-------
solids removals; (2) more color removal  was effected by the  higher  powdered
activated carbon dosages; and (3) excellent removals of BOD5,  COD,  suspended
solids and color removals were obtained by reasonably small  amounts of chem-
icals confirmed by results from Table 23.
     One of the reasons for adding chemicals ahead of the multimedia filters
was to demonstrate that average daily National  Pollutant Discharge  Elimina-
tion System Permit requirements for all  stages  could be met.  Data  for a
twenty-month period when these particular evaluations were carried  out has
been shown in Table 26.  All first stage requirements were met except for
ammonia during a two-month period; it was felt  that this was strictly an
analytical problem since no other data approached violation status  and there
should not have been any ammonia present in the effluent from such  an oxida-
tion treatment system with greater than two-days detention time where nitri-
fication had been previously shown to take place.  All second stage require-
ments were met except for BODg during December and January.   Both months  were
characterized by periods of extremely cold weather, and during both months
permit requirements were met on the majority of days.  Scattered dally viola-
tions, particularly the two days following Christmas vacation when the man-
ufacturing plants did not operate for a nine-day period, were responsible for
this.  This underscores earlier statements to the effect that (1) multimedia
filter efficiency was directly linked to secondary clarlfler efficiency and
(2) a build-up of a very fine suspended solids in the biological system,  as
did happen over the nine-day vacation period, hampered efficiency and caused
increased BOD5 levels in the effluent.
     The third stage permit requirements which must be met  in the future are
subject to some further discussion.  Average dally permit requirements for
TKN were not met during seven of the twenty months 1n this  segment of the
study period.  Effluent TKN requirements for the third stage were set seventy-
one percent lower (285 to 83 Ibs/day) than for the first and second stage re-
quirements.  It was thought that TKN 1n the final effluent  was sufficiently
refractory (biologically Inactive) to assure that no  significant deleterious
effects would occur in the  receiving streams as a result of the discharge.
The final effluent contained approximately 200 Pt-Co  Units  of color; virtually
every dye used in both manufacturing plants contained organic Nitrogen.

                                      59

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   TABLE 26.  AVERAGE  POUNDS  PER  DAY  POLLUTANTS  REMAINING  IN  FINAL  EFFLUENT
      AFTER PHYSICAL/CHEMICAL TREATMENT VIA MULTIMEDIA FILTRATION WITH
     CHEMICAL ADDITION  COMPARED  TO THREE-STAGE  NPDES  PERMIT  REQUIREMENTS

YEAR/MONTH
1975
May
June
July
Aug
Sept
Oct
Nov
Dec
1976
Jan
Feb
Mar
Apr
May
June
July
Aug
Sept
Oct
Nov
Dec
AVG.
Lft
O
CO

159
130
134
102
84
103
148
243

252
148
141
171
109
83
117
96
76
86
120
175
134
SUSPENDED
SOLIDS

294
196
227
140
157
131
167
273

189
203
129
193
147
117
143
199
137
212
154
227
182
H-

117
119
103
76
64
67
79
108

142
72
57
164
58
105
57
57
58
64
72
57
85
co
O
0.
1-'

150
119
170
121
155
93
91
121

86
114
148
164
182
141
184
191
183
161
148
136
143
T, CHROMIUM

0.7
0.7
0.7
0.7
0.8
1.0
0.7
0.7

0.7
0.7
0.8
0.8
0.7
0.8
0.8
0.9
0.8
0.7
0.6
0.9
0.8
o
z
t— <
M
H-^

8.5
5.7
5.4
2.0
3.2
2.2
2.4
4.6

3.5
3.1
4.3
3.2
2.0
4.7
5.3
1.8
2.9
2.2
1.8
3.1
3.6
j

6.6
6.6
11.9
9.4
9.8
11.9
12,0
9.8

7.2
7.4
14.3
30.9
30.4
17.9
9.5
6.3
6.7
7.7
6.3
6.8
11.5
•-«
I'-

ll.!
11.0
23.9
29.6
25.8
17.9
28.7
12.3

24.0
21.0
17.0
29.7
22.6
26.9
22.7
30.4
17.9
10.7
29.5
18.0
21.5
OL
LU
CL
O

0.8
0.8
1.5
1.3
4.5
1.5
1.3
0.7

1.0
1.3
1.4
2.1
2.3
2.0
2.2
2.3
2.8
2.1
2.5
2.9
1.9
PHENOLS

4.7
2.4
3.2
2.1
1.6
2.2
2.9
1.6

3.0
2.3
1.9
1.6
1.5
2.8
1.2
1.2
0.2
0.2
0.7
0.2
1.8
ft^ Q
00
0 0.

215
189
146
160
152
159
153
165

183
163
209
204
182
193
187
198
217
224
229
201
186

NPDES
Permi
7/75-6/78;
Stage
1
2
3

375
210
210
t Effluent Requirements:
Stage

1,013
417
417
3 was

285
285
*83
Stage
1 was
12/73-6/75;
Stage
2 was
7/78-12/78.

225
225
225

4.7
4.8
2.0

21.0
21.0
12.5

19
46
46

79
79
21

5.0
6.7
0.8

9.6
9.6
4.0

-
-
-
*TKN may be higher provided permittee can show no deleterious effects on
stream biota and water quality.
                                      60

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Furthermore, a tremendous number of chemicals  used  in normal dyeing and finish-
ing in the textile industry contain organic  Nitrogen.  A  thirty-day long term
aeration study was made comparing (a)  100% final  effluent wastewater and
(b) 75% final  effluent wastewater with 25% made  up  of water  taken upstream of
the plant discharge.   Results of these two parallel  studies  have been shown in
part in Table 27.  The final  effluent  was  found  almost completely refractory
and presented evidence for modification negotiations with regulatory agencies.

         TABLE 27. LONG TERM AERATION  EFFECT ON  TKN IN FINAL EFFLUENT

Days
Aerated


0
11
20
30
BODC
•'• • 3
A
3.5
2.9
1.4
1.6
(mg/1)

B
2.6
2.0
1.4
1.8
COD (mg/1)

A
184
165
157
157

B
142
141
137
135
TOC (mg/1)

A
59
51
39
40

B
46
38
34
32
TKN (mq/1)

A
2.6
2.3
2.2
2.3

B
1.8
1.8
1.7
1.8
Sample A = 100% Final Effluent Wastewater
Sample B =  75% Final Effluent Wastewater/25% Upstream Water
     It was noted that the COD/BOD5 ratio for both Samples A and B exceeded
fifty, which indicated a well biologically treated Industrial effluent.  It
was doubtful whether longer aeration time would have caused significant changes.
     The major problem with meeting third stage NPDES Permit requirements was
shown to be removal of Antimony and Copper (heavy metals).  The Antimony re-
sulted from a dye fixative for certain add dyes needed to meet customer's
end use colorfastness requirements for certain shades.  Alternate after-fixing
methods, as well as color reformulations, were suggested and placed under In-
vestigation.  The Copper also resulted from meeting customer's specific end-
use colorfastness requirements for certain colors.  Alternate methods of treat-
ment as well as reformulations were suggested and placed under investigation
in order to reduce the Copper content 1n the final effluent.
                                      61

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      The single instance  of not  meeting  phenol  requirements was thought to be
 due to analytical  difficulties because this  parameter's  requirement was met
 during the remaining  nineteen months of  this study  segment.
      A particle size  distribution  and particle  count  is  provided in Table 28
 where secondary clarifler (biological) effluent was compared with multimedia
 filter effluent (final effluent).   In each instance approximately three-fourths
 of  the particles were 2.5 microns  or smaller.   It was Interesting to note that
 there were approximately  seventy percent fewer  particles 1n the multimedia
 filter effluent.   These particle counts  substantiate  turbidity readings and
 visual  checks made in-plant which  show a very clear,  though colored, final
 effluent.
      The multimedia filter,  with and without chemical feeds, has been demon-
 strated to be a viable advanced  wastewater treatment  technique for biologically
 treated, secondary-clarified, chlorinated wastewater  from plants dyeing and
 finishing  fabrics  knitted  from man-made  fibers.  There is no readily apparent
 reason why this technology  cannot  be applied to secondary wastewaters from
 plants dyeing and  finishing fabrics manufactured from man-made fibers or
 dyeing and finishing  these  same yarns 1n accepted yarn and/or fabric forms.
 Small  amounts of one  or more coagulant chemicals, which may be complemented
 by  powdered activated carbon addition, has been demonstrated to further reduce
 organic pollutant  and residual color levels  1n  secondary wastewater.  The
 success of this technology  remains tied  to the  quality of wastewater influent,
 the nature of the  wastes being treated, and  responsible wastewater treatment
 plant  operation.
     The application of the multimedia filtration technique with supplemental
 chemical additions has been  shown  to provide a  very high quality effluent which
 has met very stringent NPDES Permit requirements designed to protect extremely
 small  streams used for navigation, fish and wildlife propagation and recrea-
 tion.
     The somewhat  less successful  color removal cannot be considered a failure
because of  the nature of the colored compounds  1n the wastewater.   The presence
of residual color  in this particular multimedia filter effluent made 1t very
difficult  to treat to a quality satisfactory for dyeing and finishing reuse.
                                      62

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                   TABLE 28. PARTICLE SIZE DISTRIBUTION


SIZE RANGE
SAMPLE: SECONDARY
<1.25 u
1.25 - 2.5
2.5 - 5.0
5.0 - 7.5
7.5 - 12.5
12.5 - 25
>25 u
TOTAL

PERCENT
CLARIFIER EFFLUENT
29.7
54.2
7.2
3.6
1.6
2.0
1.2
99.5
APPROXIMATE
NUMBER/ML

4.60 x 106
8.40 x 106
1.12 x 106
0.56 x 106
0.25 x 106
0.31 x 106
0.19 x 106
15.5 x 106
SAMPLE: MULTIMEDIA FILTER EFFLUENT
<1.25 u
1.25 - 2.5
2.5 - 5.0
5.0 - 7.5
7.5 - 12.5
12.5 - 25
>25 u
TOTAL

23.5
50.0
21.0
2.2
--
—

96.7
1.45 x 106
2.25 x 106
0.93 x 106
0.098 x 106
--
--

4.45 x 106

SAMPLES TAKEN 6/8/76:  PRESERVED WITH MERTHIOLATE
                                     63

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Should very stringent color requirements be imposed, then other means of re-
moval demonstrated in the pilot water reuse study of this project would have
to be applied.  The cost of doing so would be very htgh.
     An expanded table showning NPDES discharge requirements has been provided
in Table 29.  A three-month monitoring report has also been compared to these
NPDES requirements in Table 29.
          TABLE 29.  NATIONAL POLLUTANT DISCHARGE ELIMINATION SYSTEM
                         DISCHARGE MONITORING REPORT
                         PERMIT CONDITIONS
                         IN POUNDS PER DAY
POUNDS PER DAY
PARAMETERS
BOD5
Total Suspended
Solids
Total Kjeldahl
Nitrogen
Ammonia
Total Phosphorus
Total Chromium
Total Zinc
Antimony
Total Copper
Phenols
Flow (MGD*)
pH (Units*)
AVERAGE
210
417
285
46
225
4.7
21
79
6.7
9.6
5.0*
6.0-8.5*
MAXIMUM
320
689
398
92
469
8.6
41
113
9.6
75
5.5*

MINIMUM
0.0
11.2
38.8
4.8
19.1
0.71
0.97
22.4
1.45
0.89
0.000*
6.9*
AVERAGE
96.9
150.5
80.7
12.8
175.9
0.84
3.99
27.6
2.03
1.50
2.624*

MAXIMUM
195.2
329.0
180.2
33.5
283.6
1.41
7.52
38.0
3.09
2.47
3.160*
7.5*

Permit Reporting Period:  June 1, 1976 through August 31, 1976.
 * Units as shown - not pounds
                                     64

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                                  SECTION 7
                          WATER REUSE - PILOT STUDY

     The second major objective of this project was to determine  whether  dye-
ing and finishing wastewater, which had been treated biologically and  by  phy-
sical/chemical means, via multimedia filtration with chemical  addition, could
be further treated to a quality suitable for dyeing and finishing reuse.   The
pilot study was carried out using two approaches.  The first was  a mobile
trailer equipped with chemical treatment to coagulate color and other  pollu-
tants, settle it to remove the greater portion of the heavy chemical  sludge
and filter the clarifier supernatant for greatly improved removals.  The  second
was a 5-column train consisting of columns charged with sand, powdered active
carbon, organic scavenging resin, cation ion-exchange resin, and  anion ion-
exchange resin.  Wastewater treated via this entire scheme was evaluated  1n
the laboratory to determine its suitability for reuse in the dyeing and fin-
ishing of man-made fiber fabrics.  The equipment, its operation and results,
are described in the following.

THE MOBILE PILOT PLANT
     The mobile pilot plant was a wastewater treatment plant consisting of a
chemical coagulation chamber, chemical addition equipment, twin flocculator
tanks, horizontal parallel tube clarifier, and mixed media filter.  This unit,
hereinafter referred to as the MPP (mobile pilot plant), was used to chemical-
ly coagulate the majority of the color and other pollutants present In this
particular wastewater.  The reduced color/pollutant load in the MPP effluent
was further treated to remove most of the remaining color, organics, and heavy
metals.
     The MPP coagulation system consisted of an  Influent line outfitted with
an adjustable flow control valve, a soleniod valve which closed the influent
                                       65

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 line  during  backwashing, and  provisions  for the simultaneous injection of up
 to  four  different  chemicals.   Four  12-gallon chemical mixing tanks and four
 chemical  feed  pumps were provided for these chemical additions.  A 1/30 Hp
 mixer was  provided for mixing  the chemical solutions.  The coagulation system
 also  consisted of  a rapid-mix  tank which provided a rapid-mix time of one
 minute at  the  maximum flow rate of  10 gpm by means of a 1/3 Hp mixer.  The
 wastewater gravity flowed into the  first of two flocculator tanks.  The first
 flocculator  was equipped with  a flocculation paddle driven by a 1/12 Hp gear
 motor at  6 RPM.  The second flocculator was equipped with a flocculator
 paddle driven  by a 1/12 Hp gear motor at 2 RPM.  The detention time in each
 of  these  tanks was ten minutes at the maximum flow rate of 10 gpm.  The pip-
 ing to this  system was such that the first flocculation compartment could be
 by-passed  by simply closing the valve to the first compartment and then open-
 ing the valve  to the second compartment which allowed the wastewater from
 the rapid  mix  tank to flow directly into the second flocculator tank.
      The clarifier flow was from the second flocculator tank only, irrespec-
 tive  of whether one or both had been used.  This system consisted of a
 settling tank with parallel, 7 1/2° from horizontal, hexagonal, one-inch
 settling tubes thirty-nine inches long.  Detention time was twenty-five
 minutes with a tube loading rate of 1.67 gpm/sq.ft.  The flow from the clar-
 ifier was  then filtered through a two square-foot surface area single-media
 filter.  The design flow rate  for the filter was five gpm/sq.ft.  The design
 backwash rate was  17 gpm/sq.ft. with a fixed surface wash rate of two gpm/
 sq.ft.  The filter was set to automatically backwash at a headloss of seven
 feet, but  a backwash could also be initiated manually by an "initiate"
 button on  the control panel.
      Pilot plant flow rate was controlled by the adjustable flow control
 valve in the influent line and matched with a float valve above the filter.
 The flow rate was  indicated by a flow meter in the effluent line.  The back-
 wash  flow  rate was controlled and set by means of an adjustable flow control
 valve provided in  the backwash line.
 The Mobile Pi lot Plant Operating Procedure
     The influent  to the MPP unit was the final effluent wastewater which
was diverted for further treatment instead of discharged directly to the

                                      66

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receiving stream.  This dyeing and finishing wastewater had been biologically
treated, secondary clarified, chlorinated and treated through the multimedia
filter plant as previously described.  This water was taken from a chlorina-
tor feed water line under pump pressure ahead of the chlorinator; a tee and
solenoid valve provided a water supply under pressure without need of a
supplementary sump and/or pump.  The flash mix tank was not used because of
a foaming problem which developed when high alum dosages were used.  Water
and Injected chemicals were added in the first flocculator where initial
flocculatlon took place under slight agitation from the 6 RPM stlrrer.   Secon-
dary flocculator effluent, after slow mixing, was gravity fed Into the horizon-
tal tube clarifier where the heavier, rapidly settling solids were removed.
The supernatant was filtered through the single media filter to remove roost
suspended matter.  The single media filter was backwashed when floe carry-
over was easily visible.  This usually occurred at a headloss of approximately
four feet.  The backwash was initiated manually but operated by an analog con-
troller.  Backwash water used was effluent from the MPP which had been stored
In a three-hundred gallon tank.  Backwash rate was thirty-four gpm and control-
led with the backwash flow control valve.  During each backwash* the tube clari-
fier was drained to remove sol Ids and then refilled with backwash water during
the last part of the backwash cycle.  The tube clarifier was drained because It
was the only means of wasting the settled sludge and the backwash water from the
filter.  Wastewater treated 1n this manner had greatly reduced amounts of color
and pollutant levels.  It was then piped to the second phase of pilot treatment,
the 5-column train.

FIVE-COLUMN PILOT  WATER TREATMENT PLANT
     The  final effluent from  the MPP was given further  treatment In  the 5-
column  train.  This  pilot treatment  plant  consisted  of  five  pressure columns
with a  decarbonator  incorporated between the  cation  and  anlon  columns.  Flow
through the plant  was  measured by a  5/8  Inch  bronze  meter;  flow  rate was
monitored by a ball  check valve.   Influent to this portion  of  the pilot plant
was provided by  a  3/4  Hp  deep well water pump.   Dimensions  of  the five  fiber-
glass  columns were 9-5/8" I.D.  x 4  feet  9-5/16 Inches high.  Each column  was
equipped  with two  0-100 psi  pressure gauges  for  measuring  inlet  and  outlet
                                       67

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pressure and to indicate the pressure loss across the beds.  Refer to Table
30 for design parameters for this 1.5 gpm 5-column pilot water treatment
plant.  Piping was arranged so that the full 1.5 gpm Influent (from the MPP)
could be directed Individually to each of the columns except the anlon ex-
changer.  It was necessary for influent to the anion exchanger to first have
been treated through the cation exchanger and the decarbonator.   Removal of
carbon dioxide by the decarbonator was necessary so that anlon exchanger
efficiency could be kept high.  Sand and carbon columns were only backwashed
for physical removal of entrapped solids.  The remaining three columns re-
quired both backwashing for physical removal and chemical regeneration.  Note
that backwash flow rates were varied for each of the columns.  Sand filtra-
tion was for protection against suspended solids fouling of the remaining
columns' media.  No appreciable color or pollutant removals were obtained,
as this installation served only as a protection for other units.  Carbon
served as an adsorption and absorption media.  Its use has been well docu-
mented.  The organic scavenging resin was evaluated to determine what effect
it had on color removal first and on organic pollutants second.   The cation
and anion exchangers were for final polishing by removing charged color
particles, metals known to affect dyeing and finishing, and other charged
molecules which were removable.
Filter Backwash & Operations Sequence
     Table 30  provides information on backwash and regeneration requirements
for all units.   The sand filter was backwashed using pilot plant effluent
whenever headloss reached 8 psi or at least once per week.  The carbon column
was backwashed with sand filter effluent whenever headloss reached 4 psi.
The organic trap resin was backwashed and regenerated using carbon column
effluent.  The cation exchanger was backwashed and regenerated using carbon
filter effluent when effluent pH increased by 0.2 - 0.3 pH units.  The anion
exchanger was backwashed and regenerated with the cation exchanger effluent.
During the upflow backwashing, resin loss was a problem which had to be con-
trolled by operator monitored backwash rate.  Visual examination was made
and flow rate was controlled to prevent resin loss.  The operation and back-
wash/regeneration operations of this pilot plant were extremely Involved and
time consuming.  It was necessary for an operator to remain with the equipment

                                       68

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                    TABLE  3d  DESIGN DATA FOR 1.5 GPM FIVE-COLUMN PILOT WATER TREATMENT  PLANT
10

EQUIPMENT
No. Units
Max. Influent
Max. Effluent
Media Type
Media Support
0.6 - 0.8 mm
Filter Sand
Volume of
Media (Cu.Ft.)
Depth of Media
(Inches)
Diameter of
Column (In.)
Height of
Column (In.)
Regeneration
or Backwash
Backwash
Rate (GPM)
SAND
FILTER
1
1.5 GPM
1.5 GPM
.45-. 50 ran
Filter Sand
4"
1.5
36"
9 5/8"
57 5/16"
Backwash
6
CARBON
FILTER
1
1.5 GPM
1.5 GPM
20 X 50 mesh
Acti vated
Carbon
4"
1.5
36"
9 5/8"
57 5/16"
Backwash
1.5
ORGANIC
TRAP
1
1.5 GPM
1.5 GPM
Dowex 11
4"
1.3
32"
9 5/8"
57 5/16"
Backwash &
Regeneration
1.0
CATION DECARBON-
EXCHANGER ATOR
1 1
1.5 GPM 1.5 GPM
1.5 GPM 1.5 GPM
Invercarb
C-110
4" None
1.3
32"
9 5/8" 12"
57 5/16" 48"
Backwash &
Regeneration
3.0
ANION
EXCHANGER
1
1 . 5 GPM
1.5 GPM
Invercarb
A-200
4"
1.3
32"
9 5/8"
57 5/16"
Backwash &
Regeneration
1.0
     (Continued)

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                                        TABLE 30.   (Continued)

SAND
EQUIPMENT FILTER
Backwash MPP
Water Source Effluent
Regenerant
% Solution
of Regenerant
Lbs. Regenerant/
Regeneration
CARBON
FILTER
Sand
Filter
-
Nad 40%
-
ORGANIC
TRAP
Carbon
Fi 1 ter
NaCl/NaOH
NaOH 4.0%
NcCl 7.5 Ibs.
NaOH .75 Ibs.
CATION DECARBON-
EXCHANGER ATOR
Organic
Trap
HC1
30%
26 Ibs.
AN I ON
EXCHANGER
Cation
Exchanger
Soda Ash
12%
5 Ibs.

NaCl = Sodium Chloride
NaOH = Sodium Hydroxide
HC1  = Hydrochloric Acid

-------
through the entire backwash sequence.   Any scale-up  of this  equipment should
be equipped with automatic flow controls and sufficient monitoring  equipment
to insure adequate backwashing and complete chemical  regeneration.

EVALUATION OF PILOT PLANT EFFLUENT WATER QUALITY
Color Removal
     Color was measured as apparent color with a Hellige glass color disc  and
expressed as Pt-Co units of color.  Extensive color measurements were made
from influent wastewater from manufacturing through final effluent from the
pilot plant.  Table 31 provides some of the extensive color measurements made
throughout the entire process.
     Color removal between full scale wastewater treatment plant influent  and
effluent was approximately 55%, with a residual color of approximately  200
units remaining to be removed by the pilot treatment processes,
     The MPP effected various removals dependent upon the amount of alum or
alum/polymer used for coagulation.  It should be noted that approximately
eighty percent of the total dye used in both plants was disperse dye; con-
sequently coagulation was demonstrated to be effective as a removal mechanism
for large amounts of color.  Soluble color had to be removed by ion exchange
resins in the organic trap, cation and anlon exchangers of the pilot units.
It should be noted that through the MPP, approximately 7-20% color was re-
moved when 100 mg/1 alum was used along with varying dosages of polymeric
coagulant aid.  However, when alum dosages were increased, color removal was
also increased.  At 200 mg/1 alum, some 29-40% color was removed; at 250 mg/1
alum, 20-80% color was removed; and at 350 mg/1 alum,  71-62% color was re-
moved.  At 350 mg/1 alum, consistently higher amounts  of color were removed.
     Average color removal across the  5-column wastewater treatment pilot
unit was approximately ninety percent.  The sand filter  removed essentially
no color, as was expected.  The activated  carbon filter  exhibited a continuing
reduction  in color removal efficiency  with  continuing  throughput.  Mid-way
through  the  project,  color removals of 60-80  Pt-Co  units could  be obtained;
however, with new carbon,  color removals  up to  110  Pt-Co units were obtained.
Carbon in  the column  was  replaced part-way through  the project.  The organic
                                        71

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                         TABLE 31.   EVALUATION OF COLOR REMOVAL FROM TEXTILE WASTEWATER
PRESENT WASTEWATER TREATMENT PROCESS
UNTREATED
MANUFACTURING
WASTE
Uni ts
Pt-Co
500
500
400
500
350
400
800
300
500
400
500
600
400
400
300
BIOLOGICALLY
TREATED WASTE
Units
Pt-Co
200
200
200
175
175
225
250
275
225
275
300
250
225
200
175
(Continued)
CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS
s:
cc
mg/1
10
10
10
10
10
10
10
15
15
10
10
10
10
10
10

CC
LU
O
mg/1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.5
0.5
0.25
0.25
0.25
0.25
0.25
0.10

o

-------
                                          TABLE 31.  (CONTINUED)
PRESENT WASTEWATER TREATMENT PROCESS
CD
»— >
a:
0=3
LU 1—

^f ^C
LU LU LU
ce =3 H-
\— zco
•z. ^ «a:

Units
Pt-Co
400
400
400
100
500
400
500
600
300
400
500
400
500
LU
>- H-
—1 CO
1 ^^
^ 3
(J
•— O
CD LU
O t—

O LU
»— * O£
CQ h-
Units
Pt-Co
225
225
225
250
250
250
250
200
200
175
300
200
250
(Continued)
CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS







s:
=3
	 i


mg/1
10
10
10
10
10
10
10
10
10
10
10
10
10




fV*
LU
s:

o
o.

mg/1
0.10
0.10
0.10



0.05
0.05
0.05
0.05
0.10
0.05
0.10






o

•*
a.

mg/1
15
15
-





25
25
25
25
25





\—

LU
_l =3
«*_!
ZLU
1— I LU
LU LU
Units
Pt-Co
200
175
200
175
200
175
200
200
150
150
200
175
200

WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES







y
=>
*C

mg/1
250
250
250
250
250

100
100
100
100
170
200
250




ac.
UJ
s:

0
o.

mg/1






1
2
5
12
12
12
12

EFFLUENT FROM





LU
_l 1— t—
HH OZ
CQ — J «C
Et-H _J
0-Ou
Units
Pt-Co
130
90
80
140
100
200
175
160
125
140
120
125
160





cc.
LU
0*-

tO Lu
Units
Pt-Co
130
90
80
140
100
200
175
140










Z ££
O LU
03 h-
C*. _J
O Lu
Units
Pt-Co
70
45
30
90
40
120
125
100









CJ
>— 1
"5^
•0:0-
CD «a:
DC. a:
ot-
Units
Pt-Co
70
45
35
80
40
120
125
90







cc.
UJ
CD
Z Z
0<
t_> l.J
units
Pt-Co
50
40
10
50
30
80
70
70







cc
LU
CD
Z
3£ i^
O Z
z x
ff. LU
Units
Pt-Co
17
20
5
35
10
60
40
35






CO

-------
TABLE 31.   (CONTINUED)
PRESENT WASTEWATER TREATMENT PROCESS
0
•— i
C£
0 =)
LU I—
«t «=c
LU U. LU
ce ra j—
»— z: co

=5 § 3:
Units
Pt-Co
500
400
800
500
700
400
300
400
400
400
500
450
i
LU
—1 CO
—I <
0 ~~
•_• Q
CD LU
O 1—
—I <.
O LU
•— t ce
CO >—
Units
Pt-Co
250
300
250
250
250
200
250
275
275
250
250
240
CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS





*^r
ZD
j
«C

mg/1
10
10
10
10
10
10
10
10
10
10
10
10

oi
LU

^H
_J
o


mg/1
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10



0

^£

Q.

mg/1
25
10
10
10
10
10
10
10
10
10
10
10



t—
LU

g^ 1
•Z. Lu
t-t U.
U. LU
Units
Pt-Co
200
200
200
250
200
175
200
250
250
225 '
200
175
WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES





2E

	 l
-------
scavenging resin appeared to remove small  amounts  of color when it was first
used; however, during the latter half of the project period,  almost no color
removal was obtained.
     The cation and anion exchangers together removed virtually all the color
present when influent to the cation exchanger contained less  than fifty Pt-Co
units of color and when large alum dosages had previously removed most dis-
persed color.  Carbon is not effective in removing color due  to dispersed
materials.
     This complete pilot wastewater treatment plant demonstrated  that residual
color could be removed from wastewater and that it could be  rendered  satis-
factory for dyeing and finishing re-use.  The fact that soluble and  insoluble
dyes must be removed by different mechanisms, when present in the same waste
stream, was demonstrated.
pH Determinations
     The pH was measured with a Beckman pH meter equipped with reference
calomel and glass electrodes.  The meter was standardized daily with pH  4.0
and pH 9.0 buffers.  Wastewater Influent to the pilot plant had a pH of  7.0 -
7.5.  In the first treatment stage when up to 350 mg/1 alum was used in  the
MPP, the pH was reduced by approximately 1.0 unit.  No appreciable pH change
occurred during passage through sand, carbon and organic scavenging resin
filters.  Effluent from the cation exchanger had a pH of 2.4 to 3.1, because
of hydrogen ion exchange for metals and other multlvalent substances.  How-
ever, pH was increased to between 4,1 and 8.8 during passage through the
anion exchanger where hydroxide was exchanged for other anlonlc groups.   In
a scale-up for a  large plant, both add and alkaline neutralization feeds
would be required in order to insure uniform pH water  to processing.  See
Table 32 for representative pH at all parts of the  total wastewater system.
Turbidity
     Turbidity was measured with a Hach Model 2100A Turb1d1meter for all
pilot plant readings.  Turbidity was usually noticeably higher 1n the MPP
effluent than the influent, because of  fine alum  floe  carryover.  This floe
carryover, not removed by clarification and media filtration, was Increas-
ingly visible toward the end of the operating cycle.   Turbidity removed by

                                      75
-------
TABLE 32.  pH EVALUATION
PRESENT WASTEWATER TREATMENT PROCESS
UNTREATED
MANUFACTURING
WASTE
Units
7.3
7.2
7.2
7.3
7.1
7.1
7.1
6.6
7.1
7.6
7.5
7.4
7.6
8.8
BIOLOGICALLY
TREATED WASTE
Units
7.1
7.4
7.1
7.2
7.0
7.1
7.1
7.2
7.3
7.3
7.2
7.3
7.5
7.3
(Continued)
CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS
§
mg/1
10
10
10
10
10
10
10
15
15
10
10
10
10
10

POLYMER
mg/1
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.5
0.5
0.25
0.25
0.25
0.25
0.25

o
o_
mg/1
35
35
35
35
35
35
35
35
35
35
35
35
35
35

FINAL
EFFLUENT
1
Units
7.2
7.5
7.3
7.3
7.1
7.2
7.3
7.4
7.4
7.1
7.2
7.0
7.5
7.3

WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES
5
mg/1
250
250
250
250
250
250
250
250
250
250
250
250
250
250

POLYMER
mg/1















EFFLUENT FROM
dSz
3Q _J 
Units
6.5
6.4
6.5
6.4
6.8
6.5
6.4
6.8
6.7
6.7
6.6

6.6
6.5

t— i
<£ a.
CD <3T
o: ad
01—
Units
6.4
6.6
6.6
6.5
6.9
6.7
6.4
6.4
6.7
6.7
6.7

6.6
6.5

CATION
EXCHANGER
Units
2.6
2.7
2.7
2.8
2.6
3.1
2.7
2.8
2.9
2.9
2.9

2.9
2.8

AMI ON
EXCHANGER
Units
8.7
8.4
8.1
8.8
6.2
7.3
6.7
6.1
5.8
4.8
4.6

4.6
4.5

-------
TABLE 32.   (CONTINUED)
PRESENT WASTEWATER TREATMENT PROCESS
UNTREATED
'MANUFACTURING
WASTE
Units
7.7
7.8
7.4
7.7
6.9
7.4
7.4
7.8
7.5
7.4
8.0
9.2
7.3
8.3
BIOLOGICALLY
TREATED WASTE
Units
7.4
7.6
7.5
7.3
7.1
7.1
7.2
7.3
7.2
7.2
7.1
7.2
7.2
7.2
(Continued)
CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS
s:
mg/1
10
10
10
10
10
10
10
10
10
10
10
10
10
10

POLYMER
mg/1
0.10
0.10
0.10
0.10



0.05
0.05
0.05
0.05
0.10
0.05
0.10

o
o.
mg/1
35
15
15






25
25
25
25
25

»—
LU
I-H LI-
LULU
Units
7.3
7.5
7.5
7.4
7.3
7.3
7.4
7.5
7.4
7.3
7.2
7.0
7.4
7.3

WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES
z;
 U-
Units
6.6
7.0
6.7
6.7
6.4
6.3
7.1
6.9
6.8


6.6



z on
O LU
IS
CJ tL-
Units
6.7
7.0
6.8
6.7
6.5
6.4
6.7
6.7
6.8


6.5



U> 
-------
                                             TABLE 32.  (CONTINUED)
PRESENT WASTEVIATER TREATMENT PROCESS

z
i— i
o:
0=3
LU •—
H- CJ

LU ' ' LU
a: :=>•—
»— Z CO
z<«t
=> S 3
Units
7.3
7.4
7.1
7.5
9.2
7.4
8.5
7.5
9.3
8.5
7.5
10.3
LU
5- I—
_J CO

^ 2
% Q
C3 LU
O 1-
-J <
O LU
*— • Orf
CO h-
Units
7.1
7.2
7.2
7.2
7.3
7.3
7.2
7.4
7.4
7.3
7.4
7.3
CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS





J^
=D
— 1

mg/1
10
10
10
10
10
10
10
10
10
10
10
10


Q,
LU
2£
^»
_1
O
O.
mg/1
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10




CJ

<£

a.
mg/1
25
10
10
10
10
10
10
10
10
10
10
10




1—
LU
_l =>
^f 1
ZU_
1— I LU
LU LU
Uni ts
7.3
7.4
7.4
7.3
7.4
7.1
7.3
7.5
7.1
7.3
7.4
7.5
WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES






js^
"~%
^ i
«x
mg/1
250
250
250
150
200
200
250
250
350
350
350
350


Q,
LU

^»
—I
O
a.
mg/1
12
12
12
3
3
3
3
3
3
3
3
3
EFFLUENT FROM




LU

l-H OZ
ca — i 
-------
sand, carbon and organic scavenging columns  was  only  slight;  the organic
scavenging resin lost much of its turbidity  removal ability during  the  latter
half of the project.
     The most significant turbidity removals were effected by the cation  ex-
changer.  It is not known whether the removal was by  physical  or chemical
means.  As more color was removed from the wastewater,  the interference due
to turbidimeter light beam absorption was reduced giving a more accurate
reading.  See Table 33 for turdibity readings throughout the  entire full-
scale and pilot wastewater treatment facilities.
Specific Conductivity
     All specific conductivity measurements  were made with a  Beckman Conduc-
tivity Bridge.  Since addition of salt in dyeing with direct  dye  colors was
not common practice in these two manufacturing plants, the normal  final
effluent conductivity was 450 - 600 mhos with occasional readings  slightly
above and below this range.  Conductivity increased to 600 -  800 mhos in  the
MPP trailer effluent due to alum treatment.   This range was  generally con-
stant through sand, carbon and organic resin filter columns.   However, con-
ductivity increased to a typical 1500 - 3000 mhos when passing through the
cation exchanger; this was due to increased hydrogen ion concentration.
Table 34 reflects specific conductivity readings through the full-scale and
pilot treatment plants.  The abrupt reduction in specific conductivity of
anion exchanger effluent should be noted.  This indicated a high purity water
was generated.
     Specific conductivity was an excellent  indicator of breakthrough of both
the cation and anion exchangers and was employed as an operational tool.
Unusually high readings  in anion exchanger effluent, shown in Table 33, was
the signal that caused this unit to be backwashed/regenerated.
Total Solids  (TS)
     Total solids were determined gravimetrically, using  TOO milliliter
samples.  The treated wastewater effluent to  the receiving stream contained
approximately 500 mg/1 of  total solids;  this  water source became the influent
to the  pilot  plant.  Passage  through  the MPP  unit generally netted a slightly
                                      79
-------
TABLE 33.  TURBIDITY
PRESENT WASTEWATER TREATMENT PROCESS
UNTREATED
MANUFACTURING
WASTE
FTU
71
78
60
77
79
95
60
77
66
73
67
65
61
88
BIOLOGICALLY
TREATED WASTE
FTU
29
28
20
21
18
16
29
20
29
40
24
17
10
15
(Continued)
CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS
z:
mg/1
10
10
10
10
10
10
10
15
15
10
10
10
10
10

POLYMER
mg/1
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.5
0.5
0.25
0.25
0.25
0.25
0.25

o
a.
mg/1
35
35
35
35
35
35
35
35
35
35
35
35
35
35

FINAL
EFFLUENT
FTU
5.3
3.8
3.5
4.7
4.4
4.1
7.9
8.0
9.9
15.0
8.1
2.5
2.5
2.4

WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES
2:
mg/1
250
250
250
250
250
250
250
250
250
250
250
250
250
250

POLYMER
mg/1















EFFLUENT FROM
LU
^S£
CO — 1 
-------
                                             TABLE  33.   (CONTINUED)
PRESENT WASTEWATER TREATMENT PROCESS
UNTREATED
MANUFACTURING
WASTE
FTU
88
56
65
66
23
60
55
64
58
88
63
59
58
55
BIOLOGICALLY |
TREATED WASTE
FTU
8
14
14
15
21
17
18
16
22
22
19
30
18
19
(Continued)
CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS
z:
mg/1
10
10
10
10
10
10
10
10
10
10
10
10
10
10

POLYMER
mg/1
0.10
0.10
0.10
0.10



0.05
0.05
0.05
0.05
0.10
0.05
0.10

0
o.
mg/1
35
15
15






25
25
25
25
25

FINAL
EFFLUENT
FTU
2.5
6.0
6.0
6.3
5.4
5.9
7.7
5.4
5.8
3.4
2.6
4.5
4.2
4.0

WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES
_i
mg/1
250
250
250
250
250
250
-
100
100
100
100
170
200
250

POLYMER
mg/1







1
2
5
12
12
12
12

EFFLUENT FROM
LU
d££
CO _1<£
z: CL a.
FTU
5.4
8.8
8.1
4.7
12.0
6.1
5.3
9.4
8.8


8.0
5.4
5.4

or
LU
01—
CO LU
FTU
3.9
7.0
6.2
4.6
12.0
7.0
5.1
9.4
8.4


6.6



"Z. 
-------
                                            TABLE 33.   (CONTINUED)
PRESENT WASTEWATER TREATMENT PROCESS
i— <
O =3
H- O
111!1 LiJ
rv ~~^ i -


IDS 31
FTU
51
60
100
69
15
44
55
44
24
52
47
30
LU
>• t—
-i O
O 1 —

O UJ
J^S
03 »-
FTU
21
33
32
25
22
15
7
21
31
30
20
17
CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS



y*
3

•*
mg/1
10
10
10
10
10
10
10
10
10
10
10
10

cr:
UJ
^_
I
o
0-
mg/1
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10


- o

<

a.
mg/1
25
10
10
10
10
10
10
10
10
10
10
10


z:
LU
	 1 13
^C 	 I
z u.
»-t LU
Lt_ LU
FTU
4.5
4,6
4.2
7.0
4.0
2.3
2.2
5.0
9.0
11.0
17.0
5.5
WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES



"SL

^_^

-------
                                               TABLE  34.   SPECIFIC CONDUCTIVITY
oo
OJ
PRESENT WASTEWATER
TREATMENT PROCESS
CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS




i
rv
UJ

jgr
3

s: o

1 ^£
o
3: j o- a.
mg/1
10
10
10
10
10
10
10
15
15

10
10
10
10
10

mg/1 mg/1
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.5
0.5

0.25
0.25
0.25
0.25
0.25


(Continued)
35
35
35
35
35
35
35
35
35

35
35
35
35
35



I

H-

UJ
__l ~*^
^C — J
•Z. U.
«-• U.
Lu UJ
umhos
610


510


540

560


480


460



WATER
MPP CHEMICAL
FEED RATES

1 .i _
1

i
1 C£
! I UJ

*y
< *"">
i
et
mg/1
250
250
250
250
250
250
250
250
250

250
250
250
250
250






LU
S _!»—(—

1-1 OZ
_l CO _I«C
o
o.
mg/1
'


















O •— ' -J
s: a- a.
umhos
640
635
610
605
490
480
680
800
760

780
780
700
700
680



REUSE PROJECT
EFFLUENT FROM

> j


; a: : z ce.
, LU ' O UJ
. OH- , ca J—
, Z _J . DC _J

I/) U- ' <_} U-
(j
i— t

CL
^^
a: a:
O 1—
££
UJ

3Z ^
f} i^^
i—* rc
1— 0

O UJ
umhos ; umhos umhos | umhos
630 , 640 690
630 ; 630 630
i 615 ; 615
615
605 i 630 640
i 490 i 500
475 : 480
685 ', 685
i
i
770 ! 780
i
790 | 780
760 j 760
700 | 700
710 j 710
680 1 690
i
I
j
515
480
680

820

800
780
710
720
700



2300
1600
1600
1400
1400
510
1800
3000
2700

2200
2200
2100
2100
2000



a;
LU

2;
"^ ^f
OX
I-H O
Z X
CC LU
umhos
19
16
16
84
14
220
44
12
10

15
36
27
30
100



-------
                                                      TABLE 34.  (CONTINUED)
CX)
PRESENT NASTEWATER 1! •..•TO pcncr pomFfT
-REATMENT PROCESS !; "n ~* Rc°SE PRUJEC'
CHEMICAL FEED ' '• ppp nFv^ft'
RATES AHEAD OF ! .! FEED '^s" '
y'JL'IXEDIA FILTERS ! :
1 ' '
' i ' ' ' ' ' }
: ! . '1 i !
-' QJ ; z ! • a:
: .1 i i i ! I ' t < i Q£
s: ^ . ° 5: _i 2; >• ^ozoi—

O i— i u. 	 l O O ~^ — ;<•— <
< a. 'a. u_--jj cc : — 2: G. Q. • to u.
: ; i
rc/1 ma/1 ma/1 umhos mg/1 TIC/! urchos 'umhos
"*!"*'"' ' i "
10 ; 0.10 ! 35 250 I 710 710
; • ; ; •
10 0.10 i 15 ; 250 690 690
10 i 0.10 15 590 250 710 710
; •
10 : 0.10 ; 540 ! 250 650 660
!
10 0.10 ' 10 590 250 630 670

:
10 i 0.10 10 430 250 620 630
1
10 ; 540 550
i
10 I 0.05 630 100 : 1 700 690
10 = 0.05 ! 100 j 2 610 : 610
! 1 • '
10 ; 0.05 25 . 100 5 580
t i
10 i 0.05 ! 25 550 ,100 12 540 ;
10 | 0.10 i 25 170 12 ; 750 i 760
10 1 0.05 ! 25 200 | 12 '• 520 |
i 1 '
10 '' 0.10 i 25 250 ! 12 590
; 1 i
10 i 0.10 | 25 520 250 12 j 750 | 740
(Continued) j ; 1 •

iFFLUEN


1

!
O LU 1
CQ 1— '.
CC. _J
<: —i
00.

umhos i

710 ;

670
710

680 ;

670


620
1
510

700
610




730



i
j 740
i

T FROM


*
!
o :
z i
<: a. •
O ef.
C£. C£
O t— :

umhos ;

700 ;

670 i
720 !

770

720


640

550

740
630




700




730





r^ \
\ j j ,

ol i
i— i ~r" ,
h- tJ
 UJ

umhos
i
1800
1
1700
1900

4500

2300


1900

1500

2200
1500




1450




1600





^^
.
3
z <
O —
*— ^_^
Z X
-------
                                                    TABLE  34.   (CONTINUED)
C3
CJ1
PRESENT WASTEWATER
TREATMENT °ROCESS
CHEMICAL FEED !
RATES AHEAD CF
MULTIMEDIA FILTERS




2C
^^
'•
«=c
mg/1


10
10
10

10

10
10
10
10
10

10
10






I
1
.
; QC
LiJ
; 2:
} ^—
—I
• 0
' C.
f
: mg/1

i
10.10
1
0.10
0.10

0.10

0.10
0.10
0.10
0.10
0.10

010
0.10








I
| 4
i
cj 	 i :
^X -
^t p^ L
, »~^ *

WATER
REUSE PROJECT
MPP CHEMICAL
FEED RATES

z
• *
^
_• 2:
•J— ^3
.1^ ' j
Q. j 1_U i_J  i
10 ;

10
. 10 55(
10 ; 35(
10

1 200

i 200
3 250
3 250
j| 350
10 j 400 1 350

10 j
10 42C








i
350
) 350
t
H1

il
!l
i
! t
t
j i
i
ce. •
: <_U uj
, S — 1 1— 1—
>• >•— • O Z
—1 'CQ _l <
: O O •— i _J
Q,
2; Q. 0.
|
\ mg/1 umhos
j i

12
12
750
780
3 590

3 630


3 620
3
3
3
3

3
3







650
650
650
640

630
650








i
i
I or
I UJ
1 *"^ K*~
j Z —1

; (/) U.
i
'umhos


|750
j 790
I 600

1 640

• 630..
J660
i640
650
640

650
650








EFFL'JENT FROM
|
i
j z a:
OLJ
CD 1—
C£. _l
^^ >^H
' t_> U-
1 	
i umhos

i
j 745
\ 810
600

640

650
660
640
650
640

650
650








' ce
' ' LU
" ' Z Z
• z i o «c
1  UJ
i
• umhos umhos

i
750 1800
| 810
2200
620 1700
i i
660

650
680
660
1850

1500
1600
1400
630 1300
700

670
650







2600

2100
1800







o:
UJ
O

Z 
-------
 lower total solids concentration.  Only a very minor reduction in total solids
 was realized through the combined treating of sand, carbon and organic scaveng-
 ing filters; however, by the time treated wastewaters exited the anion exchang-
 er, the last step in the pilot process, 85% of the total solids had been re-
 moved.  Table 35 presents the total solids at various locations within the
 Total treatment system.  When 350 mg/1 alum was used in the MPP, the total
 solids levels in the pilot plant effluent were less than 50 mg/1, which in-
 dicated that a very high quality water had been generated.
 Biochemical Oxygen Demand (BOD,-)
     BOD5 determinations were made using the standard 5-day incubation t1r«e
 and the procedure found in the fourteenth edition of Standard Methods For The
 Examination of Water 8 Wastewater.  Dissolved oxygen was determined by a
 properly standardized dissolved oxygen meter.  All samples were seeded with
 5% secondary clarifier effluent (non-chlorinated).  Table 36 is provided to
 show 5-day values for all major locations in the full-scale and pilot treat-
 ment processes.  BODr values were too low to be particularly meaningful;
 therefore, BODg, COD and TOC values have been compared in Table 39.  BODg in
 the influent to the pilot plant averaged 5.1 mg/1 and was reduced almost
 sixty percent by the MPP unit alone; only about ten percent more reduction was
 realized through the 5-column train.
    ll cal Oxygen Demand (COD)
     Chemical oxygen demand was determined by the dichromate reflux method
found in the fourteenth edition of Standard Methods For The Examination of
Hater & Wastewater.  Less than half the total COD removal occurred 1n the MPP
unit, with most occurring during treatment through the 5-column train.  In
Table 37  COD values throughout the whole wastewater treatment process have
been shown.
Total Organic Carbon (TOC)
     A Beckman Model 215 Carbon Analyzer was used for all TOC determinations.
Acidified samples were Nitrogen sparged to remove carbonates and bi carbonates.
Twenty microliter samples were used for analysis.  Organic carbon was con-
verted to carbon dioxide by reaction with pure oxygen at 950°C. ; the newly
converted carbon dioxide was measured and recorded.  Total organic carbon was

                                      86
-------
                                          TABLE 35.  TOTAL  SOLIDS  (mg/1)
CD


I

PRESENT >,ASTE>JA-ER "EATXENT PROCESS ij *A,ER RE.SE PROJECT

i CHtMiCAi. ."
"£C3 ^ -t 	

; >- , RATES AnEAD G~ :' '"-'---"^Vl"-"" E~,ri.^E'i~
,_ .' — , v, . „-,,--...,, _-,__-. i"Ci> XM.C.J
^ ' <^ i lUi_ i ii'iCUin fiuiCKj ;
— : '_5 I/1) '
o:
; . -^
*~~ r_^
< < .^
Si E5 t^
t1" - •— o ^r < —
; — H i : ^j o 5 — _. . S a:
O« j tX- t-i-l ! ^C ^- •£— 	 — *. . -. 	 ' "~
,-ng/". ; ~g/~, ., r,-,g/", r.g/", r;/~. ,-g/". !
35 ! 250 500 390
' i
35 ! 500 ; 250 i 488
• - i i
35 :

35 520
; 250
I
250 459
35 ; 250 \ 428 , 346
35 j j 250 : 545 420 ;
f '
35 250 : 578 458

35 i 495 250 '
35

35 550
35 1 490
j
35 465
35
35
35

250 :
i ; ,
250
250 i 474 362
i
250 i 480 384
250 453 376
250 i ; 451 363
250 i 453 392
: i
~
t-_
O
z:
o re
rr x
^C L^J
,g/-,
34

33



125
26
230

88





75

37
38
82
44

-------
                                              TABLE  35.   (CONTINUED)
o>
03
PRESENT *ASTE/;ATER TREA


CHEMICAL F
7KEM PROCESS '-ATER
Htul :
» • — — - —»•-*••
RcoSE PROJEC.

>• RATES AHEAD OF ; "i:.:-":,1-^- £.-
'-

— =
~~" —^
•^C <
— - — _-f
"^ *~ — '.
— — • r/*
5 < < :

-;/-. ;

i
600



670

625 •

710








685

545
680


^^ _-_^ ^7O . i
^- _*_ 	 , O '•
»-i- ^*- 
x. z: ^: x
O i — < "-1-!
r.g/-, : r.g/-.

416 50
410 ' 47

448 76

411 , 68

!
330 ; 45
451 80
453 '. 90


i
387 \ 39
i




392 50
378 48

i
-------
                                             TABLE 35.  (CONTINUED)
PRESENT XASTEwATER
                                                                     WATER REoSE  PROJEC
                                 RATES A.-.EA5 GF

                               iXuLTIiXEDIA FILTERS
                                          FEED RATES
00
10

< <
5: ID —
•z. < <
^ ^- 3
^

860















'_> t/',
O uj
QQ 
-------
TABLE 36.  BODs (mg/1)
PRESENT WASTEWATER TREATMENT PROCESS
UNTREATED
MANUFACTURING
WASTE
mg/1
375
385
315
260
350
355
312
415
290
325
330
350
312
185
325
330
300
335
75
145
222
198
265
BIOLOGICAL
SYSTEM
EFFLUENT
mg/1

11.0
13.7
13.5
12.3
12.0
14.2
5.8
23.7
29.7
19.0
4.9
7.1
8.4
10.0
7.6
8.6


10.0
9.2
11.0
18.0
(Continued)
CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS
. s:
mg/1
10
10
10
10
10
10
10
15
15
10
10
10
10
10
10
TO
10
10
10
10
10
10
10

POLYMER
mg/1
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.50
0.50
0.25
0.25
0.25
0.25
0.25
0.10
0.10
0.10
0.10



0.05
0.05

0
Q.
mg/1
35
35
35
35
35
35
35
35
35
35
35
35
35
35
35
15
15







FINAL
EFFLUENT
mg/1
4.9
3.8
3.9
5.6
5.3
5.4
5.1
7.5
13.5
12.5
8.0
3.6
3.2
2.8
3.5
5.2
4.9
8.7
4.8
4.2
4.4
5.7
5.5

WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES
2:
_i
mg/1
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
260
250
0
100
100

POLYMER
mg/1




















0
1
2

EFFLUENT
UJ
-J h-H-
HH OZ
00 _J «t
O •-« — 1
2: o. o.
mg/1
2.4
1.8
1.7
1.8
2.6


1.9
2.4
4.7
1.8
1.4
1.5
1.4

1.8
1.5
1.9

2.1
2.7
2.5
5.2

ANION
EXCHANGER
mg/1
1.7
1.5
1.3
1.4
2.0


1.0
1.4
4.5
1.7
1.2
1.4
2.2

2.1
2.1
2.2
3.0
3.7
2.9
2.4
2.8

        90
-------
TABLE 36.  (CONTINUED)
PRESENT WASTEWATER TREATMENT PROCESS
z
1— «
o =>
UJ h-
H~ * .*
^C ^£
uj u» uj
on rs i—
>— Z t/>
z 3  lJ-
, , ^_ j^_
00 OO UJ
mg/1


9.3
10.3
11.8
15.3
10.7
12.3

6.0
5.8
8.5
7.0
8.3
4.3
7.0
7.0
CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS




•C"
^J
1
«£
mg/1
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10

rV
UJ
^F*
*^ -
	 |
o
Q-
mg/1
0.05
0.05
0.10
0.05
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10



o

0*f

CL.
mg/1
25
25
25
25
25
25
10
10
10
10
10
10
10
10
10
10
10

i—

UJ
—I Z3

z u.
<—• U.
U. UJ
mg/1
2.7
2.1
4.5
5.1
5.1
5.3
4.1
3.7


3.1
2.8
3.1
5.1
4.3
6.4
4.5
WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES




S;
3

«c
mg/1
100
100
170
200
250
250
250
250
150
200
200
250
250
350
350
350
350

Of.

«EZ
^__
i

o.
mg/1
5
12
12
12
12
12
12
12
3
3
3
3
3
3
3
3
3
EFFLUENT


UJ
•«J H* h™
I-H O 2Z
03 -»<
O +-* — J
Z O_ O_
mg/1
2.4
1.8
1.9
2.4
3.4
1.9
1.6
1.1
2.6
1.3
2.8
2.5
1.0
3.7
1.2
1.2
0.9
LU
C9
Z?
^^ ^C
oa:
<-> t_>
z x
-------
TABLE 37.   COD (mg/1)
PRESENT WASTEWATER TREATMENT PROCESS
UNTREATED
MANUFACTURING
WASTE
mg/1
500













1098




960



BIOLOGICAL
SYSTEM
EFFLUENT
mg/1










321

288



278



242
232

(Continued)
CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS
s:
<
mg/1
10
10
10
10
10
10
10
15
15
10
10
10
10
10
10
10
10
10
10
10
10
10
10

POLYMER
mg/1
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.5
0.5
0.25
0.25
0.25
0.25
0.25
0.10
0.10
0.10
0.10



0.05
0.05

o
-------
TABLE 37.   (CONTINUED)
PRESENT WASTEWATER TREATMENT PROCESS
CO
•— i
a:
O =3
1— O

LU U. LU
OC Z3 1—

§1§
mg/l

960
995








845


887



_j
0 J—
co z: LU
O LU :=}
— 1 1— — J
O 00 U-
i— i >- U_
CQ CO LU
mg/l

249















CHEMICAL FEED
RATES AHEAD OF
MULTIMEDIA FILTERS




. s:

_i
mg/l
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10

Q,
UJ
£

	 1
0
Q.
mg/l
0.05
0.10
0.05
0.10
0.10
0.10
0.10
0.1Q
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10



o

^f
CL.
mg/1
25
25
25
25
25
25
10
10
10
10
10
10
10
10
10
10
10


t—
LU
_J =3
*f, —i
z: LU
U_ LU
mg/l

170






155

152






WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES




z:
=3
_i
mg/l
100
100
170
200
250
250
250
250
150
200
200
250
250
350
350
350
350

Q,
1 if
^S^
^M
^f
o
Q_
mg/l
5
12
12
12
12
12
12
12
3
3
3
3
3
3
3
3
3
EFFLUENT


UJ
— • r™ r™
^™^ ^J 2»
BQ — J ^t
s: a! 5^
mg/l
154.

130.


104.


128.
98.4
118.
103.

173.
81.3
76.9
84.0
ce
LU
0
z?
z <
o 3:
t~H CJ
Z X
mg/l
34.4

34.4


11.6


32.0
7.9
19.0
4.0

7.5
7.4
<4.0
<4.0
         93
-------
                          TABLE 38.   TOTAL ORGANIC CARBON
PRESENT WASTEWATER TREATMENT PROCESS
CHFMICAL FEED RATES AHEAD
OF MULTIMEDIA FILTERS
ALUM
mg/1
POLYMER
mg/1
P A C
mg/1
FINAL
EFFLUENT
mg/1
WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES
ALUM
mg/1
POLYMER
mg/1
EFFLUENT
MOBILE
PILOT
PLANT
AN I ON
EXCHANGER
mg/1
TOTAL ORGANIC CARBON
15
10
10
10
10
10
10
10
10
10
10
10
0.50
0.25
0.10
0.10
0.10
-
0.10
0.10
0.10
0.10
0.10
0.10
35
35
35
15
-
-
25
10
10
10
10
10
100
67
60
66
61
64
140
62
56
62
28
74
250
250
250
250
250
250
250
150
250
250
350
350
_
-
-
-
-
-
3
3
3
3
3
3
56
-
59
42
36
30
74
60
36
31
26
28
50
4
4
10
6
5
10
12
4
<1
2
2
                                      94
-------
calculated by proportioning peak level  of sample  to  peak  level of a known
standard.  Only about fifteen percent TOC was  removed  by  the MPP unit while
seventy-five percent of the remaining TOC was  removed  by  the 5-column train.
See Table 38 for comparison.
     The BODg, COD and TOC values and removal  efficiencies  have been compared
in Table 39 for the pilot treatment plant.

                TABLE 39.  POLLUTANT REMOVALS  VIA PILOT PLANT

Total
Pollutant

Parameter
BOD5
COD
TOC

Influent
5.14
185
61
MPP Unit
Effluent
2.13
105
51
5-Column Train
Removed
59
43
16
Effluent
1.92
11
13
Removed
10
90
75
Removed
mg/1
3.22
174
48
%
63
94
79

     While most BOD5 removal  was accomplished in the MPP unit,  the 5-column
train was needed to remove most of the COD and TOC present.   The ratios  of
COD to BOD5 and TOC to BODg increase noticeably between initial  influent and
final effluent values.
The Nitrogen Group - Ammonia, Nitrates, Total Kjeldahl Nitrogen (TKN)
     Considerable data was accumulated on the Nitrogen group made up of  am-
monia, nitrates, and TKN, because of concerns over these parameters in present
and future permits to discharge wastewater to streams.
     The nitrate analysis was performed according to procedures in the 1974
edition of EPA's manual of Methods for Chemical Analysis of Water & Wastes.
The brucine method was used.   An intense yellow color resulted from the  re-
action of nitrate and brucine after a reaction time of twenty-five minutes
at 100°C. this yellow color was measured spectrophotometrlcally at 410 nm
wavelength.
     Both ammonia and TKN were determined according to procedures 1n the
fourteenth edition of Standard Methods For The Examination of Water & Waste-
water.  Ammonia was determined by adjusting pH to 9.5, distilling 1t into
                                      95
-------
 boric  acid,  titrating with 0.02  N  sulfuric acid and calculating the Nitrogen
 present as ammonia.  The  TKN was determined by converting the organic Nitro-
 gen  to a Mercury  ammonium complex.  This complex was decomposed by sodium
 thiosulfate  and the ammonia distilled from an alkaline medium and absorbed
 in boric acid.  Titration was by 0.02 N sulfuric acid and thus was calculat-
 ed.
     The determined ammonia, nitrate and TKN values have been recorded in
 Table  40.  Ammonia levels were usually less than 0.3 mg/1 when final effluent
 wastewater was received as influent to the pilot treatment plant.  Therefore,
 it was  not possible to evaluate  the effectiveness of ammonia removal via the
 steps  in this pilot plant.  A small amount of nitrates were present in the
 pilot  plant  influent, at  usually less than one mg/1 concentration.  Very
 little  nitrate was used in the dyeing and finishing plants and this par-
 ticular wastewater was considered nitrogen deficient, so that nitrate
 (as NaNO-j) was added prior to biological treatment to insure adequate nu-
 trient  levels for biological conversion.  Some nitrate was removed through
 the MPP  unit, with almost all the remaining removed through the 5-Column
 train.
     Most of the Nitrogen in the pilot plant influent was 1n the form of
 organic  Nitrogen or TKN.  Because the ammonia was usually below the accu-
 rate detection limits the organic Nitrogen level was considered to be the
 TKN level.  Addition of alum with and without polymeric coagulant aids,
 ahead of the MPP reactor/clarifler provided some TKN removal.  This re-
 moval was approximately thirty percent on the average.  The 5-Column unit
 further  reduced TKN levels by an additional seventy-four percent to approx-
 imately  0.5 mg/1.
     A major problem at this location, referred to earlier, was final ef-
 fluent TKN concentration versus NPDES permit requirements for the final
 six months of the current permit period.  This pilot study underscored a
 basic premise that the TKN remaining 1n the final  effluent to the stream,
as currently treated,  would be extremely difficult to remove technically
and that removal  would be economically prohibitive.  Further, the TKN
remaining in the MPP unit effluent was sufficiently high that 1t would not
                                   96
-------
                            TABLE 40    NITROGEN  SERIES
PRESENT WASTEWATER TREATMENT PROCESS
CHEMICAL FEED RATES AHEAD
OF MULTIMEDIA FILTERS
ALUM
mg/1
POLYMER
mg/1
P A C
mg/1
FINAL
EFFLUENT
mg/1
WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES
ALUM
mg/1
POLYMER
mg/1
EFFLUENT
MOBILE
PILOT
PLANT
AN I ON
EXCHANGER
mg/1
15
10
10
10
10
10
10
10
AMMONIA.
10
15
10
10
10
10
10
10
10
10
0.50
0.25
0.10
0.10
-
0.10
0.10
0.10
NHROGEN
0.10
0.50
0.25
0.10
0.10
-
0.10
0.10
0.10
0.10
35
35
35
15
-
10
10
10

35
35
35
35
15
-
10
10
10
10
0.2
0.2
0.2
0.3
1.6
<0.1
0.4
<0.1

<0.3
<2.0
<0.3
<0.3
<0.3
<0.3
<0.05
0.3
0.4
<0.3
250
250
250
250
250
250
350
350

250
250
250
250
250
250
250
250
350
350
-
-
-
-
-
3
3
3

-
-
-
-
-
-
3
3
3
3
0.2
0.3
0.4
<0.1
-
0.4
0.2
0.2

<0.3
<2.0
<0.3
0.45
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.1
<0.1
<0.1
<0.1
<0.3
<0.1
<0.1
<0.1

<0.3
<2.0
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
<0.3
(Continued)
                                       97
-------
                              TABLE 40.   (CONTINUED)
PRESENT WASTEWATER TREATMENT PROCESS
CHKM1CAL FEED RAILS AHEAD
OF MULTIMEDIA FILTERS
ALUM
mg/1
POLYMER
ing/1
P A C
ing /I
FINAL
EFFLUENT
mg/1
WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES
ALUM
mg/1
POLYMER
mg/1
EFFLUENT
MOBILE
PILOT
PLANT
AN I ON
EXCHANGER
mg/1
TOTAL KJELDAHL NITROGEN
15
10
10
10
10
10
10
10
10
10
10
0.50
0.25
0.10
0.10
-
0.10
0.10
0.10
0.10
0.10
0.10
35
35
35
15
-
25
10
10
10
10
10
<2.0
2.2
1.7
2.8
2.4
4.2
3.6
2.2
2.6
3.1
5.0
250
250
250
250
250
'250
150
250
250
350
350
-
-
-
-
-
-
3
3
3
3
3
<2.0
1.2
2.0
1.7
4.2
2.3
2.1
2.2
2.1
1.4
1.2
<2.0
0.3
<0.3
0.3
0.3
<0.3
0.4
0.4
0.8
0.3
0.5
                                      98
-------
be possible to meet NPDES requirements of eighty-three  pounds  per  day  final
effluent TKN level, should total  flow be increased significantly.   The
volume of sludge which would be generated with a coagulation process would
be completely disproportionate to the small  amount of TKN which  would  also
be removed, i.e. the cost for the incremental  removal would not  be justified.
Total Phosphorus
     Total Phosphorus was determined by the Ascorbic Acid method following
Persulfate digestion as prescribed in the procedures found 1n  the  1974
edition of EPA's manual of Methods for Chemical Analysis of Water & Wastes.
This parameter was monitored because of tremendous Interest in phosphorus
levels in North Carolina streams as a result of phosphate mining and  fertil-
izer plants within the state.  Total Phosphorus levels  generally present no
problem; however, on some days levels are unusually high (8 mg/1 or more).
The MPP unit removed significant amounts of Phosphorus; indications were
that the greater the alum dosage, the lower the effluent concentration as
shown in Table 41.  Approximately two-thirds of the total Phosphorus  was
removed via the MPP unit and almost all of the remaining one-third was re-
moved via the 5-Column train.
Chlorides
     Chlorides were determined according to the mercuric nitrate method given
in the fourteenth edition of Standard Methods  For the Examination of Water
& Wastewater.'
     Influent to the pilot plant contained low chloride  levels  (20-70 mg/1).
As shown in Table 41,  no consistent or  significant  change occurred 1n the
MPP  unit.  However, the 5-Column train,  largely the anlon exchanger,   removed
chlorides to below 10  mg/1 concentration.  Such a low level would offer no
problems to water reuse in dyeing and finishing.
Sulfates
     The sulfate analysis was  according to the  turbldimetric  method given
in the fourteenth edition of Standard Methods  For the Examination of  Hater
& Wastewater.
                                     99
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                    TABLE 41.   PHOSPHORUS,  CHLORIDES,  SULFATE
PRESENT WASTEWATER TREATMENT PROCESS
CHEMICAL FEED RATES AHEAD
OF MULTIMEDIA FILTERS
ALUM
mg/1
POLYMER
mg/1
P A C
mg/1
FINAL
EFFLUENT
mg/1
WATER REUSE PROJECT
MPP CHEMICAL
FEED RATES
ALUM
mg/1
POLYMER
mg/1
EFFLUENT
MOBILE
PILOT
PLANT
AN I ON
EXCHANGER
mg/1
TOTAL PHOSPHORUS
15
10
10
10
10
10
10
10
10
10
10
CHLORIDES
15
10
10
10
SUL FATES
15
10
10
10
10
0.50
0.25
0.10
0.10
-
0.10
0.10
0.10
0.10
0.10
0.10

0.50
0.25
0.10
0.10

0.50
0.25
0.10
0.10
0.10
35
35
35
15
-
25
10
10
10
10
10

35
35
35
15

35
35
35
15
10
4.9
7.9
6.2
7.4
8.6
8.7
12.1
7.7
7.0
9.9
5.8

69
19
50
25

2
<5
23
<5
33
250
250
250
250
250
250
150
250
250
350
350

250
250
250
250

250
250
250
250
350
-
-
-
-
-
-
3
3
3
3
3

-
-
-
-

-
-
-
-
3
1.1
1.0
5.7
1.4
1.1
1.3
5.2
3.3
1.3
3.9
0.4
•
73
49
49
1.9

84
73
36
66
160
0.10
<0.10
0.06
0.30
0.11
<0.10
<0.10
0.10
<0.10
<0.10
<0.10

2
2.5
4.0
3.2

<5
1
<5
<5
<5
                                      100
-------
     Sulfate levels 1n process treated wastewater varied greatly  from approx-
imately two to thirty mg/1 which resulted from variations 1n  sulfate contain-
ing chemicals useage in dyeing and finishing.   Sulfate concentration was  in-
consequential in this wastewater, which became the influent to the  pilot
plant, because the sulfate level was significantly increased  in the MPP unit
by the alum (aluminum sulfate) additions.  As  shown in Table  41,  the 5-
column train effectively removed the sulfates  to below five mg/1.   The higher
the alum dosage needed in the MPP unit for removal of any one of  several
specific parameters, the greater the sulfate level which would be removed in
the anion exchanger.  The efficiency of the anlon exchanger would be greatly
reduced if high alum dosages became necessary  1n a full-scale plant modeled
after this pilot treatment plant.
Metals
     Metals were analyzed by atomic absorption procedures.  Table 42 provides
information on metals analyses for multimedia  filter effluent. MPP  effluent
and anion exchanger effluent for the metals Aluminum, Antimony, Calcium,
Copper, Chromium, Iron, Magnesium, Manganese and Zinc.
     Only trace amounts of Chromium and Manganese were found 1n the multi-
media filter effluent, so no meaningful evaluation of their removal could be
made.  It was considered likely that the pilot plant would effect removals
of virtually any amounts of these found 1n dyeing and finishing wastewaters.
     Aluminum concentration was noticeably increased by alum dosages  in  the
MPP unit; however, the final effluent from the pilot plant showed less  than
0.5 mg/1.
     Increases in concentrations of Iron and Zinc following treatment  through
the MPP unit were determined to be from tramp metals in the alum source  used.
The 5-column train effectively removed these multlvalent metals from waste-
water.  This was important because of known metal-dye complexes which  cause
dye shade changes on fabrics; such would likely preclude reuse of any  waters
containing significant amounts (greater than 0.5 mg/1) of Chromium, Copper,
Iron, Manganese, Magnesium and Z1nc.
     The presence of significant amounts of these metals in any wastewater
being considered for reuse would have to be taken Into account when evaluating

                                     101
-------
                            TABLE 42. METAL SERIES

a:
ID
_J
mg/1
METAL
10
10
10
10
10
10
10
10
10
10
10
10
10
METAL
250
250
250
250
250
100
170
150
200
350
350
350
a.
mg/1
DC
UJ
—1
O
a.
mg/1
ANALYSES ON
35
35
35
35
15
-
10
-
25
25
10
10
10
0.10
0.50
0.25
0.10
0.10
0.10
0.10
0.05
0.05
0.10
0.10
0.10
0.10
ANALYSES ON
-
-
-
-
-
12
12
3
3
3
3
3
-
-
-
-
-
-
-
-
-
-
-
_
i
§. ALUMINUM
— j
O =)
s: •-<
•-« o
I— —1
«S o
ug/1 mg/1
c
^CHROMIUM
a:
UJ
-------
                             TABLE 42.  (CONTINUED)

s:
ID
_J
^£
mg/1
o
•a:
a.
mg/1
QC
UJ
O
(X
mg/1
s:
z:
3C
13
^c
ug/1
1
I-H
f-
^t
ug/1
z:
1—4
<_ )
mg/1
s:
o
oc.

ug/1
o:
LU
a.
a.
o
o
ug/1
1
H^
ug/l
lAGNESIUM
i.
mg/i
UJ
CO
UJ
1
3E.
uq/l
tj
•z.
»— t
t*4
ug/1
METAL ANALYSES ON ANION EXCHANGER EFFLUENT
                    800   1200   0.02 < 30   <20   < 30     .090 < 30  < 30
                    100  < 500   0.08 < 30   <20     50     .015 < 30  < 30
                    100  < 500   0.14 < 30   <20    210     .016 < 30  < 30
                    200  < 500   0.16 < 30   <20   < 30     .012 <30  < 30
                    1400  < 500   0.14 < 30   <20    470     .016<30  < 30
                                     103
-------
 various treatment methods  to render waters  suitable  for  critical manufactur-
 ing operations.

 OPERATIONAL  PROBLEMS  OF  THE  PILOT PLANT
      A number of problems  were  encountered  with  the  pilot  plant  and  its
 operation during the  approximately eleven months  of  operation.   The  MPP unit
 was operated from December 1975 through November  1976 while  the  5-column
 train was operated from  late February  1976  through November  1976.
      The  initial  problem was one of frozen  pipes  in  the  MPP  unit during the
 severe late  December  to  early February  cold.  This problem was solved by keep-
 ing water flowing through  on a  continuous basis.  Operation  as a reactor/clarl-
 fier was  carried  out  only  during the warmer part  of  the  day  and on several ex-
 tremely cold days the unit could not be operated.  The 5-column  train was pro-
 tected somewhat  by shelter and  was  operated without  damage from  freezing.
      Variable chemical feed  pumps  in the MPP  unit gave tremendous reliability
 problems.  The solution  was  finally to  calibrate  them for  a  fixed feed rate
 and vary  the chemical feed concentration in the stock solution to give the
 desired chemical  dosages.
      Two  operational  problems were  encountered with  the  MPP  unit.  A foaming
 problem occurred  in the  rapid mix  tank  when 100 mg/1 or  more alum was used.
 This  foaming  problem  was likely aggravated  by residual surface active materials
 in  the wastewater.  The  solution to this problem  was to  stop the rapid mixer
 and  depend on the slow mixer in the first flocculator tank for providing the
 level  of  contact  needed  between alum and the  suspended waste particles.  The
 second, more  important problem  was  the  very short runs when  alum dosages were
 250  -  350 mg/1.   Very large  quantities  of settleable alum  floe was generated
which  quickly  overloaded the settling tubes 1n the tube  clarifler and back-
washing was  then  required  after  only two hours operation.  This problem would
be overcome  in a  full-scale  coagulator  by provisions for intermittent and/or
continuous sludge wasting.
     The 5-column  train was operated with fewer mechanical equipment problems.
The major problem was adjusting  the regenerant feed rates  during backwashlng/
regeneration by use of an aspirator and  valve system which was very difficult
                                      104
-------
to adjust.  This problem would not be encountered 1n  a full  scale model of
this pilot plant because the aspirators would be replaced  by metering  pumps.
     Two other operational  problems were encountered  with  the  5-column train.
Resin losses from organic scavenging, cation exchanger,  and  am'on exchanger
columns during backwash regeneration was a problem which was tied to the
above mentioned problem of controlling flow during this  step.   The  second
problem was the need for an operator to be in attendance at  all  times  during
the complete regeneration cycle - a cycle which took  some  seven and one-half
hours when all five columns had to be regenerated. This regeneration  time
often had to be spread over two days which greatly reduced effective equip-
ment run time.
     Backwash/regeneration time and gallons through-put for each of the pilot
plant component parts has been shown below for normal operation. These time
requirements were often much longer when equipment problems occurred.

                          Normal Gallons Through-Put  or     Backwash and/or
   Pilot Plant            Before Backwash (BW) and/or       Regeneration
   Component              Regeneration (Reg)	     Time Required
MPP Trailer                      4200 BW                       1/2  Hour
Sand Filter                      1/wk BW                       1/2  Hour
Carbon Filter                    1/wk BW                       1/2  Hour
Organic Trap              as anionic column (BW + Reg.)        2   Hours
Cation Exchanger             1200 BW + Reg.                    2   Hours
Anion Exchanger              1900 BW + Reg.                    2-1/2 Hours

     The other limiting factor to pilot plant operation was the quality of the
influent wastewater.  If the biological plant gave problems, these problems
had to be corrected before any pilot plant runs could be made, due to  man-
power availability.  No pilot runs were made when the influent had unusually
high turbidity (70-100 JTU) which normally followed a biological plant upset.
After a manufacturing plant shutdown of two days or longer, one or more days
usually passed before initiating further pilot plant runs due to abnormally
high amounts of fine suspended matter  in the multimedia filter effluent.
     The major effects of these problems was an extension of the time  required
to complete the project and a reduction of the number of experiments possible
to run.                               105
-------
                                   SECTION 8
                         LABORATORY REUSE EVALUATIONS

     Laboratory investigations were conducted to determine if residual color
in  the multimedia filter effluent would be scavenged by fibers during conven-
tional dyeing operations.  If the residual color were not scavenged, 1t would
be  theoretically possible to find a dyeing procedure to reuse a portion of the
wastewater without considerable further treatment.  This would make treatment
for dyeing and finishing reuse more attractive economically.

LABORATORY DYE SCAVENGING EVALUATION
     Laboratory experiments were carried out in the plant dye laboratory.
Greige knitted fabric (tricot) was used for ease of handling.  The various test
fabrics were made from (a) type 6 caprolactam nylon, dull luster; (b) secondary
cellulose acetate, dull luster; (c) knitted fabric blend of 80% cellulose
triacetate, dull luster, and 2Q% type 6 caprolactam nylon, dull luster; and
(d) homopolymer polyester, dimethylterephthalate type, semi-dull luster.  It
should be stated that the 80% triacetate/20% nylon tricot construction was
used for evaluating triacetate.  The tricot knitted construction sufficiently
hides the nylon so that the discoloration noted is contributed by the triace-
tate and not by the nylon.  For the purposes of this experiment, this fabric
was considered as representative of triacetate fiber.
     In this investigation, dyeings using three different sources of water were
made on each fabric as follows:
1.  Laboratory water, ground water cation exchange treated for production use.
    Pt-Co color less than two units,  (this was the control for the experimen-
    tation.)
2.  Wastewater after full-scale multimedia filtration at the wastewater treat-
    ment plant (not the pilot installation).  Pt-Co color - 400 units.
                                       106
-------
3.  Wastewater blended with cation exchange treated  water  for  processing
    fabric in the manufacturing plant's dyeing and finishing operation,  A
    blend of 100 ml. wastewater with 900 ml.  of laboratory water.   Pt-Co
    Color - 40 Units.
     The four fabrics were also scoured in the three sources of water  identifi-
ed above.  No optical brightener was added.  Scouring of 20-gram swatches of
fabric were made in a steam-heated water bath in one-liter stainless steel
beakers.  A 50:1 liquor to goods (weight) ratio was  a standard laboratory
procedure.
     Three 20-gram swatches of each of the four grelge fabrics were prepared.
Four stainless steel beakers were then filled with each of the three types  of
water to be used, making a total of twelve.  Then each beaker  was  charged with
the following chemicals: (a) one gram per liter of a proprietary  solvent scour
(60% aromatic and aliphatic solvent blend/40% anlonic and  nonlonlc surfactant
blend), (b) one gram per liter of sodium trlpolyphosphate.  The fabric swatches
were impaled on sharp stainless steel rods colled over beaker  positions on  the
steam-heated water bath where the scours were to be  made.   A motor driven
attachment stirs the swatches by a reciprocating up/down motion  1n the beaker.
     The water and chemical charged beakers were placed on the water  bath  and
the swatches were lowered into the beakers via stainless steel rods, which  were
attached to the reciprocating stirring mechanism.  Stirring was  begun  at once
as the temperature was raised to 716C (160°F) and maintained at  that  temper-
ature for twenty minutes.  After that length of time, an additional chemical
charge of 0.2 grams per liter of citric acid was added to  each beaker  and  the
scouring was continued uninterrupted for an additional ten minutes. At the
end of this thirty-minute total scouring cycle, the  swatches were raised via
the rods from the beakers.  The change of pH during  scouring was  to allow  color
scavenging to take place under both alkaline and add conditions.   Alkaline
and acid conditions are both common in production dyeing processes.
     After this scouring cycle, each swatch was removed from the  retainer  coll
and rinsed by hand under tap water (cation exchange  treated) for thirty
seconds.  Swatches were then centrifugally extracted in a  laboratory  ten-pound
                                       107
-------
model extractor to remove excessive water (approximately 20% moisture  by weight
of fiber remaining).   Swatches were then drawn taut onto pin frames  and dried
in a forced draft laboratory oven for 75 seconds  at 190°C (375°F).   The three
scoured swatches of each fabric were dried simultaneously to minimize  any
color variation from the drying step.  After drying, swatches  were  removed
from the pin frames and allowed to come to thermal  equilibrium under ambient
laboratory conditions.   Swatches were examined visually after  they  had been
brought to equilibrium.  The observations are presented in Table 43  to show
how those scoured in  100% treated wastewater and  10% treated wastewater/90%
cation ion-exchange treated water compared to the control scoured in the
cation ion-exchange treated laboratory water.

TABLE 43.   VISUAL COMPARISON OF COLOR SCAVENGING  BY VARIOUS FIBERS  SCOURED  IN
WASTEWATER  (Secondary  Clarified, Chlorinated, Multimedia  Filterf)
 Fiber
 Type 6
 Caprolac-
 tam Nylon
 Secondary
 Acetate
 80/20%
 Triacetate/
 nylon
 Polyester
 (disperse
 dyeable)
100 ml Treated Water/
900 ml Cation ion Ex-
change Treated Water
Pt-Co Units = 40
 Very noticeable
 Discoloration
 Very slight dis-
 coloration
 Very noticeable
 Discoloration
 Very slight
 Discoloration
           100% Treated Wastewater
Position   Pt-Co Units = 400        Position
   4        Very Severe                4
            Discoloration
   2        Noticeable                 2
            Discoloration
            Severe
            Discoloration
   1        Slight
            Discoloration
 'l  =  least  amount  of  staining;  4  =  greatest  amount  of  staining
      This  series  of  experiments  shows  that  the  various  fibers  scavenge color
 from  tertiary  treated wastewater in  differing amounts.   Type 6 nylon  scavenged
 the most color, even more  than  triacetate;  these  two  fibers scavenge  several
                                       108
-------
times more color than either secondary acetate  or  polyester.  A dyeing and
finishing plant processing nylon and/or triacetate could  not use even the ten
percent blend of tertiary-treated wastewater with  ninety  percent of its reg-
                                                       o     o
ular process water for scouring at temperatures up to  71  C  (160 F) when treat-
ed wastewater color was 400 Pt-Co units or higher.  A  plant dyeing and finish-
ing only acetate and/or polyester could consider this  10/90 blend where scour-
                                               o      o
ing would be carried out at a temperature of 71 C  (160 F) or less.  However*
unless the plant was using extremely large amounts of  water for scouring below
  o      o
71 C (160 F) there would be no economic justification  for considering such a
blend of waters.
     This series of experiments indicated that  neither scouring nor dyeing
with this 10/90 blend of water could be considered in  a plant  dyeing and
finishing nylon and/or triacetate because of their severe residual color
scavenging effect.  These two fibers comprised  about 50 percent of the  fabrics
which are dyed and finished at this location.  In order to  make the color
scavenging effect of fibers in fabric form more objective,  whiteness was de-
termined for the two samples scoured in (a) 100% treated  wastewater, and
(b) 10% treated wastewater, compared to a control  scoured in  cation exchange
treated water used for in-plant processing.  Whiteness was  determined  on  these
scoured, untinted, non-optically brightened fibers in fabric  form by  use  of
American Association of Textile Chemists & Colorists Test Method  110-1975,
"Reflectance, Blue and Whiteness of Bleached Fabric."   The formula  for white-
ness found in paragraph 3.3 of this Test Method was used; it 1s:  W=4B-3G where
W = Whiteness; B = Blue reflectance; and G = Green reflectance.   See  Table  44
for a presentation of the numerical values.  The  reflectance values  for Blue
and Green filter readings were used to calculate whiteness.  The  Instrument
used to determine reflectance using blue and green filters was a  Gardner
multi-purpose refleetometer.
                                      109
-------
              TABLE 44.   INSTRUMENT WHITENESS  COMPARISON,  CONTROL
                VERSUS WASTEWATER SCOURED FIBERS  IN  FABRIC FORM
                                   100 ML Treated Water/
                                   900 ML Cation               100% Treated
 FIBER                 CONTROL      Exchange Treated Water      Uastewater
 Type 6
 Caprolactam             71                   64                    45
 Nyl on
 Secondary Acetate       68                   66                    60
 80/20% Tri-Acetate/     64                   61                    48
 Nylon
 Polyester (Dis-         68                   67                    64
 perse Dyeable)
     These whiteness readings confirmed the visual evaluation shown in Table 43.
Even if residual color remaining in the tertiary-treated wastewater was only
40 Pt-Co units, this water would be unsuitable for processing nylon and triace-
tate.  The processing of secondary acetate and of disperse dyeable homopolymer
polyester should be considered only if further residual color reduction was
accomplished by some means such as improved removal of color or even dilution
to further reduce total residual color.  The seriousness of even considering
this approach must be underscored because (a) a dyeing and finishing plant
would necessarily be handicapped by being able to process only certain fibers
and (b) the scavenging effect of other fibers, natural, animal and man-made is
unknown and would require further extensive investigation.  This experiment
further strengthened the need for a water reuse evaluation.  It was well es-
tablished that color removal from wastewater was difficult and was made even
more difficult by small amounts of residual  color contributed by several clas-
ses of both water-soluble and water-insoluble dye types.

RESULTS OF COMPARATIVE DYEINGS USING MOBILE PILOT PLANT (MPP) EFFLUENT
     Relative whiteness was used as a measure of the effect of these efforts
to obtain water sufficiently higher in quality and lower in color which could
                                      110
-------
be satisfactorily reused in the dyeing and finishing  of man-made  ftber  fabrics.
Water taken from several pilot plant runs was used to dye whites  on  nylon and
polyester; these two fibers were selected because nylon was  demonstrated to be
an effective scavenger of color bodies from this particular  treated  waste-
water, and polyester was demonstrated as being the least affected by very
large amounts of color in the dyebath water.
     Table 45 shows the relative whiteness of nylon and polyester fabrics dyed
using MPP effluent from selected pilot plant runs over the duration  of  the
pilot wastewater reuse study.  There were several apparent discrepancies when
comparing relative whiteness of the swatches dyed using control  process water
versus recycled water from the pilot plant effluent,   Samples E  and  F tn
Table 45 indicate essentially the same whiteness on the control  dyeing  and  on
recycled water dyeing.  Note however, that the color of the pilot plant
effluent used for dyeing these two samples was high.   Compare nylon  Samples  E
and F with sample  H; when sample H was dyed using pilot plant effluent hav-
ing 35 Pt-Co units of color, it showed a significant difference  1n relative
whiteness compared to the control dyeing made at the same time.   While  samples
E and F were not affected by high amounts of residual color in the pilot plant
effluent used for dyeing (20 and 40 Pt-Co units respectively); sample H,  when
dyed in pilot plant effluent containing 35 Pt-Co units of color, showed a
marked reduction in relative whiteness, 63 versus 69 for the control, which
indicated the fiber scavenged color from the pilot plant effluent.  The most
logical explanation is that the color bodies in the pilot-treated wastewater
for samples E and F had no affinity for the nylon fiber while those color
bodies present at the time sample H was dyed did have affinity for the  nylon
fiber.  This should be understood 1n view of the number and complexity  of
different dyes used in the manufacturing plants and the potential for chemical
change which could cause the above apparent difference in residual color
scavenging.
     The nylon samples J and K showed definite color scavenging  effects when
dyed in pilot plant effluent containing only two to three Pt-Co  units of color.
The only explanation given was that certain add dyes were not removed  by the
pilot treatment scheme and those were sufficiently neutral dyes  to be exhaust-
ed onto nylon at pH 6.  Dyeing results on nylon at less than two Pt-Co units

                                      111
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                          TABLE 45.  RELATIVE WHITENESS OF DYED FIBERS (FABRIC FORM)
ro
Sample
A
B
C
D
E
F
G
H
J
K
L
M
N
P
Recycled
Water
Fabric Pt-Co Units
Fiber Color
Nylon 6 125*
Nylon 6
Polyester 1
Polyester
Nylon 6
Nylon 6
Nylon 6
Nylon 6
Nylon 6

Polyester

Nylon
Polyester
Whiteness determined by Reflectance
Method 11 0-1 975.
25*
25*
25*
20
40
8
35
2
3
2
3
<2
<2
using American
*Wastewater Treatment Plant effluent recycled only
and not through 5-column train.
Water
Recycle
Date
1/14/76
1/15/76
1/14/76
1/15/76
4/7/76
5/5/76
5/26/76
6/2/76
3/8/76
3/10/76
3/8/76
3/10/76
11/8/76
11/8/76
Association
through MPP
Relative Whiteness
Control Recycled Water
79
74
77
74
68
73
67
69
76
76
74
74
63
63
69
63
73
74
69
74
65
63
71
72
74
74
63
63
of Textile Chemist & Colorfst Test
Coagul ation/Settl i ng/Fi
Itration Unit
     Control dyeings were all made from regular in-plant process water; water source was deep well; prior
     treatment was through cation exchange resin systems followed by decarbonizing.
-------
of color, however, were equal in quality to the results  of the control  dyeing.
When color was reduced below two Pt-Co units,  water was  satisfactory  for  dye-
ing all fibers in whites and very light pastel  shades,  as well  as  in a full
range of normal shades.
     Figure 6 shows the color comparison made spectrophotometrically  for  waste-
water treated on November 8, 1976.  Effluent from the full-scale wastewater
treatment plant including biological treatment, chlorination and multimedia
filtration with pre-filtration additions of 10 mg/1 alum,  0.10 mg/1 anionic
polymer and 10 mg/1 powdered activated carbon has been shown as "influent to
MPP".  This influent to the MPP had 200 Pt-Co units of color.  This wastewater
was treated in the MPP coagulation/settling/filtration unit with 350  mg/1
alum, and 3 mg/1 anionic polymer; effluent from this part of the pilot unit
shown on the graph was also found to have 45 Pt-Co units of color or  a reduc-
tion of 77.5% color.  Further treatment through the 5-Column train gave a
very clear, essentially colorless effluent, which has been shown on the top
of the graph in Figure 6 and which was found to have less than two Pt-Co
units of color.  Shown in Figure 7 for comparative purposes, 1s a pilot plant
run made on 9/16/76 and compared to laboratory tap water  (plant process water).
Note that the pilot plant effluent was essentially equally as color free as
the tap water control.
     The series of pilot plant runs made during November, 1976 using secon-
dary clarified, chlorinated wastewater having 175-250 Pt-Co  units of color
as influent, gave a pilot plant effluent essentially color free; all  four
runs were measured as having a maximum of two Pt-Co units of color.  However,
extremely heavy chemical feeds ahead of the reactor/clarlfier were used to
achieve that color level, 350 mg/1 alum and 3 mg/1 anionic polymer.  In
addition, these four runs were through the entire  5-Column train Including
sand filtration, organic scavenging, granular activated carbon, cation and
anion exchange resins.  The required high concentration of chemical feeds
created very high capital and operating costs as well as  the need for  sophis-
ticated wastewater treatment in the scale-up  to a  one million gallon-per-day
plant, presented in Section 9.
                                    113
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    100
O


JS    90
O
                Anion Exchanger'Effluent
-------
     The results of dyeing polyester indicated the greater  likelihood of suc-
cess in treating wastewater treatment plant effluent to a reduced  level of
color and other parameters which would allow it to be successfully reused for
scouring and possibly for dyeing in the manufacturing plant.   However, several
factors must be taken into consideration.   The lower the process water temper-
ature, the greater the likelihood of success with reuse of  treated wastewater.
Certain processes such as scouring at temperatures below the  boil  and scours
at high pH's would be more easily adaptable.  Extreme care  would be required,
however, when considering high temperature (110-130 C or 230-265 F) dye-
ing of polyester with this type of advanced treated wastewater.  Some dyes,
particularly Anthraquinone Red dispersed dyes, are extremely  sensitive to
certain metal ions such as Copper, Manganese and Iron.  Those individuals
responsible for dyeing must know the potential metals levels  1n process water.
These metal ions may be contributed by dyes and/or chemicals  used  in process-
ing or even from other sources if several  water streams are fed into the waste-
water treatment plant.
     Table 45 shows that dyeings on samples A and B on nylon, and  C and  D on
polyester, were made using water produced during two early  runs of the MPP
coagulation/settling/filtration unit when color was 125 and 25 Pt-Co color
units, respectively.  The nylon scavenged color efficiently as expected;
whiteness compared to the control dyeing showed about as much color scavenged
by the nylon at 25 Pt-Co units of color as when 125 Pt-Co  units of color was
in the effluent from that unit.  This suggests that the amount of  color  pre-
sent may well be secondary to what dyes or other chromophoric compounds  con-
stitute the color.  Polyester scavenged no color in sample  D when  the pilot
plant water contained only 25 Pt-Co units of color.  However, when effluent
color was Increased to 125 Pt-Co units, a noticeable lessening of  whiteness
was recorded which indicated that some color had indeed been scavenged by  the
polyester.
     It was significant that the amount of color for the two runs, through  only
the MPP unit, was only slightly different in the Influent,  but drastically.dif-
ferent in the effluent.  This is attributed to more water soluble  dyes present
in the first run which were not coagulated and removed.  The pilot plant run
on 1/14/76 (See Table 46) was made without alum.  Color reduction  1n the MPP

                                      115
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pilot coagulation/sett!ing/filtration unit apparently resulted from physical
removal only because no chemicals were usecj.   However, the pilot plant run
made the following day was made with greater than 250 mg/1 alum as the primary
coagulant.  This obviously had a very significant effect in that color was re-
duced by eighty-four percent.  The fact that the average Pt-Co units of color
varied from 400 units on one day to 300 units on the following day should be
noted.  Despite these differences, full scale wastewater treatment plant ef-
fluent for both these two days were measured at 150 Pt-Co units of color.  The
most logical explanation is that the mixture of dyes contributing to this color
were different on these two days.  These two experiments, shown in Table 46,
of by-passing the 5-column train in the pilot plant were considered sufficient
to confirm that advanced wastewater treatment beyond chemical  coagulation,
settling and filtration would be required to produce a pilot plant effluent
capable of being used in dyeing all fibers satisfactorily.


           TABLE 46.   COLOR REMOVAL -  COAGULATION/SETTLING/FILTRATION
	 . 	 .... - _,— , 	 	 ., ,. — 	 	 . 	 - ... 	 	 . - -
Full Scale Wastewater Treatment Plant
Date
1/14/76
1/15/76
Influent
400
300
Biologically Treated
Plus
Chlorination
200
175
Multimedia
Filter Final
Effluent
150
150
Pilot Plant
MPP Unit
Influent
150
150
Only
Effluent
125
25

LABORATORY TEST DYEINGS

     A large number of one-liter laboratory dyeings were made on nylon,
acetate, triacetate and polyester substrates, using many of the dyes listed
for that substrate in Table 47.  In order to obtain satisfactory dyeings 1n
a full range of shades including white and pastel shades, particularly on
nylon and triacetate fibers, it was necessary to provide an essentially color-
less treated wastewater for dyeing.  A higher color level could be tolerated
when dyeing polyester; however, care should be taken to keep this level of color
                                     116
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               TABLE 47.   LABORATORY DYE/FIBER TEST  COMBINATIONS
                Fibers

1.  Nylon 66, Antistatic Additive
2.  Nylon 6
3.  Secondary Acetate

4.  Triacetate
   *Secondary Acetate Only


5.  Polyester (Dacron T/56,
    T/92 Blend)
6.  Nylon T/66 (Automotive)
               Dyestuffs

  1.   Fluorescent  brighteners 191 & 59
  2.   Disperse Blue 3
  3.   Disperse Yellow  3
  4.   Disperse Red 91
  5.   Nylanthrene  Blue GLF
  6.   Nylanthrene  Yellow WGL
  7.   Nylanthrene  Red  ACD
  8.   Acid Blue 78
  9.   Acid Red 99
 10.   Acid Red 4
 11.   Acid Yellow  7
 12.   Direct Blue  86
 13.   Acid Red 52
 14.   Acid Red 289

  1.   Fluorescent  Brightener  135 and
      Leucophor SF
  2.   Disperse Blue 27
  3.   Disperse Blue 7
  4.   Disperse Red 91
  5.   Disperse Yellow  86
  6.   Disperse Red 117
  7.   Disperse Yellow  42
  8.   Disperse Blue 87
  9.   Disperse Yellow  82
*10.   Basic Red 15
*11.   Basic Blue 3

  1.   Fluorescent Brightener 135
  2.   Disperse Blue 56
  3.   Disperse Blue 87
  4.   Disperse Yellow 64
  5.   Eastman Poly Yellow 76T
  6.   Disperse Red 60
  7.   Disperse Red 4
  8.   Basic Blue 71
  9.   Basic Yellow 54
 10.   Basic Red 29

  1.   Acid Black 131
  2.   Acid Black 132
  3.   Acid Orange  80
  4.   Acid Yellow  129
  5.   Acid Red 213
  6.   Acid Red 263
  7.   Acid Green 40
  8.   Acid Blue 62
                                     117
-------
 low,  preferably  below  20  Pt-Co units.  The treated water should also have a
 very  low metal ion  content, preferably less than 0.1 mg/1 of any single metal.
      Laboratory  dyeings were made on 20-gram swatches of fabric in a total
 liquor  of one-liter for a 50:1 liquor to fabric weight ratio.  Preliminary dye-
 ings  were made using effluent from the pilot plant to determine whether water
 quality was sufficiently  good to consider larger scale dyeings.  The dyes and
 chemicals used were obtained from manufacturing plant stock and solutions were
 prepared according  to standard dye laboratory practices in accordance with man-
 ufacturer's and/or  seller's recommendations.   Laboratory tap water, taken from
 processing water used in  dyeing and finishing in the manufacturing plant, was
 used  for all chemical and dye stock solution preparations.
      These 20-gram  swatch dyeings, both control and exploratory, were all made
                                                   o      o
 on a  dye laboratory steam table at approximatly (99 C) 210 F for one hour,
 unless  otherwise specified.  This time included the approximately ten minutes
 required for the bath to reach the desired process temperature.  Swatches were
 rinsed  in laboratory tap water after dyeing.
     Chemicals used were selected to be compatible with the type of dye and
 fiber/fabric to be dyed.  Dispersed dyes were applied to acetate fiber/fabric
 with  the  use of 0.25 grams per liter of the sodium salt of ethylenediaminete-
 traacetic acid (EDTA) sequesterant, 0.2 grams oer liter of a blended anlonic/
 nonionic  scouring/dyeing assistant, and 1.0 gram per liter of monosodium
 phosphate to aid in scouring, without adversely affecting exhaustion or any
 color property.
     Disperse dyes were applied to nylon using 0.25 grams per liter of EDTA,
 0.2 grams per liter of a blended anionic/nonionic, scouring/dyeing assistant
 and 1.0  gram per liter of sodium tripolyphosphate to aid in scouring and to
 improve  levelling (uniform uptake by the fabric) of the dye.
     Neutral dyeing acid dyes were applied to nylon using 0.25 grams per liter
of an anionic dyeing assistant, with affinity for the fiber under acid condi-
 tions, 0.20 grams per liter of a very slightly cationic dyeing assistant with
some affinity for the anionic acid dye (this weak bond would be broken by time
and increasing temperature to allow the dye to attach Itself chemically to
                                     118
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cationic dye sites on the fiber);  1.0 gram per liter of monosodium phosphate
which gave a pH of approximately 6-6.5 to  promote  exhaustion of the dye at
                o      o
approximately 99 C (210 F).   No sequestering agent was used in making these
dyeings because any slight amount of hardness contributed by dye or chemical
would have a positive effect on dye exhaustion and the dyes used exhibited no
extreme metal sensitivity.  Experience has shown  that the amount of metal ions
normally present in the dyeing bath at this location has no serious effect on
the shade of the dyeing.
     Basic dyes, often referred to as cationic dyes because they are positively
charged, were applied in a strongly acid dyebath  at pH 3.0 - 3.5, 99 C  (210 F)
for one hour.  This dyebath  also contained three  grams per liter of a dye
carrier specific for exhaustion of this cationic  dye onto copolymer polyester,
while reducing the tendency to stain homopolymer  polyester.  In addition, six
grams per liter of sodium sulfate (Glauber's salt) was added to prevent degrada-
tion of the copolymer polyester in this particular fabric blend.  Basic dyes
                                                                         O
were applied to acetate at pH 5 using one gram per liter of carrier at  99 C
(210 F) for one hour.
     Premetallized dyes were applied to nylon using 0.4 grams  per liter of an
anionic levelling agent, 0.02 grams per liter of  copper  sulfate,  at pH  5-5.5
(using citric add for pH adjustment).  Dyeing was carried out for  1.5  hours
at 99 C (210 F).  In dyeing with premetalUzed dyes,  a  sequestering agent was
not used.  An excess of sequestering agent could  break  down  the dye to  metal
bond and destroy the high lightfastness of this group of dyes.
     Optical brighteners were applied to all fibers using  one  gram  per  liter of
monosodium phosphate plus 0.2 grams per liter of nonlonlc  surfactant  for one
hour at 99°C (210°F).
     Triacetate used in these dyeings was part of a tricot  fabric blend of 80%
triacetate/20% nylon.  The nylon was so placed 1n the construction  that 1t was
essentially hidden and had no significant effect on the final  dyed  shade.   Dye-
                           0      O
ings were carried out at 99 C (210 F) on the laboratory steam table using a
dyebath containing three grams per liter of a commercially available  carrier
(butyl benzoate is the active carrier Ingredient), 0.2  grams  per liter  of an
                                       119
-------
 anionic/nonionic  blended  surfactant/dyeing assistant at pH 4-4.5 (pH adjusted
 with  citric  acid).
      Dyeings were made on  polyester in a closed pressurized container, holding
 0.5 liters of  dyebath so  that the liquor to fabric weight ratio was 25:1 instead
 of 50:1 as in  other small  laboratory dyeings.  One-hour dyeings were done at
   o       o                   o           o
 110 C  (230 F); however, at a 3 C/minute (5 F/minute) rate of temperature rise
 and rate of cooling, the  time of actual dyeing was slightly longer than one
 hour.  The dyebaths contained three grams per liter of perchloroethylene car-
 rier,  0.3 grams per liter  of a fatty ester lubricating agent and 0.25 grams per
 liter  of sequesterant, at  pH 4.5-5 (pH adjusted with citric acid).
     Confirmatory dyeings  were made using a laboratory-size pressure beam dye-
 ing machine.  Approximately 400 grams of fabric (sixteen inches wide) was
 wrapped onto a perforated  stainless steel  cylinder and Inserted in the labora-
 tory dye machine.  Approximately eight liters of manufacturing process water
 per dyeing for control dyeings and water from the pilot plant effluent for
 evaluation dyeings were used to fill the machine.  Water was pumped into one
 end of the perforated cylinder, through the perforations, and out through the
 fabric wrapping; flow was  always in one direction, from the inside to the out-
 side.  The dyebath was charged with dyes and chemicals prepared as described
 previously for the small  laboratory swatch dyeings.  The rate of temperature
                        o               o
 rise was approximately 3 C per minute (5 F per minute) and was raised by steam
 heat exchange through tubes located in the bottom of the beam dye machine.
                                   o     o
 Rate of cooling was approximately 7 C (13 F) per minute because cooling was
 carried out by overflow cooling the dyebath by the slow addition of manufactur-
 ing process water.
                                  o      o
     The dyeing temperature was 99 C (210 F) for nylon, acetate and triacetate.
 For polyester dyeing, a stainless steel lid was bolted onto the top of the beam
                                             O      0
 dye machine and temperature was raised to  110 C (230 F).  The rate of tempera-
                                                                  o      o
 ture rise and cooling was  the same as for those dyeings made at 99 C (210 F).
Reasonably good correlation of shade was obtained between the ten or twenty gram
swatch, made in 0.5 or 1.0 liter of dyebath, with the 400 gram dyeing, made 1n
eight liters of water in  the pressure beam dyeing machine.
     The individual  laboratory dyeings for each dye/fiber combination were made
and compared in light and medium bright shades.  There was  no deleterious effect
                                     120
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on the color of the dyeings made from the highest quality  pilot plant effluent.
When the pilot plant effluent was essentially colorless, high  quality dyeings
were obtained.  Spectrophotometric evaluations confirmed the visual  ratings of
acceptability.  These instrumental readings were made using a  "Spectroscan"
spectrophotometer integrated into an Applied Color System, Inc. ACS-500 comput-
er system.

COLORFASTNESS OF FABRICS DYED USING PILOT PLANT TREATED WASTEWATER
     Based on these experiments, there was no detrimental  effect  on  colorfast-
ness to washing, sublimation, crocking (rubbing), perspiration, oxides of
Nitrogen fading, ozone fading, or lightfastness (carbon arc),  when dyeings were
made using essentially colorless pilot plant effluent for  dyeing. These
evaluations included tests made on selected dyeings of dispersed  dyes on
triacetate, basic (cationic) dyes on copolymer polyester,  acid dyes  on nylon,
a disperse blue dye on a design fabric made from a blend of both  homopolymer
and copolymer polyester, premetallized dyes on nylon, a direct blue  on nylon,
dispersed dyes on polyester, an optical brightener on polyester,  and a differ-
ent optical brightener on nylon.  The dyes used in this particular evaluation
with the exception of the direct dye on nylon, and a fluorescent disperse
yellow on copolymer polyester, were all expected to exhibit good colorfast-
ness.  There were no unexpected developments in this series of evaluations.

SUMMARY
     Laboratory dyeings were made using effluent from the  complete pilot treat-
ment plant each time the effluent quality was essentially  colorless.  Consequent-
ly, dyeings were made over a number of days and water from several  pilot runs
was used.  These variables, notwithstanding color of the swatches dyed  in pilot
plant effluent, matched the color on the control dyeings.   There was every in-
dication that similar satisfactory dyeings could have been made using full si zed
production equipment and that the dyed fabric would have been shipped as first
quality product.
     These laboratory dyeings confirmed that the pilot wastewater treatment plant,
operated in its entirety, did produce wastewater of sufficiently high quality

                                      121
-------
to be reused in dyeing fabrics of man-made fibers of nylon, acetate, triacetate
and polyester.  The dyeings made from this treated wastewater were equal 1n
quality, color, brightness and colorfastness to parallel dyeings made using con-
trol water from manufacturing process storage.
     Residual color in the wastewater normally discharged to a receiving stream
proved to be the most difficult parameter to remove, as had been anticipated.
A satisfactory treatment scheme was developed to remove this residual color and
with it almost all BOD5, COD, TOC, metals, suspended solids, etc. The system
was also capable of effectively removing TKN.  Wastewater was sufficiently treat-
ed to be reused in several dyeing processes as the vehicle for dyeing man-made
fiber fabrics satisfactorily.
                                     122
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                                 SECTION 9
     PRELIMINARY DESIGN OF A ONE MILLION GALLON PER DAY  TREATMENT  PLANT

     The application of pilot technology, as described in Section  7,  to  full-
scale operation was considered technically achievable.  Current economic con-
straints at this particular manufacturing location made a full-scale  advanced
wastewater treatment plant unattractive economically.   However, there are
those who may wish to apply this technology to produce water of reusable
quality in manufacturing.

WASTEWATER TREATMENT PLANT DESIGN FLOW SEQUENCE
     The preliminary design of a 1  MGD wastewater treatment plant has been pre-
pared to produce an effluent capable of being used as process water in a dye-
ing and finishing plant.  This wastewater treatment plant would include a nine
hundred gallon-per-mlnute reactor/clarifier with provision for the addition of
alum and polyelectrolyte coagulant aids.  The supernatant would be transferred
to a 50,000 gallon capacity clear well; heavy chemical sludge would be sent
to a holding basin for further treatment.  Transfer pumps would then transfer
up to 1,642 gpm from the clear well to three dual media filters, (anthracite
and sand), ten feet in diameter.  Table 48 and Figure 8 present the necessary
preliminary design data.  The dual media filters' function is  to remove coagulant.
     The net effluent flow of 1210 gpm from the dual  media filter would then
be treated by three nine-foot diameter activated carbon filters for color and
organic removals.  Three eight-foot diameter organic  traps would then receive
a net flow of one  thousand gallons per minute for additional organic removal.
Three cation exchangers, eight feet-six  Inches 1n diameter, would remove multl-
valent metals and  other  positively charged Ions such  as residual catlonlc dyes.
The one thousand gallons per minute effluent from the cation exchangers would
flow to a degasifier, functioning with a 2800 cfm air flow to  dislodge

                                      123
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             TABLE 48.   DESIGN DATA  FOR 1  MGD SCALE UP OF PILOT PLANT
REACTOR/
CLAR1FIER
EQUIPMENT (R/C)
No. of Units 1
Maximum Influent 900 Avg.
(GPM)
Mar.. Effluent/
Unit (GPH) 1642
Max. Effluent 164?
Media



Volume of Media/
Unit (Cu.Ft.)
Depth of Media
(Inches)
Diameter of
Column (Ft.)
Height of
Column (Ft. )
Chemical Feeds Alum
Polyelcctrolyte
Regeratlon or
Backwash
Reyonerant
1 Solution
Regenerant
Ibs. Rcyenerjnt/
Re yene ration
Backwash/HrqeniTfl-
tlon Waste GPD 5000*
DUAL MEDIA
FILTERS
(DMF)
3
1642

500
1000
Anthracite
.60-. 80 mra
Filter Sand
.45-. 60 mm
157
157
24
?4
10

6.0

-

Backwash
Only
-
-
-
30,000
ACTIVATED
CARBON
FILTERS
(GAC)
3
1210

500
1175
20 x 50
Mesh
Activated
Carbon
190

36

9

5.0

-

Backwash
Only
-
-
-
10,000
ORGANIC TRAP
(OT)
3
1000

500
1000
Dowex 11



175

4?

8

B.O

-

Backwash &
Regeneration
Nad
5*
525
40.000
CATION
EXCHANGER
(CE)
3
1000

333
1000
IR 120



434

92

R.5

14.5

-

Backwash &
Regeneration
A & B
H2S04
(A)2. (B)4
2170
75,000
ANION
AERATOR W/CLEARWELL EXCHANGER
(AC) (AE)
1 3
1000 1000

1000 350
1000 700
IR 47



245

60

8

9.75

__ —

Backwash &
Regeneration
Sodium
Carbonate
3t
1225
75.000
Simla.)' wasting r«itr
                                        124
-------
ro
in
                                  Figure 8.  Process  flow  schematic  - I mgd  plant.
-------
entrapped CC^.  Transfer pumps would then pump 1000 gallons per minute from
the degasifier clear well to three anion exchangers eight feet in diameter.
The anion exchange resins would remove excessive nutrient anions and any re-
maining, soluble, anion-charged residual color bodies.  The above system would
produce a net flow of approximately 700 gallons per minute, or 1,000,000 gallons
per day.
     The cost of the construction materials and equipment for the 1,000,000
gallon per day treatment plant is estimated to be approximately $1,500,000.
The construction and installation cost was estimated at $1,500,000 for a total
cost of $3,000,000.  The land area needed for this project was estimated to be
approximately 3.5 acres including the lagoon.
     The major difficulty with the preliminary design would be the handling of
the wastewater from the regeneration of various unit processes.  The reactor/
clarifier would generate 5000 gallons per day of sludge which could be diverted
to an existing digester or concentrator, provided the existing facility was
adequate in size.  The dual  media filters would generate up to 30,000 gallons
per day of wastewater from backwashes which could be diverted to the equaliza-
tion lagoon of the existing wastewater treatment plant provided plant hydraulic
flow through the existing equipment would permit such a flow routing.  The
effect of the existing system would have to be carefully evaluated prior to re-
routing this flow.  The nature of this wastewater and the 10,000 gallons per
day from the activated carbon filters would probably be such that 1t would be
advantageous to discharge it in to an equalization lagoon prior to any treat-
ment.   The 40,000 gallons per day of regeneration waste from the organic trap,
the 75,000 gallons per day each from the cation and anion exchangers; would
generate 190,000 gallons per day that would require separate disposal.  The
possibilities of handling this regeneration wastewater with evaporators or
reverse osmosis are solutions to this disposal problem.  The effluent from a
reverse osmosis system treating the regeneration wastewater could be diverted
back to the one million gallon per day treatment plant.  Evaporators alone or
a reverse osmosis system would be expensive to install and operate.  The fur-
ther treatment of the regenerant must be evaluated, on a site-specific basis,
for both technical and economic feasibility.  Cost estimates for treating the
regenerant wastewater were not made.  Another Important consideration with this
                                      126
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type of wastewater treatment system 1s  the  land  area  required for Installation.
This consideration of land requirements/availability  is  site-specific and must
be evaluated on a case by case basis.
                                       127
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                                 TECHNICAL REPORT DATA
                          (Please read Instructions on the reverse before completing)
 i. REPORT NO.
  EPA-600/2-78-079
                            2.
                                                       3. RECIPIENT'S ACCESSION" NO.
 4. TITLE AND SUBTITLE
 Physical/Chemical Treatment of Textile Finishing
 Wastewater for Process Reuse
                                 5. REPORT DATE
                                  April 1978
                                 6. PERFORMING ORGANIZATION CODE
 7. AUTHOR(S)
                                                       8. PERFORMING ORGANIZATION REPORT NO.
 J.M. Eaddy, Jr. and J.W. Vann
 9. PERFORMING ORGANIZATION NAME AND ADDRESS
 J. P. Stevens and Company
 P.O.  Box 21247
 Greensboro, North Carolina  27420
                                 10. PROGRAM ELEMENT NO.
                                 1B2036; ROAP 21AEC-02
                                 11. CONTRACT/GRANT NO.

                                 Grant S801211
 12. SPONSORING AGENCY NAME AND ADDRESS
 EPA, Office of Research and Development
 Industrial Environmental Research Laboratory
 Research Triangle Park, NC  27711
                                                       13. TYPE OF REPORT AND PE
                                                       Final; 3/73 - 2/78
                                                                       PERIOD COVERED
                                 14. SPONSORING AGENCY CODE
                                  EPA/600/13
 is. SUPPLEMENTARY NOTES T£RL-RTP project officer is Max Samfield, Mail Drop 62, 919/
 541-2547.
 16. ABSTRACT Tne report des cr ibes & demonstration of multimedia filtration as an effec-
 tive tertiary treatment for biologically treated textile wastewaters from two adjacent
 plants involved in dyeing and finishing fabrics of man-made fibers. Adding alum,
 polyelectrolytes, and powdered activated carbon to the treated wastewater, just
 ahead of multimedia filtration, reduced criteria pollutants and produced effluent
 meeting NPDES requirements. Treated wastewater was further treated to provide
 colorless effluent satisfactory for reuse in dyeing man-made fibers in a pilot plant
 consisting of a  coagulation/sattling/flltration unit followed by a five-column train
 comprised of a sand filter,  organic scavenging resin, granular  activated carbon,
 and cation and anion exchange resins. This water was satisfactory for dyeing a full
 range of shades , including white and pastel colors on man-made fiber fabrics.  Color
 fastness was equivalent to that of standard control dyeings.  Tramp color scavenging
 ability of different man-made fibers was found to be quite variable.  Essentially
 colorless effluent is required for reuse in dyeing white or pastel shades on nylon
 and triacetate fabrics. Although technical feasibility of further treating biologically
 treated  effluent to permit its use in critical dyeing and finishing operations was
 demonstrated,  the economics of commercial application are not attractive.
 7.
                             KEY WORDS AND DOCUMENT ANALYSIS
                 DESCRIPTORS
                    b.IDENTIFIERS/OPEN ENDED TERMS
                         c. COS AT I Field/Group
 Pollution
 Textile Industry
 Textile Finishing
 Dyeing
 Waste Water
 Water Treatment
Filtration
Manmade Fibers
Decoloring
Coagulation
Settling
Pollution Control
Stationary Sources
Biological Treatment
13 B
11E
13H
07D
 9. DISTRIBUTION STATEMENT

 Unlimited
                    19. SECURITY CLASS (This Report}
                     Unclassified
                         21. NO. OF PAGES
                            138
                    20. SECURITY CLASS (Tillspage)
                     Unclassified
                                             22. PRICE
EPA Form 2220-1 (9-73)
                  128
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