REGION V
JOINT FEDERAL/STATE
SURVEY OF ORGANICS & INORGANICS
IN
SELECTED DRINKING WATER SUPPLIES
JUNE 1975
DRAFT
U.S. ENVIRONMENTAL PROTECTION AGENCY
230 South Dearborn Street
Chicago, Illinois 60604
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4
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ACKNOWLEDGEMENT
Region V wishes to acknowledge the cooperation it received
from each of the State and local agencies and Water Treatment Plant
officials without whose participation this study would have been
impossible.
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TABLE OF CONTENTS
Page
I. Introduction 1
II. Summary of Results and Conclusions 3
1. Volatile Organic Compounds 3
2. Linear Regressions 10
3. Pesticides, PCB's and Phthalates 21
4. Non-Volatile Organic Compounds 21
5. Inorganic Parameters 25
6. Economic Considerations 31
III. Significance 31
IV. Recommendations . 34
V. Sample Collection, Analytical Procedures & Quality Assurance 35
1. Sampling Procedures 36
2. Volatile Organics 37
a) Analytical Procedures 37
b) Quality Assurance for Volatile Organics 40
3. Pesticides, PCB's and Phthalates 50
a) Introduction 50
b) Experimental Procedures 50
c) Quality Assurance .' 59
4. Non-Volatile Organic Compounds '. 64
a) Analytical Procedures 64
i) One Liter Water Grab Samples 64
ii) Carbon Filtered Samples 65
5. Metals 68
a) Analytical Procedures & Quality Assurance 68
i) Flame Atomic Absorption 68
ii) Flameless Atomic Absorption 71
ii
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TABLE OF CONTENTS (Cont'd)
6. Inorganic Parameters 75
a] Analytical Procedures 75
b) Quality Assurance 80
LIST OF FIGURES
I. Plot of CHC13 vs. BrCHCle 16
II. Plot of BrCHCl2 vs. Br2CHCl 17
III. Plot of CHC13 vs. Total Chlorine Dosage (All Plants) 18
IV, Plot of CHC13 vs. Total Chlorine Dosage (River Plants) 19
V. Frequency Distribution for Ammonia in Finished Water 20
VI. Sampling Assembly for Volatile Organics 38
VII. Analytical Assembly for Volatile Organics 39
VIII. Gas Chromatogram of Volatile Organic Compounds 44
IX. Computer Printout for List A Pesticides 54
X. Gas Chromatogram of Pesticides Containing Phosphorous 55
XI. Computer Printout for List B Pesticides (SE-30/OV-210 Column) 56
XII. Computer Printout for List B Pesticides (OV-17/OV-210 Column) 57
XIII. Dual Column-Dual Pen Recorder Tracing of Compounds in List B 58
XIV. Carbon Filter Assembly 65
LIST OF TABLES
I. Summary of Analytical Results 3
II. Analytical Results (Volatile Organics) 4
III. Volatile Organic Compound Concentration Ratios (10 highest) 8
IV. Water Supply System Information , 12
V. Pesticides, PCB's and Phthalates in Each Water Supply 22
VI. Drinking Water Standards for Inorganic Parameters . . 27
iii
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'LIST OF TABLES (Cont'd)
VII. Summary of Inorganic Parameter Drinking Water Results 28
1/III. Frequenty Distribution of the Finished Water -
Results for Inorganic Parameters 29
IX. Percentage of Raw Water COD Values Exceeding the Mean
of 15 mg/1 Versus Chloroform Concentrations 30
X. Additions of Ammonia and Phosphorus to Finished Waters 30
XI. Estimated Cost Data for the Region V Survey 32
XII. Gas Chromatograph Detector Response as a Function
of Purge Time in Arbitrary Units 42
XIII. Reproducibility of the Analytical Method (Volatile Organics) .... 42
XIV. Summary of Results for All Volatile Organic Reagent Blanks 45
XV. Analytical Results of All Volatile Organic Samples Collected
in Duplicate 47
XVI. Results of Volatile Organic Results versus Time 49
XVII. Recovery Data for Samples Spiked with Pesticides 61
XVIII. Precision for Metals Based on Analysis of Duplicate
Samples by Flame Atomfc Absorption Spectroscopy . . . . 69
XIX., Recovery Data for Samples Spiked with Metals by Flame AA 70
XX. Statistical Summary of Results from the Laboratory
Control Standards by Flame AA 70
XXI. Precision Based on the Analysis of Duplicates by Flameless AA . . . . 72
XXII. Metal Concentration Ranges in Drinking Water 74
XXIII. Summary of Quality Assurance Data for Inorganic Parameters 81
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INTRODUCTION
In response to public concern resulting from publicity about alleged toxic
organic compounds in the New Orleans, Louisiana and other municipal drinking
water supplies, Region V States asked for assistance in obtaining current data
concerning certain drinking water supplies in Region V. The study was designed
to provide frequency of occurrence and concentration values of volatile and
non-volatile organic compounds, selected pesticides, herbicides and fungicides,
polychlorinated biphenyl mixtures, certain phthalate esters, metals and other
inorganic parameters in drinking waters. Another interest was to establish
baseline concentrations for those organic compounds of health concern or thought
to result from chlorination, and therefore to be widely distributed in our water
supplies. These compounds include carbon tetrachloride (CC1.), chloroform (CHC13),
bromodichloromethane (BrCHClp), dibromochloromethane (BrpCHCl), bromoform (B^CH),
1,2-dichloroethane (Cl-C^-CI^-Cl), dichloromethane (CF^C^), aldrin, dieldrin
and DDT.
The 83 cities were selected jointly by both State and Federal personnel
to get a broad representation of Region V water supply systems. The study evalu-
ates organic pollution in drinking water supplies of most concern to State
agencies, provides appropriate background data for quality assurance purposes,
and complements the National Reconnaissance Survey in determining the concentra-
tions, sources, and potential danger of organic chemicals in drinking water.
A maximum number of parameters per sample were included to provide a com-
plete description of each water supply and to detect possible relationships -
between the more traditional inorganic parameters and the organic parameters of
current interest. In addition, since many expenses of the study, such as sampling
costs, report writing, instrument and other fixed capitol depreciations, trans-
portation, etc., remain constant, the most efficient study includes a maximum
number of parameter analyses per sample.
1
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It should be emphasized that this study occurred during winter months
when waters were cold, surface streams were generally at higher than normal
flows and contained considerable suspended solid materials, agricultural and
gardening activities were at a minimum as were certain industrial activities.
Therefore, concentrations could vary substantially from values reported in this
manuscript for samples collected at different times of the year.
1,2
Based on the data presented in Table I, it is clear that chloroform,
bromodichloromethane, dibromochloromethane and bromoform are consistently higher
in treated drinking water than in raw waters at most cities in the Region. The
-mean concentrations however are quite low.
Table II is a listing of the analytical results from which the summary
data in Table I were calculated. All concentrations are in micrograms per
liter (ug/lK It is the practice of the Central Regional Laboratory to report
detection limits based on each day's quality assurance data. Therefore, dif-
ferent detection limits are given for some parameters in Table II and other
places in this report.
Conclusions that may be reached from an examination of the data in
Table II are as follows:
a. Clear raw water results in finished water that is relatively free of
chloroform and related halogenated compounds. Of the 25 supplies
having the lowest concentrations of chloroform, 12 obtain their
water from the Great Lakes, 8 from deep wells and only 5 from
surface sources.
b. There is a correlation between concentrations of chloroform, bromo-
dichloromethane, dibromochloromethane, and bromoform in the
finished water. It appears they result from chlorination of precursors
in'the'raw water. Since there'is no'pattern to their occurrence,
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II. SUMMARY OF RESULTS AND CONCLUSIONS
1* Volatile Organic Compounds
Table I is a summary of the analytical results.
(VOLATILE ORGANICS)
_LSUMMARY_OF_ANALYIICAL_RESULTS.
_ _ nvicroarams
Chemical
Formula & Name
CHCL3 -
Chloroform
CHBrCL2 - Bromodi-
chloromethane
CHBrsCl - Dibro-
nochloromethane
CHBrg - Bromoform
CC14 - Carbon
Tetrachloride
CH2C12 - Methyl ene
chloride
C2H4Cl2 - 1,2-
Dichloroethane
% of Samples
Giving Positive
Results
Finished
Water
95
78
60
14
34t
8
13
Raw
Water
27
5
2
0
18
1
14
Mean
Concentration
(yg/1)
Finished
Water
20 yg/1
6 yg/1
1 yg/1
<1 yg/1
*2 yg/1
<1 yg/1
<1 yg/1
Raw
Water
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TABLE II
ANALYTICAL RESULTS CVOLATILE ORGANICS)
>1 programs per liter)
Raw
F = Finished
City
JURFACE SOURCE
;airo, 111.
larlyle, 111.
Chicago, 111.'
Chester, 111.
Danville, 111.
Airfield, 111.
(ankakee, 111.
"It. Carrael, 111.
Newton, 111.
Ijuincy, 111.
Rock Island, 111.
Royal ton, 111.
Streator, 111.
Bedford, Ind.
iloomington, Ind.
Evansville, Ind.
:ort Wayne, Ind.
3ary, Ind.
ianmond, Ind.
:ndianapolis, Ind.
kkorao, Ind.
.afayette, Ind.
. CHCIs
R F
2
<1
•<1
5
6
10
<1
<1
<1
<1
94
<1
<]
5
<1
<1
4
<1
<1
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TABLE II
(Cont'd)
City
CHC13
R F
URFACE SOURCE tcontlinued)
ogansport, Ind.
ichigan City, Ind.
t. Vernon, Ind.
jncie, Ind.
ew Albany, Ind.
'erre Haute, Ind.
hiting, Ind.
ay City, Mich.
essemer Township
Mich.
;adillac, Mich.
Jetroit, Mich.
Jundee, Mich.
5rand Rapids, Mich.
tenominee, Mich.
It. Clemens, Mich.
>ault St. Maria, Mich.
fyandotte, Mich.
Sreckenridge, Minn.
Irookston, Minn.
Duluth, Minn.
:ast Grand Forks,
Minn.
rairniount, Minn.
<]
<1
<1
<1
3
4
<]
<,
7
<1
51
1
xl
<1
<1
<1
<]
<0.5
.9
<0.5
1
3
<0.5
7
s
'<0.5
<0.1
0.3
0.3
<0.5
0.3
<0.1
<0.5
0.4
<2
<0.5
<1
<"[
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TABLE II
(Cont'd)
; ': "-"Guy-- •'"•'• -""
SURFACE SOURCE (conf
3ran1te Falls, Minn.
'nternatlonal Falls,
"Minn.
linneapolis, Minn.
Dslo, Minn.
St. Cloud, Minn.
St. Paul , Minn.
3erea, Ohio
fowling Green, Ohio
Cincinnati , OKio
Cleveland, Ohio
-olumbus, Oh ro
- \
Defiance, Ohio
East Liverpool, Ohio
rreraont, Ohio
3iqua, Ohio
3ortsraouth, Ohio
"oledo, Ohio
Barren, Ohio
3reen Bay, Wise.
(enosha, Wise.
tanitowoc, Wise.
terinette, Wise.
Milwaukee, Wise.
CHC13 ..
ft..' f
nued
•5
<1
<1
3
<]
4
<1
-------
TABLE II
CCont'd)
City
SURFACE SOURCE CCon"
Oshkosh, Wise.
Two Rivers, Wise.
GROUND WATER SOURCE
Galesburg, 111.
Peoria, 111.
forocco, Ind.
South Bend, Ind.
Jackson, Mich.
Kalamazoo, Mich.
.ansing, Mich.
It. Pleasant, Mich.
c/aterford Township
Wich.
•fenkato, Minn.
Richfield, Minn.
tfillmar, Minn.
Slack River Falls,
Wise.
lau Claire, Wise.
^ean
fed i an
. CHC13
R F
inue
6
1
^
<-1
<1
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TABLE III
VOLATILE ORGANIC COMPOUND CONCENTRATION RATIOS
QO HIGHEST CONCENTRATIONS)
micrograms per liter
Fremont, Ohio
Bessemer Township,
- Mien.
Fairmount, Minn.
Chester, 111.
Dundee, Mich.
Bowling Green,
Ohio
Warren, Ohio
Breckenridge,
Minn.
Piqua, Ohio . . .
Bedford, Ind.
CHC13
366
312
200
182
• 170
160
138
128
102
84
BrCHClz
18
4
31
17
26
27
19
15
10
12
Brz'CHCl
1.4
0
0.7
1.1
2
5
0.8
0
0.7
. 0.8
CHBra
"0 '
0
0
0
0
0
0
0
0
0.8
Ave.
Std. Dev.
BrCHCl2
CHC13
4.9*
1.2*
15.
9.3
15.
17.
14.
12.
10.
H
13.3
2.6
Br2CHCl
BrCHCl2
8
0
2
6
8
19
4
0
7
7
6.1
5.5
*excluded from calculation of average and standard deviation. If all data
in Table II are used, both ratio percentages and the scatter increase as
the measurements approach the detection limit
8
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it does not appear that carbon tetrachloride, methylene chloride or
1,2-dichloroethane are produced by a chemical reaction within the treat-
ment process,
c. Using only the "more accurate data (higher concentrations can be measured
more accurately than lower concentrations) for those cities having over
100 ug/1 of chloroform in their finished water, the concentration ratio
percentages [see Table III of BrCHCl2 to CHC13 range from 1.2% to 17%.
The range for the BrCHC^/B^CHCl ratios is 0 to 19$'. A careful examina-
tion of these ratios suggests that the concentration of BrCHCl2 will be
approcimately 13% that of CHC13 and the concentration of B^CHCl will be
about 6% that of BrCHCl2. This relatively constant ratio indicates a
common precursor or group of precursors of the halogenated pollutants.
Since the ratios described above are much higher than the ratio of
bromine to chlorine'-in the chlorine used to purify the raw waters, we
conclude that bromination is much faster than chlorination and that the
halogen is acting as an electrophile rather than a nucleophile during
the chemical reaction producing the subject pollutants. The ratios
for Fremont, Ohio; Bessemer Township, Michigan and certain other cities
do not follow this general pattern but have an excess of chloroform.
We suggest that a source of chloroform is 'operative that differs from
that of most cities studied. At first we suspected an industrial
discharge but that conclusion is inconsistent with a zero chloroform
concentration for the raw water. Therefore, these supplies may contain
a particularly reactive precursor for chloroform. Additional analytical
data will be required to identify any such precursor, to establish whether
or not these measured values are common throughout the year, and
9
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to suggest a .method of removal. It is suggested that check samples
Be collected to yertfy results that truly represent these water supplies.
The concentrations of brominated compounds are high relative to the
concentrations of chlorinated compounds for some cities. If this
pattern is repeated in check samples, and should the brominated com-
pounds be discovered to be of significance, the concentration of bromine
in the chlorine used for purification should be reduced.
d. The use of carbon treatment is not effective as was practiced by the
water treatment plants during the time of this study. (See Table IV)
We suspect that most of those cities presently using carbon have chosen
to do so to reduce taste and odor problems and that the carbon is much
•more effective in removing those compounds causing the water to have
a taste and odor than it is in removing the halogenated methanes or
other organic compounds that react to form chloroform.
Table IV summarizes water supply systems information. Data is reported as
it was obtained on field sheets at the time of sample collection. It can be noted
from this table that in addition to the characteristics of the raw water, chloro-
form production also depends upon the amount of chlorine applied. Another impor-
tant factor is the time of contact. For this study contact time must be considered
to be the entire elapsed time from chlorine application until sample analysis
0-5 days). Recent experiments with aliquots of southern Lake Michigan water that
were treated with 2 mg/1 of chlorine have shown chloroform production-to be cut in
half when the aliquots were again treated in one hour to remove all remaining
chlorine. Chlorine was allowed to react a number of days in the aliquots where
it was not removed after one hour.
2. Linear Regressions
Figures I, II, III, and IV show the linear regression equations and asso-
ciated F ratios calculated from the measurements for chloroform, bromodichlororaethane,
10
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dihromochJoronjetliane, and total cMo/ine dosage in river water systems, Since
the F value at tRe 0,01 probability point ts 7, the. null hypothesis of no rela-
tionship 1s rejected and it is concluded that significant correlation does exist
.between the parameters plotted on Figures I, II, III, and IV.
Further research should be directed to determining the rates of reactions
of the parameters analyzed in this study with particular attention to the source
of raw water used in treatment.
17.
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TABLE IV
WATER SUPPLY SYSTEM INFORMATION
City
SURFACE SOURCE
:airo, 111
:arlyle, 111.
Chicago, 111.
Chester, 111.
Danville, 111.
Airfield, 111:
(ankakee, 111.
-It. Carmel, 111.
tewton, 111.
3uincy, 111.
tock Island, 111.
toyalton, 111.
Greater, 111.
tedford, Ind.
Hoomington, Ind.
ivansville, Ind.
:ort Wayne, Ind.
3ary-Hobart, Ind.
temmond, Ind.
Indianapolis, Ind.
Cokomo, Ind.
CHC13
(uq/1)
14
48
7
182
16
47
52
52
4
58
79
68
35
84
19
29
29
7
4
19
30
Source
Ohio River
Kaskaskia River
Lake Michigan
Mississippi R
Vermill ion R'
.ittle Wabash
Kankakee River
Wabash River
Deep Wells
Raw
Water
Charac-
:eri sties
M/I
M/I
I
M/I
M/I
M/I -A
A
•
M/I
Clear
M/I
Mississippi R"
Big Muddy River
Vermill ion River
•/hite River
ton roe River
Dhio River
it. Joseph River
Lake Michigan
Lake Michigan
toite River
M/I
M/I
A/ 1
A
A
M/I
M/I
I
I
M/I '
I
Wildcat Creek a- A
Activated
Carbon
Powdered j
None
Powdered
None
None
None -.
Anthracite
Coal
None
None
Powdered
Clg Dose v
(ppm)/
Detention
Time (hr)
Prior to
Sample
5re- Post-
7,.0/6
7.3/7
1.2 Q.I
7.2/ 2.4/
4 1
1.2/2
6.2/*2.5/
-6.5 3.5
l.O/ 1.0
2.5
7. I/ 4.0 /
29 21
1.7/37
4-20/ 1-3/
4 i.a
3owdered j 8-12/24
lone
'owdered
tone
Jone
*
tone
Powdered
Powdered
None
3.4/7
3.3/4
4.9/5
2.8/7
3.15/6
1.4/8 0.4/2
1.7/10
7.8/6
Powdered S3. 4/2 2.2
s 1
Population
7,700
7,200
7,900
50,000
•10,100
60,000
11,500
4,900
50,000
i
52,000
3,300
20,000
17,000
50,000
*
200,000
,200,000
: 127,000- ,
700,000
53,000
i
c
12
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TABLE IV
(Continued)-
Citv
.afayette, Ind.
ichigan City, Ind.
t. Vernon, Ind.
uncie, Ind.
ew Albany, Ind.
'erre Haute, Ind.
'hi ting, Ind.
.ogansport, Ind.
3ay.City, Mich.
tessemer Township,
Mich.
Cadillac, Mich.
)etroit, Mich.
Dundee, Mich.
Srand Rapids, Mich.
denominee, Mich..
•It. Clemens, Mich.
3ault St. Marie, Mich.
tyandotte, Mich.
Jreckenridge, Minn.
>ookston, Minn.
CHC13
(uq/1)
5
5
18
31
41
5-
<*
7
17
312
47
5
170
24
42
10
27
14
128
Source t
Deep Wells
Lake Michigan
Ohio River
White River
Ohio River
Deep Wells
Lake Michigan
Eel River
Saginaw Bay
Black River"
Deep Wells
Detroit River
River Raisin
Lake Michigan
Lake Michigan
Lake St. Clair .
St. Mary's Rfyer
Detroit .River
[Otter Tail Rfyer
5
! 7 JRed Lake River
Raw •
Water
Charac-
,eri sties
Clear
I
M/I
M/I
M/I
Clear
I
A
I
C
Clear
M/I
M/I
Clear
M/C
M/I
Clear
M/I
C
Clear
Activated
Carbon
None
Powdered
Powdered
Anthracite
Coal
None
Powdered
Powdered
None
Powde red
Powdered
None
Powdered
Powdered
None
None
Carbon
Filters
None
3owdered
tone
ftone
U -I ,. \ «
Cl2 Dose"
(ppm)/
Detention
Time (hr)
Prior to
Sample
5re- Post-
.75/0.1
.9/ 0.3/7
19
1.5/6
*
4.5/3
3.9/9
^•Kf'Ki
3.8/8+Ozone
2.0/6 1.5/2
3.2/. 0.03
2.4
5.31/0.1
4.5/0.1
1.3/3 0.g/]
9/4
2.0/4
3.1/24
4.4/8 1
1.7/0.1
3.3/8
5.0/24
Population
50,000
40,000
7,000
87,000
41 ,000
78,000
7,054
19,000
75,000
Uooo
9,500
4,000,000
2,500
216,000
11,000
50,000
17,000
43,000
4,800
. j
1.6/8 9,000 I
I 5
A "
13
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TABLE IV
(Continued)
City
3uluth, Minn.
last Grand Forks,
Minn.
:ai mount, Minn.
iranite Falls, Minn.
international Falls,
Minn.
Minneapolis, Minn.
3slo, Minn.
St. Cloud, Minn
St. Paul , Minn.
3erea, Ohio
Bowling Green, Ohio
Cincinnati, Ohio
:ieveland, Ohio
Columbus, Ohio
Defiance, Ohio
East Liverpool , Ohic
Fremont ', Ohio
Pi qua, Ohio
Portsmouth, Ohio
Toledo, Ohio
CHC1
(uq/1)
26
22
200
5
26
8
79
37
82
60
160
127
10
51
14
5
366
102
25
62
Source
Lake Superior
Red Lake River
Budd Lake
Minnesota. River
Rainy River
Mississippi R
Red River
Mississippi R-
Mississippi R'
Rock River -
Coe Lake
Maumee River
Ohio River
Lake Erie
Scioto River
Maumee River
Ohio River
Sandusky River
Swift Run River
Ohio River
Lake Erie
Raw
Water
Charac-
eri sties
Clear
A
C
M/A
C
M/I
CCE
M/I
M/I
A
A/ 1
M/I
Clear
M/I
M/A
M/I
A
M/I
M/I
M/I-
__1_
Activated
Carbon
None
None
None
None
None
Powdered
None
Powdered
Powdered
Powdered
Powdered
None
Powdered
Powdered
Carbon
Filter
Powdered
(ppm)/
Detention
Time (hr)
Prior to
Sample
Pre- Post-
1.3/1
12.0/24
10. O/ 3.0/
6. 8
3.5/16
0.7/3
2.9/ 0.36/
19 12
1.2/12
1.3/4
7.0/12
3.65/1
4.5/6
3.3/6
'4.3/4 4.3/2
l.O/ 3.0/
1 0.5
2.3/7
4/5 3/2
1.39/1
— - i
Population
100,000
8,000
11,000
3,500
621,000
500
45,000
402,000
23,000
21,000
260,000
17,000
30,000
21,000
22,000
455,000
14
-------
TABLE IV
(Continued)' -
City
Warren, Ohio
Green Bay, Wise.
Kenosha, Wise.
"Manitowoc, Wise.
Marinette, Wise.
Milwaukee, Wise.
Gshkosh, Wise.
Two Rivers, Wise.
GROUND WATER SOURCE
Galesburg, 111.
Peoria, 111.
-*.
Morocco, Ind.
South Bend, Ind. '
Jackson, Mich.
Ka lama zoo, Mich.
Lansing, Mich.
Mt. Pleasant, Mich.
Waterford Township,
Mich.
Mankato, Minn.
CHC13
'uq/D
138
9
3
14
53
2
55
9
30
2
12
n
<
-------
TABLE IV
(Continued) '
.•*"
City
Richfield, Minn.
Willmar, Minn.
Black River Falls,
Wise.
Eau Claire, Wise.
M = Municipal e
A = Agricultura
I = Industrial
C-= Color-produ
T/0 = Taste and o
CCE = Carbon chlo
CHC13
(uq/1)
<\
2
6
50
fluents
runoff
f fluent
invo con
of-proc
oform e
Source
Deep Wells .
Deep Wells
Wells
Deep Wells
affect -the raw
affects the raw
s affect the raw
sounds.
jcing compounds.
xtracts have bee
Raw
Water
Charac-
teristics
Clear
Clear
Clear
Clear
/ater sour
water SOL
water SOL
detectec
Activated
Carbon
None
None
None
None
:e.
*ce.
'ce.
Clo Dose '
IPpm)/
Detention
Time (hr)
Prior to
Sample
Pre- Post-
1.0/ ].5/
15 0.1
3.5/48
0.46/3
l.l/ 0.75/
18 0.1
-
Population
47,500
15,000
3,200
47,000
i
1
-------
4001
300-
FIGURE I
Plot of CHC13 vs. BrCHClain ug/1
Region V Organic Survey
2QOr
100--
• «r
*••% •
J» %«® • ; •
t ( | j |
10 20 30 4'0 50
60 7t
SrCHCl,
ug/1- '
-------
60r
50--
40
30 ._
Plot of 3rCHCl2 vs. Br2CHCl in ug/T
Region V Organic Survey
20 ..
10 --
Br?CHCl
ug/1
17
-------
400 f
FIGURE III
Plot of CHC1 (ug/1) vs. Total C12 Dosage (mg/1) for
All Water Treatment Facilities
300^
j
i
i
200 J_
100 !
Total Ci? Dosage
mg/1
18
-------
400 T
FIGURE IV
Plot of CHCU (ug/1) vs. Total C12 Dosage (ug/1) in
Water Treatment Systems that Treat River Water
3004
200-
TOO
468
Total dp Dosage
mg/1
19
10
12
-------
Ammonia Expressed as
mg Nitrogen per Liter
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3. Pesticides, PCB's and Phthalates
Table V is a listing of those cities where pesticides, PCB's and/or
phthalates were identified. The other samples analyzed did not contain a detect-
able amount of any of the fifty pesticides included in the survey. All analytical
results are included in the appendix and from these we conclude that:
a. A large majority of the samples do not contain these types of compounds
in concentrations that can be measured with the procedures used for
this study.
b. For this class of compounds, the most commonly found are diethylhexyl-
phthalate, dieldrin, DDT, treflan, aldrin and hexochlorobenzene. The
concentrations of all pesticide type compounds identified to date
are low. The highest concentrations found were 68 nanograms per
liter (ng/1) for DDT, 11 ng/1 for dieldrin, 17 ug/1 for diethyl-
hexlphthalate and 50 ng/1 for treflan. All positive results are
given in Table V.
c. Concentrations of PCB's in those samples from Lake Michigan and the
Ohio River were too low to detect.
4. Non-Volatile Organic Compounds
Finished water was passed through small carbon filters used for sample
collection at Mt. Vernon, Evansville and Indianapolis, Indiana. Raw water samples
were also collected at Mt. Vernon. Presently the water from Whiting, Indiana
and Mt. Carmel, Illinois are being sampled for carbon filter and extraction
analyses. All of the exposed filters have been extracted with hexane, chloroform
and methanol. Each of the extracts has been separated in acidic, basic and
neutral fractions giving a total of nine concentrates per filter. The following
high boiling compounds have been identified in the Mt. Vernon and Evansville
supplies:
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Mt. Vernon Evansville
tri-n-butyl phosphate tri-n-butyl phosphate
butylphthalate butylphthalate
dioctyl phthalate dioctyl adipate
trimethyl benzene methyl palminate
toluene farnesol
n-octane and other homologs n-octane and other homologs
xylene xylene
ethyl benzene diphenylether
methyl cyclohexane
Many more of these high boiling compounds are present, but further purification
(we are attempting to accomplish the preparation by high pressure liquid chroma-
tography techniques) will be necessary to identify them. We have not yet
attempted to analyze the extracts for any low boiling compounds except for the
bis-2-chloroisopropyl and bis-2-chloroethyl ethers. Neither of these compounds
gave a gas chromatographic peak above the detection limit and therefore they
are not present to the extent they have been in Evansville samples analyzed
previously. In general, the current water samples from Evansville contain fewer
organic compounds than similar samples analyzed by the Region V laboratory and
Indiana State University-Evansville over the previous four years. This reduc-
tion in pollution is an expected product of the National Pollutant Discharge
Elimination System program and should reduce concern for Evansville water.
5. Inorganic Parameters
All samples were analyzed for the following fourteen metals: silver,
arsenic, calcium, cadmium, chromium, copper, iron, potassium, magnesium, man-
ganese, sodium, lead, selenium, and zinc. Concentrations (49 ug/1) of arsenic
were found at Kokomo, Indiana and prompted us to resample that plant. It was
subsequently found that Kokomo was using Wildcat Creek and several deep wells
as sources. The water from Wildcat Creek does not contain a measurable amount
of arsenic but water from two of the 15 deep wells contained up to 2000 ug/1.
This is apparently a very localized problem affecting only a few wells. With
proper treatment and blending the Kokomo Water Works has been able to maintain
25
-------
safe concentrations of arsenic in the finished drinking water. It is recommended
however that Kokomo analyze for the presence and quantity of arsenic in the
finished water at least once per month during periods when Wells #4 or #7 are
in use.
The arithmetic mean values for all finished water parameter concentrations
are less than drinking water standards with the exception of phenolics (Table VI &
VII). Since the detection limit of the analytical method used to measure phenol
concentrations is greater than the recommended levels, we do not interpret the
measured mean phenolic concentration to be significantly higher than the recom-
mended values.
Table VIII is an abbreviated frequency distribution of the finished water
(8)
data and shows that the Water Quality Criteria recommendations were occasionally
exceeded. In addition, the table shows the mean value for each parameter is
generally larger than the median value which indicates the data distribution
is log normal rather than gaussian. This point is illustrated in Figure 1.
It can be concluded from the data in Table IX that a high chemical oxygen
demand (COD) in the raw water is necessary for a high chloroform concentration
to result in the finished water. However, the converse is not always true as
some supplies had raw water COD's of 30 mg/1 or higher but CHCU concentrations
of 40 ug/1 or less. These data suggests that chloroform results from a single
or small group of compounds. They also support the concept that the chloroform
precursor reduces potassium dichromate and that those supplies having a low COD
need not be tested for chloroform.
25
-------
TABLE VI
DRINKING WATER STANDARDS FOR INORGANIC PARAMETERS a
PARAMETER
Ammonia - N
Alkalinity
Chloride
Chemical
Oxygen Demand
Cyanide
Dissolved
Solids
Fluoride
Mercury
Nitrate - N
Nitrite - N
PH
Phenol ics
Sil ica
Specific Cond.
Sulfate
Suspended Solid
Total Phosphoru
Total Kjeldahl
Nitrogen - N
UBLIC HEALTH
SERVICE (7)
250
0.01, 0.2b
500
0.8-1.7C
0.0002
10
0.001
250
i
i
j
WATER QUALITY
CRITERIA (8) •
0.5
250
0.2
1.4-2.4C
10
1
5-9
0.001
250
ENVIRONMENTAL PROTECTION
AGENCY (6)
0.2
1.4-2.4Cl
0.0002
10
i
a,
b.
c.
Values expressed in mg/1 except pH units.
0.01 mg/1 acceptable but 0.2 mg/1 constitutes grounds for rejection
of the supply.
Exact limits are temperature dependant. See ref. 6-8.
71
-------
TABLE VII
SUMMARY OF INORGANIC PARAMETER DRINKING WATER RESULTS.a
RAW WATER
FINISHED WATER
PARAMETER
Ammonia - N
Alkalinity - CaCOa
Chloride
COD
Cyanide
Dissolved Solids
Fluoride
Mercury
Nitrate & Nitrite - N
Nitrite - N
pH, units
Phenol ics
Silica
Specific Conductance, ys
Sulfate
Suspended Solids
Total Phosphorus - P
Total Kjeldahl - N
Hardness - CaC03b
' MEAN
0.154
141
18
15
0.004
267
0.19
0.0001
1.44
0.017
7.6
0.003
7.9
426
44
33
0.11
0.68
192
STD. DEV.
0.114
83
17
12
0.003
142
0.18
0.0001
2.02
0.024
0.3
0.002
6.4
202
39
64
0.12
0,57
105
MEAN
0.154
106
21
7
0.004
254*
0.87
0.0001
1.39
0.005
7.9
0.003
7.0
406
56
3
0.10
0.39
156
STD. DEV.
0.356
78
21
5
0.002
129
0.37
0.0001
1.91
0.004
0.8
• o.nm
5.1
198
44
5
0.18
0.44
90
a. Expressed as mg/1, except pH (units) and specific conductance
(micro Siemens, us).
b. Obtained from metals section report.
28
-------
TABLE VIII
FREQUENCY DISTRIBUTIONS OF THE FINISHED WATER RESULTS FOR INORGANIC PARAMETERS
Parameter
Ammonia - N
Alkalinity - CaC03
Chloride
COO
Cyanide
Dissolved Solids
Fluoride
Mercury
Nitrate & Nitrite-N
Nitrite - N
pH, units
Phenol ics
Silica
Specific Conductance
us
Sulfate
Suspended Solids
Total Phosphorus - P
Total Kjeldahl
Nitrogen - N
Hardness - CaCOs
i i i
Percent of Samples Less
Than Concentrations Shown
50
0.05
90
20
6
0.003
220
1.0
0.0001
<0.5
<0.005
8.0
•£0.003
7
360
48
<2
^0.02
0.25
130
75
0.15
140
24
8
0.004
300
1.2
0.0002
2.0
-------
TABLE IX
PERCENTAGE OF RAW WATER COD VALUES EXCEEDING THE
MEAN OF 15 mg/1 VERSUS CHCl^ CONCENTRATIONS
Number of Samples CHCl3(ug/1) %COD 15 mg/1
40 20 20
12 40 42
13 60 77
4 80 75
2 100 100
1 120 100
3 140 100
1 - 160 100
1 180 100
4 180 100
Numberous drinking water plants add chemicals other than chlorine to the
during the treatment process. Two commonly used chemicals are ammonia
and polyphosphate. Fluoride is also added to many supplies.
Twenty-one (21) supplies added ammonia or ammonium ion to maintain
acceptable residual chlorine concentrations as chloramines. Nineteen (19) of
these supplies had ammonia - N concentrations above the median of 0.05 mg/1 for
finished water. The average increase of ammonia - N in finished versus raw
nater was 0.195 mg/1 for these supplies compared to the overall average of
zero (0) increase for all supplies (Table X).
Thirteen (13) supplies added polyphosphate. Twelve (12) of these supplies
ivere above the median finished water total phosphorus concentration. Also the
Dverall average change in phosphorus from raw to finished water was negative
D.01 mg/1. However, these 13 supplies averaged an increase of 0.168 mg/1.
TABLE X .
ADDITIONS OF AMMONIA AND PHOSPHORUS TO FINISHED WATER
SUPPLY MEAN PHOSPHORUS, mg/1 MEAN AMMONIA - N,mg/T
Raw Finished Change Raw Finished Change
All supplies 0.11 0.10 0.01. .0.154 0.154 0
Added Ammonia 0.155 0.350 0.195
Added Phosphorus 0.125 0.293 0.168
30
-------
Most supplies add fluoride. This is evident from the median fluoride
tration of 1.0 rag/1. However, 9 supplies apparently do not add fluoride.
Nine (9) supplies had pH values between 9.0 and 10.1. Of these supplies,
') also had CHCls concentrations greater than 50 ug/1. No additional rela-
n'ps were found.
Suspended solids removal was 90 percent based on the mean raw and finished
values. The highest suspended solids value for a finished water was 42 mg/1,
econd high was 13 mg/1, and all other values were 8 mg/1 or less. No positive
ilation exists between suspended solids and the presence of halogenated organic
Dunds. However, COO removal averaged only 50 percent indicating that signi-
it amounts of organic materials remained in the filtered water. This sug-
.s that the turbidity standard (suspended solids is the cause of turbidity)
not be sufficient to protect water supplies from halogenated organic compounds.
Economic Considerations
Table XI gives estimates of resources expended to complete this survey.
dollar estimates are based on the assumption that total expenses, including
overhead, costs $40,000 per position and a year contains 260 working days.
:. SIGNIFICANCE
It is not surprising that trace amounts of various organic chemicals can
detected in drinking water. With the sensitivity available in the gas
romatograph/mass spectrometer-computer equipment it is probable that many
ch compounds can be found in almost any facet of our environment that one
ooses to look. Absolute purity is only a theoretical term and is not attain-
3le in drinking water.
Concentrations that are above a normal background and that do pose a
ignificant health risk should of course be reduced. There are currently not
:nough data to fully understand either the normal background level or the health
iignificance of the organic compounds included in this study. However, with
31
-------
TABLE U
ESTIMATED COST DATA FOR THE REGION V SURVEY
1. Number of Cities Sampled 83
2. Number of Samples collected including duplicates for
Quality Assurance (QA) purposes 210
3. Number of Bottles collected 2,940
4. Number of Analyses per Sample 94
5. Total Number of Analyses performed * 19,740
6. Total Number of Analyses reported 15,604
7. Total Number of QA measurements made 4,136
Resources Required
Labor @ $40,000/Yr. including Overhead Man-Days Cost
1. Completion of Study Plan by Project Officers
2.
3.
4.
1.
2.
3.
1.
2.
3.
4.
and Administration Officials 6
Sample collection - One man day for preparation 30
and four man days for collection per State
Laboratory Analysis - One fourth of the total 289
CRL staff of 33 positions for 7 weeks
Preparation, typing and editing of final report 15
Supplies
Sampling bottles, caps, teflon liners, etc.
Organic solvents
Miscellaneous supplies
Cost Per Unit Total
Cost per City
Cost per Sample including QA
Cost per Analysis " "
Cost per Reported Concentration Value
$ 920.00
4,620.00
44,400.00
2, 300. no
400.00
2,600.00
1,000.00
$ 56,240.00
$ 678.00
$ 268.00
$ 2.85
$ 3.60
Does not include non-volatile and carbon filter analyses although
these are included in the estimation of required resources.
'32
-------
perhaps the exception of chloroform, concentrations of organics analyzed in
these drinking waters should not be considered atypical. It is not likely that
they will be found to present a significant risk to health. Exposures to these
same compounds from ambient levels in other aspects of our environment (smoke,
air, food, medicines, etc.) can be expected to be much greater than that from
drinking water.
Chloroform, it appears, is affected by chlorine application. Concentra-
tions of chloroform in water supplies with a high chlorine demand may exceed
0.1 milligram per liter (mg/1). However, even at the highest concentration
found (0.366 mg/1), chloroform should not be considered to present an imminent
risk to health. There is no evidence that chloroform causes tumors in workers,
and the allowed occupational exposure to chloroform in air is over 100 times that
from drinking water with 0.5 mg of chloroform per liter.
The possibility must be recognized, however that traces of micropollutants
in drinking water may indeed contribute to the total exposure of persons to
environmental factors that contribute to carcinomas. An ad hoc Study Group of
EPA's independent Science Advisory Board in their May 1, 1975 report on the
health significance of drinking water chemicals, concluded that 1'some: health
risk exists." A portion of the Study Group's summary follows:
"Based upon recent, reasonably extensive, water quality data for
many U.S. water supplies and on extremely limited data from
experimental carcinogenesis studies, the Study Group concludes
that there may be some cancer risk associated with consumption
of "chloroform in drinking water. The level of risk, estimated
from consideration of the worst case and for the expected
cancer site for chloroform (the liver) might be extrapolated
to account for up to 40% of the observed liver cancer incidence .
rate. A more reasonable assumption, based upon current water
quality data which show much lower levels than the worst case in
the majority of U. S. drinking water supplies, would place the
risk of hepatic cancer much lower and possibly nil. Further,
it is emphasized that both the experimental carcinogen!city data
and the mathematical and biological extrapolation principles used
to arrive at the upper estimate of risk are extremely tenuous.
Epidemiologic studies do not, thus far, support the conclusion
of an increased risk of liver cancer; although hypothesisformulating
33
-------
studies in southern Louisiana suggest the possibility of an
association with contaminated water and overall high cancer
incidence. Critical definitive tests of this hypothesis have
not been conducted. Although some other organic contaminants
contained in the charge to the Study Group have carcinogenic
potential, the cancer risk to man is judged to be minor because
of their low concentration and/or infrequent occurrences in
drinking water."
IN SUMMARY: The study's findings do raise questions about the quality of
drinking water and there is a need for a better definition of the health rela-
tionships between these substances and man. At this point, though, there is
no evidence to justify quantum changes in current water treatment practices.
For example, EPA's statement from last November holds true . . . "the benefits
of continued use of chlorine for the disinfection of drinking water far out-
weigh the possible health risks from chlorine-derived organic compounds." While
trace organics in drinking water are an important problem which deserves investi-
gation, the situation today is not a crisis to be met with fear and precipitous
action.
IV. RECOMMENDATIONS
1. When wells contaminated with arsenic are used in Kokomo, the drinking
water should be monitored at least monthly to be certain that it
consistently meets drinking water standards. Appropriate precautions
should be taken before drilling any new wells in the area.
2. Since our results are based on individual grab samples collected at
what may not be normal conditions, the data may not reflect the long
term quality of any given supply. Therefore, the finished water of
those 31 supplies showing higher chloroform concentrations above
33 ug/1 should be re-analyzed for the volatile organic compounds and
selected metal and other inorganic parameters. In addition, a complete
organic compound analysis should be completed on as many of these water
supplies as possible.
34
-------
3. An effort should be made to identify the precursors) that react with
chlorine and bromine to produce the pollutants found in the finished
water samples. As a first step, raw waters should be analyzed com-
pletely and halogenation studies completed on potential precursors.
The best treatment for these pollutants may be removal of a precursor
rather than removal of the organic compounds found in the finished
water supplies. Raw water samples should be taken and analyzed com-
pletely at .those cities having the highest chloroform concentrations.
4. In addition to treatment methods involving carbon and ozone, aeration
should be looked at for removing volatile organic compounds.
5. The relationship of COD {or TOC) and CHC13 concentrations should be
further investigated to include raw water source comparisons and
other parameter correlations such as pH to act as indicators for
volatile organics.
V. SAMPLE COLLECTION, ANALYTICAL PROCEDURES AND QUALITY ASSURANCE
In general, all samples were collected, preserved and analyzed according
(3)
to recommended EPA procedures . In cases where official procedures have not
been recommended or approved, such as for the volatile organic and carbon filter
methods or where superior analytical methods have been developed as for the COD,
standard methods in current use in Region V were employed. All of these methods,
with corresponding quality assurance data that will permit the reader to estimate
the quality of data on a parameter or group of parameters basis are described
later in this section.
35
-------
1. Sampling Procedures
Fourteen bottles of water were collected at each city. These
bottles were divided according to sample preservative as described
below. In all cases the bottles were filled completely to avoid an
air-liquid interface. Raw water samples were collected just prior to
chlorination. Finished water samples were collected several hours
after chlorination depending on plant flow.
Bottle
For
a) four one liter glass two bottles for
bottles w/teflon lined raw water organics
caps
Preservative
ice
b) two 500 ml high
density polyethylene
bottles,
and two bottles for
finished water
organics
raw and finished
water - metals
c) two 250 ml polyethylene raw and finished
bottles water-nutrients
d) two 250 ml polyethylene raw and finished water
bottles cyanides
e) two 250 ml polyethylene raw and finished water
bottles phenolics
f) two 250 ml polyethylene raw and finished
bottles water
(pH, specific conductance,
alkalinity, etc.)
HN03
NAOH
CuS04/H3P04
ice
Since these types of bottles had been in use in the Region for some
time and were known to be clean, they were not washed prior to sample
collection. However, to insure that results due to bottle contamination
or some other contamination were not reported, the normal set of reagent
-36
-------
blanks (preservative and distilled water in a sampling bottle) were
prepared daily by each sampling team and analyzed as the samples were
analyzed. No contamination problems associated with sampling were
detected.
The maximum holding times for the organic parameters are
unknown. Therefore, all organic samples were refrigerated upon
collection and either extracted or analyzed as quickly as possible
after sample collection; usually within forty eight hours but no
later than five days after sample collection. A laboratory standard
containing the seven volatile organics of interest was analyzed daily
during the study and remained stable for four weeks. Although chlor-
inated hydrocarbon pesticides are stable, other pesticides are known
to degrade with time so only minimum concentration values can be mea-
sured for these parameters.
All inorganic parameters were analyzed within those holding
times recommended for approval by Region V to the Methods Development
and Quality Assurance Research Laboratory, National Environmental
Research Center, Cincinnati, (Appendix I).
2. Volatile Organics
a) Analytical Procedures.
The procedure described below is a modification of methods
described by Kleopfer > for air studies and by Bellar and
(1 2)
Lichtenberg for volatile organics in water/ ' We have used
the experimental apparatus and organic trap described by Kleopfer,
the water sampling method of Bellar and Litchtenberg and have
37-
-------
developed our own gas chromatographic analytical techniques.
Quality Assurance data given at the end of this section shows
the procedure to give accurate results within the defined
experimental scatter.
Ten milliters of sample are transferred to a microware
centrifuge tube with a 14/20 ground glass joint from a com-
pletely filled glass sampling bottle. The centrifuge tube
is then placed on the debubbler apparatus held in place by
two springs as shown in Figure VI•
FIGURE VI
Nitrogen Gas Source
Flow Control & Rotameter
,— Rubber Serum Cap
Teflon
v ex St°
V/^x Sample
Centrifuge Tube
Teflon Stopcock
Quick Disconnect
5" x V Stainless Steel
v\ Stopcock
'^ Sample
\« . .„ _ . V/26 Gauge Needle
38
-------
The needle of a trap that has been cleaned by being heated
to 135°C and flushed while hot with nitrogen is inserted into
the rubber septum. The stopcocks are opened permitting nitrogen
to flow through the debubbler, sample water and into the trap
where the organic compounds are adsorbed on the surface of the
Tenax. A nitrogen flow rate (Purge) of 80 ml/min for 8 minutes
is sufficient to quantitatively transfer those volatile organics
studied in this project. The trap is then removed and attached
to the gas chromatograph - desorption oven system as shown in
Figure VII
FIGURE VII
, Stopcock (switch "A'}
Quick Disconnect
Stainless Steel V Tubing
126 Gauge Needle
Flexible Tubing (Teflon,
ww*. or ;' Conductivity Detector
Flow Control 4 Polyethylene) ; '—• Gas Chromatograph
Rotameter | , standard Liquid Injector
Hitrogen Source
Heating Unit (Heating Tape
Around 12mra Glass Tubing)
The trap is placed in the desorption oven with switch "A" (see
Figure 3) in the off position and left for 2 minutes while
thermal equilibrium is being established. The syringe needle
on the trap penetrates the GC injection septum as the trap is
placed in the desorption oven. At the end of the 2 minute
period, switch "A" is opened and the sample is carried into
-39-
-------
the GC column where a standard chromatographic analysis is
completed. Quantitative data are obtained by comparing the
recorder response of standard solutions to the response of
unknowns. Operating conditions of the chromatograph and
detector are as follows: oven temperature - 30°C for 3 min.
and then raised to 200°C at a rate of 20°C/min; injector
temperature - 200°C; detector oven temperature - 800 C;
nitrogen carrier gas flow rate - 40 ml/min; detector reducing
gas (h^) flow rate - 80 ml/min; desorption gas (Ng) flow
rate - 40 ml/min; column - 6' x 1/8" aluminum packed with
10% by weight FFAP on 60/80 Mesh Anakrom. A typical gas
chromatogram of a laboratory quality assurance control
standard is shown later.
b) 'Quality Assurance for Volatile Organics
Before any samples were analyzed for the presence of
halogenated volatile crganics, extensive analytical quality
control data was collected to optimize the analytical con-
ditions and to determine the reproducibility of the method.
Table XII lists the. responses given by the seven halogenated
organics included in this study as a function of purge time.
The purge gas flow rate was maintained at 80 ml/min during
investigation of the flow time. Preliminary work indicated
that longer purging times were required if the purge rate is
lowered. The data summarized in TableXII indicates that,
with a purging rate of 80 ml/min, a purge time of 8 min.
is optimum for the seven compounds of interest.
40
-------
Table .XIII summarizes the data obtained for a standard
mixture which was analyzed five different times (three
different traps were used to trap the volatiles). The
relative standard deviation is larger for methylene chloride
and carbon tetrachloride because of time limitations peak
heights instead of peak areas were used for quantification
check. Since methylene chloride and carbon tetrachloride
give broader and more poorly resolved peaks than the other
compounds investigated, a larger amount of scatter was
observed when the peak height was used for quantification
check.
41
-------
TABLE
Gas Chromatograph Detector
Response As A Function Of Purge Time
In Arbitrary Units
RESPONSES
Purging Time
4 min.
6 min.
8 min.
10 min.
CH2Cl2
2370
2170
2370
2110
CC14
1090
1340
1150
880
CHC13
2240
2560
3260
2820
C2H2C12
5570
6140
9150
7740
Cl2BrCH
3970
4030
5500
4610
ClBr2CH
8000
8770
12030
9660
Br3CH
4350
5690
7870
7920
TABLE XIII
Reproducibility Of The Analytical Method
(Arbitrary Units Of Detector Response)
Compound
CH2Cl2
CC14
CHC13
C2H2C12
Cl2BrCH
ClBr2CH
Br3CH
Concentration
yg/l
49
59
55
54
73
85
107
Run
2880
1860
2880
7360
4740
10050
6590
Run
#2
2370
1150
3260
9150
5500
12030
7870
Run
#3
2690
1470
3070
8060
5180
11140
7420
Run
2110
770
3330
9280
4860
11840
7880
Run
#5
2430
1380
3230
9730
6270
12540
7170
Average
2500
1320
3160
8720
5310
11520
7380
Relative
Std. Deviation
t
12%
30%
6%
11%
11%
10%
8%
'42'
-------
Analytical quality control employed during analysis consisted
of routinely: 1) analyzing blank traps, 2) analyzing standards, 3) con-
firming the highest concentrations (10») qualitatively on the mass-
spectrometer and 4) collecting and analyzing 10% of the samples in
duplicate.
Blanks were analyzed at random throughout each day of the study.
A blank consisted of carrying out the complete analytical procedure
but leaving out the 10 ml of sample. Table XIV? summarizes the data
obtained for the blanks. It should be pointed out that the highest
blank values were obtained on two days when methylene chloride, carbon
tetrachloride and chloroform were being used as solvents in another
part of the laboratory and illustrates the sensitivity and extreme
care that must be used when performing these analyses. Figure VIII
shows the gas chromatogram of a typical blank.
Standards, made by dissolving approximately seven yl of a mix-
ture containing stoichiometric amounts of the seven halogenated organics
in 300 ml of water followed by diluting an aliquot of this to give a
final concentration in the 10 to 50 ug/1 range for each compound, were
analyzed at least three times a day (morning, noon and afternoon). The
average response factors were then used to calculate the concentration
of the samples. Fresh standards were made at least every 48 hours.
Fig .VIII also shows examples of chromatograms for a standard solution.
Even though the Coulson conductivity detector employed is
specific and warrants a high degree of confidence, over 10% of the
samples giving positive results were qualitatively confirmed using
gas chromatography - mass spectroscopy.
43-
-------
FIGURE VIII
Gas Chromatogram of Volatile Organic Compound^
is
h i
i-
to
c
o
o.
to
CL)
s-
o
4->
U
OJ
•M
•O)
Q
Concentrati
on 44 52. 48 41 64 76 95 (ug/1)
Glassware, instrument and reagent blank
1
4
i |
I 1 _ J 1
5 6 7 8 9 10 11
Minutes
44
-------
TABLE XIV -*
Summary of Results Obtained for All Reagent
Blanks Analyzed During the Study
Compound
CHoC 1 o
CC14
CHC13
C2H2C12
Cl2BrCH
C1Br2CH
Br3CH
Range Found
vig/1
0 - 3
0-5
0 - 7
< 1
< 0.5
< 0.5
< 0.5
Average
yg/l
< 0.7
< 1
< 2
< 1
< 0.5
< 0.5
< 0.5
45-
-------
As an overall quality control check, approximately 13% of the
cities were sampled in duplicate. The analytical results for the dupli
cate samples are summarized in Table XV and defines for the reader
the precision of the total sample collection and analytical procedures
employed.
Fourteen samples were stored in a refrigerator after being
analyzed. A month later it was decided to re-analyze the samples.
The results are given in Table X-VI,. Only the data for CHC13, and
CHCIzBr are reported. The other five compounds of interest were below
detection limits. Since there was originally no intention of re-
analyzing the samples, they were not tightly stoppered nor were they
filled completely to the top (approximately 30 ml were removed when
the samples were first analyzed). This we believe is responsible for
the lower CHC13 values obtained at the latter date in those samples
containing higher chloroform concentrations. However, the data in
Table agrees in sufficient detail to augment the other AQC data
and to increase the credibility and the validity of the reported
sample concentrations. The data also indicate that refrigerated
samples can probably be preserved for over a month prior to analysis.
46-
-------
TABLE XV
Analytical Results ( wg/1) of All Samples Collected
In Duplicate
Peoria, 111. Raw I
Raw II
Fin I
Fin II
Mt. Vernon, Raw I
Ind. Raw II
Fin I
Fin II
Gary, Ind. Raw I
Raw II
Fin I
Fin II
Detroit, Mich. Raw I
Raw II
Fin I
Fin II
Menominee , Raw I
Mich. Raw II
Fin I
Fin II
Minneapolis , Raw I
Minn. Raw II
Fin I
Fin II
Duluth, Minn. Raw I
Raw II
Fin I
Fin II
Cleveland, Ohio Raw I
' Raw II
Fin I
Fin II
MeCl2
<1
< .5
< .5
<1
4
<1
<1
2
< .5
< .5
< .5
< .5
< .5
< .5
< .5
< .5
< .5
< .5
1
1
< .5
< .5
< .5
< .5
< .5
< .5
<1
<1
< .5
< .5
<1
<1
CC14
<1
<1
1.3
1.3
2
<2
2.4
2
<1
<1
1
1
<1
<1
<1
<1
<1
<1
1
<1
3
<2
10
5
<2
3
20
25
2
<2
4
15
CHC13
<1
<1
2.0
1.6-
3
<2
20
15
<1
<2
6
7
<1
<1
2
3,4
<2
6
42
54
4
<2
8
7
20
1
28
26
<1
<1
12
8
Cl2BrC2H4
1
< 1
6.0
< 1
< 2
< 2
< 1
< 1
< 2
< 4
< 2
< 2
< 1
< 2
< 1
< 1
3
26
< 2
< 2
< 1
< 1
< 1
< 1
< 1
< 1
< 1
< 1
< 1
< 1
< 1
< 1
Cl2BrCH
<0.5
<0.5
1
0.6
< .5
< .5
g
9
< .5
< .5
5
5
< .1
< .5
9
10
< .5
'< .5
5
6
< .5
< .5
< .5
< .5
< .5
< .5
3
3
< .5
<1
6
4
ClBr2CH
<0.5
<0.5
0.5
0.5
< .5
< .5
1.5
1
< .5
< .5
1
1
< .1
< .5
2.4
2
< .5
< .5
0.6
0.4
< .5
< .5
< .5
< .5
< .5
< .5
< .5
< .5
< .5
<1
0.8
0.5
Br3CH
<0.5
<0.5
0.4
0.3
< .5
< .5
1.6
.3
< .5
< .5
< .5
< .5
< .1
< .5
< .5
< .5
< .5
< .5
0.3
0.3
< .5
< .5
< .5
< .5
< .5
< .5
< .5
< .5
< .5
<1
<1
<]
47
-------
TABLE XV (Cont'd)
Portsfflorth, ' .. Raw I
Ohio Raw II
Fin I
Fin II
Black River Raw I
Falls, Wise. Raw n
Fin I
Fin II
Green Bay Raw I
Wise. ' Raw II
Fin I
Fin II
MeCle
2
<1
3
3
<.5
< .5
<1
<1
Sample
<1
4}
<1
CC14
2
2
1
1
4
<2
8
<2
Lost du
3
<1
<.!
CHCla
2
6
29
21
3
<1
8
4
ring Ana
1
10
9
Cl20rC2H4
2
2
^1
<1
<1
<2
<1
<1
lysis
<1
<1
<3
Cl2BrCH
*.2
<.2
15
14
<.5
<.5
4.5
<.5
<.5
11
3
ClBr2CH
<.2
<.2
5
4
<.S
<.5
<.5
<.5
<.5
2
<1
Br
<.
<.
•
•
-------
TABLE XVt
VOLATILE ORGANIC CONCENTRATIONS VERSES TIME
Sample #
14313
14309
14297
14325
14289
14321
14293
14337
14853
14366
14345
14410
14317
14329
14825
14374
14301
CHCU
Analyzed On
2/20/75 3/26/75
•37
2
10
22
7
7
82
26
3
8
26
366
128
79
2
5
200
36
3.5
10
18
9
9.4
78
23
2.5
20
17
205
101
53
4
4
130
Cl£BrCH
Analyzed On
2/20/75 3/26/75
4
9
0.8
0.8
6
0.3
4
3
18
15
6
£1
31
6
8
0.7
0.4
5.4
0.9
5
2.2
19
9.6
5
1.3
16
-------
3. Pesticides, PCB's and Phthalates.
a) Introduction
The procedure used is based on "Methods for Organic
Pesticides in Water and Wastewater," 1971, EPA publication
from NERC - Cincinnati. The procedure differs from the
NERC's in that it has been expanded to include 47 pesti-
cides, 5 PCB mixtures and 2 phthalate esters. Also, the
gas chromatograph analysis step has been automated.
b) Experimental Procedures
The samples are received in glass quart bottles with
teflon lined screw caps and are transferred into clean two
liter separatory funnels. The first portion of the extract-
ing solvent is used to rinse out the sample bottle and then
is added to the separatory funnel. The samples are extracted
twice with 100 ml of 15% (v/v) ethyl ether /hexane, then
once with hexane, dried over NagSO^, and concentrated to about
5 ml in a Kuderna-Danish concentrator. The volume is reduced
to less than 4 ml using a stream of dry filtered air, diluted
to exactly 4 ml, and split into two 2 ml portions (I and II).
Portion (I) is spiked with phorate (2 yg), placed in a
2 ml vial fitted with a screw cap, and analyzed for phosphorus-
containing compounds. The analysis is performed on a Perkin-
Elmer model 900 gas chromatograph using a flame-photometric
(phosphorous mode) detector. This instrument is equipped with
50^
-------
an automatic sampler (adjusted for 10 yl injection) and a
PEP 1 G.C. data reduction system. A 6' x 1/4" glass column
packed with 14% SE-30 and 6% OV-210 on 80/100 mesh gas chrom
Q is used for the original analysis and a 6' x I/A" column
packed with 1.95% OV-17 and 1.5% 0V 210 on gas chrom Q 30/mo
mesh is used for confirmation. The gas chromatograph con-
ditions are as follows: inlet temperature - 250°C, detector
temperature -, 240°C, oven programmed from 200°C to 265°C at
4°/min, carrier gas - N2 at 60 ml/min.
Portion (II) is placed on a column of Florisil (18 q.
obtained from NERC, RTP, slurry packed with hexane) with 1/2"
of Na2$04 at the top and bottom of the florisil.
Two fractions are collected; the first is eluted with
200 ml of 6% ethyl ether in hexane, and the second with
200 ml of 50% ethyl ether in hexane. Each fraction is con-
centrated to less than 2 ml in the same manner as that used
for the extract, diluted to 2.0 ml with hexane, spiked with
Dieldrin (50% ether fraction) or Aldrin (6% ether fraction)
and placed in a 2 ml vial with a septum cap for GC analysis.
Each fraction from the Florisil column is analyzed using
a Perkin-Elmer 3920 gas chromatograph equipped with a two-
column injector splitter, automatic sampler with 10 ul syringe,
-51-
-------
two columns each leading to an electron capture detector,
and a PEP-1 data reduction system. The columns are both
6' x 1/4" glass. One is packed with 4% SE-30 and 6% OV-210
and the other with 1.95% OV-17 and 1.5% OV-210 on 80-100
mesh gas - chrom Q. The oven is maintained at 205°; the
carrier gas is 5% methane in argon for both columns.
A measured aliquot of each sample from the 6% ether
fraction which is thought to contain PCB's, as shown from
its chromatogram, is removed from the vial and placed onto_
a column of deactivated silicic acid (6 g, Bio-Rad Laboratories,
2.0% water content) which has been packed and washed with
60 ml hexane. The first fraction is eluted with hexane
(45 ml) and the second with 150 ml of a mixture of 80% methylene
chloride, 19% hexane, and 1% acetonitrile . Each fraction is
concentrated to less than 2 ml as previously described, diluted
with hexane to 2.0 ml, spiked with Dieldrin, and placed in a
vial for GC analysis. These fractions are analyzed for PCB's
and pesticides on the Perkin-Elmer model 3920 dual-column
electron capture system describe- above.
An overall flow diagram of the analysis scheme is shown
below with typical chromatograms and computer printouts for
list A & B compounds.
-52-
-------
SAMPLE
Portion I
Fraction I
Extract 3X with ethyl ether/hexane
and divide into portions I and II
Portion II
Chromatograph
with Florisil
Fraction II
Perform GC Analysis
for Phosphorous
Compounds - List A
Analyze for
List B Compounds
Aliquot I
Aliquot.- II
Chromatograph
with Silicic Acid
List D, E
GC Analysis for
List D Compounds
Perform GC
Analysis for
List C Compou
GC Analysis for
List E Compounds
LIST
D
Phosphorous
Dyfonate
Ethion
Dursban
Diazinon
Ronnel
Methyl Parathion
Ethyl Parathion
EPN
Malathion
Phencapton
DEF
Phosalone
Azinphos methyl
Azinphos ethyl
Carbophenothion
Coumaphos
Fraction I
Di-n-butyl phthalate
Di-(2-ethythexyl)
phthalate
Endosulfan I & II
Nitrofen
Oil an
2,4-0: Isopropyl
ester
DCPA
Dieldrin
Endrin
Chiorobenzilate
2,4,5-T: Iscoctyl
ester
Tetradifon
of
Aliquot II
Fraction II
Treflan
Lindane
Hexachlorobenzene
Isodrin
Gamma Chlordane
Beta-BHC
Aldrin
Zytron
Heptachlor Epoxide
0,P - DDE
PF~- DOE
W_ - ODD
PP - DOO
W - DOT
FP~ - DDT
MTrex
Methoxychlor
Aliquot I of Fraction II
Aroclor 1221
Aroclor 1242
Aroclor 1248
Aroclor 1254
Aroclor 1260
Hexachloro-
benzene
Aldrin
PP_ DDE
MTrex
Treflan
Lindane
Beta BHC
Zytron
Isodrin
Heptachlor
Epoxide
Garrma Chlorda
OP DDE
W DDD
PP DOD
OT DDT
W DOT
Flethoxychlor
•53-
-------
FIGURE" IX-
1HKESHGLDS
INST J
TIME
. 3.41
4.27
4.60
5.39
5.71
6. 63
7. 64
8. 12
8.55
9.03
9
1
3
3
6
8
9
20
21
22
87
31
92
67
98
91
52
76
1 1
04
35
25. 64
COMPUTER PRINTOUT
1200
ME1H00
AREA
7.
4.
5.
•
.
9.
2.
5.
3.
.
6.
3.
.
9.
4.
1 .
6.
13.
9.
4.
1 .
20.
6124
4668
9568
J 1 56
2465
5539
8457
3657 .-
5236
0847
4339
1 529
1847
3273
761 1
0771
6851
01 63
5878
R905
32HO
441 6
200
42
RRT
.341
.427
.460
.539
.571
.663
.764
.512
. .855
.903
.987
.131
. 192
.367
.398
. 691
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2 . 104
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FOR LIST A COMPOUNDS
LE '
RF
.7500,
.9880,
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.0539,
.0070,
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Area = Area under respective peak.
RRT'= Relative retention time as compared to a standard retention
time entered previously in the computer.
RF = Detector response factor (sensitivity factor) based on previously
Injected primary standard solutions;
/'
C = Calculated concentration using RF of named'compound.
Name = Name of standard having same retention time as unknown.
-54-
-------
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FIGURE X3;
» •
COMPUTER PRINTOUT FROM THE SE-30/OV-210 GC COLUMN
OF LIST B COMPOUNDS
300
100
IX-i, I
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-------
FIGURE XII
COMPUTER PRINTOUT FROM OV-17/OV-210 COLUMN
OF LIST B COMPOUNDS
THKESH0LOS
IN3T
300
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FILE
19
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-------
_co
-------
c) Quality Assurance For Pesticide Analysis
In order to insure validity of the analytical results,
extensive analytical quality control was performed on each
step in the analytical scheme. Ten percent of the samples
were collected in duplicates for AQC purposes.
In the laboratory, samples were analyzed in groups. A
"blank" and a "spike" were analyzed with each group to provide
analytical quality control for that group. The "blanks"
and "spikes" were prepared using distilled water. The "spike"
contained a mixture of the 47 pesticides included in this
study. The concentrations of the various compounds in the
spike were in the 0 to 5 ug/1 range for the phosphate pesticides
and 20 to 200 ng/l range for the chlorinated pesticides. A
total of ten sets of "blanks" and "spikes" were analyzed. All
the AQC samples were treated in the identical manner as the
real samples were treated.
In order to evaluate the automatic gas chromatographic
system, standards were chromatographed at least every tenth
sample* This was used to monitor any change in the retention
time and/or in the response factor for each pesticide. If
changes were noted, the system was recalibrated and the samples
re-analyzed.
-59-
-------
Recovery data for the "spikes" are summarized in Table XVII
and relates to the reader the precision on a parameter
by parameter basis. None of the blanks indicated the
presence of pesticides above the detection limits. A normal
percentage of the samples collected in duplicate gave iden-
tical results within": the precision given in Table XX. The
only serious problem is the high recovery values for phthalates
which probably indicates contamination. We have reported
uncorrected phthalate concentrations with quality assurance
information to permit the reported data to be evaluated
by the user and urge each data user to use the phthalate
results with appropriate caution.
-60-
-------
TABLE
Reco v ery Da t a Fo r
Ten Or More Samples Spiked With Pesticides
COMPOUND
Diazinon
Dyfonate
Ronnel
Dursban
Methyl parathion
Malathion
Ethyl parathion
DEF
Ethion
Carbophenathion
i
Phencapton
EPN
Methyl azinphos
Phosalone
Ethyl azinophos
Coumaphos
2,4D,isopropyT-
ester
Di-N-butyl-
phthalate
yg/1 Added
6.0
6.0
14.0
4.0
8.0
8.0
8.0
4.0
8.0
8.0
2.0
10.0
60.0
10.0
10.0
60.0
280
2000
Average %
Recovery
94
81
98
100
90
88
93
111
100
92
107
92
61
89
86
95
36
73
Standard Deviation
of % Recovery
33
38
33
30
34
28
35
33
41
32
36
34
34
36
37
25
13
58
-------
TABLE XVII* (Cont'd)
COMPOUND
DCPA
Endo I
Dieldrin
Endrin
Chi orobenzi late
Endo II ~]
Nitroflen J
0 A C T
C»H»— J 1
isooctyl ester
Oil an
DEHP
Tetradifon
Treflan
Hexachloro-
benzene
Lindane
B BHC
Aldrin
Zytron
Isodrin
Heptachlor
Epoxide
Gamma
Chlordane
yg/1 Added
48
60
48
64
80
80 "|
80 J
240
200
3200
120
24-46
12-22
20
56-400
20-40
80-98
23
20-24
20-24
Average %
Recovery
70
90
78
. 66
52
62
89
56
289
102
98
61
70
74
76
75
82
78
103
Standard Deviation
of % Recovery
50
97
42
45
36
65
67
47
200
130
20
20
28
33
28
22
29
42
19
-62-
-------
TABLE XVII (Cont'd)
COMPOUND
0-P DDE
P-P DDE
0-P ODD
0-P DDT
P-P ODD
P-P DDT
Mi rex
Methoxychlor
yg/1 Added
60
60
'60
60
60
60
40
200
/•
Average %
Recovery *
86
86
100
93
TOO
101
77
97
Standard Deviation
of % Recovery
14
21
11
13
12
22
39
17
* Calculated as follows:
Average % Recovery = Original sample concentration + Spike - OSC
Spike
We choose to use this equation because the equation recommended by
EPA makes the data appear to be of a higher quality than they really
are.
-63-
-------
4. Non-Volati 1 c Orcjanics
a) Analytical Procedures
*) One liter Fim'r.hcd Water Grab Samples.
The 970-990 mi niters of sample not used to analyze
for volatile organics is preserved with 25 ml chloroform and
later poured into a one liter separatory funnel and ex-
tracted three times with 50 milliters of ethyl ether.
The combined extracts are dried over anhydrous sodium
sulfate and concentrated to approximately 0.2 ml in a
Kuderna-Danish evaporator. One to five microliters of
the concentrate are'injected into a gas chromatograph
equipped with a 6' x T/4-" glass column packed with 52
OV-101 and a flame ionization detector. Large peaks
observed in the chromatogram are identified with the
mass spectrometer. The list below shows compounds
identified using this technique. The phthalate esters
were found much more frequently than other compounds.
1. Phthalates: dioctyl, dibutyl, Bis(2-ethyl hexyl),
diethyl, dimethyl, ethyl and butyl.
2. Olecamide
3. Bis(2-ethyl hexyl} Adipate
4. Trichlorobenzene
5. Phenylphenol
6. Di-isobutyl Adipate
7. Butyl Phthalate butyl glycolate
-------
ii) Carbon Filter Samples
Carbon is extracted prior to being used for 24 hours with
hexane and 24 hours with methanol in a soxhlet extractor and
then placed in a glass filter equipped with teflon gaskets,
copper tubing and brass fittings. At no time does the incoming
water contact rubber type materials. All sampling equipment
is washed with soap and water overnight in an ultrasonic
cleaner> then with hexane and acetone prior to use. The
filters are placed on a common garden hose type faucet such
that water enters the bottom and flows out the top to a drain
as shown in Figure-XI-^- A carbon blank is treated in the same.
manner as carbon used to sample a water supply except for
passing sampling water through it.
FIGURE XIV
Standard Faucet
5/8 Inch Connection
— Aluminum Screen Wire
— Top Steel Plate
,—Teflon Gasket
Rubber Gasket
To Drain
Carbon
• 1/2 inch Copper Tubing
'*•
Carbon
Glass Wall
Bolt (5) Which Holds
End Assembly Together
Nut
Bottom Steel Ring
-------
Since the adsorption and desorption efficiency on
carbon is not known for most organic compounds, quanti-
tative data can not be obtained and therefore only
approximate flow rates need to be obtained. These are
easily obtained by using a large (2-5 1) graduated
cylinder and stopwatch daily.during the sampling period.
Using a small stream of water, the sample volume per
week is usually between two and four thousand liters
for clean waters that do not significantly reduce
the flow by depositing foreign material in the filter.
The efficiency of adsorption is known to decrease as
the flow increases thus a greatly increased flow rate
may actually reduce the total quantity of material ad-
sorbed by the carbon. Carbon from the exposed filters
is transferred to a soxhlet and extracted for 24 hours
with hexane, 24 hours with chloroform and 24 hours with
methanol. Each extract is then divided into an acidic
basic and neutral fraction by standard techniques using
5%. HC1, 5% NaOH and the organic solvent used to extract
the solvent or toluene in the case of the methanol ex-
tract. The nine resulting extracts are dried over an-
hydrous sodium sulfate and concentrated to approximately
two millitersbefore a gas chromatographic and mass
spectrometric analysis is attempted. Experience to date
-66-
-------
shows that the separations described above are usually
adequate for all except the neutral chloroform fraction,
which contains more compounds than can be separated using
gas chromatography. High pressure liquid chromatography
techniques for further purification of this fraction are
being investigated. Compounds identified to date are
shown below. Of significant interest is that bis-2-chloro-
ethy! and isopropyl ethers are below detection limits in
these samples.
t^ Vernorr,
Indiana
Evansvilie,
Indiana
tri-n-butyl phosphate
butyl phthafate
dfoctyl phthaTate
tri methyl benzene
toluene
ethyl benzene
xylene
methyl cyclohexane
other hydrocarbons
tri-n-butyl phosphate
butyl phthalate
dioctyl phthalate
Farnesol
n-octane
methyl palmitate
xylene
di-phenyl ether
other hydrocarbons
-67-
-------
5. Metals.
a) Analytical Procedures
i) Flame Atomic-Absorption
Procedure
Standard flame atomic absorption procedures were
used for the determination of calcium, chromium, copper,
iron, magnesium, manganese, potassium, sodium, and zinc (3).
The reported results were obtained by direct aspiration
of water samples preserved with 0.5% concentrated nitric
acid. Thus the listed values represent metal concentra-
tions that were dissolved by the acid preservation, and
these will be equal to or lower than total metal concen-
trations as defined by the US EPA analytical procedures (3),
Analytical Quality Control
The accuracy and precision of the analytical
measurements were assessed by the use of duplicate samples,
spike recoveries, and intralaboratory control standards.
Data supporting the validity of the reported results and
that are pertinent to this study are listed in Tables XV111
XlX^and XX- - >;The listings are self-explanatory and show
that the determinations were performed with good accuracy
and precision.
-68-
-------
•j-j) Flameless Atomic Absorption
Procedure
Flame!ess atomic absorption procedures were used
for the determination of arsenic, cadmium, lead, selemium,
and silver. The Perkin-Elmer HGA-2000 was utilized for
this purpose. This unit was mounted on a double-beam
atomic absorption spectrophotometer equipped with a deuterium
background corrector and interfaced to a strip chart re-
corder. The technique of standard additions was applied
exclusively for sample analysis. At least 3 working standards
and a reagent blank were prepared just prior to use from
commercial atomic absorption standard concentrates using
quality water and high purity acids. The instrumental
setup was optimized for the appropriate working range of
the element to be determined, and standards were checked
for linearity prior to use. Appropriate volumes (10-50
of sample and standard were injected and analyzed by pre-
viously established operating conditions. Linear working
curves (peak height vs. concentration) were extrapolated
graphically to zero absorbance for sample concentration
results. Samples outside the linear range were diluted.
In addition, acidities were closely controlled, since it
has been established in this laboratory that for certain
-71-
-------
metals, i.e. arsenic, selemium, signal response is a
function of acid type and concentration.
Analytical Quality Control
Table XXI lists appropriate precision data based on the
analysis of duplicate samples. These results are consistent
with precision and accuracy ranges previously established
for this method. Data on recoveries and laboratory control
standards were not collected. The use of standard additions
provides points on the analytical working curve that are
in effect a measure of recovery.
TABLE XXI
Precision Based on the Analysis of Duplicates by Flameless AA
Element
Ag Silver
As Arsenic
Cd Cadmium
Pb Lead
Se Selemium
Cone. Range
(ppb)
*
1 - 10
0.2 - 0.7
2-25
Std. Dev. of
Diff. (ppb)
0.8
0.07
0.8
No. of
Determinations
10
6
12
* Insufficient Data
-72-
-------
B. Results and Discussion
Table XXII summarizes the ranges of metals found in the
water supplies covered by this study. The results reflect
the conformance of the finished drinking waters to the
proposed maximum allowable concentrations (6). One water
supply approaches the maximum suggested contamination level
for arsenic, and subsequent analytical data indicated that
this particular source was being polluted by supplemental
water originating from deep wells. In order to circumvent
potential problems, the mixing ratios of these two supplies
should be closely controlled or the use of the wells should
be discontinued , or the efficiency of the treatment plant
arsenic removal should be greatly increased.
-73-
-------
TABLE XXII
Metal Concentration Ranges In Drinking Water
Element
Ag Silver
As Arsenic
Ca Calcium
Cd Cadmium
Cr Chromium
Cu Copper
Fe Iron
K Potassium
Mg Magnesium
Mn Manganese
Na Sodium
Pb Lead
Se Selemium
Zn Zinc
Hardness, (Ca, Mg)
Concentration Range
Raw Water
<0. 0002-0. 0003
<0.001 - 0.010
5.2 - 135.0
<0. 0002-0. 012
<0. 005-0. 017
<0. 005-0. 20
<0. 02-3. 30
0.5-7.4
1.8-62.0
<0. 005-0. 76
1.1-77.0
<0. 002-0. 030
<0.005
<0. 005-0. 21
20-492
Finished Water
mg/1
<0. 0002-0. 0003
<0.001 - 0.050
4.9 - 108.0
<0. 0002-0. 0004
<0.005 - 0.006
43.005 - 0.20
<0.02 - 1.10
0.5 - 7.7
0.8 - 49.0
<0.005 - 0.35
1.0 - 91.0
<0.002 - 0.020
^0.005
<0.005 - 0.46
20-431
-74-
-------
6. Inorganic Parameters
a) Analytical Procedures
i) Ammonia - Technicon Co. method no. 154-71 W was modified
to analyze samples in the range 0-1 mg/1 P^-N. The method in-
volves a hypochlorite oxidation of an ammonia - phenol reaction
product using nitroprusside as a catalyst. The complexing reagent
and wash solutions were modified by the addition of 7.6 ml/1 of
10% NaOH and 1 ml/1 of concentrated sulfuric acid, respectively,
to compensate for the nutrient preservative.
ii) Alkalinity - Unaltered samples were titrated using an
automatic Fisher Titralyzer to an electrometrically determined
end-point of pH 4.5.
iii) Chloride - Technicon Co. method no. 9°-70 W was modified
to analyze samples in the range 0-200 mg/1 chloride by the addi-
tion of a twenty-five fold dilution loop. The method involves
the stoichiometric liberation of thiocyanate ion from mercuric
thiocyanate to form soluble but unionized mercuric chloride.
The free thiocyanate reacts with ferric ion to form ferric
thiocyanate proportional to the original chloride concentration.
iv) Chemical Oxygen Demand (COD) - The Central Regional
Laboratory semi-automated micro method was used to analyze the
drinking water samples for COD. Two and one-half ml of sample,
3.5 ml of sulfuric acid - silver sulfate solution and 2.5 ml of
potassium dichromate solution are added to 16 x ion mm borosili-
cate screw-top test tubes. The tubes are sealed with a teflon
-75-
-------
lined cap and then heated in an oven at 150°C for 2 hours.
The amount of Cr(III) produced by the oxidation of the
sample is proportional to the COO of the sample. The
appearance of Cr(III) is measured at 600 nm with Technicon
AA II equipment at 40 samples per hour. The method is
described in detail in Appendix II, which is a manuscript
that will appear in the July, 1975, issue of Analytical
Chemistry.
v) Cyanide - Technicon method no. 315-74W for cyanide
analysis was modified to improve sensitivity to lOOyg/1
full scale. The improvement was accomplished by addition
of a large diameter 13-turn coil to the manifold just be-
fore the colorimeter. The method involves an ultra-violet
digestion and distillation from acidic solution to separate
the cyanide from the sample matrix. Cyanide is converted
to cyanogen chloride by reaction with chloramine-T which
subsequently reacts with pyridine and barbituric acid to
give a red colored complex.
vi) Dissolved and Suspended Solids - The CRL micro
technique was used to' analyze the drinking water samples for
the residue parameters. Ten ml of sample were filtered
through a tared nuclepore filter and the residue weighed
to the nearest microgram to determine suspended solids. One
hundred microliters of filtrate was evaporated on 12 rm
aluminum pans and the residue weighed to the nearest inicro-
-76-
-------
gram to determine dissolved solids. A manuscript, submitted
for publication, describing the methods in detail is attached
as Appendix III.
vii) Fluoride - The EPA electrode method ("Manual of Methods
for Chemical Analysis of Water and Wastes", p. 65, 1974) for
fluoride was used without modification.
viii) Mercury - The CRL automated method was used for mercury
analysis. The method consists of a persulfate oxidation followed
by reduction with stannous chloride using hydroxylamine hydro-
chloride to reduce any residual chlorine present. The mercury
is detected by passing it through a 22 cm cell mounted in a
dual-wavelength spectrophotometer. A manuscript, submitted
for publication, describing the method is attached as Appendix
IV.
ix) Nitrate plus Nitrite - Technicon Co. method no. 100 -
70 W was modified by the addition of a 5 fold dilution loop
to analyze samples in the range of 0 - 5 mg/k NO 3 + NO;?-N.
In addition, the ammonium chloride buffer and wash solutions
were modified by adding 11.5 ml/1 of 102 NaOH and 1 ml/1 of
concentrated sulfuric acid, respectively, to compensate for
the nutrient preservative.. Nitrate plus nitrite is determined
by reducing the nitrate to nitrite with a copper-cadmium column.
The nitrite ion then reacts with sulfam'lamide at a low pH to
form a diazo compound. This compound then couples with N-l-
naph-thylethylene diamine dihydrochloride to form a reddish-
purple azo dye which is analyzed at 520 nm.
-77-
-------
x) Nitrite - Technicon method no. 102-70 X was used without
modification to analyze samples for nitrite. The analytical
method is the same as for nitrate plus nitrite except that the
copper-cadium column is deleted.
xi) pH - the pH of the drinking water samples was measured
with a pH meter equipped with a combination glass-reference
electrode.
xii) Phenolics - Technicon method no. 127 - 71 W for analysis
of phenolics was modified for samples in the range 0-200 mg/1.
The method involves the distillation of phenolics and the sub-
sequent reaction of the distillate with alkaline ferricyanide
and 4 - aminoantipyrene to form a red complex which is measured
at 505 nm.
xiii) Silica - Technicon Co. method no. 105 71 W was modified
by cutting the sample volume in half to analyze samples for
silica in the range 0-20 mg/1. This procedure for the deter-
mination of soluble silicates is based on the reduction of a
silicomolybdate complex in acidic solution to "molybdenum blue"
by ascorbic acid.
xiv) Specific Conductance - The specific conductivities were
measured with a Radiometer COM3 conductivity meter. The meter
is essentially an ohmmeter, calibrated in reciprocal ohms. A
built-in oscillator applies an ac voltage of suitable frequency
to the electrodes to avoid false readings from the polarization
of the solution.
-78-
-------
xv) Sulfate - Technicon Co. method no. 118-71 W was used
for sulfate analyses. The sample containing sulfate is passed
through a cation-exchange column to remove interferences and
then reacted with barium chloride and methylthymol blue. Barium
chloride and methylthymol blue are added in equal molar amounts
so the excess methylthymol blue corresponds to the sulfate con-
centration.
xvi) Total Phosphorus and Kjeldahl Nitrogen - The CRL methods
were used for the analysis of TP and TKN. Ten ml of samole were
mixed with 2 ml of the solution described in sections 6.2 and 6.3
of the 1974 EPA Methods Manual for TKN.^ The solution was
evaporated and then digested at 370°C for 1/2 hour. The digestate
was cooled and then diluted to 10 ml with distilled water. The
resulting solution was analyzed for phosphorus by Technicon Co.
method no. 155 - 71 W modified as follows: Five grams per liter
of sodium chloride was added to the manifold water line to com-
plex the mercury catalyst and avoid its reduction. Nitrogen
was analyzed as ammonia by the method described in paragraoh 1.
In addition, a five-fold dilution loop with 25 ml of 10 N NaOH
per liter was used for both methods. The sampler wash solution
consisted of 35 ml of concentrated sulfuric acid per liter. A
manuscript describing these methods in detail is being prepared.
-79-
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Quality Assurance Procedures for Inorganic Parameters.
The accuracy and precision of the analytical data were assessed
by the use of daily instrument calibration and the analyses of duplicate
samples and intralaboratory quality control standards. The precision
and detection limit data in Table XXILIshow that all of the methods
used (with the exception of phenolics) are much more sensitive than
necessary when compared to the drinking water quality standards (Table XXIII),
SUMMARY
The Region V Drinking Water Study has satisfied most of the goals
of the project. It has provided the most complete list of parameter
concentration values yet reported for so large a group of water supplies.
These values were from samples collected approximately two months after
. (6)
the Safe Drinking Water Act became law and therefore they can be used
as baseline concentrations from which the effects of the Act can be
measured. The study clearly supports the conclusion drawn by Bellar &
2
Lichtenberg that the chlorination water treatment process produces
chloroform in finished drinking waters. It also provides experimental
evidence of the absence of most pesticides in our drinking water sup-
plies and where these compounds are present the concentrations are very
low. It showed that the waters at Evansville, Indiana are not now as
contaminated as they were a few years ago. Because we expect these
results to be used for a long period of time and to be rigorously
evaluated, we have made available a very limited number of copies of
all data. Appendix V is a complete listing of the field sheets as
they were received and Appendix VI is a complete set of analytical
results. Generally these appendices will not accompany this report.
-80-
-------
TABLE XXIII--
SUMMARY OF QUALITY ASSURANCE DATA
FOR INORGANIC PARAMETERS51
PARAMETER
Ammonia - N
Alkalinity - CaC03
Chloride
Chemical Oxygen Demand
Cyanide
Dissolved Solids
Fluoride
Mercury
Nitrate & Nitrite - N
Nitrite - N
pH
Phenol ics
Silica
Specific Conductance
Sulfate
Suspended Solids
Total Phosphorus - P
Total Kjeldahl Nitrogen - N
PRECISION0
0.0061
0.9
1.0
1.4
0.0010
19.8
0.025
0.00005
0.019
0.0007
0.04
0.0003
0.07
2.3
1.0
1.7
0.006
0.037
DETECTION LIMIT0
0.010
10
2
3
0.002
40
0.1
0.0001
0.03
0.005
0.1
0.002
0.1
5
3
2
0.02
a 05
a. Expressed as mg/1, except pH (units) and specific conductance
(micro Siemens, us).
b. Precision was determined from the estimated standard deviations of
f 2
twenty-two duplicate samples for each parameter. T est=KAL™L)
c. Detection limits were calculated as two times the standard deviation
of the blank results.
-81-
-------
REFERENCES
1. Thomas A. Bellar and James J. Lichtenberg, "The Determination of
Volatile Organic Compounds at theug/1 Level in Water by Gas
Chromatography", EPA-670/4-74-009, November, 1974, National
Environmental Research Center, Office of Research and Oevelopment3
Cincinnati, Ohio 45268.
2. Thomas A. Bellar, James J. Lichtenberg, and Robert C. Kroner,
"The Occurrence of Organohalides in Chlorinated Drinking Waters"
EPA-670/4-74-008.
3. "Manual of Methods for Chemical Analysis of Water and Wastes"
EPA-625/6-74-003 (1974).
4. Robert Kleopfer, US-EPA, Region VII, 25 Funston Road, Kansas City,
Missouri 56115, Private Communications.
5. "Methods for Organic Pesticides in Water and Wastewater",
Environmental Protection Agency, National Environmental Research
Center, Cincinnati, Ohio 45268.
6. (a) "Safe Drinking Water Act", Public Law 93-523, 93rd Congress,
S, 433, December 16, 1974; (b) Primary Drinking Water Proposed
Interim Standards, Federal Register, 40 CFR Part 141, No. 51,
March 14, 1975.
7. "Public Health Service Drinking Water Standards - Revised 1962"
U.S. Department of Health, Education and Welfare - Public Health Service.
8. "Water Quality Criteria - 1972" EPA-R3-73-033 (March 1973)
82
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APPENDIX I
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
CENTRAL REGJ^.AL LABORATORY
SUBJECT-. Preservation and Holding Times foi Nutrient DATE: October 9, 1974
and Demand Parameters
FROM: Dr. Mark Carter, Chief
Inorganic Section, CRL
TO: Dwight BaTlinger, Director
HDQARL
ROUGH: Billy Fair!ess, Chief, Chemistry Branch, CRL
Thomas E. Yeates, Director, CRL
David A. Payne, Chief, Quality Assurance Branch, CRL
The recommended sample holding times to be appearing in the next edition
of "Methods for Chemical Analysis of Water and Wastes," for some nutrient
and demand parameters, have caused great concern in Region V. The
Surveillance and Analysis Division has been preserving surface and waste-
waters with 1 ml H-pSQ^/l of sample for ammonia, nitrate plus nitrite,
total Kjeldahl nitrogen (TKN), total phosphorus, chemical oxygen demand
(COD), and total organic carbon (TOC) parameters since early 1973. All
samples to be analyzed for the above parameters are shipped via ground
transportation to the Central Regional Laboratory (CRL) in Chicago while
maintained.at.ambient temperature. In only a few cases have samples been
analyzed within tne 24 hour holding time you are recommending fcr the
above parameters. Typically, the holding times for sulfuric acid pre-
served samples have ranged from several days to approximately one month
from the time of sample collection.
The CRL has been actively investigating the preservation of samples since
January of this year. Although our results are preliminary we feel com-
pelled to release uhe data now before critically important administrative
decisions are being made. Our conclusions and recommendations which
follow are based on the sample types studied. All the data we have col-
lected are included in Attachment A.
Conclusions:
1) On the basis of our work, and data in the literature
(Howe and Holley, 1969; Charpiot, 1969; Oenkins, 1965)
we find no support for your recommended 24 hour holding
time for ammonia, nitrate plus nitrite, Kjeldahl nitrogen,
total phosphorus, and total organic carbon.
2) The recotmended holding time for TOC (24 hours) is incon-
sistent with the 7 day holding time for chemical oxygen
demand. Since the COD method inherently takes into
account the oxidation state of a waste, any sample insta-
bility will be reflected in the COD before the TOC. In
EPA F«»m 1320-4 (Re». 6.72)
-------
- 2 -
addition, on the basis of our experimental results the
recommended holding time of 7 days for COO measurement
is unnecessarily stringent.
3) The recommendation of one holding time for each para-
meter for all sample types is unnecessarily cautious.
Howe and Holley (1969) have shown that the greatest
cause of sample instability is biological activity.
Our work has verified this observation. The data in
Attachment A shov/s a tremendous difference in stability
between samples of high biological activity (raw sewage)
and lev/ activity (clean surface water).
Interm Recommendations For Holding Times
In all cases, the samples are assumed to be stored at room temperature.
As of yet, we have not found 2 ml/1(sulfuric acid / sample)to be any
more effective than 1 ml/1 so the latter procedure is also assumed.
1) Ammonia - At least one v/eek for raw sewage and one month
for surface waters and industrial wastes low in biologi-
cal activity.
2) Nitrate plus Nitrite - At least one month for all sample
types.
3} Total KJeldahl Nitrogen - At least one month for raw
sewage. For organic nitrogen follow ammonia recommenda-
tions.
4) Total and Dissolved Phosphorus - Up to two months for all
sample types.
5) COO/TOC - At least two v/eeks for raw sewage.
These holding times are based on preliminary data and are subject to modi-
fication pending the completion of one more study. However, they are sup-
ported by data from the literature and are much longer than yours. We
request that you make available to us any analytical data or literature
references that support your recommendations and hence contradict our
results. We believe our preliminary data are accurate and that our
interm recommendations outlined above should be accepted in Region V
pending further work. We would be most happy to have your input into
our one remaining preservation study and hope to discuss this matter
with members of the Quality Assurance evaluation team during the visit
to the CRL on October 15.
-------
- 3 -
Mark Carter, Ph.D
-------
APPENDIX II
-------
Central Regional Laboratory
Environmental Protection Agency
Chicago, Illinois 60609
11-8-14-
MICRO SEMI-AUTOMATED ANALYSIS OF SURFACE AND WASTEWATERS
FOR CHEMICAL OXYGEN DEMAND
PRELIMINARY
SUBJECT TO REVISION
Andrea M. Jirka and Mark J. Carter
*Author to whom correspondence should be addressed.
-------
BRIEF
A micro semi-automated spectrophotometric method for determining the
chemical oxygen demand of surface and wastewaters is described and
compared to the standard method.
'ABSTRACT
A micro sample digestion technique for the determination of chemical
oxygen demand (COO) is described. An automated spectrophotometric
measurement of the appearance of chromium (III) after sample digestion
completes the method. Adequate sensitivity at 600 nm is achieved by
using a 50 mm flowcell to measure COD values in the range 3-900 mg/1.
The semi-automated method is compared to the standard method with
respect to precision, accuracy, ease of analysis and comparability of
data.
-------
- 2 -
INTRODUCTION
The oxidation of organic and inorganic wastes in a receiv-
ing water depletes the dissolved oxygen supply, which can have
a profound effect on aquatic life (1). A meaningful determina-
tion of the natural oxygen demand of wastewaters has been a
problem since the previous century. The biochemical oxygen
demand (BOO) test was developed to measure the natural oxygen
demand of wastes under laboratory conditions similar to those
found in receiving waters (2-4). The advantage of the BOD test
1s that it is a good indicate/ of the bid-degradcbility of a
waste. The major disadvantages of the BOD test are the long
time required for analysis, the poor precision and the indeter-
minable accuracy of the method (4,5).
In order to substantially reduce the time required to esti-
mate the ultimate oxygen demand of a wastewater, the chemical
oxygen demand (COO) test was developed (6). The addition of
silver sulfate (7, 8) and mercuric sulfate (9) to the acidic
dichromate digestion solution, increased the readability of the
COD test (10, 11). However, since chemical oxidation does not
differentiate between biologically stable and unstable wastes, a
correlation between COD and 300 values must be developed for
each sample type (12). •
Stenger and Van Hall reported a very rapid method for measur-
ing the total organic carbon (TOC) content of water samples, which •
-------
- 3 -
4
can be related to oxygen demand (13). However, the advantage
1n being able to rapidly determine TOC values is offset by the
high initial equipment cost. In addition, the informational
content of the TOC analysis is less useful than that gained
from the BOO or COD methods (14). The TOC test does not dif-
ferentiate between compounds with the same number of carbon
atoms, but which are in different stages of oxidation and hence
have different oxygen demanding potentials. Since the COD and
BOD tests measure the amount of oxygen required to stabilize
waste sample's, their values inherently reflect the original
oxidation state of the chemical pollutants.
*
The standard COD test (4) is widely used because it pro-
vides a good balance between the value of the information gained
and the speed of analysis when compared to the BOD and TOC tests
(12). However, the standard method for determining COD has
limitations which are not inherent in the concept of the test.
The back-titration of dichromate after sample digestion is an
insensitive method of detection. This lack of method sensitiv-
ity has been partially alleviated by using two different concen-
trations of dichromate and a relatively large sample volume. In
addition, the consumption of large quantities of expensive rea-
gents, the extensive bench space requirement of the COD hot plates
which limits the number of analyses that can be performed in a
day, and the difficulty of disposing of Urge quantities of highly
acidic mercury, silver and chromium wastes, are serious problems
for most industrial laboratories (15).
-------
. 4 -
Recently, there has been considerable interest in simpli-
fying the rather tedious standard COO method (16-19). Unfortun-
ately, procedures using a much shortened digestion period or
*
lower digestion temperatures produce results equivalent to those
obtained by the standard method only for very readily oxidized
wastewaters (20-22).
Bloor (23) and Johnson (24) determined the organic content
of biological materials using dichromate as an oxidant and then
measuring the excess dichrcmate spectrophotometrically. This
procedure eliminated the tedious detection procedure of the stand-
4
ard method. The spectrophotometrfc procedure has been applied to
the analysis of water samples in which the COD was determined by
measuring the appearance of Cr (III) after manual digestion (25-27)
Several COD methods which use a spectrophotornetric means of
detection and automated sample digestion have also been reported.
Sample digestion was accomplished using a continuous digestor (28,
29) or high temperature bath (30-32). However, lift and Cain
reported data which show that these automated procedures do not
produce results equivalent to the standard method for all sample
types (33). The incomparability of data was attributed to incom-
plete sample oxidation caused by the short digestion times in the
automated methods. In addition, the higher concentration of sul-
furic acid used in most automated systems requires a smaller
amount of mercuric sulfate be used to avoid its precipitation in
-------
- 5 -
the sample lines and flowcell, The lesser amount of mercuric
sulfate caused chloride to be more of an interference in these
automated methods than in the standard method,
The method reported here combines the advantages of the
reliability of the standard digestion procedure (4), with the
superior sensitivity and precision of an automated procedure
based on the spectrcphotcmetric measurement of Cr (III) (27).
Use of the resultant micro semi-automated COO method has
Increased the productivity of this laboratory three-fold and
reduced the consumption of very expensive reagents and the
quantities of wastes twenty-fold.
EXPERIMENTAL
Apparatus. Samples were digested in Corning #9949 15x100
mm screwcap (cap #9998) culture tubes. Spectrophotometric measure-
ments were made with the apparatus shown schematically in Figure 1.
The automated system was fabricated using Technicon Corporation
AutoAnalyzer II equipment consisting of a Sampler IV, Pump III,
Colorimeter II, Recorder II, and single channel Digital Printer.
The colorimeter was used in the direct mode and equipped with 600
nm interference filters and 50 mm flowcells. The Standard Calibrra-
tion control was set at 228 to attain 1000 mg/1 COO full scale on
the recorder, A glass capillary was used as a sample probe. The
sampler was operated at 40 samples/hr with a 3:1, sample to wash
ratio.
-------
- 6 -
Wastewater samples with particulate matter-were blended
with a Teckmar Model SOT homogenizer before taking an aliquot
fop analysis. An adjustable 0-5 ml Oxford pipette with dis-
posable polypropylene tips was used for aliquoting samples and
addition of reagents.
Reagents. Unless otherwise noted, all chemicals were ACS
reagent grade. All reagent water was de-ionized and distilled.
Digestion solution was prepared by adding 10.216 g of
K2Cr207 (dried at 105° C), 167 ml of cone H2S04 and 33.3 g of
HgS04 to 500 ml of water and. diluting the cooled solution to
1 1.
Catalyst solution was prepared by dissolving 22 g of Ag2S04
in a 9-lb bottle of cone H2S04.
Sampler wash solution was 50% sulfuric acid by volurne.
A stock potassium acid phthalate solution, equivalent to
10 g/1 COD, was prepared by dissolving 8.500 g of a dried portion
Of NBS standard reference material 84 h in water and diluting to
1 1. Working standards of 25, 50, 75, 100, 250, 500 and 750 mg/1
COO were prepared by diluting 2.5, 5, 7.5, 10, 25, 50 and 75 ml
of stock solution to 1 1, respectively.
Procedures. It was necessary to wash all culture tubes and
screw caps with 202 H2S04 before their first use to prevent random
contamination.
Digestion was carried out by placing 2.5 ml of sample and 1.5
sil of digestion solution in a culture tube. Three and one half ml
-------
- 7 -
'of catalyst solution were added carefully down the side of the
culture tube so that the acid formed a layer on the bottom.
The tube was capped tightly and then shaken to mix the layers.
Two blanks and a set of standards were prepared in the same
manner and analyzed with each sample set.
All samples, blanks and standards were heated in an oven
at 150° C, which is the observed reflux temperature of 50% sul-
furic acid. After two hours the tubes were removed from the
oven, cooled, and placed in the Sampler IV tray.
The analytical manifold and reagents were set up as indi-
cated in Figure 1, Two digested blanks were analyzed at the
beginning of each sample set to zero the baseline. A mid-scale
standard was used to calibrate the recorder and printer (34).
Standards were rerun periodically during the course of an ana-
lysis run to assure that the system remained in calibration.
The COD value of unknown samples v/as obtained by direct print-
out. A typical recorder trace for standards is shown in Figure 2.
RESULTS AND DISCUSSION
Sample Digestion. It has been shown that COD procedures
using a shortened digestion period and/or a reduced digestion
temperature do not attain the same degree of sample oxidation as
the standard method (20-22, 33). Any alternate test procedure
used to analyze wastewaters for COD must produce results equiva-
lent to or better than the current standard method (35). There-
fora, to insure data comparability the temperature and length of
-------
- 8 -
.sample digestion and concentration of reagents used in the
standard method were adopted for use in the semi-automated
procedure described here (4),
Since the micro colorimetric detection technique required
only 2 ml of digested sample the quantities of sample and rea-
gents used were reduced twenty-fold in comparison to the
standard method (4, 11). Use of the standard COO digestion
apparatus was eliminated and instead all samples, blanks and
standards were digested in small screw-cap culture tubes. The
potential for sample contamination from large glass surfaces
was consequently reduced.
Screw caps with phenolic resin liners were found to be
unacceptable since they were attacked by the digestion solution
giving erroneously high COD values. Teflon-lined caps greatly
reduced this problem especially if each cap was used only onca.
Any sample tube which leaked, as evidenced by a black residue
on ths outside of the tube, -was discarded.
Uniform addition of reagents and improved precision was
achieved by dissolving all chemicals in one of two solutions.
The catalyst solution was prepared by the standard method (4).
The oxidizing solution v/as prepared by combining potassium
dichromate with mercuric sulfate and making the solution 5 N
With sulfuric acid to solubilizs the mercury salt. However,
the mercuric sulfate .-/as not ccmpletsly soluble in the cooled,
combined reaction mixture. Ths height of :ha sampler probe
-------
- 9 -
was carefully -adjusted so as to avoid aspirating the precipitate.
Otherwise, aspiration of the particulate matter caused severe
baseline noise.
Spectrophotometric Analysis. The COD of wastewater samples
has been determined spectrophotornetrically, after digestion, by
measuring the decrease in Cr (VI) concentration at 352 (32) or
440 nm (19). Alternatively, the increase in Cr (III) concentra-
tionhas been measured at 600 (27) or 650 nm (25). All of these
authors found the Spectrophotometric procedure to be easier to
perform than the manual titration.
Molov and Zaleiko showed that better sensitivity could be
achieved by measuring the decrease in Cr (V!) concentration than
the increase in Cr (III) concentration (28). However, the preci-
sion of.,a method based on measuring the decrease in Cr (VI) absorb-
ance is very dependent on the reproducibility of reagent addition.
This problem was avoided and adequate sensitivity achieved by
measuring the appearance of Cr (II!) at 6GO mm, using a 50 mm
flowcell, and the scale expansion capability of the Technicon
colorimeter.
In order to increase the sensitivity of the standard method,
two different concentrations of oxidizing reagent are co.raonly
used, These correspond to tv/o levels of CCO measurement, 5-50
ing/1 and 50-3CO ~g/l (11). «!core and Walker found that the
working range cf the low level modification was limited by the
diminished oxidation potaniial of the digestion solution after
505 of the dichromata was consumed (36).
-------
- 10 -
Due to the adequate sensitivity of the spectrophotometric
semi-automated method, only one set of reagent concentrations
was necessary to cover both levels of the standard method. In
order to test the linearity of the semi-automated method, .
standards between 500 and 1000 mg/1 COD were analyzed in incre-
ments of 25 mg/1. Potassium hydrogen phthalate was chosen for
use as a standard because of its stability in solution and its
complete oxidation under the conditions of the COD test (4).
The results, presented in Figure 3, show the colorimetric method
to.be linear up to 900 mg/1 COD.
Due to the use of 50% sulfuric acid, the original automated
manifold was constructed with acidflex tubing. However, the
system exhibited very poor hydralic characteristics. This problem
was alev.iatsd by replacing the acidflex tubes with tygon pump
and transmission tubing. The recorder trace in Figure 2 was
undamped. The entire system was cleaned for about 1/2 hour before
first use with 5Q£ sulfuric acid to prevent severe baseline drift
due to Teachable organic matter. Also 1:1 dilution loop was added
to the system to reduce tha viscosity cf the sample stream so that
proper debubbling occurred in the flcwcell.
Precision, Acc'jr^cy and Detection Limit. Since it was dif-
ficult to corract the semi-autcrcated results for r.he sirall baseline
drift, the working detection limit was defined as the mean bias of
the blank plus :v/o standard deviations. Eleven blank samples
were analyzed to detamina the detection limit. The mean value
-------
-11 -
'obtained was 1 mg/1 with a standard deviation of 0.8 mg/1 COD.
These values were used to define the detection limit at 3 mg/1
COD. This number compares quite favorably with the detection
limit of 5 mg/1 COD reported by Moore and Walker for the Tow
level standard COD method (36).
The relative precision of both modifications of the stand-
ard and the semi-automated COD methods was determined by perform-
ing replicate analyzes on four wastewater samples. Since the
standard and semi-automated determinations were performed at
different times, two similar sets of water samples were chosen
so that the relative standard deviations could be meaningfully
compared. The relative standard deviations of both methods for
low COD concentrations, as shown in Table I, compare very closely.
However, the precision of the semi-automated method at high COD
concentrations was approximately seven times better than the
standard method.
Adelman pointed out that one of the factors contributing to
the poor precision of the standard method was the potential loss
of volatile components of the wastewater samples (30). This can
be caused by the heat generated by the mixing of the sample with
the concentrated acid prior to reflux or during the reflux step.
This problem was eliminated in the semi-automated procedure by
avoiding mixing the sample and acid layers until the tube is
capped and the fact that sample digestion occurs in a completely
closed system.
-------
- 12 -
The authors found that the ability to take-a representative
aliquot of a nonhomogeneous sample was the limiting component of
analysis variability regardless of method. Precision data for
the standard COD method determined from inter-laboratory analyses
of standard-like solutions must be regarded only as a lower limit
(5, 37).
The accuracy of the semi-automated method was determined by
measuring the recovery of standard addition of potassium hydrogen
phthalate to several types of water samples." The mean recovery
from 14 water and wastewater samples, shown in Table II, was 101%
with a standard deviation of 4*.
Comparison of Semi-Automated and Standard Methods. A variety of
surface and wastewater samples were analyzed by both the standard
and semi-automated COO methods to determine the comparability of
data. These samples included raw and treated sewage, industrial,
chemical and food process wastes. Results comparing the two methods
are shown in Table III. Initially the largest discrepancies between
methods occurred in samples which contained large quantities of
particulate matter, e.g., raw sewage. Homogenizing samples of
this type greatly improved the comparability of the data. Within
the standard deviation of the mean ratio of results, no significant
bias in COO values exists between methods.
In addition, several pure organic compounds were analyzed to
determine if the semi-automated method achieved a more complete
-------
- 13 -
digestion than the standard method. The experimental results
and calculated maximum theoretical COD values are shown in
Table IV. The semi-automated values were slightly higher than
the standard method results indicating that the former method
achieved a more complete sample digestion. The difference
could also be due to the fact that no volatile material can
excape from the sealed tubes during oxidation in the semi-auto-
mated method, while in the standard method, volatile material
may escape before sample oxidation is complete.
' 'Interferences. One of the major problems encountered in
other automated COD methods is the inability of the techniques
•
to compensate for the positive interference caused by the oxida-
tion of chloride present in wastewater samples (28-32). The
standard procedure for eliminating the chloride interference is
*
the addition of mercuric sulfate to form a complex and prevent
Its oxidation {4, 9). Experiments performed by this laboratory
indicate that no interference results up to 2000 mg/1 chloride
'when the standard procedure is used (9).
In other automated techniques, the high acid concentration
reduces the solubility of HgSQ4 so that the quantity of Hg(II)
1n solution is not sufficient to complex the same amount of
chloride as in the standard method (23-32),
In the semi-automated COD method, the ratio of HgS04 to
sample volume is identical to the standard method. Standards of
500 mg/1 CCD were spiked with varying amounts of chloride in
-------
- 14 -
order to determine the limiting concentration at which the inter-
ference was significant. The results, shown in Figure 4, indi-
cate that chloride does not interfere below 1000 rag/1. Above
this concentration, some precipitation occurs when the dilution
water combines with the sample stream in the automated system,
which results in a noisy recorder trace. If it is necessary to
routinely analyze samples containing between 1000 and 2000 mg/1
chloride, the dilution loop can be removed. Air spikes will then
appear at the beginning and end of each sample peak, due to
improper debubbling, but the results are not affected.
Any chemical species remaining after sample digestion, which
absorb at 600 nm, cause a positive interference in the semi-auto-
mated method. Since almost all organic matter is digested by the
COD technique the possible interference from organic compounds
was not considered (6, 8, 36).
The presence of Cr (III) in a water sample gives an apparent
COD of 1.39 times the concentration of chromium. Also, a potential
Interference from iron was investigated by spiking standards of
500 mg/1 COO with increasing amounts of ferric iron. The results,
presented in Figure 5, show no apparent COO below 5 g/1 Fe. The
positive bias caused by high concentrations of interfering sub-
stances is routinely eliminated by diluting samples prior to
analysis or correcting the reported COO values from independent
determinations of chromium, iron and chloride.
-------
- 15 -
''ACKNOWLEDGEMENT
The authors would like to thank B. J. Fair!ess and
D, A. Payne for their helpful comments during the course of
this work and their critical review of the manuscript.
.The mention of trade names or commercial products does
not constitute endorsement or recommendation for use by the
Central Regional Laboratory or the Environmental Protection
Agency.
-------
- 16 -
REFERENCES
(1) "Water Quality Criteria," Federal Water Pollution Control
Administration, Washington, D. C. ,1968, pp 32-5.
(2) E. B. Phelps, "Stream Sanitation," John Wiley and Sons,
New York, N. Y., 1944, pp 65-6.
(3) E. J. Theriault, Public Health Bulletin No. 173, U.S.
Public Health Service, Washington, 0. C., 1927.
(4) "Standard Methods for the Examination of Water and Waste-
water," 13th ed., American Public Health Association,
New York, N. Y., 1971, P4 489.
(5) D. G. Ballinger and R. J. Lishka, J_. Water Pollut. Contr.
''Fed.., • 3£, 470 (1962).
(6) W. A. Moore, R. C. Kroner and C. C. Ruchhoft, Anal. Chem.,
•21, 953 (1949).
(7) M. H. Muers, J. Soc. Chenu'Ind.. 55_, 71T (1936).
(8) W. A. Moore, F. J. Ludzack and C. C. Ruchhoft, Anal. Chem.,
' 23, 1297 (1951).
(9) R. A. Dobbs and R. T. Williams, Anal. Chem., 35_, 1064 (1963),
(10) "Water and Atmospheric Analysis," Annual Book of Standards,
Part 23, American Society for Testing and Materials,
Philadelphia, Penn., 1973.
(11) "Methods for Chemical Analysis of Water and Wastes,"
Environmental Protection Agency, Cincinnati, Ohio, 1971,
pp 17-23,
-------
- 17 -
(12) "Handbook for Monitoring Industrial Wastewater,"
?
Environmental Protection Agency, Wash., D. C., 1973.
(13) V. A. Stenger and C.E. Van Hall, Anal. Chem., 3_9, 206
(1967).
(14) C. Geisler, J. F. Andrews and G. Schierjott, Water and
'Wastes Eng., H, 26 (1974).
(15) "R. B. Dean, R. T. Williams and R. H. Wise, Environ. Sci.
Techno!, 5_, 1044 (1971).
(16) A. F. Westerhold, The Digestor, 2£, 4 (1965).
(17) 'Ibid., 22., 18 (1965),
(18) J. S. Jens, Water and Wastes Eng., 4_, 89 (1967).
*
(19) T. K. Wu, Michigan Department of Natural Resources Laboratory,
Lansing, Michigan, private communication, 1974.
(20) J. M. Foulds and J. V. Lunsford, Water'and Sewage Works, 115,
112 (1963).
(21) W. N. Wells, Water and Sewage Works. 117, 123 (1970).
(22) L. E. Shriver and J. C. Young, J_. Water Pollut. Contr. Fed.,
•44, 2140 (1972).
(23) W. R. Bloor, £. Sicl. Chem., 77_, 53 (1928).
(24) M. J. Johnson, J. Bfol. Chem., 181, 707 (1949).
(25) R. R. McNary, M. H. Dougherty and R. W. Wolford, Sewage and
'Industrial Wastes, 29_, 894 (1957).
(26) N. Chaudhuri, S. Niyogi, A. De and A. 3asu, J. 'Water Pollut.
r. Fed., 45_, 537 (1973).
-------
- 18 -
(27) A, F. -Gaudy and M. Ramanathan. J^ jjater Pollut. Contr. .Fed.,
36, 1479 (1964).
(28) A. H. Molof and N. S. Zaleiko, 19th Purdue Industrial Waste
Conference, Lafayette» Ind., May, 1964.
(29) J. H. Ickes, E. A. Gray, N. S. Zaleiko and M. H. Adelman in
"Automation in Analytical Chemistry, Technicon Symposia
1967," Mediad Inc., Tarrytown, N. Y., 1968.
(30) M. H. Adelman, 18th Pittsburgh Conference on Analytical
Chemistry and Applied Spectroscopy, Pittsburgh, Pennsylvania,
March, 1967.
(31) M, H. Adelman in "Automation in Analytical Chemistry,
Technicon Symposia 1965," Mediad Inc., Tarrytown, N. Y.,
1966.
(32) "Industrial Method No. 137-71W," Technicon Instruments Corp.,
Tarrytown, N. Y., 1973.
(33) E. C. Tifft and B. E.'.Cain in "Automation in Analytical
Chemistry, Technicon Symposia 1972," Mediad Inc., Tarrytown,
N. Y., 1973.
.»**
(34) "Technicon Operation Manual," Technicon Instruments Corp.,
Tarrytown, N. Y., 1973.
(35) federal Register, 38. 28759 (1973).
(36) W. A. Moore and W. W. Walker, Anal.'Chem.. 28, 167 (1956).
(37) J. A. Winter, "Method Research Study 3, Demand Analyses,"
Environmental Protection Agency, Cincinnati, Ohio, 1971.
-------
TABLE I, COMPARISON OF THE PRECISION OF THE SEMI-AUTOMATED
AND STANDARD CHEMICAL toGEN DEMAND I'IETHODS
SEMI-
METHOD SAMPUE
•
IPUE N:
1
2
3
4
.. Nb, OF
), DETNS,
n
10
n
10
la
MEAN .
40
230
26
270
in/ f r
RANGE
4
90
4
12
!G/!^
STD,' DEV,
L4
28,0
1,3
4','6
REL,' :
DEV,
3,5
12,2
5VO
1,7
-------
TABLE II, RECOVERIES OF POTASSIUM HYDROGEN PHTHALATE ADDED
TO MUTER SAMPLES WITH SEMi-AtrraHATED METHOD
SAMPLE SOURCE SAMPLE KHP ADDED SAMPLE +KHP RECOVERY,
•
ORGANICS INDUSTRY 13 200 217 102
RAWFSEWAGE 164 200 ' 370 1D3
RIVER KATER 31 . 100 122 91
HARBOR WATER 16 200 224 * 11)4
INDUSTRIAL COOLING 65 200 262 99
WATER
RIVER WATER 15 100 116 101
RIVER HATER 28 ' 100 '124 96
CHANNEL HATER 52 100 ' 152 100
NEAR DREDGING '
INDUSTRIAL DISCHARGE 30 100 131 IDl
INDUSTRIAL DISCHARGE 15 100 116 100
TREATED SEWAGE 40 100 .' 144 104
RECEIVING WATER 25 100 127 102
OF -SEWAGE
TREATED SEWAGE 14 103 124 110
STEEL MILL EFFLUENT 14 100. 112 98
MEAN ' 101
STANDARD DEVIATION • 4
-------
TABLE III, COMPARISON OF SEMI-/VTC.WED AI-O STANDARD
CHEMICAL OXYGEN DEMAND '
SOURCE
RAW SB'^AGE
PAPER MILL COOLING
WATER
STEEL MILL WASTE
TREATED SEWAGE
PRIMARY TREATED
SEWAGE
BOILER BLOVJDOWN
POTTERY SHOP WASTE
CREEK DOWNSTREAM
FROM POTTERY SHOP
PRIMARY TREATED
SEWAGE
PAPER MILL WASTE
RAW SEWAGE.
TREATED SB,'AGE
TREATED SEWAGE
TREATED SB-AGE
ORGANIC CHEMICAL
PLANT WASTE
STEEL MILL V-^STE
*•'... ,*«..» .(*. ... ftf M . •-
frnn i .
STANDARD KETHOD
(S)
420
39
270
50
63
180
140
94
SO
450
170
36
27
21
270
[/r,n
SEMI-/VTOMATED
{'lEOlOD (AT
421
46
273
51
t-i
p.i •
133
156
. 99
87
464
164
35
27
22
275
S/A
XJOO
99,8
.84', 8
98.9
98,0
1Z3'.V
•^•'"i
89J
94','9
103,4
97,0
103,7
102','9
103,0
95V5
98',2
'-c
STATCARD D?/IATICN
A RESULT REJECTED pen CALCULATION OF
AMD STA
CC-/IATICN,
-------
TABLE IV, COMPARISON OF CHEMICAI, OXYGEN DEMAND
. METHODS ON ORGANIC COMPOUNDS
COMPOUND
fViENOL
SODIUM ACETATE
ACETONE
ETHANOL
DEXTROSE
OXALIC ACID
SODIUM CITRATE
GLUTAMIC ACID
GLYCINE
BENZOIC ACID
PYRIDINE
3-PlCOLlNE
TETRAHYDROFURAN
LCOD/ , W3/1 •
THEORETICAL
238
470
221
197
107
150
127
490
98
64
197
223
239
244
STANDARD [-IETHOD
(S)
.230
450
200
170
103
130
120
470
90
60
190
<5
64
250
SEMI -AUTOMATED S/A
METHOD (A) X 100
240
462
207
180
115
139
128
496
98
62
202
•<3
77
242
95,8
97','4
96,6
94,4
88',8
93,5
93,8
94'.'8
91,8
96,8
94J
:•• A
83',1A
i03',3
95,0
3',5
STANDARD BP/IATION
RESULTS REJECTED FOR CALCULATION OF ^^EAN AND STANDARD DEVIATION,
-------
TITLES FOR FIGURES,
FIGURE 1, AUTOMATED SYSTEM FOR CHEMICAL OXYGEN DEMAND, NUMBERS IN
PARENTHESES CORRESPOND TO THE FLO1,-/ RATE OF THE PUMPTUBES
IN ML/MINI NUMBERS ADJACENT TO GLASS COILS AND FITTINGS
ARE TECHNICON CORP, PART NUMBERS, •
FIGURE 2, RECORDER TRACE FOR CHEMICAL OXYGEN DEMAND OF POTASSIUM
HYDROGEN PHTHALATE STANDARDS ANALYZED IN DUPLICATE,
FIGURE 3, CALIBRATION CURVE FOR AUTOMATED CHEMICAL OXYGEN DEMAND,
EACH POINT IS THE AVERAGE OF DUPLICATE DETERMINATIONS,
FIGURE 4, PLOT OF APPARENT CHEMICAL OXYGEN DEMAND CAUSED BY THE
OXIDATION OF CHLORIDE, DATA DETERMINED BY ADDING THE
INDICATED AMOUNTS OF CHLORIDE TO A SCO MG/L COD POTASSIUM
HYDROGEN PH7KALATE STANDARD,
_«• . • • •
FIGURE 5, PLOT OF APPARENT CHEMICAL OXYGEN DEMAND CAUSED BY THE
ABSORBANCE AT 600 NM FRQM FERRIC IRON IN SOLUTION, DATA
DETERMINED EY ADDING THE'INDICATED AMOUNTS OF IRON TO A
500 MG/L COD POTASSIUM HYDROGEN PHTHALATE STANDARD,
-------
o.
e
00
IN
O
ft.
I
O
o
o
I
o
< :s
in
-2
C,
v>
o"
"-> O
«
(H *J
4) CU
—, o
C. O
e 4>
a c£
to ^
O ~>n
i
c
o
n
o
ci
i
n
00
4)
K
O
I
•O
ZU «
1/1
«
ce.
at
Oi
O
cj
UJ
a;
01
z
-------
-------
ABSORBANCE, O.D.
a
«*»
-------
[COD] ,mg/i
1*0
CO
CO
CTQ
CD
CD
CD
CD
cr>
CD
CO
CD
CD
-------
Central Regional Laboratory
Environmental Protection Agency
Chicago, Illinois 60609
n-%-14-
MICRO SEMI-AUTOMATED ANALYSIS OF SURFACE AND WASTEWATERS
FOR CHEMICAL OXYGEN DEMAND
PRELIMINARY
SUBJECT TO REVISION
*
Andrea M. Jirka and Mark J, Carter
*Author to whom correspondence should be addressed.
-------
BRIEF
A micro semi-automated spectrophotometric method for determining the
chemical oxygen demand of surface and wastewaters is described and
compared to the standard method.
'ABSTRACT
A micro sample digestion technique for the determination of chemical
oxygen demand (COO) is described. An automated spectrophotometric
measurement of the appearance of chromium (III) after sample digestion
completes the method. Adequate sensitivity at 600 nm is achieved by
using a 50 mm flowcell to measure COO values in the range 3-900 mg/1.
The semi-automated method is compared to the standard method with
respect to precision, accuracy, ease of analysis and comparability of
data.
-------
- 2 -
INTRODUCTION
The oxidation of organic and inorganic wastes in a receiv-
ing water depletes the dissolved oxygen supply, which can have
a profound effect on aquatic life (1). A meaningful determina-
tion of the natural oxygen demand of wastewaters has been a
problem since the previous century. The biochemical oxygen
demand (SOD) test was developed to measure the natural oxygen
demand of wastes under laboratory conditions similar to those
found in receiving waters (2-4). The advantage of the BOD test
1s that it is a good indicator of the bio-degradcbility of a
waste* The major disadvantages of the BOD test are the long
time required for analysis, the poor precision and the indeter-
minable accuracy of the method (4,5).
In order to substantially reduce the time required to esti-
mate the ultimate oxygen demand of a wastewater, the chemical
oxygen demand (COD) test was developed (6). The addition of
silver sulfate (7, 8) and mercuric sulfate (9) to the acidic
dichromate digestion solution, increased the real lability of the
COD test (10, 11), However, since chemical oxidation does not
differentiate between biologically stable and unstable wastes, a
correlation between COD and BOD values must be developed for
each sample type (12). •
Stenger and Van Hall reported a very rapid method for measur-
ing the total organic carbon (TCC) content of water samples, which
-------
- 3 -
«
can be related to oxygen demand (13). However, the advantage
*
1n being able to rapidly determine TOC values is offset by the
high initial equipment cost. In addition, the informational
content of the TOC analysis is less useful than that gained
from the BOO or COD methods (14). The TOC test does not dif-
ferentiate between compounds with the same number of carbon
atoms, but which are in different stages of oxidation and hence
have different oxygen demanding potentials. Since the COD and
BOD tests measure the amount of oxygen required to stabilize
waste samples, their values inherently reflect the original
oxidation state of the chemical pollutents.
*
The standard COD test (4) is widely used because it pro-
vides a good balance between the value of the information gained
and the speed of analysis when compared to the BOD and TOC tests
(12). However, the standard method for determining COD has
limitations which are not inherent in the concept of the test.
The back-titration of dichromate after sample digestion is an
Insensitive method of detection. This lack of method sensitiv-
ity has been partially alleviated by using two different concen-
trations of dichromate and a relatively 1'arge sample volume. In
addition, the consumption of large quantities of expensive rea-
gents, the extensive bench space requirement of the COD hot plates
which limits the number of analyses that can be performed in a
day, and the difficulty of disposing of large quantities of highly
acidic mercury, silver and chromium wastes, are serious problems
for most industrial laboratories (15).
-------
• 4 -
Recently, there has been considerable interest in simpli-
fying the rather tedious standard COD method (16-19). Unfortun-
ately, procedures using a much shortened digestion period or
•
lower digestion temperatures produce results equivalent to those
obtained by the standard method only for very readily oxidized
wastewaters (20-22).
Bloor (23) and Johnson (24) determined the organic content
of biological materials using dichromate as an oxidant and then
measuring the excess dichromate spectrophotometrically, This
procedure eliminated the tedious detection procedure of the stand-
4
ard method. The spectrophotcmetric procedure has been applied to
the analysis of water samples in which the COO was determined by
measuring the appearance of Cr (III) after manual digestion (25-27)
Several COD methods which use a spectrophotometric means of
detection and automated sample digestion have also been reported.
Sample digestion was accomplished using a continuous digester (28,
29) or high temperature bath (30-32). However, Tift and Cain
reported data which show that these automated procedures do not
produce results equivalent to the standard method for all sample
types (33). The incomparability of data was attributed to incom-
plete sample oxidation caused by the short digestion times in the
automated methods. In addition, the higher concentration of sul-
furic acid used in most automated systems requires a smallsr
amount of mercuric sulfate be used to avoid its precipitation in
-------
- 5 -
the sample lines and flowcell. The lesser amount of mercuric
sulfate caused chloride to be more of an interference in these
automated methods than in the standard method,
The method reported here combines the advantages of the
reliability of the standard digestion procedure (4), with the
superior sensitivity and precision of an automated procedure
based on the spectrophotometric measurement of Cr (III) (27).
Use of the resultant micro semi-automated COO method has
Increased the productivity of this laboratory three-fold and
reduced the consumption of very expensive reagents and the
quantities of wastes twenty-fold,
EXPERIMENTAL
Apparatus. Samples were digested in Corning £9949 16x100
mm screwcap (cap £9998) culture tubes. Spectrophotometric measure-
ments were made with the apparatus shown schematically in Figure 1.
The automated system was fabricated using Technicon Corporation
AutoAnalyzer II equipment consisting of a Sampler IV, Pump III,
Colorimeter II, Recorder II, and single channel Digital Printer.
The colorimeter was used in the direct mode and equipped with 600
nm interference filters and 50 mm flowcells. The Standard Calibrra-
tion control was set at 228 to attain 1000 mg/1 COO full scale on
the recorder. A glass capillary was used as a sample probe. The
sampler was operated at 40 samples/hr with a 3:1, sample to wash
ratio.
-------
- 6 -
Wastewater samples with particulate matter-were blended
with a Teckmar Model SDT homogenizer before taking an aliquot
for analysis. An adjustable 0-5 ml Oxford pipette with dis-
posable polypropylene tips was used for aliquoting samples and
addition of reagents.
Reagents. Unless otherwise noted, all chemicals were ACS
reagent grade. All reagent water was de-ionized and distilled.
Digestion solution was prepared by adding 10.216 g of
K2Cr207 (dried at 105° C), 167 ml of cone H2S04 and 33.3 g of
HgSC>4 to 500 ml of water and. diluting the cooled solution to
1 1.
Catalyst solution was prepared fay dissolving 22 g of Ag2S04
in a 9-1b bottle of cone H2S04.
Sampler wash solution was 50% sulfuric acid by volume.
A stock potassium acid phthalate solution, equivalent to
10 g/1 COD, was prepared by dissolving 8.500 g of a dried portion
of NBS standard reference material 84 h in water and diluting to
1 1. Working standards of 25, 50, 75, 100, 250, 500 and 750 mg/1
COD were prepared by diluting 2.5, 5, 7.5, 10, 25, 50 and 75 ml
of stock solution to 1 1, respectively.
Procedures. It was necessary to wash all culture tubes and
screw caps with 202 H2SO^ before their first use to prevent random
contamination.
Digestion was carried out by placing 2.5 ml of sample and 1.5
ail of digestion solution in a culture tube. Three and one half ml
-------
- 7 -
of catalyst solution were added carefully down the side of the
culture tube so that the acid formed a layer on the bottom.
The tube was capped tightly and then shaken to mix the layers.
Two blanks and a set of standards were prepared in the same
manner and analyzed with each sample set.
All samples, blanks and standards were heated in an oven
at 150° C, which is the observed reflux temperature of 50* sul-
furic acid. After two hours the tubes were removed from the
oven, cooled, and placed in the Sampler IV tray.
The analytical manifold and reagents were set up as indi-
cated in Figure 1. Two digested blanks were analyzed at the
beginning of each sample set to zero the baseline. A mid-scale
standard was used to calibrate the recorder and printer (34).
Standards ware rerun periodically during the course of an ana-
lysis run to assure that the system remained in calibration.
The COD value of unknown samples was obtained by direct print-
out. A typical recorder trace for standards is shown in Figure 2.
RESULTS AND DISCUSSION
Sample Digestion. It has been shown that COD procedures
using a shortened digestion period and/or a reduced digestion
temperature do not attain the same degree of sample oxidation as
the standard method (20-22, 33), Any alternate test procedure
used to analyze wastawatars for COD must produce results equiva-
lent to or better than the current standard method (35). There-
fore, to insure data comparability the temperature and length of
-------
- 8 -
.sample digestion and concentration of reagents used in the
standard method were adopted for use in the semi-automated
procedure described here (4).
Since the micro colorimetric detection technique required
only 2 ml of digested sample the quantities of sample and rea-
gents used were reduced twenty-fold in comparison to the
standard method (4, 11). Use of the standard COO digestion
apparatus was eliminated and instead all samples, blanks and
standards were digested in small screw-cap culture tubes. The
potential for sample contamination from large glass surfaces
was consequently reduced.
Screw caps with phenolic resin liners were found to be
unacceptable since they ware attacked by the digestion solution
giving erroneously high COD values. Teflon-lined caps greatly
reduced this problem especially if each cap -.vas used only once.
Any sample tube which Isakad, as evidenced by a black residue
on the outside of the tube, was discarded.
Uniform addition of reagents and improved precision was
achieved by dissolving f.ll chemicals in one of two solutions.
The catalyst solution was prepared by the standard method (4).
The oxidizing solution was prepared by combining potassium
dichromate with mercuric sulfate and making the solution 5 N
with sulfuric acid ~o solufailize the mercury salt. However,
the mercuric sulfata .-.as not completely soluble in the cooled,
combined reaction Tnx;ure. 7ha height of the sampler probe
-------
- 9 -
was carefully 'adjusted so as to avoid aspirating the precipitate.
Otherwise, aspiration of the participate matter caused severe
baseline noise.
Spectroohotometric Analysis. The COD of wastewater samples
has been determined spectrophotometrically, after digestion, by
measuring the decrease in Cr (VI) concentration at 352 (32) or
440 nm (19). Alternatively, the increase in Cr (III) concentra-
tionhas been measured at 600 (27) or 650 nm (25). All of these
authors found the spectrophotometric procedure to be easier to
perform than the manual titration.
Molov and Zaleiko showed that better sensitivity could be
achieved by measuring the decrease in Cr (VI) concentration than
the increase in Cr (III) concentration (28). However, the preci-
sion of ..a method based on measuring the decrease in Cr (VI) absorb-
ance is very dependent on the reproducibility of reagent addition.
This problem was avoided and adequate sensitivity achieved by
measuring the appearance of Cr (III) at 603 rrm, using a 50 mm
flowcell, and the scale expansion capability of the Techm'con
colorimeter.
In order to increase the sensitivity of the standard method,
two different concentrations of oxidizing reagent are coraionly
used. These correspond to tv/o levels of CCD measurement, 5-50
mg/1 and 5C-3CO nig/1 (11). Moore and Walker found that the
working range cf the low level modification was limited by the
diminished oxidation pccan-ia! of the digestion solution after
50* of the dichrcmata was consumed (35).
-------
- 10 -
Due to the adequate sensitivity of the spectrophotometric
semi-automated method, only one set of reagent concentrations
was necessary to cover both levels of the standard method. In
order to test the linearity of the semi-automated method, .
standards between 500 and 1000 mg/1 COD were analyzed in incre-
ments of 25 mg/1. Potassium hydrogen phthalate was chosen for
use as a standard because of its stability in solution and its
complete oxidation under the conditions of the COD test (4).
The results, presented in Figure 3, show the colorimetric method
to.be linear up to 900 mg/1 COD.
Due to the use of 50* sulfuric acid, the original automated
manifold was constructed with acidflex tubing. However, the
system exhibited very poor hydra!ic characteristics. This problem
was alev.iatsd by replacing the acidflex tubes with tygon purnp
and transmission tubing. The recorder trace in Figure 2 was
undamped, The entire system was cleaned for about 1/2 hour before
first use with 50* sulfuric acid to prevent severe baseline drift
due to leachable organic matter. Also 1:1 dilution loco was added
to the system to reduce the viscosity of the sample stream so that
proper debubbling occurred in the flowcsll.
Precision, Accuracy ;nd Detection Limit, Sir.ca it was dif-
ficult to correct the semi-automated results for the "an baseline
drift, the working detection limit was defined as the mean bias of
the blank plus two standard deviations. Eleven blank samples
were analyzed to determine the detection limit. The mean value
-------
- n -
'obtained was 1 mg/1 with a standard deviation of 0.8 mg/1 COD.
These values were used to define the detection limit at 3 mg/1
COD. This number compares quite favorably with the detection
limit of 5 mg/1 COD reported by Moore and Walker for the low
level standard COD method (36).
The relative precision of both modifications of the stand-
ard and the semi-automated COD methods was determined by perform-
ing replicate analyzes on four wastewater samples. Since the
standard and semi-automated determinations were performed at
different times, two similar sets of water samples were chosen
so that the relative standard deviations could be meaningfully
compared. The relative standard deviations of both .methods for
low COD concentrations, as shown in Table I, compare very closely.
However; the precision of the semi-automated method at high COD
concentrations was approximately seven times better than the
standard method.
Adelman pointed out that one of the factors contributing to
the poor precision of the standard method was the potential loss
of volatile components of the wastewater samples (30), This can
be caused by the heat generated by the mixing of the sample with
the concentrated acid prior to reflux or during the reflux step.
This problem was eliminated in the semi-automated procedure by
avoiding mixing the sample and acid layers until the tube is
capped and the fact that sample digestion occurs in a completely
closed system.
-------
- 12 -
The authors found that the ability to take-a representative
aliquot of a nonhomogeneous sample was the limiting component of
analysis variability regardless of method. Precision data for
the standard COO method determined from inter-laboratory analyses
of standard-like solutions must be regarded only as a lower limit
(5, 37).
The accuracy of the semi-automated method was determined by
measuring the recovery of standard addition of potassium hydrogen
phthalate to several types of water samples'. The mean recovery
from 14 water and wastewater samples, shown in Table II, was 101%
with a standard deviation of 4%.
Comparison of Semi-Automated and Standard Methods. A variety of
surface and wastewater samples were analyzed by both the standard
and semi-automated COD methods to determine the comparability of
data. These samples included raw and treated sewage, industrial,
chemical and food process wastes. Results comparing the two methods
are shown in Table III. Initially the largest discrepancies between
methods occurred in samples which contained large quantities of
particulate matter, e.g., raw sewage. Homogenizing samples of
this type greatly improved the comparability of the data. Within
the standard deviation of the mean ratio of results, no significant
bias in COO values exists between methods,
In addition, several purs organic compounds were analyzed to
determine if the semi-automated method achieved a more ccmolete
-------
- 13 -
digestion than the standard method. The experimental results
and calculated maximum theoretical COD values are shown in
Table IV. The semi-automated values were slightly higher than
the standard method results indicating that the former method
achieved a more complete sample digestion. The difference
could also be due to the fact that no volatile material can
excape from the sealed tubes during oxidation in the semi-auto-
mated method, while in the standard method, volatile material
may escape before sample oxidation is complete.
' 'Interferences. One of the major problems encountered in
Other automated COD methods is the inability of the techniques
*
to compensate for the positive interference caused by the oxida-
tion of chloride present in wastewater samples (28-32). The
standard procedure for eliminating the chloride interference is
the addition of mercuric sulfate to form a complex and prevent
Its oxidation (4, 9). Experiments performed by this laboratory
Indicate that no interference results up to 2000 mg/1 chloride
when the standard procedure is used (9).
In Bother automated techniques, the high acid concentration
reduces the solubility of HgS04 so that the quantity of Hg(II)
1n solution is not sufficient to complex the same amount of
chloride as in the standard method (23-32).
In the semi-automated COD method, the ratio of HgS04 to
sample volume is identical to the standard method. Standards of
500 mg/1 COD were spiked with varying amounts of chloride in
-------
- 14 -
order to determine the limiting concentration at which the inter-
ference was significant. The results, shown in Figure 4, indi-
cate that chloride does not interfere below 1000 mg/1. Above
this concentration, some precipitation occurs when the dilution
water combines with the sample stream in the automated system,
which results in a noisy recorder trace. If it is necessary to
routinely analyze samples containing between 1000 and 2000 mg/1
chloride, the dilution loop can be removed. Air spikes will then
appear at the beginning and end of each sample peak, due to
Improper debubbling, but the results are not affected.
Any chemical species remaining after sample digestion, which
absorb at 600 nm, cause a positive interference in the semi-auto-
mated method. Since almost all organic matter is digested by the
COO technique the possible interference from organic compounds
was not considered (5, 8, 36).
The presence of Cr (III) in a water sample gives an apparent
COO of 1.39 times the concentration of chromium. Also, a potential
interference from iron was investigated by spiking standards of
500 mg/1 COO with increasing amounts of ferric iron. The results,
presented in Figure 5, show no apparent COO below 5 g/1 Fe. The
positive bias caused by high concentrations of interfering sub-
stances is routinely eliminated by diluting samples prior to
analysis or correcting the reported COO values from independent
determinations of chromium, iron and chloride.
-------
- 15 -
1-ACKNOWLEDGEMENT
The authors would like to thank B. J. Fairless and
D, A. Payne for their helpful comments during the course of
this work and their critical review of the manuscript.
The mention of trade names or commercial products does
not constitute endorsement or recommendation for use by the
Central Regional Laboratory or the Environmental Protection
Agency.
-------
- 16 -
REFERENCES
(1) "Water Quality Criteria," Federal Water Pollution Control
Administration, Washington, 0. C. ,1968, pp 32-5.
(2) E. B. Phelps, "Stream Sanitation," John Wiley and Sons,
New York, N. Y., 1944, pp 65-6.
(3) E. J. Theriault, Public Health Bulletin No. 173, U.S.
Public Health Service, Washington, D. C., 1927.
(4) "Standard Methods for the Examination of Water and Waste-
water," 13th ed., American Public Health Association,
New York, N. Y., 1971, f) 489.
(5) D. G. Ballinger and R. J. lishka, J_. Water Pollut. Contr.
"Fed.,'34, 470 (1962).
(6) W. A. Moore, R. C. Kroner and C. C. Ruchhoft, Anal. Chem.,
'21, 953 (1949).
(7) M. M. Muers, £. Soc. Chem. Ind., 5_5, 71T (1936).
(8) W. A. Moore, F. J. Ludzack and C. C. Ruchhoft, Anal. Chem.,
' 23, 1297 (1951).
(9) R. A. Dobbs and R. T. Williams, Anal. Chan., 35, 1064 (1963)
(10) "Water and Atmospheric Analysis," Annual Book of Standards,
Part 23, American Society for Testing and Materials,
Philadelphia, Penn., 1973.
(11) "Methods for Chemical Analysis of Water and Wastes,"
Environmental Protection Agency, Cincinnati, Ohio, 1971,
pp 17-23.
-------
- 17 -
(12) "Handbook for Monitoring Industrial Wastewater,"
t
Environmental Protection Agency, Wash,, D. C., 1973.
(13) V. A. Stenger and C.E. Van Hall, Anal. Chem., 39,, 206
(1967).
(14) C, Geisler, 0. F. Andrews and G. Schierjott, Water and
'Wastes Ing., 11, 26 (1974).
(15) R. B. Dean, R. T. Williams and R. H. Wise, Environ. Sci.
Techno!, 5_, 1044 (1971).
(16) A. F. Westerhold, The Digestor. 22, 4 (1955).
(17) 'Ibid.. 22, 18 (1965),
(18) J. S. Jeris, Water and Wastes'Eng., £, 89 (1967).
•
(19) T. K. Wu, Michigan Department of Natural Resources Laboratory,
Lansing, Michigan, private communication, 1974.
(20) J, M. Foulds and J. V. Lunsford, Water'and Sewage Works. 115,
112 (1963).
(21) W. N. Wells, Water and Sewaoe Works, 117, 123 (1970).
(22) L, E. Shriver and J. C. Young, £. Water Pollut. Contr. Fed.,
'44, 2140 (1972),
(23) W. 'R. Bloor, J_. Bid. Chem., 77_, 53 (1928).
(24) M. J. Johnson, J. Bid. Chem., 181, 707 (1949).
(25) R. R. McNary, M. H. Dougherty and R. W. Wolford, Sewage and,
'Industrial Wastes, 29_, 894 (1957).
(26) N. Chaudhuri, S. Niyogi, A. De and A. Basu, J. 'Water Pollut.
' Contr. Fed., 45, 537 (1973).
-------
- 18 -
(27) A, F.-Gaudy and H. Ramanathan, J. Water Pollut. Contr. .Fed.,
36, 1479 (1964).
(28) A. H. Molof and N. S. Zaleiko, 19th Purdue Industrial Waste
Conference, Lafayette, Ind., May, 1964.
(29) J. H. Ickes, E. A. Gray, N. S. Zaleiko and M. H, Adelman in
"Automation in Analytical Chemistry, Technicon Symposia
1967," Mediad Inc., Tarrytown, N. Y., 1968.
(30) M. H. Adelman, 18th Pittsburgh Conference on Analytical
Chemistry and Applied Spectroscopy, Pittsburgh, Pennsylvania,
. March, 1967.
(31) M. H. Adelman in "Automation in Analytical Chemistry,
Technicon Symposia 1965," Mediad Inc., Tarrytown, N. Y.,
1966.
(32) "Industrial Method No. 137-71W," Technicon Instruments Corp.,
Tarrytown, N. Y., 1973.
(33) E. C, Tifft and 8. E.'.Cain in "Automation in Analytical
Chemistry, Technicon Symposia 1972," Mediad Inc., Tarrytown,
N. Y., 1973.
(34) "Technicon Operation Manual," Technicon Instruments Corp.,
Tarrytown, N. Y.f 1973.
(35) Federal Register, 33, 28759 (1973).
(36) W. A. Moore and W. W. Walker, Anal.'Chem., '23, 167 (1955).
(37) J. A. Winter, "Method Research Study 3, Demand Analyses,"
Environmental Protection Agency, Cincinnati, Ohio, 1971.
-------
TABLE I, COMPARISON OF THE PRECISION OF THE SEMI-AITO-IATED
AND STANDARD CHEMICAL OXYGEN DEMAND METHODS
EMI-
•
1PLE No,
1
2
3
4
ffo, OR
DETNS,
11
10
11
10
|c
MEAN .
40
230
26
270
•On / N
RANGE
4
90
4
12
!G/L
STD, DEV,
1A
28,0
1,3
4,6
REL"(
DEV,'
3,5
12,2
5,0
1,7
-------
TABLE II, RECOVERIES OF POTASSIUM HYDROGEN PHTHAIATE ADDED
TO I-KTER SAMPLES WITH SEMI-AUTO.WED METHOD
SAMPLE SOURCE SAMPLE W ADDED SAMPLE +KHP RECOVERY/%
•
ORGANics INDUSTRY 13 200 217 102
RAWFSEWAGE 164 200 ' 370 1D3
RIVER WATER 31 . 10Q 322 91
HARBOR WATER 16 200 224 ' 104
INDUSTRIAL COOLING 65 200 262 99
RIVER WATER 15 100-116 101
RIVER HATER 28 ' 1DO '124 96
CHANNEL WATER 52 100 '152 100
NEAR DREDGING ^
INDUSTRIAL DISCHARGE 30 100 131 • 101
INDUSTRIAL DISCHARGE 16 100 115 100
TREATED SEWAGE 40 100 . * 144 104
RECEIVING WATER 25 100 127 102
OF-SEWAGE
TREATED SEWAGE 14 100 124 110
STEEL MILL EFFLUENT 14 100. 112 98
MEAN ' 101
STANDARD DEVIATION '
-------
TABLE III, COMPARISON OF SBII-ALTTCMATED AND STANDARD
CHEMICAL OXYGEN DEMAND (-ONODS
.!•:.. .. « .. . ,i . .. .-» »«. •
frnnl.
STANDARD METHOD SEMI-AJTO.WED S/A
SAMPLE SOURCE (S) ('terra (AT X 300
CHEMICAL PL-NT WASTE
9GCO
RAW SEWAGE 420 ' 421 99,8
PAPER MILL COOLING 39
WATFR
STEEL MILL WASTE 270 ... 273 93,9
TREATED SEWAGE 50 51 98,0
PRIMARY TREATED . 63 51 - 1*3.:/'
SD^GE
BOILER SLOWDOWN 180 133 y>A
POTTERY SHOP WASTE M) 155 89,7
CREEK DOWNSTREAM 94 .99 94,9
FROM POTTERY SHOP M ^
PRIMARY TREATED 90 87 103,4
SEWAGE
PAPER MILL WASTE 450 464 ' 97,0
RAW SEWAGE. 170 154 103,7
TREATED SBVAGE 35 35 102,9
TREATED SB^GE 27 27 100,0
TREATED SEV&GE 21 22 ' 95,5
ORGANIC CHBMICAL 270 275 53,2
PLANT WASTE ' _ ,_•.
STEEL MILL VCASTE bO cd ^ji-1
H CO 0
^ ~J "*,f ' y
A RESULT REJE-^ED PC?. CALCUUTICN OF M£A;J ATE 37A,\DARo C^/IATICN,
-------
TABLE IV, COMPARISON OF 0-encAi OXYGEN DEMAND
. METHODS ON ORGANIC COMPOUNDS
COMPOUND
Icon/ , MS/I •
THEORETICAL
238
470
221
197
107
150
127
490
98
64
197
223
239
244
STANDARD METHOD SEMI -AUTOMATED S/A
(S) METHOD (A) X100
.230
450
200
170
DO
- 330 •
120
470
90
60
190
* 5
64
250
240
462
207
180
113
139
128
• 496
98
62
202
• <3
77
242
9578
9774
9676
9474
8878
9375
9378
9478
91,8
9678
9471
A
83JA
1033
95,0
375
SODIUM ACETATE
ACETONE
ETHANOL
DEXTROSE
ftTHANOL
OXALIC PCID
SODIUM CITRATE
GLUTAMIC ACID
GLYCINE
BENZOIC ACID
PTRIDINE
3-PlCOLINE
TETKAHYDROFURAN
MEAN
STANDARD DEVIATION
^
RESULTS REJECTED FOR CALCULATION OF MEAN AND STANDARD DEVIATION,
-------
TITLES FOR FIGURES,
• • * *
FIGURE 1, AUTOMATED SYSTEM FOR CHEMICAL OXYGEN DEMAND, NUMBERS IN
PARENTHESES CORRESPOND TO THE FLO,-/ RATE OF THE PUMPTUBES
IN ML/MIN, NUMBERS ADJACENT TO GLASS COILS AND FITTINGS
ARE TECHNICON CORP, PART NUMBERS, •
FIGURE 2, RECORDER TRACE FOR CHEMICAL OXYGEN DEMAND OF POTASSIUM
HYDROGEN PHTHALATE STANDARDS ANALYZED IN DUPLICATE,
FIGURE 3, CALIBRATION CURVE FOR AUTOMATED CHEMICAL OXYGEN DEMAND,
EACH POINT IS THE AVERAGE OF DUPLICATE DETERMINATIONS,
FIGURE 4, PLOT OF APPARENT CHEMICAL OXYGEN DEMAND CAUSED BY THE
OXIDATION OF CHLORIDE, IkTA DETERMINED BY ADDING THE
INDICATED AMOUNTS OF CHLORIDE TO A SCO MG/L COD POTASSIUM
HYDROGEN PHTHALATE STANDARD,
• • . • • •
FIGURE 5, PLOT OF APPARENT CHEMICAL OXYGEN DEMAND CAUSED BY THE
ABSORBANCE AT SCO KM FRCM FERRIC IRON IN SOLUTION, DATA
DETERMINED BY ADDING THE'INDICATED AMOUNTS OF IRON TO A.
500 MG/L COD POTASSIUM HYDROGEN PHTHALATE STANDARD,
-------
-------
[COO], m0/1
-------
ABSORBAXCE, 0.9.
-------
[COD] ,mg/i
en
09
CD
en
CD
CD
00
C3
, I
a —,
CTQ CD
NO
C3
C=3
CD
CD
03
C3
CD
00
ro
CD
CD
-------
APPENDIX III
-------
AN AUTOMATED METHOD FOR THE DETERMINATION OF
TOTAL AND INORGANIC MERCURY IN WATER AND WASTEWATER SAMPLES
PRELIMINARY
• 'BY
ABBAS A. EL-AWADY*, ROBERT B. MILLER AND MARK J. CARTER :
? U.S. Environmental Protection Agency
| Central Regional Laboratory
1819 W. Pershing Road
Chicago, Illinois 60609
*Author to whom correspondence should be addressed; on leave (1974-1975)
from Western Illinois University, Macomb, Illinois, 61455.
-------
ABSTRACT
An automated method for the determination of total as well as
inorganic and organic mercury by the cold vapor method is given. The
method is suitable for the analysis of samples in a variety of environ-
mental water matrices. A detection limit of 0.05 yg/1 is obtained by
the use of a highly sensitive spectrometer. The method is suitable
for the analysis of samples with mercury concentrations in the range
0.05 - -6 yg/1 and a COD less than 700 mg/1. The use of potassium per-
sulfate, potassium permanganate, potassium dichromate and mixtures of
these salts as oxidizing agents for the digestion step is discussed,
and a study of sample preservation is given. Twenty samples and/or
standards per hour can be analyzed using this method.
-------
INTRODUCTION
In recent years a number of methods have been introduced for
1-10
the determination of mercury in a variety of matrices. The most
widely used method utilizes a flameless atomic absorption technique
10
first introduced by Hatch and Ott. Most of these are time consuming,
K. K. S. Pillay, C. C. Thomas, Jr., J. A. Sondel, and C. M. Hyche;
Anal. Chem., 43, 1419 (1971). ,
2V. I. Muscat, T. J. Vickers, A. Andren; ibid., 44, 218 (1972).
E. W. Bretthauer, A. A. Moghissi, S. S. Snyder, and N. W. Mathews;
ibid., 46, 445 (1974).
^
J. 0. Bisogni, Jr. and A. Wm. Lawrence; Env. Sc. Tech., 8, 851 (1974).
C. T. Elly; J_. Water Pol. Cont. Fed.. 45, 940 (1973).
R. F. Overman; Anal. Chem. 43, 616 (1971).
T. J. Rohm, H. C. Nipper, and W. C. Purdy; ibid., 44, 869 (1972).
8H. J. Issaq and W. L. Zielinski, Jr. ibid.. 46, 1436 (1974).
V F. Fitzgerald, W. B. Lyons, and C. D. Hunt, ibid., 46, 1882 (1974).
10
W. R. Hatch and W. L. Ott, ibid., 40, 2085 (1968).
however, and do not allow for the analysis of a large number of samples,
such as is generally encountered by environmental laboratories. The
solution to this problem has been to move in the direction of establishing
automated procedures, which will allow either continuous monitoring or
the analysis of reasonable numbers of samples per day. This increase
-------
in the sample analysis rate should be done without affecting either
the sensitivity or the accuracy of the procedure.
11-13
Recently a number of automated methods for the determina-
tion of mercury have appeared in print. These methods are highly suit-
able for the analysis of clean water samples and other samples with a
UB. W. Bailey and F. C. to; Anal. Chem. 43, 1525 (1971).
12
T. B. Bennett, Jr., W. H. McDaniel, and R. N. Hemphill; Advances
in Automated Analysis, 1972 Technicon International Congress, Vol. 8;
Mediad Incorp., Tarrytown, N.Y.
P. D. Kluckner, "Investigation of an Automated Method for the Deter-
mination of Total Mercury in Water and Wastewater" a report to the
Chemistry Laboratory Water Resources Service, 3650 Wesbrook Crescent,
Vancouver, British Columbia, Canada (1973).
very low content of oxidizable materials. However, for samples with a
high content of particulate matter as well as for those with high con-
centrations of oxidizable impurities, the suitability of these methods
is questionable. An automated method that addresses itself to these
questions is presented in this paper. The comparability of the des-
cribed method has been checked against the manual method presently
m
accepted by EPA and has been found suitable for the analysis of mercury
in all types of water samples including those samples with a high content
of particulate matter and oxidizable impurities.
"Methods For Chemical Analysis of Water and Wastewater", EPA Publication
No. EPA-625/6-74-003, U.S. Environmental Protection Agency, Office of
Technology Transfer, Washington, D.C., 20460, pp. 118
-------
EXPERIMENTAL
Apparatus. All glassware used In this work was borosilicate
glass. Standard mercury solutions were prepared in volumetric flasks
with glass stoppers. All glassware was first washed with water, soaked
for two hours in a 1% potassium permanganate solution, soaked for an
additional two hours in a 1:1 mixture of concentrated nitric and sul-
furic acids, and then washed with doubly deionized water. The glass-
ware was then baked for 3-4 hours at 400°C. It was found that for
subsequent use of the same glassware, a rinse with cone. HNO-j followed
by several rinses with doubly deionized water was sufficient. No traces
of mercury were observed in these flasks. All domestic and industrial
waste samples were stored in high density polyethylene, 1-liter screw-
cap bottles with polyethylene lined caps and preserved to give a final
concentration of 0.5% HNC^. Liquid transfers for dilution purposes
were made with Eppendorf pipets of 0.1, 0.25, 0.5, and 1 ml capacity.
Instrumentation. The instruments used consisted of:
1. Spectro Products Mercury Analyzer Model HG-2
2. Perkin-Elmer Model 56 multi-range chart recorder
3. Harmonically smoothed voltage stabilizer
4. Technicon Auto-Analyzer Unit consisting of:
a. Sampler IV
b. Proportioning Pump III
c. Heating bath with heating coil (20 ft. long
and 2.4 mm internal diameter).
-------
5. Gas-Liquid Separator
6. A rotameter to measure the rate of air. flow in the gas-
liquid separator.
7. High speed blender for sample homogenization
The operating principle of the mercury analyzer is based upon
o
balancing the intensity of the mercury line at 2537 A from a hollow
cathode lamp "A" against the intensity of one or more lines from a
reference hollow cathode lamp "B" in the same wavelength region as
observed by a single detector. Lamp "A" is a pulsed mercury hollow
cathode lamp, and lamp "B" is a pulsed iron hollow cathode lamp. The
two lamp sources are pulsed 180° out of phase above a sustaining base
current in a square wave mode. The. instrument is balanced with the
absorption cell swept free of any residual mercury. In the absence
of any interfering substance, any observed absorption is solely due
to mercury.- The net intensity due to mercury absorption is directly
obtained from the output of a phase sensitive, lock-in amplifier. The
instrument is equiped with an automatic gain control to the lock-in
amplifier, so that compensation for the background or extraneous ab-
sorption is accomplished automatically. In addition, a 10X scale
expansion is provided for the analysis of samples containing low con-
centration levels of mercury.
It was found necessary to modify the absorption cell supplied
with the instrument. The main modifications were: 1. To decrease the
internal diameter by a factor of two; 2. To position the inlet and
exit tubes as close as possible to the quartz windows so as to decrease
-------
the dead air space in the vicinity of the window. In order to compensate
for the factor of four decrease in signal strength caused by these modi-
fications, it was necessary to increase the gain (voltage) on the photo-
multiplier tube. The present cell's dimensions are: 22 cm long, 7 mm
internal diameter, and 11 mm external diameter. The cell is constructed
completely from quartz.
The chart recorder is equiped with a variable input voltage,
allowing several scale expansions. The recorder was operated at its
lowest chart speed of 5 mrn/min.
Reagents. All chemicals used are analytical reagent qrade or
better. The water used was doubly deionized. The reagents and their
concentrations are as follows:
]. Concentrated sulfuric acid; obtained from Baker and desig-
nated as "suitable for Hg determination".
2. 10% stannous chloride solution; prepared in a solution
10% in HC1.
'3. 1% potassium permanganate solution; a fresh stock solution
was prepared every three weeks.
4. 2% potassium dichromate solution.
5. 3% hydroxylamine hydrochloride; prepared in a solution
3% in sodium chloride.
6. 4% potassium persulfate; this solution was prepared fresh
weekly.
7. Con. nitric acid.
8, A tank of purified nitrogen.
9. Mercury stock solutions; 1 mg/ml (=1000 mg/1) of either
mercuric chloride or methyl mercuric chloride.
10. Mercury standard solutions. Mercury standard solutions
in the range 0.05 - 6.0 ug/1 were prepared by proper
dilutions of a 100 yg/1 stock solution prepared from
-------
solution 9 above. All standards were prepared in a
solution 0.5% in HN03 and 0.05£ in K2Cr207 as a pre-
servative.
11. Activated charcoal, as an absorber for elemental Hg.
Procedure. The flow diagrams for the mercury manifold are given
in Figures 1 and 2. Figure 1 represents all experiments with K2S208 as
the only oxidizing reagent used for sample digestion. Figure 2 repre-
sents all experiments in which KMn04 or i^C^Oy is used as an oxidizing
agent in addition to K2S20g. In the second system a 3% hydroxylamine-
hydrochloride solution is used as a reducing agent for the excess KMnC^
or i^C^Oy which was not reduced in sample digestion. It should be noted
here that all connections, coils, etc. in the sample train past the pump
tubes are made of borosilicate glass. The heating bath is set at 100±
2°C, and the mercury analyzer is allowed to stabilize for a one hour
warm-up period. The system is then flushed with a 1% HNOs solution and
the absorption cell is flushed with purified nitrogen gas. The rotameter
is set to give a constant gaseous flow rate of 15-25 cm^/min. The inlet
to the segmenting air tube as well as the outlet for the absorotion cell
are connected to a tube filled with activated charcoal which acts as a
mercury absorber. The reagents are then passed through the system in
the-order: a. H2S04, b. SnCl2, c. NH2OH-HCl-NaCl, d. KMn04 or
K2Cr207, e. K2S2Og; while the automatic sampler is kept in the wash
cycle. The wash is made of a 1% HN03 solution. The flow of all reagents
is maintained for a period of 15-30 min. or until a stable baseline is
obtained. In all experiments done using*K2S208 as the sole oxidizing
-------
agent, both the hydroxylamine and permanganate or dichromate reagent
lines are disconnected, and the reagents introduced in the order
^$0)4, SnC^, and K2S2Og. After a stable baseline is obtained, standards
in the range 0.05 - 6.0 yg/1 Hg are placed in a sample tube (prerinsed
with the same solutions), and transferred to the sampler. For all
samples judged to be high in mercury i.e. 0.5 - 6 yg/1, only standards
in that range are used. For low level mercury determination i.e. less
than 0.5 yg/1, standards in the range 0.05 - 0.5 ug/1 are used, and
the mercury analyzer is set at its 10X scale expansion. In addition,
a recorder scale expansion (a factor of 2) is used for runs with mercury
concentrations in the range 0.2 - 3 yg/1. Samples to be analyzed are
then placed in the sampler while the standards are running. Standards
were prepared fresh daily from the stock solution and analyzed by the
system before and after each run in order to provide a calibration curve
and to check for the stability of the standards during the analysis
period. In some experiments the same standards were run over a period
of two to four weeks to check for the effectiveness of the preservatives
used (0.05% HN03 and 0.05% K^C^O;). Both mercuric chloride and methyl
mercuric chloride standards were used to check for the recovery of or-
ganomercury compounds.
All sampling was done using a 20/hour sample cam with 2:1 wash-
sample ratio. For recovery studies, arbitrarily selected samples were
spiked with the equivalent of 0.3 yg/1 Hg for samples with less than
1 yg/1 Hg, and with 2-3 yg/1 Hg for samples containing 1-4 yg/1 Hg.
-------
8
All samples containing high concentrations of participate matter
were first homogen-ized using a Techmar Co. high speed homogenizer model
SOT. In addition, samples were stirred before and during sampling.
After the analyses are completed, all lines with the exception of
the sulfuric acid line are placed in a 1% HN03 solution until all reagents
are completely flushed out. This is followed by placing the sulfuric
acid line in the wash. All the lines are then flushed for 10 min. with
3% N^OH-HCl to remove any build-up of manganese oxides. This is then
followed by flushing the system with 1% HN03 for a period of 20-30 min.
The above flushing includes all coils in and outside the high temperature
bath. For all experiments, using K2S20g or l^C^Oy as oxidizing agents,
the system was flushed with a ]% HN03 solution for 20-30 min.
-------
SYSTEM DEVELOPMENT
During the early stages in the development of the system,
several studies were undertaken to optimize the analysis conditions.
These studies included mechanical, electrical, as well as chemical
modifications.
Modifications in the Mercury Analyzer. It was observed
that the absorption cell provided by the manufacturer was inadequate
for our purposes. The position of the inlet and outlet tubes was
too far from the quartz windows leaving a dead air space. This re-
sulted 'in the retention of mercury in the cell and slowed the response
time. The response time could not be sufficiently improved by varying
the flow rate of the nitrogen carrier gas. In addition, the volume
of the cell was too large, requiring a much longer sampling period.
In the present cell these problems were corrected as described in
the experimental section. As a result of these modifications, we
observed an increase in the sensitivity of the system, a decrease
in the background level, and a decrease in the time required for the
maximum absorption to take place.
Air or Nitrogen flow rate. Table I gives the relationship
between the scale reading on the recorder and the flow rate of air
used for aspiration, for mercury concentrations of 0.5, 1, 2, 3 and
4 yg/1. Inspection of Table I shows that the scale reading increases
with the increase of the flow rate of air up to a maximum. The max-
imum is reached at a flow rate of 20-25 cm3/min. Above 30 cm3/min,
-------
10
however, the scale reading of the recorder decreases. The variations
in the scale reading are more significant at higher mercury levels.
It should be noted here that the results will vary from one system to
another. The flow rates of the other reagents will, of course, change
the molar concentrations of mercury in the solution to be aspirated
and hence, the response of the mercury analyzer.
It should be mentioned here, however, that the total area
under the peak of a given mercury concentration remained virtually
constant up to 30 cm^/min of air. Peak separation, however, decreases
with the decrease in air flow.
Preservation of Samples and Standard^. It has been recognized
for a number of years " that aqueous solutions of mercury compounds
lose their strength on storage. This result was observed for samples
15A. E. Ballard and C. 0. W. Thornton; Ind. Eng. Chem. 13, 893 (1949).
S. Shimomura, Y. Nishihara and Y. Tanase; Jap. Anal., 17, 1148 (1968)
and 18, 1072 (1969).
stored in glass as well as polyethylene vessels. Although the mechanism
for the loss of mercury is currently unknown, several interpretations
have been given. The absorption of mercury on the surface of the con-
tainer is perhaps the most common of these interpretations. The amount
of mercury lost from aqueous solutions decreases, however, when the
sample is stored in acid solution. ~ Feldman showed that mercury
R. V. Coyne and J. A. Collins, Anal. Chem. 44, 1093 (1972).
18
C. Feldman; ibid., 46, 99 (1974).
-------
11
standards preserved in a solution 5% HN03 + 0.052 K2Cr207 will maintain
their mercury concentrations over a period of 10 days.
In an attempt to establish the stability of the standard mercury
solutions, as well as that of mercury in environmental samples, several
j
solutions were prepared and analyzed over a one month period. Table II
gives data collected on samples prepared in deionized water, surface
water containing industrial waste, sewage treatment plant (STP) effluent
and STP influent. Three different sets of solutions were prepared for
a given sample type: unpreserved, 0.5% HN03 preserved,and 0,5% HNO-^ -
0.05% KgC^Oy preserved solutions. Both polyethylene and glass bottles
were used for the unpreserved samples. All other samples were prepared
in polyethylene bottles. The mercury content of all samples was first
analyzed. Each sample was then spiked with a known amount of HgCl2,
and the total mercury present was determined within 10 minutes of sample
preparation. The volume of the samples was measured using a graduated
cylinder,and hence a difference of 2-3% between the mercury found at
zero time and the sum (Hg present and Hg added) is not significant.
Table II shows that unpreserved standards (samples prepared in
deionized water) lost 20% of their strength within 10 minutes of prepar-
ation and 60% over a 10 day period. Standards prepared in 0.5% HN03
lost 6% and 30% of their strength over a 10 minutes and a 10 day period
respectively. The use of sulfuric acid instead of nitric acid as a pre-
servative did not significantly alter the results, although sulfuric acid
preserved standards were generally 3-5% higher. This could be attributed
to the presence of trace amounts of Hg in sulfuric acid. Increasing the
-------
12
acid concentration up to 6% resulted in a mercury loss of 20% over a 10
day period. The preservation of standards in a solution containing 0.5"'
HN03 + 0.05% K2Cr2Q7, however, resulted in no significant mercury loss
over a four week period. Similar results were obtained for standards
stored in borosilicate glass, with a slight increase in stability over
polyethylene bottle stored solutions.
Further inspection of table II shows that all environmental
samples studied maintained their mercury content over a one month period
when preserved in either 0.5% HN03 or 0.5% HN03 - 0.052 K2Cr207. Although
unpreserved solutions of the same samples exhibit Kg loss, they do so at
a much slower rate than that for standards prepared in deionized water.
The rate of loss decreased with the increase in particulate matter in
the sample. The stability of these samples, could, thus be attributed
to the preferential adsorption of Hg on the particulate matter. The
stability of samples preserved in 0.5% HN03 - 0.05/3 K2Cr207, however,
was independent of the particulate matter content. The stability of
samples preserved in 0.5% HN03 alone, showed a dependence on the parti-
culate matter. The absence of particulate matter will result in lower
stability. It is thus suggested that all samples should be preserved
in 0.5% HN03 - 0.05% K2Cr20?.
Of particular interest is the comparison of the data for unpre-
served samples over a 24 hour period. Here we observe that deionized
water samples lost 30% of their strength, while environmental samples
lost up to 10% of their strength over the same period. This result
bears very heavily on the method of sampling. It is suggested that
-------
13
grab samples are collected followed by immediate preservation with 0.53
HN03 - 0.05% i^C^Oy solution. This is preferred over, say, a 24 hour
non-acidified composit sampling method. Any loss of mercury due to
surface adsorption in a grab sampling method should be recovered upon
the addition of the preservative. Thus it was observed that if a mix-
ture of 0.5% HNO^ - 0.05% K£Cr207 was added to a neutral aqueous solution
of HgCl2 (2 yg/1) which had been left standing for 24 hours, all the Hg
was recovered within 20 minutes. In addition, a comparison (table II)
of the Hg concentration in the samples prior to the addition of the
spike (HgCl2), shows that the nitric-dichromate values are significantly
higher than nitric alone, which in turn are higher than the unpreserved
samples. The difference is attributable to the redissolution of Hg
adsorbed on the surface of the flask, since the- reagents did not show any
measurable Hg contamination.
Comparison of Organic and Inorganic Standards. Methyl mercuric
chloride and mercuric chloride produced the same standard graphs over
the range 0.05 - 6.0 yg/1 Hg. All data in the range 0.05 - 0.5 yg/1
were run on the 10X scale of the mercury monitor and IX scale expansion
for the chart recorder. All data in the range 0.5 - 6.0 yg/1 Hg were
run on the IX scale of the mercury monitor and at the 2X scale expansion
of the chart recorder. Two types of standard graphs were attempted.
The first is a plot of the percent absorption due to mercury versus the
mercury concentration; the second is the absorbance (optical density)
versus the mercury concentration. Both graphs gave very good straight
lines, and the results (for real samples) calculated from both graphs
are indistinguishable. At concentrations of mercury of 10 yg/1 or above,
however, the % absorption graphs are generally non-linear.
-------
14
RESULTS AND DISCUSSIONS
Figures III and IV give typical chart recordings of measurements
made on standard solutions. Recorder plots of 0.5, 1.0, 2.0, 3.0 and
4.0 yg/1 Hg (Fig. Ill) were obtained on the IX scale of the mercury
monitor and scale expansion of 2X on the chart recorder. Attempts to
vary the damping of the instrument (without significantly affecting
the response of the monitor) were unsuccessful in decreasing the base-
line noise. The present chart recordings are done at a damping control
of 10 sec. Figure IV gives the plots of mercury concentrations of
0.05, 0.1, 0.2, 0.3, and 0.4 yg/1, all done on the 10X scale of the
mercury monitor, and a IX scale of the chart recorder. Here again
attempts to decrease the noise level of the baseline beyond what is
given were unsuccessful. The detection limit of the method (defined
as the concentration that gives a signal that is twice the level of
the baseline noise) on the range 0-0.6 yg/1 is 0,05 yg/1. The de-
tection limit could be decreased beyond the 0.05 yg/1 level to perhaps
0.02 yg/1 if an integrator is coupled with the chart recorder, which
would average the baseline noise and hence increase the sensitivity
of the procedure. Inspection of Figures III and IV shows that the
wash sample ratio of 2:1 is sufficient for our system with a complete
return to the baseline between samples. The shape of the peaks is
quite characteristic at all levels of mercury, and with a one minute
sampling time, a steady state concentration of mercury is reached in
-------
15
the absorption cell. This was established by sampling for an extended
period of time and observing that the percent absorption attained is
the same. The reproducibility of the results (precision of the method)
was established by replicate analyses of the same sample. Table III
gives the standard deviations and the coefficients of variations (per-
cent relative standard deviation) at various levels of mercury. Data
for the manual method are also given as a reference. These data were
obtained from standards run during the same day as well as over an
extended time period. Reproducibility data for real samoles were
generally within the standard deviation of the standards (for samples
with small amounts of particulate matter when run on the same day).
Reproducibility data for samples run on different days, however, were
within 2-3 standard deviations of the standards. This could be attri-
buted to sample deterioration, preferential adsorption of mercury on
particulate matter, or day to day changes in the elasticity of pump
tubing. Samples with considerable amounts of particulate matter were
sampled representatively by homogenization using a high speed blender.
The reproducibility of these samples was within 2-3 standard deviations
of the standards.
Since mercury in water can exist as organic mercury, it was
necessary to establish the completeness of the digestion procedure,
as well as the effectiveness of the various chemicals involved in the
break-down of organic mercury compounds to ionic mercury. This is
necessary since SnC^ will not reduce organic mercury under the exper-
imental condition given. It should be mentioned here that it was not
-------
16
necessary to use potassium permanganate nor potassium persulfate for
samples containing inorganic mercury only. In addition, the temperature
of the reaction need not be above room temperature.
Standards containing methyl mercuric chloride, however, required
high temperature (100°C) and the presence of persulfate. Potassium
permanganate alone gave less than 302 recovery of the mercury present.
Potassium persulfate alone was sufficient to recover all the mercury
present. Variation of the concentration of ^2^8 between °-5 " ^ dl'd
not alter the results obtained for methyl mercuric chloride. Since
the variation of the flow rates of reagents and/or the total volume of
solution in the reduction step affects the final value obtained for the
percent absorption on the chart recorder at a given concentration, all
data were obtained relative to mercuric chloride standards. Table IV
gives recovery data for methyl mercuric chloride using various reagent
combinations. The methyl mercuric chloride standard solution used
(obtained from Alpha Inorganic) was found to contain 1% HgC^. This
was established by treating a 100 yg/1 sample of CF^HgCl with SnCl-
and observing an absorbance level 1% of the expected absorbance.
The variation of the concentrations of the various reagents,
however, affected the data obtained for real samples. It was thus
observed that there is a direct correlation between the chemical
oxygen demand (COD) and the amount of persulfate and/or permanganate
required to completely oxidize all organic mercury present. The COO
19
of a sample is defined as "the quantity of oxygen required to oxidize
W. A. Moore, F. J. Ludzack, and C. C. Ruchhoft, Anal. Chem. 23, 1297
(1951)
-------
17
organic and inorganic matter in a waste sample." This definition is
based on acidic dichromate oxidation at the reflux temperature of a
2
50% H2S04 solution with a Ag2S04 catalyst. Since both S20g and Mn04
are excellent oxidizing agents, all organic matter oxidized by dichromate
should also be oxidized by persulfate or permanganate and hence the
correlation between the COD of the sample and the concentration of
these reagents. It was thus observed that the suggested concentrations
12
of 0.5% KMn04 and 0.52 K2$20g by Bennett et. al. , are insufficient
for most samples treated in this laboratory. In the present system,
a 4% K2S2Og (Fig. I) is sufficient to treat samples with a COD of up
to 700 mg/1. Attempts to increase the concentrations of these reagents
were judged inadequate for our purposes, because an increase in KMnO^
concentration would require a large increase in the hydroxylamine
needed to reduce excess MnO^~. Increasing the persulfate concentration
by the use of up to 15% (iNH^)2S2Og solutions, resulted in the formation
of high levels of ozone after the digestion step, and hence, a need
for a high concentration of SnCl2. Since over 90% of water and waste-
water samples that come to this laboratory have a COD value of less
than 500 mg/1, it was decided that a 1% KMnO^ and/or 4% <<2S2Og solutions
are sufficient. Samples with much higher COD levels (above 700 mq/1)
should therefore be diluted. It was also observed that spiked samples
with high COD levels gave a mercury concentration lower than the spike,
Here methyl mercuric chloride should be used as the spike.
Table V gives a comparison between the automated method and
the manual method for river, lake, sewage, and industrial samples. Data
-------
were included for experiments performed using persulfate alone, persulfate-
dichromate, and persulfate-permanganate as digestion solutions. Table VI
gives recovery data of spiked real samples using the above solutions.
Inspection of the two tables shows that there is no significant difference
in the values obtained for the same sample by the various methods studied,
and that potassium persulfate is sufficient as a digestion reagent. Per-
haps the main purpose for permanganate in these experiments is its five
electron oxidation property as compared to the two electron step for per-
?- ?-
sulfate. The electrode potential for the S20g /S04 couple is 2.03 V
while for the MnO^/Mn couple is 1.60, and here it appears that apart
from kinetic effects, the persulfate on a thermodynamic basis is a better
oxidizing agent. The fact that the use of MnO^" alone results in a maximum
of 30% recovery of CHJ-lgCl eliminates the value of MnO*~ for the analysis
of organic mercury compounds.
20
It was eluded to by Kopp, et al. , that the use of Mn04~ might
20
0. F. Kopp, M. C. Longbottom and L. B. Lobring; AWWA; 64, 20(1972).
be required for the oxidation of some interferences such as F^S. Since
persulfate is a strong oxidizing agent, it appears that the permanganate
will not be required for this purpose. In addition, it was observed
that sulfide concentrations as high as 20 mg/1 (as Na^S) do not interfere
with the recovery of inorganic mercury added to distilled water. This
result was obtained in experiments using persulfate, persulfate-permanganat
-------
19
and persulfate-dichromate combinations as digestion solutions. At higher
sulfide ion concentrations, however, negative interferences were observed
in experiments using persulfate alone. In experiments using persulfate-
permanganate or persulfate-dichromate, a positive interference was ob-
served. Other common ions encountered, such as chloride, did not inter-
fere in concentrations of up to 5000 mg CT/1 in all three digestion
solutions. Residual chlorine results in a positive interference, when
the K2$208 manifold is used. For these samples, a solution 3% in
N^OH-HCl-NaCl is to be added to the sample stream immediately after
the digestion step at the rate of 0.3 ml/min. CuS04 did not interfere
in concentrations of up to 1 g/1. Ethyl alcohol, methyl alcohol, glycerol ,
chloroform, and carbon tetrachloride did not interfere when added in
concentrations as high as 0.5*. Major interferences were observed,
however, from benzene and toluene. A maximum tolerance of 500yq/l was
obtained for these compounds. The above illustrates that the use of
KZ^OS as the sole oxidizing reagent in the digestion step is sufficient.
The elimination of KMn04 results in a stable base line and removes inter-
ferences caused by the precipitation of manganese oxides in the tubes.
In addition, high backgrounds generally observed in Hg determinations
using KMnO^ are eliminated.
The present method is suitable for the separate determination
of inorganic and organic mercury. For this purpose, the inorganic mercury
is determined by the removal of all reagents except for the SnCl£ solution
**+
used for the reduction of Hgc . The temperature of the system is maintaine
at room temperature, and the inorganic mercury concentration is read off
-------
20
a calibration curve made of known concentrations of HgCl2 run under
the same conditions. Inorganic mercury as determined by this method
is defined as all mercury compounds that are reduced to elemental
mercury by SnCl2 without predigestion of the sample. The total mercury
in the system is then determined, using the normal digestion and re-
duction steps and read off a calibration curve done under the same
conditions. The difference between total and inorganic mercury is
the amount of organic mercury in the samples. Table VII gives the
date for inorganic and organic mercury content of real as well as
artificial mixtures. No attempts were made to analyze for organic
mercury independently.
-------
21
ACKNOWLCDnKEflT
The authors are greatful for the help received from many
of the personnel of the U.S. Environmental Protection Agency,
Region V, Central Regional Laboratory.
The mention of trade names or commercial products does
not constitute endorsement nor recommendation for use by the
Environmental Protection Agency.
-------
TABLE I
Variation of Scale Reading with Rate of Air Flow
22
Flow Rate3
cm^/min
0
10
15 •
17
19
22
24
25
31
37
Scale Reading
0.5
10.8
12.5
13.0
13.0
12.0
10.0
9.0
1.0
22.0
24.0
26.0
25.0
23.0
20.0
19.0
2.0
32.5
41.0
42.0
44.0
40.0
35.0
32.0
3.0
48.0
58.0
58.5
63
60
55
50
4.0 yg/1
25.0
59.0
i
69.0
72.5
t
76
77
77
75
70
60
aFlow rates are those of the air used for aspiration only.
Full scale 100 division at 50% absorption.
-------
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-------
TABLE III
REPRODUCIBILITY
Hg, Level
ug/1
0.05a
0.1 Oa
0.20a
0.30a
0.40a
0.60a
0.25b
0.50b
0.75b
1.0b
2.0b
3.0b
4.0b
6.0b
Automated
Standard0
Deviation
0.005
0.007
0.01
0.008
0.02
0.04
0.04
. 0.04
0.04
0.04
0.09
0.08
0.2
0.48
Relative Std.
Deviation %
10 %
7
5
3
5
4
17
7
5
4
5
3
5
8
Manual
Standard0
Deviation
O.C63
0.083
0.13
Relative Std.
Deviation %
28.0
8.0
4.0
Standards run using 10X expansion of the Hg monitor (automated system).
"Standards run using IX scale of the Hg monitor and 2X expansion of the
recorder (automated system only).
C8ased on 10 or more replicates.
-------
TABLE IV
Recovery of Known Amounts of Methyl Mercuric Chloride
by KMnOfl, K2Cr207, and K2S208 Oxidation Procedures.^)
CH3HgCl, Added
yg/1
0.5
1.0
2.0
3.0
4.0
Thermal . .
Decomposition*- '
%
17.4
20.0
18.0
23.8
24.2
1% KMn04
%
27.3
25.0
23.4
29.7
31.5
i
2% K2Cr207
%
45.5
40.0
35.9
39.2
40.6
4£ K2S208(c)
o/
/o
100.1
100.5
98.5
103
93.0
U)j3ased on HgCl2 standards.
oxidizing agent added, all other reagents are used, however.
ar results are obtained using ]% KMnO^ - 4% K2S2Oa and
2% K2Cr207 - 4£ :<2S208.
-------
TABLE V
COMPARISON OF AUTOMATED AND MANUAL METHODS
Hg)
Sample Type
Reagent blank
Reagent blank
Well
Stream
Industrial intake
" efflu.
it n it
ii n n
n it n
n n n
N n n
n ii n
ii n n
ti ii n
n n ii
Raw Sewage
n n
n n
n n
n n
n n
n n
n ii
n n
n n
n n
ii ii
n ii
ii n
M it
a n
STP Effluentt
STP Effluent
n n
ii ii
n n
M n
n ii
n n
M II
II II
II II
COD
.
-
<3
90
9
24
26
9
72
120
38
215
179
1480*
4
278
479
521
441
567
292
329
244
554
380
407
441
-
434
447
281
29
237
301
94
225
244
29
448
199
218
Automated _J
« K2S208 '
0.07
<0.05
0.11
0.52
0.15
<0.05
0.05
0.15
0.10
0.19
0.23
1.81
0.28
0.20
0.21
0.55
0.30
0.10
0.22
1.17
0.43
1.50
0.54
0.76
0.18
0.10
0.33
0.64
0.24
0.30
0.30
4£ K2S?08
IT. KMnO/i
<0.05
0.16
<0.05
=0.05
0.45
0.20
0.13
0.15
1.96
0.11
' 0.85
0.30
0.18
0.21
0.42
0.10
0.23
0.95
0.43
1.30
0.18
0.11
0.23
0,18
0.24
4% Kp^Oo I
2* J<2.Cr2p2. '
0.07
0.13
0.16
0.26
I
Manual
<0.2
<0.2
0.8
<0.2
<0.2
<0.2
0.5
<0.2
<0.2
<0.2
0.2
^0.2
2.4
<0.2
0.62
0.27
0.38
oies
0.39
0.32
0.2
0.2
1.0
0.4
0.2
0.2
0.7
0.3
<0.2
0.3
1.0
0.3
1.7
0.5
0.6
0.9
<0.2
<0.2
0.3
0.7
0.3
0.2
0.3
0.2
0.6
0.4
0.3
'Sample diluted by a factor of three before analysis.
Sewage treatment plant effluent.
-------
TABLE VI
RECOVERY OF MERCURY FROM SPIKED SAMPLES
Sample. Type
Reagent blank
Cooling water
Industrial Effluent
it it ii it
it ii n M
ii n n n
n n n n
n n n n
n n n a
n n n n
Raw Sewage
n n
n it
n n
n n
n n
STP Effluent
a ii
n n
n ii
COO
_
30
123
13
26
120
278
252
_
23
261
1 68
120
-
448
597
40
94
218
199
wg/1 Hg
In Sample
<0.05
0.07
0.13
<0.05
0.05
0.13
0.28
0.08
0.08
0.80
1.30
0.50
2.58
0.54
0.68
0.50
2.90
0.4
0.32
0.39
ug/1 Hg
Added
0.11
0.20
0.30
0.10
0.10
3.00
0.50
0.08
0.20
1.00
2.00
2.00
1.30
0.30
1.00
2.00
1.00
2.00
0.40
1.00
ug/1 Hg
Found
0.12
0.28
0.45
0.11
0.13
3.05
0.82
0.15
0.31
1.90
2.70
2.40
2.80
O.S2
1.59
2.80
3.98
2.50
0.78
1.34
% Recovery*
109
103
105
92
87
97
105
94
no
106
82
96
98
98
95
112
102
103
108
•96
*Defined as the percent total mercury recovered.
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APPENDIX IV
-------
Environmental Protection Agency
Central Regional Laboratory
1819 West Pershing Road
Chicago, Illinois 60609
MICRO METHODS FOR THE DETERMINATION OF
NON-FILTRABLE AND FILTRABLE RESIDUES
Mark J. Carter, Madeliene T. Huston and Oliver J. Logsdon II
April 18, 1975
-------
ABSTRACT
Rapid, micro methods for the determination of non-filtrable
and filtrable residues are reported. Non-filtrable residue analysis
of wastewaters is accomplished using up to 10 ml of sample for a de-
tection limit of 1 mg/1. Using the suggested sample sizes, all filtra-
tion work is completed within ten minutes. Filtrable residues are
determined on a 100 ul sample which is dried at 180°C for one-half hour.
Thirty samples can be analyzed for both residue parameters in less
than three hours. Both micro methods were shown to produce results
comparable to the standard methods with better precision.
-1-
-------
The determination of non-filtrable and filtrable residues
are among the oldest determinations in water analysis. While old,
residue analyses remain important in assessing the quality of waste ,
surface and potable waters. At least one residue parameter is
included in a list of significant parameters for assessing the quality
of effluents from each of twenty-two major industrial groups iden-
i
tified in a recent EPA report.
The most widely used procedures for determining filtrable
residue are given in "Standard Methods". Selection of a drying
3 tj, 5
temperature of 103-105°C ' or 180°C is left to the discretion
of the analyst. Howard evaluated both drying temperatures and found
that the value for filtrable residue, based on drying at 180°C,
agreed best with the sum of the determined constituents for most
natural waters.0 The EPA has adopted the 180°C drying procedure
7 g
for routine use. ' However, a large sample volume and hence a
long drying time are required to achieve good precision with the
standard filtrable residue procedure. Another requirement to obtain
good precision is the careful desiccation of the weighing dishes
after sample evaporation.
Allen and Bacon reported a micro method for determining
filtrable residues which requires a substantially smaller sample volume
Q
and shorter drying time than the standard method.' They eliminated
the problem of sample desiccation by placing the weighing chamber
-7-
-------
of a Cahn micro balance in a drying oven at 105°C. Unfortunately,
this drying technique is not applicable to the 180°C filtrable re-
sidue procedure because the maximum operating temperature of the weighing
chamber is 11QOC.
A substantial amount of work has been performed on improving
the standard Gooch crucible-asbestos mat procedure for the deter-
io-it
ruination of non-filtrable residues. Chanin et a!., have iden-
tified the major difficulties with the asbestos mat technique as
being due to variations in asbestos quality, preparation of non-
uniform mats, mat disturbance during handling, and a slow filtration
10
rate. Degen and Nussberger found that the mat must be carefully
washed, before taring and after sample filtration, to avoid erroneous
14
results.
10 11
Chanin et a!., and Nusbaum simultaneously reported similar
non-filtrable residue methods using glass fiber filters which greatly
1 2
reduced problems with mat preparation. Engelbrecht and McKinney
used the membrane filter for non-filtrable residue analysis but re-
ported a slow filtration rate for some samples. Harada et al., also
noted this problem using glass fiber filters and reported a procedure
utilizing a combination filter mat consisting of both coarse asbestos
and a glass fiber disk.
Smith and Greenberg compared and evaluated five of the non-
filtrable residue methods in common use, including the standard
15
procedure. Three glass fiber filtration techniques were compared
to an asbestos mat and a membrane filter method. They found no
-3-
-------
statistically significant bias or different coefficients of variation
between the five methods. However, none of the procedures studied
combines speedy filtration with ease of filter media preparation.
The problem of a slow filtration rate becomes serious when a large
volume of sample must be filtered for filtrable residue analysis.
A fast, efficient and accurate method for determining non-filtrable
residues that combines a minimum of filter handling with rapid
filtration is reported in this paper. A rapid method for deter-
mining filtrable residues using only 100 yl of sample is also reported.
-4-
-------
METHODS
Apparatus. AH weighings were performed on a Mettler ME22 electronic
microbalance equipped with BE22 control and BA25 digital display units
and a Nuclear Products Co. 500 uC Po 210 ionizing source. All of the
filters evaluated are listed in Table I. The Nuclepore 25 mm diameter
0.4 ym standard polycarbonate membrane filter was chosen for routine
use. Sample filtration was performed with a Mi Hi pore thirty-place
membrane sampling manifold using 15 x 125 mm culture tubes to receive
the filtrate. Liquid transfers for non-filtrable residue analysis
were performed with a 1-5 ml or 5-10 ml Oxford Laboratories Macro-Set
pipet with disposable tips. A 100 ul Eppendorf pipet with disposable
tips was used for liquid transfers for filtrable residue determinations.
Cahn 12 mm diameter aluminum pans were used as evaporating dishes for
filtrable residue analysis. Coors 03 12-place spot plates were used
to hold the aluminum pans. Two control standards for filtrable residue
analysis were prepared with NaCl to be 400 and 500 mg/1. Non-uniform
samples were homogenized with a Tekmar model SOT.
Non-Filtrable Residue. Weigh the Nuclepore filters to the nearest
microgram directly out of the box. Pass the filters about 1 inch over
the Po 210 ionizing source in the weighing chamber to reduce the
electrostatic charge. Place the weighed filters in numbered 60 mm
aluminum weighing dishes until they are to be used. Wash and dry the
sample wells and filter supports of the sampling manifold. Load the
filtrate receiving rack with 15 x 125 mm culture tubes and assemble the
manifold as per Millipore Co. instructions. Place the filters on the
-5-
-------
manifold by first dipping each filter in distilled water so they
adhere to the support. Homogenize all non-uniform samples. Choose
a volume of a surface or wastewater to filter so that no more than
2.0 mg of residue will remain. Discard any sample which does not
filter in ten minutes and re-filter a smaller sample volume. Gener-
ally, volumes filtered are 10 ml for a surface water or wastewater
effluent (up to a concentration of 200 mg/1), and 1 ml for grossly
polluted samples (up to a concentration of 2000 mg/1). In addition,
analyze one sample in duplicate and the two filtrable residue control
standards (also used as blank filters) per set of samples. When
filtration is complete, disassemble the sampling manifold, remove
the filtrate receiving rack and reassemble the manifold. Wash each
filter with two 5 ml portions of distilled water. Remove the filters
from the sampling manifold, return them to the numbered aluminum
weighing dishes and place in an oven at 103-105°C for 1/2 hr. Remove
from the oven at one time only the number of filters that can be
weighed before the aluminum pans cool. The final non-filtrable residue
values are corrected for the change in blank filter weights. The cause
for a blank of more than 0.01 mg should be investigated before reporting
the results.
Filtrable Residue. -Weigh the Cahn 12 mm diameter aluminum pans to
the nearest microgram and place on a numbered Coors spot plate. Trans-
fer one hundred ul of each sample to the residue dishes with an
Eppendorf pi pet. Analyze the A and B control standards just like the
real samples. Carry two blank pans through the drying and weighing
process. Correct final filtrable residue values for the change in
blank pan weights. The cause for a blank of more than 0.003 mg should
-6-
-------
be investigated before reporting the results.
RESULTS AND DISCUSSION
Non-Filtrable Residue Method Development. The primary considerations
in developing a new non-filtrable residue method were the ease of
filter media handling and a rapid filtration rate. Harada et al.,
solved the filtration rate problem by using a media that was difficult
to prepare. Most investigators have found glass fiber and membrane
filters easy to use but of limited loading capacity, especially the
latter ones. One proposed solution to this problem is to use larae
11
diameter filters.
The authors decided the best solution to the media handling and fil-
tration problem was to use glass fiber or membrane filters with a
small enough water sample volume that would pass through the media
quickly. Initial experiments with grossly polluted wastewaters, using
25 mm glass and membrane filters, showed that no more than 10 and 5 ml,
respectively, could be filtered in less than 10 minutes. For monitoring
stream and wastewaters the method must be capable of measuring down to
5 mg/1. This means that residues of O.OStng (using 10 ml samples) must
be determined accurately. Since micro balances measuring to the nearest
0.0001 mg are available, the real limitation of the method is the stabil-
ity of the filters.
-7-
-------
Filter Stability. The two major causes of filter instability are
weight loss due to wash-out or "media migration" during filtering
and the volatilization of filter material during the drying process.
The bias introduced by "media migration" during sample filtration
2. 7
can be eliminated by pre-washing the filter.' However, this in-
volves an extra step in the analytical procedure. The thermal
instability problem exists mainly with the membrane-type filters and
13
has only been resolved by drying in a desiccator. However, this
procedure is more time consuming and could result in a positive bias
when compared to the 105°C drying method.
When filtering small volumes, and hence weighing small amounts of
residue, an undetected weight loss from a filter can significantly
bias the results. Ten filters were evaluated for their stability
upon filtering 10 ml of water and drying at 105°C for 1/2 hour. The
results in Table I show the weight losses for three binderless glass
fiber filters (Reeve-Angel 934 AH, Gelman type E and Millipore AP4n)
two glass fiber filters with an acrylic resin binder (Millinore APIS
and AP20) and five different membrane-type filters (Nuclepore,
Millipore MF, Gelman TCM, Millipore HATF, Gelman AN1200).
-8-
-------
TABLE I
WEIGHT CHANGES FOR TEST FILTERS (In Milligrams)5
Mean Weight
before
Mean weight
after
Mean weight
change
Std. dev. of
weight changes
Reeve-Angel ' Gelman
934 AH : Type E
25.38
25.27
-0.118
0.026
36.69
36.59
-0.106
0.020
Mill ipore
AP40
34.30
34.19
-0.117
0.023
Nuclepore
4.303
4.301
-0.003
0.002
Mi Hi pore
AP20
34.45
34.33
-0.121
0.012
Millipor
MF
29.22
28.89
-0.328
0.013
*
Mean weight
before
Mean weight
after
Mean weight
change
Std. dev. of
weight changes
Gelman
TCM
14.25
14.13
-0.120
0.008
Mill ipore
APIS
46.62
46.51
-0.107
Mi 11 ipore
HATF
28.44
28.16
-0.286
i
0.013
0.016
i
Gelman
AN12^n
27.85
27.67
-0,175
0.006
a These values are based on ten replicate experiments with each type of filter.
The filters were pre-weighed, exposed to a 10 ml deionized water filtration,
dried at 105°C for one-half hour and re-weighed.
-9-
-------
The mean weight loss and the standard deviation of weight loss based
on ten replicates were very similar for the three binder!ess glass
filters. The weight loss, if unaccounted for, would bias the results
by an average of 11 ± 5 mg/1 at the 95% confidence level. While the
mean weight loss for the bindered and unhindered filters was similar
the standard deviation of the weight loss for the former has half
that for the latter filters. These experimental results confirmed
the visual observation that the bindered filters were structurally
sounder and sloughed off less filter material during handling. Except
for the Nuclepore filter, the membrane filters exhibited either a
larger mean or standard deviation of weight loss than the glass filters.
The Nuclepore filters showed the smallest mean and standard deviation
of weight loss of all the filters tested.
Table II shows weight loss results from filters which were pre-washed
three times with 10 ml of de-ionized distilled water and dried before
filtering the test 10 ml aliquot of water. Prewashing the glass fiber
filters substantially reduced the mean and standard deviation of weight
loss. Prewashing the cellulose membrane filters substantially reduced
their weight loss during filtration.
Further experiments were performed to determine the cause of weight
loss during the filtration-drying process. Samples of the filters listed
in Table I were dried at 105°C for 1/2 hour. The Nuclepore and ail of
-10-
-------
TABLE II
WEIGHT CHANGES FOR PRE-WASHED TEST FILTERS (In Milligrams)
Mean weight
change
I
Std. dev. of
weight changes
Mil lipore
API 5
-0.012
0.004
Mill ipore
AP20
-0.012
0.011
Mil lipore
AP40
-0.031
0.007
Mi Hi pore
MF
-0.013
0.013
Gelman j
TCM j
i
-0.015
0.019 :
1
a These values are based on ten replicate experiments with each type of filter.
The filters were pre-washed three times with 10 ml of water, dried at 105°C
for one-half hour and pre-weighed. They then were exposed to a 10 ml water
filtration, dried at 105°C-for one-half hour and re-weighed.
-11-
-------
glass fiber filters were stable to 0.002 mg. The other membrane filters
showed substantial weight losses which were less than the total weight
losses from the filtering and drying process. Therefore, the glass
filters lose weight only during the filtering process whereas the cellu-
lose membrane filters lose weight during both the filtering and drying
process. This conclusion was verified by experiments which showed that
the cellulose membrane filters continued to lose weight during the drying
process even after they were thoroughly washed.
As a results of the above experiments the Nuclepore and the Mi Hi pore
AP20 hindered glass filter were chosen to evaluate the micro technique.
A drying time of 30 minutes was shown to be adequate for both filter
types by re-drying a set of particulate laden filters for 24 hours
without any addition weight loss. Due to the low heat capacity of the
filters, they could be weighed directly from the oven without cooling
in a desiccator.
The relative humidity during the course of this work was always below
30% and although a desiccator was not used no filter weight gain from
hygroscopic effects was observed. Tierney and Conner showed that at
100% relative humidity clean glass fiber filters will gain about 5% in
1 9
weight. They also showed weight gains up to 80% for particulate-
laden glass filters at 100% relative humidity. However, at relative
humidities below 55% the weight gain of three different samples was
less than 1%. A weight gain of only 0.24% has been reported for
20
Nuclepore filters immersed in water for 24 hours. This property,
combined with the low tare weight of the
-12-
-------
filter were the deciding factors in choosing the Nuclepore filter
for routine use. If cost is a serious consideration, then pre-washed
glass fiber filters can also be substituted. Whichever filter is
used, it is desirable to maintain the relative humidity below 50%
during the weighing process. It was also determined to be necessary
to keep a Po 210 alpha ionizing source in the balance weighing
chamber to eliminate an electrostatic charge build-up on the Nuclepore fil
Non-filtrable Residue Methods Comparison. The data in Table III compare
results using the micro method and the standard method. ' The ratio
of the micro (using the Nuclepore filter) to the standard method results
is 1.04 ± 0.37 which is not significantly different from one (T-test,
a = 0.05). Smith and Greenberg also reported no statistically significant
bais in results determined using the standard method with membrane and
glass filters. However, their results from the membrane filters were
slightly greater than the glass filters.
For the micro method, the ratio of results using Nuclepore and Mi Hi pore
AP20 filters is 1.07 ± 0.11, which is not significantly different from
one (T-test a = 0.05). However, the results from the Nuclepore filters
are slightly greater than from the glass filters. Cranston and Buckley
reported that both Nuclepore and glass filters quantitatively retained
2 urn beads, whereas the retention of 1 urn beads was 98 and 26% respec-
1 5
tively. Therefore, filtering the same volume of a wastewatar through
Nuclepore and glass filters of the same diameter should produce higher
results for the former filter. The magnitude of the difference would
depend on the particle size distribution of the samples.
-13-
-------
TABLE III
COMPARISON OF MICRO AND STANDARD METHODS FOR THE
DETERMINATION OF NON-FILTRABLE RESIDUE3
Sample Type
Cooling Water
Industrial Eff.
Industrial Eff.
Starch Waste
Well Water
Surface Water
Raw Sewage
Raw Sewage
Treated Sewage
Raw Sewage
Treated Sewage
Refinery Eff.
River Water
Well Water
Refinery Waste
Raw Sewage
Surface Water
Steel Eff.
Food Eff.
Steel Eff.
Steel Waste
Treated Sewage
Treated Sewaqe
Micro Method
Nuclepore
4,4
7,7
2,2
7,6
14,15
192,186
195,204
98,102
156,157
39,43
23,20
20,21
22,24
20,22
339,322
14
907,910
20
11
13
12
Micro Method
Mi Hi pore AP20
<2,4
72,74
2,3
9,10
9,9
13,15
179,183
199,202
94,96
146,151
39,41
21,21
21,19
23,17
22,19
327,320
13,13
890,860
19,19
q
11
9
9
Standard Method
<5
72
<5
12
<5
15
190
184
106
162
320
9
880
15
16
7
7
a All results are expressed in mg/1. Values separated by a comma
are results from duplicate determinations.
-14-
-------
A paper industry report presented data to show that using the standard
method, the larger the volume filtered, the higher the determined
21
non-filtrable residue concentration. Obviously, the larger the
volume of water filtered, the greater the amount of residue collected
and the more difficult it would be to thoroughly wash the filter.
Cranston and Buckley found that a rinse of 25 ml of deionized water
was not sufficient to remove trapped inorganic salts from a 25 mm
16
glass fiber filter after filtering sea water. In addition, if
enough residue was collected to act as a pre-filter, higher results
would be determined for larger volumes filtered.
Several samples were analyzed in triplicate by the micro method using
three different sample volumes. The results in Table IV show that,
using the micro technique, there is no universal increase in non-
filtrable residue results with increasing sample volume. The largest
volume filtered corresponds to no more than 3 mg of residue on a 25 mm
filter with a maximum filtration time of 10 minutes. No problem was
encountered washing the filters. The results reported in the paper
industry report correspond to a 10 mg residue on a 21 mm filter with
filtration times over 2 hours. Obviously, the paper industry filters
could not be washed properly. In order to assure proper washing of
the residue, sample volumes are chosen so that the maximum filtration
time is 10 minutes. This corresponds to a maximum of 2-3 mg residue
depending on the clogging characteristics of the sample. Any filter
that becomes clogged must be discarded to avoid erroneous results such
as those reported in the paper industry report.
-15-
-------
Initial work to define the precision of the method revealed poor
duplication of results for samples with non-uniform particulate
matter. Thereafter, all samples with non-uniform particulate matter
were homogenized with a Tekmar SDT blender. In order to show that
the process of homogenization does not alter the non-filtrable re-
sidue concentration, a raw sewage sample was analyzed ten times
before and after blending. The results (blended, 279.0 ± 4.8 mg/1;
unblended, 280.0 ±8.0 mg/1) show that the mean results are not
affected but the precision is improved by blending the samples.
The precision of the micro method on the variety of sample types
studied is 3 mg/1 below 50 mg/1 non-filtrable residue and 9 mg/1
above 50 mg/1 at the 95% confidence level. The average coefficient
of variation for all samples is 4.0%. Smith and Greenberg reported
a coefficient of variation of 4.2% using the standard method.
The absolute detection limit of the method is 0.01 mg (37}. This
corresponds to 1 mg/1 for a 10 ml sample volume.
Filtrable Residue Method Development. The method of Allen and Bacon
was evaluated for use in combination with the micro non-filtrable
9
residue method described previously. Their method used 50 yl of
sample dried at 105°C for 15 minutes and the residue was weighed to
0.0001 mg with results reported to the nearest 1 mg/1. Initial ex-
periments showed that the extra significant figure gained by weighing
-16-
-------
TABLE IV
CONCENTRATION OF NON-FILTRABLE RESIDUE
VERSES VOLUME OF SAMPLE
Non-Filtrable Residue, mg/la
Sample Volume, ml
Sewage I
Sewage II
5
74"
141
10
72
139
20
73
142
a Determined using Millipore AP20 glass fiber filters. All
filters were washed twice with 5 ml of water.
-17-
-------
to 0.0001 mg was at the expense of several minutes extra weighing
time per sample. Therefore, a 100 yl sample size was chosen, the
residue weighed to 0.001 mg and the results reported to the nearest
10 mg/1. With this sample size, a ten-fold advantage of sample
size to evaporating dish weight exists for the micro over the standard
method.
Howard showed that the figure for total dissolved solids, based
on the weight of residue after drying at 180°C, is close to the
sum of the determined constitutents for most natural waters.6
Therefore, the drying and weighing procedure of Allen and Bacon
was modified to accommodate a 180°C drying procedure. Advantage
was taken of the very large difference in heat capacities of the
aluminum pans and the supporting porcelain spot plate to simplify
the weighing process. After drying for 30 minutes (found to be
sufficient), the spot plates are removed from the oven. As each
aluminum pan is weighed, the remaining ones are kept hot by the
spot plate for up to ten minutes. This technique eliminates the
need for a desiccator.
Comparison of Filtrable Residue Methods. The micro and standard
filtrable residue methods were compared on a variety of samole
types (Table V). The mean ratio of micro to standard method results,
0.99 ±0.18 at the 95f« confidence level, is not significantly
different from one (T-tast* <* = 0.05).
-18-
-------
TABLE V
COMPARISON OF MICRO AND STANDARD METHODS
FOR THE DETERMINATION OF FILTRABLE RESIDUE
Filtrable Residue, mg/1
Sample Type
Refinery waste
Refinery effluent
Well water
River water
Refinery effluent
River water
Refinery effluent
Steel mill effluent
Steel mill waste
Treated Sewage
Lake Water
Lake water
Food process waste
Well water
Starch waste
Industrial waste
Industrial effluent
Lake water
Raw sewage
Micro3
620,590
1930,1940
720,710
370,390
830,820
500,520
910,930
670,680
510,510
880,820
230,240
240,240
1530,1530
350,330
800,790
370,350
860,850
250,250
1250,1240
Treated sewage j 520,520
Treated sewage 630,630
Raw sewage ' 510,500
Standard
635
1930
640
395
820
495
870
670
600
800
270
260
1480
370
710
310
970
250
1210
590
580
580
Spec. Cond., us
970
3370
1120
580
1410
800
1460
1050
780
1230
385
370
2.? 50
610
nan
510
1570
410
2070
850
1070
820
a Values separated by a comma are results from duplicate determinations
-19-
-------
The precision of the micro method was determined from the paired results
in Table V to be 26 mg/1, at the 95% confidence level. At a mean result
of 705 mg/1, this corresponds to a coefficient of variation of 2%.
"Standard Methods" quotes a coefficient of variation of 5% for the macro
2
method. The absolute detection limit, based on three times the standard
deviation of thirty-two blank values, is 0.0021 mg. This corresponds
to a detection limit of 21 mg/1 using a 100 yl sample volume.
There is no method of assessing the accuracy of filtrable residue
g 2.2.
determinations on real samples. Howard and Sokoloff showed that the
loss of some chloride and nitrate are unavoidable in the determination
of filtrable residues. However, the A and B control standards were
used to evaluate day-to-day bias in results. For ten determinations
on different days the values of the A and B standards were 506± 19 and
411 ±13 mg/1, respectively. Specific conductance values were also used to
assess the consistency of filtrable residue measurements. The ratio
of residue to conductivity results in Table V is 0.62 ± 0.08 at the
95% confidence level. This ratio corresponds very closely to that
o o
reported by Rainwater and Thatcher, for comparatively dilute solutions.
For solutions with dissolved salt concentrations exceeding 2000 to
3000 mg/1 or with substantial concentrations of dissolved silica and
organic matter, the ratio may be much higher. For waters high in
acidity or alkalinity the ratio can be much lower than 0.62. The
cause of a filtrable residue to conductivity ratio outside of n.62 ± 0.1
should be investigated before any results are reported.
-------
ACKNOWLEDGEMENTS
Credits
We thank Dr. Billy Fairless, Chief, Chemistry Branch, Central
Regional Laboratory, for his critical evaluation of alternative
filtrable residue drying procedures.
Authors
Mark J. Carter, Madeliene T. Huston and Oliver J. Logsdon II
are chief, chemical technician and chemist, respectively, of
the Inorganic Section, Central Regional Laboratory, Environmental
Protection Agency, Chicago, Illinois.
The mention of trade names or commerical products does not constitute
endorsement or recommendation for use by the Central Regional Laboratory,
or the Environmental Protection Agency.
-21-
-------
REFERENCES
1. "Handbook for Monitoring Industrial Wastewater", U.S. Environmental
Protection Agency, Washington, D.C. (1973).
2. "Standard Methods for the Examination of Water and Wastewater",
13th Ed., Amer. Pub. Health Assn., New York, M.Y. (1971).
3. "Official and Tentative Methods", Assoc. Official Agr. Chem.,
pp. 35-6 (1916).
4. Mason, W. P., "Examination of Water", 3rd ed.s Wiley, pp. 22-4
(1908).
5. Dole, R.B., U.S. Geol. Survey, Water Supply Paper 236, pp. 13-15,
30-1 (1909).
6. Howard, C.S., "Determination of Total Dissolved Solids in Water
Analysis", Ind. Eng. Chem., 5_, 4 (1933).
7. "Manual of Methods for Chemical Analysis of Water and Wastes",
U.S. Environmental Protection Agency, Wash., O.C. (1974).
8. Federal Register, 38_, 38759 (1973).
9. Allen, H.E. and Bacon, C.W., "Rapid Determination of Filtrable
Residue in Natural Waters", J. Amer. Water Works Assoc., 61,
355 (1969).
10. Chanin, G., et al., "Use of Glass Fiber Filter Medium in the
Suspended Solids Determination", This Journal , 30_, 1062 (1958).
11. Nusbaum, I., "New Method for Suspended Solids", This Journal,
30_> 1067 (1958).
12. Engelbrecht, R.S., and McKinney, R.E., "Membrane Filter Method
Applied to Activated Sludge Suspended Solids Determinations",
This Journal, 28_, 1321 (1956).
13. Harada, H.M., et al., "Modified Filtration Method for Suspended
Solids Analysis", This Journal, 45_, 1853 (1973).
14. Degen, J. and Nussberger, F.E., "Notes of the Determination of
Suspended Solids", This Journal, 28_, 237 (1956).
15. Smith, A.L. and Greenberg, A.E., "Evaluation of Methods for
Determining Suspended Solids in Wastewater," This Journal,
35, 940 (1963).
-22-
-------
16. Cranston, R.E. and Buckley, D.E., "The Application and Performance
of Microfliters in Analyses of Suspended Particulate Matter", un-
published manuscript, Bedford Institute of Oceanography, Dartmouth,
Nova Scotia, Canada (1972).
17. Jenkins, D., "Analyses of Estuarine Waters", This Journal, 39,
159 (1967).
18. Winneberger, J. H., et al., "Membrane Filter Weight Determinations",
This Journal, 35., 807 (1963)
19. Tierney, G.P. and Conner, W.D., Amer. Inc. Hygiene Assn. J., 28.
363 (1967).
20. "Specifications and Physical Properties", Nuclepore Corporation
(1973).
21. "A Preliminary Review of Analytical Methods for the Determination
of Suspended Solids in Paper Industry Effluents for Compliance
with EPA - NPDES Permit Terms", National Council of the Paper
Industry for Air and Stream Improvement, Inc., New York, N.Y. (1975)
22. Sokoloff, V.P., "Water of Crystallization in Total Solids of
Water Analysis", Ind. Eng. Chem., 5_, 336 (1933).
23. Rainwater, F. H. and Thatcher, L. L., "Methods for Collection
and Analyses of Water Samples", Geological Survey Water Supply
Paper 1454, Washington, D.C., p. 83 (1960).
-23-
-------
APPENDIX V
-------
CHLS 05APR
REVI
DSN=CNCRLS.RGD.IL.DW04 ON TS0009 04/19/75
•STUDY DESCRIPTION
STATTYPE SMPLDAY ATLABBY OUEDATE ACCOUNT-NUMBEf
77777777 03FE875 05FE875 03MAY75
- ILLINOIS
-SAMPLE DESCRIPTIONS
STATTYPE DEEP T M NO ENQDATE TIME PRLU
NPAR NLOG
96 73
>»REGION
L48IDNUM
14045
14046
14047
14048 %
14049
14050
14051
14052
14053
14054
14055
14056
14057
14058
14059
14060
14061
14062
14063
14064
14065
14066
14067
14068
14069
14070
14071
14072
14073
14074
14075
14076
14077
14078
14079
14080
14081
14082
14083
14084
14085
14086
14087
14088
14C89
14090
14091
U092
AGENCYID UNLOCKEY ST
77
V DRINKING WATER STU
STORETID COLLDAY TIME
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
'750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203 '
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
-------
14093 750203
14094 750203
14095 750203
14096 750203
14097 750203
14098 750203
14099 750203
14100 750203
14101 750203
14102 750203
14103 750203
14104 . 750203
14105 750203
14106 750203
14107 750203
14108 750203
14109 750203
14110 750203
14111 750203
14112 750203
14113 750203
14114 750203
14115 750203
14116 750203
14117 - 750203
>»14045 » HN03 REAGENT BLANK
>»14046 » H2S04 REAGENT BLANK.
>»14047 » NAOH REAGENT BLANK
>»14Q4S » CUS04/H3P04 REAGENT BLANK
»>14049 » OPEN
>»14050 » CAIRO RAW WATER SERIES A —
>»14051 » CAIRO RAW WATER SERIES B
»>14Q52 » CAIRO FINISHED WATER SERIES A
>»14053 » CAIRO FINISHED WATER SERIES 8
>»14054 » CHESTER RAW WATER SERIES * —
>»14055 » CHESTER RAW WATER SERIES B
>»14056 » CHESTER FINISHED WATER SERIES
»>14057 » CHESTER FINISHED WATER SERIES
»>14053 » CHESTER RAW WATER SERIES 4
>»14059 » CHESTER RAW WATER SERIES 8
>»14060 » CHESTER FINISHED WATER SERIES
»>14061 » " CHESTER FINISHED WATER SERIEb
>»14062 » QUINCY RAW WATER SERIES A
>»14063" » QUINCY RAW WATER SERIES 3
»>14064 » QUINCY FINISHED WATER SERIES A
>»14065 » • QUINCY FINISHED WATER SERIES 8
>»14066 » CARLYLE RAW WATER SERIES <\
>»14067 » CARLYLE RAW WATER SERIES 8
>»14068 » CARLYLE FINISHED WATER SERIES A
»>14069 » CARLYLE FINISHED WATER SERIES B
»>14070 » ROYALTON RAW WATER SERIES A —
>»14071 » ROYALTON RAW WATER SERIES B
>»14072 » ROYALTON FINISHED WATER SERIES A
>»14Q73 » ROYALTON FINISHED WATER SERIES 8
>»14074 » FAIRFIELD RAW WATER SERIES A ~-
>»14075 » FAIRFIELD RAW WATER SERIES R
O
37
A
8
A
B
O
-------
>»14076
»>14077
>»14078
>»14079
>»14080
>»14081
»>14082
>»14083
>»14084
>»14085
>»14086
>»14087
>»14088
>»14089
>»14090
>»14091
>»14092
>»14093
>»14C94
>»14095
>»14096
>»14097
>»14098
>»14099
>»14100
>»1
»>1
>»1
>»1
»>1
»>1
>»1
>»1
4102
4103
4104
4105
4106
4107
4108
4109
»>14113
>»14H5
»>14H6
FAIRFIELD
FAIRFIELD
MT.CARMEL
MT.CARMEL
MT.CARMEL
MT.CARMEL
A
8
FINISHED WATER SERIES
FINISHED WATER SERIES
RAW WATER SERIES A —
RAW WATER SERIES B
FINISHED WATER SERIES
FINISHED WATER SERIES
WATER SERIES A -
NEWTON RAW WATER SERIES 8
NEWTON FINISHED WATER SERIES
NEWTON FINISHED WATER SERIES
DANVILLE RAW WATER SERIES A
DANVILLE RAW W-ATER SERIES B
DANVILLE FINISHED WATER SERIES
DANVILLE FINISHED WATER SERIES
PEORIA RAW WATER SERIES A
RAW WATEP, SERIES B
FINISHED WATER SERIES
FINISHED WATER SERIES
HAW WATER SERIES A
RAW WATER SERIES 8
FINISHED WATER SERIES
FINISHED WATER SERIES
ISLAN5, RAW WATER SERIES
ISLAND
A
8
A
B
PEORIA
PEORIA
PEORIA
PEORIA
PEORIA
PEORIA
PEORIA
A
B
A
B
A
a
ROCK
ROCK ISLAND RAW WATER SERIES
ROCK ISLAND FINISHED WATER SERIES
ROCK ISLAND FINISHED WATER SERIES
STREATOR RAW WATER SERIES A -
STREATOR RAW WATER SERIES 8
STREATOR FINISHED WATER SERIES A
STREATOR FINISHED WATER SERIES B
3?.
7,4^
1>37
• Mo.H[3*0 S
-------
FPA-CRL S0003 OA S0001 OA 39782 OA S0002 OA S0004 OA 39330 OA S0005 OA *
-1975 TREFLAN HC3ENZ LINDANE B8HC DICLONE ALDRIN ZYTRON *
SAMPLE *H|_ SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL *
LOG NO, UG/L UG/L UG/L UG/L UG/L UG/L UG/L *
.4050 :<0.002 :0.010
.4052 :<0.002 t<0.002
.4054 :<0.002
K0.002
:<0.002
:<0.002
:<0.002
<0.002 .
,<0.002
<0.002
! <0.002
: <0 .002
<0.002
K0.002
.<0.002
.<0.002
: <0.002
.<0.002
.<0.002
<0.002
<0.002
<0.002
<0.002
0.004
<0.002
<0.002
<0.002
<0.002
<0.005
<0.005
<0 .005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0,005
<0.005
< 0.0 05
<0.005
<0.005
<0,005
<0.005
•< 0 . 0 0 5
<0.005
<0 .005
<0.005
<0.005
<0 .005
<0.005
<0.005
<0.005
<0.005
<0 .005
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
-------
c-PA-CRL
1975
SAMPLE
LOG NO.
14050
14052
14054
14056
14058
14062
14064
14066
14068
14070
14073
14074
14076
14078
14080
14082
14084
14086
14088
14090
14092
14094
14096
14098
14100
14102
14104
14106
14108
14114
14116
•IL.OW04
39430 OA
ISOOHIN
WHL SMPL
UG/L
:<0.003 :
:<0.003 :
:<0.003 :
:<0 .003 :
:<0.003 :
:<0.003 :
: < 0 . 0 0 3
:<0.003 :
:<0.003 :
: < 0 . 0 0 3
:<0.003
:<0.003 :
:<0.003 :
:<0.003 :
:<0.003 :
:<0.003 :
:<0.003 :
:<0.003 :
:<0'.OC3 :
:<0.003 :
: < 0 . 0 0 3
:<0.003 :
:<0.003 :
:<0.003 :
:<0.003
;<0.003 :
:<0.003 :
:<0.003 :
: < 0 . 0 0 3
:<0.003 :
:<0.003 :
3P
REGION V
39420 OA
HCHLR-EP
WHL SMPL
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
UG/L
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
9P
DRINKING
S0006 OA
CHLOROAG
WHL SMPL
<0
<0
<0
0.
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
<0
UG/L
.002 ' :
.002 :
.002 :
004 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
. 002 ' :
.002
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
.002 :
10P
S0007 OA
DDE OP
WHL SMPL
UG/L
<0.003
<0.003
<0.003
<0.003
<0»003
<0.003
<0.003
0.008
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
IIP
*
»
«
*
•
»
•
»
•
«
•
•
•
»
*
»
•
•
•
•
»
•
•
*
•
»
•
•
•
«
•
•
«
•
«
«
•
•
*
»
I
•
•
•
*
»
•
»
*
•
•
*
•
*
WATER STUDY -.ILL
S0008 OA S0009 OA S0010 OA
DDE P?
ODD OP
DDT OP
WHL SMPL WHL SMPL WHL SMPL
UG/L
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0,003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
< 0 . 0 0 3
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
12P
INOIS
UG/L
!<0.003
:<0.003
:<0.003
:<0.003
:<0.003
s<0.003
: < 0 . 0 0 3
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
;<0,003
:<0.003
:<0.003
:<0.003
: <0.003
:<0.003
:<0.003
:<0.003
:<0.003
: < 0 . 0 0 3
:<0.003
:<0.003
13P
UG/L
:<0,003
:<0.003
: < 0 . 0 0 3
:<0.003
:<0.003
: < 0 . 0 0 3
:<0.003
: < 0 . 0 0 3
:<0.003
' :<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
: < 0 . 0 0 3
:<;0.003
:<0.003
:<0.003
: < 0 . 0 0 3
:<0.003
: < 0 , 0 0 3
:<0.003
: < 0 . 0 0 3
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
14P
: 6S
: SS
: IDS
: 125
: 143
:18S
:20S
:22S
:24S
:26S
J28S
:30S
:32S
:34S
:365
:38S
:40S
:42S
: 445
:46S
:48S
:50S
:52S
:54S
:56S
: 5 3 S
:60S
:625
:64S
:70S
:7.2S
o
&
-------
EPA-CP.L S0011 OA S0012 OA S0013 OA S0014 OA 39480 OA S0020 OA S0021 OA
1975 ODD PP DOT PP CAR8PHTH MIREX MTHXYCXR 2, 4-0: IP DN8P
SAMPLE WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L
14050
14052
14054
14056
14058
14062
14064
14066
14068
14070
14073
14074
14076
14078
14080
14082
14084
14086
14088
14090
14092
14094
14096
14098
14100
14102
14104
14106
14108
14114
14116
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003~
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003 :
<0.003
<0.003 !
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003 !
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
'0.006
<0.003
0.068
K0.003
<0.003
' <0.003
<0.003
<0.003
<0.003
.<0.003
:<0.003
<0.003
•<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0^.003
<0.003
<0.003
<0.003
<0.003
<0.003
0.012
><0.003
<0.003
<0.003
<0.003
'<0.005
<0.005
<0.005
<0.005
'<0.005
<0.005
<0 .005
<0 .005
<0.005
<0.005 i
.<0.005
<0.005
<0.005 !
:<0.01
:<0.01
:<0.01
:<0.01
:<0.01
:<0.01
K0.01
:<0.01
:<0.01
:<0.01
:<0.01
: <0.01
:<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
:<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
< 0 . 0 I
<0.01
<0.01
<0.01
<.02
<.02
<.02
<.02
<.02
<.02
<.C2
<.02
<.02
<.02
<.02
<.02
<«02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<1 : 6
<1 '• 3
:io
<1 : 12
: 14
<1 :13
<1 520
<1 :22
<1 :24
<1 :26
<1 :29
<1 :30
<1 :32
<1 :34
<1 :36
<1 :3S
<1 !40
<1 :42
<1 :44
<1 :46
<1 :48
<1 :50
<1 :52
<1 :54
<1 :56
<1 :53
< 1 : 6 0'
<1 :62
<1 :64
< 1 : 7 Oi
<1 :7
15? 16P 17P 18? 19P 20P 21P
.IL.DW04 REGION v DRINKING WATER STUDY - ILLINOIS
-------
EPA-CRL 39770 OA S0023 04 39380 OA 39390 OA 39460 OA S0027 OA S0028 OA
1975 OCPA ENDOS I DIELORIN ENDRIN CLRRNZLT ENQOS II NITROFEN
SAMPLE WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L
14050
14052
14056
14062
14064
14066
14068
14070
14073
14074
14076
14078
14080
14082
14084
14086
14088
14090
14092
14094
14096
14098
14100
14102
14104
14106
14108
14114
14116
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003 •
<.003
<.003
<.003
<.003
<.003
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<,005
<.005
<.005
.004
<.003
.007
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
.011
.006
<.003
<.003
<.003
<.003
<.003
<.003
<,003
<.003
<.003
<.003
<.003
<.003
<.003
.004
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.01
<,01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.oi
<.01
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<,005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005 J 6
< . 0 0 5 : 8
<.005- :12
<.005 : 13
<.005 :20
<.005 :22
<.005 :?4
<.005 :26
<.005 :29
<.005 : 30
<.005 :32
<.005 :34
<.005 :36
< . 0 0 5 : 3 8
<.005 :40
<.005 :42
<»005 :4<+
<.005 :<«.6
<.005 :48
<.005 :50
< ,005 : 52
<.005 :5±
<.005 :56
<.005 :58
<.005 :60
<.005 :62
< . 0 0 5 : 6 4.
<.005 : 70
<.005 :72
22P 23P 24P 25P 26P 27P 28P
.IL.OW04 REGION V DRINKING WATER STUDY - ILLINOIS
-------
EPA-CRL S0029 QA S0030 OA S0031 OA S0026 OA 39808 OA 39570 OA S0016 CA
1975 245-TtIO PROLAN BULAN OEHP TED-IQN DlAZINON DYFONATE
SAMPLE WHL 3MPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL rtHL SMPL WHL SMPL
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L
14050
14052
14C54
14056
14062
14064
14066
14068
14070
14073
14074
14076
14078
14080
14082
14084
14086
14088
14090
14092
14094
U096
14098
14100
14102
14104
U106
14108
14114
14116
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.0l
<.01
<.01
<.01
<.01
<.0l
<.01
<.01
<.01
<.0l
<.01
<.01
<.0l
<.0l
<.01
<.01
<.0l
<.0l
<.01
<,01
<.01
<.01
<.01
<.01
<.01
<.0l
<.0l
<.01
<.01
<.01
<.01
<.01
<,01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01 '
<.01
<.0l
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
1
3
3
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1 -
<1
<1
<1
<1
<1
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.OL
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<,01
<.01
<.01
<.01
«.01
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1 -
<1 :
<1 :
<1 : 1,
<1 : 1
<1 :l
<1 :2
<1 :2
<1 :2
<1 :2
<1 :2
<1 :3.
<1 :3
<1 :3
<1 :3
<1 :3
<1 : 4
<1 :A
<1 !4
<1 :4
<1 :4,
<1 :5
<1 :5
<1 :5
<1 :5
<1 :5
<1 :6
<1 J6
<1 :6
<1 :7
<1 :7
29P 30P 31P 32P 33P 34P 35P
.IL.OW04 REGION V DRINKING WATER STUDY - ILLINOIS
-------
EPA-CRL S0017 OA S0032 OA 39600 OA 39530 OA 39540 OA S0033 OA 39398 OA
1975 RONNEL OURSBAN MPARATHN MALATHN PARATHN OEF ETHION
SAMPLE «*HL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L
U050
14052
14054
14056
14062
14064
14066
14068
14070
14073
14074
U076
14078
14080
14082
14084
14086
14088
14090
14092
14094
14C96
14098
14100
14102
14104
14106
14108
14114
14116
-------
EPA-CRL S0018 OA S0034 OA 39580 OA S0035 OA S0036 OA S0037 OA 39488 OA
1975 PHENCAPT £PN GUTHIQN PHOSALQN AZINFOSE COUMAFOS AROCLOR
SAMPLE WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL 1221
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L
U050
14052
14054
14056
14062
14064
U066
14068
14070
14073
14074
14076
14078
14080
14082
14084
14086
14088
14090
14092
14094
14096
14098
14100
14102
14104
14106
14108
14114
14116
^ i
» l » x CI
<1 : <5
<1 : <5
<1 : <1
<1 * £ C*
+ * ^ j
<1 :<5
ji 1 • x C
^ A * ^ j
<1 :<5
<1 :<5
<1 : <5 '
<1 : <5
<1
<1
<1
<1
< i
<1
<1
-------
EPA-CRL
1975
SAMPLE
LOG NO.
14050
14051
14052
14053
14054
14055
14056
14057
14058
14062
14063
14064
14065
14066
14067
14068
14069
U070
14071
14072
14074
14075
U076
14077
14078
14079
14080
14031
14082
14083
14084
14085
14036
14087
14088
14089
14090
14091
14092
14093
14094
14095
14096
14Q97
14098
14099
14100
14101
14102
14103
14104
14105
U106
14107
14108
14109
14114
39496 OA
AROCLOR
1242
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0,3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
39500 OA
AROCLOR
1248
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
39504 OA
AROCLOR
1254
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3 -
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
39503 OA
AROCLOR
1260
UG/L
<0.4
<0.4
<0.4
<0.4
<0,4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4 '
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0 .4
<0 .4
<0»4
<0.4
<0.4
<0.4
<0 .4
<0.4
<0 .4
<0 .4
S0047 OA
METHE CL
TOT VOL
UG/L
1
<0.5
<0.5
<0.5
<0 .5"
<1
<0.5
<0.2
<0.5
<0.5
<0.5
<0.5
<0.5
2.6
<0.5
<0.5
<0.5
<1
15
<0.5
<0.5
<1
<0.5
<1
<0.5
<0 .5
<0.5
<0.5
S0039 OA
CCL4
TOT VOL
UG/L
2
1
<1
<1
<2
<1
<0.5
<1
<1
<1
<1
<1
<2
<0.5
<1
<1
<1
^ i
^ "1
1.3
<1
4,
1.3
< i
-------
14115 : : : : :<0.5 :<1 :<1 : 71!
14116 :<0.3 :<0.3 :<0.3 :<0.4 : : : :72!
U117 : t :' : ; < 1 :<1 :30 :73!
50P 51P 52P 53P 54P 55P ' 56P <
•IL.DW04 REGION V DRINKING WATER STUDY - ILLINOIS ^
-------
;PA-CRL S0056 OA 50040 OA S0041 OA 50042 OA *i
1975 C2H4CL2 CHCL28R CHCL8R2 CH3R3 »I
;AMPLE TOT VOL TOT VOL TOT VOL TOT VOL . *i
OG NO. UG/L UG/L - UG/L UG/L *I
'051
.053
055
.057
,063
.065
.067'
,069
,071
,072
,075
,077 .
079
081
033
095
087
089
091
093
095
097
099
101
103
105
107
109
115
117
<1 : <0.2
< 1 : 1 1
<2 :<0.5
<1 • :17
<2 : <0 .5
<1 :13
< 2 : < 0 . 5
<1 :20
< 1 : < 0 . 5
<1 :29
<2 :3
<2 :16
<1 :<0.5
<1 515
<1 :<0.5
<2 :5
<2 :<0.5
<2 :6
1 : < 0 . 5
<1 :l
6 • : < 0 . 5
<1 :o.6
<5 :ll
<1 :8.3
2 :<0.5
<1 :14
<2 :<0.5
<1 :10
<1 :<0.5
< 1 : 1 3
0.3 to. 6
4 :o.8
<0.5 : <0.5
1.1 :<0.3
<0.5 :<0.5
0,5 : <0 .2
< 0 . 5 : < 0 . 5
2 :0.6
<0.5 :<0.5
6 :<0.1
<0.5 :<0.5
1.4 :<0.3
<0.5 r<0.5
1 :<0.5
<0.5 :<0.5
4 :i.3
<0.5 r<0.5
1 :o.7
<0.5 :<0.5
0.5 :0.4
<0.5 :<0.5
0.5 :0.3
<0.5 :<0.5
0.4 : <0.2
<0.5 :<0.5
1.7 :l .4
< 0 . 5 : < 0 . 5
1.1 :<0.2
<0.5 :<0.5
2 :<0.2
~
: ?S*I
: 95*1
: 11S*I
: 13S*I
: 195*1
:21S*I
S23S*I
:25S*I
:27S*I
:28S*I
:31S*I
:33S*I
:35S*I
:37S*I
:39S*I
:41S»I
:43S*I
:45S*I
:47S»I
:49S*I
:51S*I
:53S*I
:55S*I
:57S*I
:59S*I
:61S*I
:63S*I
:65S*I
:71S»!
:73S*I
57P 58P 59P 60P 61P 62P 63P »*I
L.DW04 REGION V DRINKING WATER STUDY - ILLINOIS »*I
-------
A-CRL
975
MPLE
G NO.
50
52
54
'59
62
64
66
68
70
72
74
76
78
80
!S2
34
186
!88
)90
)92
)94
196
398
.00
.02
.04
106
108
110
114
116
_.DW04
01067 MW 00916 M
NICKEL CALCIUM
NItTOT CA»TOT
UG/L MG/L
:34.2
: 4 1 . 4
:38.5
:43.4
:51.6
:35.7
:54.0
:68.9
:50.5
:50.5
:28.3
:23.4
:51.9
:37.3
:62.5
:49.9
555.7
:45.2
:91.5
:91.0
:92.7
:91.4
:52.1 '
:46.3 •
:72.1
:61.7
:67.2
:29.2
•
-------
3A-CRL
.975
iMPLE
DG NO.
350
352
354
359
362
364
366
368
370
372
374
376
378
380
382*
384
336
388
390
392
394
396
398
100
102
104
106
108
110 .
114
116
_.DW04
010<+5 MW
IRON
'FE.TOT
UG/L
:1790
:<20
:2310
:40
!440
:<20
:450
:90
:82
:<20
:1350
:<20
:1870
:130
:2810
:<20
:290
:<20
:135
:<20
:135
:<20
:140
:28
:130
:130
:74Q
:38
:<20
:1600
:85
71P
REGION
01055 MW
MANGNESE
MNfTOT
UG/L
:240 :
: <5 :
:260 :
• <5 :
:160 :
:<5 :
:130 :
: 1 7 :
:65
:B :
:240 :
:20 :
:190 :
J25 :
:320 :
:<5 :
:24
:<5 :
:760 :
ill I
:710 :
:8 :
:33
: <5 :
t <5 :
:<5 :
:92 :
: <5 :
: <5 :
: <5 :
:<5
72P
V DRINKING
01092 MW 01002 MW 01051 'M
ZINC ARSENIC
ZN,TOT AS, TOT
UG/L UG/L
25
<5
<5
c
10
<5
<5
<5
<5
<5
20
<5
17
21
<5
5
93
3
<5
<5
<5
<5
10
<5
<5
<5
<5
<5
<5
<5
<5
2
<1
9
<1
<1
<1
1
<1
1
<1
5
<1
10
< 1
4
<1
1
<1
^
<^
i
^ ^
^ j^
^ J,
<^
i
<1
^ X
£ 1
1
<1
<1
<1
<1
73P 74P
WATER STUDY - i
LEAD
PB,TOT
UG/L
: 13
:2
• 15
:3
:4
: <2
:3
:2
: <2
:3
:7
: <2
: 13
:2
:4
:2
:4
:2
: <2
:3
: <2
:2
:2
:2
:2
:5
:3
: <2
: <2
: <2
:2
75P
LLINOIS
* 01027 MW 01077 MW
CADMIUM SILVER
CO, TOT AG,TOT
UG/L UG/L
: 0 .4
:<0.2
' I • 1
:<0.2
:<0.2 .
:<0,2
:<0.2
:<0.2
:<0.2
:<0.2
:0.3
:<0.2
:0.4
:<0.2 . '
:<0,2
s<0,2
:<0.2
:<0.2
:<0.2
: < 0 . 2
:<0.2
:<0.2
:0.3
:0.3
:<0,2
:<0.2
:<0.2
:<0.2
: < 0 . 2
:<0.2
J<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0»2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
76P 77P
*K
*K
»K
*K
! 6S*K
: 8S*K
: 10S*K
: 15S*K
: 18S*K
:20S*K
:22S*K
:24S*K
:26S»K
:23S»K
:30S*K
:32S»K
:34S*K
:36S*K
:38S*K
!40S*K
:42S*K
;4iS*K
I46S*K
:48S»K
:50S*K
: 52S*K
:54S*K
:56S-*K
:53S*K
:60S»K
:62S»K
:64S*K
! 66S*K
:70S*K
:72S*K
«••»«
-------
-
A-CRL 01147 MW 01007 MW *<-
975 SELENIUM BARIUM DI-
MPLE SE»TOT BAiTOT *L
G NO. UG/L UG/L *L
50 :<5
52 :<5
54 :<5
59 :<5
62 :<5
64 :<5
566 :<5
)68 :<5
)70 :<5
172 :<5
174 :<5
176 t<5
178 :<5
180 :<5
182 :<5
384 :<5
086 :<5
088 :<5
090 :<5
092 :<5
094 . :<5
096 :<5
098 :<5
100 :<5
102 :<5
104 :<5
106 :<5
108 :<5
• 110 :<5
• 114 :<5
•
,
,
.
-
: 6S*L
: 8S*L
: 10S*L
: 15S*L
: 18S*L
:20S*L
:22S*L
:24S*L
:26S*L
:28S*L
:30S»L
. :32S*L
: 34S*L
:36S*L
:33S*L
:40S*L
:
-------
A-CRL
975
MPLE
G NO.
50
52
54
56
62 -
64
66
68
70
72
74
76
78
80
82
84
86
88
90
92
94
96
98
.00
,02
.04
.06
.08
.14
.16
..OW04
00530 IM
RESIDUE
TOT NFLT
MG/L
: ]>6
: <3
:162
: <3
: 19
:<3
:44
:4
: 1 1
:3
:153
:3
:274
:<3
:3
:<3
- 10
:<3
:4
: <3
: 14
: <3
:6
:<3
t 15
:6
131
: 13
:4
:<2
85P
REGION
70300 IM
RESIDUE
DISS-180
C MG/L
:150
:190
:200
:180
:200
:180
:290
:2.90 •
r220
:200
:160
i230
:210
:240.
:310
:310
:290
:280
:490
:420
:480
:480 -
:225 •
:200
:370
:350
:40Q
:250
1230
:310
86P
00095 IM
CNOUCTVY
AT 25C
MICROMHO
:310
:369
:376
:341
:471
:356
:494
:57S
:466
:456
:323 .
:389
:412
:441
:503
:505
:459
:468
:337
:842
:842
:843
:398
:454
:627
:638
:595
:433
:453
:461
87P •
00945 IM
SULFATE
S04
MG/L
:5l :
:65 :
:48
:49 :
:32 :
:42 J
:4b :
:96
:150 :
:149 :
:60 :
:91 t
:48 :
:68 :
:38
t36 :
:40 :
:57
155 :
:57
:57
:57 :
: 13 :
:58 :
175 :
175 :
j 101 ;
:103
:22 :
: 19 :
88? .
V DRINKING WATER STUDY - ILL
009^0 IM
CHLORIDE
CL
MG/L
X t3
1 O
17
23
20
24
23
28 '
19
22
33
35
17
21
7
9
14
18
27
29
25
28
12
16
21
24
18
21 -
7
10
39P
INOIS
00956 IM
SILICA
SI02
MG/L
:6.8
:7.3
:8.3
:7.7
:9.5
:a.5
:6.0
:5.4
1 1 »8
1 1 »3
:6.2
:5.4
:7.0
:6.7
:15.3
:15.8
:7.6
:7.6
118.0
:18.3
J17.8
:13.2
:10.0
:9.Q
54 »a
:5.2
:9»4
:7.2
:ia,2
:18.6
90P
00410 I
T ALK
CAC03
MG/L
:68
:72
: 107
:63
5175
:92
: 162
: 144
:45
531
:32
:30
:120
5106
:213
:2ni
:142
• 115
'.368
:364
:364
:354
:152
: 134
: 197
:187
: 166
:49
1 206
:201
91P
M *l
*l
»'
»!
: 6S*i
: 3S*
: 10S*
:i2S*f
: 18S*:
:20S»<
:22S*
:24S»:
J 26S*
:28S*.
:30S*N
:32S*-
: 34S».
:36S*.
: 335*
: 40S<*>
: 42 S*'
: 44S*
: 4 6 S * >
:48S*
: 5 0 S *
:52S*
: 5^S*.
: 56S*
:53S*.
: 60S*.
: 62S*.
: 64S*'
: 70S*
:72S»
*•».
**•'
-------
'A-CRL
.975
.MPLE
)G NO.
145
)50
>52
554 .
)56
)62
364
)66
168
370
)72
174
376 -
378
380
382
384
386
••88
390
392
194
396
398
100
102
104
106
103
111
112
113
114 v
116
L.DWO*-
00403 IM 00951 IM
' LAB FLUORIDE
PH FtTOTiL
SU MG/L
•
*
57.4
57.8
:7.5
:lo.l
* f • o
:9.4
:7.9
57.5
:7.9
:8.0
:7.0
:6.9
• 7 • 6
57.4
:7.5
:7.5
:7.9
57,2
:7.4
:7.3
:7.4
57.2
:7.7
:7.6
:8.0
:7.8
:7.7
:9.0
:
•
•
•
»
57.4
:7.3
•
•
0.16 :
1.2 '•
0.21 :
0,83 :
0.18 :
1.0 :
0.20 :
0.7T :
1.3 :
1.2
0.46 ' :
0.52 :
0.18 :
0.42 :
0.17
0.60 :
0.17 :
0.52 :
0.20 5
1.0 :
0.20 :
1.1 :
0.17 :
0.84 :
0.27 :
0.76 :
0.17
0.97
•
*
*
t
*
•
0.15 :
0.90 :
92? 93P
REGION V DRINKING
32730 IM
PHENOLS
UG/L
<3
<3
<3
5
4
6
6
3
3
7
6
8
4
4
3
<3
<3
3
3
<3
<3
<3 . .
<3
13
4
<3
<3
<3 '
<3
<3
<3
<3
94P
00720 I
CYANIDE
CN
MG/L
:<0.002
:0.007
:0.002
:0.005
:0.003
50.004
SO. 003
:0.003
:0.003
:0.002
:<0.002
to. 010
:0.003
:0.005
:<0.002
:<0.002
:<0.002
50.003
:0.004
:0.002
:0.002
:<0.002
: 0 . 0 0 2
50.005
50.003
50.004
5 0.004
50,004
50.003
•
•
5<0.002
•
•
: < 0 . 0 0 2
50.002
95P
WATER STUDY - I
M 00630 IN
N02sN03
N-TOTAL
MG/L
:<0.03
51.36
5 1.38
• : 1.75
5 1.64
51.53
51.53
52.55
52.60
50.55
50.51
5 1.09
51.10
53.54
53.30
52.31
52.04
56.31
56.40
50.08
50.03
5<0,03
5 < 0.03
50.78
50.80
56.13
57.58
53.90
54,08
5<0.03
•
*
*
*
5<0.03'
5<0.03
96P
LLINOIS
00610 IN
NH3-N
TOTAL
MG/L
S<0.010
50.121
5<0.010
50.219
50.023
50.107
50.520
50.155
50.010
50.047
50.014
50.129
5<0.010
50.126
50.024
50.043
5<0.010
50.088
50.014
50.229
50.241
50.225
50.191
50.034
50.013
50.034
50.021
50.095
50.033
5 <0.010
•
•
•
•
50.072
5<0.010
97P
00625 IN
TOT KJEL
N
MG/L
5<0.05
51.42
50.69
52.13
50.17
51.27
50.90
50.34
50.32
50.42
50.37
51.88
50.29
51.87
50.48
50.36
50.34
50.92
50.42
50.46
50.41
50.26
50.26 *
50. S5
50.30
50.45
50.23
50.64
50,69
5<0.05
•
•
*
*
50.12
;
-------
,-CRL
75 -
1PLE
5 NO.
.5
SO
12
14
>6
>2
54
>6
18
P0
'2
r4
'6
'8
30 '
32
34
36
38
)0
?2
34
J6
?8
30
32
34
36
38
.0
.1
, 4
16
.OW04
00665 IN
PHOS-T
P-WET
MG/L
:<0.02
:0.24
:0.04
:0.45
:0.58
:0.19
:0.19
: 0 . 1 2
:<0.02
:<0.02
:<0.02
:0.33
:0.02
:0.33
: < 0 . 0 2
: 0 .1 1
:<0.02
:0.12
:<0.02
:<0.02
:0.02
r<0»02
:<0.02
:0.15
:0.03
: 0 . 1 6
tO. 12
:0.03
:0.02
t
:
-------
S 05APR DSN=CNCR1_S.RGD.IN.DW04 ON TS0009 04/18/75 REV02 T
•STUDY DESCRIPTION
STATTYPE SMPLDAY ATLA88Y DUEDATE ACCOUNT-NUMBER
77777777 03FEB75 05FE875 03MAY75
- INDIANA
•SAMPLE DESCRIPTIONS
STATTYPE DEEP T M NO ENQOATE TIME DR!_U
R NLOG
4 90
REGION
IDNUM
18
19
20
21
22
23
24
25
26
27
28
29-
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
50
51
52
53
54
55
56
AGENCYID UNLOCKEY ST
77
V DRINKING WATER STU
STORETID COLLDAY TIME
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
-------
E>7 750203
58 750203
b9 750203
70 750203
71 750203
72 750203
73 750203
74 750203
75 750203
76 750203
77 750203
78 750203
79 750203
30 750203
31 750203
32 750203
33 750203
34 750203
35 750203
36 750203
37 750203
38 750203
39 750203
50 750203
51 750203
52 750203
53 750203
54 750203
55 750203
56 750203
57 750203
58 750203
59 750203
30 750203
31 750203
32 750203
33 750203
34 750203
35 750203
36 750203
37 750203
.4118 » HN03 REAGENT BLANK
.4119 » H2S04 REAGENT BLANK
.4120 » NAOH REAGENT BLANK
,4121 » CUS04/H3P04 REAGENT BLANK
.4122 » OPF-J 750203
4123 » MT VERNON RAW WATE* SERIES A
.4124 » MT VERNON RAW WATER SERIES 9
.4125 » MT VEPNON FINISHED WATER SERIES A
.4126 » MT VERNON FINISHED WATER SERIES 8
.4127 » MT VEPNON RAW WATER SERIES A
.4128 » MT VERNON RAW rtATER SERIES 9
.4129 » MT VERNON FINISHED WATER SERIES A
.4130 » MT VERNON FINISHED WATER SERIES 3 •*-) •> ^
.4131 » EVAMSVILLE RA* WATER SERIES A • jfr-DO '^ o / ' •> J
.4132 » EVANSVILLE PA* *ATER SERIES d
3-7. ST/^' 6LS3
-------
33 >
34 >
35 >
36 >
37 >
38 >
39 >
40 >
41 >
42 >
43 >
44 >
45 . >
46 >
47 >
48 >
49 >
50 >
51 >
52 >
53 >
54 >
55 >
56 >
57 >
58 >
59 >
60 >
61 >
62 >
63 >
64 >
65 >
66 >
67 >
68 >
69 >
70 >
71 >
72 >
73 >
74 >
75 >
76 >
77 >
78 >
79 >
80 >
81 >
32 >
83 >
34 >
85 >
86 >
37 >
88 >
> EVANSVILLE FINISHED WATER SERIES A
> EVANSVILLE FINISHED WiTER SERIES 3
> NEW- ALBANY RAW WATER SERIES A
> NEW ALBANY RAW WATER SERIES B
> NEW ALBANY FINISHED WATER SERIES A
> NEW ALBANY FINISHED WATER SERIES B
> nrnrn^n PAW WiTFP '•iFRTF'i A . -
> BEDFORD RAW WATER SERIES 8
> BEDFORD FINISHED WATER SERIES A
> BEDFORD FINISHED WATER SERIES B
> f£pp£ HAUTE PAW WATER SERIES A
> TERRE HAUTE RAW WATER SERIES 8
> TERRE HAUTE FINISHED WATER SERIES A
> ' TERRE HAUTE FINISHED WATER SERIES 8
N TMOTftNAPni TC PAW W A T F D ^FQ T F S A
> INDIANAPOLIS RAW WATER SERIES B
> INDIANAPOLIS FINISHED WATER SERIES A
> INDIANAPOLIS FINISHED WATER SERIES B'
> KOKOMO RAW WATER SERIES A
> KOKOMO RAW WATER SERIES 8
> KOKOMO FINISHED WATER SERIES A
> KOKOMO FINISHED WA-TER SERIES 8
> LOGANSPOR1 RAW WATER SERltS A r
> LOGANSPORT RAW WATER SERIES B
> LOGANSPORT FINISHED WATER SERIES 4
> LOGANSPORT FINISHED WATER SERIES B
> pQpy^YNERAWVMTFR SERIES A
> FORT WAYNE RAW WATER SERIES 8
> FORT *AYNE FINISHED WATER SERIES A
> FORT WAYNE FINISHED WATER SERIES 8
b MTfUTrtAN TTTY RAW WATFF? C F R T F S A . .......
> MICHIGAN CITY RAW WATER SERIES B
> MICHIGAN CITY FINISHED WATER SERIES A
> MICHIGAN CITY FINISHED WATER SERIES 8
> GARY RAW WATER SERIES 3
> GARY FINISHED WATER SERIES A
> GARY FINISHED WATER SERIES 8
> GARY RAW WATER SERIES A
> GARY RAW WATER SERIES 3
> GARY FINISHED WATER SERIES A
> GARY FINISHED WATER SERIES B
> U A M M O M H PAW 'J A T £" P ^FQTF^ \
> HAMMOND RAW WATER SERIES 8
> HAMMOND FINISHED WATER SERIES A
> HAMMOND FINISHED WATER SERIES 8
> HN03 REAGENT BLANK
> H2S04 REAGENT BLANK
> NAOH REAGENT BLANK
> H3P04 REAGENT BLANK
> OPEN 750203
> SOUTH BEND RAw WATER SERltS A "
> SOUTH BEND RAW WATER SERIES 3
> SOUTH SEND FINISHED WATER SERIES A
> SOUTH BEND FINISHED WATER SERIES 3
> MUNCIE RAW WATER SERTFS A
- 3 ft • / 1
<-s 0 ( /
T>
-------
-------
9
0
1
MUNCIE RAW WATER SERIES B
MUNCIE FINISHED WATER SERIES A
MUNCIE FINISHED WATER SERIES a
MOROCCO RAW WATER SERIES A •
MOROCCO RAW WATER SERIES B
MOROCCO FINISHED WATER SERIES A
MOROCCO FINISHED :VAT£P SERIES 9
LAFAYETTE RAW WATER SERIES A
LAFAYETTE RAW WATER SERIES 8
LAFAYETTE FINISHED WATER SERIES
LAFAYETTE FINISHED WATER SERIES
A
B
BLOOMINGTON
BLOOMINGTON
BLOOMINGTON
WHITING RAW
WHITING RAW
RAW WATER SERIES B
FINISHED WATER SERIES A
FINISHED WATER SERIES B
WATER SERIES A
WATER SERIES B
WHITING FINISHED WATER SERIES A
WHITING FINISHED WATER SERIES B
SAMPLE/PARAMETER DATA-
q o .S~£> |O l~)>^7 ^
40
A 0
'H1-4J
• sH- VN!
.31 k)
,3X W
-------
-PA-CRL soooa OA soooi OA 39792 OA $0002 OA 50004 OA 39330 OA sooos OA *A
1975 TREFLAN HCBENZ LIN.DAME BBHC DICLONt ALORIN ZYTRON *A
SAMPLE WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SM^L WHL SMPL WHL SMPL *A
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *A
4123 :<0.002
4125 :<0.002
4127 :<0.002
4129 :<0.002
4133 :<0.002
4135 :<0.002
4137 :<0.002
4139 :<0.002
4141 :<0.002
4143 :<0.002
4145 :<0.002
4147 :<0.002
4149 :<0.002
4150 :<0.002
4152 :<0.002
4153 :<0.002
4156 :<0.002
4157 !<0.002
4159 :<0.002
4161 :<0.002
4163 :<0.002
4165 :<0.002
4167 :<0.002
4169 :<0.002
4171 :<0.002
4173 :<0.002
4175 :<0.002
4177 :A
<0,02 :85S*A
<0.02 :87S*A
<0.002 :Q.9S^A
IP 2P 3P 4P 5P 6P 7P **A
IN.Dw04 REGION V DRINKING WATER STUDY - INDIANA **A
-------
FPA-CRL 39430 OA 39420 OA S0006 OA S0007 OA SOOOa OA S0009 OA S0010 OA *8
1975 ISODRIN HCHLR-EP CHLOROAG DDE OP DDE PP ODD OP DDT OP *R
SAMPLE WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMHL WriL SMPL WHL SMPL *fl
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *8
4123 :<0.003
4125 :<0.003
4127 :<0.003
4129 :<0.003
4133 :<0.003
4135 :<0.003
4137 :<0.003
4139 :<0.003
4141 :<0.003
4143 :<0.003
4145 ' :<0,003
4147 :<0.003
4149 :<0.003
4150 :<0.003
4152 :<0.003
4153 :<0.003
4156 :<0.003
4157 :<0.003
4159 :<0.003
4161 :<0.003
4163 !<0.003
4165 :<0.003
4167 :<0.003
4169 :<0.003
4171 :<0.003
4173 :<0.003
4175 :<0.003
*177 :<0.003
4184 :<0.003
4186 :<0.003
4188 :<0.003
4190 :<0.003
4192 :<0.003
4194 :<0.002
4196 :<0.002
4198 :<0.002
4200 :<0.002
4202 :<0.002
4204 :<0.003
4206 :<0.003
<0.002
<0.002
<0 . 002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0,002
<0.002
<0 .002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0,002
<0,003
<0,002
<0.002
<0.002
<0.002
<0.002
<0.002
<0,002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.003
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002 :
-------
EPA-CRl S0011 OA S0012 OA S0013 OA S0014 OA 39430 OA S0020 OA S0021 OA *C
1975 000 PP DDT PP CARBPHTH MIREX MTHXYCLR 2»4-D:lP DNBP *C
SAMPLE tfHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL *C
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *C
4123
4125
4127
4129
4133
4135
4137
4139
4141
4143
4145
4147
4149
4150
4151
4152
4153
4156
4157
,4159
4161
4163
4165
4167
4169
,4171
4173
4175
4177
4184
4186
4188
4190
4192
4194
4196
4198
4200
4202
4204
4206
<0.003
<0.003
<0.003
<0,003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
< 0 . 0 0 3
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
< 0 . 0 0 3
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
C
<1 :77S*C
<1 :79S*C
<1 :31S*C
<1 :H3S*C
<1 :85S*C
<1 :87S*C
<1 :39S*C
15P 16P 17P 18P 19P 20P 21P **C
TM.D404 REGION V DRINKING 'VATER STUDY - INDIANA »*C
-------
FPA-CRL 39770 OA S0023 OA 39380 OA 39390 OA 39460 OA S0027 OA S0028 OA *0
1975 DCPA ENOOS I DIELDRIN ENDRIN CLRBNZLT ENDOS II NITROFEN *D
SAMPLE dHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL VHL SMPL WHL SMPL *D
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *D
.4123
.4125
.4127
,4129
,4133
.4135
.4137
.4139
.4141
,4143 .
.4145
,4147
4149
,4151
.4153
.4157
,4159
.4161
.4163
.4165
4167
.4169
.4171
.4173
.4175
.4177
.4134
.4136
,4186
.4190
.4192
.4194
,4196
.4198
.4200
.4202
.4204
.4206
<.003
<.003
<.003
<.003
<.003
< . 003
<.003
<.003
<.003
<»003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005 •
.003
<.003
<.003
<.003
<.003
.006
<.003
.008
.006
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<,003
.007
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
.007
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
< . 0 0 3
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
s<,003
'<.003
<.003
<.003 '
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<. 003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
< . 0 0 3
<.003
< . 0 0 3
<,003
< . 0 0 3
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<,01
<.01
<.01
<.01
<.01
<,01
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005 : 6S*D
<.005 : 8S*0
<.005 :10S*D
<.005 :12S*D
<,005 :16S*0
<.005 :18S*D
<.005 :20S*D
<.005 :22S»D
<.005 :24S*D
<.005 :26S*D
<.005 :28S»D
<.005 :30S*0
<.005 :32S*0
<.005 :34S*0
<.005 :36?*0
<.005 :40S*0
<.005 :42S*0
<.005 :44S*D
<.005 :46S*D
<.005 t48S»D
<.005 :50S*D
<.005 :52S*D
<.005 :54S*D
<.005 :56S*0
<.005 :58S*0
<.005 :60S»D
<.005 :675*D
<.005 :69S*0
<.005 :71S»0
<.005 :73S*0
<.005 :75S*0
<.005 :77S*D
<.005 :79S*0
<.005 :31S*0
<.005 :33S*0
<.005 :85S*0
<.005 :87S*D
<.005 :89S*>D
22P 23P 24P 25P 26° 27P 2SP **0
.IN.DWO* REGION v DRINKING WATER STUDY - INDIANA **D
-------
-------
EPA-CRL S0029 OA S0030 OA S0031 OA S0026 OA 39808 OA 39570 OA 50016 OA *E
1975 245-T5IO PROLAM BULAN OEHP TEDION DIAZINON OYFONATE *E
?AM°LE WHL SMPL WHL SMPL WHL SMPL WML SMPL WHL SMHL *IHL SMPL 4HL SMPL «•£
LOG MO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *E
4123
4125
4127
4129
4133
4135
4137
4139
4141
4143 '
4145
4147
4149
4151
4153
4155
4157
4159
4161
416-3
4165
4167
4169
4171
4173
4175
4177
4184
4186
4188
4190
4192
4194
4196
4198
4200
4202
4204
4206
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.oi
<.01
<.01
<.oi
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<,01
<.0l
<.01
<.0l
<.01
<.0l
<.01
<.0l
<.01
<.01
<.01
<.01
<.01
<.0l
<.01
<.0l
<.0l
<.0l
<.01
<.01
<.0l
<.0l
<.01
<.01
<.0l
<,01
<.0l
<,01
<.01
<.0l
<.01
<.01
<.0l
<.0l
<.0l
<.0l
<.0l
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01 "
<.0l
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
1
4
3
<1
<1
5
17
<1
<1
<1
4
2
<1
<1
<1
<1
<1
<1
<1
<1
1
<1
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.oi •
<.01
<.01
<.01
<.01
<.01
<.0l
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1 : *S«E
<1 : RS*E
<1 :10S»E
<1 :12S»E
<1 :i*S*E
E
<1 :87S*E
<1 :89S*E
29P 30P 31P 32P 33P 34P 3SP **E
IN. 0*04 REGION V DHINKING WATER STUDY - INDIANA **E
-------
FPA-CRL S0017 OA 50032 OA 39600 OA 39530 OA 39540 UA S0033 OA 39398 OA *F
1975 RONNEL OURS8AN MPARATl-M MALATHN PARATHN DEF ETHION *F
SAMPLE WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMHL WHL SMPL 4HL SMPL *F
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *F
4123
4125
4127
4133
4135
4137
4139
4141
4143
4145
4147
4149
4151
4153
4155
4157
4159
4161
4163
4165
4167
4169
4171
4173
4175
4177
4184
4186
4188
4190
4192
4194
4196
4198
4200
4202
4204
4206
-------
EPA-CRL S0018 OA S0034 OA 39580 OA S0035 OA S0036 OA S0037 OA 39488 OA *G
1975 PHENCAPT EPN GUTHION PHOSALON AZINFOSE COUMAFOS AROCLOR *G
SAMPLE WHL SMPL WHL SMPL tfHL SMPL WHL SMPL WHL SMPL >/HL SMPL 1221 -»G
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *G
4123
4125
4127
4129
4133
4135
4137
4139
4141
4143
4145
4147
4149
4150
4151
4153
4155
4156
4157
4159
4161
4163
4165
4167
4169
4171
4173
4175
4177
4194
4186
4188
4190
4192
4194
4196
4198
4200
4202
4204
4206
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<5
<5
<5
<5
<5
•<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
r,
<0.3 :89S-»G
43P 44P 45P 46P 47P 43P 49P **G
IN.DW04 REGION V DRINK IMG ^ATER STUDY - INDIANA **G
-------
rPA-CRL
1975
9AMPLE
LOG NO.
4123
.4124
.4125
,4126
4127
4128
4129
4130
4133
4134
4135
4136
4137
4138
4139
4140
4141
4142
4143
4144
4145
4146
4147
4148
4149
4150
4152
4153
4154
4156
4157
4158
4159
4160
4161
4162
4163
4164
4165
4166
4167
4168
4169
4170
4171
4172
il73
i!74
i!75
V176
i!77
H78
v!34
^185
>186
^187
aa8
39496 OA
AROCLOR
1242
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
39500 OA
AROCLOR
1248
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
39504 OA
AROCLOR
1254
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
39508 OA
AROCLOR
1260
UG/L
H
4 :27S-»H
:28S*H
5 :29S*H
: 30S*H
<1 :31S*H
:32S*H
19 :33S*H
9 :35S*H
:36S»H
30 :37S*4
<1 :39S-;>H
: 40S<*H
7 :4lS*H
:42S*H
4 :43S«-H
!44S*H
29 :45S*M
:46S<»H
<3 :47S»H
:48S*H
5 :u-9S*ri
: 50S*H
<1 :51S*M
:52S»H
6 :53S*H
: 54S*H
<2 :55S*H
:56S<»M
7 :57S*H
; 5«C;»M
<1 :59S*H
:b05*4
4 ^IS^'r1
: 67S*M
<2 :68S*H
; £,9^
-------
.4189
.4190
.4191
4192
4193
4194
4195
4196
4197-
4198
4199
4200
4201
4202
4203
4204
4205
4206
4207
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0,3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.4
<0.4
<0.4
<0.4
<0.4
<0 .4
<0.4
<0.4
<0.4
<0.5
<1
<0.5
-------
EPA-CRL
1975
SAMPLE
LOG NO.
.4124
.4126
4128
.4130
.4134
.4136
4138
, ** X «J *-J
.4140
.4142
.4144
.4146
.4148
.4150
.4152
.4154
.4156
.4158
14160
14162
14164
14166
14168
14170
14172
14174
14176
14178
14185
14187
14189
14191
14193
14195
14197
14199
14201
14203
14205
14207
. IN.DWQ4
S0056 OA SOO^O OA S0041 OA
C2H4CL2 CHCL2BR
TOT VOL TOT VOL
UG/L UG/L
:<2 5 <0 .5
5<1 59
5<2 5<0.5
:<1 59
5<2 512
52 50.4
5<2 515
5<2 S<0.5
5<1 512
515 5<0.5
5 < 1 55
53 5<0.5
5<1 56
: <4 s<0.5
!<1 511
51 t<0.5
5 < 1 51.2
54 5<0.5
521 50.7
s<2 5<0.5
5<2 54
t<2 5<0.5
S<2 55
:<4 5 <0.5
5<2 55
S<2 5<0.5
5<2 5<0.5
5<1 s<0.5
5<1 53.4
52 5<0.5
:<1 517
5<1 5<0.5
5<1 510
52 t<0.5
5 < 1 51
: <1 : <0 ,5
:<1 :5
: s<0.5
5 <2 5 <0.5
57? 58P
REGION V DRINK
CHCLBR2
TOT VOL
UG/L
s<0.5
5 1.5
5<0.5
51
t 1.7 -
5<0.2
51.4
5<0.5
50.8
5<0.5
56
S<0.5
50.5
5<0.5
51.4
S<0.5
S<0.1
5<.5
50.4
5<0.5
51
5<0.5
51
t <0.5
5 1
5<0.5
;<0.5
5<0.5
53
:<0.5
51
5<0.5
53
5<0.5
50.3
:<0.5
50.5
5 <0.5
: <0.5
59P
ING WATER
S0042 OA *I
« »
CH8R3 *T
TOT VOL *J
«• T
UG/L *!
. -W f~ Jt T
t <0.5
5 1 .6
5<0.5
50.3
51
5 < 0 . 2
51
S<0.5
50.8
5<0.5
53
5<0.5
50.6
5<0.5
50.3
5<0.5
5 < 0 . 1
5 < 0 . 5
51
5<0.5
5 cO . 5
5 < 0 . 5
5 < 0 . 5
: <0.5
5 <0.5
:<0.5
5<0.5
5<0.5
52
5<0.5
5 <0.5
S<0.5
50.3
5<0.5
50.6
5<0,5
5<0.3
5<0.5
5 < 0 . 5
; ( ^^ L
• f> t* A T
5 95*1
• 1 1 *"* jt T
5 1 1 5*1
5135*1
* 1 T C" ii T
5 1 75<* I
5 1^5*1
5215*1
5235*1
5 255*1
5275*1
5295*1
5315*1
5335*1
5355*1
5 375*1
5 39$*I
5415*1
5435*1
545S*I
5 475*1
5495*1
5 51 5*1
5535*1
555S*I
5575*1
5595*1
561 S* I
5685*1
5705*1
572S*I
5745*1
5765*1
5 785*1
5805*1
5825*1
5«4S*I
586S*I
S88S*I
5905*1
60P 61P 62P 63P **I
STUDY - INDIANA **I
-------
EPA-CRL
1975
SAMPLE
LOG NO.
14118
14119
14120
14123
14124
14125
14126
14133
14135
14137
14139
14141
14143
14145
14147
14149
14151
14153
14155
14157
14159
14161
14163
14165
14167
14169
14171
14173
14175
14177
14179
14180
14134
14186
14188
14190
14192
14194
14196
14198
14200
14202
14204
14206
.TM.OW04
00916 MW
CALCIUM
CA.TOT
MG/L
:<1
: <1
: <1
:28.0
:29.4
:30.0
:30.2
:31.0
:32.8
:27.2
:41.9
:46.4
:98.5
:86.4
:69.7
:68.5
171.0
:81.6
:80.9
:79.9
:60.7
:23.0
:35.5
:35.4
535.7
:34,3
:36.1
:34.8
:36.3
:34.7
5<1
: <1
:63.6
:65.9
:67.2
:69.6
:57.1
:30.0
:66.8
:79.1
:11.4
:15.4
:38.o
534.9
64P
PEGION
00927 MW
MGNSIUM
MG»TOT
MG/L
: <0 . 1
. . rt i
: <-\j 1 1
511.6
511.0
510.6
5 10.6
511.1
• 1 1 £^ •
511*6
512.2
:5.4
:5.8
520.5
:82.3
510.6
511.4
55.7
:18.3
57.7
57.9
57.2
525.8
55.9
• C Q
55.8
54.0
59.2
54.6
• rt 1
59.1
55.6
55.3
• s f\ 1
5 <0 * 1
• «- n i
I <:\J * i
56.9
57.0
56.7
56.6
514.5
577.2
511.4
516.2
53.9
53.9
57.7
56.1
66P
NG WATE3
00937 MW 01034 MW
PTSSIUM CHPOMIUM
K,TOT C3»TQT
MG/L UG/L
• f n i : <5
• ^ u • i • ^» .j
• fCt 1 5 <5
• s. U • i • ^ ,J
• <0 . 1 5 <5
• ^". \J • i. • ^ w1
52.0 5<5
51.7 5<5
51.6 5<5
51.6 S<5
52.0 5<5
• o 1 • f\
5 d. . 1 • O
52.0 5<5
52.9 S<5
52.4 5<5
53.4 5<5
53.7 5<5
51.7 5<5
52.0 5<5
51.2 5<5
51.3 5<5
. * Q f * C
5 1 .9 • -5 • j C
51,3 •
. -i r- • f C
5 1 . D • <3
51.5 :<5
• s r\ i t t— •-'
5 140
5<20
5 <20
5<20
5 <20
• .X *5 A
5 <20
51160
5 <2 ^
5300
5 <2 0
5 1 130
5<20
5840
5 54
5 1 1 0
5<20
586
5<20
TOP
1 *J
*J
*J
*J
5 1S»J
5 2S»J
5 3S*J
5 6S*J
5 7S*>J
5 8S*J
• O C H> 1
• 7 ^> U
5 16S*J
5 18S»J
5205*0
!22S«'J
S24S*J
526S*J
S285*J
530S*J
« O ^ C ii 1
1 3cbw J
• 0 A C «• 1
• j ** .^ \J
536S*J
• O Q C tt |
t J *i ^ O
540S»J
• / O C ii 1
. 4c b* J
544S*J
• j. (L C A 1
• ** O z> U
548S*J
S50S«J
552S*J
5 54S*J
556S*J
55RS*J
560S*J
562S*J
• (. -5 C •» 1
t O J -5 O
567S*J
• *1 Q C •*> 1
t O 7 -5 J
571S*J
• "7 O C ^i 1
* 7o b* J
t ^ CZ C* J4 I
5 7b b* J
577S*J
* "7 Q C
-------
FPA-CRL
1975
SAMPLE
1 OG NO.
14118
14119
14120
14123
14124
14125
14126
14133
14135
14137
14139
14141
1414-3
14145
14147
14149
14151
14153
14155
14157
14159
14161
14lfr3
14165
14167
14169
14171
14173
U175
14177
14179
14180
14184
14186 .
14188
14190
14192
14194
14196
14198
14200
14202
14204
14206
.IN.QW04
01055 Mw 01092 MW 01002 MW 01051 MW 01027 M* 01077 MW
MANGNESE ZINC ARSENIC LEAD • CADMIUM SILVER
MN,TOT ZN»TOT AS»TOT PBtTOT CD.TOT AG,TOT
UG/L UG/L UG/L UG/L UG/L UG/L
:<5 :<5 :
: < 5 : < 5 :
:<5 :<5 :
:330 :30 :
:300 :40 :
:20 :20 :
:18 :18 :
:<5 :82 :
:470 :89 :
:<5 :460 :
:120 :5 :
:<5 :<5 :
:280 :6 ;
:19 :<5 :
:33 17 :
: <5 : <5
:28 :<5 ;
:9 :<5 ;
:39 :<5
: 19 : 14 ;
*.4l :14
:<5 :<5
:<5 :<5
:<5 :<5
:<5 :<5
:<5 :<5
:7 :<5
:<5 :<5
:<5 :12
:<5 :<5
:<5 :<5
:<5 :<5
:95 :<5
:37 :<5 :
:26 :<5 ;
:<5 :<5
:180 :5
:18 :<5
:640 :31
-.350 :<5
;21 :<5
:<5 :<5
:5 :<5
:<5 :<5
<1 :<2 :
: <1 :<2 :
<1 :4 ;
•8 :25 :
:6 :22 !
: < 1 : 5 :
!<1 :5 :
:<1 :3 J
i9 :15 ;
i :67S*<
:<5 :69S»K
:<5 :71S*K
:<5 :73S*K
:<5 :75S*K
:<5 :775<>K
:
-------
FPA-C&L
1975
SAMPLE
LOG NO.
14123
14124
14125
14126
14133 .
14135
14137
14139
14141
14143
14145
14147
14149
14151
14153
14155
14157
14159
14161
14163
14165
14167
14169
14171
14173
14175
14177
14184
14186
14188
14190
14192
14194
14196
14198
14200
14202
1 &.? 0 ^
i. ** C. v ™
1^206
. I N . D * 0 4
00530 IM
RESIDUE
TOT NFLT
MG/L
:181
:181
:2
:2
:<2
:329
:<2
: 140
:2
:<2
:3
:24
:<2
:9
:3
:15
:<2
:53
:<2
:7
:<2
:5
:<2
:7
:<2
:7
:<2
:2
:2
:10
:2
:<2
:3
:<2
:2
:<2
:<2
:5
:<2
78P
REGION
70300 IM
RESIDUE
DISS-180
C MG/L
:160
:160
:150
:150
:170
:180
:130
:220
:260
:510
:590
:370
:380
:340
:400
:380
:390
:310
:220
:220
:190
:200
:215
:190
:210
:200
:180
:270
:300
:340
:360
:330
:320
:325
:410
:120
: 130
: 140
: 140
79P
V DRINKI
00095 IM
CNDUCTVY
AT 25C
MICROMHO
:298
:296
J323
:322
:316
:321
: 308
:354
:404
:792
:925
:595
:587
-.537
:678
:605
:600
: 491
:327
:301
:305
:293
: 315
:295
:314
:301
:304
:555
:538
:593
:592
:507
:547
:542
:668
:154
: 168
:316
:309
SOP
NG WATEP
00945 I
SULFATE
S04
MG/L
:54
:54
:87
:87
:60
:60
• c c
! ST
:33
:56
: 103
: 149
:52
:64
;43
:100
:8l
: 107
:80
:80
:27
:34
:?4
• "3 1
531
:22
:30
:24
:28
:34
:36
:54
:62
:47
:48
:54
:67
:32
:39
:28
:32
SIP
STUDY -
M 00940 IM
CHLORIDE
CL
MG/L
:16
:17
:20
:20
: 19
:16
• 5 1
• C. i
:12
:18
:30
:32
:26
:31
:25
:33
:19
• "51
I 21
: 17
:19
:ll
:13
: 10
• 1 1
* i i
:9
: 10
: 1 0
:ll
:25
:17
:20
:24
:35
:37
:23
:33
:4
:5
: 13
: 13
82P
INDIANA
00956 IM
SILICA
SI02
MG/L
:6.5
:6.5
:6.3
:6,4
:7.0
:6.3
I 7 * 0
:7.0
:7.9
:12.8
:13.8
:7.5
:7.8
:6.7
: 1 1 . 3
:8.0
• a i
• O.I
• f /•
I O • 4
:5.9
:0.5
:0.6
:<0.2
: 0 .6
: <0 .2
: 0 .6
• A "2
I 0 w U
: 9S*L
:16S*L
: 18S*L
:20S*L
:22S^L
:24S*L
:26S*L
:28S»L
:30S*L
:32S*L
:34S»L
:36S»L
: 38S*L
: 40S<*L
: 42S*L
• "T t. ~J L_
:44S*L
:46S*L
:48S*L
!50S«L
:52S*L
• C A c*l
• J *r -^ L.
• c: A c; •»!
• j O O L.
• cp<;»i
* -J '_•«.' L*
:60S-»L
:67S*L
:69S*L
• 7 1 Q 1
i O / O l_
: 89S*L
Jt 44 t
l_
>i A i
•^^L
------L
-------
FPA-CRL
1975
SAMPLE
LOG NO.
14118
14119
1*120
14121
14123
14124
14125
14126
14133
14135
14137
14139
14141
14143
14145
14147
14149
14151
14153
14155
14157
14159
14161
14163
14165
14167
14169
14171
14173
14175
14177
1*179
14180
14184
14186
14138
14190
14192
14194
14196
14198
14200
14202
14204
14206
. IM.DW04
00403 IM 00951 IM
LAB FLUORIDE
PH F»TOTAL
SU MG/L
:
:
;
:
:7.4
:7.3
:6.5
:6.5
:7.7
:7.2
17.1
:7.3
:7.6
:7.5
:8.0
:7.5
:7.9
:7.5
:7.5
:7.7
:7.6
:7.7
S9.1
:7.9
:7.3
:7.9
:7.9
:7.9
:7.9
:7.8
:7.5
:
:
:7.3
:7.9
:7.7
:7.6
:7.5
:7.9
:8.0
:7.6
:7.4
:7.3
:7.8
:7.2
0.13
0.13
0.78
0.86
0.93
0.14
0.56
0.14
2.1
0.16
0.12
0.19
0.76
0.16
1.0
0.20
0.99
0.18
0.83
0.13
0.22
0.12
0.82
0.12
0.83
0.14
0.19
0.15
0.87
0.19
1.0
0.17
0.93
0.23
1.1
<0.10
0.80
0.16
0.13
35P 86P
32730 IM 00720 I
PHENOLS CYANIDE
CN
UG/L MG/L
:7
:8
: 3
:
• C
I 7
: <3
: <3
:6
• 3
:4
:5
: <3
:3
: <3
: 1 o
:5
:7
:3
:4
:5
:6
:5
:5
: 3
: <3
: 5
: <3
:5
:3
:8
:5
• -i
: <3
: <3
:4
:4
: <3
: <3
:3
:7
I 3
J <3
: 14
:5
<0.002
0.010
<0.002
0.002
0.006
0.006
0.003
<0.002
0.003
0.010
0.003
0.003
0.003
0.005
0.003
0.003
0.010
0.004
0.006
0.003
0.004
0.004
O.Q04
0.006
0.002
0.004
<0.002
<0.002
<0.002
0.005
<0.002
0.005
0.008
0.002
<0.002
0.003
0.004
0.003
0.003
0.002
0.005
<0 .002
0.002
0.015
0.003
87P 88P
REGION V DRINKING WATER STUDY - I
M 00630 IN 00610 IN 00625 IN
N02\N03 NH3-N TOT KJEL
N-TOTAL TOTAL N
MG/L MG/L MG/L
:<0.03
:<0.03
:<0.03
:
: 1.04
:0.99
:0.99
:0.99
:0.9S
: 1 . 1 3
! 1 . 10
:2.69
:2.60
:2.53
:3.94
:4.86
:4.44
:9.03
:6.53
:4.91
:4.80
.'3.45
:3.31
:0.23
:0.22
:0.18
:0.16
:0.17
:0,16
:0.23
:0.16
:<0.03
:<0.03
:<0.03
:<0.03
:3.13
:3.24
:0.06
-.0.12
:0.07
:0.66
:0.25
:0.23
:0.22
:0.21
<0.010
<0.010
<0.010
0.155
0.153
<0.010
<0.010
0.011
0.153
<0.010
0.064
0.012
0.281
<0.010
0.178
0.293
0.090
0.012
0.124
0.687
0.190
0.273
0.075
0.145
0.014
0.148
0.011
0.153
0.068
0.357
<0.010
<0.010
0.107
0.015
0.102
0.016
0.209
0.014
0.325
0.142
0.026
<0.010
0.231
0.375
<0.05 :
<0.05 :
<0.05
:
1.25 :
1.22 :
0.61 :
0.66
0.72 :
1.47 :
0.71 :
1.59 • :
0.80 :
1,10 :
0.76 :
0.77 :
0.64 :
0.68 :
0.23 :
0.88 !
1.15 :
1.51 :
0.58 !
0.24 :
0.22 :
0.16 :
0.23
0.16 :
0.24 :
0.20 :
0.45 :
<0.05 :
-------
EPA-CRL 00665 IN 00340 IN 00680 IN 71900 IN 00900 IN 00615 IN *,M
1975 PHOS-T COD T ORG C MERCURY TOT HAKD N02-N *N
SAMPLE P-wET HI LEVEL C HG»TOTAL CAC03 TOTAL *N
LOG NO. MG/L MG/L MG/L UG/L MG/L *G/L *N
14118 :<0.02 :<3
U119 :<0.02 :<3
14120 :<0.02 :<3
14123 :0.28 :25
14124 :0.27 :22
14125 :0.03 :4
14126 :0.02 :5
14133 :0.02 :<3
U135 :0.47 :35
14137 :0.36 :5
14139 :0.31 :30
14141 :0.03 HO
14143 :0.02 :4
14145 :<0.02 :<3
14147 !0. 15 :13
14149 J0.03 :7
14151 :0.03 :10
14153 :<0.02 :3
14155 :0.07 :16
14157 :<0.02 :8
14159 :0.16 :32
14161 :<0.02 :a
14163 :<0.02 :5
14165 :<0.02 :<3
14167 :0.02 :3
14169 :0.02 :<3
14171 :0.03 :6
14173 :0.03 :<3
U175 :0.02 :<3
14177 :0.02 :3 '
14179 :0.02 :<3
14180 :<0.0? :<3
14184 :0.03 :<3
14186 :0.03, :<3
14183 :0.09 :10
14190 :0.05 :5
14192 :0.06 :6
14194 :0,03 :5
14196 :<0.02 :4
14198 :<0.02 :<3
14200 :<0.02 :3
14202 :<0.02 :<3
14204 :0.02 :10
14806 :<0.02 :9
<0.1
<0.1
<0.1
0.3
0.2 '
0.3
0.3
0.2
0.1
<0.1
<0.1
<0.1
<0.1
<0.1
0.1
0.2
0.1
0.1
0.3
0.2
0.1
0.2
0.1
0.3
0.1
<0.1
0.1
<0.1
-------
CRLS 05APR
DSN=CNCRLS.RGD.MC.DW01 ON TS0009 04/19/75
-STUDY DESCRIPTION
STATTYPE SMPLDAY ATLABBY DUEDATE
77777777 C3FE375 05FEB75 03MAY75
- MICHIGAN
•SAMPLE DESCRIPTIONS
STATTyPE DEEP T M NO ENDDATE
NPAR NLOf
94 71
»>REGIOf
LABIONUM
14208
14209
14210
14211
14212
14213
14214
14215
14216
14217
14218
14219
14220
14221
14222
14223
14224
14225
14226
14227
14228
14229
14230
14231
14232
14233
14234
14235
14236
14237
14238
14239
14240
14241
142^2
14243
14244
14245
14246
14247
14248
14249
14250
14P51
14252
14253
14254
14255
.4256
T AGFNCYIO UNLOCKEY ST
r 77
J V DRINKING WATER STU
STORETID COLLDAY TIME
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
7502Q3
750203
750203
750203
750203
REV01 T
ACCOUNT-NUMBER
TIME PRLU
-------
1-209
r212
V215
^216
4217
4218
4219
4220
4221
4222
4223
4224
4225
4226
4227
4223
4229
4230
4231
4232
4233
4234
4235
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
HN03 REAGENT BLANK
H2S04 REAGENT 3LANK
NAOH REAGENT BLANK
H3POA- REAGENT BLANK
OPEN
DUNDEE RAW WATER SERIES A
DUNDEE RAW WATER SERIES 9
DUNDEE FINISHED WATER SERIES A
DUNDEE FINISHED WATER SERIES B
DETROIT RAW WATER SERIES A
DETROIT RAW WATER SERIES 9
DETROIT FINISHED WATER SERIES
DETROIT FINISHED WATER SERIES
DETROIT RAW WATER SERIES a
DETROIT RAW WATER SERIES 5
DETROIT FINISHED WATER SERIES
DETROIT FINISHED rfATER SERIES
j.S* iJ- 23,3*6 w)
MT.CLEMENS PAW WATER SERIES A
MT.CLEMENS.RAW WATER SERIES 8
MT.CLEMENS FINISHED WATER SERIES A
MT.CLEMENS FINISHED WATER SERIES 8
JACKSON RAW WATER SERIES 3
JACKSON FINISHED 4ATEP SERIES A
JACKSON FINISHED WATER SERIES 3
KALAMAZCO
KALAMAZOO
A
B
RAW WATER SERIES
FINISHED *ATER SERIES A
AS- rO tH-V4 vO
.11 lO
-------
36 » KALAMAZOO FINISHED WATER SERIES 8
37 » LANSING RAW WATER SERIES A Hi
38 » LANSING RAW WATER SERIES 8
39 » LANSING FINISHED WATER SERIES 'A
i-O » LANSING FINISHED WATER SERIES B . x
>1 » GRAND RAPIDS RAW WATER SERIES A -1 ^ ^ . 5 7 NJ 6 b • H O Vv
(-2 » GRAND RAPIDS RAW WATER SERIES B
>3 » GRAND RAPIDS FINISHED WATER SERIES A
v4 » GRAND RAPIDS FINISHED WATER SERIES 8 tail/
>5 ' » MT.PLEASANT RAW WATER SERIES A —- M "i v 3 U N 1> ^ • H (8 » MT.PLEASANT FINISHED WATER SERIES Q ,
^ » CADILLAC RAW WATER SERIES A —— O^ ^ . \ "S NJ 5 «S ' *- ~> V>
SO » - CADILLAC RAW WATER SERIES B
51 » CADILLAC FINISHED WATER SERIES A
52 » CADILLAC FINISHED WATER SERIES 8 \i^n\/>J>/ v
,2 » MENOMINEE RAW WATER SERIES 8
,3 » MENOMINEE FINISHED WATER.SERIES A
,4 » MENOMINEE FINISHED WATER SERIES 8
,5 » MENOMINEE RAW WATER SERIES A
,6 » MENOMINEE RAW WATER SERIES 8
,7 » MENOMINEE FINISHED WATER SERIES A
,8 » MENOMINEE FINISHED WATER SERIES B
,9 » HN03 REAGENT BLANK
'0 » H2S04 REAGENT BLANK
'1 » NAOH REAGENT BLANK
'2 » H3P04 REAGENT BLANK
'3 » BISSE.^ER TOWNSHIP RAW WATER SERIES
'4 » SISSEMER TOWNSHIP RAW WATER SERIES
'5 » 8ISSEMER TOWNSHIP FINISHED WATER
'6 » 3ISSEMER TOWNSHIP FINISHED WATER
2 » BAY CITY RAW WATER SERIES A - U^"oS~Kl ^3^
3 » BAY CITY RAW WATER SERIES 3 •M ^,^ ^ \ «
4 » BAY CITY FINISHED WATER SERIES A_
5 » BAY CITY FINISHED WATER SERIES B . . . -, ^
6 » WYANOOTTE RAW WATER SERIES A Uf 3. v \ 1 N 'h 3 > \ O
7 » WYANDOTTE RAW WATER SERIES 3
8 » WYANDOTTE FINISHED WATER SERIES A
9 » WYANDOTTE FINISHED WATER SERIES B
SAMPLE/PARAMETER DATA-
-------
FPA-CRL S0003 OA S0001 OA 39782 OA S0002 OA S0004 OA 39330 OA S0005 OA »A
1975 TREFLAN HC6ENZ LINDANt B8HC OICLONE ALDRIN ZYTRON *A
SAMPLE WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL n/HL SMPL *A
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *A
.4213
.4215
.4217
.4219
.4221
,4223
.4225
,4227
.4229
.4231
,4233
4235
.4237
,4239
.4241
.4244
,4245
.4247
.4249
.4251
.4253
.4255
.4257
.4259
.4261
.4263
U265
14267
U273
U275
14782
14784
14786
14788
0.007 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 : <0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
0.003 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0,002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002 :<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0,002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0 . 002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0,002
<0.002
<0,002
<0.002
<0.002
<0.002
<0.002
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
< 0 . 0 0 5
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
< 0.0 05'
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.002
0.006
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.02 : 6 S * A
<0.02 : »S»A
<0.02 :10S*4
<0.02 :12S*A
<0.02 :14S*A
<0.02 :16S*A
<0.002 :13S*A
<0.02 :20S*A
<0.02 :22S*A
<0.02 : 2 4 S * A
<0.02 :26S*A
<0.02 :28S*A
<0.02 :30S*A
<0.02 :32S*A
<0.02 :34S*A
<0.02 :37S*A
<0.02 :'3PS*A
<0.02 :40?*A
<0.02 :42S*A
<0.02 :44S*A
<0.02 :46S*A
<0.02 :4«S*A
<0.02 :50S»A
<0.02 :525*A
<0.02 :54S*A
<0.02 :56S*A
<0.02 : 5 8 S * A
<0.02 :60S*A
<0.02 :66S-*A
<0.02 :68S»A
<0.02 J70S»A
<0.02 :72S*A
<0.02 :74S*A
<0.02 :76S«A
IP 2P 3P 4P 5P 6P 7P **A
.^I.DWOI REGION V DRINKING WATER STUDY - MICHIGAN **A
-------
EPA-CRL 39430 OA 39420 OA 50006 OA S0007 OA S0008 OA S0009 OA S0010 OA *8
1975 ISODRIN HCHLR-EP CHLORDAG DOE OP DOE PP ODD OP DOT OP *8
SAMPLE WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL *HL SMPL v»HL SMPL **
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *3
4213 :<0.003 '
4215 :<0.003
4217 :<0.003
4219 :<0.003
4221 :<0.003
4223 :<0.003
.4225 :<0.003
,4227 :<0.003
,4229 :<0.003
.4231 :<0.003
.4233 :<0.003
.4235 :<0.003
.4237 :<0.003
,4239 :<0.003
.4241 :<0.003
,4245 :<0.003
.4247 :<0.003
.4249 :<0.003
.4251 :1.0
.4253 :<0.002
.4255 :<0.002
.4257 :<0.002 l
.4259 :<0.002
.4261 :<0.002
.4263 :<0.002
.4265 :<0.003
,4267 :<0.002
.4273 :<0.003 :
.4275 :<0.003 :
.4782 :<0.003
.4784 :<0.003
.4786 :<0.003 !
.4788 :<0.003 !
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.003
<0.003
<0.003
<0.003
<0.003
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.003
<0.003
<0.003
<0.003
<0.003
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.00?
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
: <0.003 <0.003
•<0.003 <0.003
<0.003 <0.003
.<0.003 <0.003
<0.003 <0.003
<0.003 <0.003
<0.003 <0.003
!<0.003 <0.003
!<0.003 <0.003
K0.003 <0.003
<0.003 <0,003
•<0.003 <0.003
<0.003 <0.003
!<0.003 <0.003
.<0.003 <0.003
< 0 . 0 0 3 <0.003
<0.003 <0.003
<0.003 <0.003
<0.003 <0.003
<0.003 <0.003
K0.003 <0.003
<0.003 <0.003
<0,003 <0.003
<0.003 <0.003
<0.003 <0.003
-<0.003 <0.003
<0.003 <0.003
<0.003 <0.003
<0.003 <0.003
<0.003 <0.003
<0.003 <0.003
<0.003 <0.003
<0.003 <0.003
<0.003 : 6S*»
<0.003 : 8S*8
<0.003 :10S*P
<0.003 :12S*R
<0.003 :14S*3
<0.003 :16S«8
<0.003 :iflS*8
<0.003 :20S^B
<0.003 :22S<>6
<0,003 :24?*R
<0.003 :26S«'H
<0.003 :23S»B
<0.003 :30S*B
<0.003 :3?S^9
<0.003 :34S*P
<0.003 :3es-»?
<0.003 :40S*3
<0.003 :42S«-^
<0.003 :44S*8
<0,003 :46S»3
<0.003 :48S*8
<0.003 :50S*8
<0.003 :52S»B
<0.003 :54S*R
<0.003 :56S^*9
<0.003 :58S^«
<0.003 :605*B
<0.003 :665<>g
<0.003 :68S*8
<0.003 :70S*B
<0.003 :72S<>8
<0.003 :74S*B
<0.003 :76S*B
3P 9P 10P IIP 12P 13P 14P **B
.MI.OW01 REGION V DRINKING WATER STUDY - MICHIGAN **B
-------
;PA-CRL S0011 OA S0012 OA S0013 OA S0014 OA 39*80 OA S0020 OA S0021 OA *C
1975 ODD PP DDT PP CAR8PHTH MIRFX MTHXYCLR 2. 4-0: IP HNBP *C
;AMPI_E WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL *c
OG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *C
,213
,215
.217
,219
h221
,223
,225
,227
>229
.231
,233
,.235
,237
,239
,241
,244
*245
>247
+ 249
,251
^253
^255
i257
i259
4261
4263
4265
4267
4273
4275
4782
4784
4786
4788
<0.003 :0.004
<0.003 :<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 : <0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 : <0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 t<0.003
<0.003 :<0.003
*
•
<0.003 !0.004
0.006 :<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 !<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 : <0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003 :<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0,005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.003
<0.005
<0.005
<0.005
<0.005
<0.005
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<.o?
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.Q2
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<1 : 6S*C
<1 : ss^c
<1 :10S**C
<1 :12S*C
<1 :14S*C
<1 :16S*C
<1 :18S«C
<1 :2ns*C
<1 :22S«-C
<1 :24S«C
<1 :26SttC
<1 :28S*C
<1 :30S*C
<1 :32S*C
<1 :34S»C
<1 :37S*C
<1 :3«s»c
<1 :4QS«C
<1 J42S*C
<1 :44S*C
<1 :46S*C
<1 :48S^c
<1 :50S«-C
<1 :52S*C
<1 :54S*C
<1 :56S*C
<1 :58S*C
<1 :60S*C
<1 :66S*C
<1 :63S*C
<1 :70S*C
<1 :72S<>C
<1 :74S*c
<1 :76S«-C
15P 16P 17P 13P 19P 20P 21P **C
vI.DwOl PEGION V DRINKING 4ATER STUDY - MICHIGAN **C
-------
pA-CRt_ 39770 OA S0023 OA 39380 OA 39390 OA 39460 OA S0027 OA S0028 OA *D
1975 OCPA ENDOS I DIELDRIN ENDRIN CL.R8NZLT ENOOS II NITROFEN *D
AMPLE wHL 5MPL WHL SMPL WHL SMPL WHL SMPL wHL SM^L WHL SMPL WHL SMPL *D
OG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *0
213
215
217
219
221
223
225
227
229
.231
• 233
.235
.237
.239
.241
.244
,245
,247
.249
.251
.253
.255
.257
.259
>261
.263
1.265
>267
.273
.275
.782
>784
>786
.788
< . 0 0 3
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.OC3
<.003
<.003
<.003
< . 0 0 3
<.003
<.OOT
<.003
<.003
<.003
<.003
<.003
<.003
<,003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
< . 0 0 3
<.003
<.003
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<,005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<,005
<.005
.005
<.003
<.003
<.003
<.003
<,003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.OQ3
<,003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.OQ3
<.003
<.003
<.003
<.003
<.003
< . 0 0 3
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
< . 0 0 3
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<,003
<.003
<.003
<.003
< . 0 0 3
<.003
<.003
<.003
<.003
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<»01
<,01
<.01
<,01
<.01
<.01
<.01
<.01
<,01
<,01
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.OQ5
<.005
<,005 : 6S*D
<.005 : 8S*0
<,005 :10S*0
<.005 :i2S*n
<.005 :14S*D
<.005 :16S*0
<.005 :18S*D
<.005 :20S»n
<.005 :22S*0
<.005 :24S*0
<.005 :26S*0
<.005 :28S*Q
<.005 :305*0
<.005 :32S*0
<,005 :34S*0
<.005 :37S*D
<.005 !38S*D
<.005 :40SttO
<,005 :42?*0
<.005 :44S«-D
<.005 :46S*0
<.005 :48S*D
<.005 :50S*0
<.005 :52S*0
<.oos : 545*0
<.005 :56S*0
<.005 sS^S-^n
<,005 :60S-»0
<.005 : 665*0
<.005 :68S*0
<.005 :70S*D
<.005 :72S*o
<.005 :74SJJ>D
<.005 :76S*Q
22P 23P 24P 25P 26P 27P 23P **0
•11.0X01 REGION V DRINKING WATER STUDY - MICHIGAN **0
-------
EPA-CRL
1975
SAMPLE
LOG NO.
4213
4215
4217
4219
4221
4223
4225
4227
4229
4231
4233
4237
4239
4241
4244
4245
4247
4249
4251
4253
4255
4256
4257
4259
4261
4?63
4265
4267
4273
4275
4782
4784
4786
4738
vl.0X01
S0029 OA
245-T:10
WHL SMPL
UG/L
S0030 OA
PROLAN
>4HL SM°L
UG/L
50031 OA
BULAN
WHL SMPL
UG/L
S0026 OA
DEHP
WHL SMPL
UG/L
39808 OA
TEDION
WHL SMPL
UG/L
39570 OA
DlAZINON
SMPL
UG/L
S0016 OA
OYFONATE
SMPL
UG/L
-------
-------
FPA-CRL S0017 OA S0032 OA 39600 OA 39530 OA 39540 OA S0033 OA 39398 QA *F
1975 RONNEL DUR58AN MPARATHN MALATHN PARATHN DEF ETHION »F
SAMPLE WHL SMPL WHL SMPL '.VHL SMPL WHL SMPL WHL SM^L ;VHL SMPL WHL SMPL *F
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L »F
1213
4215
4217
4219
4221
4223
4225
4227
4229
4231
4233
4235
4237
4239
4241
4244
4245
4247
4249
4251
4255
4256 .
4257
4259
4261
4263
4265
4267
4273
4275
4782
4784
4786
4788
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
-------
FPA-CRL S0018 OA S0034 OA 39580 OA S0035 OA S0036 OA S0037 OA 39488 OA *G
1975 PHENCAPT EPN GUTHION PHOSALON AZINFOSE COUMAFOS ASOCLOR *G
SAMPLE ,VHL SMPL WHL SMPL WHL SMPL \«HL SMPL WHL SMPL WHL SMPL 1221 *G
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *G
4213
4215
4217
4219
4221
4223
4225
4227
4229
4231
4233
4235
4237
4239
4241
4244
4245
4247
4249
4251
4255
4256
4257
4259
4261
4263
4265
4267
4273
4275
4782
4784
4786
4788
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<1 :<5
<0.3 : 6S*G
<0.3 : 3S*G
<0.3 :10S*G
<0.3 !12S*G
<0.3 :14S*G
-------
-PA-CRL
1975
= AMP(_E
OG NO.
i213
*214
i215
i216
i217
>213
v219
f220
>221
^222
^223
>224
>225
K226
>227
>228
^229
>230
^231
>232
^233
>234
^235
>236
,237
>238
.239
,240
.241
• 242
• 244
.245
.246
.247
248
.249
250
251
252
253
254
255
256
257
258
259
260
261
262
263
264
265
266
267
263
273
274
3949b OA
AROCLOR
1242
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0 .3
<0.3
<0.3
<0.3
<0.3
<0.03
<0.03
39500 OA
AROCLOR
1248
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
39504 OA
AROCLOR
1254
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
39508 OA
AROCLOR
1260
UG/L
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0 .4
<0.4
<0.4
<0.4
<0.3
<0.4
<0.4
< 0 . 4
<0.4
<0.4
<0 .4
S0047 OA
METHE CL
TOT VOL
UG/L
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
H
: 1«S*H
<1 : 19S«H
:20S*H
10 :215*h
:22S*H
<1 :23S«H
:24S<*H
<1 :25S*H
:26S**H
<1 :27S*M
:28S*H
4 :29S**H
:30S*H
<1 :31S^H
:32S*H
IU :33S*H
:345*H
<2 :35?*H
24 :37S*H
:3BS*H
<1 :39S*H
:40S<*H
11 :*IS*H
: 42?>ttH
<1 :43S*H
• 44S*H
47 ^SS*^
: 4 8 5 » •->
<1 :47S*H
:46S^H
27 :49S*H
:50S*H
<1 :51S*H
:52S*H
<1 :53S-»M
: S^f^n
<2 :55S*-
:56S*H
42 :57S*-i
: 5 ** S * M
6 :5QS-*M
:60S<*H
5* :61S»H
: 6 6 5 * ^
7 :67S*M
-------
4275
4276
4782
4783
4784
4785
4786
4787
4783
4789
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0 .3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.4
<0.4
<0.4
<0.4
<0.4
<.5
<0.5
<0.5
20
<0.6
<.5
<1
<1
1
2.1
:68S*H
312 :69S*H
: 70S*H
<1 !71S*»H
: 72S»H
17 :73S*H
: 74S*1-1
1 :75S«H
:765»H
14 :77S*H
50P 51P 52P 53P 54P 55P 56P *<*H
vi.owoi REGION v DRINKING WATER STUDY - MICHIGAN **H
-------
EPA-CRL S0056 OA S0040 OA S0041
1975
SAMPLE
LOG NO.
4214
4216
4218
4220
4222
^224
^226
V228
^230
>232
>234
f236
v238
f240
v242
v244
-n /. £
(• c. ^O
>248
,250
,252
,254
.256
.258 .
.260
• 262
-264
• 266
268
274
276
783
785
797
789
I.DW01
C2H4CL2 CHCL23R
TOT VOL TOT VOL
UG/L UG/L
:<1 :<1
:<1 :26
:<1 :<0.1
:<1 :9
:<2 :<0.5
:<1 : 10
:9 :<0.5
: <2 : 6
:<1 :<0.5
: 3 : 1 6
I < 1 ' < 0 1
• ^ 4. • V \/ t A
:<1 :<0.5
:4 :<0.5
:<2 :o.8
: 2 : < 0 . 5
:<2 : 10
J < 1 : <0 .5
:<1 :23
:2 :<0.5
: <2 : 8
:<1 :<0.2
:<1 :<0.2
:<1 :<0.2
: < 1 : <0 . 1
* ^ •* • ^ w • A
:3 :<0.5
:<2 :5
:26 :<0.5
:<2 :6
:<1 :<0.2
: < 1 : 4
:3 :<0.,5
:<1 :i9
:<1 :<0.5
OA S0042 OA *T
CHCLBR2 CH8R3 «i
TOT VOL TOT VOL »T
UG/L
:<1
:2
:<0.1
:2.4
:<0.5
: ?
• t.
: < 0 . 5
• 1 . "^
• J. * J
:<0.5
:14
• ^ r> i
• < u . i
:•* i
' O Q » T
• 7 J ^^ j_
• 1 1 C <(. T
• i 1 0 ^ 1
:13S*I
• ] C Co T
• i o r5 ^ i
: 175*1
• 1 Q C <>• T
• I 7 O w 1
:21S»I
:23S*I
:25S*I
:27S*I
• "5 Q C A T
• C Vc * I
: "3 1 c« T
• -J i . 3 i
• "3 T C » T
• J J O w i
: 3 5 S «• I
* •— ' — ' »-^ 1
.*37S*I
• *2 Q CT & T
• J 9 b w I
:4is*i
:43S*I
:45S*i
• A 7 C •& T
• 4. / c>w X
: 4 P s * I
• jr 1 C
-------
-------
EPA-CRL
1975
SAMPLE
LOG NO.
4208
4214
4216
4218
4220
4222
4224
4226
4228
4230
4232
4234
4236
4238
4240
4242
4244
4246
.4248
.4250
.4252
.4254
.4256
.4258
.4260
.4262
.4264
.4266
.4268
.4269
.4274
.4276
.4783
14785
U787
14789
.Ml.DWOl
00916 MW
CALCIUM
CAtTOT
MG/L
:<1 :
:58.9 5
:35.4 :
:20.9
:22.2 :
:22.1 :
:23.6 :
:33.5 :
:36.0 :
:135 :
:108 :
: 1 3 0
:89.8 :
:114 :
:16.7 :
:30.6 :
:36.9 :
:96.4 :
:82,9
:33.8 :
:43.3 :
:13.4 :
: 1 3 . 7
:62.4 :
:29.3 :
:33.4 :
:27.9 :
:32.5 :
:26.6 :
:<1 :
:14.3 :
:40.6 :
:27.1 :
:26.0 :
:20.9 :
:33.7 :
64P
REGION V
00927 MW
MGNSIUM
MG»TOT
MG/L
:
:390 :
:230 :
:220 '
:<20 J
:<20 :
: 1 3 0 0 :
:22n :
:26 :
: <20 :
:72 '
:<20 :
:<20 :
:648 :
:<20 :
:34 :
: <20 :
: 170 :
: <20 '
7 OP
*J
*j
*J
*J
1S<*J
7S*J
9S»J
11S»J
13S*J
15S*J
17S*J
19S->J
21S*J
23S*J
25S»J
27S*J
295-^J
31S*J
33S*J
35?*J
37S*J
39S*J
41S*J
43S»J
45S*J
47S^J
49S*J
51S*J
53?»J
55S«J
575*0
59S<»J
61S*J
62S*J
67S*J
695^*0
71?*J
73S*J
75S»J
77S«J
«*j
**J
-------
EPA-CRL
1975
SAMPLE
LOG NO.
.4208
.4214
.4216
.4218
,4220
,4222
.4224
.4226
.4228
.4230
4232
,4234
.4236
.4238
.4240
.4242
.4244
.4246
.4248
.4250
.4252
.4254
.4256
.4258
,4260
.4262
.4264
.4266
.4268
.4269
.4274
.4276
,4783
.4785
.4787
.4789
.MI .DW01
01055 M'W 01092 M-rf 01002 MW 01051 MW 01027 M« 01077 MW
MANGNESE ZINC ARSENIC LEAD CADMIUM SILVER
MN»TOT ZN»TOT AS,TOT P8,TOT CD»TOT AG.TOT
UG/L UG/L UG/L' UG/L UG/L~ UG/L
: <5 : <5
:46 :24
:<5 :<5
: <5 : <5
: <5 : <5
: <5 : <5
: <5 : <5
: <5 : <5
:<5 :83
:50 :<5
:44 : <5
: 61 : <5
: 1 10 : <5
:88 :<5
:<5 :<5
: <5 : <5
: <5 : <5
:95 :210
:92 :180
:35 :<5
:38 :130
:<5 :22
: <5 : <5
.'19 : < 5
: 8 : <5
:<5 :46
:8 : <5
:5 :54
:5 : <5
: <5 : <5
' 13 : <5
: 1 0 : <5
: <5 : <5
: <5 : <5
:<5 :5
: <5 : <5
<1 ' <2
2 :5
<1 : <2
< 1 '2
< 1 : <2
< 1 : <2
<1 :<2
\
<5 :39S<*K
<5 :41S*K
<5 :43S*K
<5 !45S*K
<15 :47S"*K
<5 :49S<*K
<5 tSlS^K
< 5 : 5 3 5 * K
<5 :55S*K
<5 :57S*K
<5 :59S*K
<5 :61S*K
<5 :62S'I*K
<5 : 67?*K
s a fAQc^w
v 7j »O*.JP\
< 5 I 7 1 S *• K
<5 ; "''ss^K
< 5 : 7 5 S * K
<=; :775->K
77P «•»<
-------
-------
FPA-CRL
1975
SAMPLE
LOG NO.
.4214
.4216
.4218
,4220
.4222
,4224
,4226
.4228
.4230
.4232
.4234
.4236
.4238
.4240
.4242
.4244
.4246
4248
.4250
.4252
.4254
.4256
4258
.4260
.4262
.4264
.4266
.4268
.4274
.4276
.4783
.4785
.4787
.4789
.Ml. 0*01
00530 IM
RESIDUE
TOT NFLT
MG/L
:67
:7
:<5
:<5
:7
:<5
:<5
:<5
j<5
:<5
:<5
:6
:<5
:<5
:6
':<5
:<5
:<5
:<5
:<5
:2
:2
:13
:8
:<2
:<2
:<2
:<2
:12
:<2
:2
:<2
:7
:<2
78°
REGION
70300 IM
RESIDUE
DISS-180
C MG/L
:350
:260
: 130
:120
:120
: 140
:170
: 180
:470
:690
:520
:535
:480
:130
:200
:210
:470
5460
:160
:265
:50
:50
:370
:?60
: 180
:210
:205
:170
:80
:240
: 190
:200
: 170
:160
79P
00095 IM
CNOUCTVY
AT 25C
MICROMHO
:516
: 404
:214
:215
:212
:214
:217
:246
:842
:1022
:813
:808
:687
:301
:302
:326
:702
:708
:307
:377
: 104
: 102
:625
:625
:282
:299
:279
:298
: 114
:390
:291
:261
:214
:226
80P
00945 IM
SULFATE
S04
MG/L
:64
:84
:i*
:17
:14
:15
:15
:23
:124
:150
:79
:66
:65
:6l
:24
:31
:94
:94
:17
:26
:<3
:<3
: 14
:17
:19
:43
:19
:44
:6
:ill
:21
:33
:15
:18
81P
V DRINKING WATER STUDY - Ml
00940 IM
CHLO«IOE
CL
MG/L
:23
:27
:7
:9
:8
:8
:9
:14
:44
:73
:45
:54
:9
:18
:il
:13
:35
;37
:10
:18
:<2
:2
:32
:35
:7
J 11
:a
: 11
:2
:7
:16
:17
:8
: 11
82P
CHIGAN
00956 IM
SILICA
SI02
MG/L
:6.5
:6.2
: 1.6
:2.0
: 1.6
:2.0
: 1.6
:2.4
114.7
:14.7
:12.9
:13.8
: 11.4
:9,o
:1.8
:2.1
:9.6
:9.7
:8.2
:7.4
:2.4
:3.1
:18.2
:17.3
:4.7
:5.1
:4.5
:5.1
: 14.0
:5.0
:<0.2
:0.8
: l.b
:2.2
83P
00410 IM
T AL<
CAC03
MG/L
: 146
:46
:75
:6Q
:75
:70
:75
:63
:269
:288
:286
:284
:299
143
: 111
:112
:234
:222
: 120
: 136
:43
:40
!274
:263
:113
:84
: 113
••85
: 40
:68
: 100
:66
:79
:72
84P
*L
*L
*L
*L
: 7S*L
: 9S*L
: 11S*L
: 13S*L
: 15S*L
: 17S»L
: 19S<>L
:21S^L
:235*L
:25S*L
:27S^*L
:29S*L
:31S*L
:33S*L
:35S*L
:37S*L
:39S*L
:41S*L
:^3?»L
545S*L
:47S«L
: 49S*L
:51'S*L
:53S»L
:55S*L
:57S*L
:59S»L
:615*L
:67S*L
:69S*L
:71S*L
:73S^L
:75S*L
:77S<*L
•»•>(_
«•«•[_
L
-------
EPA-CRL
1975
SAMPLE
LOG NO.
14209
U210
14214
14216
14218
14220
14222
14224
14226
14228
14230
14232
14234
14236
14238
14240
14242
14244
14246
14248
14250
14252
14254
14256
14258
14260
14262
1426*
U266
14268
14270
14271
14274
U276
14783
14785
14787
14789
.Ml.OWOl
00403 IM 00951 IM
LAB FLUORIDE
PH F. TOTAL
SU MG/L
;
;
:7.8
:9.7
:a.o
:7.6
:8.0
:7.7
:7.9
:7.4
:7.7
:7.5
:7.8
:7.9
:7.7
:9.4
: 8. 1
: 8. 1
:7.9
:7.7
: 8 . 1
:7.9
:7.5
:7.0
:7.7
:7.8
:7.8
:7.2
:7.9
:7.7
•
•
*
:6.9
: 7.2
:7.9
:a.4
:7.9
:7.5
*
*
n.19 :
1.1 :
0.10 :
0.92 :
0.11
0.90 :
o.ll :
1 .0 :
o.24 :
0.26 :
0.13 :
0.94 :
0 .f 1 :
0.40 :
0.13
1.0 :
1 ..1 :
1.1 :
<0.10 :
<0.10 :
<0.10 :
1.1 :
0.52 :
0.44 :
0.12 :
1.3 :
0.13 :
1.3 :
*
•
< 0 . 1 0
0.14 :
0.13 :
1.2 :
o.ll :
1.3 :
85P 86P
REGION v DRINKING
32730 IM
PHENOLS
UG/L
*
*
*
5 :
3 :
<3
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
<3 :
3 :
<3 :
4 :
<3 :
;
:
5 :
<3
<3 :
<3 :
<3 :
<3 :
87P
00720 IM 00630 IN
CYANIDE N02^N03
CN N-TOTML
MG/L MG/L
0.002
0.004
0.005
<0.002
<0.002
<0.002
0.002
0.003
0.003
0.007
0.004
0.004
0.003
0.008
0 .004
<0.002
0.003
0.002
0.004
<0.002
0.006
0.003
0.003
0.003
0.004
0.004
0 . 00*
0.003
<0.002
<0.002
0.004
0.004
0.003
0.006
0.003
0.003
<0.03 !
t
3.00 :
4.10 :
0.36
0.28 :
0.28 :
0.27 :
0.29 :
0.36 :
<0.03 :
<0.03 :
0.84 :
0.63 :
<0.03 :
0.04 :
0.40 :
0.40 :
0.31
0.30 :
<0.03 :
<0.03 :
0.28 :
0.29 :
<0.03 :
0.13 :
0.16 :
0.16 :
0.14 :
0.14 :
<0.03 :
:
0.17 :
0.20
0.25 :
0.26 :
0.23 :
0.30 :
88P 89P
00610 IN
NH3-N
TOTAL
MG/L
<0.010 :
:
0.228 :
0.042 :
<0.010
<0.010 :
<0.010 :
<0.010 :
0.011 :
<0.010 :
0.179 :
<0.010 :
0.156 :
0.055 :
0.277 :
0.213 :
0.34 :
<0.010 :
0.080 :
<0.010 :
0.115 :
0.022 :
0.040 :
0.013 :
0.218 :
0.159 :
0.027 :
0.013 :
0.035 :
0.013 :
< 0 . 0 1 0 :
:
0.107 :
0.030
0.029 :
0.025 :
0.022 :
0.021 :
90P
00625 IN
TOT KJEL
N
MG/L
<0.05 :
:
1.20 :
0.33 :
0.15 :
<0.05 :
0.20 :
0.11 :
0.12 :
<0.05 :
0.31 :
0.30 :
0.28 :
0.11 :
0.33 :
0.30 :
0.18 :
<0.05 :
0.24 :
0.20 :
0.22 :
0.12 :
0.08 :
0.05 :
0.35 :
0.19 :
0.32 :
0.14 :
0.31 :
0.18 :
<0.05 :
•
•
0.63 :
0.24 :
0.20 :
<0.05 :
<0.05 :
<0.05 :
91P
WATE^ STUDY - MICHIGAN
•»M
*M
«M
*M
2S*M
35*^
7S-&M
9S->M
1 1 S*M
13S*M
155^
17S*M
iqS*M
215*M
23S*M
25S*M
27S*M
29S*M
31S«M
33S*M
•o c c s> y
3 "7 c •* M
39S*M
41 S*M
43S*N*
455*^
475-ovi
49S<*M
5 1 S * M
53S'i1"*
sss*^
57S*M
59S-»M
olS*^
63S*M
64S*M
67S»M
69S*M
7 1 S * t *
73S*M
75S»M
7 7 S * M
»OM
-------
EPA-CRL 00665 IN
1975 PHOS-T
SAMPLE P-WET
LOG NO. MG/L
4208
4209
4214
4216
4218
4220
4222
4224
4226
4228
4230
4232
4234
4236
4238
4240
4242
4244
4246
4248
4250
4252
4254
4256
4258
4260
4262
4264
4266
4268
4269
4270
4274
4276
4783
4785
4787
4789
<0.02
0.13
0.14
< 0 . 0 2
0.02
<0.02
<0.02
<0.02
0.11
0.02
0.02
<0.02
0.38
<0.02
0.10
0.02
0.01
0.44
0.39
0.03.
1.10
0.02
0.02
0.05
0.06
< 0 . 0 2
<0.02
0.03
<0.02
<0.02
0.02
<0.02
0.02
0.02
0.05
<0.02
9?P
^i.owoi REGION
00340 IN 00680 IN 71900 IN
COD T ORG C MERCURY
HI LEVEL C HG»TOTAL
MG/L MG/L UG/L
:
: <3
:25
: 1 1
!6
:5
:3
* O
: 10
: <3
: 1 1
: <3
:7
: <3
: 4
: 4
:3
:<3
:6
* Q
: 13
: 4
: 1 0
:7
:3
: 4
5 16
: 9
: 18
: 8
:
: <3
:38
: 13
:9
:5
:5
:5
•
<0 . 1
<0 . 1
<0 • 1
<0 . 1
<0 . 1
<0 . 1
<0 . 1
<0 . 1
<0 . 1
<0 . 1
0.1
<0 . 1
<0 . 1
0.1
0.1
<0 . 1
<0. 1
<0 . 1
<0 . 1
<0 . 1
<0 . 1
0.2
<0 . 1
<0 . 1
0.1
<0 . 1
<0. 1
<0. 1
<0 . 1
< 0 . 1
0.2
0.1
n.l
0.1
0.2
0.1
93P 94P 95P
00900
TOT HA
CAC03
MG/L
: <3
:
'212
:97
:81
:85
:86
:87
J114
5121
:468
!417
:457
:356
:417
:97
:125
:141
:346
5311
:123
: 158
: 45
:46
:259
: 1 1 1
: 138
:124
:136
:122
: <3
:
: si
••us
: 106
:94
:83
:115
96P
V DRINKING WATER STUDY - MICHIGAN
IN 00615 IN *N
RU N02-N <>N
TOTAL *N
MG/L *N
:
:
: 0 . 0 6 1
:0.005
: 0.005
:<0.005
:0.006
:<0,005
20.007
:<0.005
:<0.005
:<0.005
:0.016
: <0.005
:0.005
:0.013
:0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
K0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
: <0.005
:
:
!0.007
:<0.005
:0.005
:<0.005
J0.005
:<0.005
j 1 S ^ N
J p C & Fvj
: 7*M
! 0 *5 ^ N
* 1 1 S ^ ^
: 13S*\
! 15S*N
: 1 7S*N
: 1 9 S * N
: 2 1 S * N
: 23S*N
: 25S*N
:27S*N
'•295*^
: 31S*N
:335*N
: 35S*N
: 37S*^J
:39S»N
:41S*N
: 43S*N
:45S*N
: k.~j S^NJ
: 49 5*N.
: 51 5'*N
:53S»N
• 55 5 *\j
; 575 ^N
: 5 9 ? » ,\
: 61 S*NJ
: 6?S*N
: 63S*N
: 6 7 S * N
:69S*N
:71S*N
: 73S*N
:75S»N
: 7 7 S * N
97P 98P * * N
-------
:RLS OSAPR DSN=
REVOI T
MPAR NL06
94 77
>»REGION
_ABID.\UM S
14277
14278
14279
14280
14281
14282
14283
14284
14285
14286
14287
14288
14289
14290
14291
14292
14293
14294
14295
14296
14297
14298
14299
14300
14301
14302
14303
14304
.4305
14306
14307
14308
14309
14310
.4311
.4312
.4313
.4314
.4315
.4316
.4317
.4318
.4319
.4320
.4321
.4322
.4323
.4324
.4325
AGEN'CVIO UNLOCKEY ST
77
V DRINKING WATER STU
TORETID COLLOAY TIME
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203 •
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
CNCPLS.RGD.MN.DW01 ON TS0009 04/19/75
STUDY DESCRIPTION
STATTYPE SMPLDAY ATLA8BY DUEDATE ACCOUNT-NUMBER
77777777 03FEB75 05FEB75 03MAY75
DY - MINNESOTA
SAMPLE DESCRIPTIONS
STATTYPE DEEP T M NO ENDOATE TIME PRLU
-------
14326
1*327
14328
14329
14330
14331
1*332
1*333
U334
U335
14336
14337
1*338
1*339
U340
1*341
U342
14343
14344
14345
14346
14347
1*343
14349
14350
U351
1 -O52
14353
»>'.*277
>»14273
>» 1*279
>>> 1*290
>»l*231 •
•* •* > 1 4 7 *l ?
f > f 1 ** C ~ C
>»1*233
>»1*234
>»1*2S5
>»14236
»>1*297
» > 1 * 2 3 8
»>1*289
>» 1*290
>»14291
>»!*292
>»1*293
>>> 14294
>» 1*295
>»i *296
»>14297
>>>14293
>»14?99
»>1*300
» > 1 4 3 0 1
>-*i1*^OJ
f > * i**J'JC
>»1*303
>»! 4304
750203
750203
750203
750^03
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750233
750203
750203 M I rt ^ £ S. 0 T A-
7 = 0203 •
750203
» H^03 =)E4oENT ?L4N<
» H2S3* =EAOEN* ?LAMK
» NAOW SEAGEM 3LANK
?> r^B^O^1 "^ c A 0 c ^ i 3L.A'*ir\
» OPE'-'
JTV||>.C .arii r r _ « >., _^TC3 ccnrrc \ — L-V f /> /^ \ 1 C^ 7
^^ ^'iiNll^^l-o^i^ ^M1 WW'^T Jt_"iu.J -» ^ — ——— i ^^ f^ | ' j >^ f-\ ^
» MlMNfirOLIS ^i* **ATE3 SERIES S '
» «IMN£A'JOLIS FIMISrEO JiATE^ SERIES i
» wi\iN£40QLIS FIMISHED '*JTE3 SERIES 3
» MINNEAPOLIS ^-i1* ^AT£P SERIES A
» ••
^^ ^T.JVM PA-J *aTF3 SF=^«; a Uj -^ ,OC ^ I ""* '
» 37, = ;,JL ^A.V WATER SERIES 3
» ST.=4UL FINISHED '-I4.TER SERIES A
» ST. PAUL FIMIi"EO HATE' SE^IEi 3 , , ,,
Linf,)^ \7.-> = ^ rt ^^T?3 -:c- rn v . '-JM 1 ^ (^ ' '-' 4 . '
» ^AN•> rr~A [ zJu.vTTjrT; »A* jiT-K <;fjr^=; i - pr /^ o ^^ ~) v_) "T~ ^ •
> > rl-t-^^ftTCTN'T 3 A * //ATE^ SERIES 9
» CAI^VIOUNT r!NI5nEO ^iTE1? SERIES i
» ^AI-JMOUNT -INIS^ED DATE'S SERIES S , v A ^- - ,
11 G^i'lITC^JLLj t\niit\Tr^';~"'T'""5i M"1^ 4<-\'Xo lj>,-?i
» G •> 4 N 1 T E F 4 '_ L 5 ^A* •lATE3 SESItS 3
» jH«NiTE 'ALLS -INIS^EO «ATE' SERIES A
-------
»>1*305 '-
>>>1*306 -
»>1*307 :
»>1*303 -
»>1*309 :
>>>1*310 '
>»1*312 ~
>»1*313 :
»>1*315 :
> » 1 * 3 1 6 =
>»1*317 :
»>1 *31 3 :
>»1*319
>»1*320 :
>» 1*321 =
>»1*322 :
>»1*323 :
>»1*32* =
>»1*225 -
»>1*327 :
»>1*32J =
>»1*329 :
>» 1 *">30
>»U331
>»1*332 •
>»1*333 =
>»1*33* :
>»1*335 :
>» 1 *336 :
>»1*337 :
>» 1*333 *
» 1*339 =
» 1 *3*0 =
» 1*3*1 :
» 1*3*2
» 1*3*3
»> 1 *3**
>»j.4346
»;> 1»3*7
»> 1 »3*S :
>»1*350
> » 1 * 3 5 1
>»l*352
»> 1*353
> GRANITE FALLS FINISHED WATER SERIES d
•> *ILLMA« RAd WATER SERIES 3
•> wIi_i_MAR FINISHED WATER SERIES A
» ^ILLMAR FINISHED wAT£3 SERIES 3 _ , \
«> 51* CLOUD RAW WATER SERIES A • -•• — — ^ ^ * ^*i ^J
» ST. CLOUD RA* WATER SERIES 3
» ST. CLOUD FINISHED *ATFR SERIES A
•> ST. CLOUD FINISHED WATER SERIES 8 LV 1 \ U K\
» 8RECKENRIOGE RAW WATER SERIES 3
» aRECKENRiDGE FINISHED WATER SERIES A
» 3RECKENRIOGE FINISHED WATER SERIES 3
•> rLjOOKSTONPi\,ifMTcoSF°IF.Si\ . ' \ ~) ' V" "~1 ^'
» CKOOKSTON RAW WATES SERIES 3 ' ' ^ ' '
» CROOKSTON PJNIS.-iED »(ATER SERIES A
» CROOK5TON FINISHED W&TER SERIES 3 v
•> EAST GRAND FORKS RAW oATER SERIES A H 7 • S b NJ C|
» EAST GRAND FORHo ^Aw ^AT£R SERIES 3
» EiST GRAND FORKS rINISH£0 WA"£= SERIES A
» EAST GRAND FO^xS FINISHED wAi£R 5£=>Ii^ 3 i
» OSl 0 RAW aAT'R SERIES A . M ^ . \ ^ K)
» OSLO RAW WATER SERIES 3
» OSLO FINISHED WATE'R SERIES A
» OSLO FINISHED WATER SERIES 8 _ |
> RICHFIELD RAW WATER SERIES 3
> y!C*FIELD FINISHED wiTER SERIES A
> Ric-iFiELO -INIS-EO WATER SERIES 3 _ ^ ,
» INTERNATIONAL FALLS RA* WATER SERIFS ^ Mo • 0 ^ N
> INTERNATIONAL FALLS RA^ WATER SERIES d
> INTERNATIONAL FALLS FINISHED WATE-^ StiIES A
•> INTERNATIONAL rALLS FINISHED »ATER st-iss 3
» nt,|_,iT-(R^fl^^TE'3^FR*rv4_ \ \. \ ^-\ ^ ^
» DULUTH RAW wATF'-? SERIES 3
» DULUTn FINISHED WA~E= SERIES A
» DULUT-i FlNlSiED WAT£P SERIES 3
» DULJTH RAW wAT£R SERIES A
» DUL'JTH RAK «AT£R SERIES 3
» OULJTH FINISHED WATER SERIES A
» DUL'JTH FLUSHED WATE3 SERIES 3
» HNQ3 REAGENT 3LAN<
» H2SO* ^'EAGENT BLANK
» NAOn ^EAGENT 3LANK
» H3PO* REAGENT 3LA'j<
» OP-N
>03\Aj
r • I o ^
C\U."
-i wJ
V 0
°\ a. \ o w
-------
AL
E
0.
01
S0003 OA
TPEFLAN
'WHL SMPL
UG/L
<0.002
<0.002
< 0 . 0 0 2
< 0 . 0 0 2
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
< 0 . 0 0 2
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0 .002
<0.002
< 0 . 0 0 2
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
< 0 . 0 0 2
<0.002
< 0 . 0 0 2
< 0 . 0 0 2
<0.002
<0.002
IP
PEGION \
S0001 OA
HC8ENZ
WHL SMPL
UG/L
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
-------
i-CRL 39430 OA 39420 OA S0006 OA S0007 OA S0008 OA S0009 OA S0010 OA *8
>75 ISODRIN HCHLR-EP CHLORDAG DDE OP ODE PP ODD OP DDT OP *B
*P|_E WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WhL SMPL WHL SMPL »8
> NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *3
\2 :<0.003
54 !<0.003
56 :<0.003
58 :<0.003
)0 :<0.003
>2 :<0.003
>4 :<0.003
)6 :<0.003
)8 :<0.003
)0 :<0.003
52 :<0.003
)4 :<0.003
)6 :<0.003
)8 :<0.003
.0 :<0.003
.2 :<0.003
.4 :<0.003
.6 :<0.003
.8 :<0.003
20 :<0.003
22 :<0.003
24 :<0.003
26 :<0.003
23 : < 0 . 0 0 3
30 :<0.003
32 :<0.003
34 :<0.002
36 t<0.002
38 :<0.002
!>0 :<0.002
R
<0.003 :3bS*H
<0.003 :38S*B
<0.003 :40S*3
<0.003 :42S<*Q
<0.003 :44S*»B
<0.003 :46S*i?
<0.003 :48S*R
<0.003 :505*«
<0.003 :52S-i>-3
<0.003 :54S*«
<0.003 :56S*3
<0.01 tS^S*'^
<0.01 : 605*9
<0.01 :62S*R
<0.01 :64S»^
<0.01 :66S-»B
<0.01 :68S*B
<0.01 :?4S*H
<0.01 :76S*«
qp gp iop UP 12P 13P 14P »*P
.0^01 REGION v DRINKING WATER STUDY - MINNESOTA **3
-------
^PA-CRL soon OA 50012 OA sooia OA sooi4 OA 39490 OA sooso OA 50021 OA *c
1975 ODD PP DDT PP CARBPHTH MIREX MTHXYCLH 2»4-D:IP DNSP *C
SAMPLE *HL SMPL WHL SMPL WHL SMPL 4HL SMPL WHL SM?L WHL SMPL WHL SMPL *C
_OG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *C
4.282
4284
4286
4288
4290
4292
4294
4296
4298
4300
4302
4304
4306
4308
4310
4312
4314
4316
4318
4320
4322
4324
4326
4328
4330
4332
4334
4336
4338
43^0
4342
4344
4350
4352
<0.003
<0.003
<0.003
<0.003
< 0 . 0 0 3
<0.003
<0.003
<0.003
<0.003
<0,003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
< 0 . 0 0 3
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
0.008
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.005
<0,005
<0 ,005
<0,005
<0,005
<0,005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.003
<0.003
<0.010
<0.010
<0.010
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.02
<.01
<.01
<.01
<.01
<.01
<.01
<1 : *>S*C
<1 : 9S*C
<1 :iOS<*c
<1 :12S*C
<1 :14S*C
<1 :i6S*c
<1 :IBS*C
<1 :20S*C
<1 :22S*C
<1 :245<*C
<1 :26S«-C
<1 :28S<*C
<1 :30S<>c
<\ !32S»C
<1 :34S*C
<1 :36S*C
<1 !38S*C
<1 :40S*c
<1 :42S*C
<1 :44S*c
<1 t46S*C
<1 :48S*c
<1 :50S*c
<1 :S2S»c
<1 :54S*C
<1 :56S-*C
<1 :58S*C
<1 :60S»C
<1 :6?S*C
<1 :64S*C
<1 :66S-*C
<1 :68S*c
: 74S*c
:76S^*c
IS=> 16° 17P 18P 19P 20P 21P **C
MN.DWOI REGION v DRINKING WATER STUDY - MINNESOTA *«c
-------
EPA-C&L 39770 OA S0023 OA 39380 OA 39390 OA 39460 OA S0027 OA S0028 OA *0
1975 DCPA ENDOS I DIELDRIN ENDRIN CL^NZLT ENDOS II NITHOFEN *0
SAMPLE WHL SMPL WHL SMPL WHL SMPL VHL SMPL WHL SM^L WHL SMPL WHL SMPL *0
LOG NO. UG/L UG/L - UG/L UG/L UG/L UG/L UG/L *0
4282
4284
4286
4288
4290
4292
4294
4296
4298
4300
4302
4304
4306
4308
4310
4312
4314
4316
4318
4320
4322
4324
4326
4328
4330
4332
4334
4336
4338
4340
4342
4344
<.003
< . 003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.OOJ
<.003
<,003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.005
<.005
<.005
<.005
<,005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<,005.
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
< .005
<.005
<.005
<. 005
<.005
<.005
<.005
<.005
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
< . 0 0 3
<.003
<.003
<.003
<«003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005 : 6S*D
<.005 : t
-------
EPA-CRL 5002^ OA S0030 OA S0031 OA S0026 OA 39808 OA 39570 OA S0016 OA *E
1975 245-T:lO PROLAN 8ULAN OEHP TEDION DIAZINON OYFONATE *E
SAMPLE WHL SMPL WHL SMPL wHL SMPL wHL SMPL WML SM^L WHL SMPL WHL SMPL *E
LOG NO. UG/L UG/L ' UG/L UG/L UG/L UG/L UG/L *£
4282
4284
4286
4288
4290
4292
4294
4296
4298
4300
4302
4304
4306
4308
4310
4312
4314
4316
4318
4320
4322
4324
4326
4328
4330
4332
4334
4336
4338
4340
4342
4344
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.0l
<.0l
<.0l
<.0l
<.01
<.01
<.0l
<.0l
<.01
<.01
<.0l
<.01
<.01
<.0l
<.0l
<.0l
<.01
<.0l
<.01
<.01
<.01
<.0l
<.01
<.0l
<.0l
<.01
<.01
<.01
<.01
<.01
<.0l
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<1
<1
A
<1
<1
<1
<1
<1
1
<1
<1
<1
<1
<1
2
<1
<1
<1
<1
1
o
1
<1
<1
<1
2
<1
<1
1
<1
40
2
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.oi
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.Q1
<.01
<.01
<.01
<.01
<.01
<.01
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1 : 6S*E
<1 : BS-^E
<1 :10S*£
<1 :i2S*t
<1 :14S*E
<1 :16S*E
<1 :ias*E
<1 :20S*E
<1 :22S*E
<1 :24S»E
<1 :26S*E
<1 :28S*E
<1 530S*E
<1 :32S*E
< 1 : 3 4 S * E
<1 :36S*F
<1 :38S«-E
<1 :4CS*E
<1 :42S*E
<1 !44S*E
<1 !46S*E
<1 :4as-»E-
<1 :SOS-*E
<1 :C52S*E
<1 :54S*E
<1 :56S*E
<1 55«S*£
<1 :60S*E
<1 :62S*E
<1 :64S*E
<1 :663*£
<1 fSSS^E
29" 30P 31P 32P 33° 34P ISP **E
wN.DWOl REGION V DRINKING WATER STUDY - MINNESOTA **E
-------
PPA-CRL S0017 OA S0032 OA 39600 OA 39530 OA 39540 OA S0033 OA 39398 OA *F
1975 RONNEL QUtfSBAN MPARATHN MALATHN PAPfiTHN DEF £THION *F
SAMPLE rtHL SMPL VvHL SMPL WHL SMPL ViHL SMPL rfHL SMPL 4hL SMPL WHL SMPL *F
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *F
4282
4284
4286
4288
4292
4294
4296
4298
4300
4302
4304
4306
4308
4310
4312
4314
4316
4318
4320
4322
4324
4326
4328
4330
4332
4334
4336
4338
4340
4342
4344
< 1
<1
<1
v. X
*>F
<1 :12S*F
<1 :16S*F
<1 : 1 -3S*P"
<1 : 20S-f>F
<1 :22S»F
<1 :24S'!*F
<1 * 5 £k t *i C*
X * C O O »
<1 :28S*F
<1 :30S*F
<1 :32S'*F
<1 .'34S*F
<1 :36S*F
<1 :38S*F
<1 :40StfF
<1 :42S*F
<1 :44S*F
<1 :46S»F
<1 :48S*F
<1 :50S*F
<1 :52S*F
<1 :54S*F
<1 :565<*F
<1 :S8S»F
<1 :60S«-F
< 1 : 625*?"
<1 :64S'l*F
<1 :66S«F
<1 :68S*F
36P 37P 38P 39P 40P 41P 42P **F
^N.OWOl REGION V DRINKING WATER STUDY - MINNESOTA *<*F
-------
PA-CRL SOOIB OA 50034 OA 39530 OA 50035 OA soo36 OA 50037 OA 39488 OA *G
1975 PHENCAPT EPN GUTHION PHOSALON AZINFOSE COUMAFOS AROCLOR *G
AMPLE WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMHL WHL SMPL 1221 *<3
,OG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *G
282
,284
,286
288
,290
292
,294
.296
.298
.300
.302
.304
.306
.308
.310
.312
.314
.316
.318
.320
.322
.324
.326
.328
.330
.332
.334
.336
.333
^40
.342
.344
.350
.352
1
<1
<1
<1
<1
^ 1
^ 1
<1
<1
^ i
<1
<1
<1
<1
<1 : <5
< 1 : <5
<1 : <5
<1 : <5
<1 : <5
<1 : <5
<1 :-<5
<1 : <5
-------
PA-CRL
1975
:AMPLE
OG NO.
282
.283
.284
,285
.286
.237
.288
.289
.290
• 291
.292
.293
.294
.295
.2=f6
.297
.298
.299
• 300
.301
.302
.303
.304
.305
.306
.307
.308
1.309
.310
.311
.312
.313
.314
.315
.316
.317
.318
1.319
.320
,321
.322
.323
.324
.325
.326
f327
.328
.329
.330
.331
.332
.333
*334
.335
.336
.337
*338
39496 OA
AROCLOR
1242
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
39500 OA
AROCLOR
1248
UG/L
<0.3
<0.3
<0.3
<0.3
<0'.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0 .3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0 .3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
39504 OA
AROCLOW
1254
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
39508 OA
AROCLOR
1260
UG/L
<0.4
<0.4
<0.4
<0.4
<0.4 *
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0 .4
<0 .4
<0.4
<0 .4
<0.4
<0.4
<0.4
<0.4
<0.4
<3.4
S0047 OA
METHE CL
TOT VOL
UG/L
<0.5
<0 .5
<0.5
<0.5
<0.b
<0.5
<0.5
<0.5
-------
^339
v340
^341
^342
^343
^344
>345
v350
v352
<0 .3
<0.3
<0.3
<0.3
<0 .3
<0.3
<0.3
<0.3
<0.3
<0,3
<0.3
<0.3
<0 .3
<0.3
<0.3
<0.4
<0.4
<0 .4
<0.4
<0.4
<0.5
<1
<0.5
<1
<2
20
3
25
20
28
1
26
!63S*H
I64S*H
!65S*H
66S*H
67S*H
68S*H
69S*H
74S*H
TfSSo*-1
50P 51P 52P 53P 54P 55P 56P **M
-(N.OW01 REGION V DRINKING WATER STUDY - MINNESOTA **H
-------
EPA-CHL S0056 OA S0040 OA S0041 OA S0042 OA * I
1975 C2H4CL2 CHCL2BR CHCL8S2 CHRn<3 *I
SAMPLE TOT VOL TOT. VOL TOT VOL TOT VOL *I
_OG NO. UG/L UG/L UG/L UG/L *I
4283
4285
i287
4289
1.291
4293
4295
+ 297
4299
4301
1-303
4305
4307
4309
4311
1313
4315
4317
4319
4321
4323
4325
4327
4329
4331
«-333
4-335
4337
4339
4341
4343
4345
<1 :<0.5
<1 :<0.5
<1 : <1
<1 :<0.5
<1 : <1
<5 :6
<0.5 :<0.5
<1 :9
<3 :<1
<5 :31
<1 : <1
<0.5 :0.5
<1 :<0.5
<0.5 :<0.2
<1 : <1
<1 :4
<1 :<0.5
<3 : 15
< 1 : < 1
<1 :o.8
<0.5 :<0.5
< 1 : 0 . 8
<2 :<1
<5 :5.0
<0.5 :<0.5
<0.5 :<0.5
<1 : <1
< 1 : 0 . 3
<1 : < 1
<1 :3
<0.5 :<0.5
<1 :3
<0.5
<0.2
<0.5
<0.2
<0.5
<0.2
<0.5
2
<0.5
0.7
<0.5
<0.2
<0.5
<0.2
<0.5
<0.2
<0.5
<0.5
<0.5
<0.2
<0.5
<0.2
<0.5
<0.2
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<1
<0.5
<0.5
<0.5
<1
<2
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<1
i
<1
< 1
<0.5
<1
' 7S*I
: 95*1
: 1155*1
: 13S*I
: 15S*I
J 17S»i
: 19S*I
: 2 1 S* I
:23S*i
! 25S*I
:27S*I
' 2^5*1
•'3 IS* I
:33S»I
:35S*I
:37S*I
:39S*I
:41S*I
:43S*I
t 45S<*I
:47S»I
: 4QS»i
:51S*i
:535»I
:55S-*I
: S7S*I
: 59S*I
•* 6 1 S * I
; s 3 s * i
: SSS^I
; 67S*I
: 69S*I
57° 58P 59P 6QP 61P 62P 63P *»I
MN.D401 REGION V DHINKING WATER STUDY - MINNESOTA »*I
-------
EPA-CRL
1975
SAMPLE
_OG NO.
4277
4282
4284
4286
4288
4290
4292
4294
4296
4298
4300
4302
4304
1306
v308
4310
4312
4314
4316'
4318
4320
4322
4324
4 3 2 6 -
4328
4330
4332
4334
4336
4338
4340
4342
4344
4346
^N.DWOl
00916 M* 00927 MW
CALCIUM MGNSIUM
CA»TOT MG»TOT
MG/L MG/L
: <0 . 1
:40.8
: 16.3
:40.8
:16.5
:42.4
:20.5
:102
:44.5
:51,4
124.0
:95.0
:77.5
:96.o
:97.2
:47.7
:22.0
:43.1
:18.6
:45.2
:44.3
:45.3
:25.6
:52.9
:18.7
:62.6
: 15 . 1
:5.2
:4.9
:12.5
:12.8
:12.ft
:12.4
: < 0 . 1
0.3 :
13.9 :
8.6 :
13.8 :
8.4 ;
14.6 :
7.4 :
40.6 :
7.3 :
32.7
15.4 :
62 :
6.0 :
41.4 :
45.6 :
17.0 :
s.6 :
31.5 :
15.8 i
15.7 :
15.5 :
15.6 :
2.1 :
22.1 :
19.4 :
26.4 :
9.7 :
1.8
1.8 :
2.9 :
3.0 :
2.9 :
2.8
<0 . 1 :
64P 65P
REGION V DRINKING
00929 MW 00937 M* 01034 Mw 01042 MW 01045 My
SODIUM
NA»TOT
MG/L
<0 . 1
5.5
6.0
4.7
5.9
6.5
7.0
33.3
33.6
9.7
39.3
35.6
85
24.5
29.2
7.5
7.0
10.1
13.6
3.8
3.8
4.2
7.4
13.0
28.4
5.7
5.8
1.3
7.6
1.4
1.4
1.4
1.3
0.1
66P
WATER
PTSSIUM CHPOMIUM COPPER IRON
K,TOT C*»TOT CU,TOT FE»T(JT
MG/L UG/L UG/L UG/L
: <0 . 1 : <5
: 1 . 7 : <5
: 1 .8 : <5
: 1 .7 : <5
: 1 .7 : <5
: 1 . 9 : < 5
: 1 .9 : <5
:4.7 :&
: 4.8 : <5
:3.7 :<5
:4.0 :<5
:7.4 :<5
:7.7 :<5
: 3. 1 : <5
:3. 1 : <5
:2.0 :<5
:2.0 : <5
: 4 , 0 : <5
:4.2 :<5
:2.4 :<5
:2.3 :<5
:2.2 :<5
:2.4 :<5
:3.3 :<5
:3.4 :<5
: 1 . 7 : <5
: 1 .8 : <5
: 0.8 :<5
: 0.7 :<5
: 0 .6 : <5
: 0. 7 : <5
: 0.6 : <5
: 0.6 :<5
: 0 * 1 : <5
<10 :<20
<10 :210
<10 :<20
<10 :170
<10 :<20
15 :46
<10 :<20
51 :370
29 :<20
<10 :36
<10 :<20
<10 :110
<10 : <20
10 U630
<10 :1050
36 1220
<10 :<20
< 10 : 14ft
<10 :26
<10 :62
<10 :56
<10 1120
<10 :<20
<10 : 140
<10 :36
<10 :300
<10 :<20
<10 :24
< 1 0 : < 2 0
<10 :66
<10 .'64
<1 0 :70
<10 :56
11 :<20
67P 68P 69P 70P
STUDY - MINNESOTA
J *J
*J
*J
«-j
: 1S»J
: 6S»J
: 85* J
: 1 OS^j
: 12S*J
: 14S<*J
: 16S*J
: 18S»J
: 205*0
: 22S<>J
'. 245-^J
: 26S*J
:2SS*J
: 30S*J
: 32S*J
: 34S-*J
: s^S^J
: 38S*J
:40S*J
:42S*J
:44S*J
I46S*J
! 48S<*J
:50S*J
:52S*J
:54S*J
:56S»J
:585**J
:60S*J
' 62S*J
:64S*J
: 66S*J
:68S*J
: 70S*J
**j
-------
EPA-CP.L
1975
SAMPLE
LOG NO.
4277
4282
4284
4286
4288
4290
4292
4294
4296
4298
4300
4302
4304
4306
4308
4310
4312
4314
4316
4318
4320
4322
4324
4326
4328
4330
4332
4334
4336
4338
4340
4342
4344
4346
MN.DdOl
01055 MW 01092 MW
MANGNESE ZINC
MN,TOT ZN»?OT
UG/L UG/L
:<5 :<5 :
:45 :19 :
:<5 :<5 :
:32 :io :
:<5 :<5 :
:28 :120 :
:<5 :<5 :
:320 :7 :
:<5 :is :
:180 :15
:<5 :6 :
:120 :9 :
:<5 :<5 :
:95 :<5 :
:70 :<5 :
:72 :a :
:6 :<5 :
:26 :i3 :
:<5 :<5 :
: 1 8 : 1 4 :
:30 :<5 :
:20 :<5
:<5 :<5 :
:36 :7 :
:5 :<5 :
:104 :7 :
:<5 r<5 :
:6 :<5 :
:<5 :<5 :
:<5 :91 :
:<5 :170
:6 :91 :
:<5 : 170 :
:<5 :<5 :
TIP 72P
4
PEGION V DRINKING
01002 MW 01051 M* 01027 «"!'
ARSENIC LEAD CADMIUfM
AS.TOT PStTOT CD»TOl
UG/L UG/L UG/L"
<1 :<2 :<0.2
<1 t<2 :<0.2
<1 :<2 J<0.2
<1 : <2 J<0.2
<1 : <2 : <0.2
1 :3 :<0.2
<1 :3 :<0.2
<1 :<2 :<0.2
<1 :<2 :<0.2
3 :<5 :<0.2
1 :3 :<0.2
4 :<2 :<0.2
1 :<2 ;<0.2
4 :<2 :<0.2
<1 :<2 :<0.2
1 :<2 :<0.2
<1 :<2 :<0.2
3 :<2 :<0.2
<1 :<2 :<0.2
1 :<2 :<0.2
1 :<2 :<0.2
1 :<2 :<0.2
<1 :<2 :<0.2
2 :3 :<0.2
1 :<2 :<0.2
<1 :<2 :<0.2
<1 :<2 :<0.2
<1 :<2 :<0.2
<1 :<2 :<0.2
<1 :<2 :<0.2
<1 :<2 :<0.2
<1 :<2 :<0.2
<1 :<2 :<0.2
<1 :3 :<0.2
73P 74P 75P
WATER STUDY - MINNESOTA
ft 01077 MW
SILVER
AG»TOT
UG/L
:<0.2
:<0.2
:<0.2 ;
:<0.2 :
:<0.2 :
:<0.2 :
:<0.2 :
:0.3 i
:0.3 !
:0.3 :
:0.3 :
: 0 .'2 :
:0.3 !
J < 0 . 2 J
:<0.2 !
:<0.2 •
:<0.2 :
:<0.2 :
:<0.2 :
' <0.2 :
:<0.2 :
:<0.2 :
:<0.2 :
:<0.2 :
:<0.2 :
:<0.2 :
:<0.2 :
:<0.2 :
:<0.2 :
:<0.2 :
: < 0 . 2 :
:<0.2 :
:<0.2 :
:0.7 :
76P
01147 MW «<
SELENIUM <*K
SE»TOT »«
UG/L *K
:<5 : 1S*K
:<5 : 6S*K
:<5 : 8S*K
• <5 : 10S*<
:<5 :12S*<
:<5 :14S*K
i<5 :16S*K
:<5 J1RS*K
:<5 :20S*K
:<5 :22S<*K
: <5 :24S-*K
i<5 :26S-*(<
i
-------
cpA-CRL
1975
SAMPLE
LOG NO.
.4282
.4284
4286
14288
14290
14292
14294
14296
14298
14300
14302
14304
14306
14308
14310
14312
14314
14316
14318
14320
14322
14324
14326
14328
14330
14332
14334
14336
14338
14340
14342
14344
.MN.DWO
• -. — — — — —
00530 IM
RESIDUE
TOT NFLT
MG/L
:2
:<2
:4
:<2
:<2
:<2
:<2
:<2
:<2
:<2
55
s<2
:74
:42
:2
:<2
:13
:<2
:6
:5
59
:2
:6
:<2
:<2
:<2
:<2
:<2
:3
:3
:4
:3
73P
( w '
1 REGION
• •-. — — — — — — —
70300 IM
PESIDUE
OISS-180
C MG/L
:220
:110
:200
: 140
:?60
: 170
:660
:360
:440
:330
:860
:690
:490
:520
:270
:200
:360
:230
:270
:280
:230
:160
:360
:250
:330
:130
:40
:50
:70
: 100
:50
:45
79P
V ORINKI
*..«_•»•«»•*»
00095 IM
CNDUCTVY
AT 25C
MICROMHO
:354
: 205
:338
:202
:352
:222
:910
:496
:585
:425
: 1070
:860
:720
:815 '
:404
:234
:487
:293
:355
:367
:348
:182
:496
:364
:525
: 193
:54
:92
: 105
: 104
: 103
: 104
80P
NG WATER
— — •""•~~*'~ —
00945 I
SULFATE
S04
MG/L
:12
:23
:ll
:23
: 12
57
:162
:162
:58
:63
:244
:279
:42
f O
: 62
:23
:35
:26
:20
:14
:25
: 13
:17
: 8
:<3
:17
:28
. . n
: < 3
: 14
• ^ "5
: <3
: <3
•^
: <3
:<3
81P
STUDY -
M 00940 IM
CHLORIDE
CL
MG/L
56
• O
« y
:7
:il
• 1 A
5 i o
• o
5 9
:25
:30
:28
:38
:23
:28
:16
• \ c*.
• 1 o
:17
518
:17
:24
514
:3
• o
5 C
:5
• -3
* J
:2
54
• /,
• 4
• X?
• ^ C.
• o
I C
* f 1
• <-c.
• x O
• <£
• x O
• L
566S»L
S68S*L
•**L
<* <* (
•»•»[_
-------
EPA-C&L
1975
SAMPLE
LOG NO.
,4278
.4279
.4230
.4282
.4284
.4286
.4288
14290
14292
14294
14296
14298
14300
14302
14304
14306
14303
14310
14312
14314
14316
14318
14320
14322
14324
14326
14328
14330
14332
14334
14336
14338
14340
14342
14344
14347
14348
.MN.DWO
00403 IM
LAB
PH
su
7.7
7.6
7.7
7.6
7.6
8.1
7.4
7.1
7.5
9.4
7.8
8.7
7.3
7.3
7.6
8.8
7.8
8.3
7.7
7.2
7.6
9.4
7.7
9.2
7.6
8.8
7.2
6.7
7.3
7.0
7.2
7.0
85P
1 REGION
00951 IM
FLUORIDE
F»TOTAL
MG/L
0.12
1.1
0.11
1.2
0.12
1.2
0.25
1.2
0.37
1.2
0.26
1.3
0.31
1.1
0.14
1.0
0.17
0.96
0.12
0.91
0.12
1,2
0.15
0.89
0.20
1.5
<0.10
0.92
<0.10
1.1
<0.10
1.1
86P
32730 IM
PHENOLS
UG/L
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
<3
87P
V DRINKING WATER
00720 IM
CYANIDE
CM
MG/L
<0.002
0.003
0.003
<0.002
0.003
0.003
0.004
0.005
0.003
0.004
0.006
0.005.
0.004
0.002
0.003
0.003
0.003
0.002
0.003
<0.002
0.006
0.002
0.004
0.002
0.004
<0.002
0.002
<0.002
0.003
0.003
0.002
0.003
0.002
0.002
88?
STUDY - M
00630 IN
N02*.N03
N-TOTAL
MG/L
: <0.03
•
•
:0.41
:0.40
:0.40
:0.39
:0.57
:0.37
:0.46
:0.59
:0.90
:0.88
:0.41
:0.41
:<0.03
:<0.03
:0.34
:o.30
:0.14
:0.16
:0.03
:<0.03
:O.OS
: 0.04
:0.15
:0.14
:<0.03
:<0.03
:0.09
:0.08
:0.25
-.0.25
:0.26
:0.27
: <0 . 03
89P
INNESOTA
00610 IN
NH3-N
TOTAL
MG/L
<0.010
0.135
0.649
0.185
0.647
0.100
0.237
0.441
<0.010
0.339
0.815
0.966
1.50
1.73
2.61
0.117
0.122
0.322
0.010
0.034
0.232
0.062
0.382
0.213
0.123
0.273
0.374
<0.010
0.182
<0.010
<0.010
<0.010
<0.010
<0.010
90P
00625 IN
TOT KJEL
N
MG/L
<0.05
0.46
0.«3
0.43
0.32
0.54
0.54
0.56
<0.05
1.05
1.12
1,«4
1.85
1.93
3.20
0.35
0.17
0.73
0.17
0.49
0.72
0.59
0.74
0.72
0.53
0.29
0.39
0.14
0.24
0.13
0.06
<0.05 •
<0.05
<0.05
91P
•»M
#M
<*M
*M
: 2S*M
: 3S*M
: 4S*M
: 6S*M
: 8S*M
• 1(1S*M
: 12S»-1
: 14S*M
: 16S»M
: l«S*^
:20S*M
S22S*-1
524S*M
:26S*M
:28S*M
:30S*M
:32S»M
:34S*^
:36S*M
:38S*M
:40S*M
: 42S*M
;44S*M
: 46S*M
:48S*M
:50S*^
:52S*M
:5*S*M
:56S*M
:S8S**
:60S*M
:62S-*M
:645^*M
: 66S*M
:58S*^
^IS*1''
: 7 2 S * "-1
**M
^ tt M
------M
-------
FPA-CRL
1975
SAMPLE
LOG NO.
4277
4278
4282
4284
4236
.4238
,4290
.4292
.4294
.4296
.4298
.4300
.4302
.4304
.4306
14308
14310
14312
14314
14316
14318
14320
14322
14324
14326
14328
14330
14332
14334
14336
14338
14340
14342
14344
14346
14347
.MN.DWO
00665 IN
PHOS-T
P-WET
MG/L
!
:<0.02
:0.08
: < 0 . 0 ?
:0.08
:0.02
:0.06
:0.03
: 0 . 0 3
:<0.02
:0.18
:0.14
:0.23
:0.26
:0.17
:0.19
:0.09
:0.28
: 0 . 2 0
:0.67
:0.05
:0.06
:0.03
:0.35
: 0 . 1 1
:0.04
:<0.02
:<0.02
:0.02
:0.02
:0.02
:0.03
:0.03
:0.04
•
•
:<0.02-
9?P
7 •»
1 REGION
00340 IN 00680 IN 71900 IN
COO T ORG C MERCURY
HI LEVEL C HGtTOTAL
MG/L MG/L UG/L
< fi . i
<3
18
8
17
10
23
13
<3
29
1 O
12
33
16
10
7
16
8
20
12
30
28
30
24
29
26
3
6
20
14
3
6
6
5
•^ v • j.
s n i
< U . 1
n l
U.I
f r, i
^ U • i
n 1
') . 1
< 0 . 1
A 1
U.I
n l
U.I
* - f\ 1
^ <0 . 1
* n i
*• U * L
*• n i
* U . i
0.1
^ l\ 1
< U • i
<0. 1
*• n i
< U . i
s t\ i
< U . 1
<0. 1
<0.1
s (\ 1
v U . 1
f C\ 1
< U . i
* r\ i
< U , i
^ n i
< U * 1
s O 1
< U . i
<0.1
<0.1
<0.1
* n 1
< U . i
-------
RLS 05APR OSN=CNCRLS.RGD.OH.DW04 ON TS0009 04/19/75 REV01 T
-STUDY DESCRIPTION)
STATTrPE SMPLDAY ATLA8BY OUEDATE ACCOUNT-NUMBER
77777777 03FEB75 05FER75 03MAY75
- OHIO
•SAMPLE DESCRIPTIONS
STATTYPE DEEP T M NO ENDDATE TIME PPLU
PAR NLOG
94 69
>>REGION
.A8IDNUM
4354
,4355
.4356
.4357
.4358
.4359
.4360
.4361
.4362
.4363
.4364
14365
14366
U367
14368
14369
14370
14371
14372
14373
14374
14375
14376
14377
14378
14379
14380
14381
14382
14383
14384
14385
14386
14387
14388
14389
14390
14391
14392
14393
14394
14395
14396
14397
14398
14399
14400
14401
14402
AGENCYID UNLOCKEY ST
77
V DRINKING WATER STU
STORETID COLLDAY TIME
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203 .
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
-------
14403
14404
14*05
14406
14407
14403
14409
14410
14*11
14*12
14413
14414
14415
14416
14417
14413
14419
14*30
14421
U422
>»1»354 >
>»1*355 >
>»14356 >
>» 1 4357 >
>»14353 >
»>14359 >
» > 1 "" "
»>1
>» 1
>»1
>»1
>»1
>»1
>»1
»>1
^ s x i
» J5 I >
4362 >
4354 >
*365 >
*366 >
*367 >
4363 >
4369 >
4370 >
/. "j T 1 -v
^ > •* i ™ j ' i "
>» 14372 >
» > 1 4373 >
» > 1 4374 >
» > 1 * 3 7 5 >
>»14376 >
>» 14377 >
»>14379 >
^
>
>
> ^ 1
»1
»1
>» i
>
>
>
>
» 1
»1
»1
»1
^
4
^
4
T g n >
331 >
332 >
383 >
^33* >
**
f+
4
365 >
336 >
337 >
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
> H\Q3 ^EAGE'
> r<2SC4 3E4G'
> NAQH 3F.4GE-
> H3P04 *£AOI
> CLEVELAND
> CLEVELAND
> CLEVELAND
NT 3LANK
^lT 3LANK
ENT 3LANK
3A»( ^ATE'-i
' A < *ATE"i
FINISHED
FINISHED
SE
-*IE3
•5IES
i 3
O\~\ } <^
Li \ i ~ . \ ^- i , ,
••• 1 1- 3 o N ^ m
«ATES SERIES 3
5c-iIE5 A
SERIES 3
•lATE^ SERIES A
*4TF_-!Sci'IE53 % G h
i^^ A __ a \ \ c iv, is 0 ^
> *A30£>j P,AH /(ATE1? SE^;E
> «A==>£'.j FLUSHED .VA'E,-}
> ,, A p = E M FINISHED « 4 r t a
^ S'iCT ' T'/C"jD^l/'M T*.. *JA^
' _ •* O 1
> EAST
> EAST
> EAST
> COL'J
> PC3"
> 3QPT
> POST
> PO-T
LIVE
LIVE
Ll'^E
MjL'i
SMOUT
SMOUT
S'JOuT
S^OUT
S 3
3E-!I
5ERI
9 = 0 OL 3AV •'ATE1' 3
30QOL FINlSr-ED *A
^=OOL FINISHED «A
-JA* ^ATE^ SERIES
rINISnED «ATE^ SE
'r> "-ii M XiTER ^
H
•-(
_
FINISr^cO
FINISHED
5A * *A TE
> =OOTS"*OUT-t ^A* '*ATE
> 3Q^T
> =0»T
> C INC
> CINC
S-^OUT
rl
SMOOTH
INNAT
INN AT
I
I
- INISnEO
FINISHED
B A tt MATE
^A*r If A TE
it a
*4
••< ?
— ! . ^ ( _
ES A
"^s A o,0,3<< fx] 'iO
ESIES 3
TE"* 3EP I ES -
TE3 SESIE3 d
A __ n n = ft \ \ ^ ^
r»IcS A
'IE3 3
3 A
O \ . J \ INJ
E .-* I E 5 d — T. c? v L T~ v \ ^0
TEP SERIES
T E R
Crt' IE
« S£-*IE
wA
1A
^ 5
S 5
TE^
TES
' H I ^
E^IE
SERIES
3 A
5 d
SERIES
SERIES
3 A
S -i
i ° !> '^ °
3
A
3
^ C\ \ "~* hj ^ ^}
^ 1- ^
uV
.'o v
>» 1 4339
INCINNATI -INI3"EO , SE
-------
>»14390
>»14391
>»14392
>»1*393
>»14394
>»14395
»>14396
>» 1*397
>»14398
»>14399
>»144£)0
>» 1 440 1
>»14402
>»14403
>»14404
>» 144 OS
>»14409
>»14410
»>14411
»> 1 *4 1 3
»>14413
» > 1 4414
4^1 7
»> 1 44.JO
CINCINNATI FINISHED wATES SERIES
°IOUA RA«j WATER SERIES A
RIQUA RAW «4TER SERIES 3
PIGUA FINISHED WATER SERIES A
=>IO'JA FINISHED WATER SERIES d
DEFIANCE RAW WATER SERIES A
DEFIANCE RAW WATER SERIES 5
DEFIANCE FINISHED WATE<* SERIES 4
DEFIANCE FINISHED wATEH SERIES 3
TOLEDO SAW WATER SERIES A
TOLEDO SAW WATER SERIES B
TOLEDO FINISHED *A"ER SERIES A
TOLEDO FINISHED WATER SERIES -3
SOILING
BOWLING
30WLING
30wLING
FREMONT
FREMONT
FREMONT
FR£MONT
H o , o
4- •
4 0 s
• 3 -
GREEN RAW *ATER SERIES 3
GREEN FINISHED WATER SERIES A
GREEN FINISHED .«4TER SERIES a
RAW *4TER SERIES A
RAW *JATER SERIES 3
FINISHED *AT£R SEJIES A
FINISHED WATER SERIES 3
HN03 REAGENT 3LANK
H2SO* REAGENT 3LANK
NAOH REAGENT BLANK
H3P04 REAGENT BLANK
OPFN
OPEN
00 f^
OPEN
OPEN
OPE'J
OP EM
-.
,
3 - o
-SAMPLE/=ARAM£TE:
-------
EpA-CRL
1975
SAMPLE
LOG NO.
14359
14361
14363
14365
14367
U369
14371
14373
14375
14377
14379
14381
14383
14385
14387
14389
14391
14393
14395
14397
14399
14401
14403
14405
14407
14409
14415
14417
.QH.DW04
S0003 OA
TPEFLAN
'•/i/HL SMPL
UG/L
<0.002
< 0,0 02
<0.002
<0.002
<0.002
< 0.0 02
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
I?
REGION
S0001 OA
HCBENZ
*HL SMPL
UG/L
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
2P
V ORINKI
39782 OA
LINDANE
WHL SMPL
UG/L
:<0.002
:<0.002
:<0.002
:<0.002
: < 0 . 0 0 2
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
:<0.002
3P
NG WATER
S0002 OA
8BHC
WHL SMPL
UG/L
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
:<0.005
: <0.005
:<0.005
:<0.005
;L
UG/L
<0.01
<0.01
<0.01
<0.01
* A
I 3bS*A
:3«S*A
: 40 S* A
!425»A
:44S*A
! 46S* A
: 4 3 S * A
:SOS*A
!52S*A
: 54S* A
:56S*A
5 62S*A
: 645* A
*•* A
**A
A
-------
F»A-CRL 39430 OA 39420 OA S0006 OA S0007 OA S0008 OA S0099 OA S0010 OA »B
1975 isooMiN HCHLR-EP CHLOROAG ODE OP ODE PP ODD OP DDT OP »e
CAMPLE WHL SMPL WHL SMPL WHL SMPL Writ SMPL WHL SM^L WHL SMPL WHL SMPL *«
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L **
U359 :
14361 :
14363 :
14365 :
14367 :
14369 :
14371 :
14373
14375 :
14377 :
14379 !
14381 :
14383 :
14385 l
14387 :
14389 i
14391 i
14393 :
14395
14397 !
14399 !
14401 :
14403 i
14405 :
14407 :
14409 :
14415 :
1 A & 1 V • X U • U ^ .J t-VV/»V«t- »'w»**ww ...-.„•-— - - „ u ~
;<0.003 :
: < 0 . 0 0 3 :
;<0.003 :
i<0.003 :
;<0.003 :
!<0.003 i
;<0.003 :
:<0.003 i
K0.003 :
;<0.003 :
K0.003 i
: < 0 . 0 0 3 i
:<0.003 J
K0.003 :
:<0.003 :
:<0.003 :
;<0.003 i
:<0.003 :
! < 0 . 0 0 3
:<0.003 i
:<0.003 :
:<0.003 :
: <0 .003 :
!<0.003 :
K0.003 :
:<0.003
:<0.003 :
:<0.003 :
:<0.002 :
i<0.002 !
i<0.002 :
K0.002 :
K0.002 !
i <0.002 i
!<0.002 !
:<0.002 :
:<0.002 :
:<0.002 !
:<0.002 :
:<0.002 i
:<0.002 :
!<0.002 !
: <0.002 i
:<0.002 i
:<0.002 :
: <0.002 :
:<0.002 ;
:<0.002 i
:<0.002 :
:<0.002 :
:<0.002 :
:<0.002 :
:<0.002 :
: <0 .002
:<0.002 :
:<0.002 :
;<0.002 :
K0.002 :
K0.002 :
K0.002 !
:<0.002 :
:<0.002 !
;<0.00? :
;<0.002
: <0.002 :
:<0.002 :
:<0.002 :
:<0.002 !
:<0.002 !
K0.002 !
:<0.002 s
! <0 .002 :
: <0.002 i
:<0.002 i
:<0.002 :
:<0.002 :
: < 0 . 0 0 2
:<0.002 ;
: <0.002 :
K0.002 :
:<0 .002 !
: <0.002 !
:<0.002 '•
K0.002 '
: < 0 . 0 0 3 :
:<0.003 !
:<0.003 :
:<0.003 !
;<0.003 :
:<0.003 :
:<0.003 :
K0.003 :
:<9.003 :
:<0.003 1
K0.003 :
!<0.003 :
;<0.003 :
K0.003 :
!<0.003 :
!<0.003 !
K0.003 :
K0.003 l
:<0.003
K0.003 :
: < 0 . 0 0 3
K0.003 :
K0.003 i
:<0.003 :
:<0.003 J
:<0.003 :
:<0.003 i
K0.003 :
: < 0 , 0 0 3 :
K0.003 :
;<0.003 :
K0.003 :
K0.003 :
K0.003 i
K0.003 !
:<0.003 :
:<0.003 i
: < 0 . 0 0 3 l
K0.003 i
:<0.003 :
i < 0 . 0 0 3 !
K0.003 :
:<0.003 i
!<0.003 i
:<0.003 :
:<0.003 :
;<0.003 :
:<0.003 J
: <0 .003 i
: <0.003 '
:<0.003 :
:<0.003 :
:<0.003 i
:<0.003 i
K0.003 :
:<0 ,003- :
: < 0 . 0 0 3 :
:<0.003 :
:<0.003 :
K0.003 :
:<0.003 !
K0.003 !
:<0.003 :
: < 0 . 0 0 3
K0.003 !
:<0.003 i
:<0.003 :
:<0.003 :
:<0.003 :
:<0.003 :
;<0.003 i
:<0.003 :
:<0.003 :
:<0.003 i
:<0.003 !
:<0.003 :
:<0.003 J
:<0.003 i
:<0.003 i
:<0.003 i
:<0.003 !
:<0.003 :
:<0.003 :
:
-------
FPA-CRL
1975
SAMPLE
LOG NO.
.4359
.4361
.4363
.4365
,4367
14369
14371
14373
14375
14377
14379
14381
14383
14385
14387
14389
14391
14392
143Q3
14395
14397
14399
14401
14403
144-07
14409
14415
14417
.OH.DW04
soon OA
ODD PP
»JHL SMPL
UG/L
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
: < 0 . 0 0 3
:<0.003
: < 0 . 0 0 3
:<0.003
:<0.003
:<0.003
: < 0 . 0 0 3
: < 0 . 0 0 3
:<0.003
•
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
: < 0 . 0 0 3
:<0.003
:<0.003
15P
REGION
S0012 OA
DOT PP
WHL SMPL
UG/L
:<0.003
:<0.003
:<0.003
:<0.003
: <0.003
:<0.003
to.oio
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
•
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
:<0.003
16P
S0013 OA S0014 OA 394RO OA
CARBPHTH MIRE* MTHXYCL*
WHL SMPL WHL SMPL WHL SMPL
UG/L UG/L UG/L
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 ; < 0 . 0 1
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.01
:<0.003 :<0,005 :<0.01
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.01
, •
* • *
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.0l
•:<0.003 :<0.005 :<0.01
:<0.003 :< 0.005 :<0.01
: <0.003 :<0.005 : <0.01
:<0.003 : <0 .005 : <0.0l
: <0.003 :<0 .005 : <0 .01
:<0.003 :<0.005 :<0.01
:<0.003 :<0.005 :<0.01
:<0.00'3 :<0.005 :<0.01
17P 18P 19P
V DRINKING WATER STUDY - OHIO
S0020 OA S0021 OA *C
2»4-D:IP DN-P *C
WHL SMPL WHL SMPL *C
UG/L UG/L *C
:<.01 :<1 : 6S*C
• <• m • <1 : fl^*C
• < » u l • *• i • --> _ i_
..n, .1 • 1 n c &r
:<,01 • 1 • i " -.1 ~
:<.01 :<1 :12S»C
• f n 1 • < 1 : 14S-*C
• < • U 1. • ** L • i -• i •-
. ,. A i . s-i :16C *c
. < » u i ' *• i • 1 1 » ^/ ^
:<.01 :<1 :18S*C
• < m : <1 :20S*C
• %. • U 1 • ^ i •*_>«- —
• <• m : *•> \+
:<.01 :<1 :32S»C
•< 01 :*C
• V.Ui »Vi «_/w_w
• f n i • < 1 5 54S*C
• V.Ul »^i »™/w-^
•< oi :<1 :56S*C
• V » V/ A • ^ * ^e -*~ -~- ^*
:<.01 '
-------
EPA-CRL 39770 OA S0023 OA 39380 OA 39390 OA 39460 OA S0027 OA S0028 OA *D
1975 DCPA EMDOS I DIELDRlN ENDRIN CLR^NZLT ENDOS II NITROFEN »0
SAMPLE WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMP|_ ,VhL SMPL */HL SMPL *0
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *0
14359
14361
14363
14365
14367
14369
U371
14373
14375~
14377
U379
14381
14383
14385
14387
14389
14391
14392
14393
14395
14397
14399
14401
14403
14405
14407
14409
14415
14417
<.OQ3
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.0"03
<.003
<,005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.OOS
<.005
<.005
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
.003
<.003
.004
<.003
<.003
<.003
<.003
<.003
<.003
.000
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.C03
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.Q03
<.003
<.003
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.oi
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.0i
<.01
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<,005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005 : 6S»D
<.005 - : PS*D
<,005 : 10S»D
<.005 :12S*0
<.005 :i4S*n
<,005 :16S*0
<.005 :18S*D
<,005 :20S«D
<.005 :22S*D
<.005 :24S*D
<.005 :26S*0
<.005 :28S*D
<,005 : 30 5*0
<,005 :32S*0
<.005 :34S*D
<.005 : 365*0
<.005 :3aS»D
<,005 :395*D
<.005 :40S*D
<.005 :42S*0"
<.005 :445*0
<.005 :46S*D
<.005 :43S*0
<.005 :50S*D
<.005 :52S*D
<.005 :5H.S*0
<.005 :56S*n
<.005 :625*D
<,005 :6^.3*0
22P 23P 24P 25P 26P 27P 23P **0
.OH. 0^04 REGION V DRINKING WATER STUDY - OHIO **n
-------
FPA-CRL
1975
SAMPLE
LOG NO.
.4359
.4361
.4363
.4365
.4367
14369
14371
14373
14375
14377
14379
14381
14383
14385
14387
14389
14391
14392
U393
14395
14397
14399
14401
14403
14405
14407
144-09
14415
14417
S002V OA S0030 OA S0031 OA S0026 OA 39808 OA 3V570 OA S0016 OA *E
?4S T-TO PROLAN BULAN OEHP TEOION OIAZINON DYFONATE *E
WH! SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMPL *E
UG/L UG/L UG/L UG/L UG/L UG/L UG/L »t
-. . ^ n i • ^ i • < D 1 K 1 K 1 • o b w r.
:<*01 !<*S! i'Sl '? K 01 :01 'l7, :< ni <1 -<1 :3fl«5*F
:<.01 :<.0l K.01 :<1 :<-01 -<1 ;<1 '^ *_
!<'01 !<-nJ !<'S '< : ' :<1 <1 !^s4
:<-01 :<>°n ^JJ :< '-<'2l <1 :<1 ««S»E
:<<01 !<*01 n J '<*ni <1 :<1 :4*S»E
:<.01 K.01 K.01 :<1 .<.01 • ] !<1 I < 1 • O c 3 w t
K.01 K.01 K.01 .i «<.tj • i j- :64S*P
K.01 K.01 K.01 :2 K.01 Kl i<1,CD L:
29P 30P 31P 32P 33P 34P 35P «•=.
-------
EPA-CRL S0017 OA 50032 OA 39600 OA 39530 OA 39540 UA S0033 OA 39398 OA *F
1975 RONNEL OURSSAN MPARATHN MALATHN PARATHN DEF ETHIOM *F
SAMPLE WHL SMPL WHL SMPL WHL SMPL WHL SMPL WHL SMHL WHL SMPL WHL SHPL *F
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *F
14359
14361
14363
14365
14367
14369
14371
14373
14375
14377
14379
14381
14383
14385
14387
14389
14391
14393
14395
14397
14399
14401
14403
14405
14407
14409
14415
144-17
-------
cPA-CRL S0018 OA S0034 OA 39580 OA S0035 OA S0036 OA S0037 OA 39486 OA *G
1975 PHENCAPT EPN GUTHION PHOSALON AZINFOSh COUMAFOS AROCLUR *G
SAMPLE WHL SMPL 'VHL SMPL WHL SMPL WHL SMPL WHL SM^L WHL SMPL 1221 *G
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *G
U359
U361
14363
14365
U367
14369
14371
14373
14375
14377
U379
14381
14383
14385
14387
14389
14391
14393
14395
14397
14399
14401
14403
14405
14407
14409
14415
14417
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<0.3 ! 6S*G
<0.3 : 8S»G
<0.3 :10?<*G
<0.3 :12S*G
<0.3 :14S*G
<0.3 :16S*G
<0.3 :13S*G
<0.3 :20S*G
<0.3 :22S*G
<0.3 :24S*G
<0.3 :26S*G
<0.3 !285*G
<0.3 :30S»G
<0.3 :32S*G
<0.3 :34S*G
<0.3 :36S*G
<0.3 :38S*G
<0.3 :40S*G
<0.3 :42S*»G
<0.3 :44S*G
<0.3 :46S»G
<0.3 :48S*G
<0.3 :50S*G
<0.3 :52S*G
<0.3 :54S*G
<0.3 :56S*G
<0,3 :62^*G
<0.3 :64S*G
43P 44P 45P 46P 47P 48P 49P **G
.OH.DW04 REGION V DRINKING WATER STUDY - OHIO **G
-------
FPA-CRL
1975
SAMPLE
LOG NO.
14359
14360
14361
14362
14363
14364
14365
14366
14367
14368
14369
14370
14371
14372
14373
14374
14375
14376
14377
14378
14379
143RO
14381
14382
14383
14384
14385
14386
14387
14388
14389
14390
14391
14392
14393
14394
14395
14396
14397
14398
14399
14400
14401
14402
14403
14404
144Q5
14406
14407
14408
14409
14410
14415
14416
14417
14418
39496 OA
AROCLOR
1242
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
50P
39500 OA
AROCLOR
1248
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3 .
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
51P
39504 OA
AROCLOR
1254
UG/L
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
52P
39503 OA
AROCLOR
1260
UG/L
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.4
<0 .4
<0.4
<0.4
<0 .4
<0.4
<0 .4
<0.4
<0.4
<0 .4
<0.4
<0 .4
<0.4
<0 .4
<0.4
<0.4
<0.4
<0.4
53P
S0047 OA
METHE CL
TOT VOL
UG/L
<0 .5
<1
<0 .5
<1
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
2
3
<0.5
3
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0 ,5
<0 .5
< 0 . ->
<1
54P
S0039 OA
CCL4
TOT VOL
UG/L
2
4
<2
15
<0.5
11
7
6
<1
<1
2
1
2
1
1
<0.5
<0.5
<1
0.7
1
<0.5
<0.5
<0.5
<0.5
1
3
<2
3
55P
S0033 OA *H
CHCL3 *H
TOT VOLA *H
UG/L *H
* A. C -i> i-l
• O o n
* i • 7 O ii LJ
< 1 I 7 b*H
• O CT 4 LJ
• H ;S-»M
1-^ • Q c: J4 .j
2 • SJ b WH
: IOS*H
<1 : 1 1 S-^H
• \ O C A l—i
J 1 c5*r
3* 1 ^ C A LJ
: 1 3SOM
• i /, r~ j^ . i
• 1 4 ."> 9 n
< 1 : 15S*H
• 1 £- C 41 i_i
• 1 6S*H
138 :17S*H
: 18S*H
<2 :19S*H
:20S*H
s : 21 ^*H
« o "3 C i> LJ
• cc s9 H
<1 :23S»H
:24S*H
51 :25S*H
!26S*H
2 J27S*H
• 28 S'&u
29 :29S<*H
• ' J A f ii i_ '
! J 0 S*H
6 131 S^H
• ~5 ""} C" f i J
! 32S*1-1
21 :33S*H
' 34 S*H
4 !35S*H
! 36S*H
127 :37S*H
5 3 8 S*H
:39S»H
: 4.0 S^M
102 :4l?»H
:42S*H
? : 43S*'1-'
: 4 4 S * H
14 !45S»H
• / C-. C" A l_l
5^65 ^H
<1 !47S*H
! 48S*H
62 :49S*H
! 50 S^H
<1 :51S*H
: 52S*H
160 :5?^<»M
I 545*^
< 1 I 5 5 5 * w
: 56^-* i-1
366 :57^<>-<
: 62?*H
<1 :63S*H
: 64S*H
60 JSSS-^M
5^p *OH
-------
F°A-CRL S0056 OA S0040 OA S0041 OA S0042 OA *J
~1975
SAMPLE
LOG NO.
14360
14362
14364
14366
14368
14370
14372
14374
14376
14378
14380
14382
14384
14386
14388
14390
14392
14394
14396
14398
14*00
14402
14404
14406
14408
14410
14416
14418
.QH.DW04
C2H4CL2 CHCL28R
TOT VOL TOT VOL
UG/L UG/L
:<0.5 :<0,5
:<1 :6
: < 1 : < 1
: < 1 : 4
:<1 :<0.2
t-
>t T
TOT VOL r
A T
UG/L l
- • V C» T
: <0.5
t
-------
RPA-CRL
1975
SAMPLE
LOG NO.
14354
14360
14362
14364
14366
U368
14370
14372
14374
14376
14378
14380
14382
14384
14386
14388
14390
14392
14394
14396
14398
14400
14402
14404
14406
14408
14410
14411
14416
14418
.OH.D//04
00916 MW
CALCIUM
CA«TOT
MG/L
: < 1
:31.5
:32.4
:32.1
:31.6
: 2 0 . 8
:33.5
:31.6
:43.4
:40.4
:45.6
:22.3
:27.7
:21.8
:27.4
:24.3
:33.1
:44.9
:29.0
:79.4
:64.8
:43.2
: 17.4
:62.7
:34.o
:45.7
:52.9
: <1
: 4 9 . 4
141.2
64P
REGION
00927 MW
MGNSIUM
MG»TOT
MG/L
: <0 . 1 :
: 6 . 5 :
:7.6 :
:7.5 :
:7.5 :
:6.0 :
:5.9 :
:8.2 :
:7.9 :
:14.5 :
: 0 . 9 :
• n * o •
:6.4 :
:5.7 :
:6.3 :
: 7 . 4 :
:7.4 :
:19.0 :
: 1 1 . 5
:21 . 1 :
:7.7 :
: 10.8 :
:5.8 :
:15.9 :
: 7 . 9
:12.8 :
:3.5 :
: <0 . 1 :
:12.2 :
:12.4 :
65P
V DRINKING
00929 MW 00937 MW 01034 Mw 01042 MW
SODIUM PTSSIUM CHROMIUM COPPER
N4.TOT K,TOT CR»TOT CU»TOT
MG/L MG/L UG/L UG/L
<0 . 1
7.7
8.1
6.9
8.1
11.0
12.8
18.1
19.8
6.0
8.5
8.9
9.7
9.5
9.5
8.9
10.3
7.0
17.1
17.1
17.6
11.1
19.9
11.3
47.5
8.8
45.0
<0 , 1
77
91
<0 . 1 : <5
1.2 :<5
1.2 :<5
1.1 :<5
1.2 :<5
3.0 : <5
2.6 :<5
2.2 :<5
2.1 :<5
2.9 :-7
3.1 :<5
1.8 : 11
1.9 :<5
1.8 :<5
1.9 :<5
1.7 :<5
1.7 :<5
2.7 :<5
2.6 : <5
2.8 :7
2.8 : <5
2.0 :<5
1.7 :<5
2.8 ;<5
2.6 :<5
3.0 :<5
2.7 :<5
<0 . 1 '• <5
2.8 :<5
3.1 :<5
<5 :
<5 :
<5 :
9 :
<5 :
8 :
<5 :
10 :
<5 :
<5 5
<5 :
39 :
<5 :
47 :
6 :
48
5 :
<5 :
<5 :
<5
<5
16
<5 :
13 :
<5 :
<5 :
<5 :
<5 :
7 :
<5 :
66P 67P 68P 69°
WATER STUDY - OHIO
01045 MW *J
IRON *J
FF»TOT *J
UG/L *J
<20
76
<2D
74
<20
120
<20
2340
<2o
1900
<20
3110
<20
3190
<20
1540
30
620
26
420
<20
760
<20
1370
590
1310
<20
<20
1070
130
1S»J
7S*J
9S<*J
11S»J
13S*J
15S*J
1 7S*J
19S*J
2 1S*J
23S*J
25S*J
27S*J
29S*J
315*J
33S*J
35S*J
37S»J
39S*J
41S*J
43S*J
45S*J
47S*J
49S*J
51S*J
53S*J
55S*J
57S*J
58S*J
63S* J
65S*J
7 OP **J
,1
-------
EPA-CRL
1975
SAMPLE
LOG NO.
14354
14360
14362
14364
14366
14368
14370
14372
14374
14376
14378
14380
14382
14384
14386
14388
14390
14392
14394
14396
14398
14400
14402
14404
I44Q6
14408
14410
14411
14416
14418
.OH.DW04
01055 MX 01092 MW 01002 MW 01051 M* 01027 MW 01077 MW
MANGNESE ZINC ARSENIC LEAD CADMIUM SILVER
MN.TOT ZN»TOT *S»TOT PB.TOT CD«TOT AG.TOT
UO/L UG/L UG/L UG/L UG/L UG/L
:<5
: 6
:<5
: 9
:7
:28
:<5
:470
:13
:52
:<5
:460
:<5
:47T
:<5
:250
:<5
:46
:<5
:29
:5
:19
:6
:55
' H
:110
:<5
: <5
:130
:32
<5
<5
<5
<5
<5
18
<5
63
<5
35
<5
72
<5
66
<5
46
<5
7
51
19
<5
<5
<5
14
<5
52
<5
<5
19
<5
<1 :<2
<1 :<2
<1 :<2
<1 :<2
<1 :<2
<1 :<2
<1 :<2
3 :25
<1 :<2
10 :T
3 :<2
4 :30
<1 :<2
7 :30
<1 :<2
3 : 12
<1 . :<2
3 :3
<1 :<2
1 :4
<1 :<2
3 :6
<1 :<2
5 :8
<1 :<2
5 :13
1 :<2
<1 :<2
<1 :il
<1 - :3
<0.2
<0.2
<0.2
<0.2
-------
EPA>-CRL
1975
SAMPLE
LOG NO.
14360
14362
14364
14366
14368
14370
14372
14374
14376
14378
14380
14382
14384
14386
14388
14390
14392
14394
14396
14398
14400
14402
14404
14406
14^03
14410
14416
14418
.QH.DW04
00530 I
RESIDUE
TOT NFL
MG/L
:3
:<2
:3
:<2
:3
:<2
:17
:<2
:203
:8
:165
:<2
:165
:2
:79
:<2
:68
:<2
:23
:<2
:53
:<2
:127
:5
:33
:<2
:34
:<2
78°
REG-ION
M 70300 I
RESIDUE
M 00095 IM
CNDUCTVY
T DISS-180 AT 25C
C MG/L
: 160
: 190
: 170
: 150
:170
:230
:200
:230
:265
:280
: 120
:170
: 145
: 140
: 150
:190
:290
:230
:440
:350
:270
:180
:380
:340
:240
:290
:390
:480
79P
V DSINKI
MICROMHO
:282
:278
:270
:277
:254
:308
:350
:397
:391
:364
:236
:266
:233
:265
:249
:307
:4M
:374
:642
:506
:376
:257
:510
:488
:392
:520
:780
:845
30P
00945 IM
5ULFATE
SO*
MG/L
:20
:26
:20
:27
:31
:56
:82
:fl9
:53
:80
:49
J54
:53
:55
:55 ,
:69
:42
:43
: 103
:113
:41
:39
:79
:109
:54
:81
:70
:82
81P
MG HATER STUDY - OH
00940 IM
CHLORIDE
CL
MG/L
:19
:18
:16
:19
:20
:25
:29
:33
U8
:21
:12
:13
:13
:15
:13
:21
: 19
:25
:32
:36
:25
:24
:26
:31
:24
:39
:142
:179
82°
10
00956 IM
SILICA
SI02
MG/L •
:<0.2
: < 0 . 2
: <0.2
:<0.2
:<0.2
:0.6
:6.3
:5.4
:6.4
:6.3
:6.2
!6.4
:6.4
:6,6
:6.6
:6.0
:6.6
:6.9
:8.1
:6.9
:3.2
:2.6
:7.o
:5.5
:6.6
:5.8
:6.4
:6.6
93P
OOMO
T ALK
CAC03
MG/L
:85
!78
:86
:76
:45
:47
:30
:50
:95
:42
:29
'.35
:29
:36
:38
!40
: 141
:85
: 171
:61
:97
:31
:122
:49
:78
: 100
:79
:42
84P
IM *L
*L
*L
•*L
: 7S*L
: 9S*L
: 11S*L
:13S^L
: 15S*L
:17S*L
: 19S*L
:21S*L
:23S*L
.•85S^L
:27S*L
:29S*L
:31S«L
:33S*L
:35S*L
:37S*L
:39S*L
:4is*L
:43S<*L
:45S*L
:47S<»L
:49S*L
:51S»L
:53S*L
:55S*L
:57S*L
:63S^L
:65S*L
»•»(_
**L
-------
EPA-CRL
1975
SAMPLE
LOG NO.
14355
14356
14357
U360
14362
14364
14366
14368
14370
14372
14374
14376
14378
14380
14382
14384
14386
14388
14390
14392
14394
14396
14398
14400
144Q2
144Q4
14406
14408
14410
14412
14413
14414
14416
14418
.OH.DW04
00403
LAB
PH
su
:
•
•
•
:7.8
:7.7
:7.8
:7.7
:7.4
:7.7
:7.2
:9.4
:7.7
:9.7
:7.0
58.4
:7.0
:8.3
:7.2
58.2
:7.7
:7.9
:7.8
:8.5
:7.8
:8.9
:7.7
:8.5
:7.7
:9.o
;
*
*
:7.8
:9.0
85^
IM 00951 IM
FLUORIDE
F, TOTAL
MG/L
* *
! ;
• •
50.13 :
: 0 . 1 3 :
:0.16 :
: 0 . 1 3 :
: 0 . 1 3 :
:l.O :
:o.l8 :
: 1.3 :
:0.21 :
:0.98 :
:0.13 :
:0.96
50.13 :
:o.96 :
:0.13 :
:0.13 :
:0.20 -:
:0.19 :
:0.26
:0.74 :
:0.18 :
:i.l :
:0.22 :
: 1 . 0
: n . 2 1 :
50.96 :
• »
• •
• •
• *
• *
• •
:o,18 :
:0.74 :
86P
REGION v DRINKING
32730
IM 00720 1!^
1 00630 IN
PHENOLS CYANIDE NO?*,NOJ
UG/L
<3
<3
<3
<3
<3
4
3
6
<3
6
5
<3'
<3
<3
<3
<3
<3
4
<3
3
<3
3
<3
5
<3
6
<3
<3
5
3
87P
WATER
CN
MG/L
*
*
: < 0 . 0 0 2
•
: 0.004
: 0.005
:0.003
:0.003
:0.005
:
-------
EPA-CRL 00665 IN 00340 IN 00680 IN 71900 IN 00900 IN 00615 IN *N
1975 PHOS-T COD T ORG C MERCURY TOT HAHQ N02-N *N
SAMPLE P-*ET HI LEVEL C HG.TOTAL CAC03 TOTAL *N
LOG NO. MG/L MG/L .MG/L UG/L MG/L MG/L *N
14354
14355
14360
14362
U364
14366
14368
14370
14372
14374
14376
14378
14380
14382
14384
14386
14388
14390.
14392
14394
14396
14398
14400
14402
14404
14406
14408
14410
14411 '
14412
14416
14418
0.31
0.03
0.02
0.04
<0.02
0.04
<0.02
0.15
0.19
0.39
0.07
0.20
<0.02
0.21
<0.02
0,14
<0.02
0.17
0.23
0.29
0.26
0.26
0.19
0.36
0.10
0.35
0.14
<0.02
0.33
0.65
5
.8
15
:7
5
.20
10
18
7
44
12
26
4
29
£•
18
3
25
7
22
7
19
8
33
6
43
7
<3
24
9
<0.1
<0.1
<0.1
<0.1
<0.1
<0 . 1
<0.1
<0.1
<0.1
0.1
0.2
0.2
0.4
0.2
0.3
0.2
0.3
0.1
<0. 1
0.1
0.3
0.1
0.3
0.2
0.2
-------
COLS 05APR
NLOG
34 53
>»PEGION
LA9IDNUM S
14801
14802
14?03
14804
14905
14306
148Q7
14808
14809
14810
14811
14812
14813
14314
U815
14816
14817
14818
14819
14820
14821
14822
14323
14324
14925
14826
U827
14828
14829
14930
14831
14832
14833
14834
14835
14836
14837
14838
14339
1^840
14341
14842
14843
14344
14845
14846
14847
14343
14349
DSN=CNCRLS.RGD.WS.DWOI UN rsooo9 04/19/75
STUDY DESCRIPTION
AGENCYID UNLOCKEY STATTYPE SMPLDAY ATLA3RY DUEDATE ACCOUNT-NUMBER
77777777 03FEB75 05FE875 03MAY75
V DRINKING WATER STUDY - WISCONSIN
SAMPLE DESCRIPTIONS
TORETID COLLDAY TIME STATTYPE DEEP T M NO ENDDATE TIME
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750P03
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
750203
-------
14350
U851
U352
14953
» > 1 480 1 >
>» 1 4302 >
>* > 1 480 3 >
>»1 43Q4 >
> » 1 4 3 0 5 >
» > 1 4 8 0 6 >
»» 1 480 7 >
>» 14?08 >
> -* •> i
>
>
>
>
>
»1 491 2 >
» 1*61 3 >
»
•»
1 4=? 1 4 >
14315 >
750203 N^vJ }
7502-13
750203
> HN03 R£AGE
> H2S04 J£AG
> NAOH - M3P04 R£AO
> QPC-VI
> EAU CLAIRE
> EAU CLAIRE
> EAU CLAIRE
> EAU CLAIRE
> SLACK RIVE
NT 3LAN<
34iV >ATE
OAX BLACK RIVER
> 3LACK RIVER
> 3LACK RIVER
> 3Li
> 3Li
C-C RIVE
C'< RIVE
R
3
>»14316 » 3LACK RIV£2
>
>
>
y
>
» 1 4 8 1 7 >
> >
> >
»»
»
1 •* "* 1 J "
14^19 >
14?20 >
itfll? >
14S23 >
> 3LA
> LA
> LA
> LA
> MIL
CK RIVE
CROSSE
CROSSE
CROSSE
VALXEE
P
BA
FI
FI
3i
3A
R SERIES A
R SERIES d
^ATER 5£Rl
WATER S£r< I
AW «ATFS >.-
-
£5 A
ES ->
3 r FS *
FALLS RA/( ^ATER SERIES 3
FALLS FINISHED «A7£3 SERIES A
FALLS FINISHED «AT£R SERIES S
FALLS R
FALLS R
FALLS f
FALLS f
* VATER
NIS-EO
MISHEO
* ^ATF"
3 C O rO j>/ KJ
- 4M-.5TC rv> cl ! .30 \-/NJ
v^ ^V\ NJ *\0'S" ) I
A* //ATER ScRIES i
AW
I.NI
^AT
SH£
FR SE
1 -AT
INISHED ,^AT
SERIE
« AT
*AT
SE
ER
£R
S 3
RIES 3
ER SERIES A
Efi SERIES 3
M3 M TA) ^-'3H
i i> . | U
SERIES A
SERIE
3 3
H T 0 o KJ ^ ^ ' S
RIES 3
> » 1 4 -( 2 4 » MILWAUKEE ~INI3-*£") d A 7 E 3
>
>
>
>
>
>
>
>
>
>
>
>
>
>
>
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>
>
>
>
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> ,,
> >
> >
^ >
> >
»
> >
> >
•> >
> >
>*
> *
»
»
»
»
»
> >
> >
^ >
»
1*825 >
1 »82"i >
14^27 >
1 4->29 >
1 ** ^ 3 0 >
14331 >
1*332 >
1*333 >
1 4^34 >
1 *335 >
1*^36 >
i *837 >
14=?33 >
I4S39 >
1 4 J » 0 >
1*8*1 >
145^2 >
14.-43 >
14344 >
14^45 >
1 i Q ^ J5 >
1*^47 >
> MIL
w A u K E E
«• n c H Si
F I
,
> OS^KOS-* RA^
> OSH MANIT"0*OC
N I
M S H £ 0
^ A 7 c R i
^AT
-R '
~ *
£ R I
r - -,
SnEO •/ATE3
> M4MITO*OC °A* /^ATFR
> ^AN
> JAN
> ••-(•,
> 1 '" 0
> T«0
> T <<0
> ORE
> 3RE
> 3«E
> Rr
> pr
> Hf
> RE
> A^
> "AR
I TO*CC
ITO*OC
K T V P" •? ^
=>ivER>
RIVERS
R I v E R 3
F N 3 A Y
•N dAY
EN 3AY
EN BAY
EN 3 A v
EN RAY
E'N dAY
EN 3 A Y
f N ?" T 7 -"
iNETTE
F r
~ I
^
P
r
F I
3A
RA
- I
r r
NI SHED
NISHEO
A* VA TE
Ad *ATE
i N i SHED
N I 3 " £ 0
,, A
~ '
FI
SA
* -»ATFR
N SHfO
'' S '-• E 0
# ^ A T "" ^
n ,1 A T £ R
>»14A
>>
> >
14340 >
1*350 >
> '.(A3
> ^ £ Vi
INET7E
0 Srt A R A
FI
w
>»l-i?51 » ,«£f.jOSrt.» RAx
•>
»
14352 >
> rfE'.'
OSnA FI
N:
N SHEO
^ T ~ •? 5
«AT£3 S
3 H E 'T >( A
-> u
3£
"A T
1 A T
.R 5
R S
,VA
* A T
3F
SE
•«A T
IF
"1 i
S 3
SERIE
S-ERIE
A
a
= I£5
S A
3 ?
S A
S a
S A
S 9
A
V f n -*
V_\ ^A . O 1 t\» ^ 'o . O
M^. 0^( M i^
\ d" ~1 'X
M- M- , 1 0 M j ' • i
'Mr '~t- * "D -i i\J ^ "£ • o (^
. _ ^ ry J X 1 . 3 '
^1 J , w^ ^^ ^J v
JL 3.v"b^ M '^-
-------
>>14853 » KENOSHA FINISHED WATER SERIES 8
SAMPLE/PARAMETEH DATA-
-------
-DA-CRL sooo'5 OA
1975 TREFLAN
SAMPLE wHL SMPL
LOG NO. UG/L
4806
4808
4810
4812
4814
4816
4822
4824
4826
4828
4830
4832
4834
4836
4839
4840
4842
48*4
4846
4848
4850
,4852
< o.o 02 :
<0.002 :
< 0 . 0 0 2 :
< 0.0 02
<0.002 :
<0.002 :
<0.002 :
<0.002 :
<0.002 :
<0.002 :
<0.002 :
<0.002 :
<0.002 :
<0.002 :
<0.002 :
<0.002 :
<0.002 :
<0.002
< 0 . 0 0 2 :
<0.002 :
<0.002 :
<0.002 :
I*3
•ws.owoi REGION v
S0001 OA 39782 OA S0002 OA
HCBENZ LINDANE BBHC
WHL SMPL WHL SMPL WHL SMPL
UG/L UG/L UG/L
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0,002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
<0.005
< 0 . 0 0 5
<0,005
2P ' 3P 4P
DRINKING WATER STUDY - Wl
sooo4 OA
DICLOME
IVHL SMPL
UG/L
: < 0 . 0 1
: <0 . 0 1
: <0 . 0 1
: <0.01
' <0 .0 1
: < 0 . 0 1
I <0 , 0 1
: <0 . 0 1
: <0 . 0 1
:<0.01
: <0 , o l
: <0.01
:<0.01
; <0 • 0 1
: <0 , 0 1
: <0 . 0 1
; < o . 0 1
J < 0 • 0 1
: <0 . 01
:<0.01
: <0 . 0 1
: <0 . 0 1
5P
SCONSIN
39330 OA
ALDRIN
WHL SMPL
UG/L
:<0.002 :
:<0.002 :
: <0.002 :
:<0.002 :
:<0.002 :
: <0.002 :
:<0.002
:<0.002 :
:<0.002 :
: < 0 . 0 0 2 :
:<0.002 :
:<0.002 :
:<0.002 :
:<0.002 :
:<0.002 :
:<0.002 :
:<0.002 :
:<0.002 :
:<0.002
:<0.002 :
:<0.002
:<0.002 :
fiP
S0005 OA
ZVTRON
WHL SMPL
UG/L
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0,02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
<0.02 :
7P
*A
*A
*A
«A
6S*A
8S**A
1 OS<*A
12S*A
14S*A
16S*A
22S-*A
24S*A
2 ^> ^* "^ A
p O C ^ A
30S^A
32S*A
34S*A
36S*A
39S*A
40S*A
42S'*A
445*A
46S*A
43S*A
C Q Q & A
^ 2 ^ ""* ^
** A
-------
EPA-CRL 39430 OA 39420 OA S0006 OA S0007 OA S0008 OA S0009 OA S0010 OA *B
1975 ISOD^IN HCHLW-EP CHLOROAG ODE OP DOE PP ODD OP DDT OP <*B
SAMPLE *HL SMPL WHL SMPL KHL SMPL WHL SMPL WHL SMPL ^ML SMPL VHL SMPL *»
LOG NO. UG/L UG/L U3/L UG/L UG/L UG/L UG/L *B
4806
4808
.4810
.4812
.4814
.4816
.4822
.4824
.4826
.4828
.4830
.4832
.4834
.4836
4839
.4P40
.4842
.4844
.4846
.4848
.4850
.4852
< 0 . 0 0 3
<0.003
<0.003
<0.003
<0.003
<0,003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
< 0.0 03
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.00?
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.002
<0.003
<0 .003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0,003
<0.003
<0,003
<0.003
<0.003
<0.003
<0.003
<0.003
<0,003
<0.003 '
<0.003
<0,003
<0.003
<0 . 003
<0.003
<0 .003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003 : 6S»a
<0.003 : SS<*R
<0.003 :10S*?
<0.003 :12S*B
<0.003 :14S»B
<0.003 :i6S-*3
<0.003 :22S*P
<0.003 :24S*B
<0.003 :26S*q
<0.003 :28S*^
<0.003 :30S*^
<0.003 :32S*
<0.003 :34S*R
<0.003 :36S*3
<0.003 :39S*B
<0.003 :40S*8
<0.003 :42S*R
<0.003 :44S*«
<0.003 :46S<*>3
<0.003 :48S*i?
<0.003 :50S*«.
<0.003 :5?S*R
3? 9P 10P IIP 12P 13P 14P **9
.HS.OWOl REGION V DRINKING WATER STUDY - WISCONSIN *•**
-------
-PA-CRL S0011 OA S0012 OA S0013 OA S0014 OA 39480 OA S0020 OA S0021 OA **C
1975 ODD PP DDT PP CAR8PHTH MIREX MTMXYCLH P, 4-0: IP DN'RP <*C
SAMPLE dHL SMPL WHL SMPL WHL SMPL wHL SMPL WHL SMPL WHL SMPL dHL SMPL *C
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L U3/L *C
4806
4808
4810
4.1U2
4814
4816
4822
4824
4826
4828
4830
4832
4834
4836
4839
4840
4842
4844
4846
4848
4850
4852
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
00 . 0 0 3
<0.003
<0.003
<0.003
<0.003
<0.003
< 0 . 0 0 3
<0.003
<0.003
< 0 . 0 0 3
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
<0.003
«>
< 1 : 14S*C
< 1 : 1 ft s •* c
<1 :22S-t*C
<1 :24S*C
<1 :26S*C
<1 :23S*C
<1 :30S*C
<1 :32S*C
<1 :34S*C
<1 :36S*C
<1 :39S*C
<1 :40S*C
<1 :42S*C
< 1 : 4 4 s * C
<1 :46S»c
<1 !48S*C
< 1 : 50S*C
<1 :52S*C
15^ 16P 17P 18P 19P 20P 21P **C
WS.OW01 REGION V DRINKING WATER STUDY - WISCONSIN **C
-------
:PA-CRL 39770 OA S0023 OA 39380 OA 39390 OA 39460 OA 50027 OA S0028 OA *D
1975 OCPA ENDOS I DIELDRIN ENDRIN CLR9NZLT ENDOS II NITROFEN *0
SAMPLE WHL SMPL WHL SMPL dHL SMPL WHL SMPL WHL SMPL WHL SMPL WML SMPL *0
.06 NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *D
h806
^08
^810
^812
>314
^816
^822
f824
^326
^828
^830
^832
v834
^836
^839
..840
^842
k844
^846
(.848
^850
t852
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
< .003
<.003
<.003
<.003
<.003
<.005
<.005
<.005
<,005
<,005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.003
<,003
<,003
<.003
<.003
<.003
<.003
<.003
<,003
<.003
<,003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
< . 0 0 3
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.003
<.01
<.oi
<.oi
<.01
<.oi
<.oi
<.oi
<.oi
<.01
<.oi
<.oi
<.oi
<.01
<.oi
<.oi
<.01
<.01
<.01
<.01
<.01
<.oi
<.01
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.OOS
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005
<.005 : 6S*Q
<.005 : 85*0
<.005 :10S<*9
<.005 '.125*1
<.005 :14S^Q
<.005 :16S*D
<.005 !22S*D
<.005 :24S*0
<.005 ^SS^D
<.005 :?«S*0
<,005 :30S*0
<.005 :32S-»0
<.005 :34S-*0
<.005 :36S*n
<.005 :39S»D
<.005 :*OS*0
<.005 :42S*0
<.005 :44S*Q
<.005 :46S*0
<.005 ;4SS<*0
<.G05 :50S*0
<.005 :52S*D
22P 23P 24P 25P 26P 27P 28P **n
/^S.OWOl REGION V DRINKING WATER STUDY - WISCONSIN ' **D
-------
EPA-CRL 50029 OA 50030 OA sooai OA 50025 OA 39808 OA 39570 OA soois OA *E
1975 245-T:IO PROLAN *BULAN DEHP TEOIQN DlAZINON OYFONATE *E
SAMPLE *HL SMPL WHL SMPL WHL SMPL WHL SMPL wHL SM^L WHL SMPL WHL SMPL *r
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *-.
4806
4808
4810
4812
4814
4816
4822
4824
4826
4828
4830
4832
4834
4836
4839
4840
4842
4844
4846
4848
4850
4852
<.01
<.01
<.0l
<.01
<.01
<.01
<.Q1
<.01
<.01
<.01
<.01
<.01
<.oi
<.oi
<.01
<.01
<.01
<»01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.0l
<.01
<.01
<.01
<.0l
<.01
<.01
<.0l
<.0l
<.01
<.01
<.01
c.Ol
<.Q1
<.01
<.0l
<.01
<.01
<.01
<.01
<.oi •
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<1
1
<1
<1
<1
<1
12
<1
<1
1 •
<1
<1
<1
ft
<1
2
<1
<1
<1
1
2
1
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<.oi
<.01
<.01
<.oi
<.01
<.01
<.01
<.01
<.01
<.01
<.01
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1 : 6S*E
<1 : fiS*E
<1 :10S*E
<1 :12S-*E
<1 :14S»E
<1 :lbS^>E
<1 :22S^*E
<1 :24S^E
<1 :26S-*E
<1 :28S*E
<1 :30S-»E
<1 :32S*E
<1 :34S*E
<1 :36S*E
<1 :39S*E
<1 :40S*E
<1 :42S*E
<1 :445-*E
<1 :46S<*E
<1 :48S*E
<1 !50S*E
<1 :52S*E
29J 30P 31P 32P 33° 34P 3SP **E
W5.DW01 REGION V DRINKING WATER STUDY - WISCONSIN **E
-------
EPA-CP-L S0017 OA S0032 OA 39600 OA 39530 OA 39540 OA S0033 OA 39398 OA *F
1975 RONNEL- OURSBAN MPARATHN MALATMNl PARATH* DEF ETHION *F
SAMPLE XHl_ SMPL WHL SMPL WHL SMPL vi/HL SMPL WHL SMr>L WHL SMPL WHL SMPL *F
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L U(3/L *F
U306
U808
14810
14812
14814
14816
14822
14824
U826
14828
14830
14832
14834
14836
14839
1484Q
14842
14344
14846
14848
14850
U852
-------
FPA-CRl SOOia OA S0034 OA 39580 OA >0035 OA S0036 UA S0037 OA 39488 OA *G
1975 PHENCAPT EPN GUTHIQN PHOSALON AZINFOSt COUMAFOS AROCLOR *G
SAMPLE VHL SMPL WHL SMPL wlHL SMPL wHL SMPL */HL SM^L WHL SMPL 1221 »G
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L -JG/L. *G
14806
14808
14810
14812
14814
14816
14822
14824
14826
14828
14830
14832
14834
14836
14839
14840
14842
14844
14846
14848
14350
14852
<1
<1
<1
<1
< 1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
< 1
<1
< 1
<1
<1
<1
<1
<1
<1
<1
< 1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<1 <5
<0.3 6S*fi
<0.3 BS*G
<0.3 10S»G
<0.3 12S«G
<0.3 14?*r-i
<0.3 16S*G
<0.3 22SJ-G
<0.3 24S*G
<0.3 2bS-»G
<0.3 2HS**G
<0.3 30S*G
<0.3 32S*G
<0.3 34S*G
<0.3 36S»G
<0.3 39S*G
<0.3 40S*G
<0.3 42S*G
<0.3 44S*G
<0.3 46S*G
<0.3 4«S*G
<0.3 50S*G
<0.3 525*^i
43P 44P 45P 46P 4?P 48P 49P **G
.WS.DW01 REGION V DRINKING XATER STUDY - WISCONSIN **G
-------
FPA-CRL 39496 OA 39500 OA 39504 OA 39508 OA S0047 OA S0039 OA S0038 OA *H
"•>975 AROCLOR AROCLOR AROCLOR AROCLOR METHE CL CCL4 CHCL3 *H
SAMP! E 1242 1248 1254 1260 TOT VOL TOT VOL TOT VOLA »H
LOG NO. UG/L UG/L UG/L UG/L UG/L UG/L _ UG/L _ ^*H
4806
.4808
.4909
.4810
.4811
.4812
,4813
.4814
.4815
.4816
.4817
.4822
4823
.4824
4825
.4326
14827
14828
14829
14830
14831
14832
14833
14834
14835
14836
14837
14839
14840
14841
14842
14843
14844
14845
14846
14847
14848
14849
14850
14851
14852
14853
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0,3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0 .3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0 .4
<0.4
<0.4
<0.4
<0.4
<0.4
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
7
<0.5
<1
<0.5
<1
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<1
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
2
4
8
<2
<2
1
3
7
<2
1
<1
10
<2
<1
3
<1
2
3
1
2
; n ^>-»n
: «S*H
SO ' 9S*H
: 1 os-*w
3 :11S*H
: 125*H
8 :13S*H
: 1 4S*H
<1 :15S*H
J 16S*H
4 • 1 7S*H
:22S*H
2 :23S»H
: 24S*H
2 :255*H
:2bS*H
6 :27S*H
' 28S*H
55 :29S*H
: 30S*H
<1 :31S*H
:32S*H
14 :33S*H
: 34S*H
1 :355*H
:36S*H
9 :37S*H
I 3 9 S * h
! 40S*H
10 :41S*H
'• 4 2 S ** H
<1 :43S-»-H
; 44S*M
9 :45S»H
.'46S*H
<1 :47S*H
: 48S*H
53 :49S*M
:50S**H
12 :51S*H
: 52S*H
3 :53S*H
5QP 51P 52P 53P 54P 55» 56P **H
.W^.DWOI REGION v DRINKING WATER STUDY - WISCONSIN **H
-------
FP4-CRL S0056 OA S0040 OA S0041 OA 50042 OA , *I
1975 C2H4CL2 CHCL29R CHCL9R2 CH8^3 *I
SAMPLE TOT VOL TOT VOL TOT VOL TOT VOL *I
LOG NO. UG/L UG/L UG/L UG/L * I
4809
4811
^813
4815
4R17
4823
4825
4827
4^29
4831
4833
4835
4837
4841
4843
4845
.4847
.4849
.4851
.4853
3
<1
<1
<1
<2
<1
<1 .0
< j
<1
<0.5
<1
,» i
<1
<1
<0.5
<3
<0.5
<1
<1
<1
<1
<0 .5
<0 .5
<1
<0.5
<0.5
<0.5
<0.5
c
<0 .5
6
<0.5
4
11
<0.5
3
<0.5
Q
3
<1
<0.5
<0.5
<0 .5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
1
<0.5~
<1
2
<0.5
<1
<0.5
<0.5
0.7
<1
<1
<0.5
<0 .5
<0.5
<0.5
<0.5
<0.5
<1
<0.5
<0.5
<0.5
<0.5
<0.5
<1
<0.5
< 1
<0.5
<0.5
<1
<1
VS»l
115*1
13S<*I
15S»I
17S*I
23S»I
25?*I
275*1
29S*I
31S*I
33S*I
355*1
375*1
415*1
43S*I
455*1
475*1
495*1
515*1
535*1
57P 58P 59P 60P 61P 62P 63P *»I
,W?.DWOI REGION v DRINKING WATER STUDY - WISCONSIN »«i
. .. . T
-------
PA-CRL
1975
AMPLE
OG NO.
801
806
809
810
812
814
316
822
824
826
828
830
832
834
836
838
840
842
844
846
848
850
852
S.DW01
0091b M*
CALCIUM
CA,TOT
MG/L
: <0 . 1
:14.3
:18.2
:9.2
:9.3
:9.0
:8.9
:33.8
:33.8
:42.o
J42.0
:33.6
:32.1
:33.6
:33.2
:34.6
:33.a
:34.3
:33.7
:33.3
:32.4
:34.4
:34.1
64P
REGION
J 00927 MW 00929 MW 00937 MW 01034 MW 01042 MW 01045 MV
MGNSIUM SODIUM OJSSIUM CHROMIUM COPPER IRON
MG»TOT NA»TOT K,TOT CO,TOT CU.TOT FF'TOT
MG/L MG/L MG/L UG/L UG/L UG/L
: 0 . 1
: ft .3
:5.3
:3.9
:3.9
:3.3
:3.8
:10.7
:10.7
:22.3
:22.5
: 11.0
:10.3
: 1 0 . 7
: 10.6
:10.7
:10.6
:10.7
:10.6
: 1 1 .6
: 1 1 . 7
: 1 1 . 0
:10.7
<0 . 1
3.2
3.0
5.0
21.0
5.4
20.7
4.3
4.3
6.3
6.5
4.6
4.4
4.5
4.9
4.4
4.2
4.2
4.3
4.3
9.5
5.4
4.5
<0 . 1 : <5
1.0 :<5
1.0 :<5
3.0 :<5
3.2 :<5
3.0 :<5
3.2 :<5
1.1 :<5
1.2 :<5
1.9 :<5
1.9 :<5
1.2 :<5
1.2 :<5
1.2 :<5
1.2 J<5
1.1 :<5
1.1 :<5
1.1 :<5
1.2 :<5
1.2 :<5
1.2 :<5
1.2 :<5
1.2 :<5
<5
<5
<5
7
<5
9
<5
<5
<5
10
<5
10
<5
<5
<5
<5
<5
<5
<5
<5
<5
112
<5
<20
28
<20
90
40
90
40
<20
<20
44
<20
28
<20
-------
3A-CRL 01055 MW 01092 MW 01002 MW 01051 MW 01027 <-1* 01077 MW 01147 MW *K
975 MANGNESE ZINC ARSENIC LEAD CADMIUM SILVER SELENIUM *<
iMPLE MN,TOT ZN»TOT A5»TOT PBtTOT COtTOT AG.TOT 3E«TOT *<
3G NO. UG/L UG/L UG/L UG/L UG/L UG/L UG/L *<
301 :<5
306 :<5
308 :<5
310 :40
312 :35
314 :30
316 :30
B22 :5
324 :<5
326 :10
328 :<5
830 :ll
832 :<5
334 :6
836 :<5
838 :<5
840 :<5
842 :<5
844 :<5
846 :<5
848 :<5
850 :<5
852 :<5
<5
<5
<5
<5
<5
<5
<5
7
<5
13
12
7
<5
7
<5
6
<5
<5
<5
<5
<5
130
14
<1 :3
<1 :<2
<1 :<2
<1 :7
<1 :<2
<1 :9
<1 :<2
1 :<2
<1 :4
<1 :7
<1 :<2
1 :<2
1 :<2
1 :<2
<1 :<2
1 :<2
<1 :<2
1 :<2
<1 :<2
1 :<2
1 :<2
<1 :2
<1 : <2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
1 < C . 2
:<0.2
<0.2
. <0.2
•<0.2
<0.2
:<0.2
! <0.2
:<0.2
• <0.2
<0.2
<0.2
: <0.2
. <0 .2
•<0.2
: <0.2
<0.2
: <0,2
• <0.2
<0,2
<0.2
<0.2
<0.2
:<5 : 1S*K
:<<5 : 6S*K
<5 ' 8S*K
:<5 :10S*K
:<5 :12S*K
<5 !14S*K
•<5 J16S*K
•<5 :22S*K
<5 :24S*K
<5 ' :26S*K
<5 :28S»K
<5 :305»K
<5 :32S»K
<5 :34S*K
<5 !36S*K
:<5 :38S*<
<5 :40S*K
<5 :42S»K
<5 :44S*K
<5 :^6S*K
<5 !48S*K
<5 :50S*K
<5 :52S*K
TIP 72P 73P 74P 75P 76P 77P **K
S.DWOI REGION V DRINKING WATER STUDY - WISCONSIN **K
-------
A-CRL
975
MPLE
G NO.
06
08
10
12
14
16
22
24
26
28
30
32
34
36
38
40
42
44
46
48
50
52
;.owoi
00530 IM
WESIDUE
TOT NFLT
MG/L
:<2
:<2
:<2
:3
:5
:<2
:<2
:<2
: STUDY - WISCONSIN
00410
T ALK
C*C03
MG/L
36
55
"28
59
28
58
105
Q4
180
153
107
100
108
100
106
103
106
101
10<3
88
107
100
84P
IM *L
*L
*L
*L
: fi^»L
: 83*L
: IOS»L
: 12S*L
: 14S»L
: 16S*L
:22S*L
:24S*U
:26S*L
:28S*L
:30S*L
:32S*L
:34S«L
:36S*L
:38S*L
: 40S*L
:42S<*L
:44S*L
:46S*L
:48S*L
:50S*L
:52S*L
*«(_
»•»(_
-------
PA-CRL
1975
AMPLE
OG NO.
801
802
806
808
810
812
814
816
822
.824
.826
.828
.830
.832
.834
• R36
.838
>840
t842
tS44
v846
t848
h850
i.«52
«S.DW01
00665 IN
PHOS-T
P-WET
MG/L
<0.02
0.10
0.11
0.08
0.08
0.08
0.08
0.03
<0.02
0.02
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
------- |