the National
Water Quality Network
operating manual
For Participating
Laboratories
U.S. DEPARTMENT OF
HEALTH, EDUCATION, AND WELFARE
Public Health Service
REVISED JUNE 1963
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NATIONAL WATER DUALITY NETWORK
§ OPERATING MANUAL
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A Guide for Laboratories Participating in Sampling
I and Analytical Activities of the
National Water Quality Network
§ Revised June, 1963
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(U.S. DEPARTMENT OF HEALTH, EDUCATION, AND WELFARE
Public Health Service
Bureau of State Services
I Division of Water Supply and Pollution Control
Basic Data Branch
I Water Quality Section
101A Broadway
Cincinnati 2, Ohio
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TABLE OF CONTENTS
Page
SECTION I
THE NATIONAL WATER QUALITY NETWORK 1
Laboratory Analyses 2
Sampling 6
SECTION II
GENERAL INSTRUCTIONS 7
Sampling Schedules 8
Shipping Instructions 9
Assistance with Sampling, Laboratory,
and Other Operational Problems 9
Addresses and Phone Numbers of
Regional Offices 11
SECTION III
ORGANICS SAMPLING BY CARBON ADSORPTION METHOD 13
I Types of Sampling Equipment in Use 13
Description of Carbon Adsorption Column 13
Presettling, Prefilter, and Backwash 13
•Installations with Manual Backwash 15
Installations with Automatic Backwash 18
Pumping Systems 22
I Precautions 22
Collection of Sample 23
Use of Carbon Column Data Sheet 23
Shipping 25
• SECTION IV
I COLLECTION OF SAMPLES FOR RADIOACTIVITY
MEASUREMENTS 2?
SECTION V
COLLECTION OP SAMPLE FOR PLANKTON ANALYSIS 29
SECTION VI
MEMBRANE FILTER DELAYED INCUBATION PROCEDURE 31
Supplies and Equipment 31
Sample Volume and Filtration 35
Shipping 39
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• SECTION VII Page
CHEMICAL AND PHYSICAL ANALYSES 4-3
g Preliminary Remarks
Temperature
_ Dissolved Oxygen (DO) •-
I PH , I/,
• Biochemical Oxygen Demand (BOD) >£
Chemical Oxygen Demand (COD) 56
•Chlorine Demand - 1 hour and 24 hour ??
Ammonia Nitrogen (NH,/N) 63
Chlorides 66
• Alkalinity (as CaCO^) 6y
Total Hardness (as CaCO,) 70
•Color 72
Turbidity £•>
Sulfates {>
I Phosphates
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• LIST OF FIGURES
Page
• Regions and Regional Offices 12
Carbon Adsorption Column and Shipping Container 14
I Details of Sand Prefilter 16
Schematic Diagram of Piping Installation
• for Sand Prefilter and Carbon Filter 1?
Carbon Adsorption Unit Model HpO-MIC
• with Pre~Sand Filter and Automatic Backwash 19
Carbon Adsorption Unit, Model H20-M2C
Iv/ith Pre-settling Tank and Auxiliary 20
Equipment in Shelter
_ Schematic Flow Diagram - Organics
• Sampling Apparatus 21
Sample Report Form for Carbon Filter Data 24
• Single Bottle and Shipping Container for
Water Samples for Radioactivity 28
J Twinpak Bottles and Shipping Container
Used when 1-liter Sample is Provided
for Radioactivity and 1-liter Sample
• for Chemical Analysis at Cincinnati 28
Plankton Bottle and Shipping Container 30
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Filtration Apparatus and Shipping Container
for Coliform Samples -33
Preparation of m-Endo Broth
Dilution Chart for Membrane Filtrations 39
• Placing Membrane on Pad Soaked with
Preservative Medium 41
Sample Report Form for Delayed Incubation
Test 44
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• LIST OF FIGURES
Page
I Nomograph for Preparation of 00025N
Thiosulfate from 1.00 N Thiosulfate 51
(Nomograph for Preparation of 0.014-1N
Mercuric Nitrate from 0.14-1N
Mercuric Nitrate 70
I Sample Report Form for Chemical Analysis 8?
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SECTION I
THE NATIONAL WATulS .JJAIITT NETWORK
THE NATIONAL WATER QUALITY NETWORK was established by
the Public Health Service in 1957« It is operated in
cooperation with state, local and other federal agencies
having related responsibilities for the collection,
interpretation and dissemination of basic data on chemical,
physical, and biological water quality as it relates to
water pollution prevention and control.
The overall objectives of the Network are to provide:
a. Information pertaining to the effect of changes in
water use and development on water quality at key
points in river systems;
b. continuing information on the nature and extent of
pollutants affecting water quality;
c. data that will be useful in the development of
comprehensive water resources programs;
d. data that will assist state, interstate and other
agencies in their water pollution control programs
and in the selection of sites for legitimate water
uses.
As of April, 196$, there were 125 sampling locations
in the Network. Each location satisfies one or more of the
following criteria:
a. Major waterway used for public water supply, propa-
gation of fish and wildlife, recreation, agricultural,
industrial and other legitimate uses;
b. interstate, coastal and international boundary waters;
c. waters on which activities of the Federal Government
may have an impact.
With its selection as one of the network of key stations,
the participating laboratory occupies a unique position.
Data collected at this and other Network stations will serve
as a foundation for the evaluation of water pollution control
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progress, both on a state and national level. The data will
also reflect trends in water quality over the years, and
thus provide an intelligence service on the quality of water
resources of the nation. Finally, the participating
laboratory will be a connecting link or reference point
in intrastate or river basin pollution abatement programs.
LABORATORY ANALYSES
The analyses to be carried out have been selected on
the basis of emerging and foreseeable problems in water
quality management, as described below:
Radi o ac t ivi ty
Interest is rapidly growing in routine monitoring of
water for radioactivity. With the development of nuclear
power reactors and other peacetime atomic energy uses
this interest will become even more intense. State and
interstate agencies and municipalities are becoming increas-
ingly concerned about establishing such programs„ Experience
with this Network will, it is hoped, encourage and stimulate
more effective state and local programs in radiation monitoring,
Organic Chemicals
Studies conducted during the past decade have shown
that products of our chemical technology, particularly
organic contaminants, are being recovered from waterways in
more and more locations as chemical plants increase in size
and number, and as their products are increasingly used in
the home, in industry, and in agriculture. Synthetic deter-
gents, pesticides of all kinds, and other petro-chemicals
are examples of these contaminants. An increasing number
of reports of water damages from these pollutants is being
made. Damages that can occur from trace amounts of contam-
inants include unpleasant tastes and odors, off-tastes in
fish, fish kills, foaming, water treatment difficulties,
and interference with recreational uses of water. It is
important to assess the kinds and quantities of such wastes
in our surface waters for the protection of all legitimate
water uses.
The measurement of the trace concentrations of organic
contaminants requires the use of special techniques since
our common procedures lack the needed sensitivity and
specificity. Concentration of the contaminants by means
of a carbon adsorption column followed by solvent elution
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and organic analyses presently offers our- "best means of
measuring the segment of organics of most interest. The
chloroform and alcohol extractable materials along with
separated groups provide a tangible material that can be
analyzed and stored for future reference, Infrared charac-
terization of the eoctractable materials makes it possible
to screen these substances for specific compounds. Gas
chromatographic analysis is also employed in these identi-
fications,
Differences in the relative adsorbability on carbon
of various organic compounds found in surface waters, as
well as the decrease in column adsorption efficiency in
heavily polluted waters make it inadvisable to consider
results as strictly quantitative,,
BioIpfiical Populations
Natural waters support a variety of organisms ranging
in size from bacteria and minute diatoms to fish. If the
water quality deteriorates, the populations change* Those
forms of life least affected, or in some cases benefited
by water quality deterioration, will find less competition
and may develop in very large numbers. Therefore, the
presence of large numbers of organisms representing only
a few of the more tolerant species is indicative of
pollution. Conversely, waters supporting a large variety
of organisms in few to moderate numbers is typical of good
water quality.
Plankton, microscopic or barely visible plant and
animal forms that have limited locomotion in water, com-
prise an important group for study in relation to water
quality. Some of these impart objectionable tastes and
odors to water, while others are troublesome because they
clog sand filters in water treatment systems. Plankton
populations that respond to the water quality changes
brought about by pollution are useful in detecting water
quality characteristics.
Studies are made of the animal life in the stream and
lake bottoms. These bottom-dwelling forms are called benthos,
They usually remain in one place and are subjected to water
that passes over them. If the water quality and bottom is
suitable they grow, reproduce, and provide important food
for fish. Water of adverse quality will, however, destroy
some or most of the forms, Benthic life varies greatly
in ability to survive water quality changes, A study of the
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kinds of life and their relative numbers is useful in
detecting both improvement or deterioration of water quality.
Fish require water that contains adequate oxygen and is
nontoxic. They must also have suitable food consisting of
either plankton, benthos, or small fish that have fed upon
plankton or benthos. Fish, like other aquatic life, vary
in their sensitivity to pollution. Observations of the
kinds of fish, their numbers, and rates of growth are useful
in evaluating suitability of water for this purpose.
Coliforms
The presence of these organisms in water is direct
evidence of the presence of sev/age. The degree of contam-
ination of the water by these organisms will be of interest
to the municipality using the stream for its source of water.
The delayed membrane filter technique will be used to carry
out this test, as it is the most reliable method available
whereby samples can be shipped long distances without deter-
ioration*
Chemical and Physical Parameters
There are many standard chemical and physical measure-
ments that can be made on water. Those of significance to
the establishment of water quality vary with the purposes
for which the water is to be used. The determinations selected
below are of basic value to most water uses. They have,
therefore, been included in the Network program. In certain
locations other determinations, of local significance, may be
added as the program develops. The measurements the Network
reports for each station are listed below in the order in
which they appear on the Field Form (PHS ?845-l, Keviscd,
6-59).
1. Temperature
2. Dissolved Oxygen
3. pH
4-. Biochemical Oxygen
Demand
5» Chemical Oxygen
Demand
6. Chlorine Demand-
1 hour
7« Chlorine Demand-
24 hours
0. Ammonia Nitrogen
9. Chlorides
10. Alkalinity
11. Total Hardness
12. Color
1J. Turbidity
14. Sulfates
15. Phosphates
16. Total Dissolved Solids
A copy of the Field Form appears on page 87 «
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The laboratory facilities of the Water Quality Section
in Cincinnati are equipped to perform the determinations
numbered 9 through 16. It is necessary for the participating
laboratories, however, to run the analyses numbered 1 through
8 since these measurements change with time.
The Water Quality Section will assist individual labor-
atories in every way possible, by furnishing expendable
equipment and prepared reagents and by personal visits, if
necessary, that these determinations may be available from
each Network station. All data collected at each sampling
point will be freely exchanged among the Public Health
Service, the participating laboratory, and the state agency
responsible for water pollution control.
In many cases where laboratories are well equipped they
are able to perform all of the requested analyses. Thirty-
five of the 125 Network stations are reporting all 16 of
the requested determinations.
Reference Samples
In a national program wherein analytical results originate
from a multitude of laboratories it is essential that lab-
oratory data be comparable as to precision and accuracy.
The Reference Sample activity is a means by which this
objective can be achieved.
This is accomplished by preparation of a large volume
of a standard sample into which the desired constituents
are measured very accurately. Similar portions of the sample
are then mailed to each of the participating laboratories,
along with a report form and complete instructions for analysis,
tVhen the analytical results are returned to the Water Quality
Section, a second report is returned to the responding lab-
oratory showing how its results compare with the true results.
Whenever possible, comments concerning sources of error and
means of correction are included. When all the groups have
reported, a final review and summary of all the data is
distributed to all Network agencies.
These samples are distributed periodically and past exper-
ience has shown that this mechanism leads to increased pro-
ficiency of the participants. In addition, it has served
to point up routine errors within a laboratory that would
otherwise have gone unnoticed.
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SAMPLING
All samples are to be of raw waters. All samples are to
"be collected from the flowing stream or from the raw water
intake prior to any treatment, including sedimentation,
prechlorination, etc.Samples for determination of radio-
activity, organic chemicals, plankton populations, and
coliforms are to be shipped to the Water Quality Section at
Cincinnati for analysis. The chemical analyses will be
performed by the participating laboratories on samples collected
at the same time. Procedures for collection, shipment and
analyses of samples are given in subsequent sections of this
manual.
All sampling containers, shipping cases, and other
materials will be provided and all shipping charges will be
paid by the Public Health Service. Carbon adsorption columns,
packed with carbon, will be furnished in individual shipping
containers. Containers and shipping cases will be provided
for the remaining samples.
Cooperating laboratories are encouraged to develop
laboratory competence in the analyses, especially in those
determinations that must be performed immediately. The
Public Health Service will furnish all possible assistance
through training, methods, consultation, reference samples,
loan of equipment, and other resources that may be available.
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SECTION II
GENERAL INSTRUCTIONS
Routine collection of samplcc for shipment to the Water
Quality Section will he carried out according to detailed
instructions for collection and shipment presented in subse-
quent sections of this manual. The program includes the
following:
a. Radioactivity Sample - weekly:
A 1-liter sample should be taken weekly.
b. Chemical Sample - weekly:
A 1-liter sample should be taken weekly at the same
time the radiological sample is taken. Since many
stations perform all the chemical measurements, a
weekly chemical sample need not be sent to the Y/ater
Quality Section. In cases where the analytical work
is performed by the Water Quality Section, a "TWIN-
PAK" container is provided by which two 1-liter
samples may be shipped together (see Section VII:
Page 43 , paragraph 4 ).
c. Coliform Sample - weekly:
This sample should be collected on the same day as
the chemical and radiological samples are taken. Note
that this sample should not be taken on a Thursday or
Friday. Membrane filtration and mailing of this
sample to the Water Quality Section should be done
as quickly as possible after collection.
d. Plankton Populations Sample - semi-monthly:
Requires a 51/£-pint sample. Collect on the same day
as the chemical and radiological samples are taken.
e. Carbon Adsorption Sample - monthly:
Start carbon adsorption mechanism on the same day that
a sample is collected for the chemical and radiological
sample.
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f. Chemical Oxygen Demand Sample - weekly and monthly:
The determination is to be performed weekly
whenever possible. For those laboratories that
cannot perform this test, a sample bottle is supplied
in the shipping box with the carbon adsorption sample.
This sample should be collected on the next sample day
after the carbon unit is put into operation, and a
portion of the sample should be placed in the bottle.
Note: This bottle will not appear in the box when a
station performs the test weekly at the collection
point.
SAMPLING SCHEDULES
Weekly and monthly sampling schedules should be set by
each participating agency to fit in best with normal routine
operations. Once the schedule is established, however, it
should be followed as closely as plant operations permit. The
preferred days are Monday, Tuesday, or Wednesday. Thursday
samples for coliform arrive either too late on Friday for
processing or are not delivered until the following Monday.
Friday samples for coliform are also unsatisfactory since
extended time in the mail causes a large percentage of these
to be unreliable, especially during warm seasons of the year.
First sample day of each month,
1. Collect chemical and radiological samples, mail to
Cincinnati. Analyze chemical sample and mail results.
2. Collect,filter, and mail the membrane filter coliform
sample.
J. Start the carbon adsorption run.
4-. Collect and ship the plankton sample.
Second sample day of the month,
1. Same as first sample day.
2. Same as first sample day-
3» Collect COD samples and place in carbon column shipping
box (if applicable).
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Third sample day of each, month,
1* Same as first sample day.
2. Same as first sample day.
3. Remove carbon column and ship to Cincinnati. (This may
be done on any day that the carbon adsorption run is
completed).
4-, Collect and ship plankton sample.
Fourth sample day of each month,
1. Same as first sample day.
2. Same as first sample day.
Fifth sample day of each month,
If the month has five sample days, repeat the fourth
week's schedule. If the sample day coincides with a
holiday, sample on the first workday following the
holiday.
SHIPPING INSTRUCTIONS
All samples, except the carbon adsorption samples, are
to be shipped by mail or parcel post to:
U. S. Department of Health,Education, and Welfare
Public Health Service
1014 Broadway
Cincinnati 2, Ohio
Attn: Chief, Water Quality Section
National Water Quality Network
The carbon adsorption samples are to be shipped by
Railway Express, Charges Collect, to the above address. See
special comments regarding shipping instructions in Section
III, page 25 .
ASSISTANCE WITH SAMPLING, LABORATORY, AND OTHER OPERATIONAL
PROBLEMS
If questions or difficulties arise in connection with
instructions and procedures outlined in this manual or any
other phase of the Network operation, the participating
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agency should contact the Water Quality Section in Cincinnati,
Ohio, "by telephone collect, or "by other means of communication
as indicated by the circumstances involved. Requests for
assistance should be directed to:
Chief, Water Quality Section
National Water Quality Network
1014 Broadway
Cincinnati 2, Ohio
Telephone:
381-2200
Ext. 2925,
2926, or
2927.
Addresses and phone numbers for each of the USPHS Regional
Offices are also listed on the following page. These are
given because there is an appointed representative in each
office to assist the Network participants in whatever way
possible. Personnel at the Network stations are urged to
contact these representatives as the circumstances demand
expecially if it appears that assistance or information may
be obtained more efficiently. A map showing the geographical
areas of the respective Regions is included on page 12 .
Requests for assistance from the Network representative
in the Regional Offices should be made through the Regional
Program Director, PHS«
The addresses and phone numbers for the various regional offices
are given on the following page.
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ReEion I
120 Boylston Street
Boston 16, Massachusetts
Telephone: 617-482-6550
Region II
Room 1200, 42 Broadway
New York 4, New York
Telephone: 212-363-2523
Region III
700 E, Jefferson Street
Charlottesville, Virginia
Telephone: 703-296-5171
Region IV
Room 453, 50 Seventh St., N. E.
Atlanta 23, Georgia
Telephone: 404-876-5737
Region V
Room 712 New Post Office Bldg.
433 W. Van Buren Street
Chicago 7» Illinois
Telephone: 312-828-5250
Region VI
560 Westport Road
Kansas City 11, Missouri
Telephone : 816-221-7000
Region VII
Ninth Floor
1114 Commerce Street
Dallas 2, Texas
Telephone: 214-748-2721
Region VIII
Room 551
621 Seventeenth Street
Denver 2, Colorado
Telephone: 303-534-1320
Region IX (San Francisco, Calif.)
447 Federal Office Bldg.
Civic Center
San Francisco 2, California
Telephone: 415-552-2350
Region 23 (Portland, Oregon)
Room 570, Pittock Block
921 S. W. Washington
Portland 5, Oregon
Telephone : 503-226-3361
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SECTION III
ORGANICS SAMPLING BY CARBON ADSORPTION METHOD
The carbon adsorption method of organics sampling consists
of the passage of up to 5»000 gallons of raw water at a rate
of 1/4- to 1/2 gallon per minute through a carbon adsorption
column,, Following the sample run, the column is shipped to
the Water Quality Section, Cincinnati, Ohio, for analysis.
TYPES OP SAMPLING EQUIPMENT IN USE
There are three types of carbon adsorption mechanisms
in current use. The first and oldest of these consists
of a piping arrangement that was originally assembled and
installed at the sampling location. This device is referred
to as the manual type installation and is discussed on
page 15* The other two types are automatic sampling devices
(designated EpO-MIC and H?0-M2C) prefabricated in the Water
Quality Section Workshop and are shipped ready for installa-
tion. The M-l is a panel unit equipped with automatic
backwash device, designed for inside-the-plant use. The
M-2 unit is similar to the M-l unit, but is built into protective
housing for operation in remote or outside-the-plant use.
Since a large number of the manual devices continue to
operate with good efficiency, it is not anticipated that they
will be replaced in the near future. A discussion of operating
procedures for both types of equipment is therefore included
in this section.
DESCRIPTION OP CARBON ADSORPTION COLUMN (CAC)
The GAG consists of a piece of pyrex glass pipe 3 inches
in diameter and 18 inches long. The ends are fitted with
brass plates and 3/4-inch galvanized nipples. A stainless
steel screen is fixed in a neoprene gasket at both ends. The
filter unit will arrive packed with activated carbon ready
for use. The special shipping container provided should
be used when returning the filter. The unit, with the ship-
ping container is pictured on page 14-.
PRESETTLING, PREPILTER, AND BACKWASH
River waters will frequently clog the CAC before the
desired volume of water has been sampled. To prevent this,
it is necessary to remove enough turbidity to permit the
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required amount of water to pass through the unit* This may
require a presettling tank and a prefilter containing sand
and gravelo
Presettling: Tank,
A standard hot water tank connected with the inlet at the
bottom and outlet at the top, with a clean-out tap at the
bottom, can serve as a presettling tank. The outlet connects
to the prefilter containing sand and gravel* The hot water
tank should be flushed at frequent intervals to prevent accum-
ulation of solids„ Open settling tanks can be used, if flow-
through time at 1/2 gpm is less than 4- hours0 With open tanks
a pump will be required to move the water through the filter,,
Figure 1 - Carbon Adsorption Column and Shipping Container^
(Note COD Sample Bottle)
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Sand Frefilter,
The sand prefilter provided by the Water Quality Section
consists of a steel pipe 3 feet long and 3 inches in diameter,
threaded at both ends , and equipped with 3 by 1-inch reducer
couplings o Two discs of stainless steel screen are fitted
to the inside diameter of the pipe0 The space between the
screens is packed with 6 inches of 1/8-inch gravel, 24- inches
of 006 to Oo8 mm sand, and another 6 inches of 1/8-inch gravel 0
No free space is left in the pipe*, The gravel is packed by
jarring the pipe while fillingo This arrangement provides a
strainer, rather than a filter, with a movable bed» By such
an arrangement backflushing can be done without disturbing the
filter,, The construction details are shown in Figure 2«
INSTALLATIONS WITH MANUAL BACKWASH
The presettling tank, the sand prefilter and the GAG should
be installed at the most convenient source of raw water., If
less than 15~psi pressure is available, it may be necessary
to pump the water through the system,, A drawing of a workable
system is shown in Figure 3° Exact lengths of pipes , etc0 are
not given 9 since these will vary with the local situation.,
Both the sand and GAG are connected with unions at both ends
for easy removal „
The raw water flows upward through the sand prefilter and
the CACo When the rate of flow through the system falls below
1/4- SPm» backwashing of the sand filter becomes necessary,
with use of a high pressure source of water,, A clean water
hose is connected to the top of the sand filter ? the valve to
the GAG is closed, the drain valve on the sand filter is opened.
The sand is backflushed until the water coming out is clear,,
The length of time between backwashings will vary0 On the
Missouri River ? for example, it has been found that once
every 8 hours is usually sufficient,,
After backwashing connect the system as before and continue
the samplingo To prevent a cross— connection, be sure to
°f sand filter after backwashingT A
pressure gauge is inserted in the system to ndcate when
clogging is taking place in the carbon filtero Total pressure
in the filter should not exceed 50
A water meter located at the end of the system is used to
measure the volume of water sampled,, A 5/8 by 3/4— inch ,
disc-type meter, or oscillating piston«type meter, registering
in gallons and capable of measuring flows as low as 1/4 gallon
per minute, may be used for this purpose,, A valve following
the meter throttles the flow, if necessary 0 A flow-regulating
device may also be used for this purpose 0
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16-18 MESH
CTAINI F^9 9TFFI
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• SAND PREFILTER — >•
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<— HOSE CONNECTION
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1 Figure 3 - Schematic Diagram of Piping Installation For
Sand Prefilter and Carbon Filter
1
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- 18 -
Fine carbon dust washes out of the CAC when it is first
startedo A few gallons of water should be passed through the
top connection and through the CAC drain before the meter is
cut in, to keep the meter free of the carbon.
The system outlined is not intended to remove all traces
of turbidity from the water before it passes through the CACo
Its purpose is to take out gross materials, most large organ-
isms, and permit the required volume of water to pass through
the carbon0
Occasionally, so*ae stations may experience clogging of the
sand filter owing to high algae coneentrations, These organ-
isms tend to penetrate into the sand and are difficult to
backwasho When this situation is anticipated, an increase
in frequency of backwashing is indicated,
Backwashing every 2 hours is not uncommon under these
circumstanceso If, even after this precaution is taken, the
sand filter becomes clogged, the only alternative is to
replace the sand»
INSTALLATIONS WITH AUTOMATIC BACKWASH
Preassembled panel units with automatic backwash of the
sand prefilter have been developed to ease installation and,
operation of the organics sampling apparatus« Figure 4 shows
the Model ^O-MIC panel unit designed for installation in water
treatment plants and other buildings„ This equipment has an
electric timer and solenoid valves to backwash automatically
the sand prefilter0 The panel includes an electric disconnect
switch of fuse plug type and grounding-type duplex outlet for
pump,, It also has three 3-way cocks, one to protect the
water meter from fine carbon at the beginning of sampling,
one to facilitate checking of the flow control valve and
water meter, and one to check backwash performance0
For remote locations the sampling apparatus is installed
in an insulated equipment shelter,. An organics-sampling
field unit, Model HpO-M2C, containing preassembled panel
apparatus? a 30-gallon presettling tank, electric space
heater, and auxiliary equipment is shown in Figure 5° The
pumping system will vary depending on the needs of the
individual sampling station, A submersible pump was used
for the field unit shown in Figure 60 The equipment shelter
contains, however, sufficient space for a jet centrifugal-
type pump, or other acceptable motor pump unit»
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Figure 4- - Carbon Adsorption Unit Model H^O-MIC with Pre-Sand
Filter and Automatic Backwash.
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Figure 5 -
P Ad?01?tio* Ynit' Model H20-M2C With Pre-
settlmg Tank and Auxiliary Equipment in Shelter,
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Figure 6 - Schematic Flow Diagram - Organics Sampling Apparatus,
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- 22 -
PUMPING SYSTEMS
Pumps, piping, and accessories are selected to suit the
specific conditions of each station. Shallow and deep well-
type jet centrifugal pump systems are in use at many network
installations to "bring raw water from a representative
sampling point to the sampling apparatus. Submersible pumps
with helical screw rotors and synthetic rubber stators,
rotary pumps with flexible impellers, and other pumping
mechanisms may be installed to meet individual needs.
It is important that the pump used does not contaminate
the sample through grease-type packing or other sources.
The pump must have a greasless-type rotary shaft seal or
special packing material to avoid contamination. New pumps
are sometimes grease-coated and should be thoroughly cleaned
before being put into service. Piping strainers, check valves,
and all other accessories that come in contact with the raw
water pumped to the GAG filter must also be cleaned (see
Precautions, paragraph below.)
A prefabricated metal building can be provided, where
required, to provide a permanent shelter for equipment and
operating personnel. This type of building is usually
installed on a reinforced concrete base. An organics-sampling
panel unit (Model HpO-MIC), a pumping system, and other samp-
ling equipment may be installed in this type of facility.
A schematic flow diagram for the Organics sampler, Models
H20-M1C and H20-M2C, is shown in Figure 6. Details of
installation, operation, and maintenance of this equipment
are contained in a separate manual, available on request.
PRECAUTIONS
The purpose of the GAG is to adsorb small amounts of
organic impurities from the water in as great quantity as
possible. It is important to avoid contamination of the carbon
from other organic sources. Hence the following precautions
should be observed:
a. New strainers, pipe fittings, and other accessories
are usually coated with oil or grease. The oil
should be removed by washing in kerosene (or chloro-
form) followed by a detergent wash before fittings are
used for making connection to the GAG.
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- 23 -
b. Ordinary organic pipe jointing compounds should not
be used. Red lead (lead oxide) mixed to a paste witli
water can "be used for this purpose. ( A small
supply of red lead is initially furnished for installa-
tion of the sampling system).
c» Plastic hose is to be avoided, and if rubber hose is
used in any connections it should be flushed thoroughly
before being connected to the GAG. Copper tubing is
ideal for connections. NOTE: Polyethylene pipe and
PVC (polyvinyl chloride) pipe meeting National
Sanitation Foundation (NSP) standards for drinking
water use are acceptable.
COLLECTION OP SAMPLE
Water should be passed through the CAC at a rate of 1/4-
to 1/2 gallon per minute until up to 5»000 gallons have
been sampled. With highly turbid waters, clogging may occur
earlier. Although a suitable sample can sometimes be obtained
with several hundred gallons, it is desirable to sample a
minimum of 2,000 gallons, if at all possible. The sampling
procedure is begun by installing the CAC and flushing with
raw river water to remove carbon fines (through three-way
cock "X" on panel units.) Make entries on data sheet as des-
cribed under "Use of Carbon Column Data Sheet."
NOTE; If the filter clogs, turn filter end to end and/or
backwash for 2 to 3 minutes once to obtain at least a 2,000
gallon sample.
If water meter does not register, measure rate of flow
several times during run by timing flow to fill a 1-gallon
container.
USE OP CARBON COLUMN DATA SHEET
Since the aim is to approach a quantitative evaluation of
organics in water, it is important to have accurate flow
measurements.
In Preparing the data sheet (see illustration 7)•
1. Pill in all of the pertinent data at the top of the
sheet, (i.e., state, station location, type of
sample, collected by).
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1
" 37
1 DEPARTMENT OF HEALTH, EDUCATION, AND WELFARE
^ PUBLIC HEALTH SERVICE
v y WATER QUALITY SECTION
1* \ ) \ *r 1014 Broadway, Cincinnati 2, Ohio
K W\ \ ^
\ T? CARBON FILTER DATA
STATE STATION LOCATION (River Mileage) J£~ ) £
1 OMtO 3H CINCINNATI - oUlo RIVER
| TYPE OF SAMPLE (Raw, Finished, Other) R ANA/
• COLLECTED BY: (Company or Agency) £T f M £ 1 N N *T | WA-T £ IS DEPARTMENT
IDATE CARBON FILTER STA
RTED 1*2.^" 43 STOPPED -4-i-(e>3
TOTAL GALLONS FILTERED ^TO 1 2-
DATE
1-2-L
I^J *"• /
3-^8-
^_ ~} ^.*^ ^i
• .;> «*• 1
•
B^ "^ — • ^v f~^
13-31
4-1
1^-2-
I ^J
•
METER READING
IN GALLONS
1C? IS"O
_2j,Uo
1.1 Z3o
2_-?*Ko
1 & Cio
•2-^j 3>-i ^
2<, 7^r
^or&r
31 IU2-
••^
REMARKS
lo*°A.M. START
_2^°AJUSA^KET
•7^A.M.
^10A^La£lLAc£
73oAl/j
tUiooji___
_1!!AH_STOP
Ji££0 cnAZ£Lf_
DATE
LEAK
REPAI
_^i^
&CX2A
METER READING
IN GALLONS
Ig
hATA ^
REMARKS
MEETS
• DISTRIBUTION: White Copy to Address Above,- Pink Copy for Retention by Collecting Laboratory or Agency.
PHs-2845-7 WATER QUALITY BASIC DATA REPORT (CARBON FILTER) FORM APPROVED.
(9.53) BUDGET DUREEAU NO. 68-R6 34
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2. Insert the date the cartridge was placed in service.
J. On the first line of the table, again enter the
date of starting and the meter reading at the time
of start.
4-. Keep a daily record of dates and meter readings
throughout the sampling period, if possible.
5. When sampling is stopped make the last entry of date
and meter reading in the table. Enter the final
date again opposite "stopped".
6. Subtract the initial meter reading from the final
meter reading and enter the difference opposite
total gallons filtered.
(NOTE; If meter reads in cubic feet, cross out "gallons" and
write in "cubic feet.")
7. Any pertinent observations related to difficulties
with the equipment, weather problems, etc. may be
entered under Remarks„
8. Place the white (top) copy of the data sheet in the
box with the column for return to the Water Quality
Section. The pink copy is retained by the cooperating
agency.
9. Upon receipt of the used GAG in Cincinnati, a new
column will be returned to the station for the next
run.
SHIPPING
When the sampling period is complete, disconnect the GAG
and drain off the excess water. Cap both ends of the GAG.
Place in the box with data sheet, and replace wooden chucking
blocks, closing securely. Affix the address label to the top
of the box. The box should be returned j *.
Pay no charges for shipment. If difficulties arise on this
point,call the Chief, Water Quality Section, collect,
381-2200, Extension 2925.
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- 26 -
*Carbon cartridges are returned from some National Water
Quality Network stations by parcel post. The parcel post
label marked "postage and fees paid, Dept. of HEW" is included
for the use of these stations in returning the box.
Other National Water Quality Network stations must use
Railway Express for return shipment. In boxes sent to these
stations, Railway Express labels have been provided. These
labels permit the box to be transported to Cincinnati (only)
with the charges being paid in Cincinnati. Pay no charges!
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- 2? -
SECTION IV
COLLECTION OE SAMPLES IOE RADIOACTIVITY MEASUEEMEFTS
A 1-liter grab sample of raw water is collected on a
weekly "basis for radioactivity measurements.
The sample should be collected at the same time that a
portion is taken for the chemical analysis. It should "be
taken from the stream or from the raw water intake line, prior
to any treatment whatever within the plant. This sample must
reflect river quality. Therefore, it should be taken before
there is any opportunity for sedimentation. Einse the bottle
with raw water before filling it to the bottle neck. Be sure
to fill out the enclosed tag and attach it to the^bottle.
Sample bottles and shipping containers are shown ill Figures
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- 28 -
Figure 8 Single Bottle and Shipping
Container for Water Samples for
Radioactivity.
Figure 9 Twinpak Bottles and
Shipping Container Used When 1-liter
Sample is Provided for Radioactivity
and 1-liter Sample for Chemical
Analysis at Cincinnati.
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- 29 -
SECTION V
COLLECTION OF SAMPLES FOR PLANKTON ANALYSIS
Plankton samples are collected twice a month. The sample
bottle is a 3-liter, polyethylene container mailed in a
fibreboard container with a reversible label.
A single bottle in a shipping container is sent to each
station several days before the sampling date. The 100 ml
of preservative in the sample bottle has approximately 0.1
percent of Merthiolate (Thimerosal), sodium carbonate, and
Lugol's solution.
The water sample should be taken from the stream or lake
at a depth of 2 to 15 feet below the surface, if possible.
The bottle should be filled to the line on the neck of the
bottle. Care should be taken to prevent spillage of the
preservative or dilution by overfilling. The preservative
is effective for at least a month, but care should be taken
to avoid exposure to excessive heat or sunlight, which will
reduce its effectiveness.
Samples should represent the typical water of the stream
or lake. Direct sampling from the water source is preferable,
but in some cases water must be taken from a pipeline. Water
that has passed through gravel or fine screens should be
avoided because the plankton can be greatly reduced by the
filtering action.
Each bottle is sent with a tape around the cap bearing
suggested date of collection, and a tag containing a station
number. The tape should be replaced on the bottle to insure
its remaining tight during shipment, and the tag filled out
with the requested station information and collection time.
Sample containers are sent to each station ten days prior
to the sampling date. If, for any reason, a sample cannot be
collected, the empty container should be returned to the
Network Laboratory so that the preservative can be renewed.
The address label provided on the shipping container may
be removed from the plastic frame. It is provided with the
Water Quality Section address on one side and the station
address on the other side. Ship the container by parcel post
making sure that the label is turned to show the Water Quality
Section address.
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Figure No. 10.
Plankton Sample Bottle and Snipping
Container.
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SECTION VI
MEMBRANE FILTER DELAYED INCUBATION PROCEDURE
Introduction
Stations of the National Water Quality Network conduct the
initial steps in the delayed incubation membrane filter coliform
test. These consist of:
1. Sample collection,
2. sample filtration,
3« placement of the inoculated membrane filter upon
preservative medium,and
4. shipment to a National Water Quality Section Laboratory
of the Water Quality Network.
Sampling and Sample Holding Considerations
The sample for the bacteriological examination is to be
collected each week directly into a separate, clean,
sterilized glass-stoppered bottle(1) at the time that the
collections are made for the chemical and radiological samples.
The bottle should not be filled beyond 1/2 to 3/4- full in order
that the sample may be well shaken. Examinations will be made
by the membrane filter delayed incubation technique. Because
of the nature of bacterial organisms, it is very important that
the sample be filtered immediately, and that the membrane be
transferred to the holding medium and mailed to the Water
Quality Section as quickly as possible. Membranes shipped long
distances into a central laboratory after an undue delay has
occurred do not represent a true picture of the bacterial
populations present at the time of sample collection. Samples
mailed on Monday, Tuesday or Wednesday are desired. Samples
mailed on Thursday or Friday remain in shipment too long for
satisfactory analysis.
SUPPLIES AND EQUIPMENT
The Water Quality Section will provide the necessary
filtration equipment used for coliform density determinations
to those cooperating laboratories which do not already have
it on hand. All other related necessary supplies will also
be provided by the Section. The filtration apparatus and
shipping containers for the samples are shown in Figure 11 .
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The Water Quality Section will also provide, at intervals,
the supplies listed below for the membrane filter coliform
test. When the current supply of most or all of the items is
exhausted, return the shipping container with any unused
materials to the Water Quality Section. Do not hesitate to
notify the Water Quality Section when supplies are near
depletion.
Each shipping container forwarded periodically to the
cooperating laboratory will contain:
m-Endo Broth MF (dehydrated), 1/4 poun
Denatured alcohol (25 ml) 2 tubes
Sodium benzoate solution, 12% aqueous
(25 ml) — 2 tubes
Sterile plastic membrane filter containers 80
Sterile MF filters with absorbent pads
(10/pack)— —-• ,—.—.. . 8 packs
Phosphate buffer concentrate (20 ml) 2 tubes
Mailing cartons——•—• • 26 each
Addressed franked labels for cartons—• 26 each
Transmittal forms——-——— • 26 each
Preparation of Equipment and Reagents
The equipment for preparation of samples is listed below:
(3)
a. Filtration assembly unit consisting of metal funnelv'
and filter support base,
b» filter flask, 1000 ml capacity,
c. vacuum source (pump or aspirator),
d. sterile graduates or pipettes for measuring sample,
e. 99«0 ml .sterilized phosphate-buffered distilled water
blanks W,
f« three sterile membranes with three absorbent pads for
each sample to be examined,
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- 33 -
g. three sterile plastic membrane filter containers,
h. forceps immersed in pure ethyl alcohol,
i. medium (see below).
ra
<4
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Procedure for Sterilizing Equipment
a. Wrap funnel and filter base in kraft paper in separate
packages and sterilize in autoclave for 15 minutes at
121° C (15 psi). Cool to room temperature before use.
If an autoclave is not available, a bottle sterilizer
or pressure cooker of sufficient size may be used.
(For emergency use, in the absence of better sterilizing
facilities, immerse funnel and filter support base in
boiling water for five minutes. Remove the equipment,
cool to room temperature and place the assembly on
the filter flask and draw enough air through the
porous support disc of the filter base to remove
excess water.)
b. Membranes and absorbent pads are supplied by the Water
Quality Section. Both the membranes and pads are supplied
in sterilized packets in kraft paper and are ready for
use in the procedure. N
c. Sterilized plastic membrane filter containers are ready
for use.
d. Pipettes, sample bottles, graduates, and other equipment
should be properly protected by kraft paper and sterilized
at 1700 C in dry heat for two hours or by steam pressure
(autoclave for JO minutes at 121° C, 15 psi).
e. Sterilized, buffered, distilled water dilution blanks
are prepared by the addition, with shaking, of 1.2 ml
of phosphate buffer (supplied by Water Quality Section)
to 1000 ml of distilled waterC^. This is dispensed
in 99.0 ml aliquots, plus or minus 2.0 ml. The bottles
are autoclaved at 121 C/15 psi for 20-30 minutes. The
sterilizer is slowly cooled and/or slowly exhausted.
Caps or stoppers are loosened prior to sterilizing, and
tightened when bottles have cooled. (Bottles may be
filled with 90.0 ml, plus or minus 2.0 ml, if such is
preferred; the use of 9«0 ml dilution blanks is not
encouraged).(5)
Preparation of m-Endo Broth
a. m-Endo Broth-MF-Dehydrated (always use the latest
shipment of medium(2).
b. Sodium benzoate solution, 1.2% aqueous (supplied as
sterile stock solution in quantity to last six months).
• to 1000 ml of distilled water^^. This is dispensed
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- 35 -
c. Ethyl alcohol (ethanol or grain alcohol, U.S.P. grade,
95%).
d. Two sterile 1 ml pipettes.
e. Erlenmeyer flask, 125 or 250 ml.
Directions for preparation of m-Endo Preservative
Medium:
a. Place 50 ml heated distilled water in a sterile and
chemically clean 125 or 250 ml Erlenmeyer flask.
b. Add 1 ml ethyl alcohol.
c. Add with gentle agitation 2.4 grams dehydrated m-Endo
Broth ME.
d. Place the flask containing the distilled water, alcohol
and m-Endo MF medium in a beaker of boiling water until
the medium is dissolved (6). DO not heat the flask
over an open flame as this may cause some deterioration
of the medium if the solution is overheated (see
illustration, p. 36, „ figure 12. -
e. Cool to room temperature.
f. Add 1.6 ml of sodium benzoate solution and mix gently.
This is the finished medium and should be prepared
fresh for each week's Basic Data test. ^-7)
SAMPLE VOLUME AND FILTRATION
Successful examination of untreated water for coliform
density is dependent upon securing at least one membrane
with between 20 and 60 coliform colonies and with not more
than two or three hundred colonies of all types.
Development of colonies of non-coliform flora is generally
restricted, to a great extent, by the indicator in the medium,
but there are exceptions. A number of non-coliform colonies
may be present on the membrane, particularly where the water
sample is obtained from certain wells, lakes, and lagoons.
Sewage, on the other hand, will show few non-coliform colonies
via the m-Endo MF technique.
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36
Figure 12. Preparation of m-Endo Broth
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When there are no existing data on the coliform density
of a water sample, the quantities to be used for routine
sampling must "be determined "by a "trial and error" method.
In this instance, begin sampling operations by using sample
volumes of 0.01, 0.1, and 1.0 ml for the three dilutions.
In the delayed incubation membrane filter procedure, the
local laboratory does not see the finished membranes to
determine conformity with the above requirements. Therefore,
the Water Quality Laboratory completing the test will
immediately report to the local laboratory when any test is
unsatisfactory due to excessive colony density or insufficient
number of colonies, and when possible, recommend changes in
quantities of water to be filtered for the test. If the sample
is not subject to great weekly changes, the Public Health
Service will then recommend volumes of approximately (1st
membrane) 1/3 below and (3rd membrane)3«0 times above that
volume (2nd membrane) which yields a total of 20 coliform
colonies.
Filtration Procedure
The Delayed Incubation Membrane Filter Procedure (Tentative
Test) for coliforms is described on Pages 513-515 of Standard
Methods for the Examination of Water, Sewage and Industrial
Wastes, llth Edition, I960.The delayed test has many pr~
cedures in common with the immediate test; Pages 508-513?
and special reference is made to the illustration, "Fig. 20,
Membrane Filter Assembly" and discussion of paragraph 1.6,
page 510 (llth Ed.), for a typical assembly of membrane
filtration equipment. The filtration of the sample after
the equipment has been assembled is as follows:
a. Place absorbent pads in bottom of sterile plastic con-
tainers.
b. Saturate each pad with benzoated m-Endo MF broth and
remove any excessive medium from pads by draining
the plates gently.
c. Flame forceps and place sterile membrane (grid side
up) in filter receptacle and seal funnel on membrane
with care in order to avoid tearing or creasing the
membrane.
d. Shake sample vigorously at least 25 times.
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- 38 -
e. Measure water sample v ' in funnel with no vacuum on
filter flask.
1. If volume of sample is 10 ml or more, transfer
measured sample directly onto dry membrane.
2. If between 1.0 ml and 10 ml, pour about 20 ml of
sterilized buffered distilled water into the
funnel before transferring the measured sample
onto the membrane. This facilitates good dis-
tribution of organisms.
3- If the volume of original water sample is less
than 1.0 ml, prepare appropriate dilutions and
proceed as in item 2.
Never pipette directly less than 1.0 ml; bacterial
distribution is unsatisfactory if this is done !
4-. Diluted samples should be filtered within 20
minutes of preparation because bacterial die-off
is detectable after 30 minutes of holding at
room temperature.
For required dilutions, the shaken sample should
be added to the dilution bottle in the following
amounts :
Dilution Vol. Sample Vol. Dilution Water
1:10
1:100
1:1,000
1:10,000
10.0 ml
1.0 ml
10.0 ml of 1:100
1.0 ml of 1:100
90.0 ml in bottle
99.0 ml in bottle
90.0 ml in bottle
99.0 ml in bottle
After the sample is added to the bottle, the bottle
is then closed tightly and shaken vigorously at least
25 times.
f. Turn on vacuum and filter sample.
g. Rinse sides of funnel down twice with at least 20 ml
of sterile buffered distilled water each time,
keeping vacuum on.
h. Remove funnel from receptacle and place on sterile paper,
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0
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Id =!
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- 4-0 -
i. Flame the forceps* Using the forceps, remove the
membrane from the filter base and lay it on the soaked
absorbent pad in the plastic container, grid side lift,
with a rolling action at one edge, as shown in Figure
14. Use gaare to avoid tapping air bubbles under the
membrane.
j. Place top of container gently over bottom and proceed
with filtration of next volume of water. All three
quantities in aacending order of volume can be
filtered in same funnel apparatus with only the
rinsing (described in "g'O between dilutions. When
using descending orders of volume, or when changing
to samples of an unknown degree of pollution, the
funnel must always be rinsed between filtrations.
k. Let membrane stand for about 5 minutes,
1, Inspect each transferred membrane for the presence
of colorless spots under its surface; these indicate
the presence of air bubbles.
m. If the membrane does not have a uniform pink color,
remove' with forceps and roll onto absorbent pad again.
n. Seal the plastic container by pressing top firmly on.
SHIPPING
a. Mark the top of each container with the station name
or code number, the sample number and the volume of
sample. A marking pen is provided for this purpose.
The sample number should correspond to the appropriate
number on the sample *s» transmittal sheet. The trans-
mittal sheet should show clearly the volume sampled,
or preferably, the dilution prepared and volume of
that dilution which was used. (See sample forms on
page 44-. Do not mail membrane samples on Thursday
or Friday since these samples are held by the Post
Office over Saturday and Sunday before delivery to
the Central Laboratory. A 72 hour delay causes un-
reliable results.
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Figure 14- . Placing Membrane on Pad Soaked with Preservative
Medium.
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- 42 -
NOTES
1. The sample of water should come into contact with no
holding vessel other than the sterilized glass container;
the raw sample is placed directly into the glass "bottle.
2. The dehydrated medium will be supplied in quarter pound
jars to those stations which have available a balance
with sensitivity of _+_ 0.1 gram.
If no balance is available, the medium can be supplied
by the Public Health Service in small vials containing
2.4/ grams each.
The dehydrated medium will absorb moisture rapidly which
results in caking and spoiling the powder. The gar
containing the dehydrated stock medium must be sealed
tightly each time after using to prevent absorption of
atmospheric moisture.
3. Eventually, through use, the fixed nylon locking wheels
of the metal funnel will develop localized flat areas.
As a result, the filtration apparatus may leak. This
can be relieved by using the small Allen wrench supplied
with the filtration apparatus to loosen the set screw.
The screw may then be loosened and the wheel rotated to
an unused bearing surface. The screw again is tightened
and the set screw drawn against it.
Do not attempt to sterilize the metal funnel in a drying
oven because the dry heat may damage the nylon locking
wheels.
The filtration apparatus should be cleaned by rinsing
with tap water or with detergent and a brush, followed
by a thorough rinse, and a final wipe with a clean,
lint-free clothe Never use scouring powder, steel
wool, or an acid cleaning treatment.
Following considerable use of the stainless filtration
apparatus, areas of exposed copper may develop, particularly
around the throat of the filtration apparatus. If exposed
areas are visible, the filtration apparatus should be
returned. A new one will be sent immediately to replace
the old one.
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- 45 -
4. If the distilled water used for dilutions and funnel
rinsings come in any contact with copper or zinc, please
notify us.
5. The dilution bottles holding the phosphate buffered dis-
tilled water should "be of heat-resistant glass. Rubber
stoppers and liners of screw caps should contain no
toxic, heat-releasable component. Specialized-usage
white liners and stoppers are preferred.
6. A small amount of grayish-black powder may remain in the
bottom of the flask after the bulk of the m-Endo MF
medium has gone into solution. This is a common
occurrence and may be ignored.
7« For stations which desire to run the immediate MF test,
the quantities can be doubled, medium divided into two
50 ml portions in step (5) and 1.6 ml of sodium benzoate
solution added to one portion. The portion without
added sodium benzoate can be used as a single step
procedure for the immediate MF test. (Fifield, C.W.
and C.P. Schaufus, JAWWA 1958: 50: 193-196.)
8. If water sample to be filtered is:
Over 20 ml, use appropriate sterile graduate.
Between 2-20 ml, use 10 ml or 20 ml sterile pipette.
Between 1.0 - 2.0 ml, use 1 or 2 ml graduated sterile
pipette-
Less than 1.0 ml, make appropriate dilutions in
sterilized buffered distilled water and use an
appropriate sterilized pipette.
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- 44 -
DEPARTMENT OF HEALTH, EDUCATION AND WELFARE
PUBLIC HEALTH SERVICE
1014 Broadway, Cincinnati 2, Ohio
DELAYED INCUBATION TEST
DATE COLLECTION JULY 1, 1965
STATION NO. 225
TIME OF SAMPLE COLLECTION 0800 BY JOHN JONES
DATE FILTRATION JULY 7, 1965
TIME OF SAMPLE FILTRATION 083° BY TOM WILSON
SAMPLE POINT LOCATION WINDING RIVER AT MILLVALE, OHIO
•RECEIVED W.Q.S. DATE 'TIME "ELAPSED TIME HOURS
LOCATION OF PLANT OR LABORATORY EASTERN MILLVALE SEWAGE TREATMENT
COLIFORH
PLANT
MLS
UNDI LUTED
2.0
, ULV0
DILUTION
2.0
6.0
CONT A 1 NE N
SEft| ES
NO .
/ *
2
3
— . . ,_»,._
wos
•LABORATORY
NUM8I 0
•COLIFORM
COLONY COUNT
•COLI FORMS
PER IOO ML .
REMARKS
f
1.0
4.0 of
1:100
2,O of
/.' 10
4 **
8
C
H ' "
•FOB iMt or WAT
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- 45 -
SECTION VII
CHEMICAL AND PHYSICAL ANALYSES
PRELIMINARY REMARKS
Samples taken for chemical and physical analyses should
"be representative of the raw water in the river. A large
enough sample should be collected to satisfy the requirements
for the chemical analyses to be performed. A special sampling
technique will be required for the dissolved oxygen (DO) and
biochemical oxygen demand (BOD) determinations and will be
described under these tests- The collected sample should be
kept in a closed container except when portions are withdrawn
for the various analyses,. A 2-liter bottle of pyrex or
polyethylene will be satisfactory for a container.
Detailed procedures are presented below for the chemical
and physical analyses of the raw water sample. In most
instances the methods described follow closely the procedures
in Standard Methods for the Examination of Water. Sewage, and
Industrial Wastes (10th Ed.. 1955: llth Ed.. 1960J.For the
sake of uniformity, it is suggested that these procedures be
used by all the cooperating laboratories in the National
Water Quality Network. The laboratories have a free choice,
however, in using any procedure found to be satisfactory,
provided its precision and accuracy are within normally
accepted limits. The Reference Samples, as sent out periodi-
cally by the Water Quality Section, will be one of the tools
by which the precision and accuracy of the various analytical
methods in use will be measured.
The procedures outlined in the following pages are in
the same order as they appear on the Report Form (Form PHS
2845-1, Rev. 6-59). Those determinations numbered 1 through
8 should be performed as soon as possible after the sample
is collected. This group includes: (1) Temperature, (2; dis-
solved oxygen (DO), (J) pH, (4) biochemical oxygen demand (BOD),
(5) chemical oxygen demand (COD), (6) chlorine demand, 1 hour,
(7) chlorine demand, 24- hours, and (8) ammonia nitrogen,
NHj/N, These tests should be performed,as far as possible,
by the cooperating agency; the data, cannot.otherwise be
obtained.
Since many of the cooperating agencies in the Network
perform all the required determinations, the outlined proced-
ures for tests 9 through 16 are also included,, These tests
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4-6
are specifically: (9) Chlorides, (10) alkalinity, (11) total
hardness, (12) color, (13) turbidity, (14) sulfates, (15) phos-
phates, and (16) total dissolved solids, and are included
for convenient reference, For those agencies with limited
analytical facilities, arrangements can be made to have the
9 to 16 group performed in the Water Quality Section
Laboratory. (See Section II, General Instructions, para-
graphs a & b).
In general, in the procedures that follow, the standard-
ization of reagents is not described. Many of these reagents
are procurable as standard solutions from reliable supply
houses. Those that cannot be easily obtained will be provided
to participants, upon request, by the Water Quality Section.
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TEMPEEATUBE (Standard Methods, llth Ed,, p. 2?0)
Accurate temperature readings are necessary for calculating
dissolved oxygen saturation values, for correlation of "biologi-
cal activity, and for many other purposes.
The temperature to "be reported should "be representative
of the temperature of the stream at the time the sample is
collected. The temperature must, therefore, "be taken at the
sampling point. The thermometer should be immersed in the
flowing stream, or in a large sample container filled with
the sample, and held until the mercury is at rest. The
temperature should then "be read before removing the thermo-
meter from the sample.
Record the temperature to the nearest fraction of a
degree Centigrade, which can be estimated from the thermo-
meter being used.
If Fahrenheit thermometer is used, convert readings to
Centigrade as follows:
Subtract 32 from the Fahrenheit reading,
multiply the results by 10 and divide by 18.
If there is a doubt as to the accuracy of the thermometer
being used, it may be sent to the Water Quality Section to
be checked against a Bureau of Standards thermometer.
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- 48 -
DISSOLVED OXYGEN (DO)
1. Collection of Sample. Whenever possible, samples
should be taken from the stream. A sampling device
should be used that provides for at least three
volumes of water to pass through the DO sampling
bottle without aeration by the atmosphere. The
device may contain two bottles, in which case the
second bottle may be incubated for the BOD. At
least 1 liter of water, in a separate container,
should be collected at the same time the DO samples
are taken. It may be needed for the BOD test, if
conditions for this test, listed under the BOD
instructions, are violated* It can also be used for
the other physical and chemical determinations. River
temperature should be recorded at the time the DO
sample is taken*
If a source of raw river water, under pressure,
is available, and it has been determined that there
is no aeration from pumping, and that no treatment
of the water has occurred ahead of the sampling point,
then this source may be used as a satisfactory samp-
ling point, but only if direct sampling from the
stream is impractical.
2. Sampling Apparatus.
2.1 Standard JOO-ml BOD bottles.
2.2 DO sampler (see p. 251, Standard Methods, 10th
Ed., or p. 308, llth Ed., for illustration).
The Water Quality Section can provide this
sampling device upon request.
3. Sampling Procedure.
3.1 Sampling from the stream;
a. Place 2 DO bottles in sampler.
b. Immerse sampler in stream to the necessary
depth (about one-half the depth at sample
point) and hold until bubbling stops before
lifting out,
c. Carefully lift off the top, taking precautions
to prevent contents of the bottle from coming
in contact with air.
d. Stopper the bottles carefully to avoid air
entrapment under the stopper.
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- 49 -
3.2 Sampling from raw water under pressure; this
procedure may be used only if it is known that
the raw water is not "being aerated during the
•pumping, and no water treatment has occurred
ahead of the point at which the sample is"
collected.
a. Place a rubber or.glass tube from the raw
water line into the bottom of a BOD bottle.
bo Hun the water into the bottle until it is
full and allow it to overflow two or three
times its volume.
c. Slowly withdraw the sampling tube while the
water is still running.
d. Carefully stopper the sample bottle, pre-
venting any air from being entrapped.
e. Repeat with the second sample bottle.
4. Reagents.
4.1 Manganous sulfate solution. Use any one of the
following compounds:
a. MnS04!4H20, 480 g
b. MnS04*2H20, 400 g
. c. MnS04'H20, 364 g
Dissolve in distilled water and make up to 1
liter.
4.2 Alkaline iodide - azide solution.
Dissolve 500 g sodium hydroxide (NaOH),
135 g sodium iodide (Nal),
10 g sodium azide (NaN,)
all together in distilled water. Make up to
1 liter.
4.3 Concentrated sulfuric acid - reagent grade.
4.4 Standard bi-iodate solution.* Weightout 0.8124 g
of potassium bi-iodate and dissolve in 1:,,liter
of water. This must be done carefully. The
accuracy of the DO test depends on the care with
which this solution is prepared.
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- 50 -
4.5 Starch solution.
a. Make a paste of about 5 to 6 g potato,
arrowroot, or soluble starch in a small
quantity of water.
b. Add it to about 1 liter of boiling distilled
water and boil a few minutes.
GO Cool, allow to stand overnight.
dc Pour off and save the clear solution,
e. Add a few drops of toluene as a preservative.
4.6 Standard thiosulfate solution.
a. Stock solution - l.ON.
a.l Dissolve 248 g NapSpO-,°5HpO (reagent
grade) in freshly boiled and cooled
distilled water. Dilute to 1 liter,
a.2 Add 5 ml chloroform or 1 g sodium
hydroxide as a preservative.
b. Titrating solution - 0.025N.
Dilute 25«0 ml of the stock solution with
distilled water to 1.0 liter. Add preserva-
tive as above,
4,7 Standardization of titrating solution 4.6b,
a« Dissolve about 2 g sodium or potassium iodide
in 100 to 150 ml distilled water.
b. Dilute 1 ml of concentrated sulfuric acid to
10 ml with distilled water and add this to
the iodide solution,,
c» Add jgxactly_ 20,0 ml of standard bi-iodate
solution,
d. Dilute to 200 ml and titrate with 0025N
J j »sulfurio-aoid until a pale yellow color is
reached.
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- 51 -
ML DISTILLED WATER TO ADD TO 100 ML OF REAGENT 4.6b
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ML OF 1.0 NORMAL THIOSULFATE TO ADD TO 100 ML
OF REAGENT 4.6b
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Add starch solution and continue the titra-
tion carefully to the disappearance of
blue color. If the 0.025N oulfuri-cr%a^4^is'
of proper strength, it should take
20.0 ml to reach the endpoiht..
Adjust this reagent, either with l
&ulf uric —aej^b or distilled water until its
strength matches that of the 0.025N bi-
iodate solution.,
Recheck this solution once a week and adjust
to proper strength.
5» Procedure.,
5.1 Add 2 ml of manganous sulfate followed by 2 ml
of alkaline iodide to the DO sample. Take care
to add these reagents with the tip of the
pipette below the water surface. Carefully
stopper and mix vigorously. DO' not allow air
to be entrapped below the stopper.
5.2 Let stand for 2 to 3 minutes and repeat the
mixing, then let stand until the precipitate
in the bottle has settled at least half way.
5.3 Add 2 ml of concentrated sulfuric acid and
stopper carefully to prevent air bubbles from
entering the bottle . Rinse the outside of the
bottle with tap water \ mix thoroughly as
before.
5<>4- Remove 204- ml of treated sample and transfer to
a 500 ml Erlenmeyer flask.
5.5 Titrate with 0.025N sodium thiosulfate until a
pale yellow color is reached.
5.6 Add approximately 5 ml of starch solution and
carefully continue the titration to the disap-
pearance of the blue color.
5.7 Record the titration.
5.8 Add 1 drop of 0.025N bi-iodate solution. This
should bring back the blue color. If more than
one drop is necessary, count the drops and sub-
tract 0.05 ml from the titration for each drop
in excess of one.
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• 6. Calculation. If the 0.025N sodium thiosulfate is of
proper strength, the volume added in the titration
I above gives the DO value directly in mg/l« Record
to the first decimal.
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HYDROGEN ION CONCENTRATION (pH) (Standard Methods, llth Ed.,
p. 193)
pH can be measured either colorimetrically or with a
pH meter. The later measurement is preferred, though
colorimetric measurement is acceptable if a pH meter is
not available.
1. Collectionof Sample. Use the raw water sample
collected for the mineral analyses.
2. Apparatus.
a. Commercial pH meter, or
b. commercial color comparator.
3. Reagents.
3.1 Buffer, pH 4:
Dissolve 10.2 g anhydrous potassium biphthalate
in boiled and cooled distilled water. Dilute
to 1 liter.
3.2 Buffer, pH 7:
Dissolve la361 g anhydrous potassium dihydrogen
phosphate and 1.420 g anhydrous disodium hydrogen
phosphate in boiled and cooled distilled water.
Dilute to 1 liter.
3.3 Buffer, pH 9:
Dissolve 3.81 g sodium tetraborate decahydrate
(borax) in boiled and cooled distilled water.
4. Procedure., Follow the recommended procedure of the
instrument manufacturer.
5o Results. Report to the nearest 0,1 pH unit.
6. Precautions.
6.1 pH meter.
Be sure that electrodes are clean, the glass
electrode is not cracked or scratched, the
calomel electrode contains saturated potassium
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chloride solution and its liquid junction (the
tip) is not plugged. Remove the rubber stopper
on the calomel electrode before use to permit
flow of the electrolyte through the tip. When
calibrating the instrument use the buffers
which will bracket the pH value of the sample.
6.2 Commercial comparators.
Comparator tubes should be matched,both as to
size and color of glass. Be sure that the
light passing through the comparator tubes is
of equal intensity. If pH reading of sample
is at either extreme of the indicator range,
check with the next indicator in the series
available before reporting pH value. If
indicator solution becomes turbid, replace
with fresh indicator.
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- 56 -
BIOCHEMICAL OXYGEN DEMAND (BOD)
1. Collection of Sample. Collect at least 1 liter of
water at the same time tiie DO samples are collected,
The water in the DO sampler may "be saved for this
purpose.
2. Procedure.
2.1 Determine the DO on one of the samples collected
for this purpose.
a. If the DO value is between 9«2 and 6.9 mg/1,
place the duplicate DO sample in the 20°C
incubator and incubate for 5 days. Be
careful to maintain the water seal on the
sample during the incubation period, then
proceed with 2.6 below.
b. If the DO value is above 9«2 or below 6.9,
discard the duplicate DO sample, and proceed
with 2.2 below.
2o2 Place about 1/2 gallon of the water collected
at the time the DO sample was taken in a
1-gallon jug. Let it stand (or warm it) in
the laboratory until it reaches room temperature.
2.J Stopper the Jug and shake the sample vigorously
to bring it to saturation with atmospheric
oxygen. During the shaking, the stopper should
be removed several times to allow the transfer
of oxygen. Siphon it carefully into duplicate
DO bottles.
2o4- Determine the initial DO on one bottle.
2.5 Incubate the other bottle for 5 days, as in
2,la above.
2.6 After 5 days of incubation determine the DO
on the incubated sample.
3. Calculation. Calculate BOD as follows:
Initial DO - Final DO = mg/1 BOD
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Note; In the event that the final DO is zero, the
BOD reported should be indicated as "greater than"0
If zero DO in the incubated bottle recurs frequently,
it will become necessary to set up dilutions of
the original sample„ Should this be necessary, follow
the instructions in Standard Methods for the prepara-
tion of BOD dilutionso
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- 58 -
CHEMICAL OXYGEN DEMAND (COD) (Reduced Strength Procedure
for River Waters)
lo Collection of Sample. Use the raw water collected
for BOD analyses (see Section II, page 8. paragraph
f)o
2. Apparatus. Every precaution should "be taken to insure
that the sample "bottles and other equipment used in
this test are clean and free from organic matter.
2.1 Reflux condenser, Friedrichs (Corning #2600),
with ground glass standard taper joint 24/40.
2.2 Erlenmeyer flask,500ml(Corning 5000) with ground
glass neck to fit the condenser; standard taper
24/40„
3. Reagents
3.1 Sulfuric acid, concentrated (reagent grade).
3.2 Ferroin indicator solution.
Dissolve 1.485 g of 1, 10-phenanthroline, with
0.695 6 ferrous sulfate*7HpO in water and
dilute to 100 ml.
3<>3 Standard potassium dichromate.
Dissolve 12.2588 g of potassium dichromate
I a. Dissolve l; ^ . ^ _
(K2Cr2t!^), previously dried at 103 °G for
2 hours, in distilled water and dilute to 1
liter. This is the stock solution 0.25 N.
bo Carefully measure 100.0 ml of the stock
solution into a 1-liter volumetric flask.
Dilute to 1.0 liter with distilled water.
This is the working solution - 0.025 N.
3.4 Standard ferrous ammonium sulfate (referred
to hereafter as FAS).
a. Dissolve 98 g FAS-6H?0 in distilled water.
Add 20 ml concentrated sulfuric acid,
reagent 3°1« Cool. Dilute to 1 liter.
This is the stock solution.
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- 59 -
"b« Place 100 ml of the stock solution in a
1-liter volumetric flask. Carefully add
20 ml of concentrated sulfuric acid. Cool.
Dilute to 1 liter. This is the working
solution. It is approximately 00025 W
and must "be standardized each time before
use by the following procedure.
4. Standardization of FAS (Reagent 3.4b).
4«1 Take 25.0 ml of 0.025 N potassium dichromate
and add to about 300 ml of distilled water in
a flask.
4.2 Add 50.0 ml of concentrated sulfuric acid care-
fully . Allow to cool.
4.J Add 8 to 10 drops of ferroin indicator.
4.4 Titrate with IAS (reagent 3<,4b) to a deep red
color. This is a sharp end point if the sample
has been cooled properly before adding the
indicator.
5. Calculating the Normality of FAS;
Normality = ml potassium dichromate X 0.025
6. Procedure for COD,
6,1 Take 50.0 ml of the well-mixed sample and add
it to the sample flasko
6.2 Add exactly 25.0 ml of 0.025 N potassium dichromate,
6.3 Carefully and with thorough mixing, add 75 ml of
concentrated sulfuric acid.
6.4 Add 8 to 10 clean glass beads or porcelain chips.
Attach the flask to the condenser, place over
the burner or hot plate and maintain at gently
boiling temperature for 2 hours.
CAUTION; Before applying heat, be sure that
the acid has been thoroughly mixed
in the flat -bottom flask and that
the condenser water has been turned
on.
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6.5 Cool. Wash down the condenser with about 25 nil
of distilled water, then transfer, with thorough
rinsing, to the titration flask. Dilute to
about 350 ml with distilled water.
6.6 Add 8 to 10 drops of ferroin indicator to the
cooled sample.
6.7 Titrate with FAS (reagent 3»4-b) to the red end
point.
6.8 If no dichromate remains, as indicated by an
immediate red color that occurs when ferroin
indicator is added, the test must be rerun
with a lesser quantity of sample. Repeat the
test with 25.0 ml of sample plus 25.0 ml of
distilled water.
?• Calculation of COD.
7«1 Dichromate consumed by digestions
/ml FAS X normality of FAS\
=» ml dichromate consumed.
7,2 al a-i<*romate consumed x = Qross Demando
ml sample
7°3 Correction for chloride;
mg/1 chloride in sample X Oo2J = chloride correction
7»4- Subtract result in 7° 3 from Gross Demand and
report as COD to the nearest mg/l0
8. COD Samples for WQS. Space has been provided in the
carbon filter shipping container to simplify for-
warding of this sample, as shown in Figure 1, page
l^r« It will be necessary, therefore, to schedule
the collection of this sample for the second week
of the month. This is necessary to avoid errors
owing to prolonged storage of COD samples. Add 50 ml
of the sample collected for the weekly mineral
analyses to the sample bottle in the carbon filter
box. Fill out the attached tag and replace in the
carbon filter shipping container. This bottle
already contains acido Do not rinse out or spill
any of it. Do not send this sample separately by
mail.
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- 61
CHLORINE DEMAND (Standard Methods, 10th Ed0, p. 63, llth Ed.
P. 83)
The results of the chlorine demand test are dependent
to a considerable degree on the procedures and techniques
used. Although there are a number of methods used for
the evaluation of chlorine demand of water, a uniform
procedure must be used when comparisons among several stations
are desired. To demonstrate changes within a river basin, each
laboratory must, therefore, use the identical test procedure.
For this reason, the procedure described below is the only
one that should be used in reporting chlorine demand results
to the Network,,
1. Collection of Sample. Use raw water collected for
the mineral analyses". You may need several liters;
be sure to collect enough water for all the tests.
2» Apparatus. About 6 to 10 clean, quart-size bottles
or flasks.
3o Reagentso
3.1 Sulfuric acid (reagent grade) 20 ml per liter.
Add 20 ml of concentrated sulfuric acid to
approximately 750 ml distilled water. Dilute
to 1 liter.
3o2 Potassium iodide, (crystals) reagent grade.
3.3 Starch solution (see DO instructions, page 50).
3o4 Sodium thiosulfate - 0.025 N (see DO instructions,
use reagent-f06b,page 50 ).
3»5 Chlorine solution (500 mg/l)0
a. Stock solution - a bottle of clorox contains
approximately 5 percent chlorine (50,000
mg/1).
b. Working solution (500 mg/l)0
Take 10 ml of (a) and dilute to 1 liter.
4. Standardizing the Chlorine Solution (Reagent 3<>5h)°
4.1 Add about 500 ml of distilled water to a
titrating flask or bottle.
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4-0 2 Add 3 to 4- crystals of potassium iodide.
4-o 3 Add 10 ml sulfuric acido
•
4-. 4- Measure accurately 25 »0 ml of chlorine working
_ solution (reagent 3<>5b) and add to the flask,
• swirling rapidly during the addition,,
4-o 5 Titrate with sodium thiosulfate to a pale yellow „
406 Add 5 to 10 ml of starch solution.
4-c, 7 Titrate carefully to the disappearance of the
blue color, adding the reagent dropwise.
I
_ 5« Calculating the Strength of Chlorine Working Solution
I (.Reagent 3.5^ J ;"
mg 01. per ml of working solution - ml of ^ioeulfate X 0.025
Ic- •&• pf? <>y
ml of working solution taken
6. Procedure for Chlorine Demand.
• 6.1 Measure out 500 ml of sample into each of 6 to
10 flasks or "bottles.
| 6.2 Add 1, 2, 3» 4-, etc. ml of working solution to
the respective samples. These should now contain
_ approximately 1, 2, 3S 4-, etc. mg/1 chlorine.
603 Set aside at room temperature in the dark for 1
hour0
• 604- After 1 hour, take the first flask and add three
or four crystals of potassium iodide.
I 605 Add 10 ml sulfuric acid solution.
_ 6.6 Add 5 to 10 ml of starch solution.
™ If blue color is observed, titrate with sodium
thiosulfate carefully to the end point. If no
•blue color is observed, repeat with the second
flask, etc.
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7» Calculation of Chlorine Residual.
7.1 Calculate the chlorine residual in the first
flask showing a blue color as follows :
mg/1 C12 residual - ml o* thiosulf ate002 X . X 1000
When the normality of the thiosulfate is exactly
0.025 and the sample size is 500 ml, this is
simplified to:
mg/1 C12 residual = ml thiosulfate X 1.78
7»2 If chlorine residual is less than 1 mg/1, repeat
the titration with the next sample in the series .
Continue until you find the first one having a
residual greater than 1«,0 mg/1 „
7.5 Hold the remaining samples 24- hours, then repeat
the titration on all of the remaining samples.
8. Calculation of Chlorine Demand.
8.1 One-hour demand „
a. Calculate the chlorine added to the first
sample that showed a residual greater than
1 mg/1 as follows :
ml chlorine working solution added X mg Cl0/ml X 2 = mg/1
C12 added d
b» Subtract the chlorine residual that was
determined for this sample. The result is
the 1-hour demand „
8.2 Twenty-four hour demand 0
a. Following the titration in paragraph 7*3
calculate the chlorine residual for each
of the remaining flasks, as in 'paragraph 7-l«
b. If your water has a breakpoint you will
notice that the chlorine residuals will
rise, then fall, then rise again1 as the
remaining samples are titrated. For
calculating the 24-- hour demand, use the
first sample having a residual above 1 ppm
after the second rise (breakpoint),,
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c. If your water lias no breakpoint, calculate
I the demand on the first sample having a
residual above 1 ppnu
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- 65 -
AMMONIA NITKOGEN (Standard Methods, llth Ed0, p6 16?)
The distillation procedure is most accurate when inter-
ferences are known to be present, and should be used if
equipment is available. In the absence of distillation
apparatus, the direct procedure can be used and should be
satisfactory for most surface waters of the Network,, It is
described below0
1. Sample Collection* Use the raw water collected for
the mineral analyses0
2<, Apparatuso
2,1 Spectrophotometer or filter photometer, or
2.2 a Nessler tube series of permanent color
standards as specified on p« 14-6, Standard
Methods, 10th Ed,, or p. 172, llth Ed., or
2,3 permanent standards for ammonia nitrogen, as
provided with commercial comparators.
5° Reagents.
3.1 Ammonia-free water«
a0 Treat distilled water by storage in a
"Quickpure" demineralizer for about 20
minutes (distributed by E0 H. Sargent &
Co., Cat. #S-2?810).
b. Pass distilled water through a column of
mixed resin such as Amberlite Mb-1, or
c0 add about 10 g of Eolin's ammonia permutit
to 1 gallon of distilled water and shake.
3<>2 Nessler reagent.
a0 Dissolve 100 g anhydrous mercuric iodide
and 70 g anhydrous potassium iodide in
about 50 to 100 ml of ammonia-free water.
b. Prepare a solution of 160 g sodium hydroxide
in 500 ml water. Cool.
Add the first solution (a) to (b) slowly
with stirring* Dilute to 1 liter with
ammonia-free water and store, well stoppered,
in pyrex.
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3.3 Standard ammonium chloride solution,
a. Prepare a stock solution by dissolving 3-819 g
anhydrous ammonium chloride in ammonia free
water, dilute to 1 liter. One ml of this
solution is equivalent to 1.00 mg of ammonia
nitrogen.
b. Dilute 10.0 ml of (a) to 1 liter with
ammonia-free water. One ml of this solution
is equivalent to 0.01 mg of ammonia nitrogen*
3.4 Bochelle salt solution.
Dissolve 500 g of potassium sodium tartrate in
1 liter distilled water. Boil off about 200 ml.
Cool. Dilute to 1 liter with ammonia-free water.
3.5 Zinc sulfate solution.
Dissolve 100 g zinc sulfate in ammonia-free
water. Dilute to 1 liter,
3.6 Sodium hydroxide.
Dissolve about 250 g sodium hydroxide in ammonia -
free water and dilute to 1 liter.
4. Procedure.
4.1 Take 100 ml of raw water sample* Add 1 ml of
zinc sulfate solution, and mix.
4.2 Add about 0.5 ml of sodium hydroxide solution.
The pH should be about 10.5 by test. Mix
thoroughly and allow the floe to settle.
4.3 Decant about 25 ml of supernatant through filter
paper and discard.
Collect the next 50 ml of filtrate (or aliquot
diluted with ammonia-free water) in 50 ml
Nessler tubes and add 1 to 2 drops of Eochelle
salt solution.
4.4 Add 1.0 ml Nessler reagent and mix by inverting
the tube. Allow to stand 10 minutes.
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- 6? -
4,5 Compare with standards or read in spectrophoto-
meter set at 400 to 425 wave lengttu
a0 Calibration curve and control test.
Prepare a calibration curve using increasing
quantities of standard ammonium chloride
solution, into 50 ml of ammonia-free water,
and carry out the Nesslerization as in steps
4.1 through 4.4. Run a known ammonia sample
concurrently with the raw river water when-
ever the quality of the Nessler reagent is
under suspicion.
5» Calculation.
Determine the concentration of ammonia nitrogen from
the spectrophotometer curve, or by comparison with
standards. Multiply by the dilution factor, if a
dilution was made, and report as mg/1 ammonia
nitrogen, to the nearest tenth.
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CHLORIDES (Standard Methods, llth Ed., p. ?9)
Three satisfactory methods are described in Standard
Methods. The mercuric nitrate method, detailed below,is
the one currently used by many laboratories «
1. Collection of Sample. Use raw sample for the mineral
analyses.
2° Apparatus. Conventional titrating equipment.
3. Reagents.
3.1 Standard sodium chloride solution, 0.0141 Ne
Dissolve 8.243 g NaCl in approximately 250 ml of
distilled water and dilute to exactly 500 ml.
Dilute 50.0 ml to 1.00 liter. Each ml contains
Oo500 mg Clo
3o2 Standard mercuric nitrate solution, 000141 N.
Dissolve 2.3 g of Hg(N03)2°2H20 in 100 ml of
distilled water containing 0.25 ml of concen-
trated HNO^. Dilute to just under 1 liter and
standardize against the 0.0141N sodium chloride
solution using the procedure described below
for samples. Adjust the mercuric nitrate
solution to exactly 0.0141 N and perform a
final standardization. Store away from the
light in a dark bottle. Standard mercuric
nitrate, 0,0141 N is equivalent to 0.500 mg
Cl per 1.00 ml.
3°3 Mixed indicator solution: Dissolve 0.5 g of
diphenylcarbazone and 0005 g of bromphenol blue
in 100 ml of 95 percent ethyl alcohol. Store in
a brown bottle.
3°4 Nitric acid solutions 0.2 N. Dilute 12.9 ml of
concentrated HNO^ to 1 liter.
4. Procedure.
4.1 Use a 100 ml sample, or an aliquot diluted to
100 ml containing less than 10 mg of chloride.
4.2 Add 10 drops of the mixed indicator solution to
the saiuplc.
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1 - 69.
• 4-o3 Add 002 N nitric acid dropwise to the sample
until the color becomes a definite yellow
• (approximately pH 3°6)0 Add 5 drops more.,
4o4 Titrate with 0.0141 N mercuric nitrate solution
_ to the first permanent tinge of violet0
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A mg/1 chloride = ml of mercuric nitrate X N of mercuric nitrate
X 35»4-6 X 1000
""""_ :_^ ml of sample
Note; If mercuric nitrate is exactly 000141 N, and if a
100-ml sample is used, this formula becomes:
mg/1 chloride = ml of mercuric nitrate X 5°
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ML OF DISTILLED WATER TO ADD TO 100.0 ML OF MERCURIC NITRATE
ML OF 0.141 N MERCURIC NITRATE TO ADD TO 100.0 OF MERCURIC NITRATE
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TOTAL ALKALINITY (Standard Methods, llth Ed., p. 44)
I 1. Collection of Sample. Use the raw water sample
collected from the mineral analyses.
V 2. Apparatus. Conventional titration equipment.
3. Reagents.
| 3.1 Standard sulfuric acid, 0.0200 N.
— 3.2 Indicator solution.
* a. Methyl purple - obtainable from Fleisher
Chemical Co., Ben Franklin Station, Washington
m 4, D. c.
b. If a pH meter is available with extended leads
§it can be used as the indicator, with endpoint
taken at pH 4.6»
4. Procedure.
4.1 Place 50 to 100 ml sample into an Erlenmeyer flask
or porcelain dish.
• 4.2 Add 2 to 4 drops indicator.
m 4.3 Titrate with 0.0200 N sulfuric acid to the endpoint,
5« Calculation; (Total alkalinity as calcium carbonate,
mg/i;
™ mg/1 Alkalinity _ ml standard acid X 1OOO
(as CaCOx) ~ ™~ml sample
I5
Note: Other indicators are available but methyl purple is
recommended for clarity of its color change.
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TOTAL HARDNESS (Standard Methods, llth Eda , p0 132)
Universal acceptance of the complexometric (EDTA) procedure
for hardness has practically eliminated the soap procedure for
this test° Standard Methods described several alternative
methods„ The procedure outlined "below has been found to be
the most used, but the others described are equally useful and
may be substituted if desiredo
lo Collection of Sample, Use the raw water collected
for the mineral analyses <>
2» Apparatuso Standard titration equipment,,
3° Reagent So
3ol Eriochrome Black T - dry mixture»
Weigh out 1 gram of indicator and thoroughly
mix with 250 g of dry sodium chloride crystals.,
Keep dry and well stoppered,,
3° 2 Buffer solution..
Take 150 ml of concentrated ammonium hydroxide,
add 17 g ammonium chloride,
dilute to 250 ml
keep well stoppered
3»3 Inhibitor solution,,
If an endpoint is not readily obtainable, it may
be due to interference from heavy metals„ (See
p« 11.5 of Standard Methods, 10th Edo, or p» 134,
llth Edo, for the preparation of inhibitor solution
to overcome this interference)„
3o4- Standard calcium solution,,
Dry several grams of pure calcium carbonate at
105°Go Weigh out 1000 g into a 500-milliliter
Erlenmeyer flasko Add dilute hydrochloric acid
dropwise until the calcium carbonate has dis-
solvedo Add 200 ml H^O and boil to remove
carbon dioxide„ Coolo Add methyl red indicator
and adjust "to orange color with dilute ammonium
hydroxideo Transfer completely to a 1-liter
volumetric flask and dilute to the mark with dis-
tilled water0 One ml of this standard contains
loOO mg of calcium, as calcium carbonate„
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3.5 EDTA titrant.
Dissolve 4oO g disodium dihydrogen ethyl ene diamine
tetraacetate dihydrate (EDTA) and 0.1 g MgCl2°6H20
in 300 ml water.
Standardize against standard calcium solution as
follows:
Put 5»0 ml of standard calcium into about 50 ml
distilled water. Add 2»0 ml buffer solution
and mix. Add a small scoop of indicator (about
.3 to .5 g)« Titrate with EDTA to the endpoint -
red to blue. The titration should take between
4.0 and 5.0 ml of titrant. Adjust the EDTA with
distilled water so that 1.0 ml equals 1.0 mg
hardness as calcium carbonate.
Repeat the titration. If the standard EDTA was
correctly adjusted, exactly 5*0 ml of titrant
should be used for bhis titration,,
Store in pyrex or polyethylene only,
4. Procedure.
4.1 Select sample size so that no more than 5-0 ml
of titrant is used, and dilute to 50 ml with
distilled water»
4.2 Add 1,0 ml buffer solution, and a scoop of indicator
powder; mix by swirl ing „
4,3 Titrate with EDTA, to blue endpoint .
5» Calculation;
mg/l hardness, as
Note: If the endpoint from red to blue is not sharp and clear,
the use of an inhibitor solution may be necessary.
See Standard Methods, llth Edition, p. 135
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COLOR (Standard Methods, llth Ed,, pe 111)
For this test to be significant, all turbidity must be
removed prior to analysis. The method for removal of turbidity
is critical since filtration through filter paper will also
remove some of the color,,
Turbidity can be removed by: (a) Centrifuging, and (b) by
filtration through a membrane filter (centrifuging is preferred)
1. Collection of Sample. Use raw water sample collected
for the mineral analyses.
2. Apparatus»
2.1 A series of Nessler tubes containing chloroplat-
inate color standards, or
2.2 permanent standards for color as provided with
the Hellige aqua tester, the Taylor analyser or
similar equipment.
3» Reagents. Hone
4. Procedure.
4.1 Take 100 ml of raw sample and remove turbidity
by centrifuge or through a membrane filter. If
the membrane filter is used, allow turbidity to
settle for 1 hour, then gently pour the super-
natant through the membrane without disturbing
the settled matter. This technique will insure
a volume of about 50 ml which is necessary for
comparison with standards.
4.2 Transfer the clear sample to the comparator and
match with the appropriate standard.
4.3 Record to the nearest color unit.
4.4 If color is too high, prepare a dilution using
distilled water. Multiply the color value
obtained by the dilution factor.
The Water Quality Section will provide color standards for
this test, if requested. Either the permanent standards used
with comparators or the Messier tube series can be provided,
as desired.
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TURBIDITY. (Standard Methods, 10th Ed., pa 207, llth Ed0 ,
p0 261). ~
Turbidity is the expression used to describe the presence
of particulate matter such as silt, clay, organic debris, algae,
or any suspended particles that obstruct' the passage of
light through water„ It is not directly related to the weight
of matter in suspension,. The Jackson Candle Turbidimeter is
the recognized instrument0 Other instruments must be cali-
brated in Jackson units before they can be used in reporting
turbidityo Unless turbidity results are reported in Jackson
units, they cannot be used by the Network,,
lo Collection of the Sample„ Use the raw water collected
for the mineral analyses,,
2o Apparatus,,
2<>1 Jackson Candle Turbidimeter, or
2o2 commercial turbidimeter, calibrated in Jackson
unitso
3 o Re agent So None
4o Procedure.
4ol For turbidities between 25 and 1,000 units:
ac Shake the sample vigorously and add 1 to 5
ml to the turbidimetero
bo Light the candle0 (Do not light the candle
while the tube is empty!)'
Co Shake sample again» Add small increments to
the turbidimeter until the image of the
candle flame is no longer distinguishable„
As the sample is added to the tube, the
flame outline will gradually fade until it
can no longer be distinguished, only diffused
light being observedo This is the prelim-
inary readingo
do Note the preliminary reading and remove the
sample from the tube0 Rinse the tube with
distilled water0
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76
e0 Shake sample again» Add sufficient sample
to the tube to give about 80 percent of the
preliminary reading, then add small incre-
ments until the flame disappears again<,
Record this value«
fo Eepeat this operation twice<, Eecord the
average of the three readings,
4,2 For turbidities greater than 1,000 units;
a0 Make a dilution of the sample such that the
turbidity falls near 500 units0
bo Carry out the steps outlined in procedure 401<
GO Multiply the average turbidity reading by
the dilution factor and record,,
4-«,3 For turbidities below 25 units:
a» Compare the sample with a series of standard
turbidities prepared at 5-tm.it intervals 0
To prepare the turbidity standards first
determine turbidity of a sample of water
that falls within the range of the Jackson
Candleo
bo Using this water, prepare dilutions with dis-
tilled water to give turbidities in the range
0 to 25 unitso
Co Transfer these, including the samples, to a
series of bottles of identical size, shape,
and type0
do Match the sample to the nearest standardo
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SULFATE (Standard Methods, llth. Ed., p. 237)
The gravimetric procedure is the most accurate for samples
containing more than 10 mg/1. It is also very time consuming.
The turbidimetric procedure is less accurate than the
gravimetric but is much shorter, and is the preferred method
for samples up to 60 mg/1. Other methods for sulfate are
available and can be used if their accuracy is comparable to
the Standard procedures. The turbidimetric method is des-
cribed in detail below.
1. Collection of Sample. Use the raw water sample
collected for the mineral analyses.
2- Apparatus. Commercial photometer or spectrophotometer.
Wave length, approximately 420 millimicrons.
3« Reagent s.
3.1 Conditioning solution:
Dissolve 75 S of sodium chloride in 300 ml of
distilled water and add 30 ml of concentrated
HG1, 50 ml of glycerine and 100 ml of 95 percent
ethyl alcohol or isopropyl alcohol.
3.2 Barium chloride crystals:
Obtain crystalline BaClp, 20 to 30 mesh.
3.3 Standard sulfuric acid solution 0.02 N:
(Use alkalinity reagent 3«1> P- 71 ).
4. Procedure.,
4.1 Measure out 50 ml of filtered sample (or aliquot
diluted to 50 ml if sulfate is above 60 mg/l)
into a 125 ml Erlenmeyer flask.
4.2 Add exactly 10 ml of conditioning solution and
mix.
4.3 Add approximately 0.4 to 0.5 g barium chloride
crystals, using a small spoon for uniform
measurement, and immediately upon addition of
the crystals begin stirring at a constant rate
for 1 minute. A magnetic stimer is very useful
for this operation.
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4.4 Let stand 4 minutes.
4.5 Transfer the suspension to the photometer cell
and read immediately. (Prepare a blank by using
50 ml of filtered water to which 1C ml of
conditioning solution has been added. Use this
to zero the photometer.
5« Preparation of Standard Curve.
5.1 (Use the 0.020 H sulfuric acid used for the
alkalinity test). Pipette 0.0, 0.5, 1.0, 1.5,
2.0, 3.0, and 4.0 ml of 0.020 N sulfuric acid
into 125 ml Erlenmeyer flasks. Dilute each
portion to 50 ml with distilled water. These
standards are respectively 0.0, 9.6, 19-2, 28.8,
38.4, 57-6, and 76.8'mg/1 of &&• .
5.2 To each flask in the series, carry out procedural
steps 4.2 through 4.5 before proceeding with the
next flask. Use the zero standard to zero the
photometer.
5.3 Prepare a calibration curve, plotting photometer
reading vs concentration of sulfate.
6. Calculation of Results,. Head the sulfate concentration
of the sample from the calibration curve, multiply
by the dilution factor, if any, and report as mg/1
sulfate.
Note; The limit of usable concentration for this test is
approximately 60 mg/1. Somewhere between the 57«6 and
76.8 mg/1 standards (paragraph 5«1) the standard curve
will begin to skew from a straight line*
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DETERMINATION OF PHOSPHATES (Ortho plus Poly)
Phosphate can be determined as three separate entities
in the water environment, as ortho, poly and organic. To
do this would require considerable laboratory time, as the
organic phosphate procedure is long and tedious, and separate
tests are necessary to differentiate ortho from poly. To
collect the information of greatest value to the Network,
and to reduce laboratory time to a minimum, it is felt that
a single determination combining ortho plus poly phosphate
will fulfill the needs of the Network without imposing an
excessive burden on the participating laboratory.
1. Collection of Sample. Use the raw water collected
for the mineral analyses.
2. Apparatus.
2.1 Spectrophotometer or filter photometer, for use
at 690 millimicrons, or
2.2 Nessler tubes, 50 ml.
3<> Reagents.
3.1 Phenolphthalein indicator: Dissolve 2.5 gms. of
phenolphthalein powder in 250 ml of ethyl alcohol,
add 250 ml of distilled water, then add 0.020 N
NaOH dropwise to a faint pink color.
3.2 Sulfuric acid: Add 310 ml of concentrated HoSO^.
slowly to about 600 ml of distilled water. Cool
to room temperature and dilute to 1.0 liter.
3.3 a° Stock standard phosphate solution (0.50 mg
P04 per ml). Dry a portion of reagent grade
potassium dihydrogen phosphate overnight at
103° before use. Dissolve 0.7164 gm of
the Iffl^O/f. in distilled water and make up
to 1.0 liter,
b. Working standard phosphate solution (0.005
mg/PO/j. per ml): Dilute 10.0 ml of the
stock standard phosphate to 1.0 liter with
distilled water. Protect this solution from
the light and make up fresh each month.
3.4 Ammonium molybdate solution: Dissolve 25«0 gms
of (NH/j.)6MonOp4.'4H20 in 1?5 ml of distilled
water. Add 155 ml of concentrated ^SO^. slowly
to 400 ml of distilled water, and cool.
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- 80
Add the molybdate solution to tlie sulfuric acid
solution (never in reverse) and dilute to 1.0
liter.
Jo5 Stannous chloride solution: Dissolve 2.5 6 of a
fresh supply of SnCl2°2H20 in 100 ml of reagent
grade glycerine. Heating in a water bath and
stirring with a glass rod are recommended to hasten
solution. This reagent is STABLE, requiring
neither the addition of preservatives nor special
storage.
4. Procedure.
Preliminary Cleaning of Glassware. Because laboratory
detergents contain phosphate, which cannot be easily
rinsed off, a preliminary treatment with phosphate
reagents is necessary to remove that adsorbed on
the glass surfaces. After the glassware has been
properly cleaned it should be reserved for this
test only.
4.1 Clean and thoroughly rinse all glassware in the
usual manner. *•
4.2 Before use, treat each container that will come
in contactwith the sample as follows:
a. Fill each container with distilled water
and add 2.0 ml of ammonium molybdate solution
and mix.
b. Add 1 ml of sulfuric acid solution and 5
drops of Stannous chloride solution; mix
thoroughly and allow to stand for 10 to 15
minutes. Make certain that all internal
surfaces of the containing vessels come in
contact with the reaction mixture. Discard
the reaction mixture and rinse each container
with*'distilled water.
Once this cleaning procedure has been performed the
glassware can be reused without repeating the treat-
ment, unless it has been cleaned with detergent.
4.5 Preparation of standards (photometric procedure),,
Observe room ^temperature. Standards and samples
must be.- run at same temperature, _+ 2°C, for
reproducible results.
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a. Add increasing volumes of working standard
phosphate solution to several vessels
(previously cleaned according to paragraph
4.2). Add 1,0 ml of sulfuric acid. Make up
to 50.0 ml with distilled water.
The following table is suggested as a convenient
series for use with a photometer.
ml of phosphate standard
(Reagent 3»3t>)
0 (Blank)
0,5
1*0
2,0
5.0
10*0
b. Add 2.0 ml
c. Add 5 drops
mg PO./50
0
.0025
.0050
.0100
.0250
.0500
ml PO^, mg/1
0 (Blank)
.050
0.10
0,20
0.50
1.00
of ammonium molybdate, and mix.
3 (0.25 ml]
) of stannous chloride
solution. Mix and allow to stand for 20
(_+ 5) minutes.
d. Read in spectrophotometer at 690 millimicrons
or in a filter photometer at 600 to 700
millimicrons. Use the blank to zero the
instrument.
e« Prepare calibration curve,
4,4 Raw water sample (photometric procedure).
a. Filter at least 100 ml of the sample to
remove turbidity.
b. Place 100 ml of the filtered sample containing
not more than 0,050 mg PO^ or an aliquot
diluted to 100 ml in a beaker or an Erlenmeyer
flask. Garry a blank of 100 ml distilled
water along with the sample.
c. Omit this step if the pH is below 8.2, Other-
wise ;
c«l Add two drops of phenolphthalein.
c.2 Add sulfuric acid solution, dropwise,
to discharge the pink color.
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1
1
IB
1
1
1
1
1
d.
e.
f.
g.
h.
- 82 -
Add exactly 2.0 ml of sulfuric acid and
boil gently for one-half hour. Add a small
amount of distilled water if volume drops
below 25 ml during the boiling period.
Cool, make up to 100 ml with distilled water
and adjust to temperature of standard curve.
Take 50 ml of the treated sample and add 2.0
ml of ammonium molybdate solution and mix.
Add 5 drops (0.25 ml) of stannous chloride,
mix, and allow to stand for 20 (_+ 5) minutes
for color development. ~~
Read in the spectrophotometer, using the
distilled water blank to zero the instrument.
4.5 Calculation:
n r\r\r»
mg
/I POi TTICP POi. ('f-r-riTn i-4-nnrln-nrl riii-nm^ Y J-WVW
1 * tf i I f^ ctmTy I Q
Report to the nearest 0.1 mg/1.
4.6 Procedure for Nessler tubes: Follow steps (a)
through (e) under photometric procedure 4.4.
f.
S«
,*
ml of Phosphate
(Reagent 3.
0
0.5
1.0
3.0
5.0
Cool, transfer 50 ml to a Nessler tube.
Add increasing volumes of working standard,
reagent 3«3b, to a series of 50 ml Nessler
tubes (previously cleaned according to
paragraph 4.2). Add 1.0 ml of sulfuric acid,
reagent 3»2. Dilute to 50 ml with distilled
water. The following table is suggested as
convenient for use in Nessler tubes.
Standard mg PO./50 ml PO, , mg/1
3b) ^ *
0 0
0.0025 0.05
0.005 0.10
0.015 0.30
0.025 0.50
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- 83 -
h. Add 2.0 ml of ammonium molybdate to each.
standard and sample and mix.
i. Add 5 drops (0.25 ELL) of stannous chloride,
mix, and let stand for 20 Q+ 5) minutes for
color development. ~~
j. Match the color in the sample,with the
closest standard.
4-. 7 Calculation:
mg/1 PO. = mg PO,^ in closest matching standard
^ ^ 1000
ml sample
Report to the nearest 0.1 mg/1.
5. Notes.
5.1 The concentration of acid in the sample and
standards has a direct effect on the amount of
color produced. It is important, therefore,
that addition of the sulfuric acid solution
be performed accurately.
5.2 The phosphomolybdate blue produced by the
reaction is not stable and tends to fade gradu-
ally after about 20 minutes. Most accurate
results are obtained when time requirements are
observed.
5.3 Temperature is another variable that affects
the color formation. Samples and standards may
be adjusted to room temperature after boiling
by allowing to stand for several hours before
addition of reagents 3«4- and 3»5»
5.4- If the phosphate concentration in the sample is
completely unknown, several dilutions of the
sample may be run simultaneously and that
aliquot used for final reading, which falls
near the middle of the standard series.
5.5 Scrupulous care should be observed in cleaning
the glassware prior to use. If color appears
in the blank, or if a particular standard appears
out of line, phosphate contamination is probably
responsible.
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- 84- -
5.6 When using the photometric procedure, only one
"blank is necessary if the standards and sample
are run at the sams time.
5.7 The working standard phosphate solution (reagent
3«3b,) should be kept in the dark to prevent
reduction of phosphate concentration through
algal growth.
5.8 In preparation of the ammonium molybdate solution
(reagent 3.4), the molybdate must be added to the
sulfuric acid, never the reverse. Reversing
the addition precipitates some of the molybdate,
which is then very difficult to dissolve.
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TOTAL DISSOLVED SOLIDS (Standard Methods, llth Ed., p, 215)
For this test all turbidity must "be removed prior to
analysis. Turbidity can be removed as in the Color Test,
page 74, or by filtration. To obtain satisfactory accuracy
the sample size selected should be large enough to produce
at least 25 mg of residue following the drying operation.
1. Collection of Sample. Use the raw water sample
collected for the mineral analyses.
2. Apparatus.
2.1 Analytical balance, capable of accurate weighing
to _+ 1 mg.
2o2 Drying oven controlled at 103°to 105°C.
3« Reagents. None
4. Procedure.
4-.1 Clean an evaporating dish (about 3 to 4 inches
diameter) thoroughly and dry in oven overnight
at 103°to 105°C.
4.2 Cool and weigh to _+_ 1.0 mg.
4.3 Set the evaporating dish in the drying oven or
on a steam batho Measure out a volume of
filtered sample that will give at least 25
mg of residue. Add this to the evaporating
dish in increments until the total volume selected
has been added.
4.4 Evaporate to dryness and hold for 1 hour at 103°
to 105°C.
4.5 Transfer to dessicator and cool.
4,6 Weigh to +_ 1.0 mg.
5. Calculation:
mg/1 total = (Wt of dish + sample - wt of dish) X 1000
dissolved solids ml of sample
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SECTION VIII
HANDLING OE ANALYTICAL DATA
Reporting of Results
Each, participating agency is furnished a supply of Form
PHS 2845-1 (Eev. 6-59; National Water Quality Network Report
(Field), for reporting the results of the determinations
performed by its laboratory. These are provided as multiple
copy '.'.snapout" forms with interleaved carbons to simplify
reporting of results. The forms consist of a white page, a
blue page,and a pink page. The white and blue copies are
sent to the Water Quality Section at Cincinnati and the pink
copy is retained by the cooperating agency for its files.
Eranked, return-addressed envelopes are provided for mailing
purposes.
The forms have been designed for easy transcription to
permanent records, because the data are to be entered later
on machine-sorted punch cards. A fixed code has been
established that cannot accommodate variations in reporting
practiceo To avoid errors in the compilation of the data,
each laboratory is requested to observe the following pro-
cedures in tabulating the analysis on the forms provided.
State: Insert the State in which the sampling point is
located.
Station location; Insert the name of the river being
sampled, the city or other geographical "land-
mark" identifying the location, and the river
mileage from the mouth to the station, if
available.
Laboratory; Insert the names of the laboratory and the
person completing the report.
In reporting data, round out the values to the nearest
unit shown on the report form. For example, a chloride value
of 20.6 mg/1 should be reported as 0021 mg/1. The form may
be completed with a hard pencil or ballpoint pen, or by
typing. Whatever the method used, care should be taken to
make each copy legible. A sample completed report form is
shown on the following page»
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- 8? -
DEPARTMENT OF HEALTH, EDUCATION, AND WELFARE
PUBLIC HEALTH SERVICE
DIVISION OF WATER SUPPLY AND POLLUTION CONTROL
PROVISIONAL DATA—SUBJECT TO REVISION
#4-0
FOR WASHINGTON USE ONLY
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CHECKED BY:
Maryland (B.C.)
STATION LOCATION
Potomac River, Great Falls, Maryland
LABORATORY
Daleca-rlia Wn.qhingtnn P.P.
Ha -P-PI n t nn
DATE SAMPLE TAKEN
94.
IQfi?
TEST RESULTS
INSTRUCTIONS: All boxes should contain a figure or proceeding zeros. If lesl is not made, put "X's" in every box
EXAMPLE- If D O is 1CV5 mg/l(ppm) enter as follows | 1 iTiTsl
If Turbidity is 50 units, enter as follows [ 0 I 0 j 5 | 0 )
1. TEMPERATURE
2. DISSOLVED OXYGEN (DO)
3. pH
4. BIOCHEMICAL OXYGEN DEMAND ( BOD )
5. CHEMICAL OXYGEN DEMAND (COD)
1
0
0
0
18
1 3 —
J7
16 —
!8
19 _
!i
22 —
|o ii
6. CHLORINE DEMAND - 1 HOUR
7. CHLORINE DEMAND - 24 HOURS
O. AMMONIA NITROGEN (N//3-N)
9. CHLORIDES
0
0
0
o p
1O. ALKALINITY (as CaCO^)
1 1. TOTAL HARDNESS (as CaCOJ
0
OtL
12. COLOR
13. TURBIDITY
14. SULFATES
D
o )3
0 b
25 —
|1
2B —
!^
31 —
lo
3-1 —
|l
37 —
19
A\ —
J3
44 —
!o
40 —
IT
•ii —
J5
1
1 5
1
16
1
21
1
24
1
1
27
1
*
30
1
Ik
31
1
*
36
1
1
40
1
1
41
1
1
47
1
1
•>()
1
1
54
1
1
3
0
2
2
8
4
o
1
8
3
0
5
]T
i
5% — 18
15. PHOSPHATES
1C. TOTAL DISSOLVED SOLIDS (TDS)
3
0 |2
!o
•,9 -
12
G2 —
1
0
f. 1
1
1
6'j
i
Degrees C. to tenths
mg// to tenths
To tenths
mf|// to tenths
mgfl in units
mtf/l to tenths
mult to tenths
m£// to tenths
mtf// in units
»ij,'// in units
rntf/f in units
In scale units
In scale units
m{£// in units
?nji/I lo tenths
1
n
J_ J until in units
DISTRIBUTION. RETAIN FINK COTY IN f ART I C I r A T I N G LABORATORY. FOHWARD ORIGINAL (WHITE.) AND BLUE COPY TO WATER QUALITY
SECTION. CINCINNATI. OHIO.
pHs-2
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Presentation of Results
The data are processed and printed by the Basic Data
Branch of the Water Supply and Pollution Control Division
in Washington, D. C. The data are transferred from the
original sheets forwarded by the Water Quality Section
to Washington D. C. to machine-punched cards for listing
in chronological order of testing in such manner that the
determinations performed by the cooperating laboratories
and by the Water Quality Section will be coordinated. Four
times a year the data will be summarized and reported back
to each agency in printout form. Each quarterly report
will include the chemical, radiological, bacteriological,
biological, and organic data collected for that portion of
the year in which the summary is prepared, plus the
summaries of the preceding quarters. A complete national
compilation containing the data from every station is
printed on an annual basis, copies of which are supplied
to each participating agency.
Interim reports can be prepared with data listed by
geographical area, such as by state or by major and/or minor
river basins. The machine tabulation operation is also
capable of carrying out statistical analyses of the data
such as the development of means, medians, and frequency
distributions. Requests for special analyses of the data
and for tabulations covering a particular area should be
made to the Public Health Service Regional Office concerned.
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