lution
Apparaf.i
    Continuous Delivery
         jus Concentrations
               n Water
             ENVIRONMENTAL HEALTH
             SERIES
             Water Supply
             and Pollution Control

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    A SERIAL-DILUTION  APPARATUS
      FOR CONTINUOUS  DELIVERY
    OF VARIOUS  CONCENTRATIONS
        OF MATERIALS IN  WATER
                    Donald I. Mount
                 Aquatic Biology Section
             Basic and Applied Sciences Branch
         Robert A. Taft Sanitary Engineering Center

                         and

                   Richard E. Warner

                Engineering Science,  Inc.
                   Oakland, California
U.S. DEPARTMENT OF HEALTH, EDUCATION,  AND WELFARE
                  Public Health Service
       Division of Water Supply and Pollution Control
                    Cincinnati, Ohio

                       June 1965

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      The ENVIRONMENTAL HEALTH SERIES of reports was estab-
lished to report the  results of scientific and engineering studies of
man's environment:  The community, whether  urban,  suburban, or
rural, where he lives,  works, and plays; the air, water, and earth he
uses and re-uses; and the wastes he produces and must dispose  of in a
way that preserves these natural resources.   This SERIES of reports
provides for professional users  a central source of information  on the
intramural  research activities of Divisions and Centers within the
Public Health Service,  and on their cooperative activities with State
and local agencies,  research institutions, and industrial organizations.
The general subject area of each report is indicated by the two letters
that appear  in the publication number; the indicators are

                WP - Water  Supply
                         and Pollution  Control

                AP - Air Pollution

                AH - Arctic Health

                EE - Environmental Engineering

                FP - Food Protection

                OH - Occupational Health

                RH - Radiological Health

      Triplicate tear-out abstract cards are provided with reports in
the SERIES  to facilitate information  retrieval.   Space is provided on
the cards for the user's accession number and key words.

      Reports in the SERIES will be  distributed to requesters, as
supplies permit.  Requests should be directed  to the Division identi-
fied on  the title page or to the Publications Office,  Robert A. Taft
Sanitary Engineering Center, Cincinnati,  Ohio 45226.
        Public Health Service Publication No.  999-WP-23

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                           CONTENTS

                                                                Page
Abstract	    v
      Introduction	    1
           Materials	    2
           General Principle of Operation	    2
           The Serial-Dilution System	    2
           Water Delivery System	    6
           Toxicant-Metering System	    9
           Calibration	    11
           Timing	    12
           Trouble Shooting	    13
           Performance	    14
      Reference	    16

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                            ABSTRACT
      This paper describes a serial-dilution apparatus designed to
deliver continuously a series of different concentrations of a material
in water.  The materials needed for construction normally would be
available in a. chemistry laboratory.   No electrical power is needed
for  operation, and the apparatus will remain accurate even if the in-
fluent waterflow varies over a wide range.  It  maintains accuracy of
10 percent or less for periods of time up to 30 days or more with
very little servicing or adjustment, and the cost is $50 or less.

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            A  SERIAL-DILUTION  APPARATUS
               FOR CONTINUOUS  DELIVERY

             OF  VARIOUS CONCENTRATIONS
                 OF MATERIALS IN  WATER

                             Introduction

      The evaluation of adverse effects of toxicants or polluting agents
 on aquatic animals is receiving increasing attention as pollution of the
 nation's water becomes more severe.   This evaluation requires that
 the aquatic animals be exposed to an environmental concentration
 rather than to an  injected dose of the agent.  It is necessary,  there-
 fore, to use tests in which the concentration in water of  the material
 being tested is known and maintained constant.  These conditions can-
 not be met in a static or  nonrenewed test because the toxicant may
 volatilize, precipitate, adsorb onto suspended material,  or be ab-
 sorbed by the test organisms, and thus the amount of toxicant in the
 water would be constantly changing.

      Static tests  often require additional aeration to  maintain the
 necessary dissolved oxygen (DO) in the water, and test animals
 cannot be fed because the water becomes foul.  Moreover,  static
 tests cannot be continued for more than a few  days because metabolites,
 such as ammonia, accumulate in the water. Periodic renewal of the
 test -water offsets some of the objections to the static test, but the
 process is laborious and does not sufficiently  maintain controlled
 conditions.

      Continuous-flow tests are the best tool available at present to
 evaluate toxic effects under controlled conditions.  For laboratory
 studies, they most closely approach actual pollutional situations,
 and are, therefore,  being used more commonly  by workers in the
 field.  The Newtown  Laboratory of the Robert A. Taft Sanitary En-
 gineering Center has been engaged in continuous  flowthrough testing
 for 3 years,  and the  problem of maintaining concentration control on
 100 or more flowthrough test chambers has been troublesome and has
 required much costly time of technicians.  The cost of metering
 pumps and valves  needed to do the job adequately have increased,
 and malfunctions have occurred regularly.   Nearly two full-time
 positions have been  required to maintain and check the systems each
 day, including weekends and holidays.   The most critical fault of the
 systems in use--a fault that became impossible  to tolerate — consisted
 in a  metering system's delivering toxicant  solution when the waterflow
 slowed or failed.  The  result was the death of  the fish in the test
 chambers.  These problems became acute when long-term studies  on
 fish  reproduction  were begun; a year's \vork could be  lost in one night
 in this manner. The apparatus described in this paper is a result of
 efforts to improve dependability of the  dosing process.
      In  1962, Mr. Richard Warner of Engineering Science, Inc.,
Oakland, California,  in an annual report on a Public Health Service
contract, described  a serial-dilution apparatus that he had built to
conduct flowthrough  tests.  Serial dilution has  many advantages:

                                 1

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 It is more accurate in most cases,  fewer controlling valves are
 needed, only one stock solution is required, and there are fewer small
 constrictions to become clogged.  We have used the principles  from
 Mr.  Warner's apparatus to build diluters suitable for our use.  We
 now have  13 of these diluters in operation; they have improved  our
 accuracy  of concentration control, at least 40 man-hours per week
 have been saved, the number of malfunctions has dropped sharply,
 and space requirements have been reduced.  In addition, the toxicant
 dose is dependent on waterflow, the cost of the metering system has
 been reduced from $600 to $800 to $50 or less,  and the system can
 handle water with plankton or suspended solids of surprisingly  large
 particles  and still not clog.

 MATERIALS

       Supplies normally available in a chemistry laboratory have been
 used to construct the apparatus. Crystallizing dishes and sidearm
 vacuum flasks are useful for making the various cells.  Epoxy  glue
 is especially convenient for  gluing  glass tubes in place and making
 watertight seals. A polyethylene hose "X" can be used for the valve
 housing.

 GENERAL PRINCIPLE OF OPERATION

       The  serial-dilution apparatus  described here consists of three
 functional  components:   the  water delivery system,  the toxicant feed
 system, and the serial-dilution system.  In essence, water delivery
 is accomplished by filling the water-metering cells, stopping the
 waterflow  to the cells, emptying the metering cells, and restoring
 the waterflow.  This sequence must be completed twice to produce
 one cycle  of the  serial-dilution system;  water containing the appro-
 priate toxicant concentration is  delivered once per cycle.  The
 sequence of delivering 1 unit volume of -water from each metering
 cell,  together with the associated changes in the serial-dilution
 system, is termed a half cycle.

 THE SERIAL-DILUTION SYSTEM

      To grasp better the major functional  concepts of this apparatus,
 temporarily disregard the water delivery and toxicant feed systems
 and consider only the serial-dilution system.  Refer to Figures 1,
 2, and 3 and cells M-l, T-l, and M-2.  For illustration, assume a
 desired volume  of 100 milliliters of dosed water for  each concentra-
 tion per cycle.  If a 2:1 dilution ratio is  used,  twice  the desired
 volume of  the first concentration must be made to have  a sufficient
 quantity for making  other dilutions.  At the first half cycle,  100 milli-
 liters is discharged into  chamber M-l along with an  appropriate
 quantity of toxicant, Figure 3A.  Chamber M-l will then be one-
half full, and during the next half cycle,  an additional 100 milli-
liters of water is added along -with toxicant,  giving a total volume of
200 milliliters,  a volume that fills cell M-l and causes the siphon
to start. T-l is  adjusted so that the transfer volume (volume of
water contained between the levels of the standpipe and the end of the

 2                                A SERIAL-DILUTION APPARATUS

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                                  VACUUM  MANIFOLD
                                                                         WATER SOURCE
                                                                     i-  VALVE
                                                               VACUUM VENTURI
     Figure  I. Diagram of the serial-dilution apparatus. Flasks I  to 6 at the top are metering
              cells, M-l to M-5 are mixing cells, T-l to T-4  are transfer cells,  and V-l  to  V-4
              are venturi tubes. The toxicant-metering system is not shown
The Serial-Dilution System

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 venturi siphon tube, Figure 2) is 100 milliliters.  As the siphon of M-1
 discharges  water into T-l,  100  milliliters remains in T-l and  100
 milliliters goes  down the standpipe to a test chamber or other location,
 Figure  3B.

       During the next half cycle, 50 milliliters of water  is delivered
 through transfer venturi  1 into  cell M-2 (Figure  1).  As  the 50 milli-
 liters passes  through the venturi, the siphon from T-l to M-2 starts
 and 100 milliliters  of the previous concentration (presently in T-l)
 is added,  making cell M-2 three-fourths full (Figure  3C).  Finally,
 50 milliliters of water is again added to M~2.   Since T-l contains no
                             VENTURI SIPHON TUBE
                  TRANSFER CELL
                                               FROM FUNNEL
                                                    TRANSFER VENTURI
                                                  •— VENTURI FLARE
                                     _J
                                                           - MIXING CELL .
                                                            AUTOMATIC
                                                           "  SIPHON
                                                    D
           Figure 2. Details of the transfer venturi, transfer cell, and mixing cell.

water that can be siphoned by the venturi siphon tube,  none is trans-
ferred from T-l to M-2 during this half  cycle.   The addition of the
second 50-milliliter volume to M-2 fills  it, and the  siphon starts and
empties 200 milliliters of solution into T-2, Figure  3D.  This 200-
milliliter volume is one-half as concentrated as the  first 200-milli-
liter  volume in M-l.  During the two half cycles when water  was
being added to M-2, 100-milliliter volumes were being added to M-l
                                     A SERIAL-DILUTION APPARATUS

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 so that when M-2 is full, M- 1 is full again, and both empty simul-
 taneously and fill T-l and T-2. The same  sequence is  continued for as
 many concentrations  as  are  desired.  Two-hundred milliliters of the
 last concentration will be discharged from the "M"  cell because no
 water is transferred  downward to make additional concentrations.

      Water is discharged on half cycles rather than once each  cycle
 to simplify timing problems.  One can see from Figure 3 that all of
 the 50 milliliters entering the venturi on T-l  must clear the venturi
 before the 200 milliliters from M-1 fills T-l  again.  This is easily
 accomplished by half-cycle operation,  but  if water were delivered
       Figure 3. General diagram illustrating the operation of the serial-dilution system.

only once per cycle, 100 milliliters of water from the metering cell
and 100 milliliters from T-l would have to arrive in M-2 before any
of the 200 milliliters from M-1 reached T-l.  If this did not  happen
and the venturi siphon on T-l was  still  discharging water to M-2
when M-l began emptying into T-l, all of the water emptied  from M-l
to T-l would subsequently be transferred to M-2 and then on to T-2,
and so forth.  Water delivery each half cycle  makes possible a safety
factor that prohibits the action referred to above and that is called
"double siphoning. "
The Serial-Dilution System

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       In addition,  by using half-cycle delivery,  the diluter  need not
 remain "in phase. "  "In phase" refers to  sequences in which all "T"
 cells are full and all "M" cells are empty.  After the  next "in phase"
 half cycle, all "M" cells are half full and all "T"-cell transfer volumes
 are empty.  By using half-cycle delivery,  cells T-l and T-3 may be
 full while  the transfer volumes of T-2 and T-4 are empty.  Conse-
 quently M-l, M-3, and M-5 would be empty and M-2 and M-4 would be
 half full when the "T" cells are as described above.  The condition
 that must  be met is that when a "T" cell is full, the "M" cell immedi-
 ately above it must be empty,  and when the transfer volume of a given
 "T" cell is empty, the "M" cell immediately above must be half full.
 Each diluter usually operates  in a particular pattern called the phase
 sequence pattern.  The latter one described above is called the alter-
 nating  sequence  pattern and is  the more common because timing is
 less critical.

      In practice,  the  total volume need not be used on any cell.  One
 can shorten the siphon tube in  the "M" cells, for instance,  and use
 only half of their volume.  In this instance the "M" cells would never
 empty completely.  If a dilution of 1:3, or any other ratio,  is desired,
 the volume transferred from the "T" chambers  to the  "M" chambers
 is changed accordingly to give  the desired ratio.  An example would be
 a transfer volume  of 75 milliliters and a half-cycle water delivery of
 112.5  milliliters to M-l and 75 milliliters to the others.

      Figure 2 shows the details of the "T" cell and the "T"-cell
 venturi. A very efficient venturi can be made from either "T"- or
 "U"-shaped glass connecting tubes if they are cut  and  modified as
 shown. One important precaution is that the venturi flare must have
 the same or slightly larger bore at its upper end as the bore of the
 venturi "U" tube.  If the upper end of the flare is smaller,  a back
 pressure will develop on the venturi siphon tube and the siphon will
 not start.
      Another suggestion for better venturi operation is the use of a
 tube bore for the funnel siphon and funnel  siphon tube (Figure 4) that
 is slightly smaller than the  bore of the "U" tube venturi.  The funnel
 siphon tube must fill with water without air for proper venturi opera-
 tion.  The  primary purpose of  the funnel siphon is to keep air out of
 the funnel  siphon tube.  Many of our diluters  operate without these
 funnel siphons because the funnel siphon tube is  small enough and the
 metering cells empty fast enough to prevent air  from entering the
 funnel siphon tube.
      Finally, the venturi flare must not be excessively large or else
 the water and air mixture (the  air enters from the venturi siphon tube
 until the water from the "T" cell arrives)  passing through the flare
 will not completely fill it and there will be no venturi.  An improper
 taper on the flare or a nonwettable film such  as  grease can cause the
 same type  of trouble.

 WATER DELIVERY SYSTEM

      Other types of water delivery systems \vere  tried in conjunction
with the serial-dilution system, but these  would not deliver water with

 6                                  A SERIAL-DILUTION APPARATUS

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                                      	WATER DELIVERY TUBE

                                      TO VACUUM MANIFOLD
        WORKING
         VOLUME
     WATER METERING CELL
                                                WATER INLET TUBE
                                                FROM WATER MANIFOLD
                                             VOLUME ADJUSTMENT COLLAR
                                              GLASS "U" TUBE
                                                   FUNNEL SIPHON

                                                '.-MINIMUM WATER LEVEL
                                             FUNNEL SIPHON TUBE
                              TO TRANSFER VENTURI
                     Figure 4. Detail of a water delivery unit.
Water Delivery System

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 an accuracy comparable to that achieved by the serial-dilution system.
 This system has the advantage that one can visually determine whether
 or not the proper volume of water is being delivered, with an error
 of 10  percent  or less.  More important,  the volume delivered each
 half cycle is not affected by the rate at which  water is  fed to the  system
 and there are no small water passages that can clog with solid material.
       As shown in Figures 1 and 4, the water delivery system is com-
 posed of a series of units,  each consisting of  a metering cell with a
 water inlet, air tube and water delivery tube,  a venturi, and a funnel.
 There is a common vacuum manifold, vacuum venturi,  and water shut-
 off valve.
                                                     .  n  ,
                                                     \7_ STOPPER
          WATER FROM CELL NO. 6
                 I
                                 VAUE SPRING

                                      SLICED STOPPER
                                                             - GLASS NEEDLE
                                      TO CONTROL   OUTLET TO WATER MANIFOLD
              Figure 5. Detail of the main water valve and vacuum venturi.

      Frequent reference to Figures  1, 4, and 5 will assist in under-
standing the operation.  A water manifold delivers water to each of
the metering cells, which fill until the water level is at the end of the
air tube.  Cell Number 6 fills last because the inlet to it is higher than
that of the others, and it empties first because its outlet  is lowest.
As  water from the last cell fills the bucket on the  needle  valve arm,
the valve is  closed by the additional weight.   When the bucket is filled
                                    A SERIAL-DILUTION APPARATUS

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to the level of the siphon tube,  the water travels through the vacuum
venturi, producing a partial vacuum in the vacuum manifold,  and is
then discharged to the control chamber.   The reduced pressure  in the
vacuum manifold causes water to rise from both ends of each water
delivery tube (from the  funnel and from the metering cell).  If distance
A' is less than distance A" (Figure 4), the water will rise over the arch
of the tubes and activate the siphons, which will empty the metering
cells down to the end of the \vater  delivery tube. By the time the si-
phons break,  the bucket on the needle valve arm will be nearly empty,
the valve will open, and the metering cells will fill again.

      The sequence in which the metering cell siphons  start is de-
termined by the realtive distance of A' of each cell.  Figure 1 illus-
trates the most desirable order, namely, Numbers  1 and 5 start at
nearly the  same time and then Numbers 4, 3, and Z begin in that
order.  Number 1 should begin emptying early because  if a 2:1 dilu-
tion is used the first cell must deliver twice as much water as the
other cells.

      The "funnel end" of each water delivery tube must remain under
water at all times so that a partial vacuum can  be created in the
vacuum manifold.  A bypass spout on the funnel is used to measure the
water delivered by the  cell during  operation.  The funnel siphon and
bypass  spout are positioned so that when the bypass is  open enough
water remains in the funnel to cover the end of the water delivery
tube and so  that all the water delivered goes through the bypass  and
none  goes over the funnel siphon to the transfer venturi.

      Major volume adjustments of the metering cells are accomplished
by moving the  volume  adjustment collar (Figure 4),  and minor ones
are made by moving the air tube.  Caution must be exercised, how-
ever, since moving the air tube changes distance A', which could
change the  sequence of delivery.  If  changed enough,  the distance
may exceed A" and then the siphon will not start.
      Care should be taken in constructing the vacuum venturi to see
that  proper  tube sizes and tapers are used to produce sufficient vacuum.
If it  is properly made,  more than enough vacuum can be produced
with ease.
TOXICANT-METERING SYSTEM
      The toxicant-metering system is not necessarily an integral
part of the  apparatus.   We have used several other types such as
metering pumps and controlled dripping rates but all have been in-
ferior to the one shown in Figure 6.   It has the important advantage
that  it will  not deliver toxicant  unless waterflow is near normal.
      The system as shown in  Figure 6 is nearly self-explanatory.
The  solution level in the funnel is kept constant by some means such
as a Mariotte bottle or float valve.  If the toxicant is a  suspension
rather than a  solution,  settling may occur.  A small peristaltic
pump may be  used to pump the  suspension to the funnel with a bypass,
overflow line  back to the bottle. In this way the level in the funnel is
maintained and the  suspension is mixed and replaced, which eliminates
settling.

Toxicant-Metering System                                          9

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       For use on the diluter apparatus, the plastic bucket of the meter-
 ing system is placed beneath the first funnel of the diluter  (Figure 1)
 and when water flows through the funnel siphon tube the bucket is
 filled with water.  This weight causes  the bucket arm to drop and the
 opposite arm rises upward taking with it a predetermined volume of
 toxicant,  which runs into M-1 through  the tube arm.

       The components are easily assembled and the tube is simply
 made by heating an appropriately sized piece  of glass tubing in a
 narrow area,  stretching it until the bore is sufficiently reduced,  cool-
 ing,  and then bending the two angles.   The bore is  constricted so  that
 minor fluctuation in the solution level in the funnel will not significantly
 change the volume delivered.
  MAfilOTTE BOTTLE
                                        DIRECTION Of ROTATION
      Figure 6. Detail of toiicant-metering system. Bottle is not in proportion to drawing.
      The accuracy of this system equals or exceeds the accuracy of
systems using metering pumps and constant waterflows  because de-
livery is balanced against a water  volume rather than a  flow; thus a
major source of variation (waterflow) is bypassed.  Obviously, for
best calculations  one  should know how many times the metering cell
empties and likewise  how many times toxicant is added.  Since it did
not seem advisable  to put a counter switch on the metering system
because of its small size, a microswitch was placed on  the needle
valve arm (It moves each time the Number 1 cell empties. ),  giving an
actual count of the number of times chemical is delivered. (Mechani-
cal counters are also very good because no electricity is needed. )
10
                                   A SERIAL-DILUTION APPARATUS

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By using a calibrated toxicant bottle, the total volume of toxicant
delivered can be read,  the number of counts can be obtained from the
counter, and the average volume of toxicant delivered each half cycle
can, therefore, be calculated.  Then,  by measuring the volume of
water delivered by metering cell 1,  the calculated accuracy of the first
concentration can be determined.

CALIBRATION

      Calibration of the various volumes  seems to be a laborious
task, but it can be completed in 10 to  15 minutes with experience.
After the wetting characteristics of the tubes have stabilized,  the
calibration needs to be checked only every 2 to 4 weeks to ascertain
that the maximum error is  10 percent or less.  The diluter should be
checked visually every day to  insure good operation and detect mal-
functions  such as that caused by a broken component.

      Only two sets of volumes need to be known in order to calculate
the error for  each concentration,  the first excluded.  These are the
amounts of diluent water being added at each half cycle and the trans-
fer volume (the volume of the next higher concentration being  mixed
•with the diluent water from the water-metering cells).

      The volume of diluent water added is  checked by  opening the
bypass on the funnel and catching the volume for one or more  half
cycles for each metering cell.  One must be careful to see that all
water delivered goes through the bypass and that none goes over the
funnel siphon.
      The transfer volume is checked  as follows:  Assume a desired
volume of  100 milliliters.  Fill a 250-milliliter graduated cylinder to
some volume  greater than  120 milliliters.  Wait until the "T" cell
to be checked is just emptied by the venturi siphon. Pour water into
the "T" cell until it is full,  then add 20 milliliters or more in addition
and catch the water that runs down the standpipe before the next half
cycle begins.   Return this water to the graduated  cylinder.  Read
the volume now remaining in the cylinder; the difference between the
present volume and the original volume represents  the transfer volume
of the "T"  cell being checked.   When adding the water to the "T" cell,
one should fill it at approximately the  same rate as it is  filled by the
"M" cell siphon above it in order to simulate actual operation.
      After all volumes  are recorded,  the error for each concentration
can be calculated.  Obviously,  the error for the first concentration
must be determined by using the volume of water  delivered from
metering cell 1 and the volume of toxicant delivered by the metering
system.
      Each diluter will usually operate in a  typical phase sequence.
Obviously, checking the volumes as described above disrupts  this
sequence because water is  being added or removed.  It is best,
therefore,  to check the transfer volumes  first,  starting with the
lowest transfer cell, and then  check the metering cell volumes.  In
this  way each transfer volume is checked when the diluter is in
its typical phase sequence.  The checks can be made while the diluter

Calibration                                                        1 1

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is operating, and the removal or addition of water for checking will
cause one or at most two errors.   The diluter will correct itself and
continue properly,  but possibly in a different phase sequence.   If a
diluter is well  timed it will stay in any phase sequence in which it  is
placed.   This pattern offers a useful visual check of proper operations.
If the pattern keeps changing every few minutes,  the diluter is  making
errors.
      Other visual  checks that can be  made for proper operation are:

      1.  Determine whether,  when an "M" cell is empty, the "T"
         cell immediately below it  is full.  (This  is a check for double
         siphoning.  See page 5.
      2.  Observe the sequence in which water runs down the stand-
         pipes  of the "T" cells.  This should occur on each second
         half cycle.  A malfunction may indicate  that a "T" cell
         venturi is  not working.
      3.  Observe whether the needle valve is turning off the water com-
         pletely and for a period long  enough to allow the metering
         cells to dump.
      4.  Observe whether each metering  cell is filling and emptying
         completely each half cycle.   Other checks will be learned by
         experience.  These checks may seem tedious,  but with
         experience, a 2-minute daily visual check is  sufficient to
         insure good operation regularly.

TIMING

      In performing the calibration, one  may find that the  system may
need to be timed more accurately.  This  may also be necessary after
the wetting characteristics have stabilized.  Timing adjustments solve
the double-siphoning problem mentioned  on page  5.   When a diluter
is optimally timed,  the serial-dilution system can be disrupted for
some reason such as for  a calibration check or accidentally by dirt,
air,  and so forth,  and the system will make only  one error and then
return to proper operation.  This ability to correct mistakes is
highly important because during normal operation things will occur that
cause an error and only  if the system can correct errors and not
repeat them can it  be considered satisfactory.

      To review:  Double siphoning occurs when all the water from a
given metering cell has not passed the transfer venturi as the asso-
ciated "T" cell begins to  fill from the next higher "M" cell. The
result is that the  venturi  siphon begins to remove water from its
"T" cell when it should not.

      There are three timing adjustments:  (1) The sequence in which
the metering cells  empty, (2) the volume of water required to start
the funnel siphons,  and (3) the volume required to start the "M" cell
siphons.   If the sequence in which the siphons of  the metering cells
start  is as described earlier, then frequently no  other adjustment  is
needed.  If difficulty is experienced in getting the desired  sequence
or if an additional safety  factor is desired, or both, the next best

12                                A  SERIAL-DILUTION APPARATUS

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timing adjustment is the "M" cell volume.  The volume of the cell is
reduced by shortening the siphon tube or by adding volume  displacers
such as marbles,  in order to make the  cell empty sooner,  or the tube
length is increased,  or volume displacers are removed to make it
empty later.   As a last resort, and this is rarely necessary,  one
can change the volume of water required to start the funnel siphon in
a manner as  described above for the "M" cells.
      As a general rule,  the greatest safety factor for timing should be
given to the higher cells.   In practice,  calibration and timing must be
done more or less simultaneously, starting at the top "M"  cell and
working downward.   After  the metering cells  have been calibrated and
one feels that the  apparatus is properly timed, the serial diluter should
be intentionally fouled by randomly adding water in order to be certain
that the diluter  can  correct errors and  resume proper operation.
TROUBLE SHOOTING
      Experience  in the use of the diluter has shown how to correct
minor malfunctions  with ease by  using  "tricks of the trade. "   Some
of these do not fit well into the text and are presented here for the
reader's convenience.

      1.  Symplon:  One or  more metering  cells are not filling or
         emptying completely.
         Trouble:  Dirt in the water  or  air tubes.

      2.  Symplon:  Last metering cell (No. 6 on Figure 1) fills and
         empties but the others remain full.
         Trouble:  One of the funnels has  insufficient water in it and
         the  water delivery tube is getting air, or there is  dirt or a
         break in the vacuum venturi or manifold.

      3.  Symplon:  One or  more metering  cells are delivering water
         continuously and other cells are  not filling.
         Trouble:  Needle valve  is not closing tightly,  or is not  re-
         maining closed long enough for all cells to empty, or a par-
         ticle of dirt caused the  valve to malfunction.  Correction may
         involve adjusting valve  seating, providing more water to in-
         crease closed period of valve, or improving efficiency of
         vacuum venturi.
      4.  Symplon: Waler rises over water delivery tubes before valve
         buckel fills and  closes valve.
         Trouble:  There is loo much waler pressure for exisling ad-
         justments or there is dirl in waler tube leading to melering
         cell 6.  Correclion may involve increasing Ihe dislances A'
         (Figure 4),  lowering Ihe level of cell 6, increasing Ihe bore
         of Ihe waler manifold and inlel lubes lo melering cells, or
         lowering curve of waler delivery lube of cell 6.

      5.  Symplon: Cell 6 fills before Ihe  olher cells are full.
         Trouble:  Cell 6 needs lo be raised slightly.
      6.  Symplon: Volumes delivered by one or more  melering cells
         vary.
         Trouble:  Valve is nol closing  properly.

 Trouble Shooline                                                   13

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     10.
Symplon: Diluter is double siphoning.
Trouble:  Improper timing.

Symplon: Diluter does nol hold a phase sequence pattern.
Trouble:  Timing is improper,  one venturi is not operating,
one metering cell does not always empty, or one of the water
volumes (either from metering cell or a transfer volume) is
grossly wrong.

Sympton:  A transfer venturi does not work every time.
Trouble:  There is air in funnel siphon tube,  dirt in water
line,  venturi "U "tube  is cracked,  flare is not completely
filling with air-water mixlure, or end of flare is under water
of next lower  "M" cell part of the time.

Sympton:  Transfer volumes vary from  day to day.
Trouble:  Venturi siphon tubes are not held securely.
PERFORMANCE
      One may expect no more than 10 percent calculated error (1 to
3 percent for any one concentration) from a diluter if it is calibrated
once every Z to 4 weeks with daily observations as  described previously.
One advantage  is that the errors tend  to be both positive and negative so
that they cancel each other.  Table  1 illustrates the usual accuracy ob-
tained from a diluter with no special efforts or precautions.   These
data were recorded in a record book during routine testing and do not
represent unusual accuracy  nor were  they recorded for demonstration
purposes.

Table 1.  THE  CALCULATED AND POLAROGRAPHICALLY MEA-
          SURED CONCENTRATIONS  OF ZINC IN mg/liter FROM A
          SERIES OF THREE 4-day TESTS.  DAILY SAMPLES WERE
          COMPOSITED FOR 4  days AND THEN THE ZINC ANALYSES
          WERE MADE.  WATER FLOW WAS 100/ml/min/concentra-
          tion.   THERE WERE  10 FISH IN EACH 10-liter TEST
          CHAMBER.   ALL  SOURCES OF ERROR INCLUDING DILUTER
          ERROR,  ERROR IN THE TOXICANT-METERING APPARATUS,
          WATERFLOW VARIATION,  REMOVAL BY  THE TEST
          ORGANISM, AND ANALYTICAL ERROR ARE REFLECTED
          IN THESE MEASUREMENTS.
Test 1
Calculated
33.5
17.0
8. ,4
4.2
2. 1
1.0
Measured
34
18.7
10.5
5. 3
2.4
1. 1
Test 2
Calculated
33.4
17.2
8.4
4. 3
2. 1
1. 1
Measured
34.9
18.5
8.5
3.4
2. 1
1.2
Test 3
Calculated
41. 3
20. 4
11.0
5.8
2.9
1. 5
Measured
41.0
20.5
10.9
5. 5
3.0
1.4
14
                          A SERIAL-DILUTION APPARATUS
                                                GPO 820—573-3

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     The choice of optimum cell size can be made by a convenient rule
of thumb as follows:  Determine the flow desired for each concentra-
tion per minute and use "T" and "M" cells that hold four times that
volume.  In this way one can obtain a 2:1  dilution ratio  by using a
1-minute half-cycle time.  The flow can be doubled by decreasing the
half-cycle time to one-half minute, about the maximum  practical speed,
and, of course,  the flow can be decreased to any desired volume by
simply increasing half-cycle time.  One-minute half cycles seem to be
optimum.
     Figure 7. A serial-dilution apparatus designed to deliver 300 ml /min of five concentrations
            and a control. Several minor changes  are used on this diluter.

Performance                                                       15

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     Some of our dilute rs have run for 6 months with no more than one
or two adjustments during that period.  Of course there were occasions
during that period when foreign material or an accident caused a. signi-
ficant error for a short period.  Figure 7 illustrates a 5-concentration
diluter designed to deliver up to 300 milliliters per minute.

     One may logically expect to build and calibrate one of these di-
luters in a week, but after several are  built,  this time may be re-
duced to 3 days or even less.  Four  professional biologists  in the
Newtown Laboratory have become proficient with these systems and
are thoroughly convinced of  their utility.  Most recently -we have been
studying effects of silt in the water,  and the diluter appears to be
     suited for that work as  well.
     The experiences of our people with the diluter have been very
similar; after the diluter is built,  a  short period is needed for final
adjustments and for solving minor problems.  Then, as the operation
becomes smooth,  satisfaction is felt because technical problems are
minimal and the biological  investigation can proceed.


                           REFERENCE


1.    Lemke, A.  E. , and D.I.  Mount,  Some effects of alkyl benzene
     sulfonate  on the Bluegill,  Lepomis macrochirus.  Trans. Am.
     Fish. Soc., 92(4):  373-378,  Oct.  1963.
16                                 A SERIAL-DILUTION APPARATUS
                                                          GPO 82O—573—2

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