EPA 600/2-76 060
March 1976
Environmental Protection Technology Series
               HYPERFILTRATION  FOR  RENOVATION OF
             TEXTILE  FINISHING PLANT  WASTEWATER


                                    Industrial Environmental Research Laboratory
                                         Office of Research and Development
                                        U.S. Environmental Protection Agency
                                   Research Triangle Park, North Carolina 27711

-------
                RESEARCH REPORTING SERIES '

 Research reports of the Office of Research and Development, U.S. Environmental
 Protection Agency, have been grouped into five series. These five broad
 categories were established to facilitate further development and application of
 environmental technology. Elimination of traditional grouping was consciously
 planned to foster technology transfer and a maximum interface in related fields
 The five series are:

      1.   Environmental Health Effects Research
      2.   Environmental Protection Technology
      3.   Ecological Research
      4.   Environmental Monitoring
      5.   Socioeconomic Environmental Studies

 This report  has been assigned to the ENVIRONMENTAL PROTECTION
 TECHNOLOGY series. This series describes research performed to develop and
 demonstrate instrumentation, equipment, and methodology to repairer prevent
 environmental degradation from point and non-point sources of pollution. This
 work provides  the new or improved technology required for the control and
 treatment of pollution sources to meet environmental quality standards.


                     E PA REVIEW NOTICE


 This report has been reviewed by the U.S. Environmental
 Protection Agency, and approved  for publication.  Approval
 does not signify that the contents necessarily reflect the
 views and policy of the Agency,  nor does mention of trade
 names or  commercial products  constitute endorsement or
 recommendation for use.
This Document is available to the public through the National Technical Informa-
tion Service. Springfield, Virginia 22161.

-------
                           EPA-600/2-76-060
                           March 1976
     HYPERFILTRATION FOR RENOVATION OF

     TEXTILE  FINISHING PLANT WASTEWATER
                     by

    Craig  A.  Brandon  and John J.  Porter
            LaFrance  Industries
         Riegel  Textile  Corporation
      LaFrance,  South  Carolina   29656
             Grant  No.  S800929
             ROAP No. 21AZT-006
         Program Element  No.  1BB036
   EPA Project Officer:  Thomas  N. Sargent

Industrial  Environmental  Research Laboratory
  Office of Energy,  Minerals, and Industry
      Research Triangle  Park, NC  27711
                Prepared  for


    U.S.  ENVIRONMENTAL  PROTECTION AGENCY
     Office of Research and Development
           Washington,  DC 20460

-------
                                CONTENTS

 Sections

 I         Conclusions

 II        Reconraendations

 III       Suitmary

           In-Plant Water Reuse
                                                                     6
            Equipment Performance                                     5
            Summary of P~

  IV        Introduction
           Sumtiary of Plant Costs Projections                        9


                                                                     11
                                                                     14
          Objective  and Scope
          Program Plan

V         La France  Plant Facility

          Fibers and Chemicals Used                                 14
          Wastewater Characterization                               16

VI        Reuse in Production Dyeings                               27

                    j -- — --y — •*- •^-"— ~ •- ->j • v»
          Reuse of Concentrate Water                                29
           Standard Dyeing Procedure                                 29
           Reuse of Concentrate Water
           Reuse of Product Water                                    33
                                                                    36
 VII       Equipment Performance

           Pilot Plant                                               3_
           Tubular Cellulose Acetate (Westinghouse)                   39
           Hollow Polyamide Fiber (DuPont)                            44
           Spiral-Wound Cellulose Acetate (Gulf)                      51
           Dynamic Zr(IV)-Polyacrylic Acid  (Selas)                    54
           Design Values for Cost Projections                        58

VIII       Treatment  Plant  Cost Projections                           61

           The Treatment System
           Equipnent  Description and Capital  Cost Projections         63
           Operating  Cost Projections                                 75
          Cost Projections for a Combined Menbrane System            79

IX        References
                                                                     82
                                 111

-------
                         CONTENTS  (continued)

Sections

X         Appendix A - Water Sampling Schedule, Procedure,
          and Chemical Analyses                                     83

          Sampling Schedule                                         84
          Collection and Storage of Samples                         84
          Analytical Procedures                                     85

XT        Appendix B - Production Scale Reuse Dyeings               89

          Cycle #1                                                  91
          Cycle #2                                                  95
          Cycle #3                                                  98
          Cycle #4                                ,                  100
          Cycle #5                                                  102
          Cycle #6                                                  104
          Cycle #7                                                  107
          Cycle #8                                                  109
          Cycle #9                                                  111
          Cycle #10                                               '  113
          Cycle #12                                                 115
          Cycle #14                                                 117
          Cycle #16                                                 119

XII       Appendix C - Performance of Hyperfiltration Modules
          in the La France Pilot Plant                              121
                                 IV

-------
                                 FIGURES

 No.


  1   BCD of the conposite wastewater                                17

  2   COD of the conposite wastewater                                18

  3   Dissolved solids content of the composite wastewater           19

  4   Calcium concentrations  of the conposite wastewater   '           20

  5   pH of the conposite wastewater                                 21

  6   Color content of the conposite wastewater                      22

  7   Turbidity of  the conposite wastewater                           23

  8   Schematic of  pilot  plant layout                                38

  9   Operating performance of Westinghouse nodule at La France       41

 10   Cperating evaluation of  Westinghouse module during final
      500 hours                                                      46


 11   Cperating performance of DuPont hollow polyamide fiber
      module at La France                                             49


 12    Cperating performance of Gulf  (U.O.P.) spiral cellulose
      acetate module at La  France                                     53


 13   Cperating performance of Selas dynamic membrane module
     at La France                                                    57


14   Simplified flow schematic of a textile dyewaste treat-
     ment system                                                    52

15   Case 1 - Details of a membrane bank design                     66
                                  v

-------
                                 TABLES

 No.                                                                Page

  1   Sunmary of performance of hyperfiltration modules in
      La France demonstration pilot plant                            7

  2   Summary of cost estimates for treatment of 7570 ra3/d
      of textile wastes at La France                                 10

  3   Comparison of hyperfiltration module configurations            13

  4   La France size characteristics                                 15

  5   Character!sties of raw composite wastewater during the
      operation of the pilot project (March 1973 to May 1974)         24

  6   Characteristics of process (tap water)  water currently
      used in the La France plant                                    26

  7   Production dyeings                                             28

  8   Standard dyeing cycle                                          29

  9   Reuse dyeings of cotton velour with concentrate water           30

 10   Analyses of concentrated residues employed in reuse dyeing      32

 11   Critical test dyeing  formulation                               33

 12   Analyses of product water                                      35

 13   Operating performance  of tubular cellulose acetate  West-
      inghouse module with La France  composite wastewater            43

 14    Operating performance  of tubular cellulose acetate  Vfest-
      inghouse module with La France  composite wastewater
      under variable conditions                                       45

 15   Operating performance of hollow polyamide  fiber DuPont
     module with La France dyehouse wastewater                       48

16   Operating performance of spiral cellulose  acetate Gulf
     module with La France wastewater                               52

17   Operating performance of ceramic tube Zr(IV)-PAA Selas
     module with La France wastewater                               56

18   Design values for cost projections                             59

-------
                         TABLES  (continued)

No.                                                               Page

19   Membrane module capital cost basis for projections             64

20   Details of capital cost projections for  hyperfiltration
     module unit                                                    68

21   Details of capital cost projections for  pretreatment
     unit                                                           71

22   Capital cost projection sumnary for hyperfiltration
     treatment of La France wastewater                              74

23   Operating cost projections sumnary for hyperfiltration
     treatment of La France wastewater                              76

24   Net operating cost projections summary including
     potential recycle credits                                      78
                                 vn

-------
                             A^KNOWLEEGEMENTS

           project of this scope obviously is indebted for its success
  to contributions of more than one or two individuals.  Therefore, Dr.
  C. A. Brandon and Dr. J. j. Porter, consultants to the Riegel Textile
  Corporation as project director, and principle expert on reuse evalua-
  tions, respectively, acknowledge the following people.
       The Texidyne pilot plant operators under the guidance of Dr. Ali
  El-Nashar, namely, Mr.  Bob Adler, Mr.  Charles Shuler, and Mr. Eric
  Snider have contributed significantly to the large degree of on-stream
  time for the pilot plant.   The La France personnel including the  plant
  engineers, Henry McAdory and  Ton Foy,  and foreman,  John Byrura,  have been
  largely responsible for the expeditious assembling of the pilot plant
  equipment and the maintenance thereof.   Mr.  Charles Smith and Mr.  Bernard
  Thompson have cooperated to achieve and evaluate  the  full scale reuse
  test dyeings.
      Several  people  less directly involved in the day-to-day  operations
  have, however, made  significant contributions, and  are due acknowledgement
  and thanks for the consultations:  Dr. R. L. Goldsmith and Mr. Sorab
 Hassain of ABCOR contributed to this report and to  the progress and
 success of the pilot plant operations with their continued surveillance
 and advice.  We also acknowledge the contributions of Dr. J. s. Johnson
' and Dr. R. E. Minturn of the Oak Ridge National Laboratory, along with
 the efforts of Mr. George V. Jordan and Mr. George L.  Bartholomew, of
 Selas Corporation, for their on-going efforts in planning, testing, and
 preparation for  the second  phase of the pilot plant project.  The  guidance
 and direction of Mr.  T.  N.  Sargent,  EPA Project Officer, was most  valuable
during  the course of this study.
                                  Vlll

-------
                               SECTION I
                              CONCLUSIONS

     Hyperfiltration  (reverse osmosis) has been studied, on a pilot
plant scale, for renovation of the composite wastewater from the textile
dyeing and finishing plant of La France Industries.  Both the purified
product water and the residual concentrate were used in full scale pro-
duction dyeings in a two-piece dye beck.  The results of this study were
presented in three categories; direct reuse, equipment performance, and
cost projections.  The conclusions based on the reuse evaluation results
are:
      (1)  The quality of the product water, purified by passing through a
hyperfiltration membrane, was satisfactory for direct reuse in all dyeing
and finishing operations at La France.
      (2)  The technical feasibility of the reuse of the concentrate water,
retained by the hyperfiltration membrane, was demonstrated by the production
of first quality fabric in nine standard shades.
     The conclusion drawn from the equipment performance results is:
      (3)  The four commercial membrane module configurations evaluated in
the pilot plant were each capable of processing textile wastewater, when
operated with proper pretreatment.
     The conclusion that attains from the results of cost projections iss
      (4)  The cost projections for a full scale 2,000,000 gallons/day
(7570 m3/day) treatment facility combining two of the commercial membranes
indicated a capital cost of $1,650,000, and a net operating saving of
43C/1000 gallons (11.3
-------
                               SECTION II
                            HECOM4ENDMTICNS

      The result of this investigation demonstrated the feasibility of
 hyperfiltration  (reverse osmosis) membranes for the renovation of
 composite textile dyeing and finishing wastewater at La France Industries.
 The scope of the study was limited to the evaluation of performance of
 commercial membranes under manufacturer specifications.  It was beyond
 the scope of this pilot plant investigation to determine optimum pretreat-
 ment for textile wastewater.  Further, this study was limited to the con-
 sideration of plant composite wastewater and the total mixed dyehouse
 effluent.  The following are recommendations directed toward the optimum
 utilization of membrane separations for the economic renovation of textile
 wastewater effluents, including direct recycle of single process effluents,
 waste treatment of any required system blow down, and modifications of the
 manufacturing process that may become economical because of recycling.
      (1)   The textile wet finishing industry employs a variety of process-
 es that each have peculiar waste characteristics. A mobile hyperfiltration
 laboratory project is recommended to  (a)   determine the engineering per-
 formance of available hyperfiltration equipment,  and  (b)   to evaluate
 potential for reuse at several plants selected to represent the major
 categories of dyeing and finishing.   A part of this  program should be the
 study of  the treatability of the concentrate since complete reuse may not
 prove to be universally practical in the immediate future.
    ' The favorable economics  implied for a  combined membrane system suggest
 the second  and  third  recontnendations.
      (2)  Basically hyperfiltration  is a separation process.   The  objective
of the application of hyperfiltration is direct recycle, both of the  chemi-
cals in the concentrate and of the product water.  It may be more  efficient
in many manufacturing processes to make the application of membranes  to
individual effluents, rather than to a mixed composite.  This  is particular-
ly true for the conservation of energy through direct recycle  of hot water.
     It is recommended that a study be made of the application of membranes

-------
 to the individual effluents of manufacturing processes.   In particular,
 this study should examine in detail both batch and continuous operations
 in order to assess the potential inpact of energy conservation,  through
 recycle of hot process water and the reuse of reconcentrated chemical
 baths, upon the textile industry.
      Since the potential for economic recovery,  for certain processes
 where significant energy and chemical savings are possible, the  accept-
 ability of membrane separation technology for point source application
 is enhanced.  The recovery of any process chemical by direct recycle  will
 also obviously reduce the pollutional load in the remaining composite
 wastewater.
      Because the economics are potentially conducive to  early adoption
 by industry, and because the removal of expensive chemicals and  energy
 by direct recycle achieve a significant reduction in the pollutional  load
 (often of the more refractive constituents,  e.g., PVA and vat dyes),  it
 is further recommended that as a second phase of the study of point source
 recycle be a full scale demonstration.   The full scale demonstration
 should involve closed cycle operation of a manufacturing process.   Closed
 cycle will provide a necessary demonstration of  the effects of recycle on
 the manufacturing process.   In addition, it will permit  the full scale
 evaluation of process modification.
      (3)   As the full scale demonstration of membrane separation for
 point source recycle is a second phase  of an assessment  study, the  full
 scale demonstration of the renovation of composite wastewater is recommend-
 ed as a second phase of this pilot plant project and the mobile  hyper-
 filtration laboratory project recommended above.   Closed cycle operation
would provide  information on  (a)  the equipment performance over an ex-
 tended period,   (b)  the  change  in process water composition, and   (c)  the
treatment  of any blow down required.  A  full  scale membrane system would
 also provide a useful test bed for the study  of pretreatment to minimize
the total cost of the treatment  system.
     The demonstration of the renovation of composite wastewater would be
beneficial because there are a number of instances in which this could be

-------
a useful intermin step to full scale totally closed cycle.  For example,
in a few cases, water availability and costs (supply and treatment)  are
such that recycle is a viable alternative to minicipal systems.  Further
full scale demonstration of the renovation of composite wastewater would
not be redundant in that application of point source recycle would only
tend to optimize the performance of the integrated system and to maximize
the rate of return from recycle.
     Since the cost of the membrane modules is the significant factor in
determination of the economic practicality of this separation technology,
the following recommendations relate to improvenent in the equipment
performance with textile wastes.
      (4)  Development of washing procedures to prevent flux decline, i.e.,
fouling, or to restore flux periodically.  Costs potentially may be
reduced up to 50%.
      (5)  Development of pretreatment to reduce membrane fouling in
order to both increase average flux and prolong membrane useful lifetime.
      (6)  Development of membranes tailored to the separation of the
specific chemicals, e.g., for use with process solvents other than water.
      (7)  Development of membrane modules designs and determination of
fluid dynamics to minimize horsepower requirements.
      (8)  Evaluation of the potential for the chemical recovery from
concentrate as a raw material for a chemical process.

-------
                                SECTION  III
                                 SUMMARY

       This report describes  the results of the hyperfiltration  (reverse
  osmosis)  demonstration pilot plant at  La France Industries which was in
  operation during 1973-74.   Both the purified product water and the con-
  centrate  water representing 65 - 95% water recovery have been recycled
  successfully in  full scale  test dyeings during the period of operation
  of this program.

  IN-PLANT WATER REUSE
     This pilot study was conducted to demonstrate the feasibility of re-
 use of treated textile wastewater in plant (full)  scale dyeing operations.
 This method of treatment was hyperfiltration which yields a relatively
 pure fraction of water, referred to as product water, and an impure
 fraction containing most of the dyes and chemicals, referred to as con-
 centrate water.
     Sixteen different treatment cycles were performed during the course
 of the project.   Thirteen of these  cycles used the treated water in plant
 scale dyeing operations.   Three cycles were devoted entirely to equipment
 performance determinations.  The product water was used in five dyeing
 operations with standard  dye formulations.  The product water was  used
 with  the concentrate in five dyeing operations.  Eight plant scale dyeings
 were made  in which the  concentrate was  used as. the initial dye bath with
 normal plant water used for  all other process steps.  A total of eighteen
 plant  scale dyeings were  performed.  A  total of eleven  different dye
 formulations evaluated  the success of using the product water and con-
 centrate water for plant  scale  dyeings.
    All of  the plant dyeings were successful.  No significant problems were
encountered with the reuse of product or concentrate water.  The light fast-
ness wash tests performed on the fabric, as a quality control measure,
established that the test dyeings were equal to normal production quality.

-------
      Test dyeings were  conducted in the  laboratory before  plant scale dye
 formulations were chosen.   The product water required no additional
 treatment and  could be  used interchangeably with plant water.   Concen-
 trate water sanples frcm each cycle contained concentrations of different
 dyes.  The dye formulation chosen for use with the concentrate  water re-
 quired  minor additions  of  dye when the concentrate water contained
 cotpatible colors and major additions of dye when  the recovered dye  was
 different. This results in dye  savings  in  seme cases and  an increase in
 dye requirements in other  cases.   The average reduction  of dyes was  16%.
                                             i
 EQUIPMENT PERFORMANCE
      Three types of hyperfiltration membranes were evaluated during  the
 course  of this demonstration pilot plant; polyamide,  cellulose  acetate,
 and Zr(IV)-polyacrylic  acid.  Cellulose  acetate was evaluated in two
 membrane configurations.   A total of four basic commercial module  con-
 figurations were therefore investigated.  These were:
      (1)   Tubular cellulose acetate on the  internal wall of 13  nm  diameter
 tubular channels,
      (2)   hollow-fine polyamide  fibers,
      (3)   spiral-wound  sheets of cellulose  acetate, and
      (4)   external  coating of Zr(IV)-PAA dynamically  deposited  on  ceramic
 tube bundles.
      The operation  of these units is summarized in Table 1.
      A  single  Westinghouse tubular cellulose acetate  module was operated
 for over 1000  hours.  Pretreatment employing 25 micron cartridge filters
was enployed.   The  pH was  maintained in  the range  5.2 -  7.0, and the
temperature controlled  below 90 F (32 C), as recoranended by the manu-
facturer.  The average  rejections of COD, total solids,  conductivity, and
color range from 92 - 99+%.   There was a decrease  in  product water flow
rate  from  the unit  with time of operation that was partially recoverable
by washing.

-------
  Table 1.  SUGARY OF PERFORMANCE OF HYPERFILTROTION MDDULES IN IA FRANCE DEMONSTRATION PILOT
MANUFACTURER
MEMBRANE
CONFIGURATION
TEST DATE
HOURS OF TEST
TEST CONDITIONS
Prefiltration
pH
Temperature, C
Pressure, Pa (x 10~6)
AVERAGE REJECTIONS, %
Total Solids
Color
Conductivity
COD
Westinghouse
Cellulose
Acetate
internal
tubular
12/73 - 1/74
1059

25 micron
cartridges
5.6 - 7.0
13 - 32
2.1 - 3.1

95
99+
92
96
DuPont
Polyaitu.de
hollow-fine
fiber
2/74 - 3/74
187

D.E.C
6.2 - 8.3
11 - 32
2.4

95
99+
94
92
Gulf13
Cellulose
Acetate
spiral-wound
4/74
804

25 micron
cartridges
5.8 - 7.0
15 - 26
2.8

96
99+
95
94
Selas Flotronics
Zr(IV)-PAA
externally coated
tube bundle
6/74 - 7/74
944

250 micron screen
6.6 - 8.5
20 - 91
2.4 - 7.2

90
98+
85
95
b Total plant composite and dyehouse wastewaters used in this
c Now ROGA, a Division of Universal Oil Products
  Diatonaceous earth - Sears swiitming pool filter - preceeded
study.

25 micron and 1 micron cartridge filters.

-------
     Three DuPont permeators employing the hollows-fine polyamide fibers
 were operated,  below 90 F (32 C),  for a total of about 600 hours.   After
 greater than 400 hours of operation on composite wastewater from the
 total plant, it was recommended by DuPont that further evaluations be
 made with wastewater from the dyehouse only,  excluding all sanitary and
 finishing wastewaters.  During the last 200 hours,  a diatomaoeous earth
 prefilter was used in addition to  the 25 micron and 1 micron cartridge
 prefliters which were used for the initial 400  hours.  The penreator
 evaluated during the last 200 hours, under these recommended conditions,
 performed satisfactorily.   The average rejection of COD,  total solids,
 conductivity, and color ranged from 92 - 99+%.   It  was possible to main-
 tain the product water flow rate from the module by intermittent deter-
 gent washing.
     The Gulf (now POGA, Division of Universal Oil Products)  spiral-wound
 cellulose acetate module was operated for 804 hours.   The pH was maintain-
 ed in the range 5.8 to 7.0,  and the temperature controlled below 90 F
 (32 C).  All wastewater was prefiltered through 25  micron cartridge filters,
 During the initial 163 hours an additional 1  micron cartridge filter was
 used in series  with the 25 micron  filter.  The average rejections of ODD,
 total solids, conductivity,  and color ranged  from 94 - 99+%.   There was
 an initial decrease in product water flow rate of the unit,  however,
 operation over  the last 600  hours  was at a stable rate.
     Two types of units containing  dynamic membranes were  used during the
 course  of this  pilot plant project.   Initially, dynamic membrane modules,
 prepared by consultants at the Oak Ridge National Laboratory, were used
 to generate sufficient product and concentrate  to demonstrate full scale
 reuse.   The performance of the ccmnercial modules provided by Selas is
 summarized in this  report.
    The  Selas dynamic membrane module contained eight,  19-tube bundles
 in  series.  The Zr(IV)-PAA membranes were deposited on these  ceramic tubes
 and then operated for 944 hours.   (This  period  included approximately 170
hours of operation with  rinse water from an indigo  dye  range.)
    The pH of the raw feed was  not adjusted.  The unit was operated with

                                   8

-------
  40 mesh prefiltration over a temperature range  fron 68  - 195 F  (20 -
  90 C).   The average rejections of conductivity, total solids, GOD, and
  color ranged from 85 - 98+%.   The product water flow rate from the unit
  decreased  sharply initially but achieved a stable rate.

  SUTWARY OF PLANT  COSTS PROJECTIONS
     The equipment performance  data were  used by each module vendor to
  prepare a  cost projection  for  a complete 2 million gallon per day
  (7570 m3/d) hyperfiltration wastewater plant for the La France facility.
 These projections  include pretreatmant costs for control  of pH, tempera-
  ture, and suspended solids, as required  for each membrane configuration.
 These estimates do not include reservoir storage facilities, or treatment
 of the 10 to 20 percent make-up water required in the plant.
     There is a wide variation in both the capital cost and the daily
 operating costs.  Major daily cost items for the polyami.de and cellulose
 acetate  membrane systems are membrane replacement and electrical power
 costs.  The major cost item for the dynamic membrane system is electrical
 power.
     The  capital cost and the operating power costs for each hyperfiltration
 plant are directly related  to the  number of module units required.  There-
 fore,  the pilot plant determinations of the product water flow rate from
 each module ware critical to meaningful cost estimate determinations.  A
 summary  of  cost estimates is given in Table 2.
     It is very important to note that these cost-data do not include the
 value  of recyclable water,  chemicals,  or  heat  (energy).   Using the esti-
 mated values of recycled materials and water as indicated in Table 2, the
 cost reduction for each  of  the  polyamide  and cellulose acetate membrane
 systems  is 57$/fegal  (15<=/m3).   Because of the possibility of direct re-
 cycle of  25% of the water at process temperature, the dynamic membrane
 system may have a cost reduction of as much as 69C/kgal  (32<:/m3).  A
 system combining two membrane types may have a cost reduction of as much
as 88.5CAgal  (23.4
-------
Table 2.  SUMMARY OF COST ESTIMATES FOR TREATMENT OF 7570 m3/d OF TEXTILE WASTES AT LA FRANCE
MEMBRANE CONFIGURATIONS
CAPITAL INVESTMENT, $
DAILY OPERATING COSTS, $/d
1. Pretreatment Chemicals
a. Filter Aid
b. Chemicals
2. Labor
a. Operating
b. Maintenance
c. Supervision
3. Maintenance Materials
4. Electric Power
5. Membrane Replacement
Total
DAILY OPERATING COSTS, C/ta3
RECYCLE POTENTIAL, C/fri3
1. Salt (80% recovery
@ 4.4<:/kg)
2. Water (80% recovery
@ 13
-------
                              SECTION IV
                             INTRODUCTION

     Increasingly stringent requirements for treatment of wastewfcter,
and significant surcharges which have been introduced by municipalities
require that we evaluate wastewater treatment systems which provide re-
cycle capabilities.  Hyperfiltration1/2 (reverse osmosis) is a technique
for economical renovation of industrial wastewaters which may yield
recovered chemicals, relatively pure product water, and energy where hot
water can be directly recycled in a process.
     Hyperfiltration is a membrane separation process that selectively
filters soluble and insoluble chemicals frcm water.  This technology has
been used successfully in selected industrial applications where the re-
covered products have significant value.  This study investigated the
application of hyperfiltration for the recovery of water and chemicals
from the wastewater of a textile plant.  The purified product water and
the concentrate water were directly recycled in full scale production
dyeings.
     The results from this study are in agreement with previous laboratory
tests of hollow-fine fiber permeators and dynamic membrane hyperfiltration
test sections.3  This deraonstration pilot plant was operated by La France
Industries, ^ Division of Riegel Textile Corporation, in cooperation with
participating equipment conpanies under an Environmental Protection Agency
grant.1*  The characteristics of the La France facility and wastewater
stream are summarized in this report.

OBJECTIVE AND SCOPE
     The primary objective of this pilot plant project was to demonstrate
the direct reuse of renovated textile wastewater in full scale production
dyeing equipment using standard procedures.  Additional  goals were to de-
monstrate the practicality of hyperfiltration equipment  and develop cost
estimates for a full scale plant.
                                   11

-------
       When a major portion of  the wastewater is  renovated and recycled  a
  blow down stream will ultimately be  required to prevent  chemicals  from
  accumulating  to intolerable levels in a closed  system.   The  composition
  and disposition of  such a blow down  were beyond the scope of this project.
       There are  several configurations of conrnercial hyperfiltration
  equipment.  The characteristics of the types  of systems  available are
  presented in Table  3.  The scope of  this project was to  demonstrate the
  performance of  each of these  conrnercial and prototype modules.2'5~7

  PROGRAM PLAN
       The  program plan included 16 monthly test cycles.   In thirteen cycles
  product water was used in plant scale dyeings.  Operation over 16 months
  permitted a complete study of the seasonal production variations in the
  mill.
       Before this project was started, tests were conducted on laboratory
  scale with hyperfiltration equipment to establish the feasibility of treat-
  ing the waste stream at La France.   Technical feasibility was indicated
 by these tests and the pilot plant was installed and full scale reuse
 tests were begun.
      The size of the pilot plant equipment was selected to permit the full
 scale operation in the dyeliouse of  a production dyeing beck,  with a capa-
 city of 92 meters of fabric.   The hyperfiltration unit was sized»to accumu-
 late, in each test cycle,  approximately 17  m3 of product water and 5.7m3
 of concentrate.   These volumes were sufficient to permit a full scale
 dyeing by standard procedures. The first week of each cycle  was devoted
 to the collection of this  purified water by the  processing of approximately
 22.7  m3 of raw wastewater  taken directly from the  corposite sewer main
 leaving the  plant.   During the latter stages  of  the project raw wastewater
 could be taken from  either the composite sewer or  the dyehouse drain.
     The original period of investigation for this grant  was  for 20 months.
The study began July 12, 1972,  the initial operation of the pilot plant
began on March 12, 1973, and was completed July  31, 1974.
                                   12

-------
Table 3.  COMPARISON OF HYPERFILTRATION MODULE CONFIGURATIONS
Membrane Material
Production Rate
m3 /fa3 /day
Method of Membrane
Replacement
High Pressure
Limitation
Particulates
in Feed
Permissible Feed
Range, pH
MaxLmun
Temperature, F (C)
Spiral
cellulose
acetate
67 - 1000

module
(on-site)
membrane
compaction

filtration
required

5.5 - 7.5

100 (38)
Tubular
cellulose
acetate
13 - 200

tubes
(on-site)
membrane
compaction

no problem

5.5 - 7.5

100 (38)
Hollow-Fine Fiber
polyamide
27 - 2000

module
(on-site)
fiber collapse

filtration
required

2-10

100 (38)
Dynamic
hydrous Zr(lV)
oxLde-polyacrylate
200 - 2000

in-situ
no problem

no problem

4-11

>195 (>90)

-------
                                SECTION V
                        LA FRANCE PLANT FACILITY

      The parameters describing the production capacity of the La France
 plant are shown in Table 4.   These data provide a basis for cortparison
 and evaluation of the results of this demonstration project.  These
 factors are inportant in the ultiinate estimation of the practicality of
 scale-up from the pilot plant.
      The process water is from La France's own filter plant.  Ninety-
 five percent of the 7570 m3  per day total water usage is in the dyehouse.
 Allowing for considerable evaporation by drying, the composite waste
 stream is at least 85% by volume dyehouse wastewater.  This is verified
 by the average total dissolved solids (TDS) measured in the composite
 waste.  The 7600 Ibs/day (3455 kg/d)  of salt  used are equivalent to
 500 mg/Jl of dissolved solids in the composite wastewater.
      The materials involved  in potential recycle with hyperfiltration are
 the water, the salt, and the unexhausted dyes.  In the case of membranes
 that can withstand high temperatures, energy  can also be recovered by
 direct recycle of renovated  hot water.  The economic potential for re-
 covery of salt, water, and energy is greater  than $1500/day.  A signifi-
 cant cost item is the $800/day cost for water treatment which may be
 reduced by recycling water.   An additional economic incentive is the
 recovery of dyes.   These potential savings will reduce the net cost of
 this type of waste treatment and may pay for  part or all of the operating
 cost.

FIBERS AND CHEMICALS USED
     The dyeing and  finishing processes  at La France involve several dif-
ferent dyes and finishes.  The dyeing is done in open-beck,  piece dyeing
machines.  The principal  classes  of dyes employed are neutral pre-metal-
lized, direct,  and acid dyes.  These  account  for about 95% of the total
dye usage.  Other dyes used in smaller quantity are  disperse,  basic,  and
                                  14

-------
    Table 4.  IA FRANCE PRODUCTION CAPACITY PARAMETERS
QUANTITIES USED

Materials :
Water  (total to plant) , m3/day                  7,197
                        (gallons/day)        (1,900,000)

Water  (to dyehouse) , m3/day                     6,818
                     (gallons/day)           (1,800,000)

Dyes, kg/day                                       225
      (pounds/day)                                 (500)

Cloth, m/day                                    20,000
       (yards/day)                              (22,000)

Salt, kg/day                                     3,454
      (pounds/day)                               (7,600)

Energy:

Fuel Oil  (for process steam),  joules/day    1.05 x 10 12
                              (Btu/day)       (1.0 x 10 9)

UNIT COSTS

Water, C/m3                                         13
       ($/1000 gallons)                           (0.50)

Fuel Oil, «/107  joules                            1.9
          ($/106  Btu)                             (2.06)

Salt,  
-------
 reactive dyes.  The finishes used include silicone, latex, wax dis-
 persions, fluoro-chemicals,  and flame retardants.  These finishes
 represent, at most, a few parts per million in the composite waste
 stream.
      The materials processed are nylon (30%), viscose (20%), and cotton
 (50%), with approximate weight percentages indicated.

 WASTEWATER CHARACTERIZATION
      The variety of dyes and finishes employed produce a complex and
 variable waste stream composition.   The quantitative characterization
 of the waste stream is important in evaluation of the pilot plant.
 Daily samples of the composite waste stream were collected at random
 times and ccmposited weekly  for analyses.   The results of typical analy-
 ses are tabulated in Table 5.   The  variation of several of the significant
 parameters is indicated in Figures  1 through 7.  The sampling and
 analytical procedures are shown in  Appendix A.
      As shown in Figure 1, the BOD  varied within the range 20 - 125 mg/2,
 with an average near 40 mg/Jl.   In Figure 2, approximately the same per-
 centage variation is indicated for  GOD,  from 125 - 900 mg/5,.   No simple
 correlation between BOD and  COD is  apparent frcm these data.   In Figure 3,
 the total dissolved solids average  1000  mg/£,  with a range from 600 - 1200
 mg/ji.   The calcium content,  Figure  4,  varies from 0.5 -  7.2 mg/£.  The
 pH,  an important parameter for selection of hyperfiltration equipment (see
 Table 3)  stays in the neutral  range, Figure 5, during most of this period;
 the maximum values about 8.  In some cases the pH was measured about 10;
 however,  this  level of pH was  noted only rarely and could be adjusted by
 equalization or chemical neutralization.
     The  color of  the waste  stream  shown in Figure 6  also varies widely.
 This was expected  and is  typical of dyehouse wastewater.   The turbidity
 shown in Figure  7  is attributable mostly to small fibers  from velvet
 fabrics sheared in the plant.
     Values of selected parameters were determined by  the  pilot plant
operators for each of the 600-gallon batches of raw feed collected for

                                  16

-------
140.
120.
   MARCH APRIL   MAY   JUNE
    1973
JULY AUGUST SEPT.  OCT.   NOV.  DEC.  JAN.   FEB.  MARCH APRIL  MAY
                                      1974
                         Figure 1.  BCD of the composite wastewater.

-------
      1000.
       80O,
00
      -6OO.
     O
     O
     U


       400
       20O
                                                     T:
            MARCH APRIL  MAY  JUNE  JULY AUGUST SEPT  OCT.  NOV.  DEC.   JAN.   FEB.  MARCH APRIL  MAY

             1973                                                          1974
                                 Figure 2.  COD of the cotposite wastewater.

-------
I20O.
    MARCH  APRIL   MAY  JUNE  JULY AUGUST SEPT  OCT.   NOV.   DEC.  JAN.  FEB.  MARCH APRIL  MAY
     1973                                                          ,974
            Figure 3.  Dissolved solids content of the conposite wastewater.

-------
MARCH  APRIL   MAY   JUNE  JULY  AUGUST SEPT  OCT.   NOV.   DEC.  JAN.  FEB. MARCH APRIL   MAY
 1973                                                           1974
           Figure 4.  Calcium concentrations of the composite wastewater.

-------













(

MARCH
1973





^

APRIL





0 QL
/\ 7^






*^





An
f 0o













^^






V




f

iy






I©«Q^-






^XSL























"- 	 ,






f*\

MAY JUNE JULY AUGUST SEPT. OCT. NOV. DEC. JAN. FEB. MARCH APNIL MAY
1974
Figure 5.  pH of the composite wastewater.

-------
       1500,
       1300.
to
to
     5
u


a
        IIOQ
       9OO.
       700.
       5OO
        300.
            MARCH APRIL  MAY   JUNE  JULY  AUGUST SEPT.  OCT.   NOV.   DEC.   JAN.   PER  MARCH APRIL  MAY
            1973                                                         1974
                           Figure 6.  Color content of the composite wastewater.

-------
      ISO.
NO
LJ
          MARCH APRIL MAT   JUNE  JULY  AUGUST SEPT.  OCT.   NOV.  DEC.   JAN.  FEB.  MARCH APRIL  MAY
                           Figure  7.  Turbidity of the composite wastewater.

-------
Table 5.  CHARACTERISTICS OF RAW COMPOSITE WASTEWATER DURING THE
          OPERATION OF THE PILOT PROJECT (March 1973 to May 1974)

COD, mgA
BOD, mgA
TOC, mgA
pH
Alkalinity/ mgA
Hardness, mgA
Total Solids, mgA
Volatile Solids, mgA
Dissolved Solids, mgA
Suspended Solids, mgA
Color (Pt-Co units)
Turbidity, F.T.U.
Conductivity (ymho/cm)
Metals
Calcium, mgA
Zinc, mgA
Magnesium, mgA
Chromium, mgA
Copper, mgA
Iron, mgA
Mercury, pg/&
Manganese, mgA
Sodium, mgA
Minimum
160
20
30
6.0
40
20
640
95
640
0
280
1.7
800

0.9
2.0
0.51
<0.1
0.04
0.2
0.46
<0.1
190
Maximum
880
125
168
7.6
90
80
1280
460
1195
135
1660
120
2160

2.9
6.0 ,
4.0
0.3
0.20
4.2
1.08
<0.1
440
Average
303
46
73
6.75
54
36
935
180
881
55
757
39.4
1290

1.4
3.8
2.9
<0.13
0.11
1.2
0.76
<0.1
290
                                24

-------
 processing by the hyperfiltration equipment.  The miniiuum, maximum, and
 average values of these parameters are presented in Table 5.
      Because of the batch-type operation of the dye becks, there are
 periods when the waste stream is predominately wash water and other
 times when spent dye solutions cause the waste to be relatively highly
 concentrated.   The sample selection for pilot plant use was randan and
 somewhat biased toward higher levels of contaminants and  color by the
 investigators'  desire to avoid dilute wastewater.   The treatment results
 are  felt to be  slightly conservative as wastewater characterization.
     A final variable not measured directly,  but of importance to all
 hyperfiltration except dynamic membranes, is  fluid temperature.   It
 was necessary to install a heat exchanger to  maintain process  temperature
 in the hyperfiltration unit in the safe operating  range,  less  than 90 F
 (32 c) for  the cellulose acetate and polyamide membranes  (see  Table 3).
     Samples of process water were  taken in the dyehouse  at the  tine of
the full scale reuse test dyeings.  The  chemical analyses were selected
to permit a direct comparison with the recycled water.  The results pf
the analyses of nine samples are summarized in Table 6.
                                 25

-------
      Table 6.   CHARACTERISTICS OF PROCESS (TAP WATER)  WATER CURRENTLY
                USED IN THE LA FRANCE PLANT

COD, mg/Jl
BOD, mg/Jl
TOC, mg/Jl
pH
Alkalinity, mg/Jl
Hardness, mg/Jl
Total Solids, mg/Jl
Volatile Solids, mg/Jl
Dissolved Solids, mg/Jl
Color (Pt-Co units)
Turbidity, F.T.U.
Conductivity (ymho/on)
Metals.
Calcium, mg/Jl
Zinc, mg/Jl
Magnesium, mg/&
Chromium, mg/Jl
Copper, rag/A
Iron, mg/A
Manganese, mg/Jl
Sodium, mg/Jl
Minimum
<1
0.2
1
5.8
12
9
45
10
45
2
0.15
60

1.0
0.07
0.40
<0.1
<0.04
<0.15
<0.05
5
Maximum
20
2
5
7.4
35
30
85
55
65
35
4.1
100

2.0
0.56
1.28
<0.1
0.04
1.2
0.11
10
Average3
9
0.8
4
6.7
22
16
61
26
56
11
1.1
75

1.32
0.24
1.02
<0.1
<0.04
0.90
_b
8
a This is the average of 9 separate samples  taken March  1973 to May  1974.
b There are too few data for manganese for a meaningful average.
                                 26

-------
                                 SECTION VI

                         REUSE IN PBDDUCTIOM DYEINGS
       The reuse dyeings were calried oufc in a ^.^ ^ fcl
  standard plant procedures.  Normally the dyeings were dons at the
  beginning of the third v«* of each of the ^nthly test cycles.   After
  the collection of 17 m3 of purified product water and 1.5  n,3 to 3.8 m3
  of residual concentrate was coated, ndxed samples  of each v^re taken
  for analyses,   rnese dyeings ware  conducted in the laboratory so  that
  production scale formulations  oould be developed.   The  production
  ayemg formula was then given  to the plant dyer who coveted the
  standard dyeing  procedure.
      Two types of pl^t dyeings ^ ^^^ ^ ^ ^ ^^
  (1   separate and independent dyeings employing only product water or
  only concentrate,  and   (2)  one dyeing coining both the concentrate
  -d Product water,  a. ^n^^^ was ^ ^ ^ ^^
  ^tronal dyes added as prescribed in the formation prepared in the
  laboratory.  The product water was  substituted for tap water in each
  step in the standard dyeing procedure.
      Eighteen separate production dyeings ware conducted with recycled
 product water arf/or concentrate in the period Ifcrch 1973 to July  1974
 These are listed  in Tab!e 7 by  cycle nu*er whi* refers to operating '
 psraods, see append* B.   me water recovery,  i.e.,  the  portion of the
 wastewater  recovered as purified product water, is  indicated for each
 test.  Also, the  performance of the nateanes  in terms of measured con-
          and color reactions is listed.  The higher rejections are
           of better c^ali^ product water and hence stronger concentrate.
         water recovery generally means lower quality product water ana
stronger concentrate.  Details of each production dyeing are given in
Appendix B.
                                   27

-------
                                         Table 7.  PRODUCTION DYEINGS
to
CO
Cycle
number3

1
2
3
4
5
6
7
8
9
10

12
14

16
Membrane
Type

Polyamide
Polyamide
Poly5ara.de
Polyamide
Polyamide
Polyamide
Zr(IV)-PAA
Zr(IV)-PAA
Zr(IV)-PAA
Cellulose
Acetate
Polyamide
Cellulose
Acetate
Zr(IV)-PAA
Type of Water Used,
for Plant Dyeings

Product & Concentrate
Product & Concentrate
Combined
Combined
Combined
Product & Concentrate
Concentrate
Concentrate
Product & Concentrate

Product & Concentrate
Combined

Combined
Concentrate
Water
Recovered
(%)
75
75
75
90
90
90
75
75
75

75
75

75
75
Conductivity
Rejection
M
90
90
90
90
82
75
85
65
72

92
95

95
88
Color
Rejections
<%>
98
98
99
99
98
86
99
98
99

99
99

99
99
       Cycles 11, 13, and 15 were equipment study cycles in which no water was saved for reuse dyeings.

       In some cycles, product and concentrate water were used separately in different dyeings and in

       seme cvcles thev were combined for a sinale dveina.
         —    »* -     —   - —		

seme cycles they were combined for a single dyeing.

-------
  STANDARD DYEING PROCEDURE

       The standard dyeing cycle involves the six-step procedure listed
  in Table 8.
                      Table 8.  STANDARD DYEING CYCLE
  Operation.


  Scouring
  Flush Bath
  Dyeing
  Adjust Ahade
  Flush Bath
  Dye Fixing Agent
Chemicals

Detergent

Dyes and Salt
Dyes
Water Used
   (m3)
    1.9
    1.9
    1.5

    2.3
Temperature
    (0
  50 - 82
     27
  50 - 93
     93
     27
     27
 REUSE OF CONCENTRATE WATER

      Two types of tests were run classified by the procedure for select-
 ing the shade to be dyed.   Routimly the procedure was to select a shade
 in the immediate production schedule and add whatever dyes were needed to
 match the shade.  Occasionally a shade was selected from the production
 catalog to be nearest that produced by the concentrate,  therefore requiring
 nammal amounts  of additional dyes.   The first type of dyeing illustrates
 the technical feasibility  of recycling the residue,  even if only occasion-
 ally the production schedule may permit  significant savings of dyes.  The
 second  type of dyeing indicates the optimum savings  of dyes in recycled
 concentrate.   Both  types result in effective recycle of the concentrate
 tod  thus avoid the  cost of waste treatment.  Successful production dyeings
were achieved  for both light and dark shades.
     All the dyeings with concentrate are listed in Table 9.  With a
single exception, 100% cotton velour fabric was used in the concentrate
                                  29

-------
                        Table 9.   REUSE DYEINGS OF COTTON VEDOUR WITH CONCENTRATE WATER
CO
o
Cycle
nurrber


1
2
3a,b
4b
5b
6
7
8C
1213
14b
16d
Weight of
Fabric (kg)


21.6
43.83
36.9
38.25
36.9
88.65
68.85
45.0
23.4
70.65
16.2
Shade


Tan
Blue-green
Light Blue
Rose
Violet
Tan
Rose
Blue-green
Burnt-orange
Gold
Green
Nurrber
Reuse
Test
3
2
1
3
2
3
3
2
3
4
3
of Dyes
Standard
Test
4
2
3
3
2
4
3
3
3
3
-
Amount of Dyes
(% of Fabric Weight)
Reuse
Test
0.412
10.48
0.055
0.233
0.130
0.305
0.310
0.485
1.450
0.990
0.235
Standard
Test
0.438
0.932
0.189
0.302
0.130
0.438
0.189
0.632
1.940
1.033
-
       Fabric conposition this test:  65% Cotton - 35% Rayon
       Product and concentrate water were used together.
       Results from Cycle #9 and #10 are incomplete.
       This shade is not a standard item.

-------
 reuse dyeings.  During Cycle #3, a 65% cotton - 35% rayon blend fabric
 was dyed.  Nine different standard shades were dyed.  The tan shade
 dyed in Cycle #1 was repeated in Cycle #6.  ihis was done to  (1)  show  '
 that the shade for the reuse dyeing could be selected independently of
 the conposition of the concentrate, and  (2)  provide a direct comparison
 of results achieved for 75% and 90% water recoveries.  In each case the
 finished product was graded as first quality.
      Dye formulations developed for the reuse tests generally were no
 nore conplex than the standards,  The number of dyes employed are in-
 dicated in Table 9 for each reuse test.   The amount of dye used  in the
 reuse tests are  listed with the standard for the shade.   The corrparison
 indicates a wide variation  in the dye savings.   In two cases,  Cycle #2
 and #7, more dye was required with the concentrate than in the standard
 formulae.   The average of the 10 comparisons is, however,  a 16 percent
 reduction in dye required to achieve  standard shades.
     A limitation of the reuse  of ^concentrated dye residues  is that
 they often yielded a dull grey  color.  Thus  a darker shade had to be  used
 so that the dullness would not  affect the color of the finished fabric.
 in the 11 test cycles, successful production dyeings were achieved  for'
both light and dark  shades, hoover.  The finished fabrics were generally
the equivalent to standards in crocking and  40-hour Fade-OMeter tests.
     The analyses of the concentrated used in the  reuse dyeings are given
in Table 10.
                                 31

-------
                   Table  10.  ANALYSES OF CONCENTRATED RESIDUES EMPLOYED IN REUSE DYEING
co
to
Constituent (mg/Jl)
COD
BOD
roc
pH
Alkalinity
Hardness
Total Solids
Volatile Solids
Dissolved Solids
Color (Pt-Co units)
Turbidity, F.T.U.
Metals
Calcium
Zinc
Magnesium
ChromLum
1
425
70
87
6.7
110
90
2360
200
2330
850
39

3.0
9.7
1.2
—
2
815
135
200
6.5
135
120
5570
450
5540
1250
31

-
-
-
<0.1
Cycle Number
3
455
60
110
7.0
110
80
2545
280
2480
1500
2

-
-
-
<0.1
4
580
102
165
7.2
160
90
3020
310
2985
1000
40

6.5
-
10.2
_
5
690
95
220
7.2
190
135
4425
405
4230
1200
30

9.0
8.5
13.8
0,1
6
435
10
-
7.4
140
130
3425
315
3435
1250
80

6.0
9.0
17.0
_
7
190
15
-
8.0
155
50
1580
165
1480
1300
8

1.0
2.4
4.5
_
8
415
45
-
7.5
115
55
2510
275
2450
1680
15

8.1
3.1
9.6
_
12
365
15
-
6.8
95
245
4320
245
4320
920
4

34.0
7.2
27.0
_
14
430
20
230
6.7
160
190
3025
275
3025
1100
35

7.5
3.0
15.0
0.6
16
255
55
100
9.0
250
130
3110
-
3055
190
18

15.5
1.8
12.0
_

-------
  REUSE OF PRODUCT WATER

       The purified product water was  used instead of tap water in each
  step of the standard dye procedure.  Two types of tests were run classi-
  fied by the use  of product water in  combination with the concentrate or
  with a standard  dye  formulation.  The use of the product water in the
  production  dyeing of a standard light shade, considered by the plant
  dyer to be  the most  difficult dye system in the plant, was expected to
  magnify any difficulties  in the recycle  of product water.  This critical
  dyeing,  done on  a 54% nylon - 46% viscose automotive upholstery fabric,
  contained the formulation given in Table 11.
              Table 11.  CRITICAL TEST DYEING FORMULATION
                Chemical          Dye Name
                Acid Dye          Nylon Fast Yellow FLW
                Acid Dye          ciba Brown 2GL
                Acid Dye          ciba Yellow 2BRL
                Acid Dye          Irgalan Black RBL
                Direct Dye        Lumicrease Grey 3LBN
                Direct Dye        Lumicrease Orange 3LG
                Direct Dye        Lunicrease Bordeau 3LR
This critical test of the reuse of product water was carried out four
times; Cycle #1, #6, #9, and #10.  This test was thus used for each type
of membrane and for each level of water recovery.  In each case, this pro-
duct water was used for all steps from scouring to final rinsing.  The shade
was obtained with no difficulty following routine procedures.  The finish-
ed fabric passed 100-hour Vfeather-O-Jfeter test for color fastness.
     In Cycle #2, product water was used to dye a yellow shade on a cotton
ribbed velour fabric.  The dyeing followed routine procedures with the
                                  33

-------
product water used in all steps.  The appearance of the finished fabric
was normal and crocking and light fastness were standard.  After
completing Cycle #2, it was apparent that the product water could be
substituted freely for normal tap water in this plant's production
dyeings.
     The analyses of the product water used in all reuse dyeings is
given in Table 12.  The average of a number of analyses of tap water,
collected at the time and at the place of the test dyeing is given for
conparison.  In general, the product water contains more solids than
the tap water, but has lower concentrations of metals.
                                  34

-------
                                   Table 12.  ANALYSES OF PRODUCT WATER
U)
tn
Constituent (mcr/ji)
COD
pnn
TCC
pH
AUcalinity
Hardness
Total Solids
Volatile Solids
Dissolved Solids
Color (Pt-Co units)
Turbidity (F.T.U.)
Metals
Calcium
Zinc
Magnesium
Chromium
Copper
Iron
Mercury (ugA)
Manganese
Sodium
1
25
10
3
6.1
10
30
100
30
100
30
2.4
0.5
<0.04
<0.01
0.04
0.3
™*
2
20
5
4
6.0
15
15
270
N.D.
270
20
0.5
0.1
<0.13
N.D.
<0.1
3
20
5
4
6.4
15
20
130
20
130
13
1.3
-
<0.4
0^56
_
4
15
4
4
6.5
15
5
280
40
280
6
0.8
0.24
0.28
-
94
Cycle Number
5
15
0.3
4
7.1
25
5
440
40
440
30
3.4
0.10
0.08
0.22
0.1

160
6
25
1
7.2
15
10
285
60
285
60
6.3
0.5
0.7
0.9
0.8
90
9
30
2.7
6.2
40
4
630
95
630
30
1.5
0.17
0.06
0.58
0.63
270
10
200
1.3
6.2
3
6
215
75
205
60
6
0.88
0.82
0.78
1.13
55
12
10
2
6.4
10
3
230
65
230
20
2.0
1.00
0.50
0.42
-
0.04
75
14
25
1
5
5.9
8
0.5
45
15
50
40
2.5
0.08
0.04
0.02
Oin
• -LU
0.04
0.14
0.03
15
Tap
Water
<4
0.6
6.7
27
19
67
36
59
13
1.11
1.45
0.07
0.96
<0.04
<0.68
<0.05
10

-------
                               SECTION VII
                          EQUIPMENT PERFORMANCE

      A major goal of the project was to demonstrate the practicality of
 hyperfiltration equipment in an actual plant-site evaluation.  This
 goal was accomplished by evaluating four commercial membrane modules in
 a pilot plant.  The layout and operation of the pilot plant are described
 prior to presentation of the performance data for each membrane module.
      Specific pretreatment of the wastewater feeds to the membrane
 modules, e.g., fine filtration, pH adjustment, and temperature control,
 was utilized as required by manufacturer specifications.  However, limited
 attention was given to the study of pretreatment, and certainly no opti-
 mization of pretreatnent for textile wastes was attempted.  Because of the
 strong influence of membrane flux on hyperfiltration treatment plant
 costs, the evaluation of means to minimize flux decline is important.
      Three membranes were evaluated;  polyamide, cellulose acetate, and
 Zr(IV)-polyacrylate.  Cellulose acetate was evaluated in two configurations,
 thus four commercial module configurations were evaluated:  (1)   tubular,
 cellulose acetate membranes on the internal wall of 13 ran diameter channels6,
 (2)   hollow-fine  polyamide fibers5,   (3)   spiral-wound sheets of cellulose
 acetate2,  and   (4)   external coatings of Zr(IV)-PAA dynamically deposited7
 on ceramic,  21 ran diameter tubes.  The  original program plan was to
 evaluate only the polyamide  and the Zr(IV)-polyacrylate membranes.   The
 project was  extended since the four configurations  represented basically
 all the commercially available configurations.
     The details operation performance of each membrane module evaluated
 is presented in this section.  The separation efficiency  (rejection per-
 centage) for the important parameters of oblor and  specific conductivity
 rejection and membrane flux are presented graphically for  the  entire
evaluation periods.  The detailed chemical analyses and percentage  re-
 jection for each measured species are presented in Appendix C.
                                  36

-------
 PILOT PLANT

      Figure 8 presents a schematic description of the pilot plant equip-
 ment.  The raw wastewater feed was introduced into the pilot plant either
 from the total plant operation downstream of a 150 m3 level-controlled
 mixing sump, or directly fron a dyehouse drain.  The dyehouse drain led
 fron only five (of 32) of the larger dye becks and was subject to wide
 variations in composition ranging from that of the spent dye liquor to
 that of comparatively clean wash water.
      The raw wastewater was introduced into 2.3 m3 elevated reservoirs
 through 40-mesh screen to remove participates, especially fibers.  In
 effect, the raw feed to the pilot plant was collected and processed as
 2.3 m3 batches.   Since the productivity and the capacity of the individual
 hyperfiltration modules was not constant, the number of batches processed
 per day varied.
      The hyperfiltration membrane modules evaluated were of two basic
 types.   The modules with pre-formed membranes (polyamide and cellulose
 acetate)  were evaluated in a low pressure,  up to 450 psi (3.1 x 106 Pa),
 system employing  a variety of prefilters, and temperature control (below
 38 C).   As  required for cellulose acetate membranes,  pH control was effect-
 ed by monitoring  and adjusting  each 2.3 m3  batch.   This system employed a
 5.6 kW motor with a centrifugal pump  (Gould BP3933).
     The ceramic  tube nodules (dynamic Zr(IV)-PAA membranes) were evaluated
 in a high pressure loop, up to  1000 psi (6.9 x 106  Pa),  employing a triplex
 positive  displacement Gaso pump with a 22 kW motor.   Since no  pretreatment
 was required, it was possible to  study the  effect of  prefiltration only by
 by-passing  feed fran the low pressure  system downstream of its pretreatment
 section.
     For evaluation of the pre-formed membranes, the  wastewater collected
 in  the 2.3 m3 elevated reservoirs was transferred by  gravity to a 0.2 m3
 pump suction reservoir.  Before entering  the membrane modules,  the waste-
water passed through a prefiltration unit, which contained  25 micron and
 1 micron cartridge filters in series.  When required, the wastewater could
also be directed through a 2.2 m2 diatonaceous earth  filter.

                                  37

-------
u>
oo
                   TOTAL PLANT OPERATIONS
                                DYE HOUSE


                                     BECK

                                     *I9
                                                  40Om3/d
7460 m Vd
                                          PILOT PLANT'
              18m3
               TORA
               TANK
        I	"
                             PRESSURE SEWER

PRO
\
J >,

Pre-formed-'''
R.0vx"
x- ^Membranes
pH Contr. | ^^
S| r~S~
Heat 1 T 'A
lExch. /'
nilf.^ ^CONCENTRATE
^ /fim 3
\
(STORAGE J Dynq
XTANK^/ PRODUCT Mem


i i
' 25 /<
Md
M
Kcscnvuino
r\~L '
1
A
Ho. f
j. 1 !
— •". |
J

|
jnk
brdnes^
i
^
j,

                              40 MESH
                              SCREENS
                              Figure 8.   Schanatic of pilot plant layout.

-------
       instrumentation was included to permit monitoring of flow rates,
  pressure,  and feed temperature.   Sampling ports were provided  to
  facilitate sample collection for monitoring module performance in
  terms of water quality and  concentration factors.
       The product  and concentrate from the hyperfiltration modules were
  collected  in stainless steel storage tanks.  Generally it was  necessary
  to collect fron 1.5  to 3.8 m3 of concentrate and from  9.5 to 17 m3 of
  product  water to  carry out a full scale production dye cycle in the
  standard t*o-piece beck.  The normal procedure was to  do  one reuse
  dyeing per month.  On  occasion,  two reuse dyeings were accomplished by
  using the product and  concentrate in separate full scale production dyeings.

 TUBULAR CELLULOSE ACETATE (Westinghouse)
      During the period from December 5,  1973,  to February 1, 1974,  a
 Westinghouse tubular, cellulose acetate membrane module (No. 4-291)  was
 operated on total plant composite wastewater for 1059  hours. The unit was
 used to process a total of 10.7 m3 of wastewater collected in four  batches.
 To simulate the operating conditions for  a full scale  treatment plant,
 the module  performance was monitored as the wastewater was concentrated
 to product  water recoveries  of 96%.   The  first two batches, a total of
 6.1 m3, were concentrated to an average recovery  of 72%.  The concentrate
 and product waters were collected and used in  a full scale dyeing  (Cycle  #10)
 Independently, the last two batches,  approximately 2.3  m3, each were con-
 centrated to 96% recovery.
     The  module evaluated was a tubular configuration having 0.86 m*  of
 cellulose acetate  membrane surface.   The tubular flow passages  consisted
 of  eighteen,  13 nm diameter channels  in a porous cylindrical block, a
 "sand  log", enclosed  in a 101 mm  diameter by 1.22 m long stainless steel
pressure vessel.   The fluid flews through each of these eighteen channels
in  series.
     Two operational modes were used.  The first was the concentration
mode.  In this mode, the product water from the module was collected for
reuse while the concentrate was directed back to the 0.2 m3 polyethelene
                                  39

-------
tank at the punp suction.  Raw feed was continuously added to this
tank from the 2.3 m3 elevated feed tanks so that the level in the
punp suction tank was constant.  The concentration of the feed in the
test loop continuously increased as the product water was withdrawn.
The variation of concentration with time simulated the variation of
concentration with location in a full scale plant.
     In the second mode, one 0.2 m3 batch of wastewater was recircu-
lated continuously through the module with both the product water and
the concentrate directed back to the pump suction tank.  Except for
minor changes in the characteristics of the wastewater with time, this
recirculation mode was a steady state condition.  This steady state
performance simulated the operating conditions of individual modules in
a full scale treatment plant.
     The main operating parameters which were varied during the course
of the tests were the feed pressure upstream of the module, 300 - 450
psi (2.7 x 106 to 3.1 x 106 Pa), the supply temperature, 55 - 90 F
(12.8 - 32.2 C), and the circulation velocity, 5-10 ft/sec (1.5 -
3 m/sec).  The operation of the loop was conducted on a continuous basis
except for maintenance downtime.  When the loop was shut down, the module
was flushed with tap water for about 10 minutes in both the normal and
reverse flow directions.
     Before any wastewater was supplied to the module, it was tested with
a solution of 500 mg/Jl NaCl in water.  The results of 150 hours of
operation using the NaCl solution are shown in Figure 9.  After an initial
decline, the product flux was constant at 8.3 GFD (0.023 on/min) for
a pressure of 300 psi (2,07 x 106 Pa), and temperature of 60 F  (15.5 C).
The conductivity rejection averaged 91% for this salt solution.
     The operating performance of the Westinghouse module is presented in
Figure 9, where the membrane flux, color, and conductivity rejections are
plotted for the initial 36 days of operation.  Following the introduction
of wastewater to the module, on the ninth day, the flux dropped 15% as the
concentration of the feed was more than doubled by recovering 66% as pro-
duct water.  Additional raw wastewater was mixed with this residual of
Batch #1 on the sixteenth day.  Operation continued to 73% water recovery;
                                  40

-------
g

i
UJ
oc
E
u
    100


     95


     90


     85
    .03
    .02
     .01
O
             COLOR  •-



  CONDUCTIVITY     /*
  ©        ©  © •'
     ©
 WW-WATER  WASH

  O  TAP WATER/SALT SOLUTION

& «  PLANT COMPOSITE (filtered ,
       •DESIGN VALUE
        FOR COST
        PROJECTION
         RECIRCULATION-f,
                   66% RECOVERY
                    Batch no: I
73%RECOVERY.fr
 Batch no: I
SHUT
DOWN
                                                                        2.7
                          46% RECOVERY-^
                           Batch no: 2
 71%
tRECOVERY
 Batch no: 2
                             10
15          20
      DAYS
                                                      25
                             30
                          35
              Figure  9,   Operating performance of Westinghouse module at La France.

-------
i.e., about 4-fold concentration of the feed to the module, was accomp-
lished on the twenty-second day.  During the processing of this combined
batch of wastewater, the flux decline increased.  The flux had declined
nearly 40% as wastewater was processed to 73% recovery; from 0.023 to
0.014 cm/min.  Both the conductivity rejection  (95 - 91%)  and color re-
jection  (99+ - 98%), however, exhibited only slight decreases as the
concentration of the feed supply to the module was increasing.
     Following the transfer of Batch #1 concentrate to storage, the
module was cleaned by flushing with tap (plant process) water for 15
minutes.  Following shut down over the weekend, the flux was 0.02 on/torn
during the initial operation with Batch #2 wastewater.  This was a re-
covery to approximately 90% of the flux with the salt water solution.
     Wastewater Batch #2 was processed to slightly more than 71% recovery
during the period from the twenty-sixth day through the thirty-fifth day
of operation.  During the next seven days as the feed to the module was
processed to about double its original concentration, the flux declined
rapidly to 50% of the original value.  A 20-minute flush with tap water
only partially restored the flux.  A second 20-minute tap water flush was
followed immediately by an increase in the operating pressure fron
2.07 x 106 to 3.1 x 106 Pa.  The flux increased correspondingly to 0.027
cm/fain.  With this high flux, wastewater Batch #2 was then concentrated to
71% product water recovery rapidly.  No flux decline was noted during the
two-day operation at this elevated pressure.  There was a significant
drop in rejections, however, color (99 - 95%), and conductivity (95 - 90%).
     These results are tabulated in Table 13.  The pH was maintained in
the range of 5.6 - 6.6.  The total solids concentration of the two batches
of wastewater were 1380 mg/£ and 2265 rng/i.  The total solids concentration
in the final mixed concentrate fron these two batches was 4000 mg/fc.
     During the final 500 hours of operation of the Westinghouse module,
the parameters of velocity, temperature, and pressure were varied while
both the product water and concentrate were recirculated to maintain a
constant feed to the module.  The recirculation prior to any concentration
of the raw wastewater feed simulated the inlet section of a treatment
plant.  Recirculation after an initial period of recovery of 96% of the
                                  42

-------
                Table 13.  OPERATING PERFORMANCE3 OF TUBULAR CEUULOSE ACETATE WESTINGHOUSE MXULE
                           WITH IA FRANCE COMPOSITE WASTEWMTER
10
Operating
time(hrs)
December 1973
1
23
95
143
185
337
January 1974
435
502

525
530
545
Flux
(on/tain)
(Pressure 2.07
0.023
0.020
0.018
0.016
0.016
0.014

0.014
0.011
(Pressure 3.1 x
0.027C
0.028
0.028

Total Solids
x 106 Pa)
-
97
96
96
-
-

97
96
106 Pa)
•»
92
92
Rejections (%)
Color

-
99.7
99.9
99.3
99.0
98.7

99.9
99.9

99.9
93.2
93.2

Conductivity

92
95
95
93
92
91

94
94

95
88
88
Recovery
i 	 Fraction (%)

0
_
_
_
66
73

27
46

46
-
71
     Operating conditions held constant.  Flow = 11 dm3/inin; pH = 5.8  - 6.9; T = 11 -  15  C.
     Color 585 - 3960 Pt-Co units; total  solids  1380 - 4155 rag/*/  conductivity 960  - 8500 yitiio/cm.
     Tap water flush increased flux 0.11  to  0.18

-------
 product water (corresponding  to about  a 20-fold increase  in concentration
 of the feed  to the module)  simulated the extreme outlet section of  a
 treatment plant.
      The  results  are  tabulated  in Table 14, and illustrated in Figure  10.
 The decline  of flux and rejections with increasing concentration, as pro-
 duct water recovery increased,  is evident for both 2.3 m3 batches of
 wastewater processed.  The  effects of  pressure  and temperature are  as
 expected. The sharp  drop in  flux that occurred at the end ,of  the test
 period is not understood.
      In summary,  the  performance of  the Vfestinghouse tubular cellulose
 acetate module exhibited a  40%  loss  in flux for product water  recoveries
 of 75 - 90%.   This result is  reflected in the selection of  a design con-
 dition of 450 psi (3.1 x 106  Pa),  which at a temperature  of 90 F  (32 C)
 yielded a flux of over 0.042  on/min.   The design value for  these operating
 conditions was taken  as 0.038 cm/min for the cost projection.  No deter-
 gent cleaning was used in this  study,  however,  this may prove  practical
 periodically, particularly  in modules  exposed to the higher concentrations
 near the  outlet of a  treatment  plant.   The quality of product  water at 75%
 recovery  was satisfactory for reuse  in all dyeing operations at La  France.

 HOLLOW POLYAMIDE  FIBER  (DuPont)
      During  the period from February 6,  1974, to March 27,  1974, a  DuPont
 hollow-fine polyamide fiber module (No.  400600)  was evaluated.  During this
 period the module was operated  for 187 hours with a continuous fresh supply
 of wastewater from five dye becks.   The limited capacities  of  the specific
 prefiltration available in  the  pilot plant made it possible to operate the
module  only an average of about 4  hours  per working day.  However,  the
module was used to process  over 79 m3  of wastewater, the  final portion of
which was reused  in Cycle #12.
     During the first several months of  operation of the pilot plant,  two
other DuPont modules were used  to process total plant composite wastewater.
Even though the earlier processed wastewater was reused in  plant dyeings,
Cycles  #1 through #6, only  the  equipment performance evaluated during

                                  44

-------
                Table 14.  OPERATING PERFORMANCE3 OF TUBULAR CELLULOSE ACETATE WESTINGHOUSE MODULE
                           WITH LA. FRANCE COMPOSITE WASTEWATER UNDER VARIABLE CONDITIONS
ui
Operating
time(hrs)

556
648
670
674
701

720
744

750
891
901
920

947
1010
1035
1059
Temperature
( C)
Pressure =
17
18
13
32
34
Flow = 11.
26
30
Pressure =
17
18
19
19
Pressure =
16
19
19
17
Flux
450 psi (3.1 x 106
.030
.025
.025
.044
.043
3 dm3/bin
.043
.045
Rejections (%)
Color
Conductivity
Pa); Flow = 22.7 dm3/min
99.3
98.9
99.5
99.7
94.7

97.0
97.1
92
93
95
93
85

92
91
300 psi (2.07 x 106 Pa)
.021
.012
.012
.012
450 psi (3.1 x 106
.024
.023
.018
.010
99.1
99.3
99.3
98.8
Pa); Flow
96.9
99.2
98.4
96.7
93
90
88
80
= 22.7 dmVnon
93
94
93
92
Recovery
Fr action (%)

0
62
73
79
97

19
45

45
96
96
96

0
0
0
0
   , Operating  conditions:  pH = 6.0 - 8.0
     Color 60 - 2085 Pt-Co  units, conductivity 650 - 11,200 yitiho/cm

-------
*>.
                                                                      COLOR
                                                                      CONDUCTIVITY
                                                                      PRESSURE, M Pa
                                                                      VELOCITY, m/sec

                                                                      TEMPERATURE,C
                        100
200
   300
HOURS
                                                         400
                                 500
             Figure 10.  Operating evaluation of Vfestinghouse module during final 500 hours.

-------
 Cycle #12 is felt to be typical for the DuPont modules.  The procedure
 followed during Cycle #12 is:  (1)  Only dyehouse wastewater (to mini-
 mize sanitary constituents) was treated,   (2)  only "fresh" feed entered
 the module; i.e., no recirculation of wastewater,  (3)  no stagnant con-
 ditions with wastewater in the modules were permitted, and  (4)  diato-
 maceous earth prefiltration (prior to 25 micron and 1 micron cartridge
 prefilters) was employed.  These conditions limited the productivity of
 the pilot plant which had limited prefiltration capacity.  As indicated
 in the cost projections for a full scale treatment plant, these procedures
 have little effect on cost of plant operation.
      These four operating procedures were followed as the module was
 evaluated for a 20 dm3>in supply rate which at 350 psi (2.4 x 106 Pa)  and
 about 60 F (15.5 C)  resulted in approximately a 50% recovery of water.
 Only during the last 15 hours of operation was recirculation of processed
 concentrate employed.   At that time the initial concentrate was collected;
 e.g., 1.2 m3 from each 2.3 m3  of dyehouse wastewater,  and reprocessed,  also
 at 20 dm3/min and 50%  recovery for in-plant reuse evaluation.
      The details of the operation of the DuPont module are presented in
 Table 15 and shown in Figure 11.   The tabulated results indicate the waste-
 water PH range was 6.2 - 8.0.   No pH adjustment was required as the poly-
 amide filers can operate in the range of pH 2 - 11. The temperature ranged
 fron 11  C - 23 C.
      Even though constant attention was  required to maintain the proper
 prefiltration, the pressure  drop  across  the module did not exceed the
 specified  limit  of 20 psi  (0.14 x 106  Pa)  until after  approximately 166
 hours of operation.  Four hours of detergent washing reduced the pressure
 drop to  its initial  level.  As  shown in Figure 11,  the product  flow rate
 was reduced only slightly at the greater nodule pressure differential,  and
 was not  significantly improved by  the detergent washing.
     In Figure 11, a very sharp decline in product  flow that occurred at
 65 hours of operation is noted.  The total solids concentration of the
wastewater supplied  to the module was 16,000 rng/u  other declines in
product flow rate occurred at 30 hours and at 187 hours.  At both of these
times the total solids were higher than the average of  about 2300 mg/A;
                                  47

-------
                    Table 15.   OPERATING PERFORMANCE3 OF HOLLOW POLYAMIDE FIBER DUPONT MODULE
                               WITH LA FRANCE DYEHOUSE WASTEWATER
oo
Operating
time(hrs)
February
1
10
16
23
27
32
48
64
65
73
81
106
129
144
160
166
Tenperature Product Flow Rate
( C) dm3/tain
1974
19 9.0
14 8.0
11 7.9
20 8.3
17 8.3
9 6.4
13 8.3
14 3.8
18 3
11 7.6
12 7.9
19 8.0
23 7.9
18 7.9
20 7.6
16 6.8
Rejections (%)
Color Conductivity

>99 96
98 97
93 94
>99 98
>99 97
>99 96
>99 97
>99 92
93
95
>99 97
>99 94
>99 93
>99 88
>99 94
>99 91
Recovery
Fraction (%)

53
49
47
49
49
56
49
22
18
44
47
49
47
47
44
40
March 1974 (shut down for detergent wash)
172
176
180
187
12 6.4
16 6.8
18 7.6
20 6.4
>99 89
98 82
>99 84
>99 86
50
50
50
50
       ,  Operating conditions:  P = 2.4 x 105 Pa; flow
         Color 30 - 1250 Pt-Co units; conductivity 610
17 dm3/kLn; pH = 6.2
22,000 umho/on.
- 8.0.

-------
    100
 2   80
uj
 C
 E
E
•o
O
u
     TO
             COLOR

             CONDUCTIVITY
                                                                             BIZ-WASH
                             TOTAL SOLIDS
                              16,OOO
                                               DESIGN VALUE FOR
                                               COST PROJECTIONS
I
E
o
w
	 1 	 	 1 	 1 	 1 	 	 	 i 	 i 	 i 	 i 	 •
               20       40       60      80       100
                                           HOURS
                                                          120
140
160
190
    Figure 11.   Operating performance of DuPont hollow polyamide fiber nodule at La France.

-------
 i.e.,  4515 mg/£ at 30 hours and 3400 mg/£ at 187 hours.   There  is
 evidently a significant effect on product flow rate of high solids  load-
 ing, even after extensive prefiltration.   It does appear that the effect
 is easily reversed by returning to a lower solids concentration.  The
 effect of total solids concentration upon the rejections is quite small.
     Following the wash with Biz detergent at 166 hours, the wastewater
 was recirculated to achieve a constant 50% product water recovery.  This
 recirculation was continued for only 15 hours,  but seemed to influence
 both product flow rate and rejection.   The conductivity  rejection de-
 creased from 90 to 85%,  while the product flow rate increased by 17%.
 Following the Biz detergent wash,  1.2 m3  of concentrate  was collected
 while  the module was operating at 50% product recovery.   When this  con-
 centrate was returned to the module as feed,  the product flow rate  dropped
 by 10%,  and the conductivity rejection increased slightly.   (The data are
 shown  as the last data points in Figure 11.)
     There is no apparent explanation for these trends.   It seems worth-
 while  to conclude,  however,  that while detergent washing was effective in
 reducing the pressure differential across the module,  the washing had no
 significant effect on either product flow rate  or rejections.
     In summary,  the performance of the DuPont  hollow  fiber module was
 evaluated for 187 hours.   With filtered dyehouse  wastewater fed continuous-
 ly to  the module, and with no recirculation of  concentrate,  the pressure
 differential across  the module exceeded desired limits after  166 hours of
 operation.   It  is possible that the daily re-charging  required for  the
 small diatomaceous earth filter allowed particulates to  enter the module
which could  account  for the pressure differential build-up.  ABCOR used
 the above data to prepare  the  cost projections  for  a full scale treatment
 plant.   The  cost analysis  included prefiltration as recommended by  EuPont.
     The quality  of  the product water  fron the  DuPont module was adequate
 for reuse in all dyeing operations  at La  France.
                                  50

-------
  SPIRAL-W3UND CELLULOSE ACETATE (Gulf)

       During the period fron March 28,  1974,  to May 7,  1974,  a  spiral-
  wound, cellulose acetate membrane module was evaluated.  During this
  interval the module was operated  for 632 hours on wastewater supplied
  from fxve dye becks and subsequently for 172 hours on  composite waste-
  water fron the total plant.  • The  unit  thus processed approximately 230 m3
  of wastewater.  A portion of the  approximately 45  m3 of composite waste-
  water processed was stored for reuse in  dye  Cycle  #14.
       The module evaluated contained  3  standard spiral-wound units in a
  101 rnn diameter x 3.65 m long pressure vessel.  The membrane surface area
  was 18 m2.
       During the evaluation, the module was supplied with 13 dm3/min of
  25 micron prefiltered wastewater and operated at 400 psi (2.76 x 10* Pa)
  in the temperature range of 14.4 - 25.5 C.   The initial product water flow
  rate was 4.5 dr^n yielding 33% product recovery.  After about 90 hours
  of operation a portion of the module effluent was recalculated directly to
  the pump suction to maintain a 75% recovery.   The PH was controlled in the
 range of 5.8 - 7.0,  except for brief exposures to PH 8.  PH control was by
 chemcal addition to each 2.3 m3 batch  of wastewater processed.
      The operating performance  of  the Gulf module  is shown  in Figure 12,
 and Table 16.   The product flow rate, color,  and conductivity rejections
 are plotted for the  entire period  of  the  evaluation.  The product flow rate
 decreased fron an initial value of 6.7  dm3>in exhibited during the treat-
 ment of a 1500 mg/£  NaCl solution  to  a  stable value of  3 dm3/min.
     The  variations  in prefiltration, wastewater source, and mode of
 operation did  not  seem to materially  influence the  membrane performance
 The performance  over the  last 170 hours of operation with 25 micron pre-
 filtration, while  processing cotposite wastewater to 75% product recovery,
was used  as the basis for  the cost projections.
     The color rejection was uniformly greater than 99%.  The conductivity
rejection averaged approximately 95%.  The slight decrease in conductivity
rejection, shown in Figure 12, is apparently related to higher total solids
concentration in the wastewater.
                                  51

-------
           Table 16.  OPERATING PERFORMANCE3 OF SPIRAL CELLULOSE ACETATE GULF MODULE
                      WTTH LA FRANCE WASTEWATER
Operating
time(hrs)
Product Flow Rate
dm3/fran
Rejections (%)
Color Conductivity
Recovery
Fraction (%)
March 1974
  1
  20

  1
  20
  91
April 1974
  95
  120
  146

  165
  193
  259

  272
  440
  630
               (1500 mg/A NaCl)
               6.4                    -                   95               37
               6.4                    -                   96               37
               (dyehpuse wastewater,  1 micron filter)
               4.5                    97                   97               33
               4.2                    97                   98               32
               3.8                    98                   98               29

               4.5                    99                   97               75
               4.5                    99                   97               75
               4.5                    99                   97               75
               (dyehouse wastewater,  25 micron filter)
               4.5                    99                   96               75
               4.5                    99                   96               75
               4.5                    99                   93               75
               (closed  circuit recycle started)
               3.0                    99                   95               75
               3.0                    99                   95               75
               3.0                    99                   93               75
               (end recycle - 1 hour  tap water flush)
               (composite wastewater  - collection for dye Cycle #14)
633
May 1974
660
708
780
3.8

3.0
3.0
3.0
99

99
99
99
97

97
97
97
75

75
75
75
,  Operating
  Color 57 •
conditions:  P =  2.8 x 106  Pa;  Flow = 19  dm3/inin;  T
• 2800 Pt-Co units; conductivity 1450 - 5900 pinho/cm,
=14-26 C; pH = 5.8 - 7.0.

-------
          100,.
                                                                                    COLOR (> 99%



                                                                                    CONDUCTIVITY
ui
u>
             XD
          O TAP WATER/SALT SOLUTION
6
5
4
c
•5 »
•o
I .
u.
PRODUCT
O _
.
1




1
33%^ ^7*1

% WATER
^^•••_
lju ^
V* ^
FILTERS
FRESH F

yi
?EED
TO MODULE
RECOVERY
.. . . .\

• DYE HOUSE WASTEWATER
• COMPOSITE WASTEWATER
DESIGN VALUE
FOR COST
PROJECTION
RECIRCULATION OF 0.2m3 fc- FRESH FEED
OF WASTEWATER TO MODULE
                    IOO     200     300     4OO     500


                                                   HOURS
600
700
800
    Figure 12.  Operating performance of Gulf  (U.O.P.) spiral cellulose acetate module at La Francs

-------
       In sunmary, the Gulf spiral-wound cellulose acetate module exhibited
  a flux decline of approximately 40% for treatment of composite wastewater
  to 75% recovery of product.   The product flow rate was stable over an
  extended period of operation.  The quality of product water was satisfactory
  for reuse in all dyeing operations at La France.

  DYNAMIC Zr(IV)-POLYACRYLlC ACID (Selas)
      During  the period  June  4,  1974,  to  July  2, 1974,  a Selas  ceramic
  tube,  Zr(IV)-polyacrylic acid membrane was  operated  for 650  hours.  The
  unit was  evaluated first with wastewater from five dye becks and then with
  the  composite wastewater from the  total  plant.  In addition, the membranes
  were used in a  separate evaluation of indigo wash water.  The  concentrate
  from the  treatment of the dyehouse wastewater was reused in Cycle #16.
      The module evaluated was a tubular  configuration employing eight units
  in series.  Each unit consisted of 19, 5.5 mm diameter porous ceramic tubes.
 The membranes were deposited on the external surface of the tubes.  With
 a 0.16 m3/min wastewater  supply rate to the module, the ratio of product
 water or permeate flow to wastewater flow through the module was consider-
 ably less than 1%.
      Two modes of operation were used.  The first was the concentration
 mode.  In this mode of operation product water from the module was collect-
 ed while the  concentrate was recirculated to a 0.3 m3 stainless steel tank
 at the  pump suction.  Raw wastewater was  continuously added from the
 2.3 m3  elevated reservoir to maintain a controlled level in the 0.3m3
 tank.   The concentration of the  feed to the module continuously increased
 as the  product water was withdrawn.  In the second mode of  operation,  one
 0.3m3  batch  of wastewater was recirculated continuously through the
module with both  the product water  and concentrate directed back to the
punp  suction  tank.
     The operating parameters varied during  the course  of the evaluation
were:   (1)  type of wastewater,   (2)  degree of prefiltration,   (3)  pres-
sure, 300 - 700 psi  (2.07  x 106 to  4.8  x  106 Pa),   (4)   temperature, 80 -
190 F (26 - 88 C), and   (5)  circulation  velocity, 2.3  - 4.6 m/sec.  The
                                  54

-------
  PH was not controlled, sinoe dynamic nentoranes can operate in a range of
  PH 4 - 11, well within the range observed for the wastewater at La
  France.
       Previously, dynamic membranes in laboratory test nodules provided
  by the Oak Ridge National Laboratory were used to provide the renovated
  wastewater reused in Cycles #7,  #8, and #9.   since these test nodules
  were not ccmnercially available,  only the performance of the Selas module
  is considered appropriate for use in the cost projections.
       Before any wastewater was supplied to the Selas  nodule,  it was test-
  ed with a 500 mgA Nad  solution.   At 700 psi (4.8 x  10*  Pa)  and 50 C
  the  flux was 0.33 cm>in ^ ^  conductivity ^^^ wafi  gi%>  ^
  operating performance of the Selas nodule is  described in Figure 13,  and
  TabJe 17,  where the  flux,  color,  and conductivity  rejections  axe presented
  for  30 days  of operation.   To evaluate  the effect  of wastewater conposition
  and prefiltration on the rate of flux decline, the nodule was evaluated
  under what was expected to be increasingly more difficult conditions.
  Because the characteristic of high temperature operation permits the
 possibility of energy recovery, the tests were carried out at elevated
 temperatures.
      Initially, the nodule was supplied with wastewater fron five dye becks
 This wastewater was prefiltered through the 25 micron cartridge filters.
 The flux declined sharply from greater than 0.33 cm/min to 0.045  cn^min!
 Subsequently, a flush with tap water returned the flux to 0.1 cm/min.   A
 repeated concentration of dyehouse wastewater to about 75% product  recovery
 produced a similar decline in flux to about 0.055 cm/min.  Another  flush
 with  tap water resulted in a flux  of about 0.1 cm/min.
      A series of tests with indigo rinse water was  carried out from the
 fourteenth to the twenty-first day.   During this  tine  the  flux recovered
 to  over  0.22  cm/min.   ^ sharp drop in  conductivity rejection that occur-
 red on the  seventeenth day corresponds to a total solids concentration of
 57,000 mg/Jl.
     Beginning on the twenty-first day,  the module was  then supplied with
 total plant composite wastewater through 25 micron prefilters.  The flux
decline was again rapid.  After about 20 hours, the module supply was
                                  55

-------
                    Table 17.  OPERATING PERFORMANCE3 OF CERAMIC TUBE Zr(IV)-PAA SELAS MODULE

                               WITH LA, FRANCE WASTEWATER.
en
ov
Operating
time(hrs)
June 1974
22
Flux Temperature
(cm/min) ( C)
(salt solution)
.34 50
Reiections
Color conductivity

91
(dyehouse wastewater, 25 micxon filter)
30
76
98

148
.23 43
.05 46
.04 48
(salt solution)
.10 36
>99 83
>99 88
88 87

92
(dyehouse wastewater, 25 micron filter)
167
190
238
262

330

338
356
375
402
497
.07 30
.12 48
.07 48
.06 48
(tap water)
.12 54
(indigo)
.13 58
.15 60
.12 46
.16 60
.29 55
>99 89
>99 88
97 ' 88
95 86

_ _

91
>99 88
>99 88
>99 61
>99 87
(composite wastewater, 25 micron filter)
502
518

535
571
.23 55
.12 57
(composite wastewater, 250 micron)
.16 53
.13 58
97 80
98 81

>99 80
>99 75
        f* Operating conditions:  P = 4.8 x 10s Pa;  Flow = 0.15 m3/friin.

          Color 715 - 19,575 Pt-Co units;  conductivity 960 - 36,650 nmho/cm.

-------
    100
   90
a?
 -  80
 t  70
 u
 s  *rt
 a:  60
       •O
£
u
    .4
                                              AA
                                  O O
                                                            DA    A COLOR
                                                           cAA A A A CONDUCTIVITY
                                                           D
                                                           O TAP WATER/SALT SOLUTION
                                                           • DYE HOUSE  WASTE(filtered,25/<)
                                                           A INDIGO WASH (Concentrating)
                                                           A INDIGO (RECYCLE)
                                                           • PLANT COMPOSITE(filtered,25/<)
                                                           D PLANT COMPOSITE (filtered, 25O/<)
                                                                     DESIGN VALUE FOR
                                                                     COST PROJECTION
     02466


       Figure  13.  Operating performance of Selas dynamic membrane module at La France,
                           10   12   14   16  18  20   22  24   26  28   30
                                              DAYS

-------
 changed to total plant  composite wastewater,  through only  250 micron
 prefliter.   For 55 hours the  flux remained at about 0.11 cm/roin.  The
 evaluation was  concluded with a period of 90  hours of operation with
 recirculation of indigo rinse water.  The flux remained stable at
 0.14 on/nin.
     Throughout the period of evaluation, the color rejection remained
 near 99%.   The  conductivity rejection decreased gradually  frcm about
 90 to 80%.  This membrane has subsequently been exposed to a variety
 of dye wastewaters and  retains these percentage rejections after about
 4000 hours  of operation.
     In  surtmary, the dynamic  membrane operating performance exhibited a
 characteristic  of quick accormodation to particular feed conditions.
 The  design  value for the treatment plant cost projection was 0.14 cm/tain
 based on 950  pai (6.5 x 106 Pa) operation, which corresponds to a value
 of 0.11  cm/min  based on the performance data  at 700 psi (4.8 x 106 Pa)
 and  50 C.   The  performances indicate best operation on unfiltered (ex-
 cept for 40-mesh screening) total plant conposite wastewater.  The
 quality  of  the  product water was satisfactory for reuse in all dyeing
 operations  at La France.

 DESIGN VALUES FOR COST  PROJECTIONS
     The operating performance data obtained during the pilot plant pro-
 gram form the basis for the cost projections  for a 7570 m3/day treatment
 plant.  The four membrane modules were evaluated within the manufacturers
 recomended operating limitations.  The parameter of primary importance
 in the cost projections is the membrane flux, i.e., the product water flow
 rate per module.  The long-time membrane flux, estimated from the test
data, is listed in Table 18.   In the case of the hollow fiber polyamide
membrane, the estimate of long-term flux is 20% below the value observed
during the relatively brief operating time during the pilot plant program
 (less than  200 hours).
     The membrane flux is directly dependent upon the operating pressure
 and  is strongly influenced by  the operating temperature .  Both the pilot

                                  58

-------
                                 Table  18.  MEMBRANE FLUX FOR OOST PROJECTIONS
vo
MEMBRANE
MODULE
CCNFIGURATICN
PILOT PLANT RESULTS
Pressure, M Pa
Temperature, C
Flux, cnymin
DESIGN VALUES
Pressure, M Pa
Temperature , C
Flux, cm/min
Polyamide

hollow fiber

2.4
21
0.004a

2.4
32
0.005
Cellulose
Acetate

spiral-wound

2.8
21
0.017

2.8
30
0.020
Cellulose
Acetate

tubular

2.1
16
0.017

2.8
30
0.028
Dynamic
Zr(W)-PAA

tubular

4.8
50
0.15

5.2
45C
0.15
      20% reduction from value measured at less than 200 hours operation
      Temperature effects based on manufacturers data.
      Thermodynamic mean temperature of plant effluents.

-------
plant test values ard the design values of pressure and temperature to
be used in the cost projections are tabulated in Table 18.  The design
value of flux for each membrane module configuration, in Table 18, is
thus the valve measured in the pilot plant corrected to the design
temperature and pressure.
                                   60

-------
                                SECTION VIII

                     TRES3MEOT ELROT COOT PEOGECTIONS
      ae equips perform^ data detsrndned in the pilot plant in-
 vestigation are used in the follo^ ^ projections for .     .
                                               oecons  or . ^.
  gallons per day ,7570 m'/day,  hyperfiltration treats plant for the

                         "" ™1»~ *«"—  ~ at-nt, i.e., pH
                       control,  arf suspend solids
          f                          a°-  H-ver, no allo,      is
          for storage reservoirs, nor for the 10 - 20* *^ water
                                                 -
  nor for treataent of any retired bio, do™ of concentrate.
       Ihere is a wide variation in both the capital cost and operating
  costs a^ong the four .M. systaje.  ^ ^^ ^^ ^     ^

  poly^  and cellulose  aoetate ^rbran, system is for ^toane replace-
  ment.   ae ra:0r operating cost for the dynamic ,,3*^ vstem is
  etectrical pc^er for punping.  ae major capital cost for all the systems
  is for the mambrane modules.
     ae polye^dde and spirals*       ^ ^^ ^^
are of interest for water treataent applications because of their relative-
ly lor capital and operating costs.  They generally require fine pre-
fitoauon  heaver.  ^^ ^^ ^^ ^^ ^

high „*»! capital cost,  but are saIEwhat easier  to cerate since they
re^re only relatively coarse prefiltration.  The  tubular
                                             .            r nanes
 relatively easier to mechanically clean, a possibly significant advantage
 for so^ industrial applications.  a» dynaMc ZrflVJ-PM mitlmm ^
 a relatively high initial cost, but require the least prefiltraticn.  a.
 aa^ntage of high temperature operation (to 100 c, precludes pretreafcj
 ten^ature oontro! requirenants « may,  t^h recycle of L water,
 permit significant energy conservation.
THE TREATMENT SYSTEM
     A schematic materia! balance for the treatnsnt of
by hyperfiltration is she™ in figars M.
                                  61

-------
     FEED VOLUME- 7575 m3/day
     FEED COMPOSITION
      TOTAL SOLIDS" 100 to SOOOmgA*
      COD =  20O to 300 mg /A
      COLOR » 3OO to 600 Pt-Co Units
a\
NJ
              PRETREATMENT
CONCENTRATE WATER
For Dyebath Use
VOLUME" I5l5m3/day
TOTAL SOLIDS » 7,OOO to I5,000mg//
COD - 350 to 550 mg/*
COLOR = 6OO to I ZOO Pt_Co Units
                                                              HYPERFILTRATION
                                                              MODULE  UNIT
                                                      PRODUCT WATER
                                                      Reuse for Plant  Water
                                                      VOLUME = 6O60 m3/day
                                                      TOTAL SOLIDS" 100 to 6OO
                                                      COD ° 25 to 50 mg ft
                                                      COLOR = 20 to 50 Pt-Co Units
           Figure 14.  Simplified flow schematic of a textile dyewaste treatment system.

-------
  at a rate of 2^nillion-gallons per day (7570 mVday)  is processed through
  a pretreatatent section.   The pretreatment section may consist of  equipnant
  for PH adjustment, coarse and/or fine filtration to remove  suspended
  matter, and heat exchangers to cool the feed stream to about  32 c, the
  normal operating temperature for the pre-forned  membranes.
      As shown in Figure 14,  80%  of  the wastewater feed will be recovered
  as product  (desalted and decolored)  by the hyperfiltration  unit,  and re-
  cycled to the textile plant  for  use as process water.  The  concentrate
  will be recycled to the dyeing prooess for salt  and/or dye  reuse.  The
  point  of recycle mst be determined by the chemical exposition of the
  concentrate stream and the details of  the dyeing prooess.
      The complete and continued recycle of wastewater within the textile
  mill may cause a gradual build up of impurities in the prooess water.   If
  the level of impurities reaches an undesirable level,  there must be a
  blow down of some concentrate fron the system.  Selection of a treatment
 method for the concentrate must be determined for the  particular waste-
 water.  Wastewater or blew down disposal fron the hyperfiltration plant
 has not been included in the plant design presented here.

 EQUIPMENT DESCRIPTION AND CAPITAL COST PPOJBCTIQNS
      Four capital cost  estimates for full  seals hyperfiltration treatment
 plants are presented.   Each deals with a particular membrane configuration.
 Case 1 involves the hollow fiber polyamide membranes (DuPont);  Case 2  in-
 volves  the spiral^ound cellulose acetate  membranes (Gulf);  Case 3 involves
 tubular cellulose acetate membranes  (Vfes tollhouse);  and Case 4 involves
 dynamic membranes (Selas).  Cost  and characteristics for the four  types
 of  membrane modules are given in  Table  19.  Costs of pumps and filters
 are based on quotations f ran  vendors  and other equip***  costs and estimated
 in  1975 prices.
     The  cost projections are developed for the hyperfiltration module
unit and  then for the pretreatment units separately.  The cost projections
for the total plant are obtained by combining the costs of these two
major units with auxilliary equipment and engineering costs
                                  63

-------
Table 19.  MEMBRANE MODULE CAPITAL COST BASIS FOR PROJECTIONS
MEMBRANE
CONFIGURATION
MODULE DIMENSIONS,
Diameter x Length, m
MEMBRANE AREA, m2
DESIGN PRODUCT FLOW,
dm3 /tain
OPERATING PRESSURE,
M Pa
FEED RATE, dm3/min
PRESSURE DROP, M Pa
BARE MEMBRANE COST
HOUSING AND ASSEMBLY
Polyamide
hollow fiber
0.2 x 1.2
603
32
2.4 - 2.8
49
0.14
$2500
$1000
Cellulose
Acetate
spiral-^wound
0.2 x 1.0
28
5.8
2.4 - 2.8
189
0.27
$665
$1200
Cellulose
Acetate
tubular
.15 x 1.8
2.6
0.7
2.4 - 2.8
340
0.14
$271
$230
Dynamic
Zr(IV)-PAA
ceramic
0.07 x
0.8
1.2
6.5
227
.10
<1
$585
tubes
0.9








-------
  Hyperfiltration Module Unit Cost Projections
       The cost projection for  the hyperfiltration module unit are
  tabulated in Table  20.   The specific characteristics of the design for
  each menbrane nodule configuration are individually discussed as Cases 1
  through  4.

  CaseJ. - The membrane module product flow rate depends on membrane life
  and cleanliness.  Although new polyamide membrane nodules will yield
  about 37 dm3>in of product per nodule,  the plant has been sized for
  32 dmVmin per nodule.   If the product flow rate is too high initially,
  it can be controlled by decreasing the operating pressure of the
  system.  Three-and-one-half percent extra membrane area has been pro-
 vided for operation during membrane cleaning for emergency situations.
      The hollow fiber nodule requires periodic back-flushing and cleaning.
 It is assumed that enough product will be available to back-flush and
 forward-flush every module for at least two hours  per week.  This will
 require about 163 m3/day of product water.   The plant  size  is augm-nted
 to 7774 m3/day.   Thus the number of nodules required is given by the
 ratio of  the plant size to  the product flow rate multiplied by the per-
 cent  product recovery,  i.e., 134 modules.  Ten extra nodules are included,
 bringing  the total to 144.
      The  144 polyamide membrane  modules are  incorporated into 16 parallel
 banks consisting of  two stages per bank, as  shown in Figure 15.  Each
 bank  consists  of nine modules.   The first stage of each bank includes
 six modules  in parallel.  The second stage has three nodules in parallel.
 Fifteen of the 16 banks must operate at all times while one may be idle
 for maintenance  or cleaning.
     Each module requires 49 dm3/tnin of wastewater feed.  The total flow
 of 331 dmVmin through each module bank,  once through both stages one and
 two, will yield  80% product water recovery.  The concentrate and product
 effluents from each bank will be monitored by flow indicators.   They are
designed to be 66 dm3/toin and 265 dm3/tain, respectively.
     For equal distribution of wastewater flow through the parallel,  a
                                  65

-------
o\
                                                FLUSH TO FEED
         ©














,— ^ »


) PUMP
TO C



Fl i i^w TT» PFP n
x~x
* CPJ
T V*/
1 1
4OOosi

(2,7 M Po )







ITHER BANKS





















- 9


- 9


- 9

B — Q
S»

B_ Q
y

BA
9
1
T
4
1 II


1 II
I II

(ii
ft

1 II


-4—4


i ii


\ 9
1



B - !








;



— »•





9




•\
y

1
7








1 II
1 H




1 II
i II

1 II
i II








CONCENTf






r^ 	 • -^



PRODI


,
             KEY
             B-9 DUPONT
P - PRESSURE  GAUGE
                        Figure 15.  Case 1 - Details of a meirbrane bank design.

-------
  flew balancing resistance equivalent to 0.137 x 10* Pa pressure differ-
  ential is incorporated at the discharge of each module.  Whenever the
  pressure drop across any stage becomes high and/or the product flow
  rate of any bank drops below a set limit, the membrane bank in question
  is isolated and cleaned.
       High flew at low pressure are necessary for efficient nodule clean-
  ing.   A separate cleaning punp in a quick^isconnecting piping system
  are provided for cleaning.   The details of the pumping requires
  for the modules are  included in Table  20,  with the  suntnary of  character-
  istics and costs of  the hyperfiltration module unit.   Cost projections
  for the pumping station required to flush,  or clean, the module are also
  included.  The  cost  projections  for piping and installation, electrical
  serves,  and instrunentation required  for  the hyperfiltration membrane
  unit are the same for each membrai*  type.   These are also tabulated in
  Table 20.

 Casej. - The design product flow rate per module is based on the pilot
 plant results.  At the pilot plant test conditions,  the membrane flux
 in the spiral^ound module was measured as 0.017 cm/min.  This flux
 corresponds to a product flow rate of 5.8 dmVmin per module under the
 design pressure of 2.7 M Pa and temperature of 30 C. Therefore, 750
 modules in 125 pressure vessels yields  82.7% product water recovery
 This provides for 204 m3/day for module flushing.
     These 125 pressure vessels are incorporated into three stages. The
 first  stage will contain 504 modules, the second 162 modules, and  the
 third  84 modules.  A  tapered arrangement of modules,  similar to that
 shown in Figure  15, is employed.   Six modules,  and one  pressure vessel
 assenbly may te  idle  for maintenance  or  cleaning.  A separate cleaning
pump is provided  for  cleaning.
     The details of the pumping requirements for the modules are included
in Tabl* 20, with the suitmary of characteristics and costs of the hyper-
filtration nodule unit.  Cost projections for the pumping station required
to flush, or clean, the module are a!so included.  The cost projections
                                  67

-------
Table 20.  DETAILS OF CAPITAL COST PROJECTIONS FOR HYPERFILTRATION MODULE UNIT
                       (7570 m3/day & 80% Product Recovery)
CASE NUMBER
MEMBRANE MODULES
Configuration
Number
Cost, $
Maiibrane Cost
Included
PUMPS
Flow, m3/tain
en Head, M Pa
00 Power, kW
Cost, $
CLEANING STATION, $
PIPING COST, $
ELECTRICAL AND
INSTRUMENTS
TOTAL COST, $
1

hollow fiber
144
504,000

360,000

5.3
2.4
410
75,000
17,400
150,000

100,000
846,400
2

spiral-wound
750
648,750

498,750

5.3
2.7
410
75,000
17,400
150,000

100,000
991,150
3

tubular
5932
2,971,932

1,230,000

5.3
2.7
745
75,000
17,400
150,000
-
100,000
3,314,332
4

ceramic tube
3600
2,109,600

3,600

5.3
6.5
2600
337,124
17,400
150,000

100,000
2,714,124

-------
 for piping and installation, electrical services, and instrumentation
 required for the hyperf iltration membrane unit are the sane for each
 membrane type.  These are also tabulated in Table 20.
 3 ~
              design product flow rate per module is based on the pilot
 plant results.  For the pilot plant test conditions, the cellulose
 acetate membrane flux for the tubular configuration was measured as
 0.017 cm/min.  This flux corresponds to a product flow rate of
 0.7 dm3/toin per module under the design pressure of 2.7 M Pa and temp-
 erature of 30 C.  Therefore, 5933 modules are required to provide 82.1%
 product water recovery.   This provides 159 m3/day for module flushing.
 A tapered arrangement of modules,  similar to that shown in Figure 15,
 is employed.   Additional horsepower is required for recirculation of
 feed to provide the required flow rates per module.
      The details of the  pumping  requirements for the modules are included
 in Table 20,  with the summary of characteristics and costs of the hyper-
 filtration module unit.   Cost projections for the pimping station required
 to flush,  or  clean,  the  module are also included.  The cost projections
 for piping and installation,  electrical services,  and instrumentation
 required for  the hyperf iltration membrane unit are the same for  each
 membrane type.   These are also tabulated in Table 20.
4 ~
             design product flow rate per module is based on the pilot
plant results.  For the pilot plant test conditions, the dynamic Zr-
polyacrylate membrane flux was measured as 0.15 cm/min.  This flux corre-
sponds to a product flow rate of 1.2 dm3/mirt per module under the design
pressure of 5.2 M Pa and temperature of 45 C.  Therefore, 3600 nodules
are required to provide 82.1% project water recovery.  This provides
159 m3/day for module flushing.
     A tapered arrangement of modules, similar to that shown in Figure 15,
is employed.  Additional horsepower is required  (1)  to pressurize the
feed to 950 psi (6.5 M Pa) , and  (2)   to recirculate feed to provide the
required flow rate per nodule.
                                  69

-------
       The details of the pimping requirements for the nodules are included
  in Table 20,  with the sunmary of characteristics and costs of the hyper-
  filtration module unit.   Cost projections for the punping station required
  to flush,  or  clean,  the  module are  also included.  The cost projections
  for piping and  installation,  electrical services, and instrumentation
  required for  the hyperfiltration membrane unit are the sane for  each
  membrane type.   These  are also tabulated  in Table 20.

  Pretreatment  Unit Cost Projections
      The cost projections for- the pretreatnent  unit are tabulated in
  Table 21.  The specific characteristics for each membrane module con-
  figuration are individually discussed as Cases  1 through 4.
      In general, pretreatment costs are not a large part of the total costs
  for the complete hyperfiltration system.  The iitproved performance of the
 membrane modules often effects savings to offset pretreatment expenditures.
 The design case for each module configuration includes the pretreatment
 recoimendations from the general experience of the manufacturers and the
 pilot plant results for operation with La France's textile wastewater.
 It was beyond the scope of this project to optimize the pretreatnent.

 Case 1 - Based on the pilot plant experience with both total plant com-
 posite and segregated dyehouse wastewater, the hollow polyamide fiber
 membrane modules require very fine prefiltration, and wastewater cooling
 to 32  C.   Even though not required in the  pilot plant tests, pH control
 is included in the cost projections.
     Based on  the pilot experience,  the hollow polyamide fiber module is
 very sensitive to wastewater feeds containing collodial solids below 1
micron in diameter.  Depth-type cartridge  filters, 1 micron size, were  found
to be insufficient in preventing hollow fiber module plugging during pro-
longed operation with the  total plant composite wastewater.   Segregated
wastewater from the dyehouse,  after  filtration  through a pre-coat system,
could be processed for about 200 hours without  substantial module plugging
       substantial increase in module pressure  loss),  or deterioration  in

                                  70

-------
Table 21. DETAILS OF CAPITAL COST PROJECTIONS FOR PPETREATMENT UNIT
(7570 m3/day & 80% Product Recovery)
CASE NUMBER
MEMBRANE

CONFIGURATION

PREFILTER
Type
Removal
Cost* $
COOLING TOWER
Utilized Power, kW
Range, C
Cost, $
pH CONTROL
Cost, $
TOTAL PRETREATMENT, $
1
Polyaraide

hollow fiber


pre-coat
(<1 micron)
123,950

75
13
220,000

8,000b
351,950
2
Cellulose
Acetate
spiral-^wound


rotary screen
(>25 micron)
35,000

85
15
240,000

8,000
283,000
3
Cellulose
Acetate
tubular


rotary screen
(>25 micron)
35,000

85
15
240,000

8,000
283,000
4
Dynamic
Zr-PAA
external
tubular

screen
(>250 micron)
25,000


a


8,000b
33,000
,  Dynamic membranes require no temperature control.
  Polyamide and dynamic Zr-PAA membranes have pH ranges of 2
- 10 and 4-10, respectively.

-------
membrane flux or rejection.  Consequently, a pre-coat  (leaf) filter
is included in this Case 1 design.
     Diatonaceous earth pre-coat was used in the pilot plant.  Other
similar filter-aid material is expected to be equally effective.  The
use of wood flour is assumed in this design.8  The cost projection in-
cludes all the necessary equipment to handle 453 kg as body feed to
50 mg/H.  The cost projection is $123,950 for this prefiltration.
     A cooling tower is designed to reduce the wastewater feed tempera-
ture to 32 C.  The maximum operating temperature of the hollow fiber
module is 35 C.  The cooling tower basin also serves as a feed surge tank
and a mixing zone for pH adjustment and any required water treatment
chemicals.  Since the mixed temperature of the hot and cold dyehouse
effluents is 45 C in the summer, the cooling tower must provide a cooling
range of 13 C.  The cooling tower and auxiliary equipment cost projection
is $220,000.

Case 2 - Based on the pilot plant experience with total plant composite
wastewater, the spiral cellulose acetate membrane modules require   (1)
25 micron prefiltration,   (2)  wastewater cooling to 30 C, and   (3)  pH
control to pH 3 - 6.
     During the pilot plant evaluation, depth-type cartridge filters,
25 micron size, were sufficient in preventing performance deterioration
of the spiral-wound module.  A rotary screen filter is included in the
cost projection.
     The cooling requirements for cellulose acetate membranes are similar
to those for the polyamide fdJxsrs.  The reccrmended temperature is 30 C
for cellulose acetate, so the cooling range on the cooling tower is 15 C.
The cooling tower and auxiliary equipment cost projection increased
$20,000 from the Case 1 estimate because of the higher cooling load.
     The acceptable range for operation of cellulose acetate at the
temperature of 30 C is pH 3 - 6.  PH control is required for the La France
textile wastewater that averages nearly PB 1, but has peaks up to PH  10
or more.

                                  72

-------
 Case 3 - Based on the pilot plant experience with total composite waste-
 water, the tubular cellulose acetate membrane modules require  (1)  25
 micron prefiltration,  (2)  wastewater cooling to 30 C, and  (3)   pH
 control to pH 3 - 6.
      These are the same requirements listed for the spiral module.  How-
 ever, since previous experience suggested finer prefiltration,  these
 cost projections include a 25 micron rotary screen filter.
      The cooling requirements and pH control are exactly the same as
 for Case 2.

 Case 4 - Based on the pilot plant experience with both total plant com-
 posite aid segregated dyehouse wastewater, the dynamic Zr-EM. mcdbles
 require only coarse  (>250 micron prefiltration).   In fact, performance
with only this coarse prefilter was actually superior to that observed
with depth-type cartridge  filters, 25 micron size.
     No wastewater cooling nor pH control was needed in the pilot plant.
Since this membrane can operate at elevated temperatures, it is  desirable
to take advantage of increased flux.  The cost of PH control is  included
since there was some indication of optimal performance at PH 8.5 - 9.5
that might make pH adjustments desirable.

Capital Cost Projections Summary
     The total capital cost projections include auxiliary equipment and
services common to systems, independent of the type of membrane module.
The two main items are  (1)  a building to house equipment and controls,
and  (2)  the engineering  services  (including design, equipment procurement,
construction, supervision, and start-up).
     The capital cost projections are summarized for each  of the four
cases in Table 22.  The principal differences among the four cases are, of
course, in the cost of the membrane modules.  There are also major diffe-
rences among the costs of required pretreatment.  The cost of the  auxiliaries
are the same except for Case 3  (Westinghouse).  In Case 3  the engineering
costs are considered part of the module cost.

                                  73

-------
Table 22.  CAPITAL COST PROJECTION SUMMARY FOR HYPERFILTRATION TREATMENT OF LA FRANCE WASTEWATER
                                 (7570 m3/day & 80% Recovery)
CASE NUMBER
PRETREATMENT UNIT, $
MEMBRANE MODULE UNIT, $
AUZILIARY EQUIPMENT, $
ENGINEERING, $
TOTAL, $
CONTINGENCY (10%), $
TOTAL CAPITAL, $
MEMBRANE COSTS INCLUDED
IN CAPITAL, $
UTILIZED HORSEPOWER
1
351,950
846,400
117,500
300,000
1,615,850
161,585
1,777,435

360,000
585
2
283,000
991,150
117,500
300,000
1,691,650
169,165
1,860,815

498,750
595
3
293,000
3,314,332
117,500
a
3,714,832
371,483
4,086,315

1,230,000
932
4
33,000
2,714,124
117,500
300,000
3,164,624
316,462
3,481,086

3,600
2,600
Included in cost of membrane module unit.

-------
 OPERATING COST PROJECTIONS
     The operating cost projections tabulated in Table 23 are based on
 365 operating days per year.  The costs are increnental for treating
 wastewater at an existing textile plant.  The operating costs are items
 in three principal categories:  (1)   labor,  (2)   electric power, and
 (3)  membrane replacement.  The costs are based on the wages and prices
 typical for the Southeast in the fall of 1975.   The operating cost pro-
 jections in Table 23 do not include  the value of recycleable water,
 chemicals,  or heat (energy).  The recycle potential for textile waste-
 water renovated by hyperfiltration is estimated separately in Table 24.
     The estimates of labor requirements by the  four membrane manufacturers
 were different.   However, the same labor cost is  used in the projection
 for each membrane system for consistency in comparison.   Even though the
 pilot plant experience supports the  existence of  scma variation in labor
 requirements,  this variation should  not be a major consideration in the
 comparisons among the four membrane  systems.
     The membrane life,  i.e., the replaceirEnt interval, for the polyamide
 fiber membrane and both configurations of the cellulose  acetate is taken
 as  three years.   The  replacement costs are depreciated linearly over this
 time period.   The dynamic Zr-PAA membrane replacement interval is taken
 to be one year.   Of course,  determination of  membrane life for textile
 wastewater  treatment  is beyond the scope of this pilot plant program.   The
 maximum evaluation period in the pilot plant  study was about 1000 hours.
 The experiences of the  manufacturers in other applications were the basis
 for the selection of  the replacement period for the polyamide and cellulose
 acetate membrane  systems.  For the prototype dynamic  Zr-PAA membrane system,
 the membrane replacement is a minor item.  Thus, the  accuracy of the re-
 placement interval is not significant in the total operating  cost project-
 ions.  Data with textile wastewater do support the estimated  one-year
 replacement period, however.
    The cost projections do not include amortization of capital.  Because
of effects of legislation on capital investment for environmental protection
and the fluctuations in the prime interest rate, inclusion of the amortization
                                  75

-------
Tab* 23.  OPERATE COST HOJBCnWB SUWKK FOE HYPERFIL^IO, TREMMENT OF LA FRANCE
                                             ($/day)
CASE NUMBER
PRETREMMENT UNIT
Filter Aid (@6.6<=Ag)
Chemicals (detergent & acid)
LABOR
Operating (6 man-yrs)
Maintenance (0.5 man-yrs)
Supervision
MAINTENANCE MATERIAL
ELECTRIC POWER (@ 1.5
-------
  would add no significant information to the capital cost projections
  already presented.
       The operating costs for pretreatavent are not a major item.for any
  membrane system.  The labor, electric power, and irembrane replacement
  costs are about equal for the polyamide membrane system.  The membrane
  replacement costs become progressively more important for the spiral-
  wound and tubular cellulose acetate, being the major factor for the
  tubular configuration.  The major operating cost for dynamic 2r-PM
  membranes is the electric power costs.   In-situ membrane replacement is
  a particularly small cost for the dynamic membranes.
       The daily operating cost ranges fron 12.1<:/m3  (45.7
-------
           Table 24.  NET OPERATING COST PROJECTIONS SUMMARY INCLUDING POTENTIAL RECYCLE CREDITS
-4
CO
CASE NUMBER
RECYCLE POTENTIAL, i3)
2. Salt (@ 4.4<=Ag)
3. Energy «§ 1.9C/107 J)
TOTAL RECYCLE CREDITS
UNIT OPERATING COSTS*1
NET OPERATING COSTS, «/m3
NET OPERATING COSTS, <=Agal
1

10.6
1.5
3.4
15.5
12.1
(3.4)b
(12.9)b
2

10.6
1.5
2.8
14.9
13.6
(1.3)b
(4.9)b
3

10.6
1.5
2.8
14.9
25.5
10.6
40.1
4

10.6
1.5
6.2
18.3
18.7
0.4"
1.5
         Fran Table 23
         Indicates net savings

-------
      The net operating costs, Table 24, includes credit for recycle.
 A small net savings is projected for the polyamide membrane and the
 spiral cellulose acetate membrane systems.

 COST PROJECTIONS FOR A COMBINED MEMBRANE SYSTEM
      Because of the relatively low capital and operating costs of both
 the polyamide and cellulose acetate (spiral)  mambrane systems and the
 high teitperature capability of the dynamic Zr-PAA membrane system, a
 hyperfiltration treatment facility combining two types of membranes has
 advantages over any single membrane system.
      The dye procedure employed at La France, Table 8, involves the dilution
 of the 210 F (99 C)  spent scouring and dyeing baths.  The dilution is
 accomplished with clean,  cold rinse water introduced to the dyeing machine.
 This procedure results in a slow quenching of the cloth to 165 F (74 C).
 Approximately 25% of the  water used in dyeing cycle is exhausted to the'
 drain at an average  temperature of 165 F (71  C).   The final rinsing of
 the cloth results in a mixed effluent of about 90 F (32 C).
      A dynamic Zr-PAA membrane unit can process the relatively hot portion
 (25%)  of the wastewater and effect energy recovery since with procedural
 modifications  the 165  F (71 C)  water could be directly recycled in many
 dyeing operations.   Either spiral or hollow-fiber membranes can process
 the  remaining portion  (75%)  of the wastewater without requiring a cooling
 tower.  The  following  approximations of capital and operating costs
 illustrate the  cost  advantages of such a combined system.   A detailed
 economic analysis of a combined system was not carried out, however.
     Because of the  increased membrane  flux with  temperature,  each dynamic
 Zr-PAA membrane module has  a product- flow rate of 2.06 dmVmin at 71  C.
 Therefore, to process  25% of the  7570 mVday wastewater to  82.1% product
 recovery requires 524 modules.  This is  14% the size of the membrane  unit
 used in the cost projections summarized in Table  22.  As a  first approxi-
mation then, the  capital costs of this smaller unit is  14%  of  $3,481,086
 or $487,352.
                                   79

-------
      The capital cost of the polyanti.de, or spiral cellulose acetate,
 portion of the combined unit would be simply 75% of the value given in
 Table 22 with the exception that the entire cost of the cooling tower
 my be eliminated since the mixed effluent temperature is 32 C.  The
 capital cost for the unit to process the relatively cool rinse water is
 then $1,151,576 for a polyamide membrane unit, or $1,197,611 for a
 spiral cellulose acetate membrane unit.
      The approximate total capital cost for a combined membrane treatment
 is $1,650,000.  A comparison with Table 22 indicates this is less than
 the capital cost of any single membrane system.
      The operating costs for the combined membrane system are also
 approximated from the details developed for the individual membrane
 systems.  The operating costs, excluding labor, are proportional to
 system size.   That is, the operating cost for the dynamic Zr-PAA manbranes
 is 14% of $1162.88 (Table 23), or $162.80.  The operating cost of the
 polyamide membrane unit is 75% of $661.72 (Table 23),  or $496.29.  The
 labor costs are not reduced,  but are taken to be the same for the combined
 system as for any other membrane unit,  i.e.,  $252.56.   The approximate
 operating costs for the combined system is the sum of $162.80,  $496.29,
 and $252.56,  or $911.65.  The unit operating cost is 12<=/m3 (45.6C/1000
 gallons)  of wastewater processed.   Comparison of this  result with Table  23
 shows that the operating cost of the combined system is less than for
 any single membrane system.
      The  credit for recycled  water and salt is the same for all membrane
 systems  (Table 24),  10.6
-------
that a combined system to take advantage of the relatively low costs
of sore roeirfcranes and the energy conservation potential, by direct re-
cycle of hot water, of other nembranes, should be considered for each
application characterized by the utilization of hot dye baths and
relatively cooler, 'higher volunes of rinse water.  Further, procedural
alterations to permit direct recycle of dye baths renovated at full
process tenperature couM possibly yield even further energy con-
servation.
                                  81

-------
                              REFERENCES


 1.   Kraus, K. A., A. J. Shor, and J. S. Johnson, Jr.  Desalination.
     2_:243.   1967.                                     	

 2.   Larson,  T. J.  Desalination.  7^:187.  1970.

 3.   Brandon, C. A., J. S. Johnson, Jr., R. E. Minturn, and J. J. Porter.
     Journal  of Textile Chemists and Colorists.  _5{7) :134.  1973.

 4.   Environmental Protection Agency, Demonstration Project #8800929;
     Thomas N. Sargent, Project Officer, Southeast Water Laboratory,
     Athens, Georgia.

 5.   Anonymous.  Chemical Engineering.  7£(27):53.  1971.

 6.   Coit, R. L.  Proceedings of Third International Symposium on Fresh
     Water fran the Sea.  2;351.   WTol       	  	

 7.   Johnson, J. S., Jr.  "Polyelectrolytes in Aqueous Solutions."  Reverse
     Osmosis Membrane Research.   379-403.   1972.                    	

8.   Fremont,  H. A., D.  C.  Tate,  and R.  L.  Goldsmith.  "Color Removal frcm
     Kraft Mill Effluents by Ultrafiltration."   Final Report,  Project
     #3800261, Environmental Protection Agency.  1973.
                                 82

-------
SECTION  X





APPENDIX A
    83

-------
                                APPENDIX A
         WATER SAMPLING SCHEDULE,  PROCEDURE,  AND CHEMICAL ANALYSES

  SAMPLING SCHEDULE
       During this project,  the detailed chemical analyses of a number of
  samples were required for  the following reasons:   (1)   to characterize
  the La France composite wastewater,   (2)  to characterize the product
  water and concentrate employed in direct reuse  dyeing operations, and
  (3)   to evaluate the  performance of the pilot plant hyperfiltration units.
  In  order to achieve these  goals, a sampling schedule and chemical analysis
  routine was established and maintained  by pilot plant operators.  This
 Appendix describes the sampling schedule, sampling procedures, and the
 chemical tests performed on the collected water samples.
      In order to characterize the composite wastewater frcm the La France
 plant,  several 0.1 dm3 samples of raw wastewater were collected during
 work hours and the samples were mixed at the end of the week to yield a
 composite sample of wastewater.
      The sample described as composite product water and composite con-
 centrate were drawn from the 5.6 m3 storage tanks at the end of each
 collection period.  The composite raw waste sample which was used as
 feed for the pilot plant was prepared by collecting a sample of raw waste
 from each 2.3 m3 raw feed batch to be processed and mixed at the end of
 the  collection period. A sample of tap water was analyzed for comparison
 with the composite product  water for each reuse dyeing.

 COLLECTION AND STORAGE OF SAMPLES
     To insure that representative  samples were obtained, the following
 guidelines were established for sample storage  during the project.   Samples
 were analyzed within a two  week period after collection  and  stored before
 analyses at  a temperature of less than 5 C.  No additives or preservatives
were added to any of the samples because they often affect the results of
many of  the analyses.

                                  84

-------
  ANALYTICAL PROCEDURES
       The chemical analyses were performed by Texidyne, Inc.  Those
  chemical parameters  subject to rapid change after sample collection
  
-------
 Total Organic Carbon  (TQC)
      TOG is evaluated by difference.  Total carbon is first determined
 by passing a sample aliquot into a 950 C furnace and conversion of all
 carbon present to carbon dioxide.  Inorganic carbon is found by passing
 a second aliquot into a 150 C oven where only the inorganic carbon is
 converted to carbon dioxide.  The carbon dioxide from both channels is
 determined by an infrared detection system.  Standard solutions of
 sodium carbonate and biocarbonate ,  and potassium acid phthalate are used
 to calibrate the carbon channels.  Total organic carbon is then evaluated
 as the difference between total carbon and inorganic carbon.
      Determination of pH is made with a potentiometric pH meter calibrated
 with buffers of known pH value.

 Alkalinity
      Alkalinity is determined by titrating a known volume for the sample
 to a pH of 4.5  with a standard acid solution.  The results  are expressed
 as mg/A calcium carbonate.

 Hardness
      Hardness is determined by cotplexing  the calcium and magnesium ions
 present in an aliquot of the sample with EDTA solution to a titrimetric
 end point  indicated by Eriochrcme Black  T.  The results are expressed as
mg/£ calcium  carbonate.

Total Solids
     Total solids is taken as  the weight of solid residue after an aliquot
of the homogeneous sample is dried  at 105 C for 24 hours.  The results
are expressed as mg/£ solids.
                                  86

-------
 Volatile Solids
      Volatile solids is taken to be the weight of solid material which
 volatilizes when the residue of the total solids determination is heat-
 ed to 650 c for 15 minutes.   The result is expressed as rag/A.
 Dissolved Solids
      Dissolved solids is the weight of solid matter remaining after a
 sampOfi is filtered at roan temperature through Whatman #42 filter paper
 or equivalent, and a measured  aliquot of the filtrate is dried at 105 C
 for 24 hours.   The result is expressed as mg/£.

 Color

      The determination of color  is  made by  comparing the absorbance of
 the sample at  410  m with those  of  standard platinum-cobalt color solutions,
 also at 410 rm.  The results are expressed  as platinum-cobalt color units.

 Turbidity

      Turbidity is  measured using a  nephelcmeter type turbidimster.   Light
 scattered by the sample  is incident upon a  photo-tube, which is connected
 to a meter movement.   Calibration is made against standards of known
 turbidity.   The results  are expressed  in Formazin Turbidity Units (PTU).

 Conductivity

      A conductance bridge  and cell  of known cell constant calibrated
 against standard potassium chloride solutions is used for determining
 conductivity.  The result  is expressed  in micranhos  per  centimeter
 (nmho/cm).

Metals

     Metals are determined by atonic absorption spectrophotoitetry with
comparison made to standards formulated for the various metals according

                                  87

-------
to guidelines presented in Perkin-Elmer Analytical Msthods for Atomic
Absorption Spectrophotometry.
     All metals except mercury were determined with an air acetylene
flame.  Msrcury was determined by the flameless technique.  It should
be noted that, because of this special technique, mercury can be
reported in the yg/£ range, while other metals are limited to the
mg/£ range.

Rajection
     The observed rejection is defined by the relationship

                      R    = i -  concentration of product
                       obs        concentration of feed
                                  88

-------
SECTION XT





APPENDIX B
    89

-------
                                APPENDIX B
                      PRODUCTION SCALE FEUSE DYEINGS

      The production scale reuse dyeings demonstrated the technical
 feasibility of direct recycle of both the product water and concentrate
 from hyperfiltration of cotposite wastewater.  After collection of
 sufficient water for reuse, 1.9 - 5.7 m3 of concentrate and 11.4 - 17 m3
 of product water, mixed samples were used in the laboratory, at the
 plant, to develop production scale dye formulations for use in a two-
 piece beck, Machine No. 19.
      The product water was found to be reuseable with no adjustment of
 standard dye formulations.  Even the most critical shade, a light covert
 shade on a 54% nylon - 46% viscose blend fabric, was repeatedly achieved
 with no difficulties.   The concentrate required special formulations to
 produce standard comtercial shades.
      For each test dyeing, standard production procedures were followed
 in the dyehouse.   The  standard dyeing procedure, given in Table 8 in the
 text,  involves scouring and rinsing steps  in addition to the dyeing and
 shade  adjustment.
     Two types of  plant dyeings were carried out:   (1)   separate dyeings
 with the product water and with the  concentrate, and  (2)  one dyeing
 combining both the concentrate and the product water.   When  used separately,
 the product water was used in  all  of the six scouring,  rinsing,  and dyeing
 steps in the standard procedure.   When used  in combination,  the product
water was used in  all steps except the dyeing;  the dyebath was the  concen-
trate.  When used separately,  the  normal process water  was used for scour-
ing and rinsing with the concentrate as the dyebath.
     In this Appendix are given the details of  the water analyses of  the
product water and concentrate, the standard and special dye  formulations,
and the evaluation of each test cycle.  Cycle #11, #13, and  #15  are omit-
ted because no dyeings were done during these periods which were  devoted
solely to equipment performance evaluations.
                                   90

-------
CYCLE #1


     The analyses of the average feed to the DuPont module, the product

water, and the concentrate are tabulated in Table B-l.



      Table B-l.  WATER ANALYSES FOR CYCLE #1 (March 22, 1973)
COD, mg/£
BOD, mg/Jl
TOC, mg/Jl
pH
Alkalinity, mg/Jl
Hardness, mg/fc
Total Solids, mg/Jl
Volatile Solids, mg/Jl
Dissolved Solids, mg/&
Color (Pt-Co units)
Turbidity, F.T.U.
Conductivity (wriho/cm)
Metals
Calcium, mg/Jl
Zinc, mg/Jl
Magnesium, mg/H
Chranium, mg/Jl
Copper, mg/A
Iron, mg/Jl
Mercury, ygA '••",
Manganese, mg/£
Sodium, mg/Jl
Feeda
Water
Analyses
160
45
36
6.5
50
40
1030
140
980
500
44.0
1150

1.0
4.8
0.51
-
0.04
0.3
-
-
—
Product
Water
Analyses
25
10
3
6,1
10
30
100
30
100
30
2.4
180

0.5
<0.04
<0.01
-
0.04
0.3
-
-
-
Concentrate
Water
Analyses
425
70
87
6.7
110
90
2360
200
2330
850
39.0
2200

3.0
9.7
1.18
-
0.18
3.0
-
-
-
 a This is the analyses of a composite sample taken from the feeds that
   were used during Cycle #1 for the DuPont nodule,


                                 91

-------
Product Water
     The first plant dyeing using product water was conducted on a 54%
nylon - 46% viscose blended fabric using a dye formulation containing
7 different dyes, Table B-2.  Laboratory dyeings were conducted to
establish the suitability of the product water with the shade chosen
before the plant dyeing was performed.  This particular fabric and dye
formulation were chosen because, in the opinion of the plant dyer and
chemist, this was one of the most difficult dye systems in use in the
plant.


          Table B-2.  CYCLE #1 PRODUCT WATER REUSE DYEING3


Chemical
Acid Dye
Acid Dye
Acid Dye
Acid Dye
Direct Dye
Direct Dye
Direct Dye
Salt


Dye Name
Nylon Fast Yellow FLW
Ciba Brown 2GL
Ciba Yellow 2BRL
Irgalan Black RBL
Lumicrease Grey 3LBN
Lumicrease Orange 3LG
Lumicrease Bordeau SLR

Weight Used
Based On
% Fabric Wt.
0.018
0.039
0.017
0.016
0.027
0.030
0.006
10.
  43 kg of fabric in a dyebath of 1.5 m3 at pH = 6 - 7.
     The color obtained from the above dye formulation was a gold shade
 (light  covert).  While the causes for the production difficulties with
this shade are not documented, it is known to give more problems than most
of the dye/fabric systems used.  The problems have been attributed to the
quality of the plant water, improper cleaning of the dyeing equipment,
improper temperature control during the dyeing operation, and inaccurate
                                  92

-------
 measure of dyes and chemicals used for dyeing.  It was assumed that this
 dye/fabric system constituted a critical test for the reuse of product
 water in the plant.
      A light shade of gold was produced with the product water.  The
 dyeing operation proceeded normally with no visible problems occurring.
 The product water was used in all steps in the dyeing operation.   This
 particular fabric passed a 100-hour Weather-CHMeter Test, a severe test
 of light fastness.

 Concentrate Water
      Before a dye/fabric system was selected to be used with the  con-
 centrate water,  the plant laboratory conducted trial dyeings using the
 concentrate water as the dyebath.   This was done to select a system to
 best use the dyes present in the concentrate.  This could be successful
 only when the current production shades were similar to the shade of the
 concentrate water.   At other times a production shade had to be chosen
 that obscured the dyes present in  the concentrate water.
      The concentrate produced by the  hyperfiltration module  for the
 first cycle was a grey-green  color.   Laboratory dyeings gave grey-green
 shades on standard test fabrics.  Since no green dye shades were
 scheduled for the plant production this particular week, a tan  shade
 (Color No. 133) on a 100% cotton velour fabric was chosen for use with
 the concentrate for  this test, Table B-3.
     The tan shade was produced on the velour fabric with no difficulty
being encountered during the dyeing operation.  The results of  the light
fastness test and crock test were the sama as that obtained with normal
dyeing procedures.  The fabric was graded as first quality and  sold.
                                 93

-------
       Table B-3.  CYCLE #1 CONCENTRATE WATER REUSE DYEING3
Chemical
Direct Dye
Direct Dye
Direct Dye
Direct Dye
Direct Dye
Salt
Dye Name
Bellchem Yellow EPC
Calco Rsd 6ELL
Diphenyl F Blue 4GL
Sol Brown GEL
Sup F Blue 8GUN

Dye Used Based
Test Dyeing
0.349
0.044
0.019


20.
on % Fabric Wt
Normal Dyeing
0.341
0.025

0.043
0.029

a
  21.8 kg of fabric in a dyebath of 0.87 m3 at pH = 7.
  The fabric was finished with a Scotchgard,
                                 94

-------
CYCLE #2

     The analyses of the average feed to the DuPont module, the product
water, and the concentrate are tabulated in Table B-4.

       Table B-4.  WATER ANALYSES FOR CYCLE-#2  (April 24, 1973)
 COD,  mg/Jl
 BOD,  mg/Jl
 TOC,  mg/Jl
 pH
 Alkalinity, mg/Jl
 Hardness, mg/Jl
 Total Solids, mg/Jl
 Volatile  Solids, mg/Jl
 Dissolved Solids, mg/Jl
 Color (Pt-Co units)
 Turbidity, F.T.U.
Conductivity  (piriho/cm)
Metals
  Calcium, mg/£
  Zinc, mg/A
  Magnesium, mg/£
  Chromium, rag/A
  Copper, mg/£
  Iron, mg/Jl
  Mercury, vg/l
  Manganese, mg/Jl
  Sodium,  mg/Jl
Feeda
Water
Analyses
315
35
65
6.0
55
40
1155
175
'I 1095
810
19,0
i) 1900
Product
Water
Analyses
20
5
5
6.0
15
15
270
N.D.
270
20
0,5
580
Concentrate
Water
Analyses
815
135
200
6.5
135
120
5570
450
5540
1250
31.0
1030
                                 3.30
                                 0.25
                                 0.75
 0,1
<0.13
 N.D.
                                                              10.4
2.0
7.2
       iS^ a^yses of a cotiposite sample taken fron the feeds that
 were  used during Cycle #2 for the DuPont nodule.
                                95

-------
Product Water
     The product water was used to dye a yellow shade (Color No.  114)
on a ribbed, 100% cotton velour fabric, Table B-5.  The dyeing operation
was conducted by normal plant procedures with no problems being en-
countered.


           Table B-5.  CYCLE #2 PRODUCT WATER REUSE DYEING3


Chemical
Direct Dye
Direct Dye
Salt


Dye Name
Bellchem Yellow ETC
Intralite F Yellow 2GLL

Weight Used
Based On
% Fabric Wt.
0.046
0.600
20.
a 64.8 kg of fabric in a dyebath of 1.5 m3 at pH = 6 - 7.
Concentrate Water
     The concentrate water was used to dye a medium dark blue-green shade
 (Color No.  676 ) on a 100% cotton velour fabric, Table B-6.
     The concentrate in the laboratory produced a dull grey shade on a
test fabric.  Since the plant had no production color to match this dull
grey color, a darker color had to be used so that the dullness would not
affect the color of the final dyed fabric.  This is a limitation that
arises when the concentrate contains many different dyes and chemicals.
     The dyeing operation proceeded normally with no apparent problems.
The desired blue^green shade was obtained on the 100% cotton velour
fabric.  The crocking test was good and comparable to results obtained
with fabric dyed in the normal manner.  The fabric in that test did show
significant facing after 40-hours exposure in the Fade-O-Meter.  This was
not considered unusual for this particular shade and therefore was not

                                  96

-------
 attributed to the use of the concentrate water,   The fabric was graded
 as first quality and sold.
         Table B-6.  CYCLE #2 CONCENTRATE WATER REUSE DYEING*1
a
  44.1 kg of fabric in a dyebath of 1.5 m3 at pH = 7.
Chemical          Dye Name                  Dye Used Based on % Fabric Wt.
	          *vye iMcune                   Test Dyeing    Normal DyelnT

Direct Dye        Solo Green 5BL               i.03            0.900
Direct Dye        Intralite F Yellow 2GLL      0.018           0*032
Salt
                                                               15.
                                 97

-------
CYCLE #3

     The analyses of the average feed to the DuPont module, the product

water, and the concentrate are tabulated in Table B-7.


       Table B-7.  WATER ANALYSES FOR CYCLE #3 (May 21, 1974)
COD, mgA
BOD, mgA
TOC, mgA
pH
Alkalinity, mgA
Hardness, mgA
Total Solids, mgA
Volatile Solids, mgA
Dissolved Solids, mgA
Color (Pt-Co units)
Turbidity, F.T.U.
Conductivity (ymho/on)
Metals
Calcium, mgA
Zinc, mgA
Magnesium, mgA
Chromium, mgA
Copper, mgA
Iron, mgA
Mercury , vg/a
Manganese, mgA
Sodium, mgA
Feeda
Water
Analyses
220
40
70
6.75
45
40
855
140
825
680
1.7
1300

-
-
2.06
0.2
1.08
-
•"
Product
Water
Analyses
20
5
5
6.4
15
20
130
20
130
13
1.3
200

-
-
-
<0.4
0.56
—
"
Concentrate
Water
Analyses
455
60
no
7.0
110
80
2545
280
2480
1500
1.6
3800

-
-
-
0.84
0.3
1.24
••

   This is the analyses of a composite sample taken from the feeds that
   were used during Cycle #3 for the DuPont module.
                                 98

-------
  Product Water and Concentrate

      To establish the conpatibilit* of the product water and concentrate
  xt was  decided to use them together in a plant production dyeing.  The
  product water was used for all water needs in the dyeing procedure ex-
  cept the actual dyeing operation, *hen the concentrate was used as the
  dyebath.
                         *
      A  light blue shade (Color No. 662)  was dyed on a 65% cotton - 35%
  rayon velour, Table B-8.  The shade was selected to achieve good utili-
  zation of the dyes in the concentrate.  A 71% reduction of dyes, compared
 to that required in standard formulation, was achieved.
      The light fastness and crocking fastness of the dyed fabric was
 normal.   Even though the shade was not in the production schedule,  it is
 a catalog shade and demonstrates that savings can be achieved frcm dye
 recycling.
      This  cloth was  graded first quality  but  sold as second because the
 small yardage of  fabric  dyed was not part of  the scheduled  production.


            Table B-8.  CYCLE *3 COMBINED PRODUCT WATER
                        AND CONCENTRATE REUSE'DYEING^
Chemical          Dye Name                  Pye Used Based On % Fabric wfa.
-          ^yename                   Test Dyeing    Normal Dyeing'
Direct Dye        Sup F Blue 8GUJ
Direct Dye        Bellchem Yellcw ETC
Direct Dye        Direct Fast Red 8BIN
Direct Dye        Pyrazol F Blue
Salt
                                                  n,
  37 kg of fabric in a dyebath of 1.5 m3  at PH = 7.
                                  99

-------
CYCLE #4

     The analyses of the average  feed to the DuPont module, the product
water, and the concentrate are  tabulated in Table B-9.


        Table B-9.  WATER ANALYSES FOR CYCLE 14 (June 12, 1973)



COD, mgA
BOD, mgA
TOC, mgA
pH
Alkalinity, mgA
Hardness, mgA
Total Solids, mgA
Volatile Solids, mgA
Dissolved Solids, mgA
Color (Pt-Co units)
Turbidity, F.T.U.
Conductivity (pmho/cm)
Metals
Calcium, mgA
Zinc, mgA
Magnesiun, mgA
Chrcmium, mgA
Copper, mgA
Iron, mgA
Mercury, V9A ?
Manganese, mgA
Sodium, rag/ 1
3 rnui „ i a *-Vi*a analvrRAfi of £
Feed3
Water
Analyses
245
49
70
6.8
55
30
970
95
945
470
40
1600

2.3
-
2.9
—
—
—
—
-
240
» coiDOsite sartrx
Product
Water
Analyses
15
4
5
6.5
15
5
280
40
280
6
0.8
540

0.24
-
0.28
—
~
™"
™
—
94
Le taken from the
Concentrate
Water
Analyses
580
102
165
7.2
160
90
3020
310
2985
1000
40
4800

6.5
••
10.2
M>
" *


^*
980
feeds that
    ill^O  t^o  »»*»^* **+u*^~j ~ —^ —•— — 	a. —        •
   were  used during Cycle #4 for the DuPont module.
                                  100

-------
Product-Water and Concentrate

     The procedure of combining the product water and concentrate in
a single reuse test dyeing  (as in Cycle 13) was repeated.  The con-
centrate yielded a grey shade on the laboratory test fabric.  A rose
shade  (Color No. 405) was selected to get maximm use of the dyes in
the concentrate.  A 100% cotton velour fabric was dyed in the full
scale reuse test, Table B-10.
     The light fastness of the fabric dyed with the concentrate was
equal to the standard material.  The plant scale dyeing proceeded
normally.  The fabric was sold as first quality.
            Table B-10.  CTCIE #4 COMBINED PRODUCT WATER
                         AND OaONTRATE REUSE DYEING^
Chemical
Direct Dye
Direct Dye
Direct Dye
Direct Dye
Salt
CL *^ n f» t *• »
Dye Name
Direct Fast Red 8BIW
Bellchem Yellow ETC
Superlite Blue 8GEN
Calco Red G BLL
•• 	
Dye Used Based
0.094
0.092
0.047

10.
On % Fabric Wt.
Noxiiial Dyeina
0,167
0.047
0.088
10.
                                101

-------
CYCLE #5

     The analyses of the average feed to the DuPont module,  the product

water, and the concentrate are tabulated in Table B-ll.



       Table B-ll.  WATER ANALYSES FOR CYCLE #5  (July 7,  1973)



COD, mgA
BOD, mgA
TOC, mgA
pH
Alkalinity, nigA
Hardness, mgA
Total Solids, mgA
Volatile Solids, mgA
Dissolved Solids, mgA
Color (Pt-Co units)
Turbidity/ F.T.U.
Conductivity (ymho/on)
Metals
Calcium, mgA
Zinc, mgA
Magnesium, mgA
Chrcmium, mgA
Copper, mgA
Iron, mgA
Mercury, ygA
Manganese, mgA
Sodium, mgA
Feeda
Water
Analyses
230
45
50
6.4
45
25
990
135
930
510
45,0
2000

1.10
4.40
3.10
0.1
—
—
—
-
300
Product
Water
Analyses
15
0.3
5
6.5
25
5
440
40
440
30
3.4
1000

0.10
0.08
0.22
0.1
*""
"
"
~
160
Concentrate
Water
Analyses
690
95
220
7.2
190
135
4425
405
4230
1200
30.0
9500

9.0
8.50 ,
13.8
0.1




1400
• «• ^ i »_ •
    This is
    were used during Cycle
 (•••^•••i^mwi^BM"*"^^^^^^"-      	

. a composite sample taken from the feeds that

#5 for the DuPont module.
                                  102

-------
Product Water and Concentrate
     The procedure of combining the product water and concentrate in
a single reuse test dyeing  (as in Cycle #3) was repeated.  The con-
centrate yielded a grey shade on the laboratory test fabric.  A violet
shade  (helio) was selected to get maximum use of the dyes in the con-
centrate.  A 100% cotton velour fabric was dyed in the full scale reuse
test, Table B-12.
     The light fastness of the fabric dyed with the concentrate was
equal to the standard material.  The plant scale dyeing proceeded normally.
The fabric was sold as first quality.
            Table B-12.  CYCLE #5 COMBINED PRODUCT WATER
                         AND CONCENTRATE REUSE DYEING3
Chemical
Direct Dye
Direct Dye
Salt
Dye Name
Direct Fast Red 8BLN
Pyrazol Fast Violet 4BL

Dye Used Based
Test Dyeing
0.01
0.12
25.
On % Fabric Wt.
Normal Dyeing
0.01
0.12
25.
  37 kg of fabric in a dyebath of 1.5 m3 at pH = 7.
                                 103

-------
CYCLE #6
     The analyses of the average feed to the DuPont module, the product
water, and the concentrate are tabulated in Table B-13.

    Table B-13.  WATER ANALYSES FOR CYCLE #6 (September 20, 1973)
COD, Itq/SL
BOD, rcq/SL
Feeda
Water
Analyses
170
15
Product
Water
Analyses
25
1
Concentrate
Water
Analyses
435
10
 TOC,
 pH
 Alkalinity, mg/fc
 Hardness, mg/Jl
 Total Solids, mg/£
 Volatile Solids, mg/£
 Dissolved Solids, mg/Jl
 Color  (Pt-Co units)
 Turbidity, F.T.U.
 Conductivity  (ymho/on)
 Metals
   Calcium, icg/a
   Zinc, mg/£
   Magnesium, mg/£
   ChratuLum, mg/Jl
   Copper, mgA
   Iron, mg/£
   Mercury,
   Manganese,
   Sodium, mg/£
6.6
45
45
780
130
755
595
55
850

1.0
4.0
4.0

0.08
250
7.1
15
10
285
60
285
60
6.3
520

0.5
0.7
0.9

0.08
90
7.4
140
130
3425
315
3435
1250
80
6200

6.0
9.0
17

2.0
                             1120
 a This is the analyses of a corposite sample taken frcm the -feeds that
   were used during Cycle #6 for the DuPont nodule.
                                 104

-------
 Product Water

      The product water was used with the same dye/fabric system as
 Cycle #1, i.e. a goJd shade (light covert) on a 54%'nylon - 46% viscose
 bland.  During Cycle #6, 90% of the wastewater was recovered as product
 water.  Therefore, the product water contained more impurities than in
 the previous reuse tests.  Thus it was decided to again check separately
 its suitability for plant use, see Table B-2.  In Cycle #6, 45.4 kg of
 fabric were dyed in a 1.5 m3 dyebath at a pH of 6 - 7.
      The light fastness and wash fastness of the dyed fabric was good
 and comparable to that obtained with normal plant dyeings.   No adverse
 results were observed fron the use of the product water in the plant
 dyeing.

 Concentrate Water

      The concentrate  water was used with the same tan shade (Color No  133)
 on  100% cotton velour fabric,  dyed in Cycle #1.   This shade was repeated
 so  that a comparison  could be  made of the results obtained  with the dyeing
 in  Cycle #1, Table B-14.   This corparison was desired because at 90%
water recovery, the concentrate contains more dyes and dinpurities.
      The dyeing operation proceeded normally with no apparent problems.
The same shade was produced on the cotton velour  fabric as  was used for
the concentrate in Cycle #1.  The  light  fastness  of  the dyed fabric was
comparable to that obtained with regular production  dyeings.   The material
was graded as first quality and sold.
                                  105

-------
      Table B-14.  CYCLE #6 CONCENTRATE WATER REUSE DYEINGa
Dye Used Based OH % Fabric Wt.
Chemical
Direct Dye
Direct Dye
Direct Dye
Direct Dye
Direct Dye
Salt
Dye Name
Bellchem Yellow EPC
Calco Red 6BLL
Diphenyl F Blue 4GL
Sol Brown GRL
Sup F Blue 86IN

Test Dyeing
0.280
0.015
0.010


20.
Normal Dyeing
0.341
0.025

0.043
0.029
20.
89.4 kg of fabric in a dyebath of 1,5 m3  at pH = 7.
                               106

-------
CYCLE #7



     The analyses of the average feed to the ORNL module, and the

concentrate are tabulated in Table B-15.




      Table B-15.  WATER ANALYSES FOR CYCLE #7 (November 6,  1973)



GCD, mg/Jl
BCD, mg/A
TOC, mg/£
pH
Alkalinity, mg/A
Hardness, rcg/i
Total Solids, mg/£
Volatile Solids, itg/H
Dissolved Solids, mg/£
Color (Pt-Co units)
Turbidity, F.T.U.
Conductivity (varho/cm)
Metals
Calcium, mg/Jl
Zinc, mg/&
Magnesium, mg/Jl
Chromium, mg/£
Copper, mg/A
Iron, mg/£
Mercury, yg/s, t
Manganese, mg/Jl
Sodium, mg/A
Feed3
Water
Analyses
150
10
25
8.1
75
15
860
120
820
510
35
1400

0.53
1.70
1.87
—
_
4.0
—
_
250
Concentrate
Water
Analyses
190
15
_
8.0
155
50
1580
165
1480
1300
8.5
1700

0.96
2.4
4.5
^

18
_

470
          , , -.—-— °f a oonpcsite sample taken from the feeds that
  were used during Cycle #7 for the OHNL nodule.


                                107

-------
Concentrate Water
     For Cycle #7, the concentrate water was used for the dyebath formu-
lation and regular process water was used for all other phases of the
dyeing operation.  The product water had been used interchangeably with
process water in previous dyeings and its suitability for plant use had
been demonstrated.  In Cycle #7, the primary interest was in the use of
the concentrate to further demonstrate dye recovery.
     The concentrate water produced a dyeing with a light pink shade on
cotton test fabric.  Because of this, a rose shade  (Color No. 405) was
chosen for the plant dyeing of a 100% cotton velour fabric, Table B-16.
The plant dyeing proceeded normally with no problems being observed with
the use of the concentrate water.
     The light fastness was the same as that normally obtained with
fabric dyed this shade.  The fabric was sold as first quality.


        Table B-16.  CYCLE # 7 CONCENTRATE WATER REUSE DYEING3

Chemical
Direct Dye
Direct Dye
Direct Dye

Dye Name
Sup F Blue 8GLN
Bellchem Yellow ETC
Direct Fast Red 8BLN
Dye Used Based
Test Dyeing
0.060
0.125
20.
On % Fabric Wt.
Normal Dyeing
0.146
0.028
15.
  69.4 kg of fabric in a dyebath of  1.5 m3  at pH = 7,
                                  108

-------
CYCLE #8
     The analyses of the average feed to the OKNL module, and the
concentrate are tabulated in Table B-17.

      Table B-17.   WATER ANALYSES FOR CYCLE #8 (November 26,  1973)
COD, rcg/i
BOD, Kg/a
TOC,
                                      355
                                      970
                                      450
                                      2.8
                                       Feedc
                                       Water
                                       Analyses^
                                       220
                                       35

 P                                     6.8
 Alkalinity, mg/Ji                      35
 Hardness,  mg/A                        20
 Total Solids,  mg/SL
 Volatile Solids, mg/SL
 Dissolved  Solids, mg/a
 Color (Pt-Co units)
 Turbidity,  F.T.U.
 Conductivity (yirho/cm)
 Metals
  Calcium,  rng/A
  Zinc, mgA
  Magnesium, mg/fc
  dhromium, mg/£
  Copper,
  Iron, mg/A
  Mercury
  Manganese
  Sodium, mg/A                        325

a This is the analyses of a composite saitple taken from
  were used during Cycle #8 for the ORNL module.
                                      1.90
                                      2.63
 Concentrate
 Water
 Analyses
 415
 45

 7.5
 115
 55
 2510
 275
 2450
 1680
 15.0
 1850

 8.1
3.14
9.6
                                                          40.0



                                                          780
                                                          •^M^Wi
                                                        the feeds that
                                109

-------
Concentrate Water
     As in Cycle #7, the concentrate water was used with the regular
process water and the product water was not used in the plant.
     The concentrate water produced a dyeing with a light blue-grey
shade on cotton test fabric.  Because of this a blue-green shade (Color
No. 616) was chosen for the plant dyeing on a 100% cotton velour,
Table B-18.
     The light fastness of the dyed fabric was the same as that obtained
with fabric dyed by normal procedures.  The dyed fabric did show some
slight side-to-center shading.  This was probably the result of a twist
in the fabric rope during dyeing.  This problem was not associated with
the concentrate water.  The fabric was sold as first quality.
        Table B-18.  CYCLE #8 CONCENTRATE WATER REUSE DYEING3

Chemical
Direct Dye
Direct Dye
Direct Dye
Direct Dye
Salt

Dye Name
Sup F Blue SOU
Sup Yellow ETC
Direct Fast Red 8BLN
Pyrazol Blue 2GLN

Dye Used Based
Test Dyeing
0.420
0.065


25.
On % Fabric Wt.
Normal Dyeing

0.099
0.016
0.517
15.
  45.4 kg of fabric in a dyebath of 1.5 m3 at pH = 7.
                                  110

-------
CYCLE #9

     The analyses of the average feed to the ORNL meddle, the product

water, and the concentrate are tabulated in Table B-19.


      Table B-19.  WATER ANALYSES FOR CYCLE #9 (January 23, 1974)
OCD, mgA
BOD, mgA
TOG, mgA
pH
Alkalinity, mgA
Hardness, mgA
Total Solids, mgA
Volatile Solids, mgA
Dissolved Solids, mgA
Color (Pt-Co units)
Turbidity, F.T.U.
Conductivity (yitiho/an)
Metals
Calcium, mgA
Zinc, rogA
Magnesium, mgA
Chromium, mgA
Copper, ngA
Iron, mgA
Marcury, ygA
Manganese, mgA
Sodium, mgA
Iteeda
Water
Analyses
230
35
-
6.6
45
25
1085
170
1050
180
20
1050

0.88
5.20
2.76
—
-
2.38
-
-
350
Product
Water
Analyses
30
2.7
—
7,2
40
4
630
95
630
30
1.5
715

0.17
0.06
0.58
-
-
0.63
-
-
270
Concentrate
Water
Analyses
265
30
-
7.1
105
95
1515
285
1445
470
30
1200

6.40
7.04
5.76
-
-
18.1
-
-
505
  a This is the analyses of a oorrposite sanple taken from the feeds that
    were used during Cycle #9 for the OINL nodule.

                                  Ill

-------
Product Water
     The product water was used to dye the same shade  (light covert) and
fabric  (54% nylon - 46% viscose) used with the product water in Cycle #1.
This was done so a comparison could be made between tiie product water
from the DuPont hollow fiber polyamide membrane module and the product
water from a dynamic membrane module.  This light shade provided a
critical test for the reuse of the product water, see Table B-2,  In
Cycle #9, 48 kg of fabric were dyed in a dyebath of 1.5 m3 at pH of 6 - 7.
     The desired shade was obtained with no problems being encountered.
The dyed fabric passed all of the tests for light fastness and crocking.

Concentrate Water
     The concentrate water was used to dye a light tan shade (oyster) on
100% cotton velour, Table B-20.No dyes were added to the concentrate water
and the shade produced was due solely to the dyes in the concentrate.
     The dyeing operation proceeded normally with no apparent problems.
The fabric exhibited satisfactory light fastness and was sold commercially.
        Table B-20.  CYCLE #9 CONCENTRATE WATER REUSE DYEING
Chemical
Salt
Dye Name
Dye Used Based On % Fabric Wt.
 Test DyeingNormal Dyeing
  10.                 -b
  21.8 kg of fabric in a dyebath of 1.5 m3 at pH = 7.
  No dyes were added to the  dyebath.
                                  112

-------
CYCLE #10
     The analyses of the average  feed to the Westinghouse module, the
product water, and the concentrate  are tabulated in Table B-21.

    Table B-21.  WATER ANALYSES FOR CYCLE #10  (January 22, 1974)
COD, icq/l
BCD. ma/A
Feed3
Water
Analyses
150
15
Product
Water
Analyses
200
1.3
Concentrate
Water
Analyses
385
25
 TOC, mgA
 P»
 Alkalinity, mgA
 Hardness, ragA
 Total  Solids, mgA
 Volatile Solids, mgA
 Dissolved Solids, mgA
 Color  (Pt-Co units)
 Turbidity,  F.T.U.
 Conductivity  (ymho/cm)
 totals
    Calcium,  mgA
    Zinc, mgA
    Magnesium, mgA
    Qiromiun, mgA
    Copper,  mgA
    Iron, rag A
    Mercury, pg/A ' •
    Manganese,
    Sodium, mg/Jl
6.6
25
30
655
120
645
490
25
950

1.43
6.00
5.84
 2.38
 190
6.2
3
6
215
75
205
60
6
340

0.88
0.82
0.78
 1.13
 55
7.1
90
105
1765
240
1740
960
125
2250

2.57
16.0
8.00
 3.00
 600
  a This is the analyses of a cottposite sanple taken from the feeds that
    were used during Cycle #10 for the Westinghouse module.
                                  113

-------
 Product Water
      The product water was used to dye the same shade  (light covert) and
 fabric  (54% nylon - 46% viscose) used with the product water in Cycle #1.
 This was done so a comparison could be made between the product water
 from the DuPont hollow fiber polyamide membrane module and product water
 from the Westinghouse cellulose acetate membrane module.  This shade
 provided a critical test for the reuse of the product water, see Table B-2,
 In Cycle #10, 46.2 kg of fabric were dyed in a dyebath of 1.5 m3 at pH
 of 6 - 7.
      The desired shade was obtained with no problems being encountered.
 The dyed fabric passed all of the tests for light fastness and crocking.

 Concentrate Water

      The concentrate water was  used to  dye a burnt-orange shade (Color
 No.  214), on 100% cotton velour fabric, Table  B-22.   The concentrate
 water gave  a light grey  shade by itself so little  dye was present in the
 concentrate.
     The dyeing operation proceeded normally with  no  apparent problems.
A burnt-orange shade was produced on a cotton velour  fabric.  The  light
fastness of the dyed fabric was comparable to that obtained with regular
production dyeings and the fabric was sold as first quality.
        Table B-22.  CYCLE #10 CONCEOTMTE WATER REUSE DYEING3

Chemical
Direct Dye
Direct Dye
Direct Dye
Salt
Dye Used Based On % Fabric Wt.
Dye Name
Fastusol Orange LTG
Supra Light Fast Blue 8GLN
Fast Red 8 BLN

Test Dyeing
1.500
0.020
0.065
20.
Normal Dyeincj
1.500
0.040
0.080
20.
 44 kg of fabric in a dyebath of  1.5 m3  at pH = 7.

                                 114

-------
CYCLE #12
     The analyses of the average feed to the DuPont module, the product
water, and the concentrate are tabulated in Table B-23.

      Table B-23.  WATER ANALYSES FOR CYCLE #12  (March 4, 1974)
 OCD, mg/£
 BOD, lug/Si
 TOC, mg/£
 pH
 Alkalinity, mg/£
 Hardness, mg/&
 Total Solids,  icg/Si
 Volatile Solids, mg/t
 Dissolved Solids, ng/i
 Color (Pb-Co units)
 Turbidity,  F.T.U.
 Conductivity (vimho/on)
 Metals
  Calcium, mg/£
  Zinc, mg/Jl
  Magnesium, mg/Ji
  Chronvium, mg/£
  Copper, mg/Jl
  Iron,
  Mercury,
  Manganese, mg/i
  Sodium, mg/A

a This is the analyses of a coiposite sartple taken from the
  were used during Cycle #12 for the DuPont nodule.
 Feed3
 Water
 Analyses
 no
 15

 6.5
 30
 50
 1160
 155
 1150
 320
 5.5
 1400

 7.20
 3.60
 9.00
0.07
395
 Product
 Water
 Analyses
 10
 2

 6.4
 10
 3
 230
 65
 230
 20
 2.0
 400

 1.00
 0.50
 0.42
0.04
75
  Concentrate
  Water
  Analyses
  365
  15

  6.8
  95
  245
  4320
  245
  4320
  920
  3400
  3400

  34.0
  7.20
  27.0
 0.45
 1470
•••••••••VH^
feeds that
                                115

-------
Product Water and Concentrate
     The product water and concentrate were used together in this dye
cycle.  The concentrate gave a light tan shade on a cotton velour test
fabric.  After checking several production shades for which the con-
centrate could be used, a burnt-orange shade (Color No. 212) was select-
ed, Table B-24.
     A burnt-orange shade was produced on a 100% cotton velour fabric.
No problems were encountered during the dyeing operation and the fabric
was graded as first quality.
           Table B-24.  CYCLE #12 COMBINED PRODUCT WATER
                        AND CONCENTRATE REUSE DYEING21
Chemical
Direct Dye
Direct Dye
Direct Dye
Direct Dye
Salt
Dye Name
Diaz-Orange 5JA
LumHDR-Brown 3LB
Dir. F-Fted 8BIN
Sol Brown GRUST

Dye Used Based
Test Dyeing
1.350
0.020
0.080

25.
On % Fabric Wt.
Normal Dyeing
1.780
-
0.090
0.070
15.
  23.6 kg of fabric in a dyebath of 1.5 m3 at pH 6 - 7,
                                  116

-------
CYCLE #14

     The analyses of the average feed to the Gulf module, the product
water, and the concentrate are tabulated in Table B-25.


      Table B-25.  WATER ANALYSES FOR CYCLE #14 (May 7, 1974)



COD, mg/Jl
BOD, rag/A
TOC, mgA
pH
Alkalinity, mg/ji
Hardness, mg/A
Total Solids, rrg/A
Volatile Solids, mg/Ji
Dissolved Solids, mg/£
Color (Pt-Co units)
Turbidity, F.T.U.
Conductivity (yrriho/cm)
Metals
Calcium, mg/&
Zinc, mg/fc
Magnesium, mg/fc
Chromium, mg/A
Copper, mg/Jt
Iron, icg/i
Mercury, yg/A1
Manganese, mg/£
Sodium, mg/Jl
Feeda
Water
Analyses
160
10
35
6.2
50
75
670
145
655
280
30
580

1,80
0.96
3.10
0.30
0,12
0.14
-
0.14
225
Product
Water
Analyses
25
1
5
5.9
8
0.5
45
15
50
40
2.5
80

0.08
0.04
0.02.
0.10
0.04
0.14
-
0.03
15
Concentrate
Water
Analyses
430
20
230
6.7
160
190
3025
275
3025
1100
35
2000

7.50
3.04
15.0
0.60
2.50
0.14
_
0.60
1090
                  i.         .     v
  were used during Cycle #14 for the Gulf module.
fran the feeds that
                                  117

-------
Product Water and Concentrate
     The product water and concentrate were used together in this dye
cycle, also.  The concentrate gave a grey-green shade on a cotton test
fabric.  After checking several production shades for which the con-
centrate could be used, it was decided to select a gold shade  (Color
No. 175) which had not previously been used in the pilot study, Table
B-26.
     The gold shade was produced on a 100% cotton velour fabric.  No
problems were encountered during the dyeing operation and the fabric
was graded as first quality.
           Table B-26.  CYCLE #14 COMBINED PRODUCT Wk
                        AND CONCENTRATE REUSE DYEING3
Chemical
Direct Dye
Direct Dye
Direct Dye
Direct Dye
Salt
Dye Name
Diaz-Orange 5JA
Intralite Green RT.T.
Intralite Red 6BLL
Bellchem Yellow EFL

Dye Used Based
Test Dyeing
0.900
0.040
' 0.020
0.030
20.
On % Fabric Wt.
Normal Dyeing
0.950
0.061
0.022
-
15.
  71.2 kg of fabric in a dyebath of 1.5 ra3 at pH = 6 - 7.
                                 118

-------
CYCLE #16
     The analyses of the average feed to the Selas module,  the product
water, and the concentrate are tabulated in Table B-27.

      Table B-27.  WATER ANALYSES FOR CYCLE #16  (July 9,  1974)
 COD, rag/A
 BOD, mg/Jl
 TOC, mg/Jl
 PH
 Alkalinity, mg/Ji
 Hardness, rag/A
 Total Solids, mg/A
 Volatile Solids,
 Dissolved Solids,  nvg/£
 Color (Pt-Co units)
 Turbidity,  F.T.U.
 Conductivity (prriho/cm)
 Metals
  Calcium,  itg/s,
  Zinc, mg/SL
  Magnesium, mg/£
  Chromium, mg/Ji
  Copper, mg/A
  Iron, rag/A
  Mercury, yg/jj,
  Manganese, mg/Ji
  Sodium, rog/A
Feed3
Water
Analyses^
160
—
30
7,1
40
55
805
780
295
6.3
1250
5.20
0.94
4.40
Product
Water
Analyses
15
-
5
9.2
20
20
195
190
30
0.45
450
0.20
0.02
0.26
Concentrate
Water
Analyses
255
55
100
9.0
250
130
3110
3055
190
18
4200
15.5
1.80
12.0
                                119

-------
Concentrate Used with Regular Plant Water
     The product water was not used in a plant scale dyeing because of
the results of several earlier recycle dyeings which established that
water of this quality could be used interchangeably with process water.
The concentrate gave a grey-green shade on a cotton velour test fabric.
After checking several production shades for which the concentrate
could be used, a green shade (special) was selected, Table B-28.
     A medium green shade was produced on a 100% cotton velour fabric.
No problems were encountered during the dyeing operation and the fabric
was graded was first quality.
        Table B-28.  CYCLE #16 CONCENTRATE WATER REUSE DYEING3
Chemical
Direct Dye
Direct Dye
Direct Dye
Salt
Dye Name
Int. Green KT.T.
Sup Yellow ETC
Dir. Red 5BIW

Dye Used Based
Test Dyeing
0.050
0.170
0.015
20.
On % Fabric Wt.
Normal Dyeing
_b
-
-
—
  16.3 kg of fabric in a dyebath of 1.5 m3 .at pH = 6 - 7.
 No dyes were added to the dyebath.
                                  120

-------
SECTION  XII





 APPENDIX C
    121

-------
                        Table 0-1.   PEHTORttNOS OF HYPEFFnaj»nCN tfXVIES IN TOE IA FRNEE PHOT PIJWT

                                     Rejection and Absoluts Values of OOD, BCD, TOC, and
to
NJ
Sanple Operating
nunber tirae(hrs)
4
7
12
16
22
23
24
25
26
27
28
29
31

33
35
36
37
39
42
44
46
48
50
52
53
Cycle No.
7
16
13
27
37
49
55
61
70
• 76
84
88
92
Cycle No.
94
102
106
108
119
131
145
150
155
161
170
179
CCD
S
P
C R%
S
BCD
P
C
R%
1 - DuPont Penneator I7753N
730 20 1370 97.3 -
400 20 590 95.0 -
DuPont Penneator I7725N
160 10 350 93.8 -
200
195
130
295
300
205
190
170
215
175
20
20
10
10
10
15
15
35
60
15
430 90.0
405 89.7
300 92.3
505 96.6
415 96.7
280 92.7
270 92.1
380 79.4
315 72.1
250 91.4
_
35
_
20
—
-
-
50
—
—
_
<1
_
2
-
-
-
20
_
_
_
125
—
40
-
-
-
130
—
-
_
>97.1
_
90.0
-
-
-
60.0
-
_
S
140
45
30
35
25
30
75
70
65
45
35
45
45
TOC
P
5
5
2
3
15
3
4
2
7
3
7
-
4
C
245
135
100
75
70
55
160
115
90
80
75
65
80
S*
96.4
88.9
93.3
91.4
40.0
90.0
94.7
90.7
89.2
93.3
80.0
-
91.1
S
7.0
7.8
6.1
6.4
6.8
6.3
6.8
6.6
6.8
6.8
6.6
6.6
6.8
PH
P
8.0
8.0
5.6
5.7
6.1
5.8
6.3
6.2
6.4
6.2
6.2
6.4
6.4

C
7.2
7.2
6.4
6.8
6.9
6.6
7.2
6.9
6.8
7.0
7.3
6.8
6.5
2 - DuPont Penneator I7725N
700
415
540
940
330
375
445
650
795
1040
970
1155
20
1
1
30
15
30
70
85
100
195
180
195
870 97.1
615 99.8
790 99.8
1235 96.8
445 95.5
525 92.0
620 84.3
995 86.9
1260 87.4
1590 81.3
1515 81.4
1795 83.1
90
—
—
—
-
-
65
-
-
220
-
—
15
-
-
-
-
_
15
-
-
60
-
-
125
-
-
-
-
-
105
-
-
295
-
-
83.3
-
-
-
-
-
76.9
-
-
72.7
-
-
130
110
130
260
70
100
115
190
335
310
380
315
10
10
5
15
10
5
15
20
25
50
10
60
185
190
235
445
125
140
175
385
605
655
495
590
92.3
90.9
96.2
94.2
85.7
95.0
87.0
89.5
92.5
83.9
97.4
81.0
6.7
6.3
6.2
6.4
6.3
6.4
6.4
6.6
6.8
6.7
6.9
7.1
5.9
6.0
6.1
6.0
6.0
6.2
5.9
6.2
5.9
6.3
6.2
6.3
6.9
6.8
6.7
6.4
6.5
6.6
6.5
7.0
7.3
7.0
7.1
7.2

-------
                                                       Table C-l.  (continued)
hJ
CJ
Saople
nunber

55
60
61
65
frm
67
f A
69
71
73
"TC
75

77
79
81
82
84
86
88
89
91

94
96
99
101
104
108

116
117
118
120
Operating
time(hrs)
Cycle No,
188
209
217
231
284
326
400
423
427
Cycle No.
24
28
37
41
49
62
148
170
218
Cycle No.
236
251
275
284
305
337
Cycle No.
437
439
442
445
COD
S P C R% S
. 3 - DuPont Pexmeator I7725N
500 55 760 89.0 -
645 45 850 93.0 -
235 35 330 85.1 -
245 . 40 455 83.7 25
45 15 85 66.7 -
45 15 60 66.7 -
280 40 380 85.7 55
130 30 165 76.9 -
85 35 165 58.8 -
4 - DuPont Pezneator I7753N
590 30 850 94.9 -
440 25 615 94.3 -
390 35 485 91.0 -
350 30 495 91.4 -
290 20 495 93.1 -
280 55 380 80.4 36
440 25 560 94.3 75
450 15 575 96.7 -
150 10 190 93.3 -
5 - DuPont Pezneator I7753N
540 5 735 99.1 -
690 40 790 94.2 -
440 40 495 90.9 -
260 30 290 88.5 55
840 35 1025 95.8 -
420 20 460 95.2 -
6 - DuPont Pezneator I7725N
150 35 160 76.7 -
175 35 275 80.0 -
205 40 250 80.5 -
425 50 500 88.2 -
BOD
P

5
-
5
-

-
-
-
-
-
7
15
-
-

-
-
-
10
-
-

-
-
-
-
C

45
-
60
—

-
-
-
-
-
60
85
-
-

-
-
-
60
-
-

-
-
-
-
R%

80.0
—
90.9
-

-
—
-
-
-
80.6
80.0
-
-

-
-
-
81.8
-
-

-
-
-
-
S

140
200
40
65
10
10
40
30
25

150
115
95
105
90
100
115
115
-

145
220
125
55
265
100

20
30
30
25
TOC
P

15
10
5
10
2
3
10
5
10

5
5
5
5
6
20
7
5
_

10
10
5
10
10
5

15
6
15
15
C

235
245
55
140
25
15
70
45
45

245
165
125
160
140
145
155
165


245
255
145
65
475
115

25
35
40
45
R%

89.3
95.0
87.5
84.6
80.0
70.0
75.0
83.3
60.0

96.7
95.7
94.7
95.2
93.3
80.0
93.9
95.7


93.1
95.5
96.0
81.8
96.2
95.0

25.0
80.0
50.0
40.0
S

7.7
7.0
7.0
7.1
7.2
7.2
7.0
6.9
7.0

6.9
6.7
6.6
7.0
6.6
7.0
7.1
6.9
7.1

7.2
7.0
7.1
7.2
7.6
7.4

6.8
6.8
7.0
6.8
f*
P

6.7
6.5
6.2
6.6
6.6
6.5
6.7
6.4
6.6

5.9
6.2
6.2
6.1
6.0
6.3
6.8
6.4
6.2

6.7
6.5
6.2
6.2
6.4
6.6

6.4
6.6
6.5
6.8

C

8.1
7.2
7.1
7.5
7.2
7.5
7.2
7.0
7.1

7.0
6.8
6.7
7.0
6.9
7.1
7.4
7.1
7.2

7.4
7.4
7.2
7.2
7.7
7.4

6.8
7.0
7.1
6.8

-------
Table C-l. (continued)
Saaple
nunfcer
121
124
126
128
129
139
141
141
142
143
144

149
150
151
153
154
155

158
159
160
162
163
164
167
169
172
179
183
188
194
Operating
time(hrs)
452
463
471
503
506
Cycle No.
—
~
-
™
Cycle No.
-
™
-
™
~
Cycle No.
-
—
-
-
-
-
-
-
—
—
-
-
-
ODD
S f C
780 130 975
90 15 125
150 25 195
105 15 110
130 25 155
7 - OBNL Module
150 15
225 5
135 15
160 15
150 15
8 - OBNL Module
225 40
290 45
195 30
265 35 -
320 50 -
335 50
9 - ORE, Module
110 5
190 10
370 20
445 10
1105 20
1260 30
1630 55
270 65
690 65
210 35
505 40
835 70
970 55
BOD
R%
83.3
83.3
83.3
85.7
80.8
90.0
97.8
88.9
90.6
90.0

82.2
84.5
84.6
86.8
84.4
85.1

95.5
94.7
94.6
97.8
98.2
97.6
96.6
75.9
90.6
83.3
92.1
91.6
94.3
S
15
-
-
^
_

7
-
25
-
_

—
_
-
-
—
-
—
-
—
-
—
—
-
P
5
_
-
:
_

2
-
7
-
_

_
_
-
-
_
-
-
-
-
-
_
-
-
C R%
15 66.7
_ _
— —
— —
_ _

71.4
- _
72.0

_ _

_ _
_ _
- -
- _
. _
— —
- -
- -
- -
- -
- -
-
-
S
90
15
20
7
10
25
30
15
30
20

55
30
35
50
65
65

35
65
95
85
105
295
315
80
185
65
145
200
190
TOC pH
P
15
2
7
2
4
10
1
4
10
5

15
8
6
10
7
4

-
—
10
4
8
15
4
15
10
4
15
15
15
C
120
40
25
8
15
_
_
-
^

—
_
-
_
—

_
—
_
_
_
_
_
_
_
_
M
_
-
R%
83.3
86.7
65.0
71.4
60.0
60.0
96.7
73.3
66.7
75.0

72.7
73.3
82 v 9
80.0
89.2
93.8

-
-
89.5
95.3
92.4
94.9
98.7
81.3
94.6
93.8
89.7
92.5
92.1
S
7.0
7.2
7.3
7.9
7.4
8.7
7.6
6.8
8.9
7.9

8.1
6.6
7.1
6.2
6.6
6.6

7.4
7.8
8.4
7.8
8.2
10.0
7.4
10.2
8.4
7.0
7.4
7.6
7.8
P
6.7
6.6
7.0
7.2
6.9
8.7
7.0
8.6
9.8
9.6

8.2
6.4
6.8
7.0
6.9
6.9

6.9
8.6
9.0
8.4
8.8
10.3
7.6
10.1
8.8
7.6
7.8
7.2
8.1
C
7.0
7.1
7.4
7.7
7.4
^
—
-


_
—
-
^
_

_
_
^
—
_
^
—
—
—
_
—
--
—

-------
                                                        Table 0-1. (continued)
to
en
Saple
renter

165
168
173
174
176
177
178
180

182
192
195

203
204
208
209
210
212
218
220
223
225
230
232
235
236

205
207
Operating
tineOirs)
Cycle No.
23
95
143
387
435
502
530
545
Cycle No.
556
701
744
Cycle No.
1
10
22
26
31
48
63
80
105
128
160
165
176
178
Cycle No.
—
—
COO
S P
C R%
10 - Meetinghouse Module
265 75
520 10
625 10
825 20
1230 25
1630 25
890 30
1140 90
260 71.7
98.1
98.4
97.6
97.8
98.5
96.6
92.1
11 - Westinghcuse Module
130 6
685 15
145 35
12 - DuPcnt
470 15
75 10
635 10
425 20
290 10
190 2
360 25
145 35
120 10
145 210
320 20
155 30
55 20
160 30
95.4
97.8
75.9
BOD
S P C R%
14-291
— — - _
- - _ _
- - - -
- _ _ _
— _ _ _
— — _ •
- _ _ _
— _ _ _
#4-291
- _ _ _
— - — _
— - - -
TOC
S

50
no
55
150
210
135
155
240

45
140
115
P

8
7
10
5
6
10
8
20

6
5
10
C

60

_
.
w
—
_
_

.»
_
_
R%

84.0
93.6
81.8
96.7
97.1
92.6
94.8
91.7

86.7
96.4
91.3
Pezseator 1400600
1135 96.8
110 86.7
1215 98.4
910 95.3
430 96.6
270 98.9
760 93.1
210 75.9
225 91.7
255 -
575 93.8
230 80.6
70 63.6
225 81.3
— — _ _
— — — —
- _ _ _
- _ _ _
— — _ _
_ _ _ _
_ _ _ _
— _ _ _
_ - • - _
_ _ _ _
_ _ _ _
- _ -
— _ _ _
— _ _ _
80
15
105
105
45
20
15
30
30
25
75
50
15
20
9
10
10
10
-
-
2
1
6
7
2
n
i
5
150
70
215
170
65
30
15
35
60
40
75
50
15
45
88.8
33,3
90.5
90.5
-
-
86.7
96.7
80.0
72.0
97.3
78.0
93.3
75.0
S

7.0
7.5
7.3
6.9
7.0
7.2
7.0
7.0

6.8
7.6
6.9

6.6
6.3
6.8
6.5
6.5
6.5
6.4
6.3
8.0
6.6
6.4
6.4
6.7
6.3
PH
P

6.2
6.0
6.0
5.9
6.1
6.1
6.2
6.4

5.6
6.7
6.4

6.2
6.0
8.6
6.2
5.6
5.3
6.1
5.9
9.6
6.0
6.2
6.0
6.2
6.2
13 - OWC Module
— —
- -
— —
-
_ _ _ _
_ _ _ _
_
—
_
—
_
_
_
-
_
_
_
_

C

7.1

^
_
—

_
—

_
^
_

6.5
6.4
7.2
6.7
6.6
6.6
6.4
6.4
7.4
6.4
6.5
6.5
6.7
6.4

—
—
                     Cycle No. 14 - Gulf Nodule

-------
                                            Table C-l.  (continued)
Sanple
ranter
239
246
250
252
254
256
257
258
259
260
262
263
264

272
273
274
277
278
281
282
287
289
290
Operating
time(hrs)
93
165
193
252
272
316
434
583
631
633
684
708
779
Cycle No.
-
-
-
-
-
-
-
-
-
*"
GOD
S
255
280
180
315
795
655
720
660
630
345
390
440
380
P
9
20
15
85
15
35
25
30
35
15
20
15
20
16 - Selas
240
-
-
360
-
380
390
160
210
250
20
20
20
—
30
10
-
15
10
15
C
330
350
290
400
1175
675
795
790
740
480
480
570
460
Module
-
—
-
-
-
—
-
—
—
~
R%
96.5
92.9
91.7
73.0
98.1
94.7
96.5
95.5
94.4
95.7
94.9
96.6
94.7

91.7
—
—
-
—
97.4
-
90.6
95.2
94.0
S
m
_
20
175
205

_
_
_
_
_
_
15

20
—
—
-
—
—
-
_
_
~
BCD
P
—
_
2
60
6

..
_
_
_
_
—
3

2
-
-
-
-
_
-
_
_
~
C
mf
_
25
205
260

_
_
_
_
_
_
20

-
-
-
-
-
—
-
—
-
~
R%
•
_
90.0
65.7
97.1

_
_
_
_
_
_
80.0

90.0
—
_
-
_
—
-
—
—
~
S
60
65
30

155
160
no
170
145
90
80
no
135

55
—
—
80
—
145
145
30
55
70
TOC
P
7
3
2
-
4
8
8
15
8
5
10
6
7

7
7
7
-
10
6
9
5
2
5
C
90
75
45
-
225
165
165
170
220
105
95
120
195

—
—
-
-
-
-
-
—
-
—
R%
88.3
95.4
93.3

97.4
95.0
92.7
91.2
94.5
94.4
87.5
94.5
94.8

87.3
_
—
-
—
95.9
93.8
83.3
96.4
92.9
S
6.7
5.8
6.8
6.4
6.7
6.6
6.8
7.1
7.2
6.9
6.4
6.7
7.0

7.4
—
—
7.6
—
8.2
7.5
7.1
8.2
8.3
I*
P
5.7
6.6
6.2
5.2
6.9
5.9
6.2
6.4
5.9
6.2
6.1
5.9
6.1

6.6
6.3
6.3
—
9.3
9.4
7.3
7.7
8.9
9.2

C
6.8
6.0
6.8
6.4
7.0
6.6
6.9
7.0
7.2
6.8
6.6
6.6
7.0

—
_
_
—
—
_
—
—
—
~
a  S - supply to module; P = permeate  (or product); C = concentrate  (or residue); R = 1 -  (P/S) - rejection
   An results are in mg/i except for pH  (unitless).

-------
                           Table C-2.  PERPOBCWCE OF HYPERFmTRATICN MODULES IN THE IA FRANCE PHOT PLANT

                      Rejection and Absolute Values of Alkalinity, Hardness, Total Solids, and Volatile Solids3
H
to
Sanple
nuober
4
7
12
16
22
*>•>
23
24
25
26
27
28
29
31

33
35
36
37
39
42
44
46
48
50
52
53
Operating
timefrrs)
Cycle No.
7
16
13
27
37
49
55
61
70
76
84
88
92
C^cle No.
94
102
106
108
119
131
145
150
155
161
170
179

S
Alkalinity
P
C

R%
Hardness
S
1 - DuPont Pezmeator I7753N
110 10 250 90.0 40
DuPont Penneator I7725N
30 5 100 83.3 35
30
45
60
90
130
125
120
70
no
105
10
10
10
10
10
10
10
10
20
15
2 - DuPont
115
150
105
105
no
90
130
245
385
195
230
320
20
10
15
15
15
25
15
20
30
25
25
30
85
120
135
190
195
160
185
170
160
140
66.7
77.8
83.3
88.9
92.3
92.0
91.7
85.7
81.8
85.7
40
45
40
35
45
45
45
50
60
60
P
30
20
25
15
15
15
10
10
15
10
10
10
C
140
70
100
110
95
70
60
60
65
90
90
90
R%
25.0
42.9
37.5
66.7
62.5
57.1
77.8
77.8
66.7
80.0
83.3
83.3
Total Solids
S
5390
1250
840
1490
830
850
1095
1560
1550
1490
1315
2105
1660
P
230
40
60
135
80
75
85
85
95
100
170
180
155
C R%
8930 95.7
3600 96.8
2460 92.9
4070 90.0
2360 90.4
2150 91.2
2420 92.2
2380 94.6
2090 93.9
2370 93.3
3445 87.1
3270 91.4
2570 90.7
Volatile Solids
S
420
Mt
155

195

—
^
155
195
175
Penneator I7725N
150
195
150
115
155
no
190
380
615
285
355
480
82.6
93.3
85.7
85.7
86.4
72.2
88.5
91.8
92.2
87.2
89.1
90.6
70
50
45
no
60
120
40
70
120
90
110
165
15
15
15
10
15
15
15
10
15
10
10
15
80
65
80
135
70
165
50
110
185
no
165
235
78.6
70.0
66.7
90.9
75.0
87.5
62.5
85.7
87.5
88.9
90.9
90.9
10650
3350
2380
4175
1420
3020
910
1730
2765
1575
1940
2660
1200
240
130
390
85
380
80
135
220
150
185
235
15920 88.7
4965 92.8
3720 94.5
5505 90.7
2095 94.0
4245 90.7
1370 91.2
2760 92.2
4610 92.0
2365 90.5
2945 90.5
4135 91.2
275
215
190
545
200
225
215
355
485
355
380

P
60
^^
40

35

^
^
65
70
75

95
85
60
95
55
85
25
40
55
65
70

C R%
550 85.7
_ _
320 74.2

325 82.1

_
_ _
295 58.1
260 64 1
••w w^*A
240 57.1

3935 88.7
330 60.5
365 68.4
645 82.6
280 72.5
325 62.2
295 88.4
525 88.7
925 88,7
510 81.7
575 81.6


-------
                                                      Table C-2.  (continued)
        Senple
        ranter
                   Operating
                   tiroe(hrs)
    Alkalinity
Hardness
Total Solids
Vblatile Solids
S
                                                 R%
                                                                          R%
                                                                    R%
                                                                                            R%
00
                    Cycle No.  3 - DuPont PentEator I7725N
         55         188        120   10    185   91.7   50    10
         60         209        110   25    140   77.3   295   20
         61         217        50    10    65    80.0   85    10
         65         231        no   30    200   72.7   30    5
         67         284        60    25    110   58.3   10    2
         69         326        65    25    110   61.5   5     1
         71         400        70    25    110   64.3   40    10
         73         423        70    30    105   57.1   25    5
         75         427        65    30    100   53.8   20    5
                    Cycle No.  4 - DuPont Perneator I7753N
         77         24         80    15    130   81.3   55    5
         79         28         85    15    no   82.4   75    5
,_,       81         37         75    25    105   66.7   55    5
to       82         41         100   15    135   85.0   70    5
         84         49         65    15    105   76.9   50    5
         86         62         105   20    145   81.0   40    4
         88         148        120   25    150   79.2   65    5
         89         170        85    15    105   82.4   50    5
         91         218        80    15    100   81.3   55    5
                    Cycle No.  5 - DuPont Penneator #7753N
         94         236        115   20    145   82.6   80    5
         96         251        170   30    210   82.4   150   5
         99         275        155   25    175   83.9   115   5
         101        284        210   35    245   82.3   75    5
         104        305        205   35    250   82.9   225   5
         108        337        160   25    180   84.4   90    5
                    Cycle No.  6 - DuPont Perneator I7725N
         116        437        65    25    80    61.5   90    15
         n7        439        55    20    70    63.6   15    5
         US        442        70    25    85    64.3   20    5
         120        445        40    10    50    75.0   30    5
60
390
100
40
20
12
50
80.0
93.2
88.2
83.3
80.0
80.0
75.0
2020
3385
1185
8000
530
520
1160
150
315
115
240
160
160
310
3105
4410
1525
1610
885
880
1825
92.6
90.7
90.3
97.0
69.8
69.2
73.3
295
380
245
100
US
150
175
55
75
60
85
105
55
70
400
505
285
365
220
245
215
81.4
80.3
75.5
15.0
8.7
63.3
60.0
                                      45     80.0    1040   385    1630  63.0   US   60    160  47.8
                                      30     75.0    965   '475    1600  50.8   100   60    145  40.0

                                      105    90.9    2525   270    4400  89.3   400   no   495  72.5
                                      105    93.3    2535   325    3575  87.2   265   80    360  69.8
                                      75     90.9    1730   410    2295  76.3   290   85    350  70.7
                                      100    92.9    2990   290    4290  90.3   205   30    270  85.4
                                      90     90.0    1440   145    2415  89.9   170   85    260  50.0
                                      80     87.5    1200   200    1760  83.3   155   50    230  67.7
                                      65     92.3    2130   285    2855  86.6   265   90    355  66.0
                                      70     90.0    2020   225    2650  88.9   290   90    365  69.0
                                      65     90.9    1925   155    2370  91.9   165   25    210  84.8

                                      110    93.8    3835   560    5055  85.4   370   50    490  86.5
                                      190    96.7    5245   650    6305  87.6   360   85    470  76.4
                                      135    95.7    3945   360    4050  90.9   275   50    295  81.8
                                      90     93.3    1980   355    2315  82.1   320   80    320  75.0
                                      270    97.8    5400   690    6675  87.2   715   60    620  91.6
                                      105    94.4    3785   455    4420  88.0   345   55    315  84.1
125
20
35
30
83.3
66.7
75.0
83.3
1150
790
1020
680
330
175
260
165
1500
1030
1360
865
71.3
77.8
74.5
75.7
200
135
145
230
65
80
45
65
220
135
175
270
67.5
40.7
69.0
71.7

-------
                                                     Table C-2. (continued)
K
Ssnple
nuifcer
121
124
126
128
129

139
141
142
143
144

149
150
151
153
154
155

158
159
160
162
163
164
167
169
172
179
183
188
194
Operating
time(hrs)
452
463
471
503
506
Cycle Mo.
-
—
_
_
_
Cycle No.
.
_
_
„»
_
—
Cycle No.

_
_
M
_
_
w
_
—
—
_
_
-
Alkalinity
S
90
40
105
50
75
P
25
10
40
10
20
C
120
50
130
60
90
B%
72.2
75.0
61.9
80.0
73.3
S
85
15
45
30
55
Hardness
P
10
5
5
5
10
C
110
20
60
40
70
R%
88.2
66.7
88.9
83.3
81.8
Total Solids
S P
1810 385
520 125
1555 350
515 105
920 225
C
2330
650
2010
630
1100
R%
78.7
76.0
77.5
79.6
75.5
Volatile
S
425
185
140
85
120
P
150
55
45
25
40
Solids
C R%
535 64.7
170 70.3
160 67.9
95 70.6
140 66.7
7 - QRNL Module
55
120
75
95
140
20
25
30
40
40
-
—
_
_
—
63.6
79.2
60.0
57.9
71.4
15
80
10
20
15
2
1
0.5
0.5
0.5
-
—
_
—
-
86.7
98.8
95.0
97.5
96.7
890 190
1730 235
1170 220
525 70
705 80
-
-
-
-
-
78.7
86.4
81.2
86.7
88.7
-
-
105
140
155
—
-
50
40
30
— —
— —
52.4
71.4
80.6
8 - ORNL Module
150
45
35
25
60
75
60
20
15
15
25
30
_
_
_
_
_
-
60.0
55.6
57.1
40.0
58.3
60.0
55
30
40
120
60
90
10
3
3
10
4
2
-
-
_
-
—
-
81.8
90.0
92.5
91.7
93.3
97.8
2480 980
470 3.60
695 175
1190 360
1365 445
1460 490
-
-
-
-
-
-
60.5
66.0
74.8
69.7
67.4
66.4
180
355
135
265
175
160
55
45
50
50
45
50
69.4
87.3
63.0
81.1
74.3
68.8
9 - OFNL Module
45
60
85
90
105
235
180
175
175
55
105
115
35
15
25
35
30
35
95
50
65
55
25
30
20
20
_
_
_
_
_
_
_
_
—
_
_
—
-
66.7
58.3
58.8
66.7
66.7
59.6
72.2
62.9
68.6
54.5
71.4
82.6
42.9
30
25
45
40
80
30
75
20
65
100
100
170
190
<0.5
1
2
1
2
0.5
2
0.4
3
3
4
6
9
-
_
-
—
—
_
_
_
_
_
_
_
-
98.3
96.0
95.6
97.5
97.5
98.3
97.3
98.0
98.4
97.0
96.0
96.5
95.3
865 155
1290 240
2400 440
1905 295
3230 500
3905 560
4670 780
1360 210
3555 800
1385 445
2545 725
3515 930
3950 1080
-
-
-
-
-
-
-
-
-
-
-
-
-
82.1
81.4
81.7
84.5
84.5
85.7
83.3
84.6
77.5
67.9
71.5
73.5
72.7
220
150
300
315
650
765
845
215
410
155
375
555
685
70
25
85
95
80
90
60
85
110
45
110
105
80
68.2
83.3
71.7
69.8
87.7
88.2
92.9
60.5
73.2
71.0
70.7
81.1
88.3

-------
                                  Table C-2. (continued)
Sanple
nunber

165
168
173
174
176
177
178
180
182
192
i ne
195
203
204
208
209
•). A
210
212
*\1 ft
218
220
223
225
230
232
235
236

205
207
Operating
timeQirs)
cycle No.
23
95
143
387
435
502
530
545
Cycle No.
556
701
744
Cycle No.
1
10
22
26
31
48
63
80
105
128
160
165
176
178
Cycle No.
-
-
Altelinitv
p
t:
10 - Westinghovae
75 5 75
150 5
180 10
170 6
245 7
325 9
190 10
225 20
11 - Westinghouse
40 2
380 10
135 8
12 - DuPont
150 15
30 7
95 10
100 6
80 7
30 2
25 6
45 5
80 15
60 7
100 20
60 7
30 8
45 10
™


Module
93.3
96.7
94.4
96.5
97.1
97.2
94.7
92.2
Module
95.0
97.4
Hardness
S
P
C
R%
Total Solids
S P
C R%
Volatile
S
P
Solids
C R%
14-291
60
150
190
124
605
370
150
200
14-291
30
100
94.1 225
Permeator 1400600
265
50
180
170
120
55
30
75
140
80
125
85
40
45
90.0
76.7
89.5
94.0
91.3
93.3
76.0
88.9
81.3
88.3
80.0
88.3
73.3
77.8
40
n
35
30
30
40
70
30
70
35
75
150
80
60
0.5
1
2
1
30
2
5
15
2
6
3
1
5
1
0.05
1
1
10
1.5
10
6
2
2
4
6
60
:
—
150
20
60
65
50
70
30
70
340
40
75
215
120
105
99.2
99.3
98.9
99.2
95.0
99.5
96.7
92.5
93.3
94.0
98.7
97.5
54.5
97.1
99.8
96.7
97.5
85.7
95.0
85.7
82.9
97.3
98.7
95.0
90.0
1380 40
3190 130
3915 155
2265 80
3210 no
4155 170
2365 115
3115 255
505 15
4955 225
4190 220
5475 215
1260 25
4925 90
2715 50
4515 110
1615 35
16035 1040
700 20
865 25
3020 175
1905 100
1735 140
770 85
1085 135
13 - ORNL Module
_ _
-
_
-
—
«
_
_
—
—
_
—
_
—

—
1380 97.1
95.9
96.0
96.5
96.6
95.9
95.1
91.8
97.0
95.5
93.6
11380 96.1
2345 98.0
14755 98.2
5515 98.2
6820 97.6
9255 97.8
19490 93.5
1170 97.1
1505 97.1
5190 94.2
3140 94.8
2570 91.9
1265 89.0
1760 87.6

~ ~

150
370
405
430
660
815
470
590
115
515
370
940
100
840
245
490
55
335
90
170
140
210
205
105
135



10
50
50
25
45
20
35
40
7
30
45
105
15
40
45
1
1
60
15
15
US
35
25
40
45



150 93.3
86.5
87.7
94.2
93.2
97.5
92.6
93.2
93.9
94.2
87.8
2055 88.8
130 85.0
7090 95.2
845 81.6
1175 99.8
170 98.2
540 82.1
180 83.3
245 91.2
240 17.9
365 83.3
275 87.8
165 61.9
180 66.7



Cycle No. 14 - Gulf Module

-------
Table C-2.  (continued)
SanixLe Operating
nunber time(hrs)
239
246
250
252
254
256
257
258
259
260
262
263
264

272
273
274
277
278
281
282
287
289
290
a s-
b All
93
165
193
252
272
316
434
583
631
633
684
708
779
Cycle No.
-
—
-
—
_
_
-
-
—
•
S
110
45
50
60
300
150
225
315
290
195
no
135
150
16 -
35
-
-
45
-
55
80
40
70
90
simply to module; P
results are in
rag/*.
.AUcalinity
P
10
8
5
10
15
15
20
25
25
10
9
20
10
Selas
15
15
15
—
10
10
30
10
15
20
C
150
55
60
70
365
210
265
370
345
240
135
165
180
Module
-
-
-'
-
—
-
-
-
-
™*
- permeate (or


R% S
90.9 60
82.2 70
90.0 40
83.3 30
95,0 105
90.0 145
91.1 230
92.1 100
91.4 75
94.9 100
91.8 95
85.2 155
93.3 95

57.1 50
— _
- -
70
_ _
81.8 65
62.5 200
75.0 55
78.6 100
77.8 130
product); C

Hardness
P
2
9
2
3
1
1
1
0.5
0.5
0.5
0.5
0.5
0.5

15
20
15
-
15
10
15
15
15
20
C
85
70
45
60
310
210
230
280
175
110
135
305
210

-
_
-
_
_
-
-
-
-
••
R%
96.7
87.1
95.0
90.0
99.0
99.3
99.6
99.5
99.3
99.5
99.5
99.7
99.5

70.0
_
_
_
_
84.6
92.5
72.7
85.0
84.6
= concentrate (or



Total Solids
S P
1240 15
1995 45
1290 25
1210 70
5135 175
5720 195
5495 195
5335 210
4990 185
1465 40
3340 95
4215 115
2175 60

1065 125
210
215
1330 -
120
1705 140
2080 180
805 70
1415 125
2005 195
residue); R

C R%
1685 98.8
2520 97.7
1680 98.1
1520 94.2
6340 96.6
6850 96.6
6645 96.5
6535 96.1
6070 96.3
1855 97.3
4385 97.2
4855 97.3
2665 97.2

88.3
_ _
_ _
_ —
_ _
91.8
91.3
91.3
91.2
90.3
= 1 - (P/S) =

Volatile Solids
S P
220 1
155 6
95 5
175 40
460 9
654 20
595 75
585 45
430 30
315 25
295 15
480 75
280 30

— _
_ „
_ _
_ _
M —
_ _
- -
_ _
** *
•• ~
rejection

C R%
280 99.5
225 96.1
130 94.7
180 77.1
555 98.0
690 96.9
620 87.4
635 92.3
550 93.0
365 92.1
760 94.9
440 84.4
215 89.3

_ _
_ ^
_ _
_ „
— ^
_ _
_ . _
_ _
_ _
— —



-------
                           Table C-3.   PERFORMANCE OP HXPERFILTRATICtI MODULES IN THE LA FRANCE PHOT PLANT


                       Rejection and Absolute Values of Dissolved Solids,  Color, Turbidity, and Conductivity*


                                                              (mg/t)b
C
ro
Sanple
ntnber

4
7

12
16
22
23
24
25
26
27
28
29
31

33
35
36
37
39
42
44
46
48
50
52
Operating
time(hrs)
Cycle No.
7
16

13
27
37
49
55
61
70
76
84
88
92
Cycle No.
94
102
106
108
119
131
145
150
155
161
170
Dissolved Solids
S P
1 - DuPont
5235 230
— —
DuPont
-
— —
810 80
— —
1085 90
— -
— _
— —
1265 170
— —
- -
2 - DuPont
C R%
Color
S P
C
R%
Turbidity
S
P
C
R%
Conductivity
S
P
C R%
Perroeator I7753N
8880 95.6
— -
1450 5
850 5
2400
990
99.7
99.4
0.7
54
0.1
0.33
0.1
1.7
85.7
99.4
5000
1450
400
65
8000 92.0
2500 95.5
Perraeator I7725N
-
— -
2275 90.1
— —
2350 91.7
-
— —
- -
3445 86.6
- -
— -
485 5
395 15
250 10
180 15
1300 10
1300 10
900 10
800 10
305 5
400 5
550 10
1390
990
600
650
2300
1900
1150
1200
650
550
700
99.0
96.2
96.0
91.7
99.2
99.2
98.9
98.8
98.4
98.8
98.2
1.7
15
7.0
2.0
2.0
0.61
0.69
0.84
5.8
4.5
3.7
0.21
0.52
0.4
0.35
0.24
0.25
0.25
0.1
0.43
0.36
0.31
0.3
26
2.8
3.1
0.25
0.24
0.35
0.31
2.4
3.0
2.4
87.6
96.5
94.3
82.5
88.0
59.0
63.8
88.1
92.6
92.0
91.6
1100
1650
1000
1100
1350
1750
1800
1750
1900
2900
2250
130
250
140
145
180
175
200
205
300
320
290
Pexmeator I7725N
10650 1200 14090 88.7
- -
- -
- -
- -
— —
910 80
- -
- -
1565 135
-
- -
- -
- -
- -
- - -
1370 91^2
- -
- -
2340 91.4
-
590 30
1000 15
1150 15
1800 20
1350 10
1300 10
650 20
950 30
1000 35
1350 50
790 50
800
1750
1400
1650
1800
1750
950
1400
1450
1910
1140
94.9
98.5
98.7
98.9
99.3
99.2
96.9
96.8
96.5
96.3
93.7
25
31
10
25
45
14.0
6.0
3.0
2.8
3.0
1.9
0.84
0.33
0.22
0.54
0.24
0.46
1.0
0.35
0.3
0.36
0.34
22
30
0.70
23
41
0.61
11.0
1.70
1.9
2.0
1.5
96.6
98.9
97.8
97.8
99.5
96.7
83.3
88.3
89.3
88.0
82.1
25600
6400
4100
7200
2600
6000
1320
2820
4840
2600
3050
2760
610
255
860
175
850
112
245
420
230
260
2600 88.2
2900 84.8
2500 86.0
2000 86.8
2700 86.7
2400 90.0
2300 88.9
2500 88.3
5000 84.2
3750 89.0
2900 87.1

38000 89.2
9500 90.5
6400 93.8
10300 88.1
3750 93.3
7200 85.8
2400 91.5
4330 91.3
7150 91.3
3600 91.2
5000 91.5

-------
                                                         Table C-3 (continued)
CO
Saiple
ranter
53
55
60
61
V^
65
67
W *
69
71
73
/ J
75
77
70
77
Dl
ol
ftO
o&
86
88
DO
89
01
yj.
94
Af
96
AA
99
101
* A *
104
108

116
117
Operating
timeQirs)
179
Cycle No.
188
209
217
^~LI
231
*)AA
401
one
*JAV
400
A?"*
4^J
427
cycle No.
24
OQ
£0
*)"T
37
M T
4J.
•Irt
49
62
148
"1 *TA
170
*)l a
218
Cycle No.
236
251
275
284
305
337
Cycle No.
437
439
Dissolved Solids
g p j.
t; MS
Color
S P
- 750 55
. 3 - DuPont Fenneator I7725N
^ «
790 210
~
1150 305
1 - DuPont
- -
"" ^
«. •
™* ^
1180 200
2090 260
l— ~
5 - DuPont
-
~ —
1980 345
•• ~
— ••
- -
1565 73.4
^ ^
1790 73.5
780 20
4100 35
25 . 10
545 45
50 10
35 10
625 60
205 40
160 35
Perneatar I7753N
-
~ ~
— —
*~ ^
1730 83.1
2835 87.6
~ —
710 8
1250 8
520 6
410 6
460 4
440 4
1000 8
1600 8
- 450 8
Permeator I7753N
-
— —
2315 82.6
— —
— —
320 4
1100 4
800 8
2200 6
1600 25
1100 10
C
1130
1000
4400
55
830
90
60
800
325
245
1120
1600
600
590
675
605
1500
2200
550
450
1400
920
250
2000
1210
R%
92.7
97.4
99.1
60.0
91.7
80.0
71.4
90.4
80.5
78.1
98.9
99.4
98.8
98.5
99.1
99.1
99.2
99.5
98.2
98.8
99.6
99.0
97.3
98.4
99.1
Turbidity
§
0.93
0.51
5.3
2.4
45
2.3
0.7
23
2.5
2.0
2.5
1.5
40
16.0
20
4.5
55
210
2.6
2.2
3.8
13.0
16.0
12.0
32.0
P t
0.25 0.71
0.25 0.36
1.2 3.9
0.45 2.8
6.2 50
0.56 3.0
0.4 0.9
2.9 16
0.56 1.95
0.45 1.9
0.12 1.0
0.25 0.8
0.18 40
0.16 17
0.18 6.9
0.43 2.7
0.52 55
0.42 160
0.43 2.4
0.5 1.7
0.5 2.1
0.2 11.0
0.28 17.0
0.4 10.0
0.3 27.0
6 - DuPont Permeator f 7725N
- -
•" • '
-
~ —
65 10
330 40
75
360
84.6
87.9
8.0
20.0
3.0 8.0
3.1 20.0
R%
73.1
51.0
77.4
81.3
86.2
75.6
42.9
87.4
77.6
77.5
95.2
83.3
99.6
99.0
99.1
90.4
99.1
99.8
83.5
77.3
86.8
98.5
98.3
96.7
99.1

62.5
84.5
Conductivity
S P
5000 465
4100 360
5200 470
1750 90
1260 270
740 230
925 275
1960 540
1890 550
1730 850
4050 370
4200 610
2750 780
5100 550
2300 240
2000 300
3300 480
3200 340
3250 265
6700 1100
8100 1350
6100 560
3800 650
8600 1600
7600 870

2100 600
1500 310
C Kft
7900 90.7
6200 91.2
6300 91.0
2150 94.9
2600 78.6
1500 68.9
1500 70.3
3200 72.4
2950 70.9
2700 50.9
7000 90.9
5900 85.5
3650 97.5
7200 89.2
3700 89.6
2950 85.0
4300 85.5
4000 89.4
4100 91.8
8000 83.6
9800 83.3
6900 90.8
4600 82.9
10000 81.4
8900 88.6

2700 71.4
1900 79.3

-------
Table C-3.  (continued)
Sample
nuiber
118
120
121
124
126
128
129

139
141
142
143
144

149
150
151
153
154
155

158
159
160
162
163
164
167
169
172
179
Operating
tijne(hrs
442
445
452
463
471
503
506
Cycle No.
-
_
—
_
-
Cycle No.
_
_
_
_
_
—
Cycle No.
_
_
_
_
_
_
_
_
w
-
Dissolved
S P
.. _
- —
— -
— -
1540 340
— -
— —
Solids
C
_
-
—
_
1985
—
—
Color
t*
,^
_
_
_
77.9
_
—
S
335
1670
3080
240
390
120
175
P
45
215
465
25
60
20
25
C
425
2230
3830
295
490
155
200
Rft
86.6
87.1
84.9
89.6
84.6
83.3
85.7
Turbidity
S
15.0
230
200-
25.0
20
10.0
9.0
P C
3.3 15.0
40 240
80 180
3.5 30.0
5.0 25.0
1.4 11
1.5 9.0
R%
78.0
82.6
60.0
86.0
75.0
86.0
83.3
Conductivity
S
2000
930
3000
940
3100
820
1650
P
485
255
625
250
650
175
405
C R%
2600 75.8
1300 72.6
3800 79.2
1300 73.4
4000 79.0
1000 78.7
2100 75.5
7 - OFNL Module
840 160
1695 220
1125 210
490 65
660 80
—
-
—
_
-'
81.0
87.0
81.3
86.7
87.9
480
1100
515
535
525
10
5
4
4
8
-
„
_
_
-
97.9
99.5
99.2
99.3
98.5
20
20
6.0
80
50
0.2 -
0.27 -
0.43 -
0.47 -
0.4 -
99.0
98.7
92.8
99.4
99.2
1500
2750
1925
780
1050
315
400
380
180
160
79.0
85.5
80.3
76.9
84.8
8 - OPNL Module
2465 945
_ _
_ _
1140 335
— _
— —
_
_
_
_
—
—
61.7

_
70.6
—
—
750
280
325
915
585
635
15
10
10
15
15
20
_
—
_
_
_
-
98.0
96.4
96.9
98.4
97.4
96.9
5.1
5.8
6.0
35
4.4
3.8
0.8 -
0.4 -
0.4 -
0.5 -
0.4 -
0.46 -
84.3
93.1
93.3
98.6
90.9
87.9
3850
870
940
1625
2100
2350
1725
26Q
28S
560
770
870
55.2
70.1
69.7
65.5
63.3
63.0
9 - OFNL Module
850 155
1285 240
2395 440
1760 295
2965 500
3505 560
4300 780
1320 195
3490 775
1355 445
—
_
_
_
_
_
—
..
_
-
81.8
81.3
81.6
83.2
83.1
84.0
81.9
85.2
77.8
67.2
315
670
1420
1165
3500
2960
4400
490
1540
715
1
10
25
4
1
4
10
2
8
8
-
_
—
—
—
-
-
_
_
-
99.7
98.5
98.2
99.7
99.9
99,9
99.8
99.6
99.5
98.9
25
40
60
90
135
140
no
20
25
55
0.4 -
0.6 -
0.65 -
0.55 -
0.35 -
0.4 -
0.65 -
0.35 -
0,35 -
0.4 -
98.4
98.5
98.9
99.4
99.7
99.7
99.4
98.3
98.6
99.3
1200
1950
3230
2700
4100
4900
4600
2150
4600
2150
230
370
715
580
900
1050
1220
410
1300
780
80.8
81.0
77.9
78.5
78.0
78.6
73.5
80.9
71.7
63.7

-------
Table C-3.  (continued)
Seof>le
mxber
183
TOO
188
1 /\ *
194

165
1 ftt
168
173
« « .
174
176
177
178
180

182
192
195

203
204
208
209
210
212
218
220
223
225
230
232
235
236
Operating
tine(hrs)
-
'"
"
cycle No.
23
95
143
387
435
502
530
545
Cycle No.
556
701
744
Cycle No.
1
10
22
26
31
48
63
80
105
128
160
165
176
178
Dissolved Solids
S P C
2500 715 -
3475 930 -
3875 1070 -
10 - Westinghouse
- -. -
— — _
— — —
— — _
- — -
— - —
2280 115 -
3040 255 -
11 - Westinghouse
475 15
4900 225 -
4125 270 -
R*
71.4
73.2
72.4
Module
-
-
-
-
-
-
95.0
91.6
Module
96.8
95.4
93.5
Color
S P
1625 15
3270 8
4150 20
14-291
585 2
990 1
1090 8
1880 3
2840 2
3960 2
2100 50
2710 185
14-291
310 2
920 50
1560 45
C
_
-
_

590
—
-
—
_
_
-
-

_
-
—
R%
99.1
99.8
99.5

99.7
99.9
99.3
99.8
99.9
99.9
97.6
93.2

99.4
94.6
97.1
Turbidity
S
60
45
35

30
20
15
200
230
210
220
230

35
20
0.02
P C
0.55 -
0.35 -
0.30 -

0.35 30
0.4 -
0.28 -
0.4 -
0.3 -
0.35 -
15
40

0.6 -
2.0 -
0.80 -
R%
99.1
99.2
99.1

98.8
98.0
98.1
99.8
99.9
99.8
93.2
82.6

98.3
90.0

Conductivity
S P
3500 1150
4200 1500
4500 1750

1950 100
4100 210
4900 325
2700 140
3650 225
4500 260
2650 190
3400 390

650 50
5300 825
5300 490
12 - DuPont Permeates: 1400600
_
— — -
- _ _
- - -
— - —
- - _
- - -
- - -
- _ _
- _ _
_ _ _
- - -
_ _ _
- - -
-
-
_
-
-
-
-
-
-
-
—
-
-
-
160 2
110 2
575 6
575 2
315 2
225 2
40 2
265 2
1250 2
390 2
725 2
915 2
105 2
590 2
380
195
1100
1080
490
390
45
435
2350
665
1300
1500
160
1100
98.8
98.2
99.0
99.7
99.4
99.1
95.0
99.2
99.8
99.5
99.7
99.8
98.1
99.7
1.5
2.6
2.2
4.8
0.90
1.4
4.5
3.5
1.8
2.1
3.7
6.3
3.0
3.0
0.45 12
0.3 3.6
0.29 0.9
0.33 5.4
0.40 0.70
0.33 1.1
0.36 3.0
0.35 4.0
0.59 2.3
0.62 2.0
0.35 2.0
0.40 5.1
0.38 3.3
0.40 2.5
70.0
88.5
86.8
93.1
55.6
76.4
92.0
90.0
67.2
70.5
90.5
93.7
87.3
86.7
6200 215
2000 60
5600 140
3700 120
5900 210
2150 70
21000 1550
820 25
960 60
4000 275
2400 150
2150 200
980 140
1350 215
C R%
67.1
77.1
61.1

2000 94.9
94.9
93.4
94.8
93.8
94.2
92.8
88.5

92.3
84.4
90.8

8000 96.5
3300 97.0
9000 97.5
6100 96.8
8000 96.4
3700 96.7
23000 92.6
1250 97.0
1575 93.8
6200 93.1
380 93.8
3000 90.7
1500 85.7
2150 84.1

-------
                                                      Table C-3.  (continued)
CO
CTl
Sanple


205
207
239
246
250
252
254
256
257
258
259
260
262
263
264
272
273
274
277
278
281
282
287
289
290
Operating
4-1 nw* /U_e>l
i-Liit; inrsj
Cycle No

Cycle No.
93
165
193
252
272
316
434
583
631
633
684
708
779
Cycle No.
:
_
~
_

- — 	 	 — — , —
Dissolved Solids
S
— ••••fc™ «_
10 _ r

P C
— — — — — — _

JKNL Module
R%


14 - Gulf Module


1285 25 1680
1200 70 1520
4950 170 5990
2155 55 2510
16 - Selas Module
970
_
1300

1665
2010
780
1385
1970
-••Vi^IMH
no -
150 -
200

115
130 -
180 -
70
115 -
190 -
	

98.1
94.2
96.6
97.4
88.7



92.2
91.0
91.0
91.7
90.4
	 • 	 	 	
Color
S p "


760 205
635 385

135 1
300 2
160 2
40 1
2800 6
2450 6
2460 5
2680 5
2580 10
960 2
445 1
685 1
605 1
635 4
— R

- 6
QT; _

- 10
1050 10
1210 15
295 2
490 20
670 30
C
• .

™

180
375
200
45
3710
3290
3300
3340
3150
1165
555
710
710
-

™
~

R%
•^•V^B^M^B

73.0
39.4

99.3
99.3
98.8
97.5
99.8
99.8
99.8
99.8
99.6
99.8
99.8
99.9
99.8
99.4
~
~
*•
99.0
98.8
99.3
95.9
95.5
THwHiHi t-v
S P C R%


60 25
50 35

1.3 0.55
6.1 0.64
3.6 0.55
1.8 0.5
0.05 0.37
0.02 0.32
0.01 0.30
0.01 0.50
0.01 0.50
35 0.34
4.5 0.22
5.1 0.30
40 0.20
4.7 0.18
0.20
0.36
5.3 -
0.21
6.6 0.31
7.5 0.55
6.3 0.29
8.6 0.3
15 0.45


58.3
30.0

1.35 57.7
6.3 89.5
4.2 84.7
2.2 72.2
0.04 -
0.01 -
0.01 -
0.01 -
0.01 -
30 99.0
4.0 95.1
4.4 94.1
40 99.5
96.2
— —
-
- -
95.3
92.7
95.4
96.5
97.0

Conductivity
S P c R%


2050 770
1950 1250

1300 40
2350 90
1575 60
1350 90
5450 300
5900 290
5500 290
5500 400
5500 360
1575 50
3900 180
5200 165
2550 80
1125 180
295
295
2200 -
290
2450 290
2100 275
1250 160
2350 280
3200 450


62.4
35.9

1820 96.9
2825 96.2
2050 96.2
1775 93.3
6500 94.5
7100 95.1
6700 94.7
6700 92.7
6700 93.5
2000 96.8
4600 95.4
5900 96.8
2800 96.9
84.0

• _
*• w
88.2
86.9
87.2
88.1
85.9
         S - supply to module; P = permeate (or product); C = concentrate (or residue); R = 1 -  (P/B) - rejection

         All results  are  in mg/* except conductivity (pmho/cm), color (Pt-Co units), and Turbidity  (F.T.U.).

-------
Co
                           Table  G-4.  PERFOFMMJCE OP HYPEFFffinWTION MOOUIES IN THE IA FTONCE PILOT PLMJT
                              Rejection  and Absolute Values of Calcium, Zinc, Magnesium, and Copper*
Ssnple
nuifcer

4
7
Operating
tune(hrs)
Cycle No.
7
16

S
Calcium
P C

R% S
Zinc
P C

R%

S
Magnesium
P C

R%

S
t^rffo/f
P C R%
1 - DuPont Pezmeator I7753N
5.0
1.4
0.3 6.0
0.1 17.0
94.0 3.0
92.9 1.7
0.05 4.0
0.06 1.9
98.3
96.5
21.5
0.4
DuPont Peraeator I772SN
12
16
22
23
24
25
26
27
28
29
31

33
35
36
37
39
42
44
46
48
50
52
13
27
37
49
55
61
70
76
84
88
92
Cycle No.
94
102
106
108
119
131
145
150
155
161
170
1.0
2.0
:..o
1.0
1.0
2.0
2.0
2.0
2.0
3.0
2.0
<0.1 2.0
0.5 11.0
<0.1 7.0
<0.1 2.0
<0.1 2.0
<0.1 2.0
<0.1 5.0
<0.1 5.0
<0.1 7.0
<0.1 8.0
<0.1 7.0
>90.0 2.0
75.0 3,8
>90.0 3.7
>90.0 1.6
>90.0 4.3
>95.0' 4.3
>95.0 2.1
>95.0 2.7
>95.0 -
>96.7 -
>95.0 -
<0.02 4,0
0.04 10.4
0.05 6.7
0.02 4.7
0.04 8.3
0.02 6.0
0,06 3.7
0.02 4.0
-
_ _
— —
>99.0
98.9
98.6
98.8
99.1
99.5
97.1
99.3
-
_
_
0.28
0.55
0.59
0.5
0.45
0.77
0.74
0.83
0.50
—
—
0.04 38
0.003 2.6

0.002 1.22
0.008 1.6
0.003 2.0
0.002 1.4
0.004 1.1
0.003 1.1
0.003 1.1
0.003 1.3
0.005 1.3
— —
— _
99.8
99.3

99.3
98.5
99.5
99.6
99.1
99.6
99.6
99.6
99.0

_
0.3

_
^
0.08

_
^
0.12
0.20
_
0.24
2 - DuPont Penneator #7725N
-
—
•
—
-
-
2.7
—
8.9
5.6
7.9
-
— —
— —
— —
- -
-
0.7 3.4
- -
0.14 25
0.25 6.9
<0.13 10.8
12.0
2.65
5.0
5.05
3.25
7.50
74,1 1.50
1.70
98.4 -
95.5 3.6
>98.4 2.00
0.26 14.5
0.06 3.50
0.06 11.0
0.08 10.0
0,04 3.80
0.54 11.0
0.06 1.94
0.02 2.60
-
0.06 4.65
0.06 3.20
97.8
97.7
98.8
98.4
98.8
92.8
96.0
98.8
-
98.3
97.0
3.90
3.90
3.40
13.0
4.40
12.8
2.80
5.70
14.6
8.00
13.2
0.16 4.20
0.05 4.30
0.01 5.40
0.09 16.0
0.06 5.30
0.40 18.0
0.03 3.70
0.07 10.1
0.15 24.8
0.10 11.0
0.15 25
95.9
98.7
99.7
99.3
98.6
96.9
98.9
98.8
99.0
98.8
98.9
0.48
0.08
0.36
«.
—
0.24
0.32

0.32
0.12
0.12
<0.04 0.6 >86.7


_ _ _
0.08 0.16 -


-
<0.04 0.18 >66.7
<0.04 0.44 >80.0

<0.04 0.32 >83.3

0.12 0.56 75.0
<0.04 0.16 >50.0
<0.04 0.52 >88.9

- - -
0.08 0.32 66.7
0.08 0.40 75.0

0.04 0.32 87.5
<0.04 0.20 >66.7
<0.04 0.16 >66.7

-------
                                                   Table C-4. Continued)
C
oo
Saqple
lumber
53
55
60
61
65
67
69
71
73
75

77
79
81
82
84
86
88
89
91

94
96
99
101
104
108

116
117
Operating
tiite(hrs)
179
Cycle No.
188
209
217
231
284
326
400
423
427
Cycle No.
24
28
37
41
49
62
148
170
218
Cycle No.
236
251
275
284
305
337
Cycle No.
437
439
Calcium zinc
S P C R% s P
25 0.13 40 99.5 1.78 0.04
3 - DuPont Penneator I7725N
4.2 0.1 5.6 97.6 0.44 0.10
6.6 0.4 8.5 93.9 -
- 14.8 0.1
- 1.56 0.18
1.6 0.2 2.2 87.5 -
- 0.14 0.06
2.2 0.4 3.3 81.8 4.45 0.38
- 1.40 0.24
1.9 0.6 2.7 68.4
4 - DuPont Penneator I7753N
3.9 0.2 6.8 94.9 7.50 0.06
3.9 0.3 4.8 92.3 11.5 0.06
4.5 0.6 5.7 86.7 2.70 0,08
6.9 0.12 9.5 98.3 5.10 0.02
4.0 0.04 5.9 99.0 6.25 0.06
4.2 0.12 5.6 97.1 4.4 0.06
4.0 0.04 5.1 99.0 4.85 <0.02
3.5 0.08 4.3 97,7 5.15 0.04
5.0 0.08 6.1 98.4 1.70 0.12
5 - DuPont Penneator I7753N
7.9 0.16 10.1 98.0 3.0 0.1
17.5 0.12 20.0 99.3 3.4 0.16
7.8 <0.04 8.9 >99.5 3.1 0.10
2.48 0.04 2.88 98.4 3.0 0.08
25.0 0.16 31.5 99.4 11.0 0.08
2.56 <0.04 2.92 >98.4 2.20 0.1
6 - DuPont Penneator 1 7725N
2.0 0.4 3.0 80.0 10.0 1.00
1.0 0.3 2.0 70.0 2.00 0.20
C
2.90
0.64
_
18.0
2.65
—
0.24
5.20
2.05
-

12.3
14.8
3.50
8.0
11.0
5.5
6.5
6.25
2.06

3.8
3.9
3.5
3.30
14.0
2.3

12.0
2.00
R%
97.8
77.3
_
99.3
88.5
_
57.1
91.5
82.9
—

99.2
99.5
47.0
99.6
99.0
98.6
>99.6
99.2
92.9

96.7
95.3
96.8
97.3
99.3
95.5

90.0
90.0
Magnesium
S
19
_
6.60
2.02
_
_
2.00
2.80
2.20

5.60
8.00
6.10
7.8
5.6
5.9
4.0
5.1
6.3

9.3
20.6
16.8
10.0
32.4
U.I

15.0
2.00
P
0.21
_
0.05
0.24
_
_
0.44
0.66
0.54

0.08
0.20
0.64
0.08
0.02
0.08
0.02
0.06
0.06

0.2
0.36
0.16
0.17
0.42
0.1

2.00
0.40
C
35
—
8.80
3.80
_
_
4.80
4.80
4.20

10.2
13.4
10.6
11.6
8.4
8.3
5.9
7.4
7.7

13.0
25.3
19.2
12.6
40.8
14.4

19.0
3.00
R%
98.9
„
99.2
88.1
_
_
78.0
76.4
75.5

98.6
97.5
89.5
99.0
99.6
98.6
99.5
98.8
99.0

97.8
98.3
99.0
98.3
98.7
99.1

86.7
80.0
S
0.64
1.96
0.08
0.12
0.16
0.20
0.44
_
0.32

_
—
_
0.76
—
0.40
1.28
-
-

-
-
-
0.40
-
-

-
-
Copper
P
0.04
<0.04
<0.04
<0.04
<0.04
0.04
0.12
_
0.08

_
_
_
0.04
—
0.08
0.04
-
-

-
-
-
0.08
-
-

-
-
C R%
1.08 93.8
2.56 >98.0
0.12 >50.0
0.20 >66.7
0.24 >75.0
0.28 80.0
0.76 72.7
_ _
0.48 75.0

.» _
— _
_ _
1.24 94.7
_ -
0.56 80.0
1.72 96.9
— —
_ _

— -
— - '
— _
0.5 80.0
— _
— _

— -
— -

-------
                                                       Table C-4.  (continued)
10
Sanple
ruiber
118
120
121
124
126
128
129

139
141
142
143
144

149
150
151
153
154
155

158
159
160
162
163
164
167
169
172
179
Operating
time(hrs)
442
445
452
463
471
503
506
Cycle No.
-
~
—
—
—
Cycle No.
—
—
—
—
—
-
Cycle No.
-
—
-
—
—
-
-
-
-
—

S
1.0
1.0
2.0
1.0
2.0
1.0
1.0
Calciun
P C
0.4 2.0
0.3 1.0
0.7 3.0
0.2 1.0
0.6 2.0
0.4 2.0
0.5 2.0
Zinc
K*
60.0
70.0
65.0
80.0
70.0
60.0
50.0
S
2.00
4.00
8.00
0.40
1.00
4.00
6.00
P
0.40
0.60
1.00
0.20
0.40
0.80
0.90
C
3.00
4.00
10.0
1.00
2.00
8.00
7,00
R%
80.0
85.0
87.5
50.0
60.0
80.0
85.0
7 - ORNL Module
0.36
1.40
0.40
0.84
0.60
<0.04 -
<0.04 -
<0.04 -
<0.04 -
<0.04 -
>88.9
>97.1
>90,0
>95.2
>93.3
1.30
1.00
0.80
3.10
1.20
<0.02
0.04
0.04
0,02
<0.02
_
—
_
—
_
>98.5
96.0
95.0
99.4
>98.3
Magnesium
S P
3.00 0.60
4.00 0.50
10.0 2.00
3.00 0.30
5.00 0.90
4.00 0.60
7.00 1.00

1.30 0.06
4.50 0.26
1.80 0.04
2.50 0.02
2.40 0.06
C
5.00
4.00
13.0
3.00
7.00
5.00
10.0

_
_
_
_
_
Comer
^***n
P% S P C R%
80.0 -
87.5 -
80.0 -
90.0 -
82.0 1.0 0.2 1.0 80.0
85.0 - - - -
85.7 - - - -

95.4 -
94.2 -
97.8 -
99.2 -
97.5 -
8 - ORNL Module
5.88
1.40
1.86
4.%
1.64
1.88
0.78 -
0.24 -
0.20 -
0.48 -
.0.32 -
0.16 -
86.7
82.9
89.2
90.3
80.5
91.5
2.71
_
—
2.35
—
—
<0.02
-
—
0.02
-
_
—
—
_
_
_
-.
>99.3
—
_
99.1
_
_
8.30 1.70
4.50 0.51
5.20 0.53
10.0 1.50
2.00 0.54
2.23 0.35
_
_
m
_
_
_
9 - OFNL Module
1.16
1.68
3.12
2.56
5.82
4.32
8.00
0.80
4.32
2.66
<0.04 -
<0.04 -
<0.04 -
0.04 -
0.06 -
<0.04 -
0.08 -
<0.04 -
0.04 -
0.09 -
>96.6
>97.6
>98.7
98.4
99.0
>99.1
99.0
>95.0
>99.1
96.6
1.16
-
2.60
2.32
-
7.92
13.2
-
-
3.00
0.02
-
<0.02
<0.02
-
0.02
0.02
_
-
0.04
-
—
—
—
—
-
_
—
-
-
98.3
—
>99.2
>99.1
—
>99.7
>99.8
_
_
98.7
2.00 0.09
2.92 0.16
4.80 0.33
4.5 0.17
9.67 0.30
8.00 0.08
13.0 0.38
_ _
6.30 0.21
3.76 0.28
_
_
_
_
_
_
_
_
_
-
79.5 -
88.7 -
89.8 -
85.0 -
73.0 -
84.3 -

95.5 -
94.5 _
93.1 -
96.2 -
96.9 -
99.0 ~
97.1 -

96.7 -
92.6 -

-------
Table c-4.  (continued)
Sarple
nurtber
183
188
194

165
168
173
174
176
177
178
180

182
192
195

203
204
208
209
210
212
218
220
223
225
230
232
235
236
Operating
time(hrs)
-
Cycle No.
23
95
143
387
435
502
530
545
Cycle No.
556
701
744
Cycle No.
1
10
22
26
31
48
63
80
105
128
160
165
176
178

S
12.6
19.1
38.2
Calcium
P C
0.11 -
0.48 -
0.60 -
10 - Westinghouse
2.22
6.24
8.32
1.97
2.43
2.86
2.29
0.24
0.12 2.68
0.16 -
0.16 -
0.03 -
0.03 -
0.09 -
0.17 -
0.50 -
11 - Vfestinghouse
0.10
8.40
4.20
0.08 -
0.50 -
0.40 -

R%
99.1
97.5
98.4
Module
94.6
97.4
98.1
98.5
98.8
96.9
92.6
-
Module
92.7
94.0
90.5

S
12.0
24.0
21.1
#4-291
8.00
21.2
25.8
21.6
27.6
38.8
21.2
26.8
#4-291
3.92
30.8
6.80
Zinc
P C
0.04 -
0.07 -
0.08 -

0.04 8.28
0.19 -
0.22 -
0.12 -
0.06 -
0.12 -
0.72 -
2.00 -

0.20 -
0.24 -
0.26 -

R%
99.7
99.7
99.6

99.5
99.1
99.1
99.4
99.8
99.7
96.6
92.5

94.9
99.2
96.2
12 - DuPont Penteator #400600
7.90
2.90
5.40
8.20
4.50
3.10
4.00
1.60
0.86
3.20
3.30
3.60
6.90
7.10
0.20 31.0
0.03 5.00
0.17 9.60
0.09 16.0
0.07 8.40
0.05 5.30
2.50 7.10
<0.03 2.90
<0.03 0.98
0.06 5.60
0.05 6.50
0.06 6.20
1.30 11.0
1.40 15.0
97.5
99.0
96.9
98.9
98.4
98.4
37.5
>98.1
>96.5
98.1
98.5
98,3
81.2
80.3
5.90
1.80
1.10
2.60
5.10
6.40
2,90
1.50
3.00
1.50
3.00
14.0
6.00
3.20
0.02 11
0.04 2.60
0.02 2.80
0.02 5.10
0.05 7.40
0.02 8.00
0.20 3.60
0.02 2.80
<0.02 4.90
0.02 2.40
<0.02 4.90
0.02 21.0
1.70 7.80
0.36 4.60
99.7
97.8
98.2
99.2
99.0
99.7
93.1
98,7
>99.3
98.7
>99.3
99.9
71.7
88.8
Magnesium
S
7.70
16.0
19.6

5.00
15.8
19.0
14.2
1.96
28.8
15.6
19.0

2.92
31.6
11.2

3.50
2.80
2.50
3.10
1.80
5.30
5.80
4.50
7.40
5.50
3.40
26.0
14.0
10.0
P
0.70
1.22
1.60

0.03
0.11
0.18
0.08
0.12
0.22
0.54
1.44

0.04
0.50
0.38

0.01
0.02
0.01
0.02
0.05
0.02
1.20
<0.02
0.02
0.03
<0.02
0.08
0.20
0.78
C
-

5.33

—
^_
—
m_
_
—

_
—
—

9.60
5.10
5.40
6.40
3.40
7.10
7.50
9.30
12.0
9.60
7.30
39.0
20.0
16.0
R% S^
90.9 -
92.4 -
91.8

99.4 -
99.3 -
99.1
99.4
93.9
99.2 -
96.5
92.4

98.6
98.4 -
96.6 -

99.7 -
99.3 -
99.6
99.4 -
97.2 -
99.6
79.3 -
>99.6 -
99.7 -
99.5 -
>99.4 -
99.7 -
98.6 -
92.2 -
Copper
P C R%
_

-


- _ _

- _ I
- - _


-
- --- _
- - _

-
™ V
_ _ _
- - _
^ ^^
- - _
- - _ '
— • -m
- - _
_ _ _
_ _ _
•«• • «
-
• ~ _

-------
                                             Table C-4.  (continued)
Sanple
ranker

205
207

239
246
250
252
254
256
257
258
259
260
262
263
264

272
273
274
277
278
281
282
287
289
290
Operating
ti»e(hrs)
Cycle No.
—
-
Cycle No.
93
165
193
252
272
316
434
583
631
633
684
708
779
Cycle No.
—
—
-
—
-
—
—
—
—

Calcium
S P C
13 - CTOIL Module
_ _ _
— — _
14 - Gulf Module
4.40 0.06 6.50
6.60 0.16 10.0
9.60 0.06 12.6
11,6 0.09 16.2
8.80 0.04 16.0
8.40 0.04 12.0
11.0 0.04 12.0
9.80 0.04 12.0
11.0 0.04 13.0
5.20 0.04 6.60
10.8 0.04 12.5
15.0 0.04 17.0
3.60 0.10 4.00
16 - Selas Module
3.50 0.07 - •
0.10 -
0.12 -
5.10 -
0.07 -
6.00 <0.03 -
7.70 0.08 -
5.20 0.05 -
10.2 0.13 -
14.2 0.20 -

R%

_
_

98.6
97.6
99.4
99.2
99.5
99.5
99.6
99.6
99.6
99.2
99.6
99.7
97.2

98.0
-
-
-
-
>99.5
99.0
99.0
98.7
98.6

S

_
w

1,20
1.30
0.22
0.09
0.84
0.40
0.10
0.12
0.08
0.58
1.80
5.80
3.04

1.20
-
-
1.20
-
1.40
1.50
0.94
1.40
1.90
Zinc
P C

*• —
mm _

0.03 1.60
<0.02 1.60
<0.02 0.27
<0.02 0.08
<0.02 0.88
0.02 0.47
0.02 0.06
<0.02 0.04
<0.02 0.02
<0.02 0.62
<0.02 2.10
<0.02 6.80
0.04 3.72

0.04 -
0.04 -
0.05 -
- -
0.02 -
0.02 -
<0.02 -
0.03 -
0.05 -
0.02 -

R%

_
^

97.5
>98.5
>90.9
>77.8
>97.6
95.0
80.0
>83.3
>75.0
>96.6
>98.9
>99.7
98.7

96.7
-
_
—
—
98.6
>98.7
96.8
96.4
98.9

S

_
fm

5.90
7.00
3.90
4.40
18.0
17.0
16.0
14.0
13.0
7.00
10.0
19.0
13.0

3.40
_
_
4.40
—
5.10
6.70
4.40
7.50
11.0
Magnesium
P C

_ _
_

<0.02 8.80
0.02 9.20
0.03 5.30
0.03 6.00
0.04 22.0
0.04 22.0
80.0 21.0
<0.02 16.0
0.04 15.0
<0.02 10.0
<0.02 12.0
<0.02 23.0
0.02 15.0

0.10 -
0.13 -
0.19 -
_ _
0.07 -
0.07 -
0.14 -
0.04 -
0.14 -
0.26 -

R%

_
_

>99.7
99.7
99.2
99.3
99.8
99.8
99.9
>99.9
88.7
>99.7
>99.8
>99.9
99.8

97.1
_
_
_
_
98.6
97.9
99.1
99.5
97.6

S




2.40
0.24
0.12
0.20
0.48
0.60
0.40
0.24
0.12
2.40
0.26
4.80
1.10

w
_
_
_
_
mm
_
—
_
"*
GODDST
w***x • •
P C R%




0.08 3.28 96.7
<0.04 0.36 >83.3
<0.04 0.12 >66.7
<0.04 0.22 >80.0
0.04 0.62 91.7
<0.04 0.64 >93.3
0.40 0.48 >90.0
0.04 0.36 83.3
0.04 0.20 66.7
<0.04 3.00 >98.3
<0.04 0.36 >84.6
0.04 6.60 99.2
<0.04 1.40 >96.4

— • mm
mm mm mm
mm mm _
mm _ —
— — *
*• .. .
— — —
• mm mm
mm mm mm
— — —
S = supply to module; P = permeate  (or product); C = concentrate (or residue); R =  1 -  (P/S) - rejection
All results are in mg/l.

-------
10
                           Table C-5.   PERTOBMANCE OF HYPERFILTRATION MODULES  IN THE LA. FRANCE PILOT PLANT
                           Rejection and Absolute Values of Iron,  Sodium, Sulfate, and Suspended Solids3
Sample
ranter
4
7
12
16
22
23
24
25
26
27
28
29
31

33
35
36
37
39
42
44
46
48
50
52
Operating
time(hrs)
Cycle No.
7
16
13
27
37
49
55
61
70
76
84
88
92
cycle No.
94
102
106
108
119
131
145
150
155
161
170

S
Iron
p

C
R%
S
1 - DuPont Perneator £7753N
- - - - 1500
DuPont Penneator #7725N
<0.3 <0.3 1.0 -
<0.3 <0.3 0.3 -
- 2.32
-
<0.2
—
_
<0.2
<0.2
<0.2
-
-

<0.2
_
_
CO
<0
<0
-


.2
.2
.2

_
<0.2
_
_
<0.2
<0.2
<0.2
_
_
_
—
^
--
M
_
_
300
335
_
_
^
^
w
—
Sodium
P
90
21
25
30


_
—
_
_
C
2800
640
745
780


_
^
_
_
Sulfate
R% S P C R%
94.0 -
90.0 -
91.7 -
91.0 -



- _
— • — • •
- — - _ _
Suspended Solids
S P C R%
-
- — - _
- - _ _




- - I I

2 - DuPont Penneator #7725N
0.63
—
-
0.38
0.25-
-
<0.13
0.13
-
-
-
<0
_
-
0.
<0
—
<0
<0
-
-
-
.13


13
.13

.13
.13



0.88
_
-
0.50
0.38
-
<0.13
0.25
-
-
-
>79.4
_
—
65.8
>48.0
_
_
_
-
-
-
_
_
640
—
_
_
_
_
780
400
-
_
_
50
_
_
_
_
_
80
40
-
_
_
1040
—
_
_
_
_
1040
600
—
— — . — « _
^ 	 m 	
92.2 -
— — — — »
— — v ~ •
— — — • —
^ — ^ „ 	
•• • — •- •
89.7 -
90.0 - -
— — — _ _
- - — _

I I
•• ^ ^
- - _ _
- - — _
- — — _
- - - _
"• •» ^ ^
- — - -
— — » ^

-------
                                                        Table c-5.  (continued)
U)
Sanple
nunfcer
53

55
60
61
65
67
69
71
73
75

77
79
81
82
84
86
88
89
91

94
96
99
101
104
108

116
117
118
Operating
time(hrs)
179
Cycle No.
188
209
217
231
284
326
400
243
427
Cycle No.
24
28
37
41
49
62
148
170
218
Cycle No.
236
251
275
284
305
337
Cycle No.
437
439
442
Iron
S P C R
- - _ _
3 - DuPont Perneator
- - - _
-
<0.1 <0.1 <0.1 —
0.1 <0.1 0.2 -
<0.1 <0.1 <0.1 -
<0.1 <0.1 0.1 -
- _ _ _
<0.15 <0.15 <0.15 -
- - _ _
4 - DuPont Permeatar
- - _ _
- - ~ -
-
- - _ _
-
_ _ _
- - _ _
-
- - _
5 - DuPont Permeator
-
- _ _ _
- _ _ _
- - _ -
- _ _ _
_ _ _ _
Sodiim
% S
760
#7725N
560
1060
.. .
.
220
—
360
400
360
$775311
780
840
580
_
320
140
620
620
720
#7753N
1260
1720
1140
590
1740
1280
P
65

45
125
fm
^
75
_
105
180
175

105
115
150
_
45
45
80
75
60

250
230
100
100
240
150
C
5120

860
1240
^
^
300
_
680
520
660

1600
1220
660
_
680
480
800
960
940

1600
2040
1300
720
2125
1480
Sulfate
R% S P C R%
91.4 -

92.0 -
88.2 -

I
65.9 -

70.8 -
55.0 - - - -
51.4 -

86.5 -
86.3 -
74.1 -

86.0 -
67.9 -
87.1 -
87.9 -
91.7 -

80.2 -
86.6 -
91.2 -
83.1 -
86.2 -
88.3 -
Suspended Solids
S P C R%









_ _ _
- _ _ _

_ _ _ _

-

I I
- - - _
i— ^
••• ^ ^ •»
- - _ _

^ — • •
•• — •» •
~ — — •»
" ™ — *»
— • *• •
— — — *.
6 - DuPont Permeator #7725N
_ _ _ _
_ _ _ _
- _
340
230
310
100
50
80
430
315
450
70.6 -
78.3 -
74.2 - - - -
» •• ^ ^
— — _ _
— — _ m*

-------
Table C-5. (continued)
Sample Operat
nunber time (hi

120 445
121 452
124 463
126 471
128 503
129 506
Cycle
139
141
142
143
144
H Cycle
£ 149
150
151
153
154
155
Cycle
158
159
160
162
163
164
167
169
172
179
183
ing Iron
•°t i> P C
	 — — — __ 	
No. 7 - OFNL Module
4.0 <0.1 -
26 <0.1 -
No. 8 - ORNL Itodule
8.0 <0.1 -
0.5 <0.1 -
2.0 <0.1 -
22.0 <0.1 -
1.0 <0.1 -
4.0 0.1 -
No. 9 - OKNL Module
6.67 <0.11 -
17.8 <0.11 -
5.00 <0.13 -
31.0 <0.13 -

R%
— •^-^•^— .^^^—
>97.5
>99.6
>98.8
>80.0
>95.0
>99.5
- >90.0
97.5

>98.4
>99.4
>97.4
>99.6

S

180
480
175
500
150
275
290
610
330
130
195
800
160
170
290
455
470

265
400
800
580
920
1080
1230
390
1250
465
670
Sodium
P C


R%


S

Sulfate
P C

Suspended Solids
R%

S

P

C R%

35 240 80.6 ---_ -___
110 620 77.1 --__ -___
40 210 77.1 ---_ -___
110 765 78.0 --__ ____
35 255 76.7 --__ ____
65 310 76.4 --__ -___
55 - 81.0 --__ ____
85 - 86.1 -___ -___
70 - 78.8 ---_ -___
25 - 80.8 ---_ - _ _ .
30 - 84.6 - - - - ._ _ __
390 - 51.3 ---_ --__
45 - 71.9 --__ --__
55 - 67.6 - _
115 - 60.3 --__ -___
150 - 67.0 --__ --__
175 - 62. R

55
75
150 -
95
165 -
185 -
270 -
75
255 -
130 -
215 -

79.2
81.3
81.3
83.6
82.1
82.9
78.0
80.8
79.6
72.0
67.9

57
63
128
64
253
240
555
150
615

2,3 -
2.3 -
8.9 -
9.6 -
30
30
55
2
30

96.0
96.3
93.0
85.0
88.1
87.5
90.1
98.7
95.1

15
5
5
145
265
400
370
40
65
30
45
~
0
0
0
0
0
0
0
15
25
0
10
*"" ™
100
100
100
100
100
100
100
62.5
61.5
100
77.8

-------
                                                         Table C-5.  (continued)
Ln
Sanple
ranter
188
194

165
168
173
174
176
177
178
180

182
192
195

203
204
208
209
210
212
218
220
223
225
230
232
235
236

205
Operating
time(hrs)
-
-
Cycle No.
23
95
143
387
435
502
530
545
Cycle No.
556
701
744
Cycle No.
1
10
22
26
31
48
63
80
105
128
160
165
176
178
Cycle No.
-

b
—
-
10
-
-
-
-
-
-
-
-
JJ.
-
-
-
12
-
-
-
-
-
_
-
-
-
-
-
-
-
-
13
16
Iron
P C
— _
- -
- Westinghouse
- -
- - '
- -
- -
-
— -
- -
— -
- Westinghouse
- -
— -
- -
Sodium
R%
_
-
Module
-
-
-
-
-
-
-
-
Module
-
-
-
S
U70
1360
#4-291
370
1130
1140
745
1280
1520
695
720
14-291
170
1855
1600
P
330
470

14
20
55
25
35
65
30
60

2.5
65
80
C
_
—

375
-
-
_
-
-
-
-

-
—
-
Sulf ate Suspended Solids
R% S P
71,8 -
65.4 -

96.2 -
98.2 -
95.2 -
96.6 -
97.3 -
95.7 -
9S.7 -
91.7 -

98.5 -
96.5 -
95.0 -
c R% s
40
- - 75

_ _ _
_ _ —
_ _ _
_ _ _
— — —
_ _ _
- - 85
- - 75

_ _ _
_ _ —
_ _ _
P
0
10

_
—
-
_
-
—
0
0

-
-
-
C R%
100
86.7

_ —
— —
— —
_ _
-
— —
100
100

— -
— -
— -
- DUPont Permeator 1400600
- -
- -
- -
- -
- -
_ _
— -
-
- -
-
- -
_ _
- -
-
- QRNL Module
.9 3.8 -
-
-
-
-
-
-
-
-
-
-
-
—
-
-

77.5
1760
400
1390
815
1425
520
6080
210
250
1070
745
625
255
360

-
65
5
25
14
30
7
385
3
7
60
35
60
30
50

-
3280
745
2945
1600
2135
1120
7520
360
390
1705
1120
895
410
570

-
96.3 -
98.8 -
98.2 -
98.3 -
97.9 -
98.7 -
93.7 -
98.6 -
97.2 -
94.4 -
95.3 -
90.4 -
88.2 -
86.1 -

- - -
_ _ _
_ _ _
_ _ _
_ _ _
_ _ _
_ _ _
_
_ - _
_ _ _
_
- - -
_ - -
_ - _
_ _ _

— — —
-
-
-
-
-
-
-
-
-
-
-
-
-
-

—
- -
- -
- -
— -
— -
- _
- -
- -
— -
-
— -
— -
- -
— -

— —

-------
                                              Table C-5. (continued)
Sanple
ranter
207

239
246
250
252
254
256
257
258
259
260
262
263
264

272
273
274
277
278
281
282
287
289
290
Operating
time(hrs)
H
cycle No.
93
165
193
252
272
316
434
583
631
633
684
708
779
Cycle No.
—
-
-
-
-
-
-
-
—
"
Iron
S P C R%
11.9 6.0 - 49.6
14 - Gulf Module
<0,17 <0.17 <0.17 -
<0.17 <0.17 <0.17 -
<0,17 <0.17 <0.17 -
2.20 <0.17 3.30 >92.3
<0.17 <0.17 <0.17 -
<0.17 <0.17 <0.17 -
<0.17 <0.17 <0.67 -
<0.17 <0.17 3.30 -
<0.17 <0.17 <0.17 -
<0.17 <0.17 0.67 -
<0.17 <0.17 <0.17 -
<0.17 <0.17 <0.17 -
<0.14 <0.14 <0.14 -
16 - Selas Module
— — — —
_ _ _ -
_ _ _ -
- - - -
- - - -
_ _ - -
_ _ _ _
- - - -
— - - -
.
Sodiixn
S
_

350
655
440
390
1620
2175
1855
2175
1825
465
1310
1345
335

~
—
-
—
—
—
—
—
—

P
—

5
20
10
20
60
45
60
65
60
9
30
35
15

~
—
—
—
—
—
-
—
™

C
-

495
830
600
495
1890
2495
2335
2400
2210
610
1570
1730
800

—
—
""
—
™
~
—
~
~

Sulfate
Ri S P C R%
_

98.6 - - - -
96.9 .- -
97.7 - - - -
94.9 - - - -
96.3 -
97.9 - - - _ -
96.8 - - - -
97.0 - - - -
96.7 - - - -
98.1 - - - -
97.7 - - - -
97.4 - - - -
95.5 - - - -

_ _ - - -
_ — — — —
_ — — — —
• w • — •
_ - - - -
• • •• ^
^ ^ ™" **
^ ^ ^ ••
^ ^

Suspended Solids
S P C R%
_

^ •• •• ^
• -» — —
«. — •• —
_ — — —
••" •• ^ ^
^ ^ •• ^
^ ^ ^ ^
«i •• ** ™
•~ ™" — —
. — — —
•• « ~ ""
^ — •• ^
_ •. — —











a  S = supply to nodule; P = penneate  (or product); C = concentrate  (or residue); R = 1 - (P/S) = rejecticn
b  All results are in mg/i.

-------
                                TECHNICAL REPORT DATA
                          (Please read Instructions on the reverse before completing)
\. REPORT NO.
 EPA-600/2-76-060
                           2.
                                                       3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
Hyperfiltration for Renovation of Textile Finishing
Plant Waste water
                                  5. REPORT DATE
                                  March 1976
                                  6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
Craig A. Brandon and John J. Porter
                                                       8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING OR3ANIZATION NAME AND ADDRESS
LaFrance Industries
Riegel Textile Corporation
LaFrance, SC 29656
                                                       10. PROGRAM ELEMENT NO.
                                   1BB036; ROAP 21AZT-006
                                   11. CONTRACT/GRANT NO.

                                   Grant S800929
12. SPONSORING AGENCY NAME AND ADDRESS
 EPA, Office of Research and Development
 Industrial Environmental Research Laboratory
 Research Triangle Park, NC 27711
                                   13. TYPE OF REPOHT AND PERIOD COVERED
                                   Final; 7/72-8/75	
                                   14. SPONSORING AGENCY CODE

                                    EPA-ORD
15. SUPPLEMENTARY NOTES  pr0ject officer for this reportis T.N.Sargent, ERL-Athens,
IB. ABSTRACT
              repOr£ gives results of experimental work showing that wastewater from
a textile dyeing and finishing operation can be recycled. The wastewater was run
through a set of hyperfiltration membranes ,  which separated it into purified water
and a very concentrated dye residue fraction. Over the 15-month evaluation, up to
90% of the wastewater was recovered and was found to be a satisfactory substitute
for the normal water supply in all parts of the dyeing  operation. A total of 1,348
meters of first quality fabric was produced during this period.  The concentrated dye
residue can also be used to dye fabric in the dyeing operation. The cost of recycling
the wastewater was projected to be #0.121 per cubic meter of wastewater.  However,
reusing the wastewater results in a potential savings of $0.234   per  cubic  meter,
offsetting the operating cost.  The textile industry presents an excellent opportunity
for recycling industrial wastewater after  treatment with hyperfiltration membranes.
The direct recycle will achieve pollution  abatement with significant reduction in
operating costs brought about by savings in water, chemicals, and energy.  Results
are being studied further by EPA at several other textile plants  in cooperation with
the South Carolina Textile Manufacturers  Association and Clemson University.
17.
                              KEY WORDS AND DOCUMENT ANALYSIS
                 DESCRIPTORS
                                           b.lDENTIFIERS/OPEN ENDED TERMS
                                               c.  cos AT i Field/Group
Pollution
Textiles
Textile Processes
Dyeing
Finishing
Waste Water
Circulation
Filtration
Cost Effectiveness
Pollution Control
Stationary Sources
Recycling
Hyperfiltration
13B
HE      07D
13H      14A
18. DISTRIBUTION STATEMENT

 Unlimited
                       19. SECURITY CLASS (ThisReport)
                       Unclassified
                             155
                                                                            ,GES
                      2O. RFCURITY CLASS fTliit navel
                                               22. PRICE
                                           Unclassified
EPA Form 2220-1 (9-73)
                                         T4T

-------