WATTS NICKEL AND RINSE WATER RECOVERY
    VIA AN ADVANCED REVERSElJSWTOSTS^SYSTEM
                        by
         Curtis Schmidt and Ilknur Erbas-White
      Science Applications International Corporation
                Santa Ana, CA 92705
          Contract No. 68-C8-0062, WA 3-18
                   Project Officer

                   Lisa M. Brown
           Waste Minimization, Destruction
            and Disposal Research Division
         Risk Reduction Engineering Laboratory
                Cincinnati, Ohio 45268
              This study was conducted
                 in cooperation with
                   Robert Ludwig
Office of Pollution Prevention and Technology Development
       California Environmental Protection Agency
             Sacramento, CA  95812-0806
    RISK REDUCTION ENGINEERING LABORATORY
     OFFICE OF RESEARCH AND DEVELOPMENT
     U.S. ENVIRONMENTAL PROTECTION AGENCY
              CINCINNATI, OHIO 45268

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NOTICE



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                                           FOREWORD


        Today's rapidly developing and changing technologies and industrial products and practices
frequently carry with them the increased generation of materials that, if improperly dealt with  can
threaten both public health and the environment.  The U.S. Environmental Protection Agency (EPA) is
charged by Congress with protecting the Nation's land, air, and water resources.  Under a mandate of
national environmental laws, the Agency strives to formulate and implement actions leading to a
compatible balance between human activities and the ability of natural systems to support and nurture
life.  These laws direct the EPA to perform research to define our environmental problems measure the
impacts, and search for solutions.

        The Risk Reduction Engineering Laboratory Is responsible for planning, implementing  and
managing research, development, and demonstration programs to provide an authoritative defensible
engineering basis in support of the policies,  programs, and regulations of the EPA with respect to
drinking water, wastewater, pesticides, toxic substances, solid and hazardous wastes  Superfund-related
activities and pollution prevention. This publication is one of the products of that research and provides
a vital communication link between the researcher and the user community.

        Passage of the Pollution Prevention  Act of 1990 marked'a strong change in the U S  policies
concerning the  generation of hazardous and nonnazardous wastes. This bill implements the national
objective of pollution prevention by establishing a source reduction program at the EPA and by assistinq
States in providing information and technical assistance regarding source reduction.  In support of the
emphasis on pollution prevention, the "Waste Reduction Innovative Technology Evaluation (WRITE)
Program' has been designed to identify,  evaluate, and/or demonstrate new ideas and technologies that
lead to waste reduction. The WRITE Program emphasizes source reduction and on-site recycling
These methods reduce or eliminate transportation, handling, treatment,  and disposal of hazardous
materials in the environment. The technology evaluation project discussed in this report emphasizes the
study and development of methods to reduce waste.
                                                   E. Timothy Oppelt, Director
                                                   Risk Reduction Engineering Laboratory
                                               iii

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                                       'Si
                                          ABSTRACT


       An Advanced Reverse Osmosis System (ARCS) manufactured by Water Technologies, Inc. was
installed in the Hewlett-Packard (HP) Printed Circuit Division plant in Sunnyvale, California during an 8
month test program from December 1989 through July 1990. This report uses information from Hewlett-
Packard to assess the effectiveness of the ARCS  unit in the recovery of Watts Nickel plating bath
solution and rinse water. In addition, the report estimates the incremental cost savings resulting from
reduced deionized water use, reduced wastewater vdume being pretreated, lower effluent and sludge
disposal quantities, and recovery of plating solution.

       A major achievement was that rinse water quality was maintained at a low level of nickel
contamination. The recycling of the rinse water resulted in a dramatic reduction in the use of new
deionized water makeup for this plating process.  The AROS unit also successfully produced
concentrated Watts Nickel solution of adequate quality for reuse in the plating bath solution.

       The HP cost evaluation showed an estimated net annual savings of approximately $17,000/year
through use of the AROS unit.  This compares to a capital expenditure of approximately $75,000
($62,600 for the unit, plus installation and training costs). For Hewlett-Packard, the payback'period was
approximately 4'/6 years and a return on investment of about 23 percent.

       The AROS unit at HP was operated at less than 50 percent of its hydraulic capacity. The
economic benefits would have been more favorable if the Watts Nickel plating process had  operated for
more hours and treated more printed circuit boards.  For example, the plating solution dragout at HP
was estimated to average only about 0.2 to 0.3 gph,  whereas the AROS unit is designed to  recover 2 to
3 gph of Watts Nickel solution:  ten times as much as was actually recovered.

       This report was submitted in fulfillment of Contract No. 68-C8-0062 by Science Applications
International Corporation, under the sponsorship of the U. S. Environmental Protection Agency.  This
report covers a period from February 14, 1990, to September 30, 1992; work was completed as of
September 27, 1992.
                                              Iv

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                                    TABLE OF CONTENTS
                                                                                       Page

 Notice  	
                        	  ii

 Forward	
                         	iii

 Abstract	
                        	iv

 List of Tables	
                               	vi

 List of Figures  	
                             	vi

 Acknowledgements	
                              	vii

 1.  Introduction	
                            	 1

       Project Background   	

       Project Description	'.'.'.'.'.'.'.'.	 1


 2.  Description of the AROS  Unit Installation	                                    0
                                                   '	 3

 3.  Identification of Data Needs  	


       Existing Data 	

       Sampling Program to  Obtain Additional Data	'.'.'.'.'.'.	 7


 4.  Analysis of Sampling Results  	
                                                              *""**"**••*•••••«•••... y

 5.  Overall System Performance	


 6.  Economic Analysis of the AROS System	


       Cost Effectiveness of the AROS System in the
       Hewlett-Packard Plant Setting 	

       Cost Effectiveness of the AROS System at Other Sites  '.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.',	  ]g


 7.  Bibliography  	
                                          	  18



Appendix A. Summary of Field Activities	

Appendix B. West Coast Analytical Sampling Results	  1-

Appendix C. Water Technologies Inc. Continuous Data Summary  	  oo
Appendix D. QAPP  	                                   	  3Z
                          		  35

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                                      LIST OF TABLES


Number                                                                               £agg

1   Analyses Done During Additional Sampling and Monitoring  ........................      8

2   Sampling Results of AROS Unit Performance at
    Hewlett-Packard During One Day ..................................
3   Continuous Monitoring Results Analysis  ...............................              1 1

4   Estimated Annual Incremental Savings From Use of the AROS
    Unit as Reported by Hewlett-Packard Corporation. 1990 Costs .........................  15
5   Details of Deionized Water Production Cost Used in Previous
    Table 6-1.  Approximate Annual Production of D.I. Water
    is 9.1 Million Gal	
6   Details of Wastewater Treatment Cost Used in Previous
    Table 6-1.  Approximate Annual Volume of Water Treated
    is 31.25  Million Gal	
                                                                                        15
                                                                                        16
                                      LIST OF FIGURES


Number               '                                                                Page

1   Schematic Diagram of the Advanced Reverse Osmosis System
    (AROS) for the Nickel Plating Operation  	           4

2   Schematic Diagram of Internal AROS Unit Components
    (Courtesy of Water Technologies Inc.)	             6
                                                vi

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                                     ACKNOWLEDGEMENTS
    This report was prepared by Science Applications International Corporation (SAIC) under EPA
Contract No. 68-C8-0062, Work Assignment 3-18. Mr. Curtis Schmidt was the project manager
Principal investigator was Ms. Ilknur Erbas-White. Project direction was provided by EPA Project Officer
Lisa M. Brown. Significant input and review was provided by Robert Ludwig. Project Officer Office of
Pollution Prevention.  California Environmental Protection Agency. The assistance of Tom Von Kuster
Water Technologies.  Inc., Edina. Minnesota, which supplied the equipment tested, is gratefully
acknowledged. Special thanks go to the staff of the Hewlett-Packard Printed Circuit Division In
Sunnyvale. California, including Joe Burquist.  Mary Clifford and David Brooks, for the large amount of
information provided  and cooperation in obtaining samples for analysis.
                                              vii

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                                           SECTION 1

                                         INTRODUCTION
PROJECT BACKGROUND
        This study was performed under the Califomla/U.S. Environmental Protection Agency (EPA)
Waste Reduction Innovative Technology Evaluation (WRITE) Program, and was a cooperative effort
between EPA's Risk Reduction Engineering Laboratory (RREL), the Office of Pollution Prevention of the
Calrfornta Environmental Protection Agency, the Hewlett-Packard Co. (HP) Printed Circuit Division
Sunnyvale, California operation, and Water Technologies. Inc.. Edina, Minnesota, which supplied the
Advanced Reverse Osmosis System (AROS) used in the test program.  Under the WRITE Program  the
cooperative efforts of the EPA and State or local environmental programs are used to identify develoo
demonstrate, and evaluate innovative pollution prevention techniques. Specifically, the WRITE Program
provides engineering and economic evaluations plus information dissemination for methodologiesTtnat
have the potential of reducing the quantity and/or toxicity of waste produced at the source of
generation, or to achieve practicable on-site reuse through recycling.

PROJECT DESCRIPTION

        An AROS unit manufactured by Water Technologies, Inc. was installed in the  HP plant in
Sunnyvale, California to treat and recover Watts Nickel sulfate plating bath solution and rinse water  This
report uses information from HP, plus contractor testing, to assess the effectiveness of the AROS unit in
the treatment and recovery of metal plating bath solution and rinse water. In addition the report
estimates the incremental cost savings resulting from reduced deionized water use, reduced wastewater
volume being pretreated, lower effluent and sludge disposal quantities, and recovery of plating solution.

        Prior to installation of the AROS unit, the overflow rinse water from the Watts  Nickel platina
process (approximately 1.3 million gal/yr) was added to the overall plating wastewater stream generated
by HP operat.ons (approximately 31 million gal/yr). At HP the overall plating wastewater stream is
pretreated pnor to discharge into the City of Sunnyvale sewer system. The pretreatment process
includes chemical precipitation of metals using sodium hydroxide and ferrous sulphate; PH adjustment
using sulfunc acid; and activated carbon adsorption. The chemical sludge generated by metals
precipitation is dewatered and transported to a remote RCRA approved disposal site.

        The makeup water to the rinse tank of the Watts nickel plating process is deionized by passaqe
through an ion exchange resin.  The ion exchange resin is regenerated using caustic and acid rinses  In
addition, a percentage of the old resin is periodically replaced with new resin. The AROS unit recovers
for reuse a high percentage of the deionized water used in the Watts Nickel plating process
(approximately 1.3 million gal/yr) out of HP's total deionized water production of approximately 9 million


        The AROS unit was installed in November 1989.  After installation and debugging  the system
was operated and tested from November 21, 1989 to December 18. 1989.  The system was temporarily
taken off line in late December, 1989 to allow HP to test and evaluate the plating bath solution quality

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and to create a baseline of comparison for plating bath contents and performance. Results were
considered acceptable and the AROS unit was restarted in January 1990, and the test continued through
July 31. 1990.  Counting one month in 1989 and seven months in 1990 the test totaled approximate!v 8
months.                                                                                  '

       This report summarizes the performance data provided by HP and also provides the results of a
one day snapshot of the AROS unit operation as measured by chemical analyses of various process;
input and output streams. Section 1  provides background information about the  project and Section 2
contains a technical description of the AROS unit.  Existing data and the sampling program for the
additional data are discussed in Section 3.  Details about the design of the sampling program are
provided in Section 4.  The AROS unit performance was considered excellent by  HP though some
problems were experienced, as discussed In Section 5.  Section 6 presents the economic analysis of the»
AROS system. Section 7 contains bibliographic information.  Appendix A summarizes the field activities
Appendix B presents analytical sampling results. Appendix C summarizes the continuous data  and
Appendix D is the Quality Assurance  Project Plan.

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                                            SECTION 2

                         DESCRIPTION OF THE AROS UNIT INSTALLATION
        The HP facility in Sunnyvale, California manufactures printed circuit boards for use in HP
 personal computers.  As one step in the manufacturing process, Watts Nickel plating is used to plate a
 thin layer of conductive material on a non-conductive surface, like epoxy/plastic or ceramic  Watts
 Nickel is also widely used in other industries for decorative plating operations.  During the test program
 the HP product line was operated from one to three shifts per day.

        Figure 1 is a schematic flow diagram of how the AROS unit was used in the nickel plating
 operation at HP. In the upper half of the figure the flow of the production parts (printed circuit boards)
 is shown from left to right as follows:

        •       First, the printed circuit (PC) boards are attached to moving racks. The moving  racks
                carrying the parts move through the Watts Nickel sulfate solution plating bath of about
                1.400 gallons capacity where the nickel plating is electroiytically applied to the PC
                boards. When the PC boards are removed from the bath, plating  solution adheres to
                them.  The PC boards are briefly held over the plating bath to allow plating solution to
                drip back into the plating bath before moving on. The plating solution that adheres to
                the PC boards is called "dragout."

        •       Second, the PC boards move through the 'dirty" rinse tank which  is the first of two rinse
                tanks in series. As shown in Figure 1, the clean rinse water enters the second rinse tank
                on the right and flows in the opposite direction (right to left) from the movement  of the
                PC boards. In this way, the PC boards encounter the cleanest rinse water last just
                before exiting the second "clean" rinse tank.  This method of having the parts and the
                rinse water move in opposite directions is called countercurrent rinsing. Each of the
                rinse tanks has a capacity of 450 gallons.

        The AROS unit accepts as an influent the waste steam of overflow rinse water containing
dissolved  metal  compounds from the "dirty" rinse tank. As illustrated in Figure 1, the AROS unit then
treats this rinse water to separate out the metal compounds. This separation creates two product
streams. First, a stream of deionized water called the permeate,  and second, a liquid stream of
concentrated metal compounds called the  concentrate.  Both of these product streams are reused in the
production process. The permeate stream is returned to the "clean" water rinse tank.  The concentrate
stream of metal  compounds is returned to the plating bath.  This recycling eliminates the need for
normal wastewater discharge, although, as seen In Figure 1, there is a standby emergency bypass
connection to the existing wastewater pretreatment facility if needed.  In addition to providing near zero
discharge capability, the AROS unit also greatly reduces the volume of new deionized makeup water
needed for the rinse tank.  It also reduces the quantity of new nickel sulfate solution that must be added
to the plating bath to maintain the required nickel concentration.

        Because of the intermittent flow of various streams into and out of the AROS unit it is difficult to
provide a snapshot of the flow volume in various streams.  Reported flow volumes  for the test period,

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 which comprised nearly 5000 hours, are approximately as follows:


        •      Rinse water cleaned and recycled = 190,000 gal. (38 gph)

        •      Concentrated Watts Nickel solution recycled  =  1.100 gal. (0 2 gph)
        •      New makeup deionized water used =  31,000 gal. (6.2 gph)
 ra™^D rl"9 th® test P6^ tne PC manufacturing line was operating at substantially below maximum
 capacrty.  The reader should note that the manufacturer reports that the AROS unit has a sustaiSd

 capacfty of 180 to 240 gph to dean and recycle rinse wateVand 3 to 4 gph to reTydl con
 Watts Nickel sdubon. Obviously, the unit at HP was operating significantly below ££SJ
 adversely affected the economic benefits as discussed later in Section 6.



        DUItn9 the teSt Peri°dl the PC manufacturina »ne was operating substantially below maximum

            "        Ca             WOU'd ^ ^en °Perati"9 al*>ut 8.500 hoirs annuTand^

                                                 haV8'been about 1'275 mi!Iion galloS (150
       The,A£?S Unit evaluated bV HP 's manufactured by Water Technologies Inc (WTI)  Edina

nf     on^l03"8 the Unit their ZDR S*stem: an abbreviation for zero discharge reSy  Th
of he AROS unrt ,s a specialized reverse osmosis unit.  Reverse osmosis is a physical pr«Sss in

                                       Separated from those dissolv^ ^eriaS pSSfre is
 no                   -
2S^ ?  1   ^" °n.?ne SWe °f 3 membrane banter-  Water passes through the membrane  but
other matenalsindud.ng dissolved metal ions remain behind, thus becoming mo>e concentrated   T fe

o^Tl tTil^T Tde °f ^f^ tWn fflm P1^05 that can P«fom.;*B under a wS Snge of
pH (1 to 13.5) and high pressures (400 to 1100 psi) as needed to reconcentrate a wide range of dilute
rinse waters to produce recyded  plating. bath solutions.                               9
^.,rfirt 'H f^111?" f the reverse °Sm°sis membrane. the AROS unit contains pumps, valves  interim
solut.on holdmg anks, sensors and piping needed to manage the flows into and ou? of the memb^ e

            f ' °n^ automatical|y controlled by a computer program that monitors tw qS (us

                ^                          ^— ' "*» 2 " a -hematic d,g?am^f £"
a.,             ''e2uir?ment for the AROS unit js relatively small. The unit is enclosed in a lidded box

aorar to h9  , ?  ,  ^ by ^^  ™* **Umblng- electrical' and communications connect,
appear to be relatn/ely s.mple and do not require major modifications to existing utilities     necilon°

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                              o
Figure 2.  Schematic Diagram of Internal AROS Unit Components. (Source: Water Technologies)

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                                           SECTION 3

                                IDENTIFICATION OF DATA NEEDS
 EXISTING DATA
 M- , -i JT'1"9   ta wa! Provided bV HP ab«ut their sampling and monitoring program for the Watts
 Nickel pla&ng process.  The program included continuous monitoring (every 15 seconds) of Paramete
     JT ^"H 6l COISUCtIvrty and PH at various monitoring points in the sysfem.  Streams
                               make'up line> the emefgency bypass line- the
        In addition to the continuous monitoring program, plating bath No. 1 was sampled and analyzed
 weekly.  Analyses were conducted for nicke!, PH, Nikal PC-3 (Saccharin), boric acid. cKS* ^uS ^

 PC 5 h J ™ a°  l^T*1 ^T^ ** concentration '* Important to buffer the plating bath.  Nikal
 PC-3 is an organ* additive that must be maintained at a desirable level; neither too high or too low a
 cones nir3t ion.
        HP uses ductility testing as a key indication of the plating process performance  If the nato
 layer * too brittle, then future component failure can occur  HP was particEfarly concerned thaUhe
 recovered concentrated Watts Nickel solution from the AROS unit might contah3 ^ impuSefthat would
 adversely effect ductilrty, but the recovered solution proved satisfactory in this regard  The to* b
 performed on a coupon removed from samples of printed circuit board products at final inspection and
 on a separate coupon plated from the recovered AROS unit concentrate  The procedure ^ is

        2  followin"           16 Sh66t ^ rem°Ved from the coupon and the s3"1^6 is subJect to the
           a.  A ball is pushed through the sample sheet at a controlled pressure and rate
           b.  Pressure at which the metal sheet breaks is measured.

        3.  The results are compared with base line acceptable standards.
H   ,-ISK Th(! ^P'6* plated from the recovered concentrate were all within the acceptable bounds of the
ductHrty test, according to HP.  However, to be conservative HP only recycled alx)uthaW the concen rate
recovered from the AROS unit. During the first months of the test period;  HP otearded the
concentrate until satisfied that recycling would not harm product quality.     aiscaraed tne

SAMPLING PROGRAM TO OBTAIN ADDITIONAL DATA
anah, •             ** a™monal s*™^ and monitoring was to spot-check the HP laboratory's
analysis results and continuous monitoring readings with independent laboratory results.

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       Four streams were identified as target streams for sampling (Figure 1):

       •   Dirty rinse water stream influent to the AROS unit
       •   Deionized water (water make-up to the AROS unit)
       •   Permeate stream (recycled clean rinse water return)
       •   Concentrate Watts Nickel stream from the AROS unit (returned to the plating bath)

       Laboratory analyses done for the samples are shown in Table 1 and indude nickel, sulfate
chlor.de. pH, conductivity. TDS and TOC.  Details about sampling activities are provided in Appendix A.


         TABLE 1.  ANALYSES DONE DURING ADDITIONAL SAMPLING AND MONITORING
PARAMETER
Nickel
Sulfate
Chloride
pH
Conductivity
TDS
TOC
Color
METHOD
ICPMSf
EPA 300.6/ICC
EPA 300.6/IC0
EPA 9040/1 50.1
EPA 120.1
EPA 160.1
EPA 9060
SM 204A
Li___ ••• ... i 	 	
	 . .. >—
DETECTION LIMIT*
0.01
0.1
0.1
.,
0.5
6
0.5
10
  All units are ppm except pH. conductivity (umhos/cm) and color (APHA platinum cobalt units)

  Inductively Coupled Plasma Mass Spectrometry - ICPMS (similar to EPA 200.8 - a recently acceotpd
  method)                                                                      *     v '

  EPA 300.6/lon Chromatography method - a similar equivalent method to EPA 300.0
                                             8

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                                          SECTION 4

                               ANALYSIS OF SAMPLING RESULTS


   Details of the one day sampling analysis results are shown in Appendix B and summarized in Table 2
The AROS unit achieved good separation of contaminants from the influent dirty rinse water The
composite permeate showed better than a 93% removal of nickel, sulfate, TDS and conductivity
Removal of chloride (76% removal) and TOO (77% removal) were less. The AROS unit normally
achieves removals in the 95 to 97 percent range, as measured by on-line conductivity meters  The
sampling done at  3 hour intervals happened to be grab samples (four were taken) that represented
unusually high levels of conductivity (139 umhos/cm)  and TDS (165 ppm). Normally, the conductivity of
the permeate rinse water makeup is substantially less  than 100 umhos/cm.

   For comparison purposes, a continuous monitoring data summary was  obtained from WTI for the
period the sampling was conducted.  Table 3 summarizes and Appendix C details the reading of
conductivity, flow, etc. for four passes through the AROS  unit membrane.  Each pass indicated a
different valve switch arrangement within the AROS unit that activated flow to or from internal tanks.

   Conductivity values were averaged for each of the four passes and the removal  rates were estimated
based on discrete conductivity readings at various times listed in Table 3.  A direct comparison of
conductivity readings cannot be made between the data obtained from WTI and the results in Table 2
because of the internal storage of influents and effluents within the AROS unit. A snapshot does not
necessarily reflect the performance over a longer time. In addition, the influent conductivity shown in
Table 3 is the influent conductivity on the high pressure side of the membrane, not the influent
conductivity entering the AROS unit.  Similarly, the concentrate conductivity shown in Table 3 is not the
concentrate level in the final product concentrate leaving the AROS  unit. The concentrate  conductivities
shown in Table 3 'are intermediate values achieved internally within the AROS unit.

   The permeate conductivities shown in Table 3, however, are representative of the actual dean rinse
water product, and average less than 80 umhos/cm based on 4 passes (compared to 139 umhos/cm in
Table 2).                                                                               '

   The continuous monitoring removal rates shown in  Table 3 were  higher  than those obtained from
SAIC s one-time sampling event. The continuous monitoring removal rates based on conductivity varied
from 98.3 to 99.4 percent; whereas the snapshot (one  time) sampling result indicated a removal rate of
93 percent, based on conductivity. One sample was composited over a period of 16 hours for the
influent, and permeate samples.  The concentrate was a composite of two shifts. Initially Hewlett-
Packard's laboratory was going to analyze the duplicate sample for accuracy and precision calculations
Split samples were collected for the Hewlett-Packard laboratory; however, the analysis was never done
As explained in Appendix A, no field blanks, equipment blanks and trip blanks were collected. The
quality control related to each sample depended on the quality control procedures followed by the
laboratory. Recovery rates for all parameters were within  the acceptable range (refer to Appendix B)
As previously discussed, the continuous monitoring results reflect internal sensors inside the AROS unit
and do not represent actual removals by the AROS unit, which usually range from about 95 to 97
percent based on  conductivity.

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-------
                                           SECTION 5

                               OVERALL SYSTEM PERFORMANCE


        Overall the HP staff regard the ARCS unit as having shown good performance during the test
period.  A major achievement was that rinse water quality was maintained at a low level of nickel
contamination. This is critical to the quality of the Watts Nickel plating process, which in turn is crucial
to the acceptability of the final PC board products.  It was reported that no PC boards were rejected
because of Watts Nickel plating deficiencies.

        Conductivity is used as an indication of nickel contamination. In the rinse water, approximately
11 umhos of conductivity represent 1 ppm of nickel. Prior to  using the AROS system the deionized rinse
water supplied from the ion exchange units maintained a rinse water quality of 4 to 30 umhos
conductivity. The AROS system generally supplied rinse water quality ranging from 25 to 40 umhos
conductivity. The highest reading recorded during the test period was 211  umhos. The recycling of the
rinse water resulted in a 98 percent reduction in the use of new deionized water makeup for this plating
process.

        The AROS unit also successfully produced concentrated Watts Nickel solution of adequate
quality to return to the plating bath solution. About half the concentrate produced by the AROS unit
was recycled.  As discussed in Section 3, under existing data, HP did not start recycling concentrate
until totally satisfied that the quality was satisfactory for reuse. After extensive testing for the first half of
the trial period. HP did start recycling concentrate to supplement normal additions of fresh Watts Nickel
solution. Fresh Watts Nickel solution is expensive at about $5.00/gallon, so recovery and recycling of
about 500 gallons represented a direct savings of $2,500.  Obviously, the savings would have been
greater if the concentrate had been recycled during the entire trial period. It was also calculated that
approximately 3 tons of category F006 sludge wasjnpt generated by the industrial waste water treatment
system that otherwise would have been without recycling.  The sludge produced is shipped  to Arizona
for treatment and recycling.

        The AROS unit demonstrated excellent reliability during most of the test period. For example,
during the period February 28 through June 29, 1990 the system was on-line 3,594 hours  and
experienced down-time of only 20 hours.  However, mechanical failures experienced in July  and August,
1990 caused down-time of over 200  hours during this period.  The mechanical problems included failure
of the pressure pump and two high pressure concentrate control valves, plus some minor leakage at
fittings. A failure of the membrane occurred in September 1990, apparently caused by failure of a
temperature sensor that resulted in membrane overheating. As a result, AROS systems are  now
equipped with cooling jackets around the pressure vessel to prevent membrane overheating. In
addition, the manufacturer has upgraded the sensors used and the  control software.
                                               12

-------
        Over a period of several weeks the recycled Wafts Nickel plating solution experienced an
unacceptable bu.ld-up ,n the concentration of organic additive.  A small  in-line carbon filter was added to
the system to remove these organics prior to recycling the concentrate solution back to the plating bath
      "                'S'"   difeCtl  int° the Pipe'ine Connectin9 the concentrate discharge of^e '
                                                                                        '    at
                                               13

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                                         SECTION 6


                         ECONOMIC ANALYSIS OF THE AROS SYSTEM



COST EFFECTIVENESS OF THE AROS SYSTEM IN THE HEWLETT-PACKARD PLANT SETTING


       At HP the savings from use of the AROS unit were directiy related to the incremental reduction
in spending for the following cost items:


       «   Sewer discharge fees.and fresh water cost, estimated by HP at $0.004/gal. or $4 per 1000
           gal.


       •   Deionized (Dl) water  production cost, estimated by HP at $0.0064/gal., or $6.40 per 1000
           gal.


       •   Plating wastewater treatment costs, estimated by HP at $0.0062/gal., or $6.20 per 1000 gal.

       These plating wastewater treatment costs include:
              Labor
              Power
              Chemicals
              Expendable parts and supplies replacement
              Monitoring, e.g. analysis of influent and effluent
           -   Sludge treatment, handling, manifesting, transport and disposal


       •   Purchase of new plating chemicals estimated by HP at $5.00/gal. to make up for platina
           solution drag-out losses                                                      a


.•.  *™he ab°Ve listed Cost items are the "^J01" incremental cost savings resulting to HP from use of
the AROS system. As shown in Table 4, HP estimates the annual savings listed above to total
$26.250/year. Tables 5 and 6 provide additional cost details.


       This incremental cost savings is balanced against the estimated annual expenditure for
and operating the AROS system,  as follows:


       •   Electrical Power

       •   R.O. Membrane Replacement                                                  $2200

       •   Labor and Expendable Parts                                                   $5000

       •   Carbon Filters                                                               ^  ...
                                                                                      $  90
          Telephone Modem  Contact With AROS Mfg.                                     $ 50Q
                                                                               $9419

                                      14
•

-------
TA8LE 4
lid 1 1 I^VJ


1
2
3
4
uescription


Sewer Discharge Fees and Water Costs
Deionized (Dl) Water Production Cost1
Plating Wastewater Treatment Costs2
Purchase of New Plating Chemicals at an
85 Percent Reduction
Estimated
Savings
($/gai)
0.004
0.0064
0.0062
5.00
Quantity
(gai)

— -
1.275.000
1,275.000
1,275,000
1260 X
0.85
Total
Annual
^S)v/in/"io /^\
OaVings ($)
5,100
8,16)3
7,905
5,355
 Dl water production cost is for chemicals, electricity and resin replacement onlv  No labor
                              ^


                                       "*
  TABLE 5. DETAILS OF DEIONIZED WATER PRODUCTION COST USED IN TABLE 41
tern No.
1
2
3
4
5
6

Description
Electricity
Resin Replacement
Caustic (NaOH)
Hydrochloric Acid
Sulfuric Acid
Labor, Amortization and
Other Costs
Annual Cost ($}
$13,440
$10,000
$27,412
$5,151
$ 2,475
No Difference

Estimated Unit
Cost {$)
6.730/KWH
$2.43/gal.
$0.57/gal.

Approximate Annual Production of D.I. Water is 9.1 Million Gal.
     Cost per gallon =
                                    $58,478
                                9.1 million gal/yr.
                                                          = $0.0064/gaJ.
                                      15

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           TABLE 6. DETAILS OF WASTEWATER TREATMENT COST USED IN TABLE 41
Item No. Description
1 Electricity
2 Sludge Disposal
3 Caustic (NaOH)
4 Sulfuric Acid
5 Ferrous Sulphate
6 Activated Carbon
7 Labor, Amortization and Other Costs
TOTAL
Annual Cost
($)
$46,455
$52,800
$ 49,941
$ 9,000
$19,600
$ 16,900
No Difference
$194,696
Estimated Unit Cost
($)
6.73C/KWH
$275/Ton
$2.43/Gal.
$0.57/Gal.
$0.10/Lb.
—
—

       Approximate Annual Volume of Water Treated is 31.25 Million Gal.
         Cost per gallon =
                                       $194,696
                                  31.25 million gal/yr
= $0.0062/gal
       Subtracting $9,419/Yr. from $26,250/yr., HP estimates that the net annual savings from use of
the AROS unit would be approximately $17,100/yr.  Investment is approximately $75,000, which
represents approximately $63,000 for the AROS unit plus another $12,000 for making the installation
permanent and training of operating personnel. Dividing $75,000 by $17,100 results in a payback period
of 4.4 years and a return on investment of 23 percent. As discussed below the economics would have
been more favorable had the AROS unit been utilized to a higher percentage of its capacity.

COST EFFECTIVENESS OF THE AROS SYSTEM AT OTHER SITES

       The AROS unit at HP was operated at less than 50 percent of its volumetric flow capacity and
only about 10 percent of its design capacity to recover Watts Nickel solution. The economic benefits
would have been more favorable if the Watts Nickel plating process had operated for more hours and
produced more printed circuit boards.  For example, the plating solution dragout at HP was estimated to
average only about 0.2 to 0.3 gph, whereas the AROS unit is designed to recover 2 to 3 gph of Watts
Nickel solution:  ten times as much as was actually recovered.  Similarly, the AROS unit volumetric
design capacity for influent rinse water is over twice the volume of rinse water processed at HP.

       A second economic factor is that at HP the AROS unit treated only a small fraction, e.g.  about 3
percent, of the total  site wastewater flow. Therefore, in its cost analysis HP made no allowance for
reduced labor cost at its main wastewater pre-treatment plant.  It was logical for HP to do this, since a 3
percent reduction in wastewater flow volume would not make a measurable difference in operating and
maintenance labor.  However, at another facility where the AROS unit treated a larger percentage of the
total potential wastewater flow a labor reduction credit might have been included in the cost analysis.
                                              16

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17

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                                         SECTION 7

                                       BIBLIOGRAPHY


1.      Excel Tech, Inc.  Hewlett-Packard Application Project to Evaluate a Total Rinse Recycle and
       Reclamation System Provided by Water Technologies, Inc., Water Technologies Inc., April 1991.

2.      PEI Assoc. Inc.  Characterization and Treatment of Wastes from Metal Rnishing Operations.
       Order No. PB91-125 732/AS, March 1991.

3.      Planning Research Corporation.  Waste Audit Study. Printed Circuit Board Manufacturers,
       Department of Health Services, June 1987.

4.      Water Technologies Inc., Various Items of Promotional Literature.

5.      U.S. Environmental Protection Agency.  Reducing Water Pollution Control Costs in the
       Electroplating Industry, EPA/625/5-85/016, Office of Research Program Management, Office of
       Research and Development. September 1985.
                                               18

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                                         APPENDIX A

                                SUMMARY OF FIELD ACTIVITIES
 SAMPLING RATIONALE
 c     H f 'ft!?8 'n    .OUt °f the AROS unit were sanded on October 1 7, 1990 to obtain a one dav
 snapshot of the system's operation. The samples were split for independent analysis by the HP    Y
 laboratory and an outs.de laboratory. The sample results from the two laboratories were to be

                                    Pr°Vided l° HP ^ 'OSt ^ a direC< C0m^is- ^- the
 SAMPLING PROCEDURES


 A   i ;•  ^1 HP Staf Cu0nducted the samPlin9-  The sample containers were prepared by Western
 2SS   therVh'Cnf Laborat°fY- labels were fil!ed out and chain of custody maintaTned, ar^Jmples
 placed .n the bottles as explained in the QAPP (Appendix D). In addition to SAIC personnel™
 representative .from Water Technologies, Incorporated which manufactures the AROS unftand Robert
 s^r              Department of Toxic Substances Control were also present to observe


        Four liquid streams were sampled  as shown in Figure A-1 :

        1)  Influent to the AROS treatment unit, which is the rinse water from "Dirty" rinse tank No. 1

        2)  Deionized water used as makeup water to the AROS unit


        3)             610  Z6d "dean" W3ter) Produced bv tne AROS unit that is returned to 'clean'
                                                                                   the AROS


               1< 3; and 4 K6'6 C°l!eCted 3S comP°sftes as described in the following subsections
           tn      me gf^ ^""P'8- Upon collecti°n. a" samples were stored on ice wfththe
       n of the concentrate (stream 4), which would have crystallized if put on ice  At the end of the
day samples were poured into the prepared  bottles for shipment to the laboratory A split sample of
each (except de,on,zed water) was provided to HP in bottles prepared by them  SamplTs from Seams
12, and 3 were shipped to the laboratory in  a cooler with blue tee. The conrent

SSff F       ^ 3 hard°US material 3nd W3S not "-""am* °" 'ce-  The
                                            19

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-------
LU
   S
UL.O
u.
                                                  20

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Sampling of the Influent Stream

       An I SCO sampler was installed to automatically take samples of the influent to the AROS unit.
Due to the time lapse during treatment of the wastewater entering the unit, the influent to the unit cannot
be calibrated directly with the effluents (permeate and concentrate) from the unit.  However, collection of
samples automatically throughout the day gave a good indication of the influent composition. Beginning
at 9:15 a.m., the ISCO was programmed to obtain approximately 165 mL of influent every 30 minutes.
The composite sample was collected from the  ISCO sampler at 5:15 p.m.  To chill the sample, ice was
packed around the Nalgene collection bottle located within the sampler.

Sampling of the Deionized Water

       A one-time grab sample of deionized water was taken from a tap of the deionlzed water
production system at approximately 1:35 p.m.  Hewlett Packard did not want a split sample of the
deionized water, as they are  already knowledgeable about its composition.

Sampling of the Permeate

       Grab samples of permeate were obtained from a tap off the AROS unit, at approximately three
hour time intervals throughout the day, for a total of four grab samples. The first sample was collected
at 9:20 a.m. As each sample was collected, it  was placed into an acid-rinsed plastic one gallon bottle.
This composite bottle was kept on ice in a cooler.  After the final sample was collected the composite
container was mixed by shaking. The composite sample was then poured into properly labeled bottles
prepared with preservative for the various analyses.

Sampling of the Concentrate

       Concentrate is discharged from the AROS unit periodically, not continually. Two grab samples
of concentrate were collected from different batches. The first batch was  discharged from the AROS
unit at about 11:00 a.m. It was collected in a five-gallon bucket.  The contents of the bucket were
swirled to mix, and a sample was poured into a one-liter glass bottle. This sample was not  chilled due
to the likelihood of crystallization of the highly  concentrated plating solution. The remainder of the batch
was poured into a 55-gallon  drum that HP uses to collect the concentrate. At approximately 4:30 p.m.,
another batch of concentrate was discharged from the unit. A sample from this batch was collected in
the same manner as the first. The contents of both liter bottles were then poured into a compositing
container (one-gallon plastic), and swirled to mix.  The bottles prepared by the laboratory were filled with
concentrate and shipped to the laboratory for analysis as described below.

PACKING, PRESERVATION, AND TRANSPORT OF SAMPLES

       Ail bottles were taped with duct tape to prevent loosening of the caps in transit. The samples of
influent, deionized water, and permeate were placed into a small cooler, and packs of blue ice were put
in.  Remaining gaps were filled with styrofoam "peanuts,' and a small amount of ice was added to the
top.  The laboratory confirmed that the samples were still cold when they arrived the next morning.
                                               21

-------
nmv/H JS?   f        WK3S ^i"1 ^P^y and shipped as a hazardous material. Hewlett-Packard
provKied the informat.on, box, and proper label for this shipment. Taped bottles were placed deep in an
absorbent matenal in the box.  The remaining airspace was stuffed wSTcrumpled newsptrSs  The box

Tn^ H^ rf^ With the Pf0per Shippin9 "a™ of the ^bstance, 'Co^ive UqK O S ' and
the UN number. UNI 760. The  Federal express office accepted the samples after a 4?PPt>s

nnnf!CSrf   ^r    artldeS" W3S comP)eted-  The ^ent determined that since the total quantity
consisted of more than one quart, the shipment would have to go on a cargo rather than a passenXr
plane.  The laboratory confirmed receipt of this box by 10 a.m. The following mornfng      paSSengeT
                                            22

-------
                            APPENDIX B


                       WEST COAST ANALYTICAL
                         SAMPLING RESULTS
June 25, 1987
To Our Customers:

Ref: Sample Storage Policy

With each report as it  is completed we include a Sample Storage
Card.  This card is to  be returned each time,  so that proper
handling of your samples can be maintained.

Our policy as stated on the card will be adhered to in the  future
unless we receive back  the  sample storage card indicating
samples to be returned  at customers expense.   We do not store
samples after 30 days of job being completed.

Thank you in advance for your cooperation.

Sincerely,

WEST COAST ANALYTICAL SERVICE,  INC.1
R.'Northington
Controller

RN/ds
                               23

-------
October 31, 1990
SAIC
1720 E. Wilshire Ave.
Santa Ana, CA 92705

Attn:  .   Ilknur Erbus-White

JOB NO.   16864
                       LABORATORY REPORT
Samples Received; Nine (9) water samples and three  (3)
Date Received: 10-18-90
Purchase Order No:  R5503467
The samples were analyzed as follows:

Samples Analyzed.

Four (4) samples

One (1) sample

Four (4) samples
                      Nickel by ICPMS

                      QC Summary for ICPMS
One (1) sample

Four (4) samples &
two (2) duplicates

Four (4) samples &
two (2) duplicates

Four (4) samples &
two (2) duplicates

Four (4} samples t
two (2) duplicates
Chloride and Sulfate by
EPA 300.6/IC

QC Summary for EPA 300.6/IC

pH by EPA 9040/150.1


Total Dissolved Solids
by EPA 160.1

Conductivity by EPA 120.1


Color by SM 204A
    Result^

    Table 1

    Table 2


    Table 3

    Table 4

    Table 3



    Table 6

   . Table 7


    Table 8


Page 1 of 7
      Michael Shelton
     Technical Director
                    .  Northington, Ph.D.
                        President
                             24

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               WEST COAST ANALYTICAL SERVICE, INC.

SAIC                                           Job | 16864
Ms. Ilknur Erbas-White                         October 31, 1990


                        LABORATORY REPORT
Samples Analyze4      Analysis                       Resultg

Four (4) samples      Total Organic Carbon  (TOC)
                      by EPA 9060                    Table 9

One (l) sample        QC Summary for EPA 9060        Table 9
                                        Page 2 of 7
                              25

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               WEST COAST ANALYTICAL SERVICE,  INC.
SAIC                                                     '    ' •
Ms. Ilknur Erbas-Whita                         Sctoberll?  1990
                        LABORATORY REPORT
                             TABLE
                   Parts Per Million
Sample NO,                   NjLcjs£i
S?nSentrat*                  S2700
DI Water                         0 ,«
Influent                       65J'19
Permeate                        20 5
Detection Limit                  o!oi

Dates Analyzed: 10-23-90 &  10-25-90
                             TABLE 2,
                  QC Summary for Nickel by ICPM$

              m    % Recpvery.   MSfi   % Recovery   RPD
20'5         107        87        107       87        0
Spike Level: 100 ppn
Date Analyzed:  10-25-90
                                         Page 3  of 7
                             26

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               WEST COAST ANALYTICAL SERVICE,  INC.
SAIC
Ms. Ilknur Erbas-Whit«
                           •  Job  f  16864
                             October  31,  1990
                        LABORATORY REPORT
Sample  ID

Concentrate
DI Water
Influent
Permeate
Detection  Limit

ND-Not  Detected

** values  in nig/Kg
 Dates Analyzed:  10-19-90
                 10-22-90*
           TABLE ?

   Parts Per Million

       bv EPA 300.6/IC

   Chloride        Sulfate
    7800**
      ND
     120
      29
       0.1
          79000**
              0.11
           1100*
             18 •
              0.1
 Component

 Chloride
 Sulfate
.29
18
              TABLE 4

    PC Summary for EPA 300.6/IC

        Sample ID; Permeatq

       CUE   EEC  BS   MSP   %
 Detection Limit:  0.1 ppm
29
18
                             RED
0
0
17
31
17
31
81
65
0
0
                 Spike Level - 20 ppm
                                         Page 4 of 7
                              27

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               WEST COAST ANALYTICAL SERVICE, INC.

SAIC
H3. Ilknur Erbas-wnite                          OctoberS®" 1990

                                         ^«BM»«MMamaMMBOQMB»aMBa*M
                        LABORATORY  REPORT
                            •M^BHBVEMMMM

                            TABLE 5.

                        bv EPA  9040/150,1

gftPPle IP                  PH  (Units)

Concentrate                   4. j
Concentrate (DUP)             4.1
DI Water                      6  1
DI Water (DUP)                6fi
Influent                      6  0
Influent (DUP)                6.0
Permeate                      5.7
Permeate (DUP)                5]^

Date Analyzed: 10-25-90
                             TABLE  $

                     Parts Per Million
                           bv EPA
Sample IP             Total Pis?Piv^

Concentrate                    172000
Concentrate DUP                171000
DI Water                          ND
DI Water DUP                      ND
Influent                        2490
Influent DUP                    2560
Permeate                         180
Permeate DUP                     150
Detection Limit                    6

ND-Not Detected

Date Analyzed:  10-19-90
                                         Page 5 of 7
                             28

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               WEST COAST ANALYTICAL SERVICE, INC.
SAIC
Ms. Ilknur Erbas-White                         October 31  1990


                         LABORATORY REPORT
                             TABLE
                     Micromhos Per
                             (umhos/cm)

Sample IP            Conductivity bv EPA 120.1

Concentrate                   53700
Concentrate DUP               53800
DI Water                          3.7
DI Water DUP                      3.8
Influent                       1980
Influent DUP   •          .      1990
Permeate                        137
Permeate DUP     '               142
Detection Limit                   '0.5

Date Analyzed:   10-19-90

                             TABLE
                     APHA Plati,nyirc Cobalt

Sample ID                Color bv SM 204 ft

Concentrate                  9700
Concentrate DUP              9500
DI Water                       NO
DI Water DUP                   ND
Influent                      140
Influent DUP                  140
Permeate                       ND
Permeate DUP                   ND
Detection Limit                10

ND-Not Detected

Date Analyzed:   10-19-90
                                       Page 6 of 7
                              29

-------
               WEST COAST ANALYTICAL SERVICE, INC.
SAIC
Ms. Ilknur Erbas-White
                            Job I 16864
                            October 31,  1990
                        LABORATORY REPORT
                             TABLE 9
                           Per Million
                           bv EPA
Sample ID
Total Organic carbon
Concentrate
Concentrate DUP
Influent
Permeate
Permeate DUP °
DI Water -
External Reference Standard
Detection Limit

Date Analyzed: 10-26-90
           1610
           1640
             30.8
              6.91
              7.10
              0.'74
             20   (100* Recovery)
              0.5
                                        Page 7 of 7
                              30

-------
    Ktmr

                   £
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WEST COAST ANALYTICAL SERIVCE. INC.
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                                                    ID 1 6 8 6 4
                              31

-------
       APPENDIX C

 WATER TECHNOLOGIES INC
CONTINUOUS DATA SUMMARY
          32

-------
• File  Program*
 Hewlett Packard
 Watts nickel
Archive  Option*  System  Calib  Rinse  Membrane
ZDR-513             P*SS • ! PERFORMANCE DATA
                     (LAST 6 TIMES IN PASS)
                                                                     Uog
date
time o? day
'Pass time, *in
Rinse tine, *in
Control time, min
Rinse volu»«. 9*1
Control volume, gal
Permeate temperature, deg F
Concentrate temperature
Pump flow rate, gpn
Permeate flow, rate, flpa _
Concentrate flow rate, gpra
System pressure, psi
Membrane pressure drop, psi
Feed tank conductivity, umho
permeate conductivity, umho
Concentrate conductivity
Membrane separation ratio
"Min. permeate conductivity
10-17
13:56
18.72
16.62
16.53
21.9
17.4
74
71
5.02
1.40
0.55
217
12
5984
12.
4776
388.5
12
10-17
15:15
18.16
16.02
18.02
21.4
17.4
75
71
5.05
1.44
0.49
217
12
5608
12
4344
365.5
11
10-17
12:28
9.28
6.92
9.27
•«.4
14.0
73
70
4.54
1.31
0.47
195
5
5368
11
5068
282.5
11
10-17
12: *
3.45
1.45
2.58
0.3
6.0
30
75
3.69
0.38
1.87
118
3
6184
106
7928
74.9
71
10-17
11:41
7.22
1.50
7.20
0.0
14.7
79
71
3.70
0.29
i.eo
74
2
5256
157
1968
12.5
73
ravw^KP^Pvr^^
10-17
u: 4
6.32
st. BO
6.30
0.3!
H2.f ||
71=i
69
3.67
0.38J
:i.ao =
79 .
2
4064 •
.77.
U86U
15.31
32;
£RR(0) OK
                	 Copyright (c) 1990 Water Technologies,  Inc.
 •  File  Programs
 Hewlett
 Watts nicw*l
 Archive  Options  System • Calib  Rinse  Membrane
 ZOR-S13            PASS 82 PERFORMANCE DATA
                     (LAST 6 TIMES IN PASS)
                log
                    10-.'L7-9(
                    14:,SO:2(
date
time of day
Pass time, ain
Rinse time, »in
Control tix.e, .-nin
Rinse volume, gal
Control volume, gal
Permeate temperature, deg F
Concentrate tsc-perature
Pump flew rate, gpn
Permeate flew rate, gpra
Concentrate flow rate, gpra
System pressure, psi
Menbrana pressure drop, psi.
Feed tank cc«cuctivity, un»no
Ferireate conductivity , uisho
Concantrsia conductivity
feff-brane *.e.s*ration ratio
Max. cc'-,ce--':rate conductivity
10-17
14:28
3.97
3.90
1.27
8.3
2.1
79
76
4.94
3.15
1.78
564
7
2836
17
9616
S91..0
9616
10-17
14: 5
7.00
7.00
3.70
8.7
5.5
80
75
5.O5
0.75
1.40
137
11
2804
46
3288
180.0
9120
10-17
13:22
9.23
9.23
4.50
11.9
4.2
80
75
5.00
1.00
1.11
175
2
2464
47
7840
167.8
9024
10-17
12:39
11.27
11.10
5.40
13.0
4.9
79
75
4.36
1.20
0.69
197
0
2460
54
7664
142.5
9120
»T .'.jp-v v •^*"irj
10-17
11:56
14.83
11.87
9.17
11.6
5.7
80
76
3.69
0.98
O.40
186
3
2516
47
SS44
182.8
69U
10-17
11:17
12.67
1:1.20
6.43
11. 5
4.8
76
7<
3.67.
i.oe
0.49
197
0
780*
S&
7926
1-«2.S
894*.
 £R«i(0) CK
                 --- Copyright
1990 Water TecM-.olsgies. I
                                       33

-------
• rile  Programs
 Hewlett Packard
 Watt* nickel
Archive  Option*  Syst«a  Calib   Rir.se   Membrane
ZOR-513            PASS 03 PERFORMANCE  DATA
                    (CA3T « TIMES IN  PASS)
                                                                    Cog
date
time of day
Pass tin*. «in
Rinse time, nin
Control time, nin
Rinse volume, 3*1
Control voluae, gal
Perneat* temperature, deg F
Concentrate temperature
Pump flow rate, gpm
Perweate flow r*t«, gpm
Concentrate flow rate, gpa
System pressure, psi
Membra no pressure drop, psi
Feed tank conductivity, umho
Persieate conductivity, umho
Concentrate conductivity
Membrane separation ratio
Max. concentrate conductivity

10-17
14:10
6.90
6.30
0.00
9.0
0.0
83
81
4.95
2.89
o.ss
729
12
12368
50
20334
410. S
20334

10-17
13:29
6.93
6.43
0.00
8.6
0.0
83
80
5.02
1.49
O.S8
385
5
10664
74
19040
257.0
19040

10-17
12:47
7.40
5.97
o.oo
7.5
0.0
83
80
5.01
1.40
0.60
388
5
9648
79
18848
239.5
18848

10-17
12:11
4.97
4.10
0.30
10.9
0.2
83
81
3.54
3.02
0.64
850
7
11216
54
22688
423.5
22683

10-17
12: 2
6.05
3.80
0.00
3.7
0.0
82
79
3.69
0.91
0.58
244
4
8208
94
15520
165.8
15536

tO- 1 7
A 1 : 26
9.O"1!
1
5.271
O.OO'
5.0i
o.o
I*
811
78
3.69
0.87
0.62
281
4
11600
109
18080
166.5
16080

CRft(O) OK
               	 Copyright (c) 1990 Water Technologies, Inc
• File  Programs  Archive
 Hewlett Packard  ZOR-513
 Watts
         Options  System  Calib  Rinse  Membrane
                   PASS *4 PERFORMANCE DATA
                    (CAST 6 TIMES IN. PASS)
                                                                    cog
date
time of rfay
Pass tiir.e, nin
Rinse tiise, win
Control tine, min
Rinse vol-.iae, gal
Control vsluiR*, gal
Permeate temperature, deg F
Concentrate temperature
Pump flow rate, gpm
Permeate flow rate, gpm
Concentrate flow rate, gpm
System pressure, psi
Menbrare cressure drop, psi
Feed tar* conductivity , ur.ho
Permeate conductivity, umho
Concentrate conductivity
Per-fcra-e stearaticn ratio
fax. cc^ce^trate conductivity
1O-17
9:36
4.62
• 1.02
2.88
2.5
1.7
84
82
1.70
O.96
0.62
951
10
20384
149
22443
218.5
32448
10-17
2:22
4.75
3.50
2.92
6.3
1.7
86
84
1.51
1.C2
O.58
1003
8
20384
131
30432
231.8
30432
10-16
22:31
5.05
2.93
2.25
4.8
1.3
87
85
1.50
1.04
0.56
999
9
19963
123
29792
242.3
30112
10-16
16:47
4.95
3.40
2.52
6.1'
1.3
83
81
1.47
1.00
O.S1
998
8
19968
127
30400
239.8
30400
ERR(O) C<
                                	Copyright  (c)  199O
                                     34

-------
                     APPENDIX D
       QUALITY ASSURANCE PROJECT PLAN
                       FOR
   THE EVALUATION OF AN ADVANCED REVERSE
OSMOSIS SYSTEM AT THE SUNNYVALE, CALIFORNIA
           HEWLETT-PACKARD FACILITY
                    July 20, 1990
                   Submitted to:

         U.S. Environmental Protection Agency
        Risk Reduction Engineering Laboratory
          26 West Martin Luther King Drive
               Cincinnati, Ohio 45268
                   Submitted by:

     Science Applications International Corporation
          635 West Seventh Street, Suite 403
               Cincinnati, Ohio 45203
EPA Contract No. 68-C8-0062, Work Assignment No. 1-18
          SAIC Project No. 1-832-03-959-00
                         35

-------
   6.6.1
                      QUAU7Y ASSURANCE PROJECT PLAN APPROVAL FORM
                                             for
                         Contracu/lAG./CooporatJve Aflreemenu/in-houM Project,
   RREL QA ID No:
                               RREL Project Category: _m_   RREL
                                       ,    	m~-1 •         nnci
   Contractor:	Science Applications International Corporation

COMMITMENT TO IMPLEMENT THi ABOVE QA PROJECT

     womractor-i Projocvra«kM^g9r(print)
     	Thomas J. Wagner
     contractor OA Mana8er (pnmj	:

     utner as AppropriateyAnill.tlon- (print)

     otn«r at Appropriate/Affiliation* (print)

     wuier a* Appropriate/Affiliation- (print)
                                                    PLAN:
 APPROVAL TO PROCEED IN ACCORDANCE TO THE
                                           ABOVE QA PROJECT PLAN:
      RREL Technical Project Mana8er (print
CONCURRENCES:
RHEL (QAPJP AF)
(Sept. 198S)
                                                                                Data
     RREL Section or Branch Chief (print)
                                                                               Date
                                           36

-------

-------
                                                             HP - QAPJP
                                                             Section No.:   Q
                                                             Revision No.:  Q
                                                             Date:        IxbJfL
                                                             Pa«e:        l-sLl
                                 TABLE OF CONTENTS
 SECTION
                                                        .EASES
  1.0   INTRODUCTION	
                                          """**""*""**"*"""      «5

  2.0   PROJECT DESCRIPTION	

  3.0   QUALITY ASSURANCE OBJECTIVES
                                        «*"•«»•«.......,.,.„„,....      ^

 4.0   SITE SELECTION AND SAMPLING PROCEDURES
             FOR CRITICAL MEASUREMENTS	      7

 5.0    ANALYTICAL PROCEDURES AND
             CALIBRATION	              l

 6.0    DATA REDUCTION, VALIDATION AND
             REPORTING	


 7.0    INTERNAL QUALITY CONTROL CHECKS	      2

 8.0    PERFORMANCE SYSTEMS AUDITS	       !

 9.0    CALCULATION OF DATA QUALITY
            IMPLJCATORS	_             2

10.0    CORRECTIVE ACTION	             t


11.0   QA/QC REPORTS TO MANAGEMENT	1	      1
£Eyjsjo_N,


    0

    o

    0


    0


    0


    0

   0

   0


   0

   0

   0
 7/20/90

 7/20/90

 7/20/90


 7/20/90


 7/20/90


 7/20/90

 7/20/90

 7/20/90


7/20/90

7/20/90

7/20/90
                                         37

-------
                                                      HP - QAPJP
                                                      Section No.:
                                                      Revision No.:
                                                      Date:
                                                      Page:
                                          My 20. 1990
                                          2 of 2
DISTRIBUTION LIST:
Lisa Brown,
Guy Simes,
Robert Ludwig,
Mary Clifford,
Joe Burquist,
Tom von Kuster,
Curtis Schmidt,
Ilknur Erbas-White,
Thomas Wagner,
Joe Arlauskas,
U.S. EPA
U.S. EPA
California DHS
Hewlett-Packard
Hewlett-Packard
wn
SAIC
SAIC
SAIC
SAIC
                                     38

-------
                                                          HP - QAPjP
                                                          Section No.:   i.
                                                          Revision No.:  0
                                                                      July 20.
                                                                      1 of 3

 1.0    INTRODUCTION

        The objective of the Waste Reduction Innovative Technology Evaluation (WRITE)
 Program is to identify, develop, demonstrate, and evaluate innovative pollution prevention
 techniques.  The WRITE Program  is part  of the EPA  Risk Reduction Engineering
 Laboratory's (RREL) pollution  prevention research program and is a cooperative effort
 between  the U.S. EPA and state and local environmental programs to identify, develop,
 demonstrate and  evaluate innovative pollution prevention  techniques.  Specifically, the
 Waste Reduction Program provides engineering and economic evaluations plus information
 dissemination for methodologies that  have the potential of reducing the quantity and/or
 toxicity of waste generated at the source, or to achieve practicable on-site reuse through
 recycling.

       An  Advanced  Reverse  Osmosis System  (AROS)  manufactured  by  Water
 Technologies, Inc. (WTI), Minnesota was installed in the Hewlett-Packard (HP) plant in
 Sunnyvale, California to treat and recover nickel sulfate plating rinse water. The technology
 provides zero discharge capability.  A test program is ongoing to evaluate the effectiveness
 of the AROS in the  treatment and recovery of metal plating rinse water and compare its
 costs with that of an existing chemical  precipitation system.

      The AROS unit was installed  in November  1989.  After initial installation and
 debugging, the system was  tested from November 21, 1989 to December 18, 1989. The
 system was temporarily taken off-line at the end of 1989, to allow HP to test and evaluate
 the plating bath quality and  to  create a  baseline of comparison for bath contents and
 performance.  Results were considered acceptable and  the AROS unit was restarted in
 January 1990, and has been operated on-line since then.

      The operation of the AROS unit is monitored with  computers  using specialized
software.  Samples are collected and analyzed by  HP to assess the chemical content of
various streams into and out of the AROS unit  This plan describes proposed activities
                                        39

-------
                                                           HP • QAPJP
                                                           Section No.:    J	'
                                                           Revision No.:   Q	
                                                           Date:        July 20. 199Q_
                                                           Pa«e:        2 of 3
 required to assess the AROS technology and evaluate data. Results of the evaluation will
 be presented in a final report and papers will be submitted to related technical journals and
 conferences.

       The existing wastewater treatment system for plating wastes is designated by HP as
 the "Water Purification System" (WPS).  A schematic of the processes is shown in Figure
 1-1.

       The design flow of the WPS is about 120 gallons per minute (gpm).  Rinse waters
 from various plating operations, including nickel, copper and tin are collected. Sulfuric acid
 is added to lower the pH and ferrous sulfate is added to reduce the bivalent  copper to
 monovalent copper and to form ferrous complexes with the free EDTA that is used as a
 complexing agent to solubilize copper.  The pH is then raised to 11 in a separate tank with
 the addition of sodium hydroxide causing metals to precipitate out as hydroxide salts.  The
 chemical addition is done in a completely mixed reactor. Settling occurs in three.subsequent
 tanks.  Chemical sludges are pumped to a recessed plate filter press system for dewatering.
 Dewatered sludges are disposed to an off-site RCRA-approved facility at a reported cost of
 about $275/ton for transport and disposal.  Dewatered sludge generation is about 11.5 tons
 per month.

       The effluent from the recirculation/settling tanks is pumped to 48 ultrafilters for final
 polishing.  Solids collected by the filters are recirculated back to the recirculation/settling
 tanks.  The filtrate is  discharged to the city sewer.

       A minor side stream from the ultrafiltration system is an hydrochloric acid solution
used to periodically (every 3 months) clean the filter elements.  The acid solution can be
used several times  for cleaning. Approximately 50 gallons of acid are used every 6 months.
The acid  collected from  the cleaning  process  is pumped into an onsite low flow  high
concentration neutralization system for batch treatment and disposal.  HP has good records
for the performance and costs of the existing water treatment system.
                                         40

-------
             ui    ^




           Il^l
           ^ i — m 5
           E oo > 8

           =J «2 o uj «
           u. a H- 
-------
                                                          HP - QAPjP
                                                          Section No.:   JL_	
                                                          Revision No.:  Q    	
                                                          Date:        July 20. 199Q
                                                          pa«e:        l-of 11
 2.0   PROJECT DESCRIPTION
 2.1   Background

       The demonstration ARCS unit is currently installed to treat and recycle nickel sulfate
 and nickel chloride rinse solutions.  A schematic flow diagram of the plating process units
 and the ARCS unit is shown in Figure 2-1. The nickel plating line consists of two plating
 baths followed  by a "dirty" rinse  tank  and a "clean" rinse tank.  Rinse  water flows
 countercurrent to the flow of the items being plated. The overflow from the "dirty" rinse
 tank is the influent to the AROS unit at a flow of about 4 to 5 gpm. The treated effluent
 (permeate) produced by the AROS unit becomes the clean water supply to the "clean" rinse
 tank.  A supply  of fresh  deionized water provides additional makeup water to replace
 evaporative losses.

       The AROS unit generates a concentrate at different intervals, depending upon the
 conditions of flow, conductivity and pH within the AROS  unit.  Sensors  and controls
 required to manage the membranes set the valves on and off to allow or prevent flow to or
 from the concentrate stream pipes (Figure 2-2). The concentrate is returned to the plating
 bath, as shown in Figure 2-1.

       The AROS unit is basically a reverse osmosis (RO) unit with a highly sophisticated
 design that allows recovery of rinse water and plating bath solutions.  The AROS differs
 from other reverse osmosis units by its ability to use tolerant membranes that do not require
 pH adjustment to neutral. Membrane materials and system components have been specially
 adapted to plating environments and can concentrate dilute rinse solutions to near bath
 strength (initial conductivity of the solution) without the  need for additional concentration
 technology.  The unit also contains a continuous monitoring system that monitors the
 influent, permeate and concentrate temperatures,  flow rates and conductivities every 15
 seconds.  At the HP facility, the unit has demonstrated the ability to produce concentrate
 at a nickel concentration that is about 40 to 50 percent of the original bath strength.  Figure
2-2 is an schematic diagram of the AROS unit
                                       42

-------
                                          Section

                                          Revision

                                          Date:

                                          Page;
                                                         uj   0
                                                             July 20.1990

                                                             2 of 11
        i~ UJ
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-------
                                                                  Section No.:    2_
                                                                  Revision No.:   0
Pa«e:
                                                                              3 of  11
  CLEAN RINSE
     TANK 2
                                            Specialized Rtwrsi Osmosis
DIRTY RINSE
  TANK1
                                                                           TO PLATING BATH 1
                          Figure 2-2.   Inside of a Topical AROS Unit"
     • Courtesy of Water Technologies, Inc.
                                               44

-------
                                                          HP - QAPJP
                                                          Section NOJ   2_
                                                          Revision No.:   0
                                                                         _
                                                          Date:        Ju]y 20. 199Q
                                                          Pa«e:        4L of 11.
       Existing Sampling and Monitoring Program
 22.1  Existing WPA Sampling and Monitoring Program
       The existing WPS operation performance is monitored by an on-going sampling
 program of the effluent.  The effluent from the ultrafilters is collected using 50 ml samplers
 6 times  a day at three-hour intervals during the first  two day-shifts.  These  samples are
 composited into one sample which is analyzed for parameters such as nickel, copper, iron
 and pH.  Sludge disposed to an offsite facility is not analyzed by HP.
       Existing AROS Sampling and Monitoring Program
       The existing monitoring program for the AROS includes the parameters of flow,
 conductivity and pH at various points in  the  system.  Streams monitored include the
 deionized  water makeup line, the emergency overflow to the WPS line, the concentrate
 return line and the permeate return line shown in Figure 2-2.  Readings are taken every 15
 seconds  and are displayed on screen instantaneously at an onsite monitor located at the
 facility.  Preset values of conductivity and flow control the valves.

       In addition to the continuous monitoring described above,  the first plating bath is
 sampled and analyzed weekly, collecting 1 liter samples. The analyses conducted are nickel,
 pH, Nikal  PC-3  (saccharin),  boric acid, chloride,  and  ductility of a "plate" from the
 concentrate solution. Nickel concentration is measured  to estimate how much nickel is
 recovered  and returned to the plating bath.  The quantity of recovered nickel reduces the
 amount  of new nickel that  must be added to  the plating bath to maintain the proper
 concentration for  optimum  plating conditions.   Boric acid  (approximately 50 ppm) is
 measured because the amount of boric acid needs to be determined in the plating  bath
solution for buffer. Nikal PC-3 containing an aqueous solution of organic salts (the only salt
identified on MSDS is sodium saccharin) is  added for plating operations and needs to be
maintained at a desirable level (1.4 ppm). Chloride (approximately 15 ppm) is present in
the plating bath as nickel chloride and needs to be maintained at a certain desirable level.
Ductility tests are run to check for impurities.
                                        45

-------
                                                           HP - QAPJP
                                                           Section No.:   2	
                                                           Revision No.:  Q	.
                                                           Date:        July 20. 199Q
                                                           Page:        5 of 11
       Other  analyses are conducted to estimate the  purity of the return concentrate.
During the reverse osmosis process, chemicals other than nickel are concentrated. These
parameters include VersaCLEAN 400, containing sulfamic acid and resistant breakdown
products. VersaCLEAN 400 is present in the plating bath water as a residue from previous
cleaning operations,  and resistant breakdown products result  from the high operating
temperatures  of the  nickel  plating bath.  Buildup of these compounds present in the
concentrate stream may affect the ductility of the nickel layer plated  on the circuit boards.
The ductility is tested to determine the suitability of the return concentrate to maintain the
quality in  the nickel  plating bath.  Impurities have to be kept  to  a minimum to avoid
brittleness.

       There are two kinds of ductility tests. The first one is visual and the other uses a ball
bearing method.  For visual ductility tests, a 3-inches by 5-inches brass panel is first plated
using  the  concentrate solution.  The  piece  is  then  inspected visually  for impurities
(discoloration, spots, dark or light areas, etc.).  For ball bearing tests, a piece of stainless
steel panel, 2 inches by 2 inches, is placed in the concentrate solution and plated.  The thin
metal  is then  peeled from the plate and subjected to a laboratory ductility test developed
by HP. The thin metal rectangle is placed in a ductility test apparatus and a ball bearing
is pushed slowly into it. The distance the ball moves before breaking the sheet is measured
and compared to the  known distance that provides satisfactory ductility.

       During the first month of operation of the AROS unit, concentrate was collected into
55-gallon drums before being returned to the nickel plating bath solution.  Chemical and
ductility tests  were run  to  evaluate  plating quality of the concentrate to  establish the
integrity of the  concentrate.   Chemical tests included  nickel concentration  and pH
measurements. Ductility tests were both visual and ball bearing type.

       The first 19 tests  were run on the plating  bath solution  to establish the baseline
organic impurities concentrations. Then, the AROS unit was hooked up and subsequent
ductility test results were compared to the baseline results. These tests showed that the
                                         46

-------
                                                         HP - QAPJP
                                                         Section No.:   2	
                                                         Revision No.:   Q	
                                                         Date:         July 20. 1990
                                                         Pa*c:         6 of 11
 integrity of the plating bath solution would not be in jeopardy when the concentrate stream
 is in-line with the plating operation.

 2.3    Purpose and Experimental Design
       The purpose of additional sampling and monitoring is to compare the HP laboratory's
 analysis results with the ones of an independent laboratory (SAICs) and to obtain a one-day
 snap shot of the AROS unit  operation at the facility.  It is planned to conduct additional
 analyses on a daily composite sample collected from each of the following streams (see
 Figure 2-1):
       •     Concentrate stream (returned to the plating bath)
       •     Permeate stream (recycled rinse water return)
       •     Influent stream to  the AROS unit (the dirty water rinse overflow)
       •     Deionized water (water makeup to the AROS unit)

       Due to the internal storage capacity of the AROS unit, the concentrate and deionized
water (DI) makeup streams are not continuous (Figure 2-2). Only a discrete sample can be
taken from these two streams, whereas, a one-day composite over a period of 16 hours will
be collected from the influent and permeate streams.   Dip samples will be taken from the
"dirty" rinse tank 1 and the deionized water,  storage tank for the influent stream  to the
AROS unit  and deionized water samples.  Concentrate and permeate  samples will be
obtained from ports.  Temporary storage of the concentrate during the 16-hour sample may
be necessary due to the non-continuous nature of the concentrate flow.

      The collected samples will be split and  analyzed by both the  HP laboratory and
SAICs laboratory.  HP analyses  to be run on the samples are listed in Table 2-1. SAICs
laboratory analyses will include parameters listed in Table 2-2. All measurements made by
SAIC, except TOC/Color, are critical measurements. The TOC and/or Color analyses are
proposed as possible methods to monitor the organic impurities.  One or both of these
methods will be used. However,  it is  possible that these general methods may not be able
to distinquish between the buildup of a partiepgdar compound or compounds that affect the

-------
                                                        HP - QAPjP
                                                        Section No--
                                                        Revision No.:
                                                        Date:
                                                        Page:
July 20. 199Q
7 of 11
quality of the metal plate and higher concentrations of organic compounds in general. In
other words, the buildup of a particular compound or compounds (not identified) would be
a problem; however, no noticeable change in the total organic content is observed, i.e, the
concentration of the offending compound is only a very small fraction of the total organic
or "colored" (UV and visible) compounds.
                                 TABLE 2-i

          ANALYSES WHICH WILL BE DONE BY HEWLETT-PACKARD
Parameter
Nickel (1)

pH(2)


Conductivity (2)


Method
AA
•
pH meter


Cond. meter


Detection
Limit
(ppm)
0.5

NA


NA


Stream
Influent to ARCS
Permeate
Concentrate
Influent to ARCS
Permeate
Concentrate
Influent to ARCS
Permeate
   (1)  The collected composite sample will be split and analyzed
      by the Hewlett-Packard Laboratory and SAIC's Laboratory

   (2)  One-day of monitoring data (every 15 seconds) will be provided
      by Hewlett-Packard

   NA  Not applicable
                                       48

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HP - QAPjP
Section No.:    2
Revision No.:   Q_
Date:
Page:
                                                                        -8-of 11
                               TABLE 2-2

ANALYSES PROPOSED FOR ADDITIONAL SAMPLING AND MONITORING
Pawacier
Nickel



Sulfate


Chloride



PH



Conductivity



TDS



TOC(b)



Color (b)



Method ft)
AA (EPA 249.1)
or (EPA 200.7)
AA (EPA 249.2)
or (EPA 200.7)
Gravimetric (EPA 375.3)
or
Ion chromatography (EPA 300.0)

Titrametric (EPA 325.3)



pH meter (EPA 150.1)



EPA 120.1



EPA 160.1



EPA 415.1



EPA 110.3



Detection
Limit
(ppra)
0.04
0.015
0.001
0.015
— .


—



—



—



— .



—



— _



Stream
Concentrate
Influent to AROS
Permeate
DI water
Concentrate
Influent to AROS
Permeate
DI water
Concentrate
Influent to AROS
Permeate
DI water
Concentrate
Influent to AROS
Permeate
DI water
Concentrate
Influent to AROS
Permeate
DI water
Concentrate
Influent to AROS
Permeate
DI water
Concentrate
Influent to AROS
Permeate
DI water
Concentrate
Influent to AROS
Permeate
DI water 	
   (a) Methods for Chemical Analysis of Water and Wastes. EPA/600/4-79/020, March 1979
   (b) Methods are optional; one of the two methods will be selected.
                                        49

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                                                          HP - QAPJP
                                                          Section No.:    	
                                                          Revision No.:   0
                                                          Date:        l!lIX_2fiL122Q
                                                          Pa«c:        3-of  11

 2A    Comparative Cost Etiolates for WPS and ARQ§

        An economic evaluation will be made of the ARCS system on a side-by-side basis
 with the existing WPS system. The capital cost of the AROS is $62,650. The savings from
 the AROS unit are directly related to the reduction in spending for:

        •      Water and sewer charges related to discharges to the city sewer
        »      DI production
        »      Batch waste treatment for small quantities of waste -and sludge treatment
        »      Sludge transport and disposal
        •      Purchase of new plating chemicals to make up for drag-out losses
        »      Power costs for the WPS
        «      Ultrafiltration membrane replacement
                    cos* for *« WPS (Jt  m*y be  impossible  to  quantify the  slight
             difference, if any, resulting from a 5% volume reduction)
       •     Liability costs (if applicable)
       «     Worker health and safety training costs (if applicable)
       The AROS unit will be analyzed for costs of:
       •     Power
       •     Replacement of the AROS membranes
       •     Labor
       •     Part replacement

Savings related to the recirculation of streams in the AROS unit, paybacks, health and safety
benefits, and tradeoffs, will be examined. HP has generally kept good records of costs that
can be analyzed to conduct this evaluation.
                                        50

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                                                          HP - QAPJP
                                                          Section No.:   2   _
                                                          Revision Nou   jQ __
                                                          Datc:         Julv 20. 1990
                                                                      Jfl-of  11
2-5    Organization and Responsibility

       A project organization and authority chart is shown in Figure 2-3.  The California
DHS and HP are cooperating with the Risk Reduction Engineering Laboratory (RREL) on
this  evaluation.  Mr.  Curtis Schmidt  is the SAIC Work  Assignment Manager and  is
responsible for the technical and budgeting aspects of this work assignment  Mr. Thomas
Wagner is QA Manager and prepared this QAPJP and is responsible for QA oversight on
this work assignment.  Mrs. Ilknur Erbas-White will handle the day-to-day activities of the
project.

2.6    Schedule

       The sampling is scheduled  for mid to late August or early September, 1990.
                                       51

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                      HP - QAPJP
                      Section No.:
                      Revision No.:
                      Date:
                      Page:
July 20. 199Q
11  of  11
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-------
                                                          HP- QAPJP
                                                          Section No,:
                                                          Revision No.:
                                                                      July 20. 199Q
                                                         Page:         1 of 2
3.0    QUALITY ASSURANCE OBJECTIVES
3<1    Precision. Accuracy, Completeness, and Method Detection Ljmits
       Objectives for accuracy, precision, method detection limits, and completeness for the
critical measurements are listed in Table 3-1.   Accuracy (as percent  recovery) will be
determined from matrix spike recovery for nickel, sulfate, and chloride, and from laboratory
control samples for pH,  conductance and TDS.  Precision (as relative percent difference)
will  be determined from the results of matrix spike duplicates for nickel,  sulfate, and
chloride, and from laboratory duplicate analyses for pH, conductance and TDS.  The
completeness will be determined from the number of data meeting the criteria in Table 3-1
divided by the number of samples collected.

3-2    Representativeness and Comparability
       Representativeness  and Comparability are qualitative parameters.  The samples
obtained will be as representative  of a  typical day's operation as the day's operation is
typical.  Regardless of how typical the  operation is,  the purpose will  be accomplished
because a independent comparison of the HP laboratory's analysis will be obtained.  The
data obtained in this program will be comparable because all the methods are taken from
a standard EPA reference manual.

3-3    Method Detection Limits
       It is anticipated that the deionized water and the permeate sample might have values
below the method detection limits.  Since both streams approach a "distilled water" matrix,
listed detection limits should apply.  All other streams are also aqueous streams; therefore,
the only adjustments that should be necessary are those caused by dilutions necessary to
remain within the calibration range of the methods.
                                        53

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                     HP- QAPjP
                     Section No.:
                     Revision No.:
                     Date:
                     Page:
July 20..
   of 2






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54

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                                                            HP - QAPJP
                                                            Section No.:
                                                            Revision No.:
                                                            Date:
                                                                       i-2LJ
        The sampling points were shown in Figure 2-2.  Each influent stream (dirty water
  rinse overflow and  DI makeup) and each effluent stream (concentrate returned to the
  plating bath and permeate added to the final rinse bath) of the AROS unit will be sampled.

        The one-day  composite sample schedule is given in Table 4-1.  HP personnel will
  colJect the samples and SAIC will observe the collection and handling of the samples.

        Table 4-2 lists each parameter to be determined, the required preservation method
  the maximum holding, the nominal analytical volume, the minimum volume required for
  analysis including  QC,  and  the  sample  size  to  be obtained  in the field.  The sample
  container size is roughly twice the minimum required volume.

       A separate 1 liter bottle will be used for each of the four streams to preclude any
 cross contamination.  The aliquots for the composite  samples will be stored in  5-galIon
 plastic containers with lids until all portions are obtained. These 5-gallon containers will
 be mixed by swirling anddispensed into triplicate bottles of 500, 180 and 2000 ml each and
 preserved according to Table 4-2. One set will be given to HP, one will be shipped to the
 laboratory for analysis, and one will be shipped to  the laboratory and held in reserve.

      The DI water permeate and concentrate samples (aliquots) will be obtained from
 taps in  these lines.   These taps will be opened momentarily  and flushed into  a waste
 container prior to obtaining each aliquot The influent samples (aliquots) will be obtained
 by dippmg a 1 liter container into the dirty rinse tank near the outfall to the AROS influent
 line.

      Sample bottles  win either be purchased from I-CHEM (precleaned) or cleaned by
the procedure for metals in SW-846, 3rd. Ed., Chapter 3.
                                        55

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                            HP - QAPjP
                            Section No.:   1
                            Revision No.:  JJ.
                            Date:
                            Page:
                                                                       July 20.
TABLE 4-1.   Proposed Sampling Schedule
       Location
               Sampling Procedure
    Influent to the
    AROS unit.
Composited over a period of 16 hours
during two shifts. Two 2-liter dip samples
from the dirty rinse tank will be taken
per shift.  Final composite will be split;
one sample will be sent to SAIC's laboratory,
the other will be analyzed by the Hewlett-
Packard laboratory.
    Permeate
Composited over a period of 16 hours
during two shifts. Two 2-liter samples will
be taken per shift from a sample port. Final
composite will be split; one sample will be
sent to SAIC's laboratory,  the other will be
analyzed by the Hewlett-Packard laboratory.
    Concentrate
One 8-liter sample will be collected during
the two shifts. When the concentrate flow
occurs as observed from the AROS unit computer
monitor, a sample will be collected from the
sample port, or temporary storage will be
provided to get an 8-liter sample.  The
sample will be split; one sample will be sent
to SAIC's laboratory, the other will be
analyzed by the Hewlett-Packard laboratory.
   DI water
One 8-liter sample will be collected from the
DI water storage tank.  The sample wuTbe
split; one sample will be sent to SAIC's
laboratory, the other will be analyzed by
the Hewlett-Packard laboratory.
                                        56

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                       HP - QAPjP
                       Section No.:
                       Revision No.:
                       Date:
                       Page:
July 20.
  of  7
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                                                           HP - QAPJP
                                                           Section No.:
                                                           Revision No.:
                                                                       July 20. 1900
                                                          Pa8«:         4 of 7
       The field personnel will document, on data sheets (Figure 4-3), the date and time
each aliquot is obtained from each stream.  The volumes obtained for each aliquot will be
the same because the same 1 liter container (one bottle for each stream) will be filled'each
time an aliquot is obtained.  (The 1 liter container will be filled more than once to obtain
the required volume for each aliquot or sample.)

       The amount of preservative added will also be recorded. Samples will be labeled
(see Figure 4-4) and shipped  by overnight delivery service to the  laboratory in coolers
containing ice.  If "blue" ice is used in the coolers,  samples will be initially  cooled .with
regular ice prior to being packed in the coolers with blue ice.

       The Chain of Custody Record shown in Figure 4-5 will be completed for each cooler
shipped to a laboratory.
                                         58

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                                                HP - QAPJP
                                                Section No.:
                                                Revision No.:
                                                Date:
                                                Page:
                                             July 20.
                                             5 of 7
            QUALITY ASSURANCE AND QUALITY  CONTROL FORMS
          FOR THE HEWLETT-PACKARD ARCS UNIT SAMPLING EVENT
 SAMPLE:  COMPOSITE       GRAB
 (Circle) DUPLICATE       BLANK
                       DIP
                                PORT
                                  OTHER
SAMPLE NUMBER:
SAMPLE TYPE:
(Circle)
 LOW CONC.
        AVERAGE CONC.
                                    HIGH CONC.
SAMPLE TAKEN AT:
        DATE
                                          TIME:
                                                      AM/PM
FOR  COMPOSITE SAMPLES ONLY:
Composite 1:
Composite 2:
Composite 3:
Composite 4:
Composite 5:
Composite 6:
Composite 7:
SHIFT:
SHIFT:'
SHIFT:"
SHIFT:"
SHIFT:"
SHIFT:"
SHIFT:"
Composite 8: SHIFT:"
DATE:
•DATE:
DATE:
DATE:
DATE:
DATE:
DATE:
DATE:
    90 TIME: 	
    90 TIME: 	
    90 TIME: 	
    90 TIME: 	
	/90 TIME: 	
	/90 TIME: 	
    "90 TIME: 	
    90 TZME:
AM/PM
AM/PM
AM/PM
AM/PM
AM/PM
AM/PM
AM/PM
AM/PM
VOL:
,VOL:
VOL:
VOL:
VOL:
VOL:
VOL:
VOL:
.I/ml
.I/ml
.I/ml
.I/ml
.I/ml
.I/ml
COMMENTS:
                     Figure 4-3.  Sampling Data Sheet
                                 59

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                                                    HP - QAPjP
                                                    Section No.:   ±_
                                                    Revision No.:  0
                                                    Date:         July 20. 199Q
                                                                  6 of  7
                 8400 Westpark Drive, McLean, Virginia 22102
Location:	        Project No.:
Sample Date/Time:
Sample No.:	Sample Location:
Analysis:
Collection Method:      	.	Purge Volume:

Preservative:	
Comments:

                                              Collector's Initials:
                  Figure 4-4.   Example Sample Label
                                  60

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                       HP - QAPJP
                       Section No.:    £_	
                       Revision No.:   Q_	
                       Date:          July ffl I99Q
                       Pa«e:          7 of 7
                                                         •s
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                                                        *s
                                                        £

                                                        §
61

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                                                         HP - QAPJP
                                                         Section No.:    	
                                                         Revision No.:   ^
                                                         Datc:         Julv 20. iQgp
                                                         Pa8c:         JLfl£_l__

 5.0    ANALYTICAL PROCEDURES AND CALIBRATION
       Analytical procedures for all critical measurements are referenced in Table 3-1. The
 only other measurement is color or TOC that will be performed according to method 1103
 or 415.1 from the same reference. These are all EPA procedures and specify the required
 calibration to be performed. The samples for metal analysis will be digested according to
 the procedure in Section 4.1.3 of the same reference. For those procedures requiring a
 calibration curve, the calibration will be verified after this sample set is ma  For example,
 there will be two samples for metals analysis by flameless AA plus three QC samples for
a total of five samples. After initial calibration, these five samples will be analyzed followed
by a calibration check that must agree within _+ 20 percent of its original value.
                                       62

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                                                          HP - QAPJP
                                                          Section No.:    &	
                                                          Revision No.:   Q_	
                                                          Date:         July 20. 199Q
                                                          Pa8e:         1 of 1
6.0    DATA REDUCTION, VALIDATION, AND REPORTING
       Data will be reduced by the procedures specified in the methods and reported by the
laboratory in the units also specified in the methods.  The work assignment manager or his,
designee will review the results and compare the QC results with those listed in Table 3-1.
Any discrepancies will be discussed with the QA Manager.

       All data will be reviewed to ensure that  the correct codes and units have  been
included.  After reduction, data will be placed in tables or arrays and reviewed again  for
anomalous values.  An inconsistencies discovered will be resolved immediately, if possible,
by seeking clarification from the sample collection personnel responsible for data collection,
and/or the analytical laboratory.
                                        63

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                                                       HP - QAPJP
                                                       Section No.:   1	,
                                                       Revision No.:   Jl_	
                                                       Date:        July 20. 1990
                                                       PaS«-'        I of 2
7.0   INTERNAL QUALITY CONTROL CHECKS
      Due to the nature of this project, the collection of field blanks, equipment blanks,
and trip blanks are not deemed necessary.  The internal QC checks appropriate for the
measurement methods to be utilized for this project are summarized in Table 7-1.  These
items are taken from the methods and the QC program outlined in Section 3 of this QAPjP.
Because the number of samples to be analyzed for this project is small, all samples and
related QC will be analyzed in one batch.

      For this project, a  matrix spike/matrix spike duplicate (MS/MSD) or laboratory
duplicate analysis will be performed on two samples, because the pure water streams (DI
water and permeate) and the contaminated water streams (AROS influent and concentrate)
are considered different matrices.
                                       64

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                        Section No.:
                        Revision No.:
                        Date;
                        Page:
July 20. 1990
JL of 2
j

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                                                         HP - QAPJP
                                                         Section No.:    &_
                                                         Revision No.:   0
                                                         Dale:         July 20. 1990
                                                         Pa«c:         1 of 1
8.0   PERFORMANCE AND SYSTEM AUDITS

      No audits are planned for this project.
                                       66-

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                                                          HP - QAPJP
                                                          Section No.:
                                                          Revision No.:
                                                          Date:
                                                          Page:
  9.0    CALCULATION OF DATA QUALITY INDICATORS

  9.1    Accuracy

        Accuracy for nickel, sulfate, chloride, and TOC will be determined as the percent
  recovery of matrix spike samples (two per matrix).  The percent recovery  is calculated
  according to the following equation:
              % R  =  100% x
Q-c0
 where
       %R   =  percent recovery
       Q     ==  measured concentration in spiked sample aliquot
       ^0     -  measured concentration in unspiked sample aliquot
       <-,     =  actual concentration for spike added


       Accuracy for the other critical measurements, except PH, will be determined from
 laboratory control samples according to the equation:
                   »  100%
                             '  Q
 where
       %R   =  percent recovery
       Cm    =  measured concentration of standard reference material
       <~t     -  actual concentration for standard reference material

       For pH, accuracy will be determined as bias according to the equation:


               B  =  PH, - pH,
where
      B     == bias
      pHm  = measured pH of standard reference material
            = actual pH of standard reference material
                                       67

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                                                        HP-QAPJP
                                                        Section No.:   $_
                                                        Revision No.:  0_
                                                                    JuK 20. 1990
                                                        Pa«e:        2  of 2
 93,    Precision
       Precision will be determined from the difference of percent recovery values; of MS

 and MSDs for nickel, sulfate, chloride, and TOC, and duplicate laboratory analyses for other

 parameters.  The following equation will be used for all parameters except pH:


             RPD  =     [Ci - CJ x  100%

                         IP, .+  CJ/2

 where
       RPD  =  Relative percent difference
       CL    =  The larger of two observed values
       GZ    =  The smaller of the two observed values


       Precision for pH will be estimated by calculation of the range using the following
 equation:                                                                      6
             D(pH) =   PHX - PH2

where
      D(pH)      =  precision limits for pH
      pHi,pH2     =  observed values for duplicate samples
93   JComp]etenes$

      Completeness will be calculated as the percent of valid data points obtained from the
total number of samples obtained.


      % Completeness = VDP x  100
                         TOP
where

      VDP = number of valid data points
      TDP = total number of samples obtained.
                                        68

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                                                           HP - QAPJP
                                                           Section No.:    JQ	
                                                           Revision No.:   0
                                                           Daf<«-         T i_ ~* ~	'
                                                                        jUfV 7f) 10QQ
                                                           Page:         -UoL-L—
 10.0   CORRECTIVE ACTION


        Corrective actions will, be initiated whenever quality control limits (e.g., calibration
 acceptance criteria) or QA objectives (e.g., precision, as determined by analysis of duplicate
 matrix spike samples) for a particular type of critical  measurement are not being met
 Corrects actions may result from any of the following functions:
•
•
             Performance evaluation audits
             Technical systems audits
       •     Interlaboratory/interfield comparison studies

       All corrective action initiations, resolutions, etc. will be implemented immediately and
will be reported in Sections One and Two (Difficulties Encountered and Corrective Actions
Taken, respectively) in the  existing monthly progress reporting mechanisms  established
between  SAIC  and EPA-RREI.  and in the  QA section  of the final report  Tne QA
Manager will determine if a correction action has resolved the QC problem.
                                       69

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                                                         HP - QAPJP
                                                         Section No.:    1}
                                                         Revision No.:   0 .
                                                         Date:        July 20. 199Q
                                                         Pa««:        -Lof 1
11.0   QA/QC REPORTS TO MANAGEMENT
       This section describes the periodic reporting mechanism, reporting frequencies, and
the final project report which will be used to keep project management personnel informed
of sampling and analytical progress, critical measurement systems performance, identified
problem conditions, corrective actions, and up-to-date results of QA/QC assessments  As
a minimum, the reports will include, when applicable:

       •     Changes to the QA Project Plan, if any.
       •     Limitations or constraints on the applicability of the data, if any.
       •     The status of QA/QC programs, accomplishments and corrective actions.
       •     Assessment  of data quality in terms of precision, accuracy, completeness,
             method detection limit, representativeness, and comparability.
       •     The final report shall include a separate QA section that summarizes the data
             quality indicators that document the QA/QC activities that lend support to
             the credibility of the data and the validity of the conclusions.

       For convenience, any QA/QC reporting will be incorporated into the already well-
established monthly progress reporting system between SAIC and EPA-RREL for all TESC
Work Assignments.   Any information  pertaining to the above-listed categories will be
reported under Sections One thru  Three (Difficulties Encountered, Corrective Actions
Taken, and Current Activities, respectively) in the monthly reports.
                                         70

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July 21, 1993

Format review for R-2022
WATTS NICKEL AND RINSE WATER RECOVERY VIA AN ADVANCED REVERSE
OSMOSIS SYSTEM
Project Officer: Lisa M. Brown

This draft report requires a few adjustments before it is ready for publication. This review
is for format only, not for editorial or for content. Needed changes are listed below.
Assistance in making these changes can be found in the Handbook for Preparing Office of
Research .and Development Reports.

1. The Abstract should have the work done under statement as the last paragraph.
   (samples enclosed). Delete advertising of the company name and/or address at the top
   or bottom of pages in Appendix B

2. The final camera ready copy must be typed within the image area shown on the
   enclosed typing guide sheets with the page numbers centered. All text, including
   figures and tables, must fit within the image area. Furnish originals or very good
   reproducible copies of the figures and tables.

3. Your Project Summary has been sent out for editing and will be returned to you as
   soon as possible.

4. After the adjustments are made, prepare your project report/project summary package
   for clearance using the forms indicated in the checklist for clearance packages. After
   clearance, we will need the adjusted camera-ready copy of the report plus two copies if
   the report is going to NTIS only or camera-ready plus one if the report will be printed.
   Adjust the project  summary  and supply us with corrected hard copy and a 31/2
   in. disk,  with latest  revisions  in  WordPerfect 5.1 format. Be sure to
   include all  tables and graphics (with format identified) on the disk.

If you have any questions, please call.

Robert M. Roetker (513) 569-7926

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