Ml.
-0
-1
LABORATORY
PROCEDURES
ANALYSIS
4 FOR WASTEWATER
TREATMENT
PLANT OPERATORS
ENVIRONMENTAL PROTECTION AGENCY
WATER PROGRAMS- REGION VII
911 WALNUT STREET
KANSAS CITY, MISSOURI 64106
-------
LABORATORY PROCEDURES
ANALYSIS FOR WASTEWATER
TREATMENT PLANT OPERATORS
by: David Vletti
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
Construction Grants
Operation and Maintenance
911 Walnut Street
Kansas City, Missouri 64106
June 1971
-------
This is the
Superintendent of Documents
classification number:
EF 2.8:
W28
-------
INDEX
Introduction 1
Glassware 2
Cleanliness, Sterilization, Chemicals, Contamination, Equipment, and
Technique 3
Sampling 6
Full Bottle Winkler Method for Dissolved Oxygen Test 10
Dissolved Oxygen Kits and Probes 17
Inhibitor Flocculation Modification Dissolved Oxygen Test 17
Solubility of Oxygen in Fresh Water Table 18
Biochemical Oxygen Demand (BOD) Test 19
Relative Stability - Methylene Blue Test 27
Settleable, Total and Suspended Solids Discussion 29
Settleable Solids Test 32
Total Solids Test 33
Volatile Solids Test 35
Total Volatile Solids Sludge Test (Short Cut) 36
Centrifuge Method for Suspended Solids Test 37
Gooch Crucible Method for Suspended Solids Test 38
Volatile Suspended Solids Test 42
Settleable Solids in Activated Sludge Test 44
Sludge Volume .Index 44
Sludge Density Index 44
Sludge Age 44
Specific Gravity of Sewage Sludge 45
Sludge Condition for Vacuum Filtration 46
-------
INDEX (Continued)
Ammonia Nitrogen Test 47
Nitrite Nitrogen Test 48
Nitrate Nitrogen Test 48
Sulfite Test 49
Sulfate Test 50
Carbon Dioxide Test 51
Hydrogen Sulfide Test * 51
Chlorides in Sewage Test 52
Phosphate Test 53
Alkalinity Sewage Test 53
Alkalinity Sludge Test 54
Acidity Sewage Test 55
Acidity Sludge Test 56
Chlorine Demand and Standard Solutions 56
Solution for Chlorine Demand Test 57
Jar Test for Blue Green Algae Control 58
Oil and Grease Test 58
Grease (Soxhlet Extraction Method) Test 59
pH of Sewage Sludge - Colorimetric Method 60
pH of Sewage - Colorimetric Method 61
Hydrogen-Ion Concentration Discussion 61
Acids - Volatile 63
Carbon Dioxide in Sewage Gas 64
Hydrogen, Methane and B.T.U. in Sewage Gas 65
Bacterial Examination 67
-------
INDEX (Continued)
Total Coliform 69
Fecal Coliform 70
Fecal Streptococcus , 71
Appendix - Bacterial Sampling Dilution Procedure 73
Conversion Factors 74
Units 77
Conversion Table 79
Discharge From A Parshall Flume 80
Discharge From Triangular Notch Weirs With End Contractions 83
Report of Laboratory Results 84
Sample Collection and Preservation 87
Glossary 88
References 90
Acknowledgement 91
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-1-
INTRODUCTION
The need for basic straight-forward procedures and qualified
wastewater laboratory analysts is increasing at a rapid rate. With
more and more emphasis being placed upon the quality of treated waste
discharged into the interstate and intrastate streams, lakes, rivers and
waterways, the need for better laboratory control is apparent.
This wastewater laboratory manual is furnished by the Environmental
Protection Agency as an aid to the laboratory analyst for making waste-
water analyses. It is not meant to be the ultimate answer for the most
precise and accurate tests. However, the procedures contained herein for
the most widely used parameters in a treatment plant are of the highest
precision.
The most accurate and precise results are obtained by following the
procedures found in the latest edition of Standard Methods and WQO Methods
For Chemical Analysis of Water and Wastes. Many of the tests found in
these texts are not economically feasible for many wastewater treatment
plants, and this manual is meant to provide alternate test procedures
which will provide results of sufficient accuracy.
In addition to this laboratory manual, the analyst should have available
the latest editions of Standard Methods for the Examination of Water and
Wastewater. ASTM Standards, and WQO Methods for Chemical Analysis of Water
and Wastes, and the latest edition of Laboratory Manual for Chemical and
Bacteriological Analysis of Water and Sewage by Theroux, Eldridge and Mailman.
-------
- 2 -
GLASSWARE
ERLENMEYER
FLASK
17
B.O.D.
BOTTLE
BEAKER
BURETTE
PIPETTE
GRADUATED
CYLINDER
-------
-3-
CLEANLINESS, STERILIZATION, CHEMICALS,
CONTAMINATION, EQUIPMENT, AND TECHNIQUE
Glassware is an essential part of most chemical analysis procedures.
It can be cleaned by rinsing with an acid cleaning mixture made up by
adding 1 liter of concentrated sulfuric acid, slowly with stirring,
to 35 mis saturated sodium dichromate solution. Acetone is a very good
organic solvent and can be used as a cleaning solution also. After
cleaning the glassware, rinse thoroughly with warm tap water and finally
distilled water.
A clean container is usually defined by the" layman as one which is
visibly free from dirt or foreign material. Since many cleaning solutions
are not bactericides, a visibly clean piece of equipment does not
necessarily mean that the equipment is free of microorganisms since they
are not visible to the naked eye. The cleaning agent used might leave
a film on the equipment which could cause erroneous results. Sterilization
of equipment as practiced in the microbiological laboratory is accomplished
by heating or steaming the object to be sterilized sufficiently long to
kill all living organisms. This is usually done with the use of an
autoclave. The bottles used to send in water samples need to be sterilized
so that foreign matter and living microorganisms will not be present.
The reagents used in the determinations of chemical quality of
water and sewage have been compounded to give accurate results and have
been standardized for the purpose intended. Contamination of reagents
by using dirty glassware or by using the same pipette for several reagents
will cause erroneous results. The purpose of laboratory control thus is
defeated. Rinsing of all glassware in distilled water prior to use is
necessary. All droplets of water should be shaken from the apparatus to
prevent continuous dilution of reagents. Reagents can be purchased in
standardized form from chemical houses. This is slightly more expensive
than is the preparation of reagents in the laboratory.
Work in the chemistry laboratory consists of combining chemicals
under controlled conditions to establish a knowledge of comparison
between a standard and an unknown. Certain procedures have been
devised whereby simple tests will provide the knowledge desired. The
laboratory as known to water and sewage works operators should be
considered a tool to assist in control of plant processes.
-------
- 4 -
Many chemicals, when combined, react violently. Knowledge in
the field of chemistry is necessary to predict what combinations of
chemicals or compounds will react as desired. A few precautionary
measures should be followed in the laboratory:
1. Follow instructions
2. Combine only those materials as instructed
3. Consider the laboratory as a tool and use as directed
4. Keep equipment clean
5. Record findings immediately
6. Do not contaminate reagents
Much of the technique employed in a chemistry laboratory can be
learned from observing and practicing the various operations and
procedures. Many of the chemicals used are strong acids and bases
which are harmful to eyes, skin and clothing. The first and most
important .technique to practice is caution. The following items
should be remembered and practiced in all laboratory work:
1. When adding an acid to an aqueous solution permit
the acid to enter by sliding down the side of the
container slowly. Never add water to acid.
2. Do not apply suction with the mouth when filling a
pipette with a strong reagent. Rather dip the tip
of the pipette into the reagent and cover upper
opening with the finger before removing.
3. If glassware slips, let it fall. An attempt to
catch falling glassware might result in a
dangerous cut.
4. If in doubt of the contents do not sniff strongly
at the mouth of a container.
-------
- 5 -
5. To neutralize strong acid on skin or clothing
wash with tap water and apply dilute Ammonium
Hydroxide solution.
6. To neutralize strong alkali or base chemical on
skin or clothing wash with excess of tap water
and apply dilute acetic or hydrochloric acid.
7. If any chemical gets in the eye wash with
excess of tap water and see your physician
immediately.
The analytical balance is a precision instrument that plays a
very important role in a laboratory. With the aid of the balance,
solutions of the proper strength may be prepared to be used in the
accurate determination of a particular substance. Determinations
may be made directly by employing weighing procedures, and it is
the standard for accuracy in the laboratory.
The balance is an expensive apparatus that must be used with
care because of its relative delicateness. Rough use will damage
the balance and decreases its accuracy or even impair its operation.
The balance should be centrally located in an even-temperatured
room and carefully guarded against radiations from heating apparatus
and excessive vibrations. When not in use the beam should be
supported by the beam rests and the pans should be supported by the
pan rests.
-------
-6-
SAMPLING
PURPOSE
The analysis cannot be any better than the sample itself.
Therefore, the sample must be as correct as possible.
Samples are taken to allow the operator to test for the amount
of improvement in water quality by each unit in the plant and for
the plant as a whole. In order to further evaluate the efficiency
of his plant, he must know the condition of the raw sewage entering
his plant, the effluent from the plant and the condition of the
receiving stream above and below the effluent discharge.
Normal sampling points are listed below. These may be changed
or modified to suit the Individual plant.
1. Influent (Raw Sewage) - At a convenient point
prior to any treatment where one can obtain a
representative sample.
2. Effluent of primary tanks - This point should
be selected near the lower end of the effluent
channel to allow thorough mixing of effluent
from entire unit.
3 Aeration tank.
4. Effluent of trickling filters.
5. Effluent of final clarifier.
6. Receiving stream - At least fifty yards upstream
from entry of effluent.
7. Receiving stream - At least fifty yards below
entry of effluent.
The points may be established to fit the individual plant,
but should be so arranged to give a uniform and true picture of the
operation of each unit of the plant and the influence of the plant
on the condition of the stream.
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- 7 -
METHODS
For most of the tests, the samples should be collected in
a wide-mouth bottle of a predetermined capacity. Each grab
sample for the composite should be at least 300 mis in size. A
holding device should be constructed so that the collection
bottle can be held below the surface, mouth pointed in the
direction of flow.
RATIO OF SAMPLING TO FLOW
In order to accurately evaluate the data, it is desirable
that the volume of sample collected each time be related by
simple ratio to the total flow at that particular moment.
COLLECTION
The importance of collecting and handling sewage samples
in the most careful manner cannot be overemphasized. The
procedures and equipment used in the laboratory are assumed to
be the most accurate and precise obtainable. If the results
from the tests are to be accurate, precise and representative,
the same precision and accuracy must be exercised in the
collection, handling and storage of the samples prior to the
actual laboratory procedures. It is even more important that
samples be collected during the time that any unit of the plant
is out of operation. The results of the plant operation during
a breakdown are often valuable evidence in the event of a lawsuit,
FREQUENCY
The more frequent the sampling, the more complete the results.
If it is impossible to run samples quite frequently, a five-day
•schedule has the advantage of permitting titrations for the DO of
present samples and BOD of the previously incubated samples, all at
one set-up.
If the sampling is to be done on a weekly basis, the samples
should be taken on different days of the week in order that any
daily variations in the sewage characteristics may be found.
-------
COMPOSITES
A grab sample taken at any particular hour of day or night does
not give a true picture of the over-all plant operation. Therefore,
if the grab samples are collected and composited hourly or at some
suitable time interval over the working day or the 24-hour period in
volumes related by ratio to the total flow, we have then a Composite
Sample, which closely represents the conditions which existed over the
period in which samples were collected.
Rate of flow at time of collection x total sample needed = amount of
Number of portions x average rate of flow single portion
NOTE: A composite sample is composed of two or more portions added
together. It may be collected over any desired period of time and
the portions may be collected at any desired intervals. To obtain
a representative sample each single portion must be measured proportional
to the rate of flow at the time of collection. The rate of flow may
be in either gpm or gpd.
EXAMPLE: Samples are collected at intervals of four hours over a
24-hour period making a total of six portions. The rate of flow at
the successive sampling times are 1.5 mgd - 1.2 mgd, 2.0 mgd • 1.3 mgd -
1.6 mgd and 1.4 mgd. The average rate of flow is 1.5 mgd; the required
total amount of sample is 1200 mis.
Find the size of each portion in mis
g = 200 mis size of first portion
2> ]'l * ]2j?° = 160 mis size of second portion
= 267 mls S1'ze of third P°rtl'on
4. .1.3 x 1200 = 173 m]s Si2e Qf fourth portion
OX 1.9
5. 1..6 x ,fcuu a 2>3 mls Slze Qf fifth portion
V n I • w
6. 1.4 x 1200 B 187 mls size Qf sixth portl-on
ox I.t>
totil samPle
-------
STORING
The samples should be stored at 4°C. This retards any further
bacterial action until you are ready to run the sample. The volume
of each hourly or bi-hourly sample should be calculated to fill a
gallon container about 3/4 full.
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- 10 -
FULL BOTTLE WINKLER METHOD
FOR DISSOLVED OXYGEN TEST
PURPOSE
The test measures the oxygen present as a gas in solution. This
information may be valuable in:
1. Studies of septicity of sewage
2. Odor control
3. Operation of pre-aeration units
4. Operation of secondary treatment facilities
5. Pollution control.
The azide full bottle modification of the Winkler Method is the
most accurate and precise dissolved oxygen (DO) test. The azide
eliminates the nitrites sometimes found in sewage. The nitrites will
cause an error in the DO value if the azide is not used.
OUTLINE OF PROCEDURE
1. Addition of test materials (reagents) to sample, see
diagram.
W-
Ar\
SAMPLE
2ml.
>- MnS04 -*•
Solution
ri
,. j
2 ml.
AlkKI __
NaN3
Solution
^
O"O
WHITE
FLOC
^ 2ml.
"^" H2S04 "^"
CLEAR
SOLU-
TION
kl«t
NO
•^"
A A
T"T fo\
/_ V ft JX.
*-
'vto \
BROWN
FLOC
kj tf ^^
^ 2ml.
~^" H2S04 "^"
f//A
BROWN
SOLU-
TION y
1 / / /.
^^ D.O.
*" Present
-------
2. Ticracion:
- 11 -
•THIO' TOTAL
(0.0375 N N32S203) 'TWO'
£
J
*
\
I
READ THIS
LEVEL ~~"
> <
7
X
X
X
l£
X
> 1
1 ml.
STARCH
ADDED
^
7
X
X
X
X
X
x
X
X
X
x
,x
X
1
. ml.
USED
r
J
^
READ THIS
LEVEL "•""
>
I
»
^•H
c
7
x
^
^
•••
BROWN
PALE YELLOW
BLUE
CLEAR
3. Recording of results. Record volume of 0.0375 N sodium
thiosulfate (thio) used in the titration.
(1 ml thio " 1 mg/1 or ppm of Dissolved Oxygen)
PREPARATION OF TEST MATERIALS (REAGENTS)
CHEMICALS REQUIRED (All chemicals should be of "analytical
reagent grade.")
1. Manganous sulfate, MnSO^.AH20 or MnSO^H-O, or MnSO^.H-O
2. Sodium hydroxide or potassium hydroxide, NaOH or KOH
3. Sodium iodide or potassium iodide, Nal or KI
-------
- 12 -
4. Sodium azide, NaN,
5. Sulfuric acid, I^SO,, concentrated
6. Soluble starch
7. Sulfamic acid, NH SO-OH, technical grade
8. Copper sulfate, CuSO^-Sl^O
9. Sodium thiosulfate, Na2S20
10. Chloroform, CHC13
11. Potassium dichromate, l^C^
12. Acetic acid, concentrated
13. Distilled water.
PREPARATION
Manganous_ Sulfate jolution (MnSO/ solution)
1. Dissolve 480 grams MnS04.4H20 or 400 grams MnSO,.2H20 or 364
grams MnSO^.l^O in distilled water. This is difficult to
dissolve. Use electric stirrer if possible.
2. Add enough distilled water to make one liter and mix thoroughly.
Alkaline Iodide-Sodium Azidc Solution (KI NaN3)
1. Dissolve 500 grams NaOH or 700 grams KOH and 135 grains Nal or
150 grams KI in distilled water. Each substance should be
dissolved separately and in small amounts of distilled water.
Mix them when they are cool. CAUTION: Add water slowly with
stirring, avoid breathing fumes, and avoid bodily contact
with the solution. Heat is produced when the water is added
and the solution is very caustic.
2. Dissolve 10 grams NaN. in 75 ml distilled water. CAUTION:
is poisonous.
-------
- 13 -
3. Add the NaN3 solution with constant stirring to the
cooled solution of alkaline iodide.
4. After the cooled solutions are mixed, add enough
distilled water to make a final volume of 1 liter
and mix thoroughly.
Sulfuric Acid, concentrated
Handle carefully, since this material will burn hands and clothes,
Rinse affected parts with tap water to prevent injury.
Starch Solution
1. Take 5 to 6 grams of Arrowroot or soluble starch and add
the least quantity of cool distilled water necessary to
make a paste.
2. Pour this emulsion into 1 liter of boiling water.
3. Allow to boil a few minutes and settle overnight.
4. Use clear supernatant.
5. Add 10 mis chloroform and keep refrigerated.
6. Stable for about 1 month.
Sodium Thiosulfate Stock Solution (Na2S203) - (0.75 N)
1. Dissolve 372.30 grams of Na2S203-5H20 in 1500 mis of
boiled and cooled distilled water.
2. Add distilled water to make 2 liters and mix thoroughly.
3. Add 10 mis chloroform.
Working Sodium Thiosulfate Standard Solution - (0.0375 N)
1. Take 50 mis of sodium thiosulfate stock solution and add
enough distilled water to make 1 liter. Mix thoroughly.
2. Add 10 mis chloroform.
3. Stable for about 1 month.
-------
- 14 -
Copper Sulfate - Sulfamic Acid Inhibitor Solution
1. Dissolve 32 g sulfamic acid in 475 mis distilled water.
2. Dissolve 50 g copper sulfate in 500 mis water.
3. Mix the two solutions together and add 25 mis concentrated
acetic acid. Bring up to 1 liter and mix thoroughly.
Potassium Dichromate Stock Solution (I^C^O) - (0.375N)
1. Dissolve 18.39 grams of I^C^Oy in distilled water and
add enough distilled water to make exactly 1 liter. Mix
thoroughly.
Working Potassium Dichromate Solution - (0.0375N)
1. Take 100 mis of Potassium Dichromate Stock Solution and
add enough distilled water to make 1 liter. Mix
thoroughly.
Standardization
1. Add 250 mis of distilled water to a 500 ml, wide mouth,
E-flask.
2. Dissolve approximately 2 grams KI in the distilled water.
3. Add 2 mis of concentrated 112804.
4. Pipette exactly 10.00 mis of 0.0375N ^C^Oy into the
solution.
5. Allow to stand in the dark for 10 minutes. The brown
color which is developed is due to the liberation of
iodine in solution.
6. Titrate this iodine with the sodium thiosulfate being
standardized. When the color is pale yellow, add 1 or
2 mis of starch solution and continue adding thiosulfate
solution until the blue color disappears.
7. Record burette readings.
-------
- 15 -
8. Assuming the burette reading was 9.50 ml of sodium
thiosulfate used, the following calculations are done to
find the amount of distilled water which must be added to a
volume of sodium thiosulfate working solution to make it
0.0375N. For the following example, it is assummed that
800 ml of sodium thiosulfate working solution is being
adjusted to 0.0375N.
[(ml) K2Cr207] [(N) K2Cr207] = [(ml) Na2S203] [(N) Na2S203]
From step 4 10.0 ml of 0.0375N K2Cr207 were used.
[10 ml] [0.0375N] = [9.50 ml] [(N) Na2S203]
[(N) Na2S203] = 0.03947
9. [800.00 ml] [0.03947] = [(ml) Na2S203] [0.0375N]
[842.03] = [(ml) Na2S203]
842.03 ml - 800 ml = 42.03 ml
42,03 ml of distilled water are to be added to the 800.00 ml
of sodium thiosulfate working solution to give the desired
normality of 0.0375N.
HOW TO MAKE THE TEST
1. Fill completely a 300 ml BOD bottle with the sample to be
analyzed without allowing air to get into the bottle.
2. By holding the tip of the pipette below the surface of the
liquid add:
(1) 2 mis manganous sulfate solution,
(2) 2 mis alkaline-iodide-azide solution.
3. Replace stopper, avoiding trapping air bubbles, and shake well.
Repeat shaking after, floe has settled halfway. Allow floe to
settle again, about three-quarters of the way down from the
top.
4. Remove stopper and add 2 mis of concentrated sulfuric acid
down the neck of the bottle. Be sure to hold pipette above
the surface of the liquid.
5. Mix to dissolve the floe. Handle carefully to prevent acid
burns.
6. If solution has no yellowish brown color, or is only slightly
colored, add 1 or 2 mis of starch solution. If no blue color
develops, there is zero DO. If a blue color develops proceed
-------
- 16 -
as in Step 7.
7. If solution is yellowish brown, pour into a wide mouth, 500 ml,
Erlenmeyer flask, and titrate with 0.0375N sodium thiosulfate.
8. Add the thio until the color becomes pale yellow, then add
1 or 2 mis of starch solution and continue adding thio until
the blue color disappears.
9. Record the number of mis of thio used.
10. Reading the burette:
MENISCUS
1.2 ml. IS
THE READING
UPPER SECTION
ONLY OF BURETTE
Wiicn the burette is to be used, ti.c
initial reading must be taken. Tnc
correcc place to look is the bottom
of the curve that the surface of the
liquid forms. This curve is called
the meniscus. After seeing where
the liquid level is, record the
result and proceed to add the
thiosulfaie solution (titrate). When
the required amount of solution has
been added, that is, when the blue
color disappears, the final burette
reading is made and recorded. Read
the bottom of the meniscus as before.'
Subtract the initial reading from
the final reading. This difference
represents the net volume in
milliliters (ml.) of solution used.
11. Calculation of the DO:
If the brown solution (Step 7) is titrated with the 0.0375N'
thio, then:
DO in mg/liter (or ppm) - ml of thio used.
12. Discussion £
The sample for the dissolved oxygen test is usually
collected in the bottle that will be used in the test.
Extreme caution must be used to avoid contact of the
sample with the air. The sample must be prepared
immediately after collection.
-------
- 17 -
DISSOLVED OXYGEN KITS AND PROBES
Portable kits and probes are available for field work.
These kits are satisfactory for operation control analysis. They
may be obtained from companies that supply laboratory equipment.
INHIBITOR FLOCCULATION MODIFICATION
DISSOLVED OXYGEN TEST
Copper Sulfate - Sulfamic Acid Floccu-lation Modification Dissolved Oxygen
Test
PURPOSE
This modification is used for biologic floes, such as activated-
sludge mixtures, which have high oxygen utilization rates.
How To Make The Test
1. Add 10 ml copper-sulfamic acid inhibitor to a 1 quart
wide-mouth bottle.
2. Add the sample to the bottle, at least 500 mis, stopper,
and mix by inversion.
3. Allow the suspended solids to settle quiescently and
siphon the relatively clear supernatant liquor into
DO bottle.
4. Continue the sample treatment as rapidly as possible by
the Full Bottle Winkler Method For Dissolved Oxygen
Test °n Pa8e 13.
-------
- 18 -
SOLUBILITY OF OXYGEN IN FRESH WATER TABLE
Temperature
°C
0
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
°F
32.0
33.8
35.6
37.4
39.2
41.0
42.8
44.6
46.4
48.2
50.0
51.8
53.6
55.4
57.2
59.0
60.8
62.6
64.4
66.2
68.0
69.8
71.6
73.4
75.2
77.0
78.8
80.6
82.4
84.2
86.0
Dissolved Oxygen
p .p .m.
14.6
14.2
13.8
13.5
13.1
12.8
12.5
12.2
11.9
11.6
11.3
11.1
10.8
10.6
10.4
10.2
10.0
9.7
9.5
9.4
9.2
9.0
8.8
8.7
8.5
8.4
8.2
8.1
7.9
7.8
7.6
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- 19 -
BIOCHEMICAL OXYGEN DEMAND (BOD) TEST
PURPOSE
The test measures primarily the organic polluting material in a
sample. This information may be valuable in:
1. Studying the organic (pollutional) load on a plant or
receiving stream
2. Determining the efficiency of sewage treatment
3. Pollution "control
OUTLINE OF PROCEDURE
1. Preparation of dilution water:
Aerate distilled water for 15 minutes or shake well
Add 1 ml of
buffer
CaCl2
FeCl3
Per liter of
Distilled Water,
Aerate for
15 minutes or
shake well
2. Pretreatment of samples, if indicated conditions exist.
-------
- 20 -
3. DILUTION PROCEDURE
SIPHON DILUTION WATER INTO CYLINDER
T
1100 ml.
DILUTION WATER
ADD SAMPLE TO THE CYLINDER
WITH THE USE OF A PIPETTE
OR GRADUATED CYLINDER
AIR
(for mixing)
1100 ml.
STIR
GRADUATED PLASTIC
CYLINDER
SIPHON SAMPLE INTO BOD BOTTLE
-------
- 21 -
4. IMMEDIATE 0.0. DETERMINATION AND INCUBATION
DILUTED
SAMPLE
2 DILUTED
SAMPLE (S)
DILUTION
WATER
DILUTION
WATER
DETERMINE
INITIAL D.O.
DETERMINE INITIAL
D.O. TO CHECK WATER
20 C. INCUBATOR
MAINTAIN WATER SEAL
WITH ALUMINUM FOIL OR
SMALL GLASS BEAKERS
IF NECESSARY. THIS
REDUCES WATER SEAL
EVAPORATION.
DETERMINE D.O. AFTER 5 DAYS INCUBATION
-------
- 22 -
PREPARATION OF REAGENTS
CHEMICALS REQUIRED (All chemicals should be of "analytical
reagent grade"-)
1. All chemicals and reagents for making dissolved oxygen
determination
2. Potassium acid phosphate, KJ^PO^
3. Potassium dibasic phosphate, K.HPO,
4. Sodium dibasic phosphate, Na HPO^-Tl^O
5. Ammonium chloride, NH^Cl
6. Magnesium sulfate, MgSO^*7H.O
7. Calcium chloride, CaCl2 (anhydrous)
8. Ferric chloride, FeCl3-6H 0
PREPARATION
Phosphate Buffer Solution
1. Dissolve 8.5 grams KH2P04, 21.75 grams K2HP04, 33.4 grams
Na2HP04•7H20, and 1.7 grams NfyCl in about 500 mis distilled
water.
2. Add distilled water to make 1 liter and mix thoroughly.
3. Stable for about 1 month.
Magnesium Sulfate Solution
1. Dissolve 22.5 grams MgS04'7H20 in distilled water.
2. Add distilled water to make 1 liter and mix thoroughly.
Calcium Chloride Solution
1. Dissolve 27.5 grams anhydrous CaCl2 in distilled water.
2. Add distilled water to make 1 liter and mix thoroughly.
-------
- 23 -
Ferric Chloride Solution
1. Dissolve 0.25 grams Fed -6H 0 in distilled water.
2. Add distilled water to make 1 liter and mix thoroughly.
How To Make The Test
1. Make sure that all the equipment and glassware are
thoroughly clean.
2. Preparation of Dilution Water:
(1) Store distilled water at 20°C for at least 24 hours.
This can be accomplished in an incubator set at
20°C.
(2) Bubble air through the volume of distilled water
needed for the samples for approximately 15 minutes.
(3) To the volume of distilled water add 1 ml of each
of the following reagents per liter of distilled
water:
a. Phosphate buffer
b. Magnesium sulfate
c. Calcium chloride
d. Ferric chloride.
(4) Aerate the dilution water for approximately
15 minutes.
3. Pretreatment of Sample:
(1) The sample must not contain residual chlorine. If
the residual is high, take a 100 ml portion of the
sample, add about 2 grams KI and 1 ml of concentrated
H2SO,. Titrate with 0.0375N Sodium thiosulfate, using
starch as an indicator just as in the DO test. Add
to the sample itself the amount of 0.0375N Sodium
thiosulfate Just determined as necessary to neutralize
the residual chlorine per 100 ml of chlorinated sewage
sample. Mix well and after 10 minutes check a portion
to be sure all residual chlorine is gone. Use this
for the BOD determination.
-------
- 24 -
(2) The sample must not be supersaturated with oxygen.
If the sample has a dissolved oxygen of more than
9.2 mg/liter (parts per million, ppm) at 20°C, it
is supersaturated. Shaking a bottle partially filled
with the sample, or bubbling air through it for
several minutes will remove the excess oxygen and
the sample may then be used without further
treatment.
4. Dilution Procedure:
Strong sewage must be diluted to give accurate results
in the BOD test. Accurate results can be obtained
by making the dilutions as follows in the ranges noted:
Recommended Dilution ml Sewage
Sewaee Strength Dilution Factor in 1100 ml
From 1-7 No Dilution 1 1100 ml
From 2-14 50% 2 550 ml
From 4-28 25% 4 275 ml
From 5-35 20% 5 220 ml
From 10-70 10% 10 110 ml
From 20-140 5% 20 55 ml
From 50-350 2% 50 22 ml
From 100-700 1% 100 11 ml
From 200-1400 1/2% 200 5.50ml
From 400-2800 1/4% 400 2.75ml
After the approximate strengths are estimated:
Raw is usually between 200 and 400 mg/1 BODs
Primary effluent between 30 and 233 mg/1 BOD5
Plant effluent between 10 and 50 mg/1 BOD5
The ml sewage can be determined from the end column above.
Place the needed amount of sewage in a one liter graduated
cylinder marked off at 1100 mis. Then fill the cylinder
with BOD dilution water to the 1100 ml mark. Mix by
bubbling air through. During this mixing the air bubbles
have only a minimum effect. From this point on, however,
one must exert every precaution to prevent any air
bubbles in bottles.
From the graduated cylinder fill (3), 300 ml BOD bottles
by siphoning from the cylinder and placing the tubing in
-------
- 25 -
the bottom of the BOD bottles filling to the point
of overflowing. Before inserting the stoppers be
certain no small air bubbles exist on sides of the
bottles. The best way to prevent any air bubbles
is to have the bottles clean and free of all grease.
Insert glass stopper and twist to seal. Maintain
water seal during incubation period.
Record the bottle numbers on the record sheet along with
the per cent dilution made. Place the two to be
incubated into ;lie incubator. The third sample is
ready to be titrated to determine the amount of
Dissolved Oxygen in the sample.
BOD results are most accurate when the oxygen in the
sample is just half consumed. If less than 20% or
over 70% of oxygen is consumed the results are of
questionable accuracy. If this happens when the next
dilutions are made, the dilutions should be increased
or decreased to try to obtain results in which approximately
half of the oxygen is consumed. A good "rule of thumb"
is at least 2 mis of depletion and 1 ml of oxypan left.
EXAMPLE FOR BOD CALCULATION
A 1/2% dilution has been made for a sewage with a strength of
between 200 and 1400 mg/1. 7.6 milliliters of 0.0375 normal sodium
thiosulfate were used in the initial titration on the dilution.
4.0 milliliters of the sodium thiosulfate were used in the incubated
dilution.
What is the BOD?
Initial
-Incubated
Multiply by
mg/1 BOD.
DISCUSSION
1. The biochemical oxygen demand determination is a measure of
the amount of oxygen required to oxidize the organic
matter in a sample in 5 days at 20° centigrade.
-------
- 26 -
2. The collection of the BOD sample must follow a
standard procedure. The same sampling points
are used for each successive sample.
3. A composite sample will be most representative
of the sewage to be tested. Eight hour composites,
hourly, should be the minimum.
4. The test consists of the determination of dissolved
oxygen prior to and following a period of incubation.
5. If the oxygen demand of the sample is greater than
the available dissolved oxygen then a dilution must
be made.
i
6. The amount of dilution depends upon the oxygen demand.
A series of dilutions are required for unknown sewage
samples.
7. Good overall operation of a secondary plant will
usually remove 85 to 95 per cent of the BOD.
-------
- 27 -
RELATIVE STABILITY - METHYLENE BLUE TEST
PURPOSE
The test for relative stability determines qualitatively the
stability of sewage or a treated effluent, namely the percentage
of the organic solids in the sewage which had been decomposed or
digested by the action of biological organisms and converted into
inert or stable chemical compounds not subject to further decomposition.
If all the available oxygen is consumed in a short period of
time, the sewage under examination contains a large amount of undigested
organic matter and therefore has a low stability value.
If the blue color remains for twenty or more days, complete
digestion or stability of all the sewage matter in the sample can
be assumed.
PREPARATION
Methylene Blue Solution
1. Dissolve 0.5 grams Ci6H18CIN3S-3H20 in about 500 mis
distilled water.
2. Add distilled water to make 1 liter and mix thoroughly.
HOW TO MAKE THE TEST
1. Clean a 300 ml DO bottle and rinse thoroughly.
2. Immerse the bottle in the liquid to be sampled and
completely fill with as little agitation as possible.
Chlorinated effluents cannot be used.
3. Add 0.8 ml of the methylene blue solution below the
surface of the liquid and mix by inversion.
4. Restopper the bottle so that no air bubbles remain
under the stopper.
5. Place in an incubator maintained at 20°C.
6. Observe daily and record the number of days or fractions
of days that elapse before the blue color disappears.
-------
- 28 -
Relative-Stability Numbers
Time required for
decolorization at
20°C, days
0.5
1.0
1.5
2.0
2.5
3.0
4.0
5.0
6.0
7.0
Relative stabil-
ity, per cent
11
21
30
37
44
50
60
68
75
80
Time required for
decolorization at
20 °C, days
8.0
9.0
10.0
11.0
12.0
13.0
14.0
16.0
18.0
20.0
Relative stabil-
ity, per cent
84
87
90
92
94
95
96
97
98
99
-------
- 29 -
SETTLEABLE, TOTAL AND SUSPENDED SOLIDS DISCUSSION
DISCUSSION
1. The settleable solids test is a measure of the amount
of solids in ml per liter which will settle in a given
period of time in an Imhoff cone or a graduated cylinder.
2. The sample should be a composite sample, although timed
grab samples are often used with the Imhoff cone. The
settleable solids of the mixed liquor using a graduated
cylinder is always a grab sample.
3. The test using an Imhoff cone gives the results of
settling in ml per liter and can be used to calculate
the efficiency of settling tanks, as well as to
calculate the amount of sludge which needs to be
removed from settling tanks.
A. The settleable solids test using a graduated cylinder
is used to determine the settlcability of the mixed
liquor in an activated sludge plant and in the
calculation of Che sludge index.
5. Total solids in sewage include suspended, dissolved,
settleable, and organic as well as inorganic solids.
The test is made in the following manner: An
evaporating dish is weighed and placed on a steam
or water bath. 50 or 100 ml of the sample is placed
in the dish and evaporated. The sample and dish is
then dried in the oven, cooled in the disiccat9r and
weighed. The increase in weight x 1,000,000 divided by
the ml of sample is equal to the mg/1 of total solids.
6. The results of suspended solids tests may be used to
evaluate the efficiency of the plant or the units in
a plant. These are the solids in suspension that may
be removed by filtering. A typical domestic sewage
of 1000 ppm of total solid will contain about 300 mg/1
suspended solids and approximately 85% of these solids.
or more, will be organic solids.
-------
- 30 -
Suspended solids may be determined by the Gooch Crucible
method or by the use of a spectrophotometer. Suspended
solids by the spectrophotometer method can be made in
approximately 5 to 10 minutes time, where as the Gooch
Crucible method will take about 2 or 3 hours or more.
The Gooch Crucible method, however, is the more reliable
and preferred test. The procedure for the spectro-
photometer method is as follows:
a. Shake sample well and pour about 700 ml
into the cylinder of a blender.
b. Blend for 90 seconds and transfer blended
liquor to a battery jar and stir.
c. While stirring siphon about 25 ml into the
cuvette.
d. With a 10,000 A setting on the spectrophotometer,
read the transmittance or absorbance scale
using distilled water as a blank.
e. Just before reading, invert the cuvette
gently to make sure all of the particles
are in suspension, (Do not shake.').
£. Read concentration of suspension solids
from prepared graph.
g. References: Determining Suspended Solids
Using a Spcctrophotoinetcr, Sewage and
Industrial Wastes, October, 1959.
h. Dissolved solids are inportant because
about 70% of total solids are in a dissolved
state and cannot be removed with primary
treatment. The greater portion of the
organic load on secondary treatment units
is dissolved solids.
-------
- 31 -
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200
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-------
- 32 -
SETTLEABLE SOLIDS TEST
IV
Settleable Solids; The determination
of settleable solids in sewage may be
accomplished by use of an Imhoff cone. The
Imhoff cone (as illustrated) is made of glass
or pyrex, is cone shaped and holds one liter
when filled to the graduation mark near the
top. The apex of the cone is graduated in
milliliters, usually 0 to 40 ml.
To determine the efficiency of a settling
tank or other plant unit two Imhoff cones
are necessary, as samples to both the influent
and effluent must be tested. The samples used
in this test may be either grab, timed grab,
or composite.
Imhoff Cone
PROCEDURE
1. Fill Imhoff cone to mark with well mixed sample of sewage
influent.
2. Fill another Imhoff cone to mark with well mixed sample of
sewage effluent.
3. Allow to stand for a period corresponding to detention time
in settling tank. (Usually two hours).
4. After sample has been standing for about three-fourths of
total time, dislodge material clinging to sides of cone
by giving it several twists, being careful not to disturb
solids already settled to bottom.
5. At the end of total time, read results and record as milliliters
per liter.
-------
- 33 -
CALCULATION OF RESULTS (Example)
Milliliters per liter in influent
'Less
Milliliters per liter in effluent
Milliliters per liter removed
9.0
.5
8.5
To find amount of settleable solids removed in percentage, the
following formula may be used:
Milliliters per liter removed x 100 = ent removed
Milliliters per liter in influent
TOTAL SOLIDS TEST
PURPOSE
1. The test measures the amount of suspended and dissolved
materials.
2. It may be used in studying plant loading and efficiency.
OUTLINE OF PROCEDURE
I. PREPARATION OF EVAPORATING DISH
MUFFLE FURNACE
COOL IN DESICCATOR
IGNITE DISH AT 600o C.
WEIGH
-------
- 34 -
2. TREATMENT OF SAMPLE
OVEN
POUR MEASURED VOLUME OF
SAMPLE INTO WEIGHED
EVAPORATING DISH
STEAM BATH
EVAPORATE ON STEAM BATH
OR IN A DRYING OVEN
WEIGH
COOL IN DESICCATOR
3. Recording of results
(1) record weight of evaporating dish
(2) record weight of dish with sample
(3) record volume of sample
HOW TO MAKE THE TEST
1. Ignite evaporating dish at 600°C. (If volatile solids are
not to be determined, the dish may be dried instead of
ignited).
2. Cool in desiccator for 20 - 30 minutes.
3. Weigh.
-------
- 35 -
4. Measure a 100 ml portion of well mixed sample in a
graduated cylinder.
5. Pour sample into ignited evaporating dish.
6. Evaporate to dryness on a steam bath or in a drying oven.
If a steam bath is used, the dish must be given a final
drying in a drying oven at 103°C.
7. Cool dish in desiccator for 20 - 30 minutes.
8. Weigh and record weight.
9. Calculation of total solids:
mg/liter (or ppm) total solids
• (weight in mg of evaporating dish with sample - weight in
mg of dish) x 1000
ml of sample
VOLATILE SOLIDS TEST
PURPOSE
1. The test measures the amount of volatile solids, that is,
the solids which are largely organic in nature and can be
destroyed by burning.
2. It may be used in studying
(1) plant loading
(2) digester loading
(3) active material needed for biological treatment by
activated sludge
Volatile solids may be determined on either total or suspended
solids.
-------
- 36 -
OUTLINE OF PROCEDURE
I. VOLATILE TOTAL SOLIDS
MUFFLE FURNACE
IGNITE DISH AT 600o C.
AFTER DETERMINATION OF
TOTAL SOLIDS
COOL IN DESICCATOR
WEIGH
TOTAL VOLATILE SOLIDS SLUDGE TEST (SHORT CUT)
1. Weigh a prepared evaporating dish on the balances. Record
weight.
2. Place a 100 gram weight on the balance.
3. Pour 100 grams well mixed sludge sample into the evaporating
dish.
4. Record the weight of the dish plus the 100 grams.
5. Evaporate to dryness , ignite at 600°C.
-------
- 37 -
6. Cool in desiccator.
7. Place on balances, add the weight of the dish. Add
weights to determine weight of sludge.
8. The weight of the dry sludge in grams is equal to the
percent total solids.
Example: Assume the evaporating dish weighs 75 grams. The
dish and sample would weigh 175 grams. After evaporation the'dish
and sample weigh 85 grams.
The percent total solids = weight of dish and sample - weight
of dish = 85 - 75 « 10 grams •= 10 percent total solids.
Ignite and cool percent ash =
(Weight of evaporating dish and sample - Weight of dish) 100
Weight of evaporated sample
Assume the weight of sample and dish is 75 grams after evaporation.
Percent Ash - (75 - 70) 100
10 Percent ash « 50
CENTRIFUGE METHOD FOR SUSPENDED SOLIDS TEST
PURPOSE
In this method the suspended solids are determined by centrifuging
tubes containing mixed liquor at a specific rate of spinning for a
definite period of time, reading the volumes of the sludge directly
in per cent from the graduations on the centrifuge'tubes, and multiplying
this reading by a factor to convert to mg/1 (ppm).
Outline of Procedure
Apparatus Required:
1. Centrifuge, clinical, with 4-place head for 15-ml
tubes.
\
2. Centrifuge tubes, API, 12.5 ml capacity graduated
In per cent.
3. Six beakers, low form, 250 ml capacity.
-------
- 38 -
How To Make The Test
1. Thoroughly mix the sample of the activated sludge
sample and pour about 100 mis into a 250 ml beaker.
2. Immediately pour the mixed liquor into two
centrifuge tubes up to the 100 per cent mark.
3. Centrifuge the tubes at about 2500 rpm for exactly
15 minutes.
4. When the centrifuge comes to a stop, read the
volumes of the sludge in the tubes directly in
per cent from the graduation on the outside of
the tubes.
5. Multiply this reading by a factor to roughly convert to
ppm (mg/1). The factor will range from 600 for a "young"
large floe sludge to 1000 for an "old" small floe sludge.
Example
Reading on the centrifuge tubes 4.5%
Multiplying reading by 800 gives 3600ppm
Notes
More accurate results may be obtained from data
showing direct relationships between actual results
of suspended solids by the Gooch Crucible Method
and the centrifuge tube readings.
GOOCH CRUCIBLE METHOD FOR SUSPENDED SOLIDS TEST
PURPOSE
This method is applicable to surface water, domestic and
industrial wastes, and saline waters. The practical range of the
determination is 20 mg/1 to 20,000 mg/1. A well-mixed sample
is filtered through a standard glass fiber filter, and the residue
retained on the filter is dried to constant weight at 103-105°C.
Non-homogenous particulates such as leaves, sticks, fish and lumps
of fecal matter should be excluded from the sample. Too much
residue on the filter will entrap water and may require prolonged
drying.
-------
- 39 -
Outline of Procedure
Apparatus Required:
1. Glass fiber filter discs, 4.7 cm or 2.2 cm,
without organic binder, Reeve Angel type 984H,
Gelman type A, or equivalent.
2. Filter holder, membrane filter funnel or Gooch
crucible adapter.
3. Suction flask, 500 ml.
4. Gooch crucibles, 25 ml (if 2.2 filter is used).
5. Drying oven, 103-105°C.
6. Desiccator.
7. Desiccant.
8. Analytical balance, 200 g. capacity, capable
of weighing to 0.1 mg.
How To Make The Test;
' *
1. Insert the disc into the bottom of a suitable
Gooch crucible.
2. While vacuum is applied, wash the disc with three
successive 20 ml volumes of distilled water.
Remove all traces of water by continuing to apply
vacuum after water has passed through.
3. Dry Gooch crucible and filter in an oven at
103-105°C for one hour. Remove to desiccator and
store until needed. Weigh immediately before use.
4. Assemble the filtering apparatus and begin suction.
Shake the sample vigorously and rapidly transfer
100 mis to the funnel by means of a 100 ml volumetric
cylinder. If suspended matter is low, a large
volume may be filtered.
5. Place in drying oven and dry at 103-105°C to constant
weight (usually overnight).
-------
- 40 -
6. Calculations:
Suspended Solids • (wt. of filter + residue - wt,
(mg/1) of Filter) X 1000
ml of sample filtered
Outline of Procedure (Graphically)
I. PREPARATION OF GOOCH CRUCIBLES
OVEN
COOL IN DESICCATOR
WEIGH
2. Treatment of Sample
Pour measured volume of sample
into Gooch crucible
(See next page.)
-------
- 41 -
PREPARED. WEIGHED GOOCH CRUCIBLE
DISTILLED WATER FOR WASHING
l^GOOCH CRUCIBLE WITH SAMPLE
— SUCTION
COOL IN DESICCATOR
WEIGH
-------
VOLATILE SUSPENDED SOLIDS TEST
MUFFLE FURNACE
PREPARE GOOCH CRUCIBLES AS
FOR SUSPENDED SOLIDS TEST
GO THROUGH PRODEDURE FOR SUSPENDED
SOLIDS. AFTER FINAL WEIGHING -
IGNITE CRUCIBLE AT 600o C.
J
COOL IN DESICCATOR
IGNITE AT 6000 C.
COOL IN DESICCATOR
WEIGH
-------
- 43 -
Recording of Results
1. Record weight of ignited dish or crucible.
2. Record weight of dish or crucible with sample (as in
total or suspended solids determinations).
3. Record weight of ignited dish or crucible with sample.
4. Record volume of sample.
HOW TO MAKE THE TEST '
1. Determine total solids in a pre-ignited evaporating dish
or suspended solids in a pre-ignited Gooch crucible.
2. Ignite dish and sample at 60QOC for 10-15 minutes, or until
a white ash remains.
3. Cool in desiccator for 20-30 minutes.
4. Weigh and record weight.
5i Calculations.
(1) Volatile total solids
mg/1 (or ppm) volatile total solids
«» (weight in mg. of ignited dish with sample - weight in mg.
of ignited dish with ignited sample) X 1000
ml of sample
per cent (%) volatile total solids
= mg/1 volatile total solids
mg/1 total solids X 10°
(2) Volatile suspended solids
mg/1 (or ppm) volatile suspended solids
• (weight in mg of ignited crucible with sample - weight
in mg of ignited crucible with ignited sample) X 1000
ml of sample
per cent (%) volatile suspended solids
* rcg/1 volatile suspended solids
mg/1 suspended solids X 1.°°
-------
- 44 -
(3) Fixed total solids
• total solids - volatile total solids
(4) Fixed suspended solids
• suspended solids - volatile suspended solids
SETTLEABLE SOLIDS IN ACTIVATED SLUDGE TEST
1. Fill Mallory Direct Reading Settlometer or any other large
diameter graduated cylinder to 1000 cc/1 mark with thor-
oughly mixed activated sludge.
2. Allow solids to settle quietly for 30 minutes.
3. Read the volume of solids in the bottom of the container.
4. Report the results as mis of settleable solids per liter.
SLUDGE VOLUME INDEX
Sludge volume index is defined as the volume in milliliters
occupied by 1 gram of activated sludge.
Settleable solids in ml per liter x 1000 „, ,
mg/1 suspended solids = SludSe Volume Inde*
SLUDGE DENSITY INDEX
Sludge density index is defined the reciprocal of the sludge
volume index multiplied'by 100.
Sludge Volume Index x 10° = Slud8e Density Index
SLUDGE AGE
In the activated sludge process, sludge age is defined as a measure
of the length of time a particle of suspended solids .has been undergoing
aeration, expressed in days. It is usually computed by dividing the
weight of the suspended solids in the aeration tank by the daily addition
of new suspended solids having their origin in the raw waste. Assuming
that no sludge blanket exists in the final clarifier:
-------
- 45 -
Volume of aeration tank (million gal.) x 8.34 x mg/1 SS _
Settled sewage daily flow (million gal.) x 8.34 x (P.E.-F.E.) mg/1 SS
= Sludge Age
Where P.E. = primary effluent SS and F.E. = final effluent SS.
Total pounds of activated sludge _ = Sludge Aee
Total pounds SS removed from primary effluent per day B
SPECIFIC GRAVITY OF SEWAGE SLUDGE
A. REAGENTS AND APPARATUS:
1. Distilled water.
2. Trip scale or balance.
3. One wide mouth glass stoppered bottle or flask of
about 8 oz. capacity or more.
B. PROCEDURE
1. Weigh the bottle or flask to the nearest 0.1 gram,
2. Fill to overflowing with distilled water, insert the
stopper, dry with a cloth and weigh.
3. Completely empty the bottle, fill to overflowing with the
wall-mixed sludge and insert the stopper.
4. Wash the sludge from the outside of the bottle or flask,
dry with a cloth and weigh.
C CALCULATIONS:
Example: Weight of bottle and distilled water 550.5 grams
Weight of bottle _ 250.5- grams
Weight of distilled water 300.0 grams
Weight of bottle and sludge 556.5 grams
Weight of bottle _ 250.5 grams
Weight of sludge 306.0 grams
306
30Q • 1.02 Specific gravity
-------
SLUDGE CONDITION FOR VACUUM FILTRATION
Grab a sample of ferric chloride and lime from the conditioning
tanks. (These chemicals may be other than ferric chloride and lime).
1. Measure five 200 ml portions of sample into five
400 ml beakers. Number beakers 1 to 5.
2. Add 1.0, 2.0, 3.0, 4.0 and 5.0 mis of ferric chloride
to the respective samples. Stir gently about 30
seconds.
3. Determine filtration time as described above.
4. Using that quantity of ferric chloride that requires
three or four minutes to filter, repeat the test as
follows.
5. Add the ferric chloride dose to each of five 200 ml
samples. Stir 30 seconds and then add 1.0, 2.0,. 3.0,
4.0 and 5.0 mis of the well-mixed lime solution to
each sample. Stir and determine filtration time as
above. pH value should not exceed 1.0.
6. Determine the optimum combination of ferric chloride and
lime that will yield a filtration time of about two
to three minutes. Less than one minute is better
than necessary and more than four minutes is unsatisfactory.
CALCULATIONS
Ml of ferric chloride used = gallons ferric chloride per-200 gallons sludge.
Ml lime solution used = gallons lime solution per 200 gallons-sludge.
-------
- 47 -
AMMONIA NITROGEN TEST
A. REAGENTS
1. Ammonia free water
2. Permanent ammonia standards
3. Standard ammonium chloride
4. Messier reagent
5. Sodium hydroxide, 12N
6. Copper sulfate solution, 10 percent
B. PROCEDURE
1. Place 100 ml. of the sample in a Nessler tube and add 1 ml.
copper sulfate solution.
2. Mix by rotating and add 1 ml. of sodium hydroxide.
3. Mix again and allow to settle.
4. Pipette a measured portion of the clear supernatant liquor.,
25 mis., depending upon the ammonia content, into a
second Nessler tube and dilute to 100 ml. with ammonia free
water.
5. If permanent ammonia standards are available, proceed to
Step 6. If not, make up temporary standards by adding
0.2, 0.4, 0.6, 0.8, 1.0, 1.4, 1.7, 2.0, 2.5, 3.0 ml. of
standard ammonia chloride to 100 ml. Messier tubes and
dilute to the mark with ammonia free water.
6. Add 2 ml. of Nessler reagent to the sample and to each
temporary standard (if used).
7. After 10 minutes compare the colors and record the standard
having a color nearest to that of the sample.
C. CALCULATIONS
a. Using permanent standards:
mg NH-j-N in permanent standard x 1000 ,, .
ml. portion used in step 4 = mg/1 Ammonla nitr°S**
b. Using temporary standards:
ml. NH4C1 in standard x 10 „ fi Ammonia nitrogen as „
ml. portion used in step 4
-------
- 48 -
NITRITE NITROGEN TEST
A. REAGENTS
1. Aluminum hydroxide
2. Standard sodium nitrite
3. Sulfanilic acid
4. A - napthylamine
B. PROCEDURE - FILTER SAMPLE
1. If the sample is colored or turbid, clarify 150 ml by
adding 2 ml of aluminum hydroxide.
2, Place a measured portion of the filtrate (10-50) ml,
depending upon the nitrite content, into a 100 ml
Nessler tube and make up to the mark with distilled water.
3. If permanent standards are available, proceed to Step 4;
if not, make up temporary standards by adding 0.2, 0.4,
0.6, 0.8, 1.0, 2.0, or 2.5 ml of standard sodium nitrite
in 100 ml Nessler tubes and make up to the mark with
nitrite free water.
4. Add 2 ml of sulfanilic acid and 2 ml of a-naphthylamine to
the sample and to each temporary standard if used.
5. Mix and allow to stand 10 minutes. Compare the colors and
record the stand, rd having a color nearest *to that of the
sample.
C. CALCULATIONS
a. Using permanent standards:
mg NQa-K in permanent standard x 1000 ,, .„„ .
-* 2 ml of sample ' **fl Nitrite nitrogen as N
b. Using temporary standard:
ml standard NaN02 x 0.5 * mg/i Nitrite nitrogen as N
ml of sample
NITRATE NITROGEN TEST
A. REAGENTS
1. Phenoldisulfonic acid
2. Sodium hydroxide, 12N
3. Standard nitrate solution
-------
- 49 -
B. PROCEDURE
1. Determine chloride content of water using the CHLORIDES
IN SEWAGE TEST found on page 52.
2. Remove the chlorides present by the CHLORIDES REMOVAL PROCEDURE
found on page 72.
3. Filter 30-35 ml of sample through filter paper.
4. Evaporate 25 ml or the filtrate to dryness on a water bath,
(use a smaller amount if nitrate content is high).
5. Moisten the residue with 1 ml of phenoldisulfonic acid.
6. Dilute to about 20 ml with distilled water.
7. Add 12N sodium hydroxide until the maximum yellow color is
developed (not more than 5 to 6 ml or sodium hydroxide will be
required).
8. Filter into a 100 ml Nessler tube and rinse the dish and paper
with distilled water. Add the filtered rinsings to the filtrate
and make up to the mark with distilled water.
9. If permanent standards are available, proceed to Step 8; if not,
make up temporary standards by placing 0.2, 0.4, 0.6, 0.8, 1.0,
2.0, 3.0, 4.0, and 5.0 ml of standard sodium nitrate solution in
100 ml Nessler tubes and adding 2 ml of 50% sodium hydroxide.
10. Dilute to the mark with distilled water.
11. Compare the color and record the standard having a color nearest
to that of the sample.
C. CALCULATIONS
a. Using permanent standards:
mg NOq-N in permanent standard x 1000 .
ml of sample in step 2" rag/1 Nitrate nitrogen as N
b. Using temporary standards:
ml of standard NaNO-i x 10 ,,
ml of sample in Step 2 " m*/l Nltra^ nitrogen as N
SULFITE TEST
1. Place 10 ml of 0.025N iodine and 5 ml of glacial acedic
acid into each of two 250 ml Erlcnmeyer flasks.
2. Add 100 ml of the freshly collected and cooled, but
unfiltered, sample slowly and with constant mixing to one
flask and 100 ml of distilled water to the other.
-------
- 50 -
3. To the flask containing the sample add from a burette
0.025N sodium thiosulfate until the color of the iodine
almost disappears. Add 1 ml of starch indicator and
continue the addition of thiosulfate until the blue color
just disappears. Record the ml of thiosulfate used.
CALCULATIONS
Let D = ml of thiosulfate used for distilled water
Let S = ml of thiosulfate used for sample
(D-S) x 0.91 = gpg sodium sulfite (Na2S03)
To convert gpg to mg/1 multiply by 17.1
SULFATE TEST
SULFATES - BENZIDINE METHOD
1. If the sample contains suspended matter, filter about
70 ml through a filter paper.
2. Measure 58.3 ml of the filtered sample into a 250 ml
Erlenmeyer flask.
3. Add 10 ml of benzidine hydrochloride solution (2 per cent)
and mix by giving the flask a whirling motion.
4. Allow the mixture to stand for about ten minutes.
5. Filter the precipitated benzidine sulfate onto a small
filter paper. The solution should be refiltered through
the same paper until filtrate is clear.
6. Add 1 ml of benzidine hydrochloride solutibn to the
filtrate. If further precipitation takes place, filter
through the same paper. Repeat the addition of benzidine
sulfate until all of the sulfate is precipitated and
removed to the paper.
7. Wash the flask and precipitate on the paper with several
small portions of distilled water. Allow each portion to
drain through the paper before the next is added.
8. Transfer the paper containing the benzidine sulfate to
the original flask, add obout 25 ml of distilled water and
two drops of phenolphthalein indicator.
-------
- 51 -
9. Add 0.143N (N/7) sodium hydroxide from a burette
until the first permanent pink color is obtained.
Be sure that the paper is completely disintegrated
and that the color is permanent.
10. Record the ml sodium hydroxide used.
CALCULATIONS
Ml of NaOH x 10 = gpg 804 as sodium sulfate (Na2S04>
Ml of NaOH x 6.32 =• gpg 804
To convert gpg to mg/1 multiply by 17.1
CARBON DIOXIDE TEST
1. Fill a 100 ml Nessler tube to the mark with the sample.
2. Add 10 drops of phenolphthalein indicator.
3. Add N/44 sodium hydroxide from a burette, stirring gently,
until a slight permanent pink color appears. Record the
number of ml of sodium hydroxide used.
CALCULATIONS
Ml of N/44 NaOH X 10 = mg/1 C02
Test should be made at time the sample is collected. If the sample
has a high C02 content, about 3/4 of the NaOH required should be
added to the beaker before adding the sample.
HYDROGEN SULFIDE TEST
A. EQUIPMENT NEEDED
1. One 1000 ml capacity graduated cylinder.
2. Two 250-500 ml capacity Erlenmeyer flasks.
3. Pipette
4. Siphon
B. CHEMICALS NEEDED
1. 0.025 N iodine solution
2. Potassium iodide crystals
3. 0.025 N sodium thiosulfate
4. Starch indicator
-------
- 52 -
C. METHOD
1. Siphon 500 ml of the sample into a graduated cylinder.
2. Pipette 10 ml of the Q.Q25 X iodine solution into each of
two Erlenmeyer flasks.
3. Add about 1 gram of potassium iodide crystals.
A. Add 200 ml of distilled water to one flask.
5. Siphon 200 ml of sample from graduate into other flask.
6. Titrate both the distilled water blank and the sample
with 0.25N Sodium thiosulfate using starch as an
indicator near end of titration. Record ml of thiosulfate
used.
D. CALCULATIONS
Let x = ml of Sodium thiosulfate used for sample
Let y *> ml of Sodium thiosulfate used for distilled water
(y-x) x 426 ., . „ J ,rjj
ml of sample " mg/1 of Hydr°8en sulfide
CHLORIDES IN SEWAGE TEST
REAGENTS AND APPARATUS
1. Standard silver nitrate solution (1 ml equivalent of
0.5 mg chloride ion)
2. Potassium chromate indicator - 5 per cent solution
3. Chloride free sodium bicarbonate
A. 25 ml burette
5. 200 ml Erlenmeyer flask or porcelain casserole
PROCEDURE
1. Pipette 50 or 100 mis of the sample into the flask or
casserole, depending upon the chloride content•
2. Add 1 ml potassium chromate indicator.
-------
- 53 -
3. Titrate to first permanent red color with standard
silver nitrate. If more than 7 or 8 mis of silver
nitrate are required, repeat entire procedure, using
a smaller sample diluted to 50 mis with chloride
free distilled water.
4. Calculate chloride content as follows:
(ml silver nitrate - blank) x 500 /, , , J ,
ml of sample - mg/1 chloride
PHOSPHATE TEST
Phosphates are usually found in wastewater. Detergents contain
phosphates and polyphosphates may be present in addition to the usual
orthophosphate.
For differentiation of ortho and polyphosphates, consult
"Standard Methods" and "FWPCA Methods For Chemical Analysis Of Water
and Wastes," November, 1969.
Color comparators are available for making phosphate analyses.
These analyses are satisfactory for field work and operation control
analyses.
ALKALINITY SEWAGE TEST
NOTE: The alkalinity determination may be performed more accurately
using the Potentiometric Titration Method given for the
ALKALINITY SLUDGE TEST.
1. Pipette 100 mis of the sample in an Erlenmeyer flask or
beaker.
2. Add three drops of phenophthalein indicator to the
sample.
3. If the sample becomes pink, add 0.02N sulfuric acid from
a burette until the pink color just disappears and record
the number of mis of acid used.
4. Add 3 drops of methyl orange indicator to the sample.
5. If the sample becomes yellow, add Q.02N sulfuric acid until
the first difference in color is noted. The end point is
orange. Record the mis of acid used.
-------
- 54 -
CALCULATIONS
Total alkalinity as mg/1 CaC03 = total mis acid used x 10
Hydroxide (OH) - normal carbonate (C03> - and bicarbonate (HC03>
are determined below.
P • ml of 0.02N sulfuric acid used for the titration with phenolphthalein
T • ml of acid used for total titration (phenolphthalein plus methyl
orange)
There are five possible conditions:
1. P « T
Hydroxide mg/1 = P x 10
2. P > 1/2 T
Hydroxide mg/1 - (2P - T) x 10
Normal carbonate mg/1 = 2(T - P) x 10
3. P - 1/2 T
Normal carbonate mg/1 = T x 10
4. P
-------
- 55 -
4. Titrate with 0.02N sulfuric acid stirring the sample
during titration. When the meter reads 8.3 record
mis acid used.
5. Continue to titrate with 0.02N sulfuric acid until
meter reads 4.5. Record mis acid used.
CALCULATIONS
Total alkalinity as mg/1 CaC03 = total mis acid used x 10
Hydroxide (OH) - normal carbonate (C03) - and bicarbonate (HC03)
are determined below.
P " ml of 0.02N sulfuric acid used for the titration to pH 8.3
T » ml of acid used for total titration (above pH 8.3 plus acid
used to 4,5)
There are five possible conditions:
1. P - T
Hydroxide mg/1 » P x 10
2. P 5*1/2 T
Hydroxide mg/1 = (2P - T) x 10
Normal carbonate mg/1 • 2(T - P) x 10
3. P • 1/2 T
Normal carbonate mg/1 a T x 10
4. P < 1/2 T
Normal carbonate mg/1 = 2P x 10
Bicarbonate mg/1 - (T - 2P) x 10
5. P - 0
Bicarbonate mg/1 • T x 10
All of the above results are in terms of mg/1 as CaC03.
ACIDITY SEWAGE TEST
1. Pipette 100 mis of the sample into an Erlenmeyer flask
or beaker.
2. Add 3 drops of phenolphthalein indicator.
3. Add 0.02N sodium hydroxide from a burette until the first
permanent pink color appears and record the number of mis
of sodium hydroxide used.
-------
- 56 -
CALCULATIONS
Ml of 0.02N NaOH x 10 = mg/1 total acidity expressed in terms
of CaC03
ACIDITY SLUDGE TEST
APPARATUS
Use a commercial instrument for measuring pH with a glass electrode.
Adjust meter to a pH of 7.0.
1. Measure 100 mis of the settled sample and pour into
a beaker.
2. Measure the pH.
3. Add 0.02N sodium hydroxide from a burette until the
pH meter reads 8.3. Record number of mis of sodium
hydroxide used.
CALCULATIONS
Ml of 0.02N NaOH x 10 • mg/1 total acidity expressed in terms of CaC03.
CHLORINE DEMAND AND STANDARD SOLUTIONS
1. Chlorine demand of a water must be satisfied before a
residual can be produced. The materials causing the
chlorine demand are: bacteria, organic matter, and
some minerals.
2. Chlorination of water and sewage for sterilization and
odor control is being practiced in many treatment plants.
To calculate the dosage, the demand will have to be
known. There are a number of methods used for the
chlorine demand determination. The one used in this
manual is simple and accurate. This method uses a series
of samples treated with varying amounts of chlorine.
The sample with the least amount of added chlorine, which
shows a residual, is used in calculating the chlorine
demand.
-------
- 57 -
3. The chlorine demand of sewage varies widely from
hour to hour. This variation is greater for raw and
settled sewage than for final effluents. The
chlorine demand of raw sewage is usually greater in
warm weather than in winter. There is a close
relationship between the chlorine demand and the oxygen
demand of sewage.
4. The greatest benefit from the use of chlorine in
sewage works operation is for disinfection of the
plant effluent. A dosage sufficient to produce a
residual of 0.5 mg/1 after 30 minutes contact time
should be maintained. The purpose of chlorination
is to destroy harmful bacteria. Other uses may be
made of chlorine as it is a strong oxidizing agent.
5. Bleach is often used for preparing solutions for
the chlorine demand test.
SOLUTION FOR CHLORINE DEMAND TEST
Pipette exactly 20 mis of "purex" (5% chlorine solution) into a one
liter volumetric flask and fill to the mark with distilled water.
This solution will contain 1000 mg/1 of chlorine.
1 ml of solution in 1 liter of sample is equal to 1 mg/1.
1. Measure 250 mis of the well-mixed sewage to be
tested into a series of eight 300 ml capacity
beakers.
2. Add 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8 mis
of the chlorine solution to the beakers in'
succession.
3. Mix each beaker by gently shaking and allow to
stand for 30 minutes.
4. Add a crystal of potassium iodide and 1 ml of
starch solution to each beaker and mix.
5. Record the mis of chlorine water in the beaker
containing the least amount of chlorine water
which shows a blue color.
-------
- 58 -
6. Ml of chlorine water in first bottle to show
a blue color x 4 •= mg/1 chlorine demand.
JAR TEST FOR BLUE GREEN ALGAE CONTROL
(Amount of HTH to Control Blue Green Algae)
Pipette exactly 20 mis of "pur ex" (5% chlorine solution) into
a one liter volumetric flask and fill to the mark with distilled
water. This solution 'will contain 1000 mg/1 of chlorine.
One ml of solution added to one liter of sample is equal to
one mg/1.
Measure 250 mis of the well-mixed sewage to be tested into a
series of eight 300 ml capacity beakers. Quart jars can be
substituted for the beakers. Add 1.0, 1.5, 2.0, 2.5, 3.0, 3.5, 4.0
and 4.5 of the chlorine solution to the beakers in succession.
Mix each beaker gently shaking and allow to stand for one
hour.
Observe the containers. The first one indicating the algae
has been bleached out is the correct dosage.
Pounds HTH per acre lagoon Milliliter chlorine water
3-foot depth " applied to jar _ x 8.34 x 4
70
EXAMPLE: Assume jar No. 5 indicated the algae had been bleached.
OIL AND GREASE TEST
1. Determine the tare weight of a clean and dried
125 ml E-flask.
2. Place 500 mis of sample in a 1000 mis separatory
funnel. Add 1.25 ml of concentrated ^SO^ to the
sample. Rinse the sample container with 15 mis
of Petroleum Ether (30°-60°C).
-------
- 59 -
3. Add 25 mis of additional Petroleum Ether to the
separatory funnel, shake, and allow the ether
layer to separate out. Drain out the H2
-------
- 60 -
4. Filter the acidified sample through the prepared
filter. Apply vacuum until no water passes through
the filter.
5. Remove the filter paper to a watch-glass by means
of forceps, adding the materials adhering to the
edges of the muslin cloth disc; wipe the collecting
vessel, the stirring rod, and Buchner funnel with
filter paper to remove all grease and solids
materials. Add the filter paper to that on the
watch-glass and roll them together and fit in a
paper extraction thimble.
6. Dry at 103°C - 30 minutes.
7. Weigh extraction flask and extract grease in a
Soxhlet apparatus using petroleum ether at a rate
of 20 cycles per hour for 4 hours.
8. Distill ether from the extraction flask in a
water bath at 70°C.
9. Dry by placing the flask on a steam bath and draw
air through the flask by means of vacuum applied
for 15 minutes.
10. Cool in a desiccator one-half hour and weigh.
CALCULATIONS
Total grease mg/1 - mg increase in weight of flask x 1000
ml sample
pH OF SEWAGE SLUDGE — COLORIMETRIC METHOD
HYDROGEN ION CONCENTRATION (pH) OF SEWAGE SLUDGE
COLORIMETRIC METHOD
1. Place about 20 ml of the sludge in a 100 ml.
graduate and dilute with distilled water to 100 ml mark.
2. Mix well and settle. (The sludge may be clarified
by centrifuging instead of using the procedure
given in Steps 1 and 2.)
-------
- 61 -
3. Place 10 ml of supernatant liquor into each of
the two or three tubes provided with the pH
apparatus.
4. To one tube add the correct amount of indicator.
5. Place the tubes in the comparator in such a manner
that the color standards are opposite the tubes
not containing the indicator. The color comparison
must be made by looking through the same thickness
of liquid having the same color and turbidity as
the sample.
6. Compare the colors and select the standard having
a color nearest to that of the sample.
HYDROGEN ION CONCENTRATION (pH) OF SEWAGE
pH OF SEWAGE — COLORIMETRIC METHOD
1. Place 10 mis of sample into each of the two or
three tubes provided with the pH apparatus.
2. To one tube add the correct amount of indicator.
3. Place the tubes In the comparator in such a
manner that the color standards are opposite the
tubes not containing the indicator. The color
comparison must be made by looking through the
same thickness of liquid having the same color
and turbidity of sample.
4. Compare the colors and select the standard having
a color nearest to that of the sample.
HYDROGEN-ION CONCENTRATION DISCUSSION
The acid or alkali intensity, hydrogen-ion concentration, of a
solution is found by determining the pH.
Ions are electrically charged atoms or groups of atoms. When
acid base or salt is dissolved in a suitable solvent the molecules
dissociate into smaller units, some of which have a positive electric
charge and others are equal negative charge. For example:
-------
- 62 -
Hydrochloric acid dissociates into positively charged hydrogen
ions and negatively charged chlorine ions. HCl-?=i_H"*' + Cl~
Water dissociates into positively charged hydrogen ions and
negatively charged hydroxyl ions. HOHf=? H+ + OH~
It has been determined that there are 1/10,000,000 grams of
hydrogen ions and the same quantity of hydroxyl ions in one liter
of pure water.
The product of the H and OH ions equal a constant"value.
Therefore, if the concentration of H ions is increased there is a
corresponding decrease in OH ions. For example:
If the concentration of H ions is increased from 1/10,000,000
(10~7) to 1/100,000 (10~5) then the OH ions are decreased from
1/10,000,000 or (10-7) 1/1,000,000 (10~9) gram.
The acidity or alkalinity, hydrogen-ion concentration, of a
solution is given in terms of the pH. For convenience the negative
exponent of the hydrogen ion concentration is used to express the
amount of hydrogen ions present: For example:
If a solution has a hydrogen-ion concentration of 1/100,000
or 10~5, the pH value is 5.0.
The pH scale extends from 0 to 14 with the neutral point at
7.0. As the pH value decreases the hydrogen-ion concentration
increases, and vice versa. A change in pH value is not in direct
proportion to the numerical values. A change of 1 in pH value
means the hydrogen ion concentration has changed 10 times. A
change of 2, 100 times etc.
pH value may be determined colorimetrically. The color of
certain dyes change as the pH value of the solution changes.
Indicators available for use and their effective range in
determining pH value are as follows:
INDICATORS FOR pH DETERMINATION
NAME pH RANGE COLOR CHANGE
Methyl Red A.4 to 6.0 Red to Yellow
Brom Cresol Purple 5.2 to 6.8 Yellow to Purple
Brom Thymol Blue 6.0 to 7.6 Yellow to Blue
Phenol Red 6.8 to 8.4 Yellow to Red
-------
- 63 -
NAME pH RANGE COLOR CHANGE
Cresol Red 7.2 to 8.8 Amber to Red
Thymol Blue 8.0 to 9.6 Yellow to Blue
Color comparators can be purchased for making this test. Electric
pH meters can also be purchased for making this test. Determination of
pH with an electric pH meter may be more accurate than with colorimetric
methods.
ACIDS — VOLATILE
This test is useful for early detection of malfunction in
digesters. The distillation procedures are cumbersome and give
results varying with the type of apparatus, composition of the
acids, distillation rate, and amount distilled. In this method,
no distillation is necessary. The volatile acids are titrated
directly after removal of the bicarbonate ions as carbon dioxide.
APPARATUS AND REAGENTS
Buffer solution, 4.00 and 7.00
Standard 0.02N sulfuric acid solution
Standard 0.02N sodium hydroxide (NaOH)
25 ml pi,ctte or graduate to measure sample
10 ml graduated pipette or burette for titrating
250 ml beaker
Adjustable hot plate
Electronic' pH meter
PROCEDURE
1'. Set the pH meter at 7.0 using the 7.0 pH buffer
or centrifuging sample.
2. Measure a known quantity of clear sample into a 250 ml
beaker or Erlenmeyer flask and insert the glass electrode
of the pH meter. Usually 25 ml is sufficient, but smaller
amounts may be advisable if the alkalinity is high.
3. Titrate with .02N sulfuric acid to pH 4.0 while swirling
the contents of the beaker. The glass electrode should
be held firmly against the side of the beaker during
this procedure Co prevent breakage. Record this value
as alkalinity. Continue titrating to pH 3.5 to 3.3.
-------
- 64 -
4. Carefully set the pH meter by using a 4.00 pH
buffer while lightly boiling the sample a minimum
of 3 minutes. Cool in cold water to original
temperature.
5. Titrate sample with standard 0.02N sodium hydroxide
up to pH 4.00 and note reading. Continue titrating
to pH 7.0 and note readings.
6. Calculate volatile acid alkalinity (volume required in
#5 to go from pH 4.0 to pH 7.0).
Volatile Acid Alkalinity = ml 0.02N NaOH x 1000
ml sample
7. Calculate Volatile Acids
Volatile Acids = Volatile acid alkalinity (when this
value is less than 180 mg/1)
Volatile Acids - 1.5 x Volatile Acid Alkalinity (when
this value is more than 180 mg/1)
CARBON DIOXIDE IN SEWAGE GAS
1. Waste a portion of the gas to the air in order to
clear the lines and to obtain a representative
sample. If the gas is not piped to the laboratory,
a sample may be collected at any convenient
place on the gas domes or from the lines to the
burners. It should be collected in a flat rubber
gas bag capable of holding about 1 liter.
2. Raise the leveling tube and fill the measuring
pipette completely with the liquid (mercury is
preferred).
3. 'Attach the bag or pipe line and draw about 100 mis
of the gas into the pipette by lowering the
leveling tube.
-------
- 65 -
4. Close the stopcock connecting the gas bag or gas
line and carefully measure the volume of gas in
the pipette. Let this volume in ml = A. (The
volume of gas in the pipette should always be
measured by holding the level of the liquid in
the leveling tube at '•.he same elevation as that
in the pipette.)
5. Open the connection to the potassium hydroxide
(100 grams dissolved in 200 mis distilled water)
pipette and pass the gas into the pipette, allowing
it to remain in contact with the solution for some
time.
6. By lowering the leveling tube, bring back the entire
volume of remaining gas into the measuring pipette.
7. Close the connection and measure the volume
as before.
8. Repeat steps 5, 6 and 7 until there is no further
gas absorbed from contact with the potassium hydroxide
solution.
NOTE - The apparatus must be free from leaks. Keep the glass stopcocks
well greased.
CALCULATIONS
ml of gas absorbed X 100
£ • per cent carbon dioxide
Gas analysis equipment can be obtained from companies supplying
laboratory equipment. They are easier for the operator to use for
making gas analysis.
HYDROGEN, METHANE AND B.T.U. IN SEWAGE GAS
1. Record the volume of gas remaining in the measuring
pipette from the carbon dioxide determination. Let
the volume in mis « B.
-------
- 66 -
2. Discard all but 10 mis of this gas.
3. Lower the leveling tube and open the stopcock to
the air, drawing in air until the volume is about
95 to 100 mis.
4. Measure accurately the volume in mis of the mixture.
5. Allow the gases to mix thoroughly.
6. Close the stopcock and the clamp on the leveling
tube connection and explode or burn the gas in the
pipette.
7. Allow the gas to cool to room temperature, open the
check on the leveling tube and read the volume in
mis of gas remaining in the pipette.
8. Determine the amount of carbon dioxide produced
by passing the gases into the potassium hydroxide
pipette several times until no further loss in
volume is obtained.
9. Again read the volume of gas in measuring pipette.
Let mis in step No. A - mis in step No. 7 = C.
Let mis in step No. 7 - mis in step No. 9 • D.
CALCULATIONS
10BD
—j— = ..per cent methane
6.67 B (C - 2D) L ,
£ • per cent hydrogen
(Per cent methane X 10.03) + (per cent hydrogen X 3.29) = B.T.U.
per cubic foot (high heat value, 62°F and 760 mm)
(Per cent methane X 9.13) + (per cent hydrogen X 2.81) = B.T.U.
per cubic foot (low heat value, 62°F and 760 mm)
Gas analysis equipment can be obtained from companies supplying
laboratory equipment. They are easier for the operator to use for
making gas analysis.
-------
- 67 -
BACTERIAL EXAMINATION
(Membrane Filter Method)
SAMPLE COLLECTION
Take the sample with top of the bottle upstream or into flow;
If no flow, use a sweeping motion moving top of bottle away from
hand. Fill bottle only about two-thirds full to allow room for
shaking. The hand must be kept away from the mouth of the bottle.
PREPARATION OF MED'IA AND REAGENTS
Buffered Dilution Water
Stock Phosphate Buffer Solution
Dissolve 34 grams potassium dihydrogen phosphate (KH2P04) in
500 mis distilled water, adjust to pH 7.2 with IN NaOH and make
up to 1 liter with distilled water. Add 1.25 mis stock phosphate
buffer to each liter of distilled water used for dilution bottles,
rinse water and dilution water used in filter apparatus.
Autoclave at 121°C at 15 psi for 20 minutes.
Dilution Bottle Preparation
The bottle should be filled with the proper amount of the
buffered dilution water so that after autoclaving the volume
is 99 mis + 2 mis.
M-Endo Media
To each 980 mis distilled water add 20 mis 95% ethel alcohol
and dissolve 48 grams dehydrated media. Place flask containing
media in water bath, bring media just to the boiling point.
Dispense 1.8 to 2.0 mis to each dish with pad to be used (make
sure pad is saturated).
M.F.C. Broth Media
Dissolve 3.7 grams dehydrated M.F.C. Broth Base in 100 mis
distilled water. Add one ml IX rosolic acid solution. Place
flask containing media in water bath, heat media to boiling,
cool to room temperature, and add about 2 mis to each dish and pad
to be used.
(Rosolic Acid Preparation - Dissolve one gram rosolic
acid in 100 mis. 0.2N sodium hydroxide)
-------
- 68 -
K.F. Streptococcus Agar
Dissolve 7.6 grams dehydrated media In 100 mis distilled water
in sterile flask with aluminum foil cover, Place the flask In a
boiling water bath, melt the dehydrated medium and leave In the
boiling water bath an additional 5 minutes. Cool the medium to
50-60°C, add 1.0 ml of TPTC reagent and mix. Pour 5-8 mis to each
50 mm dish.
(TPTC -2,3, 5 triphenyl tetrazolium chloride is
prepared by adding one gram to 100 mis distilled
water bringing to a boil. Store in screw-capped
tube in refrigerator until use.)
PREPARATION OF APPARATUS
Sample Bottles
Autoclave at 121°C at 15 pounds pressure for 20
minutes.
Pipettes
Sterilize in oven at 180°C for 2 hours in pipette cans, or
autoclave at 121°C at 15 psi for 20 minutes.
Filter Apparatus
Autoclave at 121°C at 15 pounds pressure for 20 minutes,
or use ultraviolet light. The funnel need not be sterilized
between samples of low bacterial density, but should be
rinsed well. Where samples are highly contaminated,
apparatus should be sterilized between each sample either by
boiling or ultraviolet light.
Forceps
Sterilize between each operation by dipping in ethyl
alcohol and burning off.
-------
- 69 -
TOTAL COLIFORM
EQUIPMENT AND REAGENTS NEEDED
Balance (sensitivity .1 gram)
Filtration apparatus
Filters (grided) and pads (47 mm size with a pour size of
0.45 microns)
Forceps
Bunsen burner or alcohol lamp for sterilizing forceps
Petri dishes (50 mm size)
M-Endo media (Difco, Baltimore Biological Laboratory, etc.)
Vacuum flask
Source of vacuum (pump, vacuum line, water asperator, etc.)
15 psi maximum vacuum
Ethyl alcohol (not denatured)
Standard dilution bottles
Pipettes 1.0 and 1.1 ml
10 and 11 ml wide bore
10 ml serological
Pipette cans (aluminum or stainless steel)
Sterilizer (autoclave or pressure cooker)
Hot air oven (200°C)
Source of suitable distilled water
Sample bottles (100 to 200 ml size wide mouth) autoclave
Erlenmeyer flasks (100 mis or more depending on amount of
media needed at a time)
Graduated cylinders (100 mis, 250 mis, and 1000 mis)
Erlenmeyer flask screw-capped (leter size or other convenient
size for storing sterilized rinse water)
Water bath for heating media
Gas burner or hot plate for heat source
Hand-tally
Fluorescent light in housing permitting placement close to
and as directly as possible over membrane filter for
counting
Optical assistance in counting colonies (preferred wide field
binocular microscope 10 times or 15 times) (less
desirable simple lens with magnification of 5 times)
-------
- 70 -
PROCEDURE
1. Select dilution range that is expected to give a 20 to
80 plate count, then plate one dilution above and one
dilution below making a total of three dilutions. When
no information is known about the sample, more dilutions
may be needed. Where there have been several samples
analyzed at a given point, less dilutions may be used.
See appendix.
2. Place filter on filter apparatus.
3. If 20 mis or less of sample is to be filtered, add 20 mis
of sterilized buffered dilution water to funnel, then
add the sample and filter. If more than 20 mis of sample is
used, add directly to funnel and filter.
4. Rinse funnel with sterilized dilution water and draw
through filter.
5. Remove filter and place on M-Endo pad in dish.
6. Place in incubator inverted for 24 hours 1 2 hours at
35°C + 0.5°C.
7. Remove from incubator and count all colonies that
develop metallic sheen.
8. Record number of colonies and report number per 100 mis
of sample. See appendix.
FECAL COLIFORM
EQUIPMENT AND REAGENTS NEEDED
Same as Total Coliform except:
Roslic acid
M.F.C. broth base in place of M-Endo media
Plastic bags (water tight)
PROCEDURE
1. Same except plate should be 20-60 colonies. See
appendix.
-------
- 71 -
2. Place filter on filter apparatus.
3. If 20 mis or less of sample is to be filtered, add 20 mis
of sterilized buffered dilution water to funnel, then
add the sample and filter. If more than 20 mis of sample
is used, add directly to funnel and filter.
4. Rinse funnel with sterilized dilution water and draw
through filter.
5. Place on pad saturated with M.F.C. broth media.
6. Incubate inverted in water bath at 44.5°C for 22 hours
I 2 hours.
7. Count all blue colonies that develop.
8. Record the number and report the count per 100 mis of
sample. See appendix.
FECAL STREPTOCOCCUS
EQUIPMENT AND REAGENTS NEEDED
Same as Total Coliform except:
K.F. Streptococcus agar in place of M-Endo media
PROCEDURE
1. Same except plate count should be 20-100 colonies•
See appendix.
2. Place filter on filter apparatus.
3. If 20 mis or less of sample is to be filtered, add 20 mis
of sterilized buffered dilution water to funnel then
add the sample and filter. If more than 20 mis of sample
is used, add directly to funnel and filter.
4. Rinse funnel with sterilized dilution water and draw
through filter.
-------
- 72 -
5. Place filter on the K.F. Streptococcus agar.
6. Incubate inverted-at 35°C ± 0.5°C for 48 hours.
7. Count all colonies that develop a pink to dark wine
color.
8. Record number and report count per 100 mis of
sample. See appendix.
CHLORIDE REMOVAL PROCEDURE
A. REAGENTS
1. Standard silver sulfate solution:
Dissolve 4.40 grains Ago SO^, free from nitrate, in
distilled water and dilute to 1.0 liter.
B. PROCEDURE
1. Determine chloride content of the water.
2. Treat 100 ml of sample with standard silver sulfate solution;
1.00 ml of standard silver sulfate solution should be added
for each mg of chloride found in step 1.
3. Remove the precipitated chloride by either filtration or by
centrifugation. Formation of the precipitate may be aided
by heating the solution.
-------
APPENDIX — BACTERIAL SAMPLING DILUTION PROCEDURE
(Membrane Filter Method)
RAW
WATER
SAMPLE
ml.
#1
99ml.
OIL.
WATER
I ml.
99ml.
OIL.
WATER
I ml.
#3
99ml.
OIL.
WATER
PLATE COUNT
MULTIPLIED
BY I
NUMBER OF
BACTERIA
PER 100 ml.
FILTER
APPARATUS
P.C. P.C.
X X
10.000.000 100,000.000
NO. OF NO. OF
BAC./ BAC./
ml.
100 i
100 ml.
NO. OF NO. OF
BAC. / BAC. /
100 ml. 100 ml.
NO. OF NO. OF
BAC. / BAC./
100 ml. 100 ml.
NO. OF
BAC./
100 ml.
NO. OF
BAC./
100 ml.
-------
- 74 -
CONVERSION FACTORS
for Operators
The following factors have been extracted from "Conversion Factors
for Engineers" with permission of Dorr Oliver, Inc.
MULTIPLY
Acres
Acre-feet
Acre-feet
Centimeters
Cubic feet
Cubic feet
Cubic feet
Cubic feet/second
Cubic feet/second
Cubic yards
Degrees (angle)
Feet
Feet
Feet
Feet
Feet of water
Gallons
Gallons
Gallons
Gallons
Gallons, Imperial
Gallons U.S.
Gallons water
Gallons/rain.
Gallons/min.
Grains/U.S. gal.
Grains/U.S. gal.
Grams
Grams
Grams/Liter
BY
43,560
43,560
325,851
0.3937
1728
7.48052
28.32
448.831
0.646317
27
60
30.48
12
0.3048
1/3
0.4335
0.1337
3.785
8
4
1.20095
0.83267
8.3453
2.228x10"3
8.0208/area
(sq. ft.)
17.118
142.86
0.03527
2.205xlO~3
58.417
TO OBTAIN
Square feet
Cubic feet
Gallons
Inches
Cubic inches
Gallons
Liters
Gallons/minute
Million gallons/day
Cubic feet
Minutes
Centimeters
Inches
Meters
Yards
Pounds/square inch
Cubic feet
Liters
Pints (liq.)
Quarts (liq.)
U.S. gallons
Imperial gallons
Pounds of water
Cubic feet/sec.
Overflow rate (ft/hr)
Parts/million
Lbs./million gal.
Ounces
Pounds
Grains/gal.
-------
- 75 -
CONVERSION FACTORS (Continued)
MULTIPLY
Grams/liter
Horse-power
Horse-power
Horse-power
Inches
Inches of mercury
Inches of mercury
Inches of water
Inches of water
Kilowatt-hours
Liters
Liters
Liters
Width (in)xThickness (in)
12
Meters
Meters
Miles
Miles
Milligrams/liter
Million gals./day
Ounces
Ounces
Overflow rate (ft/hr)
Parts/million
Parts/million
Pounds
Pounds
Pounds
Pounds of water
Pounds of water
Pounds/sq. inch
Pounds/sq. inch
Revolutions
Square feet
Square feet
BY
1000
33,000
0.7457
745.7
2.540
1.133
0.4912
0.07355
0.03613
1.341
0.03531
0.2642
1.057
Length (ft)
3.281
39.37
5280
1760
1
1.54723
TO OBTAIN
Parts/million (approx.)
tfoot-lbs/min.
Kilowatts
Watts
Centimeters
Feet of water
Lbs./sq. inch
Inches of mercury
Lbs./sq. inch
Horse-power-hrs.
Cubic feet
Gallons
Quarts (liq.)
Board feet
Feet
Inches
Feet
Yards
Parts/million (approx.)
Cubic ft./sec.
0.0625 Pounds
28.349527 Grams
0.12468xarea sq ftGals./min.
0.0584 ~~Grains/U.S. gal.
8.345 Lbs./million gal.
16
7000
453.5924
0.01602
0.1198
2.307
2.036
360
2.296x10
144
,-5
Ounces
Grains
Grams
Cubic feet
Gallons
Feet of water
Inches of mercury
Degrees
Acres
Square inches
-------
MULTIPLY
Square feet
Square inches
Square meters
Square miles
Square yards
Temp. (°C) + 17.78
Temp. (°F) - 32
Watts
Yards
Yards
Yards
- 76 -
CONVERSION FACTORS (Continued)
BY
TO OBTAIN
1/9
6.542
10.76
640
9
1.8
5/9
1.341xlO-3
3
36
0.9144
Square yards
Square centimeters
Square feet
Acres
Square feet
Temp. (°F)
Temp. (°C)
Horse-power
Feet
Inches
Meters
-------
- 77 -
UNITS
1 milligram per liter « 1 part per million @ 4°C
1 kilogram » 2.205 pounds
1 pound B 453.6 grams
1 grain per gallon • 17.12 parts per million
1 grain per gallon • 142.9 pounds per million gallons
1 part per million - 0.0584 grain per gallon
1 gallon • 231 cubic inches
1 cubic foot - 7.48 gallons
1 cubic foot of water » 62.4 pounds
1 gallon of water - 8.34 pounds
1 gallon • 3.785 liters
1 liter » 0.2642 gallon
1 liter a 1.057 quarts
1 liter » 61.02 cubic inches
1 inch • 2.54 centimeters
1 centimeter • 0.3937 inch
1 cubic foot per second - 646,300 gallons per 24 hours
1 cubic foot per second • 449 gallons per minute
1,000,000 gallons per 24 hours.. - 1.547 cubic feet per second
1,000,000 gallons per 24 hours.. • 694 gallons per minute
1 part per million • 8.34 pounds per million gallons
1 pound per million gallons - 0.1199 parts per million
j. acre • A3,560 square feet
1 gram • 15,432 grains
-------
- 78 -
UNITS (Continued)
1 pound = 7000 grains of wheat
1 meter ° 39.37 inches
1 cubic centimeter = 0.0610 cubic inch
1 cubic inch = 16.387 cubic centimeters
1 quart = 0.946 liter
1 gram « 0.0353 ounce
1 ounce «• 28.3495 grams
Centigrade temperature » (Fahrenheit - 32) x 5/9
Fahrenheit temperature • (Centigrade x 9/5) + 32
-------
- 79 -
CONVERSION TABLE
G.P.M. G.P.D. C.F.S. M.G.D.
10 14,400 0.022 .014
20 28,800 0.045 .028
30 43,200 0.067 .043
40 57,600 0.089 .057
50 72,000 0.111 .072
75 108,000 0.167 .108
100 144,000 0.223 .144
125 180,000 0.279 .180
150 216,000 0.334 .216
175 252,000 0.390 .252
200 288,000 0.446 .288
250 360,000 0.557 .360
300 432,000 0.668 .432
350 504,000 0.780 .504
400 576,000 0.891 .576
450 648,000 1.00 .648
500 720,000 1.11 .720
550 792,000 1.23 .792
600 864,000 1.34 .864
650 936,000 1.45 .936
700 1,008,000 1.56 1.00
750 1,080,000 1.67 1.08
800 1,152,000 1.78 1.15
850 1,224,000 1.89 1.22
900 1,296,000 2.01 1.29
950 1,368,000 2.12 1.36
1000 1,440,000 2.23 1.44
1200 1,728,000 2.67 1.72
1400 2,016,000 3.12 2.02
1600 2,304,000 3.57 2.30
1800 2,592,000 4.01 2.59
2000 2,880,000 4.46 2.88
G.P.M. - U.S. Gallons per Minute
G.P.D. - U.S. Gallons per 24-hour Day
C.F.S. - Cubic Feet per Second
M.G.D. - Million Gallons per Day
-------
- 80 -
DISCHARGE FROM A PARSHALL FLUME
Gage Reading-Inches
1 3/16
1 5/16
1 7/16
1 9/16
1 11/16
1 13/16
1 15/16
2 1/16
2 3/16
2 1/4
2 3/8
2 1/2
2 5/8
2 3/4
2 7/8
3
3 1/8
3 1/4
3 3/8
3 1/2
3 5/8
3 3/4
3 13/16
3 15/16
4 1/16
4 3/16
4 5/16
4 7/16
4 9/16
4 11/16
4 13/16
4 15/16
5 1/16
5 3/16
5 1/4
5 3/8
5 1/2
5 5/8
5 3/4
5 7/8
Discharge in cu
3
Inch
.028
.033
.037
.042
.04-7
.053
.058
.064
.070
.076
.082
.089
.095
.102
.109
.117
.124
.131
.138
.146
.154
.162
.170
.179
.187
.196
.205
.213
.222
.231
.241
.250
.260
.269
.279
.289
.299
.309
.319
.329
6
Inch
.05
.06
.07
.08
.09
.10
.11
.12
.14
.15
.16
.18
.19
.20
.22
.23
.25
.26
.28
.29
.31
.32
.34
.36
.38
.39
.41
.42
.45
.47
.48
.50
.52
.54
.56
.58
.61
.63
.65
.67
. ft. per sec. for various throat widths
9
Inch
.09
.10
.12
.14
.15
.17
.19
.20
.22
.24
.26
.28
.30
.32
.35
.37
.39
.41
.44
.46
.49
.51
.54
.56
.59
.62
.64
.67
.70
.73
.76
.78
.81
.84
.87
.90
.94
.97
1.00
1.03
1
Foot
____
____
— —
____
____
— _
.35
.37
.40
.43
.46
.49
.51
.54
.58
.61
.64
.68
.71
.74
.77
.80
.84
.88
.92
.95
.99
1.03
1.07
1.11
1.15
1.19
1.23
1.27
1.31
1.35
-------
- 81 -
DISCHARGE FROM A PARSHALL FLUME (Continued)
Gage Reading-Inches
6
6 1/8
6 1/4
6 3/8
6 1/2
6 5/8
6 3/4
6 13/16
6 15/16
7 1/16
7 3/16
7 5/16
7 7/16
7 9/16
7 11/16
7 13/16
7 15/16
8 1/16
8 3/16
8 1/4
B 3/4
8 1/2
8 5/8
8 3/4
8 7/8
9
9 1/8
9 1/4
9 3/8
9 1/2
9 5/8
9 3/4
9 13/16
9 15/16
10 1/16
10 3/16
10 5/16
10 7/16
10 9/16
10 11/16
10 13/16
10 15/16
11 1/16
11 3/16
11 1/4
11 3/8
Discharge in cu. ft. per sec, for various throat widths
3
Inch
.339
.350
.361
.371
.382
.393
.404
.41-5
.427
.438
.450
.462
.474
.485
.497
.509
.522
.534
.546
.558
.571
.584
.597
.610
.623
.636
.649
.662
.675
.689
.702
.716
.730
.744
.757
.771
.786
.800
.814
.828
.843
.858
.872
.887
.902
.916
6
Inch
.69
.71
.73
.76
.78
.80
.82
.85
.87
.89
.92
.94
.97
.99
1.02
1.04
1.07
1.10
1.12
1.15
1.17
1.20
1.23
1.26
1.28
1.31
1.34
1.36
1.39
1.42
1.45
1.48
1.50
1.53
1.56
1.59
1,62
1.65
1,68
1.71
1.74
1.77
1.81
1.84
1.87
1.90
9
Inch
1.06
1.10
1.13
1.16
1.20
1.23
1.26
1.30
1.33
1.37
1.40
1.44
1.48
1.51
1.55
1.59
1.63
1.66
1.70
1.74
1.78
1.82
1.86
1.90
.194
1.98
2.02
2.06
2.10
2.14
2.18
2,22
2.27
2.31
2.35
2.39
2.44
2.48
2.52
2.57
2.61
2.66
2.70
2.75
2.79
2.84
1
Foot
1.39
1.44
1.48
1.52
1.57
1.62
1.66
1.70
1.75
1.80
1.84
1.88
1.93
1.98
2.03
2.08
2.13
2.18
2.23
2.28
2.33
2.33
2.43
2.48
2.53
2.58
2.63
2.68
2.74
2.80
2.85
2.90
2.96
3.02
3.07
3.12
3.18
3.24
3.29
3.35
3.41
3,46
3.52
3.58
3.64
3.70
-------
- 82 -
DISCHARGE FROM A PARSHALL FLUME (Continued)
Gage Reading-Inches Discharge in cu. ft. per sec, for various throat width?
11 1/2
11 5/8
11 3/4
11 7/8
12
3
Inch
.931
.946
.961
.977
.992
6
Inch
1.9T
1.97
2.00
2.03
2.06
9
Inch
2.88
2.93
2.98
3.02
3.07
1
Foot
3.76
3.82
3.88
3.94
4.00
-------
- 83 -
DISCHARGE FROM TRIANGULAR NOTCH WEIRS
WITH END CONTRACTIONS
Flow In Gallons Per Minute
Head In Inches 90° Notch 60° Notch
1
1 1/4
1 1/2
1 3/4
2
2 1/4
2 1/2
2 3/4
3
3 1/4
3 1/2
3 3/4
4
4 1/4
4 1/2
4 3/4
5
5 1/4
5 1/2
5 3/4
6
6 1/4
6 1/2
6 3/4
7
7 1/4
7 1/2
7 3/4
8
8 1/4
8 1/2
8 3/4
9
9 1/4
9 1/2
9 3/4
10
10 1/2
11
11 1/2
12
2.19
3.83
6.05
8.89
12.4
16.7
21.7
27.5
34.2
41.8
50.3
59.7
70.2
81.7
94.2
108
123
139
156
174
193
214
236
260
284
310
338
367
397
429
462
498
533
571
610
651
694
784
880
984
1094
1.27
2.21
3.49
5.13
7.16
9.62
12.5
15.9
19.7
24.1
29.0
34.5
40.5
47.2
54.4
62.3
70.8
80.0
89.9
100
112
124
136
150
164
179
195
212
229
248
267
287
308
330
352
376
401
452
508
568
632
-------
- 84 -
REPORT OF LABORATORY RESULTS
Prepared June 22, 1970
PARAMETER
Dissolved Oxygen
pH
Conductance
0-999 umhos
>1000 umhos
Turbidity
0.0-1.0
1-10
10-40
40-100
100-400
400-1000
>1000
Alkalinity
Hardness
Chloride
0.0-1.0
Sulfate
0-9.9
10-1000
>1000
Phosphorus (Total and Dissolved)
0-9.99
>10.0
Ortho
0-9.99
>10.0
Nitrogen
Total KJeldahl
0-2
2-10
REPORT TO NEAREST;
0.1 mg/1
0.1 units
1 umhos
5 umhos
0.05
0.1
1
5
10
50
100
Jackson units
Jackson units
Jackson units
Jackson units
Jackson units
Jackson units
Jackson units
1 mg/1
1 mg/1
0.1 mg/1
1 mg/1
0.1 mg/1
1 mg/1
10 mg/1
0.01 mg/1
0.1 mg/1
0.01 mg/1
0,1 mg/1
0.01 mg/1
0.1 mg/1
1 mg/1
-------
PARAMETER
- 85 -
REPORTING OF LABORATORY RESULTS (Continued)
REPORT TO NEAREST:
Ammonia
0-2
2-10
Nitrogen
Nitrates
0-10.0
>10.0
Nitrites
0-10.0
>10.0
Solids
1-1000
71000
Biochemical Oxygen Demand
0-9.9
10-499
500-1000
>1000
Chemical Oxygen Demand
0-9.9
10-1000
>1000
Sodium and Potassium
0-9.9
10-1000
Fluoride
Phenols (Chloroform Extraction and 50 mm Cell)
0-99
100-1000
?1000
Cyanide
0-9.99
10.0-99.9
0.01 mg/1
0.1 mg/1
1 mg/1
0.01 mg/1
0.1 mg/1
0.01 ing/1
.0.1 mg/1
1
10
mg/1
mg/1
0.1 mg/1
1 mg/1
10 mg/1
100 mg/1
0.1 mg/1
1 mg/1
10 mg/1
0.1
1
mg/1
mg/1
0.1 mg/1
1 mg/1
10 mg/1
100 mg/1
0.01 mg/1
0.1 mg/1
-------
- 86 -
REPORTING OF LABORATORY RESULTS (Continued)
PARAMETER REPORT TO NEAREST;
Organic Carbon
10-100 9'1 •Bfl-
>100 J "S/1
5 mg/1
Oil and Grease
0-99
100-1000 J "8/1
>1000 ,JJ '"g/1
100 mg/1
-------
- 87 -
SAMPLE COLLECTION AND PRESERVATION
ANALYSES
Nutrients
Phosphorus
Nitrogen
Cyanide
Fhenolics
Acidity or Alkalinity
Calcium
Chloride
Fluoride
Hardness
PH
Solids
Sp Cond
Sul fates
TMT-M«Mt-U
Bact. Sample
Metals
(Total)
BOD2 * 5
DO
COD
Organic Carbon
Oil and Crease
Biology Samples
CONTAINER
L-Cubitainer
L-Cubitainer
L-Cubitainer
L-Cubitainer
Bact. Bottle
,-Cubitainer
4 oz. bottle
L gallon Jug
90 Bottle
-Cubitainer
oz. bottle
L Glass
stoppered
bottle
-Cubitainer
PRESERVATION
(0 mg/1 HgCl, (4 mis
of 1% Sol) at 4°C
NaOH to pH 10 or grtr.
1 gram of CuSO^+H.PO,
to pH of 4-» 4°C or
5 ml of 20% CuS04
2-3 ml of 80% H3P04
4°C
None Required
ii
it
ii
None Available
n
ii
4°C
ii
4°C
5 ml cone. HNO,
0.6 ml cone. HNO 3
4°C
Flocculated with Hach
Reagents 4°C- dark
! ml cone HC1
0.25 ml cone HC1
2 ml HjSO^/liter
35 ml of 4X Formalin
MAXIMUM
HOLDING PERIOD
7 days
24 hours
24 hours
24 hours
7 days
6 hours
6 months
8 hours
6 hours
7 days
24 hours
Forever
COLOR
IDENTIFICATION
(TAG)
Yellow
Green
Red
Manila
(2 sides)
Manila
(1 side)
White
Manila
(1 side)
Manila
(1 side)
Pink
Manila
(1 side)
Blue
-------
GLOSSARY
1. Anhydrous - means dry or free from water.
2. Buffer - is a chemical substance which is used to prevent
or reduce changes in the pH.
3. Burette - (volume burette) is a graduated apparatus used
to measure accurately the volume of a solution delivered.
4. Caustic - highly alkaline like lye.
5. Desiccator - is a container in which heated objects which
are to be weighed are allowed to cool down to room temperature.
It should contain a chemical (such as calcium chloride or
silicagel) which will pick up water from the air which entered
the desiccator.
6. Fixed Solids - (total or suspended) are the residue after ignition.
This may also be called ash. It is inorganic in nature.
7. gpg - grains per gallon.
8. Ignite - means to burn. In this case it means burning off the
organic material leaving a white ash.
9. Mix thoroughly - if a volumetric flask is used, stopper and invert;
15 times. Otherwise, mix with a clean glass rod at least 5 minutes.
10. mJL - is short for milliliter. C£ is short for cubic centimeter.
They are both units of volume. 1.00000 ml = l.OOOOScc. For
practical purposes, ml and cc are the same. There are 1000 mis
in a liter.
11. me - (or milligram) is 1/1000th of a gram. To change grams to
mg multiply by 1000.
12. mg/1 - is milligrams per liter, a weight to volume ratio.
Strictly, mg/1 is not equal to ppm, but for practical purposes
they are the same. Standard Methods recommends using mg/1.
t*
13. ppm - is short for parts per million. This is a weight to weight
ratio meaning one part of one substance in one million parts of
the total.
14. Reagent - is a substance used to act upon another substance
in a chemical reaction. In this case, the reagents are
solutions which carry active ingredients of a definite strength.
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GLOSSARY (Continued)
15. Saturated - in such a condition (whether in solid, gaseous,
or liquid state) that another material held within a given
state is in an amount such that no more of such material
can be held within in the same state.
16. Septicity - is a condition of decomposition in which there is
no DO and odors may be produced.
17. Solvent - liquid used to dissolve a substance.
18. Stability - the ability of any substance, such as wastewater,
chemicals, or digested sludge, to resist change though it may
change slightly at different times of the year.
19. Thio - is short for sodium thiosulfate solution.
20. Titration - is the operation of accurately adding a solution of
known concentration (standard solution) to a solution which is
being tested. The exact amount to add is determined with the
aid of another substance (indicator) which will change color at
the proper time. This point of change is called the "end-point."
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REFERENCES
1. Laboratory Procedure For Wastewater Analysis - Department of
Public Health and Welfare, Missouri Water Pollution Board.
2. Standard Methods For The Examination of Water and Wastewater -
Twelfth Edition, 1965.
3. FWPCA Methods For Chemical Analysis of Water and Wastes -
November, 1969.
4. Laboratory Guide For Sewage Works Operators - D. Paul Rogers,
M.A., Pennsylvania Water Pollution Control Association.
5. Laboratory Manual For Chemical and Bacteriological Analysis
of Water and Sewage - Theroux, Eldridge and Mailman.
6. ASTM Standards - October, 1968.
7. Work Book. - California Sewage and Industrial Waste Association.
8. Laboratory Procedures For Wastewater Treatment Plant Operators -
New York State Department of Health.
9. Simplified Laboratory Procedures For Wastewater Examination -
Water Pollution Control Federation, 1969.
10. Glossary - Water and Wastewater Control Engineering - APHA, ASCE,
AWWA, WPCF.
11. Case Histories; Improved Activated Sludge Plant Performance by
Operations Control - Proceedings 8th Annual Environmental and
Water Resources Engineering Conference. Vanderbilt University -
West, A.W., 1969.
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ACKNOWLEDGEMENT
It is a pleasure to credit the Department of Public Health
and Welfare, Missouri Water Pollution Board, for their work In
regard to this manual. The manual, "Laboratory Procedures for
Wastewater Analysis," as published by the Missouri Water Pollution
Board Is a genuine aid to the wastewater treatment operators and
laboratory technicians. It has brought down to the level of the
average person what always has been available In scientific
literature.
We have modified the procedures and equipment discussed In
the Missouri manual In order to keep up with the rapidly changing
and complex pollution problems, and tied together our experiences
In the water pollution field and made Improvements with up-to-date
methods and Instrumentation. This should further reduce the Intricate
parts of the tests and upgrade the accuracy and precision of the
analysis. Without using the Missouri Water Pollution Manual as
a format, this would not have been possible.
GSA-KC-71-I027H
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