboratory. Next, all zero, negative and non-detected
data were rejected. Subsequently, the Thompson outlier test (6)
was used to reject individual outliers.
Tables 11 through 16 tabulate the number of retained data
points for each water type. The maximum number of retained data
points for a Youden pair ampule is 10, achievable when all the data
submitted by the ten participating laboratories for that ampule are
deemed representative. Data rejection was not done indiscriminately,
but was done in a manner which would remove only those data that
would create non-representative summary statistics and not those
data that are a result of some artifact of the analytical method.
All rejected data are identified in Appendix C Raw Data tables by
the symbol "*".
-72-
-------
TABLE 11. NUMBER OF RETAINED DATA POINTS FOR LAB PURE WATER
Element
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Aq
Tl
V
Zn
Youden
Pair
11
7
7
7
8
5
6
9
9
9
9
7
6
10
8
6
6
7
4
Youden
Pair
12
7
7
8
8
5
6
8
9
9
8
7
5
10
9
6
7
8
4
Youden
Pair
13
7
8
8
8
9
10
9
9
8
8
7
9
9
9
8
7
8
8
Youden
Pair
14
7
7
7
8
8
10
9
9
9
8
7
9
10
9
8
7
8
7
Youden
Pair
15
7
8
8
8
8
10
9
9
9
9
8
9
10
9
8
7
8
8
Youden
Pair
#6
7
8
8
6
9
10
9
9
8
9
7
9
10
8
8
7
8
8
%
Rejected
30
25
23
23
27
13
12
10
13
15
28
22
2
13
27
32
22
35
-73-
-------
TABLE 12. NUMBER OF RETAINED DATA POINTS FOR DRINKING WATER
Element
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Ag
Tl
V
Zn
Youden
Pair
#1
8
5
8
7
7
7
8
9
8
8
9
5
7
9
6
8
10
4
Youden
Pair
#2
8
5
7
7
4
8
9
9
8
7
8
6
6
9
5
7
10
4
Youden
Pair
#3
8
6
7
8
8
8
8
9
7
10
9
7
7
9
9
8
9
5
Youden
Pair
#4
8
6
7
8
8
7
9
10
8
10
9
8
7
9
9
8
9
5
Youden
Pair
#5
8
6
8
8
7
7
8
9
9
9
9
8
7
9
9
8
9
7
Youden
Pair
#6
8
6
8
8
8
8
8
10
9
8
9
7
7
9
9
8
9
7
%
Rejected
20
43
25
23
30
25
17
7
18
13
12
32
32
10
22
22
7
47
-74-
-------
TABLE 13. NUMBER OF RETAINED DATA POINTS FOR SURFACE WATER
Element
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Ag
Tl
V
Zn
Youden
Pair
#1
7
8
9
8
6
6
9
9
8
5
8
3
9
8
7
7
7
3
Youden
Pair
12
8
6
8
8
4
8
9
9
9
7
7
0
8
8
8
9
8
4
Youden
Pair
#3
8
8
9
9
8
8
8
9
9
8
8
4
9
8
9
9
8
3
Youden
Pair
#4
4
8
9
9
8
8
9
9
9
8
8
6
9
8
9
9
8
4
Youden
Pair
15
7
8
8
9
9
8
9
9
9
9
8
7
9
8
10
8
9
5
Youden
Pair
#6
6
7
9
9
8
8
9
9
9
7
8
5 .
8
8
9
9
8
3
%
Rejected
33
25
13
13
28
23
12
10
12
27
22
58
13
20
13
15
20
63
-75-
-------
TABLE 14. NUMBER OF RETAINED DATA POINTS FOR EFFLUENT 1
Element
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Ag
Tl
V
Zn
Youden
Pair
#1
7
6
8
9
7
4
8
8
9
10
7
9
7
5
6
7
7
7
Youden
Pair
#2
7
7
8
8
6
5
8
8
9
9
7
9
6
7
8
7
7
6
Youden
Pair
#3
8
8
8
9
7
8
8
8
8
9
9
9
6
9
8
7
7
8
Youden
Pair
#4
7
8
8
9
8
8
8
7
9
10
9
9
6
9
8
7
7
8
Youden
Pair
#5
8
7
8
9
8
8
9
8
9
10
9
9
6
9
8
7
7
8
Youden
Pair
16
8
8
8
9
8
8
8
8
8
10
8
9
7
8
8
7
7
8
%
Rejected
25
27
20
12
27
32
18
22
13
3
18
10
37
22
23
30
30
25
-76-
-------
TABLE 15. NUMBER OF RETAINED DATA POINTS FOR EFFLUENT 2
Element
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Ag
Tl
V
Zn
Youden
Pair
#1
8
7
7
8
5
7 .
7
8
7
8
8
9
9
7
6
6
8
6
Youden
Pair
#2
8
7
7
7
4
8
8
8
8
6
8
8
9
7
7
7
9
4
Youden
Pair
#3
7
8
8
8
7
9
8
8
8
8
7
8
9
7
8
7
8
7
Youden
Pair
#4"
8
7
8
9
6
9
8
7
8
7
8
9
9
8
7
7
8
8
Youden
Pair
#5
6
8
8
9
7
8
8
8
8
9
8
9
9
8
8
6
9
8
Youden
Pair
#6
8
8
8
9
6
9
9
8
8
9
8
8
8
8
8
7
8
6
%
Rejected
25
25
23
17
42
17
20
22
22
22
22
15
12
25
27
33
17
35
-77-
-------
TABLE 16. NUMBER OF RETAINED DATA POINTS FOR EFFLUENT 3
Element
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Aq
Tl
V
Zn
Youden
Pair
#1
8
4
7
7
5
8
6
8
6
8
7
3
6
5
8
7
9
4
Youden
Pair
#2
8
6
6
7
3
8
6
7
4
9
7
4
4
6
8
7
7
3
Youden
Pair
#3
9
8
9
6
8
10
7
8
9
9
7
7
8
8
8
7
9
6
Youden
Pair
#4
8
8
9
7
8
10
7
6
9
9
7
8
7
8
7
7
8
5
Youden
Pair
#5
7
8
9
7
9
10
7
7
9
9
7
9
7
8
8
7
9
4
Youden
Pair
#6
8
8
9
5
9
10
7
6
9
9
7
9
7
7
8
7
9
7
%
Rejected
20
30
18
35
30
7
33
30
23
12
30
33
35
30
22
30
15
62
-78-
-------
For the entire project, the IMVS program rejected 23% of the
data. The percentage of rejected data did not vary significantly
by water type. The lowest rejection was for laboratory-pure water
for which 21% of the data was rejected; the highest, 27%, was for
effluent 3.
For a single metal/water type, 63% of the data for zinc in
surface water and 62% of the data for zinc in effluent 3 were
rejected.
Data rejection by laboratory varied from 12% to 36% rejected
and is presented in Table 17.
STATISTICAL SUMMARIES
Subsequent to the rejection of outlier and non-useable data,
the IMVS program calculated several summary statistics on the
remaining data base. These summary statistics are mean recovery,
percent relative error, overall (i.e., precision associated with
all laboratories) standard deviation, percent relative pverall
standard deviation, single-analyst standard deviation and percent
relative single-analyst standard deviation.
To facilitate review and comparison of the summary statistics,
percent relative error and percent overall relative standard
deviation data have been compiled by water type in Tables 18-23.
Included in these tables are mean values averaged by Youden pair
concentration (increasing concentration from 1 to 6) and by element.
A review of these tables yields the range of the accuracy (percent
relative error) (0.13%-17,720%) and overall precision (overall
percent relative standard deviation) (0.55%-171%) values for all the
participating laboratories when analyzing a certain concentration
of a given element in a given water type. Further review of these
tables also indicates which elemental analyses in which water types
yield poor accuracy and precision.
-79-
-------
TABLE 17. PERCENTAGE OF DATA REJECTED FOR EACH LABORATORY
Laboratory Number % Rejected
1 26
2 . 17
3 24
4 14
5 36
6 30
7 23
8 21
9 24
10 . 12
-80-
-------
TABLE 18. ACCURACY AND PRECISION SUMMARY TABLE FOR LAB PURE WATER
Element
Ave
by
Ave
by
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Ag
Tl
V
Zn
%Error-Acc
»RSD-Prec
%Etroc-Acc
%RSD-Prec
%Error-Acc
»RSD-Prec
%Error-Acc
»RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
»RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
»RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
»RSD-Prec
%Error-Acc
%RSD-Prec
%Er roc-Ace
»RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
*RSD-Prec
%Error-Acc
Youden Pair
%RSD-Prec
Youden Pair
Youden
Pair
»1
114.13
52.47
-41.56
44.22
-10.94
15.61
33.37
27.47
-15.82
15.86
13.19
18.45
-3.13
23.23
-10.38
15.68
-5.61
38.7
146.44
92.3
-7.43
23.85
321.4
80.25
-18.36
35.22
10.65
16.92
34.43
46.01
-9.76
11.13
-15.35
14.1
455.04
51.52
55.01
34.61
Youden
Pair
12
24.99
57.03
-43.31
53
5.88
44.13
36.21
35.05
-5.56
77.69
12.94
20.05
-1.71
8.72
-4.67
13.45
-4.72
29.17
27.68
61.07
-6.28
21.52
275.51
62.54
-8.01
27.93
7.64
44.53
24.37
37.31
-16.18
13.52
1.32
20.51
209.00
68.63
20.72
38.66
Youden
Pair
13
42.53
57.87
-25.88
36.93
-10.26
5.87
1.21
31.81
-16.35
18.36
-7.74
21.54
-12.47
25.44
-10.43
24.19
-1.43
-4.3
71.36
60.08
-8.14
16.39
28.53
47.01
-15.5
12.5
1.09
IP. 62
-2.09
11.74
-10.77
8.1
-28.4
48.3
423.97
82.76
23.30
26.62
Youden
Pair
14
11.83
46.58
-28.39
19.2
-5.25
8.65
.97
27.71
-10.08
17.52
-9.14
18.43
-7.7
13.2
-11.88
24.18
-4.86
20.07
36.14
15.44
-15.02
33.58
34.23
47.40
-14.79
20.11
1.39
14.6
-4.74
16.49
-12.82
12.63
-22.29
47.99
189.16
141.81
7.05
30.31
Youden
Pair
*5
-11.52
50.51
-14.27
36.46
-5.86
23.56
-5.24
18.85
-4.17
17.22
-.45
33.4
.61
7.65
-12.03
21.25
-6.66
53.96
4.92
14.15
-25.23
39.94
-13.17
54.88
3.48
27.75
-3.01
19.8
-11.57
32.34
-12.42
12.39
-15.3
43.05
172.57
95.96
2.26
33.5
Youden
Pair
*6
-3.
36
-25
46
-4.
11
-10
9.
12
20
15
.98
.03
.46
12
.7
.53
42
.59
.68
.98
29.43
-5.
14
-10
26
-3.
10
51
39
-13
19
-1.
36
-5.
35
-4.
18
10
21
-10
10
-17
37
84
82
15
.32
.76
.2
61
.14
.34
.57
.68
.32
66
.96
79
.16
27
.21
.98
.05
.48
.84
.05
.05
.91
.07
Average
29
50
-29
39
-5.
18
9.
25
-6.
27
1.
23
-4.
15
-10
20
-4.
24
56
47
-12
25
.8
.24
.74
.37
09
.25
33
.05
56
..88
63
.55
92
.42
.02
.82
48
.62
.31
.1
.63
.76
107.47
54.84
-9.
26
2.
20
8.
27
-12
11
-16
35
82
.44
24
.78
56
.49
.07
.43
.17
.16
255.78
87.12
2.54
28
.08
-81-
-------
TABLE 19. ACCURACY AND PRECISION SUMMARY TABLE FOR DRINKING WATER
Element
Ave
by
Ave
by
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Ag
Tl
V
Zn
*Error-Acc
%RSD-Prec
%Error-Acc
»RSD-Prec
»Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
*Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
»RSD-Prec
*Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
»Error-Acc
»RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%PSD-Prec
%Error-Acc
Youden Pair
%RSD-Prec
Youden Pair
Youden
Pair
11
132.59
29.88
24.18
15.53
.71
17.95
58.35
16.61
.36
30.35
46.62
35.05
9.95
39.52
-14.22
22.89
72.76
69.68
130.23
75.57
-7.57
42.32
259.06
49.85
-23.83
27.73
25.44
40.42
223.44
66.59
-18.33
14.76
-.91
31.06
3603.36
82.66
251.228
39.35
Youden
Pair
»2
152.61
61.71
41.1
40.06
-3.08
33.18
50.66
28.43
-21.47
29.92
18.84
46.17
4.44
51.73
-.82
32.5
-16.6
43.14
-3.12
63.45
-12.84
48.26
277.93
76.15
-7.4
46.72
-5.4
45.71
36.04
24.9
-19.4
12.3
-12.98
26.47
726.67
124.44
68.80
46.40
Youden
Pair
*3
64.47
29.35
-19.28
13.67
-10.89
10.18
4.4
38.94
-.38
21.95
6.46
22.92
-6.24
13.58
3.58
17.96
-20.65
36.98
12.16
37.35
-15.88
26.65
-6.29
52.77
-26.57
33.48
3.82
19.79
-.37
17.29
-8.46
20.82
-16.53
24.24
409.02
89.88
20.52
29.32
Youden
Pair
14
64
55
-9.
11
-7.
12
-1.
38
-1.
12
-2.
21
5.
24
1.
15
-11
49
38
54
-11
16
8.
46
-25
37
4.
20
-10
23
-4.
17
-2.
20
.69
.86
2
.95
77
.21
67
.76
96
.23
44
.23
62
.21
94
.19
.34
.8
.53
.84
.6
33
.58
.06
.96
29
.15
.87
.55
8
.15
38
.28
145.93
85.93
10
31
.01
.29
Youden
Pair
»5
56
24.61
-15.63
9.11
-4.22
17.06
10.22
34.68
.13
16.64
-15.35
40.19
3.5
10.96
-11.06
14.23
16.64
36.15
19.05
19.93
-14.04
23.28
4.90
34.09
-11.44
16.25
6.61
16.11
2.99
17.83
-11.27
29.34
4.01
20.82
306.17
134.63
19.28
28.65
Youden
Pair
*6
29.17
29.71
-15.55
41.71
-5.75
16.27
8.3
26.91
-2.48
14.42
-2.44
22.6
-.46
8.37
-24.13
46.93
1.77
21.33
10.7
25.19
-15.48
28.55
6.78
46.17
-15
21.35
10.66
17.1
1.57
15.97
-19.84
31.49
.64
17.41
315.68
103.00
15.79
29.69
Average
83
38
.25
.52
.93
22
-5.
17
21
30
-4.
20
8.
31
2.
24
-7.
24
12
42
34
46
-12
30
91
50
-18
30
7.
26
42
27
-13
20
-4.
23
16
.8
.71
.72
79
.91
61
.36
8
.72
45
.95
.62
.71
.63
.94
.94
.79
.94
.21
.58
57
.54
.13
.68
.68
.97
69
.38
917.80
103.42
-82-
-------
TABLE 20. ACCURACY AND PRECISION SUMMARY TABLE FOR SURFACE WATER
Element
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Ag
Tl
V
Zn
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
»RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
»Error-Acc
%RSD-Prec
%Error-Acc
*RSD-Prec
»Error-Acc
%RSD-Prec
»Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
Ave %Error-Acc
by Youden Pair
Ave
by
SRSD-Prec
Youden Pair
Youden
Pair
#1
306.63
103.19
-19.32
22.61
-26.43
41.8
44.68
29.72
11.02
18.83
-1.1
48.18
-.49
22.25
-4.16
14.4
10.97
26
367.3
44.56
-7.36
35.22
962.64
32.87
.04
52.95
-.83
37.32
87.44
63.51
-26.16
24.51
-10.78
15.11
602.74
102.01
127.60
40.83
Youden
Pair
12
344.4
117.3
-34.12
36.46
-17.2
46.22
44.4
24.74
5.24
10.2
92.79
97.36
-10.28
26.9
1.53
20.63
-16.76
36.1
335.58
77.63
-23.85
36.13
UNO
UNO
-21.66
51.56
-9.29
28.9
992.43
171
-25.55
23.19
-13.33
14.02
2350.00
114.23
234.96
48.96
Youden
Pair
*3
70.38
84.05
-24.32
23.25
-8.62
22.15
1.85
52.77
-6.21
18.76
-10.19
25.65
-13.64
27.23
-5.26
15.27
1.07
24.04
41.42
48.61
-16.85
17.34
47.00
44.07
-19.25
29.62
-1.19
15.97
-8.84
26.52
-16.27
19.91
-20.02
12.68
157.52
134.65
9.37
35.69
Youden
Pair
#4
-48.45
80.3
-29
29.13
-7.1
17.53
2.77
14.53
3.4
17.93
-8.22
24.13
-10.27
51.44
-8.44
13.12
-6.51
22.53
62
37.55
-2.22
29.97
6.71
57.27
-23.1
22.49
-10.76
27.3
-16.71
33.79
-20.61
25.77
3.3
21.83
313.27
103.16
11.12
34.98
Youden
Pair
IS
-1.
43
-20
23
-10
12
9.
27
-16
46
-6.
23
-7.
11
-6.
15
4.
14
16
41
-14
13
-5.
42
-11
19
4.
12
-20
32
-21
20
-6.
13
71
.85
.19
.02
.1
22
.83
.18
.83
05
.88
78
.85
64
.61
82
.41
.73
.2
.67
.1
98
.35
.97
.22
27
.43
.71
.03
.18
.63
18
.74
58.99
103.39
-3.
28
06
.75
Youden
Pair
*6
12
46
.91
.77
-7.71
.55
-14
13
3.
24
-8.
17
16
42
-2.
14
-7.
26
2.
18
44
47
-5.
20
11
37
-16
9.
4.
16
-8.
19
-17
23
-2.
12
11
78
0.
26
.43
.78
72
.51
77
.52
.67
.63
12
.27
54
.58
63
.7
.55
.57
98
.43
.02
.63
.52
82
93
.64
42
.64
.93
.02
28
.8
.88
.89
92
.21
Average
114.02
79.24
-22.41
22.53
-13.96
25.59
' 17.77
29.01
-1.91
21.67
13.98
43.63
-7.43.
25.65
-5.08
17.6
-.63
23.63
144.59
59.52
-11.82
25.36
204.28
42.84
-15.41
30.94
-2.14
23.09
170.86
57.74
-21.28
22.83
-8.21
15.03
582.40
106.06
-83-
-------
TABLE 21. ACCURACY AND PRECISION SUMMARY TABLE FOR EFFLUENT 1
Element
Ave
by
Ave
by
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Aq
Tl
V
Zn
%Error-Acc
%RSD-Prec
»Error-Acc
%RSD-Prec
»Error-Acc
*RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%PSD-Prec
%Error-Acc
%RSr-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%PSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
»RSD-Prec
»Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
Youden Pair
%RSD-Prec
Youden Pair
Youden
Pair
11
-12
49
-19
61
.43
.11
.05
.03
126.17
27.6
93
49
2.
60
63
35
9.
58
4.
21
-5.
38
-9.
36
-8.
16
-11
47
-10
41
-41
24
2.
20
-33
33
-4
29
-43
S3
.15
.86
41
.85
.22
.37
49
.8
23
.18
29
.62
85
.34
78
.82
.18
.7
.09
.75
.72
.7
4
.3
.11
.11
.53
.47
.78
.21
5.62
40
.87
Youden
Pair
»2
-11.4
42.02
-28.57
62.42
74.97
42.72
128.1
61.4
22.02
50.25
33.69
71.51
-20.59
57.24
5.54
13.24
-5.14
29.02
-9.52
17.53
7.28
26.55
-8.32
48.1
22.62
18.59
29.43
64.35
-7.71
14.94
-37.07
24.95
2.98
21.24
25.13
61.91
12.41
40.44
Youden
Pair
13
-4.87
46.25
-10.66
41.99
35.89
10.42
47.98
33.1
-9.4
23.3
-19.34
36.88
-12.58
13.02
-9.54
22.67
-1.56
4.49
-6.15
25.52
-27.04
29.24
-1.45
19.94
-19.37
27.78
-14.25
21.99
-1.86
18.16
-28.4
20.75
-7.9
26.27
-33.76
71.63
-6.9
27.41
Youden
Pair
*4
3.04
42.29
-13.58
21.61
41.54
12.93
44.74
1<= 32
r."3
34.32
-21.05
37.55
-6.9
19.53
-3.4
14.86
-4.89
20.1
38.34
77.62
-19.76
23.39
-14.8
37.64
-25.94
16.67
-15.07
23.23
.91
18.19
-19.38
35.95
11.33
30.28
-16.14
74.1
-.86
32.03
Youden
Pair
»5
4.
27
-16
7.
10
25
18
27
-9.
25
-15
29
-16
43
-15
24
-6.
53
17
.76
.89
42
.96
.49
.85
.16
09
.16
.07
.86
.8
.47
.01
.89
73
.98
-.27
12.93
-12
20
-2.
. 18
-38
10
-10
24
-11
35
-23
34
5.
18
-46
80
-10
28
.07
.41
87
.06
.83
.78
.94
.57
.83
.01
.78
.7
16
.75
.92
.7
.44
.95
Youden
Pair
16
11.61
20.64
-10.27
21.09
9.72
22.72
-2.45
48.56
-3.04
20.16
-22
27.37
-9.12
18.82
-10.35
14.88
-3.63
10.15
3.45
25.54
-8.54
21.87
-4.29
18.33
-32.66
21.78
-15.21
12.11
-10.35
23.2
-28.57
28.43
5.91
24.38
-38.95
70.21
-9.37
25.01
Average
-1.64
38.01
-16.5
. 35.92
49.87
23.64
55.06
42.73
1.4
35.67
3.24
39.75
-9.41
35.14
-4.75
18.62
-4.54
26.06
2.66
32.58
-11.48
23.04
-7.15
31.62
-17.37
22.89
-11.29
28.49
-4.74
21.63
-28.38
29.64
2.15
25.06
-25.73
73.62
-84-
-------
TABLE 22. ACCURACY AND PRECISION SUMMARY TABLE FOR EFFLUENT 2
Element
Ave
by
Ave
by
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Aa
Tl
V
Zn
%Error-Acc
»RSD-Prec
%Error-Acc
%RSD-Prec
*Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Er rot-Ace
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
»RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
»Error-Acc
%RSD-Prec
%Error-Acc
Youden Pair
%RSD-Prec
Youden Pair
Youden
Pair
11
4.06
40.67
19.21
80.1
-10.53
39.07
56.85
37.87
-3.97
22.48
18.23
32.59
3.63
38.98
5.69
19.91
-25.66
12.99
9.67
21.54
-25
47.68
-37.27
27.36
-26.93
42.98
1.85
50.58
-57.53
73.38
-45.35
41.36
-12.8
6.02
49.61
58.56
-4.23
38.56
Youden
Pair
. »2
14.65
39.13
38.76
98.77
-13.09
66.21
58.48
19.5
19.42
61.3
-4.06
38.76
7.36
32.13
-13.5
21.75
-17.53
15.66
9.42
21.52
-39.18
39.48
-16.84
19.52
-36.4
63.36
-30.43
55.07
-42.32
67.25
-50.35
42.66
-22.15
43.4
1.22
72.6
-7.58
45.44
Youden
Pair
13
-.75
27.46
-16.92
30.89
-12.42
23.85
8.34
44.13
5.26
15.73
-9.76
31.74
1.53
17.62
-4.25
14.86
-17.79
25.02
4.14
15.93
-17.52
16.64
-29.52
9.12
-22.34
22.6
15.05
17.02
-46.53
63.2
-37.55
7.93
-16.93
17.91
113.27
95.3
-4.7
27.6
Youden
Pair
*4
-5.51
28.38
-31.86
8.52
-7.74
17.62
6.55
34.79
5.4
9.91
-21.68
23.74
-16.86
12.73
-5.19
9.55
-7.06
14.64
-.78
8.59
-10.48
17.29
-41.26
57.38
-22.61
25.1
2.59
20.18
-55.14
69.02
-33.49
18.13
-6.78
14.3
-4.08
46.49
-14.22
24.24
Youden
Pair
15
-5.
9.
-18
23
-12
14
-5.
64
10
14
-16
24
-1.
IS
-3.
17
89
53
.7
.13
.11
.24
65
.13
.23
.45
.66
.51
04
.68
99
.22
-.36
13.65
-1.
22
-17
30
-16
40
-3.
34
8.
21
-54
67
-44
12
-7.
24
4.
66
-10
28
76
.23
.65
.28
.93
.51
95
.44
95
.74
.91
.04
.59
.13
45
.8
79
.17
.42
.66
Youden
Pair
*6
-13
19
-18
16
4.
22
-1.
42
12
12
-15
16
.94
.99
.26
.52
23
.17
83
.76
.69
.21
.69
.41
-.19
16.56
-4.
11
-2.
8.
7.
31
-19
26
-10
12
-16
21
5.
23
-51
68
-36
25
-8.
9
-26
85
-10
26
16
.57
85
07
76
.91
.6
.84
.01
.75
.38
.63
27
.1
.27
.11
.81
.96
2
.55
.96
.87
.19
Average
-1.23
27.52
-4.62
42.98
-8.61
30.52
20.45
40.53
8.17
22.68
-8.26
27.95
-.92
22.28
-4.23
15.81
-11.87
15
4.74
20.28
-21.57
29.7
-25.3
27.77
-21.43
35.01
.54
31.28
-51.28
68
-41.37
24.69
-12.38
19.23
23.04
70.84
-85-
-------
TABLE 23. ACCURACY AND PRECISION SUMMARY TABLE FOR EFFLUENT 3
Element
Ave
by
Ave
by
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Aa
Tl
V
Zn
%Error-Acc
%RSD-Prec
%Error-Acc
*RSD-Prec
%Error-Acc
%PSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
»RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
»RSD-Prec
%Error-Acc
»RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
tRSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
%RSD-Prec
%Error-Acc
Youden Pair
%RSD-Pcec
Youden Pair
Youden
Pair
11
118.14
56.49
-22.38
65.12
-22.76
43
63.6
32.99
-13.5
63.25
24.43
' 62.31
-8.81
23.31
-8.02
19.64
-3.63
87.33
'156.5
75.33
-15.26
57.24
192.40
3.46
-61.07
100.9
-22.41
69.83
7.09
23.01
-35.67
24.27
-16.74
19.1
4773.29
90.57
283.61
50.95
Youden
Pair
12
123.75
50.36
-51.78
31.53
-9.68
43.8
17.37
48.83
-12.95
21.91
1.22
28.7
-22.48
28.98
-20.96
21.16
-26.71
78.39
139.2
84.53
-21.25
53.38
699.76
114.41
-42.76
80.8
-46.33
84.83
17.09
30.06
-34.46
22.92
-13.24
4.54
17719.62
137.18
1023.09
53.68
Youden
Pair
*3
35.72
54.73
-49.98
47.84
-19.53
25.2
-52.24
44.72
-19.16
17.61
.76
24.49
-9.25
29.55
-14.51
10.41
-21.89
55.4
6.69
30.89
-18.65
33.4
9.71.
45.11
-14.93
38.53
-27.93
58.42
12.52
35.31
-18.4
17.77
-6.39
14.45
570.60
90.56
20.18
37.47
Youden
Pair
14
42
44
-36
29
-11
20
-43
70
-5.
19
-7.
35
-2.
30
-12
9.
-27
32
4.
36
-9.
35
-15
25
-20
15
-22
55
-5.
33
-17
14
-3.
8.
.83
.43
.53
.08
.54
.16
.69
.87
74
.43
31
.8
13
.74
.55
93
.35
.2
33
.98
18
.88
.37
.99
.37
.93
.47
55
.35
.26
.87
77
09
1805.08
90.44
89
33
.53
.84
Youden
Pair
15
27.14
8.76
-40.22
24.55
-11.75
15.44
-43.18
60.21
-4.24
29.25
-2.22
29.96
-14.58
20.74
-23.91
27.89
-16.72
21.21
37.55
44.34
-41.5
24.54
-12.28
34.08
-22.23
14.99
-15.1
27.89
-21.04
41.51
-22.61
20.14
-5.78
18.64
109.59
81.47
-6.83
30.30
Youden
Pair
16
56.54
44.28
-28.08
32.51
-10.34
14.57
-60.14
7.11
-8.33
15.38
1.95
29.28
-6.42
9.27
-16.82
13.49
-6.89
29.08
32.56
47.87
-38.1
52.29
-16.86
26.66
-22.31
13.8
-7.96
29.97
-41.35
26.85
-23.62
23.4
-5.53
22.23
503.76
124.69
16.78
31.26
Average
67.35
43.17
-38.16
38.43
-14.26
27.02
-19.71
44.12
-10.65
27.8
3.13
35.09
-10.61
23.76
-16.12
17.08
-17.19
50.6
62.8
53.32
-23.99
42.78
142.89
41.62
-30.55
44.06
-23.77
54.4*
-5.2
31.68
-25.33
20.56
-8.57
14.5
4246.99
102.48
-86-
-------
REGRESSION EQUATIONS
The IMVS code regresses overall precision and single analyst
precision against the mean recovery of a particular element in a
given water type and regresses accuracy against the true concentra-
tion. The resulting output (refer to Section 2, Table 1) includes
the slopes and the intercepts of the straight lines which best
approximate the functional relationship between the values.
For laboratory-pure water (Table 18) which contained minimal
background levels of the 18 metals, the average percent relative
error decreases as spike concentrations increase. A larger average
relative error exists for the low Youden pairs (1 and 2) than
exists for the high concentration pairs (5 and 6). This trend is
as expected; i.e., analyses at or near the detection limit are less
accurate. However, for certain specific elements (Ag, Cd, Ni) the
relative error is lowest for the medium concentration spikes,
possibly indicating that the high Youden pairs were analyzed above
the upper limit of the linear range. The corresponding trend
(dependence on concentration) for precision is less pronounced but
for all waters the average percent relative standard deviation is
highest for the low Youden pairs and generally lowest for the high
Youden pairs.
EFFECTS OF WATER TYPE
The multiplicative model (Equation 10) discussed in Section 4
was fitted separately to the data for each element to test for
effects due to water type. The detailed analysis of variance
tables and the 95% confidence limits for the slopes and intercepts
are presented with the raw data in Appendix C. The elements
showing statistically significant differences by water type
are summarized in Table 24.
-87-
-------
Table 24. EFFECT OF WATER TYPE
Element
As
Be
Cu
Fe
i
00
00
' Mn
Ni
Se
Ag
Tl
Water
Type
Effluent
Effluent
Surface
Effluent
Surface
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Surface
Effluent
Observed
F-Value
2
3
2
2
1
2
3
1
3
2
2
14
14
3
7
6
9
7
13
13
6
6
15
6
6
.78
.78
.02
.89
.74
.72
.60
.35
.35
.33
.33
.17
.00
.88
F Test Significant
Statistically Effect
Significant Established
at the at the 95% CI
P(
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F>F0bs)
.0000
.0000
.0207
.0007
.0001
.0001
.0009
.0000
.0000
.0000
.0000
.0000
.0002
.0009
95% Level
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
Slope
yes
no
yes
yes
. yes
yes
yes
yes
yes
no
yes
no
no
no
Intercept
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
Practical
Importance
Established
yes
yes
yes
no
no
no
no
yes
yes
yes
yes
yes
yes
yes
Zn
Effluent 3
14.73
0.0000
yes
yes
yes
no
-------
In order to determine if any of the statistically signifi-
cant effects were of practical importance, the summary statistics
and raw data were reviewed. A discussion of the summary statis-
tics by element follows:
Arsenic - The mean recoveries for effluents 2 and 3 are lower
than for lab pure water or effluent 1. In fact, the percent
relative errors for lab pure water and effluent 1 are positive
(high recoveries) while the percent relative errors for
effluents 2 and 3 are negative (low recoveries). The overall
standard deviations and single-analyst standard deviations
show no clear differences between water type indicating no
practical difference in precision. The accuracy, however,
does appear to be matrix dependent.
Beryllium - The 95% confidence limit for the slope of the
regression line for surface water does not contain zero. This
indicates a statistically significant difference that may be
concentration-dependent. An examination of the raw data for
the low Youden Pair for lab pure water and surface water shows
that 50% of the data points were rejected and that 17 out of
40 of these were reported as "less than" values implying that
the concentration dependent effect may be that the low spikes
were too close to the method detection limit. The method
detection limit was not achieved in 17 instances and is most
likely too optimistic. The overall standard deviation and
single-analyst standard deviation for all six water types were
generally large and were larger for the low spike pairs.
Copper - Effluent 2 had a statistically significant effect
established by the confidence limit for the slope again
indicating the possibility of a concentration dependent effect.
The background concentration of copper in effluent 2 (from the
-89-
-------
homogeneity test data) was approximately 200 ug/L which is
near the upper limit of the linear range of the method.
Consequently, spiking levels for effluent 2 were dramatically
different from levels for all other waters and multiple
dilutions would have been necessary for the high spikes.
The single-analyst relative deviation for the high Youden
pair spikes however show better precision (3.5%) for efflu-
ent 2 than for the lab pure water (12.9%) and the percent
relative error for the high pair indicates better accuracy
for effluent 2 than for the spiked lab pure water. The
percent relative error and single-analyst percent relative
standard deviations are reversed for the low spikes i.e.
analysis of the lab pure water was more accurate and more
precise than for effluent 2 due to the high copper back-
ground concentration in effluent 2. This most likely
indicates no practical importance to the statistical dif-
ference for effluent 2.
Iron - The surface waters and effluent 2 both had signifi-
cant slope and intercept differences from lab pure water.
Given the range of values for the percent relative standard
deviation (8.59% to 92.3%) the percent relative error
(-25.2% to +367%) and single-analyst errors (5.5% to 76.8%)
it is doubtful that any practical significance may be
attached to the differences. Although there is insufficient
evidence to support any conclusion, random contamination of
the samples is highly possible for an analyte as ubiquitous
as iron.
Manganese - The data for manganese exhibited several
unusual effects. The recoveries for the low Youden pairs
for lab pure water, surface water, drinking water, and
-90-
-------
effluent 3 were extremely high and 60% of these data points
were rejected as outliers. These waters contained no
detectable background levels of manganese and consequently
the low spikes were near the reported method detection
limit. The accuracy and precision as well as the high data
rejection all suggest that the published detection limit is
too low.
In addition, effluent 1 had significant slope and intercept
differences from lab pure water. An examination of the raw
.data and summary statistics reveals that for one low spike
of the lab pure water the percent relative error was 135.7%
while for all other spikes the percent relative error was
below 15%. The raw data seem to indicate that the concen-
tration in the spiking solution was in error by a factor of
two or that the amount of solution spiked was in error
(i.e.,-an error in the spiking instructions). However, all
ampules analyzed during the homogeneity study gave the
correct concentration and the ampule contained four
other elements which would have also exhibited a factor
of two error if the spiking instructions were at fault.
In addition, the same ampule was used to spike the effluent
with a percent relative error of 11.18%. The ampules for
the Youden pair in question are designated 4a and 4b in
Table 9 with 4a being the "incorrect" concentration. It
is doubtful that the statistically significant difference
has any practical importance.
Nickel - Both effluents 2 and 3 exhibited low recovery and
extremely high percent relative standard deviations partic-
ularly at the low spike levels. For effluent 3 the low
spike levels were less than the background concentration,
50% of the data was rejected, and poor precision is not
-91-
-------
surprising. All other spike levels are well above the
background concentrations and the statistically significant
differences are probably of practical importance.
Selenium - Both effluents 1 and 3 exhibited consistently
low recoveries and poor precision, therefore the statis-
tically significant differences are of practical importance.
Silver - Effluent 2 was a silver containing photographic
industry waste. The average recoveries were only 50% at all
spike levels and the percent relative standard deviations were
above 60%. The method did not work well for this matrix. In
fact, in Tables 6 and 7 where the homogeneity data and ICAP
data are summarized, the furnace AA values for the silver
content of effluent 2 ranged from 4.6 to 7.6 ug/L while the
ICAP value was 62 ug/L.
Thallium - Recoveries of thallium were consistently low for
all water types at all spike levels. Surface water and
effluent 2 had significant differences in intercept, indica-
tive of a concentration independent effect of practical
importance. Observation of the raw data reveals that the
method is also subject to systematic error. Laboratories 3
and 6 had over 70% of their data points rejected as outliers.
Zinc - Effluent 3 showed a statistically significant differ-
ence in both slope and intercept when compared to lab pure
water. However, the scatter in the data is so large at the
spike levels used (ca. 0.5, 5, and 15 ug/L) it is doubtful
that there is any practical importance to the difference.
The percent relative errors for both lab pure water and
effluent 3 were all positive errors and ranged from 84.8%
to 17,719%. Less than half the data was retained for the
-92-
-------
low spike pairs. The data strongly suggests environmental
contamination of the samples during digestion or analysis.
For eight of the elements, no statistically significant
differences from laboratory-pure water were found for the other
waters or effluents. It should not be assumed that the furnace
methods worked well for these elements. In fact there are four
reasons for finding no significant differences:
1. There are none - the methods work well for all matrices
for a particular element.
2. There were universally low recoveries for all matrices for
a particular element.
3. There were universally high recoveries for all matrices
for a particular element.
4. The method worked so badly or was subject to such large
random error that, statistically, nothing could be proven.
These eight elements are discussed below.
Aluminum - All data were erratic regardless of the matrix. In
fact more laboratory-pure water data were rejected than were
effluent 3 data. For a low spike into laboratory-pure water
(at 28 ug/L) values were reported from not detected to 4940
ug/L. Aluminum requires high atomization temperatures in
furnace AAS and is sensitive to temperature fluctuations as
well as to the condition of the graphite. These effects as
well as random contamination or carry-over made it impossible
to discern any effects related to matrix (water type) or
concentration.
-93-
-------
Antimony - All recoveries were low for this element regard-
less of water type and the overall precision rather poor
(20-40% RSD). In addition, certain laboratories had large
amounts of data rejected; i.e., experienced difficulties with
antimony analysis. All data for laboratory 5 were rejected;
over 50% of all data for laboratory 7 and over 70% of all low
spikes for laboratories 4 and 8 were rejected.
Barium - Most water types had a low data rejection for barium.
Recoveries for low spikes were generally high and for high
spikes slightly low except for effluent 3. For effluent 3 the
medium and high spikes experienced very low recoveries; in
fact so many laboratories achieved low recoveries for these
spikes that laboratories achieving the "true" value were
rejected.
Cadmium - The method worked well for cadmium in all water
types. Almost all of the rejected data were low spikes near
the method detection limit and overall, only approximately
10% of the data points were rejected. The (photographic)
effluent 2 had a slight (8%) bias toward low recoveries which
may be indicative of a slight problem with the complexing
agents which severely affected silver analyses in this water
type.
Chromium - The method generally worked well for chromium. Of
the data rejected, almost half came from laboratory 6.
Cobalt - The method generally worked well for cobalt. Data
rejection was higher for the effluents than for the surface
and drinking waters but only slightly higher.
-94-
-------
Lead - Most of the data rejected for lead were high spikes
and recoveries for high spikes were low. This may indicate
that analyses were being performed outside the linear range.
Vanadium - For the retained data, recoveries of vanadium were
slightly low. However, all rejected data points were high
values, i.e., above the "true" concentration. Only in ef-
fluent 3 (which contained significant background levels of
vanadium) were low data points rejected.
-95-
-------
REFERENCES
1. Methods for Chemical Analysis of Water and Wastes, EPA
600-4/79-020, U.S. Environmental Protection Agency,
Environmental Monitoring and Support Laboratory, Cin-
cinnati, Ohio, March 1979.
2. Youden, W.J. Statistical Techniques for Collaborative
Test, Association of Official Analytical Chemist,
Washington, D.C., 1979.
3. Outler, E.G. and McCreery, J. H., Interlaboratory Method
Validation Study: Program Documentation. battelle
Columbus Laboratories, 1982.
4. Sokal, R.R. and Rohlf, F.J., biometry, W.H. Freeman and Co.,
San Francisco, 1969.
5. Annual book of ASTM Standards, Part 31. American Society for
Testing and Material, Philadelphia, Pennsylvania.
6. Thompson, W.R., Annals of Mathematical Statistics, Vol. 6,
1935, p. 214.
7. Draper, N.R. and Smith H., Applied Regression Analysis,
2nd Edition, John Wiley and Sons, New York, 1981.
8. bishop, T., brydon, F. and Outler, E.G., battelle Report
for EPA contract 68-03-2624, Development of Statistical
Technique to Compare Analytical Methods Across Wastewaters.
-96-
-------
APPENDIX A
SAMPLE INSTRUCTIONS SUPPLIED TO LABORATORIES
NOTICE!! PLEASE READ INSTRUCTIONS BEFORE UNPACKING
The ampules contained in this package are packed in vermiculite
Please be careful when removing the vermiculite that ampule necks
are not broken.
Ampules are placed in order corresponding to that on the
packing list. It will make your life easier to remove them in
order according to the list.
A-l
-------
Packing List - Shipment consists of 3 boxes
1. 1 set instructions - Box 1
2. 2 1-qallon containers for Effluent 1 - Box 2
3. 2 1-gallon containers for Effluent 2 - Box 2
4. 2 1-gallon containers for Effluent 3 - Box 3
5. 1 10-ml of NBS SRM 1643a with certified values - Box 1
6. Spike Ampules - Box 1
Effluent
Description
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Spike
Designation
LP-l-A
LP-l-B
LP-2-A
LP-2-B
LP-3-A
LP-3-B
LP-4-A
LP-4-B
LP-5-A
LP-5-B
LP-6-A
LP-6-B
Total # Of
Ampule Identification Ampules
LP-l-A-1 to LP-l-A-5
LP-l-B-1 to LP-l-B-5
LP-2-A-1 to LP-2-A-5
LP-2-B-1 to LP-2-B-5
LP-3-A-1 to LP-3-A-2
LP=3-B-1 to LP-3-B-2
LP-4-A-1 to LP-5-A-5
LP-4-B-1 tp LP-4-B-5
LP-5-A-1 to LP-5-A-2
LP-5-B-1 to LP-5-B-2
LP-6-A-1 to LP-6-A-2
LP-6-B-1 to LP-6-B-2
5
5
5
5
2
2
5
5
2
2
2
2
42
A-2
-------
Effluent Spike Total # of
Description Designation Ampule Identification Ampules
Drinking water DW-l-A DW-l-A-1 to DW-l-A-2 2
Drinking water DW-l-B . DW-l-B-1 to DW-l-B-2 2
Drinking water DW-2-A DW-2-A-1 to DW-2-A-2 2
Drinking water DW-2-B DW-2-B-1 to DW-2-B-2 2
Drinking water . DW-3-A DW-3-A-1 to DW-3-A-2 2
Drinking water DW-3-B DW-3-B-1 to DW-3-B-2 2
12
Surface water SW-l-A SW-l-A-1 to SW-l-A-2 2
Surface water SW-l-B SW-l-B-1 tp SW-l-B-2 2
Surface water SW-2-A SW-2-A-1 to SW-2-A-2 2
Surface water SW-2-B SW-2-B-1 tp SW-2-B-2 2
Surface water SW-3-A SW-3-A-1 to SW-3-A-2 2
Surface water SW-3-B SW-3-B-1 tp SW-3-B-2 2
12
Effluent 1 El-l-A El-l-A-1 to El-l-A-3 3
Effluent 1 El-l-B El-l-B-1 to El-l-B-3 3
Effluent 1 E1-2-A E1-2-A-1 to E1-2-A-3 3
Effluent 1 E1-2-B E1-2-B-1 to E1-2-B-3 3
Effluent 1 E1-3-A E1-3-A-1 to E1-3-A-3 3
Effluent 1 E1-3-B E1-3-B-1 to E1-3-B-3 3
18
Effluent 2 E2-1-A E2-1-A-1 to E2-1-A-3 3
Effluent 2 E2-1-B E2-1-B-1 to E2-1-B-3 3
Effluent 2 E2-2-A E2-2-A-1 to E2-2-A-3 3
Effluent 2 E2-2-B E2-2-B-1 to E2-2-B-3 3
Effluent 2 E2-3-A E2-3-A-1 to E2-3-A-3 3
Effluent 2 E2-3-B E2-3-B-1 to E2-3-B-3 3
18
A-3
-------
Effluent Spike Total # of
Description Designation Ampule Identification Ampules
Effluent 3 E3-1-A E3-1-A-1 to E3-1-A-3 3
Effluent 3 E3-1-B . E3-1-B-1 to E3-1-B-3 3
Effluent 3 E3-2-A E3-2-A-1 to E3-2-A-3 3
Effluent 3 E3-2-B E3-2-B-1 to E3-2-B-3 3
Effluent 3 . E3-3-A E3-3-A-1 to E3-3-A-3 3
Effluent 3 E3-3-B E3-3-B-1 to E3-3-B-3 3
18
A-4
-------
1. INTRODUCTION
The purpose of this study is to define the precision and
accuracy of approved atomic absorption furnace procedures for
the analysis of 1.8 metals in effluent and water samples. The
18 metals of interest are aluminum (Al), antimony (Sb)f arsenic
(As), barium (Ba), beryllium (Be), cadmium (Cd), chromium
(Cr), cobalt (Co), copper (Cu), iron (Fe), lead (Pb), manganese
(Mn), nickel (Ni), selenium (Se), silver (Ag), thallium (Tl),
vanadium (V), and zinc (Zn). Samples are to be prepared and
analyzed using digestion methods and instrumental methods
specified by EPA (1979).a
Analyses are to be performed on the three effluent
samples supplied by ERGO and three water samples supplied by
subcontractor laboratories (a laboratory-pure water sample, a
finished drinking water sample, and a surface water sample).
Samples are to be prepared for analysis using spike solutions
contained in the enclosed package.
a"Methods for Chemical Analysis of Water and Wastes,"
EPA 600-4/79-020, U.S. Environmental Protection Agency,
Environmental Monitoring and Support Laboratory, Cincinnati,
Ohio, March 1979.
A-5
-------
2. ANALYTICAL PROCEDURES
2.1 Preliminary Steps
2.1.1 Verification of Package Contents
The three effluent samples and spike ampules are contained in
the enclosed package. An itemized list of the package contents is
enclosed. .Each ampule contains an identification number and a
serial number. Please verify that the package contents are correct
and complete by checking against the packing list. Also record the
serial number and identification number for each ampule.
2.1.2 Collection of lab-pure, drinking, and surface water samples
Each participating laboratory is responsible for collection of
the following types of water for use in the study:
1) laboratory-pure water (distilled or deionized water
equivalent to ASTM Type I or Type II reagent water)a
2) finished drinking water
3) surface water vulnerable to contamination
Samples should be collected using appropriate methods and
preserved immediately upon collection. Preservation methods
should be those specified by EPA.b Collect sufficient
a"Annual Book of ASTM Standards," Part 31. American
Society for Testing and Material, Philadelphia, Pennsylvania.
b"Methods for Chemical Analysis of Water and Wastes," EPA 600-4/
79-020, U.S. Environmental Protection Agency, Environmental Monitoring
and Support Laboratory, Cincinnati, Ohio, March 1979.
A-6
-------
Quantity of sample that the same material can be used for the
entire study. It is suggested that at least two gallons of
each water type be collected.
2.2 Preparation of Test Sample
Spike ampules are enclosed for each of the sample types
to be utilized in the study. The lab-pure water is to be
spiked at 6 concentration levels with each level consisting of
2 spikes prepared as a Youden Pair (similar but distinctly
different concentrations). All other sample types are to be
spiked at 3 levels with each level consisting of a Youden
Pair. Please note that each spike level may consist of more
than one ampule. A summary of the study design with appro-
priate identifying information is presented in Table 1. The
ampules which comprise each spike are identified in Table 2.
Each water and effluent sample should be dosed with spike
solutions according to the following instructions:
1. Remove a 200-ml aliquot of the sample and place
in appropriate container.
2. Remove a 10-ml aliauot from each spike ampule
specific for that spike level and add to sample.
3. Cap and shake vigorously for 30 seconds.
4. Allow sample to remain unshaken for 5 minutes, then
shake vigorously for an additional 30 seconds.
5. Store at room temperature in a dark place for 7 days.
Be sure to label sample with appropriate identification,
6. Adjust pH to <2 with 1:1 nitric acid.
7. Cap and refrigerate for 24 hours.
8. Remove aliguots for analysis.
A-7
-------
Table 1.Summary of test design and identification information
Sample Type
Lab-pure water
(LP)
Drinking water
(DW)
Surface water
(SW)
Effluent 1
(El)
Effluent 2
(E2)
Effluent 3
(E3)
Spike
Level
0
1
2
3
4
5
6
0
1
2
3
0
1
2
3
0
1
2
3
0
1
2
3
0
1
2
3
Youden Pairs
None
A and B
A and B
A and B
A and B
A and B
A and B
None
A and B
A and B
A and B
None
A and B
A and B
A and B
None
A and B
A and B
A and B
None
A and B
A and B
A and B
None
A and B
A and B
A and B
Spike Designation
Background
LP-l-A, LP-l-B
LP-2-A, LP-2-B
LP-3-A, LP-3-B
LP-4-A, LP-4-B
LP-5-A, LP-5-B
LP-6-A, LP-6-B
Background
LP-l-A, LP-l-B
LP-2-A, LP-2-B
LP-3-A, LP-3-B
Background
SW-l-A, SW-l-B
SW-2-A, SW-2-B
Sw-3-A, SW-3-B
Background
El-l-A, El-l-B
E1-2-A, E1-2-B
E1-3-A, E1-3-B
Background
E2-1-A, E2-1-B
E2-2-A, E2-2-B
E2-3-A, E2-3-B
Background
E3-1-A, E3-1-B
E3-2-A, E3-2-B
E3-3-A, E3-3-B
A-8
-------
Table 2.Summary of ampules to be used for each spike
Effluent
Description
Spike
Designation
Total # of
Ampule Identification Ampules
Lab pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Lab-pure water
Drinking water
Drinking water
Drinking water
Drinking water
Drinking water
Drinking water
LP-l-A
LP-l-B
LP-2-A
LP-2-B
LP-3-A
LP-3-B
LP-4-A
LP-4-B
LP-5-A
LP-5-B
LP-6-A
LP-6-B
DW-l-A
DW-l-B
DW-2-A
DW-2-B
DW-3-A
DW-3-B
LP-l-A-1 to LP-l-A-5
LP-l-B-1 to LP-l-B-5
LP-2-A-1 to LP-2-A-5
LP-2-B-1 to LP-2-B-5
LP-3-A-1 to LP-3-A-2
LP=3-B-1 to LP-3-B-2
LP-4-A-1 to LP-5-A-5
LP-4-B-1 tp LP-4-B-5
LP-5-A-1 to LP-5-A-2
LP-5-B-1 to LP-5-B-2
LP-6-A-1 to LP-6-A-2
LP-6-B-1 to LP-6-B-2
DW-l-A-1 to DW-l-A-2
DW-l-B-1 to DW-l-B-2
DW-2-A-1 to DW-2-A-2
DW-2-B-1 to DW-2-B-2
DW-3-A-1 to DW-3-A-2
DW-3-B-1 to DW-3-B-2
5
5
5
5
2
2
5
5
2
2
2
2
42
2
2
2
2
2
2
12
Surface water
Surface water
Surface water
Surface water
Surface water
Surface water
SW-l-A
SW-l-B
SW-2-A
SW-2-B
SW-3-A
SW-3-B
SW-l-A-1 to SW-l-A-2
SW-l-B-1 tp SW-l-B-2
SW-2-A-1 to SW-2-A-2
SW-2-B-1 tp SW-2-B-2
SW-3-A-1 to SW-3-A-2
SW-3-B-1 tp SW-3-B-2
2
2
2
2
2
2
12
A-9
-------
Table 2.Continued
Effluent
Description
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
Effluent
1
1
1
1
1
1
2
2
2
2
2
2
3
3
3
3
3
3
Spike
Designation
El-l-A
El-l-B
E1-2-A
E1-2-B
E1-3-A
E1-3-B
E2-1-A
E2-1-B
E2-2-A ..
E2-2-B
E2-3-A
E2-3-B
E3-1-A
E3-1-B
E3-2-A
E3-2-B
E3-3-A
E3-3-B
Ampule Identification
El-l-A-1
El-l-B-1
E1-2-A-1
E1-2-B-1
E1-3-A-1
E1-3-B-1
E2-1-A-1
E2-1-B-1
E2-2-A-1
E2-2-B-1
E2-3-A-1
E2-3-B-1
E3-1-A-1
E3-1-B-1
E3-2-A-1
E3-2-B-1
E3-3-A-1
E3-3-B-1
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
El-l-A-3
El-l-B-3
E1-2-A-3
E1-2-B-3
E1-3-A-3
E1-3-B-3
E2-1-A-3
E2-1-B-3
E2-2-A-3
E2-2-B-3
E2-3-A-3
E2-3-B-3
E3-1-A-3
E3-1-B-3
E3-2-A-3
E3-2-B-3
E3-3-A-3
E3-3-B-3
Total f of
Ampules
3
3
3
3
3
3
18
3
3'
3
3
3
3
18
3
3
3
3
3
3
18
A-10
-------
Table 4.Method references for graphite furnace analysis
Element Method Reference3
Al
Sb
AS
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Ag
Tl
V
Zn
202.2
204.2
206.2
208.2
210.2
213.2
218.2
219.2
220.2
236.2
239.2
243.2
249.2
270.2
272.2
279.2
286.2
289.2
aMethods for Chemical Analysis of Water and Wastes,
EPA 600-4/79-020, U.S. Environmental Protection Agency,
Environmental Monitoring and Support Laboratory, Cincinnati,
Ohio, March 1979.
A-ll
-------
Table 3.Summary of analyses to be conducted for method validation study
Analysis type
Background
Background
Background
Background
Background
Background
i
to
Spike
Spike
Spike
Spike
Spike
Spike
Sample type
Lab-pure water
Drinking water
Surface water
Effluent 1
Effluent 2
Effluent 3
Lab-pure water
Drinking water
Surface water
Effluent 1
Effluent 2
Effluent 3
# of spikes
0
0
0
0
0
0
12
6
6
6
6
6
# of elements
18
18
18
18
18
18
18
18
18
18
18
18
Total number
of analyses3
18
18
18
18
18
18
216
108
108
108
108
108
864
aAn analysis is the determination of one element in one sample
-------
INTERLABORATORY METHOD STUDY
Data Reporting Form
Laboratory Number:
Spike Designation:
Concentration (ug/1)
Element Total Background Difference
Al
Sb
As
Ba
Be
Cd
Cr
Co
Cu
Fe
Pb
Mn
Ni
Se
Ag
Tl
V
Zn
A-13
-------
4. DATA REPORTING REQUIREMENTS
Data Generated during the actual method study will be due
within 45 days of sample receipt. All data must be reported
to ERGO on standardized report forms enclosed with this package,
For each spiked sample, the total and background concentrations
must be reported as well as the difference.
Quality control data generated during each analytical run
must be reported for each element. The quality control/quality
assurance requirements are summarized in Section 3. Quality
control data are to be reported on the enclosed forms.
A-14
-------
The final volumes of water and effluent samples will vary
according to the number of ampules that must be added. No correc-
tion or dilution is necessary to account for this since these
factors were compensated for during the ampule preparation.
A background sample (unspiked aliquot) should be removed from
each water and effluent sample. This aliauot should be preserved
and stored in the same manner as spiked samples.
2.3 Procedures for Sample Digestion .
A sample must be digested prior to instrumental analysis.
Procedures for sample digestion are specified in Section 4.1.3
of EPA (1979) as modified for determinations of antimony, arsenic,
and selenium by Methods 204.2, 206.2, and 270.2, respectively'.
2.4 Procedures for Instrumental Analysis
Instrumental analyses will be performed using conditions and
methods specified by EPA (1979) and the instrument manufacturer.
Applicable method references are summarized in Table 3.
The number and types of samples to be analyzed for the method
validation study are summarized in Table 4. A total of 48 samples
(exclusive of blanks, duplicates, and quality control spikes) must
be prepared and analyzed. Six of these samples will be background
analyses of laboratory-pure water, drinking water, surface water,
and the three effluents. Twelve of the samples will be spiked
laboratory-pure water samples. The remaining 30 samples will be
composed of six spiked drinking samples, six spiked surface water
samples, and 18 spiked effluent samples (6 spikes per effluent).
A-15
-------
Total and background concentrations as well as the
differences are to be reported for each spiked sample.
Using instrumental analysis, all Youden Pairs (A and
B samples for each spike level) should be run together. In
addition, effluent and water samples should be run in the
following order to avoid systematic errors:
Analytical order
ratory Number
1
2
3
4
5
6
7
8
9
10
1
El
LP
E3
El
SW
El
LP
LP
E2
E2
2
SW
E3
DW
OW
E3
SW
E2
DW
LP
LP
3
E3
E2
El
E3
DW
E3
DW
E2
E3
SW
4
LP
SW
LP
SW
E2
E2
SW
El
El
E3
5
E2
DW
SW
E2
El
DW
E3
E3
SW
SW
6
DW
El
E2
LP
LP
LP
El
SW
DW
El
A-16
-------
3. QUALITY CONTROL/QUALITY ASSURANCE REQUIREMENTS
Each participating laboratory will be required to implement
quality control/quality assurance protocols for this program.
These protocols must include the following procedures:
1. Preparation of calibration curves for each element.
Each curve will consist of a blank and at least four
calibration standards.
2. Analysis of check standards at the beginning and end
of each working day and at a frequency of 10% during
analytical runs. If analysis of a check standard is
not within 4- 5% of the expected value, analysis must
be terminated, the instrument must be recalibrated,
and all samples run since last successful check
standard must be reanalyzed.
3. Preparation and analysis of one procedural blank
for every 15-20 samples.
4. Preparation and analysis of one spiked sample for
every 15-20 samples.
5. Preparation and analysis of one duplicate sample for
every 15-20 samples.
6. Analysis of an outside reference standard having known
values. This sample will be provided by ERCO and will
be analyzed during each analytical run.
7. Maintenance of accurate written records that trace all
samples from collection through preparation, analysis,
and final data submittal. Each contractor will be
required to maintain all pertinent raw and final data
until informed otherwise by ERCO or EPA.
8. Maintenance of logs documenting instrument repairs
or modifications performed during the time frame of
this study.
A-17
-------
APPENDIX B
TRACE METALS LABORATORY QUALITY ASSURANCE PLAN
4. SUMMARY OF LABORATORY QA/AC PROGRAM
4.1 Quality Assurance Objectives
The ultimate objective of any laboratory Quality Assurance
program is to detect and correct all errors of analytical problems
as they occur and guarantee that all data are as accurate and
precise as technically possible.
The Quality Assurance program implemented at ERGO is intended
to meet the requirements of this program. Design of the protocols
is the responsibility of Dr. John P. Maney and the system is imple-
mented by the laboratory manager, Mr. Keith A. Hausknecht. A
systematic use of laboratory check standards, interference check
standards, standard reference materials, spiked samples, duplicates,
and blanks will ensure early detection and identification of any
analytical problems that may result. Documentation of quality
control data will assist in the detection of any longer-term shifts
in the quality of the analyses being performed.
To preclude any transcription of other errors from being
included in a final data report, all data are checked by the
laboratory manager, Mr. Keith A. Hausknecht, and the divisional
Quality Assurance officer, Dr. John P. Maney, prior to delivery to
the client.
B-l
-------
.2 Quality Control Procedures
The following pages are a summary of ERCO's standard quality
control procedures as excerpted from the Trace Metals Laboratory
Manual. Project-specific quality control requirements will be
implemented if modifications of ERCO's procedures are necessary.
The laboratory will stand and fall by the quality of work
performed. For this reason, a variety of quality control mech-
anisms have been initiated. The first type of quality control is
outlined in the protocols; this includes blanks, handling proce-
dures, etc., which should be followed by all laboratory personnel
in performing the analyses. A second type of quality control is
afforded by close supervision of the lab managers and lab supervisor,
A third type of quality control is performed by spot checks in the
laboratory. These checks are performed by the laboratory director,
division manager and other chemically oriented individuals. A
small percentage of errors are, from a practical point of view,
impossible to eliminate. The sole purpose of Quality Control and
Quality Assurance programs are to identify and correct these errors
at the time that they occur.
Quality Control begins with the receipt of chemicals. All
chemicals and standards are dated upon arrival. The chemicals with
the oldest receiving date are used first. Standards are not used
once their expiration date has passed. All standards are kept
refrigerated. Standards employed for regulatory work are purchased
in duplicate. Two different suppliers (Fisher, Ventron, Spex or
MCB) will be used to supply the standards. Before using, these two
standards are analyzed and the concentrations compared. If the
standards differ in concentration, a third or fourth standard is
employed to determine the correct concentration.
B-2
-------
A service contract is maintained on all balances. A person
cannot make use of a balance unless they have been checked out by
laboratory personnel and their name added to the list of authorized
persons posted near the balance. A set of "S" weights will be kept
in the Trace Metal Laboratory for the purpose of checking accuracy.
The atomic absorption instrumentation, the water purification
system, and clean benches are maintained according to specifications
of the manufacturers and appropriate logs are maintained.
All samples for trace metals analysis are acidified or checked
for acid preservation upon arrival.
To maintain guality control of results the following methods
are employed for all priority pollutant work performed by atomic
absorption spectroscopy (AAS).
4.2.1 Minimum Daily Requirements for AAS
Calibration curves are composed of a minimum of a blank and
three standards. A calibration curve is made for every hour
of continuous sample analysis.
A check standard is run approximately every 15 samples. (For
priority pollutant work this standard is at the Maximum
Contamination Level.)
One duplicate sample is run every 15 samples. A duplicate
sample is a sample brought through the whole sample preparation
process.
B-3
-------
A minimum of one spike sample is run every 15 samples. The
spiked concentration should be at least 10 times the detection
limit concentration.
Standard deviation is documented for all measurements being
made.
Reported concentrations cannot be less than the lowest stan-
dard analyzed.
Samples are diluted if they are more concentrated than the
highest standard or if they fall on the plateau of a calibra-
tion curve.
All preparations employ a minimum of one blank per sample
batch.
If a significant dilution factor would be necessary to analyze
a sample by the graphite furnace, the flame atomizer is used.
Each sample batch requires a minimum of one precision deter-
mination and accuracy determination. Accuracy is determined
by percent recovery of a spike.
When available appropriate Standard Reference Materials are
analyzed to evalute new procedures.
The presence of matrix effects are determined by recoveries
of standard spikes to the samples. If recovery is within 10
percent of the expected value, no interference is assumed.
This test is performed for every new sample type.
B-4
-------
4.2.2 Quarterly Requirements for AAS
A known reference sample is analyzed once per quarter for the
metals measured.
4.2.3 Annual Requirements for AAS
Unknown performance samples (when available) are analyzed at
least once a year.
4.2.4 General Requirements for AAS
All Quality Control Data are maintained and available for easy
reference or inspection using a quality control reference form
(Figure 1).
ERCO's Trace Metals Laboratory routinely participates in the
performance of evaluation tests required by U.S. EPA and other
federal or state agencies.
The calibration blank is analyzed once every 10 samples. The
results should be within two standard deviations of the
mean.
An inter-element interference check sample is analyzed at the
initiation, end, and at periodic intervals throughout the
sample run.
One of every 10 samples will be prepared and analyzed in
duplicate.
B-5
-------
Date
QUALITY CONTROL REPORT FORM
ELEMENT
Analyst
ERGO IDI
SRM or CHECK STD.
Certified or Prepared cone.
Average Reported Cone.
% Difference
DUPLICATES
Concentration A_
Concentration B_
RECOVERY
C spiked (
A-B
x 100 =
(A+B/2)
) - C unspiked (
) x 100 =
C True Spiked (
Method of Standard Additions Employed?
Highest Std run Flame
Lowest Std run
yes
no
Flameless
Detection Limit_
Blank levels
BKG. Corr. yes
no
COMMENTS:
Figure 1. Quality Control Report Form
B-6
-------
A minimum of one sample per every 20 samples is spiked with
multi-element standard and analyzed. If recoveries are not in
the 90-110% range, the samples are analyzed by the method of
standard additions.
A procedural blank is required once for every 15 samples or
every sample batch, whichever is smaller.
A new sample matrix is evaluated by analyzing serial dilutions
and spike additions. The serial dilutions must agree to
within 5% and the standard addition recovery must be within
10%.
Spectral interferences are evaluated using a wavelength scan
of the spectral region of interest or comparative testing by
atomic absorption spectroscopy should be performed.
4.3 Data Reporting Management System
All data generated during this program will be reported to
Versar Inc. using coding forms provided by the prime contractor.
Analytical and quality control data will be entered on forms by
staff by the Trace Metals Laboratory. Data will be verified prior
to transcription by Mr. Keith A. Hausknecht and Dr. John P. Maney
to ensure accuracy and adherence to contract requirements. Fol-
lowing transcription, data will be verified for accuracy by Mr.
Hausknecht and Dr. Maney before delivery to Versar Inc. All
project documentation will be maintained on-file at ERGO and will
be provided to Versar Inc. on request.
B-7
-------
4.4 Corrective Action Procedures
Samples will be prepared and analyzed in batches. Each batch
will have the appropriate number of duplicates, blanks, spiked
samples, and standard reference materials. The analytical results
for these quality control samples will be indicative of the caliber
of the batch analysis and will be helpful in locating any problems
that may occur.
Reagent and procedural blanks will be used to detect con-
tamination from reagents, ambient dust fallout, or unclean glass-
ware. Standard reference materials will be useful in evaluating
the efficiency of sample preparation while check standards and
spiked and duplicate samples will document the accuracy and pre-
cision of the analysis and the analytical program in its entirety.
This system of quality control samples is used to determine if
problems are preparation-, standard-, or instrument-related. After
identifying the source of the problem, corrective measures are then
a matter of routine.
Implementation of quality control in the laboratory is the
responsibility of Mr. Hausknecht. He monitors the progress and
quality of work on a daily basis and is notified by staff members
if results do not meet project requirements. Analytical procedures
are then examined in consultation with Dr. Maney to determine the
source of the problem, and corrective action is taken. These
actions may include, but are not limited to, preparing new stan-
dards or reagents, recalibrating the analytical instruments,
repairing the analytical instruments, preparing new samples,
reanalyzing sample digestates, and analyzing samples by standard
additions. Quality assurance is monitored by Dr. Maney on a weekly
B-8
-------
basis. If quality assurance protocols do not meet project specifi-
cations, the laboratory manager is notified and procedures are
reevaluated to ensure adherence to contract requirements.
B-9
-------
APPENDIX C
RESULTS OF INTERLABORATORY METHOD VALIDATION STUDY
Laboratory Pure, Drinking, and Surface Water:
Raw data for analysis by water type.
Statistical summary for analysis by water type.
Effect of water type on analysis.
Effluent 1:
Raw data for analysis by water type.
Statistical summary for analysis by water type
- Effect of water type on analysis.
Effluent 2:
Raw data for analysis by water type.
Statistical summary for analysis by water type,
Effect of water type on analysis.
Effluent 3:
Raw data for analysis by water type.
Statistical summary for analysis by water type
Effect of water type on analysis.
01
-------
o
I
to
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ALUMINUM ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
R
9
10
1
28.00
101.90
43.00
72.40
43.00
12.00*
27.00
- 19.00*
32.40
4940.00*
100.00
2
33. BO
54.00
51.00
70.60
49.00
12.00*
17.00
- 23.00*
1.50
3530.00*
50.00
1
2B.OO
77.00
83.00
42.00
43.00
31.00*
47.00
90.00
60.00
79.00
0.00*
2
33.50
173.00
126.00
30.00
42.00
32.00*
57.00
80.00
36.00
125.00
0.00*
1
28.00
5.00
74.00
< 10.00*
- 260.00* -
22.00
120.00
250.00
26.00
- 14.00* -
300.00
2
33.50
126.00
82.00
40.00
290.00*
14.00
59.00
400.00
20.00
5.00*
450.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR ALUMINUM ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAR PURE WATER DRINKING WATER SURFACE WATER
n
i
u>
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
74.10
219.30
43.00
114.00
95.00
6.00*
37.00
- 1.00*
131.00
3060.00*
100.00
4
64.50
113.80
39.00
105.00
65.00
4.00*
34.00
- 34.00*
4S.10
2590.00*
100.00
3
74.10
118.00
181.00
92.00
140.00
19.00*
69.00
155.00
115.00
105.00
50.00*
4
64.50
94.00
52.00
65.00
87.00
16.00*
88.00
195.00
64.80
204.00
50.00*
3
74.10
- 112.50*
221.00
100.00
- 310.00*
31.00
49.00
310.00
89.00
10.00
200.00
4
64.50
- 74.00*
210.00*
10.00
- 250.00*
38.00
< 0.20*
950.00*
69.00
16.00
0.00*
-------
o
I
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ALUMINUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER
DRINKING WATER
SURFACE WATER
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
B
9
10
5
125.00
138.20
42.00
185.00
140.00
9.00*
66.00
8440.00*
53.00
2970.00*
150.00
6
111.00
107.50
51.00
142.00
120.00
9.00*
55.00
8440.00*
127.00
2500.00*
150.00
5
125.00
220.00
171.00
145.00
130.00
16.00*
171.00
245.00
214.00
264.00
100.00*
6
111.00
109.00
94.00
132.00 <
140.00 -
24.00*
108.00
155.00 -
211.00
198.00
50.00*
5
125.00
53.00
163.00
10.00*
190.00*
62.00
102.00
40.00*
151.00
129.00
200.00
6
111.00
*
- 15.00*
108.00
< 10.00*
- 210.00*
90.00
44.00
- 90.00*
126.00
184.00
200.00
-------
o
I
ui
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR ALUMINUM ANALYSES BY WATER TYPE
WATER 1
WATER 2
WATER 3
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY(%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, I
SINGLE STO DEV, (SR)
ANALYST REL DEV, I
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (WEL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
1
7
28.00
59.%
114.13
31.46
52.47
17
34
3
7
74.10
105.61
42.53
61.12
57.87
30
34
5
7
125.00
110.60
-11.52
55.87
50.51
27
24
2
7
33.50
41.87
24.99
23.88
57.03
.47
.31
4
7
64.50
72.13
11.83
33.60
46.58
.50
.31
6
7
111.00
107.50
-3.15
39.75
36.98
.08
.84
1
8
28.00
65.13
132.59
19.46
29.88
27
37
3
8
74.10
121.88
64.47
35.77
29.35
48
42
5
8
125.00
195.00
56.00
47.99
24.61
31
18
2
8
33.50
84.63
152.61
52.22
61.71
.98
.38
4
8
64.50
106.22
64.69
59.34
55.86
.61
.62
6
8
111.00
143.38
29.17
42.60
29.71
.20
.44
1
7
28.00
113.86
306.63
117.49
103.19
61
46
3
8
74.10
126.25
70.38
106.11
84.05
32
40
5
7
125.00
122. P6
-1.71
53.87
43.85
32
25
2
8
33.50
148.88
344.40
174.63
117.30
.66
.94
4
4
64.50
33.25
-48.45
26.70
80.30
.23
.41
6
6
111.00
125.33
12.91
58.62
46.77
.12
.89
WATER LEGEMD
1 - LAB PURE WATER
2 - DRINKING WATER
3 - SURFACE WATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON ALUMINUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:r,AMMA(l) = .67942
HATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 .5299 ' -.0136
3 1.1780 -.2312
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 14.83706 14.83706
REGJWATER/OISTILLED) 4 4.89298 1.22324 2.55 .0426
O ERROR 115 55.07978 .47895
I
TOTAL 120 74.80981
** TABLE OF 95S CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .5299 ( -2.2077 , 3.2675) -.0136 ( -.6678 , .6406)
3 1.1780 ( -1.6571 , 4.0130) -.2312 ( -.9118 , .4495)
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.
-------
o
I
-o
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAM DATA FOR ALUMINUM ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - MG/L
LAB PURE WATER EFFLUENT 1
AHPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
12.60
24.88*
10.92
12.28*
11.55
0.06*
13.65
0.18
14.28
10.02
16.80
2
11.00
11.51
10.32
14.38*
10.50
0.10*
12.07
10.44
12.07
10.27
12.60
1
12.60
18.74
14.80
5.00
5.00
30.30*
5.60*
32.00*
11.40
7.30
15.00
2
11.00
11.32
12.20
2.70
11.00
29.00*
6.40*
35.20*
9.90
6.10
15.00
-------
n
i
00
LAB PURE HATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ALUMINUM ANALYSIS BY HATER TYPE
MEDIUM YOUOEN PAIR, UNITS - MG/L
EFFLUENT 1
AMPUL MO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
21.70
25.71
21.10
33.81*
23.10
0.05*
28.77
7.81
23.63
0.45
21.00
4
25.70
31.47
26.46
28.56*
26.25
0.01*
34.75
6.87*
26.46
28.01
21.00
3
21.70
37.74
27. RO
9.20
16.00
27.20
10.60*
33.90*
19.70
12.50
15.00
4
25.70
47.26
33.50
16.30
14.00
78.50*
8.20*
35.20*
25.90
23.40
25.00
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR ALUMINUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - MG/L
EFFLUENT 1
n
I
vo
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
58.30
65.52
S2.39
65.20*
54.60
0.35*
50.40
26.14
60.69
46.18
63.00
6
49.60
26.35
54.39
69.82*
46.20
0.49*
51.45
31.39
50.19
5.65
52.50
5
58.30
81.96
48.40
48.50
52.00
90.80
12.80*
75.70*
57.70
61.50
45.00
6
49.60
70.56
43.30
67.90
65.00
48.70
8.50*
83.10*
44.10
58.30
45.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR ALUMINUM ANALYSES BY WATER TYPE
WATER 1 WATER 2
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE COMC (C) MG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD OEV (S)
OVERALL REL STO OEV, %
SINGLE STD OEV, (SR)
ANALYST REL OEV, I
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, %
SINGLE STD OEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAM RECOVERY (X)
ACCURACY (IREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, I
SINGLE STD DEV, (SR)
ANALYST REL DEV, t
1
7
12.60
12.34
-2.05
2.69
21.79
1
10
3
8
21.70
18.95
-12.68
9.68
51.11
6
27
5
8
58.30
52.37
-10.18
12.48
23.83
12
27
2
8
11.00
11.22
2.03
0.95
8.45
.25
.59
4
7
25.70
27.77
8.06
4.36
15.70
.51
.88
6
8
49.60
39.77
-19.83
17.22
43.31
.62
.40
1
7
12.60
11.03
-12.43
5.42
49.11
2
27
3
8
21.70
20.64
-4.87
9.55
46.25
3
13
5
8
58.30
60.73
4.17
16.86
27.76
13
22
2
7
11.00
9.75
-11.40
4.10
42.02
.82
.11
4
7
25.70
26.48
3.04
11.20
42.29
.08
.06
6
8
49.60
55.36
11.61
11.43
20.64
.20
.73
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 1
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON ALUMINUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAHMA(1) = .85731
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 -.8729 ' .3145
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 35.83426 35.83426
REGfWATER/DISTILLED) 2 1.20953 .60476 2.36 .1010
ERROR 78 19.97960 .25615
O
I
£ TOTAL 81 57.02339
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-OISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.8729 ( -2.1295 . .3837) .3145 ( -.0673 , .6964)
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.
-------
o
I
I
to
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ALUMINUM ANALYSIS BY WATER TYPE
LOW YOUOEN PAIR, UNITS - MG/L
LAB PURE WATER EFFLUENT 2
AMPUL MO:
TRUE CONC:
LAR NUMBER
1
2
3
4
5
6
7
8
9
10
1
0.46
0.92*
0.41
0.46*
0.43
0.00*
0.51
0.34
0.53
0.37
0.62
2
0.51
0.53
0.47
0.66*
0.48
0.00*
0.55
0.48
0.55
0.47
0.58
1
0.46
0.25
0.31
1.23*
0.43
0.03*
0.72
0.39
0.43
0.82
0.50
2
0.51
0.26
0.30
0.58*
0.40
0.03*
0.69
0.83
0.83
0.75
0.50
-------
o
I
M
UJ
ENVIRONMENTAL MONITORING AND SUPPORT LARORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ALUMINUM ANALYSIS BY HATER TYPE
MEDIUM YOUOEN PAIR, UNITS - MG/L
LAB PURE WATER EFFLUENT 2
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
a
9
10
3
1.01
1.20
0.9fl
1.58*
1.08
0.00*
1.34
0.36
1.10
0.02
0;98
4
1.11
1.35
1.13
1.22*
1.13
0.00*
1.49
0.29*
1.13
1.20
0.90
3
1.01
0.74
0.90
4.53*
1.00
0.02*
1.14
3.94*
0.65
1.48
1.10
4
1.11
0.80
1.10
1.69*
1.10
0.02*
1.31
0.51
1.08
1.49
1.00
-------
n
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ALUMINUM ANALYSIS BY MATER TYPE
HIGH YOUOEN PAIR, UNITS - MG/L
LAB PURE WATER EFFLUENT 2
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
2.18
2.43
1.9S
2.42*
2.03
0.01*
1.87
0.97
2.25
1.71
2.34
6
1.76
0.93
1.92
2.46*
1.63
0.02*
1.81
1.11
1.77
0.20
1.85
5
2.18
1.73
1.90
2.92*
2.20
0.02*
2.09
4.24*
2.19
0.94*
2.20
6
1.7fi
1.25
1.54
2.43*
l.PO
0.02*
1.P8
1.20
1.55
1.10
1.80
-------
n
i
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR ALUMINUM ANALYSES BY HATER TYPE
WATER 1 WATER 2
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD DEV, %
SINGLE STO DEV. (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY (SREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD OEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAM RECOVERY (X)
ACCURACY (SREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STO DEV, (SR)
ANALYST REL OEV, %
1
7
0.46
0.46
-0.77
0.10
21.77
0.
8.
3
a
1.01
0.88
-12.44
0.45
51.10
0.
29.
5
8
2.18
1.94
-10.78
0.46
23.84
0.
27.
2
8
0.51
0.51
1.38
0.04
8.46
04
45
4
7
1.11
1.19
7.25
0.1Q
15.72
30
07
6
8
1.76
1.40
-20.38
0.61
43.31
45
00
1
8
0.46
0.48
4.06
0.20
40.67
0
26
3
7
1.01
1.00
-0.75
0.28
27.46
0
11
5
6
2.18
2.05
-5.89
0.20
9.53
0
5
2
8
0.51
0.58
14.65
0.23
39.13
.14
.80
4
R
.1.11
1.05
-5.51
0.30
28.38
.12
.57
6
8
1.76
1.51
-13.94
0.30
19.99
.10
.62
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 2
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AMD DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON ALUMINUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) = .B40fl9
WATER INTERCEPT(MATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 .1062 ' . .0320
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAM SQUARE F PROB
REG(DISTILLED) 1 21.75032 21.75032
REG(WATER/DISTILLED) 2 .26147 .13073 .49 .6144
ERROR 80 21.34386 .26680
O
I
& TOTAL B3 43.35565
** TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(HATER-OISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .1062 ( -.1370 , .3495) .0320 ( -.3908 , .4547)
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.
-------
n
i
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TEST CATEGORY ***
RAW DATA FOR ALUMINUM ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 3
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
26.80
97.80
41.00
70.00
41.00
11.50*
2fi.OO
- 19.00*
31.10
4742.00*
96.00
2
32.00
51.80
49.00
68.00
47.00
11.50*
16.00
- 23.00*
1.40
3389.00*
48.00
1
26.80
85.00
39.00
114.00
68.00
40.00
< 0.20*
-1720.00*
67.00
4.70
50.00
2
32.00
139.00
47.00
114.00
64.00
72.00
< 0.20*
-1730.00*
39.00
47.80
50.00
-------
o
I
t->
00
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LARORATORY
OFFICE OF RESEARCH ANO DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TEST CATEGORY ***
RAM DATA FOR ALUMINUM ANALYSIS BY MATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
EFFLUENT 3
AMPUL MO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
a
9
10
3
70.90
210.50
41.30
109.00
91.00
5.80*
36.00
- 1.00*
126.00
2938.00*
96.00
4
61.70
109.30
37.40
101.00
62.00
3.80*
33.00
- 34.00*
46.00
2486.00*
96.00
3
70.90
85.00
59.00
176.00
100.00
58.00
4.00
-1440.00*
150.00
134.00
100.00
4
61.70
127.00
44.00
130.00
83.00
19.00
< 0.20*
-1610.00*
90.00
112.00
100.00
-------
n
i
M
VO
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TEST CATEGORY ***
RAW DATA FOR ALUMINUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR. UNITS - UG/L
LAB PURE WATER EFFLUENT 3
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
fl
9
10
5
120.00
132.70
40.30
178.00
134.00
8.60*
63.00
8102.00*
51.00
2851.00*
144.00
6
107.00
103.20
49.00
136.00
115.00
8.60*
53.00
8102.00*
122.00
2400.00*
144.00
5
120.00
161.00
61.00*
147.00
130.00
342.00*
172.00
700.00*
160.00
148.00
150.00
6
107.00
99.00
63.00
191.00
120.00
X8500.00*
230.00
3100.00*
290.00
197.00
150.00
-------
o
to
o
ENVIRONMENTAL.MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TEST CATEGORY ***
STATISTICAL SUMMARY FOR ALUMINUM ANALYSES RY WATER TYPE
WATER 1 WATER 2
LOW YOUOEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO DEV (S)
OVERALL REL STO DEV, %
SINGLE STO OEV, (SR)
ANALYST REL OEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (tREL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD DEV, %
SINGLE STO DEV, (SR)
ANALYST REL OEV, %
HIGH YOUOEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO OEV (S)
OVERALL REL STD OEV, %
SINGLE STD OEV. (SR)
ANALYST REL OEV, %
I
7
26.80
57.56
114.77
30.27
52.58
16.
34.
3
7
70.90
101.40
43.02
58.58
57.77
29.
34.
5
7
120.00
106.14
-11.55
53.72
50.61
26.
24.
2
7
32.00
40.17
25.54
23.03
57.34
81
40
4
7
61.70
69.24
12.23
32.27
46.61
34
39
6
7
107.00
103.17
-3.58
38.06
36.89
06
90
1
8
26.80
58.46
118.14
33.02
56.49
19.
29.
3
9
70.90
96.22
35.72
52.67
54.73
22.
24.
5
7
120.00
152.57
27.14
13.36
8.76
43.
26.
2
8
32.00
71.60
123.75
36.05
50.36
42
87
4
8
61.70
88.13
42.83
39.15
44.43
23
12
6
8
107.00
167.50
56.54
74.17
44.28
11
94
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 3
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIROWENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TEST CATEGORY ***
EFFECT OF WATER TYPE ON ALUMINUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) = .67955
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 .0709 ' .0545
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTlLLED) 1 13.86420 13.86420
REGlWATER/DISTILLED) 2 1.73R41 .86921 1.99 .1433
ERROR 78 34.04081 .43642
D
I
to
I- TOTAL 81 49.64342
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
INTERCEPT(WATER-OISTILLED) SLOPE(WATER-OISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .0709 ( -2.2883 , 2.4302) .0545 ( -.5132 , .6223)
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
AMD ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
o
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to
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR ANTIMONY ANALYSIS BY HATER TYPE
LOW YOUOEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4 <
5
6
7
8 <
9
10
1
11.00
10.00
9.00
5.30
5.00* <
28.00*
5.00
3.00
5.00* <
3.70
9.00
2
12.70
11.50
13.00
7.40
5.00* <
30.00*
6.00
4.00
5.00* <
2.50
6.00
1
11.00
n.20
10.00
20.10*
5.00*
38.00*
8.00
4.00*
5.00* <
6.50
9.00
2
12.70
9.50
10.00
20.10*
5.70*
45.00*
9.00
4.00* <
5.00*
2.90
6.00
1
11.00
11.40
8.00
10.80 <
7.70 <
31.00*
9.00
2.00* <
11.00
7.10
6.00
2
12.70
11.50
11.00
4.80*
5.00*
37.00*
8.00
2.00*
9.00
7.70
3.00
-------
o
I
NJ
U)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ANTIMONY ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE MATER
DRINKING MATER
SURFACE HATER
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
56.80
43.60
74.00
26.80
24.00*
156.00*
27.00
30.00
42.00
43.40
50.00.
4
47.30
35.90
107.00*
41.30
22.00*
90.00*
22.00
32.00
37.00
38.90
30.00
3
56.80
54.10
41.00
77.00*
26.00*
168.00*
49.00
30.00*
51.00
40.00
40.00
4
47.30
46.70
37.00
62.50*
17.00*
131.00*
40.00
20.00*
43.00
51.00
40.00
3
56.80
51.10
53.00
33.20
35.00
117.00*
49.00
18.00*
54.00
28.60
40.00
4
47.30
39.60
47.00
19.50
21.00
70.00*
41.00
11.00*
31.00
36.40
30.00
-------
o
to
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ANTIMONY ANALYSIS BY MATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER
DRINKING HATER
SURFACE HATER
AMPUL MO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
240.00
231.00
205.00
349.00
150.00*
897.00*
85.00
152.00
230.00
194.00
200.00
6
200.00
210.00
191.00
195.00
140.00*
520.00*
78.00
86.00
190.00
39.60
210.00
5
240.00
231.00
192.00
317.00*
130.00*
721.00*
195.00
91 .00*
180.00
217.00
200.00
6
200.00
209.00
174.00
316.00*
97.00*
742.00*
164.00
74.00*
159.00
47.40
260.00
5
240.00
240.00
192.00
108.00
120.00
616.00*
205.00
87.00*
240.00
181.00
- 250.00
6
200.00
208.00
172.00
72.90*
190.00
535.00*
173.00
70.00*
196.00
163.00
190.00
-------
n
i
to
Ul
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR ANTIMONY ANALYSES BY WATER TYPE
WATER 1
WATER 2
WATER 3
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACYUREL ERROR)
OVERALL STO OEV (S)
OVERALL REL STO DEV, *
SINGLE STO OEV. (SR)
ANALYST REL OEV, %
MEOIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (WEL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, I
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY(WEL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, I
1
7
11.00
6.43
-41.56
2.84
44.22
1.
23.
3
8
56.80
42.10
-25.88
15.55
36.93
7.
19.
5
8
240.00
205.75
-14.27
75.01
36.46
45.
25.
2
7
12.70
7.20
-43.31
3.82
53.00
61
56
4
7
47.30
33.87
-28.39
6.50
19.20
36
37
6
8
200.00
149.«5
-25.02
69.67
46.46
82
76
1
5
11.00
8.34
-24.18
1.30
15.53
1
20
3
6
56.80
45.85
-19.28
6.27
13.67
5
12
5
6
240.00
202.50
-15.63
18.45
9.11
52
28
2
5
12.70
7.48
-41.10
3.00
40.06
.62
.46
4
6
47.30
42.95
-9.20
5.13
11.95
.35
.05
6
6
200.00
168.90
-15.55
70.45
41.71
.73
.39
1
8
11.00
8.87
-19.32
2.01
22.61
1
17
3
8
56.80
42.99
-24.32
9.99
23.25
6
16
5
8
240.00
192.00
-20.00
54.12
28.19
29
15
2
6
12.70
8.37
-3V12
3.05
36.46
.50
.40
4
8
47.30
33.19
-29.84
9.67
29.13
.20
.27
6
7
200.00
184.57
-7.71
15.79
8.55
.67
.76
WATER LEGEND
1 - LAB PURE WATER
2 - DRINKING WATER
3 - SURFACE WATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON ANTIMONY ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) = 1.10775
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 .2737 -.0139
3 .2993 -.0402
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLEO) 1 1<>8.89603 198.89603
O REG(WATER/DISTILLED) 4 .34176 .08744 .81 .5182
^ ERROR 110 11.80203 .10729
a\
TOTAL 115 211.04781
** TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .2737 ( -.3897 , .9371) -.0439 ( -.2014 , .1136)
3 .2993 ( -.3107 , .9092) -.0482 ( -.194? , .0978)
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.
-------
n
t
K)
-J
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ANTIMONY ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4 <
5
6
7
8 <
9
10
1
10.50
7.20
9.80
17.40
5.00* <
42.00*
4.00
2.30
5.00* <
6.40
13.00
2
12.20
8.70
8.70 <
12.20
5.00*
51.00*
4.60
3.30
5.00* <
6.60 .
6.50
1
10.50
9.10
6.00*
17.50
9.70
4.00*
2.00
3.00*
5.00* <
6.70
6.00
2
12.20
11.10
6.00
19.70
6.80
28.00*
3.00
4.00*
5.00* <
8.40
6.00
1
10.50
5.00
6.00
25.60
10.00
31.00*
25.00
4.00*
5.00* <
4.50
9.00
2
12.20
6.50
7.00 <
34.10
7.60 <
39.00*
47.00 <
5.00*
5.00* <
4.30
12.00
1
10.50
4.20
6.00*
13.40
5.00*
29.00*
0.50*
3.00
5.00* <
2.50*
12.00
2
12.20
5.80
6.00
48.00*
6.50
44.00*
4.00
4.00
5.00*
1.20*
9.00
-------
o
I
to
CD
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ANTIMONY ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
54.30
52.10
44.50
10.30
22.80
157.00*
21.00
29.00
18.00
35.30
52.00
4
45.20
40.50
39.10
11.00
15.20
115.00*
2?. 00
16.00
14.00
23.10
42.00
3
54.30
68.40
52.00
33.70
30.00
73.00*
37.00
17.00*
63^00
24.00
80.00
4
45.20
48.10
35.00
50.40
41.00
71.00*
39.00
19.00*
23.00
36.00
40.00
3
54.30
36.00
34.00
44.30
48.00
231.00*
31.00
29.00*
61.00
36.60
70.00
4
45.20
29.00
30.00
32.60
27.00
213.00*
32.00
24.00*
48.00*
35.00
30.00
3
54.30
25.50
28.00
4.80
33.00
74.00*
20.00
24.00
31.00
15.30*
51.00
4
45.20
23.70
23.00
31.80
24.00
114.00*
18.00
28.00
42.00
15.40*
39.00
-------
n
i
to
VO
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR ANTIMONY ANALYSIS BY «ATFR TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
AMPUL NO:
TRUE CONC:
LAR NUMBER
1
2
3
4
5
6
7
fl
9
10
5
230.00
267.00
201.00
204.00
119.00
720.00*
78.00
119.00
195.00
108.00
195.00
6
191.00
222.00
174.00
153.00
94.00
671.00*
78.00
86.00
160.00
179.00
141.00
5
230.00
304.00*
178.00
214.00
180.00
251.00*
176.00
80.00*
200.00
190.00
200.00
6
191.00
237.00
158.00
134.00
150.00
301.00*
136.00
77.00*
160.00
196.00
200.00
5
230.00
156.00
187.00
200.00
150.00
ein.oo*
121.00
124.00*
200.00
252.00
230.00
6
191.00
151.00
164.00
143.00
130.00
957.00*
122.00
87.00*
181.00
158.00
200.00
5
230.00
127.00
183.00
101.00
150.00
380.00*
112.00
94.00
173.00
14.RO*
160.00
6
191.00
104.00
160.00
135.00
120.00
210.00*
98.00
85.00
187.00
13.90*
210.00
-------
o
4
U>
O
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR ANTIMONY ANALYSES BY WATER TYPE
HATER 1
MATER 2
WATER 3
WATER 4
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD OEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE COHC (C) UG/L
MEAN RECOVERY (X)
ACCURACY(%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, I
10
8
-18
5
61
54
31
-41
15
48
230
165
-28
61
37
1
7
.50
.59
.23
.26
.24
2
28
3
9
.30
.67
.68
.21
.04
3
13
5
9
.00
.11
.21
.31
.13
27
17
2
7
12.20
7.23
-40.75
2.95
40.85
.26
.57
4
0
45.20
24.77
-45.21
12.42-
50.15
.78
.39
6
9
191.00
143.00
-25.13
48.43
33.87
.22
.67
1
6
10.50
8.50
-19.05
5.19
61.03
1.
15.
3
8
54.30
48.51
-10.66
20.37
41.99
16.
37.
5
7
230.00
191.14
-16.89
14.18
7.42
20.
11.
2
7
12.20
8.71
-28.57
5.44
62.42
36
79
4
R
45.20
39.06
-13.58
8.44
21.61
33
30
6
8
191.00
171.38
-10.27
36.15
21.09
3"
25
1
7
10.50
12.16
15.78
9.20
75.69
5
40
3
8
54.30
45.11
-16.92
13.93
30.89
10
26
5
8
230.00
187.00
-18.70
43.26
23.13
21
12
12.
16.
38.
16.
98.
.8R
.43
45.
30.
-31.
2.
8.
.13
.69
191.
156.
-18.
25.
16.
.84
.73
2
7
20
93
76
72
77
4
7
20
80
86
62
52
6
8
00
13
26
79
52
10.
a.
-22.
5.
65.
54.
27.
-49.
12.
47.
230.
137.
-40.
33.
24.
1
4
50
15
38
31
12
1.
25.
3
8
30
16
98
99
84
8.
31.
5
8
00
50
22
76
55
20.
15.
2
6
12.20
5.88
-51.78
1.86
31.53
77
20
4
8
45.20
28.69
-36.53
8.34
29.08
88
81
6
8
191.00
137.38
-28.08
44.66
32.51
85
17
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 1
3 - EFFLUENT 2
4 - EFFLUENT 3
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON ANTIMONY ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) = 1.04577
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 .0392 ' .0476
3 .6648 -.0979
4 -.1230 .0118
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLEO) 1 249.89424 249.89424
0 REGlWATER/DISTILLED) 6 4.23787 .70631 3.81 .0014
I ERROR 165 30.61802 .18556
CA)
(- .
TOTAL 172 284.75014
** TARLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE!WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .0392 ( -.8042 , .8827) .0476 ( -.1552 , .2504)
3 .6648 ( -.1623 , 1.4919) -.0979 ( -.2%5 , .1006)
4 -.1230 { -1.0051 , .7590) .0118 ( -.1968 , .2204)
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AMD THE CORRESPONDING WASTE WATER FOR THE ASSOCIATED PARAMETERUNTERCEPT/SLOPE).
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE MOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
n
i
CO
N)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS Bt AA ***
RAW DATA FOR ARSENIC ANALYSIS RY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9 <
10
1
12.40
8.60
12.00
13.20
13.00
10.00
22.00*
8.00*
10.50
3.00*
10.00
2
10.20
4.80
10.00
9.10
17.00
8.00
19.00
8.00*
8.50
4.60*
10.00
1
12.40
18.00*
13.00
14.40
11.00
5.00*
8.80
15.00
11.70 <
11.00
15.00
2
10.20
12.60*
8.00
11.80
12.00
4.00*
8.80
5.00
3.00*
8.60
15.00
1
12.40
13.20*
11.00
11.20
12.00
5.00
5.90
3.00
15.00
9.00
10.00
2
10.20
12.50*
12.00
11.20
11.00
4.00
8.40
1.00
9.90
0.00*
10.00
-------
n
i
CO
Ul
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ARSENIC ANALYSIS BY MATER TYPE
MEDIUM YOUOEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
51.80
48.50
44.00
44.60
47.00
42.00
47.00
15.00*
48.80
40.50*
50.00
4
61.80
86.60*
52.00
58.40
57.00
47.00
58.00
22.00*
60.20
51.80*
60.00
3
51.80
67.70*
44.00
47.90
48.00
36.00*
42.00
22.00*
55.00
41.20
45.00
4
61.80
76.60*
49.00
56.50
60.00
55.00*
53.00
15.00*
66.00
49.50
65.00
3
51.80
88.20*
42.00
35.50
58.00
38.00
47.00
58.00
54.00
33.50
60.00
4
61.80
102.60*
51.00
67.70
75.00
51.00
55.00
64.00
48.00
44.50
60.00
-------
n
i
u>
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ARSENIC ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
AHPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
237.00
324.90
220.00
248.00
200.00
218.00
218.00
80.00*
221.00
163.00*
135.00
6
211.00
240.50
211.00
212.00
180.00
191.00
187.00
79.00*
172.00
149.00*
225.00
5
237.00
259.00*
226.00
235.00
210.00
34.00*
282.00
148.00
236.00
224.00
255.00
6
211.00
232.00*
206.00
207.00
210.00
39.00*
253.00
146.00
192.00
212.00
165.00
5
237.00
383.00*
230.00
250.00
210.00
198.00
87.00*
163.00
208.00
227.00
220.00
6
211.00
317.00*
207.00
207.00
180.00
188.00
126.00
173.00
165.00
184.00
195.00
-------
n
i
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR ARSENIC ANALYSES BY WATER TYPE
WATER 1 WATER 2 WATER 3
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD DEV, %
SINGLE STO DEV, (SR)
ANALYST REL DEV, I
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, t
SINGLE STD OEV, (SR)
ANALYST REL DEV, *
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (IREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
1
7
12.40
11.04
-10.94
1.72
15.61
1
17
3
8
51.80
46.49
-10.26
2.73
5.87
1
3
5
8
237.00
223.11
-5.86
52.57
23.56
35
16
2
8
10.20
10.80
5.88
4.77
44.13
.94
.78
4
7
61.80
56.09
-9.25
4.B5
8.65
.96
.83
6
8
211.00
202.31
-4.12
23.67
11.70
.49
.68
1
8
12.40
12.49
0.71
2.24
17.95
2.
24.
3
7
51.80
46.16
-10.89
4.70
10.18
3.
6.
5
8
237.00
227.00
-4.22
38.72
17.06
20.
9.
2
7
10.20
9.89
-3.08
3.28
33.18
69
06
4
7
61.80
57.00
-7.77
6.96
12.21
30
40
6
8
211.00
198.88
-5.75
32.37
16.27
50
63
1
9
12.40
9.12
-26.43
3.81
41.80
1
18
3
9
51.80
47.33
-8.62
10.49
22.15
7
14
5
8
237.00
213.25
-10.02
25.81
12.10
13
6
2
8
10.20
8.44
-H.28
3.90
46.22
.59
.10
4
9
61.80
57.36
-7.19
10.05
17.53
.62
.56
6
9
211.00
180.56
-14.43
24.88
13.78
.21
.71
WATER LEGEND
1 - LAB PURE HATER
2 - DRINKING WATER
3 - SURFACE WATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON ARSENIC ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMAl1) = 1.00050
WATER INTERCEPT(WATER-OISTILLED) SLOPE(WATER-OISTILLED)
2 .0688 -.0092
3 -.4418 .0922
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 228.15218 228.15218
_ RECfWATER/DISTILLED) 4 .75614 .1B903 2.53 .0435
V ERROR 128 9.55621 .07466
u>
Oi
TOTAL 133 238.46452
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLEO) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .0688 ( -.4198 , .5573) -.0092 ( -.1251 , .1068)
3 -.4418 ( -.9154 , .0318) .0922 ( -.0213 , .2057)
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.
-------
o
I
u>
-j
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ARSENIC ANALYSIS BY HATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 1 EFFLUENT 2 EFFLUENT 3
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
11.80
13.50
16.30 '
32.90*
17.40
16.30
19.60
8.70*
7.90
4.80
16.30
2
9.78
18.30
13.20
28.30*
12.00
18.50
16.30
6.50*
8.50
15.20
10.90
1
11.80
21.60
8.00* <
33.60
39.00
27.00
20.00
16.00*
17.00
30.30
25.00
2
9.78
10.60
8.00* <
4.00
16.00
27.00
17.00 <
11.00*
18.00
24.30
20.00
1
11.80
5.00
8.00* <
13.10
17.00
6.00
0.20* <
3.00*
12.00
10.80
10.00
2
9.78
*
1.10
8.00* <
8.40 <
14.00
1.00
0.20*
3.00*
11.00
9.00 -
15.00
1
11.80
5.80
8.00* <
1.00* <
11.00
10.00
5.00
12.00
15.00
7.30* -
5.00 <
2
9.78
7.00
8.00*
1.00*
11.00
10.00
2.00
10.00
13.00
10.30*
5.00*
-------
o
I
U)
oo
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR ARSENIC ANALYSIS BY WATER TYPE
MEDIUM YOUOEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 1 EFFLUENT 2 EFFLUENT 3
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
49.60
70.40
47.86
79.50*
47.90
65.30
57.70
13.10*
46.20
35.90
60.00
4
59.10
' 93.10
59.80
121.00*
68.50
52.20
76.10
18.50*
66.80
49.20
70.70
3
49.60
74.10
28.00*
75.30
59.00
65.00
57.00
50.00*
65.00
73.80
70.00
4
59.10
100.10
49.00*
97.30
76.00
75.00
71.00
68.00*
80.00
79.80
90.00
3
49.60
41.20
20.00*
29.20
28.00
45.00
54.00
13.00*
51.00
44.10
55.00
4
59.10
53.90
31.00*
45.00
65.00
41.00
51.00
11.00*
69.00
51.30
60.00
3
49.60
t
45.60
27.00
24.60
45.00
45.00
42.00
47.00
53.00
22.90*
30.00
4
59.10
52.00
32.00
41.50
56.00
55.00
57.00
58.00
69.00
31.60*
50.00
-------
n
i
OJ
vo
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ARSENIC ANALYSIS BY WATER TYPE
HIGH YOUOEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 1 EFFLUENT 2 EFFLUENT 3
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
227.00
312.70
217.80
359.00*
207.00
211.00
243.00
163.00*
173.00
190.00
272.00
6
202.00
271.90
199.00
266.00*
207.00
193.60
226.00
130.50*
198.00
170.00
207.00
5
227.00
256.00
138.00*
207.00
220.00
200.00
287.00
130.00*
182.00
378.00
285.00
6
202.00
287.00
112.00*
258.00
180.00
171.00
250.00
140.00*
172.00
275.00
180.00
5
227.00
196.00
155.00*
238.00
210.00
225.00
221.00
79.00*
176.00
165.00
165.00
6
202.00
293.00
130.00*
18R.OO
200.00
212.00
259.00
68.00*
210.00
143.00
180.00
5
227.00
*
191.00
192.00
219.00
220.00
236.00
240.00
147.00
188.00
187.00*
170.00
6
202.00
212.00
173.00
185.00
190.00
197.00
205.00
127.00
186.00
46.20'
155.00
-------
o
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR ARSENIC ANALYSES BY WATER TYPE
HATER 1
WATER 2
WATER 3
WATER 4
LOU YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV. I
SINGLE STD OEV, (SR)
ANALYST REL DEV, *
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STO DEV, (SR)
ANALYST REL DEV, *
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (tREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
1
a
11.80
14.01
18.75
5.08
36.28
3
27
3
8
49.60
53.91
8.68
11.40
21.15
8
13
5
8
227.00
228.31
0.58
45.73
20.03
18
8
2
8
9.78
14.11
44.30
3.58
25.39
.92
.88
4
8
59.10
67.05
13.45
13.98
20.85
.13
.45
6
8
202.00
209.06
3.50
29.84
14.27
.70
.55
1
8
11.80
26.69
126.17
7.37
27.60
7.
35.
3
8
49.60
67.40
35.89
7.02
10.42
4.
6.
5
8
227.00
251.88
10.96
64.21
25.49
39.
16.
2
8
9.78
17.11
74.97
7.31
42.72
85
87
4
8
59.10
83.65
41.54
10.82
12.93
58
06
6
8
202.00
221.63
9.72
50.34
22.72
45
66
1
7
11.80
10.56
-10.53
4.12
39.07
2.
25.
3
8
49.60
43.44
-12.42
10.36
23.05
9.
19.
5
8
227.00
199.50
-12.11
28.41
14.24
32.
15.
2
7
9.78
8.50
-13.09
5.63
66.21
43
51
4
8
59.10
54.52
-7.74
9.61
17.62
34
08
6
8
202.00
210.63
4.27
46.70
22.17
18
69
1
7
11.80
9.11
-22.76
3.92
43.00
1
12
3
9
49.60
39.91
-19.53
10.06
25.20
3
7
5
9
227.00
200.33
-11.75
30.93
15.44
13
7
2
6
9.78
8.83
-9.68
3.87
43.80
.13
.62
4
9
59.10
52.28
-11.54
10.54
20.16
.52
.63
6
9
202.00
181.11
-10.34
26.39
14.57
.48
.07
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 1
3 - EFFLUENT 2
4 - EFFLUENT 3
-------
ENVIRONMENTAL MONITORING AMD SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF HATER TYPE ON ARSENIC ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) = .92941
HATER INTERCEPT(HATER-DISTILLED) SLOPE(HATER-DISTILLED)
*
2 .6338 -.1034
3 -.9734 .1753
4 -.8470 .1350
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 261.60674 261.60674
9 REG(HATERXDISTILLED) 6 12.17275 2.02879 14.78 .0000
JL ERROR 174 23.87803 .13723
M
TOTAL 181 297.65753
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETHEEN SLOPES **
INTERCEPT(HATER-OISTILLED) SLOPE(HATER-DISTILLED)
HATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .6338 ( -.0357 , 1.3033) -.1034 { -.2663 , .0595)
3 -.9734 ( -1.6620 , -.2848) .1753 ( .0092 , .3414)
4 -.8470 ( -1.5452 , -.1488) .1350 ( -.0314 , .3013)
NOTE: IF ZERO IS CONTAINED HITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETHEEN
DISTILLED HATER AND THE CORRESPONDING HASTE HATER 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.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR BARIUM ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
o
1
£>.
to
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
q
10
62
25
114
112
64
91
91
68
45
106
90
1
.70
.00*
.00
.00*
.00
.00
.00
.00
.00
.00
.00
59.
23.
120.
91.
83.
80.
83.
56.
28.
104.
90.
2
10
00*
00
70*
00
00
00
00
00
00
00
62
1
68
111
100
104
117
99
110
597
90
1
.70
.00*
.00
.00
.00
.00*
.00
.00
.00
.00*
.00
2
59.10
34.00*
45.00
101.00
110.00
217.00*
114.00
73.00
297.00*
75.30
105.00
62.
312.
77.
86.
80.
< 12.
128.
79.
67.
138.
70.
1
70
00*
00
30
00
00*
00
00
20
20
00
2
59.10
264.00*
73.00
80.30
90.00
< 7.00*
115.00
70.00
50.20
104.20
100.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAM DATA FOR BARIUM ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER
DRINKING WATER
SURFACE WATER
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
165.00
142.00*
212.00
259.00*
170.00
246.00
185.00
132.00
98.00
193.00
100.00
4
194.00
139.00*
250.00
243.00*
180.00
176.00
217.00
175.00
87.00
252.00
230.00
3
165.00
14.00*
120.00
241.00
210.00
256.00*
246.00
169.00
90.00
82.10
220.00
4
194.00
20.00*
118.00
294.00
220.00
332.00*
297.00
1R3.00
150.00
104.10
160.00
3
165.00
302.00
180.00
10.10
220.00
129.00*
220.00
165.00
98.20
227.20
90.00
4
194.00
176.00
198.00
194.00
250.00
47.00*
208.00
189.00
181.20
238.20
160.00
U)
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR BARIUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
o
*».
*».
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
379.00
22.00*
282.00
5%. 00*
320.00
485.00
362.00
363.00
427.00
334.00
300.00
6
437.00
32.00*
346.00
460.00*
370.00
583.00*
407.00
403.00
787.00*
370.00
450.00
5
379.00
84.00*
244.00
456.00
470.00
469.00*
333.00
409.00
720.00
300.00
410.00
6
437.00
126.00*
322.00
555.00
530.00
853.00*
397.00
469.00
660.00
293.00
560.00
5
379.00
529.00
286.00
515.00
430.00
249.00*
501.00
374.00
183.20
437.20
470.00
6
437.00
582.00
328.00
413.00
510.00
68.00*
617.00
463.00
271.20
475.20
420.00
-------
o
I
£>.
(J\
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR BARIUM ANALYSES BY HATER TYPE
HATER 1
HATER 2
HATER 3
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (WL ERROR)
OVERALL STD OEV (S)
OVERALL REL STO OEV, I
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (*REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, *
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD DEV, *
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
1
8
62.70
83.63
33.37
22.97
27.47
8.
9.
3
8
165.00
167.00
1.21
53.12
31.81
40.
22.
5
8
379.00
359.13
-5.24
67.70
18.85
30.
8.
2
8
59.10
BO. 50
36.21
28.21
35.05
20
99
4
8
194.00
195.88
0.97
54.28
27.71
66
41
6
6
437.00
391.00
-10.53
36.85
9.42
52
14
i
7
62.70
99.29
58.35
16.49
16.61
11
12
3
8
165.00
172.26
4.40
67.09
38.94
27
15
5
8
379.00
417.75
10.22
144.88
34.68
45
10
2
7
59.10
89.04
50.66
25.32
28.43
.88
.61
4
8
194.00
190.76
-1.67
73.94
38.76
.59
.20
6
8
437.00
473.25
8.30
127.34
26.91
.27
.16
1
8
62.70
90.71
44.68
26.96
29.72
13
15
3
9
165.00
168.06
1.85
88.68
52.77
58
31
5
9
379.00
413.93
9.22
115.21
27.83
50
11
2
fl
59.10
85.34
44.40
21.11
24.74
.41
.23
4
9
194.00
199.38
2.77
28.96
14.53
.48
.83
6
9
437.00
453.27
3.72
111.10
24.51
.32
.61
HATER LEGEND
1 - LAB PURE HATER
2 - DRINKING HATER
3 - SURFACE HATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON BARIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(l) = .81406
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED) .
*
2 .1221 -.0002
3 .0404 .0021
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 56.28216 56.28216
.- REG(WATER/DISTILLEO) 4 .31291 .07823 .53 .7108
I ERROR 129 18.89010 .14643
*>.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR BARIUM ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
o
-J
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
60.00
152.00
172.00
150.00
106.00
212.00*
145.00
93.00
136.00
117.00*
161.00
2
56.50
123.00
177.00
130.00
89.00
145.00*
145.00
103.00
85.00
72.70*
161.00
1
60.00
-2960.00*
114.00
168.00
80.00
165.00
220.00
62.00
116.00
53.00
65.00
2
56.50
-4100.00*
98.00
91.00
100.00
263.00
244.00
51.00
109.00
461.00*
75.00
1
60.00
52.00*
87.00
77.10
120.00
*
130.00
104.00
23.00
81.80
130.00
2
56.50
45.00*
75.00
69.00
100.00
263.00*
95.00
118.00
10.00*
74.80
95.00
1
60.00 .
*
- 10.00* -
68.00
130.00
120.00
215.00*
255.00*
102.00
130.00
92.10
45.00
2
56.50
4.00*
25.00
84.20
93.00
250.00*
277.00*
90.00
84.00
73.00
15.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR BARIUM ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
o
*>
00
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
157.00
148.00
283.00
320.00
215.00
368.00*
27.00
156.00
400.00
35.40*
236.00
4
185.00
203.00
335.00
311.00
215.00
312.00*
25.00
189.00
221.00
48.50*
258.00
3
157.00
-3400.00*
158.00
304.00
210.00
207.00
233.00
94.00
348.00
282.00
255.00
4
185.00
-3660.00*
190.00
377.00
240.00
368.00
220.00
103.00
320.00
377.00
215.00
3
157.00
65.00*
121.00
234.00
250.00
491.00*
192.00
179.00
81.00
58.70
245.00
4
185.00
84.00*
119.00
249.00
310.00
179.00
254.00
191.00
89.00
208.00
175.00
3
157.00
- 66.00*
52.00
50.20
240.00*
353.00*
234.00*
110.00
51.00
61.70
125.00
4
185.00
- 46.00*
92.00
34.20
230.00
360.00*
241.00*
121.00
4.00
143.00
105.00
-------
'ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR BARIUM ANALYSIS BY HATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
362.00
220.00
369.00
512.00
333.00
849.00*
521.00
394.00
394.00
314.00*
483.00
6
418.00
231.00
399.00
590.00
376.00
805.00*
465.00
419.00
437.00
360.00*
537.00
5
362.00
-1590.00*
190.00
564.00
490.00
505.00
540.00
418.00
420.00
320.00
425.00
6
418.00
-2370.00*
304.00
632.00
570.00
367.00
702.00
469.00
287.00
114.00
225.00
5
362.00
97.00*
127.00
460.00
300.00
237.00
810.00
459.00
206.00
100.00
375.00
6
418.00
124.00* -
135.00
451.00
440.00
553.00
687.00
532.00
330.00
190.00
375.00
5
362.00
95.00*
92.00
98.20
210.00
359.00*
673.00*
340.00
399.00
95.60
205.00
6
418.00
- 97.00*
100.00*
162.00
150.00
2B4.00*
741.00*
411.00*
177.00
179.00
165.00
VO
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR BARIUM ANALYSES BY WATER TYPE
WATER 1
'WATER 2
WATER 3
WATER 4
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (JREL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (JREL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD DEV, t
o SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (JREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, *
SINGLE STD DEV, (SR)
ANALYST REL DEV, J
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 1
3 - EFFLUENT 2
4 - EFFLUENT 3
1
8
60.00
139.38
132.29
27.02
19.39
14.
10.
3
8
157.00
223.13
42.12
115.33
51.69
53.
23.
5
8
362.00
403.25
11.40
101.36
25.13
28.
6.
2
8
56.50
126.63
124.12
33.35
26.34
53
92
4
8
185.00
219.63
18.72
94.30
42.94
00
94
6
8
418.00
431.75
3.29
108.16
25.05
01
71
60
115
93
57
49
157
232
47
76
33
362
430
18
116
27
1
9
.00
.89
.15
.78
.86
34
28
3
9
.00
.33
.98
.89
.10
45
18
5
9
.00
.22
.85
.86
.16
102
24
2
8
56.50
128.88
128.10
79.13
61.40
.67
.33
4
9
185.00
267.78
44.74
97.26
36.32
.78
.31
6
9
418.00
407.78
-2.45
198.00
48.56
.32
.42
60
94
56
35
37
157
170
8
75
44
362
341
-5
219
64
1
8
.00
.11
.85
.64
.87
12
13
3
8
.00
.09
.34
.02
.11
44
24
5
9
.00
.56
.65
.03
.13
86
23
56
89
58
(7
19
.20
.29
185
197
6
68
34
.89
.45
418
410
-1
175
42
.95
.13
2
7
.50
.54
.48
.46
.50
4
9
.00
.11
.55
.41
.70
6
9
.00
.33
.83
.46
.76
1
7
60.00
98.16
63.60
32.38
32.99
9
11
3
6
157.00
74.98
-52.24
33.53
44.72
32
36
5
7
362.00
205.69
-43.18
123.85
60.21
86
46
2
7
56.50
66.31
17.37
32.38
48.83
.59
.66
4
7
185.00
104.17
-43.69
73.83
70.87
.85
.67
6
5
418.00
166.60
-60.14
11.84
7.11
.17
.29
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF HATER TYPE ON BARIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED HATER SLOPE:GAMMA(1) = .58320
HATER INTERCEPT(HATER-DISTILLED) ^SLOPElHATER-DISTILLED)
2 -.5028 .0940
3 -.7873 .1060
4 .0685 -.1704
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
O REG(DISTILLED) 1 42.63186 42.63186
I REG(HATER/DISTILLED) 6 16.66139 2.77690 9.09 .0000
jl! ERROR 173 52.87321 .30563
TOTAL 180 112.16647
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETHEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(HATER-DISTILLED) SLOPE(HATER-OISTILLED)
HATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.5028 ( -2.4217 , 1.4161) .0940 ( -.2801 , .4681)
3 -.7873 ( -2.7512 , 1.1765) .1060 ( -.2757 , .4877)
4 .0685 ( -1.9911 , 2.1280) -.1704 ( -.5749 , .2340)
NOTE: IF ZERO IS CONTAINED HITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED UATER AND THE CORRESPONDING WASTE HATER 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.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR BERYLLIUM ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
n
Ul
N)
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3 <
4 <
5
6 <
7
8 <
9
10
1
0.63
0.60
0.40 <
0.60* <
0.50* <
1.00*
0.30* <
0.50
0.50* <
0.56
0.60
2
0.47
0.07
0.50*
0.60* <
0.50*
1.00
0.30*
0.30
0.50* <
0.44
0.40
1
0.63
0.69
0.60 <
0.60* <
0.50 <
1.00 <
0.80*
0.70
0.50* <
0.55
0.40
2
0.47
0.24
0.50*
0.60*
0.50* <
0.50* <
0.40*
0.50
0.50* <
0.33
0.40
1
0.63
0.83
0.50 <
0.80 <
0.50* <
0.50* <
1.00*
0.80
0.50* <
0.68
0.60
2
0.47
0.50
0.50*
0.60*
0.50*
0.50*
0.90*
0.50
0.50*
0.57
0.40
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR BERYLLIUM ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8 <
9
10
3
1.59
1.37
1.60
1.50
1.20
1.00
1.70
1.10
0.50* <
1.10
1.40
4
1.91
1.64
1.90
2.20
1.20
4.00*
1.90
1.50
0.50* <
1.60
1.80
3
1.59
1.76
1.40
1.10
1.10
2.00
1.70*
1.70
0.50* <
1.83
1.40
4
1.91
2.11
1.80
1.80
1.40
2.00
3.20*
2.00
0.50*
2.07
1.80
3
1.59
.66
.60
.50
.20
.00
2.10*
1.80
10.00*
1.77
1.40
4
1.91
2.56
1.80
1.90
1.50
2.00
2.40*
2.30
5.00*
2.14
1.60
OJ
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR BERYLLIUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
n
i
en
*>.
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
m
5
9.09
8.89
10.10
10.50
6.50
10.00
17.00*
7.70
6.50*
7.00
9.00
6
11.40
11.42
13.20
13.20
8.40
14.00
17.00
16.00
11.00*
11.30
11.00
5
9.09
11.31
17.00*
8.90
7.60
8.00
17.00*
9.20
7.40*
10.70
8.00
6
11.40
12.54
10.80
10.60
9.60
10.00
19.00*
11.00
10.10*
14.40
10.00
5
9.09
12.30
8.80
8.90
7.10
4.00
11.00*
11.00
6.90
0.57
9.00
6
11.40
11.80
11.80
10.70
9.30
7.00
12.00*
12.50
9.10
1.19*
11.00
-------
n
i
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR BERYLLIUM ANALYSES BY WATER TYPE
WATER 1
WATER 2
WATER 3
LOU YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD OEV (S)
OVERALL REL STO OEV, %
SINGLE STD DEV, (SR)
ANALYST REL OEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACYdREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, %
SINGLE STD OEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACYdREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
1
5
0.63
0.53
-15.82
0.08
15.86
0
26
3
9
1.59
1.33
-16.35
0.24
18.36
0
9
5
8
9.09
8.71
-4.17
1.50
17.22
1
13
2
5
0.47
0.44
-5.56
0.34
77.69
.13
.47
4
8
1.91
1.72
-10.08
0.30
17.62
.15
.67
6
9
11.40
12.84
12.59
2.65
20.68
.47
.68
1
7
0.63
0.63
0.36
0.19
30.35
0
25
3
8
1.59
1.54
-3.38
0.34
21.95
0
8
5
7
9.09
9.10
0.13
1.42
15.64
0
5
2
4
0.47
0.37
-21.47
0.11
29.92
.13
.99
4
8
1.91
1.87
-1.96
0.23
12.23
.14
.08
6
8
11.40
11.12
-2.48
1.60
14.42
.55
.41
1
6
0.63
0.70
11.02
0.13
18.83
0
11
3
8
1.59
1.49
-6.21
0.28
18.76
0
12
5
9
9.09
7.62
-16.18
3.57
46.83
0
8
2
4
0.47
0.49
5.24
0:07
14.20
.07
.86
4
8
1.91
1.97
3.40
0.35
17.93
.22
.48 - o
6
8
11.40
10.40
-8.77
1.82
17.52
.78
.67
WATER LEGEND
1 - LAB PURE WATER
2 - DRINKING WATER
3 - SURFACE WATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON BERYLLIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) = 1.10692
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-OISTILLED)
2 .1543 ' -.0738
3 .2403 -.2182
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 167.76915 167.76915
REG(WATER/DISTILLED) 4 1.52294 .38073 3.02 .0207
0 ERROR 114 14.37090 .12606
I
ui
*" TOTAL 119 183.66299
** TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .1543 ( -.0934 , .4019) -.0738 ( -.2385 , .0909)
3 .2403 ( -.0108 , .4914) -.2182 ( -.3850 , -.0513)
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(INTERCEPTXSLOPE).
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR BERYLLIUM ANALYSIS BY HATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3 <
4 <
5
6 <
7
8 <
9
10
1
0.60
0.21
0.43
0.60* <
0.50* <
2.72*
0.30* <
0.33
0.50* <
0.53
0.43
2
0.45
0.17
0.11
0.60*
0.50* <
1.50*
0.30*
0.22
0.50* <
0.47
0.43
1
0.60
0.07 -
0.50 <
1.20
0.50*
1.00
1.30*
0.40
0.50* <
0.56
0.60
2
0.45
0.30* -
0.50*
0.70
0.50 <
1.00
1.00*
0.20
0.50* <
0.48
0.40
1
0.60
6.18* -
0.50 <
0.70 <
0.50* <
4.00*
1.50*
0.70
0.50* <
0.40
0.60
2
0.45
0.67*
0.50* <
0.60* <
0.50* <
1.00
1.20*
0.50
0.50* <
0.24
0.40
1
0.60
0.09 -
0.50* <
0.60* <
0.50* <
1.00 <
1.50*
0.40
0.50* <
0.52
0.60
2
0.45
0.01*
0.50*
0.60*
0.50*
0.50*
1.00*
0.30
0.50*
0.47
0.40
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR BERYLLIUM ANALYSIS BY HATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
o
Ul
oo
AMPUL NO:
TRUE CONC: 1
LAB NUMBER
1
2
3
4
5
6
7
8 < (
9
10
3
.52
.79
.74
.96
.09
>.40*
.85
.20
).50* <
1.20
1.74
4
1.83
2.75
2.29
1.85
1.41
9.20*
3.30
1.50
0.50* <
1.60
1.52
3
1.52
1.40
1.40
1.90
1.30
2.80*
3.50*
0.80
0.50* <
1.44
1.40
4
1.83
2.29
1.80
2.40
1.00
3.00
5.10*
1.10
0.50* <
1.86
2.00
3
1.52
1.60
1.60
1.70
1.10*
2.00
4.20*
1.70
0.50* <
1.20
1.40
4
1.83
*
1.61
2.00
2.10
1.40*
3.00*
5.20*
2.10
0.50* <
1.93
1.80
3
1.52
.27
.20
.40
.00
.00
3.70*
1.00
0.50* <
1.56
1.40
4
1.83
1.84
2.20
1.80
1.30
2.00
4.80*
1.20
0.50*
1.66
1.80
-------
ENVIRONMENTAL MONITORINO AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR BERYLLIUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
o
1
Ul
VD
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
.
5
8.70
6.71
11.50
10.80
7.10
34.80*
16.30
8.00
2.40*
7.65
8.70
6
10.90
6.99
13.90
13.40
8.80
40.20*
19.70
10.40
7.90*
8.40
10.90
5
8.70
8.72
8.10
11.10
6.00
7.00
24.00*
4.80
5.60*
9.55
8.00
6
10.90
12.45
10.00
13.90
7.60
10.00
19.00*
8.40
7.70*
12.20
10.00
5
8.70
10.40
9.60
12.00
7.00*
8.00
19.00*
9.60
6.50*
9.53
8.00
6
10.90
12.30
10.80
14.20
8.30*
14.00
24.00*
11.40
8.90*
20.30*
11.00
5
8.70
10.97
12.10
9.50
6.90
6.00
20.00*
4.40
7.60
9.51
8.00
6
10.90
10.73
11.30
11.60
8.90
8.00
26.00*
8.00
9.30
12.10
10.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR BERYLLIUM ANALYSES BY WATER TYPE
HATER 1
HATER 2
HATER 3
HATER 4
n
I
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD DEV, *
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (SREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD OEV. (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
I
5
0.60
0.39
-36.09
0.12
31.39
0.
26.
3
B
1.52
1.57
3.37
0.35
22.06
0.
21.
5
8
8.70
9.59
10.29
3.20
33.36
0.
6.
2
5
0.45
0.28
-37.50
0.16
57.37
09
76
4
8
1.83
2.03
10.79
0.69
34.08
38
39
6
8
10.90
11.56
6.07
4.06
35.12
72
82
1
7
0.60
0.62
2.41
0.38
60.85
0
23
3
7
1.52
1.38
-9.40
0.32
23.30
0
15
5
8
8.70
7.91
-9.09
1.99
25.16
0
6
2
6
0.45
0.55
22.02
0.27
50.25
.13
.05
4
8
1.83
1.93
5.53
0.66
34.32
.26
.52
6
8
10.90
10.57
-3.04
2.13
20.16
.55
.00
1
5
0.60
0.58
-3.97
0.13
22.48
0.
2.
3
7
1.52
1.60
5.26
0.25
15.73
0.
9.
5
7
8.70
9.59
10.23
1.39
14.45
1.
11.
2
4
0.45
0.53
19.42
0.33
61.30
02
93
4
6
1.83
1.92
5.10
0.19
9.91
16
16
6
6
10.90
12.28
12.69
1.50
12.21
22
17
1
5
0.60
0.52
-13.58
0.33
63.25
3
8
1.52
1.23
-19.16
0.22
17.61
5
9
8.70
8.33
-4.24
2.44
29.25
2
3
0.45
0.39
-12.95
0.09
21.91
0.05
11.84
4
8
1.83
1.72
-5.74
0.34
19.43
0.24
16.33
6
9
10.90
9.99
-8.33
1.54
15.38
0.96
10.51
HATER LEGEND
1 - LAB PURE HATER
2 - EFFLUENT 1
3 - EFFLUENT 2
4 - EFFLUENT 3
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON BERYLLIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) = 1.13352
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 .1623 * -.1312
3 .2424 -.0980
4 .0399 -.0771
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROR
REG(DISTILLED) 1 238.56398 238.56398
O REGfWATER/DISTILLED) 6 1.25327 .20888 1.86 .0919
^ ERROR 146 16.41387 .11242
t->
TOTAL 153 256.23112
** TABLE OF 95? CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .1623 ( -.0792 , .4037) -.1312 ( -.2937 , .0314)
3 .2424 ( -.0163 , .5011) -.0980 ( -.2728 , .0768)
4 .0399 ( -.2186 , .2984) -.0771 ( -.2483 , .0941)
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.
**
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR CADMIUM ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2 <
3 <
4
5
6
7
8 <
9
10
1
0.45
0.63
0.20* <
0.50* <
0.50
1.00*
0.50
0.50
0.50* <
0.36
0.60
2
0.79
0.85
0.20*
0.50*
1.00
2.00*
0.70
0.80
0.50* <
0.81
1.20
1
0.45
0.61
0.80
3.05*
1.10
2.00*
0.70
0.40
0.50* <
0.46
0.60
2
0.79
1.15
0.80
2.30* <
1.80
1.00
0.40
0.70
0.50* <
0.57
1.10
1
0.45
0.30
0.80
0.50*
0.60
1.00*
0.20
0.40
0.50* <
2.29*
0.40
2
0.79
0.56
1.30
4.20
O.«0
1.00*
0.30
0.70
0.50*
3.54
0.80
ro
-------
n
i
CTi
U>
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
4.55
5.66
4.60
2.85
5.10
4.00
4.40
3.50
3.60
3.27
5.00
LAB PURE WATER
4
5.32
5.64
4.30
4.70
5.50
5.00
5.40
4.50
4.40
2.90
6.00
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAM DATA FOR CADMIUM ANALYSIS BY HATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
DRINKING WATER
SURFACE WATER
3
4.55
4.61
5.20
6.40*
5.50
7.00
3.90
3.50
2.60*
4.04
5.00
4
5.32
5.06
10.10*
6.25*
5.50
6.00
4.90
3.90
3.80*
3.97
7.00
3
4.55
3.93
5.40
2.15
4.80
9.00*
4.50
3.80
2.00*
3.21
4.90
4
5.32
4.41
7.00
3.25
5.50
8.50*
4.40
4.40
1.00*
4.20
5.90
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR CADMIUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER DRINKING HATER SURFACE HATER
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
n
1
5
12.50
13.90
20.60
7.60
11.00
12.00
10.90
15.00
13.90
5.54
14.00
6
10.10
11.60
16.30
7.50
10.00
9.00
9.20
9.90
11.50
4.99
12.00
5
12.50
2.97
53.90*
25.10*
12.00
16.00
11.00
7.90
10.80*
10.20
14.00
6
10.10
9.15
12.70
10.40*
9.70
12.00
9.30
6.70
6.00*
7.28
12.00
5
12.50
14.05
16.90
10.20
12.00
25.00*
10.40
7.90
10.20*
12.60
9.90
6
10.10
12.55
15.90
22.10
10.00
19.00*
8.90
7.10
6.70*
7.82
9.90
-------
n
i
CTi
U1
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR CADMIUM ANALYSES BY HATER TYPE
WATER 1
WATER 2
WATER 3
LOW YOUOEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD OEV (S)
OVERALL REL STO OEV, t
SINGLE STO OEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUOEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO OEV, %
SINGLE STD OEV, (SR)
ANALYST REL DEV, %
1
6
0.45
0.51
13.19
0.10
18.45
0.
16.
3
10
4.55
4.20
-7.74
0.90
21.54
0.
10.
5
10
12.50
12.44
-0.45
4.16
33.40
1.
9.
2
6
0.79
0.89
12.94
0.18
20.05
11
32
4
10
5.32
4.83
-9.14
0.89
18.43
49
95
6
10
10.10
10.20
0.98
3.00
29.43
11
84
1
7
0.45
0.67
46.62
0.23
35.05
0.
30.
3
8
4.55
4.84
6.46
1.11
22.92
0.
13.
5
7
12.50
10.58
-15.35
4.25
40.19
2.
23.
2
8
0.79
0.94
18.84
0.43
46.17
25
79
4
7
5.32
5.19
-2.44
1.10
21.23
66
20
6
8
10.10
9.85
-2.44
2.23
22.60
37
18
1
6
0.45
0.45
-1.10
0.22
48.18
0
10
3
8
4.55
4.09
-10.19
1.05
25.65
0
7
5
8
12.50
11.74
-6.05
2.80
23. R8
3
. 30
2
8
0.79
1.52
92.79
1.48
97.36
.10
.19
4
8
5.32
4.88
-8.22
1.18
24.13
.36
.93
6
8
10.10
11.78
16.67
5.02
42.63
.53
.02
WATER LEGEND
1 - LAB PURE WATER
2 - DRINKING WATER
3 - SURFACE WATER
-------
I
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF MATER TYPE ON CADMIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE : GAMMA{ 1 ) = .91fl37
HATER INTERCEPT(WATER-DISTILLEO) SLOPE(WATER-DISTILLED)
2 .0751 . -.0390
3 -.0453 .0444
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLEO) 1 165.66889 165.66889
REG(WATER/DISTILLED) 4 .25561 .06390 .53 .7125
ERROR 128 15.37604 .12013
TOTAL 133 181.30054
** TABLE OF 95S CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .0751 ( -.1894 , .3396) -.0390 ( -.1905 , .1125)
3 -.0453 ( -.3150 , .2244) .0444 { -.1079 , .1967)
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.
I M V S: PAGE 15
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR CADMIUM ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8 <
9
10
1
0.43
0.80
0.44 <
5.22*
0.44
1.10
0.76
0.54
0.50* <
0.29*
0.54
2
0.76
1.12
0.20* <
2.94* <
0.87 -
2.20 N
0.44
0.76
0.50* <
0.75*
1.10
1
0.43
1.04*
0.20* <
0.50*
0.60* -
0.00* N
0.90
0.80
0.50*
0.34
0.80
2
0.76
1.66*
0.20*
7.90*
0.60*
0.00* N
2.20
0.30
1.10
0.66
0.80
1
0.43
0.60
0.30*
17.70*
0.40
0.00*
0.40
0.50
0.80
0.60
0.30
2
0.76
0.70
0.40*
1.10 <
O.QO
1.00
0.20
0.60
2.30*
0.71
0.60
1
0.43
0.44
0.20
0.50* <
0.50
1.00
1.10
0.40
10.00* <
0.19
0.50
2
0.76
0.94
0.60
0.50*
0.80
1.00
1.00
0.60
0.50*
0.39
0.80
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR CADMIUM ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER EFFLUENT 1 EFFLUENT 2 EFFLUENT 3
AMPUL NO: 343434 34
TRUE CONC: 4.35 5.09 4.35 5.09 4.35 5.09 4.35 5.09
LAB NUMBER
1 4.89 5.87 4.98* 5.54* 4.00 4.50 6.04 6.68
2 2.00 4.70 < O.?0* < 0.20* 2.30* 1.80* 3.70 1.10
3
4
5
6
7
8
9
10
n
i
a\
co
8.37*
4.20
5.40
4.60
3.80
3.30*
2.01*
4.60
9.30*
5.20
5.40
5.00
4.70
4.50*
3.92*
5.30
2.70
5.20
2.00
4.30
3.20
1.80
4.97
3.90
4.05
3.00
2.00
4.40
4.20
2.50
5.60
6.40
2.30
5.00
4.00
5.10
3.30
3.00
2.63
6.00
2.70
5.40
4.00
4.90
4.10
2.80
3.08
4.40
4.35
5.00
4.00
5.90
3.70
3.20
2.94
5.00
4.40
5.50
6.00
5.00
4.70
3.00
4.30
6.50
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR CADMIUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
n
i
(Ti
VO
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
12.00
10.70
18.10
13.90*
13.10
10.90
11.00
14.80
11.00*
10.10*
15.20
6
9.70
9.43
13.70
14.40*
10.90
9.80
9.10
8.50
7.60*
7.84*
10.90
12
14
8
14
10
8
11
10
5
7
13
5
.00
.62*
.90*
.30
.00
.00
.90
.80
.30
.83
.40
*
6
9.70
12.67*
5.00*
9.30
7.70
4.00
9.90
8.70
5.00
8.53
7.40
12.
13.
6.
23.
11.
8.
11.
8.
9.
6.
11.
5
00
90
10*
50*
00
00
50
20
80
21
40
6
9.70
7.80
3.50*
9.10
9.40
7.00
10.20
7.00
7.00
6.70
9.40
5
12.00
*
15.55
5.80
9.80
12.00
17.00
13.50
12.30
7.50
9.89
14.00
6
9.70
13.30
4.30
12.00
9.70
14.00
10.60
9.60
7.00
8.39
10.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR CADMIUM ANALYSES BY WATER TYPE
WATER 1 WATER 2 WATER 3 WATER 4
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, I
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
0 OVERALL REL STD DEV, %
1
o SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, *
SINGLE STD OEV, (SR)
ANALYST REL DEV, I
1
7
0.43
0.66
51.72
0.24
36.53
0
37
3
7
4.35
4.21
-3.15
1.10
26.07
0
12
5
7
12.00
13.40
11.67
2.79
20.82
1
11
2
6
0.76
1.08
42.89
0.60
55.66
.33
.60
4
7
5.09
5.17
1.52
0.41
8.02
.60
.82
6
7
9.70
10.33
6.52
1.73
16.74
.38
.66
1
4
0.43
0.71
63.22
0.25
35.37
0.
62.
3
8
4.35
3.51
-19.34
1.29
36.88
0.
25.
5
8
12.00
10.19
-15.07
3.04
29.86
1.
18.
2
5
0.76
1.01
33.69
0.72
71.51
54
34
4
8
5.09
4.02
-21.05
1.50
37.35
95
33
6
8
9.70
7.57
-22.00
2.07
27.37
61
10
1
7
0.43
0.51
18.23
0.17
32.59
3
9
4.35
3.93
-9.76
1.25
31.74
5
8
12.00
10.00
-16.66
2.45
24.51
2
8
0.76
0.73
-4.06
0.28
38.76
0.17
26.69
4
9
5.09
3.99
-21.68
0.95
23.74
0.50
12.67
6
9
9.70
8.18
-15.69
1.34
16.41
1.36
14.97
1
8
0.43
0.54
24.43
0.34
62.31
0
21
3
10
4.35
4.38
0.76
1.07
24.49
0
20
5
10
12.00
11.73
-2.22
3.52
29.%
1
11
2
8
0.76
0.77
1.22
0.22
28.70
.14
.44
4
10
5.09
4.72
-7.31
1.69
35.80
.95
.88
6
10
9.70
9.89
1.95
2.90
29.28
.22
.24
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 1
3 - EFFLUENT 2
4 - EFFLUENT 3
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF HATER TYPE ON CADMIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) = .91517
WATER INTERCEPT(WATER-DISTILLEO) SLOPE(WATER-DISTILLED)
2 -.0711 ' -.0991
3 -.2614 .0133
4 -.1847 .0648
** ANALYSIS OF VARIANCE **
SOURCE OF SDH OF SQUARES MEAN SQUARE F PROB
REG(OISTILLED) 1 220.80653 220.80653
_ REG(WATER/DISTILLED) 6 2.31937 .38656 3.39 .0035
I ERROR 171 19.50300 .11405
-g
M
TOTAL 178 242.62890
** TABLE OF 95? CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.0711 ( -.3770 , .2349) -.0991 ( -.2693 , .0710)
3 -.2614 ( -.5277 , .0049) .0133 ( -.1404 , .1670)
4 -.1847 ( -.4428 , .0734) .0648 ( -.0856 . .2152)
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 N01 THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR CHROMIUM ANALYSIS BY HATER TYPE
LOH YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER
DRINKING HATER
SURFACE HATER
AMPUL NO:
TRUE CONC:
LAR NUMBER
1
2
3
4
5
6
7
8
9
1°
0
1
-j
to
1
10.30
11.91
9.00
8.20
12.00
5.00
14.00*
11.00
12.00
9.69
11.00
2
13.50
13.15
11.00
12.40
14.00
6.00*
19.00*
14.00
13.00
14.60
14.00
1
10.30
9.40
11.00
4.60
20.00
195.00*
32.00*
14.00
9.00
12.60
10.00
2
13.50
19.60
11.00
6.30
18.00
266.00*
28.00
11.00
4.00
13.00
16.00
1
10.30
8.05
12.00
8.40
11.00
9.00
15.00*
10.00
7.20
13.60
13.00
2
13.50
12.31
13.00
9.00
13.00
9.00
19.00*
10.00
9.10
18.60
15.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAM DATA FOR CHROMIUM ANALYSIS BY WATER TYPE
MEDIUM YOUDEM PAIR. UNITS - UG/L
LAB PURE MATER DRINKING HATER SURFACE MATER
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
113.00
76.55
89.00
96.60
120.00
76.00
115.00*
62.00
110.00
136.00
124.00
4
95.90
73.35
76.00
84.50
110.00
91.00
104.00*
78.00
95.00
94.80
94.00
3
113.00
91.40
92.00
88.20
120.00
359.00*
172.00*
124.00
108.00
120.00
104.00
4
95.90
82.60
80.20
77.80
110.00
322.00*
152.00
124.00
101.00
100.00
84.00
3
113.00
79.00
130.00
84.70
120.00
48.00
156.00*
247.00*
98.00
117.00
104.00
4
95.90
69.40
95.00
73.10
110.00
7.00
124.00*
167.00
51.00
108.00
94.00
o
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR CHROMIUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
0
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
. 9
10
5
200.00
172.95
212.00
205.00
200.00
214.00
287.00*
204.00
190.00
189.00
224.00
6
246.00
217.05
264.00
228.00
230.00
192.00
325.00*
274.00
239.00
182.00
274.00
5
200.00
58.40*
233.00
194.00
220.00
338.00*
210.00
184.00
180.00
241.00
194.00
6
246.00
73.90*
227.00
252.00
220.00
666.00*
230.00
274.00
230.00
262.00
264.00
5
200.00
146.00
198.00
176.00
200.00
217.00
240.00*
167.00
167.00
195.00
194.00
6
246.00
198.00
229.00
209.00
230.00
230.00
272.00*
287.00
219.00
291.00
274.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR CHROMIUM ANALYSES BY WATER TYPE
WATER 1
HATER 2
WATER 3
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (*REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, I
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
9 OVERALL STD DEV (S)
^j OVERALL REL STD DEV, *
Ul
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO OEV (S)
OVERALL REL STO DEV, %
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
I
9
10.30
9.98
-3.13
2.32
23.23
0.
8.
3
9
113.00
98.91
-12.47
25.16
25.44
13.
14.
5
9
200.00
201.22
0.61
15.40
7.65
21.
9.
2
8
13.50
13.27
-1.71
1.16
8.72
97
39
4
9
95.90
88.52
-7.70
IK 69
13.20
13
01
6
9
246.00
233.34
-5.15
33.41
14.32
10
71
1
8
10.30
11.32
9.95
4.48
39.52
3
27
3
8
113.00
105.95
-6.24
14.39
13.58
4
4
5
8
200.00
207.00
3.50
22.70
10.96
24
10
2
9
13.50
14.10
4.44
7.29
51.73
;51
.61
4
9
95.90
101.29
5.62
24.52
24.21
.67
.51
6
8
246.00
244.88
-0.46
20.49
8.37
.30
.75
1
9
10.30
10.25
-0.49
2.28
22.25
1
11
3
8
113.00
97.59
-13.64
26.57
27.23
11
12
5
9
200.00
184.44
-7.78
21.93
11.89
24
11
2
9
13.50
12.11
-10.28
3.26
26.90
.25
.16
4
9
95.90
86.06
-10.27
44.26
51.44
.57
.60
6
9
246.00
240.78
-2.12
34.36
14.27
.98
.75
WATER LEGEND
1 - LAB PURE WATER
2 - DRINKING WATER
3 - SURFACE WATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF HATER TYPE ON CHROMIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMAf1) = 1.00212
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 -.0270 .0014
3 -.0054 -.0127
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 241.26772 241.26772
REG(WATERXOISTILLED) 4 .10228 .02557 .30 .8745
ERROR 141 11.83424 .08393
I
oi TOTAL 146 253.20425
** TABLE OF 95S CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
IMTERCEPT(WATER-OISTILLED) SLOPE(WATER-OISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.0270 ( -.5276 , .4735) .0014 ( -.1139, .1166)
3 -.0054 { -.4972 , .4863) -.0127 ( -.1254 , .0999)
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.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR CHROMIUM ANALYSIS BY HATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
9.87
8.87
9.80
6.90
10.90
5.40*
10.90*
4.40
6.50
14.60
10.90
2
12.90
11.24
10.90
7.90
13.00
6.50*
14.00*
7.60
12.00
9.00
17.00
1
9.87
11.55
1.20
7.10
11.00
24.00
19.00*
119.00*
10.00
11.60
10.00
2
12.90
16.35
2.70
7.70
6.00
20.00
35.00* N
59.00*
6.00
13.20
10.00
1
9.87
12.60
8.00
10.70
15.00
5.00*
0.00* N
32.00*
6.00
14.30
5.00
2
12.00
19.90
10.00
10.50 <
16.00
4.00*
0.00*
19.00
10.00
16.40
9.00
1
9.87
*
4.19*
11.00
4.10* <
12.00
8.00
23.00*
7.00
7.00
12.90*
9.00
2
12.90
7.62*
12.00
4.10*
13.00
10.00
22.00*
7.00
6.00
18.80*
12.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR CHROMIUM ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
108.00
42.34
92.40
86.10
100.00
65.00*
140.00*
646.00*
103.00
150.00
113.00
4
91.70
22.77*
82.60
73.50
87.00
70.00*
147.00*
483.00*
77.00
66.10
91.00
3
108.00
86.15
96.80
74.40
98.00
4.00*
147.00*
109.00
97.00
84.00
110.00
4
91.70
72.30
85.60
67.40
110.00
2.00*
139.00*
109.00
89.00
69.70
flo.oo
3
108.00
97.00
101.00
90.20
100.00
33.00*
149.00
192.00*
115.00
125.00
100.00
4
91.70
85.00
70.00
69.80
83.00
79.00*
71.00
172.00*
90.00
61.10
80.00
3
108.00
»
25.70*
89.00
76.10
110.00
135.00
166.00*
127.00
52.00
146.00*
97.00
4
91.70
19.10*
78.00
63.20
94.00
114.00
134.00*
127.00
50.00
107.00*
102.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR CHROMIUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
192.00
120.71
166.00
140.00
185.00
121.00*
282.00*
148.00
175.00
187.10
189.00
6
236.00
175.28
140.00
202.00
228.00
109.00*
323.00*
189.00
235.00
310.00
265.00
5
192.00
106.70
181.00
256.00
200.00
11.00
279.00*
169.00
174.00
140.00
200.00
6
236.00
131.90
206.00
197.00
230.00
17.00*
296.00*
229.00
228.00
274.00
220.00
5
192.00
170.00
253.00
166.00
200.00
3.00*
361.00*
162.00
178.00
186.00
205.00
6
236.00
199.00
224.00
214.00
210.00
174.00*
289.00
242.00
215.00
312.00
215.00
5
192.00
*
134.00*
187.00
165.00
210.00
117.00
240.00*
137.00
140.00
267.00*
192.00
6
236.00
175.00*
246.00
211.00
250.00
216.00
269.00*
207.00
194.00
300.00*
222.00
vo
-------
o
I
oo
o
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR CHROMIUM ANALYSES BY WATER TYPE
HATER 1
WATER 2
WATER 3
WATER 4
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO OEV (S)
OVERALL REL STO OEV, I
SINGLE STD OEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO OEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, t
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 1
3 - EFFLUENT 2
4 - EFFLUENT 3
1
8
9.87
9.11
-7.71
3.18
34.95
2.
25.
3
7
108.00
98.12
-9.15
32.22
32.84
19.
22.
5
8
192.00
163.85
-14.66
25.16
15.35
29.
15.
2
8
12.90
11.08
-14.11
3.07
27.75
54
15
4
6
91.70
79.53
-13.27
9.16
11.52
90
40
6
8
236.00
218.03
-7.61
53.54
24.56
30
35
1
8
9.87
10.81
9.49
6.35
58.80
3
8
108.00
94.42
-12.58
12.30
13.02
5
9
192.00
159.74
-16.80
69.44
43.47
2
8
12.90
10.24
-20.59
5.86
57.24
2.43
23.09
4
8
91.70
85.37
-6.90
16.67
19.53
8.55
9.52
6
8
236.00
214.49
-9.12
40.36
18.82
37.85
20.23
1
7
9.87
10.23
3.63
3.99
38.98
1
14
3
8
108.00
109.65
1.53
19.32
17.62
17
18
5
8
192.00
190.00
-1.04
29.79
15.68
33
15
2
8
12.90
13.85
7.36
4.45
32.13
.74
.48
4
8
91.70
76.24
-16.66
9.73
12.77
.05
.35
6
9
236.00
235.56
-0.19
39.01
16.56
.53
.76
1
6
9.87
9.00
-8.81
2.10
23.31
1.
10.
3
7
108.00
98.01
-9.25
28.96
29.55
6.
7.
5
7
1<»2.00
164.00
-14.58
34.02
20.74
16.
8.
2
6
12.90
10.00
-22.48
2.90
28.98
00
53
4
7
91.70
89.74
-2.13
27.59
30.74
67
11
6
7
236.00
220.86
-6.42
20. 4R
9.27
03
33
-------
ENVIRONMENTAL MONITORING AND SUPPORT LARORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF HATER TYPE ON CHROMIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) = 1.00700
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 -.0770 .0035
3 .1833 -.0194
4 -.0759 .0265
** ANALYSIS OF VARIANCE **
SOURCE DF SIM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 284.98911 284.98911
n REG(WATER/DISTILLEO) 6 .73232 .12205 .86 .5277
I ERROR 165 23.49018 .14236
oo
M
TOTAL 172 309.21161
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.0770 ( -.7831 , .6290) .0035 ( -.1598 , .1668)
3 .1833 ( -.5293 , .8959) -.0194 ( -.1845 , .1457)
4 -.0759 ( -.8359 , .6P42) .0265 ( -.1473 . .2002)
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AMD THE CORRESPONDING HASTE WATER FOR THE ASSOCIATED PARAMETER(INTERCEPT/SLOPE).
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE MOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR COBALT ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
o
1
00
to
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
31.50
31.36
30.00
33.80
23.00
46.00*
29.00
32.00
23.00
21.90
30.00
2
29.70
29.73
27.00
27.40
21.00
38.00*
31.00
29.00
26.00
28.70
35.00
1
31.50
496.00*
26.00
32.20
27.00
38.00
29.00
26.00
15.00
25.00
25.00
2
29.70
404.00*
30.00
31.50
30.00
37.00
32.00
24.00
10.00
25.60
45.00
1
31.50
35.00
30.00
27.50
34.00
34.00
32.00
22.00*
21.00
28.20
30.00
2
29.70
32.00
26.00
25.70
31.00
31.00
38.00
22.00*
20.00
27.70
40.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR COBALT ANALYSIS BY HATER TYPE
MEDIUM YOUDEN PAIR. UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
n
i
00
u>
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
186.00
206.33
162.00
195.00
160.00
196.00*
225.00
176.00
140.00
145.00
90.00
4
216.00
238.13
186.00
193.00
180.00
236.00*
254.00
196.00
150.00
216.00
100.00
3
186.00
218.00
216.00
199.00
180.00
205.00
246.00
128.00
165.00
177.00
400.00*
4
216.00
265.00
198.00
225.00
220.00
236.00
213.00
151.00
250.00
1P4.00
250.00
3
186.00
175.00
198.00
147.00
170.00
180.00
235.00
124.00*
170.00
161.00
150.00
4
216.00
189.00
198.00
168.00
200.00
228.00
216.00
143.00*
204.00
227.00
150.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR COBALT ANALYSIS BY HATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
o
1
00
£>.
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5 .
420.00
377.43
400.00
472.00
360.00
563.00*
455.00
368.00
364.00
329.00
200.00
6
314.00
304.03'
312.00
278.00
260.00
423.00*
403.00
302.00
244.00
294.00
125.00
5
420.00
35.30*
392.00
411.00
390.00
468.00
399.00
352.00
340.00
310.00
300.00
6
314.00
38.30
277.00
314.00
310.00
348.00
335.00
256.00
190.00
264.00
50.00
5
420.00
399.00
343.00
262.00
440.00
472.00
428.00
340.00*
376.00
409.00
400.00
6
314.00
299.00
315.00
239.00
330.00
283.00
436.00
256.00*
294.00
272.00
145.00
-------
n
i
00
Ln
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR COBALT ANALYSES BY WATER TYPE
WATER 1
WATER 2
WATER 3
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (IREL ERROR)
OVERALL STD OEV (S)
OVERALL REL STO DEV, %
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACYUREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, t
1
9
31.50
28.23
-10.38
4.43
15.68
3
10
3
9
186.00
166.59
-10.43
40.30
24.19
14
8
5
9
420.00
369.49
-12.03
78.50
21.25
32
10
2
9
29.70
28.31
-4.67
3.81
13.45
.06
.82
4
9
216.00
190.35
-11.88
46.03
24.18
.57
.16
6
9
314.00
280.23
-10.76
73.43
26.20
.94
.14
1
9
31.50
27.02
-14.22
6.19
22.89
5
17
3
9
186.00
192.67
3.58
34.60
17.96
24
11
5
9
420.00
373.56
-11.06
53.17
14.23
42
13
2
9
29.70
29.46
-0.82
9.57
32.50
.07
.96
4
10
216.00
220.20
1.94
33.46
15.19
.52
.88
6
10
314.00
238.23
-24.13
111.81
46.93
.36
.85
1
9
31.50
30.19
-4.16
4.35
14.40
3.
11.
3
9
186.00
176.22
-5.26
26.92
15.27
18.
9.
5
9
420.00
392.11
-6.64
61.20
15.61
59.
17.
2
9
29.70
30.16
1.53
6.22
20.63
39
22
4
9
216.00
197.78
-8.44
25.%
13.12
59
94
6
9
314.00
290.33
-7.54
77.17
26.58
42
41
WATER LEGEND
1 - LAB PURE WATER
2 - DRINKING WATER
3 - SURFACE HATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON COBALT ANALYSIS
** POINT ESTIMATES **
DISTILLED HATER SLOPE:GAMMA(1) = .97236
MATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 -.0125 . -.0051
3 .0363 .0002
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(OISTILLED) 1 171.82590 171.82590
REG(HATER/DISTILLED) 4 .15006 .03752 .47 .7600
ERROR 149 11.97486 .08037
O
I
o> TOTAL 154 183.95082
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.0125 ( -.6549 , .6300) -.0051 ( -.1335 , .1233)
3 .0363 ( -.6067 , .6794) .0002 ( -.1286 , .1291)
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS HO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED HATER 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.
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS*BY AA ***
RAH DATA FOR COBALT ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
EFFLUENT 1
n
i
CO
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
30.20
30.10
28.80
32.50
22.10
44.10*
27.80
30.70
22.10
21.00
28.80
2
24.80
25.00
22.70
23.00
17.60
31.90*
26.00
24.40
21.80
24.10
29.40
1
30.20
33.03
33.00
29.00
21.00
43.00
37.00*
32.00
25.00
30.90*
35.00
2
24.80
28.09
21.00
24.30
30.00
31.00
31.00*
23.00
27.00
32.90*
25.00
-------
LAB PURE HATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR COBALT ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
EFFLUENT 1
n
i
00
00
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
203.00
225.00
177.00
213.00
174.00
214.00*
245.00
192.00
153.00
158.00
98.00
4
164.00
181.00
141.00
147.00
137.00
179.00*
193.00
149.00
114.00
164.00
76.00
3
203.00
208.00
203.00
198.00
160.00
110.00
253.00*
160.00
180.00
386.00*
250.00
4
164.00
164.00
167.00
138.00
200.00
26.00*
227.00*
126.00
154.00
235.00*
160.00
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR COBALT ANALYSIS BY HATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
EFFLUENT 1
n
i
00
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
309.00
287.00
304.00
359.00
274.00
428.00*
346.00
280.00
277.00
250.00
152.00
6
407.00
395.00
406.00
361.00
338.00
550.00*
524.00
393.00
317.00
382.00
163.00
5
309.00
289.00
312.00
306.00
340.00
214.00
367.00*
190.00
290.00
541.00*
160.00
6
407.00
382.00
373.00
318.00
420.00
394.00
444.00*
252.00
380.00
667.00*
400.00
-------
o
I
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR COUALT ANALYSES BY WATER TYPE
WATER 1 WATER 2
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD OEV, %
SINGLE STO DEV, (SR)
ANALYST REL DEV. %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY(JREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, I
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
1
9
30.20
27.10
-10.26
4.25
15.69
2
11
3
9
203.00
181.67
-10.51
43.93
24.18
14
8
5
9
309.00
281.00
-9.06
59.73
21.26
41
12
2
9
24.80
23.78
-4.12
3.21
13.50
.82
.09
4
9
164.00
144.67
-11.79
34.97
24.17
.21
.71
6
9
407.00
364.33
-10.48
95.38
26.18
.28
.79
1
8
30.20
31.48
4.23
6.67
21.18
5
18
3
8
203.00
183.63
-9.54
41.63
22.67
2R
16
5
8
309.00
262.63
-15.01
65.38
24.89
51
16
2
8
24.80
26.17
5.54
3.46
13.24
.24
.17
4
7
164.00
158.43
-3.40
23.54
14.86
.04
.40
6
8
407.00
364.88
-10.35
54.31
14.88
.56
.43
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 1
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON COBALT ANALYSIS
** POINT ESTIMATES **
DISTILLED HATER SLOPE:GAMMA(1) = .97650
WATER INTERCEPT(HATER-DISTILLEn) SLOPE(WATER-DISTILLED)
2 .3144 f -.0479
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(OISTILLED) 1 110.50401 110.50401
REG(WATER/DISTILLEO) 2 .21979 .10990 2.65 .0763
ERROR 88 3.64980 .04148
O
TOTAL 91 114.37361
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
INTERCEPT(WATER-OISTILLED) SLOPE(WATER-OISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .3144 ( -.0957 , .7244) -.0479 { -.1309 , .0350)
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.
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR COBALT ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
EFFLUENT 2
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
21.10
21.00
20.10
15.40
15.40
30.80*
19.40
21.40
15.40
14.70
20.10
2
25.00
25.00
22.70
23.00
17.60
31.90*
26.00
24.40
21.80
24.10
29.40
1
21.10
21.70
21.00
21.10
18.00
27.00
31.00*
19.00
31.00
19.60
15.00*
2
25.00
25.50
19.00
21.10
19.00
26.00
38.00*
20.00
14.00
28.40
20.00*
K)
-------
LAB PURE HATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR COBALT ANALYSIS BY HATER TYPE
- MEDIUM YOUDEN PAIR, UNITS - UG/L
EFFLUENT 2
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
250.00
276.00
217.00
261.00
214.00
263.00*
302.00
236.00
1R8.00
194.00
121.00
4
212.00
233.00
182.00
189.00
176.00
231.00*
249.00
192.00
147.00
212.00
98.00
3
250.00
270.00
239.00
191.00
210.00
243.00
271.00*
210.00
300.00
252.00
200.00*
4
212.00
237.00
198.00
199.00
450.00*
187.00
221.00*
176.00
210.00
200.00
150.00*
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAM DATA FOR COBALT ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 2
0
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
q
10
5
461.00
415.00
440.00
519.00
396.00
619.00*
501.00
405.00
400.00
362.00
220.00
6
403.00
389.00
399.00
356.00
333.00
541.00*
516.00
387.00
312.00
376.00
160.00
5
461.00
435.00
473.00
350.00
450.00
593.00
497.00*
396.00
370.00
474.00
250.00*
6
403.00
392.00
308.00
363.00
400.00
451.00
447.00
362.00
380.00
434.00
200.00'
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR COBALT ANALYSES BY WATER TYPE
HATER 1 WATER 2
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, I
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (IREL ERROR)
H OVERALL STD DEV (S)
.J, OVERALL REL STD DEV, «
Ul
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (SREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
I
9
21.10
18.10
-14.22
2.79
15.43
1.
0.
3
0
250.00
223.22
-10.71
53.91
24.15
17.
8.
5
9
461.00
406.44
-11.83
86.38
21.25
39.
10.
2
9
25.00
23.78
-4.89
3.21
13.50
99
52
4
9
212.00
186.44
-12.05
45.11
24.19
33
46
6
9
403.00
358.67
-11.00
94.02
26.21
08
22
1
8
21.10
22.30
5.69
4.44
19.91
5
23
3
8
250.00
239.38
-4.25
35.56
14.86
20
9
5
8
461.00
442.63
-3.99
76.21
17.22
45
11
2
8
25.00
21.62
-13.50
4.70
21.75
.24
.85
4
7
212.00
201.00
-5.19
19.20
9.55
.90
.49
6
8
403.00
386.25
-4.16
44.70
11.57
.78
.05
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 2
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON COBALT ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMAf1) = .98610
HATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 -.0343 . .0156
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(OISTILLED) 1 160.33999 160.33999
REG(WATERXOISTILLED) 2 .04642 .02321 .79 .4584
ERROR 88 2.59586 .02950
n
I TOTAL 91 162.98227
-------
LAB PURE HATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR COBALT ANALYSIS BY HATER TYPE
LOH YOUDEN PAIR, UNITS - UG/L
EFFLUENT 3
0
1
VD
-o
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
29.30
29.20
27.90
31.40
21.40
42.80*
28.80
27.00
24.20
20.40
27.90
2
34.70
34.80
31.60
32.10
24.60
44.50*
36.30
33.90
30.40
33.60
41.00
1
29.30
21.40
24.00
30.80
27.00
46.00*
49.00*
29.00
27.00
36.40
20.00
2
34.70
26.50
24.00
25.40
33.00
45.00*
42.00*
30.00
18.00
35.10
55.00*
-------
LAB PURE MATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR COBALT ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
EFFLUENT 3
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
211.00
233.00
183.00
220.00
181.00
221.00*
254.00
199.00
158.00
164.00
102.00
4
166.00
183.00
143.00
149.00
139.00
Ifl2.00*
196.00
151.00
116.00
166.00
77.00
3
211.00
196.00
167.00
194.00
200.00
233.00*
242.00*
157.00
200.00
169.00
160.00
4
166.00
156.00
138.00
135.00
160.00
169.00*
205.00*
125.00
390.00*
157.00
50.00*
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR COBALT ANALYSIS BY WATER TYPE
HIGH YOUOEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 3
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
435.00
393.00
416.00
491.00
374.00
586.00*
473.00
383.00
379.00
342.00
208.00
6
326.00
316.00
325.00
289.00
270.00
440.00*
419.00
314.00
254.00
306.00
130.00
5
435.00
398.00
1060.00*
345.00
420.00
452.00*
441.00*
298.00
310.00
396.00
150.00
6
326.00
304.00
839.00*
261.00
320.00
340.00*
324.00*
218.00
270.00
254.00
50.00*
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR COBALT ANALYSES BY HATER TYPE
WATER 1 HATER 2
n
i
h~*
O
0
LOU YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (IREL ERROR)
OVERALL STO OEV (S)
OVERALL REL STD DEV, t
SINGLE STD DEV, (SR)
ANALYST REL DEV, t
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD DEV, *
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (SREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, S
SINGLE STD OEV, (SR)
ANALYST REL OEV, %
1
9
29.30
26.47
-9.67
3.70
13.96
2
10
3
9
211.00
1*8.22
-10.80
45. 38
24.11
14
8
5
9
435.00
384.33
-11.65
81.65
21.25
34
10
2
9
34.70
33.14
-4.48
4.46
13.46
.99
.02
4
9
166.00
146.67
-11.65
35.39
24.13
.63
.74
6
9
326.00
291.44
-10.60
76.36
26.20
.33
.16
1
8
29.30
26.95
-8.02
5.29
19.64
3.
13.
3
8
211.00
1R0.38
-14.51
18.78
10.41
10.
6.
5
7
435.00
331.00
-23.91
92.31
27.89
23.
7.
2
7
34.70
27.43
-20.%
5.80
21.16
80
97
4
6
166.00
145.17
-12.55
14.41
9.93
95
73
6
6
326.00
271.17
-16.82
36.5B
13.49
36
76
HATER LEGEND
1 - LAB PURE HATER
2 - EFFLUENT 3
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF HATER TYPE ON COBALT ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMHA(1) - .97208
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 -.0614 ' .0001
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLEO) 1 100.44051 100.44051
REG(WATER/D1STILLED) 2 .08265 .04133 1.30 .2770
ERROR R4 2.66309 .03170
O
I
o TOTAL 87 103.18626
** TABLE OF 95S CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.0614 ( -.4484 , .3256) .0001 { -.0779 , .0780)
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 PARAMETERHNTERCEPT/SLOPE).
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENV1ROWENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR COPPER ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR. UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
AMPUL NO: 1
TRUE CONC: 10.60
2
12.20
1
10.60
2
12.20
1
10.60
2
12.20
LAB NUMBER
0
I
o
K)
1
2
3
4
5
6
7
R
9
10
10.35
15.00
9.30
9.00
5.00
16.00
10.00
4.40
2.40*
11.00
11. nz
17.00 <
10.20
11.00
9.00
11.00
15.00 -
5.60
3.50*
14.00
44.00
8.00* <
15.00
9.00
32.00
14.00
22.00*
8.70
12.80
11.00
23.50
8.00*
14.40
12.00
22.00
15.00
8.00*
4.60
11.30
11.00
13.00
38.00*
11.30
9.00
14.00
12.00
15.00
5.80
2.70*
14.00
15.40
12.00
9.70
8.00
8.00
13.00
7.00
4.30
3.60*
14.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR COPPER ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
n
i
i »
r^
o
U)
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
72.70
88.00*
71.00
73.00
68.00
73.00
71.00
70.00
69.30
29.40*
78.00
4
97.30
109.00
104.00
95.80
87.00
77.00
115.00
94.00
53.30
38.40*
98.00
3
72.70
79.00
< 8.00*
73.30
68.00
17.00
218.00*
38.00*
63.00
42.50
61.00
4
97.30
90.00
0.00*
93.20
89.00
20.00
171.00
38.00*
84.00
56.90
86.00
3
72.70
64.20
66.00
70.50
61.00
96.00
107.00
53.00
63.60
33.40*
80.00
4
97.30
88.00
87.00
86.00
85.00
12R.OO
118.00
77.00
59.70
48.20*
90.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR COPPER ANALYSIS BY WATER TYPE
HIGH YOUOEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
O
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
205.00
198.20
407.00
202.00
180.00
111.00
216.00
15.00
185.00
59.00*
208.00
fi
245.00
247.30
232.00
246.00
200.00
212.00
262.00
17.00*
222.00
64.00*
26Q.OO
5
205.00
195.00
200.00
174.00
190.00
386.00
243.00
148.00*
170.00
388.00
206.00
6
245.00
254.00
295.00
202.00
230.00
352.00
269.00
148.00*
210.00
176.00
256.00
5
205.00
211.00
216.00
192.00
200.00
262.00
267.00
172.00
209.00
100.00*
205.00
6
245.00
244.00
230.00
242.00
220.00
309.00
346.00
192.00
245.00
119.00*
235.00
-------
n
i
(-
o
un
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR COPPER ANALYSES BY WATER TYPE
WATER 1
WATER 2
WATER 3
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, t
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (SREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, »
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, «
SINGLE STD DEV, (SR)
ANALYST REL DEV, *
1
9
10.60
10.01
-5.61
3.87
38.70
2
18
3
8
72.70
71.66
-1.43
3.08
4.30
12
15
5
9
205.00
191.36
-6.66
103.24
53.95
58
27
2
9
12.20
11.62
-4.72
3.39
29.17
.00
.47
4
9
97.30
92.57
-4.86
18.58
20.07
.85
.65
6
8
245.00
236.16
-3.61
23.94
10.14
.87
.54
1
8
10.60
18.31
72.76
12.76
69.68
5.
33.
3
7
72.70
57.69
-20.65
21.33
36.98
5.
7.
5
9
205.00
239.11
16.64
86.43
36.15
63.
26.
2
8
12.20
14.22
16.60
6.14
43.14
45
51
4
8
97.30
86.26
-11.34
42.27
49.00
33
41
6
9
245.00
249.33
1.77
53.17
21.33
65
06
1
8
10.60
11.76
10.97
3.06
26.00
2
22
3
9
72.70
73.48
1.07
17.67
24.04
7
9
5
9
205.00
214.89
4.82
30.96
14.41
14
6
2
9
12.20
10.16
-16.76
3.67
36.10
.47
.56
4
9
97.30
90.97
-6.51
20.50
22.53
.53
.16
6
9
245.00
251.44
2.63
47.03
18.70
.15
.07
WATER LEGEND
1 - LAB PURE WATER
2 - DRINKING WATER
3 - SURFACE WATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON COPPER ANALYSIS
** POINT ESTIMATES **
DISTILLED MATER SLOPE:GAMMA(1) « .98393
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLEO)
2 .4070 -.0696
3 -.1206 ' .0481
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 228.67460 228.67460
REG(WATER/DISTILLED) 4 .89276 .22319 1.49 .2083
ERROR 139 20.81268 .14973
O
I
o TOTAL 144 250.38004
** TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-OISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .4070 ( -.2579 , 1.0719) -.0696 ( -.2233 , .0840)
3 -.1206 ( -.7709 , .5297) .0481 ( -.1039 , .2001)
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.
-------
n
i
M
O
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR COPPER ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 1 EFFLUENT 3
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
10.10
*
17.60*
3.00
3.90
14.00
10. 00
19.00
6.00
2.80
0.50* -
2
11.70
*
21.70*
12.00
16.30
15.00
2.00
14.00
7.00
4.90
1.70*
1
10.10
9.89
14.30
8.90
8.60
4. 80
15.30
9.60
4.20
2.30*
10.50
2
11.70
11.29
16.20 <
9.70 <
10.50
8.60
10.50
14.30 -
5.40
3.30*
13.40
1
10.10
2.90*
8.00* <
3.90* <
3.00
16.00 <
10. 00
12.00* -
23.20
1.20
5.00 <
2
11.70
12.80*
8.00*
3.W*
2.00
1.00*
12.00
12.00*
16.30
4.00
1.00*
-------
o
I
M
O
00
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR COPPER ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 1 EFFLUENT 3
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
69.60
*
111.00*
67.00
67.50
78.00
79.00
65.00
53.00
33.50
23.00*
4
93.00
*
138.00*
90.00
91.10
93.00
89.00
92.00
69.00
77.30
34.70*
3
69.60
84.10*
67.80
69.70
65.00
69.70
67.80
66.90
66.20
28.10*
75.00
' 4
93.00
104.00
99.30
91.50
83.10
73.50
110.00
89.80
50.90
36.70*
94.00
3
69.60
98.40*
33.00
35.30
94.00
94.00
64.00
18.00
78.00
18.00
55.00
4
93.00
132.00*
60.00
55.30
84.00
86.00
83.00
48.00
91.00
25.80
75.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAM DATA FOR COPPER ANALYSIS BY HATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAR PURE WATER EFFLUENT 1 EFFLUENT 3
o
1
AHPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
196.00
*
292.00*
202.00
146.00
200.00
176.00
195.00
153.00
141.00
92.00*
6
234.00
*
361.00*
210.00
197.00
240.00
38.00*
232.00
263.00
189.00
112.00*
5
196.00
189.00
389.00
193.00
172.00
106.00
206.00
14.30
177.00
56.40*
199.00
6
234.00
236.00
222.00
235.00
191.00
202.00
250.00
16.20*
212.00
61.00*
256.00
5
196.00
307.00*
139.00
123.00
200.00
195.00
177.00
168.00
170.00
102.00
195.00
6
234.00
353.00*
175.00
164.00
310.00
315.00
214.00
208.00
228.00
122.00
225.00
-------
o
I
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR COPPER ANALYSES BY WATER TYPE
WATER 1
WATER 2
WATER 3
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (tREL ERROR)
OVERALL STO OEV (S)
OVERALL REL STO DEV, t
SINGLE STD DEV, (SR)
ANALYST REL OEV. %
MEDIUM YOUDEM PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY ttREL ERROR)
OVERALL STD OEV (S)
OVERALL REL STO DEV, *
SINGLE STO DEV, (SR)
ANALYST REL DEV, t
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE COHC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD OEV, *
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
1
7
10.10
8.39
-16.97
6.23
74.28
5
54
3
7
69.60
63.29
-9.07
15.76
24.91
7
10
5
7
196.00
173.29
-11.59
26.51
15.30
23
12
2
7
11.70
10.17
-13.06
5.53
54.37
.Ofi
.59
4
7
93.00
65.91
-7.62
9.13
10.63
.80
.46
6
6
234.00
221.83
-5.20
28.15
12.69
.73
.01
1
9
10.10
9.57
-5.29
3.R9
38.62
1
18
3
8
69.60
68.51
-1.56
3.08
4.49
12
15
5
9
196.00
182.81
-6.73
OT.68
53.98
56
27
2
9
11.70
11.10
-5.14
3.22
29.02
.91
.44
4
9
93.00
88.46
-4.89
17.78
20.10
.30
.67
6
8
234.00
225.50
-3.63
22.89
10.15
.13
.49
1
6
10.10
9.73
-3.63
8.50
87.33
3
33
3
9
69.60
54.37
-21.89
30.12
55.40
10
16
5
9
196.00
163.22
-16.72
34.61
21.21
25
13
2
4
11.70
8.57
-26.71
.6.72
78.39
.11
.98
4
9
93.00
67.57
-27.35
21.76
32.20
.05
.48
6
9
234.00
217.89
-6.89
63.36
29.08
.27
.26
WATER LEGEND
1 - LAR PURE WATER
2 - EFFLUENT 1
3 - EFFLUENT 3
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON COPPER ANALYSIS
** POINT ESTIMATES **
DISTILLED MATER SLOPE:GAMMA(1) « 1.10921
WATER INTERCEPT(WATER-OISTILLED) SLOPE(WATER-OISTILLED)
2 .4282 / -.1241
3 -.1881 -.0059
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 225.27030 225.27030
REGIWATER/DISTILLED) 4 1.53943 .38486 1.79 .1346
ERROR 124 26.63094 .21477
O
I
M TOTAL 129 253.44067
** TABLE OF 951 CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
INTERCEPT(WATER-DISTILLEO) SLOPE(WATER-DISTILLEO)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .42B2 ( -.3942 , 1.2505) -.1241 ( -.31B5 , .0703)
3 -.1881 ( -1.1104 , .7343) -.0059 ( -.2181 , .2063)
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.
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LAIJORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAM DATA FOR COPPER ANALYSIS BY WATER TYPE
LOW YOIIOEN PAIR, UNITS - MG/L
EFFLUENT 2
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
0.36
0.39
0.39
0.30
0.29
0.35
0.28
0.03*
0.32
0.11*
0.32
2
0.30
0.30
0.38
0.23
0.28
0.27
0.30
0.02*
0.27
0.15*
0.30
1
0.36
0.31
0.24
0.32
0.24
0.49*
0.26
0.24
0.50*
0.22*
0.25
2
0.30
0.27
0.21
0.27
0.22
0.44*
0.25
0.19
0.28
0.12*
0.30
-------
ENVIRONMENTAL MONITORING AMD SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
***.EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR COPPER ANALYSIS BY HATER TYPE
MEDIUM YOUDEN PAIR, UNITS - MG/L
LAB PURE HATER EFFLUENT 2
0
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
0.65
0.65
0.72
0.66
0.41
0.54
0.55
0.06*
0.57
0.26*
0.65
4
0.55
0.56
0.56
0.57
0.33*
0.56
0.54
0.05*
0.50
0.01*
0.54
3
0.65
0.61
0.53
0.72
0.41
0.79*
0.54
0.30
0.64
0.46*
0.50
4
0.55
0.52
0.63
0.58
0.51
0.71*
0.4R
0.37
0.53
0.35*
0.50
-------
LAB PURE MATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR COPPER ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - MG/L
EFFLUENT 2
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
B
9
10
5
1.30
.40
.3B
.35
.19
.18
.21
0.11*
1.07
D.77*
1.08
6
1.67
1.78
1.44
1.8«
1.19
LSI
1.41
0.13*
1.23
0.81*
1.83
5 6
1.30 1.67
.45 .74
.29 .67
.29 .70
.10 .50
.60* .81*
.07 .43
.20 .50
.36 .64
.01* 0.95*
.60 1.80
o
I
-------
o
ENVIRONMENTAL MONITORING AND SUPPORT LARORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS RY AA ***
STATISTICAL SUMMARY FOR COPPER ANALYSES BY WATER TYPE
HATER 1 WATER 2
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD OEV, t
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY (tREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD OEV, t
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY (IREL ERROR)
OVERALL STO OEV (S)
OVERALL REL STO DEV, t
SINGLE STD DEV, (SR)
ANALYST REL DEV, *
1
8
0.36
0.33
-7.54
0.04
12.85
3
R
0.65
0.60
-8.06
0.10
16.28
5
8
1.30
1.23
-5.27
0.13
10.71
2
8
0.30
0.29
-3.42
0.04
14.35
0.03
8.23
4
7
0.55
0.55
-1.19
0.02
4.41
0.04
7.69
6
8
1.67
1.53
-8.14
0.27
17.50
0.18
12.99
1
7
0.36
0.27
-25.66
0.03
12.99
0.
9.
3
8
0.65
0.53
-17.79
0.13
25.02
0.
13.
5
8
1.30
1.30
-0.36
0.18
13.65
0.
3.
2
8
0.30
0.25
-17.53
0.04
15.66
02
45
4
8
0.55
0.51
-7.06
0.08
14.64
07
16
6
8
1.67
1.62
-2.85
0.13
8.07
05
52
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 2
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON COPPER ANALYSIS
** POINT ESTIMATES **
DISTILLED HATER SLOPE:GAMMA(1) « .984B5
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 .0229 / .1532
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROS
REG(DISTILLED) 1 41.46190 41.46190
REGtWATER/DISTILLED) 2 .24674 .12337 7.R9 .0007
ERROR 82 1.28151 .01563
O
^ TOTAL 85 42.9
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS OY AA ***
RAW DATA FOR IRON ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
100
1
31.80
50.70
214.00
30.60
13.00
69.00
28.00
76.00
< 3.00*
187.00
37.00
2
26.10
44.00
243.00*
26.60
12.00 -
29.00 <
29.00
76.00
6.00*
13.00
37.00
1
31.80
166.00
142.00 <
34.00
40.00*
8.00* <
26.00
96.00
60.00
26.70
35.00
2
26.10
105.00*
11.00*
23.40
20.00
8.00*
14.00
56.00
7.00
21.60
35.00
1
31.80
- 104.00*
< 10.00*
720.00*
620.00*
86.00
132.00
250.00
175.00
- 13.90*
100.00
2
26.10
177.00
< 10.00*
< 20.00*
720.00*
51.00
185.00
250.00
59.00
23.80
50.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
' ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR IRON ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE HATER
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
236.00
243.30
332.00
553.00
660.00
816.00
203.00
136.00
178.00*
4283.00*
292.00
4
200.00
292.30
218.00
290.00
311.00
311.00
198.00
286.00
166.00*
86.00*
272.00
3
236.00
349.00
375.00
286.00
170.00
48.00
228.00
346.00
288.00
237.00
320.00
4
200.00
331.00
10.00
334.00
570.00
140.00
245.00
256.00
363.00
177.00
350.00
3
236.00
404.00
550.00
< 20.00*
920.00*
75.00
260.00
470.00
462.00
199.00
250.00
4
200.00
315.00
497.00
< 20.00*
720.00*
261.00
211.00
520.00
269.00
319.00
200.00
CD
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY .
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR IRON ANALYSIS BY HATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER DRINKING HATER SURFACE HATER
AMPUL MO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
455.00
496.30
497.00
432.00
450.00
620.00
433.00
396.00
432.00*
530.00
442.00
6
389.00
422.30
1070.00
530.00
541.00
655.00
353.00
3%. 00
403.00*
839.00
492.00
5
455.00
625/00
44.00*
554.00
480.00
727.00
353.00
536.00
511.00
469.00
620.00
6
3B9.00
533.00
< 11.00*
1150.00*
330.00
540.00
343.00
536.00
259.00
434.00
470.00
5
455.00
889.00
577.00
1RO.OO
1000.00*
321.00
317.00
600.00
611.00
685.00
600.00
6
389.00
417.00
1090.00
< 20.00*
920.00*
504.00
307.00
390.00
728.00
- 42.00*
500.00
o
-------
o
I
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR IPON ANALYSES RY WATER TYPE
WATER 1 WATER 2 WATER 3
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, *
SINGLE STD DEV, (SR)
ANALYST REL DEV, t
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, t
SINGLE STO OEV, (SR)
ANALYST REL DEV, t
1
9
31.80
78.37
146.44
72.34
92.30
42
76
3
8
236.00
404.41
71.36
242.97
60.08
156
46
5
9
455.00
477.37
4.92
67.55
14.15
147
27
2
a
26.10
33.32
2.7.68
20.35
61.07
.78
.61
4
8
200.00
272.29
36.14
42.03
15.44
.90
.37
6
9
389.00
588.70
51.34
232.95
39.57
.00
.58
1
8
31.80
73.21
130.23
55.32
75.57
15
30
3
10
236.00
264.70
12.16
98.87
37.35
133
49
5
9
455.00
541.67
19.05
107.95
19.93
64
13
2
7
26.10
25.29
-3.12
16.04
63.45
.04
.55
4
10
200.00
277.60
38.80
151.39
54.53
.58
.26
6
8
389.00
430.63
10.70
108.48
25.19
.00
.16
1
5
31.80
148.60
367.30
66.21
44.56
44
33
3
8
236.00
333.75
41.42
162.25
48.61
86
26
5
9
455.00
531.11
16.73
218.81
41.20
221
40
2
7
26.10
113.69
335.58
B8-.25
77.63
.17
.68
4
8
200.00
324.00
62.00
121.65
37.55
.03
.16
6
7
389.00
562.29
44.55
267.45
47.57
.22
.47
WATER LEGEND
1 - LAB PURE WATER
2 - DRINKING HATER
3 - SURFACE WATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON IRON ANALYSIS
** POINT ESTIMATES **
DISTILLED HATER SLOPE:GAMMA(1) - .95790
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 -.1970 ' .0051
3 2.2718 -.4042
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROS
REG(DISTILLED) 1 129.11791 129.11791
REG(WATER/DISTILLEO) 4 9.71488 2.42872 6.74 .0001
O ERROR 132 47.58961 .36053
I
M
M TOTAL 137 1R6.42239
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.1970 ( -1.5561 , 1.1622) .0051 ( -.2607 , .2709)
3 2.2718 ( .8452 , 3.6983) -.4042 ( -.6805 , -.1279)
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.
-------
LAB PURE HATER
0
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
1.03
1.48
0.94
1.82
1.03
1.18
1.16
0.74
1.00
3.13*
1.26
2
1.22
1.60
0.50
1.53
1.19
1.11
1.39
0.93
0.79
5.88(
1.35
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR IRON ANALYSIS BY HATER TYPE
LOW YOUDEN PAIR, UNITS - MG/L
EFFLUENT 1
1
1.03
1.10
0.96
0.74
1.70
0.47
0.91
0.60
0.91
1.09
0.80
2
1.22
1.23
0.94
0.82
1.10
0.21*
1.23
1.45
1.20
0.96 .
1.00
NJ
-------
LAB PURE WATER
AHPUL NO: 1
TRUE CONC: 2.18
LAB NUMBER
0
1
to
U)
1
2
3
4
5
6
7
8
9
10
2.4B
2.60
1.89
2.27
1.97
2.50
2.51
2.52
2.55
2. 85
2.93
ENVIRONMENTAL MONITORING AND SUPPORT LAPORATORY
OFFICE OF RESEARCH AMI DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR IRON ANALYSIS BY HATER TYPE
MEDIUM YOUDEN PAIR, UNITS - MG/L
EFFLUENT 1
4
2.58
3.35
2.10
2.31
2.69
2.30
3.00
2.72
2.81
2.98
3
2.18
2.00
10.00*
1.67
2.90
2.09
2.07
1.58
2.88
1.52
4
2.58
2.60
9.71
7.39
2.50
1.06
2.61
1.60
3.29
1.73
1.70
3.20
-------
AMPUL NO: 5
TRUE CONC: 4.78
LAB NUMBER
O
1
1 _l
P^
NJ
*>.
1
2
3
4
5
6
7
8
9
10
4.85
4.75
3.%
5.17
5.56
5.12
4.75
4.84
4.04
«!.62
LAB PURE WATER
6
5.59
5.39
5.88
4.61
5.80
5.85
5.86
6.21
5.07
4.36
6.71
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR IRON ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - MG/L
EFFLUENT 1
5
4.78
05
RO
84
80
93
67
12
19
84
4.20
6
5.59
5.21
3.92
4.22
6.80
5.58
5.07
5.22
8.87
5.51
6.20
-------
WATER 1
ENVIRONMENTAL MONITORING AMD SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR IRON ANALYSES BY WATER TYPE
WATER 2
LOW YOUOEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY(%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, *
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
0 OVERALL STO OEV (S)
1 OVERALL REL STO DEV, t
£f SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD OEV, *
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
1
9
1.03
1.18
14.42
0.32
27.03
0.
14.
3
10
2.18
2.41
10.72
0.29
12.06
0.
9.
5
10
4.78
4.87
1.86
0.55
11.35
0.
5.
2
9
1.22
1.15
-5.33
0.36
31.38
17
46
4
10
2.58
2.72
5.41
0.38
14.13
25
66
6
10
5.59
5.57
-0.27
0.72
12.93
29
48
1
10
1.03
0.93
-9.85
0.34
36.34
0.
27.
3
9
2.18
2.05
-6.15
0.52
25.52
1.
49.
5
10
4.78
4.94
3.45
1.26
25.54
0.
12.
2
9
1.22
1.10
-9.52
0.19
17.53
28
06
4
10
2.58
3.57
38.34
2.77
77.62
38
33
6
10
5.59
5.66
1.26
1.41
24.82
66
44
HATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 1
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF HATER TYPE ON IRON ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) - .99617
MATER INTERCEPT(WATER-OISTILLED) SLOPE(WATER-DISTILLED)
2 -.1542 ; .1005
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 50.14372 50.14372
REG(WATER/DISTILLED) 2 .23333 .11666 1.36 .2619
ERROR 103 8.85215 .08594
n
M TOTAL 106 59.22920
** TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
INTERCEPT(HATER-DISTILLED) SLOPE(HATER-DISTILLED)
HATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.1542 ( -.3672 , .0589) .1005 ( -.0940 , .2951)
NOTE: IF ZERO IS CONTAINED HITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED HATER AND THE CORRESPONDING HASTE HATER 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.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR IRON ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - MG/L
LAB PURE WATER EFFLUENT 2
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
0.42
0.60
0.38
0.74
0.42
0.48
0.47
0.30
0.41
1.27*
0.51
2
0.37
0.49
0.15 <
0.47
0.36
0.34
0.42
0.28
0.24
1.80*
0.41
1
0.42
0.44
0.01*
0.44 <
0.42
0.65 -
0.35
0.52
0.51
1.05*
0.35
2
0.37
0.38
0.38
0.02*
0.39
0.18*
0.28
0.54
1.03*
1.01*
0.45
-------
AMPUL NO: 3
TRUE CONC: 0.88
LAB NUMBER
O
1
1 I
r^
NJ
00
1
2
3
4
5
6
7
8
9
10
1.00
1.05
0.76
0.92
0.80
.01
.02
.02
.03
.15
LAB PURE HATER
4
0.95
1.24
0.77
0.85
0.99
0.95
1.11
1.00
1.04
1.10
1.08
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH ANO DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR IRON ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - MG/L
EFFLUENT 2
3 '
0.88
0.86
0.83
0.71
1.10
1.15
0.84
0.93
1.71*
1.38*
0.90
4
0.95
1.04
0.96
0.%
1.00
0.11*
0.%
0.79
1.32*
1.55*
0.90
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAM DATA FOR IRON ANALYSIS BY HATER TYPE
HIGH YOUOEN PAIR, UNITS - MG/L
LAB PURE WATER EFFLUENT 2
AMPUL NO: 5 6 5 6
TRUE CONC: 2.61 2.05 2.61 2.05
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
O
I
M
KJ
VO
4.B5
4.75
3.96
5.17
5.56
5.12
4.75
4.H4
4.04
5.62
1.99
2.17
1.70
2.14
2.16
2.16
2.29
1.87
1.61
2.48
2.93
2.03
2.15
3.00
3.61
2.45
1.80
2.R1
3.51*
2.30
1.73
1.81
1.62
2.30
2.63
2.65
1.70
3.74
5.71*
1.70
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR IRON ANALYSES BY HATER TYPE
WATER 1 HATER 2
Q
1
U)
o
LOU YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY (*REL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV. %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, t
SINGLE STD OEV, (SR)
ANALYST REL OEV, t
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, *
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
1
9
0.42
0.48
13.65
0.13
27.00
0
14
3
10
0.88
0.9B
11.28
0.12
12.06
0
9
5
10
2.61
4.87
R6.S4
O.SS
11.35
0
7
2
9
0.37
0.35
-3.99
0.11
31.41
.06
.38
4
10
0.95
1.00
5.44
0.14
14.13
.09
.48
6
10
2.05
2.06
0.37
0.27
12.94
.26
.43
1
8
0.42
0.46
9.67
0.10
21.54
3
8
0.88
0.91
4.14
0.15
15.93
5
9
2.61
2.56
-1.76
0.57
22.23
2
6
0.37
0.40
9.42
0.09
21.52
0.05
11.49
4
7
0.95
0.94
-0.78
0.08
8.59
0.10
11.19
6
9
2.05
2.21
7.76
0.70
31.91
0.46
19.17
HATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 2
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON IRON ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(I) « 1.20614
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 -.1167 '* -.2480
** ANALYSIS OF VARIANCE **
SOURCE . DF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 64.65182 64.6S182
REG(WATER/DISTILLED) 2 1.14760 .573BO 9.72 .0001
ERROR 92 5.43106 .05903
I
I--
i*J TOTAL 95 71.23049
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.1167 ( -.2261 , -.0073) -.2480 ( -.3962 , -.0999)
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 PARAMETERllNTERCEPT/SLOPE).
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
LAB PURE WATER
ENVIRONMENTAL MONITOR IMG AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAM DATA FOR IRON ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
EFFLUENT 3
AMPUL NO: 1
TRUE CONC: 30.40
2
25.00
1
30.40
2
25.00
LAB NUMBER
n
i
OJ
to
1
2
3
4
5
6
7
8
9
10
49.70
205.00
29.40
12.50
66.00
26.90
73.00
< 3.00*
1RO.OO
35.50
42.20
233.00*
25.50 <
11.50
27.80
27.80
73.00
5.80*
12.50
35.50
60.00
42.00
1.80*
190.00
134.00
545.00*
86.00
31.00
10.80
70.00
30.00
101.00
101.00
150.00
24.00
416.00*
86.00
11.00
10.20
25.00
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR IRON ANALYSIS BY HATER TYPE
MEDIUM YOUDEN PAIR. UNITS - UG/L
EFFLUENT 3
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
226.00
234.00
319.00
531.00
634.00
783.00
195.00
131.00
171.00*
4112.00*
280.00
4
191.00
280.60
209.00
278.00
299.00
299.00
190.00
275.00
159.00*
82.60*
261.00
3
226.00
269.00
160.00
293.00
130.00
180.00
500.00*
216.00
347.00
320.00
255.00
4
191.00
299.00
220.00
185.00
80.00
98.00
360.00*
186.00
282.00
208.50
235.00
-------
ENVIRONMENTAL MONITOR INO AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR IRON ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 3
o
1
AMPUL NO:
TRUE CONC:
LAR NUMBER
1
2
3
4
5
6
7
8
9
10
5
435.00
476.40
477.00
415.00
432.00
595.00
416.00
380.00
415.00*
509.00
424.00
6
372.00
405.40
1027.00
509.00
529.00
629.00
339.00
380.00
387.00*
805.00
472.00
5
435.00
611.00
930.00
1080.00
370.00
370.00
655.00*
326.00
512.00
461.00
725.00
6
372.00
543.00
871.00
427.00
310.00
336.00
540.00'
2«6.00
902.00
328.00
425.00
U)
-------
WATER 1
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RF.SEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR IRON ANALYSES BY HATER TYPE
HATER 2
n
i
1 i
U)
en
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (*REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD OEV, (SR)
ANALYST REL DEV, *
MEDIUM YOUOEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO DEV (S)
OVERALL REL STO DEV, t
SINGLE STO DEV, (SR)
ANALYST REL OEV, I
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UIEL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, *
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
1
9
30.40
75. 22
147.44
69.43
92.30
41
76
3
8
226.00
388.38
71.85
233.12
60.03
150
46
5
9
435.00
458.27
5.35
64.81
14.14
140
27
2
8
25.00
31.97
27.90
19.55
61.14
.17
.82
4
8
191.00
261.45
36.88
40.53
15.50
.48
.31
6
9
372.00
566.16
52.19
223.32
39.45
.99
.52
1
8
30.40
77.97
156.50
58.74
75.33
33
49
3
9
226.00
241.11
6.69
74.49
30.89
41
18
5
9
435.00
598.33
37.55
265.27
44.34
193
35
2
9
25.00
59.80
139.20
50.55.
84.53
.97
.31
4
9
191.00
199.28
4.33
73.69
36.98
.53
.86
6
9
372.00
493.11
32.56
236.07
47.87
.70
.49
HATER LEGEND
1 - LAB PURE HATER
2 - EFFLUENT 3
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF MATER TYPE ON IRON ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) « .95452
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 .4885 ' -.1136
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 108.90628 108.90628
REG(WATER/DISTILLED) 2 .54537 .2726fl .77 .4668
ERROR 91 32.29562 .35490
O
I
^ TOTAL 94 141.74727
U)
** TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(HATER-DISTILLED) SLOPE(WATER-DISTILLEO)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .4885 ( -.6720 , 1.6490) -.1136 ( -.3430 , .1159)
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.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR LEAD ANALYSIS BY HATER TYPE
LOH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING HATER SURFACE HATER
AMPUL NO:
TRUE CONC:
LAR NUMBER
1
2
3
4
5
6
7
8
9
10
1
14.10
16.17
8.00
11.50
29.00*
13.00
13.00
8.00*
12.20
17.50
24.00*
2
10.90
13.9fl
11.00
8.30
12.00
8.00
9.00
7.00*
41.00*
9.23
18.00*
1
14.10
8.24*
13.00
14.30
10.00
22.00
14.00
17.00
12.60 <
1.40
13.00
2
10.90
6.05*
15.00
8.60
7.00
14.00
10.00
12.00
2,00*
0.40
9.00
1
14.10
9.80
11.00 <
14.20
8.00
10.00
23.00*
8.00*
11.70
20.80
19.00
2
10.90
6.50
10.00*
8.30
5.00
6.00
30.00*
6.00*
8.fiO
9.70
14.00
n
i
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR LEAD ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
AMPUL NO: 3
TRUE CONC: 55.50
4
47.30
3
55.50
4
47.30
3
55.50
4
47.30
LAB NUMBER
0
1
l--j
| i
U)
00
1
2
3
4
5
6
7
8
9
10
51.66
51.00
55.50
140.00*
42.00
50.00
38.00*
41.00
65.70
59.00*
51.66
49.00
47.90
100.00*
47.00
44.00
37.00*
24.00
17.80
79.00*
31.47*
22.00
53.90
44.00
39.00
59.00
43.00
48.00
47.30
65.00
28.44*
32.00
47.90
47.00
36.00
50.00
32.00
40.00
45.40
45.00
41.70
60.00
35.80
45.00
55.00
77.00*
25.00*
48.00
39.70
44.00
33.00
52.00
50.60
48.00
45.00
71.00*
24.00*
30.00
37.40
74.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR LEAD ANALYSIS BY HATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
0
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
q
10
5
254.00
30.34
269.00
233.00
250.00
154.00
192.00
178.00*
225.00
166.00
359.00*
6
211.00
25.80*
222.00
190.00
200.00
214.00
159.00
148.00*
169.00
121.00
239.00*
5
254.00
156.40*
190.00
227.00
220.00
110.00
279.00
202.00
214.00
248.00
275.00
6
211.00
133.50*
168.00
183.00
170.00
74.00
217.00
162.00
170.00
196.00
265.00
5
254.00
181.00
262.00
226.00
220.00
173.00
231.00*
200.00*
219.00
219.00
234 iOO
6
211.00
153.00
225.00
153.00
180.00
238.00
226.00*
160.00*
197.00
177.00
264.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR LEAD ANALYSES BY WATER TYPE
HATER 1 WATER 2 WATER 3
n
i
i *
4^
O
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (IREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV,
-------
ENVIRONMENTAL MONITOR INC. AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON LEAD ANALYSIS
** POINT ESTIMATES **
DISTILLED HATER SLOPE:GAMMA( 1) = .91930
MATER INTERCEPT(WATER-DISTILLEO) SLOPE(WATER-DISTILLED)
2 -.6566 * .1336
3 -.4235 .1111
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLEO) 1 205.69443 205.69443
REG(WATER/OISTILLED) 4 I.lfl098 .2°524 1.61 .1751
ERROR 12fl 23.44156 .18314
TOTAL 133 230.31697
** TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
IHTERCEPT(HATER-DISTILLED) SLOPE(WATER-OISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.6566 ( -1.4282 , .1151) .1336 ( -.0495 , .316B)
3 -.4235 ( -1.2154 , .3684) ,1111 ( -.0776 , .29W)
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.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LARORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR LEAD ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
0
1
1 .
p^
£>.
N)
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
13.50
17.60*
8.70
11.90
15.00
6.50
9.50
7.60*
12.90
11.90
15.00
2
10.40
12.60*
7.60 <
6.90
13.00
4.40
7.10
5.50*
10.50
8.40
13.00
1
13.50
4.09*
10.00* <
14.00
11.00
9.00
11.00
15.00
2.00* <
13.70
13.00
2
10.40
0.34*
11.00*
6.50
14.00
9.00
9.00
14.00
2.00*
12.60
13.00
1
13.50
2.29*
14.00
12.10
2.00
9.00
13.00
5.00*
10.60
4.30
16.00
2
10.40
1.47*
8.00
7.90
2.00
B.OO
8.00
4.00*
7.00
2.70
7.00
1
13.50
2.48
1.00* <
9.00
17.00*
13.00
12.00
2. SO*
8.20
11.40
24.00
2
10.40
2.73
10.00*
4.30
9.00*
13.00
14.00
1.50*
5.10
8.?0
10.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAM DATA FOR LEAD ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
n
i
AMPUL NO:
TRUE COHC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
53.00
78.00*
56.70
52.70
55.00
46.00
48.00
44.00*
159.00*
54.30
53.00
4
45.20
69.30*
79.60
45.10
49.00
31.00
40.00
36.00*
149.00*
68.70
53.00
3
53.00
21.15*
19.00
46.80
34.00
56.00
46.00
41.00
45.00
29.20
31.00
4
45.20
16.80*
44.00
43.60
41.00
41.00
35.00
35.00
24.00 .
41.80
21.00
3
53.00
18.30*
37.00
103.00*
34.00
50.00
48.00
18.00*
43.00
40.00
54.00
4
45.20
11.50*
33.00
41.30
55.00
40.00
40.00
21.00*
37.00
33.40
44.00
3
53.00
.
18.09
27.00*
39.70
110.00*
63.00
39.00
12.00*
43.00
42.00
57.00
4
45.20
14.67
19.00*
35.30
160.00*
43.00
33.00
11.00*
53.00
51.40
57.00
-------
ENVIRONMENTAL MONITOR INC, AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR LEAD ANALYSIS BY WATER TYPE
HIGH YOUOEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER.
1
2
3
4
5
6
7
8
9
10
5
243.00
316.50*
326.00
215.00
229.00
174.00
229.00
205.00*
215.00
227.00
271.00
fi
202.00
254.40*
237.00
178.00
196.00
243.00
171.00
140.00*
182.00
210.00
271.00
5
243.00
98.80*
283.00
215.00
170.00
159.00
252.00
180.00
180.00
233.00
251.00
6
202.00
98.00*
247.00
166.00
140.00
244.00
191.00
150.00
169.00
514.00*
171.00
5
243.00
96.00*
172.00
170.00
200.00
290.00
221.00
50. PO*
190.00
93.SO
264.00
6
202.00
73.00*
124.00
165.00
180.00
23fi.OO
183.00
41.00*
160.00
«7.20
164.00
5
243.00
*
75.05
36.00*
123.00
220.00*
162.00
168.00
58.00*
134.00
166.00
167.00
6
202.00
40.25
10.00*
97.90
130.00*
101.00
122.00
48.00*
178.00
235.00
87.00
*».
-------
ENVIRONMENTAL MONITORING ANT) SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR LEAD ANALYSES BY WATER TYPE
MATER 1
HATER 2
HATER 3
HATER 4
n
i
h- '
*».
Ul
LOH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (WEI ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, t
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, *
SINGLE STD OEV, (SR)
ANALYST REL OEV, t
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (JREL ERROR)
OVERALL STO OEV (S)
OVERALL REL STD DEV, f
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
13.
11.
-15.
3.
26.
53.
52.
-1.
3.
7.
243.
235.
-2.
45.
19.
1
8
50
42
37
01
38
0.
8.
3
7
00
24
43
86
39
9.
18.
5
8
00
75
98
09
12
32.
14.
2
8
10.40
8.R6
-14.78
3.06
34.54
84
27
4
7
45.20
52.34
15.80
16.75
31.99
64
43
6
8
202.00
211.00
4.46
35.97
17.05
71
64
1
7
13.50
12.31
-8.78
2.07
16.82
2
19
3
9
53.00
38.67
-27.04
11.31
29.24
10
27
5
9
243.00
213.67
-12.07
43.60
20.41
35
17
10.
11.
7.
2.
26.
.26
.25
45.
3fi.
-19.
".
23.
.35
.63
202.
184.
-8.
40.
21.
.20
.67
2
7
40
16
28
96
55
4
9
20
27
76
48
39
6
8
00
75
54
40
87
1
8
13.50
10.12
-25.00
4.83
47.68
2
25
3
7
53.00
43.71
-17.52
7.27
16.64
7
18
5
8
243.00
200.10
-17.65
fiO.59
30.28
21
12
2
8
10.40
6.32
-39.18
2:50
39.48
.08
.30
4
8
45.20
40.46
-10.48
7.00
17.29
.75
.42
6
8
202.00
162.40
-19.60
43.58
26.84
.81
.04
1
7
13.50
11.44
-15.26
6.55
57.24
3.
38.
3
7
53.00
43.11
-18.65
14.40
33.40
7.
17.
5
7
243.00
142.15
-41.50
34.60
24.34
38.
29.
2
7
10.40
8.19
-21.25
4.37
53.38
74
13
4
7
45.20
41.05
-9.18
14.73
35.88
22
16
6
7
202.00
123.02
-39.10
64.33
52.29
9fi
38
HATER LEGEND
i - LAB PURE HATER
2 - EFFLUENT 1
3 - EFFLUENT 2
4 - EFFLUENT 3
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF MATER TYPE ON LEAD ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) 1.06568
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-OISTILLED)
2 .2694 ' -.0961
3 -.3729 .0302
4 .3997 -.1468
** ANALYSIS OF VARIANCE **
SOURCE f)F SIIM OF SQUARES MEAN SQUARE F PROR
REG(DISTILLED) 1 273.95189 273.95189
_ REG(WATER/DISTILLED) 6 2.90558 .4B426 4.55 .0003
, ERROR 167 17.78549 .10650
!-
'£*
<* TOTAL 174 294.64296
** TABLE OF 95S CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(HATER-DISTILLED) SLOPE(WATER-DISTILLEO)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .2694 ( -.3481 , .8868) -.0961 ( -.2443 , .0522)
3 -.3729 ( -.9748 , .2289) .0302 ( -.1163 , .1768)
4 .3997 ( -.2269 , 1.0264) -.1468 ( -.2985 , .0048)
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.
-------
1 N V S BREAK: WATER(S) REJECTED DUE TO INSUFFICIENT OR BAD AMPUL DATA - NO MULTIPLICATIVE MODEL ANALYSIS WILL RE PRINTED.
O
I
-------
ENVIROHMENTAl MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR MANGANESE ANALYSIS BY HATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER
DRINKING HATER
SURFACE HATER
AMPUL NO: 1
TRUE CONC: 0.60
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
n
i
0.26
< 2.00* <
3.70
5.10
< 0.10* <
4.00
< 1.00* <
< 2.00* <
0.60 <
1.40
2
0.44
0.68
2.00*
1.70 <
2.30 -
0.10*
3.00
1.00*
2.00* <
0.60*
0.60
1
0.60
2.30
1.00* <
0.50* <
1.70* -
3.00
3.00
13.00*
2.00* <
0.40
2.00
2
0.44
1.60 -
2.00* <
0.50*
1.70* -
1.00 <
4.00
1.00
2.00*
0.40 -
2.00 <
1
0.60
4.80* -
2.00* <
8.00 <
2.00* -
1.00*
15.00*
7.00 -
4.00 <
2.00* -
1.00*
2
0.44
33.00*
2.00*
0.50*
2.00*
10.00*
14.00*
2.00*
2.00*
0.30*
5.00*
oo
-------
n
i
VO
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIROWENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAM DATA FOR MANGANESE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
AHPUL NO:
TRUE COMC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
5.00
4.04
158.00*
4.50
5.30
3.00
10.00
ll.no
10.00
4.80
5.20
4
7.95
5.94
182.00* <
7.20
6.80
8.00 <
15.00
8.00
20.00 <
16.30
8. BO
3
5.00
2.80
2.00* <
3.30
3.30
1.00*
9.00
5.00
2.00* <
2.40
7.00
4
7.95
5.80 -
2.00* <
6.10 <
7.10
16.00
7.00
14.00 -
2.00*
5.90
7.00 -
3
5.00
54.60* -
2.00*
0.50* <
10.00
6.00
16.00*
10.00*
10.00
3.40
5.00*
4
7.95
43.80*
131.00*
0.50*
16.00
12.00
20.00*
3.00
9.00
5.90
5.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR MANGANESE ANALYSIS BY MATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
o
h-1
Ul
0
AMPUL NO:
TRUE CONC:
LAB NUMRER
1
2
3
4
5
6
7
8
9
10
5
14.80
14.36
2.60
12.70
13.00
18.00
26.00
15.00
4.00
334.00*
10.00
6
11.80
10.14
6.50 <
9.80
10.00
12.00
21.00
12.00
8.00
236.00*
15.00
5
14.80
11. PO
2.00* <
11.20
11.00
26.00
18.00
18.00
6.00*
11.10
17.00
6
11.80
9.70 -
2.00* <
8.90
9.10
24.00
17.00
11.00
6.00*
8.50
47.00*
5
14.80
18.00*
2.00* <
6.00 <
20.00
20.00
30.00*
14.00 -
19.00
8.40
10.00 <
6
11.80
7.00
2.00*
0.50*
17.00
16.00
24.00*
7.00*
17.00
8.50
1.00*
-------
n
i
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR MANGANESE ANALYSES BY WATER TYPE
WATER 1
WATER 2
WATER 3
LOU YOUOEN PAIR
NUMBER OF OATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (SREL ERROR)
OVERALL STO OEV (S)
OVERALL REL STD DEV, «
SINGLE STO OEV, (SR)
ANALYST REL DEV, t
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY URF.L ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STO OEV, (SR)
ANALYST REL DEV, I
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD DEV, %
SINGLE STO DEV, (SR)
ANALYST REL DEV, *
1
6
0.60
2. SI
321.14
2.01
80.25
0
41
3
9
5.00
6.43
28.53
3.02
47.01
3
36
5
9
14.80
12.S5
-13.17
7.05
54.88
3
24
2
5
0.44
1.66
275.51
1.04
62.54
.B7
.64
4
9
7.95
10.67
34.23
5.06
47.40
.11
.43
6
9
11.80
11.60
1.66
4.29
36.%
.04
.83
1
5
0.60
2.14
259.06
1.07
49.85
0.
41.
3
7
5.00
4.69
-6.29
2.47
52.77
2.
36.
5
8
14.80
15.52
4.90
5.29
34.09
1.
9.
2
6
0.44
1.67
277.93
1.27
76.15
78
17
4
a
7.95
8.61
8.33
4.01
46.58
43
53
6
7
11.80
12.60
6.78
5.82
46.17
38
83
1
3
0.60
6.33
962.64
2.08
32.87
3
4
5.00
7.35
47.00
3.24
44.07
5
7
14.80
13.91
-5.98
5.89
42.35
2
0
0.44
UNO
.UNO
UMD
UNO
UNO
UNO
4
6
7.95
8.48
6.71
4. 86
57.27
2.37
!9.93
6
5
11.80
13.10
11.02
4.93
37.63
1.24
9.17
WATER LEGEND
1 - LAB PURE WATER
2 - DRINKING HATER
3 - SURFACE HATER
-------
o
I
N)
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR MANGANESE ANALYSES BY WATER TYPE
HATER 1
HATER 2
LOU YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, *
SINGLE STO DEV, (SR)
ANALYST REL DEV, I
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD DEV, t
SINGLE STD OEV, (SR)
ANALYST REL DEV, * .
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, t
SINGLE STO OEV, (SR)
ANALYST REL DEV, 1,
I
8
91.00
214.50
135.71
22.16
10.33
16
10
3
8
192.00
181.50
-5.47
14.72
8.11
16
8
5
7
484.00
442.57
-8.56
23.72
5.36
23
5
2
ft
107.00
109.38
2.22
18.56
16.97
.23
.02
4
8
220.00
207.75
-5.57
23.53
11.33
.43
.44
6
8
420.00
422.50
0.60
51.21
12.12
.93
.53
1
9
91.00
80.82
-11.18
38.55
47.70
45
50
3
9
192.00
189.22
-1.45
37.73
19.94
41
21
5
9
484.00
470.11
-2.87
84.88
18.06
71
16
2
9
107.00
98.10
-8.32
47.18
48.10
.46
.82
4
9
220.00
187.44
-14.80
70.55
37.64
.00
.77
6
9
420.00
402.00
-4.29
73.70
18.33
.25
.34
HATER LEGEND
1 - LAB PURE HATER
2 - EFFLUENT 1
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR MANGANESE ANALYSIS RY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 1
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
q
10'
1
91.00
207.00
189.00
192.00
211.00
244.00
221.00*
235.00
198.00
145.00*
240.00
2
107.00
109.00
104.00
95.00
108.00
84.00 <
111.00*
138.00
102.00
83.00*
135.00
1
91.00
120.50
78.00
62.90
90.00
1.00*
79.00
140.00
76.00
1.00
80.00
2
107.00
134.00
65.00
71.90
80.00
< 1.00*
130.00
130.00
96.00
166.00
10.00
01
-------
ENVIRONMENTAL MONITORING AMD SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR MANGANESE ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 1
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
fl
9
10
3
192.00
175.00
152.00
188.00
189.00
179.00
227.00*
203.00
187.00
134.00*
179.00
4
220.00
213.00
186.00
207.00
226.00
164.00
289.00*
204.00
227.00
146.00*
235.00
3
192.00
218.00
128.00
152.00
220.00
< 1.00*
180.00
254.00
179.00
192.00
180.00
4
220.00
250.00
147.00
166.00
180.00
< 1.00*
180.00
308.00
169.00
57.00
230.00
Ul
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR MANGANESE ANALYSIS BY WATER TYPE
HIGH YOUDF.N PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 1
AMPUL NO: 5
TRUE COHC: 484.00
6
420.00
5
484.00
fi
420.00
LAB NUMBER
n
1
h-1
(Jl
01
1
2
3
4
5
6
7
8
9
10
470.00
436.00
406.00
460.00
439.00
699.00*
465.00
422.00
336.00*
598.00*
455.00
465.00
346.00
405.00
376.00
593.00*
418.00
409.00
1.50*
506.00
592.00
426.00
600.00
520.00
56.00*
447.00
447.00
430.00
339.00
430.00
442.00
373.00
3B3.00
340.00
49.00*
479.00
408.00
379.00
284.00
530.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON MANGANESE ANALYSIS
** POINT ESTIMATES **
DISTILLED HATER SLOPE:GAMMA(1) ' .65345
HATER INTERCEPT(HATER-DISTILLED) SLOPE(HATER-DISTILLED)
2 -3.3268 .' .5813
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLEO) 1 36.32748 36.32748
REG(HATER/DISTILLEO) 2 4.35484 2.17742 7.60 .0009
ERROR 88 25.22618 .28666
O
,1 TOTAL 91 65.90850
en
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES RETHEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(HATER-DISTILLED) SLOPE(HATER-DISTILLEO)
HATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -3.3268 ( -5.3970 , -1.2567) .5813 ( .1961 , .9664)
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED HATER AND THE CORRESPONDING WASTE HATER FOR THE ASSOCIATED PARAMETERMNTERCEPT/SLOPE).
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR MANGANESE ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 2
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
151.00
147.00
134.00
136.00
150.00
173.00
156.00*
167.00
140.00
103.00*
170.00
2
111.00
113.00
108.00
99.00
112.00
87.00
115.00* -
143.00
105.00
86.00*
140.00
1
151.00
126.00
84.00
125.00
90.00
74.00
70.00* -
103.00
120.00
80.50
50.00
2
111.00
91.00
92.00
83.00
130.00
Ifl9.00*
80.00*
89.00
87.00
66.50
100.00
Ul
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR MANGANESE ANALYSIS BY WATER TYPE
MEDIUM YOUOEN PAIR, UNITS - UGA
EFFLUENT 2
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
a
9
10
3
227.00
206.00
179.00
221.00
222.00
211.00
267.00*
239.00
220.00
15ft. 00*
210.00
4
302.00
291.00
253.00
282.00
307.00
223.00
393.00*
277.00
308.00
198.00*
320.00
3
227.00
142.00
176.00
151.00
160.00
537.00*
63.00*
183.00
169.00
149.00
150.00
4
302.00
183.00
204.00
233.00
190.00
5.00
152.00*
247.00
97.00
87.50
350.00
CO
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR MANGANESE ANALYSIS BY WATER TYPE
HIGH YOUOEN PAIR, UNITS - UG/L
EFFLUENT 2
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
666.00
643.00
597.00
556.00
630.00
602.00
958.00*
636.00
578.00
460.00*
819.00*
6
577.00
633.00
646.00
481.00
563.00
523.00
826.00*
581.00
569.00
2.10*
704.00
5
666.00
650.00
548.00
SfiO.OO
540.00
191.00
367.00*
606.00
572.00
312.00
1000.00
6
577.00
570.00
537.00
503.00
460.00
613.00
293.00
526.00
546.00
399.00
950.00
VO
-------
n
i
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR MANGANESE ANALYSES RY WATER TYPE
HATER 1
WATER 2
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STO OEV (S)
OVERALL REL STD OEV, t
SINGLE STD OEV, (SR)
ANALYST REL DEV, t
MEDIUM YOUOEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (IREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD OEV, (SR)
ANALYST REL DEV, »
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY («REL ERROR)
OVERALL STO OEV (S)
OVERALL REL STD DEV, t
SINGLE STD OEV, (SR)
ANALYST REL OEV, X
1
8
151.00
152.13
0.75
15.78
10.37
13
10
3
8
227.00
213.50
-5.95
17.26
8.09
22
8
5
7
666.00
606.00
-9.01
32.21
5.32
33
5
2
8
111.00
113.38
2.14
19.23
16.97
.96
.52
4
8
302.00
282.63
-6.42
32.00
11.32
.12
.92
6
8
577.00
587.50
1.82
71.27
12.13
.31
.58
1
9
151.00
94.72
-37.27
25.91
27.36
24.
26.
3
8
227.00
160.00
-29.52
14.60
9.12
60.
35.
5
9
666.00
553.22
-16.93
224.10
40.51
121.
22.
2
8
111.00
92.31
-16.84
18.02
19.52
54
25
4
9
302.00
177.39
-41.26
101.79
57.38
37
79
6
8
577.00
519.25
-10.01
66.20
12.75
03
57
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 2
-------
ENVIRONMENTAL MONITOR I HP, AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON MANGANESE ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) = .97778
WATER INTERCEPT(WATER-DISTILLEO) SLOPE(WATER-DISTILLED)
2 -1.0018 ; .1148
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 43.54711 43.54711
REGlWATER/niSTILLED) 2 3.05148 1.52574 7.9<» .0007
ERROR 86 16.43024 ..19105
n
I
TOTAL «9 63.02R82
** TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -1.0018 ( -2.7291 , .7255) .1148 ( -.1906 , .4202)
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.
-------
o
ro
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND OEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAU DATA FOR MANGANESE ANALYSIS BY WATER TYPE
LOW YOUOEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 3
AMPUL HO:
TRUE CONC:
LAB NUMBER
1
2 <
3
4
5 <
6
7 <
8 <
9
10
1
0.57
0.25
2.00* <
3.60
4.90
1.00* <
3.80
1.00* <
2.00* <
0.58 <
1.30
2
0.42
0.65 -
2.00* <
1.60 <
2.20
1.00* <
2.90
1.00* <
2.00* <
0.60*
0.5R
1
0.57
0.9B* -
2.00* <
0.50*
1.70
1.00* <
12.00*
1.00*
2.00* <
1.70 -
1.60
2
0.42
0.98*
2.00*
0.90
0.80
1.00*
10.00*
9.00
2.00*
1.10*
2.80
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND OEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR MANGANESE ANALYSIS BY WATER TYPE
MEDIUM YOUOEN PAIR, UNITS - UG/L
EFFLUENT 3
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
4.78
3.88
152.00*
4.30
5.10
2.90
9.60
10.60
9.60
4.60
5.00
4
7.61
5.70
172.00*
6.90
6.50
7.70
14.40
7.70
19.20 <
15.70 -
8.50
3
4.78
2.61
10.00
4.10
5.20
6.00
21.00*
5.00
2.00* <
1.50*
3.80
4
7.61
5.12
5.00
5.80
7.70
8.00
17.00*
7.00
2.00*
4.10
8.80
o
-------
ENVIRONMENTAL MONITORING AND SUPPORT LARORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR MANGANESE ANALYSIS RY HATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 3
n
i
AMPUL NO:
TRUE CONC:
LAR NUMBER
1
2
3
4
5
6
7
8
9
10
5
14.20
13.80
2.50
12.20
12.50
17.30
25.00
14.40
, 3.flO
321.00*
9.60
6
11.30
9.73
6.24
9.40
9.60
11.50
20.00
11.50
7.70
227.00*
14.40
5
14.20
10.31
9.00
10.40
14.00
19.00
29.00*
9.00
14.00
7.60
18.80
6
11.30
8.05
6.00
8.80
11.00
13.00
24.00*
6.00
12.00
10.90
8.80
-------
o
I
en
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR MANGANESE ANALYSES BY WATER TYPE
WATER 1
WATER 2
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X )
ACCURACY (tREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, *
SINGLE STO OEV. (SR)
ANALYST REL DEV, *
MEDIUM YOUOEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (IREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, I
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD DEV, t
SINGLE STD DEV, (SR)
ANALYST REL DEV, »
1
6
0.57
2.40
321.93
1.94
80.62
0
42
3
9
4.78
6.18
29.20
2.91
47.06
3
36
5
9
14.20
12.34
-13.07
6.79
54.98
2
25
2
5
0.42
1.59
275.83
1.00
62.99
.85
.56
4
9
7.61
10.26
34.76
4.86
47.40
.00
.56
6
9
11.30
11.12
1.60
4.07
36.62
.94
.09
1
3
0.57
1.67
192.40
0.06
3.46
1
41
3
7
4.78
5.24
9.71
2.37
45.11
2
37
5
9
14.20
12.46
-12.28
4.24
34.08
2
23
2
4
0.42
3.37
699.76
3.R6
114.41
.05
.65
4
8
7.61
6.44
-15.37 .
1.67
25.99
.18
.32
6
9
11.30
9.39
-16.86
2.50
26.66
.51
.01
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 3
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON MANGANESE ANALYSIS
** POINT ESTIMATES **
DISTILLED HATER SLOPE:GAMMAj1) - .62440
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 .1957 ; -.0842
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(OISTILLED) 1 40.98493 40.98493
REG(WATER/DISTILLED) 2 .2P611 .14305 .56 .5760
ERROR 74 19.04432 .25736
O
h- TOTAL 77 60.31535
o>
Ol
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLEO)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .1957 ( -.2251 , .6165) -.0842 ( -.2879 . .1195)
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 PARAHETER(INTERCEPT/SLOPE).
THE SLOPE AHD INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AMD DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR NICKEL ANALYSIS RY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAR PURE WATER DRINKING WATER SURFACE WATER
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
B
9
10
1
27.40
35.50
16.00
19.00
17.00
32.00
11.00
26.00
23.00
16.20
28.00
2
31.10
39.90
17.00
25.00
25.00
32.00
21.00
33.00
26.00
25.20
42.00
1
27.40
37.70*
19.00 <
10.90
23.00
< 10.00*
25.00
27.00
25.00
16.20
35.00*
2
31.10
39.70*
10.00*
12. BO
51.00
26.00*
28.00
28.00
35.00
IB. 00
35.00*
1
27.40
30.00
19.00
50.40
19.00
45.00
36.00
24.00
4.00
19.30
28.00*
2
31.10
32.80
18.00
94.20*
22.00
22.00
46.00
28.00
2.00
24.10
42.00*
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR NICKEL ANALYSIS BY HATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
200.00
175.00
150.00
163.00
190.00
157.00
212.00
167.00
164.00
143.00
280.00*
4
240.00
229.00
217.00
208.00
240.00
129.00
188.00
199.00
174.00
181.00
280.00
3
200.00
201.00*
82.00
164.00
180.00
34.00*
211.00
153.00
79.00
159.00
250.00*
4
240.00
260.00*
94.00
187.00
270.00
31.00*
264.00
159.00
110.00
175.00
250.00*
3
200.00
175.00
214.00
180.00
180.00
64.00
221.00
136.00
152.00
131.50
260.00*
4
240.00
229.00
238.00
186.00
220.00
124.00
199.00
166.00
127.00
172.00
320.00*
00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR NICKEL ANALYSIS BY HATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER DRINKING HATER SURFACE HATER
AMPUL NO: 5 6 5 6 R 6
TRUE CONC: 402.00 482.00 402.00 482.00 402.00 482.00
LAB NUMBER
O
1
1
2
3
4
5
6
7
8
9
10
362.00
533.00
276.00
370.00
454.00
457.00
383.00
500.00
225.00
600.00
498.00
392.00
290.00
500.00
528.00
516.00
439.00
810.00
268.00
300.00
511.00*
272.00
407.00
410.00
49.00*
419.00
344.00
300.00
340.00
750.00*
560.00*
330.00
464.00
540.00
73.00*
385.00
392.00
470.00
287.00
750.00*
352.00
295.00
480.00
360.00
406.00
356.00
392.00
272.00
272.00
450.00*
414.00
353.00
585.00*
400.00
3%. 00
420.00
416.00
472.00
348.00
700.00*
vo
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR NICKEL ANALYSES BY HATER TYPE
WATER 1
WATER 2
WATER 3
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL OEV, t
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD OEV (S)
n OVERALL REL STO OEV, t
tj SINGLE STD DEV, (SR)
0 ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X) .
ACCURACY (%REL ERROR)
OVERALL STO DEV (S)
OVERALL REL STO DEV, *
SINGLE STD DEV, (SR)
ANALYST REL DEV, *
1
10
27.40
22.37
-18.36
7.88
35.22
3
11
3
9
200.00
169.00
-15.50
21.13
12.50
24
12
5
10
402.00
416.00
3.48
115.44
27.75
115
26
2
10
31.10
28.61
-8.01
7.99
27.93
.04
.91
4
10
240.00
204.50
-14.79
41.12
20.11
.03
.87
6
10
482.00
454.10
-5.79
159.65
35.16
.71
.60
1
7
27.40
20.87
-23.83
5.79
27.73
7
29
3
7
200.00
146.86
-26.57
49.16
33.48
20
12
5
7
402.00
356.00
-11.44
57.85
16.25
56
14
2
6
31.10
28.80
-7.40
13.46
46.72
.43
.94
4
7
240.00
179.86
-25.06
68.27
37.96
.84
.76
6
7
482.00
409.71
-15.00
87.46
21.35
.63
.79
1
9
27.40
27.41
0.04
14.51
52.95
7
27
3
9
200.00
161.50
-19.25
47.84
29.62
21
12
5
q
402.00
353.89
-11.97
68.00
19.22
43
11
2
8
31.10
24.36
-21.66
12.56
51.56
.02
.11
4
9
240.00
184.56
-23.10
41.50
22.49
.78
.59
6
8
482.00
402.38
-16.52
39.50
9.82
.37
.47
WATER LEGEND
1 - LAB PURE HATER
2 - DRINKING WATER
3 - SURFACE WATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF HATER TYPE ON NICKEL ANALYSIS
** POINT ESTIMATES **
DISTILLED HATER SLOPE:GAMMAl1) 1.03994
WATER INTERCEPT(HATER-DISTILLED) SLOPE(WATER-OlSTILLED)
2 .0459 '. -.0225
3 -.1410 .0092
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(OISTILLED) 1 216.29453 216.29453
REGlHATER/DISTILLEO) 4 .20247 .07062 .51 .7287
ERROR 137 18.98417 .13B57
I
-J TOTAL 142 235.56118
** TABLE OF 95S CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(HATER-DISTILLED) SLOPE(HATER-DISTILLEO)
HATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .0459 ( -.7964 , .8882) -.0225 ( -.1871 , .1421)
3 -.1410 ( -.9232 , .6«12) .0002 ( -.1444 , .1628)
NOTE: IF ZERO IS CONTAINED WITHIN A RIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED HATER 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.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR NICKEL ANALYSIS RY WATER TYPE
LOW YOUDEN PAIR, UNITS - IIG/L
LAB PURE WATER EFFLUENT 1 EFFLUENT 2 .EFFLUENT 3
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
26.20
60.50*
21. BO
26.10
IB. 50
16.30
45.70
23.90
26.10
40.30
39.10
2
29.70
60.60*
32.60
23.90
22.80
23.90
30.40
27.20
29.40
48.20
41.30
1
26.20
27.60
17.30
28.00
34.00*
39.00
61.00*
17.00
9.00 <
1.40*
27.00
2
29.70
46.50
40.00
30.00
69.00*
40.00
72.00*
30.00
5.00*
11.00*
32.00
1
26.20
34.20
21.00
16.00
24.00
24.00
7.00* <
15.00
5.00
13.10
20.00
2
29.70
*
45.10
14.00 <
16.00 <
22.00
25.00
2.00*
20.00
3.00 <
16.70
B.OO
1
26.20
2.00
10.00* <
4.00* <
17.00
2B.OO
3.00
4.00
5.00* <
7.20 -
70.00*
2
29.70
8.00
10.00*
4.00*
25.00
32.00
3.00
124.00*
5.00*
13.40*
60.00*
to
-------
ENVIRONMENTAL MONITORING AND SUPPORT LARORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR NICKEL ANALYSIS BY MATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 1 EFFLUENT 2 EFFLUENT 3
0
1
AMPUL NO:
TRUE CONC:
LAR NUMBER
1
2
3
4
5
6
7
8
9
10
3
191.00
240.00*
126.00
163.00
174.00
207.00
148.00
165.00
146.00
103.00
261.00
4
230.00
309.00*
145.00
204.00
218.00
96.00
176.00
187.00
163.00
145.00
283.00
3
191.00
398.00*
179.00
201.00
230.00*
132.00
214.00*
160.00
80.00
72.70*
172.00
4
230.00
514.00*
174.00
202.00
210.00*
121.00
304.00*
173.00
160.00
148.00*
192.00
3
101.00
179.00
116.00
168.00
190.00
120.00
162.00*
143.00
120.00
109.00
190.00
4
230.00
235.00
244.00
170.00
220.00
156.00
39.00*
166.00
140.00
122.00
140.00
3
191.00
#
294.00
1R4.00
104.00
160.00
< 10.00*
14R.OO
149.00
174.00
86.80
220.00*
4
230.00
388.00*
212.00
155.00
200.00
< 10.00*
162.00
109.00
213.00
147.00
340.00*
U)
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR NICKEL ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 1 EFFLUENT 2 EFFLUENT 3
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
385.00
547.00*
346.00
238.00
413.00
314.00
297.00
371.00
424.00
200.00
489.00
6
461.00
624.00*
313.00
339.00
446.00
466.00
350.00
419.00
620.00
309.00
435.00
S
385.00
188.00
260.00
229.00
380.00*
244.00
358.00*
390.00*
250.00
180.00*
242.00
6
461.00
252.00
301.00
287.00
460.00*
361.00
405.00*
440.00
260.00
242.00*
272.00
5
385.00
398.00
416.00
406.00
370.00
228.00
162.00*
384.00
240.00
246.00
640.00
6
461.00
471.00
473.00
401.00
440.00
282.00
207.00*
408.00
360.00
249.00
790.00*
5
385.00
*
' 282.00
295.00
329.00
370.00
< 10.00*
251.00
324.00
99.00*
245.00
390.00*
6
461.00
331.00
358.00
418.00
420.00
< 10.00*
316.00
373.00
113.00*
291.00
640.00*
-------
o
I
en
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR NICKEL ANALYSES BY HATER TYPE
WATER 1
WATER 2
WATER 3
WATER 4
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, »
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO DEV (S)
OVERALL REL STO DEV, t
SINGLE STD OEV, (SR)
ANALYST REL DEV, I
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO OEV (S)
OVERALL REL STO DEV, *
SINGLE STO DEV, (SR)
ANALYST REL DEV, t
WATER LEGEND
1 - LAB PURE HATER
2 - EFFLUENT 1
3 - EFFLUENT 2
4 - EFFLUENT 3
1
9
26.20
28.64
9.33
10.45
36.48
5.
18.
3
9
1 91 .00
165.89
-13.15
46.20
27.85
33.
19.
5
9
385.00
343.56
-10.76
92.19
26.84
57.
15.
2
9
29.70
31.08
4.64
8.59
27.63
41
10
4
9
230.00
179.67
-21.88
53.02
29.51
91
62
6
9
461.00
410.78
-10.89
98.41
23.96
63
28
26.
23.
-10.
9.
41.
191.
154.
-19.
42.
27.
*
385.
235.
-38.
25.
10.
1
7
20
56
09
84
75
6.
21.
3
6
00
00
37
79
78
23.
14.
5
6
00
50
83
3P
78
26.
9.
29.
36.
22.
6.
18.
47
57
230.
170.
-25.
28.
16.
48
48
461.
310.
-32.
67.
21.
01
53
2
6
70
42
62
77
59
4
6
00
33
94
40
67
6
7
00
43
66
60
78
26.
19.
-26.
8.
42.
191.
148.
-22.
33.
22.
385.
369.
-3.
127.
34.
1
9
20
14
93
23
98
4.
24.
3
9
00
33
34
59
64
33.
20.
5
9
00
78
95
34
44
29.
7.
2
9
29.70
18.87
-36.48
11.95
63.36
73
89
4
9
230.00
178.00
-22.61
44.75
25.14
09
28
6
8
461.00
385.50
-16.38
83.39
21.63
03
69
1
6
26.20
10.20
-61.07
10.29
100.90
2
17
3
8
191.00
162.47
-14.93
62.61
38.53
10
6
5
7
385.00
209.43
-22.23
44.89
14.99
10
3
2
4
29.70
17.00
-42.76
13.74
80.80
.42
.76
4
7
230.00
184.00
-20.00
28.28
15.37
.99
.34
6
7
461.00
358.14
-22.31
49.41
13.80
.81
.29
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF HATER TYPE ON NICKEL ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) .92332
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLF.O)
2 .1356 ' -.0644
3 -1.3151 .2194
4 -2.6897 .4596
** ANALYSIS OF VARIANCE **
SOURCE PF SUM OF SQUARES MEAN SOUARE F PROfl
REG(DISTILLED) 1 265.2002B 265.20028
0 REG(WATER/DISTILLED) 6 11.838fiO 1.97310 13.35 .0000
I ERROR 167 24.67543 .14776
M
~J
** TOTAL . 174 301.71431
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
IHTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .1356 ( -.7977 , 1.0689) -.0644 ( -.2492 , .1204)
3 -1.3151 ( -2.1719 , -.4584) .2194 ( .0492 , .38%)
4 -2.6897 ( -3.6894 , -1.6001) .4596 { .2653 , .6540)
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 PARAMETERUNTERCEPT/SLOPE).
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE MOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR SELENIUM ANALYSIS BY HATER TYPE
LOU YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
12.10
13.31
11.00
13.90*
12.00
1.00*
11.00
13.00
14.00
17.80
15.00
2
10.50
11.32
9.00 <
13.20*
12.00
1.00
13.00
12.00
13.00
20.40
10.00
1
12.10
4.60
8.00* <
16.80
13.00
9.00
21.00
14.00
1P.OO
25.20
15.00
2
10.50
1.40
8.00* <
14.90
9.00
6.00
17.00
11.00
10.00
10.10
10.00
1
12.10
8.70
8.00*
17.30*
13.00
13.00
17.00
6.00
17.00
6.30
15.00
2
10.50
7.20
5.00*
12.60*
10.00
9.00
15.00
6.00
11.00
8.00
10.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS RY AA ***
RAW DATA FOR SELENIUM ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
n
M
-J
oo
3
76.40
73.20
83.00
89.90*
83.00
83.00
89.00
65.00
71.00
67.90
80.00
4
96.80
113.94
98.00
126.00*
110.00
88.00
109.00
75.00
100.00
79.40
110.00
3
76.40
54.40
36.00*
93.80
94.00
75.00
91.00
71.00
88.00
56.70
90.00
4
96.80
70.00
43.00*
115.00
130.00
9fl.OO
115.00
87.00
110.00
73.60
110.00
3
76.40
64.80
44.00*
113.00*
96.00
75.00
84.00
57.00
78.00
69.10
80.00
4
96.80
80.20
50.00*
131.00*
120.00
52.00
110.00
67.00
65.00
96.90
100.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR SELENIUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING HATER
SURFACE HATER
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
205.00
237.50
204.00
272.00*
260.00
184.00
204.00
140.00
174.00
156.00
230.00
6
246.00
278.00
254.00
322.00*
230.00
44.00*
250.00
150.00
256.00
196.00
270.00
5
205.00
258.00
140.00*
272.00
190.00
171.00
245.00
226.00
180.00
205.00
220.00
6
246.00
324.00
162.00*
313.00
280.00
195.00
288.00
246.00
211.00
273.00
320.00
5
205.00
254.00
148.00*
2°2.00*
190.00
234.00
224.00
202.00
174.00
232.00
200.00
6
246.00
292.00
167.00*
334.00*
220.00
225.00
327.00
212.00
255.00
234.00
300.00
ID
-------
ENVIRONMENTAL MONITORING AND SUPPORT LARORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR SELENIUM ANALYSES BY WATER TYPE
MATER 1
HATER 2
WATER 3
n
i
00
o
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (f REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, t
SINGLE STD DEV, (SR)
ANALYST REL DEV, t
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, t
SINGLE STD DEV, (SR)
ANALYST REL DEV, I
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD DEV, t
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
1
8
12.10
13.39
10.65
2.27
16.92
1.
13.
3
9
76.40
77.23
1.09
8.20
10.62
8.
9.
5
<»
205.00
198.83
-3.01
39.36
19.80
23.
10.
2
9
10.50
11.30
7.64
5.03
44.53
70
80
4
9
96.80
98.15
1.39
14.33
14.60
20
35
6
8
246.00
235.50
-4.27
42.88
18.21
12
65
1
9
12.10
15.18
25.44
6.14
40.42
2
22
3
9
76.40
79.32
3.82
15.70
19.79
4
4
5
9
205.00
218.56
6.61
35.21
16.11
20
B
2
9
10.50
9.93
-5.40
4.54
45.71
.89
.99
4
9
96.80
100.96
4.29
20.35
20.15
.38
.86
6
9
246.00
272.22
10.66
46.55
17.10
.35
.29
1
8
12.10
12.00
-0.83
4.4R
37.32
1
16
3
8
76.40
75.49
-1.19
12.05
15.97
13
16
5
8
205.00
213.75
4.27
26.56
12.43
31
13
2
8
10.50
9.52
-.9.29
2. 75
28.90
.82
.87
4
8
96.80
86.39
-10.76
24.02
27.80
o
.39
.54
6
8
246.00
258.13
4.93
42.95
16.64
.56
.38
WATER LEGEND
1 - LAB PURE WATER
2 - DRINKING HATER
3 - SURFACE HATER
-------
o
I
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON SELENIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) - .99591
WATER INTERCEPT(HATER-OISTILLED) SLOPE(WATER-DISTILLED)
2 -.1625 ' .0443
3 -.1991 .0443
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 251.88890 251.88R90
REG(WATER/DISTILLED) 4 .13646 .03411 .32 .8657
ERROR 139 14.92250 .10736
TOTAL 144 266.94786
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.1625 ( -.7131 , .3880) .0443 ( -.0835 , .1721)
3 -.1991 ( -.7646 , .3fi64) .0443 ( -.0874 , .1759)
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.
-------
ENVIRONMENTAL MONITOR INC, AND SUPPORT LABORATORY
OFFICE OF RESEARCH AHO DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR SELENIUM ANALYSIS RY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
0
M
00
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
q
10
1
11.60
8.30*
9.60
21.30*
13.10
6.50
9.70
14.00
13.10
10.40
16.30*
2
10.00
4.90*
8.70 <
20.70*
8.70
2.20*
7.30 <
8.70
10.90
9.00
10.90*
1
11.60
3.04*
8.00* <
5.80
66.00*
9.00
0.50* <
8.00
6.00
23.20*
5.00
2
10.00
0.75*
8.00* <
1.20 <
10.00
1.00
0.50*
7.00
7.00
13.20
10.00
1
11.60
0.71* -
8.00* <
0.60* <
13.00
22.00
9.00
12.00
9.00
2.70
15.00
2
10.00
*
0.13* -
8.00* <
0.60* <
12.00
7.00
2.00
9.00
2.00
6.70 -
10.00
1
11.60
1.89*
8.00* <
0.60*
15.00
22.00*
2.00
3.00
10.00
25.00* -
15.00
2
10.00
0.30*
8.00*
1.20
11.00
14.00*
2.00
1.00
7.00
27.00*
10.00
-------
ENVIRONMENTAL MONITOR ING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AMD DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS .BY AA ***
RAW DATA FOR SELENIUM ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
n
i '
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
73.00
44.50*
51.10
118.00*
74.00
71. BO
75.00
55.00
92.50
59.20
97.90*
4
92.60
47.20*
71.80
162.00*
89.20
84.90
101.00
59.00
99.00
77.30
131.00*
3
73.00
23.40*
58.00
72.20
63.00
62.00
60.00
37.00
74.00
52.20
85.00
4
92.60
32.20*
74.00
92.20
79.00
73.00
92.00
44.00
87.00
61.60
105.00
3
73.00
16.00*
37.00*
76.70
16.00*
"0.00
105.00
58.00
85.00
88.20
85.00
4
92.60
17.10*
46.00*
104.00
98.00
65.00
108.00
67.00
93.00
110.00
115.00
3
73.00
.
' 15.90*
lfl.00
31.90
52.00
67.00*
100.00
35.00
69.00
25.00
90.00
4
92.60
16.55*
23.00
90.90
66.00
97.00*
131.00
44.00
95.00
21.00
100.00
00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR SELENIUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UGA
LAB PURE WATER EFFLUENT I EFFLUENT 2 EFFLUENT 3
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
197.00
38.80*
169.00
292.00*
228.00
159.00
211.00
185.00
212.00
164.00
229.00*
6
235.00
62.50*
197.00
368.00*
261.00
207.00
237.00
218.00
218.00
172.00
261.00*
5
197.00
63.40*
136.00
243.00
170.00
101.00
169.00
197.00
177.00
161.00
225.00
6
235.00
74.90*
166.00
301.00*
210.00
183.00
208.00
207.00
194.00
181.00
245.00
5
197.00
46.00*
145.00*
237.00
200.00
281.00
263.00
197.00
138.00
176.00
225.00
6
235.00
61.70*
163.00*
237.00
220.00
357.00
223.00
247.00
178.00
212.00
305.00
S
197.00
.
44.70*
98.00
226.00
160.00
235.00*
229.00
135.00
148.00
142.00 -
200.00
6
235.00
49.20*
100.00
293.00
200.00
357.00*
263.00
235.00
173.00
99.70*
250.00
00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON SELENIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(I) « 1.00959
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-OISTILLED)
2 -.9856 ' .1710
3 -.6253 .1353
4 , -1.4455 .2367
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 326.21277 326.21277
_ REG(WATER/DISTILLEn) 6 7.0fl554 1.1R092 6.33 .0000
V ERROR 159 29.68013 .18667
t->
oo
1/1 TOTAL 166 362.97844
** TABLE OF 95S CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-OISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.9856 ( -1.8755 , -.0957) .1710 ( -.032R , .3747)
3 -.6253 ( -1.4822 , .231fi) .1353 ( -.0642 , .334«)
4 -1.4455 ( -2.3520 , -.5390) .2367 ( .0282 , .4453)
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(INTERCEPTXSLOPE).
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
n
i
i'
00
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR SELENIUM ANALYSES BY HATER TYPE
WATER 1
WATER 2
WATER 3
WATER 4
LOW YOUDEN 'PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY(*REL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD DEV, 1
SINGLE STD OEV, (SR)
ANALYST REL DEV, I
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO OEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, t
HIGH YOUOEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STO DEV (S)
OVERALL REL STO OEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, f
1
7
11.60
10.94
-5.67
2.63
24.04
1
12
3
7
73.00
68.37
-6.34
14.32
20.95
5
7
5
7
197.00
189.71
-3.70
27.30
14.39
10
5
2
6
10.00
8.8ft
-11.17
1.16
13.02
.19
.01
4
7
92.60
83.17
-10.18
15.03
18.07
.48
.23
6
7
235.00
215.71
-8.21
28.44
13.18
.45
.15
1
5
11.60
6.76
-41.72
1.67
24.70
3.
51.
3
9
73.00
62.60
-14.25
13.77
21.99
5.
7.
5
9
197.00
175.44
-10.94
43.10
24.57
16.
R.
2
7
10.00
7.06
-29.43
4.58
64.95
55
33
4
9
92.60
78.64
-15.07
18.27
23.23
28
48
6
R
235.00
199.25
-15.21
24.13
12.11
07
58
1
7
11.60
11. Rl
1.85
5.98
50.58
4
44
3
7
73.00
83.99
15.05
14.29
17.02
13
14
5
8
197.00
214. fi3
8.95
46.66
21.74
28
12
2
7
10.00
6.P6
-30.43
3.83
55.07
.17
.45
4
8
92.60
95.00
2.59
10.17
20.18
.28
.84
6
8
235.00
247.38
5.27
57.14
23.10
.0?
.13
1
5
11.60
9.00
-22.41
6.28
69.83
1
18
3
8
73.00
52.61
-27.93
30.73
58.42
13
22
5
8
197.00
167.25
-15.10
46.65
27.89
22
11
2
6
10.00
5.37
-46.33
4.55
84.83
.36
.93
4
8
92.60
71.36
-22.93
39.59
55.47
.95
.50
6
7
235.00
216.29
-7.9fi
64.83
29.97
.23
.59
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 1
3 - EFFLUENT 2
4 - EFFLUENT 3
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR SILVER ANALYSIS BY WATER TYPE
LOU YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER DRINKING HATER SURFACE HATER
n
M
00
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3 <
4
5
6 <
7
8 <
9
10
1
0.45
0.72
0.70
0.90* <
0.60
2.00*
0.05* <
1.00
0.50* <
0.15
0.50
2
0.59
0.83
0.70 <
0.90*
0.60
1.00*
0.05*
1.00
0.50* <
0.28 -
1.00
1
0.45
0.63
0.70* <
1.20 <
0.60
1.00
2.80
26.00*
0.50* <
1.65* <
2.60
2
0.59
0.82
0.70*
0.90*
0.60
1.00 <
1.00
19.00*
0.50* <
0.20*
0.60
1
0.45
0.91
0.90
1.50 <
0.60
1.00*
0.10
15.00*
0.50*
1.56 <
0.40
2
0.59
0.95
0.40
0.90*
0.50
1.00
0.30
20.00
2fl.OO
0.20*
0.50
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR SILVER ANALYSIS BY MATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
3 4
5.68 4.09
4.82 3.45
5.10 3.70
0.90* < 0.90*
5.50 3.10
6.00 4.00
5.60 4.60
5.00 2.00
7.40 4.90
2.18 1.31
5.00 3.60
AMPUL NO: 3
TRUE CONC: 5.68
4
4.09
3
5.68
4
4.09
LAB NUMBER
O
1
h~J
oo
oo
1
2
3
4
5
6
7
8
9
10
5.87
6.20
5.20
5.90
6.00*
4.60
5.00
5.30*
5.22
6.50
4.60
3.70
3.70
4.00
7.00*
3.80
3.00
2.40*
3.37 -
5.00
6.23
4.90
5.70
5.70
6.00
7.10
4.00
4.70
1.92* -
6.60
4.41
2.80
4.10
4.00
4.00
4.20
2.00
2.90
2.20*
4.40
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR SILVER ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR. UNITS - UG/L
LAB PURE MATER DRINKING WATER SURFACE WATER
AMPUL NO: 5
TRUE CONC: 11.40
6
13.60
5
11.40
6
13.60
5
11.40
6
13.60
LAB NUMBER
O
1
J "*
CD
VO
1
2
3
4
5
6
7
8
9
10
8.83
11.90
10.20
11.00
18.00*
13'. 00
8.00
7.00*
3.72
14.00
12.85
14.20
12.50
13.00
26.00*
15.00
21.00
11.00*
13.20
19.00
13.17
10.40
10.30
11.00
13.00
15.00
9.00
9.80
1.50*
14.00
14.12
12.60
14.10
14.00
18.00
13.00
12.00
10.50
1.77*
16.00
10.60
9.60
5.60
11.00
7.00
9.60
9.00
13.00
3.49
11.50
15.40
11.00
9.60
12.00
10.00
11.60
12.00
17.00
2.06'
13.50
-------
o
I
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR SILVER ANALYSES BY WATER TYPE
WATER 1 WATER 2 WATER 3
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY(IREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD OEV, »
SINGLE STO DEV, (SR)
ANALYST REL DEV, S
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (SREL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD DEV, I
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (tREL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD DEV, *
SINGLE STD DEV, (SR)
ANALYST REL DEV, S
1
6
0.45
0.61
34.43
0.2B
46.01
0
20
3
8
5.68
5.56
-2.09
0.65
11.74
0
7
5
8
11.40
10.08
-11.57
3.26
32.34
2
23
2
6
0.59
0.73
24.37
0.27
37.31
.14
.35
4
8
4.09
3.90
-4.74
0.64
16.49
.36
.70
6
8
13.60
15.09
10.98
3.18
21.05
.90
.03
1
6
0.45
1.47
223.44
0.98
66.59
0
67
3
0
5.68
5.66
-0.37
0.98
17.29
0
5
5
9
11.40
11.74
2.99
2.09
17.83
1
11
2
5
0.59
0.80
36.04
0.20
24.90
.76
.15
4
9
4.09
3.65
-10.87
0.86
23.55
.27
.84
6
9
13.60
13.81
1.57
2.21
15.97
.44
.24
1
7
0.45
0.85
87.44
0.54
63.51
3
9
5.68
5.18
-8.84
1.37
26.52
5
10
11.40
9.04
-20.71
2.90
32.03
2
8
0.59
6.46
992.43
1.1.04
171.00
0.19
5.28
4
Q
4.09
3.41
-16.71
1.15
33.79
0.52
12.12
6
q
13.60
12.46
-8.42
2.45
19.64
0.92
8.53
WATER LEGEND
1 - LAB PURE WATER
2 - DRINKING WATER
3 - SURFACE WATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON SILVER ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) .93317
WATER INTERCEPT(UATER-DISTILLED) SLOPE(WATER-DISTILLEO)
2 .2422 . -.1706
3 .2184 -.2108
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(OISTILLED) 1 144.54030 144.54030
REG(WATER/DISTILLED) 4 1.97970 .49493 1.59 .Ifl02
ERROR 128 39.78208 .31080
n
i
TOTAL 133 186.30207
** TABLE OF 95» CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-OISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .2422 ( -.2089 , .6934) -.1706 ( -.4077 , .0665)
3 .2184 ( -.1943 , .6312) -.2108 ( -.4345 , .0130)
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.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LARORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR SILVER ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
o
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
8.48
11.40
10.50
fl.50
9.30
13.00*
12.00
8.70
5.20
4.00*
13.00*
2
10.70
14.70
12.80
10.10
10.90
18.50*
10.40
8.70
7.60
7.50* -
15.20*
1
8.48
10.80
37.20*
8.00
11.00
8.00
0.90*
7.00
7.30
0.01*
11.50*
2
10.70
12.50 -
9.70 <
8.30 <
9.00
10.00
1.00*
8.00
10.80
10.70
13.00*
1
8.48
1.20*
0.70*
0.90*
6.60
5.00
0.50
6.00
2.70
0.81 -
10.00*
2
10.70
9.70* '
1.20
7.20
11.00
6.00
0.70
6.00
11.10
0.46*
16.00*
1
8.48
7.12
8.70
6.60
9.30
9.00
1.10*
7.00
13.40
5.15*
11.50
2
10.70
10.03
10.70
10.60
11.00
14.00
1.30*
fl.OO
16.90
0.67*
19.00
vo
-------
EMVIROMHEMTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAM DATA FOR SILVER ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE MATER EFFLUENT 1 EFFLUENT 2 EFFLUENT 3
AMPUL NO: 3
TRUE CONC: 21.50
4
17.80
3
21.50
4
17.80
3
21.50
4
17.80
3
21.50
4
17.80
LAB NUMBER
O
1
t-~*
10
U)
1
2
3
4
5
6
7
8
4
10
26.10
22.00
19.50
21.70
43.50*
30.40
19.60
20.60
6.90*
30.40*
16.50
18.30
16.00
17.40
31.50*
28.30*
48.90*
16.30
17.90*
25.00*
23.40
21.50
20.50
17.00
28.00
2.10*
16.00
19.40
23.00
28.00*
20.10 -
16.50
14.50
20.00
23.00
1.70*
15.00
14.40
20.20
21.00*
6.85* -
8.10
21.50
14.00
4.00
1.80
17.00
18.60
6.96
34.00*
7.50*
6.60
6.70
11.00
51.00*
1.60
14.00
14.80
1.19
22.00*
' 21.83
19.20
21.00
22.00
34.00
1.10*
10.00
29.50
11.30*
36.00
17.38
15.80
13.50
19.00
28.00
0.90*
12.00
263.00*
3.69*
12.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR SILVER ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 1 EFFLUENT 2 EFFLUENT 3
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
42.70
40.30
8.80*
38.90
39.10
76.10*
36.40
41.30
28.30*
7.20*
56.50*
6
56.50
33.90
11.40
49.70
59.80
72.80*
38.00
3fi.90
41.30
33.40*
76.10*
5
42.70
47.30
43.90
21.00
41.00
61.00
4.20*
28.00
26.00
33.00
54.00*
6
56.50
63.50 -
52.00
43.70
53.00
71.00
5.20*
40.00
37.00
45.00
70.00*
5
42.70
6.50* -
32.40
19.30
24.00
26.00
3.60
10.00
36.60
2.12
62.00*
6
56.50
.
7.40*
45.70
52.50
21.00
36.00
4.70
20.00
39.00
1.37
66.00*
5
42.70
25.83
27.00
37.30
39.00
52.00
4.30*
12.00
24.60
4.40*
52.00
6
56.50
16.98
31.30
34.00
36.00
32.00
3.70
28.00
38.80
4.38
48.00
n
i
-------
o
I
Ul
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR SILVER ANALYSES BY WATER TYPE
WATER 1 WATER 2 WATER 3 WATER 4
\~t
LOW YOUOEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD DEV, I
SINGLE STD DEV, (SR)
ANALYST REL OEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACYUREL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD DEV, *
SINGLE STD DEV, (SR)
ANALYST REL DEV, I
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (SREL ERROR)
OVERALL STO DEV (S)
OVERALL REL STO DEV, «
SINGLE STO DEV, (SR)
ANALYST REL DEV, t
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 1
3 - EFFLUENT 2
4 - EFFLUENT 3
1
7
8. 48
9.37
10.51
2.27
24.22
1.
11.
3
7
21.50
22.84
6.25
4.01
17.55
1.
9.
5
5
42.70
39.20
-8.20
1.R4
4.70
7.
20.
2
7
10.70
10.74
0.40
2.40
22.32
17
64
4
5
17.80
16.90
-5.06
0.94
5.57
80
08
6
7
56.50
38.71
-31.48
14.97
38.67
97
47
1
6
8.48
8.68
2.40
1.76
20.30
1
14
3
8
21.50
21.10
-1.86
3.83
18.16
2
10
5
R
42.70
37.65
-11.83
13.18
35.01
3
7
2
8
10.70
9.87
-7.71
1.48
14.94
.31
.13
4
8
17.80
17.96
0.91
3.27
18.19
.09
.69
6
8
56.50
50.65
-10.35
11.75
23.20
.21
.27
1
6
8.48
3.60
-57.53
2.64
73.38
2
52
3
8
21.50
11.49
-46.53
7.26
63.20
3
35
5
8
42.70
19.25
-54.91
12.91
67.04
8
35
2
7
10.70
6.17
-42.32
. 4.15
67.26
.54
.05
4
7
17.80
7.08
-55.14
5.51
69.02
.42
.09
6
8
56.50
27.53
-51.27
18.75
68.11
.22
.16
1
8
8.48
9.08
7.05
2.36
26.01
1
13
3
8
21.50
24.19
12.52
8.54
35.31
5
28
5
8
42.70
33.72
-21.04
14.00
41.51
8
25
2
8
10.70
12.53
17.09
3.77
30.06
.48
.68
4
7
17.80
16.81
-5.55
5.61
33.35
.«!
.36
6
8
56.50
33.13
-41.35
8.90
26.85
.40
.13
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF HATER TYPE ON SILVER ANALYSIS
** POINT ESTIMATES **
DISTILLED MATER SLOPE:GAMMA(1) « .79850
WATER INTERCEPT WATER-OI STILLED) SLOPE (WATER-DISTILLED)
2 -.5369 '. .1651
3 -1.3926 .1612
4 .1400 -.1213
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 56.25263 56.25263
REG(WATERXDISTILLED) 6 22.27050 3.71175 15.17 .0000
7 ERROR 158 38.64740 .24460
M
VD
** TOTAL 165 117.17053
** TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-OISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.5369 ( -1.8468 , .7729) .1651 ( -.2546 , .5848)
3 -1.3<»26 ( -2.7166 , -.0686) .1612 ( -.2612 , .5836)
4 .1400 ( -1.1410 , 1.4211) -.1213 ( -.5329 . .2903)
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 AME NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
r>
i
M
ID
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR THALLIUM ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
10.50
9.95
10.00
8.10*
11.00
8.00
13.00*
9.00
8.90
92.50*
9.00*
2
13.00
12.48
10.00
10.40*
12.00
10.00
16.00*
12.00
8.40
11.40
15.00*
1
10.50
9.40
8.00
3.10*
10.00
10.00
15.00*
8.00
6.30 <
7.90
9.00
2
13.00
10.50
9.00
4.30*
11.00
12.00
10.00*
10.00 <
3.00*
8.85
12.00
1
10.50
6.90
7.00
5.40
10.00
21.00*
10.00
1.00*
62.00*
5.97
9.00
2
13.00
8.17
8.00
7.70
11.00
18.00*
13.00
10.00
7.00
9.24
13.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR THALLIUM ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER DRINKING WATER SURFACE WATER
AMPUL NO: 3
TRUE CONC: 120.00
4
99.60
3
120.00
4
98.60
3
120.00
4
98.60
LAB NUMBER '
O
1
t*
VD
CD
1
2
3
4
5
6
7
8
9
10
100.50
112.00
68.10*
110.00
97.00
124.00*
98.00
112.00
120.00
140.00*
83.20
98.00
56.80*
95.00
66.00
100.00*
92.00
80.00
87.50
110.00*
108.00
04.00
54.90*
110.00
148.00
154.00*
84.00
91.80
103.00
140.00
90.00
79.00
44.60*
90.00
118.00
130.00*
89.00
79.90
85.00
120.00
88.60
88.00
80.70
100.00
211.00*
126.00
88.00
89.00
104.00
140.00
75.20
75.00
68.30
89.00
163.00*
93.00
71.00
51.00
62.00
120.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR THALLIUM ANALYSIS BY MATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
o
1
I1
VO
VO
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
203.00
173.55
191.00
80.50*
190.00
201.00
222.00*
185.00
170.00
134.00
300.00*
6
252.00
216.20
245.00
91.00*
230.00
266.00
247.00*
225.00
200.00
197.00
300.00*
5
203.00
197.00
104.00
68.90*
180.00
241.00
310.00*
125.00
168.00
166.00
260.00
.
6
252.00
227.00
97.00
83.20*
220.00
310.00
358.00*
150.00
190.00
182.00
240.00
5
203.00
146.00
140.00
. 132.00
190.00
302.00*
351.00*
120.00
160.00
172.00
220.00
6
252.00
175.00
173.00
224.00
220.00
459.00*
405.00
140.00
217.00
206.00
300.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR THALLIUM ANALYSES BY HATER TYPE
WATER 1 WATER 2 WATER 3
n
i
o
0
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (IREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, I
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (tREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, *
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (tREL ERROR)
OVERALL STO OEV (S)
OVERALL REL STD DEV, 1,
SINGLE STO DEV, (SR)
ANALYST REL DEV, X
1
6
10.50
9.47
-9.76
1.05
11.13
3
7
120.00
107.07
-10.77
8.67
8.10
5
7
203.00
177.79
-12.42
22.02
12.39
2
7
13.00
10.90
-16.18
1.47
13.53
1.00
9.77
4
7
98.60
85.96
-12.B2
10.86
12.63
7.51
7.78
6
7
252.00
225.60
-10.48
24.46
10.84
9.27
4.59
1
8
10.50
8.57
-18.33
1.27
14.76
3
8
120.00
109.85
-8.46
22.87
20.82
5
fl
203.00
180.13
-11.27
52.85
29.34
2
7
13.00
10.48
-19.40
1.29
12.30
0.55
5.80
4
8
98.60
93.86
-4.80
16.10
17.15
7.04
6.92
6
8
252.00
202.00
-19.84
63.62
31.49
19.36
10.13
1
7
10.50
7.75
-26.16
1.90
24.51
3
9
120.00
100.48
-16.27
20.00
19.91
5
fl
203.00
IfiO.OO
-21.18
33.00
20.63
2
q
13.00
9.68
-25.55
'2,24
23.19
0.85
9.80
4
9
98.60
78.28
-20.61
20.17
25.77
8.57
9.58
6
9
252.00
228.89
-9.17
79.66
34.80
lfl.75
9.64
WATER LEGEND
1 - LAB PURE WATER
2 - DRINKING WATER
3 - SURFACE WATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON THALLIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED HATER SLOPE:GAMMA(1) » 1.00818
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 -.1063 . .0069
3 -.3634 .0400
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PR08
REG(DISTILLED) 1 226.62423 226.62423
REG(WATER/DISTILLED) 4 .56728 .14182 6.00 .0002
ERROR 124 2.92933 .02362
O
J, TOTAL 129 230.12085
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.1063 ( -.3970 , .1844) .0069 ( -.0589 , .0726)
3 -.3634 ( -.6549, -.0719) .0480 ( -.0171 , .1131)
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS NO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AMD 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.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LAPORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR THALLIUM ANALYSIS RY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
AMPUL NO:
TRUE CONC: 10
1
.00
2
12.40
1
10.00
2
12.40
1
10.00
12
2
.40
1
10.00
2
12.40
LAB NUMBER
O
1
to
0
to
1
2
3
4
5
6
7
8
9
10
2
6
< 2
9
8
9
6
< 3
4
10
.10*
.50
.10*
.90
.70
.80*
.50
.00*
.00
.90*
3.50*
9.80 <
4.50* <
10.60
12.00
14.00*
9.80
8.30
9.80
11.90*
4.95
3.00* <
2.10* <
11.00
20.00*
7.00
5.00
5.40
5.47
8.00
6.74
3.00*
2.10* <
9.60
29.00*
8.00
6.00
5.60 <
7.68
11.00
5.20
4.00
2.10*
9.60*
7.00
9.00
5.00
3.00*
2.59
9.00*
6
4
3
13
8
10
8
4
2
12
.20
.00
.80* <
.00*
.00
.00
.00
.00
.91
.00*
4.70
5.00
2.10*
8.40
7.00*
8.00
5.00*
7.70
5.23
6.00
6.32
6.00
3.70*
11.00
12.00*
10.00
7.00*
8.50
7.07
8.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR THALLIUM ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
EFFLUENT 1
EFFLUENT 2
EFFLUENT 3
AMPUL NO: 3
TRUE CONC: 115.00
4
94.30
3
115.00
4
94.30
3
115.00
4
94.30
3
115.00
4
94.30
LAB NUMBER
O
1
o
U)
1
2
3
4
5
6
7
8
9
10
39.80*
101.00
21.80*
109.00
83.00
129.00*
105.00
64.60
103.00
136.00*
31.60*
33.70*
17.70*
96.00
100.00
97.00*
88.00
84.60
85.50
114.00*
73.00
56.00*
51.20*
99.00
291.00*
84.00
64.00
64.00
83.40
109.00
57.00
40.00*
45.30*
120.00
236.00*
70.00
53.00
54.00
69.20
109.00
73.00
61.00
54.RO*
110.00*
71.00
75.00
69.00
75.00
78.70
189.00*
62.00
50.00
42.50*
96.00*
85.00
59.00
54.00
61.00
67.40
109.00*
"77.36
88.00
65.00*
100.00
114.00*
79.00
66.00*
91.50
94.00
127.00
62.46
72.00
49.40*
85.00
123.00*
68.00
57.00*
82.20
79.50
97.00
-------
ENVIRONMENTAL MOMI TORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AMD DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR THALLIUM ANALYSIS BY HATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER EFFLUENT 1 EFFLUENT 2 EFFLUENT 3
n
i
ro
o
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
194.00
83.50*
93.00
26.40*
174.00
164.00
199.00*
163.00
119.00
lftl.00
228.00*
6
241.00
95.40*
227.00
33.00*
217.00
227.00
241.00*
206.00
203.00
85.00*
282.00*
5
194.00
104.00
96.00*
95.50*
200.00
447.00*
124.00
108.00
125.00
135.00
239.00
6
241.00
128.00
120.00*
120.00*
240.00
540.00*
146.00
122.00
160.00
170.00
239.00
5
194.00
112.00
107.00
105.00*
220.00*
175.00*
119.00
84.00
104.00
119.00
169.00*
6
241.00
119.00
156.00
120.00*
240.00*
164.00
134.00
106.00
160.00
227.00
309.00*
5
194.00
129.00
125.00
118.00*
170.00
210.00*
123.00
100.00*
153.00
144.00
207.00
6
241.00
147.00
130.00
193.00*
210.00
314.00*
146.00
132.00*
200.00
189.50
257.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR THALLIUM ANALYSES BY WATER TYPE
WATER 1
WATER 2
WATER 3
WATER 4
o
1
K)
O
Ln
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (tREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, %
SINGLE STD OEV, (SR)
ANALYST REL OEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (SREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, S
SINGLE STD DEV, (SR)
ANALYST REL DEV, «
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (tREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, *
SINGLE STD DEV, (SR)
ANALYST REL DEV, I
1
5
10.00
7.12
-26.60
2.26
31.97
1
14
3
6
115.00
94.27
-18.03
17.09
18.13
13
14
5
6
194.00
149.00
-23.20
34.95
23.45
26
14
2
6
12.40
10.05
-18.95
1.21
12.07
.2fl
.85
4
5
94.30
90.82
-3.69
6.82
7.51
.3fl
.45
6
5
241.00
216.00
-10.37
11.31
5.24
.79
.68
1
7
10.00
6.69
-33.11
2.21
33.11
1
14
3
7
115.00
62.34
-28.40
17.09
20.75
9
11
5
7
194.00
147. R6
-23.78
51.31
34.70
9
6
2
7
12.40
7.60
-37.07
1.95
24.95
.02
.03
4
7
94.30
76.03
-19.38
27.33
35.95
.29
.74
6
7
241.00
172.14
-28.57
4B.P4
28.43
.91
.19
10
5
-45
2
41
115
71
-37
5
7
194
107
-44
13
12
1
6
.00
.46
.35
.26
.36
0.
12.
3
7
.00
.81
.55
.70
.93
7.
10.
5
6
.00
.50
.59
.03
.13
26.
20.
2
7
12.40
6.16
-50.33
2.63
42.66
74'
70
4
7
94.30
62.63
-33.59
11.35
18.13
37
97
6
7
241.00
152.29
-36.81
39.53
25.96
36
30
1
7
10.00
6.43
-35.67
1.56
24.27
3
7
115.00
93.84
-18.40
16.68
17.77
5
7
194.00
150.14
-22.61
30.25
20.14
12
6
-34
1
22
0.44
6.03
94
78
-17
11
14
4.74
5.52
241
184
-23
43
23
10.69
6.39
2
7
.40
.13
.46
.66
.92
4
7
.30
.02
.26 .
.60
.87
6
7
.00
.07
.62
.07
.40
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 1
3 - EFFLUENT 2
4 - EFFLUENT 3
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF MATER TYPE ON THALLIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED HATER SLOPE:GAHMA(1) « 1.04062
MATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-OISTILLED)
2 -.2054 '' .0052
3 -.4827 .0447
4 -.2425 .0295
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(OISTILLED) 1 2flO.13304 280.13304
O REG(HATER/DISTILLEO) 6 1.63231 .27205 6.88 .0000
I ERROR 141 5.57431 .03953
to
o
TOTAL 148 287.33967
** TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-OISTILLED) SLOPE(MATER-DISTILLED)
MATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.2054 ( -.6287 , .2180) .0052 ( -.0916 . .1021)
3 -.4827 ( -.9110 , -.0544) .0447 ( -.0536 , .1431)
4 -.2425 ( -.665B , .1809) .0295 ( -.0673 , .1264)
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 ORTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LAnORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR VANADIUM ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UGA
LAB PURE WATER
DRINKING WATER
SURFACE WATER
n
i
to
o
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
175
213
Ifl4
161
150
119
242
141
292
132
150
1
.00
.00*
.00
.00
.00
.00
.00*
.00
.00*
.00
.00
151
298
185
147
130
mo
197
110
180
125
150
2
.00
.00*
.00
.00
.00
.00
.00
.00
.00*
.00
.00
1
175.00
226.00
206.00
197.00
150.00
250.00
174.00
120.00
70.00
141.00
200.00
151.
133.
190.
163.
140.
114.
131.
99.
2
00
00
00
00
00
00
00
00
63.00
131.
150.
00
00
175
520
173
157
140
296
235
131
200
142
150
1
.00
.00*
.00
.00
.00
.00*
.00*
.00
.00
.00
.00
2
151.00
543.00*
121.00
135.00
120.00
109.00
201.00*
114.00
162.00
136.00
150.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR VANADIUM ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
AMPUL NO: 3
TRUE CONC: 404.00
4
318.00
3
404.00
4
318.00
3
404.00
4
318.00
LAB NUMBER
n
1
o
oo
1
2
3
4
5
6
7
8
9
10
682.00*
328.00
411.00
330.00
139.00
423.00
36.00
1040.00*
247.00
400.00
612.00*
301.00
383.00
270.00
160.00
310.00
24.00
800.00*
179.00
350.00
429.00
274.00
411.00
350.00
168.00
412.00
336.00
1450.00*
305.00
350.00
384.00
342.00
380.00
290.00
182.00
342.00
313.00
1760.00*
261.00
300.00
311.00
359.00
332.00
308.00
253.00
440.00*
855.00*
390.00
332.00
300.00
309.00
299.00
257.00
280.00
448.00
413.00*
87R.OO*
380.00
256.00
400.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR VANADIUM ANALYSIS BY HATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE HATER
DRINKING HATER
SURFACE HATER
AMPUL NO: 5
TRUE CONC: 982.00
6
855.00
5
982.00
6
855.00
5
982.00
6
855.00
LAB NUMBER
n
i
NJ
O
vo
1
2
3
4
5
6
7
8
9
10
1649.00*
945.00
1200.00
190.00
426.00
930.00
1120.00
3620.00*
743.00
1100.00
1236.00*
865.00
82*. 00
160.00
549.00
795.00
962.00
1500.00*
612.00
900.00
881.00
1001.00
1330.00
920.00
658.00
1230.00
1200.00
2970.00*
872.00
1100.00
861.00
766.00
1060.00
770.00
603.00
1002.00
1040.00
2570.00*
B42.00
800.00
1009.00
980.00
759.00
710.00
983.00
1102.00*
1080.00
1000.00
821.00
950.00
785.00
928.00
658.00
720.00
2017.00*
1000.00*
900.00
830.00
963.00
900.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR VANADIUM ANALYSES BY MATER TYPE
WATER 1
WATER 2
WATER 3
o
1
NJ
1
0
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, t
SINGLE STO DEV, (SR)
ANALYST REL DEV, t
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (SREL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD OEV, I
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACYUREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, *
SINGLE STO DEV, (SR)
ANALYST REL DEV, S
175
148
-15
20
14
404
289
-28
139
48
982
831
-15
358
43
1
7
.00
.14
.35
.89
.10
21
13
3
8
.00
.25
.40
.71
.30
28
10
5
8
.00
.75
.30
.07
.05
100
13
151
153
1
31
20
.04
.98
318
247
-22
118
47
.53
.64
855
708
-17
262
37
.13
.00
2
8
.00
.00
.32
.39
.51
4
8
.00
.13
.29
.59
.99
6
8
.00
.88
.09
.62
.05
1
10
175.00
173.40
-0.91
53.85
31.06
29.
19.
3
9
404.00
337.22
-16.53
81.74
24.24
30.
9.
5
9
982.00
1021.33
4.01
212.61
20.82
74.
7.
151
131
-12
34
26
77
54
318
310
-2
62
20
43
40
855
860
0
149
17
82
95
2
10
.00
.40
.98
.78
.47
4
9
.00
.44
.38
.96
.28
6
9
.00
.44
.64
.78
.41
175
156
-10
23
15
404
323
-20
40
12
982
921
-6
126
13
1
7
.00
.14
.78
.59
.11
12.
8.
3
8
.00
.13
.02
.96
.68
67.
20.
5
9
.00
.33
.18
.59
.74
83.
9.
2
8
151.00
130.88
-13.33
IB. 35
14.02
67
83
4
8
318.00
328.63
3.34
71.73
21.83
44
69
6
8
855.00
835.50
-2.28
107.28
12.84
80
54
WATER LEGEND
1 - LAB PURE WATER
2 - DRINKING WATER
3 - SURFACE WATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF MATER TYPE ON VANADIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED HATER SLOPE:GAMMAf1) .87855
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-OISTILLED)
2 -.8929 " .1859
3 -.7075 .1549
** ANALYSIS OF VARIANCE **
SOURCE OF SIM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 76.03353 76.03353
REGfWATER/DISTILLED) 4 1.85319 .46330 3.32 .0125
ERROR 136 18.97582 .13953
TOTAL 141 96.86254
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-OISTILLEO)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.8929 ( -2.4440 , .6582) .1859 ( -.0738 , .4455)
3 -.7075 { -2.3216 , .9067) .1549 ( -.1143 , .424?)
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 AMD INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR VANADIUM ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 1 EFFLUENT 2
n
i
ro
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
167.00
204.00*
176.00
154.00
143.00
114.00
231.00*
135.00
279.00*
126.00
143.00
2
144.00
2B5.00*
177.00
141.00
124.00
172.00
188.00
105.00
172.00*
119.00
143.00
1
167.00
250.00*
183.00
134.00
110.00
73.00*
167.00
147.00
250.00
377.00*
125.00
2
144.00
199.00*
122.00
142.00
140.00
15.00*
185.00
124.00
200.00
190.00*
125.00
1
167.00
141.00
155.00
143.00
140.00
130.00
248.00*
103.00*
150.00
15fi.OO
150.00
2
144.00
104.00
135.00
115.00
120.00
fl.OO
241.00*
102.00
130.00
195.00
100.00
K)
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR VANADIUM ANALYSIS BY HATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 1 EFFLUENT 2
h
i
to
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
387.00
652.00*
313.00
3P3.00
315.00
133.00
404.00
34.00
994.00*
236.00
382.00
4
304.00
585.00*
288.00
366.00
258.00
153.00
296.00
23.00
764.00*
171.00
334.00
3
387.00
498.00*
357.00
390.00
280.00
40.00*
545.00
29fl.OO
350.00
523.00*
275.00
4
304.00
546.00*
448.00
347.00
300.00
24.00*
502.00
247.00
300.00
433.00*
225.00
3
387.00
300.00
443.00
264.00
280.00
674.00*
593.00*
333.00
360.00
2"2.00
300.00
4
304.00
307.00
267.00
212.00
250.00
275.00
500.00*
336.00
320.00
470.00*
300.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR VANADIUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT I EFFLUENT 2
n
i
KJ
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
o
10
939.
1S76.
903.
1147.
182.
407.
089.
1070.
3459.
710.
1051.
5
00
00*
00
00
00
00
00
00
00*
00
00
6
617.00
1181.00*
827.00
791.00
153.00
525.00
760.00
919.00
1433.00*
585.00
860.00
939.
1338.
1040.
10RO.
920.
607.
1280.
667.
950.
5653.
975.
5
00
00*
00
00
00
00*
00
00
00
00*
00
817
1048
945
1010
700
573
1207
570
850
1113
775
6
.00
.00*
.00
.00
.00
.00*
.00
.00
.00
.00*
.00
939.
829.
1140.
691.
850.
457.
1150.
1040.
898.
1113.
800.
5
00
00
00
00
00
00
00*
00
00
00
00
6
817.00
797.00
885.00
664.00
730.00
746.00
1050.00*
718.00
760.00
1133.00*
700.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR VANADIUM ANALYSES RY HATER TYPE
WATER 1
WATER 2
WATER 3
n
i
h-'
m
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD DEV, t
SINGLE STD DEV, (SR)
ANALYST REL DEV, t
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACYUREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, «
SINGLE STD DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (tREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, t
SIHGLE STO DEV, (SR)
ANALYST REL DEV, *
WATER LEGEND
1 - LAR PURE WATER
2 - EFFLUENT 1
3 - EFFLUENT 2
167
141
-15
19
14
387
276
-28
133
48
939
794
-15
342
43
1
7
.00
.57
.23
.96
.10
20
13
3
8
.00
.25
.62
.53
.34
27
10
5
8
.00
.88
.35
.07
.03
95
13
144.
146.
1.
30.
20.
.06
.95
304.
236.
-22.
113.
47.
.30
.66
817.
677.
-17.
250.
37.
.85
.02
2
8
00
13
48
07
58
4
8
00
13
33
25
96
6
8
00
50
07
88
03
1
7
167.00
159.43
-4.53
46.99
29.47
24
15
3
7
387.00
356.43
-7.90
93.64
26.27
38
11
5
7
939.00
987.43
5.16
185.16
18.75
43
4
144
148
2
31
21
.44
.89
304
338
11
102
30
.42
.06
817
865
5
210
24
.43
.69
2
7
.00
.29
.98
.50
.24
4
7
.00
.43
.33
.48
.28
6
7
.00
.20
.91
.94
.38
167
145
-12
8
6
387
321
-16
57
17
939
868
-7
215
24
1
8
.00
.63
.80
.77
.02
31
24
3
8
.00
.50
.93
.57
.91
45
14
5
9
.00
.67
.49
.41
.80
120
16
2
9
144.00
112.11
-22.15
48.66
43.40
.55
.48
4
8
304.00
283.38
-6.78
40.52
14.30
.08
.91
6
8
817.00
750.00
-8.20
67.47
9.00
.64
.02
-------
n
I
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON VANADIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMAj1) .87319
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
2 -.7094 * ' .156?
3 -1.3806 .2547
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 72.93324 72.93324
REG(WATERXDISTILLED) 4 1.71256 .42814 2.37 .0562
ERROR 124 22.41261 .18075
TOTAL 129 97.05841
** TABLE OF 95t CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.7094 ( -2.5922 , 1.1734) .1562 ( -.1605 , .4730)
3 -1.3806 ( -3.1699 , .4086) .2547 ( -.0466 , .5559)
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.
I M V S: PAGE 15
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR VANADIUM ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - MG/L
EFFLUENT 3
o
1
ro
AMPUL NO:
TRUE CONC:
LAB NUMBER
1 !
2
3
4
5
6
7
e
9 (
10
1
.58
>.48*
.88
.84
.52
.24* (
.57
.52
1.40* <
).91* (
.52 1
2
.36 1
.88*
.37
.57
.19
.93* (
.35
.26
>.38*
).65* (
.30 1
1
.58 1
.20
.43
.57
.40
.81 (
.04
.55
.38
).70* (
1.45
?.
1.36
.15
.15
.55*
.10
).56*
.24
.25
.17
).72*
1.20
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR VANADIUM ANALYSIS BY MATER TYPE
MEDIUM YOUDEH PAIR, UNITS - MG/L
LAB PURE HATER EFFLUENT 3
n
i
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
B
9
10
3
2.34
4.32*
2.55
2.06
2.17
0.88*
2.11
2.15
5.10*
1.22*
1.85
4
2.70
5.25*
2.78
2.36
2.50
0.75*
2.51
2.93
4.40*
1.41*
2.06
3
2.34
2.46
2.13
2.69
2.00
1.60
2.34
2.32
1.97
1.49*
2.20
4
2.70
?.38
2.72
2.86
2.30
1.54*
2.83
2.55
2.44
1.80*
2.70
00
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR VANADIUM ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - MG/L
EFFLUENT 3
n
i
ro
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
5.29
5.96*
6.03
6.23
4. 56
0.22*
4.92
4.92
8.97*
2.82*
4.35
6
6.03
12.23*
6.68
9.04*
5.87
0.17*
6.12
5.82
11.41*
3.32*
5.98
5
5.29
4.33
3.72
4.99
4.80
5.76
6.34
4.08
4.63
3.12*
6.20
6
6.03
5.36
5.66
3.51
5.40
7.86
7.14
4.93
5.20
3.87*
6.20
-------
n
i
to
NJ
o
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR VANADIUM ANALYSES BY HATER TYPE
WATER 1 WATER 2
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MGA
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO OEV (S)
OVERALL REL STO OEV, t
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUOEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STO DEV
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON VANADIUM ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMAf1) » .99654
WATER INTERCEPT(WATER-OISTILLED) SLOPE(WATER-DISTILLED)
2 -.1207 * ' .0662
"ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 28.22095 28.22095
REG(WATERXDISTILLED) 2 .07865 .03932 1.73 .1R50
ERROR 74 1.68535 .02278
n
I
^ TOTAL 77 29.98494
N)
** TABLE OF 95t CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
IHTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 -.1207 ( -.2787 , .0373) .0662 ( -.0686 , .2010)
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(INTERCEPVSLOPE).
THE SLOPE AND INTERCEPT ESTIMATES FROM THIS ANALYSIS ARE NOT THE SAME AS THOSE OBTAINED FROM THE PRECISION
AND ACCURACY REGRESSIONS PERFORMED EARLIER.
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS RY AA ***
RAW DATA FOR ZINC ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
0
1
AMPUL NO:
TRUE CONC:
LAB NUMBER
I
2
3
4
5
6
7
8
9
10
1
0.54
3.60
4.50
< 0.20*
400.00*
57.00*
< 40.00*
< 1.00*
2.60
4658.00*
1.00
2
0.75
4.00 -
16.90*
< 0.20*
480.00*
< 5.00*
< 40.00* <
< I. 00* -
3.00 <
0.27 -
2.00
1
0.54
6.00*
19.80
17.60 <
500.00*
41.00
2.00* <
18.00* -
1.00*
18.58* -
1.00
2
0.75
6.00 -
71.10*
0.20* <
400.00*
17.00
2.00* <
20.00* -
0.80
1.50* -
1.00
1
0.54
22.60*
2. no
0.20*
300.00*
6.00
2.00*
2.00*
290.00*
10.50*
0.50
2
0.75
49.00
< 0.30*
< 0.20*
1000.00*
15.00
< 2.00*
4.00
320.00*
- 15.30*
5.50
N)
-------
ENVIRONMENTAL MOM I TOR INC, AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ZINC ANALYSIS BY MATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER
DRINKING WATER
SURFACE WATER
o
1
KJ
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
5.32
5.RO
50.60
14.90
860.00*
52.00
< 40.00*
5.00
60.00
27.20
7.50
4
6.14
0.00*
4.60
2.40
360.00*
57.00
< 40.00*
3.00
52.00
0.78
4.50
3
5.32
8.10
3R.80
543.00*
900.00*
63.00
< 2.00*
- 18.00*
22.00
- 5.60*
3.50
4
6.14
2.10
15.40
< 0.20*
100.00*
34.00
< 2.00*
- 20.00*
20.00
284.00*
4.00
3
5.32
- 10.20*
3.10
< 0.20*
640.00*
35.00
< 2.00*
< 1.00*
188.00*
- 15.30*
3.00
4
6.14
- 6.20*
1.00
207.00*
720.00*
49.00
< 2.00*
47.00
230.00*
- 11.90*
4.50
-------
n
i
K)
to
ENVIRONMENTAL MONITORING AMD SUPPORT LABORATORY
OFFICE OF RESEARCH AMD DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ZINC ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER DRINKING WATER SURFACE WATER
AMPUL MO:
TRUE CONC:
LAR NUMBER
J
2
3
4
5
6
7
e
9
10
5
13.90
18.40
42.50
112.00
2600.00*
71.00
< 40.00*
9.00
14.00
2«.20
12.00
6
17.40
18.90
58.80
85.00
670.00*
14.00
< 40.00*
9.00
29.00
2R.20
14.50
5
13.90
3.70
176.00
8.00
400.00*
26.00
< 2.00*
10.00
158.00
- 2.00*
13.50
6
17.40
17.50
135.00
98.00
500.00*
10.00
< 2.00*
- 8.00*
202.00
20.30
14.50
5
13.90
- 8.60*
4.00
< 0.20*
2200.00*
49.00
< 2.00*
4.00
70.00*
45.00
8.50
6
17.40
- 34.80*
8.40
< 0.20*
1120.00*
37.00
< 2.00*
- 1.00*
370.00*
- 5.90*
13.00
-------
n
i
K)
K)
Ul
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT .
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR ZINC ANALYSES BY WATER TYPE
WATER 1 WATER 2 WATER 3
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (*REL ERROR)
OVERALL STD OEV (S)
OVERALL REL STO OEV, I
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (tREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, t
SINGLE STO OEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACYttREL ERROR)
OVERALL STO DEV (S)
OVERALL REL STD DEV, I
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
1
4
0.54
2.97
455.04
1.53
51.52
0
11
3
8
5.32
27.57
423.97
23.07
82.76
12
54
5
R
13.90
37.89
172.57
36.36
95.96
17
49
2
4
0.75
2.32
209.00
1.59
68.63
.29
.12
4
7
6.14
17.75
189.16
25.18
141.81
.38
.26
6
8
17.40
32.17
84.91
26.41
82.07
.38
.62
1
4
0.54
19.85
3603.36
16.41
82.66
12.
92.
3
5
5.32
27.08
409.02
24.34
89.88
9.
44.
5
7
13.90
56.46
306.17
76.01
134.63
32.
49.
2
4
0.75
6.20
726.67
7.59
122.44
00
13
4
5
6.14
15.10
145.93
12.98
85.93
43
71
6
7
17.40
72.33
315.68
74.50
103.00
04
75
1
3
0.54
3.77
602.74
3.84
102.01
3
3
5.32
13.70
157.52
18.45
134.65
5
5
13.90
22.10
58.99
22.85
103.39
2
4
0.75
18.38
2350. 00
20.99
114.23
1.00
9.03
4
4
6.14
25. 3«
313.27
26.18
103.16
5.98
30.58
6
3
17.40
19.47
11.88
15.3fi
78.89
6.72
32.31
WATER LEGEND
1 - LAB PURE HATER
2 - DRINKING WATF.R
3 - SURFACE WATER
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF MATER TYPE ON ZINC ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) = .71375
HATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
»
2 .5557 ' -.1R64
3 .5955 -.4219
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROP
REG(DISTILLED) 1 41.32224 41.32224
REG(HATER/D1STILLED) 4 5.31561 1.32890 1.13 .3506
0 ERROR 80 94.48602 1.18108
I
K>
c* TOTAL 85 141.12387
** TABLE OF 95* CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERC£PT(HATER-DISTILLED) SLOPE(WATER-01 STILLED)
HATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .5557 { -.5543 , 1.6657) -.1864 ( -.7180 , .3453)
3 .5P55 ( -.5886 , 1.7796) -.4219 ( -.9989 , .1551)
NOTE: IF ZERO IS CONTAINED WITHIN A GIVEN CONFIDENCE INTERVAL THEN THERE IS HO STATISTICAL SIGNIFICANCE BETWEEN
DISTILLED WATER AND THE CORRESPONDING HASTE HATER 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.
-------
ENVIRONMENTAL MONITORING AHD SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR ZINC ANALYSIS BY HATER TYPE
LOH YOUDEN PAIR, UNITS - HG/L
LAB PURE HATER EFFLUENT 1
n
N)
NJ
AMPUL HO:
TRUE CONC:
LAB NUMBER
1
2
.3
4
5
6
7
8
9
10
1
1.74
1.45
1.59
9.63*
2.25
0.02*
1.97
1.06
1.37
0.69
1.60
2
1.31
1.07
0.94
1.74 <
1.39
0.01*
1.24 <
0.95
1.19
0.66
2.14
1
1.74
1.59
2.08
0.40* <
1.60
0.01
0.00* -
1.85*
0.05
0.52
1.00 -
2
1.31
1.22
3.20
0.40*
1.70
O.OP
0.28*
2.65*
1.64
1.99
0.50*
-------
ENVIRONMENTAL MONITORING AND SUPPORT LARORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ZINC ANALYSIS BY WATER TYPE
MEDIUM YOUOEN PAIR, UNITS - MG/L
LAB PURE WATER EFFLUENT 1
AMPUL NO: 3
TRUE CONC: 3.40
4
2.83
3
3.40
4
2.83
LAR NUMBER
n
1
N)
to
00
1
2
3
4
5
6
7
8
9
10
3.40
6.03
7.32
4.28
0.23*
3.19
3.84
5.41
6.44
3.74
2.45
5.08
1.14 <
3.3")
0.02*
3.17
2.96
5.65
0.02
3.18
3.78
3.67
0.40* <
3.30
0.04
0.4fl
3.9fl*
1.66
1.09
4.00
2.04
2.19
0.40*
3.20
0.03
0.12
3.74*
2.47
5.54
2.50
-------
LAB PURE WATER
o
1
N)
NJ
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
5
5.19
5.15
4.38
13.57*
6.25
0.03*
6.11
5.29
fl.30
3.73
6.36
6
6.41
5.69
4.02
3.91
7.10
0.02'
7.17
5.61
7.93
4.83
6.89
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR ZINC ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - MG/L
EFFLUENT 1
5
5.19
5.37
3.26
0.40* <
5.60
0.04
0.96
7.40*
0.06
2.75
4.00
6
6.41
6.01
4.38
0.40*
8.20
0.05
1.44
7.10*
3.35
1.88
6.00
-------
o
I
M
OJ
O
ENVIRONMENTAL MONITOR IMP, AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIROW1ENTAL PROTECTION AGENCY
*M EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR ZINC ANALYSES BY WATER TYPE
WATER 1 WATER 2
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY (tREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STO DEV, *
SINGLE STD OEV, (SR)
ANALYST REL DEV, %
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY (*REL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD DEV, *
SINGLE STO DEV, (SR)
ANALYST REL DEV, %
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) MG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD OEV, J
SINGLE STD DEV, (SR)
ANALYST REL DEV, I
I
8
1.74
1.50
-13.92
0.49
32.53
0
23
3
9
3.40
4.93
45.01
1.41
28.55
1
44
5
8
5.19
5.70
9.75
1.40
24.62
0
7
2
9
1.31
1.26
-3.91
0.45
35.69
.32
.30
4
9
2.83
3.01
6.19
1.74
57.82
.77
.65
6
9
6.41
5.91
-7.88
1.45
24.62
.41
.02
1
7
1.74
0.9R
-43.78
o.ni
83.21
0
44
3
8
3.40
2.25
-33.76
1.61
71.63
1
58
5
R
5.19
2.75
-46.92
2.22
80.70
0
29
2
6
1.31
1.64
25.13
1.01
61.91
.59
.85
4
R
2.83
2.37
-16.14
1.76
74.10
.35
.50
6
8
6.41
3.91
-38.95
2.75
70.21
.9fl
.45
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 1
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY.
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR ZINC ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
EFFLUENT 2
o
r
to
U)
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
1
30.20
25.60
28.30
171.00*
39.90
0.36*
35.00
in. no
24.30
12.30
28.50
2
24.60
20.00
17.60
32.60
26.00
0.20*
23.20
17.80
22.20
12.40
40.00
1
30.20
- 50.00*
24.60
52.40
4300.00*
95.00
360.00*
28.00
< 1.00*
41.10
30.00
2
24.60
- 71.00*
9.50
< 0.20*
500.00*
< 5.00*
- 240.00*
9.00
< 1.00*
41.10
40.00
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ZINC ANALYSIS BY HATER TYPE
MEDIUM YOUflEN PAIR, UNITS - UG/L
EFFLUENT 2
n
i
K)
U>
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
3
50.70
50.90
90.20
109.00
64.00
3.50*
58.20
57.40
81.00
96.30
56.00
4
65.00
55.60
115.00
25.90
76.80
0.53*
71.80
67.00
128.00
0.53
72.00
3
50.70
- 36.00*
66.00
21.90
800.00*
65.00
1200.00*
41.00
300.00
203.00
60.00
4
65.00
74.00
55.70
28.40
1800.00*
58.00
1080.00*
44.00
120.00
38.70
80.00
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ZINC ANALYSIS BY HATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 2
AMPUL NO: 5
TRUE CONC: 148.00
6
189.00
5
148.00
6
189.00
LAB NUMBER
O
I
to
CO
CO
1
2
3
4
.5
6
7
e
9
10
146.00
124.00
384.00*
177.00
0.99*
173.00
150.00
235.00
106.00
180.00
167.00
117.00
114.00
208.00
0.68*
210.00
164.00
232.00
141.00
202.00
111.00
63.70
154.00
200.00*
18.00
360.00
204.00
1960.00*
170.00
160.00
- 6.00*
36.90
< 0.20*
300.00*
35.00
120.00
174.00
1670.00*
357.00
IIO^OO
-------
O
I
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND" DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON ZINC ANALYSIS
** POINT ESTIMATES **
DISTILLED HATER SLOPE:GAMMAf1) = 1.10687
HATER INTERCEPT(HATER-DISTILLED) SLOPE(HATER-DISTILLED)
2 .1363 ' -.5418
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROB
REG(DISTILLED) 1 21.03910 21.03910
REG(WATER/DISTILLED) 2 6.715WI 3.35794 4.23 .0178
ERROR 84 66.69991 .79405
TOTAL fl7 94.45480
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLED)
HATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 .1363 ( -.8154 , 1.0880) -.5418 ( -1.2834 , .1997)
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.
-------
n
i
NJ
U)
Ul
WATER 1
ENVIRONMENTAL MONITORING AN!) SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR ZINC ANALYSES BY WATER TYPE
WATER 2
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (%REL ERROR)
OVERALL STO OEV (S)
OVERALL REL STO DEV, %
SINGLE STD OEV, (SR)
ANALYST REL OEV, J
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (tREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD OEV, *
SINGLE STD DEV, (SR)
ANALYST REL DEV, I
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (IREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD OEV, %
SINGLE STD DEV, (SR)
ANALYST REL OEV, *
1
8
30.20
26.59
-11.96
8.66
32.59
5.
23.
3
q
50.70
73.67
45.30
20.96
20.46
34.
49.
5
R
148.00
161.38
9.04
39.60
24.54
11.
7.
2
9
24.60
23.53
-4.34
8.41
35.74
83
26
4
9
65.00
68.07
4.72
39.36
57.83
77
06
6
<)
189.00
172.78
-8.58
42.83
24.79
72
01
1
6
30.20
45.18
49.61
26.46
58.56
9.
27.
3
7
50.70
108.13
113.27
103.04
95.30
60.
71.
5
8
148.00
155.09
4.79
102.62
66.17
96.
65.
2
4
24.60
?4.00
1.22
18.03
72.60
52
17
4
8
65.00
62.35
-4.08
28.99
46.49
72
24
6
6
189.00
138.82
-26.55
119.3?
85.96
74
83
WATER LEGEND
'1 - LAB PURE WATER
2 - EFFLUENT 2
-------
n
i
ENVIRONMENTAL MONITORING ANT) SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON ZINC ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) « 1.01292
WATER INTERCEPT(WATER-OISTILLED) SLOPE(WATER-DISTILLED)
2 1.6857 * -.3539
** ANALYSIS OF VARIANCE **
SOURCE OF SUM OF SQUARES MEAN SQUARE F PROB
REG(OISTILLED) 1 37.81808 37.81808
REGIWATER/DISTILLEO) 2 2.13765 1.068«2 1.86 .1622
ERROR 78 44.77322 .57402
TOTAL 81 84.72895
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
IHTERCEPT(WATER-DISTILLED) SLOPE(WATER-DISTILLEO)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 1.6857 ( -.4529 , 3.8242) -.3539 ( -.8522 , .1443)
NOTE: IF ZERO IS CONTAINED WITHIN A RIVEN 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.
-------
LAB PURE WATER
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ZINC ANALYSIS BY WATER TYPE
LOW YOUDEN PAIR, UNITS - UG/L
EFFLUENT 3
n
i
M
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
0.
3.
4.
< 0.
384.
55.
< 40.
< 1.
2.
4472.
0.
1
51
60
30
20*
00*
00*
00*
00*
50
00*
96
0.
3.
16.
< 0.
461.
0.
< 40.
< 1.
2.
0.
1.
2
72
80
20*
20*
00*
50
00*
00*
90
26
90
0.
- 268.
2.
< 0.
880.
28.
- 30.
55.
< 1.
2670.
15.
1
51
00*
00
20*
00*
00
00*
00
00*
00*
00
0.
- 190.
< 0.
< 0.
1200.
20.
330.
- 2.
< 1.
33.
< 1.
2
72
00*
30*
20*
00*
00
00
00*
00*
30
00*
-------
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
O
I
NJ
OJ
00
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAW DATA FOR ZINC ANALYSIS BY WATER TYPE
MEDIUM YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 3
3
5.09
5.60 <
48.60
14.30
826.00*
49.90
40.00* <
4.80
57.60
26.10
7.20
4
5.87
1.00*
4.40
2.30
346.00*
54.70
40.00*
2.90
49.90
0.74
4.30
3
5.09
- 232.00*
8.90
1210.00*
1500.00*
10.00
90.00
< 1.00*
32.00
17.40
46.50
4
5.87
- 83.00*
- 11.00*
267.00
2400.00*
< 5.00*
150.00
1.00*
86.00
9.64
46.50
-------
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AMD DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
RAH DATA FOR ZINC ANALYSIS BY WATER TYPE
HIGH YOUDEN PAIR, UNITS - UG/L
LAB PURE WATER EFFLUENT 3
n
i
to
u>
AMPUL NO:
TRUE CONC:
LAB NUMBER
1
2
3
4
5
6
7
8
9
10
13.
17.
40.
108.
2496.
68.
< 40.
8.
13.
23.
11.
5
30
70
80
00
00*
20
00*
60
40
20
50
16.
18.
56.
81.
643.
13.
< 40.
8.
27.
27.
13.
6
70
10
40
60
00*
40
00*
60
80
10
90
13.
- 167.
< 0.
< 0.
1900.
< 5.
50.
3.
477.
44.
14.
5
30
00*
30*
20*
00*
00*
00
00
00*
00
50
16.
- 64.
< 0.
276.
2500.
14.
60.
4.
290.
29.
32.
6
70
00
*
30*
00
00
00
00
00
00
30
50
*
-------
n
i
K)
WATER 1
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
STATISTICAL SUMMARY FOR ZINC ANALYSES BY WATER TYPE
WATER 2
LOW YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY (IREL ERROR)
OVERALL STD OEV (S)
OVERALL REL STO DEV, %
SINGLE STO DEV, (SR)
ANALYST REL OEV, t
MEDIUM YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACY UREL ERROR)
OVERALL STD OEV (S)
OVERALL REL STD DEV, %
SINGLE STD DEV, (SR)
ANALYST REL DEV, »
HIGH YOUDEN PAIR
NUMBER OF DATA POINTS
TRUE CONC (C) UG/L
MEAN RECOVERY (X)
ACCURACYUREL ERROR)
OVERALL STD DEV (S)
OVERALL REL STD DEV, *
SINGLE STD OEV, (SR)
ANALYST REL DEV, %
1
4
0.51
2.84
453.61
1.46
51.27
0.
11.
3
8
5.09
26.76
425.79
22.14
82.73
11.
54.
5
8
13.30
36.42
173.87
35.06
96.24
16.
49.
2
5
0.72
1.87
161.09
1.52
81.26
27
49
4
7
5.87
17.03
190.19
24.16
141.85
89
30
6
8
16.70
30.86
84.81
25.36
82.16
74
76
1 2
4 3
0.51 0.72
25.00 127.77
4773.29 17719.62
22.64 175.27
90.57 137.18
UNO
UNO
3 4
6 5
5.09 5.87
34.13 111.83
570.60 1805.08
30.91 101.13
90.56 90.44
25.01
34.28
56
4 7
13.30 16.70
27.88 100.83
109.59 503.76
22.71 125.72
81.47 124.69
9.92
15.41
WATER LEGEND
1 - LAB PURE WATER
2 - EFFLUENT 3
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ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL PROTECTION AGENCY
*** EPA METHOD STUDY - TRACE METALS BY AA ***
EFFECT OF WATER TYPE ON ZINC ANALYSIS
** POINT ESTIMATES **
DISTILLED WATER SLOPE:GAMMA(1) .84336
WATER INTERCEPT(WATER-DISTILLED) SLOPE(WATER-OISTILLEO)
2 2.4134 . -.8250
** ANALYSIS OF VARIANCE **
SOURCE DF SUM OF SQUARES MEAN SQUARE F PROD
REG(DISTILLED) 1 20.92135 20.92135
REG(WATERXDISTILLED) 2 33.74910 16.87455 14.73 .0000
ERROR 57 65.31854 1.14594
O
I
M TOTAL 60 119.98899
** TABLE OF 95% CONFIDENCE INTERVALS FOR THE DIFFERENCES BETWEEN INTERCEPTS AND THE DIFFERENCES BETWEEN SLOPES **
INTERCEPT(WATER-DISTILLEO) SLOPE(WATER-DISTILLED)
WATER ESTIMATE INTERVAL ESTIMATE INTERVAL
2 2.4134 ( 1.4131 , 3.4137) -.8250 ( -1.3086 . -.3414)
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.
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