Environmental Research
                       Laboratory
                       Ouluth MN 55804
                        EPA-600/3-78-07 2
                        July 1978
            Research and Development
<>EPA
Manual
for  Construction
and  Operation
of Toxi city-Test ing
Proportional Diluters

-------
                                          EPA-600/3-78-072
                                          July  1978
  MANUAL FOR CONSTRUCTION AND OPERATION OF

   TOXICITY-TESTING PROPORTIONAL DILUTERS
                     by

A. E. Lemke, W. A. Brungs, and B. J. Halligan

  Environmental Research Laboratory-Duluth
          Duluth, Minnesota  55804
  ENVIRONMENTAL RESEARCH LABORATORY-DULUTH
     OFFICE OF RESr^RCH AND DEVELOPMENT
    U.S. ENVIRONMENTAL PROTECTION AGENCY
          DULUTH, MINNESOTA  55804

-------
                                   ABSTRACT
     This paper presents a discussion of  the testing procedures  using
proportional diluters.   The construction,  calibration,  and operation of the
equipment is explained,  and trouble shooting techniques necessary for success-
ful use of such equipment are given.

     A bibliography includes many related published  materials  that are not
discussed in the text but which should be useful to  the reader.   Included are
numerous citations on physical toxicity testing methods, but papers on statistics
or biological test procedures are not included.
                                      iv

-------
                                   CONTENTS
Foreword	ill
Preface	   iv
Abstract 	    v
Figures	vii
Tables	viii
Acknowledgments	   ix

     1.  Introduction  	    1
     2.  Diluter Operation - General 	    3
     3.  Diluter Construction  	    5
              Equipment  	    5
              Diluter-board construction 	    6
              Glass cutting	    6
              Glass assembly	   13
     4.  Diluter Operation 	   19
              Mechanisms of action 	   19
              Flow rate requirements	i	   22
              Accessory parts  	   23
              Diluter assembly 	   23
     5.  Diluter Calibration 	   26
              Precalibration 	   26
              Final calibration	   26
     6.  Toxicant Metering 	   29
     7.  Diluter Modifications 	   35
     8.  Trouble-Shooting  	   42
     9.  Diluter Safety Devices  	   44

References	   47
Bibliography 	   49
Appendices
     A	55
     B	66
     C	70

-------
                                   FIGURES


dumber                                                                    PaSe

  1    Completed mounted diluter  	    4

  2    Diluter board with shelves mounted   	    8

  3    Glass-cutting layout   	   11

  4    Glass-cutting layout   	   12

  5    Glue-application system                                               14

  6    Gluing layout for W and C  cells	15

  7    Gluing procedure 'for W cells	17

  8    Final assembly plan for all cells	18

  9    Tubing and accessory plan  for  assembled diluter  	   20

 10    Valve bucket assembly  	   21

 11    Toxicant metering assembly plan  for  the "dipping bird"  system ...   30

 12    Construction plan for  a "dipping bird" toxicant  metering  system
        using volumetric pipette 	   31

 13    Toxicant-metering assembly using "McAllister  system"   	   32

 14    Safety system for the  "McAllister  toxicant-metering system"  ....   33

 15    General plan for synchronous multiple diluter system   	   36

 16    Timing system for multiple diluter system 	   37

 17    Diluter modifications  for  effluent dilutions   	   38

 18    Diluter system modified to include the addition  of a  food supply
         (microorganisms)  	   40

 19    "Dipping bird" safety  device   	   45

 20    Diluter malfunction safety system  	   46

                                      vi

-------
                                    TABLES


Number                                                                     Page

  1    Metric Conversion Table 	 ....   7

  2    Dimensions of Principal Glass Parts for the 2-Liter Diluter ....   9

  3    Accessory Parts Needed to Construct a Diluter 	  10

  4    Cell Delivery Volumes for 2-Liter Diluters with Five Concentra-
         tions and Control	27
                                     vix

-------
                                ACKNOWLEDGMENTS
     We wish to thank those present and former associates who have,  over the
years, provided suggestions for design changes,  operation, and other features
of proportional diluters.   Without such positive influence this report would
be no improvement on the original 1967 publication.
                                    VI11

-------
                                   SECTION 1

                                 INTRODUCTION
     The physical aspects or characteristics of testing toxicity of chemicals
and aqueous effluents with aquatic organisms were minor considerations before
the initiation of continuous-flow procedures.  Initial recommendations called
for the use of "round (cylindrical) glass jars 9 to 12 inches in diameter,  10
to 12 inches high, of good quality clear glass 1/8 to 1/4 inch thick and with
a capacity of 2 1/2 to 5 gallons" (Hart et al., 1945).  Equipment for
temperature control and oxygenation completed the procedures.  Similar
recommendations persisted (Doudoroff et al., 1951) until more details were
presented by Henderson and Tarzwell (1957) that included a floor plan of a
proposed toxicity-testing laboratory for static procedures with industrial
effluents.

     A serial-dilution apparatus was described by Mount and Warner  (1965) that
delivered continuously a series of different concentrations of a material
dissolved in water.  The proportional diluter, to be discussed in detail
throughout this report, was developed shortly thereafter (Mount and Brungs,
1967).  This system is simpler to build and operate than the serial diluter
and its use is more flexible.  These systems and others (see Bibliography)
helped initiate the conversion to continuous-flow testing procedures to
alleviate some of the toxicity-testing problems inherent in the static
procedures.

     The use of continuous-flow techniques received added impetus with the
addition of general procedures to the 13th edition of "Standard Methods for
the Examination of Water and Wastewater" (American Public Health Association
et al., 1971).  Only static tests had been described in earlier editions.
After 1971, numerous detailed toxicity test procedures were developed that
used or required continuous-flow techniques.  The Environmental Research
Laboratory-Duluth (1971, 1972a, 1972b) recommended chronic toxicity test
procedures for the fathead minnow (Pimephales promelas), the brook,  trout
(Salvelinus fontinalis), and the flagfish (Jordanella floridae).  The U.S.
Environmental Protection Agency (1973) published methods that included, among
others, those just cited for the fathead minnow and the brook trout.  The
European Inland Fisheries Advisory Commission '(1975) in its discussion of fish
toxicity-testing procedures concluded that a continuous-flow procedure was
ideal for obtaining reproducible results for a wide variety of substances.
The Committee on Methods for Toxicity Tests with Aquatic Organisms of the U.S.
Environmental Protection Agency (1975) published both static and continuous-
flow methods for toxicity tests with aquatic organisms.  The American Society
for Testing and Materials (1976) is drafting standard procedures for static

-------
and flow-chrough toxicity tests for chemicals and aqueous effluents.  Methods             J
for both static and contr.uous-flow toxicity tests are included in the 14th
edition of "Standard Methods for the Examination of Water and Wastewater"
(American Public Health Association et al.,  1976).  This latest edition has
been expanded to contain procedures to test  algal productivity, phytoplankton,
zooplankton,  scleractinian coral,  marine polychaete annelids, crustaceans,
aquatic insects, and molluscs.

     As interest increases in the  need for continuous-flow toxicity testing,
we believe that this manual will expedite the generation of data with which to
better protect the aquatic ecosystem.

-------
                                   SECTION  2

                          DILUTEE OPERATION -  GENERAL
     The purpose of the proportional  diluter  (Mount and Brungs,  1967)  is simply
to provide several different mixtures,  or  proportions, of a  toxic  solution
with dilution water.   Such diluters typically provide  five different  toxicant
concentrations and a  control,  which is  dilution water.  The  automatic  and
consistent production of dilutions permits the conduct of continuous-flow
toxicity tests with aquatic organisms.

     The following description and reference  to Figure 1 will  clarify  the basic
components of an operational diluter  and their function.  Dilution water enters
the upper left of the top row  of  glass  cells, called the W,  or water,  cells.
During operation these W cells will empty  to  mix with water  from the  lower
C, or chemical, cells.  The left  W cell will  empty into the  M, or  mixing cell,
and cause the introduction of  a small volume  of the toxic solution.   The two
volumes mix before overflowing into the third level of cells,  the  FS  cells.
When the W cells empty, they cause the  matching C cells to empty by venturi
action.  Different proportions or volumes  of  dilution and toxic-solution waters
are mixed to provide  the different toxicant concentrations to  be tested.
These mixtures enter  the fourth level of cells, the FS or flow-splitting cells,
that divide each concentration into equal  volumes for distribution to  the
replicate test chambers containing the  organisms being exposed.

     A more detailed  discussion of the  diluter operation will  follow  after the
basic components and  construction details  have been described.

-------
Figure 1.  Completed mounted diluter.

-------
                                   SECTION 3

                             DILUTER CONSTRUCTION
EQUIPMENT

     Diluter construction is greatly simplified and much improved by having
the proper equipment,  such as sharp glass cutters,  a glass  cutting table,  a
glass saw, a set of glass drills,  which are used on a standard  heavy duty
drill press, and a power stopper borer.

     Sharp glass cutters are needed to obtain straight,  smooth  cuts to  prevent
leaks.  An optional piece of equipment is the glass cutting board,  similar to
those used by hardware stores to cut window panes.   One  style is  available from
Fletcher Terry Co., Bristol, Conn.   06010.   A large flat surface  and a  good
straight edge may be substituted.   The glass saw is used for cutting glass
tubing and is generally useful for a variety of cutting  purposes.   It is used
to make cut ends on tubing, both square and angled, as required during  diluter
construction.  A rolling table model, such as the Model  C manufactured  by
Pistorius Machine Co., Hicksville,  New York  11801,  is desirable,  but if only
diluter and other glass tubing is to be cut, their  Model CC12,  which has a
tilting table, is satisfactory.  The glass drills are necessary to drill holes
in the various glass cells and are listed as diamond impregnated  tube drills
in the catalog of Sommer and Maca,  Glass Machinery  Co.,  5501 W. Ogden Ave.,
Chicago, 111.  60650.   These drills are relatively  expensive, but  enable the
diluter builder to also drill drain holes in aquaria and test chambers.  The
drill press can be of  any type, but should be sturdy and vibration free.   Hand-
held drills may be used, but breakage is increased.

     The boring of stoppers for various parts of a  diluter  is time consuming,
and a power stopper-borer, such as that manufactured by  E.  H. Sargent Co.
(Model No. S-232DT),  is very useful.   Some glass bending is necessary,  and if
a glass shop is not available,  an  air-blast-type burner,  such as  that
manufactured by Fisher Scientific  Co.,  is very convenient.   This burner enables
the operator to apply  sufficient heat to the tubing to allow uniform bending.
If much glass work is  to be accomplished, a ribbon  burner of at least 6 inches
flame length is also very useful.

     Accurate rulers and steel tapes, a micrometer  for inside and  outside
measurement, felt marking pens, and a sufficiently  large work area to prevent
moving of assembled parts during construction and assembly  also save time  and
increase efficiency.

-------
DILUTER-BOARD CONSTRUCTION

     We'll begin our detailed procedures  with  the  simplest part of  the diluter,
the board and shelves on which the glass  parts for the 2-liter diluter will be
placed.

     The pieces are most precisely cut on a  table  saw, but hand-held saws may be
used as necessary.  Although metric measurements are used in  this report, some
of the materials used in the construction of a diluter are not yet  available
commercially in metric dimensions  (see Table 1 for conversions).  All pieces
should be cut from 2-cm exterior plywood  and assembled as shown in  Figure 2.
The holes necessary to permit exit of the tubing from the bottom of the various
chambers should be marked accurately with the  drilled glass bottom  (to be
discussed later) as a pattern.  They should  be larger than the holes in the
glass to permit manipulation of the stoppers or plastic  tubing.  The bracing
also must be placed so as not to interfere with the glass tubing, but at the
same time to prevent sagging in the shelf.

     The board size shown and the  placement  of the shelves do not need to be
exact, but the W and C cell shelves should slope down to the  right  about 1.3-1.5
cm.

     We have modified these dimensions in various  ways where  space, especially
height, is a limiting factor.  The dimensions  shown have been found to be
useful with regard to cleaning, calibration, and construction ease.


GLASS CUTTING

     The primary skill needed to be successful in  building a  diluter is the
ability to cut glass with straight edges  and parallel sides.  A commercial
glass cutting board, if well maintained,  is  particularly good for long cuts.  A
second technique is to use a large flat sturdy table and a heavy ruler or other
straight edge to guide the cutter.  This  latter technique is  faster and more
versatile once mastered.  All pieces should  be cut with minimum tolerance.
After cutting, all edges should be dulled with a stone or fine-grit sand paper
to prevent hand cuts.  The pieces  should  be  cleaned by washing in a detergent
solution and then rinsed thoroughly and dried.  Removal of grime is necessary
to ensure good glue adhesion.  Glass should  be double strength, but the "B"
or second grade is satisfactory.  Flint glass  tubing is preferred to pyrex
because the lower melting point of the former  makes bending and cutting the
glass easier. •

     The dimensions for all the flat glass and tubing used to construct a
diluter are listed in Table 2; a list of  accessory parts is given in Table 3.
Figures 3 and 4 contain layouts to guide  the builder toward an efficient use of
30.5- by 61-cm glass sheets, a readily available and handy size to  use.  These
layouts will ensure that the proper number of  pieces are available before
assembly begins.  The crosshatched areas  are waste.  The 2-cm drain holes
should be cut before assembly as shown in Figures  3 and 4.  The exact location
of each hole in the W, C, and FS cells should  be marked so that they are
centered between the cell dividers or cell ends (in the case of the FS cells).

-------
TABLE 1.  METRIC CONVERSION TABLE
Inches
48
24
16
14
12
11
10
8
6
5
4
3
2
1
0.75
0.5
0.25
Centimeters
122
61
40.6
35.5
30.5
28.0
25.4
20.3
15.2
12.7
10.2
7.6
5.1
2.54
1.91
1.27
0.64

-------
 27cm
30.5cm
  27cm
 30cm
          DILUTER BOARD
          2cm x 61cm x 122 cm
           W CELL SHELF
           12.7cm x 61cm
           M CELL SHELF
           15cm x 20cm
         - V//////////////////A
              ¥
                C CELL SHELF
                8cm x 41cm
                                      1.3cm
                               !.3cm
 7.5cm
   I
           FS CELL SHELF
           15cm x 61cm
¥
¥
¥
       Figure 2.  Diluter board with shelves mounted.

                          8

-------
           TABLE 2.  DIMENSIONS OF PRINCIPAL CLASS  PARTS  FOR  THE  2-LITER  DILUTER
W Cells



C Cells



M Cells


FS Cells


1
2
2
5
1
2
2
4
1
2
2
6
12
12
bottom
sides
ends
dividers
bottom
sides
ends
dividers
bottom
sides
ends
bottoms
sides
ends
12.7
26.7
12.7
11.8
7.0
21.6
7.0
6.0
21.6
21.6
17.8
10.2
10.2
15.2
cm
cm
cm
cm
cm
cm
cm
cm
cm
era
cm
cm
cm
cm
X 61
X 61
X 27
X 24.1
X 40.6
X 40.6
X 21.6
X 20
X 18.7
X 20.3
X 21.6
X 21.6
X 17.3
X 17.8
cm
cm
cm
cm
cm
cm
cm
cm
cm
cm
cm
cm
cm
cm
5
11
5
4 3/4
3
9
3
2 1/2
6
6
6
4
'•4
6
in
in
in
in
in
in
in
in
in
in
in
in
in
in
X
X
X
X
X
X
X
X
X
X
X
X
X
X
24
24
11
10
16
16
9
8
8
8
6
6
7
7
in
in
in
in
in
in
in
in
in
in
in
in
in
in
Siphon tube length
(W-l through W-6)
(C-2 through C-5)
(M)
(valve bucket)
                               (FS)
   30.5 cm
   25.4 cm
   20.3 cm
dependent upon
    bucket
  dimensions
   17.8 cm
Siphon tube diameter
Siphon tube U's glass
Venturi and siphon tube T's
  connecting tubes (flint
  glass)
Tygon tubing
Siphon sleeve diameter
(W-l)
(W-2 through W-6)
(C-2 through C-5)
(M)
(valve bucket)
(FS)

(W-2 through W-5)
(C-2 through C-5)
(Water blocks  to  C  siphon  U's)
(C siphon  T's  to  FS cells)

(miscellaneous)
   16 mm 00
   12 mm OD
   14 mm OD
   12 mm OD
   10 mm OD
   10 mm OD

   10 mm 3/8 in OD
   12 mm 1/2 in OD
   12 mm
   15 mm

   as needed to
   connect glass
   tubing
(all)    ID area  to  be  ac  lease double of OD area
        of siphon  tube as A « T2 - satisfactorv
        sizes  below
Outer siphon tubes;  size  and length
Wl
W2
H3
W4
W5
M
Cl
C2
C3
C4
C5
FS 12 each
40
18
18
18
18

18
18
18
18
18
14
mm
mm
mm
mm
mm

mm
mm
mm
mm
mm
mm
                                                                 18.5 cm
                                                                 11.8 cm
                                                                 19.8 cm
                                                                 21.2 cm
                                                                 variable depending
                                                                 on cvcle time
                                                                 19 cm
                                                                 11.4 cm
                                                                 11.5 cm
                                                                 10.8 cm
                                                                  7.7 cm
                                                                 13 cm

-------
                  TABLE 3.   ACCESSORY PARTS NEEDED TO CONSTRUCT A DILUTER
Item
Glass cubing
Glass T's
Glass U's
Tygon Y's or glass
T's as available
Glass sheets
Tygon tubing
Box of tissues
Neoprene stoppers
Polyethylene plastic bottles
Plastic container
Glass cutter
Glass glue
Plastic syringes
Dimension
8— nun
10-tnm
12-nna
14-tam
16-mm
18— mm
25-mm
10-mm (3/8-inch)
10-iam (3/8-inch)
12-mm (1/2-inch)
10-mm (3/8-inch)
30.5- X 61- X 0.3-cm
8-mm (5/16- inch)
10-mm (3/3- inch)

For 19-mm (3/4-inch) holes
Size 11
Size 8
125-nl
150-tnl
1-qt


10-ml
20-ral
30-ml

1
6
5
2
1
4
1
6
4
5
4
11
10
10
1
3
2
1
5
1
1
1
2
a?
Number
1-m length
1-m lengths
1-ta lengths
1-m lengths
1-m length
1-m lengths
1-m length
(or pvc pipe
of same size)




ft
ft

dozen



tubes
needed
it
it
Microswitch (Burgess CT2 KRA2 is
  satisfactory)

Solenoid valve, stainless steel
  (Valcor 15P19C8-4 is satisfactory)
                                            10

-------





E
u









2
!S

z
IS
i
UJ
; e
'" (\l
in


IT
u.
ft
i
u.























E
<\
£



0
o


in
o 1
BOTTOM 01

o
'o
!
J c\
If











o
c


0
o

0
0
„
1 "

f
4
j

u
CD
1





t
5
in
cri
t
t
crt
»
I
1
o>
*
1
a>
4
r?
£
u
in
oi
>.

»
r
I

F
g
1



/


u
2

Z
O
3)



-------
g
(M
I
UJ |
* 3 ^
5

f
u
I o
UJ



, u
i fe
u o
u Z
u

1 5
L— i-— —




u
3 i
UJ S
Q 3
(fl



•
1

















IL E
* M
Q £l
z N
UJ



*
E
o 
-------
After the holes are drilled in the cell bottoms,  they can be used as templates
to mark the position of the holes to be drilled in the wooden shelves of  the
diluter board.  These latter holes should be larger than those in the glass.

     The most critical cutting is for the W and C dividers since leakage  will
occur between individual cells if the width of the dividers varies.
GLASS ASSEMBLY

     The most important construction material  is  the  silicone  sealant  or  glass
glue.  Dow Corning Glass and Ceramic Cement and General  Electric  Corporation
RTV are both satisfactory.   Glues that are listed as  dish-water safe are
preferable so that cleaning the assembled diluter with hot water  will  not
cause the joints to fail.  Disposable 10- or 15-ml plastic syringes with
enlarged bores in the tips  for faster application are useful for  applying a
thin bead of glue as needed and can be used with  one  hand  (Figure 5).
Application with the original collapsible tube requires  two hands to maintain
a steady and constant flow  of glue from the tube  to the  edges  of  the glass.  If
the bead of glue is too thin, any irregularities  in glass  cutting will not be
filled by glue and will leak.

     Assembly should begin  with the M and FS cells, since  they are the simplest
in terms of number of pieces.  Waxed or other  paper is placed  on  the table top
to catch any excess glue.  The paper can be removed easily after  the glue has
dried.

     Before placing glue on the glass edges, follow the  assembly  procedures in
a dry run.  For the M and FS cells, glue is placed on all  four edges of the
bottom before it is placed  on the waxed paper.  Next, one of the  two longer
pieces (the right and left  side of the FS cell or the front and back of the M
cell) is held and glue placed on the two end edges.   This piece of glass  is
placed against the bottom and propped in a vertical position.  The opposing
piece is glued and placed similarly.   The remaining two  pieces are placed
against the glued edges already in place.  Slight pressure at  all glued joints
distributes the glue, helps prevent leaks,  and places the glass surfaces  in
closer contact.  To ensure  against leaks, a pencil eraser or rounded wooden
dowel may be used to spread the freshly applied,  excess  glue along each seam.
Use care to avoid moving the glass.

     The fronts, backs,  and bottoms of the W and  C cells should first  be  placed
as shown in Figure 6 and the lines drawn as indicated to show  the location of
the cell dividers during assembly.  A wax pencil  or felt pen can  be used.
It is important to remember during assembly, however, that these  marked surfaces
should be on the outside of the cells so that glue adhesion is not affected by
these lines.

     The W and C cell assembly procedures are identical.  The  initial
difference between this procedure and that used for the M and  FS  cells  is
that the W and C cells are  built beginning with the back piece placed  on  the
table top.


                                      13

-------
                                (SIDE VIEW)
                                       TABLE TOP
                                (TOP VIEW)
GLASS
    Figure 5.  Glue-application system.  Syringe tip to be bored out to
             approximately 4 mm to give sufficient bead size.
                               14

-------
   W CELLS
27 S

<
12'
f
cm

•

'cm
J
27 <


'
>cm


SACK



BOTTOM
o
FRONT
u 20.3
cm





o

76
••cm-*





o

_7.6_
cm





o

_76 _
cm





o

76
cm





o

_ 10.2 _
cm
                      -61cm-
          C CELLS
k
229cm
*
I
76cm
i
22.9cm

.,

BACK


BOTTOM
O
FRONT
177
cm





o

8.9_
cm





0

§
v





o

1
po





o

63
cm
                     • 40.6cm •
Figure 6.   Gluing layout for W  and C cell;
                     15

-------
     A bead of glue is  placed on the bottom edge and ends of the back piece of
the W or C cell,  and it is placed on the paper covering the table top.  Glue is
placed on each end of the cell bottom, which is then placed against the large
edge and supported as shown  in Figure 7.  If the angle between the back side
and bottom is kept at slightly more than 90°, the first divider can be placed
more easily.  Beads of  glue  are placed on three edges of the first divider;
none is added to  the top edge.  This divider is placed on edge on one of the
lines on the back side  of the cell so that the two bottom edges are in line
(Figure 7).  The  bottom of the cell is rotated up to a 90° angle with the back
so that the bottom edge of the divider matches the line drawn on the cell
bottom.  Continue to support the bottom with a block.  Glue is added to three
edges of each of  the remaining dividers and each is carefully placed in
position.  The next step is  to place a bead of glue on the bottom edge and
ends of the front side. This edge is placed in the corner formed by the
bottom of the dividers  and the bottom of the cell.  The front side is then
lowered to rest on the  dividers so that those edges match the lines drawn on
the front side.  If difficulty is encountered with multiple gluing of the W
and C cell dividers, each may be glued on one short to long side only and set
individually, leaving a 2-hr setting period between each.  After these are
dry, glue may be  applied to  the long exposed edge of each divider.  The long
edge of the eventual front is also glued, and the front is placed on the glued
edges as above.  The ends can now be put in place without glue since they will
contact previously glued edges.  As with the M and FS cells, a pencil eraser
or wooden dowel can be  used  to smooth the glue before drying to help prevent
leaks if this is  necessary.  With practice, this procedure may not be necessary
as the glue beads should then be placed evenly enough and thick enough to
avoid leaks.

     After all cells have dried overnight, they should be tested for leaks after
plugging the drilled holes.  The exposed edges should be smoothed with a file
or sandpaper to eliminate cuts.  All cells can now be placed on the diluter
board in the approximate positions shown in Figure 8.

     Other assembly procedures may become more desirable after experience has
been gained.  The above details should be acceptable for beginners.
                                      16

-------
                                                                        0)
                                                                        o
                                                                        3
                                                                        T3
                                                                        01
                                                                        
-------
                                        • 61cm •
          127cm

          /
        279cm
                             i	,
                              /  0
                       /
                      ,'  0
                                                      	f...
               /   0
                                                      .DIVIDER (5)
                                                       12 Icm x 25 4cm
                                76 ,L 76 ,1 76  !  76
                                cm^~ cm ~^~ cm~^~ cm
                                          102  J
                                           cm"*
     152cm
                                   - 40.6cm -
7Scrr
i
A




Q__.
.7cm
i
I



+
/











i

f











	


0
A
/
/
•







" 7
/
/
i











— — -i


0
A
/
t
'







-1

t
v°
/
1
/
t
1
1
t
1
t
1
1
•*--L
| J

'rH
\A
y
4








7-7
/

'











	


0
I
1




























                          178     J.  S 9  ,-1.45,1221-,  73
                          cm         cm   cmHcnv  cfn
                                                         .DIVIDER (4)
                                                          7cm x 20.3cm
   15 2cm-
17.8cm
              >
      /   0
     U-I02-
        cm
                 *
                *
/  o
                               .....Ji.
                  -10.2 -
                   cm

•   o
 -102-
  cm
-102—J
 cm
         Figure 8.   Final assembly  plan for all  cells.
                                       18

-------
                                   SECTION 4

                               DILUTER OPERATION
MECHANISMS OF ACTION

     The operation of the proportional diluter (Figures  1,  9,  and  10)  depends
on the venturi action of water flowing past a  tube  which is part of  a  closed
air system.  The principal is the reverse of that of  a carburetor  in which
incoming air sucks gasoline from the carburetor jets.  As water flows  through
the W cells and overflows by siphon by siphon  W-6 into the  valve bucket,  the
weight of the valve bucket increases and operates the microswitch, which  causes
the valve bucket to come to rest on the bucket stop.  This  closes  the  diluent
water valve allowing the water levels in the W cells  to  drain  down to  the tops
of the dividers.  As the valve bucket fills, its siphon  begins to  empty
through the venturi T (Figure.10).   As water passes the  opening of the vacuum
line, air is removed resulting in a reduction  in air  pressure  in the vacuum
line.  This water from W-6 passes through the  venturi T  and to FS-6  as the
control test water.  The vacuum line connects  to the  siphon U's.in cells  W-l
through W-5 (Figure 9).   Each siphon U is covered on  one end by water  in  its
corresponding W cell and on the other end by water  in the water block.
Consequently, the air volume within the vacuum line is closed  to the atmosphere
at the time the vacuum is applied by the venturi action  of  the venturi T.  As
the air pressure decreases in the vacuum line, water  is  pushed into  each  end
of each siphon tube in cells W-l through W-5 by the atmospheric pressure, which
exceeds the pressure in the vacuum line.   As the water enters  the  top  of  the
siphon tube a siphon begins, which empties these five cells.   The  W-l  cell
empties into the M cell where the toxic solution is added,  resulting in the
highest toxicant test concentration.  Cells W-2 through  W-5 empty  through the
C cell Venturis from cells C-2 through C-5. Again, the  pressure inside the C
siphon tubes is reduced, and those cells containing the  toxic  solution are
emptied into the FS cells together with the dilution  water  from the  corresponding
W cells.  Since the W-l cell contains the greatest  volume of water,  the
remaining W and C cells should be empty before the  M  cell containing the  water
from W-l and the added toxic solution overflows to  refill the  C cells.  (If
the M cell begins to empty before the siphons  are broken in W-2 and  C-2,  the
water from the M cell will be siphoned out through  the C-2  siphon.)  Cells
C-2 through C-5 are filled, and the remaining  2 liters of the  highest  toxicant
test concentration water enters C-l to flow to FS-1.  All the  tubes  emptying
into and from the M cell and into the valve bucket  and into the FS cells  should
be cut at about a 45° angle so that the tube drains completely after siphoning.

     The selection of the tubing sizes controls the flow rate  of water from
W-6 through the venturi T to FS-6 so that the  valve bucket  contains  water long
enough to keep the dilution-water flow from entering  W-l before W-l  has

                                      19

-------
  OIUJTION
  WATER
SWITCH
                                                          VACUUM
                                                          .LINE
                                                          TRIGGER
                                                          LINE
                                                          SPRING
                                                          T VENTURI
Figure  9.   Tubing and accessory plan for assembled diluter.
                               20

-------
TRIGGER LINE
FROM
MICROSWITCH.
VALVE
BUCKET.
                   1—SPRING
               P
BUCKET STOP	/
                                .FLOW NOTCH

                                .SIPHON ASSEMBLY
                                VACUUM
                                  LINE
                                       ,VENTURI T
                                WATER
         Figure 10.  Valve bucket assembly.
                      21

-------
completely emptied into  the M cell.  If dilution-water flow begins before the
W-l siphon is broken, water will continuously flow directly through W-l
preventing the filling of  the remaining W cells and subsequent proper
functioning of the diluter.

     When most of the control test water from W-6 has flowed out of the valve
bucket allowing it to rise from the bucket stop and causing the microswitch to
open the dilution-water  valve,  the diluter should be in the following mode:
(1)  All W cells are empty and  their siphons broken; and (2) the M cell has
emptied to fill cells C-2  through C-5.  The cycle will begin again at this
time.
FLOW RATE REQUIREMENTS

     The flow rate of the  dilution water  determines the length of each cycle
of operation, and this flow rate  is  adjusted  t3 obtain the desired flow to the
test chambers.   If duplicate test chambers are used, as this design allows,
1 liter of test solution will enter  each  test chamber each cycle from the
2-liter diluter.   The total test  solution for the diluter is 12 liters per
cycle.   If each test chamber contains  20  liters and the experimental design
requires 10 volume exchanges per  day,  a total of 200 liters is necessary for
each chamber each day.  Consequently,  200 diluter cycles per day are required;
this is just over 7 min per cycle (1,440  min  •=• 200).  The dilution-water flow
rate is then set  to provide 12 liters  of  water plus the rest of the cycle in
7 min.

     Coordination between  flow rate  and volume is necessary for the diluter
to function.  The flow rate of dilution water and the height and size of the
siphon cell W-6 must be such that the  amount  of water flowing between the
time the valve bucket turns off the  dilution  water and cell W-6 empties is
equal to the delivery volume (2 liters) of one cycle to the rest of the pairs
of cells.  The size of the bucket and  the height of the siphon must be such
that the water begins to flow out of the  valve bucket just before the water
stops flowing from cell W-6.  The line from the valve bucket must be just small
enough so that all of the  other operations of the cycle will be completed
before it empties.  A smaller line will work, but it will lengthen the cycle
time needlessly.   The venturi T must be sized so that it will draw a stream of
bubbles from the vacuum line during  the flow  from the valve bucket.  The
siphon in the M cell must  be adjusted  so  that nearly all of the water from the
W-l cell has entered before the siphon starts the flow into cell C-2.  This
siphon should be irather large so  that  after the flow starts it will empty fast
and not delay the cycle time.  The last consideration for smooth operation is
at the venturi below the C cells. In  this case, the size of the pipe from the
W cells must be such that  a good  vacuum is formed.  The main consideration
here is that the tube from the W  cells is not too large causing the water to
back up into the C cell outlet tubing  rather  than forming the necessary vacuum.
                                      22

-------
ACCESSORY PARTS

     By now the reader should have an adequate general understanding of the
proportional diluter and should be able to begin the connections between the
various W, M, C, and FS cells.  The principal accessories are the valve
bucket, venturi T, microswitch, dilution-water valve,  water blocks,  siphon
tubes, neoprene stoppers, and miscellaneous glass and plastic fittings  and
tubes (Table 3).  The toxicant-metering devices will be discussed in a  later
section.

DILUTER ASSEMBLY

     First cut the required five tubes for cells W-2 through W-5 31.5 cm (1 ft)
long from 10-mm OD glass tubing.  Notch one end of each tube about 12 mm deep
with the glass saw; remove about one-half  of the wall.  All tubes should be
notched approximately the same.

     Bore stoppers to fit the tubes,  and install into bored holes in W  cells.
In chambers W-2 through W-5 the bottom of  the tube notch must be above  the
tops of the dividers to prevent premature  siphoning.  The siphon in cell W-6
is installed with all of the tube below the dividers so it is self initiating.

     Cut the required five tubes 25.5 cm long from 10-mm OD tubing for  the C
cells.  Notch and install in cells C-l through C-4 with notch bottoms above
the dividers and in cell C-5 with the complete tube below the dividers.

     Cut the one required tube 25.0 cm long from 10-mm OD tubing.  Notch and
install with all of the tube 25 mm below the top edge of the M cell.

     Cut the required 12 tubes 23.0 cm long from 8-mm OD tubing.  Notch and
install with all of the tubes 25 mm below the top edge of the FC cells.   (Note:
If notches are not of identical depths, install with the bottom of all  notches
35 mm below the top of FC cells.)

     Cut the one required tube 34.0 cm long from 18-mm OD tubing; bore  a 4-mm
hole in the side of the tube 48 mm from one end.   Notch the opposite  end to
install in cell W-l with the 4-mm side hole at a 45° angle to the divider
between cells W-l and W-2 and just below the bottom of the chamber support.
Glue in place with silicone sealant.

     Select and remove the tube restrictions from four 14-mm OD glass T's.   Y's
may be used, -but one arm of the Y must be  bent to clear the W cell supports.

     Select four 10-mm OD glass T's,  remove the tube restrictions from  the
opposite ends, and fasten together with suitable Tygon pieces with all  the
right-angle outlets in the same plane to make the vacuum manifold.   Fasten to
the top of the W cells.

     Cut 10-mm-diameter center holes  in the bottom of  four 125-ml plastic
bottles.  Select and remove the tubing restrictions from four 14-mm OD  T's
(1/2-inch).  Drill a 14-mm hole in neoprene stoppers of suitable size to fit
the tops of the 125-ml bottles.

                                     23

-------
     Insert one cut end of a T into each stopper, and add 40 ram of 14-mm  (1/2-
inch) tubing to each to make a water block.

     Cut four 46.0-cm lengths of 12-mm OD glass tubing.  Heat the plastic
bottles slightly (hot water or careful use of burner or heat gun) and force
the tubing into the predrilled hole in each bottle to within 10 mm of the inside
top of the bottle.

     Make four 90°  smooth bends (90 mm around the curve) from 14-mm tubing.
Select and remove the tubing construction from two ends at the right angle of
14-mm T's.  Connect the T to the C cell siphons with the right angles and
appropriate Tygon tubing.  Attach the T water-block assembly with suitable
Tygon tubing to the standpipes of cells W-2 through W-5 and to the C cell T's.

     Mount the valve-bucket stop 32 cm below and the spring support just below
the bottom of the W cells.  Attach the microswitch to the spring support by
using a small block of wood.  The spring should have just sufficient power to
lift the empty bucket.

     Cut both ends from a 250-ml (6-ounce) polyethylene bottle leaving a
cylinder 70-75 mm long.  Select two size 11 stoppers to fit the ends of the
cylinder and bore a 19-mm (3/4-inch) hole in each near one edge.  Bore a
14-mm hole in a size 2 stopper, cut a piece- of 14-mm glass tubing 90 mm long
and insert both into one large stopper.  Mount the W-l cell water block onto
the W-l outlet to just below the 4-mm hole with the second large stopper.
Insert a short piece of 4-mm tubing into the hole and connect with suitable
tubing to the vacuum manifold.

     The preceding assembly instructions result in a diluter system that will
function normally.   The given dimensions, however, are not in most cases  the
only ones that will work.  The most usual and easiest changes are those required
by vertical space limitations found in many laboratories.  All of the glass
chambers, W, M, C,  and FC cells, can be made shorter and deeper from front
to rear if necessary.  This, of course, makes the cutting of glass more
wasteful, but the diluter will function.  The simplest procedure is to determine
the total height available.  Distribute this between the four layers; then,
using that dimension vertically, use the given dimension horizontally to
determine the depth dimension by dividing these into the volume.  All vertical
tube lengths must then be adjusted to fit depending upon the amount of change
decided upon.  One precaution that must be taken is to adjust the siphon
lengths carefully as a small vertical dimension change has a large effect
because the two horizontal dimensions contribute much more to the volume.

     When the diluter has been assembled and all tubing is connected, the
equipment should be checked for leaks.  When it is leak free, all of the
chambers should be fastened to the diluter board with small clips and screws
(mirror clips work well) to prevent breakage during cleaning or other manipulation.

     The valve bucket  (either a cut-off 2-liter bottle or a 2-quart plastic
freezer box is satisfactory) is mounted by putting a stainless steel light rod
or heavy wire across the bucket as a hanger.  The siphon venturi of 10 mm (3/8


                                      24

-------
inch) is positioned  under  the  bucket  (Figure 10).  The venturi is prepared
by cutting off the tubing  restrictions on  two right-angle ends of the T and
mounting the T with  the  remaining  restriction towards the bucket.  The siphon
in the bucket is 10-mm tubing  15 cm long,  and the outer tube is 15-mm tubing 10
cm long.  (If very short or  long cycle times are desired, these dimensions must
be modified to suit.)  The bucket  is  hung  from the upper bracket with a
spring and light stainless steel wire.  The operating arm of the microswitch
is fastened to the bucket  hanger by a piece of monofilament line set so that
the microswitch is on  when the bucket is up and off when the bucket is resting
on the bucket stop.   (See  section  on  Mechanisms of Action for further
explanation.)

     Care must be taken  to leave enough slack in the exit tube of the valve
bucket where it is attached  to the venturi T so that the tubing does not hinder
the action of the spring.  If  very cold water is run through the diluter this
becomes an important consideration as the  tubing becomes very stiff and may
cause malfunction of the switch.
                                    25

-------
                                   SECTION 5

                              DILUTEE  CALIBRATION
PRECALIBRATION

     Table 4 contains the necessary cell  delivery volumes  for 50% and  33%
dilution ratios for 2-liter diluters with five  test concentrations and a
control.  The easiest procedure for initial  precalibration requires  th&t the
W-l through W-5 and C-2 through C-5 cells be filled with an excess that
overflows into the W-6 and C-l cells.  A  siphon emptying into a  graduate
cylinder is used to remove the appropriate volume in a cell; the contents of
the siphon itself are returned to  the  cell.   A  mark is then made at  the
resultant water level.  The siphon sleeve is cut to end at this  mark.  The
core from a neoprene stopper can be used  in  the top of the siphon sleeve (see
Benoit and Puglisi, 1973 in Appendix).  Adjustments in the position  of this
neoprene core in the siphon sleeve allow  for final, more precise calibration
if necessary.

     Calibration of the M cell and valve  bucket is different since these
containers should be nearly empty  after siphoning.  The appropriate  volume
(Table 4) is added, and a mark is  made to represent the water level.   The top
of the siphon tube is set at this  level.   The siphon sleeve is placed  so that
it is near the bottom of the container, but  not so near as to restrict the
water flow.  Since the siphon tube is  notched at the top,  a siphon effect will
begin just before the total volume enters the container.   The volume of control
water entering the valve bucket is dependent upon the flow rate, and any
variation in the latter will change this  volume.  If the valve bucket  does not
empty completely, the spring may not be strong  enough to reset the microswitch.

     The top of the W-6 siphon tube is below the top of the cell divider.  The
siphon sleeve should be set so that less  than the required 2-liter volume is
needed to start the siphon to accommodate the time lapse between the beginning
of the siphon and the turning off  of the  valve.  Also, after dilution  water
stops entering"the W-l cell, some  water will continue to enter W-6 as  it
drains down from the other W cells. As a start, have the  W-6 siphon begin
after about 1.5 liters have entered the W-6  cell and adjust if necessary.  The
reader is referred to Benoit and Puglisi  (1973) in the Appendix  for  details
on calibration of the flow-splitting cells.
FINAL CALIBRATION

     After precalibration has been completed,  the  diluter should operate at
least overnight before making final adjustments.   These  final adjustments

                                     26

-------


J
o
OS
f— 1
z
o
u
a
z


CO
z
o

«t
^J*
o-
c—
z

CJ
z
o


bJ

M
Pi
—•
£-,
^_4
3

cn
as
a
c_t
3
M
O

OS

M
N-3
1
CN1

oi
O


CO
bJ
2"
3
J
O
'>
s-
OS
U
r-l
, 1
rTl
Q
,
t i
W
U


•
—

rT1
rJ
3

H












C
O
•H
3
r«4
•rt
-O
5^5
C"*!
co






















C
Q
i-t
4-1
3
rH
•r-l
•o
8-8
O
m












































^•^
>^
u
o
>
•H
^^
01

\^s

s
g
3

O

















^^
^
j.,
01
>
•H
r-l
01
-o


CO
01
s

I— 1
o











4-1
•H

C
3
cr











e
0)
u
M







4J
Ol
3
0

^2
sH'g'S 1 3 "3 "3 -H
3
. • .r-l
co r^« CJN co r^ co i— i r^ CN S
C^ ^40 00 ^ 00 CO •— 1 CO r-|

CN t-^ f-^ rH rH in
**
CN

T
r-4
O
^

4-1
CO
3
S




4-1
U

4^
3
O

^
4J
•H
i— t iH •— * , "s
^ CO
01
4-1 T3 O
cfl O
oi :N
c —i CN
•—* 4_)
^
C 11
"^ ^
ca —i
01 oo
^
0
3 4J
0
T-H r-l
U-l g





O
O
00
M
CO

4-1
3
O ^
•4^ CO rH
CO rH S
Ol
4J -a o
co O
4) 
oo -i-i
01 00
^
o
3 4-1
O
r-l r-l
i[ j p






•vO





cn

p— t
01
CJ

co
c
•H
ij
4-1
•H
t-4
p-
1
3
o
r-l
ti,
01
«
w
3
C
r^
U-i
C
.r4

CO
c
G
4J
CC
••H
r4
73
>


•
01
r-l
^2
•H
CO
cn
c
c.
cn
CO

r-l
g

O
o
o
*l
CN
o


0)
cn
o
I—I
0

cn
C3

rJ
0)
>
•r^
r-l
01
•o

•a
f^
3
O
^
cn
rH
(— i
OJ
^J
^-^
r-4
o
r4
U
C
Q
CJ

r4
O
v"^

vO
1

4)
^
H
CO




























































^
j^
CO
>
0
u

e
3
r-l
0
>

cn
«rJ
-"-
U

01
cn
3
a
CJ
r^
r-l
•rH
3

27

-------
should take place while the diluter  is  functioning but with the delivery tubes
to the test chambers themselves  diverted  so  that any accidents during calibra-
tion while tests are ongoing will not adversely affect the test.  The delivery
volume from each cell should be  checked at least twice for proper accuracy.

     The W-l volume is collected by  an  appropriate graduate cylinder or other
container as it enters or  leaves the M-l  cell.  Necessary adjustments are made
based on common sense by moving  the  neoprene stopper core up or down in the
siphon sleeve to increase  or decrease,  respectively, the volume transferred.
By common sense we mean that only the necessary level of accuracy (1 to 5
percent usually) is desirable.   Finer adjustment is only time consuming.  Cells
W-2 through W-5 are calibrated one at a time by disconnecting at the C cell
venturi the tube that connects the water  block to the C cell venturi.  The
water from the M cells is  then collected  when the diluter functions.  The
corresponding C cell will  not empty  during this calibration step.  After some
experience, two W cells can be checked  at once.  The W-6 volume, as discussed
earlier, is flow dependent and should only be calibrated at the intended flow
rate.  Its delivery volume can be taken at the discharge from the valve bucket
or where it enters the control flow-splitting cell.  Do not take it before it
enters the valve bucket since the valve will not function.  Adjustments in the
delivery volume are made fay the  neoprene  stopper core in the siphon sleeve of
W-6.  Once the transfer volumes  of cells  W-2 through W-5 are fixed, cells C-2
through C-5 are calibrated by collecting  the total flow from the paired W and
C cells before it enters the flow-splitting  cells.  The C cell volumes are
calculated and adjusted by difference between the total volume of the two cells
and that corresponding W cell volume previously determined.  The C-l cell
volume is measured as a double check on the  calibrations of cells W-l and C-2
through C-5.  Finally, the flow-splitting cells are calibrated after the
delivery tubes are replaced to simulate normal operation.  The transfer volumes
are collected at the test  chambers,  again to simulate normal operation.  These
flow-splitting cell volumes should be checked weekly and after any cleaning or
other manipulation.
                                     28

-------
                                   SECTION 6

                               TOXICANT METERING
     The bibliography to this report contains numerous citations for toxicant-
metering systems.  Any system should be activated only by diluter operation to
avoid overuse of the toxicant.   We have had significant experimental experience,
with three systems, and we will discuss them in the order of their development.

     The "dipping-bird" system (Figure 11)  was described by Mount and Brungs
(1967).  Details can be found in the Appendix.  This metering device is useful
for water-soluble,  non-volatile toxicants and some suspended solids.  It can
be made most easily from a volumetric pipette (Figure 12) of an appropriate
size, usually between 2 and 50 ml.  The dipping bird is located between the
W-l cell and the M cell.  The cup is filled when W-l empties and the weight
and force of water rotates the arm about the pivot to introduce a known and
constant volume of stock solution.  A small-diameter tube from the side of the
W-l water block above its normal water level should be used to put water in
the cup.  The force of all the water from cell W-l could damage the dipping-bird
assembly.  After cell W-l is empty, the cup contents empty through the drain
hole allowing the arm to return and refill.  The adjustable weight is necessary
to ensure proper rotation.  By adding successive known quantities of water
(100 ml) to the Mariotte bottle (2- to 5-gal) it can be calibrated by marking
with a diamond point pencil so that the amount of toxicant used each day can
be determined.  When the amount of toxicant is divided by the number of
diluter cycles over a known time period, the mean toxicant-delivery volume per
cycle can be determined by calculation.  An electric counter wired to the
microswitch will provide the number of cycles.  Also, the mean cycle time can
be determined.  For example, over a 24-hr period (1,440 min) there were 576
cycles and approximately 1,210 ml of stock solution were used.  The mean cycle
time was 2.5 min, and the mean dipping-bird volume was 2.1 ml.  This procedure
is used for calibration of the dipping bird, and it is required daily to
monitor dilution-water flow rate and nominal toxicant concentration.

     The McAllister system (McAllister et al., 1972) is described in the
original paper.   It also requires a Mariotte bottle system.   The detail of its
relationship to a proportional diluter is shown in Figure 13.   This device is
more useful for volatile toxicants or toxicants dissolved in a solvent as there
is reduced contact with air.  Figure 14 shows a modification of the McAllister
system by Puglisi (unpublished data) to protect against a malfunction of the
Mariotte bottle that would permit the introduction of excessive amounts of the
stock solution.   The McAllister system can  be calibrated and monitored in the
same manner as the dipping bird.   When constructing this device,  the capillary
tube should be as small as possible to prevent variations in the addition of
the toxic solution if variations  in siphoning by cell W-l occur.

                                      29

-------
                                                             e
                                                             
-------
                           .NOTCH
    CUT.
           VOLUMETRIC PIPETTE
              BEND
  FIRE POLISH
  TO
  FfcRTIALLY CLOSE
FILLING NOTCH
              FINAL PRODUCT
Figure 12.  Construction plan for a "dipping bird" toxicant metering
         system using volumetric pipette.
                        31

-------
                                                               en
                                                               ^
                                                               en
                                           -1
                                           LU
                                           O
                                                               ao
                                                               c
                                                               en
                                                               3
                                                               0)
                                                               cn
                                                               en
                                                               rt

                                                               oo
                                                               C
                                                               OJ
                                                               £
                                                                I
                                                               u
                                                               C
                                                               ctt
                                                               oo
32

-------
_7mm O.D. TUBING
                                               MOVABLE
                                               SLEEVE
                 2cm

               CAPILLARY TUBING
        DELIVERS
                                                         LIQUID LEVEL


                                                      .  INVERTED BOTTLE
                                                      U or BEAKER

                                                        VENT

                                                        CUT OFF STOPPER

                                                               FROM
                                                               MARIOTTE
                                                               BOTTLE
                                                          "SAFETY DRAIN'
  Figure 14.  Safety system
                            for the "McAllister  toxicant-metering system"
                                     33

-------
     The third system is  the  multiple syringe injector as described by DeFoe
(1975) and included in the Appendix.  This system completely eliminates
vaporization problems and is  useful  for highly toxic chemicals dissolved in
organic solvents.   An additional very useful aspect of this system is the
ability to change the dilution factor without recalibration of the diluter.
Since each concentration  has  its own stock bottle, dilution factors can be
changed by changing stock-solution concentrations.

     Since two of these three systems require a Mariotte bottle, some advice
as to their construction  and  use is  necessary.  The glass bottle itself should
be of 1- to 5-gal capacity and have  a narrow mouth for filling.  The mouth will
be sealed with a neoprene stopper while in use.  A small hole should be drilled
in the shoulder of the bottle into which will be placed a neoprene stopper with
a glass tube (not capillary),  the bottom of which will determine the liquid
level in the metering system.   An additional small hole near the bottom is
used for connection to the metering  system.  As the stock solution initially
drains from the bottle, a partial vacuum is produced and air will enter the
bottle through the air tube until the air pressure stabilizes.  This initial
flow may exceed the capacity  of the  metering system and should not enter the
M cell.  After stabilization,  air will enter the bottle whenever any liquid
is removed by diluter operation.  Wide variation in room temperature causes
variation in the pressure in  the bottle and subsequent delivery of the toxic
solution.  In this case the bottle should be insulated in such a fashion that
the calibrations can be read  daily for monitoring-diluter operation.
                                     34

-------
                                  SECTION 7

                            DILUTEE MODIFICATIONS
     The proportional diluter lends itself to numerous modifications.   An
experienced person who has built several diluters can usually modify them to
adapt to special cases.  It is recommended that a regular diluter be made and
used first, before modifications are tried.   The following directions assume
familiarity with the basic diluter.  Some of the modifications that we have
used are multiple synchronous cycle systems; low toxicity effluent, i.e., 100%
effluent; superimposed additions, i.e.,  turbidity or food added in equal amounts
to all concentrations and then a toxicant added and diluted;  and equal solvent
concentrations with dilution of only the toxicant and including a solvent
control.

     The use of multiple diluters in synchronous set (Figure  15) is accomplished
as follows (Arthur et al., 1975).  An extra  W cell is added and fitted with an
overflow to waste, and the regular sixth or  control cell is fitted with a
water block and starting siphon.  The other  cells are the same as in an
unmodified diluter.  The flow-adjusting  valves on the separate diluters are
adjusted to fill the W cells just a little faster than the required cycle time.
All of the vacuum lines are connected together and are started by a side-arm
vacuum aspirator from a water line by having the valve-bucket switch turn on
the water as needed.  Timing is accomplished by building a separate timing
chamber such as shown in Figure 16 (Halligan and Eaton,  1978).  The fill
time for this upper bucket is slightly longer than that of the W cells.  When
this chamber cycles into the valve bucket, the supply solenoids are shut off
and the vacuum aspirator is activated.  The  emptying time must be sufficient
to allow all diluters to cycle, and when the valve bucket finally empties the
cycle is repeated.  Equal flows are not  necessary once all diluters are started
as long as the valve bucket stays down until the last diluter completes its
cycle.  We have successfully operated three  2-liter and three 1-liter  diluters
synchronously for nearly a year (Arthur  et al., 1975).

     In many instances it will be necessary  to determine the  toxicity of
industrial and municipal wastes or other materials that may not be extremely
toxic.  Mariotte bottles or similar stock solution supplies are inadequate
when toxicity is measured in percentage  instead of milligrams per liter.  The
details for a modified diluter whose highest test concentration is 100% effluen'
are shown in Figure 17.  Only a few changes  need to be made on a standard
diluter to convert it to an effluent-testing diluter.

     1)  The vacuum tube to cell W-l is  clamped so that the cell cannot empty

     2)  The M cell and chemical-metering device may be removed.

                                     35

-------
                                                                 I
                                                                 4-1
                                                                 tn
                                                                 >!
                                                                 Cfl

                                                                 u
                                                                 01
                                                                 4-1
                                                                  3
                                                                 r-l
                                                                 •H
                                                                 •o

                                                                  0)
                                                                  f-1
                                                                  o.
                                                                   §

                                                                   05
                                                                   3
                                                                   O

                                                                    0
                                                                    !->

                                                                    O
                                                                    c
                                                                     l-i

                                                                     O
                                                                     C
                                                                     ca
                                                                      0)
                                                                      u
                                                                       ea
36

-------
                                                                B

                                                                01
                                                                0)
                                                                u
                                                                3
                                                                01
                                                               i-l
                                                                a.
                                                                3
                                                                00
                                                               •H
37

-------
        DILUTION
        WftTER
EFFUJENT
 WATER
Figure 17.  Diluter  modifications  for effluent  dilutions.
                             38

-------
     3)  A new C-l is constructed and placed on the M cell shelf.  It will
have a standpipe siphon to deliver 2 liters.  A water block is connected to
the vacuum line.  The vacuum line that had gone to the W-l cell can be extended
to go to the new C-l cell.  The old C-l cell will empty to waste.  The new C-l
cell is built to overflow into the old C-2 cell.  The tube from the new cell
C-l water block will go to the same FS cell as did the old cell C-l.  The
siphon standpipe in the new cell C-l must be slightly higher than the over-
flow tube to cell C-2 to prevent a premature siphon.

     4)  An additional water valve is used to discharge effluent into the new
C-l cell and fill the remaining cells.  This valve is also connected to the
microswitch under the valve bucket.  Consequently, both valves open and close
together.  The effluent flow rate is set so that cell C-5 overflows into the
old cell C-l and then to waste before the valve is turned off.  If the flow
rate is too slow, one or more of the last C cells will not be full when the
diluter cycles.  The dilution-water flow rate may need adjustment since the
large W-l volume is not needed in this mode.

     5)  All changes can be made in a temporary fashion for easy conversion
back to the basiic diluter.

     If there is a continuing need for an effluent-testing diluter, the above
modifications can be incorporated into the original design.

     Additions of food, suspended solids, or other similar materials in equal
concentrations to all of the test tanks (Brungs and Bailey, 1967) as well as
variable toxicant concentrations can be accomplished as follows.  A special
chamber much like that described fay Brungs and Mount (1967) is used.  Each
diluter receiving the material requires one cell (Figure 18).  An extra cell
is used for timing, and the water coming from it is sent to waste.  Water
flowing from those cells used to supply the diluter is used to activate a
metering device that meters the desired amount of material into the mixing
chamber, which in turn empties into the W-l cells of the diluters of standard
design.  Operation of this system is quite similar to regular operation.  This
modified system differs in two important ways:  (1) each of the initial
chambers must be calibrated to deliver exactly the required amount of water
to feed the diluter including the control (i.e., 12 liters for five concentra-
tions and a control on a 2-liter diluter); and (2) a microswitch or dilution-
water valve is not needed on the diluter since the diluter itself does not
control the flow rate.  If suspended solids are used and settling of these
solids is undesirable, the siphon tubes can be set to nearly empty the cells
and thus reduce settling.

     The injector system of DeFoe (1975) described in Section 6 is an
additional useful modification.  In the standard diluter, when materials with
high toxicity and low solubility are tested, acetone, ethyl alcohol, or similar
low-toxicity water-miscible organic solvents are used to disperse the low-
solubility material in the water.  This dispersant is then diluted in the
same proportions as the toxicant.  In certain cases it is necessary to
maintain a constant dispersant concentration and vary only the toxicant
concentration.  This system is a series of equal-sized chambers.  As these
empty, a ratchet-driven syringe is activated for each concentration.  The


                                      39

-------
                                                                                                  01

                                                                                                  H
 V)
 3


1
 O
 o
 0)
 tn
 S  en
 Cfl  iH
•M  (fl
 C  -H
 (0  h
 oo cj
 M  U
 O  cj
 o  6
 V4
 O  M
•H  nj
 6  ^
-^ -H
     e
 >, -H
r-l   tfl
 O.
 Q.  W
 3   0)
 en  £
    u
 T3   O
 O
 O   M
 «-i   O

 (Q  u
 C
 O
                                                                                                       C
                                                                                                       o
                                                                                                   •U  T-l
                                                                                                       •O
                                                                                                   Ol  TJ
                                                                                                    O  JS


                                                                                                   T-l


                                                                                                    O   O
                                                                                                   •a  -o
                                                                                                    >  >1
                                                                                                    en
                                                                                                    ai   e
                                                                                                    u   01
                                                                                                    3   4J
                                                                                                    rH   «
                                                                                                    •H   X
                                                                                                   00
                                                                                                    3
                                                                                                    00
                                    40

-------
syringes are set to deliver a constant amount of dispersant containing various
amounts of the toxicant.   It is also  possible with this  system to test several
compounds simultaneously  for screening purposes,  if desired.
                                    41

-------
                                   SECTION 8

                               TROUBLE-SHOOTING


     Most dilutee malfunctions occur during the  first  days  of  operation or
after modification or calibration.   Listed below are some of the most common
problems (A-D) and their causes (1-4).

     A)  Loss of water flow.

         1)  Electric power failure or  accidental disconnection.

         2)  Defective microswitch  or water valve.

         3)  Weak valve-bucket spring that will  not lift valve bucket.

         4)  Too much water remaining in valve bucket  after emptying.  Adjust
             siphon sleeve.

     B)  W cell siphons won't start.

         1)  No water in one or more of the water blocks.

         2)  Disconnected vacuum line.

         3)  Dirt or other debris in vacuum tube.

         4)  Venturi T not functioning  properly.

     C)  Diluter-cell or test-chamber overflow.

         1)  W-l cell siphon does not break before the dilution-water valve
             opens, water will continuously siphon and the  M cell will commonly
             overflow (see Section 9 for safety  devices).  The timing needs
             adjustment.  The problem can usually be eliminated by slowing the
             flow through the valve bucket.

         2)  C-2 or other C cell siphon not functioning properly.  If the C-2
             or other C cell siphon does not  break before the  M cell empties,
             water will continuously siphon until the  M cell is empty.  The
             timing needs adjustment.  For example, the siphon tube from the
             W-l cell can be restricted to slow  the filling of the M cell.
                                     42

-------
D)  Premature siphon.

    1)  Top of W or C  siphons too low as compared to the cell dividers.

    2)  Water tubes not totally emptied by previous siphon action.  This
        difficulty should be eliminated by the 45° angle cuts at the ends
        of the water tubes.   The FS siphons may also function improperly.
                                43

-------
                                   SECTION 9

                            DILUTEE SAFETY DEVICES
     Several procedures or devices will alleviate  problems  that  occur during
diluter operation and increase the probability of  conducting successful toxicity
tests.  If no tests are expected to last more than a few days, then the
importance of these devices is reduced.

     The use of a calibrated stock-solution container and an electric counter
connected to the microswitch (see Section 6)  will  monitor the chemical-metering
apparatus with regard to diluter cycle time and toxicant introduction.

     The dipping-bird metering device can occassionally overflow into tHe M
cell if the air-pressure changes significantly in  the Mariotte bottle or if
air leaks into this bottle.  A two-chambered toxicant enclosure  (Figure 19)
can be used with a central divider over which excess toxicant can flow to a
drain tube.  This overflow commonly occurs when the Mariotte bottle is refilled
and the air pressure inside is stabilized.

     A safety device to indicate the continued operation of a proportional
diluter is very important.  This device can initiate an audible  or visual
signal, turn on aeration in the test chambers to protect against lowering
dissolved oxygen concentrations, or perform any other important  function.   We
have used the W-6 cell most frequently with a small capillary drain at the
bottom of this cell (Figure 20).  This permits the water level in W-6 to fall
below the bottom of the siphon sleeve.  Since the  flow is slow through the
capillary, several minutes or more are required for this level to drop very
far.  A float level switch (FPC level switch, Fluid Products Co., Hopkins,
Minn.  55343) located in the W-6 cell is used to activate alarms and aeration
when the water level drops significantly as the result of an elimination of
dilution-water flow to the diluter.  This capillary drains  to waste.  The
capillary tube should be checked daily and frequently cleaned as clogging can
occur.
                                      44

-------
                                        DRAIN
OVERRjOW
DIVIDER
     .TO MARIOTTE
         Figure 19. "Dipping-bird" safety device.
                      45

-------
   W
 CELLS
                  WIRES  TO
                  .ALARM SYSTEM
                  .1/2" PIPE
              ^COUPLING
                     FLOAT
                     SWITCH
U
                           W
                                 CAPILLARY   .
                                 DRIP TUBE_/
Figure 20.  Diluter malfunction safety system.
                    46

-------
                                  REFERENCES
American Public Health Association, American Water Works Association,  and Water
     Pollution Control Federation.   1971.   Standard Methods for the Examination
     of Water and Wastewater.   13th ed.  Washington, D.C.  874 p.

American Public Health Association, American Water Works Association,  and Water
     Pollution Control Federation.   1976.   Standard Methods for the Examination
     of Water and Wastewater.   14th ed.  Washington, D.C.  1193 p.

American Society for Testing and Materials.   1976.  Proposed Standard Practice
     for Conducting Acute Toxicity  Tests with Fish, Macroinvertebrates, and
     Amphibians.  Mimeo.   51 p.

Arthur, J. W., R. W. Andrew, V. R.  Mattson,  D. T.  Olson, G. E. Glass,  B. J.
     Halligan, and C. T.  Walbridge.  1975.   Comparative Toxicity of Sewage-
     Effluent Disinfection to Freshwater Aquatic Life.   U.S. Environmental
     Protection Agency, Ecol.  Res.  Ser.  EPA-600/3-75-012.  71 p.

Benoit, D. A., and F. A.  Puglisi.  1973. A Simplified  Flow-Splitting Chamber
     and Siphon for Proportional Diluters.   Water  Res.  7:1915-1916.

Brungs, W. A., and G. W.  Bailey. 1967.  Influence of Suspended Solids on the
     Acute Toxicity of Endrin to Fathead Minnows.   Proc. Purdue Industrial
     Waste Conf.  21:4-12.

Brungs, W. A., and D. I.  Mount.  1967.   A Device for Continuous Treatment of
     Fish Holding Chambers.  Trans. Am.  Fish. Soc. 96:55-57.

DeFoe, D. L.   1975.  Multichannel Toxicant  Injection System for Flow-Through
     Bioassays.  J. Fish. Res. Board Can.  32:544-546.

Doudoroff, P., G. B. Anderson, G. E. Burdick, P. S. Galtsoff, W. B. Hart, R.
     Patrick, E. R. Strong, E. W. Surber, and W. M. Van Horn.  1951.  Bioassay
     Methods  for the Evaluation of  Acute Toxicity  of Industrial Wastes to Fish.
     Sew. Ind. Wastes  23:1380-1397.

Halligan, B.  J., and J. G. Eaton.  1978. Survival and  Reproduction of Gammarus
     lacustris and J3. pseudolimnaeus Under  Two Experimental Conditions.  Prog.
     Fish-Cult.  40(2):59-62.

Hart, W. B.,  P. Doudoroff, and J. Greenbank.  1945.  The Evaluation of the
     Toxicity of Industrial Wastes, Chemicals and  Other Substances  to Fresh-
     Water Fishes.  Waste Control Laboratory, The  Atlantic Refining Co.,
     Philadelphia, Pa.  347 p.
                                     47

-------
Henderson, C.,  and C.  M.  Tarzwell.   1957.   Bioassays for Control of Industrial
     Effluents.  Sew.  Ind.  Wastes  29:1002-1017.

McAllister, W.  A., Jr., W.  L.  Mauck,  and F.  L.  Mayer,  Jr.  1972.  A Simplified
     Device for Metering  Chemicals  in Intermittent-Flow Bioassays.   Trans.
     Am.  fish.  Soc.  101:555-557.

Mount, D. I.,  and W.  A. Brungs.   1967.  A Simplified Dosing Apparatus for
     Fish Toxicology Studies.  Water Res.  1:21-29.

Mount, D. I.,  and R.  E. Warner.   1965.  A Serial-Dilution Apparatus for
     Continuous Delivery  of Various Concentrations  of Materials in Water.
     U.S. Public Health Service  Publ. 999-WP-33.  16 p.

U.S. Environmental Protection Agency.  1973.  Biological Field and Laboratory
     Methods for Measuring the Quality of Surface Waters and Effluents.  Enviror
     Monitor.  Ser. EPA-670/4-73-001.

U.S. Environmental Protection Agency.  Committee  on Methods for Toxicity Tests
     with Aquatic Organisms.  1975.  Methods for  Acute Toxicity Tests with
     Fish, Macroinvertebrates, and  Amphibians.  Ecol.  Res. Ser. EPA-660/3-75-
     009.  67  p.

U.S. Environmental Protection Agency.  Environmental Research Laboratory-Duluth.
     1971.  Recommended Procedure for Brook Trout Salvelinus fontinalis
     (Mitchill) Partial Chronic  Tests.  Mimeo.  12  p.

U.S. Environmental Protection Agency.  Environmental Research Laboratory-Duluth.
     1972a.  Recommended  Bioassay Procedure for Fathead Minnows Pimephales
     promelas  (Rafinesque)  Chronic  Tests.   Mimeo.  13 p.

U.S. Environmental Protection Agency.  Environmental Research Laboratory-Duluth
     1972b.  Recommended  Bioassay Procedures for  Jordanella floridae (Good of
     Bean) Chronic Tests.  Mimeo.  9 p.
                                     48

-------
                                 BIBLIOGRAPHY
Abram, F. S. H.  1970.  Automatic Water Mixing Device.  Lab. Pract. 19:915-916.

Abram, F. S. H.  1973.  Apparatus for Control of Poison Concentration in
     Toxicity Studies with Fish.  Water Res. 7:1875-1879.

Banner, L. H., and D. R. Nimmo.  1975.  A Salinity Controller for Flow-Through
     Bioassays.  Trans. Am. Fish. Soc. 104:388-389.

Banner, L. H., C. D. Craft, and D. R. Nimmo.  1975.  A Saltwater Flow-Through
     Bioassay Method with Controlled Temperature and Salinity.  Prog. Fish-Cult.
     37:126-129.

Ballard, J. A., and W. D. Oliff.  1969.  A Rapid Method for Measuring the
     Acute Toxicity of Dissolved Materials to Marine Fishes.  Water Res.
     3:313-333.

Bengtsson, B. E.  1972.  A Simple Principle for Dosing Apparatus in Aquatic
     Systems.  Arch. Hydrobiol. 70:43-45.

Benville, P. E., Jr., and S. Korn.  1973.  A Simple Apparatus for Metering
     Volatile Liquids into Water.  J. Fish. Res. Board Can.  31:367-368.

Betts, J. L., T. W. Beak, and G. G. Wilson.  1967.  A Procedure for Small-
     Scale Laboratory Bioassays.  J. Water Poll. Cont. Fed. 39:89-96.

Borthwick, P. W., M. E. Tagatz, and J. Forester.  1975.  A Gravity-Flow
     Column to Provide Pesticide-Laden Water for Aquatic Bioassays.  Bull.
     Environ. Contain. Toxicol.   13:183-187.

Brenniman, G., R. Hartung, and  W. J. Weber, Jr.   1976.  A Continuous Flow
     Bioassay Method to Evaluate the Effects of Outboard Motor Exhausts and
     Selected Aromatic Toxicants on Fish.  Water Res. 10:165-169.

Brown, V. M.  1973.  Concepts and Outlook in Testing and Toxicity of
     Substances to Fish, p. 73-95.  _In  Bioassay Techniques and Environmental
     Chemistry.  Ann Arbor Science Publishers,  Inc., Ann Arbor, Mich.

Brown, V. M.  1976.  Advances in Testing the Toxicity of Substances to Fish.
     Chem. Ind.    .-143-149.

Brungs, W. A.  1973.  Continuous-Flow Bioassays with Aquatic Organisms:
     Procedures and Applications.  Biological Methods for the Assessment of
     Water Quality.  American Society for Testing and Materials, STP 528.
     p. 117-126.

                                     49

-------
Brungs, W. A.,  and D.  I.  Mount.   1970.   A Water Delivery System for Small
     Fish-Holding Tanks.   Trans.  Am.  Fish.  Soc.  99:799-802.

Buikema, A. L., Jr.,  D. R. Lee,  and J.  Cairns,  Jr.   1976.   A Screening
     Bioassay Using Daphnia pulex for Refinery  Wastes  Discharged into
     Freshwater.  J.  Test. Eval.   4:119-125.

Burke, W. D., and D.  E. Ferguson.- 1968.   A Simplified Flow-Through
     Apparatus for Maintaining Fixed Concentrations  of Toxicants in Water.
     Trans. Am. Fish.  Soc. 97:498-501.

Burress, R. M.   1975.   Development and Evaluation of On-site Toxicity Test
     Procedures for Fishery Investigations.  U.S.  Fish and Wildlife Service,
     Investigations in Fish Control 63.   8 p.

Cairns, J., Jr.  1969. Fish Bioassays - Reproducability and Rating.  Revist.
     Biol.  7:7-12.

Cairns, J., Jr., K. L. Dickson,  and G.  Lanza.   1973.  Rapid Biological
     Monitoring System for Determining, Aquatic  Community Structure in
     Receiving Systems.   Biological Methods for the  Assessment of Water
     Quality.  American Society for Testing and Materials, STP 528.  p. 148-163.

Cairns, J., Jr., J. W. Hall, E.  L. Morgan,  R. E. Sparks, W.  T. Waller, and
     G. F. Westlake.   1973.  The Development of an Automated Biological
     Monitoring System for Water Quality.  Virginia  Water Resour. Res. Center
     Bull. 59.   50 p.

Cairns, J., Jr., R. E. Sparks, and W. T.  Waller.  1973.   The Design of a
     Continuous Flow Biological Early Warning System for Industrial Use. Proc.
     Purdue Industrial Waste Conf.  27(1972): 34 p.

Chandler, J. H., Jr.,  and S. K.  Partridge.   1975.  A Solenoid-Actuated
     Chemical-Metering Apparatus for Use in Flow-Through Toxicity Tests.
     Prog. Fish-Cult.  37:93-95.

Chandler, J. H., Jr.,  H.  0. Sanders, and D. F.  Walsh.   1974.  An Improved
     Chemical Delivery Apparatus for Use in Intermittent-Flow Bioassays.
     Bull. Environ. Contain. Toxicol.  12:123-128.

Cherry, D. S.,  K. L.  Dickson, and J. Cairns,  Jr.  1975.   The Use of a Mobile
     Laboratory to Study  Temperature Response of Fish.  Proc.  Purdue Industrial
     Waste Conf. 29(1974): 28 p.

Cline, T. F., and G.  Post.  1972.  Therapy for  Trout Eggs Infected with
     Saprolegnia.  Prog.  Fish-Cult. 34:148-151.

Davis, J. C., and B.  J. Mason.  1973.  Bioassay Procedures to Evaluate Acute
     Toxicity of Neutralized Bleached Kraft Pulp Mill  Effluent to Pacific
     Salmon.  J. Fish. Res. Board Can.   30:1565-1573.
                                     50

-------
Drummond, R. A., and W. F. Dawson.  1970.  An Inexpensive Method for
     Simulating Diel Patterns of Lighting in the Laboratory.  Trans.
     Am. Fish. Soc. 99:434-435.

Eaton, J. G.  1973.  Recent Development in the Use of Laboratory Bioassays
     to Determine "Safe" Levels of Toxicants for Fish, p. 107-115.   _In
     Bioassay Techniques and Environmental Chemistry.  Ann Arbor Science
     Publishers, Inc., Ann Arbor, Mich.

Esvelt, L. A., and J. D. Conners.  1971.  Continuous-Flow Fish Bioassay
     Apparatus for Municipal and Industrial Effluents, p. 159-224.   _In_
     Toxicity Removal from Municipal Wastewaters.  Sanitary Engineering
     Research Laboratory, Univ. California.  SERL Report No. 71-7,  Vol. IV.

European Inland Fisheries Advisory Commission.  1975.  Report on Fish Toxicity
     Testing Procedures.  Food and Agriculture Organization of the  United
     Nations, Rome.  Tech. Pap. 24.  25 p.

Falk, M. R.  1973.  Simple Apparatus for Conducting Acute Toxicity  Bioassays
     Under Field Conditions.  Water Res. 7:821-822.

Freeman, R. A.  1971.  A Constant Flow Delivery Device for Chronic  Bioassay.
     Trans. Am. Fish. Soc. 100:135-136.

Granmo, A., and S. 0. Kollberg.  1972.  A New Simple Water Flow System for
     Accurate Continuous Flow Tests.  Water Res. 6:1597-1599.

Gregg, B. C., and A. G. Heath.  1975.  A Method for Intermittent Chlorine
     Dosing in Continuous-Flow Toxicity Tests.  Bull. Environ.  Contain.
     Toxicol. 13:588-592.

Grenier, F.  1960.  A Constant Flow Apparatus for Toxicity Experiments  on
     Fish.  J. Water Poll. Control Fed. 32:1117-1119.

Henderson, C.  1957.  Application Factors to be Applied to Bioassays for the
     Safe Disposal of Toxic Wastes.  Biology of Water Pollution. Seminar
     on Biological Programs in Water Pollution, Cincinnati,  Ohio (1956).
     p. 31-37.

Henderson, C., and Q. H. Pickering.  1963.  Use of Fish in the  Detection of
     Contaminants in Water Supplies.  J. Am. Water Works Assoc.  55:715-720.

Herbert, D. W. M.  1952.  Measurement of the Toxicity of Substances to
     Fish.  Inst. Sewage Purification J. and Proc.  Part I.  p.  60-66.

Hublou, W. F.  1959.  A Plexiglas Constant-Flow Siphon.  Prog.  Fish-Cult.
     21:47-48.

Hughes, J. R., T. H. Blahm, and D. R. Craddock.  1976.   A Mobile Laboratory
     with Flow-Through Capability for Thermal Tolerance Studies  of  Aquatic
     Organisms.  Marine Fish.  Rev. 38:24-27.
                                     51

-------
Jackson, H. W.,  and W.  A.  Brungs.   1967.   Biomonitoring of  Industrial
     Effluents.   Proc.  Purdue Industrial Waste  Conf.  21(1966):117-124.

Lake, W., and J. S. Loch.   A Mobile Field  Laboratory  for Aquatic  Toxicity
     Studies.  Environ. Canada Resour.  Manage.,  Tech. Rep.  Ser. CEN/T-73-13.
     52 p.

LaRoche, G., R.  Eisler, and C. M.  Tarzwell.   1970.  Bioassay Procedures for
     Oil and Oil Dispersant Toxicity Evaluation. J.  Water  Poll.  Control
     Fed. 42:1982-1989.

Lemke, A. E.  1964.  A New Design  for Constant-Flow Test Chambers.   Prog.
     Fish-Cult.  26:136-138.

Lemke, A. E.  1969.  A Water Hardener for  Experimental Use. J. Am.  Water
     Works Assoc.  61:415-416.

Lennon, R. E., and C. R. Walker.   1964. 1.  Laboratories and Methods for
     Screening Fish-Control Chemicals.  U.S. Fish and Wildlife  Service,
     Investigation in Fish Control 1.  p.  1-15.

Lichatowich, J.  A., P.  W.  O'Keefe, J. A. Strand, and  W. L.  Templeton.   1973.
     Development of Methodology and Apparatus for the Bioassay  of Oil,
     p. 659-666.  In  Proc. of Joint Conference on  Prevention and Control of
     Oil Spills.  American Petroleum Institute,  Environmental Protection
     Agency, and U.S. Coast Guard, Washington,  D.C.

Little, L. W.  1976.  Bioassays-Procedures and  Results.  J. Water Poll.
     Control Fed. 48:1356-1367.

Lowe, J. I.  1964.  Chronic Exposure of Spot, Leiostomus xanthurus,  to
     Sublethal Concentrations of Toxaphene in Seawater.  Trans. Am.  Fish.
     Soc. 93:396-399.

Maciorowski, A.  F.  1975.   An Inexpensive  Macroinvertebrate Bioassay Table
     for Use in Continuous-Flow Toxicity Tests.   Bull. Environ. Contam.
     Toxicol. 13:420-423.

Marking, L. L.  1969.  Toxicological Assays with Fish.  Bull. Wildlife
     Disease Assoc. 5:291-294.

Myers, R. L. -1977.  Modifications of the  SERL  Proporitional Diluter.   J.
     Water Pollut. Control Fed. 49:859-861.

Ohio River Valley Water Sanitation Commission (ORSANCO).  1974.   ORSANCO
     24-hr Bioassay.  Cincinnati,  Ohio. 21 p.

Poels, C. L. M.   1975.   Continuous Automatic Monitoring of  Surface Water
     with Fish.   Water Treat. Exam. 29:46-56.

Riley, C. W.  1975.  Proportional  Diluter  for Effluent Bioassays. J.
     Water Pollut. Control Fed. 47:2620-2626.

                                     52

-------
Roberts, R. F.,  and H. E.  Allen.  1972.  The Control of pH and Total
     Alkalinity or Total Carbonate in Aquatic Bioassays.   Trans.  Am. Fish.
     Soc. 101:752-756.

Scheier, A., and D. T. Burton.   1973.  A Description of Bioassay  Flow-
     Through Techniques, and the Use of Bioassay to Measure the Effects
     of Low Oxygen at the Whole-Animal and the Molecular Level, p.  335-344.
     In  Bioassay Techniques and Environmental Chemistry.   Ann Arbor Science
     Publishers, Inc., Ann Arbor, Mich.
                                                                         Ti
Schimmel, S. C., D. J. Hansen,  and J. Forester.  1974.   Effects of  Aroclor
     1254 on Laboratory-Reared  Embryos and Fry of Sheepshead Minnows
     (Cyprinodon varie^atus).   Trans. Am.  Fish. Soc.  103:582-586.

Shumway, D. L.,  and J. R.  Palensky.   1973.  Impairment  of  the Flavor of
     Fish by Water Pollutants.   U.S. Environmental Protection Agency,  Ecol.
     Res. Ser. EPA-R3-73-010.   80 p.

Smith,  A. D., J. R. Butter, and G. W. Ozburn.  1977.  A Pneumatic Dosing
     Apparatus for Flow-Through Bioassays.  Water Res.   11:347-349.

Solon,  J. M., J. L. Lincer, and J. H. Nair,  III.   1968. A Continuous  Flow,
     Automatic Device for Short-Term Toxicity Experiments.  Trans.  Am.  Fish.
     Soc. 97:501-502.

Sprague, J. B.  1969.  Measurement of Pollutant Toxicity  to Fish.   I.   Bioassay
     Methods for Acute Toxicity.  Water Res.  3:793-821.

Sprague, J. B.  1970.  Measurement of Pollutant Toxicity to Fish.   II.
     Utilizing and Applying Bioassay Results.  Water  Res.  4:3-32.

Sprague, J. B.  1971.  Measurement of Pollutant Toxicity to Fish.   III.
     Sublethal Effects and "Safe" Concentrations.   Water Res.  5:245-266.

Sprague, J. B.  1973.  The ABC's of  Pollutant Bioassay  Using Fish.   Biological
     Methods for the Assessment of Water Quality,  American Society  for
     Testing and Materials, STP 528.  p. 6-30.

Stark,  G. T. C.   1967.  An Automatic Dosing  Apparatus Made with Standard
     Laboratory  Ware.  Lab. Pract. 16:594-595.

Stephan, C. E.  1973.  Chemistry and Fish  Toxicology, p. 97-105.  _In Bioassay
     Techniques  and Environmental Chemistry.   Ann  Arbor Science Publishers,
     Inc.,  Ann Arbor, Mich.

Stephan, C. E.,  and D. I.  Mount.  1973.  Use of Toxicity Tests with Fish
     in Water Pollution Control, p.  164-177.  ^n_  Biological Methods for  the
     Assessment  of Water Quality.  American  Society for Testing and Materials,
     STP 528.

Syrett, R.  F., and W. F. Dawson.  1972.  An  Inexpensive Electronic  Relay
     for Precise Water-Temperature Control.   Prog.  Fish-Cult.   34:241-242.


                                     53

-------
Syrett, R.  F.,  and W.  F.  Dawson.   1975.   An  Inexpensive  Solid-State  Temperature
     Controller.   Prog.  Fish-Cult.  37:171-172.

U.S. Environmental Protection Agency.   1976.  Bioassay Procedures  for the
     Ocean  Disposal Permit Program.   Environmental  Research  Laboratory,  Gulf
     Breeze,  Florida.   EPA-600/9-76-010.   106 p.

Vanderhorst,  J. R., C.  I.  Gibson,  L.  J. Moore,  and  P. Wilkinson. *1977.
     Continuous-Flow Apparatus for Use in Petroleum Bioassay.   Bull.  Environ.
     Contam.  Toxicol.  17:577-584.

Veith, G. D. ,  and V. M.  Comstock.   1975.   Apparatus for  Continuously Saturating
     Water with Hydrophobia Organic Chemicals.  J.  Fish.  Res.  Board  Can.  32:
     1849-1851.

Walden, C., D.  McLeay,  and D. Monteith.   1975.  Comparing Bioassay
     Procedures for Pulp and Paper Effluents.   Pulp Pap.  Mag.  Can. 76:68-72.

Warner, R.  E.   1967.  Bio-assays  for Microchemical  Environmental Contaminants.
     Bull.  World Health Organ. 36:181-207.

Weiss, C. M.   1955. A Constant Temperature  Tank  for Fish Bioassay Aquaria.
     Sew. Ind.  Wastes  27:1399-1401.

Westlake, G.  F.,  W. H.  van der Schalie, J. Cairns,  Jr.,  and  K. L.  Dickson.
     1976.   The Use of Fish to Continuously  Monitor an Industrial  Effluent.
     The Institute of  Electrical  and Electronics  Engineers,  Inc.   Annals
     No. 75 CH 1004-1  18-4.  3 p.

Wuerthele,  M.,  J. Zillich, M. Newton, and C.  Fetterolf.   1973. Descriptions
     of a Continuous-Flow Bioassay Laboratory Trailer and the  Michigan
     Diluter,  p.  345-354.  Iji  Bioassay Techniques  and Environmental Chemistry.
     Ann Arbor Science Publishers, Inc.,  Ann Arbor, Mich.
                                    54

-------
                                APPENDIX A


Hater Research, Pergamon Press 1967. Vol. 1, pp. 21-29. Printed in Great Bntain.


       A SIMPLIFIED  DOSING  APPARATUS  FOR FISH
                       TOXICOLOGY STUDIES
                  DONALD I. MOUNT* and WILLIAM A. BRUNGS*

     Aquatic Biology Activities, Basic and Applied Sciences Program, Cincinnati Water
           Research Laboratory, Federal Water Pollution Control Administration,
                           U.S. Department of the Interior
                            (Received 12 Septemher 1966)

   Abstract—A simplified diluter for maintaining a scries of constant concentrations of a material
   in flowing water is described. It depends on water flows, metering cells, and venturi tubes to
   proportion volumes of water and toxicant to  give  desired concentrations. Construction
   requires less than 2 days, and only readily available materials are needed. An injector for mixing
   pesticides in water is also described.

                               INTRODUCTION
MOUNT and WARNER (1965)  have described  a  serial dilution  apparatus suitable for
maintenance  of constant concentrations of  materials in  flowing water.  They have
discussed the need for reliable systems  that cannot deliver an excessively high con-
centration of toxicant in long-term fish toxicity studies. At the Newtown Laboratory
of the  Cincinnati  Water  Research  Laboratory,  Federal  Water Pollution Control
Administration, Cincinnati, Ohio, we have used this system for several years in fish
toxicology studies and have been well satisfied with its performance. Because of a need
for more narrow concentration series, such as 1, 0.8.0.64, 0.51, etc., we have modified
the serial diluter in order to make it more suitable for such uses. We have  also found
that some of those who have constructed serial diluters have had problems before they
were able to achieve satisfactory operation. Apparently selection  of tubing sizes was
troublesome. Some of the components and principles herein  described, particularly
the water delivery  system, can be used advantageously on the serial diluter and  are
discussed later.
  The modified diluter, called a proportional diluter, is not based on serial dilution
but rather on simultaneous  dilution of one  concentration. It  has these advantages
over the serial diluter: (1) water is delivered to each chamber each half cycle so that the
(low rate can be twice as great; (2) timing problems are minimal; (3) operation is much
simpler and easier to understand; (4) malfunctions are less frequent than in the serial
diluter  system;  (5) it can deliver a  series of concentrations,  each concentration as
much as 90 per cent of each preceding concentration; and (6) much less vertical space
IN needed. The main disadvantage is that it is impractical to deliver a series of con-
vcntrations with a dilution factor greater than  50 per cent between each concentration;
c u. a concentration series such as 1, O.I, 0.01, etc.
  The proportional diluter shown in  FIG. 1 and described in this paper is one that can
deliver  5 toxicant concentrations and a  control at any desired flow rate per concen-
tration  up to 400 ml/min, and with a dilution factor  from 50 to 25 per cent between
  * Respectively Fisheries Research Biologist and Aquatic Biologist.
                                     55

-------
22                    DONALD I. MOUNT and WILLIAM A. BRUNOS
successive concentrations. Metering and chemical cells can be exchanged so that the
dilution interval between successive concentrations can be decreased down to 10 per
cent, that is, a concentration sequence such as 1, 0.9, 0.81, 0.73, etc. Because persons
have requested additional details of the serial diluter, more specifications are given in
this paper.  Throughout the following  description,  a delivery vol. of 500 ml per
concentration is assumed with a maximum flow of 400 ml/min per concentration.

                                 MATERIALS
  As  before (MOUNT  and WARNER, 1965),  every effort has been made  to utilize
materials readily available. Four sheets  of 12 x 24-in. single-strength window glass,
appropriate glass tubing, glass glue, a hand glass cutter, rubber  stoppers, a 1-in.
plastic hose "T", plastic bottles, and optionally a mechanical counter, constitute the
materials needed. If one wishes, local glass stores will cut the glass to desired sizes,
and for a very modest price they will cut the necessary three holes. The availability
of an excellent silicone rubber glass glue (Clear Seal produced by General Electric
or Glass and Ceramic  glue produced by Dow-Corning*) has made the construction
of the chambers extremely simple. Clean glass can be glued without etching or scratch-
ing, and the pieces can be assembled by  simply pressing the pre-glued edges together.
TABLE 1 lists the recommended cell sizes for the diluter described in this paper.

                 TABLE 1. DIMENSIONS AND CAPACITIES OF METERING CELLS
Cell No.
W-l
W-2
. W-3
W-4
W-5
W-6
M-l
C-2
C-3
C-4
C-5
C-l
Size
(cm)
H W L
12x6x23
12x6x4
12x6x6
12x6x7
12x6x7
12x6xg
lOx 11 x ]6
12x3x U
12x3x9
12x3x7
12x3x5
12x3x6
Maximum
capacity
(ml)
1656
288
432
504
j04
576
1760
3%
324
252
180
216
               Height does not include 3 cm of freeboard for sides and ends.


                        PRINCIPLES OF OPERATION
  A series of water-metering cells are filled, the  water is turned off, the cells are
emptied, and the water flow is restored. (The reader is referred to FIG. 2 for a better
understanding of the following.) Cell W-l fills first from IT then overflows into W-2,
etc. When cells W-2 to  5 are emptied, appropriate quantities of a higher concentration
  * Mention of commercial products does not constitute endorsement by Federal Water Pollution
Control Administration.
                                   56

-------
FIG. I. Photograph of a proportional diluter built as suggested in this paper.
                                     57

-------
               A Simplified Dosing Apparatus for Fish Toxicology Studies
23
(concentration 1) from cells C-2 to 5 are mixed with the diluent water to give the
desired lower concentrations. While the water from cells W-2 to 5 is being emptied
through tubes WS-2 to 5 and WS-2A to 5A, the water from W-l  is emptied through
WS-1 into mixing chamber M-l where the toxicant is added, and then the chemical
cells C-2 to 5 are filled from cell M-l through tube S-7. Cell C-2  fills first then over-
flows into cell C-3, etc. The vol. of W-l is  adjusted so that after cells  C-2 through
C-5 are filled, 500 ml flows into C-l and then to the test chamber to furnish test water
for the high concentration. Water for a control test chamber is emptied from W-6 and
operates the water valve (NV1)  to turn off the influent water from tube IT while
cells W-l to 5 empty. It also flows through the vacuum venturi, (VaV) to produce a
partial vacuum in the vacuum manifold (VaMa), which is connected to each water
venturi (WV-1 to 5) by the tubes Va-1 to 5.  The partial vacuum applied  by the water
venturi  causes water from the water cells  to  rise through the water siphon tubes
(WS-1 to 5) and start the siphoning action to empty the water cells. The  water blocks
(WB-1 to 5) serve to prevent air from entering the system through water  siphon tubes
WS-1 A to 5A. The distance from the water level of each filled water-metering cell to
the top of its water siphon tube, distance "A" (Fio. 2A), must be less than the distance
from the water  level in its respective water block to the bottom of the "U" in its
water venturi, distance "A"'. Otherwise the water siphons  will not  start but rather
                          -as
                                                  ,     .
                                    ~   ,rtr  *   t ^!
                                        1'J   ir-r * V-*-»  TT~ «  Y/«* »       .!




7
\ ""
L




r »~Y -^Tf '
*S !* *S i» ' •' «*



i

1
-.. z [I
C !


!'
!
i
I
[
t



F^W..
r:.^
ii
ill
i





-
|ui - • 'i


i
i
       cuoss SCCTION «r CCLL w« a C4
                                                   r*onT VIEW
                                                   Figure Z-a
                     FIG. 2. Semi-schematic scale drawing of diluter.
    Legend: B—block; Bu—bucket; By—by pass spout; C—chemical: I—influent; M—mixing;
    Ma—manifold; N—needle; S—siphon;  T—tube; V—venturi;  Va—vacuum;  VI—valve;
                                   W—water.
                                        58

-------
24                   DONALD I. MOUNT and WILLIAM A. BRUNGS
water will enter the vacuum tubes Va-1 to 5. As the water passes the chemical venturi
tubes, CV-2 to 5, the chemical siphons, CS-2 to 5, are started and chemical cells C-2
to 5 are emptied.
  Only  two timing adjustments must be  checked: (1) the 'vater flow through the
vacuum venturi (VaV) must be fast enough to produce sufficient vacuum to start the
water siphons but  slow enough so that the water valve remains closed sufficiently
long to  allow water siphon WS-1 to empty cell W-l before the influent water again
enters W-l  from tube IT; and (2) cells W-2 and C-2 must be emptied and the siphon
in tube T-2 broken  before water from mixing  cell M-l enters cell C-2 through tube
S-7. Obviously, the siphon in T-3, T-4, and T-5 must also be broken before their
respective cells fill. This latter problem should not occur if the tube sizes suggested in

                          TABLE 2. TUBE USED ON DILUTER
Tube No.
WS-1
WS-2 to 5
WV-2 to 5
WS-2A to 5A
WS-1 A
WS-6
S-7
CS-2 to 5
CV-2 to 5
T-l to 5
VaV
T-6
Va-1 to 5
VaMa
VIBuT
IT
NV1
VIBuS
o.d.
(mm)
15
8
8
8
15
8
10
10
10
10
5
8
5
5
7
10
25 (1 in.)
6
Material
Glass
Glass
Glass
Glass
Glass
Glass
Glass
Glass
Glass
Glass
Glass
Glass
Plastic
Plastic
Rubber
Glass
Plastic hose "T"
Glass
TABLE 2 are used. If water enters C-2 too soon, the flow rate through tube WS-1 A
can be slowed by restricting  the opening. The siphon WS-6 is adjusted in height so
that the total vol. delivered from cell W-6 is 500 ml. The valve bucket (VIBu) should
have a capacity of approximately  500 ml and is best made from a polyethylene bottle.
The tube WS-6 must fill the valve bucket at a rate so that the valve closes quickly,
giving ample time for the water level in the water cells to drain down to the top of the
cell partitions.  This drainage must be completed before  the  water  begins flowing
through the valve venturi. The time required for drainage is reduced by sloping the
cells approximately 1 cm in 10 cm. The chemical cells should be sloped as well. This
can be accomplished by sloping the back board of the diluter or by sloping the two
shelves on the board as shown in FIG. 1.

                               CALIBRATION
   The vol. delivered from water cell W-l can best be measured by catching the delivery
from tube WS-1A. The delivery vol. from cells W-2 to 5 can be measured by opening
                                    59

-------
               A Simplified Dosing Apparatus for Fish Toxicology Studies              25

the bypass (By) on the water blocks WB-2 to 5 (shown only on FIG.  1 and 2A) and
catching the flow. The bypass must be sufficiently large and positioned so that no
water goes down WS-2A to 5A. These vols. should be checked while the diluter is
cycling normally  in  the  event  that the drain-down is not entirely  complete.  The
delivery vol. of cells C-2 through C-5 are determined as follows. The influent water to
the diluter is stopped just as the water cells begin to empty. After the "C"  cells have
been filled and the overflow into cell C-l  has stopped, 5-10 ml of water should be
added to cells W-2 through W-5 to prevent air from entering WS-1 to 5. Suction should
then be applied to tube T-2 with a suction bulb and the water delivered caught in a
graduated cylinder. This procedure should be repeated for cells C-3 to 5 and then the
water flow restored.
  The volumes in W-l through W-5 and C-2 through C-5 cells are adjusted  as needed
by increasing or decreasing the depth to which the siphon tubes extend into the cell.
The WS-1 to 5 tubes  and CS-2 to 5 tubes should be glued to the outside of the water
and chemical cells so they are rigid, but they should be cut off approximately at the top
level of the cell partition and then an adjustable extension added to furnish the desired
length. This arrangement allows for maximum adjustment of vol. The cell ends of the
WS-1 to 5 and CS-2  to 5 tubes  should be exactly parallel to the water surface in the
cell so that the siphon breaks abruptly. Placing a funnel-shaped flare on the end of
the tube enhances abrupt breaking.
             TABLE 3. REQUIRED WORKING VOLUMES OF EACH CELL FOR DILUTION
                FACTORS OF 50 AND 25 PER CENT BETWEEN CONCENTRATIONS


Cell No.
W-l
W-2
W-3
W-4
W-5
W-6
M-l
C-2
C-3
C-4
; C-5
C-l
Vol.
(ml)
50 % Factor
968
250
375
438
469
500
968
250
125
62
31
500


25 "/Factor
1525
125
219
289
342
500
1525
375
281
211
158
500
  TABLE 3 lists the requisite working volumes for 50 per cent and 25 per cent dilution
factors between concentrations. These two series of concentration intervals represent
the recommended extremes for this particular diluter. One should construct water
and chemical cells of different dimensions for better accuracy for greater or smaller
dilution factors.
                                       60

-------
26                    DONALD I. MOUNT and WILLIAM A. BKUNOS
                  DETAIL FOR SPECIFIC  COMPONENTS
(A) Needle valve
  FIGURE 3, from MOUNT and WARNER (1965), is reproduced here for convenience in
constructing the needle valve. For the diluter described in this paper, an inlet and outlet
rubber tube of J-in. i.d. is suggested and a  needle made of 13-mm glass tubing. The
glass rod should be approximately 5 mm in dia. The taper below the vacuum venturi
should be from  5-8 mm in a distance of 1.5-2.5 cm.  A string,  pulley, and bucket
filled with sand makes a fine counterbalance weight to  replace the valve spring.
                    WATER PROM
                    CtLL r» 6
                                                          OUTLET TO
                                                        WATER MANtfOLO
                    FIG. 3. Needle valve and vacuum venturi detail.
(B) Vacuum connexion for WS-\  tube
  Since "U" shaped connecting tubes are not easily obtainable in 15 mm o.d., the
vacuum line Va-1 is best connected to the WS-1 tube by blowing or grinding a small
hole in the side of the tube and gluing over the hole a short piece of 3 mm o.d. glass
tubing. Care must be taken to keep the A and A' distances in the proper relationship
as discussed earlier.

(Q Chemical-metering apparatus
  Many types  of metering apparatus can be used to introduce the toxicant; the
specific choice depends on the chemical characteristics of the toxicant. Pumps can be
used satisfactorily for short-duration tests in which no great damage will occur if the
water flow fails or slows drastically. (The pump would continue to introduce to~:~
                                      61

-------
                A Simplified Dosing Apparatus for Fish Toxicology Studies
27
and kill the animals.) For longer tests, a safer device is needed. FIGURE 4 (taken from
MOUNT and WARNER, 1965) illustrates the method of choice for highly water-soluble
materials. By this method, the water solution is kept at a constant level in the funnel
by a Mariotte bottle. (The  bottle must be  insulated against rapid air  temperature
fluctuations or the funnel may overflow.)
                     FIG. 4. Detail of chemical-metering apparatus.


  When water enters the plastic bucket of the chemical-metering apparatus from cell
W-l (labelled funnel No. 1 on drawing), the tube rotates and the toxicant solution runs
through the tube and into the mixing chamber (M-l) beneath. The tube is made by
heating and drawing an appropriate sized piece of glass tubing and then bending it to
the necessary angle. By experience, we have found that partially closing the funnel
end of the tube (by firepolishing) and cutting a hole in the top for filling and releasing
air gives slightly better accuracy. (Note: The Mariotte bottle is not drawn to scale.)
   Foi organics that are slightly soluble in water, we have used an injector as sketched
in FIG.  5. It is simply a lever arm actuated by the water filling the plastic bucket and
causing the arm to rotate. On the end opposite the bucket, a small pawl advances a
gear, 1, 2, or 3 teeth; the gear wheel turns the nut a few degrees, advancing the bolt
and piston a very short distance and displacing a few /il of solution through the needle
into the water from cell W-l. We have used a gear with 42 teeth and a bolt  with 40
threads/in, so that by advancing the gear, one tooth at a time, there are 1680 injections/
m. of piston travel. With a 1-ml syringe, this gives approximately 0.25 ^I/injection;
this can be increased up to 30 ^1 if a 50-ml  syringe is used and the gear is advanced
three teeth. Thus, one full syringe lasts for 3-10 days, depending on the cycle time of
the diluter. Although the injector may seem difficult to construct, if one has a suitable
gear and the bolt, the rest can be made from  glass tubing, rubber stoppers and burette
clamps.
  Acetone  solutions of organics can be used in the syringe as a stock  solution, or if
the toxicant is a liquid and is water miscible, it can be used without further dilution.
                                      62

-------
28
DONALD I. MOUNT and WILLIAM A. BRUNGS
                   ,»»«L    ..PIVOT
                 i 4    COUCCNTHiC
U                       «.«$'« ".SING
                       CXL«5
                                   TOP VIEW
                                                                0" CELL W-l
                Fio. 5. Injector system for adding //I quantities to the water.
For such toxicants as pesticides we have  found the following procedure to be the
only way in which we can measure as much pesticide in the water as is introduced.
  First the injector is used to inject air into a small closed vessel such as  a 60 ml
stoppered bottle. The air then forces  the  slurry through a capillary tube from the
bottle  into the water in chamber M-l.  (The syringe and bottle must be insulated
against sudden  temperature changes.) The  bottle is placed on  a magnetic stirrer
located slightly below the M-l cell, and  the slurry is stirred continuously.
  The slurry is made as follows: (1) 25 mg of Triton X-100 is dissolved in 15-25 ml
of water; (2) 1-2 ml of acetone containing the requisite amount of pesticide is then
added,  or if the pesticide is  a liquid, it is added directly without  being dissolved
first in acetone; (3)  the mixture is shaken vigorously and then made up to 50 ml
for use. Depending  on  the  amount of  pesticide  present, the slurry is  usually
white.
  We have successfully maintained as much as 10 g of parathion in suspension in 50
ml of slurry in this way without exceeding 10.0 ppb of Triton in the test water,  and
no acetone was present. The  decided advantage of this slurry is  that it is a micro-
suspension that disperses readily in the water and then goes into true solution,  whereas
when pesticides are  dissolved in acetone  and introduced directly into water,  they
usually precipitate and only violent agitation will disperse them in the  water. Ludzack
(personal communication) stated that in  tests he performed there  was a  marked
tendency for aldrin and dieldrin to appear in the surface film or above the water surface
on the sides of the container, when they were dissolved in organic solvents before they
were introduced into water.
                                     63

-------
                A Simplified Dosing Apparatus for Fish Toxicology Studies              29
(D) Modifications of the serial diluter
  The type of water-metering cell described in this paper is superior to that described
by MOUNT and WARNER (1965). The main advantage is that the problem of pushing
water over the water siphon tubes does not exist because the system is an open one
and no  pressure can develop. In addition, volume adjustments can be made  more
readily,  either by moving the tubes or using volume dispiacers.
  Only  one minor change need  be made to adapt the open cell system to the  serial
diluter.  The water siphon tubes WS-1  to  5 must be set so that the siphons start in
proper order. This is achieved by setting WS-1 and WS-5 as close to the cell edge as
possible (as shown in FIG. 2B) and then raising WS-4 approximately 5 mm, WS-3,
10 mm,  and WS-2, 15 mm above the cell edge. Funnels may be used for water blocks
as previously described or plastic bottles may be used as shown in FIG. 1. It is neces-
sary, as  for the proportional diluter, to slope the cell unit so that when the influent
water is shut off by the valve, the water will  drain down  quickly to the level of the
partition tops.

                                  SUMMARY
  The diluter herein described has been found by testing to be as dependable  as or
more  dependable than the serial diluter described by MOUNT and WARNER  (1965).
It operates simply and is much easier to understand and construct. The diluter shown
in FIG.  1 was built in approximately 13 hr. For very wide concentration ranges with
very large dilution factors between each concentration, the serial diluter (MOUNT and
WARNER,  1965)  is best, but for dilution factors, 50 per  cent and  smaller, the one
described  here is superior.

                                 REFERENCE
MOUNT D. I. and WARNER R. E. (1965) A Serial-dilution Apparatus for Continuous Delivery of Variou
    Concentrations of Materials in Water. U.S. Public Health Service Publ. No. 999-WP-23,  16 p-
                                       64

-------
                                            APPENDIX  B
        Multichannel Toxicant Injection System for Flow-Through Bioassays

                                          DAVID L. DEFOE

      U.S. En\ironmental Protection Agency, National Water Qualm Laboratory Dultith. Minn  .5.5
-------
                                              NOTES
                                                                                               545
tions can be changed independently of each other
and to any  proportion with only  minor  adjust-
ments.
   2) The device  can be used in bioassays where
measurement of toxicant in solution, such as  a
polyelectrolyte,  is impractical  or  difficult.  The
toxicant concentrations  of the  test water can be
precisely  calculated from the amount of toxicant
injected and the volume of water used.
   3) The system  operates mechanically by using
the  force of falling water; the  operation of each
injector unit ceases to operate  if the water flow
stops. This reduces the possibility of toxicant over-
dosing or flushing of individual concentrations in
the event of  a support-system failure.
   4) The commercial availability of the injection
units minimizes the amount  of  construction done
by the researcher,  and the durability and simplicity
reduce  the maintenance demand.
   During  the  30-mo evaluation of the injector
system, the coefficient of variation (C.V.) of dis-
pensing  water  soluable  toxicants  into bioassay
systems  ranged from  8 to  12%.  The  injected
volume of polyelectrolytes measured over a  month
period  showed  a  C.V.  of 8%. The  C.V. for  a
4-mo cadmium  zinc  mixture study ranged from
10 to \2cfc. Concentrations ranged from 4.8 to  8.0
and  25-140 ^a/liter,  respectively, for the  two
metals.  These C.V.s  represent injector error and
analytical error.
   For insoluble compounds, such  as  PCBs  and
methoxychlor. the C.V.  increased. A 14-mo PCB
exposure  with  concentrations ranging from  0.1
to  10  fiz/ liter,  resulted  in  C.V.  of 24-42%.
Methoxychlor measurements after a month  period
showed  a C.V  of 20%. These  C.V.s include
dissolution, sorption,  and analytical  error in addi-
tion to  injector error.

   Operation — The delivery system is diagrammed
in  Fig.  1A.  Incoming water  controlled  by  a
solenoid enters  water-metering  cell 0. Consecu-
tively, each cell fills  and overflows, and fills  the
subsequent cell. The last cell, 7, has a self-starting
standpipe siphon described by Benoit  and Puglisi
(1973).  This siphon delivers water from  cell  7
to a bucket suspended  over  a microswitch  which
shuts off  the incoming  water. From  this  bucket
the water siphons  off and flows through a U-tube
creating the venturi vacuum,  which  starts  the
flow through the remaining metering cell siphons
(1-6). Equal volumes of water are discharged to
each of the mixing cells  below.
   Each mixing  cell is mounted  on the operating
lever of the injector (Fig.  IB) and  triggers  an
injection each time water enters  it. The operating
lever turns a cogged wheel that drives a threaded
rod  against  the syringe  plunger.  The  injected
liquid  is transported by  a teflon tube  from  the
syringe to  the  mixing cell, where the turbulence
of the incoming water ensures adequate mixing.
Proper calibration of the standpipe  siphon in the
mixing cell ensures that nearly all of the toxicant
and  water is  present  and  mixed  before being
discharged into the flow-splitting cell.  This cell
is also equipped with a standpipe siphon for more
accurate flow splitting and easier cleaning.
  Control water can come from any of the  water-
metering cells:  in  this  system cell  2 was used
(Fig.  1A).  An individual metering cell ensures
that  the control will  always receive  an amount
of water (1 liter) equal to that of other test tanks.
The  proportional diluter uses the water remaining
after all metering cells are filled to supply control
water.  Therefore, if flow rates  change  for  any
reason, the control  \vater volume  could vary  as
much  as 50%  until  adjustments are made.
  The dispersant  control  has  one  injection  unit
to dispense the  dispersant only, while the control
water  empties directly into the flow-splitting  cell.
  Total cycling time for this system depends on
the flow rate of incoming water; in practice  the
fastest was approximately one cycle per minute
  The toxicant concentrations can  be varied by
one or all of the following adjustments:
  1)  The toxicant stock solution for the syringes
can  be changed. This adjustment will  vary each
concentration independently  of the others.
  2)  The  quantity  of toxicant solution  injected
can be controlled by syringe  size  (10-50  ml)  and
by  adjusting  the set  screws  on  the operating
lever (Fig. IB). These screws control the amount
of pivot of the operating lever,  which  can turn
from 1 to  10 cogs of the wheel per cycle.  These
adjustments allow an  injection volume  range of
2.3-85 fj.1
  3)  The amount of water receiving the injection
can be altered  by recalibrating the  siphon  in  the
water-metering  cell.
  Materials  — Most  of the materials  needed  are
similar  to  those  described  by  Mount  and  Brungs
(1967)  for  the proportional diluter.  The  following
materials are needed for the injection units  —  one
mechanical injector  for  each  toxicant concentration
and  for  the  dispersant  control. The injectors  are
available commercially; however, there  is no patent
on the injector so it can  be  copied or constructed by
any  individual.  For each injector one gas-tight gas-
chromatograph  syringe  is required. Sizes 10-50  ml
have  been  used successfully This type syringe  was
used  because of the resistance  of the teflon plunger
tip to toxicants and their dispersams.  Teflon tubing
                                                66

-------
 546
                                J. FISH.  RES.  BOARD CAN.. VOL. 32(4), 1975
                                                                                      urn uiniM am
                        FIG.  1.   Front (A) and lateral (B)  views of injector system.
was also used to transport the injected material. The
injection  mixing cells are  Erlenmeyer  flasks; one
flask is mounted on each injector operating lever. A
spring  is needed to  return  each  mixing  cell and
operating lever  lo original position. Counterbalances
can be used instead of springs, if smaller  mixing cells
are necessary.
  The  approximate  cost  for  one complete injection
unit  is from $100 to $130, this includes  the injector
cost  of $85 and syringe cost  which varies with size.
The  cost  of  this  system  containing five units  is
approximately $600-700.
BENOIT. D  A..  *ND F. A PLGLISI  1973 A simplified
    Row-splitting chamber and siphon for proportional di-
    luters. Water Res. 7: 1915-1916.
MOUNT. D.  1.. A.ND W. A BRLNGS  1967 A simplified
    dosing apparatus for fish toxicology studies. Water
    Res. 1:21-29
                                                 67

-------
                                APPENDIX  C
Water Research Pergamon Press 1973. Vol. 7, pp. 1915-1916. Printed in Great Britain
                                   NOTE

     A  SIMPLIFIED FLOW-SPLITTING CHAMBER  AND
           SIPHON  FOR PROPORTIONAL DILUTERS
                    DUANE A. BENOIT and FRANK A. PUGLISI
   U.S. Environmental Protection Agency, National Water Quality Laboratory, 6201 Congdon
                     Boulevard, Duluth, Minnesota 55804, U.S.A.

                              (Received 9 May 1973)
   Abstract—Simplified flow-splitting chambers and siphons were designed and tested for use
   with proportional diluters in bioassay systems. The apparatus allows each concentration from
   the diluter to be thoroughly mixed and divided four ways for delivery to duplicate fry and
   adult exposure tanks. Test water delivered to each exposure tank varied by only 5-10 per cent
   of the calculated volumes.

THE PROPORTIONAL diluter developed  by  MOUNT  and BRUNGS (1967) provided  a
dosing apparatus which can maintain a series of constant concentrations  of toxicant in
flowing water for bioassay systems. A typical faioassay system usually requires that
each concentration be  divided four ways for  delivery to duplicate fry and adult
exposure tanks. Flow-splitting chambers and siphons described in this report were
designed to be used with a proportional diluter which delivers 2 1. per concentration,
but the system can be modified to fit a diluter of any  size. The simplified siphon has
several advantages  over the conventional  U-tube siphon: difficult tube bending  is
eliminated,  water  volumes  siphoned  through  each  flow-splitting tube are easily
adjusted, and tubes can be disassembled for cleaning simply by removing each sleeve
from the standpipe.
A
j

ft
!
^
~-iP

5
\
K


\
P

1 i
s
a
1 :i
i
1
I i
i 
-------
1916                   DUANE A. BENOIT and FRANK A. PUGLISI

  The apparatus consists of six identical chambers with four flow-splitting siphons per
chamber (FiG.  1). Glass flow-splitting chambers measured 10 x 15 x 18cm high.
Four 2-5 cm holes were drilled in the bottom of each chamber. Glass-tube standpipes,
with two notches cut in one end (0-6 cm wide by 1 -6 cm deep) and a neoprene stopper
around  the other end,  were inserted in each of the four holes so the bottom of the
notches measured 15 cm above the bottom of the chamber. Glass-tube sleeves, with a
neoprene stopper around the outside of one end and the core from the hole bored in
the stopper  inserted in the other end, were placed o\er each standpipe. The flow-
splitting chambers  with siphons were then positioned beneath  the diluter  so the
toxicant-bearing water  and  dilutant  water fell  directly into each chamber. This
arrangement allows additional mixing before delivery to each exposure tank.  As the
test water rises slightly above the top of the sleeves in each chamber, water is forced
through the notches and down the standpipes.  This  action creates a siphon which
empties the chamber and delivers test water to each exposure tank.
  The diameter of each standpipe and  sleeve was determined by the flow rate of each
concentration delivered from the 2-1. diluter into each chamber. If the diameters of the
standpipes are too large, some siphons will not start: and if they are too small, some
siphons will start ahead of the others.  Siphon tubes for  each duplicate fry and adult
exposure tank delivered 150 and 850 ml per cycle, respectively, and were calibrated by
moving the stoppers, in or out, on either end of the siphon sleeve. Siphon sleeves for
the adult tanks must be kept as long as possible so each mixing chamber empties after
every cycle. Test water delivered to each exposure tank varied by only 5-10 per cent
of the calculated volumes.
  Delivery tubes from the flow-splitting chamber to each exposure tank should be
large enough to fit loosely over the lower end of each standpipe. The air break between
standpipe and delivery tube eliminates back pressure which can cause the siphon to
malfunction. If delivery tubes must be attached directly  to the standpipes, they must
slope downward toward the exposure tanks so each delivery tube empties after every
cycle.

                                REFERENCE
MOUNT D. I. and  BRUNGS W. A. (1967) A simplified dosing apparatus for fish toxicology studies.
    Water Research I,  21-29.
                                     69

-------
                                   TECHNICAL REPORT DATA
                            (Please read Instructions on the reverse before completing)
1. REPORT NO.
  EPA-600/3-7S-072
                              2.
                                                            3 RECIPIENT'S ACCESSION NO
4. TITLE AND SUBTITLE
  Manual for Construction and Operation  of  Toxicity
  Testing Proportional Diluters
                                                            5 REPORT DATE
                                                             July 1978  issuing date
             6 PERFORMING ORGANIZATION CODE
7 AUTHOR(S)
                                                            a. PERFORMING ORGANIZATION REPORT NO.
  A. E. Lemke, W. A.  Brungs, and B. J. Halligan
9 PERFORMING ORGANIZATION NAME AND ADDRESS
  U.S. Environmental  Protection Agency
  Environmental Research Laboratory-Duluth
  6201 Congdon Bou2 evard
  Duluth, Minnesota  55804
             10. PROGRAM ELEMENT NO
                      1BA608
             1 1. CONTRACT/GRANT NO
12. SPONSORING AGENCY NAME AND ADDRESS
  Environmental  Research Laboratory  -  Duluth
  Office of Research  and Development
  U.S.  Environmental  Protection Agency
  Duluth,  Minnesota  55804
             13 TYPE OF REPORT AND PERIOD COVERED
             14 SPONSORING AGENCY CODE
                                                                     EPA/600/03
15 SUPPLEMENTARY NOTES
16 ABSTRACT

       This paper  presents a discussion  of the testing procedures using proportional
  diluters.  The construction, calibration,  and operation  of the equipment  is  explained,
  and trouble shooting techniques necessary  for successful use of such equipment are
  given.

       A bibliography includes many  related  published materials that are not discussed
  in the text but  which should be useful to  the reader.  Included are numerous citations
  on physical toxicity testing methods,  but  papers on statistics or biological test
  procedures are not included.
17
                                KEY WORDS AND DOCUMENT ANALYSIS
                  DESCRIPTORS
  Dilution
  Construction
  Toxicity
                                               b IDENTIFIERS/OPEN ENDED TERMS  c.  COSATI 1 idd (iroup
  Testing procedures
  Dilution equipment
  Diluters proportional
  Operation calibration
                               14-B
18. DISTRIBUTION STATEMENT


  RELEASE  TO PUBLIC
19 SECURITY CLASS /This Report/

  UNCLASSIFIED	
                            21 NO OF PAGES
                               7 8
                               /0
20 SECURITY CLASS I This paget
  UNCLASSIFIED
                            22 PRICE
 EPA Form 2220-1 (Re». 4-77)   PREVIOUS  EDITION 15 OBSOLE
                                              70
                                                               •6 US GOVERNMENT PRINTING OFFICE 1978- 757-14OM442

-------