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

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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

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This is the
Superintendent of Documents
classification number:

       EF 2.8:
       W28

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                                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

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                          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

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                          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.

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                         - 2 -


                     GLASSWARE
ERLENMEYER
  FLASK
    17
  B.O.D.
 BOTTLE
BEAKER
                             BURETTE
                 PIPETTE
                                               GRADUATED
                                                CYLINDER

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                                -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.

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                                - 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.

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                                - 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.

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                                 -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.

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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

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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

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                               -  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.

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                               - 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.

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                               - 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.

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                              - 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

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                              -  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.

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                              - 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.

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                - 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

-------
                               - 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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-------
                              - 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.°°

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                               - 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:

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                               - 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

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        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.

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                             -  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

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                            -  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

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                                - 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.

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                                - 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.

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                             - 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

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                             - 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.

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                              - 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.

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                              - 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.

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                             - 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.

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                             - 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.

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                            - 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.)

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                               - 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:

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                             - 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

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                              - 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

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                                - 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

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                              - 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.

-------
                               - 89 -

                        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."

-------
                               -  90 -


                          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.

-------
                                 -91-
                     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

-------