Revision 0-6/15/01
Concttrteni
Technologies
U.S. Environmental Protection Agency
Environmental Technology Verification Program
For Metal Finishing Pollution Prevention Technologies
Verification Test Plan
for the
Evaluation of Hydrometrics, Inc. High Efficiency Reverse Osmosis
(HERO™) Industrial Wastewater Treatment System
Revision 0
June 15, 2001
Concurrent Technologies Corporation is the Verification Partner for the EPA ETV Metal
Finishing Pollution Prevention Technologies Center under EPA Cooperative Agreement
No. CR826492-01-0.
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Revision 0-6/15/01
Technvfogies
U.S. Environmental Protection Agency
Environmental Technology Verification Program
For Metal Finishing Pollution Prevention Technologies
Verification Test Plan
for the
Evaluation of Hydrometrics, Inc. High Efficiency Reverse Osmosis
(HERO™) Industrial Wastewater Treatment System
June 15, 2001
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TITLE: Evaluation of Hydrometrics, Inc. High Efficiency Reverse Osmosis
(HERO™) Industrial Wastewater Treatment System
ISSUE DATE: June 15, 2001
DOCUMENT CONTROL
This document will be maintained by Concurrent Technologies Corporation in accordance with
the EPA Environmental Technology Verification Program Metal Finishing Technologies Quality
Management Plan. Document control elements include unique issue numbers, document
identification, numbered pages, document distribution records, tracking of revisions, a document
MASTER filing and retrieval system, and a document archiving system.
ACKNOWLEDGMENT
This is to acknowledge Valerie Whitman and Marvin South (CTC), Mike Stites (Honeywell
FM&T), and Mark Reinsel, Ph.D., P.E. (Hydrometrics, Inc.) for their help in preparing this
document.
Concurrent Technologies Corporation is the Verification Partner for the EPA ETV Metal
Finishing Pollution Prevention Technologies Center under EPA Cooperative Agreement
No. CR826492-01-0.
11
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Environmental Technology Verification for Metal Finishing Technologies Program
(ETV-MF) Verification Test Plan for the Evaluation of Hydrometrics, Inc. High Efficiency
Reverse Osmosis (HERO™) Industrial Wastewater Treatment System.
PREPARED BY:
a
C.hns
RTV-MF Project Manager
f'* Project
APPROVED BY:
Clittfon E.
CTTQAManecr
Dunn W. Rr(m--n
CTC ETV-Mf Program
AWQ£.
EPA ETV Center
Inc.
7/S/o i
Date
^r% r^
Signature denotes acceptance of this test plan as written regarding experimental design, quality assurance, test and
analysis methods, operational procedures, equipment configuration, project management and current HERO™
system operating effectiveness prior to testing.
in
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TABLE OF CONTENTS
Page
1.0 INTRODUCTION 1
1.1 Background 2
1.2 Data Quality Objectives (DQO) 3
2.0 TECHNOLOGY DESCRIPTION 3
2.1 Theory of Operation 3
2.2 Commercial Status 5
2.3 Pollution Prevention Classification 5
2.4 Environmental Significance 6
3.0 PROCESS DESCRIPTION 8
3.1 Equipment and Flow Diagram 8
3.2 Test Site 9
3.3 KCP Conventional Wastewater Treatment System 10
3.3.1 Copper Recovery & Cyanide Oxidation 10
3.3.2 Chromium Reduction 11
3.3.3 Lime Precipitation & Clarification 11
3.4 Hydrometrics Mobile HERO™ Unit Installation at KCP 12
3.4.1 Pretreatment 12
3.4.1.1 Prefiltration & SAC Ion Exchange Treatment 12
3.4.2 HERO™ System 12
3.4.2.1 WAC Ion Exchange Treatment 12
3.4.2.2 Membrane Degasification 12
3.4.2.3 pH Adjustment and Reverse Osmosis (RO) 12
4.0 EXPERIMENTAL DESIGN 13
4.1 Test Goals and Objectives 13
4.2 Critical and Non-Critical Measurements 14
4.3 Test Matrix 15
4.3.1 HERO™ System Wastewater Recovery-Test #1 15
4.3.2 WAC Ion Exchange Unit Copper Recovery - Test #2 15
4.4 Operating Procedures 18
IV
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4.5 Sampling, Process Measurements, and Analytical Methods 18
4.5.1 Sampling Responsibilities & Procedures 18
4.5.2 Process Measurements 22
4.5.3 Testing Parameters 25
4.5.3.1 Flow Rate 25
4.5.3.2 Temperature 25
4.5.3.3 pH 25
4.5.3.4 Specific Conductivity 25
4.5.3.5 Total Suspended Solids (TSS) 26
4.5.3.6 Total Dissolved Solids (TDS) 26
4.5.3.7 Oil & Grease (O&G) 26
4.5.3.8 Metals 26
4.5.3.9 Additional Proposed MP&M Limits 27
4.5.3.10 Additional KCP Recycled Water Quality Standards 27
4.5.4 Calibration Procedures and Frequency 28
4.5.5 Mass Balance 28
4.5.6 Energy Use 30
4.5.7 Cost Analysis 30
4.5.8 Waste Generation Analysis 31
5.0 QUALITY ASSURANCE/QUALITY CONTROL REQUIREMENTS 31
5.1 Quality Assurance Objectives 31
5.2 Data Reduction, Validation, and Reporting 31
5.2.1 Internal Quality Control Checks 31
5.2.2 QA/QC Requirements 32
5.2.2.1 Duplicates 32
5.2.2.2 Matrix Spikes 33
5.2.2.3 Field Blanks 33
5.2.3 Calculation of Laboratory Data Quality Indicators 33
5.2.3.1 Precision 34
5.2.3.2 Accuracy 34
5.2.3.3 Comparability 35
5.2.3.4 Completeness 35
5.2.3.5 Representativeness 35
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5.2.3.6 Sensitivity 35
5.3 Quality Audits 36
6.0 PROJECT MANAGEMENT 37
6.1 Organization/Personnel Responsibilities 37
6.2 Test Plan Modifications 38
6.3 Schedule/Milestones 38
6.4 Documentation/Records 38
7.0 EQUIPMENT 38
7.1 Equipment List and Utility Requirements 38
7.2 Monitoring/Sampling Equipment 39
8.0 HEALTH AND SAFETY PLAN 40
8.1 Hazard Communication 40
8.2 Emergency Response Plan 40
8.3 Hazard Controls Including Personal Protective Equipment 40
8.4 Lockout/Tagout Program 41
8.5 Material Storage 41
8.6 Safe Handling Procedures 41
9.0 WASTE MANAGEMENT 41
10.0 TRAINING 41
11.0 REFERENCES 42
12.0 DISTRIBUTION 42
LIST OF FIGURES
Figure 1: HERO™ Wastewater Treatment Diagram - Simplified 4
Figure 2: HERO™ System Chemical Reactions 7
FigureS: HERO™ Wastewater Treatment System 9
Figure 4: HERO™ Wastewater Treatment System Diagram -Detailed 11
Figure 5: KCP's Mobile HERO™ System 13
Figure 6: Test Data Collection Form 23
Figure 7: Fundamental Material Balance Equation 29
Figure 8: Material Balance Equation for KCP HERO™ System 29
VI
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LIST OF TABLES
Table 1: Objectives and Related Test Measurements for Evaluation of the HERO™ System.... 17
Table 2: Sample Quantities 19
Table 3: Test Matrix 20
Table 4: Aqueous Samples 21
Table 5: QA Objectives for Precision, Accuracy, and Detection Limits 24
Table 6: Equipment List and Utility Requirements 39
Table 7: Monitoring/Sampling Equipment 40
LIST OF APPENDICES
APPENDIX A: ETV-MF Operation Planning Checklist A-l
APPENDIX B: Job Training Analysis Form B-l
APPENDIX C: ETV-MF Project Training Attendance Form C-1
APPENDIX D: Test Plan Modification D-l
vn
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amp
ATC
C
°C
cm
coc
CSR
CTC
CWA
DOE
DQO
EPA
ETV-MF
FM&T
ft2
ft3
gal
gfd
gpd
gpm
HOPE
HEM
HERO™
hp
hr)
Hz
1C
ICP-AES
ID
IDL
KCP
kWh
JTA
L
LM
MBS
MDL
mg
mg/L
mL
MMTC
MP&M
MRL
MS
ACRONYMS & ABBREVIATIONS
Ampere(s)
Automated Temperature Compensated
Specific Conductivity
Degrees Celsius
Centimeter
Chain of Custody
Code of State Regulations
Concurrent Technologies Corporation
Clean Water Act
U.S. Department of Energy
Data Quality Objectives
U.S. Environmental Protection Agency
Environmental Technology Verification for Metal Finishing
Federal Manufacturing & Technology
Square Feet
Cubic Feet
Gallon
Gallons of Permeate Produced per Square Foot of Membrane per Day
Gallons per Day
Gallons per Minute
High Density Polyethylene
Hexane Extractable Material
High Efficiency Reverse Osmosis System
Horsepower
Hour
hertz
Ion Chromatography
Inductively Coupled Plasma - Atomic Emission Spectroscopy
Identification
Instrument Detection Limit
Kansas City Plant
Kilowatt-Hour
Job Training Analysis
Liter
Laboratory Manager
Metabisulfite
Method Detection Limit
Milligram
Milligrams per Liter
Milliliter
Michigan Manufacturing Technology Center
Metal Products & Machinery
Method Reporting Limit
Matrix Spike
Vlll
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MSD
MSDS
Hg
us
NA
O&G
O&M
OOP
P
PARCCS
PM
POC
POTW
PPE
ppm
psi
PVD
QA/QC
QMP
R&D
RO
RPD
SAC
SP-
SR
SSR
IDS
TEFC
TOC
ISA
TSS
U.S.
VOC
WAC
ACRONYMS & ABBREVIATIONS (continued)
Matrix Spike Duplicate
Material Safety Data Sheet
Microgram
Micro-Siemens
Not Applicable
Oils and Grease
Operating & Maintenance
Open Drip-Proof
Percent Recovery
Precision, Accuracy, Representability, Comparability, Completeness and
Sensitivity
Program Manager
Point of Contact
Publicly Owned Treatment Works
Personal Protective Equipment
Parts per Million
Pounds per Square Inch
Physical Vapor Deposition
Quality Assurance/Quality Control
Quarterly Management Plan
Research & Development
Reverse Osmosis
Relative Percent Difference
Strong Acid Cation
Sampling Point
Sample Result
Spiked Sample Result
Total Dissolved Solids
Totally Enclosed Fan-Cooled
Total Organic Carbon
Technical System Audit
Total Suspended Solids
United States
Volatile Organic Carbon
Weak Acid Cation
IX
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1.0 INTRODUCTION
The purpose of this test plan is to document the objectives, procedures, equipment, and
other aspects of testing that will be utilized at Honeywell Federal Manufacturing &
Technology's (FM&T's) Kansas City Plant (KCP), in Kansas City, Missouri, during
verification testing of a three-stage reverse osmosis wastewater treatment system
manufactured by Hydrometrics, Inc. (Hydrometrics). Hydrometrics' High Efficiency
Reverse Osmosis (HERO™) wastewater treatment system is a pollution prevention
technology applicable to metal finishing operations that generate wastewater from
chemical rinses and spent baths, as well as collected storm water and spill residues. This
test plan has been prepared to evaluate the performance of the technology in conjunction
with the U.S. Environmental Protection Agency's (EPA's) Environmental Technology
Verification for Metal Finishing (ETV-MF) Program. The objective of the ETV-MF
Program is to identify promising and innovative pollution prevention treatment
technologies through EPA-supported performance verifications and to provide objective
performance data to providers, purchasers, and permitters of environmental technologies.
Hydrometrics, founded in 1979 and located in Helena, Montana, distributes the HERO™
industrial wastewater treatment system, which uses a three-stage reverse osmosis
treatment process to remove and concentrate metals for recovery while producing a high
quality product water for recycle and reuse. The three steps involved in the HERO™
process are ion-exchange, membrane degasification, and reverse osmosis. The system
reportedly recovers nearly 100 percent of valuable metals, which may be suitable for
direct recycle back to the process as a liquid or recovered as scrap metal using traditional
electro winning technologies. Treated water produced in the process is reported to be
high quality and may be suitable for direct recycle as process water make-up, cooling
water make-up, boiler feed water, or direct discharge. The HERO™ technology was
developed by Deb Mukhopadhyay in 1996 to provide ultra-pure water to the
microelectronics industry. Since that time, the now-patented technology has been tested
on several industrial wastewater applications in industries where large quantities of
wastewater are typically generated.
FM&T is evaluating a 15 gallon per minute (gpm) pilot scale HERO™ system at the
KCP, and upon successful completion of the evaluation, they have the option to install a
full-scale 100-200 gpm unit, which will treat all KCP wastewater. The 15 gpm HERO™
system is commercially available from Hydrometrics, Inc. KCP is owned by the U.S.
Department of Energy (DOE), and is operated by Honeywell FM&T. KCP manufactures
a wide variety of products for national defense systems. More than 95 percent of the
work done at the KCP is for the DOE. For over 50 years, the KCP has manufactured
some of the DOE's most intricate and technically demanding products. They produce
over 40 different lines of products ranging from semiconductors to semi-trailers, which
include electronic, mechanical, engineered material, and plastics manufacturing
technologies. The large size and wide array of operations associated with the KCP make
it an ideal site for demonstrating the diversity of the HERO™ system for metal finishing
industries in general.
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This project will evaluate the ability of the Hydrometrics HERO™ system to treat and
recycle the KCP's combined wastewater for reuse in the plant. A separate Hydrometrics
copper recovery unit will also be evaluated in its ability to recover copper from a cyanide
waste stream. Metal recovery is normally done within the HERO™ system, but due to
precipitation and removal of the copper during a pretreatment step, the installation of a
second ion exchange unit is required. This ion exchange unit uses identical resin to the
integral HERO™ system ion exchange unit, but on a smaller scale, and must be installed
before the KCP's conventional cyanide destruction pretreatment step. Evaluating and
verifying the performance of the Hydrometrics system will be accomplished by collecting
operational data and in-process samples for analysis. The resultant test data will be used
to prepare a material balance and determine the efficiency of water treatment/reuse and
metals recovery for a given set of operating conditions.
The test plan described in this document has been structured to allow the above
objectives to be met using sound scientific principles. This document explains testing
plans with respect to areas such as test methodology, procedures, parameters, and
instrumentation. Section 5.0 describes Quality Assurance/Quality Control (QA/QC)
requirements of this task that will ensure the accuracy of data. Also presented within this
document are data interpretation procedures and hypothesized results. Worker health and
safety considerations are covered in section 8.0.
This test plan will be available at the test site, and verification testing will be conducted
in accordance with the test plan requirements.
1.1 Background
There are more than 15,000 companies in the U.S. that perform metal finishing
operations. These companies discharge their process wastewaters either directly to
waterways or indirectly to Publicly Owned Treatment Works (POTWs). Metal finishing
generates more individual wastewater discharges than any other industrial category [Ref.
1]. Many pollutants contained in metal finishing process waters are toxic, so to comply
with Clean Water Act (CWA) requirements, the wastewaters are treated before being
discharged. Regulations, in general, require reduction of hexavalent chromium, oxidation
of cyanides, removal of heavy metals, and pH control.
The KCP has several plating, coating, and other metal processing operations that generate
wastewaters that are combined with other non-process industrial wastewaters and treated
in a conventional on-site wastewater treatment system, and then discharged to a POTW.
The HERO™ system will be installed before or after the conventional system to process
the wastewater so it can be reused at KCP. Copper from the cyanide process rinse water
will be concentrated in a separately installed recovery unit, and calculated using a copper
mass balance on the influent and the effluent to this unit. The recycle of metal finishing
wastewaters is of great importance, not only from a financial standpoint, but a regulatory
standpoint as well. Many of the heavy metals found in metal finishing wastewaters are
considered toxic by EPA. Heavy metals such as copper and chromium have also been
identified as high priorities for reduction/elimination and off-site recovery from plating
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operations by the National Metal Finishing Research & Development (R&D) Plan, and
are addressed in the Strategic Goals Program regarding toxic metals reduction/utilization.
Typical reverse osmosis (RO) wastewater treatment systems can be costly and difficult to
operate. Membranes may foul easily and require replacement, organics in the wastewater
are only moderately rejected, and costly anti-sealant additions and activated carbon
pretreatment are often required. Conventional RO systems typically exhibit a low
operating flux and a product water recovery of only 75 percent. Due to the high
operating pH of the reverse osmosis step, Hydrometrics' HERO™ system is essentially
immune to fouling, thus extending the membrane life and increasing the operating flux by
up to two times that of conventional RO. The HERO™ system exhibits a higher rejection
of organics, requires no anti-sealant additions, and has a product water recovery of up to
95 percent. This results in the potential for low-cost, zero-liquid discharge operations, or
wastewater that meets most existing discharge permits. Recycling wastewater on-site and
metals off-site reduces water consumption and discharge levels, resulting in lower water
and waste disposal costs. The HERO™ system reportedly solves the problems normally
associated with standard RO systems, and does so with reduced installation investment
and operating costs.
1.2 Data Quality Objectives (DQO)
The systematic planning elements of the data quality objectives process identified in
"Guidance for the Data Quality Objectives Process" (EPA QA/G-4, August 2000), were
specifically utilized during preparation of this verification test plan. The project team,
composed of representatives from CTC, the testing organization, the technology vendor,
the host site, and the US EPA, who assisted in preparing this test plan, jointly developed:
the test objectives, critical and non-critical measurements, the test matrix, sample
quantity, type, and frequency, analytical methods, and quality assurance objectives to
arrive at an optimized test designed to verify the performance of the technology.
2.0 TECHNOLOGY DESCRIPTION
2.1 Theory of Operation
The patented HERO™ process for which Hydrometrics is licensed combines "off-the-
shelf technologies to convert wastewater into reusable water. Figure 1 shows a
simplified diagram of the HERO™ process for wastewater purification.
In the first step of the HERO™ process, ion exchange removes ions that form scale.
Removing the hardness from the wastewater results in a waste being generated as a
concentrated brine solution. The second step is membrane degasification, which removes
the buffering effect from carbon dioxide to lower caustic demands in the final step of the
process. Carbon dioxide is the only byproduct of the second step, where the wastewater
alkalinity is removed. The final step in the HERO™ process is reverse osmosis. The
high pH of the wastewater entering this stage eliminates fouling of the RO membrane. A
concentrated brine solution waste is generated from this step as well.
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According to Hydrometrics, the combined, concentrated brine solutions from the
HERO™ process represent a single waste stream, generally less than five percent of the
feed stream and usually suitable for direct discharge to a POTW. Alternatively, the waste
stream could be evaporated to dry solids, since the volume of water is greatly reduced
compared to waste streams generated in a traditional RO system. Evaporation of the
waste stream may help in becoming a zero-liquid discharging facility.
Hydrometrics claims the HERO™ system can handle more total suspended solids (TSS),
oil & grease (O&G), residual chlorine, and biological activity than traditional RO
systems. They have installed units capable of treating a broad range of wastewater
streams with total dissolved solids (IDS) ranging up to 30,000 mg/L.
Waste
Water
Step #1
Ion
Exchange
^^ Step #2
co R"nRl Membrane
Degasification
Step #3
C Reverse
Osmosis
Purified
Water
Figure 1: HERO™ Wastewater Treatment Diagram - Simplified
The diagram in Figure 2 illustrates the reactions that typically take place within each step
of the HERO™ process. Hydrometrics has designed permanently installed HERO™
systems in a wide range of wastewater flow. For the verification testing, KCP will have a
mobile, 15 gpm unit installed following their conventional wastewater treatment system.
The 15 gpm unit will only be treating a portion of the KCP wastewater effluent for
demonstration purposes.
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2.2 Commercial Status
The HERO™ system was introduced to the market in 1996 by Deb Mukhopadhyay. The
target market was providing ultra-pure water to the microelectronics industry. Several
units in this application have been operating at electronics manufacturing facilities such
as Intel and Micron.
In 1998, Hydrometrics licensed the process and began providing the technology for
industrial wastewater applications. The HERO™ process was patented in 1999.
Approximately ten wastewater applications have been tested using the HERO™ process.
Wastewaters tested came from the following industries: mining and smelting, petroleum
refining, water produced from oil and gas drilling, natural gas power generation, and
metal finishing. Within the metal finishing industry, a range of potential applications are
possible for addressing plating baths, etching baths, or rinse waters from metal finishing
operations, circuit board manufacturing, and related processes. The HERO™ system is
reportedly especially suited for applications where large quantities of fresh water are
required, fresh water is in short supply, or environmental requirements are stringent. The
HERO™ system is also reportedly beneficial for applications where traditional RO
systems have failed or are too costly to operate. There are approximately a dozen
HERO™ systems of various flow capacities in operation in the U.S., Asia, Europe, and
South America.
2.3 Pollution Prevention Classification
Hydrometrics' HERO™ system is a wastewater treatment technology that falls under the
water use reduction/recycle focus area. Tested industrial wastewaters have exhibited
efficient separation of individual metals for recovery and recycle (near 100 percent), and
very high product water recovery (up to 95 percent, compared to 75 percent for
traditional RO). This results in minimized fresh water consumption and the elimination
or reduction of wastewater discharge. The unit also minimizes energy consumption in
relation to traditional RO systems. The HERO™ system waste stream is five times more
concentrated than traditional RO waste, reducing the required evaporation time
associated with mechanical dryers, and thereby reducing energy consumption for zero-
liquid discharge applications status.
Due to the rising costs of chemicals, energy, and treatment/disposal fees, and increasingly
more stringent environmental requirements, wastewater reduction/reuse has become a
greater priority to metal finishing companies, and the methods and technologies they
employ have increased in sophistication. Today, firms are willing to expend significant
amounts of capital and operating funds for equipment and methods that primarily reduce
the disposal frequency and amount of their process wastewaters. By recovering water
and valuable metals for reuse/resale, the HERO™ process makes large steps toward
achieving these goals.
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2.4 Environmental Significance
Wastewaters containing up to 30,000 parts per million (ppm) TDS and heavy metals have
been treated by the HERO™ process to meet drinking water standards. Purified water
from the HERO™ system is normally suitable for reuse or direct discharge, meeting
existing wastewater discharge compliance limits. With reuse, facilities can make
significant strides toward zero-liquid discharge, water conservation, and reduced
environmental liability.
The high recovery, concentration, and possible reuse/recycle of heavy metals from the
HERO™ process results in a reduction of metals emissions to the environment, a high
priority in the Metal Finishing Industry's Strategic Goals Program regarding toxic metals
reduction/utilization, and is consistent with the recommendations of the National Metal
Finishing R&D Plan.
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Wastewater from Pretreatment
1
HP1 h,
(Regenerating Solution)
Air ^
STEP #1: WEAK ACIE
EXCHANGE (HAR1
Ca "1 f(HC03)2 Ca
Mg ^ SO4 + H2Z = M|
Na2J [d2 Na
Cal
During Regeneration: Mg >Z
Na2J
Her) ^
i
> CATION (WAC) ION
MESS REMOVAL)
"1 f"2CO2
5 \- Z + 2H2O + ^ H2SO4
2J [_2HC1
pH « 4.5
r
STEP #2: MEMBRANE DEGASIFICATION
(ALKALINITY REMOVAL)
H2C03 *
MiOTT ^
]
Hr> i
pH « 4.5
r
STEP #3: HIGH PH REVERSE OSMOSIS
(CONTAMINANT REMOVAL)
pH « 10.0
H20
Cal
Na2J 1
To Pretreatment
Clarifier ^-ToPOT^
(if available)
OR
^ CO-
1
Atmosphere
y
O&G, SS, Metals, Biologicals & Other
Organics
^ (Waste Brine Solution)
1
To POTW
+
Recycled Water (RO Permeate)
To Process or POTW
Figure 2: HERO™ System Chemical Reactions
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3.0 PROCESS DESCRIPTION
3.1 Equipment and Flow Diagram
The technology utilizes proven and available "off-the-shelf equipment components. The
equipment is compact (about 8' x 20' depending on flow and application), skid mounted,
and modular for simple expansion. Electrical service of 480 volt, 50 amp, 3-phase, 60 Hz
is required. Operations are automated and simple, reportedly resulting in low operation
and maintenance costs. The unit usually operates in a continuous mode, although it also
has the capability to operate in a batch mode. Existing RO systems can be easily
retrofitted to operate in the HERO™ configuration.
In the HERO™ process, weak acid cation (WAC) ion exchange is used to remove sodium
and hardness associated with alkalinity. Other cations (such as copper, barium, iron,
manganese and zinc) are also removed. Treated water is slightly acidic. The bicarbonate
alkalinity in the water is converted to carbon dioxide. Additional acid may be added to
convert the remaining alkalinity to carbon dioxide. After degasification in the next step,
the TDS is reduced according to Hydrometrics. The WAC is regenerated periodically
using sulfuric or hydrochloric acid. The concentrated waste brine solution is mixed with
the RO reject stream for disposal. Alternatively, Hydrometrics says the brine solution
could be recirculated to a clarifier, if one is used as pretreatment to the HERO™ system
for further precipitation of any remaining contaminants.
After WAC ion exchange treatment, the water is passed through a counter-current air
stripper (membrane degasifier) to remove the carbon dioxide created in the WAC ion
exchange process. This step removes the buffering capacity of the water, thereby
minimizing caustic addition in the next step. In the high pH RO step, a small amount of
caustic is used to increase the pH prior to treatment. Operating at high pH has several
important advantages:
• Fats and oils are emulsified. These materials are kept in solution and rejected rather
than plating out on the membrane surface.
• Silt fouling is eliminated. Membranes used in normal RO systems become fouled
with silt, biological growth and organic matter. When this occurs, the membranes are
cleaned with softened water at pH 10. HERO™ systems operate continuously with
softened feed water at pH 10. Silt and organic matter are continuously cleaned from
the membrane surface and biological growth is eliminated.
• Silica solubility is increased. Increased silica solubility at high pH prevents silica
scaling on the membrane. Silica can often be a limiting factor controlling the
recovery limit of an RO system.
• Weak organic acids are ionized. Low concentrations of these acids can foul
membranes unless they are ionized. Once ionized at high pH, the membranes reject
these acids.
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Industrial wastewater quality is inherently site-specific. Accordingly, wastewater
treatment systems are generally designed for specific applications. For example, feed
water with elevated hardness, total hardness in excess of total alkalinity, high TSS, or
high oil and grease may require additional pretreatment prior to the HERO™ system.
This pretreatment may include filters, strong acid cation (SAC) ion exchange, or
clarifiers. For reasons like this, HERO™ systems are designed to address the specific
wastewater quality characteristics of the host facility.
Figure 3 shows a photograph of a full-scale, 90 gpm, permanently installed HERO™
system.
Figure 3: HERO™ Wastewater Treatment System
3.2 Test Site
The host site selected for testing is Honeywell FM&T's KCP in Kansas City, Missouri.
Honeywell FM&T, a prime contractor for the DOE, manages and operates the
approximately one million square foot KCP. Honeywell FM&T is a division of
Honeywell, headquartered in Morristown, New Jersey. Honeywell and its divisions
produce many high-tech products for consumer and government use. Virtually every
form of air transportation depends on at least one of Honeywell's systems, including
every manned space flight since the beginning of the U.S. space program.
The KCP is a state-of-the-art facility that manufactures a wide array of mechanical,
electrical, and engineered material components for the DOE. The KCP was established
in 1949.
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The KCP manufactures electronic, mechanical, and engineered material components for
national defense systems. Within the engineered material components operations they
have capabilities for applying and evaluating low and zero volatile organic carbon (VOC)
paints, dry film lubricants, and powder coatings. Plasma, electrophoresis, and chemical
surface pretreatments are also available. Electroplated coating applications include
copper, tin, tin-lead, zinc, cadmium, nickel, electroless nickel, hard and soft gold,
rhodium, and black and brown oxides. They electroform copper, nickel, and gold. On
difficult-to-plate substrates, a combination of vacuum deposition and electroplating is
used to achieve adherent coatings.
The microelectronics manufacturing division of the facility consists of 19,000 square feet
(ft2) of clean-rooms, 1,800 ft2 of laser rooms, and 26,000 ft2 of manufacturing and
support area.
Capabilities include Thin Film Networks, Thick Film Networks, and Low Temperature
Co-fired Ceramic Networks. Several film materials including titanium, palladium,
palladium-gold, platinum-gold, gold, silver, copper, and chromium are applied to a
variety of substrate materials using processes such as electroplating, sputtering and
physical vapor deposition (PVD).
Figure 4 shows a detailed schematic of the HERO™ industrial wastewater treatment
application complete with sampling points.
3.3 KCP Conventional Wastewater Treatment System
3.3.1 Copper Recovery & Cyanide Oxidation
Copper will be recovered from the plating shop cyanide rinse water waste stream
by employing a separate WAC ion exchange unit supplied by Hydrometrics, Inc.
Copper/cyanide bearing rinse waters are formed when drag-out or drippage from
cyanide plating baths contaminate rinse baths during normal copper plating
operations. This separate unit will remove copper that is complexed with cyanide.
Normally, metals recovery with the HERO™ process is achieved in the WAC ion
exchange unit that is integral to the three-step treatment process. However, since
cyanide oxidation results in copper precipitation, copper removal is more efficient
prior to the cyanide oxidation process. A full-scale separate WAC ion exchange
unit would be regenerated with sulfuric acid; however, no regeneration will be
necessary during the verification test. The quantity of recovered copper will be
calculated by doing a mass balance for copper on the influent and effluent of the
WAC unit. The treated water will then go through the normal cyanide oxidation
process. This is necessary to prevent health and safety issues associated with the
release of cyanide gas later in the treatment system.
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SP-A = HERO™ Influent
SP-B = HERO™ Effluent
SP-C = WAC Waste Solution
SP-D = RO Waste Solution
SP-E = Metals Recovery Influent
SP-F = Metals Recovery Effluent
= Plating Process Wash Waters
Q = Existing KCP Water Treatment System
| = HERO™ Pretreatment Steps For KCP Water
fj = Standard HERO™ Wastewater Treatment System
(R) = Regeneration Solution
Figure 4: HERO™ Wastewater Treatment System Diagram - Detailed
3.3.2 Chromium Reduction
A conventional step of the KCP wastewater treatment process is the reduction of
chromium in the chromium plating rinse waters. The chromium plating rinse
waters are treated with metabisulfite (MBS) in order to reduce chromium in the
hexavalent state to the more stable and less toxic trivalent chromium state. The
effluent from this step moves directly to the next step, precipitation/clarification.
3.3.3 Lime Precipitation & Clarification
Spent rinse water from the cyanide oxidation, chromium reduction, acid and
caustic rinse water, and other finishing rinse water (aqueous degreasing, cleaning
and rinsing) are then commingled in 3,750 gal flash mix tanks, where they are
treated with a sodium hydroxide/lime slurry and mechanically mixed. They are
pumped at a rate of approximately 170 gpm into the conventional wastewater
treatment system. Up to 80,000 gal of combined wastewater per day are treated in
this conventional lime precipitation/clarification unit during the single 10-hour
operating shift. This system removes metals and O&G, and provides a consistent
water quality feed to the remainder of the treatment system.
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The concentrated reject from the clarifier will continue to be pressed, dried, and
sent for disposal as an F006 waste.
3.4 Hydrometrics Mobile HERO™ Unit Installation at KCP
3.4.1 Pretreatment
3.4.1.1 Prefiltration & SAC Ion Exchange Treatment
The HERO™ system will be installed online and operated continuously.
Wastewater from the prefilter is pumped through the HERO™ system at a
flow rate of about 15 gpm. In addition to the normal three-step HERO™
process, prefiltration of the post-clarified feed water to remove residual
suspended solids and a SAC ion exchange process will be used for
verification testing due to the high hardness-to-alkalinity ratio. (SAC ion
exchange treatment will not be required for full-scale treatment if pre-
softened water is used. A standard water softener would be used to treat
all make-up water and eliminate hardness from the process water circuit.)
SAC ion exchange treated water is then sent to the first step in the
standard HERO™ process, the WAC ion exchange unit.
3.4.2 HERO™ System
3.4.2.1 WAC Ion Exchange Treatment
Wastewater from the SAC ion exchange flows into the WAC ion
exchange step of the HERO™ process to remove all remaining hardness.
Because the WAC resin is in acid form, this step also lowers the pH of the
water to 4.5, and converts carbonate and bicarbonate to carbon dioxide.
This unit is regenerated using a dilute solution of hydrochloric acid.
3.4.2.2 Membrane Degasification
From the WAC ion exchange outlet, the wastewater goes through
degasification to remove carbon dioxide. This inexpensive step removes
the buffering capacity of the water, minimizing pH adjustment costs. Acid
addition prior to the degasifiers may be necessary to lower the pH to 4.5
for complete carbon dioxide conversion.
3.4.2.3 pH Adjustment and Reverse Osmosis (RO)
The final step in the HERO™ system is adjustment to pH 10 and RO
treatment. Operating the RO at high pH avoids bio-fouling and silica
scaling, and enhances silt rejection. Treated wastewater is returned to the
rinse water make-up system at a flow of about 15 gpm. Dissolved solids
are discharged to the sewer.
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The 15 gpm unit installed at the KCP for verification will process about
7,200 gallons per day (gpd) (based on 8 hrs/day operation). If selected for
permanent installation, a 100-200 gpm HERO™ system would be
scheduled to be installed in late 2001/early 2002 and will treat all of the
KCP process wastewater, with a capacity of 48,000-96,000 gpd (based on
8 hrs/day operation). The concentrated brine solution that is generated
during the ion exchange step will be recirculated back to the conventional
wastewater treatment system where any remaining metal cations will settle
out in the clarifier. The waste brine solution from the reverse osmosis step
of the HERO™ process will be directly discharged to the sewer in the
permanent installation configuration. Zero liquid discharge is not being
pursued at the Honeywell facility. With the 15 gpm unit, Hydrometrics
estimates that about 5 percent or 360 gpd of waste brine solution will be
generated by the HERO™ process (also based on 8 hrs/day operation). If
selected for permanent installation at the KCP, the full-scale, 100-200
gpm HERO™ system waste brine generation will increase to about 4,000
gpd (based on 5 percent of 80,000 gpd - KCP's current treatment flow).
This wastewater discharge volume sounds like a large quantity, but would
be a 95 percent reduction in wastewater discharges to the POTW from
their current 80,000 gpd.
Pictures of a 15 gpm, mobile HERO™ system like the one that will be
installed at the KCP for the verification test are provided for reference in
Figure 5
Figure 5: KCP's Mobile HERO™ System
4.0 EXPERIMENTAL DESIGN
4.1 Test Goals and Objectives
The overall goal of this project is to establish the technical and economic performance
parameters that will enable a potential user to determine if the Hydrometrics HERO™
wastewater treatment system is appropriate and feasible under their specific operating
conditions. The objective of testing is to generate the analytical data and performance
observations required in supporting these technology verification efforts.
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The following are statements of specific project objectives:
• Evaluate, document, and verify the performance of the separate HERO™ wastewater
WAC ion exchange treatment technology for the recovery of copper that builds up in
the process rinse water during the cyanide-containing finishing operations.
Characterize the recovered copper for salability options.
• Evaluate, document, and verify the HERO™ wastewater treatment technology's
removal efficiency for IDS, O&G (as HEM), Ag, Al, As, Ba, Ca, Cd, Cl, CN, Cr, Cu,
Fe, Hg, Mg, Mn, Mo, Na, Ni, Pb, Sn, Zn, total residual chlorine, sulfate, nitrate,
sulfides, chloride, fluoride, dissolved silica, total alkalinity, TOC, and TSS that
accumulate in process rinse waters during finishing operations.
• Quantify the energy required to operate the system. Primary energy users include the
electrical service to the automated system, instrument readouts, and the liquid feed
pumps. This information will be used to estimate operating costs for the HERO™
wastewater treatment system.
• Quantify environmental benefit by determining the reduction in wastewater disposal
quantities versus HERO™ waste sludge quantities/characteristics.
4.2 Critical and Non-Critical Measurements
Measurements that will be taken during testing are classified below as either critical or
non-critical. Critical measurements are those that are necessary to achieve project
objectives. Non-critical measurements are those related to process control or general
background readings.
Operational data will be collected on the HERO™ wastewater treatment system
performance during the treatment of process wastewater. The following operational data
will be collected:
Critical Measurements
• Concentrations of TDS, O&G (as hexane extractable material (HEM)), Ag, Al, As,
Ba, Ca, Cd, CN, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Na, Ni, Pb, Sn, Zn, total residual
chlorine, sulfate, nitrate, sulfides, chloride, fluoride, dissolved silica, TOC, total
alkalinity, and TSS in the HERO™ system influent and effluent
• Specific conductivity and total alkalinity of rinse water influent/effluent
• Rinse water processing rate and total volume
• Waste volumes, characteristics (TDS, O&G (as HEM), Ag, Al, As, Ba, Ca, Cd, CN,
Cr, Cu, Fe, Hg, Mg, Mn, Mo, Na, Ni, Pb, Sn, Zn, total residual chlorine, sulfate,
nitrate, sulfides, chloride, fluoride, dissolved silica, total alkalinity, TOC, and TSS),
and disposal costs
• Concentrations and volumes of copper in cyanide rinse water, WAC process influent
and effluent
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Non-Critical Measurements
• Membrane flux/fouling
• Membrane vessel pressure
• pH of rinse water influent/effluent and waste products
• Temperature of rinse water influent/effluent and waste products
• Operating and Maintenance (O&M) labor requirements
• Reagent (lime, sulfuric acid and caustic) use rates
This data will be used to determine the system material balance, wastewater purification
rate, O&M requirements, and the cost-effectiveness for a given set of operating
conditions.
Historical Data
Historical data on the KCP's wastewater disposal quantities prior to installation of the
HERO™ wastewater treatment system will be collected and provided in the verification
report to determine the environmental benefit.
The KCP's records regarding plating rinse water quality measurements will also be
reviewed and summarized in the verification report in order to alleviate plating quality
concerns regarding the implementation of the HERO™ wastewater treatment system.
4.3 Test Matrix
The unit will be evaluated on its ability to efficiently treat and recover metal finishing
process wastewater. The specific tests planned are described in Table 1. In order to gain
the valuable system performance information desired for the ETV-MF Program,
sampling, testing, and documentation will take place over a four-day period.
4.3.1 HERO™ System Wastewater Recovery - Test #1
A large portion (46 percent) of the combined KCP wastewater is dilute, non-
production wastewater. This non-production wastewater consists of non-contact
cooling water, boiler blow-down water, laboratory sink water, etc. The remaining
54 percent of the KCP's spent process water consist of non-metal-finishing
industrial process wastewaters, and rinse waters from metal finishing. The
HERO™ system will be evaluated on its ability to separate chemical contaminants
from the wastewater and recycle the water back to the metal finishing process
rinse tanks.
4.3.2 WAC Ion Exchange Unit Copper Recovery - Test #2
A very small amount or KCP's wastewater, about 330 gpd, is cyanide-bearing
rinse water from the KCP metal finishing shop's copper plating operations.
Copper is a potential recyclable/salable metal, and this verification test will
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include a separate WAC ion exchange unit installed between the cyanide rinse
water storage tank and the first step of the cyanide oxidation process. This WAC
unit uses resin identical to the WAC unit within the HERO™ system where
metals recovery would normally take place, but on a smaller scale. Due to KCP's
conventional wastewater treatment system, a separate WAC unit must be installed
upstream of that system in order to recover the copper. Because of the small
amount of cyanide-bearing rinse water generated at KCP, copper recovery will
not be economically feasible at KCP. The verification on this WAC unit will
demonstrate the HERO™ system's ability to remove valuable metals for recovery,
recycle and/or sale.
4.3.3 HERO Effluent Water Recycling
The rinse water used in KCP metal finishing operations is standard Kansas City
tap water. Recycled water from the HERO™ system must meet the minimum
quality standards equal to this tap water. A sample of KCP's tap water was
analyzed before the verification test for TDS, O&G (as HEM), Ag, Al, As, Ba,
Ca, Cd, Cl, CN, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Na, Ni, Pb, Sn, Zn, total residual
chlorine, sulfate, nitrate, chloride, sulfides, fluoride, dissolved silica, total
alkalinity, TOC, and TSS and will be compared to recycled water from the
HERO™ treatment system in the verification report.
4.3.4 RO Waste Solution
According to Hydrometrics, the single waste stream produced in the process is
generally less than 10 percent of the feed stream. This concentrated waste brine
solution is generated from the ion exchange and reverse osmosis steps of the
HERO™ treatment system, and Hydrometrics claims it is generally suitable for
direct discharge to a POTW. This waste consists primarily of sodium sulfate, but
may also contain heavy metals, suspended solids, O&G, biological materials, and
other organic materials that have been removed from the wastewater. The KCP's
waste brine solution has been tested in a bench-top test, and it meets all current
KCP wastewater discharge limits. The KCP must sample and test their
wastewater every six months, according to their sewer discharge permit; however,
they typically sample and test every other month. The RO waste solution will be
evaluated to ensure it meets KCP's discharge limits.
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Test
1. HERO™ System
Wastewater
Recovery
2. WACIon
Exchange Unit
Copper Recovery
Test Objectives
Prepare a material balance for wastewater constituents.
Evaluate the ability of the HERO™ system to process
wastewater and separate chemical contaminants from water.
Determine the wastewater recovery rate of the system,
normalized based on production throughput of wastewater.
Determine the labor requirements needed to operate and
maintain the HERO™ system.
Determine the quantity of energy consumed by the
HERO™ system during operation.
Determine the cost of operating the wastewater recycle
system for the specific conditions encountered during the
testing.
Quantify /identify the environmental benefit.
Prepare a material balance for copper recovered from the
cyanide-bearing rinse waster.
Evaluate the ability of the WAC ion exchange unit to
process wastewater and separate copper contaminants from
water.
Determine the copper recovery rate of the system,
normalized based on production throughput of wastewater.
Determine the labor requirements needed to operate and
maintain the WAC ion exchange unit.
Determine the cost of operating the WAC ion exchange unit
for the specific conditions encountered during the testing.
Quantify /identify the environmental benefit.
Test Measurement
• Chemical characteristics of influent.
• Chemical characteristics of effluent.
• Volume and chemical characteristics of the RO waste solution.
• Quantity of treatment chemicals used during testing.
• Chemical characteristics of influent.
• Chemical characteristics of effluent.
• Volume of water recovered.
• Production throughput of wastewater.
• O&M labor requirements during test period.
• Quantity of energy used by pumps and motors.
• Costs of O&M labor, materials, and energy required during test period.
• Quantity and price of treatment chemicals used during testing.
• Review of historical waste disposal records and compare to verification
test practices.
• Chemical characteristics (Cu) of influent.
• Chemical characteristics (Cu) of effluent.
• Volume and chemical characteristics of copper removed from
wastewater.
• Quantity of treatment chemicals used to recover the copper.
the
• Chemical characteristics (Cu) of influent.
• Chemical characteristics (Cu) of effluent.
• Volume of copper recovered.
• Production throughput of wastewater.
• O&M labor requirements during test period.
• Costs of O&M labor and materials required during the test period.
• Quantity and price of chemicals used during copper recovery.
• Review of historical waste disposal records and comparison
verification test practices.
to
Table 1: Objectives and Related Test Measurements for Evaluation of the HERO™ System
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4.4 Operating Procedures
The 15 gpm, trailer-mounted HERO™ system will be parked on a concrete pad adjacent to the
building housing the existing lime precipitation clarifier wastewater treatment system. A blind
sump surrounds the concrete pad, as this is a designated chemical loading/unloading area,
complete with secondary containment. The separate copper recovery ion exchange unit will be
installed within the KCP wastewater treatment plant, inside the secondary containment wall, next
to the cyanide rinse water holding tank. Treated water from KCP's conventional wastewater
treatment plant will be piped to the HERO™ system. The HERO™ system will polish pre-
treated water from an estimated 80,000 gpd combined flow of non-production wastewater, non-
metal finishing process wastewater, acid/caustic rinse water, and metal finishing rinse waters.
Hydrometrics and KCP personnel will perform normal operation and maintenance activities
during testing. These activities will be observed and noted by the ETV-MF Project Manager.
The HERO™ system will be operated six to eight hrs/day. The exact number of operating hours
will depend on the KCP work-load schedule. The verification test period will be four workdays.
4.5 Sampling, Process Measurements, and Analytical Methods
4.5.1 Sampling Responsibilities & Procedures
By using a dual wastewater holding tank system at the facility, it is anticipated that
contaminant concentration should remain relatively stable over each day of testing. The
incoming wastewater is stored in large holding tanks where it is isolated at the start of
each day from incoming wastewater, and agitated with mixing pumps. The stream is then
fed into the traditional wastewater treatment plant and on into the HERO unit at a
uniform rate.
Grab samples will be taken from the sampling ports associated with the corresponding
sampling points specified in Figure 4. Sampling will occur in the quantities listed in
Table 2, and the frequency listed in Table 3 for each parameter. The KCP waste
treatment operators will use their dual-waste holding tank system to isolate, collect, mix
and provide consistent wastewater flows for the duration of the four day verification test.
The appropriate sampling container will be used as outlined in Table 4 for each test
parameter. Each sample bottle will be labeled with the date, time, sample identification
(ID) number, and test parameters required. Sampling will take place at least one hour
after any system shut-down/start-up operations. Sample preparation methods are
described in each individual analytical method.
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TSS
TDS
TOC
O&G
(as HEM)
Metals
Sulfide
Total Cyanide
Chloride
Sulfate
Nitrate, as N
Fluoride
Total
Alkalinity
Dissolved Silica
SP-A
HERO™ Unit
5axlL
5axlL
10cx500mL
12exlL
5axlL
5ax500mL
5ax500mL
5axlL
5axlL
5axlL
5axlL
5axlL
5ax500mL
SP-B
HERO™ Unit
5axlL
5axlL
10cx500mL
12exlL
5axlL
5ax500mL
5ax500mL
5axlL
5axlL
5axlL
5axlL
5axlL
5ax500mL
SP-C
HERO™ Unit
5axlL
5axlL
10cx500mL
12exlL
5axlL
5ax500mL
5ax500mL
5axlL
5axlL
5axlL
5axlL
5axlL
5ax500mL
SP-D
HERO™ Unit
5axlL
5axlL
10cx500mL
12exlL
5axlL
5ax500mL
5ax500mL
5axlL
5axlL
5axlL
5axlL
5axlL
5ax500mL
SP-E
2nd WAC Unit
-
-
-
-
5axlL
(Cu only)
-
-
-
-
-
-
-
-
SP-F
2nd WAC Unit
-
-
-
-
5axlL
(Cu only)
-
-
-
-
-
-
-
-
Field Blank -
Lab DI Water
lbxlL
lbx!L
2d x 500 mL
2dxlL
lbxlL
lbx500mL
lbx500mL
lbxlL
lbxlL
lbxlL
lbxlL
lbxlL
lbx500mL
Notes:
a Sample quantities of 5 include 1 grab sample on 4 successive days, and 1 duplicate.
b Sample quantities of 1 include 1 grab sample (laboratory DI water).
0 Sample quantities of 10 include 1 grab and 1 archive sample on 4 successive days, 1 duplicate and 1 duplicate archive.
d Sample quantities of 2 include 1 sample and 1 archive (laboratory DI water).
e Sample quantities of 12 include 1 grab and 1 archive sample on 4 successive days, 1 duplicate, 1 duplicate archive, 1 MS
and 1 MSD.
One duplicate sample will be collected from each sample location during the verification test period.
Matrix spike (MS) and matrix spike duplicate (MSD) analysis will be performed on each duplicate sample for all applicable
parameters.
The duplicate, MS and MSD samples must be collected on the same day at approximately the same time.
The archive samples will not be analyzed unless necessary; they will be identified as "Archive" and transported in a shipping
container separate from the other samples.
Table 2: Sample Quantities
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SAMPLE
LOCATION
SP-A
HERO™ Influent
SP-B
HERO™ Effluent
SP-C
WAC Waste
Solution
SP-D
RO Waste Solution
SP-E
Metals Recovery
Influent
SP-F
Metals Recovery
Effluent
# OF SAMPLES
5
(4 + one duplicate)
5
(4 + one duplicate)
5
(4 + one duplicate)
5
(4 + one duplicate)
5
(4 + one duplicate)
5
(4 + one duplicate)
FIELD
BLANK
1
1
FREQUENCY
1 grab
sample/day
1 grab
sample/day
1 grab
sample/day
1 grab
sample/day
1 grab
sample/day
1 grab
sample/day
TEST
DURATION
4 days
4 days
4 days
4 days
4 days
4 days
PARAMETERS
TSS, IDS, TOC,
O&G (as HEM),
Specific
Conductivity,
Total Alkalinity,
Ag, Al, As, Ba,
Ca, Cd, Cl, Cr,
Cu, Fe, Hg, Mg,
Mn, Mo, Na, Ni,
Pb, Sn, Zn, Total
Residual
Chlorine, Sulfate,
Sulfide, Nitrate,
Fluoride, CN,
Dissolved Silica,
Temp., pH, Flow
Rate
Same as SP-A
Same as SP-A
Same as SP-A
Copper, Temp.,
pH, Flow rate
Same as SP-E
Table 3: Test Matrix
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ANALYTE
TSS
IDS
TOC
O&G (as HEM)
Metals
(except Hg)
Hg
Sulfide
Total Cyanide
Chloride
Sulfate
Nitrate, as N
Fluoride
Total Alkalinity
Dissolved Silica l
METHOD
EPA 160.2
EPA 160.1
SW-846
9060
EPA 1664
EPA 200.7
EPA 245.1
EPA 376.1
EPA 335.3
EPA 300.0
EPA 300.0
EPA 300.0
EPA 300.0
EPA 3 10.1
EPA 370.1
SAMPLE BOTTLE
1 L (HOPE)
1L HOPE
500 mL amber glass
1 L amber glass
1LHDPE
1LHDPE
500 mL HOPE
500 mL HOPE
1 L HOPE
1 L HOPE
1 L HOPE
1 L HOPE
1 L HOPE
500 mL HOPE
PRESERVATION
Cool to 4°C
Cool to 4°C
H2SO4 to pH < 2
& cool to 4°C
H2SO4 to pH < 2
& cool to 4°C
HNOa to pH < 2
& cool to 4°C
HNOa to pH < 2
& cool to 4°C
NaOH to pH>9/Zn
Ac, & cool to 4°C
NaOHtopH> 12
& cool to 4°C
None
Cool to 4°C
Cool to 4°C
None
Cool to 4°C
Cool to 4°C
HOLD TIME
7 days
7 days
28 days
28 days
6 months
28 days
7 days
14 days
28 days
28 days
48 hours
28 days
14 days
28 days
Table 4: Aqueous Samples
Samples to be analyzed at the off-site laboratory will be accompanied by a chain-of-
custody (COC) form. The samples will be stored and transported in appropriate sample
transport containers (e.g., coolers with packing and blue ice) by common carrier. The
transport containers will be secured with tape seals to ensure sample integrity during the
delivery process to the analytical laboratories. The ETV-MF Project Manager will
perform sampling and labeling, and ensure that samples are properly stored and secured
for transport to the analytical laboratory. Pace Analytical Services Inc. will perform all
aqueous analytical transportation and the testing of all samples.
1 Digestion is not required, due to lack of molybdate unreactive silica. Filtration shall be prepared by the laboratory
immediately upon receipt
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4.5.2 Process Measurements
Monitoring during the verification test period will be accomplished by recording key
operating data. Monitoring instrumentation will be calibrated and used by the ETV-MF
Project Manager according to manufacturer recommendations. See section 4.5.4 for
specific calibration procedures. Process measurements will be recorded on the test data
collection form (Figure 6) at the same time that aqueous sampling occurs, that is to say,
once a day, in accordance with Table 3. On-site measurements will be performed three
times for each sampling activity in order to determine compliance with the QA objectives
stated in Table 5.
Wastewater flow rates for this verification test will be measured by an Omega
Engineering, Inc., Model FD-7000 multi-liquid ultrasonic flowmeter with non-
penetrating transducers. Wastewater pH and temperature will be measured on-site with a
Davis Instruments Model #9214 microprocessor controlled, automatic temperature
compensated pH meter with built-in temperature sensor. See Table 5 for equipment
performance details. Wastewater specific conductivity will be measured with an Oakton
Acorn® Series CON 5 microprocessor controlled, automatic temperature compensated
conductivity meter with built-in temperature sensor. See Table 5 for equipment
performance details. Total residual chlorine will be measured on-site immediately after
sampling with a Hach® Pocket Colorimeter™ filter photometer with total chlorine reagent
set. See Table 5 for equipment performance details.
Membrane flux is the decrease in permeate flow rate due to membrane performance
deterioration, caused by the membrane becoming fouled with contaminants. Flux will be
calculated as the gallons of permeate product per square foot of membrane per day (gfd).
Increasing the flux results in lower capital costs and better effluent quality. In
conventional RO systems, membranes foul with scale (divalent metal precipitates),
organics (oil and hydrocarbons), and microbial growth. The HERO™ process reportedly
eliminates this by removing the divalent metal ions and then operating the RO at a high
pH where organics are emulsified and biological growth does not occur. Hydrometrics
claims the HERO™ system achieves an operating flux that is up to two times that of
traditional RO. RO reject flowrate will be collected, then membrane flux will be
calculated upon completion of the verification test.
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Test Data Collection Form
DATE:
Revision 0-6/15/01
OPERATION: HERO™ Wastewater Treatment System
SAMPLE DATA
Date
Time
Sample
Location
Initials
INFLUENT (FEED) WATER
PARAMETERS
Temp.
(°C)
pH
Flow
Rate
(gpm)
SC
(US)
Total
C12
(mg/L)
RO REJECT / WAC WASTE
PARAMETERS
Temp.
(°O
pH
Flow
Rate
(gpm)
Total
Volume
(gal)
EFFLUENT (PERMEATE) WATER
PARAMETERS
Temp
(°O
pH
Flow
Rate
(gpm)
SC
(US)
Total
C12
(mg/L)
Figure 6: Test Data Collection Form
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Measurement
TOC
O&G (as HEM)
Metals (- Hg)
Hg
Sulfide
Total Cyanide
Chloride
Sulfate
Nitrate
Fluoride
Total Alkalinity
Dissolved Silica
TSS
TDS
Total Residual C12
Flow Rate
Temperature
pH
Specific Cond.
Membrane Flux
Matrix
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Aqueous
Method
EPA 9060
EPA 1664
EPA 200.7
EPA 245.1
EPA 376.1
EPA 335.3
EPA 300.0
EPA 300.0
EPA 300.0
EPA 300.0
EPA 3 10.1
EPA 370.1
EPA 160.2
EPA 160.1
EPA 330.5
EPA 3. 1.9
EPA 170.1
EPA 150.1
EPA 9050A
-
Units
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
L/hr
°C
pH
M-S/cm
gfd
Method of
Determination
Combustion / Oxidation
Gravimetric
ICP-AES
Manual Cold Vapor
Titrimetric, Iodine
Colorimetric, Automated UV
Ion Chromatography
Ion Chromatography
Ion Chromatography
Ion Chromatography
Colorimetric (Methyl Orange)
Colorimetric
Gravimetric
Gravimetric
DPD-Colorimetric
Ultrasonic Flowmeter
Thermometric
Electrometric
Wheatstone Bridge-Type
Calculated
MRL
10.0
5.68
0.004-1.0
0.0002
0.5
0.005
1.0
1.0
1.0
0.2
1.0
1.0
5.0
5.0
0.01
0.3-3.6
0.1
0.01
1.0
N/A
Precision
(RPD)
<30
<30
<30
<30
<30
<30
<30
<30
<30
<30
<30
<30
<30
<30
<2
<1
< 1
<0.2
<2
N/A
Accuracy
(% Recovery)
70-130
70-130
70-130
70-130
70-130
70-130
70-130
70-130
70-130
70-130
70-130
70-130
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
Completeness
90
90
90
90
90
90
90
90
90
90
90
90
90
90
90
90
90
90
90
N/A
EPA/821/C-99/004:
EPA SW-846:
N/A - Not applicable
EPA Methods and Guidance for Analysis of Water
EPA Test Methods for Evaluating Solid Waste
Table 5: QA Objectives for Precision, Accuracy, and Detection Limits
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4.5.3 Testing Parameters
4.5.3.1 Flow Rate
Liquid transfer pumps deliver process water to various parts of the
HERO™ system during the purification process. The rate at which these
liquids are transferred is of major importance in the HERO™ system.
Liquid flow rates will be determined at all liquid sampling points (SP-A
through SP-F) with an Omega Engineering, Inc., Model FD-7000 multi-
liquid ultrasonic flowmeter with non-penetrating transducers. (EPA
Method 3.1.9 and equipment manufacturer's instructions)
4.5.3.2 Temperature
While temperature is not a critical parameter in the HERO™ process, it
will be monitored at all liquid sampling points (SP-A through SP-F) in
order to determine the temperature range of the wastewaters being treated
as they enter and exit the HERO™ process during the verification test
(EPA Method 170.1 and equipment manufacturer's instructions).
Temperature will be measured with a Davis Instruments Model #9214
microprocessor controlled, automatic temperature compensated pH meter
with built-in temperature sensor. Wastewater entering the HERO™
system is not temperature controlled, and is typically ambient temperature.
4.5.3.3 pH
pH of the wastewater is a critical parameter in the HERO™ process. The
wastewater is acidified before the degasification step, and the pH is
increased before the reverse osmosis step. The pH of the wastewater will
be monitored at all liquid sampling points (SP-A through SP-F) in order to
determine the pH range of the wastewaters being treated as they enter and
exit the HERO™ process during the verification test (EPA Method 150.1
and equipment manufacturer's instructions). pH will be measured with a
Davis Instruments Model #9214 microprocessor controlled, automatic
temperature compensated pH meter with built-in temperature sensor.
4.5.3.4 Specific Conductivity
Conductivity is the measurement of a material's ability to conduct electric
current. The ability to transmit an electrical current depends on the
concentration of charged or ionic species in the material. Hence, the
measure of the conductance is used to approximate the total concentration
of ionic species present. This measurement is an estimator of water
contamination. Specific conductivity will be measured at the HERO™
system influent and effluent (SP-A & SP-B), and waste products (SP-C &
SP-D). (EPA Method 9050A and equipment manufacturer's instructions).
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Specific conductivity will be measured with an Oakton Acorn® Series
CON 5 microprocessor controlled, automatic temperature compensated
conductivity meter with built-in temperature sensor.
4.5.3.5 Total Suspended Solids (TSS)
TSS are non-filterable particles of solids dispersed but undissolved in the
wastewater, which cloud the water's appearance and impair the efficiency
of the rinse waters. It is important to remove these contaminants in order
to meet regulatory requirements and give the recovered wastewater a clean
and clear appearance. Samples will be collected at the HERO™ system
influent, effluent, and waste streams (SP-A through SP-D) and analyzed
for TSS according to EPA Method 160.2.
4.5.3.6 Total Dissolved Solids (TDS)
TDS are the total of disintegrated organic and inorganic materials
contained in the wastewater. TDS also impair the efficiency of the rinse
waters; therefore, it is critical to remove TDS in order to make the water
fit for recycling back to the industrial processes. Samples will be
collected at the HERO™ system influent, effluent, and waste streams (SP-
A through SP-D) and analyzed for TDS according to EPA Method 160.1.
4.5.3.7 Oil & Grease (O&G)
Oil and grease are contributed to the wastewater as oily parts are rinsed.
The O&G is a combination of machining and cutting oils and coolants that
are used in metalworking. These fluids may contain mineral oils, natural
oils, fats and derivatives, or synthetic lubricants. O&G in the wastewater
must be removed before the water can be recycled to the process rinse
baths. Samples for total recoverable O&G (as HEM) will be collected at
the HERO™ system influent, effluent, and waste streams (SP-A through
SP-D), and analyzed for O&G (as HEM) by EPA Method 1664.
4.5.3.8 Metals
Certain contaminant metals will accumulate in the process rinse waters
based on the type of substrate being finished and the finishing processes.
Most of these metals will come from drag-out or drippage into the rinse
waters. These metals need to be removed before the water can be recycled
to the process rinse baths. Samples will be collected at the HERO™
system influent, effluent, and waste streams (SP-A through SP-D) and will
be analyzed according to EPA Method 200.7 for all metals except
mercury, which will be analyzed by EPA Method 245.1.
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For the 2nd WAC unit installed on the KCP CN wastewater stream, only
copper will be sampled and analyzed in the influent and effluent of this
unit (SP-E and SP-F).
4.5.3.9 Additional Proposed MP&M Limits
The proposed Metal Products & Machinery (MP&M) rule discharge limits
will have a major impact on the metal finishing industry. Fortunately for
the KCP, they are already monitoring their wastewater effluent for most of
the proposed MP&M contaminants. Installing the HERO™ system should
enable the KCP to recycle approximately 95 percent of their current
wastewater for reuse. The remaining five percent consist of the
regeneration waste from the ion exchange step and the waste brine
solution from the reverse osmosis step. These waste streams will be
commingled and tested for the standard contaminants that the KCP is
required to monitor for discharge to the sanitary sewer. In addition to
these standard contaminants, the waste stream will be tested for additional
contaminant parameters, which will require monitoring under the new
proposed MP&M limits for metal finishers. These new parameters for the
KCP are: manganese, molybdenum, tin, sulfide, total cyanide, TSS, and
total organic carbon (TOC). Samples will be taken at the HERO™ system
influent, effluent, and waste streams (SP-A through SP-D) (MP&M
metals: EPA Method 200.7; total cyanide: EPA Method 335.3; TSS: EPA
Method 160.2; TOC: SW-846 Method 9060; sulfide: EPA Method 376.1).
4.5.3.10 Additional KCP Recycled Water Quality Standards
KCP has stated that the recycled water from the HERO™ system should
be of a water quality that meets or exceeds the Kansas City tap water that
KCP currently used for rinse bath make-up, non-contact cooling water,
boiler water, etc. The Missouri Code of State Regulations (CSR),
Department of Natural Resources, Public Drinking Water Program,
Contaminant Levels and Monitoring Regulations (10 CSR Division 60 -
Chapter 4) sets forth the maximum allowable contaminant levels for
drinking water. It is to these standards that KCP would like to polish their
wastewater. Fortunately for the KCP, they are already monitoring their
wastewater effluent for most of the contaminants. The recycled water will
be tested for the following additional contaminant parameters that require
monitoring under the drinking water program: chloride, total residual
chlorine, sulfate, nitrate as N, fluoride, total alkalinity and dissolved silica.
Samples will be taken at the HERO™ system influent, effluent, and waste
streams (SP-A through SP-D) (chloride, fluoride, nitrate as N and sulfate:
EPA Method 300.0; total residual chlorine: EPA Method 330.5; total
alkalinity: EPA Method 310.1; dissolved silica: EPA Method 370.1).
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4.5.4 Calibration Procedures and Frequency
The following procedures will be used to calibrate the instruments/equipment that
will be used to collect critical measurements:
2) Instruments used to perform aqueous analytical methods will be calibrated
according to the laboratory quality assurance plan by Pace Analytical
Services.
3) The ultrasonic liquid flowmeter, used to measure the flow rate of liquids
within the HERO™ system, is on an annual calibration schedule. The
flowmeter is calibrated by the equipment manufacturer. The ETV-MF
Project Manager will verify the flowmeter has been calibrated prior to use.
An operational check will be conducted at the start of each sampling day,
and in accordance with the equipment manufacturer's instructions by the
ETV-MF Project Manager.
4) Wastewater temperature is not a controlled parameter; however, pH is
controlled throughout the conventional wastewater treatment system.
Temperature and pH measurements will be taken each time a sample is
drawn from its respective sampling port. The digital pH reader/temperature
probe will be calibrated at the start of each sampling day by the ETV-MF
Project Manager. The following calibration information will be collected
and recorded in the field notebook: buffer supplier, lot number, expiration
date, and date of usage.
5) Specific conductivity measurements will be taken each time a sample is
drawn from its respective sampling port. The digital conductivity meter will
be calibrated at the start of each sampling day by the ETV-MF Project
Manager. The following calibration information will be collected and
recorded in the field notebook: standard solution supplier, lot number,
expiration date, and date of usage.
6) Total residual chlorine measurements will be taken each time a sample is
drawn from its respective sampling port. The digital filter photometer has
been calibrated by the equipment manufacturer and is on an annual
recalibration schedule. The ETV-MF Project Manager will verify the
photometer meter has been calibrated prior to use.
4.5.5 Mass Balance
The conservation of mass/energy in any isolated system is one of the most
fundamental laws in science and engineering. The mass/energy balance is a tool
that was developed to account for the inputs, outputs, consumption, and
accumulation in a system. To determine system efficiency, measuring or
quantifying all of the elements for a mass balance in an industrial setting is very
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difficult. The greatest challenge is generally defining the system boundaries and
what degree of accuracy is required. Sampling, measurement, and analytical
errors preclude absolute precision; however, the mass/energy balance provides us
with a fundamental tool for evaluating the performance of environmental
technologies where we are generally evaluating some form of efficiency.
Figure 7 illustrates the most fundamental form of the material balance equation.
Batch systems and continuous systems can both be modeled using this general
form.
Mass
Accumulation
Within the
System
Equals
Mass Input
Through
System
Boundaries
Less
Mass Output
Through System
Boundaries
Plus
Mass
Generated
Within the
System
Less
Mass
Consumed
Within the
System
Figure 7: Fundamental Material Balance Equation
Figure 8 illustrates the material flow into and out of the KCP HERO™ system.
Wastewater
Influent
HERO™
System
Wastewater Effluent
Waste Brine Solution
Recovered Metals Solution
Figure 8: Material Balance Equation for KCP HERO™ System
The goal of the Hydrometrics HERO™ system verification project is to determine
performance, and this can generally be measured in terms of efficiency. For
water recovery technologies, percent contaminant removal and percent water
recovery are measures of system efficiency.
To determine efficiency, the fundamental material balance equation can be
simplified as:
where:
X,
Xw
Xe
X; — Xw + Xe
Mass in influent
Mass in waste
Mass in effluent
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Sampling will occur in the quantities listed in Table 2, at the frequency and
duration specified in Table 3. Historical operating records at the KCP indicate
that there is an average of 78 ppm of copper in the untreated cyanide-bearing rinse
water. At the current KCP flow rate, this equates to a potential 50 pounds of
copper recovered per year. Conventionally treated KCP wastewater meets current
sewer disposal limits, but is not recyclable due to elevated levels of sodium,
chloride, nitrates, sulfates, and zinc. The HERO™ system is designed to reduce
these contamination levels so that the treated water can be recycled. Four days of
sampling was selected in order to show the treatment of a significant volume of
wastewater at a steady contaminant-loading rate.
To determine the contaminant removal efficiency for any parameter, the material
balance equation for the KCP HERO™ system is expressed as:
where:
Ceff = Target contaminant removal efficiency
C; = Influent target contaminant concentration (mg/L)
IVoi = Influent volume processed during the test (L)
Ce = Effluent target contaminant concentration (mg/L)
Eyoi = Effluent volume processed during test (L)
The removal efficiency will be calculated on a daily basis.
4.5.6 Energy Use
Energy requirements for the HERO™ unit will be calculated by determining the
power requirements and cycle times of pumps and other powered devices. For
motors and pumps, summing the total quantity of horsepower hours and dividing
by 1.341 HP-hr/kWh will determine electrical consumption.
4.5.7 Cost Analysis
This analysis will quantify the accumulative cost benefit of the technology. The
cost of operating the mobile HERO™ unit at the KCP will be calculated for
comparison to operating costs for a time period prior to utilization of the unit.
Operating costs will then be extrapolated, using normalized data, for a full scale
HERO™ unit for treating all of the KCP's wastewater. Operating costs may be
offset by recovered metals, recycled water, and less waste requiring disposal. For
the baseline conditions, the most recent applicable data available, collected by the
KCP, will be used. The cost analysis will compare operating costs, including:
chemical costs and savings, waste treatment/disposal costs and savings, and costs
for labor, utilities, maintenance and other materials.
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4.5.8 Waste Generation Analysis
This analysis will quantify the environmental benefit of the technology. The
waste generation rates for operating the mobile HERO™ unit at the KCP will be
calculated and compared to waste generation rates for a time period prior to
utilization of the unit. Waste generation rates will then be extrapolated, using
normalized data, for a full scale HERO™ unit for treating all of the KCP's
wastewater. For the baseline conditions, the most recent applicable data
available, collected by the KCP, will be used. The waste generation analysis will
consider type/characteristics, volume, and frequency of waste generated.
5.0 QUALITY ASSURANCE/QUALITY CONTROL REQUIREMENTS
QA/QC activities will be performed according to the applicable sections of the
Environmental Technology Verification Program Metal Finishing Technologies Quality
Management Plan (ETV-MF QMP) [Ref. 3].
5.1 Quality Assurance Objectives
One QA objective is to ensure that the process operating conditions and test methods are
maintained and documented throughout each test and laboratory analysis of samples.
Another QA objective is to use standard test methods for laboratory analyses. The test
methods to be used are shown in Tables 3 & 4. The analytical methods that will be used
for analyzing the samples are standard EPA methods.
5.2 Data Reduction, Validation, and Reporting
5.2.1 Internal Quality Control Checks
Raw Data Handling. Raw data is generated and collected by laboratory analysts
at the bench and/or sampling site. These include original observations, printouts,
and readouts from equipment for sample, standard, and reference QC analyses.
Data is collected both manually and electronically. At a minimum, the date, time,
sample ID, instrument ID, analyst ID, raw signal or processed signal, and/or
qualitative observations will be recorded. Comments to document unusual or
non-standard observations also will be included on the forms, as necessary. Data
collected on-site will be recorded onto the form presented in Figure 6. The ETV-
MF Project Manager will complete COC forms that will accompany samples
during shipment to the respective labs. Raw data will be processed manually by
the analyst, automatically by an electronic program, or electronically after being
entered into a computer. The analyst will be responsible for scrutinizing the data
according to laboratory precision, accuracy, and completeness policies. Raw data
bench sheets and calculation or data summary sheets will be kept together for
each sample batch. From the standard operating procedure and the raw data
bench files, the steps leading to a final result can be traced. The CTC ETV-MF
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Program Manager (PM) will maintain process-operating data for use in report
preparation.
Data Package Validation. The generating analyst will assemble a preliminary
data package, which shall be initialed and dated. This package shall contain all
QC and raw data results, calculations, electronic printouts, conclusions, and
laboratory sample tracking information. A second analyst will review the entire
package and check sample and storage logs, standard logs, calibration logs, and
other files, as necessary, to ensure that all tracking, sample treatments, and
calculations are correct. After the package is reviewed in this manner, a
preliminary data report will be prepared, initialed, and dated. The entire package
and final report will be submitted to the Laboratory Manager (LM). The LM shall
be ultimately responsible for all final data released from the laboratory. The LM
or designee will review the final results for adequacy to the QA objectives. If the
manager or designee suspects an anomaly or non-concurrence with expected or
historical performance values, the raw data will be reviewed, and the generating
and reviewing analysts queried. If suspicion about data validity still exists after
internal review of laboratory records, the manager will authorize a re-test. If
sufficient sample is not available for re-testing, a re-sampling shall occur. If the
sampling window has passed, or re-sampling is not possible, the manager will flag
the data as suspect. The LM signs and dates the final data package.
Data Reporting. A report signed and dated by the LM will be submitted in
duplicate to the ETV-MF Project Manager and CTC Project Manager. The ETV-
MF Project Manager will decide the appropriateness of the data for the particular
application. The final report contains the laboratory sample ID, date reported,
date analyzed, the analyst, the method used for each parameter, the process or
sampling point identification, the final result, the units, and the quality control
sample results. The CTC QA Manager shall review the data packages as required
by the ETV-MF QMP [Ref 3]. The CTC ETV-MF Program Manager shall retain
the data packages as required by the ETV-MF QMP.
5.2.2 QA/QC Requirements
For those measurements where duplicates, spikes, and spike duplicates are
inappropriate (e.g., flow rate, pH, temperature, specific conductivity, total residual
chlorine and membrane flux) additional measurements will take place. A
minimum of three repetitions will be conducted for each measurement for each
sampling day in order to ensure compliance with the QA objectives stated in
Table 5. The instrument will be recalibrated if the objectives for these
measurements are not met.
5.2.2.1 Duplicates
Duplicate samples collected in the field will be used to quantify sample
representativeness associated with the entire sampling and analysis
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system. Duplicate samples (submitted as two aliquots) will be submitted
at least once during the test period. Duplicate samples will be collected
from both the influent and effluent of the HERO™ system during the
treatment of the combined wastewater and cyanide-bearing wastewater.
The duplicate samples will be analyzed for all analytical parameters listed
in Table 3.
5.2.2.2 Matrix Spikes
Matrix spike/spike duplicates will be performed at least once during the
test period for each applicable parameter. For example, several different
process streams will be sampled as shown in Table 3 (SP-A through SP-
F). Test parameters that can undergo matrix spike/spike duplicate
procedures are: TOC, O&G (as HEM), metals, and sulfide, sulfate,
fluoride, nitrate, chloride, dissolved silica and total cyanide (TSS, TDS,
and total alkalinity cannot undergo matrix spike/spike duplicate
procedures). A matrix spike/spike duplicate for each of these test
parameters will be performed on the duplicate sample for each sampling
point during the four-day sampling period. Sample splitting will occur at
the analytical laboratory with the exception of O&G (as HEM), which
requires additional bottles to be collected at the time of sampling in order
to provide enough sample to perform matrix spike/spike duplicate
procedures.
5.2.2.3 Field Blanks
Field blanks of laboratory-supplied deionized water will be prepared on-
site and submitted to the analytical laboratory during the verification test
period. The analysis of these samples for the normal test parameters
(TOC, TSS, TDS, O&G (as HEM), metals, and sulfide, sulfate, fluoride,
nitrate, chloride, dissolved silica, total cyanide and total alkalinity) will
ensure that (1) analytical equipment-cleaning protocols adequately remove
residual contamination from previous use, (2) sampling and sample-
processing procedures do not result in contamination, and (3) equipment
handling and transport between periods of sample collection do not
introduce contamination.
5.2.3 Calculation of Laboratory Data Quality Indicators
Analytical performance requirements are expressed in terms of precision,
accuracy, representability, comparability, completeness, and sensitivity
(PARCCS). Summarized below are definitions and QA objectives for each
PARCCS parameter.
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5.2.3.1 Precision
Precision is a measure of the agreement or repeatability of a set of
replicate results obtained from duplicate analyses made under identical
conditions. Precision is estimated from analytical data and cannot be
measured directly. The precision of a duplicate determination can be
expressed as the relative percent difference (RPD), and calculated as:
where:
RPD =
Xi = sample result
X2 = duplicate result
X,-X,
(X.+XJ
x 100%
Multiple determinations will be performed for each test on the same test
specimen. The replicate analyses must agree within the relative percent
deviation limits provided in Table 5.
5.2.3.2 Accuracy
Accuracy is a measure of the agreement between an experimental
determination and the true value of the parameter being measured.
Accuracy is estimated through the use of known reference materials or
matrix spikes. It is calculated from analytical data and is not measured
directly. Spiking of reference materials into a sample matrix is the
preferred technique because it provides a measure of the matrix effects on
analytical accuracy. Accuracy, defined as percent recovery (P), is
calculated as:
P =
(SSR-SR)
SA
xlOO%
where:
SSR = spiked sample result
SR = sample result
SA = the concentration added to the spiked sample
Analyses will be performed with periodic calibration checks with
traceable standards to verify instrumental accuracy. These checks will be
performed according to established procedures in the contracted laboratory
that have been acquired for the HERO™ system verification testing.
Analysis with spiked samples will be performed to determine percent
recoveries as a means of checking method accuracy. QA objectives are
satisfied if the average recovery is within the goals described in Table 5.
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5.2.3.3 Comparability
Comparability is another qualitative measure designed to express the
confidence with which one data set may be compared to another. Sample
collection and handling techniques, sample matrix type, and analytical
method all affect comparability. Comparability is limited by the other
PARCCS parameters because data sets can be compared with confidence
only when precision and accuracy are known. Comparability will be
achieved in the HERO™ technology verification by the use of consistent
methods during sampling and analysis and by traceability of standards to a
reliable source.
5.2.3.4 Completeness
Completeness is defined as the percentage of measurements judged to be
valid, compared to the total number of measurements made for a specific
sample matrix and analysis. Completeness is calculated using the
following formula:
_ , Valid Measurements .,„„„.
Completeness = x 100%
Total Measurements
Experience on similar projects has shown that laboratories typically
achieve about 90 percent completeness. QA objectives will be satisfied if
the percent completeness is greater than the value specified in Table 5.
5.2.3.5 Representativeness
Representativeness refers to the degree to which the data accurately and
precisely represents the conditions or characteristics of the parameter
represented by the data. For the purposes of this demonstration,
representativeness will be achieved by presenting identical samples (field
duplicates) to the specified lab(s) and executing consistent sample
collection and mixing procedures. Three identical samples (one each of
influent, effluent, and sludge) will be collected during the course of the
verification test. Representativeness will be satisfied if the analytical
results for each parameter is less than 30 percent of the results for the
associated duplicate sample.
5.2.3.6 Sensitivity
Sensitivity is the measure of the concentration at which an analytical
method can positively identify and report analytical results. The
sensitivity of a given method is commonly referred to as the detection
limit. Although there is no single definition of this term, the following
terms and definitions of detection will be used for this program.
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Instrument Detection Limit (IDL) is the minimum concentration that can
be measured from instrument background noise.
Method Detection Limit (MDL) is a statistically determined
concentration. It is the minimum concentration of an analyte that can be
measured and reported with 99 percent confidence that the analyte
concentration is greater than zero as determined in the same or a similar
matrix. (Because of the lack of information on analytical precision at this
level, sample results greater than the MDL but less than the method
reporting limit (MRL) will be flagged).
MDL is defined as follows for all measurements:
MDL=t(n.u.a = 0.9
where:
MDL = method detection limit
t(n-i,i-a = o.99) = students t-value for a one-sided 99 percent
confidence level and a standard deviation
estimate with n-1 degrees of freedom
s = standard deviation of the replicate analyses
Method Reporting Limit (MRL) is the concentration of the target analyte
that the laboratory has demonstrated the ability to measure within
specified limits of precision and accuracy during routine laboratory
operating conditions. (This value is variable and highly matrix-dependent.
It is the minimum concentration that will be reported as "unqualified" by
the laboratory).
5.3 Quality Audits
Technical System Audits. An audit will be performed during verification testing by the
CTC QA Manager according to section 2.9.3 Technical Assessments of the ETV-MF
QMP [Ref. 3] to ensure testing and data collection are performed according to the test
plan requirements. In addition to the CTC Technical System Audit (TSA), the EPA QA
Manager will also conduct an audit to assess the quality of the verification test.
Internal Audits. In addition to the internal laboratory quality control checks, internal
quality audits will be conducted to ensure compliance with written procedures and
standard protocols.
Data Quality Assessments. The CTC QA Manager will also perform data quality
(statistical) assessments on data collected during the analysis of one metal and one anion.
Corrective Action. Corrective Action for any deviations to established quality assurance
and quality control procedures during verification testing will be performed according to
section 2.10 Quality Improvement of the ETV-MF QMP [Ref. 3].
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Laboratory Corrective Action. Examples of non-conformances include invalid
calibration data, inadvertent failure to perform method-specific QA, process control data
outside specified control limits, failed precision and/or accuracy indicators, etc. Such
non-conformances will be documented on a standard laboratory form. Corrective action
will involve taking all necessary steps to restore a measuring system to proper working
order and summarizing the corrective action and results of subsequent system
verifications on a standard laboratory form. Some non-conformances are detected while
analysis or sample processing is in progress and can be rectified in real time at the bench
level. Others may be detected only after a processing trial and/or sample analysis is
completed. Typically, the LM detects these types of non-conformances. In all cases of
non-conformance, the LM will consider sample re-analysis as one source of corrective
action. The LM will contact the ETV-MF Project Manager if reanalysis does not correct
the non-conformance. If insufficient sample is available or the holding time has been
exceeded, complete re-processing may be ordered to generate new samples if a
determination is made by the ETV-MF Project Manager that the non-conformance
jeopardizes the integrity of the conclusions to be drawn from the data. In all cases, a non-
conformance will be rectified before sample processing and analysis continues.
6.0 PROJECT MANAGEMENT
6.1 Organization/Personnel Responsibilities
The ETV-MF Project Team that is headed by CTC will conduct the evaluation of
Hydrometrics' HERO™ system. The CTC ETV-MF Program Manager, Donn Brown,
will have responsibility for all aspects of the technology verification, including
appointment of a Project Manager, making ETV-MF Project Team personnel
assignments, and coordination of technology testing. The ETV-MF Project Manager
assigned to the HERO™ verification is Chris Start of the Michigan Manufacturing
Technology Center (MMTC). MMTC is one of four partner organizations under contract
to CTC for the ETV-MF Program. Mr. Start and/or his staff/subcontractors will conduct
or oversee all sampling and related measurements, and ensure that required laboratory
QC analyses (spikes/duplicates) are performed.
Hydrometrics will arrange transport of the mobile HERO™ unit to the test site.
Hydrometrics will perform start-up. Once the system is performing per the design
objectives, verification testing will commence. Hydrometrics personnel will continue to
operate the system. A Hydrometrics representative (Steve Ackerlund) will assist in
verification testing of the HERO™ system and will be on-call during the test period for
response in the event of equipment problems.
Pace Analytical Services is responsible for performing aqueous chemical analysis of all
samples taken during the verification test. Pace Analytical Services is accredited by
NELAC for the analyses identified in this Test Plan. Jim Dowse is the Pace Analytical
Services point of contact (POC).
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The ETV-MF Project Manager and the KCP have the authority to stop work when unsafe
or unacceptable quality conditions arise. The CTC ETV-MF PM will provide periodic
assessments of verification testing to the EPA ETV Center Manager.
6.2 Test Plan Modifications
In the course of verification testing, it may become necessary to modify the test plan due
to unforeseen events. These modifications will be documented using a Test Plan
Modification Request form (Appendix D), which must be submitted to the CTC ETV-
MF Program Manager for approval. Upon arrival, the modification request will be
assigned a number, logged, and transmitted to the requestor for implementation.
6.3 Schedule/Milestones
The schedule/milestones will be determined mutually by CTC, Hydrometrics, and KCP.
6.4 Documentation/Records
Original documentation generated during verification testing (COC forms, data collection
forms, analytical results, etc.) will be maintained at the CTC office in Largo, Florida.
7.0 EQUIPMENT
7.1 Equipment List and Utility Requirements
The FtERO™ 15 gpm unit consists of the following equipment:
Prefiltration System: 20-micron bag filter (with in-line spare) followed by a 36"
diameter by 84" tall multi-media depth filter. These filters are fed by a 5-hp totally
enclosed fan-cooled (TEFC) pump that produces approximately 20 gpm at 50 pounds per
square inch (psi) during normal operation, and 100 gpm at 45 psi when cleaning the
multi-media filter. Filtered solids are periodically back-washed to the clarifier, where
they are removed.
SAC System: 36" diameter by 84" tall pressure vessel containing 20 cubic feet (ft3) of
SAC resin (with in-line spare). This vessel is regenerated using a salt brine while the in-
line spare is in operation.
WAC System (x2): The HERO™ unit contains a pressure tank containing 10 ft3 of WAC
resin and can be piped for either up-flow or down-flow operation. The copper recovery
WAC ion exchange unit will be installed at KCP adjacent to the cyanide rinse water
holding tank.
Degasification System: This portion of the FtERO™ unit consists of two 4" by 28"
Celgard Liqui-Cel Membrane Contractors, which can be operated either in series or
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parallel. Air for these strippers is provided by a 1-1/2 hp compressor and exits through a
stack above the roof of the mobile HERO™ trailer.
RO System: The HERO™ unit RO system consists of five stages of 120" pressure
vessels, each containing three or four membranes. The first stage consists of two 4"
vessels rated for 600 psi and is fed by a 10-hp open drip-proof (ODP) pump. The reject
from the first stage is fed to the second stage (a single 4" vessel rated for 600 psi). The
third stage consists of a single 4" pressure vessel rated for 1000 psi and is fed via another
10-hp ODP booster pump. The fourth and fifth stages each consist of a single 2.5"
pressure vessel rated for 1000 psi. The permeate from each pass is combined in a single
stream with a flow of approximately 15 gpm. The reject from the fifth pass is
approximately 1 gpm. Equipment and utility requirements are identified in Table 6.
EQUIPMENT
Number Req'd
1
1
1
1
2
2
1
3
2
1
2
Type of Equipment
Prefilter System
20-micron bag filter
Multi-media depth filter
Pump - 5 hp TEFC
SAC System
Pressure vessel w/ 20 ft3 of SAC resin
WAC System(s)
Pressure vessels w/ 15 ft3 of WAC resin
Degasification System
Celgard Liqui-Cel Membrane Contractors
Air compressor
RO System
4 Pressure vessels w/ 4 membranes
Pumps- 10 hp ODP
4 Pressure vessel w/ 4 membranes
2.5 Pressure vessels w/ 3 membranes
Comments
Contains in-line spare
36 diameter by 84 tall
Normal=20 gpm @ 50 psi; Cleaning=100
gpm @ 45 psi
36 diameter by 84 tall; contains in-line
spare
Can be piped for either up-flow or down-flow operation
4 x 28 each; can be operated either in series or parallel
1-1/2 hp
Rated for 600 psi
Rated for 1,000 psi
Rated for 1,000 psi
SPARE PARTS
12
4
6
4
2
10
4 Brackish water RO membranes
4 Seawater RO membranes
2.5 Seawater RO membranes
5 -micron cartridge filters (set + spare)
1 -micron cartridge filters
20-micron bag filters
Required Utilities
Utilities to include: Electrical • Automated control panel: 50 amp, 480 volt, 3-phase, 60 Hz Air
• Liquid transfer pumps: 110 VAC Water
• None
• None
Table 6: Equipment List and Utility Requirements
7.2 Monitoring/Sampling Equipment
All monitoring/sampling equipment to be used during testing is identified in Table 7.
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Equipment
Omega Engineering, Inc. Model FD-7000 Multi-Liquid
Ultrasonic Flowmeter
Davis Instruments Model #9214 ATC pH Meter with
Integral Temperature Sensor
Oakton Acorn® Series CON 5 Conductivity Meter with
Integral Temperature Sensor
Hach® Pocket Colorimeter™ Filter Photometer with Total
Chlorine Reagent Set
Purpose
Flow of System Liquids
Process pH and Temperature
Process Specific Conductivity
Process Total Residual Chlorine
Table 7: Monitoring/Sampling Equipment
8.0 HEALTH AND SAFETY PLAN
This Health and Safety Plan provides guidelines for recognizing, evaluating, and
controlling health and physical hazards that could occur during verification testing. More
specifically, the Plan specifies for assigned personnel; the training, materials, and
equipment necessary to protect them from hazards; and any waste generated. The KCP
Hazcom/Personal Protective Equipment (PPE) Plan/Program will be used throughout the
HERO™ verification testing for any activities related to the conventional wastewater
treatment system that operates at the KCP. For activities involving the HERO™ system,
Hydrometrics will provide operating procedures and all associated health and safety
plans/procedures.
8.1 Hazard Communication
All personnel assigned to the project will be provided with the potential hazards, signs
and symptoms of exposure, methods or materials to prevent exposures, and procedures to
follow if there is contact with a particular substance during verification testing. Hazard
communication will take place during training and will be reinforced throughout the test
period. All appropriate Material Safety Data Sheets (MSDSs) will be available for the
chemical solutions used during the testing.
8.2 Emergency Response Plan
The KCP has a contingency plan to protect employees, assigned project personnel, and
visitors in the event of an emergency at the facility. This plan will be used throughout the
project. All assigned personnel will be provided with information about the plan during
training.
8.3 Hazard Controls Including Personal Protective Equipment
All assigned project personnel and visitors will be provided with appropriate PPE and
any training needed for its proper use, considering their assigned tasks. The use of PPE
will be covered during training.
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8.4 Lockout/Tagout Program
The KCP's lockout/tagout procedure will be implemented when necessary and will be
explained to anyone required to perform such duties. Equipment installation performed
by Hydrometrics and the KCP is not included within the scope of this test plan. No
lockout/tagout activities are anticipated during the verification test.
8.5 Material Storage
Any materials used during the project will be kept in proper containers and labeled
according to Federal and state law. Proper storage of the materials will be maintained
based on associated hazards. Secondary containment, spill trays, or similar devices will
be used as needed to prevent material loss to the surrounding area.
8.6 Safe Handling Procedures
All chemicals and wastes or samples will be transported on-site in non-breakable
containers used to prevent spills. Emergency spill clean-up will be performed according
to the KCP procedures.
9.0 WASTE MANAGEMENT
The HERO™ system will process wastewater generated by manufacturing operations at
the KCP. Prior to processing by the HERO™ system, the wastewater will be treated by
the conventional wastewater treatment system at the KCP. After treatment by the
HERO™ system, the wastewater will be returned to the conventional wastewater
treatment system. The existing wastewater treatment system is fully permitted, and
achieves compliance with discharge requirements in accordance with local, state, and
Federal laws. Hydrometrics says the reagents to be added to the HERO™ process during
verification test will increase the TDS, but they will not upset existing clarifier
operations. Hydrometrics will retain any unused acid or caustic.
10.0 TRAINING
It is important that the verification activities performed by the ETV-MF Center be
conducted with high quality and with regard to the health and safety of the workers and
the environment. By identifying the quality requirements, worker safety and health, and
environmental issues associated with each verification test, the qualifications or training
required for personnel involved can be identified. Training requirements will be
identified using the Job Training Analysis (JTA) Plan [Ref. 4].
The purpose of the JTA Plan is to outline the overall procedures for identifying the
hazards, quality issues, and training needs for each verification test project. The JTA
Plan establishes guidelines for creating a work atmosphere that meets the quality,
environmental, and safety objectives of the ETV-MF Center. The JTA Plan describes the
method for studying ETV-MF project activity and identifying training needs. The ETV-
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MF Operation Planning Checklist (Appendix A) will be used as a guideline for
identifying potential hazards, and the JTA Form (Appendix B) will be used to identify
training requirements. After completion of the form, applicable training will be
performed. Training will be documented on the ETV-MF Project Training Attendance
Form (Appendix C).
11.0 REFERENCES
1) Thomas J. Weber, Wastewater Management Inc., "Wastewater Treatment" Metal
Finishing Guidebook and Directory Issue, 1999, pg. 801.
2) U.S. EPA Office of Environmental Information, "Guidance for the Data Quality
Objectives Process EPA QA/G-4", EPA/600/R-96/055, August 2000.
3) Concurrent Technologies Corporation (CTC), "Environmental Technology
Verification Program Metal Finishing Technologies (ETV-MF) Quality
Management Plan" Revision 1, March 26, 2001.
4) Concurrent Technologies Corporation (CTC), "Environmental Technology
Verification Program Metal Finishing Technologies (ETV-MF) Pollution
Prevention Technologies Pilot Job Training Analysis Plan" May 10, 1999.
5) US EPA Office of Research and Development, "Waste Reduction in the Metal
Fabricated Products Industry" EPA/600/SR-93/144, September 1993.
6) George C. Cushnie Jr., CAI Engineering, "Pollution Prevention and Control
Technology for Plating Operations" NCMS/NAMF, 1994.
12.0 DISTRIBUTION
Alva E. Daniels, EPA (3)
W. Steve Ackerlund, Hydrometrics, Inc.
Don J. Fitzpatrick, Honeywell FM&T - KCP
Chris L. Start, MMTC (2)
Donn W. Brown, CTC (2)
Clinton E. Twilley, CTC
Scott W. Maurer, CTC
Jim Dowse, Pace Analytical Services, Inc.
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APPENDIX A
ETV-MF Operation Planning Checklist
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ETV-MF OPERATION PLANNING CHECKLIST
The ETV-MF Project Manager prior to initiation of verification testing must complete this form.
If a "yes " is checked for any items below, an action must be specified to resolve the concern on
the Job Training Analysis Form.
Proj ect Name:
ETV-MF Project Manager:
Expected Start Date:
Will the operation or activity involve the following:
Yes No
Initials & Date
Completed
Equipment requiring specific, multiple steps for controlled shutdown?
(e.g., in case of emergency, does equipment require more than simply
pressing a "Stop" button to shut off power?) Special Procedures for
emergency shut-down must be documented in Test Plan.
Equipment requiring special fire prevention precautions? (e.g., Class D fire
extinguishers)
Modifications to or impairment of building fire alarms, smoke detectors,
sprinklers, or other fire protection or suppression systems?
Equipment lockout/tagout or potential for dangerous energy release?
Lockout/layout requirements must be documented In Test Plan.
Working in or near confined spaces (e.g., tanks, floor pits) or in cramped
quarters?
Personal protection from heat, cold, chemical splashes, abrasions, etc.? Use
Personal Protective Equipment Program specified in Test Plan.
Airborne dusts, mists, vapors and/or fumes? Air monitoring, respiratory
protection, and /or medical surveillance may be needed.
Noise levels greater than 80 decibels? Noise surveys are required.
Hearing protection and associated medical surveillance may be necessary.
X-rays or radiation sources? Notification to the state and exposure
monitoring may be necessary.
Welding, arc/torch cutting, or other operations that generate flames and/or
sparks outside of designated weld areas? Follow Hot Work Permit
Procedures identified in Test Plan.
The use of hazardous chemicals? Follow Hazard Communication
Program, MSDS Review for Products Containing Hazardous Chemicals.
Special training on handling hazardous chemicals and spill clean-up may
be needed. Spill containment or local ventilation may be necessary.
Working at a height of six feet or greater?
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ETV-MF OPERATION PLANNING CHECKLIST
The ETV-MF Project Manager prior to initiation of verification testing must complete this form.
If a "yes " is checked for any items below, an action must be specified to resolve the concern on
the Job Training Analysis Form.
Proj ect Name:
ETV-MF Project Manager:
Will the operation or activity involve the following:
Yes No
Initials & Date
Completed
Processing or recycling of hazardous wastes? Special permitting may be
required.
Generation or handling of waste?
Work to be conducted before 7:00 a.m., after 6:00 p.m., and/or on
weekends? Two people must always be in the work area together.
Contractors working in CTC facilities? Follow Hazard Communication
Program.
Potential discharge of wastewater pollutants?
EHS aspects/impacts and legal and other requirements identified?
Contaminants exhausted either to the environment or into buildings?
Special permitting or air pollution control devices may be necessary.
Any other hazards not identified above? (e.g., lasers, robots, syringes)
Please indicate with an attached list.
The undersigned responsible party certifies that all applicable concerns have been indicated in
the "yes" column, necessary procedures will be developed, and applicable personnel will receive
required training. As each concern is addressed, the ETV-MF Project Manager will initial and
date the "initials & date completed" column above.
ETV-MF Project Manager:
(Name)
(Signature)
(Date)
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APPENDIX B
Job Training Analysis Form
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JOB TRAINING ANALYSIS FORM
ETV-MF Project Name:
Basic Job Step
Potential EHS Issues
Potential Quality
Issues
Training
ETV-MF Project Manager:
Name
Signature
Date
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APPENDIX C
ETV-MF Project Training Attendance Form
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ETV-MF Project Training Attendance Form
ETV-MF Pilot Project:
Date
Training
Completed
Employee Name
Last First
Training Topic
ETV-MF Project Manager:
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APPENDIX D
Test Plan Modification
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Test Plan Modification
In the course of verification testing, it may become necessary to modify the test plan due to
unforeseen events. The purpose of this procedure is to provide a vehicle whereby the necessary
modifications are documented and approved.
The Test Plan Modification Request form is the document to be used for recording these
changes. The following paragraphs provide guidance for filling out the form to ensure a
complete record of the changes made to the original test plan.
The person requesting the change should record the date and project name in the form's heading.
The CTC ETV-MF PM will provide the request number.
Under "Original Test Plan Requirement," reference the appropriate sections of the original test
plan, and insert the proposed modifications in the section titled "Proposed Modification." In the
"Reason" section, document why the modification is necessary; this is where the change is
justified. Under "Impact," give the impact of not making the change, as well as the
consequences of making the proposed modification. Among other things, the impact should
address any changes to cost estimates and project schedules.
The requestor should then sign the form and obtain the signature of the ETV-MF Project
Manager (Partner). The ETV-MF Project Manager (Partner) should sign both lines if he is the
requestor. The form should then be transmitted to the CTC ETV-MF PM, who will either
approve the modification or request clarification. Upon approval, the modification request will
be assigned a number, logged, and transmitted to the requestor for implementation.
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TEST PLAN MODIFICATION REQUEST
Date: Number: Project:
Original Test Plan Requirement:
Proposed Modification:
Reason:
Impact:
Approvals:
Requestor:
ETV-MF Project Manager:
CTC ETV-MF Program Manager:
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